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Previous Issue

Oct 1994

Volume 3, Issue 4, pp. 299-409


Characterization of 1,1-Dihydroperfluorooctyl Acrylate (PFOA) by XPS

Camille M. Kassis, Jack K. Steehler, and Richard W. Linton

Surf. Sci. Spectra 3, 299 (1994); http://dx.doi.org/10.1116/1.1247742 (8 pages)

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A sample of 1,1-dihydroperfluorooctyl acrylate (PFOA), a low surface energy polymeric material prepared by homogeneous free radical solution polymerization in supercritical CO2, has been investigated by x-ray photoelectron spectroscopy (XPS) using a Perkin-Elmer Physical Electronics Model 5400 spectrometer with monochromatic Al Kα x rays. Knowledge of the surface composition of PFOA is significant since potential applications of this homopolymer include use in polymer blends where this material would be expected to be the surface active species. Controlled surface studies were conducted on a thick polymer film (∼0.5 μm) spun cast from solution onto silicon. Although the F 1s and O 1s regions were structurally straightforward to interpret, the C 1s window showed the expected pattern of functional group components. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Characterization of 1,1-Dihydroperfluorooctyl Methacrylate (PFOMA) by XPS

Camille M. Kassis, Jack K. Steehler, and Richard W. Linton

Surf. Sci. Spectra 3, 307 (1994); http://dx.doi.org/10.1116/1.1247743 (8 pages)

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A sample of 1,1-dihydroperfluorooctyl methacrylate (PFOMA), a low surface energy polymeric material prepared by homogeneous free radical solution polymerization in supercritical CO2, has been investigated by x-ray photoelectron spectroscopy (XPS) using a Perkin-Elmer Physical Electronics Model 5400 spectrometer with monochromatic Al Kα x rays. Knowledge of the surface composition of PFOMA is significant since potential applications of this homopolymer include use in polymer blends where this material would be expected to be the surface active species. Controlled surface studies were conducted on a thick polymer film (∼0.5 μm) spun cast from solution onto silicon. Although the F 1s and O 1s regions were structurally straightforward to interpret, the C 1s window showed the expected pattern of functional group components. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Characterization of 1,1,2,2-Tetrahydroperfluorooctyl Acrylate (PTAN) by XPS

Camille M. Kassis, Jack K. Steehler, and Richard W. Linton

Surf. Sci. Spectra 3, 315 (1994); http://dx.doi.org/10.1116/1.1247786 (8 pages)

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A sample of 1,1,2,2-tetrahydroperfluorooctyl acrylate (PTAN), a low surface energy polymeric material prepared by homogeneous free radical solution polymerization in supercritical CO2, has been investigated by x-ray photoelectron spectroscopy (XPS) using a Perkin-Elmer Physical Electronics Model 5400 spectrometer with monochromatic Al Kα x rays. Knowledge of the surface composition of PTAN is significant since potential applications of this homopolymer include use in polymer blends where this material would be expected to be the surface active species. Controlled surface studies were conducted on a thick polymer film (∼0.5 μm) spun cast from solution onto silicon. Although the F 1s and O 1s regions were structurally straightforward to interpret, the C 1s window showed the expected pattern of functional group components. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

High Resolution Spectra of Hexatriacontane and Polyethylene

Elizabeth Thomas, Catherine S. Lawson, Brian J. Tielsch, and Julia E. Fulghum

Surf. Sci. Spectra 3, 323 (1994); http://dx.doi.org/10.1116/1.1247761 (14 pages)

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The C 1s photoelectron spectra are compared for the aliphatic hydrocarbons, hexatriacontane and polyethylene. An asymmetric C 1s envelope is observed regardless of sample form. © 1997 American Vacuum Society. polymers; hydrocarbon 00207; hexatriacontane film on silicon 00208; silicon 00209; hexatriacontane powder 00210; polyethylene film 00211; polyethylene film
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Analysis of Poly(Ethylene Terephthalate) (PET) by XPS

Aurora Doren, Michel J. Genet, and Paul G. Rouxhet

Surf. Sci. Spectra 3, 337 (1994); http://dx.doi.org/10.1116/1.1247762 (5 pages) | Cited 2 times

