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Nov 1985

Volume 3, Issue 6, pp. 2077-2707


The growth of thin oxides on a‐Si and a‐Si:H in an O2 plasma

R. W. Collins, C. J. Tuckerman, C.‐Y. Huang, and H. Windischmann

J. Vac. Sci. Technol. A 3, 2077 (1985); http://dx.doi.org/10.1116/1.572927 (5 pages) | Cited 4 times

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We have used in situ and spectroscopic ellipsometry measurements to study the growth of thin oxide layers on the surface of both unhydrogenated and hydrogenated amorphous silicon (a‐Si and a‐Si:H) using an oxygen rf discharge. Spectroscopic ellipsometry data were taken on samples both before and after oxide growth to derive the maximum information about the surface structure of the films. In situ single wavelength ellipsometry measurements taken during plasma oxidation showed that the growth curves were nearly identical for glow discharge a‐Si:H and both ion‐beam sputtered a‐Si and a‐Si:H. The initial stages of oxide growth could not be easily fit to a model of uniform or planar growth, probably because of a surface modulation or roughness which exists on the film before growth. Further growth appeared to follow, or at least approach, a layer‐by‐layer process. The thickness of the surface roughness layer on the a‐Si:H before growth matched that observed at the oxide/a‐Si:H interface after growth. For oxide thicknesses greater than 10–20 Å, the growth rate is consistent with a diffusion limited model. Under our plasma conditions, the diffusion coefficient of the plasma species through the oxide is 2.1×10−17 cm2/s for all samples.
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81.65.-b Surface treatments
68.55.-a Thin film structure and morphology

On the nature of oxides on InP surfaces

G. Hollinger, E. Bergignat, J. Joseph, and Y. Robach

J. Vac. Sci. Technol. A 3, 2082 (1985); http://dx.doi.org/10.1116/1.572928 (7 pages) | Cited 47 times

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The chemical composition of surface oxides grown on InP is investigated using x‐ray photoelectron spectroscopy. Native oxides prepared by various chemical treatments, anodic oxides, and thermal oxides are examined. Core level energies and intensities and valence band spectra are compared with data for standard compounds. In a first step we show that, depending on the preparation procedure, oxides can be classified into three groups which have properties similar to crystalline In(OH)3, InPO4, and In(PO3)3, respectively. The large variations observed in atomic compositions and the shape of valence band spectra suggest that the oxides could be amorphous nonstoichiometric phases. A description based on a mixture of well defined compounds (e.g., In2O3+P2O5 or In2O3+InPO4) seems to be inadequate. Chemical and anodic phosphorus‐rich oxides are identified as Inx(PO3)y polyphosphates.
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81.65.-b Surface treatments
68.60.-p Physical properties of thin films, nonelectronic
71.20.Nr Semiconductor compounds
71.20.Ps Other inorganic compounds
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties

A computer model for postdeposition annealing of porous thin films

Karl‐Heinz Müller

J. Vac. Sci. Technol. A 3, 2089 (1985); http://dx.doi.org/10.1116/1.572929 (4 pages) | Cited 10 times

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The changes that a porous thin film undergoes during annealing are studied by means of a two‐dimensional computer simulation. The model allows a detailed investigation of thermally activated hopping processes, which result in the migration of excess vacancies and smaller voids quenched‐in during film formation. To simulate fluctuations in vibrational energy, Boltzmann‐ordered statistics are used. For thin gold film the coalescence of vacancies, their merging with preexisting voids, and the deterioration in adhesion due to the potential diffusion of vacancies to the film–substrate interface are predicted.
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81.40.Ef Cold working, work hardening; annealing, post-deformation annealing, quenching, tempering recovery, and crystallization
66.30.J- Diffusion of impurities
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

Deposition of conducting thin films of organometallic monomers by plasma polymerization

R. K. Sadhir and H. E. Saunders

J. Vac. Sci. Technol. A 3, 2093 (1985); http://dx.doi.org/10.1116/1.572930 (5 pages) | Cited 3 times

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There has been a growing interest in depositing metal‐containing thin films by plasma polymerization for various applications. These films have been deposited by two methods (a) by plasma polymerization of volatile organometallic monomers, and (b) by simultaneous plasma etching and polymerization in the same system, resulting in metal‐containing fluoropolymers. Heretofore, most films so deposited have had low metal to carbon ratios and are insulating in nature. In our laboratories, we have been working on the plasma polymerization of volatile organometallic monomers with an aim to producing conducting films. We have observed that there is a critical threshold value of metal to carbon composition above which the films become electrically conductive. The key to depositing films having higher metal to carbon ratios is the plasma conditions. In this paper, we will review the work in our laboratories on plasma polymerization of organometallic monomers and discuss the preparation and properties of organotin monomers with various tin to carbon ratios. We will also discuss some of our recent results on plasma polymerization of an organoiron monomer. These films have been characterized by ESCA, IR, SEM, TEM, and x‐ray diffractograms.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
82.35.-x Polymers: properties; reactions; polymerization
68.60.-p Physical properties of thin films, nonelectronic

Transition metal containing plasma polymers

N. Morosoff, R. Haque, S. D. Clymer, and A. L. Crumbliss

J. Vac. Sci. Technol. A 3, 2098 (1985); http://dx.doi.org/10.1116/1.572931 (4 pages) | Cited 1 time

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The plasma polymerization of the C2 hydrocarbons in the presence of Fe(CO)5 vapor can lead to the formation of soluble cluster complexes (I) and/or high oxidation state iron both in the form of the oxide (II) and associated with the carboxylate or β‐diketonate ion (III). Analysis of the electron spectroscopy for chemical analysis (ESCA) spectra obtained yields information regarding the nature of I on the one hand, and regarding the prevalence of II relative to III, on the other. The relative yield of I with respect to (II+III) can be controlled, at will, by variation of W/F. This permits control of the coating’s morphology (continuity) as shown by the electrodeposition of Prussian blue on smooth surfaces coated with plasma polymer containing I+II+III.
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82.35.-x Polymers: properties; reactions; polymerization
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
68.55.-a Thin film structure and morphology
36.20.Hb Configuration (bonds, dimensions)

Secondary ion mass spectrometry/digital imaging for the three‐dimensional chemical characterization of solid state devices

S. R. Bryan, W. S. Woodward, R. W. Linton, and D. P. Griffis

J. Vac. Sci. Technol. A 3, 2102 (1985); http://dx.doi.org/10.1116/1.573263 (6 pages) | Cited 5 times

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The use of a microcomputer based digital imaging system for automated acquisition of secondary ion image depth profiles is demonstrated. By combining the ion microscope’s capabilities of elemental imaging and depth profiling, image depth profiling provides information on the three‐dimensional distribution of elements within microvolumes of the near surface region of solids. The technique is used for the three‐dimensional multielement characterization of a solid state device (a npn bipolar transistor). Several methods for processing and displaying the multidimensional data are presented.
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07.78.+s Electron, positron, and ion microscopes; electron diffractometers
07.05.Hd Data acquisition: hardware and software
07.05.Kf Data analysis: algorithms and implementation; data management
07.05.Rm Data presentation and visualization: algorithms and implementation
85.30.De Semiconductor-device characterization, design, and modeling
85.30.Pq Bipolar transistors

Auger electron spectroscopy and sputter/Auger analyses of thin films of SiCx

P. Morgen, K. L. Seaward, and T. W. Barbee

J. Vac. Sci. Technol. A 3, 2108 (1985); http://dx.doi.org/10.1116/1.573262 (8 pages) | Cited 5 times

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Thin SiCx films, fabricated in a two‐source sputtering apparatus, are analyzed with Auger electron spectroscopy in combination with inert gas (Ne) sputtering. The compositional depth profiles and local bonding properties of the films are the object of the analysis. Different aspects of the application of Auger electron spectroscopy and sputtering to SiC are critically evaluated. These include the chemical information available from the structure of the Auger spectral lines from C and Si, and the effects of ion bombardment, i.e., preferential sputtering, radiation induced diffusion and segregation, as well as disorder. The samples all contain cubic (polycrystalline) SiC( β‐SiC). The films are found to be homogeneous in the bulk, with a thin layer at the surface strongly enriched in carbon. A film with a high percentage of Si was found to be inhomogeneous, and to have a significant amount of SiO2 formed at the surface during storage and handling in a room ambient. The films with higher surface concentrations of carbon clearly showed less tendency to form oxides. Chemical information relating to the local bonding of Si and C is obtained from the Si(L23VV) and C (KVV) Auger spectra. The Si (KLL) Auger spectrum is also included in the discussion. Here a comparison with pure silicon allows assignment of plasmon loss structures, as well as shifts in peak energies.
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68.60.-p Physical properties of thin films, nonelectronic
61.80.Jh Ion radiation effects
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)

Surface analysis of TiC coated graphite limiters exposed to JIPPT‐II

K. Kamada, Y. Hori, N. Sugiyama, K. Akaishi, N. Noda, S. Tanahashi, J. Fujita, S. Yamaguchi, N. Fujimori, and A. Doi

J. Vac. Sci. Technol. A 3, 2116 (1985); http://dx.doi.org/10.1116/1.573264 (5 pages)

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Titanium carbide (TiC) coated carbon limiters, which suffered 1972 shots of tokamak discharge and 672 shots of stellarator discharge in JIPPT‐II for about 3 months, are analyzed by AES and RBS. The stoichiometry and composition of a subsurface layer is found to be affected by the plasma exposure. In this region a large amount of oxygen and nitrogen are observed. These concentration profiles and the subsurface layer affected have systematic positional dependencies on the limiter, suggesting an inhomogeneous interaction between the plasma and limiter. The analysis of RBS data gave roughly 0.4 and 0.2 C and Ti atoms, respectively, being sputtered off for every impinging O atom.
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52.40.Hf Plasma-material interactions; boundary layer effects
52.55.Jd Magnetic mirrors, gas dynamic traps
68.60.-p Physical properties of thin films, nonelectronic
81.05.Je Ceramics and refractories (including borides, carbides, hydrides, nitrides, oxides, and silicides)
81.65.-b Surface treatments

Stress modification of WSi2.2 films by concurrent low energy ion bombardment during alloy evaporation

D. S. Yee, J. Floro, D. J. Mikalsen, J. J. Cuomo, K. Y. Ahn, and D. A. Smith

J. Vac. Sci. Technol. A 3, 2121 (1985); http://dx.doi.org/10.1116/1.573265 (8 pages) | Cited 4 times

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The effect of ion bombardment on alloy film stress was studied by coevaporating W and Si in the presence of 100 and 400 eV Ar+ ion bombardment at room temperature, 350 and 500 °C. In the absence of ion bombardment, internal stress increases and becomes more tensile as deposition temperature increases. At room temperature, increasing ion bombardment causes the stress to go from tensile to compressive. At 350 °C tensile stress increases as a function of ion flux and decreases slightly at higher flux value. At 500 °C, the effect on stress due to ion bombardment is less pronounced. The correlation between the effect of ion bombardment on stress, deposition temperature, and the structure of the material is discussed using the concept of enhanced surface diffusion and local atomic rearrangement as a mechanism responsible for ion beam stress modification. By using this mechanism, we explain the diminished effect of ion bombardment on stress in the WSi2 films that contain compound phases compared to the amorphous WSi2 in which ion bombardment is more effective. We also attribute this diminished effect of ion bombardment to the more dominant effect of stress due to phase transformation occurring during deposition. The effect of improving the crystalline order and increasing the grain size due to ion bombardment has also been observed. The modification of stress during deposition has been found to have no consequence on the internal stress obtained after 1000 °C postdeposition annealing.
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61.80.Jh Ion radiation effects
68.60.-p Physical properties of thin films, nonelectronic
66.30.-h Diffusion in solids
68.55.-a Thin film structure and morphology

High rate reactive magnetron sputtered tungsten carbide films

P. K. Srivastava, V. D. Vankar, and K. L. Chopra

J. Vac. Sci. Technol. A 3, 2129 (1985); http://dx.doi.org/10.1116/1.573266 (6 pages) | Cited 5 times

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Tungsten carbide films have been deposited on stainless steel substrates held between 300 to 500 °C in a planar rf magnetron sputtering system at rates as high as that of pure tungsten (825 A°/min). The effect of substrate temperature on formation of WCx films has been investigated. A mixture of hexagonal WC, A‐15 W3C and carbon in graphitic and diamond form have been observed by AES and XRD techniques. The microhardness of these films has been found to be as high as 2365 kgf/mm2. The adhesion of these films as measured from indentation crack patterns has been found to depend on substrate temperature as well as on the amount of dispersed carbon in the film.
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81.15.Cd Deposition by sputtering
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

Magnetic field effects in the plasma‐enhanced chemical vapor deposition of boron nitride

T. H. Yuzuriha, W. E. Mlynko, and D. W. Hess

J. Vac. Sci. Technol. A 3, 2135 (1985); http://dx.doi.org/10.1116/1.573267 (6 pages) | Cited 6 times

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The effect of a low intensity magnetic field on the deposition rate of boron nitride films in a parallel plate plasma reactor was investigated. Operating impedance bridge measurements and optical emission spectroscopy were used to characterize the rf glow discharge consisting of diborane, ammonia, and hydrogen. The deposition rate was greater with the applied magnetic field at pressures below 400 mTorr, while at pressures above this value, the deposition rate was higher without magnetic field enhancement. These effects appear to be due to the change in ion flux and energy upon the application of the magnetic field.
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81.15.Gh Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)
52.80.Hc Glow; corona

Effects of charge neutralization on ion‐beam‐deposited boron nitride films

Ward Halverson and Dennis T. Quinto

J. Vac. Sci. Technol. A 3, 2141 (1985); http://dx.doi.org/10.1116/1.573268 (6 pages) | Cited 6 times

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Thin films of ion‐beam‐deposited boron nitride (i‐BN) were formed on various substrates from an ion source operating with borazine (B3N3H6). Without space charge neutralization of the beam, the films were severely damaged, with indications of melting, cracking, and delamination. Surface (‘‘Malter’’) discharges were visible in the deposition chamber; surface charging caused tracking and puncture through the dielectric i‐BN film. With charge neutralization, the Malter discharges ceased and the films became smooth, uniform and adherent. The neutralizing electrons prevented the buildup of surface charge on the i‐BN film and stopped the damage from surface discharges; the bulk properties of the films apparently were not affected by the neutralization. The films were close to stoichiometric BN with typically 2–7 at. % of C and O impurities. The higher impurity levels were found in those formed without neutralization. X‐ray diffraction indicates that the film is quasicrystalline, with a lattice parameter somewhat larger than that of cubic‐BN.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
73.61.Ng Insulators
77.55.-g Dielectric thin films
68.55.-a Thin film structure and morphology

Primary Ar+ ion bombardment effect on Ni–Fe film composition formed by ion beam sputtering

Yasuhiro Nagai, Chikara Nishimura, and Tomoyuki Toshima

J. Vac. Sci. Technol. A 3, 2147 (1985); http://dx.doi.org/10.1116/1.573269 (5 pages) | Cited 2 times

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This paper reports results of experimental and analytic investigations concerning the Ni–Fe film composition formed by ion beam sputtering under various forming conditions. From experiments involving the substrate angle and temperature that had dramatic influence on the Ni–Fe film composition, it is found that the primary Ar+ ion bombardment dominates the composition variation. Also, the Ni fraction in Ni–Fe film and its deposition rate decrease as the ion current density increases. As a result of simple analysis, this composition variation is found to be caused by preferential resputtering. Conversely, the Ni fraction increases as the substrate temperature increases without a deposition rate change under primary ion bombardment. This phenomenon cannot be explained only by preferential resputtering. It also includes the formation of an Fe‐rich layer on the film surface.
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68.60.-p Physical properties of thin films, nonelectronic
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces

Elevated‐temperature sputtering of Ni–Au alloys: Surface and subsurface composition modifications measured by ion scattering spectroscopy

N. Q. Lam, H. A. Hoff, and P. G. Régnier

J. Vac. Sci. Technol. A 3, 2152 (1985); http://dx.doi.org/10.1116/1.573270 (9 pages) | Cited 2 times

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The effects of 3‐keV Ne+ ion sputtering on surface and subsurface compositions of a Ni–6 at. % Au alloy at temperatures between 25 and 600 °C were investigated using ion scattering spectroscopy. The equilibrium composition in the surface atom layer during heating prior to sputtering, the time evolution of the surface composition during sputtering, and subsurface concentration profiles after rapid specimen quenching to room temperature were measured as a function of temperature. The steady‐state composition at the alloy surface was found to be temperature dependent during sputtering at temperatures above ∼400 °C, which was attributed to significant contributions of the second atom layer to the sputtered‐atom flux. This interpretation was supported by the results of theoretical modeling which was performed using the kinetic model of Lam and Wiedersich. From the steady‐state concentration profiles measured, the effective altered‐layer thicknesses were determined, and information about radiation‐enhanced diffusion in the bombarded alloy was also obtained.
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79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties
68.90.+g Other topics in structure, and nonelectronic properties of surfaces and interfaces; thin films and low-dimensional structures (restricted to new topics in section 68)
61.80.Jh Ion radiation effects

Effect of ion bombardment during deposition on the x‐ray microstructure of thin silver films

T. C. Huang, G. Lim, F. Parmigiani, and E. Kay

J. Vac. Sci. Technol. A 3, 2161 (1985); http://dx.doi.org/10.1116/1.573271 (6 pages) | Cited 14 times

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The effect of argon ion bombardment, during deposition on the microstructure of several tens of nanometers thick Ag films, has been studied. The structure of the Ag films was analyzed by x‐ray powder diffraction method. Results show that Ar ion bombardment not only influenced the film growth process but had a significant effect on the structure of the resulting films. In comparison to an evaporated thin Ag film, our films showed much less [111] preferred orientation and a lattice expansion normal to the film surface instead of contraction, with compressive rather than tensile surface strain and plane stress. We also observed much smaller grain sizes, and higher twin fault probabilities, microstrains and dislocation densities. These structural parameters varied systematically with the normalized energy En, that is, the energy deposited by incident energetic Ar+ at the film surface per arriving Ag atom; at first rapidly, then leveling off when En≥42% eV/Ag atom. Preferential orientation is believed to be dependent on film thickness as well as on En. Unlike other parameters, twin fault probability increased to a maximum at En=20 eV/Ag atom and then decreased as En increased further due to self‐annealing during deposition.
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61.80.Jh Ion radiation effects
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

