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Oct 2001

Volume 8, Issue 4, pp. 247-328


Plasma-Enhanced CVD CeO2 Nanocrystalline Thin Films Analyzed by XPS

Lidia Armelao, Davide Barreca, Gregorio Bottaro, Alberto Gasparotto, and Eugenio Tondello

Surf. Sci. Spectra 8, 247 (2001); http://dx.doi.org/10.1116/11.20020601 (11 pages) | Cited 2 times

Online Publication Date: 17 March 2003

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CeO2 nanocrystalline films were deposited on SiO2 and SiO2/Si(100) substrates by plasma enhanced-chemical vapor deposition (PE-CVD) in Ar–O2 atmospheres. Ce(dpm)4 (dpm = 2,2-6,6-tetramethyl-3,5-heptanedionate) was used as a precursor, which allows a clean conversion into CeO2 due to the presence of Ce–O bonds. The coatings were pale yellow in color, homogeneous and crack-free. In this study, an x-ray photoelectron spectroscopy (XPS) investigation of the principal core levels (O ls, Ce 3d) of CeO2 films was performed. The relative Ce(III)/Ce(IV) amount was estimated by evaluating the ratio of the Ce 3d3/2(u′′′) satellite to the total Ce 3d integral area. The relative content of Ce(III) and Ce(IV) amount can be tailored by controlling the O2 partial pressure and substrate temperature during the depositions. The reported results represent the extension of a recently published article (Ref. 1). © 2003 American Vacuum Society.
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79.60.Dp Adsorbed layers and thin films
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.07.Bc Nanocrystalline materials
81.15.Gh Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)

A Study of Nanophase Tungsten Oxides Thin Films by XPS

Davide Barreca, Giovanni Carta, Alberto Gasparotto, Gilberto Rossetto, Eugenio Tondello, and Pierino Zanella

Surf. Sci. Spectra 8, 258 (2001); http://dx.doi.org/10.1116/11.20020801 (10 pages)

Online Publication Date: 17 March 2003

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Nanophasic tungsten oxides thin films have been deposited at 500 °C on quartz and glass substrates starting from W(CO)6 using the metal organic chemical vapor deposition technique (MOCVD). Two series of deposition experiments were carried out to make a comparison between the results obtained employing, as reactant gases, O2 mixed with water vapor and a dry mixture of N2 with 25% H2, respectively. The obtained tungsten oxides were analyzed by x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM) in order to investigate their microstructure, chemical composition, and surface morphology. In this work, XPS analyses of two tungsten oxides thin films deposited in different atmospheres are presented. Besides the wide scan spectra, charge corrected binding energies for the W 4f7/2, W 4f5/2, O ls, and C 1s surface photoelectron signals are reported. In particular, the film obtained in H2 atmosphere shows the presence of W in an oxidation state lower than VI. © 2003 American Vacuum Society.
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79.60.Dp Adsorbed layers and thin films
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.07.Bc Nanocrystalline materials

ZrO2 Sol-Gel Thin Films by XPS

Lidia Armelao, Eugenio Tondello, Laura Bigliani, and Gregorio Bottaro

Surf. Sci. Spectra 8, 268 (2001); http://dx.doi.org/10.1116/11.20020307 (6 pages) | Cited 1 time

Online Publication Date: 17 March 2003

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ZrO2 thin films were prepared by dip-coating on silica glass via sol-gel processing. Ethanolic sols of zirconium butoxide were used as precursors. The ZrO2 films were prepared under controlled atmosphere and resulted transparent, homogeneous, crack-free, and well adherent to the substrates under heating up to 900 °C. The composition of the films was investigated by x-ray photoelectron spectroscopy. In particular, the principal core levels were analyzed for the sample annealed for 1 h at 900 °C. The microstructure of the films was studied by glancing incidence x-ray diffraction as a function of the annealing temperature. The coatings were amorphous up to 400 °C and crystalline ZrO2 with tetragonal structure was observed at 600 °C. Nanostructured layers with an average crystallite dimension of 15 nm were obtained up to 900 °C. © 2003 American Vacuum Society.
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79.60.Dp Adsorbed layers and thin films
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.10.Dn Growth from solutions
81.10.Fq Growth from melts; zone melting and refining
81.15.Lm Liquid phase epitaxy; deposition from liquid phases (melts, solutions, and surface layers on liquids)
81.07.Bc Nanocrystalline materials

Alkyl Monolayers on Silica Surfaces Prepared from Neat, Heated ClSi(CH3)2(CH2)17CH3 Analyzed by XPS

Ghaleb A. Husseini, Lloyd W. Zilch, Eric T. Sevy, Matthew C. Asplund, and Matthew R. Linford

Surf. Sci. Spectra 8, 274 (2001); http://dx.doi.org/10.1116/11.20020502 (10 pages)

