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Journal Articles

Study on the relation between the crystal structure and thermal stability of FeUO$$_{4}$$ and CrUO$$_{4}$$

Akiyama, Daisuke*; Kusaka, Ryoji; Kumagai, Yuta; Nakada, Masami; Watanabe, Masayuki; Okamoto, Yoshihiro; Nagai, Takayuki; Sato, Nobuaki*; Kirishima, Akira*

Journal of Nuclear Materials, 568, p.153847_1 - 153847_10, 2022/09

FeUO$$_{4}$$, CrUO$$_{4}$$, and Fe$$_{x}$$Cr$$_{1-x}$$UO$$_{4}$$ are monouranates containing pentavalent U. Even though these compounds have similar crystal structures, their formation conditions and thermal stability are significantly different. To determine the factors causing the difference in thermal stability between FeUO$$_{4}$$ and CrUO$$_{4}$$, their crystal structures were evaluated in detail. A Raman band was observed at 700 cm$$^{-1}$$ in all the samples. This Raman band was derived from the stretching vibration of the O-U-O axis band, indicating that Fe$$_{x}$$Cr$$_{1-x}$$UO$$_{4}$$ was composed of a uranyl-like structure in its lattice regardless of its "x"' value. M$"o$ssbauer measurements indicated that the Fe in FeUO$$_{4}$$ and Fe$$_{x}$$Cr$$_{1-x}$$UO$$_{4}$$ were trivalent. Furthermore, Fe$$_{x}$$Cr$$_{1-x}$$UO$$_{4}$$ lost its symmetry around Fe$$^{mathrm{III}}$$ with increasing electron densities around Fe$$^{mathrm{III}}$$, as the abundance of Cr increased. These results suggested no significant structural differences between FeUO$$_{4}$$ and CrUO$$_{4}$$. Thermogravimetric measurements for UO$$_{2}$$, FeUO$$_{4}$$, and CrUO$$_{4}$$ showed that the temperature at which FeUO$$_{4}$$ decomposed under an oxidizing condition (approximately 800 $$^{circ}$$C) was significantly lower than the temperature at which the decomposition of CrUO$$_{4}$$ started (approximately 1250 $$^{circ}$$C). Based on these results, we concluded that the decomposition of FeUO$$_{4}$$ was triggered by an ``in-crystal'' redox reaction, i.e., Fe$$^{mathrm{III}}$$ $${+}$$ U$$^{mathrm{V}}$$ $$rightarrow$$ Fe$$^{mathrm{II}}$$ $${+}$$ U$$^{mathrm{VI}}$$, which would not occur in the CrUO$$_{4}$$ lattice because Cr$$^{mathrm{III}}$$ could never be reduced under the investigated condition. Finally, the existence of Cr$$^{mathrm{III}}$$ in FexCr$$_{1-x}$$UO$$_{4}$$ effectively suppressed the decomposition of the Fe$$_{x}$$Cr$$_{1-x}$$UO$$_{4}$$ crystal, even at a very low Cr content.

Journal Articles

Experimental observation of temperature and magnetic-field evolution of the 4${it f}$ states in CeFe$$_{2}$$ revealed by soft X-ray magnetic circular dichroism

Saito, Yuji; Yasui, Akira*; Fuchimoto, Hiroto*; Nakatani, Yasuhiro*; Fujiwara, Hidenori*; Imada, Shin*; Narumi, Yasuo*; Kindo, Koichi*; Takahashi, Minoru*; Ebihara, Takao*; et al.

Physical Review B, 96(3), p.035151_1 - 035151_5, 2017/07

AA2017-0611.pdf:0.36MB

 Times Cited Count:1 Percentile:7.19(Materials Science, Multidisciplinary)

We revisit the delocalized character of the 4$$f$$ states of CeFe$$_2$$ in the ferromagnetically ordered phase by X-ray magnetic circular dichroism (XMCD) in X-ray absorption spectroscopy (XAS) with improved data quality using single crystals. Surprisingly, the Ce $$M_{4,5}$$ XMCD spectral shape changes significantly as a function of temperature and applied magnetic field, with no concomitant changes in the spectral shape of the Ce $$M_{4,5}$$ XAS as well as the Fe $$L_{2,3}$$ XAS and XMCD. This unusual behavior is characterized by the $$J=7/2$$ states in a 4$$f^1$$ configuration mixed into the $$J=5/2$$ ground state. Such extreme sensitivity of the Ce 4$$f$$ states to the external perturbations can be related to the magnetic instability toward an antiferromagnetic phase in CeFe$$_2$$. Our experimental data presented here provide valuable insights into the underlying physics in strongly-hybridized ferromagnetic Ce compounds.