Planarization by radio‐frequency bias sputtering of aluminum as studied experimentally and by computer simulation

H. P. Bader and M. A. Lardon

J. Vac. Sci. Technol. A 3, 2167 (1985); http://dx.doi.org/10.1116/1.573272 (5 pages) | Cited 3 times

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Aluminum was deposited on silicon grooves with an aspect ratio (depth/width) of 0.27 ⋅ ⋅ ⋅ 0.5 by rf sputtering with substrate bias leading to the planarization of the silicon structure. This process was also studied by computer simulation. Excellent agreement between experimental and simulated profiles was achieved. The simulation makes it possible to study the influence of single parameters (redeposition and ion energy) on profile evolution separately, which cannot be done experimentally.
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81.15.Cd Deposition by sputtering
68.55.-a Thin film structure and morphology
81.65.-b Surface treatments
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Laser‐induced desorption from a temperature‐regulated substrate

Jacques S. Mercier and Terrill A. Cool

J. Vac. Sci. Technol. A 3, 2172 (1985); http://dx.doi.org/10.1116/1.573273 (5 pages)

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A surface temperature regulation method is described which demonstrates the feasibility of studying the direct laser‐induced quantum desorption of admolecules from surfaces under isothermal substrate conditions. The method is illustrated with an investigation of the desorption of CO molecules from a palladium substrate exposed to cw CO infrared laser radiation at intensities of up to 5 W/cm2. The temperature regulation obtained was sufficiently precise (±0.2 °C) to reduce the thermal desorption background to an upper limit of 3×10−8 desorbed molecules per absorbed photon and to show that, for the adsorption system investigated, nonthermal desorption effects were not present above this threshold.
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68.03.Fg Evaporation and condensation of liquids
68.43.Mn Adsorption kinetics
79.20.Ds Laser-beam impact phenomena
68.43.-h Chemisorption/physisorption: adsorbates on surfaces

A differential pressure‐rise method for measuring the net outgassing rates of a solid material and for estimating its characteristic values as a gas source

Nagamitsu Yoshimura

J. Vac. Sci. Technol. A 3, 2177 (1985); http://dx.doi.org/10.1116/1.573274 (7 pages) | Cited 1 time

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A differential pressure‐rise method for measuring net outgassing rates of solid materials is introduced, which has an outstanding advantage in that the error due to chamber walls and the vacuum gauge is much reduced. The differential method was successfully applied to measuring net rates of solid materials. The net rate K per unit surface area of a solid material at a pressure P could be practically expressed as K=K0(1−P/Px), where the characteristic values Px and K0 are estimated by measuring two net rates at two different pressures.
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68.03.Fg Evaporation and condensation of liquids
68.43.Mn Adsorption kinetics
07.30.Bx Degasification, residual gas

Frequency dependence of a quartz oscillator on gas pressure

K. Kokubun, M. Hirata, M. Ono, H. Murakami, and Y. Toda

J. Vac. Sci. Technol. A 3, 2184 (1985); http://dx.doi.org/10.1116/1.573275 (4 pages) | Cited 8 times

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The frequency shifts of a tuning‐fork‐shaped quartz oscillator with gas pressure were studied experimentally and theoretically. The experimental measurements showed that the frequency shift of the oscillator was very small in the pressure region below 1 Torr and much larger in the higher pressure region above 1 Torr. The experimental results were theoretically analyzed on the basis of a string‐of‐beads model for a quartz oscillator. The theoretical analysis showed that the resonance frequency shift of the quartz oscillator was small in the molecular flow region. In the viscous flow region the frequency shift was found to be proportional to the pressure. These theoretical results are in good agreement with the experimental data. The frequency shift of the oscillator in the higher pressure region was also found to be proportional to the molecular weight of the gas species in both theory and experiment.
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43.40.At Experimental and theoretical studies of vibrating systems
43.20.Ks Standing waves, resonance, normal modes
07.30.Dz Vacuum gauges

Thermal outgassing from aluminum alloy vacuum chambers

J. R. Chen, K. Narushima, and H. Ishimaru

J. Vac. Sci. Technol. A 3, 2188 (1985); http://dx.doi.org/10.1116/1.573276 (4 pages)

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A special aluminum alloy tube, primarily A6063 alloy clad inside with A1050 al pumpdown at room temperature and ∼1×10−13 Torr⋅l/s cm2 10 h after a 1 day bakeout at 150 °C. When the tube was vented to air for 1 day, the vacuum performance was not degraded. Outgassing rates for another type of tube, made of A6063 alloy but using a special extrusion method, were measured for several cases: (1) after exposure to air for about 1.5 years, (2) after partially filled with water for 1 day, and (3) after partially filled with water for 1 week. The outgasssing rate 10 h after baking was ∼1.5×10−13 Torr⋅l/s cm2 for case (2) and <5×10−13 Torr⋅l/s cm2 for case (3). Some surface parameters, adsorption isotherms, surface coverages, mean residence times, and adsorption energies were calculated to describe the surface conditions for all the above cases.
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07.30.Hd Vacuum testing methods; leak detectors
68.03.Fg Evaporation and condensation of liquids
68.43.Mn Adsorption kinetics

Ion current modulation of a residual gas analyzer

F. Watanabe and H. Ishimaru

J. Vac. Sci. Technol. A 3, 2192 (1985); http://dx.doi.org/10.1116/1.572888 (4 pages) | Cited 2 times

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A residual gas analyzer (RGA) is described with a modified quadrupole mass filter. This change permits a separate analysis of ions created in the gas from those created by electron impact in the RGA. Electrically, the electron energies are modulated and the ion current is measured in a phase‐lock loop. Experimental results on H+ and O+ indicate that the spurious electron‐stimulated‐ion‐desorption peaks are eliminated.
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07.75.+h Mass spectrometers
07.77.-n Atomic, molecular, and charged-particle sources and detectors
29.27.-a Beams in particle accelerators
82.80.Ms Mass spectrometry (including SIMS, multiphoton ionization and resonance ionization mass spectrometry, MALDI)

Mercury vapor streaming effect in McLeod gauges

J. K. N. Sharma and D. R. Sharma

J. Vac. Sci. Technol. A 3, 2196 (1985); http://dx.doi.org/10.1116/1.572889 (4 pages)

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In this paper the authors explain the experimental results, reported earlier, on the error made in measuring pressures below the vapor pressure of mercury with a McLeod gauge. Mercury vapor streaming effects the pressure measurement made by a cold trapped McLeod gauge. The percentage of errors in the pressure measured (i.e., Δp/P2%) agrees with Gaede’s transport theory and Takaishi’s kinetic theory of gas analysis of this problem. Below the vapor pressure of mercury the percentage error starts rising and rises to 10.3% forming a plateau and increases to 17%–19% below 2.67×10−3 Pa (2×10−5 Torr). This increase in pressure measurement error below 2.67×10−3 Pa (2×10−5 Torr) has been found to be in quantitative agreement with that predicted by Rambeau.
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07.30.Dz Vacuum gauges

A large aluminum alloy molecular beam epitaxy chamber with an ultimate pressure of 7.5×10−12 Torr

J. R. Chen, K. Narushima, M. Miyamoto, and H. Ishimaru

J. Vac. Sci. Technol. A 3, 2200 (1985); http://dx.doi.org/10.1116/1.572890 (5 pages) | Cited 1 time

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An ultimate pressure of 7.5×10−12 Torr was reached in a large molecular beam epitaxy (MBE) chamber made of aluminum alloy A1050, after baking and after liquid nitrogen was introduced. Most of the components were made of aluminum alloys, except a gauge and the Ti‐sublimation pump. For the seals between aluminum and stainless steel flanges, aluminum gaskets or helicoflexes were used and no problems resulted. It was also found that the Ti‐sublimation pump was effective in the 10−10 Torr range but not in the lower 10−11 Torr range. The pressure limits of the turbomolecular pump used in the system was 6×10−11 Torr. Pumping speeds of the ion pump and the shroud cooled with liquid nitrogen were about 60 and 250 l/s, respectively. The outgassing rate of the chamber was estimated to be 1×10−13 Torr ⋅ l/s cm2. After a situation in which the ion pump was turned off at room temperature and in a second case in which the liquid nitrogen supply was stopped, surface conditions of the system were studied.
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07.30.Kf Vacuum chambers, auxiliary apparatus, and materials

Absolute densities of reaction products from plasma etching of quartz

E. M. van Veldhuizen, Th. Bisschops, E. J. W. van Vliembergen, and J. H. M. C. van Wolput

J. Vac. Sci. Technol. A 3, 2205 (1985); http://dx.doi.org/10.1116/1.572891 (4 pages) | Cited 19 times

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The plasma of a CF4‐quartz etching system is investigated with optical methods. The presence of CF2, CF, F, and CO is demonstrated from ultraviolet and visible emission. Using infrared absorption the absolute densities of the reaction products SiF4 and CO are found to be 2.5±0.4×1020 and 3±2×1020 m−3. CF2 radicals are not found with infrared absorption which means that their density is below 1019 m−3. The results indicate that quartz is etched through the reaction SiO2+2CF2 → SiF4+2CO.
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81.65.-b Surface treatments
82.30.Hk Chemical exchanges (substitution, atom transfer, abstraction, disproportionation, and group exchange)
82.30.Cf Atom and radical reactions; chain reactions; molecule-molecule reactions
82.20.Hf Product distribution

An effective background removal technique for inelastic electron tunneling spectra

G. J. Gajda and W. H. Weinberg

J. Vac. Sci. Technol. A 3, 2208 (1985); http://dx.doi.org/10.1116/1.572892 (3 pages) | Cited 1 time

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This report describes a simple, rapid, and effective computer algorithm for background removal in inelastic electron tunneling spectra.
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07.05.Hd Data acquisition: hardware and software
07.05.Kf Data analysis: algorithms and implementation; data management
07.05.Rm Data presentation and visualization: algorithms and implementation
07.78.+s Electron, positron, and ion microscopes; electron diffractometers

Continuous dynode electron multiplier using lead zirconate titanate ceramic

A. V. Dixit and S. V. Bhoraskar

J. Vac. Sci. Technol. A 3, 2211 (1985); http://dx.doi.org/10.1116/1.572893 (2 pages)

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84.47.+w Vacuum tubes

A quantitative appraisal of the backstreaming of forepump oil vapor

G. Lewin

J. Vac. Sci. Technol. A 3, 2212 (1985); http://dx.doi.org/10.1116/1.572894 (2 pages)

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If a vacuum vessel is evacuated with the forepump alone for some time, oil will be deposited on the vessel walls. Therefore, it is recommended to switch over from the roughing pump to the high vacuum pump as soon as possible. The effect of the pertinent parameters is calculated to obtain quantitative information. It is found that it is essential to remain in the viscous flow range and that this requirement is met, when the product of nitrogen (or air) pressure and tube inside diameter is at least 50 Pa cm. In addition, venting to atmospheric pressure is necessary during prolonged stand‐by periods.
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07.30.Kf Vacuum chambers, auxiliary apparatus, and materials

The use of anhydrous WO3 layers to record the position of 5–15 keV H+2 beams

Scott Walck and A. D. Buonaquisti

J. Vac. Sci. Technol. A 3, 2214 (1985); http://dx.doi.org/10.1116/1.572895 (2 pages)

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This note reports the use of anhydrous WO(3) powderr as a medium which can record the position of the 5−15 keV hydrogen ion beams. The process is quick v ersatile and simple. Beam position can be determined directly without need for chemical processing or extensive specimen preparation. The technique is recomm ended for those applications in which line of sight cannot be used to detect bea m position. (AIP)
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29.27.Eg Beam handling; beam transport
29.40.-n Radiation detectors
61.80.Jh Ion radiation effects
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces

Behavior of Ga atoms on a tungsten surface

Hyunwoo Kim and Kimo Okuno

J. Vac. Sci. Technol. A 3, 2215 (1985); http://dx.doi.org/10.1116/1.572896 (3 pages)

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The variation of the work function and the preexponential term of the Fowler–Nordheim (FN) plots and field emission current from a Ga covered tungsten surface have been studied using a field emission microscope (FEM). The work function and preexponential terms both vary in the same way with coverage and desorption temperature. Both are decreased to 4.25 and −0.6 eV, respectively, at θ=0.2. In spite of a small decrease in work function, the field emission current decreased to about half of its initial value, because of a decrease in the emitting areas of the Ga covered tungsten surface. The polarizability of Ga, at this coverage, is also obtained as ∼3 A3.
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73.30.+y Surface double layers, Schottky barriers, and work functions
79.70.+q Field emission, ionization, evaporation, and desorption
68.03.Fg Evaporation and condensation of liquids
68.43.Mn Adsorption kinetics

Tent‐type bakeout oven

B. V. Hess and T. E. Felter

J. Vac. Sci. Technol. A 3, 2218 (1985); http://dx.doi.org/10.1116/1.572897 (1 page)

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A bakeout oven has been designed and built using quartz infrared lamps bring the vacuum system chamber to a bakeout temperature of 200 C in 75 mi nutes. (AIP)
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07.30.Kf Vacuum chambers, auxiliary apparatus, and materials

Performance of titanium nitride diffusion barriers in aluminum–titanium metallization schemes for integrated circuits

I. Suni, M. Blomberg, and J. Saarilahti

J. Vac. Sci. Technol. A 3, 2233 (1985); http://dx.doi.org/10.1116/1.572898 (4 pages) | Cited 21 times

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Three different contact schemes Al–Si, Al/Ti–Si, and Al/TiN/Ti–Si have been studied for their electrical characteristics and thermal stability on shallow n+p‐junctions. Contact resistance and leakage current measurements indicate that the Al/Ti structure remains stable up to 450 °C and the Al/TiN/Ti structure up to 500 °C for 15 min, whereas Al–Si contacts degrade already at 400 °C. The stability of the Al/Ti contacts is limited by the thin film reaction between Al and Ti while the failure of the Al/TiN/Ti structure is attributed to local defects such as pinholes in the TiN barrier.
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73.40.Ns Metal-nonmetal contacts
85.40.Bh Computer-aided design of microcircuits; layout and modeling
66.30.J- Diffusion of impurities
73.40.Cg Contact resistance, contact potential

Ion‐implanted, electron‐beam annealed TiN films as diffusion barriers for Al on Si shallow junctions

A. Armigliato, M. Finetti, J. Garrido, S. Guerri, P. Ostoja, and A. Scorzoni

J. Vac. Sci. Technol. A 3, 2237 (1985); http://dx.doi.org/10.1116/1.572899 (5 pages) | Cited 7 times

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TiN films are prepared by N+2 implantation onto evaporated Ti films. By properly selecting the Ti thickness, implantation energy and annealing process, a TiSi2/TiN structure can be formed. In particular, in this work a postimplant rapid isothermal annealing is carried out at 800 °C for 30 s by using an electron beam. The effectiveness of these TiN films as a diffusion barrier is then evaluated when put in contact with a thick Al overlayer. Both the TiN/Al and TiSi2/TiN/Al contact structures are tested, after thermal treatments up to 600 °C, on shallow junction diodes and four terminal resistor test patterns for contact resistance measurements. The electrical performances of the TiSi2/TiN/Al contact system are found to be good, although the degradation resistance is slightly worse than the one observed on similar structures annealed in a vacuum furnace after the nitrogen implantation.
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81.40.Rs Electrical and magnetic properties related to treatment conditions
81.40.Ef Cold working, work hardening; annealing, post-deformation annealing, quenching, tempering recovery, and crystallization
73.40.Qv Metal-insulator-semiconductor structures (including semiconductor-to-insulator)
66.30.J- Diffusion of impurities

Diffusion of nickel through titanium nitride films

W. B. Nowak, R. Keukelaar, W. Wang, and A. R. Nyaiesh

J. Vac. Sci. Technol. A 3, 2242 (1985); http://dx.doi.org/10.1116/1.572900 (4 pages) | Cited 1 time

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TiN is among the candidates for thin film diffusion barriers on integrated circuit contacts. We have deposited titanium nitride (approximately TiN) and TiN+Sm films onto Ni substrates near room temperature by ion plating. Ti was e‐beam evaporated in a chamber containing about 2.8 Pa (21 mTorr) of N2 in the vicinity of the substrate. A plasma was excited between the substrate and a gas source‐tube near the substrate by a combination of electrons from the e‐beam (or backscattered from the Ti melt) and from an electric field generated by a constant current power supply (usually set at 100 mA) connected with negative polarity to the substrate. Deposition rates were 0.5 μm/min and the film thicknesses were 2 μm. The films are crystalline, slightly burnt gold in color, and are less dense and have an order of magnitude higher electrical resistivity than TiN produced by CVD methods. The addition of at least 12 at. % Sm produced amorphous films. The diffusion of Ni through these films was measured by energy dispersive analysis in a SEM. The amorphous material showed substantially lower diffusivities. Values of D0 and Q, in the equation D=D0 exp (−Q/RT), were determined to be 0.82×10−7 cm2/s and 29 kcal/mol for crystalline TiN, and 0.56 cm2/s and 67.3 kcal/mol for amorphous TiN+12 at. % Sm films. Because of film variation in structure and composition, these values vary. However, there is still a large improvement in the diffusion barrier property of TiN films by using amorphous films containing Sm. Ni diffuses very slowly into amorphous TiN+Sm at temperatures up to 655 °C. One must increase the temperature to 765 °C in order to observe diffusion rates comparable to crystalline TiN at 590 °C.
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66.30.J- Diffusion of impurities
81.15.Jj Ion and electron beam-assisted deposition; ion plating
73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors
68.55.-a Thin film structure and morphology