Online Publication Date: 17 March 2003

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Silane monolayers on silica, prepared from mono-, di- and trichlorosilanes, are widely used in industry for surface functionalization and modification. However, unlike di- and trichlorosilanes, monochlorosilanes are particularly easy to work with because they can dimerize, but not polymerize, upon reaction with water. Typically, an organic solvent is used when depositing a silane monolayer. Here we show XPS spectra of monolayers of ClSi(CH3)2(CH2)17CH3 (octadecyldimethylchlorosilane, CAS# 18643-08-8) on silicon oxide (silicon wafer) prepared using a rapid, solvent-free approach. Reaction conditions are 120 °C for 10 min using the neat (pure) compound, and no inert atmosphere or special treatment of the compound is required. © 2003 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.05.Lg Polymers and plastics; rubber; synthetic and natural fibers; organometallic and organic materials

Alkyl Monolayers on Silica Surfaces Prepared from Neat, Heated ClSi(CH3)2(CH2)6CH=CH2 Analyzed by XPS

Ghaleb A. Husseini, Amarchand Sathyapalan, Eric T. Sevy, Matthew R. Linford, and Matthew C. Asplund

Surf. Sci. Spectra 8, 284 (2001); http://dx.doi.org/10.1116/11.20020503 (7 pages)

Online Publication Date: 17 March 2003

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Silane monolayers on silica, prepared from mono-, di-, and trichlorosilanes, are widely used in industry for surface functionalization and modification. However, unlike di-and trichlorosilanes, monochlorosilanes are particularly easy to work with because they can dimerize, but not polymerize, upon reaction with water. Typically, an organic solvent is used when depositing a silane monolayer. Here we show XPS spectra of monolayers of ClSi(CH3)2(CH2)6CH=CH2 (octenyldimethylchlorosilane, CAS# 17196-12-2) on silicon oxide (silicon wafer) prepared using a rapid, solvent-free approach. Reaction conditions are 120 °C for 10 min using the neat (pure) compound, and no inert atmosphere or special treatment of the compound is required. © 2003 American Vacuum Society.
Show PACS
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.05.Lg Polymers and plastics; rubber; synthetic and natural fibers; organometallic and organic materials

Alkyl Monolayers on Silica Surfaces Prepared from Neat, Heated 3-Glycidoxypropyldimethylethoxysilane Analyzed by XPS

Ghaleb A. Husseini, Matthew R. Linford, Matthew C. Asplund, Justin Peacock, and Eric T. Sevy

Surf. Sci. Spectra 8, 291 (2001); http://dx.doi.org/10.1116/11.20020504 (6 pages)

Online Publication Date: 17 March 2003

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Show Abstract
Silane monolayers on silica, prepared from mono-, di-, and trichlorosilanes, are widely used in industry for surface functionalization and modification. However, unlike di- and trichlorosilanes, monochlorosilanes are particularly easy to work with because they can dimerize, but not polymerize, upon reaction with water. Typically, an organic solvent is used when depositing a silane monolayer. Here we show XPS spectra of monolayers of 3-glycidoxypropyldimethylethoxysilane (CAS# 17963-04-1) on silicon oxide (silicon wafer) prepared using a rapid, solvent-free approach. Reaction conditions are 100 °C for 10 min using the neat (pure) compound, and no inert atmosphere or special treatment of the compound is required. © 2003 American Vacuum Society.
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79.60.Fr Polymers; organic compounds
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
82.65.+r Surface and interface chemistry; heterogeneous catalysis at surfaces
81.05.Lg Polymers and plastics; rubber; synthetic and natural fibers; organometallic and organic materials

Stoichiometric and Ar-ion Sputtered Uranium Dioxide (111) Single Crystal by XPS

Shen V. Chong, Mark A. Barteau, and Hicham Idriss

Surf. Sci. Spectra 8, 297 (2001); http://dx.doi.org/10.1116/11.20020804 (6 pages)

Online Publication Date: 17 March 2003

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XPS was performed on UHV O2 annealed and Ar-ion sputtered UO2(111) single crystal surfaces. Ar-ion sputtering for 1 h decreased the XPS O 1s/U 4f corrected total peak areas ratio from 2.11 to 1.19. A shoulder at ∼377.4 eV attributed to Ux atoms (x close to zero) is also observed. Annealing the UO2(111) at 873 K for at least 1 h in the presence of 1E−4 Pa of molecular oxygen was required for restoring the oxygen defects created by Ar-ion bombardment. © 2003 American Vacuum Society.
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79.60.Bm Clean metal, semiconductor, and insulator surfaces
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
81.65.Cf Surface cleaning, etching, patterning

Surface Segregation Study of Transparent ZnGa2O4 Films by XPS

Pierre Delichere, Stephane Daniele, and Liliane G. Hubert-Pfalzgraf

Surf. Sci. Spectra 8, 303 (2001); http://dx.doi.org/10.1116/11.20020501 (9 pages)

