New method to calibrate binding energy using Au nanocolloids in X-ray photoelectron analysis of diamondlike carbon films with different electrical resistivities

Takabayashi, Susumu; Okamoto, Keishi; Motomitsu, Kunihiko; Terayama, Akira; Nakatani, Tatsuyuki; Sakaue, Hiroyuki; Suzuki, Hitoshi; Takahagi, Takayuki

doi:10.1016/j.apsusc.2007.10.002

Cited by 12 publications

(11 citation statements)

References 46 publications

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“…This effect is a consequence of inhomogeneous positive charging of insulator surfaces after photoemission. The high resistivity precludes a fast charge neutralization after photoemission, which results in a variety of differently charged zones on the surface, leading to different retarding potentials and hence to peak broadening16, 44, 45. The broadening of the Au 4f 7/2 line on the Al‐Si‐N insulating surfaces of 1.7 eV (Fig.…”

Section: Discussionmentioning

confidence: 99%

Charge referencing issues in XPS of insulators as evidenced in the case of Al‐Si‐N thin films

Pélisson-Schecker

Hug

Patscheider

2011

Surface & Interface Analysis

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Accurate charge referencing in XPS of insulating specimens is a delicate issue. This difficulty is illustrated in the case of Al-Si-N composite thin films deposited by reactive magnetron sputtering with variable composition from pure aluminum nitride to pure silicon nitride. The samples were mounted with Au-coated metallic clamps. Argon sputter cleaning was required to remove a surface native oxide before analysis. For charge referencing implanted argon atoms from the sputter gas and a small amount of gold re-deposited from the metallic clamps onto the specimen surface during sputter cleaning were evaluated. For the argon atoms, a surprisingly large chemical shift (∼1 eV) and a significant peak broadening (0.6 eV) of the Ar 2p 3/2 photoelectron line were found with varying the Si content of the films. This could be related to chemical and structural changes of the Al-Si-N films. Hence implanted argon could not be used for charge referencing of Al-Si-N samples. In contrast to the implanted argon, the Au 4f 7/2 line width of the gold re-deposited onto the sample surface did not depend on the Si content of Al-Si-N films. A constant energy shift (∼1.2 eV) of the Au 4f 7/2 line as compared with bulk gold was, however, found, which was related to the size of gold particles formed on the insulating films. Therefore gold could be reliably used to study chemical shifts of sample-relevant species in Al-Si-N films, but the absolute binding energies of Al 2p, Si 2p and N 1s photoelectrons could not be determined.

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Section: Discussionmentioning

confidence: 99%

Charge referencing issues in XPS of insulators as evidenced in the case of Al‐Si‐N thin films

Pélisson-Schecker

Hug

Patscheider

2011

Surface & Interface Analysis

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“…All the measurements were performed in ultrahigh vacuum below 4.0 × 10 −9 Torr. The binding energy was calibrated by setting the Au 4 f 7/2 peak of gold nanocolloids dropped on a spot of the DLC surface at 84.0 eV . Differential charge‐up, owing to the spot‐dependent imbalance between photoemission and electron compensation, was not observed at the surface.…”

Section: Methodsmentioning

confidence: 99%

Surface oxidation process of a diamond-like carbon film analyzed by difference X-ray photoelectron spectroscopy

Takabayashi

Takahagi

2014

Surf. Interface Anal.

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Difference X‐ray photoelectron spectroscopy (D‐XPS) revealed the surface oxidation process of a diamond‐like carbon (DLC) film. Evaluation of surface functional groups on DLC solely by the C 1s spectrum is difficult because the spectrum is broad and has a secondary asymmetric lineshape. D‐XPS clarified the subtle but critical changes at the DLC surface caused by wet oxidation. The hydroxyl (C―OH) group was dominant at the oxidized surface. Further oxidized carbonyl (CO) and carboxyl (including carboxylate) (COO) groups were also obtained; however, the oxidation of CO to COO was suppressed to some extent because the reaction required C―C bond cleavage. Wet oxidation cleaved the aliphatic hydrogenated and non‐hydrogenated sp2 carbon bonds (C―H sp2 and C―C sp2) to create a pair of C―OH and hydrogenated sp3 carbon (C―H sp3) bonds. The reaction yield for C―H sp2 was superior at the surface, suggesting that the DLC film was hydrogen rich at the surface. Oxidation of aromatic sp2 rings or polycyclic aromatic hydrocarbons such as nanographite to phenols did not occur because of their resonance stabilization with electron delocalization. Non‐hydrogenated sp3 carbon (C―C sp3) bonds were not affected by oxidation, suggesting that these bonds are chemically inert. Copyright © 2014 John Wiley & Sons, Ltd.