Sputtered W–N diffusion barriers

H. P. Kattelus, E. Kolawa, K. Affolter, and M‐A. Nicolet

J. Vac. Sci. Technol. A 3, 2246 (1985); http://dx.doi.org/10.1116/1.572901 (9 pages) | Cited 27 times

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The thermal stability of reactively sputtered tungsten–nitrogen alloy thin films is investigated for the application as diffusion barriers in silicon contact metallizations. The composition of W–N barriers is varied over a wide range including pure W. Aluminum, gold, and silver are used as low resistivity overlayers. Metallurgical interactions at temperatures ranging from 500 to 900 °C are studied. Incorporating nitrogen into tungsten advantageously stabilizes all three systems. The overall failure takes place rapidly above critical temperatures that depend on both the metal overlayer and the microstructure of the barrier. In some cases, W–N alloys can effectively prevent interdiffusion at temperatures as high as 800 °C for 30 min.
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66.30.Ny Chemical interdiffusion; diffusion barriers

TiB2 and ZrB2 diffusion barriers in GaAs Ohmic contact technology

J. Shappirio, J. Finnegan, R. Lux, D. Fox, J. Kwiatkowski, H. P. Kattelus, and M‐A. Nicolet

J. Vac. Sci. Technol. A 3, 2255 (1985); http://dx.doi.org/10.1116/1.572902 (4 pages) | Cited 7 times

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The transition metal diboride compounds, ZrB2 and TiB2, interposed between Ni/Ge/Au Ohmic contact metallization on n‐type GaAs wafers and an overlying thick Au contact layer, have been investigated to evaluate their effectiveness in stabilizing the Ohmic contact by limiting the in‐diffusion of Au. All of the metal layers were e‐beam deposited except the ZrB2 which was rf‐diode sputtered. The barrier layer thicknesses were 50 and 100 nm for the TiB2 and the ZrB2, respectively. Postdeposition alloying of the contacts was performed at 400, 425, or 450 °C. Auger electron spectroscopy depth profiling of the resultant Ohmic contacts demonstrates that the barrier layers effectively preclude penetration of Au to the Ohmic contact structure. Specific contact resistivities for such contacts are in the low 10−7 Ω cm2 range; although some degradation of the contact resistivity is observed after long term annealing, the values of resistivities do not exceed 1.5×10−6 Ω cm2 after 92 h at 350 °C.
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73.40.Sx Metal-semiconductor-metal structures
66.30.J- Diffusion of impurities

Electrical characteristics of fast radiatively processed titanium silicides thin films

C. S. Wei, J. Van der Spiegel, and J. Santiago

J. Vac. Sci. Technol. A 3, 2259 (1985); http://dx.doi.org/10.1116/1.572903 (5 pages) | Cited 1 time

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A fast radiative processing technique using quartz‐halogen tungsten lamps is employed for the formation of titanium silicides on either high purity single crystal or undoped polycrystalline Si substrates. Characterization techniques such as four‐point probe, x‐ray diffraction, SEM, and backscattering spectrometry (BS) show complete TiSi2 formation after 17 s exposure to 18 W/cm2 radiation. Electrical characterization was performed by galvanomagnetic measurements. The results show a metallic and highly conductive silicide whose resistivity varies linearly with temperature in the temperature interval from 80 to 300 K. Films grown on (111) oriented single crystals and (110) textured polycrystalline Si showed both electrons and holes, with the holes as the predominant carriers at low temperature.
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73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors
68.60.-p Physical properties of thin films, nonelectronic
68.55.-a Thin film structure and morphology

Formation of TiSi2 and TiN during nitrogen annealing of magnetron sputtered Ti films

E. D. Adams, K. Y. Ahn, and S. B. Brodsky

J. Vac. Sci. Technol. A 3, 2264 (1985); http://dx.doi.org/10.1116/1.572904 (4 pages) | Cited 6 times

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Rutherford backscattering analysis was used to evaluate TiSi2 films which were prepared by sputtering Ti on various substrates and nitrogen annealing. The resulting properties were then compared with that of films prepared by thermal evaporation. Ti films were deposited on single crystal Si, polycrystalline Si, thermally grown SiO2, and CVD Si3N4 by dc‐magnetron sputtering in an Ar plasma at a typical deposition rate of 20 Å/s. Some films were passivated with a thin amorphous film of Si to compare the reaction kinetics with the samples without passivation. The temperature dependence of the electrical resistivity is basically the same as with the evaporated films [Ref. 1: C. Y. Ting et al., in Proceedings of the First International Symposium on VLSI Science and Technology (Electrochemical Society, New York, 1982), p. 224.], and the minimum value obtained after an 800 °C anneal is similar. Typical resistivity after taking into account the presence of TiN on the surface is approximately 13.9 μΩ‐cm. The presence of a thin Si passivation layer (300 Å) appears to prohibit the formation of TiN while allowing the formation of stoichiometric TiSi2 at a lower temperature, with a similar resistivity.
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68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors
81.15.Cd Deposition by sputtering

Structure and properties of coevaporated WSix films

K. Y. Ahn, S. R. Herd, J. E. E. Baglin, and J. U. Han

J. Vac. Sci. Technol. A 3, 2268 (1985); http://dx.doi.org/10.1116/1.572905 (4 pages) | Cited 2 times

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The crystallization behavior and electrical resistivity of WSix films (coevaporated on poly‐Si on SiO2) with x ranging from 1.0 to 2.4 were examined in a high‐resolution TEM before and after annealing at 1000 °C. The amorphous as‐deposited films with high resistivities (up to 650 μΩ cm) become crystalline WSi2 after annealing accompanied by a precipitous drop in resistivity to values below 30 μΩ cm. The as‐deposited Si‐rich films showed a reduction in thickness, up to −15% for x=2.4, while metal‐rich films showed an increased thickness, up to 13% for x=1.0. The minimum resistivity of 28 μΩ cm was found in a sample with as‐deposited composition of WSi1.4 which also had the largest thickness. The difficult problem of determining the thicknesses before and after the interaction of WSix with the CVD poly‐Si was solved by first measuring the thin SiO2 thickness (220 Å) using the Si lattice fringes, and then comparing the thicknesses of poly‐Si and WSix with that of SiO2. Annealed WSix films with thickness ranging from 1200 to 2500 Å showed one to two grains per film thickness for an as‐deposited x=2.4 to 1.4. The grain size appeared smaller (three to four grains per thickness) for x<1.4. For a film with x=1.0, W5Si3 and WSi2 were identified by electron diffraction. The density of annealed films was determined by counting the number of atoms per cm2 by Rutherford backscattering spectrometry, and it ranged from 11 to 12.5 g/cm3.
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73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors
68.55.-a Thin film structure and morphology
81.40.Ef Cold working, work hardening; annealing, post-deformation annealing, quenching, tempering recovery, and crystallization

Effects of biased cosputtering on resistivity and step coverage in tungsten silicide films

K. W. Choi and K. Y. Ahn

J. Vac. Sci. Technol. A 3, 2272 (1985); http://dx.doi.org/10.1116/1.572906 (6 pages)

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Electrical resistivity and step coverage on thick oxide steps of various slopes were examined in tungsten silicide films sputter deposited by multilayering of W and Si utilizing magnetron targets. The desired composition was obtained by adjusting power levels to the targets and bias voltage. A broad minimum in electrical resistivity was obtained with bias voltage ranging from −40 to −80 V. Typical resistivity in films of 2500 Å thickness after annealing at 1000 °C was 52–66 μΩ cm when deposited on poly‐Si substrates. The effect of bias was found to produce films with much lower levels of impurity such as N, O, C, and H and the sputtering gas Ar. Proper bias voltage (−50 V) was necessary to achieve good step coverage on thick oxide step with various slopes. Zero‐bias sputtering provided minimum step coverage, while too high bias (−100 V) led to poor step coverage and formation of rounded corners and faceting.
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73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors

Laser‐induced chemical vapor deposition of titanium silicide films

G. A. West, K. W. Beeson, and A. Gupta

J. Vac. Sci. Technol. A 3, 2278 (1985); http://dx.doi.org/10.1116/1.572907 (5 pages) | Cited 5 times

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Films of titanium silicide have been deposited from gas mixtures of SiH4 and TiCl4 using laser irradiation to initiate chemical vapor deposition. Two different laser excitation sources have been used. A CO2 laser initiates deposition through the thermal decomposition of silane, whereas an ArF excimer laser causes deposition by the photolytic dissociation of titanium chloride. Both methods permit control of the substrate temperature independently from the reactor gas temperature. The substrate temperature has been found to strongly influence the resulting titanium silicide film morphology and crystal structure. The different chemistries initiated by the CO2 and excimer lasers have much less influence on the final film properties. Smooth films with a resistivity of 20 μΩ cm are obtained with either method by depositing the films at a low substrate temperature (400 °C) followed by an annealing step at elevated temperature (650–800 °C).
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81.15.Gh Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)
82.50.-m Photochemistry
68.55.-a Thin film structure and morphology

Summary Abstract: Structural and electrical characterization of reactively sputtered Pt–Si films

R. C. Budhani, B. P. O’Brien, H. J. Doerr, C. V. Deshpandey, and R. F. Bunshah

J. Vac. Sci. Technol. A 3, 2283 (1985); http://dx.doi.org/10.1116/1.572908 (1 page)

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68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors

Formation and electrical properties of Hf Si2 grown thermally from evaporated Hf and Si films

F. C. T. So, C.‐D. Lien, and M‐A. Nicolet

J. Vac. Sci. Technol. A 3, 2284 (1985); http://dx.doi.org/10.1116/1.572909 (5 pages) | Cited 5 times

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2 MeV 4He+ backscattering spectrometry and x‐ray diffraction have been used to study Hf Si2 formed by thermal annealing of a Hf Si film on evaporated Si (Sie) at temperatures between 575 and 650 °C. A laterally uniform layer of Hf Si2 forms and its thickness is proportional to the square root of time at a fixed temperature. The activation energy of this reaction is found to be 3.5±0.3 eV. This transport‐limited process differs from that observed on single crystal Si, where Hf Si2 forms at temperatures above 700 °C by a process believed to be nucleation controlled. Four‐point probe measurements of resistivity and Hall coefficient at room temperature on samples with both Hf Si and Hf Si2 were used to determine that both Hf Si and Hf Si2 are electron conductors. For Hf Si2, the electron concentration is 2.9±0.2×1021 cm−3 and the mobility is 36±4 cm2/Vs, giving a resistivity of 60±3 μΩ cm. Schottky barrier diodes formed either by reacting a Hf film deposited directly on 〈111〉 Si or by reacting a Hf film with Sie in a 〈111〉 Si/Hf/Sie/Hf configuration at temperatures above 600 °C were prepared. The Schottky barrier height of Hf Si2 on n‐type 〈111〉 Si as evaluated from forward and reverse I–V characteristics is 0.54±0.01 eV in both cases.
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68.55.-a Thin film structure and morphology
73.61.Cw Elemental semiconductors
73.61.Ey III-V semiconductors
73.61.Ga II-VI semiconductors
73.61.Jc Amorphous semiconductors; glasses
73.61.Le Other inorganic semiconductors
82.65.+r Surface and interface chemistry; heterogeneous catalysis at surfaces
73.30.+y Surface double layers, Schottky barriers, and work functions

Characterization of electron‐beam deposited tungsten films on sapphire and silicon

J. H. Souk, J. F. O’Hanlon, and J. Angillelo

J. Vac. Sci. Technol. A 3, 2289 (1985); http://dx.doi.org/10.1116/1.572866 (4 pages) | Cited 5 times

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In this work, the electrical and structural properties of e‐beam deposited tungsten films on sapphire are described. Tungsten thin films (200–400 nm) were evaporated on sapphire substrates at different substrate temperature Ts. Film resistivity varied from 95 μΩ cm deposited at room temperature to 5.5 μΩ cm deposited at Ts between 440 and 500 °C. The resistivity value of 5.5 μΩ cm is comparable to the bulk resistivity value of 5.50–5.65 μΩ cm. The crystalline structure of these films was characterized by x‐ray diffraction and scanning transmission electron microscopy (STEM) (Kikuchi lines). The films show a distinct increase in the degree of crystal orientation as Ts approaches 400 °C. The films deposited at 400 °C and above shows (100) epitaxial growth on the (11̄02) plane or r plane of sapphire, which has a distorted fourfold symmetry. Film stresses which vary from tensile (7.3×109 dyn/cm2) to compressive (−4.4×109 dyn/cm2) between 100 and 500 °C were measured by the interference fringe technique. The intrinsic stress was determined to vary from 8.3×109 dyn/cm2 at Ts=100 °C to 2.4×109 dyn/cm2 at Ts=500 °C. The observed intrinsic stresses (tensile) in epitaxial films are regarded as produced by the lattice misfit at the film–substrate interface. The minimum total film stress was obtained between Ts=350 and 400 °C, where tensile intrinsic stress was compensated by the compressive thermal stress. The properties of tungsten films on silicon, silicon oxide, and polysilicon substrates are also discussed.
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73.61.At Metal and metallic alloys
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
81.40.Rs Electrical and magnetic properties related to treatment conditions

The effect of substrate temperature on topography related defect formation in evaporated aluminum based thin films

James G. Ryan, Richard Douse, Loren Hahn, and Michael Luciano

J. Vac. Sci. Technol. A 3, 2293 (1985); http://dx.doi.org/10.1116/1.572867 (5 pages)

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The severe topography of high density integrated circuits has always caused step coverage problems for metallization layers. A technique has been developed to reveal the presence of Al2O3 in steep step regions for aluminum based metallization layers. This Al2O3 defect may increase the susceptibility of metallization layers to metal step opens. Aluminum oxide formation was studied as a function of substrate temperature, AlCu evaporation rate and slope angle. Al 1% Cu (1.0 μm thick) with a 0.1 μm thick titanium underlayer and 1.0 μm thick Al 1.4% Cu films were evaporated on substrates containing slope angles from 40° to 100° using substrate temperatures of approximately 30 to 200 °C. For Al 1% Cu with a Ti underlayer, the Al2O3 formation angle increases from 61° for the film evaporated at ambient substrate temperature (∼30 °C) to 91° for the film evaporated at 200 °C. Increasing the Al 1% Cu evaporation rate from 0.5 to 9.2 nm/s increased the Al2O3 formation angle from 71° to 92°. No effects on Al2O3 formation were observed due to step height or the presence of a titanium underlayer.
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68.55.-a Thin film structure and morphology
81.05.Bx Metals, semimetals, and alloys
85.40.-e Microelectronics: LSI, VLSI, ULSI; integrated circuit fabrication technology

Selective deposition of tungsten—prediction of selectivity

Jan‐Otto Carlsson and Mats Boman

J. Vac. Sci. Technol. A 3, 2298 (1985); http://dx.doi.org/10.1116/1.572868 (5 pages) | Cited 3 times

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Preferential or selective chemical vapor deposition to a substrate region is based on a difference in thermochemical stability between different substrate regions. The higher this difference is, the higher selectivity is expected. In this paper a thermodynamic analysis of selective deposition of tungsten from H2 and WF6 on silicon regions in the presence of silicon dioxide is presented. At the initial stages of growth—silicon present in the vapor—the selectivity is favored by a low temperature, a low total pressure and a high WF6 concentration in the vapor. For the continuation—growth on the deposited tungsten—a low total pressure, a low WF6 concentration in the vapor and a higher temperature than that used initially should be chosen for highest selectivity. From the analysis it is also seen that simultaneous etching and tungsten oxide/tungsten deposition may occur on the silicon dioxide. The technique used to analyze the selective tungsten deposition process seems to be a useful tool for optimizing the selectivity in a given system and for reducing or eliminating undesired side reactions.
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81.15.Gh Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)

Contact resistance behavior of titanium nitride

C. Ernsberger, J. Nickerson, A. Miller, and D. Banks

J. Vac. Sci. Technol. A 3, 2303 (1985); http://dx.doi.org/10.1116/1.572869 (5 pages) | Cited 2 times

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This paper describes a highly automated contact resistance probe developed as part of our study of the contact properties of materials based on stoichiometric titanium nitride. Comparative results are shown for selected TiN samples, noble metal, and non‐noble metal contacts under conditions of accelerated environmental aging and wear. Contact resistance and its temperature dependence as a function of H2O+O2 levels present during reactive sputtering are also presented.
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73.40.Cg Contact resistance, contact potential

Electromigration in aluminum films prepared with a high rate magnetron sputtering cathode

Y. H. Park, P. Roessle, E. Majewski, and J. F. Smith

J. Vac. Sci. Technol. A 3, 2308 (1985); http://dx.doi.org/10.1116/1.572870 (4 pages) | Cited 2 times

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Electromigration has been studied in pure aluminum films prepared by high rate magnetron sputtering. Deposition was performed under various bias and wafer preheat conditions, including those producing planarization of the aluminum. Film structure was determined by transmission electron microscopy (TEM) and x‐ray diffraction (XRD). Films prepared with high bias power exhibited a relatively narrow grain size distribution; those prepared without bias had a bimodal grain size distribution. Annealing under normal alloying conditions led to the development of small voids in the latter, and the behavior of these during electromigration was ascertained.
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66.30.-h Diffusion in solids
82.45.-h Electrochemistry and electrophoresis
68.55.-a Thin film structure and morphology

Laser‐induced gold deposition on a silicon substrate

S. Tamir and J. Zahavi

J. Vac. Sci. Technol. A 3, 2312 (1985); http://dx.doi.org/10.1116/1.572871 (4 pages) | Cited 1 time

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In recent years, substantial progress in the electronics industry has been witnessed. The growth of this industry led to intensive competition in the field of microelectronic devices and to more rigorous performance requirements with regard to the products. Extensive research has been undertaken with a view to improving the integrated circuits used. The trend today is to miniaturize the devices as much as possible, and one of the main problems involved is realization of metal deposition lines a few microns in width with high width resolution, so that the spacing of adjoining lines would be of the same order with no interaction between them.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
79.20.Ds Laser-beam impact phenomena
85.40.Bh Computer-aided design of microcircuits; layout and modeling
81.65.-b Surface treatments