Journal Articles

Chemical states of trace-level strontium adsorbed on layered oxide by XPS and XANES under total reflection condition

Baba, Yuji; Shimoyama, Iwao

Photon Factory Activity Report 2016, 2 Pages, 2017/00

In order to elucidate the adsorption states of radioactive Sr-90 in soil, chemical bonding states of non-radioactive strontium adsorbed on layered oxide (mica) have been investigated by X-ray photoelectron spectroscopy (XPS) and X-ray absorption near edge structure (XANES) spectroscopy. Since the number of atoms in radioactive Sr-90 is extremely small, the XPS and XANES were measured under total reflection condition of the incident X-rays. The detection limit in total reflection XPS was about 150 pg/cm$$^{2}$$, which corresponds to 300 Bq of Sr-90. The Sr 2p$$_{3/2}$$ core-level energy in XPS shifted to lower energy with the decrease in the thickness of Sr layer. Also, the Sr 2p$$_{3/2}$$ $$rightarrow$$ Sr 4d$$^{*}$$ resonance energy in XANES shifts to lower energy with the decrease in the thickness. On the basis of a simple point charge model, it was elucidated that the chemical bond between Sr and mica surface becomes ionic with the decrease in the adsorbed amount of strontium.

Journal Articles

Valence state in Ce-based heavy fermion compounds at high magnetic fields

Matsuda, Yasuhiro*; Her, J.-L.*; Michimura, Shinji*; Inami, Toshiya; Ebihara, Takao*; Amitsuka, Hiroshi*

JPS Conference Proceedings (Internet), 3, p.011044_1 - 011044_6, 2014/06

Synchrotron X-ray absorption spectroscopy of CeRh$$_2$$Si$$_2$$ has been performed in pulsed high magnetic fields of up to 32 T. The Ce valence is slightly larger than 3+ at 5 K and decreases with increasing magnetic above 20 T. The field-induced valence change seems to correspond to the metamagnetic transition in the magnetization process. This phenomena is similar to our previous result on CeRu$$_2$$Si$$_2$$ and seems to be common in Ce-based heavy fermion compounds.

Journal Articles

Characterization of F$$^{+}$$-irradiated graphite surfaces using photon-stimulated desorption spectroscopy

Sekiguchi, Tetsuhiro; Baba, Yuji; Shimoyama, Iwao; Nath, K. G.

Surface and Interface Analysis, 38(4), p.352 - 356, 2006/04

 Times Cited Count:3 Percentile:7.57(Chemistry, Physical)

We investigated the orientation nature at the top-most layers of F$$^{+}$$-irradiated graphite using polarization dependent near-edge X-ray absorption fine structure (NEXAFS) spectroscopy which incorporates partial electron yield (PEY) detection and photon-stimulated ion desorption (PSID) techniques. The fluorine K-edge NEXAFS spectra conducted in PEY mode show no significant dependence on polarization angles. In contrast, NEXAFS spectra recorded in F$$^{+}$$ ion yield mode show enhanced yields at a feature of $$sim$$689.4 eV assigned as a $$sigma$$*(C-F) state relevant to =C-F sites, which depend on polarization angles. The C-F bonds prefer relatively tilting down the surface at the top-most layer, while the C-F bonds are randomly directed at deeper regions. We conclude that the difference in the orientation structures between the top surface and bulk is reflected in the NEXAFS recorded in the two different detection modes. It was also found that H$$^{+}$$- and F$$^{2+}$$- PSID NEXAFS spectra are helpful in understanding desorption mechanism, thus in analysing NEXAFS data.

Journal Articles

Mechanism of state-specific enhancement in photon-stimulated desorption as studied using a polarization-dependent technique

Sekiguchi, Tetsuhiro; Baba, Yuji; Shimoyama, Iwao; Wu, G.*; Kitajima, Yoshinori*

Surface Science, 593(1-3), p.310 - 317, 2005/11

 Times Cited Count:2 Percentile:12.09(Chemistry, Physical)

Using a newly developed rotatable time-of-flight mass spectrometer(R-TOF-MS) and polarized synchrotron radiation, orientation effect on fragmentation and desorption pathways occurring at the top-most layers of molecular solids have been investigated. Reported will be polarization-angle dependencies of TOF mass spectra, high-resolution electron- and ion-NEXAFS in condensed chlorobenzene.