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Poly(ethylene terephthalate) is used in numerous industrial applications. Successful medical applications are in the area of cardiovascular surgery. Its chemical functionality makes it propitious to grafting biochemical compounds; surface modification by plasma treatment may also be used to improve biocompatibility and modify wetting properties. The analyzed specimen was a commercial film (Mylar A). The main C 1s region was decomposed into three main components which were clearly identified on the recorded spectrum: 284.8, 286.4, and 288.8 eV attributed, respectively, to carbon only bound to carbon and hydrogen [math(C,H)], carbon making a single bond with oxygen [mathO] and carbon of ester [mathOO]. Satellite peaks were found at 291.3, 293.5, and 295.8 eV. The molar ratios math(C,H):math�O:mathOO were 3:0.92:0.91 excluding the satellite peaks, to be compared with the expected values of 3:1:1. The O 1s peak showed two partially resolved components at 531.6 [mathCO] and 533.3 eV [OCmath] with a satellite at 538.2 eV. The O:C ratio was 27.8:72.2, to be compared with the expected values of 28.6:71.4. The FWHM of the main C 1s components was in the range of 0.90 to 1.23 eV depending on the component and the mode of decomposition; the FWHM of O 1s components was about 1.40 eV. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Poly(Amino Acids) by XPS: Analysis of Poly(L-Serine)

Stéphane Bartiaux, Jean-Benoît Lhoest, Michel J. Genet, Patrick Bertrand, and Paul G. Rouxhet

Surf. Sci. Spectra 3, 342 (1994); http://dx.doi.org/10.1116/1.1247763 (6 pages)

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Poly(L-serine) was analyzed as a model compound representative of poly(amino acids) with uncharged polar pendant groups. The sample powder was pressed on an indium foil to obtain a relatively smooth surface. The C 1s peak was recorded first, and recorded again at the end; no difference was found between the two records, indicating that poly(L-serine) did not suffer beam damage. The C 1s peak was split in four components. The [OmathN] component, characteristic of amide, was fixed at 288.0 eV; a component found at 286.2 eV was attributed to [mathN] and [mathOH]. The ratio ([mathN]+[mathOH])/[OmathN] was 1.85, while the stoichiometric value is 2.00. Two additional peaks were found: one set at 284.8 eV attributed to [math(C;H)] of contaminants and one at 289.1 eV attributed to [OmathOH] of chain ends and possible contaminants. The O 1s peak was split into two components at 531.4 and 532.6 eV attributed to [mathCN] and [CmathH], respectively, which were not resolved. The ratio between the two peaks ([mathC]/[CmathN=0.95) was close to the stoichiometric value of 1. The N 1s peak at 399.8 eV attributed to the amide nitrogen appeared with a small tail reflecting the presence of traces of protonated nitrogen. The overall N:O:C atomic ratios were 0.30:0.61:1.00 to be compared with the expected value of 0.33:0.66:1.00. These spectra could be used as references for the characterization of polypeptides and proteins. © 1997 American Vacuum Society.
Show PACS
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
87.64.ks Electron and photoelectron
87.15.M- Spectra of biomolecules

Poly(Amino Acids) by XPS: Analysis of Poly-L-Leucine

Jean-Benoît Lhoest, Stéphane Bartiaux, Patrick A. Gerin, Michel J. Genet, Patrick Bertrand, and Paul G. Rouxhet

Surf. Sci. Spectra 3, 348 (1994); http://dx.doi.org/10.1116/1.1247787 (9 pages)

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Poly(L-leucine) was analyzed as a model compound representative of poly(amino acids) with alkyl pendant groups. Two specimens of different origins and molecular masses were examined. One (A) was pressed on an indium foil to allow recording time of flight secondary ion mass spectrometry (TOF SIMS) spectra in parallel and, therefore, insure good electrical charge dissipation. The other one (B) was placed in a stainless steel trough and then pressed. The C 1s peak was recorded first and recorded again at the end; no difference was found between the two records, indicating that poly(L-leucine) did not suffer beam damage. The C 1s peak of specimen A was split into three components: one fixed at 284.8 eV and due to math—(C,H), the other two found at 286.1 and 287.8 eV and due to mathN and O�mathN, respectively. The O 1s peak centered at 531.2 eV and due to mathCN showed a tail which indicated the presence of a small component at 533.0 eV, possibly due to water or C�mathH of contaminating compounds. The N 1s peak was symmetric and centered at 399.7 eV. The position of the peak components of specimen B were coincident with specimen A within 0.1 eV. The ratio of the molar concentration, with respect to N, of [mathCN], [O�mathN], and [mathN], on the one hand, and of [math(C,H)], on the other hand, fitted the expected values of 1 and 4 within 5%, except for one component of one specimen which showed a deviation of 15%. The choice of the background shape (S shape or linear) has no significant influence on the results. These spectra may be used as references for the characterization of polypeptides and proteins. © 1997 American Vacuum Society.
Show PACS
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
87.64.ks Electron and photoelectron
87.15.M- Spectra of biomolecules