Ion beam mixing of Au–Ge and Au–Ge–Ni deposited on GaAs

R. S. Bhattacharya, A. K. Rai, A. Ezis, M. H. Rashid, and P. P. Pronko

J. Vac. Sci. Technol. A 3, 2316 (1985); http://dx.doi.org/10.1116/1.572872 (4 pages) | Cited 5 times

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We have investigated the feasibility of applying ion beam mixing techniques to the fabrication of Ohmic contacts in GaAs. The approach has been to deposit alternating layers of Au, Ge and Au, Ge, Ni with e‐beam evaporation on GaAs and then to irradiate these layers with energetic Si+ ions. Mixing has been studied by employing Rutherford backscattering, Auger electron spectroscopy, and cross‐sectional transmission electron microscopy (X‐TEM). Differing amounts of mixing have been achieved for Au–Ge layers by using 125 keV Si+ at doses in the range of 1×1015 to 1×1016 cm−2. The kinetics of mixing is greatly reduced in the case of Au–Ge–Ni layers. Ni layers in between Au–Ge layers seem to act as inhibitors for ion beam mixing. It has been observed by X‐TEM that a band of dislocation loops is produced in GaAs at a depth of about 600 Å from the interface although computer simulation of range and damage indicate shorter penetration distances. Even at an incident ion energy low enough so that no direct penetration across the interface takes place, dislocation loops are found to be present. Contacts in the presence of a damaged region at the interface showed non‐Ohmic behavior. However, selected Au–Ge contacts fabricated with low energy and low dose irradiation showed Ohmic behavior with resistivity ∼10−4 Ω cm2 after annealing at 340 °C for 5 min. Ion beam mixed metallizations showed remarkable improvement in surface morphology after annealing compared to conventionally alloyed contacts.
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73.40.Ns Metal-nonmetal contacts
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces
61.80.Jh Ion radiation effects
64.75.-g Phase equilibria

Structural and electrical characteristics of vacuum‐evaporated erbium fluoride thin films

R. Ramanujam, M. Radhakrishnan, and C. Balasubramanian

J. Vac. Sci. Technol. A 3, 2320 (1985); http://dx.doi.org/10.1116/1.572873 (3 pages) | Cited 1 time

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Thin‐film capacitors of erbium fluoride were fabricated by thermal evaporation. The film structure was analyzed by x‐ray diffractogram and confirmed by the x‐ray small‐angle surface reflection technique. The current–voltage characteristics of these films were studied at different temperatures in the range of 300–390 K. It was observed that at high electric fields the current increases linearly with the square root of the field. The conduction mechanism was found to be predominantly by Poole–Frenkel emission in these films and is an activated process with the activation energy decreasing with increasing electric field.
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68.55.-a Thin film structure and morphology
73.61.Ng Insulators
84.32.Tt Capacitors

Epitaxial growth of CeF3 and NdF3 on Si(111)

S. Sinharoy, R. A. Hoffman, R. F. C. Farrow, and J. H. Rieger

J. Vac. Sci. Technol. A 3, 2323 (1985); http://dx.doi.org/10.1116/1.572874 (4 pages) | Cited 7 times

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We report the first epitaxial growth of two members of the rare earth lanthanide trifluoride family, namely cerium trifluoride (CeF3) and neodymium trifluoride (NdF3), on silicon (111). These materials are known to have superior physical and chemical properties in comparison with the group II fluorides for several potential applications including protective antireflection coatings and insulating layers in various semiconductor device structures. The films of thicknesses up to 3400 Å were grown under ultrahigh vacuum (UHV) conditions using a specially designed evaporator. They were characterized in situ by low‐energy electron diffraction (LEED) and Auger electron spectroscopy (AES), and ex situ by reflection high energy electron diffraction (RHEED) and Nomarski optical microscopy. Good quality epitaxial films were obtained on both the (1×1) and the (7×7) structures of Si(111). The optimum growth temperatures were found to be 600 °C for CeF3 and 500 °C for NdF3. In both cases, the c axis was parallel to the Si[111], consistent with the hexagonal symmetry of the trifluorides and the Si(111) surface. Cracking problems were encountered at nonoptimum growth temperatures.
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68.55.-a Thin film structure and morphology

Summary Abstract: Characterization of ion beam deposited diamondlike carbon coating on semiconductors

P. V. Koeppe, V. J. Kapoor, M. J. Mirtich, B. A. Banks, and D. A. Gulino

J. Vac. Sci. Technol. A 3, 2327 (1985); http://dx.doi.org/10.1116/1.572875 (2 pages) | Cited 1 time

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73.61.Ng Insulators
68.60.-p Physical properties of thin films, nonelectronic
77.55.-g Dielectric thin films
85.30.De Semiconductor-device characterization, design, and modeling

Frictional and structural characterization of ion‐nitrided low and high chromium steels

Talivaldis Spalvins

J. Vac. Sci. Technol. A 3, 2329 (1985); http://dx.doi.org/10.1116/1.572876 (5 pages) | Cited 2 times

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Low Cr steels AISI 4140, AISI 4340, and high Cr austenitic stainless steels AISI 304. AISI 316 were ion nitrided in a dc glow discharge plasma consisting of a 75% H2–25% N2 mixture. Surface compound layer phases were identified, and compound layer microhardness and diffusion zone microhardness profiles were established. Distinct differences in surface compound layer hardness and diffusion zone profiles were determined between the low and high Cr alloy steels. The high Cr stainless steels after ion nitriding displayed a hard compound layer and an abrupt diffusion zone. The compound layers of the high Cr stainless steels had a columnar structure which accounts for brittleness when layers are exposed to contact stresses. The ion nitrided surfaces of high and low Cr steels displayed a low coefficient of friction with respect to the untreated surfaces when examined in a pin and disk tribotester.
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81.40.Pq Friction, lubrication, and wear
81.05.Bx Metals, semimetals, and alloys
62.20.Qp Friction, tribology, and hardness
66.30.-h Diffusion in solids

The influence of process conditions on the friction and wear of electrodeposited chromium coatings

D. T. Gawne and N. J. Despres

J. Vac. Sci. Technol. A 3, 2334 (1985); http://dx.doi.org/10.1116/1.572877 (6 pages)

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The friction and wear behavior of chromium coatings produced by different process conditions have been investigated under dry sliding conditions. Crack‐free deposits give markedly higher friction coefficients and wear rates than heat treated conventional coatings with the same hardness. The high friction coefficient of crack‐free chromium is mainly due to the large plastic strains generated in its surface layers during sliding. The chromium coating showed pronounced increases in hardness at low loads which is attributed to enhanced strain hardening in the very small stressed volumes. The conventional and heat treated coatings are strengthened by the same microstructural mechanisms and conform to the Archard wear equation. The crack‐free deposits possess distinctly different crystallographic and metallurgical structures and do not obey the same Archard relationship.
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81.40.Np Fatigue, corrosion fatigue, embrittlement, cracking, fracture, and failure
62.20.Qp Friction, tribology, and hardness
46.55.+d Tribology and mechanical contacts

Tribological properties of boron nitride synthesized by ion beam deposition

Kazuhisa Miyoshi, Donald H. Buckley, and Talivaldis Spalvins

J. Vac. Sci. Technol. A 3, 2340 (1985); http://dx.doi.org/10.1116/1.572878 (5 pages)

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An investigation was conducted to examine the adhesion and friction behavior of boron nitride films (BN coating, 2 μm thick) on 440‐C bearing stainless steel substrates. The thin films containing the boron nitride were synthesized using an ion beam extracted from a borazine (B3N3H6) plasma. Sliding friction experiments were conducted with BN in sliding contact with itself and various transition metals (Ti, Zr, V, Fe, Ni, Pd, Re, and Rh) at a sliding velocity of 3 mm/min with loads to 0.2 N at room temperature and in a vacuum of 30 nPa. The results of the investigation indicate that the surfaces of ion sputter cleaned BN coating film contain a small amount of oxides and carbides, in addition to boron nitride. The coefficients of friction for the BN in contact with metals have been correlated with the relative chemical activity of the metals. The more active the metal, the higher is the coefficient of friction. The adsorption of oxygen on ion sputter cleaned metal and BN increases the shear strength of the metal–BN contact and increases the friction. The friction for BN–BN contact is a function of the shear strength of the contacts. Ion sputter cleaned BN surfaces exhibit relatively strong interfacial adhesion and high friction. The presence of adsorbates such as adventitious carbon contaminants on the BN surfaces reduces the shear strength of the contact area. In contrast, chemically adsorbed oxygen enhances the shear strength of the BN–BN contact and increases the friction.
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62.20.Qp Friction, tribology, and hardness
46.55.+d Tribology and mechanical contacts
68.60.-p Physical properties of thin films, nonelectronic

Summary Abstract: Wear resistant carbide–boride composite coatings

H. Holleck, Ch. Kühl, and H. Schulz

J. Vac. Sci. Technol. A 3, 2345 (1985); http://dx.doi.org/10.1116/1.572879 (3 pages) | Cited 1 time

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Abstract Unavailable
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46.55.+d Tribology and mechanical contacts
81.40.Pq Friction, lubrication, and wear

Rolling contact fatigue behavior of Cu and TiN coatings on bearing steel substrates

R. F. Hochman, A. Erdemir, F. J. Dolan, and R. L. Thom

J. Vac. Sci. Technol. A 3, 2348 (1985); http://dx.doi.org/10.1116/1.572880 (6 pages)

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In this study the characteristics of film morphology, thickness, microstructure, and chemistry of sputter deposited and ion plated films have been studied in relation to their rolling contact fatigue (RCF) properties. Coatings were prepared on standard RCF samples of 440C and AMS 5749 bearing steels. Films were deposited in a range of thicknesses from approximately 2000 Å to 2 μm. Copper was chosen to evaluate the potential of a soft metal coating, and the TiN was used as an example of an ultrahard material. The rolling contact fatigue was markedly improved for pure copper tested on 440C but was degraded for copper on AMS 5749. The thinner titanium nitride films (2000 Å) were found to behave favorably on these bearing steels at RCF stress levels of 786 ksi. Scanning electron microscopy (SEM) was used to characterize the ‘‘as‐plated’’ coatings, and the wear tracks following rolling contact fatigue tests. Chemical characterization of the films was performed by x‐ray diffraction (XRD) and electron spectroscopy for chemical analysis (ESCA).
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68.60.-p Physical properties of thin films, nonelectronic
62.20.M- Structural failure of materials
46.55.+d Tribology and mechanical contacts
46.50.+a Fracture mechanics, fatigue and cracks

Developments in ionization assisted processes

A. Matthews

J. Vac. Sci. Technol. A 3, 2354 (1985); http://dx.doi.org/10.1116/1.572881 (10 pages) | Cited 6 times

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Recent developments in ionization assisted vapor deposition processes are traced, with special attention being given to PVD ceramic coating systems. The relative ionization performance of the various techniques is evaluated and shortcomings in terms of coating variability and control are identified; some solutions to these problems are suggested. To date, the systems outlined have been primarily exploited for titanium nitride deposition, and information is given on these coatings. Alternatives to that material are also discussed, indicating their potential advantages and research relevant to their deposition.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating

Process control with optical emission spectroscopy in triode ion plating

K. Salmenoja, A. S. Korhonen, and M. S. Sulonen

J. Vac. Sci. Technol. A 3, 2364 (1985); http://dx.doi.org/10.1116/1.572882 (4 pages) | Cited 2 times

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Physical vapor deposition (PVD) techniques used to prepare, e.g., hard TiN, HfN, or ZrN coatings include a great variety of processes ranging from reactive evaporation to sputtering and ion plating. In ion plating one effective way to enhance ionization is to use a negatively biased hot filament. The use of an electron emitting filament brings an extra variable to be taken into account in developing the process control. In addition, proper control of the evaporation source is critical in ensuring reproducible results. With optical emission spectroscopy (OES) it should be possible to control the coating process more accurately. The stoichiometry and the composition of the growing coating may then be ensured effectively in subsequent runs. In this work the application of optical emission spectroscopy for process control in triode ion plating is discussed. The composition of the growing coating is determined experimentally using the relative intensities of specific emission lines. Changes in the evaporation rate and the gas flow can be seen directly from emission line intensities. Even the so‐called poisoning of the evaporation source with reactive gas can be detected. Several experimental runs were carried out and afterwards the concentration profiles of the deposited coatings were checked with the nuclear resonance broadening (NRB) method. The results show the usefulness of emission spectroscopy in discharge control.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating

Magnetically confined sputter source with high ion flux

B. Window, F. Sharples, and N. Savvides

J. Vac. Sci. Technol. A 3, 2368 (1985); http://dx.doi.org/10.1116/1.572883 (5 pages) | Cited 2 times

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A magnetically confined deposition source based on the Penning geometry is described. The discharge characteristics for various gas pressures and magnetic fields resemble those of conventional magnetrons, and it is shown using probes that the ion flux approaches the deposition flux at typical target‐to‐substrate distances. The ion flux can be varied by changing the magnetic field, and the ion energy by biasing the substrates. The system has been used to deposit TiN by sputtering Ti in a reactive Ar–N2 gas mixture. Results are reported for the properties of the films (resistance, hardness, structure) for various substrate temperatures and ion bombardments and demonstrate the usefulness of this source for hard tool coating. The source is readily scaled to production applications.
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81.15.Cd Deposition by sputtering
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces
07.77.-n Atomic, molecular, and charged-particle sources and detectors
52.80.Sm Magnetoactive discharges (e.g., Penning discharges)

Plasma spray synthesis of TiB2–Fe coatings

B. Champagne and S. Dallaire

J. Vac. Sci. Technol. A 3, 2373 (1985); http://dx.doi.org/10.1116/1.572884 (5 pages) | Cited 1 time

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Titanium boride possesses so high a hardness that it could be considered a good candidate for the production of wear‐resistant coatings. However, conventional coating processes failed to achieve thick TiB2 coatings with appropriate mechanical strength for industrial application. To overcome their brittleness and take advantage of their hardness, titanium boride should be adequately dispersed in an appropriate metal matrix. To meet these requirements, TiB2–Fe coatings were produced via a synthesis process. In this work, TiB2–Fe coatings have been synthesized through the endothermic reaction of ferrotitanium with ferroboron. The fabrication technique consists in plasma spraying micropellets comprising the reagents and in depositing the as‐reacted products onto a substrate. Spraying parameters were studied and optimized to ensure the synthesis of TiB2. By this one‐step process, thick abrasion resistant TiB2–Fe coatings have been obtained.
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81.05.Mh Cermets, ceramic and refractory composites
81.05.Je Ceramics and refractories (including borides, carbides, hydrides, nitrides, oxides, and silicides)

Structures and composition before and after annealing of coatings in the Cr–C binary system produced by reactive physical deposition

G. Cholvy and J. L. Derep

J. Vac. Sci. Technol. A 3, 2378 (1985); http://dx.doi.org/10.1116/1.572885 (6 pages)

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Coatings in the Cr–C binary system are deposited by reactive physical vapor deposition. Two types of deposition were used in an argon–methane atmosphere: chromium reactive evaporation by arc discharge and rf reactive sputtering. The objective of the study is to determine the nature and structure of the deposits as a function of deposition parameters before and after annealing. Phases are identified by x‐ray diffraction. Deposit morphology is observed, both on the surface and in fractography, by scanning electron microscopy. A more particular study of coating structure, for a given configuration of deposition parameters, was conducted using transmission electron microscopy.
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81.40.Ef Cold working, work hardening; annealing, post-deformation annealing, quenching, tempering recovery, and crystallization
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
64.70.-p Specific phase transitions

Summary Abstract: Hard coatings of carbon, boron nitride, and composites based on these materials

C. Weissmantel

J. Vac. Sci. Technol. A 3, 2384 (1985); http://dx.doi.org/10.1116/1.572886 (2 pages)

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Abstract Unavailable
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68.60.-p Physical properties of thin films, nonelectronic
81.15.Jj Ion and electron beam-assisted deposition; ion plating
81.05.Mh Cermets, ceramic and refractory composites
46.55.+d Tribology and mechanical contacts

Diamondlike amorphous carbon films prepared by magnetron sputtering of graphite

N. Savvides and B. Window

J. Vac. Sci. Technol. A 3, 2386 (1985); http://dx.doi.org/10.1116/1.572887 (5 pages) | Cited 26 times

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Amorphous carbon films, a‐C, were prepared by employing dc magnetron sputtering of a graphite target in an argon plasma. A series of a‐C films were deposited as a function of sputtering power. The power was varied in the range 5–500 W and the target effective sputtering area was about 20 cm2. The physical and optical properties of the a‐C films show a dependence on the sputtering power. The films, although unhydrogenated, possess diamondlike properties such as high hardness, HV=1200–2400 kgf mm−2, and are transparent in the infrared (IR) region with optical gap Eopt =0.40–0.74 eV. We observe a systematic variation of film properties with increasing sputtering power which suggest a transition from fourfold (diamondlike) to threefold (graphitic) coordination of the carbon atoms. For films prepared at low sputtering power about 3/4 of the carbon atoms have tetrahedral coordination and 1/4 have trigonal coordination. At the highest sputtering power the a‐C films consist of equal mixtures of tetrahedrally and trigonally bonded carbon atoms.
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81.15.Cd Deposition by sputtering
68.60.-p Physical properties of thin films, nonelectronic
75.20.Ck Nonmetals
68.55.-a Thin film structure and morphology

Micromechanical investigations of amorphous hydrogenated carbon films on silicon

J. B. Pethica, P. Koidl, J. Gobrecht, and C. Schüler

J. Vac. Sci. Technol. A 3, 2391 (1985); http://dx.doi.org/10.1116/1.572844 (3 pages) | Cited 7 times

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Amorphous hydrogen containing carbon films (α‐C:H) can be obtained on various substrates by exposure to an rf‐glow discharge in a low pressure hydrocarbon atmosphere. The films show interesting optical and mechanical properties and are thus attractive candidates for hard and wear resistant coatings. In this paper results of microhardness measurements on thin (0.8 μm) α‐C:H films are presented which were taken with a specially designed microhardness tester which allows indentation depth as low as 50 nm. In this way the influence of the substrate on the hardness results can be minimized. A large influence of the film deposition parameters was found. The hardness of films deposited under high dc bias voltage (>1000 V) is comparable to or better than that of bulk silicon. Heat treatment of the films above 350 °C decreases the hardness significantly. The elastic properties of α‐C:H may be estimated using the elastic relaxation of the indents.
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68.60.-p Physical properties of thin films, nonelectronic
46.55.+d Tribology and mechanical contacts
81.40.Jj Elasticity and anelasticity, stress-strain relations
81.40.Pq Friction, lubrication, and wear