Journal Articles

Direct and indirect processes in photon-stimulated ion desorption from condensed formamide

Ikeura, Hiromi*; Sekiguchi, Tetsuhiro; Baba, Yuji; Imamura, Motoyasu*; Matsubayashi, Nobuyuki*; Shimada, Hiromichi*

Surface Science, 593(1-3), p.303 - 309, 2005/11

 Times Cited Count:5 Percentile:26.91(Chemistry, Physical)

no abstracts in English

Journal Articles

Viscosity and density measurements of melts and glasses at high pressure and temperature by using the multi-anvil apparatus and synchrotron X-ray radiation

Otani, Eiji*; Suzuki, Akio*; Ando, Ryota*; Urakawa, Satoru*; Funakoshi, Kenichi*; Katayama, Yoshinori

Advances in High-Pressure Technology for Geophysical Applications, p.195 - 209, 2005/09

This paper summarizes the techniques for the viscosity and density measurements of silicate melt and glasses at high pressure and temperature by using the X-ray radiography and absorption techniques in the third generation synchrotron radiation facility, SPring-8, Japan. The falling sphere method using in situ X-ray radiography makes it possible to measure the viscosity of silicate melts to the pressures above 6 GPa at high temperature. We summarize the details of the experimental technique of the viscosity measurement, and the results of the measurements of some silicate melts such as the albite and diopside-jadeite systems. X-ray absorption method is applied to measure the density of the silicate glasses such as the basaltic glass and iron sodium disilicate glass up to 5 GPa at high temperature. A diamond capsule, which is not reactive with the glass, is used for the density measurement of the glasses. The present density measurement of the glasses indicates that this method is useful for measurement of the density of silicate melts at high pressure and temperature.

Journal Articles

Substitution effect on orientation of organosilicon compounds (CH$$_{3}$$)$$_{3}$$SiX (X = F, Cl, Br, I, NCO) as studied using NEXAFS spectroscopy

Sekiguchi, Tetsuhiro; Baba, Yuji; Shimoyama, Iwao; Nath, K. G.*; Uddin, M. N.*

Journal of Physics; Condensed Matter, 17(36), p.5453 - 5466, 2005/09

 Times Cited Count:1 Percentile:6.49(Physics, Condensed Matter)

The orientation nature of multilayer organosilicon compounds has been investigated by measuring the dependence of the Si K-shell near-edge X-ray absorption fine structures (NEXAFS) on the polarization angle. Two approaches helped to elucidate the orientation mechanism: the substitution effect and the deposition-rate dependence. The orientation angles of Si-X bond axes were obtained for trimethylsilyl halides, (CH$$_{3}$$)$$_{3}$$SiX (X =F Cl Br I NCO, condensed on Cu(111) at a low (82 K) temperature: the angles are 60, 73, 61, 55, and 55 degrees with respect to the surface normal, for X =F, Cl, Br, I, and NCO, respectively. Chloride (X =Cl) produces the most parallel tilt angle. The specific orientation nature of chloride is attributed to its strong dipole moment as well as the regular tetrahedron shape of the molecule. The molecular volumes calculated verify this view. Furthermore, deposition rates are found to greatly influence the growth manner: namely, high deposition rates led to a slightly perpendicular orientation of Si-X bond axis.

Journal Articles

X-ray absorption fine structure spectra of rust layers on Fe-based binary alloys exposed to Cl-rich environment

Konishi, Hiroyuki; Yamashita, Masato*; Uchida, Hitoshi*; Mizuki, Junichiro

Proceedings of 16th International Corrosion Congress (CD-ROM), 6 Pages, 2005/09

XANES measurements of rust layers formed on Fe, Fe-Cr alloys and Fe-Ni alloys exposed to a Cl-rich atmosphere have been performed using synchrotron radiation in order to clarify the relation between the structural properties of the rust layer on weathering steel and anticorrosive alloying elements and/or chloride ions. The XANES spectra around Cl K-edge revealed that the rust layer on the Fe-based binary alloys contains unidentified chloride in addition to akagan$'e$iteite. The Fe K-edge XANES results indicated that the rust layers are composed mainly of well-known iron oxides, goethite, akagan$'e$ite, lepidocrocite and magnetite. In particular, the mole ratio of akagan$'e$ite in the rust layers on the Fe-Ni alloys is relatively higher than that of the Fe-Cr alloys. The Cr K-edge XANES spectra of the rust layers on the Fe-Cr alloys depends on the Cr alloy content. Therefore, the local structure of Cr in the rust layer is variable with the Cr density. In contrast, the Ni K-edge XANES results show that the local structure of Ni in the rust layer are unique in a certain Ni content range.