Effect of Crystallinity on the XPS Spectrum of Poly(Ethylene Terephthalate)

G. Beamson, D. T. Clark, N. W. Hayes, and D. S-L. Law

Surf. Sci. Spectra 3, 357 (1994); http://dx.doi.org/10.1116/1.1247788 (9 pages) | Cited 1 time

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High resolution x-ray photoelectron spectra (XPS) are reported for poly(ethylene terephthalate) (PET) in the form of biaxially oriented crystalline film and amorphous polymer melt (i.e., molten inside the spectrometer during analysis). A small(∼0.14 eV) but unambiguous shift of the C 1s glycol component, relative to the aromatic and carboxyl components, is observed on going from crystalline film to amorphous polymer melt. It is known from x-ray diffraction data and infrared spectroscopy that the crystalline to amorphous transition is accompanied by a change from trans to gauche conformation of the glycol unit of the polymer repeat unit, and we ascribe the observed C 1s glycol shift to the same effect. Small differences between crystalline and amorphous PET are also observed in the valence band. Under the conditions of the XPS analysis the polymer melt appears to be electrically conducting. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Observation of Electrical Conductivity During XPS Analysis of Organic Oils

G. Beamson, D. T. Clark, N. W. Hayes, and D. S-L. Law

Surf. Sci. Spectra 3, 366 (1994); http://dx.doi.org/10.1116/1.1247789 (9 pages) | Cited 2 times

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Under the conditions of x-ray photoelectron spectra (XPS) analysis organic liquids appear to behave as electrical conductors. Here we report x-ray photoelectron spectra for pentaphenylether and pentaphenyltrimethyltrisiloxane oils at room temperature. These materials are commercially available as diffusion pump fluids (Santovac 5 and DC705, respectively). Their room temperature vapor pressures are ∼2 × 10−8 Pa and they can be studied by XPS without hazard to the spectrometer vacuum system. Both materials were investigated as relatively thick liquid films (∼10 μm, as determined by weighing) on a piece of silicon wafer. A solid organic film of this thickness would be expected to be an XPS insulator. The oil films on silicon required no external charge compensation and gave high resolution C 1s spectra with the first component of the envelope very close to 285 eV binding energy. Measured binding energies closely followed a bias voltage applied to the silicon wafer. Oil films thicker than 10 μm behaved as XPS insulators. Insulating behavior was also observed on cooling the samples by passing liquid nitrogen through the spectrometer manipulator during analysis. The explanation of these phenomena is not yet clear but the apparent electrical conductivity allows XPS study of low vapor pressure organic liquids in a straightforward way, without charging effects. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds
66.10.Ed Ionic conduction

Pristine and Overoxidized Polypyrrole by XPS

I. Losito, C. Malitesta, L. Sabbatini, and P. G. Zambonin

Surf. Sci. Spectra 3, 375 (1994); http://dx.doi.org/10.1116/1.1247790 (9 pages)

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An x-ray photoelectron spectroscopy (XPS) analysis was performed of polypyrroles (PPy) electrosynthesized on Pt in aqueous solution. Spectra were recorded both for the as-synthesized (pristine) polymer (specimen 1) and for the so-called “overoxidized” PPy (specimen 2). Electrosynthesis was accomplished potentiostatically at +0.7 V vs SCE in KCl 10 mM containing pyrrole 0.4 M. Overoxidized PPy was obtained by keeping the pristine polymer at the electrosynthesis potential for 5 h, in phosphate buffer solution (pH 7). C, N, O (1s), and Cl 2p (pristine) spectra are included. Some minor elements, P (in the overoxidized polymer), Na (in some overoxidized samples), and Si (in other samples of both types of PPy, but not in those here reported), were also detected. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Fr Polymers; organic compounds

Poly(p-Phenylenevinylene) UPS Valence Band Spectra

M. Lögdlund and W. R. Salaneck

Surf. Sci. Spectra 3, 384 (1994); http://dx.doi.org/10.1116/1.1247782 (3 pages) | Cited 2 times