Adhesion of TiC and Ti(C,N) coatings on steel

P. A. Steinmann and H. E. Hintermann

J. Vac. Sci. Technol. A 3, 2394 (1985); http://dx.doi.org/10.1116/1.572845 (7 pages) | Cited 10 times

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The scratch test has been used to measure the adhesion of CVD TiC coatings on various steels by comparing the critical load factors. The critical load (Lc) of a coating–substrate interface determined by the scratch test depends not only on the adhesion but also the substrate hardness and coating thickness. For identical deposition conditions, the coating thickness depends strongly on the carbide forming elements in the steel. In this work, a careful separation of these effects has allowed us to quantify the adhesion of a given system from the critical load. Of the nine steels tested, two had improved adhesion which was shown to be caused by diffusion of substrate elements into the coating. Adhesion measurements of Ti(C,N) coatings deposited by PVD are discussed and compared to the adhesion values of CVD TiC on the same steel substrates.
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46.55.+d Tribology and mechanical contacts
68.60.-p Physical properties of thin films, nonelectronic

Techniques for evaluating mechanical properties of hard coatings

P. K. Mehrotra and D. T. Quinto

J. Vac. Sci. Technol. A 3, 2401 (1985); http://dx.doi.org/10.1116/1.572846 (5 pages) | Cited 5 times

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This paper describes specialized methods for measuring coating adhesion, microhardness, and microfracture toughness of hard coatings. Coating adhesion is an interfacial property which may be characterized by scratch or indentation techniques which yield a decohesion critical load or an interfacial fracture toughness parameter. Microhardness measurements are shown to be satisfactory if light indenter loads are applied to polished coating surfaces; microhardness profiles may be measured at room and elevated temperatures on a taper section of the coating. The Palmqvist microfracture toughness of hard coatings may additionally be determined from the same microhardness indentations.
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46.80.+j Measurement methods and techniques in continuum mechanics of solids
46.55.+d Tribology and mechanical contacts
68.60.-p Physical properties of thin films, nonelectronic

Morphology and properties of sputtered HfN layers as a function of substrate temperature and sputtering atmosphere

Hermann A. Jehn, Uwe Kopacz, and Siegfried Hofmann

J. Vac. Sci. Technol. A 3, 2406 (1985); http://dx.doi.org/10.1116/1.572847 (5 pages) | Cited 2 times

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HfN layers were prepared by reactive rf‐magnetron sputtering onto polished flat high speed steel (HSS) surfaces. Rectangular samples were mounted on a special holder providing temperatures in the range of 775 to 300 K along the length of the sample. The HfN layers were deposited at various total pressures and different N2/Ar ratios. The film morphology and composition was studied by scanning electron microscopy (SEM) and Auger electron spectroscopy (AES), respectively, and correlated with mechanical properties like microhardness and adhesion. The results are discussed with respect to the sputtering conditions.
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81.15.Cd Deposition by sputtering
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

TiN coating adhesion studies using the scratch test method

J. Valli, U. Mäkelä, A. Matthews, and V. Murawa

J. Vac. Sci. Technol. A 3, 2411 (1985); http://dx.doi.org/10.1116/1.572848 (4 pages) | Cited 8 times

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The development of the scratch test method of adhesion assessment is reported. The tangential friction force between the indenter and coating is recorded rather than the acoustic emission which has previously been used to detect the critical load. This method is shown to provide a sensitive and simple means of condition monitoring. Results obtained with this new technique are compared to those obtained by the authors and others using the conventional system, showing that good agreement is achieved. The results of tests on a number of substrate/interface/pretreatment combinations are reported. The implications of the method are discussed especially with regard to the influence of friction on adhesion.
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46.80.+j Measurement methods and techniques in continuum mechanics of solids
46.55.+d Tribology and mechanical contacts
68.60.-p Physical properties of thin films, nonelectronic
81.40.Pq Friction, lubrication, and wear

Angular resolved x‐ray photoelectron spectroscopy study of reactively sputtered titanium nitride

C. Ernsberger, J. Nickerson, A. E. Miller, and J. Moulder

J. Vac. Sci. Technol. A 3, 2415 (1985); http://dx.doi.org/10.1116/1.572849 (4 pages) | Cited 19 times

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Moisture and O2 levels present during the reactive sputtering deposition of TiN have a marked impact on measured contact resistance. Results of an angular resolved x‐ray photoelectron spectroscopy (XPS) study of sputter deposited TiN as well as Auger electron spectroscopy (AES) show that oxynitrides are the predominant surface species on TiN. Two distinct oxynitride phases with different oxygen contents have been observed on TiN and the relative abundance of each phase appears to be a function of H2O and oxygen levels present during reactive sputtering.
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73.61.Ng Insulators
73.40.Cg Contact resistance, contact potential
68.60.-p Physical properties of thin films, nonelectronic
81.15.Cd Deposition by sputtering

Ti–N phases formed by reactive ion plating

J. M. Molarius, A. S. Korhonen, and E. O. Ristolainen

J. Vac. Sci. Technol. A 3, 2419 (1985); http://dx.doi.org/10.1116/1.572850 (7 pages) | Cited 9 times

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Thin Ti–N films were prepared by reactive triode ion plating. The nitrogen content was varied from 17 to 50 at. % nitrogen. Two series of experiments corresponding to differing values of deposition rate and cathode current density were carried out. The nitrogen depth profiles were analyzed using the nuclear resonance broadening (NRB) technique. The performance of the coatings was evaluated in cutting tests. The films corresponding to a high deposition rate showed columnar growth morphology and consisted of metastable α‐titanium and cubic titanium nitride. Dense and noncolumnar films approaching the structures predicted on the basis of the bulk phase diagram could be produced with a lower deposition rate and higher current density. The best cutting performance was obtained with substoichiometric films containing about 36 to 42 at. % N and consisting of a Ti+Ti2N structure. The lifetimes corresponding to critical crater wear in turning increased ninefold after coating with substoichiometric Ti+Ti2N film, while a threefold increase was observed after coating with stoichiometric TiN. Annealing at temperatures ranging from about 765 to 1175 K did not result in any major phase transformations, except at 40 at. % N, where transformation from α‐Ti to δ‐TiN was observed at 1175 K. The annealing did not greatly affect the cutting performance, which in some cases even decreased slightly after the heat treatment.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
68.60.-p Physical properties of thin films, nonelectronic
68.55.-a Thin film structure and morphology
81.30.-t Phase diagrams and microstructures developed by solidification and solid-solid phase transformations

Surface analysis of diffusion zones in multiple chemical vapor deposition coatings

R. L. Moore, L. Salvati, G. Sundberg, and V. Greenhut

J. Vac. Sci. Technol. A 3, 2426 (1985); http://dx.doi.org/10.1116/1.572851 (6 pages)

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In this investigation, a multilayer carbide coated cutting tool was examined. The cutting tool was produced through the sequential chemical vapor deposition (CVD) of TaC, TiC, Al2O3, and TiN layers over a WC/Co substrate. The purpose of this study was to characterize the interdiffusion of materials at each of the interfacial regions as a function of deposition conditions. To accomplish this, several surface analysis techniques were used including scanning Auger microscopy (SAM), scanning electron microscopy (SEM), and small spot x‐ray photoelectron spectroscopy (XPS). The samples were prepared using a modified lapping technique. The lapping angle used was ∼0.25°, which yielded at least a 250× expansion of the interfacial regions. This allowed interface characterization without instrumental resolution limitations. Scanning AES and small spot XPS were performed on interfaces to investigate interface chemistry and interdiffusion. Argon sputter depth profiling was also used to further characterize diffusion zone composition and dimension.
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66.30.Ny Chemical interdiffusion; diffusion barriers
81.15.Gh Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)
68.60.-p Physical properties of thin films, nonelectronic
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Summary Abstract: Grazing‐incidence x‐ray methods for the characterization of coatings and coating/substrate interfaces

S. M. Heald, J. M. Tranquada, H. Chen, and D. O. Welch

J. Vac. Sci. Technol. A 3, 2432 (1985); http://dx.doi.org/10.1116/1.572852 (2 pages) | Cited 1 time

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Abstract Unavailable
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07.85.-m X- and γ-ray instruments
78.66.-w Optical properties of specific thin films
78.67.-n Optical properties of low-dimensional, mesoscopic, and nanoscale materials and structures
78.70.-g Interactions of particles and radiation with matter
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Friction and wear properties of TiC–Al2O3 composite and Al2O3/TiC layered coatings

H. Memarian, R. C. Budhani, A. A. Karim, H. J. Doerr, C. V. Deshpandey, R. F. Bunshah, and A. Doi

J. Vac. Sci. Technol. A 3, 2434 (1985); http://dx.doi.org/10.1116/1.572853 (5 pages)

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The measurement of wear, the coefficient of static and dynamic friction and the hardness of TiC–Al2O3, and Al2O3/TiC coatings deposited on stainless steel and TiC precoated stainless steel substrates are reported. The results of the studies are compared with similar studies on TiC coatings deposited by the activated reactive evaporation (ARE) process. It has been found that the wear in both types of TiC–Al2O3 and Al2O3/TiC coatings is a sum total of abrasive and adhesive contributions. The values of the coefficients of friction are higher compared to stainless steel TiC ARE wear couple.
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46.55.+d Tribology and mechanical contacts
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy

Computational design of wear coatings

Bruce M. Kramer and Patrick K. Judd

J. Vac. Sci. Technol. A 3, 2439 (1985); http://dx.doi.org/10.1116/1.572854 (6 pages) | Cited 12 times

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Quantitative models for the relative abrasive and chemical dissolution wear rates of potential tool coating materials are presented. Inputs to the models include the free energy of formation of the tool material, the excess free energies of solution of the constituent elements of the tool material in the workpiece, the hardness of the coating, and the cutting temperature. The models have been implemented on a VAX 11/750 minicomputer to allow screening of candidate materials for improved wear coatings. Sample calculations are included and suggest that it may be possible to develop coatings with significantly better performance than current titanium nitride coatings.
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46.55.+d Tribology and mechanical contacts
81.20.-n Methods of materials synthesis and materials processing

Microstructural study of TiN‐coated threading taps

S. Vuorinen, E. Niemi, and A. S. Korhonen

J. Vac. Sci. Technol. A 3, 2445 (1985); http://dx.doi.org/10.1116/1.572855 (5 pages)

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Since the early 1980s TiN‐coated high‐speed steel (HSS) tools have become generally available in various cutting applications. Thin TiN‐coating layers are mostly deposited by various physical vapor deposition (PVD) methods including ion plating, reactive evaporation, arc erosion, or sputtering. In this work commercially available TiN‐coated taps were studied. Three series of different TiN‐coated taps were chosen for cutting tests where both cast iron and quenched and tempered steel were used as work materials. Microstructural characterization of the coatings was mainly carried out using transmission electron microscopy (TEM). Nitrogen depth profiles were determined accurately using nuclear resonance broadening (NRB). The PVD TiN‐coated tools showed distinctly different coating structures and thicknesses. Two of the coatings studied exhibited essentially stoichiometric TiN compositions throughout the whole coating layers. In the third coating the nitrogen content increased gradually, reaching the stoichiometric TiN in the immediate vicinity of the coating surface. These differences were clearly reflected in the microstructures of the coatings studied. The microstructural variations between individual coatings were, however, not clearly reflected in the performance of these coatings.
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68.55.-a Thin film structure and morphology
06.60.Vz Workshop procedures (welding, machining, lubrication, bearings, etc.)
68.60.-p Physical properties of thin films, nonelectronic

Fabrication of ceramic substrate‐reinforced and free forms by mandrel plasma spraying metal–ceramic composites

R. J. Quentmeyer, G. McDonald, and R. C. Hendricks

J. Vac. Sci. Technol. A 3, 2450 (1985); http://dx.doi.org/10.1116/1.572856 (6 pages)

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Components fabricated of, or coated with, ceramic have lower parasitic cooling requirements. Techniques are discussed for fabricating thin‐shell ceramic components and ceramic coatings for applications in rocket or jet engine environments. Thin ceramic shells with complex geometric forms involving convolutions and re‐entrant surfaces were fabricated by mandrel removal. Mandrel removal was combined with electroplating or plasma spraying and isostatic pressing to form a metal support for the ceramic. Rocket engine thrust chambers coated with 0.08 mm (3 mil) of ZrO2–8Y2O3 had no failures and a tenfold increase in engine life. Some measured mechanical properties of the plasma‐sprayed ceramic are presented.
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81.05.Ni Dispersion-, fiber-, and platelet-reinforced metal-based composites
81.05.Je Ceramics and refractories (including borides, carbides, hydrides, nitrides, oxides, and silicides)
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy

Film and interstitial formation of metals in plasma‐sprayed ceramics

R. C. Hendricks, G. McDonald, and R. L. Mullen

J. Vac. Sci. Technol. A 3, 2456 (1985); http://dx.doi.org/10.1116/1.572857 (3 pages)

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A method is described to electrodeposit noble metals such as platinum and ordinary metals such as copper on and within plasma‐sprayed ceramic materials and ceramic fiber materials. Low‐density ceramic fiber bodies were vacuum impregnated with plating solution and attached to an electrode. Light micrographs illustrating the density and location of deposited materials are presented and discussed. Voids in the plasma‐sprayed ceramic were filled with deposits that vary from spherical to lens‐shaped acircular and have particle size corresponding to the full range of void size. Multiple coatings of ceramic and metal can be sequenced.
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81.15.Lm Liquid phase epitaxy; deposition from liquid phases (melts, solutions, and surface layers on liquids)
68.55.-a Thin film structure and morphology

A comparison of low‐pressure arc and low‐pressure plasma sprayed titanium coatings

H.‐D. Steffens, E. Ertürk, and K.‐H. Busse

J. Vac. Sci. Technol. A 3, 2459 (1985); http://dx.doi.org/10.1116/1.572858 (5 pages) | Cited 1 time

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Titanium coatings for protection in chemical plants are required to withstand severe corrosion attack. Low‐pressure plasma spraying (LPPS) and low‐pressure arc spraying (LPAS) of titanium were investigated as a means of producing such coatings. Metallographic, mechanical examination, and x‐ray diffraction analyses of titanium coatings arc and plasma sprayed in a low pressure atmosphere, show that both coatings are dense and nearly free of contaminating phases. However, results of the comparison show that low‐pressure arc sprayed titanium coatings had lower hardness, lower interstitial gas content, higher bond strength with the substrate, and were sprayed with higher efficiency than the low‐pressure plasma sprayed titanium coatings.
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81.05.Bx Metals, semimetals, and alloys
68.60.-p Physical properties of thin films, nonelectronic
46.55.+d Tribology and mechanical contacts

Plasma spray deposition efficiencies

G. Wuest, S. Keller, A. R. Nicoll, and A. Donnelly

J. Vac. Sci. Technol. A 3, 2464 (1985); http://dx.doi.org/10.1116/1.572859 (5 pages)

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The plasma spraying of coatings on aeroengine components in an economic and consistent manner requires proper equipment selection, precise control of the plasma torch and component movement together with efficient deposition rates. The latter are achieved using careful control of the plasma parameters with respect to the design of the torch. Deposition experiments were carried out using thermal spray powders for the production of abradable, wear, and zirconia coatings. Attention was paid to component‐torch working distance, optimization of the plasma parameters, and powder–plasma interactions.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
52.75.-d Plasma devices

Vacuum plasma spraying of tantalum and niobium

E. Lugscheider, H. Eschnauer, B. Häuser, and D. Jäger

J. Vac. Sci. Technol. A 3, 2469 (1985); http://dx.doi.org/10.1116/1.572860 (6 pages) | Cited 1 time

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Vacuum plasma spraying is a suitable process for producing high quality coatings of reactive metals such as tantalum and niobium. Ta and Nb coatings used for corrosion protection must be extremely dense, homogeneous, and of high purity and adhesion. Hence, the process parameters have to be carefully optimized even with regard to the spraying powder, its grain size and morphology. Spraying equipment with vacuum systems which allow for a final pressure of 10−3 mbar, which have heated and evacuated powder feeder units, and heated substrates, as well as the use of powders with high purity and low gas content, are required for producing high quality Ta and Nb coatings. Corrosion tests in sulfuric acid and aqua regia at different concentrations show that Ta and Nb coatings sprayed under optimized conditions have high resistance to both general and localized corrosion.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
07.30.Kf Vacuum chambers, auxiliary apparatus, and materials
81.05.Bx Metals, semimetals, and alloys
81.15.Jj Ion and electron beam-assisted deposition; ion plating

Transmission electron microscopy characterization of plasma sprayed TiC coatings

D. Fournier, R. G. Saint‐Jacques, C. Brunet, and S. Dallaire

J. Vac. Sci. Technol. A 3, 2475 (1985); http://dx.doi.org/10.1116/1.572861 (4 pages) | Cited 1 time

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In plasma spraying of high melting point materials like TiC, complete fusion is difficult to obtain and also not always desirable. This paper reports the transmission electron microscopy (TEM) study of the microstructure relation between the melted and the unmelted material in the coating. TEM samples were prepared by ion beam milling of mechanically ground coatings. We found that, under our spraying conditions from which sound coatings were obtained, the original grain structure of the powder was partially retained in the deposited coatings. The average particle size of the powder was ∼40 μm and scanning electron microscopy (SEM) observations indicated that these particles had a grain size of ∼10 μm. TEM study of the coatings showed two families of grain sizes. The first one is similar to that of the starting powder, i.e., 30 μm aggregates of ∼10 μm grains. This indicates that the core of many of the particles did not melt during the plasma spraying process. The second family consists of regions of ∼0.2 μm grains surrounding the 30–40 μm aggregates. This region has crystallized from the melted layer around the particles or from melted small particles. In addition, the plasma spraying process caused an important lowering of C/Ti. This was found by crystal lattice measurements using x‐ray diffraction.
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68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