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“…29 To remove surface contamination, the DLC films were stabilized at 170°C in the chamber before temperature scanning, which was from 170 to 1000°C at a rate of 1°C s −1 . 31 Electrical resistivity measurements were performed using the four-point probe method 13,14 with a vacuum chamber with four metallic probes designed by Seinan Kogyo Co., Ltd. The ion currents were amplified by the SEM with a voltage of 1200 V. The base pressure was below 1 ϫ 10 −9 Torr, and the pressure during heating was maintained below 3 ϫ 10 −8 Torr.…”

Section: Methodsmentioning

confidence: 99%

“…Clues to decompose the spectrum can be obtained by systematically comparing the spectral features taken under different conditions. 13,14 We concluded that the C 1s spectra of the DLC films were decomposed into four chemical components: sp 3 carbon with carbon-carbon bonds ͑C-C sp 3 carbon͒, sp 2 carbon with carbon-carbon bonds ͑C-C sp 2 carbon͒, sp 2 carbon with hydrogen-carbon bonds ͑H-C sp 2 carbon͒, and sp 3 carbon with hydrogen-carbon bonds ͑H-C sp 3 carbon͒. 8 Hydrogen in DLC plays an important role: hydrogencarbon ͑H-C͒ bonds in DLC produce large free spaces in the structure, which inhibit conductive routes and lead to high electrical resistivity.…”

Section: Introductionmentioning

confidence: 99%

Annealing effect on the chemical structure of diamondlike carbon

Takabayashi

Okamoto

Sakaue

et al. 2008

Journal of Applied Physics

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Electron cyclotron resonance deposition, structure, and properties of oxygen incorporated hydrogenated diamondlike amorphous carbon films J. Appl. Phys. 96, 5456 (2004); 10.1063/1.1804624Effects of thermal annealing on the structural, mechanical, and tribological properties of hard fluorinated carbon films deposited by plasma enhanced chemical vapor depositionThe effect of annealing in an ultrahigh vacuum on the chemical structure of diamondlike carbon ͑DLC͒ was investigated using photoelectron spectroscopy, thermal desorption spectroscopy, electrical resistivity, and micro-Raman spectroscopy measurements. The line shapes of the C 1s photoelectron spectra depended on annealing temperature. The relative intensities of four chemical components in the spectra were quantitatively evaluated: sp 3 carbon with carbon-carbon bonds ͑C-C sp 3 carbon͒, sp 2 carbon with carbon-carbon bonds ͑C-C sp 2 carbon͒, sp 2 carbon with hydrogen-carbon bonds ͑H-C sp 2 carbon͒, and sp 3 carbon with hydrogen-carbon bonds ͑H-C sp 3 carbon͒. The variation of the ratio of the components demonstrated that hydrogen in DLC is emitted to the outside in between 450 and 600°C, and the remaining DLC is graphized above 600°C. The increase in the asymmetry of the C 1s spectra and the decrease in the electrical resistivity of the DLC film with annealing temperature agree with the picture that the H-C bonds in DLC produces large free spaces in the structure, which inhibit conductive routes and lead to high electrical resistivity.

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New method to calibrate binding energy using Au nanocolloids in X-ray photoelectron analysis of diamondlike carbon films with different electrical resistivities

Cited by 12 publications

References 46 publications

Charge referencing issues in XPS of insulators as evidenced in the case of Al‐Si‐N thin films

Charge referencing issues in XPS of insulators as evidenced in the case of Al‐Si‐N thin films

Surface oxidation process of a diamond-like carbon film analyzed by difference X-ray photoelectron spectroscopy

Annealing effect on the chemical structure of diamondlike carbon

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