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The research field of conjugated polymers is rapidly increasing due to their potential, and demonstrated, use as electroactive materials. In particular, in connection with the progress made in the fabrication of light emitting diodes (LEDs) from conjugated polymers, some of the most promising results have been obtained with poly(p-phenylenevinylene), or PPV, as the light emission medium [J. H. Burroughes, D. D. C. Bradley, A. R. Brown, R. N. Marks, K. Mackay, R. H. Friend, P. L. Burn, and A. B. Holmes, Nature 347, 539 (1990); R. H. Friend, in Nobel Symposium in Chemistry: Conjugated Polymers and Related Materials; The Interconnection of Chemical and Electronic Structure, edited by W. R. Salaneck, I. Lundstrom, and B. Ranby (Oxford Science, Oxford, 1993)]. The electronic structure of these conjugated polymers gives important information towards a better understanding of the performance of the devices [D. A. dos Santos, C. Quattrocchi, R. H. Friend, and J. L. Bredas, J. Chem. Phys. 100, 3301 (1994)]. Here, ultraviolet photoelectron spectroscopy (UPS) valence band spectra of PPV are presented. Other valence band spectra of PPV can be found in the literature [M. J. Obrzut and F. E. Karasz, Macromolecules 22, 458 (1989); K. Seki, S. Asada, T. Mori, H. Inokuchi, I. Murase, T. Ohnishi, and T. Nogushi, Solid State Commun. 74, 677 (1990)]. The present spectra are, however, better resolved and agree very well with theoretical modeling [M. Lögdlung, W. R. Salaneck, F. Meyers, J. L. Bredas, G. A. Arbuckle, R. Friend, A. B. Holmes, and G. Froyer, Macromolecules 26, 3815 (1993)]. © 1997 American Vacuum Society.
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79.60.Fr Polymers; organic compounds
71.20.Rv Polymers and organic compounds

Elemental Palladium by XPS

Maria C. Militello and Steven J. Simko

Surf. Sci. Spectra 3, 387 (1994); http://dx.doi.org/10.1116/1.1247783 (8 pages) | Cited 2 times

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X-ray photoelectron spectroscopy (XPS) spectra of elemental palladium (Pd) are presented. The specimen is a polycrystalline foil and was analyzed after chemical cleaning and ion-sputtering to remove surface contamination. The spectra were collected with a Surface Science Instruments SSX-101 M-Probe ESCA instrument using monochromatized Al Kα x rays. Spectra include a survey scan and the Pd 3d,3p,3s,4s,4p, and valence band regions. Also included are the Pd MNN and MNV Auger transitions. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Bm Clean metal, semiconductor, and insulator surfaces

Palladium Oxide (PdO) by XPS

Maria C. Militello and Steven J. Simko

Surf. Sci. Spectra 3, 395 (1994); http://dx.doi.org/10.1116/1.1247784 (7 pages)

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X-ray photoelectron spectroscopy (XPS) spectra of palladium oxide (PdO) are presented. Clean, ground PdO powder was pressed into In foil and analyzed with a Surface Science Instruments SSX-101 M-Probe ESCA instrument using monochromatized Al Kα x rays. Spectra include a survey scan, the Pd 3d,3p,3s,4s,4p regions, the O 1s, and valence band regions, and the O KLL, Pd MNN and MNV Auger transitions. © 1997 American Vacuum Society.
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82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Bm Clean metal, semiconductor, and insulator surfaces

Palladium Chloride (PdCl2) by XPS

Maria C. Militello and Steven J. Simko

Surf. Sci. Spectra 3, 402 (1994); http://dx.doi.org/10.1116/1.1247785 (8 pages)

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X-ray photoelectron spectroscopy (XPS) spectra of palladium chloride (PdCl2) are presented. Ground PdCl2 powder was pressed into Al foil and analyzed with a Surface Science Instruments SSX-101 M-Probe ESCA instrument using monochromatized Al Kα x rays. Spectra include a survey scan, the Pd 3d, 3p,3s,4s,4p regions, the Cl 2p,2s, and valence band regions, and the Pd MNN and MNV Auger transitions. © 1997 American Vacuum Society.
Show PACS
82.80.Pv Electron spectroscopy (X-ray photoelectron (XPS), Auger electron spectroscopy (AES), etc.)
79.60.Bm Clean metal, semiconductor, and insulator surfaces
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