Journal Articles

High-pressure induced structural changes in metastable Ge$$_{2}$$Sb$$_{2}$$Te$$_{5}$$ thin films; An X-ray absorption study

Fons, P.*; Kolobov, A.*; Tominaga, Junji*; Katayama, Yoshinori

Nuclear Instruments and Methods in Physics Research B, 238(1-4), p.160 - 162, 2005/08

 Times Cited Count:5 Percentile:41.85(Instruments & Instrumentation)

Super-resolution (SR) media offer up to a factor of ten increase in areal storage density over conventional DVD media. Although SR has been realized, there is a strong need for a deeper understanding of structural and electronic changes in Ge$$_{2}$$Sb$$_{2}$$Te$$_{5}$$ (GST), a principal optical memory component, with external perturbations. Recording of SR disks leads to the formation of gas-phase bubbles that in turn lead to the development of large stresses on the underlying GST layer. In this paper we report on XAFS of nominally hydrostatic (0-10 GPa) compressive stress-induced structural changes of the metastable crystalline phase of GST. An analysis showed that the initial splitting of Ge Te bond lengths of the room-temperature distorted rocksalt structure decreased to a small but finite splitting for $$p$$ $$_sim^{>}$$ 6 GPa. The implications of this upon the proposed ferroelectric catastrophe super-RENS readout mechanism are discussed.

Journal Articles

Synchrotron radiation photoabsorption and photoemission spectroscopy for thermal-induced reoriented Si polymer

Nath, K. G.; Shimoyama, Iwao; Sekiguchi, Tetsuhiro; Baba, Yuji

Journal of Electron Spectroscopy and Related Phenomena, 144-147, p.323 - 326, 2005/06

 Times Cited Count:5 Percentile:28.29(Spectroscopy)

The effect of laser annealing on electronic atructures and molecular orientation for poly(dimethylsilane), {PDMS, [Si(CH$$_{3}$$)$$_{2}$$]$$_{n}$$} has been studied by synchrotron radiation photoemission and photoabsorption spectroscopy. Prior to annealing, PDMS powder was mounted on the basal plane of highly oriented pyrolytic graphite. Both Si 1s X-ray photoemission spectroscopy and near-edge X-ray absorption fine structure (NEXAFS) spectroscopy at Si 1s edge show that electronic structures have been modified due to annealing. Furthermore, the angle-dependent NEXAFS spectra clearly indicate that the annealed products maintain a specific orientation. Interestingly, no such kind of orientation is present in as-received PDMS powder as no angle-dependency is observed before annealing.

Journal Articles

Characterization of rust layer formed on Fe, Fe-Ni and Fe-Cr alloys exposed to Cl-rich environment by Cl and Fe K-edge XANES measurements

Konishi, Hiroyuki; Yamashita, Masato*; Uchida, Hitoshi*; Mizuki, Junichiro

Materials Transactions, 46(2), p.329 - 336, 2005/02

 Times Cited Count:26 Percentile:80.2(Materials Science, Multidisciplinary)

Chloride in atmosphere considerably reduces the corrosion resistance of conventional weathering steel containing a small amount of Cr. Ni is an effective anticorrosive element for improving the corrosion resistance of steel in a Cl-rich environment. In order to clarify the structure of the protective rust layer of weathering steel, Cl and Fe K-edge X-ray absorption near edge structure (XANES) spectra of atmospheric corrosion products (rust) formed on Fe, Fe-Ni and Fe-Cr alloys exposed to Cl-rich atmosphere were measured. The Fe K-XANES measurements enable the characterization of a mixture of iron oxides such as rust. The chemical composition of the rust was determined by performing pattern fitting of the measured spectra. All the rust is composed mainly of goethite, akagan$'e$ite, lepidocrocite and magnetite. Among these iron oxides, akagan$'e$ite in particular is the major component in the rust. Additionally, the amount of akagan$'e$ite in the rust of Fe-Ni alloy is much greater than that in rust of Fe-Cr alloy. Akagan$'e$ite is generally considered to facilitate the corrosion of steel, but our results indicate that akagan$'e$ite in the rust of Fe-Ni alloy is quantitatively different from that in rust of Fe-Cr alloy and does not facilitate the corrosion of steel. The shoulder peak observed in Cl K-XANES spectra reveals that the rust contains a chloride other than akagan$'e$ite. The energy of the shoulder peak does not correspond to that of any well-known chlorides. In the measured spectra, there is no proof that Cl, by combining with the alloying element, inhibits the alloying element from acting in corrosion resistance. The shoulder peak appears only when the content of the alloying element is lower than a certain value. This suggests that the generation of the unidentified chloride is related to the corrosion rate of steel.