Tungsten carbide phase transformation during the plasma spray process

D. Tu, S. Chang, C. Chao, and C. Lin

J. Vac. Sci. Technol. A 3, 2479 (1985); http://dx.doi.org/10.1116/1.572862 (4 pages) | Cited 1 time

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Tungsten carbide coatings applied by the plasma spray process have been widely used in wear applications. In the W–C–Co ternary system, tungsten carbide can either be present as WC or W2C. Frequently WC transforms into W2C during the plasma spray process. In this study, tungsten carbide/17% cobalt coatings were applied by both the air plasma and the vacuum plasma spray processes using different power levels and plasma gases. The W2C phase was found by X‐ray diffraction techniques in the air plasma sprayed coatings. Decarburizing of the WC in the presence of the oxygen took place in the plasma. In this study air plasma sprayed coating hardness and microstructure are superior to those of the vacuum plasma sprayed ones. However the vacuum plasma coatings were found to be more wear and impact resistance than the air plasma coatings. This performance difference may be attributed to the presence of hard and brittle W2C phase in the air plasma sprayed tungsten carbide coatings.
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64.70.K- Solid-solid transitions
68.60.-p Physical properties of thin films, nonelectronic
81.40.Pq Friction, lubrication, and wear
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy

Plasma sprayed WC–Co coatings: Influence of spray conditions (atmospheric and low pressure plasma spraying) on the crystal structure, porosity, and hardness

M. E. Vinayo, F. Kassabji, J. Guyonnet, and P. Fauchais

J. Vac. Sci. Technol. A 3, 2483 (1985); http://dx.doi.org/10.1116/1.572863 (7 pages) | Cited 8 times

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Ten WC–Co (12, 17, and 20 wt.% Co) powders manufactured by different techniques (sintering, atomization, coating) were studied. Both open atmosphere Ar–H2 plasma spraying and controlled atmosphere Ar–He chamber plasma spraying were performed. Pressures of 60, 150, 400, and 700 Torr were employed. To optimize controlled atmosphere spray conditions, particles splatted on glass slides rapidly traversing the jet at different distances from the nozzle exit were studied. The melting conditions were determined as a function of the plasma power level, the particle composition, and structure for particles with the same size distribution. Crystal structure analysis showed a strong decomposition of the carbides when sprayed in open atmosphere. Less decomposition occurred in the coated or atomized particles. The decomposition was reduced and coating density increased by reduced pressure spraying. The best results were obtained at 60 Torr. The hardness depended on the cobalt content, the degree of decomposition and on the density of the coatings.
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81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties
81.20.-n Methods of materials synthesis and materials processing

On plasma sprayed WSi2 and Cr3C2–Ni coatings

O. Knotek, R. Elsing, and H.‐R. Heintz

J. Vac. Sci. Technol. A 3, 2490 (1985); http://dx.doi.org/10.1116/1.572864 (4 pages)

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WSi2 and Cr3C2–Ni composite powders were applied to AISI 321 and 347, and Nimonic 80 A substrates by the plasma spray process in a nontransferred arc mode. The adhesive shearing strength, the adhesive tensile strength, and the fatigue resistance of the coatings were evaluated. The wear properties of the two coatings on AISI 347 and pin‐on‐disk tests were compared. Corrosion resistance of the two coatings was determined in 1n‐H2SO4 by current density‐potential diagrams.
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46.55.+d Tribology and mechanical contacts
46.50.+a Fracture mechanics, fatigue and cracks
81.65.-b Surface treatments
81.40.Np Fatigue, corrosion fatigue, embrittlement, cracking, fracture, and failure

Structure‐thermal properties—relationship in plasma sprayed zirconia coatings

Lech Pawlowski, Didier Lombard, and Pierre Fauchais

J. Vac. Sci. Technol. A 3, 2494 (1985); http://dx.doi.org/10.1116/1.572865 (7 pages) | Cited 2 times

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Plasma sprayed coatings of zirconia stabilized with 7, 8, and 20 wt.% of yttria were investigated. The microstructure of the coatings was characterized by optical microscopy and x‐ray diffraction. The thermal properties of the coatings, i.e., thermal diffusivity, thermal dilatation, specific heat, and resulting thermal conductivity were determined for each zirconia coating and the results were correlated with the microstructure.
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61.66.Fn Inorganic compounds
65.40.-b Thermal properties of crystalline solids
65.60.+a Thermal properties of amorphous solids and glasses: heat capacity, thermal expansion, etc.
65.80.-g Thermal properties of small particles, nanocrystals, nanotubes, and other related systems
65.40.De Thermal expansion; thermomechanical effects
66.70.-f Nonelectronic thermal conduction and heat-pulse propagation in solids; thermal waves

Summary Abstract: Quantitative phase analysis of partially stabilized zirconia −8.5% yttria by a random fitting least chi‐squared method

Ichiro Sone, R. D. Sisson, and R. R. Biederman

J. Vac. Sci. Technol. A 3, 2501 (1985); http://dx.doi.org/10.1116/1.572822 (2 pages)

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Abstract Unavailable
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64.70.K- Solid-solid transitions
61.05.C- X-ray diffraction and scattering
81.40.Np Fatigue, corrosion fatigue, embrittlement, cracking, fracture, and failure
65.40.De Thermal expansion; thermomechanical effects

Behavior of plasma‐sprayed TiC coatings under electron beam thermal shocks

C. Brunet, S. Dallaire, and R. G. St‐Jacques

J. Vac. Sci. Technol. A 3, 2503 (1985); http://dx.doi.org/10.1116/1.572823 (3 pages)

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Within the framework of a research program on materials for fusion machine, plasma‐sprayed TiC coatings over Inconel 625 substrates were investigated. In order to evaluate the potential of these coatings in fusion environment, the existing thermal flux conditions on limiters of tokamaks are simulated with an electron beam thermal shock experiment. TiC coatings sprayed in air show severe damages when exposed to 2.5  kW  cm−2, 1.0  s, heat pulses. Coatings sprayed in an inert gas enclosure withstood 3.0 kW cm−2, 1.0 s, heat pulses without melting. Surface melting and subsurface crystal growth are observed in the case of coatings sprayed in air.
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61.80.Fe Electron and positron radiation effects
66.70.-f Nonelectronic thermal conduction and heat-pulse propagation in solids; thermal waves
28.52.-s Fusion reactors
64.70.D- Solid-liquid transitions

An acceleration method for measuring the adherence of plasma‐sprayed coatings at elevated temperatures

S. D. Brown and M. K. Ferber

J. Vac. Sci. Technol. A 3, 2506 (1985); http://dx.doi.org/10.1116/1.572824 (3 pages)

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Presently, no satisfactory method for measuring the coating–substrate adherence in plasma‐sprayed ceramic–metal systems exists. Conventional pull‐off methods must rely upon adhesives or other means of attachment that become unreliable at elevated temperatures. Nevertheless, an accurate method for determining the adherence of plasma‐sprayed coatings to their substrates at elevated temperatures would be useful. Many applications of such coatings are in high‐temperature environments. An acceleration method reported in 1957 by May, Smith, and Snow for organic coatings has been analyzed and found promising, in modified form, for the determination of coating–substrate adherence of plasma‐sprayed coatings. Calculations indicate that adherences as high as 103 MPa (15 000 psi) should be measurable. Moreover, the modified scheme appears easily adaptable to the making of adherence measurements at elevated temperatures. Unlike pull‐off tests, the method is not dependent upon the thermal stability or properties of any adhesive or braze alloy. The relevant literature is reviewed. Our analysis is presented along with a schematic representation of the apparatus now under construction.
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46.55.+d Tribology and mechanical contacts

Coating requirements in gas turbine engines

G. W. Meetham

J. Vac. Sci. Technol. A 3, 2509 (1985); http://dx.doi.org/10.1116/1.572825 (7 pages)

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The complex thermal, chemical, and mechanical environment of the gas turbine engine makes it extremely difficult for one material to meet all of the different requirements imposed on the various engine components. Coatings are thus required to provide corrosion, resistance, wear resistance, insulation, and abradability. In the turbine section of the engine, in particular, the overall operating conditions are becoming progressively more hostile in terms of temperature and mechanical environment as engine efficiency and performance are improved. In certain types of operation the corrosive environment is emphasized. Thus, coatings must provide increasing protection, the need for which is often aggravated by the limitations which considerations such as strength requirements may place on the inherent environmental resistance of the base material. Perceived future coating needs are discussed. It is probably only in the last decade that coating requirements, in terms of application and behavior, have been recognized as an essential aspect of the design process. Significant future work remains to be done and this aspect is also discussed.
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89.40.-a Transportation
68.60.-p Physical properties of thin films, nonelectronic
81.40.Pq Friction, lubrication, and wear

Flame rig testing of thermal barrier coatings and correlation with engine results

G. Johner and K. K. Schweitzer

J. Vac. Sci. Technol. A 3, 2516 (1985); http://dx.doi.org/10.1116/1.572826 (9 pages)

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To minimize detrimental thermal stresses in high‐performance aeroengines, attempts are made to protect hot components, e.g., combustion chambers, blades, vanes, etc., with plasma‐sprayed zirconia coatings. In the present evaluation, the best coating material is first defined using an appropriate rig test. Two different types of test rig, one simulating mainly thermal fatigue stresses and the other centrifugal stresses, are described in detail. The results obtained in each rig with thermal barrier coatings of different chemical composition are also discussed. For the application of thermal barrier coatings in aeroengines, it is necessary to analyze the main stresses on the component to be coated. The paper uses a turbine vane and a blade as examples. In addition, another flame rig is presented which permits the simulation of stresses very similar to those in jet engines. The results of these tests are compared with the behavior of thermal barrier coatings on turbine blades and vane segments in a production‐type engine.
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68.60.-p Physical properties of thin films, nonelectronic

Summary Abstract: Performance evaluation of coatings for jet engine turbine blades by servicelike tests

K. K. Schweitzer and G. Johner

J. Vac. Sci. Technol. A 3, 2525 (1985); http://dx.doi.org/10.1116/1.572827 (1 page)

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Abstract Unavailable
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68.60.-p Physical properties of thin films, nonelectronic
81.70.-q Methods of materials testing and analysis
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties

Experience with MCrAl and thermal barrier coatings produced via inert gas shrouded plasma deposition

T. A. Taylor, M. P. Overs, B. J. Gill, and R. C. Tucker

J. Vac. Sci. Technol. A 3, 2526 (1985); http://dx.doi.org/10.1116/1.572828 (6 pages) | Cited 3 times

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Plasma spray deposition of MCrAlY coatings for corrosion resistance and rub tolerance on gas turbine blades, vanes and seal surfaces has received a great deal of attention in recent years. While most of the literature has described coatings produced with low pressure spray systems, substantial advantages can be realized using inert gas shrouded torches operating in the open air. This paper discusses some of these advantages and describes the coatings produced with efficient argon shrouded torches. In addition, specific examples of production MCrAlY and thermal barrier coatings are given.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
52.75.-d Plasma devices
72.15.Eb Electrical and thermal conduction in crystalline metals and alloys

Performance comparison of plasma spray and physical vapor deposition BC23 coatings in the LM2500

David J. Wortman

J. Vac. Sci. Technol. A 3, 2532 (1985); http://dx.doi.org/10.1116/1.572829 (5 pages)

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Operation of U. S. Navy Component Improvement Program LM2500 engines on the GTS Callaghan has provided an at‐sea test bed for evaluation of hot corrosion on gas turbine engine components. In a presentation at a previous International Conference on Metallurgical Coatings, (ICMC), comparison of several coatings applied by physical vapor deposition (PVD) techniques were compared after LM2500 service. A three‐step coating BC23 consisting of PVD CoCrAl followed by codeposition of hafnium and aluminum and an electroplated platinum layer was identified as the most corrosion‐resistant coating of several PVD coatings tested. In this paper, a plasma sprayed version of BC23 is compared to the three‐step BC23 coating on LM2500 Stage 2 HPT blades from the GTS Callaghan. The plasma sprayed coating PBC23 was produced by an argon‐shrouded plasma spray process using prealloyed CoCrAlHfPt powder. The results showed that in this application, where low temperature hot corrosion (type 2) is the predominant mode of corrosion, the plasma sprayed coatings had less attack. These results are compared to laboratory hot corrosion tests and microprobe analysis to explain the improved corrosion resistance of PBC23.
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81.05.Bx Metals, semimetals, and alloys

Hot corrosion behavior of low pressure plasma sprayed NiCoCrAlY+Ta coatings on nickel base superalloys

M. Frances, P. Steinmetz, J. Steinmetz, C. Duret, and R. Mevrel

J. Vac. Sci. Technol. A 3, 2537 (1985); http://dx.doi.org/10.1116/1.572830 (8 pages) | Cited 2 times

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The hot corrosion behavior of NiCoCrAlY+Ta coatings obtained by low‐pressure plasma spraying has been investigated (type I hot corrosion with T=850 °C). These coatings have been deposited on two nickel‐base superalloys and on a cast alloy of the same composition as the coating. Comparison of the cyclic oxidation behavior at 850 °C between the sprayed coating and the cast alloy shows that the sprayed material exhibits a satisfactory and higher resistance than the cast alloy. In the latter case, repeated spalling of the oxide scale results from fractures often associated with Y‐rich oxide protrusions. Hot corrosion experiments (salt‐spraying test with T=850 °C and thermal cycling in air every hour) have been conducted on two cast alloys, NiCoCrAl+Ta and NiCoCrAlY+Ta. The Y‐containing alloy has a better corrosion resistance than the other alloy which is subject to extensive oxide spallation. In both cases, morphologies typical of basic fluxing processes, involving Cr, Al, Y, and Ta can be observed in highly attacked zones. Finally, tests on plasma sprayed coatings show a high resistance to hot corrosion of these coatings, regardless of the substrate used: a fine adherent alumina layer is formed, and only a limited fluxing of Cr, Al, and Y takes place. The quite different results obtained on cast and sprayed alloys imply that data relative to cast alloys can be unreliable when one wants to predict high temperature behavior and especially lifetimes of overlay coatings.
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81.05.Bx Metals, semimetals, and alloys

Resistance of tantalum and columbium coatings to propellant gas erosion

H. Grabatin, V. Schlett, H. Stuke, and H. Weiss

J. Vac. Sci. Technol. A 3, 2545 (1985); http://dx.doi.org/10.1116/1.572831 (6 pages) | Cited 3 times

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Alloy steel tubes of 70 mm length and 20 mm bore diameter were coated with tantalum or niobium by the wire explosion technique. This process uses the energy of an electric current pulse to melt or vaporize the coating material which is in the form of a wire in the center of the tube, and to deposit it on the bore surface. For testing, these tubes were mounted as outlet nozzles on a vented vessel and subjected to propellant gas pulses of 30 ms duration and 2500 K. The pressure buildup inside the vessel was 1000 bar. After each pulse the erosive wear of the test pieces was determined and after testing the reaction zone of the coatings was sputtered to a depth of 2 μm and analyzed by AES and SIMS during the process. Both coating materials showed excellent adhesion and their erosion resistance proved superior to the unprotected alloy steel. Tantalum, however, exhibited a much better performance than niobium. This was due to the different properties of the gas/metal reaction layers formed. In both cases the bore surface was covered with propellant gas residue of 1 μm thickness, that was built up and carried out with each pulse. Underneath, a layer consisting of Ta2O5 or Nb2O5 was formed. While Ta2O5 was mechanically stable and therefore, built up to a considerable thickness providing good protection, the Nb2O5 layer was formed and removed continuously with every round. This pattern exposed the unprotected Nb to the next pulse and caused a much faster wear rate.
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81.05.Bx Metals, semimetals, and alloys
46.55.+d Tribology and mechanical contacts
81.40.Pq Friction, lubrication, and wear

Pretreatment effects on the morphology and properties of aluminum oxide thermally grown on NiCoCrAlY

S. Prakash, R. C. Budhani, H. J. Doerr, C. V. Deshpandey, and R. F. Bunshah

J. Vac. Sci. Technol. A 3, 2551 (1985); http://dx.doi.org/10.1116/1.572832 (6 pages)

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This report is part of the investigation on thin film temperature sensors for turbine blade applications. The effect of pretreatments on the morphology and properties of aluminum oxide thermally grown from NiCoCrAlY was investigated. The goal was to optimize process steps to produce a highly adherent, continuous, and insulating aluminum oxide. Two pretreatments were carried out, one in vacuum (∼10−4 Torr) at 1350 K for 5 h, and the other consisting of deposition of a 1 μm thick Al2O3 film by ARE (activated reactive evaporation). Samples were subsequently oxidized thermally at 1000 °C for 50 h at 0.5 Torr oxygen pressure. The two pretreatments were carried out on electron‐beam evaporation NiCoCrAlY, ∼120 μm thick, deposited on a superalloy turbine blade substrate. The results showed that the thermally grown oxide was significantly different in microstructure, surface topography and in its adherence to the NiCoCrAlY for the two pretreatments. Optimum results were obtained by combining the two pretreatments to produce an adherent, continuous, and insulating oxide film on the NiCoCrAlY coated superalloy substrate.
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81.40.Gh Other heat and thermomechanical treatments
46.55.+d Tribology and mechanical contacts
81.05.Bx Metals, semimetals, and alloys
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Surface morphology of platinum modified aluminide coatings

D. H. Boone, P. Deb, L. I. Purvis, and D. V. Rigney

J. Vac. Sci. Technol. A 3, 2557 (1985); http://dx.doi.org/10.1116/1.572833 (7 pages)

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The processing variables which lead to the rough, convoluted surface topologies of platinum modified aluminide coatings were studied. Platinum deposition techniques such as electroplating, ion plating, and sputtering were examined as were postplating diffusion treatments and aluminizing processes. It was found that while the initial Pt surface could be varied by the deposition process and procedures selected, the principal factor influencing surface topology was Pt substrate (IN‐738) interdiffusion. Subsequent aluminizing processing had a much smaller additional effect. The effects of the surface roughness and phases and porosity found in the Pt layer on subsequently aluminized coatings performance are not known.
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68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Scanning electron microscope analysis of the microstructure of aluminide diffusion coatings on Ni–Cr alloys