Online Publication Date: 17 March 2003

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Sol-gel colloidal suspensions were used to elaborate ZnGa2O4 films by spin coating on glass and MgO substrates. Those films were annealed at 600 °C (10°/min) for l h in air and showed good mechanical resistance as well as very good transparency. XPS spectra recorded from 0 to 1200 eV indicated that the films contained zinc, gallium, oxygen, and a significant amount of carbon. In the absence of depth profiling analysis of the film composition, it has been impossible to determine whether this is due to surface contamination or film incorporation. Surprisingly, the data show that the Zn:Ga stochiometry of ZnGa2O4 is disrupted by interaction with the glass substrate with a Ga/Zn ratio of 4. The result is a multiphasic material namely crystallites of ZnGa2O4 (as shown by AFM measurements) in an amorphous matrix of zinc and gallium oxides. This interaction was confirmed by the fact that deposition on MgO substrate and thermal annealing in similar conditions than for the previous deposits gave XPS data confirming the retention of the Zn:Ga 1:2 stoichiometry. © 2003 American Vacuum Society.
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79.60.Dp Adsorbed layers and thin films
68.35.Dv Composition, segregation; defects and impurities
81.15.Rs Spray coating techniques
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)

Polypyrrole Latex: Surface Analysis by XPS

Peter J. Tarcha, Lawrence Salvati, and Robert W. Johnson

Surf. Sci. Spectra 8, 312 (2001); http://dx.doi.org/10.1116/11.20020102 (5 pages)

Online Publication Date: 17 March 2003

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Polypyrrole colloids are synthesized by an oxidative polymerization of pyrrole by ferric chloride in aqueous media containing a steric stabilizer. Polyvinyl alcohol (125,000 to 186,000 mol. wt., 99% hydrolyzed) was used as the stabilizer to prepare the particles for this study. Depending on the synthesis conditions, polypyrrole colloids typically have diameters between 100 and 200 nm, as evidenced by transmission electron microscopy and disk centrifuge photosedimentometry. The conjugated pyrrole polymer imparts intense black coloration to the colloid. Molecules of biological interest, such as antibodies, can be immobilized in active form on the particle surface. Thus these nanoparticles can be used as colored “markers” for immunodiagnostic assays. © 2003 American Vacuum Society.
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82.70.Dd Colloids
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)

Carboxylated Polypyrrole-Silica Nanocomposite: Surface Analysis by XPS

Steven P. Armes, Peter J. Tarcha, Lawrence Salvati, and Robert W. Johnson

Surf. Sci. Spectra 8, 317 (2001); http://dx.doi.org/10.1116/11.20020103 (6 pages)

Online Publication Date: 17 March 2003

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Carboxylated polypyrrole-silica colloids are synthesized in aqueous media by the oxidative copolymenzation of molar equivalents of pyrrole and 1-(2-carboxyethyl) pyrrole in the presence of ultrafine (20 nm) silica particles [see Maeda et al., Macromolecules 28, 2901 (1995)]. The resulting nanoparticles have a diameter of ∼100 nm as evidenced by transmission electron microscopy and disk centrifuge photosedimentometry and obtain 24–43 wt. % of silica. The conducting polymer component imparts intense coloration to the nanoparticle and the silica component ensures good colloidal stability. The surface carboxylic groups allow the covalent attachment of biological ligands of interest, such as antibodies. Thus these functional nanoparticles can be used as colored “markers” for immunodiagnostic assays. © 2003 American Vacuum Society.
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81.07.Wx Nanopowders
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)

Carboxylated Polypyrrole Latex: Surface Analysis by XPS

Peter J. Tarcha, Lawrence Salvati, and Robert W. Johnson

Surf. Sci. Spectra 8, 323 (2001); http://dx.doi.org/10.1116/11.20020104 (6 pages)

Online Publication Date: 17 March 2003

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Carboxylated polypyrrole colloids are synthesized by post-modification of polypvrrole latex in organic media. The modification begins with solvent exchange of the aqueous colloid into N-methyl pyrrolidone, followed by reaction with bromoacetyl bromide. The last reaction is a nulceophilic substitution on the bromoacetyl pendant group with mercaptoacetic acid. After reaction the particles are solvent-exchanged into water. Depending on the synthesis conditions of the base polypvrrole colloid, the resulting nanoparticles can have diameters between 100 and 200 nm, as evidenced by transmission electron microscopy and disk centrifuge photosedimentometry. The conjugated pyrrole polymer imparts intense, intrinsic coloration to the colloid. The surface carboxylic groups allow the covalent attachment of biological ligands of interest such as antibodies. Thus these functional nanoparticles can be used as colored “markers” for immunodiagnostic assays. © 2003 American Vacuum Society.
Show PACS
82.70.Dd Colloids
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
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