Nimal deLanerolle and L. L. Siegle

J. Vac. Sci. Technol. A 3, 2564 (1985); http://dx.doi.org/10.1116/1.572834 (5 pages)

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Using energy dispersive spectroscopy, a microanalytical study of the coating microstructures in a series of pack‐aluminized Ni–15Cr to Ni–35Cr alloys was performed, in order to obtain a more precise chemical analysis of the constituents that can be obtained using the electron microprobe. Composition determinations close to the α/β and α+β/γ phase boundaries were made, as well as across precipitates and the matrix. It was possible to determine the concentration of individual phases present in the diffusion zone of the coatings in the above alloys. It was found that the nonisolated α‐Cr lamellar precipitates had a Cr concentration about 95 at. %, whereas the isolated α‐Cr had around 60 at. %. Composition traverses on the γ‐phase agrees well with the available NiCrAl phase diagram at 1025 °C.
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68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
66.30.-h Diffusion in solids
64.70.K- Solid-solid transitions

The use of ion implantation techniques to study protective oxide scale adherence effects

J. G. Smeggil, E. L. Paradis, A. J. Shuskus, and N. S. Bornstein

J. Vac. Sci. Technol. A 3, 2569 (1985); http://dx.doi.org/10.1116/1.572835 (5 pages) | Cited 5 times

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Data supporting a new mechanism to account for the beneficial effects of active elements such as yttrium on the adherence of protective alumina scales is presented. Previous work involving cast alloys had shown that, in the absence of yttrium, indigenous sulfur at tramp levels segregated to and weakened the bond between the scale and the underlying metal. Yttrium interacted with sulfur to form refractory compounds, thereby reducing the amount of sulfur available for segregation. In this study, the ion implantation of 27Al+ and 32S+ was used to modify alloy chemistries of Ni–Cr–Al–Y alloys. Results of oxidation tests on implanted alloys confirmed the role of yttrium in inhibiting interface segregation of sulfur. Al+ ion implantation did not modify the adherence of alumina scales on Ni–Cr–Al–Y alloys, thereby ruling out radiation damage effects. However, S+ implantation caused scale exfoliation.
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81.05.Bx Metals, semimetals, and alloys
61.72.U- Doping and impurity implantation
61.80.Jh Ion radiation effects
66.30.J- Diffusion of impurities

Role of dispersed oxides in reducing substrate/coating interdiffusion

Krishan L. Luthra

J. Vac. Sci. Technol. A 3, 2574 (1985); http://dx.doi.org/10.1116/1.572836 (4 pages)

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Theoretical calculations have been performed to evaluate the usefulness of dispersed oxides in a barrier layer in reducing substrate/coating interdiffusion. The important variables influencing interdiffusion are (1) the ratio of the thickness of the barrier layer to the total coating, (2) the volume fraction of oxides in the barrier layer, and (3) a tortuosity factor that depends on the distribution of oxides in the barrier layer. The results of calculations suggest that it may be possible to increase the operating life by a factor of up to about 2.5 or increase the operating temperature by a maximum of about 75 °C in systems where life is limited by substrate/coating interdiffusion.
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66.30.Ny Chemical interdiffusion; diffusion barriers

Platinum aluminide coating structural effects on hot corrosion resistance at 900 °C

P. Deb, D. H. Boone, and R. Streiff

J. Vac. Sci. Technol. A 3, 2578 (1985); http://dx.doi.org/10.1116/1.572837 (4 pages)

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Studies have shown that platinum modified aluminide coatings can exhibit a range of structural variations depending on initial platinum thickness, prealuminizing heat treatment, aluminizing cycle, and postcoating heat treatment. It had been speculated earlier that such structural variation could account at least in part for some of the reported variation of performance of these coatings. A series of archetype structures was prepared on IN738 by two aluminizing processes: (i) low aluminum activity and (ii) high aluminum activity; and tested at 900 °C under conditions producing so called Type I high temperature hot corrosion. The results of the present investigation showed that the addition of platinum greatly improved the hot corrosion resistance. It is observed that the low aluminum activity process has better corrosion resistance than that of the high aluminum activity process. It is also found that the surface degradation of both aluminizing processes is quite severe when the specimens were given prolonged prealuminizing diffusion heat treatment. Microstructural observation revealed a significant difference in coating thickness in both the processes and it depends on prealuminizing diffusion and the subsequent aluminizing treatment employed.
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81.05.Bx Metals, semimetals, and alloys
81.40.Gh Other heat and thermomechanical treatments
68.55.-a Thin film structure and morphology

Thermal and sputtered aluminum oxide coatings for high temperature electrical insulation

Kenneth G. Kreider and Stephen Semancik

J. Vac. Sci. Technol. A 3, 2582 (1985); http://dx.doi.org/10.1116/1.572838 (6 pages) | Cited 2 times

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Aluminum oxide coatings have been investigated as electrically insulating layers for mounting thin film Pt–Pt/Rh thermocouples on gas turbine blade and vane alloys (MAR M200 + Hf and MAR M509). Thermal oxides were grown directly onto NiCoCrAlY and FeCrAlY coatings on these alloys at temperature between 1300 and 1400 K in oxygen partial pressures 10−7 to 2×104 Pa. Although these thermal oxides exhibited good adherence, analytical characterizations using electron and optical microscopy, as well as x‐ray photoelectron spectroscopy (XPS) showed that they had defects and impurities which limited their insulating ability. The insulating quality of the coating was greatly improved however by reactively sputtering an aluminum oxide film over the thermal oxide. Results are presented on the electrical performance of the 2–5 μm thick composite layers for temperatures up to 1300 K.
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73.61.Ng Insulators
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic
81.05.Bx Metals, semimetals, and alloys

A wavy versus straight interface in the explosive welding of aluminum to steel

A. Szecket, O. T. Inal, D. J. Vigueras, and J. Rocco

J. Vac. Sci. Technol. A 3, 2588 (1985); http://dx.doi.org/10.1116/1.572839 (6 pages)

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Waveless, explosively welded interfaces between aluminum and steel are seen to be devoid of intermetallic formation and maintain integrity with heat exposures of up to 8 h at 550 °C. Microhardness determinations as well as tensile testing of the samples indicate the interface to be a zone of higher hardness than the weaker of the bonded materials (Al‐1100) and of extremely high adhesion strength. The hardness profiles taken were utilized to determine the difference in the energy deposited at the wavy and waveless interface as well as the presence of extraneous byproducts of these energies in the respective interfaces. The study conclusively shows the superior characteristics of the waveless interface for this weld and its resistance to intermetallic formation that would lead to the consequential deterioration of the associated adhesion properties of these transition joints.
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68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics
81.05.Bx Metals, semimetals, and alloys
46.55.+d Tribology and mechanical contacts

Summary Abstract: Structural analysis of ultrathin epitaxial films

L. C. Feldman

J. Vac. Sci. Technol. A 3, 2594 (1985); http://dx.doi.org/10.1116/1.572840 (2 pages)

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68.55.-a Thin film structure and morphology

Interfacial sharpnesses and thicknesses of layers in a GaAs0.2P0.8/GaP strained‐layer superlattice measured by Auger sputter profiling

M. B. Chamberlain and W. O. Wallace

J. Vac. Sci. Technol. A 3, 2596 (1985); http://dx.doi.org/10.1116/1.572841 (4 pages) | Cited 1 time

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The interfacial sharpnesses and thicknesses of the layers in a strained‐layer superlattice were measured using Auger sputter profiling. The 950‐nm‐thick SLS laminate was fabricated by organometallic chemical vapor deposition and it consisted of 24 alternating layers of GaAs0.2P0.8 and GaP. The Auger sputter profile through these layers measured the intensity of the P LMM Auger emission plotted as a function of time sputtering through the layers with a 700‐eV Ar‐ion beam. The average layer thickness measured was 39.6 nm with a standard deviation of 1.1 nm. The measured depth resolution was 0.7% at a sputtered depth of 950 nm, which is as good as the best values of 1%–10% reported at this depth in profiles of amorphous specimens. The superb depth resolution measured here is attributed to the following characteristics of the SLS material: a very low surface roughness; a uniform crystal structure throughout the SLS laminate even though the lattice constant changes between adjacent layers; a very pure material; and an absence of misfit dislocations near the area profiled.
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68.60.-p Physical properties of thin films, nonelectronic
68.55.-a Thin film structure and morphology
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Determination of film stresses during sputter deposition using an in situ probe

D. W. Hoffman and C. M. Kukla

J. Vac. Sci. Technol. A 3, 2600 (1985); http://dx.doi.org/10.1116/1.572842 (5 pages) | Cited 1 time

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Previous work has established that the internal stresses and physical properties of sputter‐deposited metals can be markedly affected by relatively small changes in the sputtering process. For instance, lowering the gas pressure or raising the discharge current can reverse the stress from tensile to compressive and, at the same time, produce more bulklike properties in the resultant coatings. Consequently, film stress observations can be utilized to map out the nature of the material produced in a given coating process and locate the boundary of the bulklike deposition regime as a function of process parameters. A principal obstacle to the implementation of this technique has been the laborious procedure of generating individual samples over a matrix of different process conditions. Residual film stresses were then determined by observing the resulting curvature of the thin substrates. In the present work substrate deflection was sensed capacitively using a miniature probe that was inserted into the deposition chamber and monitored in a remote manner. The probe signal was linear with film thickness, enabling detection of intrinsic stress in molybdenum layers as thin as 30 nm with sensitivity undiminished by multiple applications. The known compressive‐to‐tensile stress transition was accurately reproduced by the probe with significant additional detail. Effects of discharge current, source proximity, and argon flow conditions in shifting the stress transition were readily mapped out.
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68.60.-p Physical properties of thin films, nonelectronic

Explosive welding of Ti–6Al–4V to mild‐steel substrates

O. T. Inal, A. Szecket, D. J. Vigueras, and H‐r. Pak

J. Vac. Sci. Technol. A 3, 2605 (1985); http://dx.doi.org/10.1116/1.572843 (5 pages) | Cited 2 times

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Ti–6Al–4V sheets were explosively welded to mild steel base plates with an attachment zone that approximates a straight, waveless interface devoid of vorticity and thus the attendant formation of the Fe–Ti intermetallics. The welded interface is seen to be harder than either of the bi‐alloys joined and the attachment strength, measured in terms of shear stress required for fracture of the weld zone, is seen to be stronger than the weaker of the materials (mild steel) joined. Stress relief treatments given at 525 °C is seen to induce ductility to the brittle interface without the introduction of recrystallization and/or the formation of Fe–Ti intermetallics at the weld zone. Approximate energy calculations indicate that explosively induced welds that comprise a nearly straight interface make efficient use of the detonation introduced energy, and thus the plastic straining of the alloys adjacent to the weld are minimal as confirmed by the microhardness and tensile test data obtained on the as‐welded and stress relieved samples.
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06.60.Vz Workshop procedures (welding, machining, lubrication, bearings, etc.)
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics
81.40.Lm Deformation, plasticity, and creep
81.40.Np Fatigue, corrosion fatigue, embrittlement, cracking, fracture, and failure

Summary Abstract: Nucleation and growth studies in polycrystalline films by ultrahigh vacuum in situ transmission electron microscopy

P. B. Barna

J. Vac. Sci. Technol. A 3, 2610 (1985); http://dx.doi.org/10.1116/1.572797 (2 pages)

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68.55.-a Thin film structure and morphology
07.79.Cz Scanning tunneling microscopes
61.05.-a Techniques for structure determination

Preparation and characterization of beryllium coatings

A. K. Dua, R. P. Agarwala, and P. B. Desai

J. Vac. Sci. Technol. A 3, 2612 (1985); http://dx.doi.org/10.1116/1.572798 (6 pages) | Cited 1 time

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The application of low Z coatings on various structurally strong components of a controlled thermonuclear tokamak fusion reactor is expected to reduce the plasma contamination and power loss. With this view, coatings of beryllium have been given on different substrates like (304 and 316) stainless steel, monel‐400, molybdenum, copper, and graphite in a specially designed vacuum deposition unit employing physical vapor deposition technique, and its morphology studied as a function of deposition parameters such as substrate temperature, coating thickness, deposition rate, and angle of deposition. It has been characterized using various analytical techniques. Its morphology has been studied with the help of a scanning electron microscope. Coating adherence and hardness have been measured. Results obtained have been analyzed and discussed.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
28.52.-s Fusion reactors
46.55.+d Tribology and mechanical contacts

Metastable solid solutions in vapor deposited Cu–Cr, Cu–Mo, and Cu–W thin films

A. G. Dirks and J. J. van den Broek

J. Vac. Sci. Technol. A 3, 2618 (1985); http://dx.doi.org/10.1116/1.572799 (5 pages) | Cited 9 times

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The equilibrium phase diagrams of Cu–Cr, Cu–Mo, and Cu–W show no measurable solid solubility except for a small solubility of Cr in solid Cu at higher temperatures. Even in the liquid state, the mutual solubilities in these systems are very limited. Simultaneous vapor deposition of elements on unheated substrates was used to produce alloy films covering the complete composition range of those three binary alloy systems. The films were characterized with the help of x‐ray diffraction, transmission electron microscopy, and electron diffraction. In fcc Cu films, at least 10 at.% Cr, Mo, or W may be dissolved, whereas the bcc Cr, Mo, or W alloy films may accommodate at least 40 at.% Cu; the fcc and bcc solid solutions are separated by narrow two‐phase fields. We further measured the composition dependence of the internal stress and of the electrical resistivity. Discontinuities in the measured curves generally coincide with the presence of phase boundaries in the (metastable) alloy films.
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64.75.-g Phase equilibria
81.30.Bx Phase diagrams of metals, alloys, and oxides
68.60.-p Physical properties of thin films, nonelectronic
73.61.At Metal and metallic alloys

A transmission electron microscopy study of rf‐ and dc‐magnetron‐sputtered thin film chromium and chromium–platinum coatings

M. R. Fishkis, R. D. Sisson, and R. R. Biederman

J. Vac. Sci. Technol. A 3, 2623 (1985); http://dx.doi.org/10.1116/1.572800 (4 pages)

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Microstructural features of sputtered chromium and chromium‐50 wt.% platinum thin films on carbon substrates are presented. Films produced by rf sputtering and dc magnetron sputtering are compared using analytical electron microscopy techniques. All rf‐sputtered films are uniform in chemistry and thickness and are amorphous. The chromium film became crystalline with a grain size of less than 100 Å after a 320 °C heat treatment for 1 h. The chromium‐50 wt. % platinum film remained amorphous after the same heat treatment. The as‐sputtered dc magnetron chromium film was crystalline.
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68.55.-a Thin film structure and morphology
81.40.Gh Other heat and thermomechanical treatments
81.15.Cd Deposition by sputtering
07.79.Cz Scanning tunneling microscopes
61.05.-a Techniques for structure determination

Summary Abstract: Mechanisms of polymerization in discharges of fluorocarbons

Riccardo d’Agostino

J. Vac. Sci. Technol. A 3, 2627 (1985); http://dx.doi.org/10.1116/1.572801 (2 pages) | Cited 2 times

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82.35.-x Polymers: properties; reactions; polymerization
52.80.-s Electric discharges
82.40.-g Chemical kinetics and reactions: special regimes and techniques

29Si nuclear magnetic resonance study of plasma‐polymerized hexamethyldisiloxane

R. A. Assink, A. K. Hays, R. W. Bild, and B. L. Hawkins

J. Vac. Sci. Technol. A 3, 2629 (1985); http://dx.doi.org/10.1116/1.572802 (5 pages) | Cited 5 times

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The structure of plasma‐polymerized hexamethyldisiloxane (PP‐HMDSO) was studied by 29Si nuclear magnetic resonance (NMR) using magic angle spinning and cross‐polarization techniques. Spectra of the PP‐HMDSO were recorded before and after it had been subjected to successive heat treatments in air at 100, 200, and 300 °C. The spectra exhibit major peaks at +11 ppm, −18 ppm, −55 to −64 ppm, and −99 to −106 ppm with respect to tetramethylsilane. These shifts correspond to silicon bonded to one, two, three, and four oxygens, respectively. The broadness of the tri‐ and tetrafunctional silicon peaks is attributed to SiOH or SiOCH3 functional groups in addition to the normal SiOSi moieties. Minor peaks at −5 and −33 ppm are attributed to mono‐ and difunctional silicons in which one of the methyl groups has been replaced by a hydrogen. As the material is heat treated there is a tendency for the PP‐HMDSO to form additional silicon–oxygen bonds. Spectra simulations show that the oxygen content increases from 16 to 30 wt. % during the course of the heat treatment. The silicon to oxygen weight percent ratios measured by NMR spectra simulation and neutron activation analysis are comparable and decrease monotonically as the heat treatment progresses.
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36.20.Hb Configuration (bonds, dimensions)
36.20.Kd Electronic structure and spectra
76.60.-k Nuclear magnetic resonance and relaxation
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties

Synthesis and characterization of zinc thin films formed in a glow discharge

W. J. James and Pei‐Li Tseng

J. Vac. Sci. Technol. A 3, 2634 (1985); http://dx.doi.org/10.1116/1.572803 (5 pages) | Cited 3 times

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The synthesis of continuous pinhole‐free, mirrorlike, thin (<2000 Å) crystalline zinc films is affected by introducing diethyl zinc vapor into an inductively coupled, rf glow discharge reactor. The deposition rate profile of films formed on the back sides of the glass substrates is strongly correlated with the shape of the plasma waves, which in turn is dependent upon the reactor operating parameters, in particular the ratio of power to the initial system pressure, W/P0. Those Zn films which are highly reflective and exhibit sharp x‐ray diffraction spectra appear to be virtually free of carbon when examined by Auger–ESCA spectroscopy. Sheet electrical conductivities of these films exhibit values approaching those of bulk metal zinc, namely, 104Ω−1 cm−1.
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68.55.-a Thin film structure and morphology
78.66.Bz Metals and metallic alloys
73.61.At Metal and metallic alloys
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy

Characterization of plasma deposited halocarbon polymer films containing small gold particles

L. Martinů and H. Biederman

J. Vac. Sci. Technol. A 3, 2639 (1985); http://dx.doi.org/10.1116/1.572804 (4 pages) | Cited 6 times

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Composite thin films were prepared by simultaneous plasma polymerization of chlorotrifluoroethylene and sputtering of gold in an rf glow discharge (20 MHz) excited by a planar magnetron. The concentration depth profile analyses including AES and ESCA have disclosed that the amount of fluorine and chlorine decreases with increasing gold concentration and that the film surface is not representative for the bulk of the layer. Structural examination using TEM observations evidenced that gold is incorporated in an amorphous polymer matrix in the form of polycrystalline grains 10–20 nm in diameter in the case of low film filling factors ( f ≲0.1). Two particle size systems have been found at higher filling factors when the grain diameters reached about 130 nm ( f ∼0.5). Spectral dependence of the absorption coefficient is described in terms of optical resonance. A hypothesis of energetic particle bombardment of the growing layer was suggested to explain the film structure and composition.
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68.60.-p Physical properties of thin films, nonelectronic
68.55.-a Thin film structure and morphology
75.20.Ck Nonmetals
81.15.Cd Deposition by sputtering

Comparison of microwave and lower frequency plasmas for thin film deposition and etching

M. R. Wertheimer and M. Moisan

J. Vac. Sci. Technol. A 3, 2643 (1985); http://dx.doi.org/10.1116/1.572805 (7 pages) | Cited 28 times

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We review the literature on cold plasma chemistry, dealing with the plasma deposition of organic (plasma polymers) and inorganic thin films, and with plasma etching, in which the plasma excitation frequency is the principal variable. Based on recent theoretical results by Ferreira and Loureiro, we propose that some observed frequency effects should be interpreted as resulting from different electron energy distribution functions (EEDF), as the shapes of these EEDF depend upon the ratio ν/ω (ν being the electron‐neutral collision frequency for momentum transfer and ω the angular frequency of the applied electromagnetic field) of the plasma under consideration. For gas pressures in the range 50–500 mTorr, this leads one to distinguish between low frequency (LF, ≤13.56 MHz, where ν/ω≥1) and microwave plasmas (>300 MHz, the microwave frequency range, for which ν/ω ≪ 1); the microwave plasmas have a comparatively higher population of very energetic electrons. We then present a selection of our own experimental data comparing LF and microwave (2.45 GHz) plasma deposition of organosilicon plasma polymers, and of plasma deposited silicon nitride. Deposition rates in microwave plasmas are found to be about ten times higher than in LF plasmas, and films tend to differ in their structures and physical properties. These results are tentatively attributed to differences in the EEDF, pending confirmation by selected plasma diagnostic experiments.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
81.65.-b Surface treatments

Effect of an intermediate tungsten layer on thermal properties of TiC coatings ion plated onto molybdenum

M. Fukutomi, M. Fujitsuka, T. Shikama, and M. Okada

J. Vac. Sci. Technol. A 3, 2650 (1985); http://dx.doi.org/10.1116/1.572806 (5 pages)

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Among the various low‐Z coating‐substrate systems proposed for fusion reactor first‐wall applications, molybdenum coated with titanium carbide is considered very promising since it has a good capability of receiving heat from the plasma. The thermal stabilities of TiC layers ion plated onto the molybdenum substrate are discussed with particular reference to the interfacial reaction between the TiC coating and molybdenum. The deposition of an intermediate tungsten layer was found to be very effective in suppressing the formation of reaction layers, resulting in a marked improvement in thermal stabilities of TiC–Mo systems. Thermal shock test using a pulsed electron beam showed that the TiC coatings remained adherent to the molybdenum substrates during energy depositions high enough to melt the substrates within the area of beam deposition. The melt area of the TiC coatings apparently decreased when a tungsten intermediate layer was applied.
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65.20.-w Thermal properties of liquids
65.40.gd Entropy
68.35.-p Solid surfaces and solid-solid interfaces: structure and energetics

Summary Abstract: Metallic and metalloceramic coating by thermal decomposition

G. McDonald and R. C. Hendricks

J. Vac. Sci. Technol. A 3, 2655 (1985); http://dx.doi.org/10.1116/1.572807 (2 pages)

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81.15.Lm Liquid phase epitaxy; deposition from liquid phases (melts, solutions, and surface layers on liquids)

Diffusion chromium coating of iron magnetic circuit parts for relays

M. Jenko, A. Kveder, R. Tavzes, and E. Kansky

J. Vac. Sci. Technol. A 3, 2657 (1985); http://dx.doi.org/10.1116/1.572808 (4 pages)

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With diffusion chromizing the iron magnetic circuit parts in relays, the following improvements were accomplished: surface hardening, corrosion protection, and better magnetic properties. From various procedures under consideration the chromium diffused coating in vacuum was selected. The specimens of pure iron 99.95% of Fe, were buried in a granular chromium (150 μm) and heated at the temperature from 950–1150 °C in vacuum (10−2–10−3 mbar) for durations from 3 to 12 h. The chromized layer thickness, the chromium concentration profiles, the microhardness, the coercive force, and corrosion resistance were measured.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
81.05.Bx Metals, semimetals, and alloys
75.70.-i Magnetic properties of thin films, surfaces, and interfaces
84.32.Dd Connectors, relays, and switches

Fabrication of electrically conductive metal oxide coatings by reactive ion plating

V. F. Hock, L. D. Stephenson, J. H. Givens, and J. M. Rigsbee

J. Vac. Sci. Technol. A 3, 2661 (1985); http://dx.doi.org/10.1116/1.572809 (4 pages)

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Electrically conductive metal oxide (ceramic) coatings produced by reactive ion plating are being investigated at USA‐CERL for potential application in cathodic protection systems. Ceramic materials are advantageous because of their very low dissolution rates (typically less than 1 g/A/yr in 3.5% NaCl solution) and ease of fabrication. Among the ceramic anode materials currently under investigation are two systems: (1) a mixture of titanium oxide and ruthenium oxide and (2) a mixture of titanium oxides ‘‘doped’’ with niobium, each ion plated on niobium substrates. The mixed oxide coatings were fabricated by a reactive ion plating process involving oxygen and dual electron beam evaporation sources. An enhanced plasma was used to increase reactivity. X‐ray diffraction, scanning electron microscopy, and energy dispersive x‐ray spectroscopy have been used for characterization of the microstructure, crystallography, and elemental composition of the coating.
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81.15.Jj Ion and electron beam-assisted deposition; ion plating
81.05.Je Ceramics and refractories (including borides, carbides, hydrides, nitrides, oxides, and silicides)
81.65.-b Surface treatments
68.55.-a Thin film structure and morphology
68.60.-p Physical properties of thin films, nonelectronic

Production of large vaporized metal clusters and their applications to functional metallurgical coatings

Hiroshi Takaoka, Isao Yamada, and Toshinori Takagi

J. Vac. Sci. Technol. A 3, 2665 (1985); http://dx.doi.org/10.1116/1.572810 (5 pages) | Cited 5 times

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Cluster formation mechanism with large vaporized metal clusters is discussed, and several specific applications of ionized cluster beam (ICB) to films of metallurgical interest are described. In the ICB deposition and epitaxy, the crystallographic, mechanical, electrical, optical, and magneto‐optical properties of the metal and intermetallic compound films can be controlled by adjusting the acceleration voltage and the electron current for ionization. Metal‐based and intermetallic compound‐based films with characteristic advantages are reported; Cu films with strong adhesion and high packing density, Cu–Ni alloy films with controllable crystal structure and high strain gage, CdTe–PbTe superlattice with very thin and multilayered structures, and Cd1−xMnxTe films with large Faraday rotation and controllable composition and crystallinity. Thus, the ICB technique is found to have a high potential and unique features as an emerging technique for functional film formation and surface modification.
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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
81.20.-n Methods of materials synthesis and materials processing
68.55.-a Thin film structure and morphology

Wear improvement of surgical titanium alloys by ion implantation

Piran Sioshansi, Richard W. Oliver, and Frank D. Matthews

J. Vac. Sci. Technol. A 3, 2670 (1985); http://dx.doi.org/10.1116/1.572811 (5 pages)

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Titanium based alloys are being considered as orthopaedic implants for a variety of reasons such as excellent corrosion resistance, high fatigue strength, low modulus of elasticity, and most importantly, excellent biocompatibility. The only questionable property of these alloys is their wear resistance. While Ti–6Al–4V has recently been introduced for construction of the femoral component in knee‐joint systems, the questionable wear performance of the Ti–6Al–4V is a barrier for a more widespread acceptance of the alloy for this application. The ion implantation process as shown in this study is being considered as an effective method for improving the wear performance of titanium based alloys for orthopaedic implants. Ion beams of carbon and nitrogen have been used to implant the surface of Ti–6Al–4V hemispherical samples. The samples were tested in a pin‐on‐disk machine against ultrahigh molecular weight polyethylene (UHMWPE) with loads representative of total joint replacements. Deionized water and Ringer’s solution have been used as lubricants for the wear tests. The wear data of the UHMWPE and implanted samples are presented. The results show that the implantation process is effective in reducing the wear associated with the Ti–6Al–4V alloy used for prosthesis purposes.
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81.40.Pq Friction, lubrication, and wear
61.72.U- Doping and impurity implantation
46.55.+d Tribology and mechanical contacts

Summary Abstract: Ion beam enhancement of vapor deposited coatings

R. A. Kant and B. D. Sartwell

J. Vac. Sci. Technol. A 3, 2675 (1985); http://dx.doi.org/10.1116/1.572812 (2 pages)

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Abstract Unavailable
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68.55.-a Thin film structure and morphology
61.80.Jh Ion radiation effects
68.60.-p Physical properties of thin films, nonelectronic
81.15.Jj Ion and electron beam-assisted deposition; ion plating

Summary Abstract: The effect of Fe and Ce ion implantation on the high temperature deformation behavior of a 2124 aluminum alloy

K. V. Jata and G. K. Hubler

J. Vac. Sci. Technol. A 3, 2677 (1985); http://dx.doi.org/10.1116/1.572813 (3 pages)

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81.40.Lm Deformation, plasticity, and creep
61.72.U- Doping and impurity implantation
62.20.F- Deformation and plasticity

Corrosion behavior of amorphous Ni based alloy coatings fabricated by ion beam mixing

R. S. Bhattacharya, A. K. Rai, C. N. Raffoul, P. P. Pronko, and M. Khobaib

J. Vac. Sci. Technol. A 3, 2680 (1985); http://dx.doi.org/10.1116/1.572814 (4 pages) | Cited 1 time

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Amorphous thin films of MoNi, TiNi, MoNiCr, and TiNiCr with thicknesses in the range of 650–1500 Å were prepared by high energy (1 MeV) Au+ and Pt+ ion beam mixing. The compositions of these films were Mo50Ni50, Ti50Ni50, Mo35Ni54Cr11, and Ti40Ni50Cr10. Aqueous corrosion behavior of these amorphous films were studied in 1 N HNO3 and 0.1 N NaCl solutions by the potentiodynamic polarization method. The amorphous coatings showed significantly lower corrosion rates in both acidic and basic aqueous solutions compared with their polycrystalline counterpart which were obtained by annealing the amorphous layers at temperatures above the amorphous to crystalline transition temperature. The corrosion behavior of amorphous films was also significantly improved in comparison with pure elemental constituents.
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81.05.Bx Metals, semimetals, and alloys
68.60.-p Physical properties of thin films, nonelectronic

Ion implantation and ion assisted coating of metals

G. Dearnaley, P. D. Goode, F. J. Minter, A. T. Peacock, and C. N. Waddell

J. Vac. Sci. Technol. A 3, 2684 (1985); http://dx.doi.org/10.1116/1.572815 (7 pages) | Cited 3 times

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The ion implantation of nitrogen into steels and titanium alloys can markedly improve their wear resistance especially under mild abrasive conditions, but it is significantly less successful in overcoming metal–metal adhesive wear under high loads. Certain metallic species such as Ti, Ta, Nb, Y, and Sn give better performance under such conditions when implanted into steels, but most of these additives are effective only in the presence of carbon or nitrogen. Among them, yttrium is particularly successful in reducing wear and friction after implantation at relatively low fluences (1016 ions cm−2), thus avoiding problems due to surface sputtering and limited retention in work pieces of complex geometry. Yttrium and other oversized species (e.g., Sn) may act by forming a complex with interstitial carbon or nitrogen: this nonspherical defect interacts strongly with mobile dislocations and so strengthens the material. Ion implantation provides a nonequilibrium method for introducing significant quantities of large atoms on substitutional sites. Abrasive wear is lessened by the application of hard, chemically inert coatings such as the nitrides or carbonitrides of titanium, boron or hafnium, but conventional CVD or PVD coatings of these compounds are often lacking in adhesion to the substrate. When deposited at relatively low temperatures, moreover, they may have an undesirable columnar structure and a nodular surface topography. To overcome such problems research is now being carried out on thin coatings of Ti, B, or Hf on steel which are bombarded heavily with energetic ions. This can bring about ion beam mixing at the interface, followed by the conversion of at least part of the coating to a nitride or carbonitride. It is advantageous to support such coatings by implanting the metal substrate first. Ion assisted coatings of TiN or BN appear promising from the standpoint of their microhardness, friction, adhesion and oxidation properties and so they may reduce adhesive wear.
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61.72.U- Doping and impurity implantation
81.15.Jj Ion and electron beam-assisted deposition; ion plating
81.40.Pq Friction, lubrication, and wear
61.80.Jh Ion radiation effects

Summary Abstract: Nitrogen ion implantation for wear applications: A review

J. K. Hirvonen

J. Vac. Sci. Technol. A 3, 2691 (1985); http://dx.doi.org/10.1116/1.572816 (2 pages) | Cited 2 times

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Abstract Unavailable
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81.40.Pq Friction, lubrication, and wear
61.72.U- Doping and impurity implantation

Summary Abstract: Modification of metals by low energy ions during thin film deposition

J. M. E. Harper and J. J. Cuomo

J. Vac. Sci. Technol. A 3, 2693 (1985); http://dx.doi.org/10.1116/1.572817 (1 page) | Cited 1 time

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61.80.Jh Ion radiation effects
68.60.-p Physical properties of thin films, nonelectronic
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy

Modification of the grain size of sputtered copper with additions of oxygen, krypton, silver, or yttrium

R. W. Moss and M. D. Merz

J. Vac. Sci. Technol. A 3, 2694 (1985); http://dx.doi.org/10.1116/1.572818 (6 pages) | Cited 2 times

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Several 800 to 1100 μm thick films of oxygen‐free high‐conductivity (OFHC) copper and copper with additions of oxygen, krypton, silver, or yttrium were deposited at rates of 0.5 to 1.2 μm/min using an enhanced thermionically supported‐discharge (ETSD) sputtering apparatus. To obtain fine‐grained materials, several deposition parameters, such as partial pressure of oxygen in the sputtering gas, bias, and substrate temperature, were varied. Oxygen and krypton were incorporated by trapping the sputtering gas; silver and yttrium were added by means of the target design. The structures and microstructures were examined with standard x‐ray diffraction (XRD), transmission electron microscopy (TEM), and optical microscopy techniques. The grain sizes varied from 14 μm for the OFHC copper to 0.0073 μm for the Cu‐4 at. % Y deposits. XRD data indicated an amorphous structure for the Cu‐9 at. % Y deposits.
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61.72.Mm Grain and twin boundaries
61.66.Dk Alloys
46.55.+d Tribology and mechanical contacts
81.40.-z Treatment of materials and its effects on microstructure, nanostructure, and properties

Summary Abstract: Properties of ion plated oxide films

H. K. Pulker, W. Haag, M. Bühler, and E. Moll

J. Vac. Sci. Technol. A 3, 2700 (1985); http://dx.doi.org/10.1116/1.572819 (2 pages) | Cited 6 times

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75.20.Ck Nonmetals
68.60.-p Physical properties of thin films, nonelectronic
81.15.Jj Ion and electron beam-assisted deposition; ion plating

Summary Abstract: Reactive dual ion beam sputtering of oxide films

S. Scaglione and G. Emiliani

J. Vac. Sci. Technol. A 3, 2702 (1985); http://dx.doi.org/10.1116/1.572820 (2 pages) | Cited 4 times

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81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
79.20.Rf Atomic, molecular, and ion beam impact and interactions with surfaces
68.55.-a Thin film structure and morphology

Additive thin film technology for hybrid circuit fabrication

H.‐J. Krokoszinski, H. Oetzmann, H. Gernoth, and C. Schmidt

J. Vac. Sci. Technol. A 3, 2704 (1985); http://dx.doi.org/10.1116/1.572821 (4 pages)

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Thin film hybrid circuits usually are fabricated by photolithographic structuring of an evaporated or sputtered metal layer sequence (substractive technology). In contrast to this, we discuss the abilities of ‘‘evaporation masking,’’ i.e., evaporation through metal masks (additive technology). Its main advantage is the local deposition of several different materials (conducting, resistive, semiconducting, insulating, electroluminescent, etc.) enabling the production of multilayer thin film devices. In this work we emphasize the possibility of producing complex hybrid circuits in one vacuum cycle including local insulations for capacitors, crossovers, and passivating oxide layers. Moreover, we discuss the equipment used, the electrical properties of some standard materials (NiCr, Al, Al2O3, etc.) and the resulting design rules for the hybrid layout. As a typical example, a thin film hybrid circuit on 2×2 in. glazed ceramics is presented which includes 800 crossovers, 56 thin film resistors, and 3 evaporated capacitors.
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85.40.-e Microelectronics: LSI, VLSI, ULSI; integrated circuit fabrication technology
81.65.-b Surface treatments
85.40.Xx Hybrid microelectronics; thick films
81.15.-z Methods of deposition of films and coatings; film growth and epitaxy
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