Journal Articles

Cl K-edge XANES spectra of atmospheric rust on Fe, Fe-Cr and Fe-Ni alloys exposed to saline environment

Konishi, Hiroyuki; Yamashita, Masato*; Uchida, Hitoshi*; Mizuki, Junichiro

Materials Transactions, 45(12), p.3356 - 3359, 2004/12

 Times Cited Count:9 Percentile:51.48(Materials Science, Multidisciplinary)

Cl K-edge XANES measurements of atmospheric corrosion products (rust) formed on Fe, Fe-Ni and Fe-Cr alloys in chloride pollution have been performed using synchrotron radiation in order to clarify roles of anticorrosive alloying elements and of Cl in the corrosion resistance of weathering steel. The spectra of binary alloys show a shoulder structure near the absorption edge. The intensity of the shoulder peak depends on the kind and amount of the alloying element, whereas the energy position is invariant. This indicates that Cl is not combined directly with alloying elements in the rust.

Journal Articles

O 2$$p$$ hole-assisted electronic processes in the Pr$$_{1-x}$$Sr$$_{x}$$MnO$$_{3}$$ (x=0.0, 0.3) system

Ibrahim, K.*; Qian, H. J.*; Wu, X.*; Abbas, M. I.*; Wang, J. O.*; Hong, C. H.*; Su, R.*; Zhong, J.*; Dong, Y. H.*; Wu, Z. Y.*; et al.

Physical Review B, 70(22), p.224433_1 - 224433_9, 2004/12

 Times Cited Count:28 Percentile:75.17(Materials Science, Multidisciplinary)

no abstracts in English

Journal Articles

MCD measurement at the Tb $$M$$$$_{4,5}$$-edges of Tb$$_{17}$$Fe$$_{x}$$Co$$_{(83-x)}$$ perpendicular magnetization films

Agui, Akane; Mizumaki, Masaichiro*; Asahi, Toru*; Sayama, Junichi*; Matsumoto, Koji*; Morikawa, Tsuyoshi*; Nakatani, Takeshi; Matsushita, Tomohiro*; Osaka, Tetsuya*; Miura, Yoshimasa*

Transactions of the Magnetics Society of Japan, 4(4-2), p.326 - 329, 2004/11

The electronic and spin state of the perpendicular magnetization film Tb$$_{17}$$Fe$$_{x}$$Co$$_{(83-x)}$$ was investigated by means of magnetic circular dichroism spectroscopy for each element. The samples are Tb$$_{17}$$Fe$$_{x}$$Co$$_{(83-x)}$$ while the ratio of a rare-earth metal Tb to transition metals Fe and Co is constant, the composition ratio of Fe and Co is changed. Changing the ratio, we estimated the expected orbital moments $$<$$$$L$$$$_{z}$$$$>$$ of Tb 4f electrons. The macroscopic magnetic property is studied from the microscopic point of view.

Journal Articles

EPR studies of 5-bromouracil crystal after irradiation with X rays in the bromine K-edge region

Yokoya, Akinari; Takakura, Kaoru*; Watanabe, Ritsuko; Akamatsu, Ken*; Ito, Takashi*

Radiation Research, 162(4), p.469 - 473, 2004/10

 Times Cited Count:3 Percentile:10.46(Biology)

X-ray absorption spectra from single crystals of 5-Bromouracil were measured with the transmission mode in the energy range from 13.41 to 13.50 keV using the linearly polarized synchrotron radiation (SR). A characteristic resonance structure, consisting of four peaks, was recognized in the spectra in the Br K-edge region. The intensities of these peaks were strongly dependent on the crystal rotation about the normal of the crystal b-c plane, which was set perpendicular to the X-ray beam direction. (SR X-rays are polarized in the horizontal plane.) Molecular orbital calculations indicate that these resonance peaks are associated with the transitions from the 1s electron of Br to the Br-C molecular antibonding orbitals and to a shape resonance. The observed anisotropy of each photoabsorption peak might originate from the angular dependences of these molecular orbitals.

Journal Articles

Macroscopic Separation of Dense Fluid Phase and Liquid Phase of Phosphorus

Katayama, Yoshinori; Inamura, Yasuhiro*; Mizutani, Takeshi*; Yamakata, Masaaki*; Utsumi, Wataru; Shimomura, Osamu*

Science, 306(5697), p.848 - 851, 2004/10

 Times Cited Count:129 Percentile:96.34(Multidisciplinary Sciences)

Structural transformation between two liquid structures of phosphorus that occurred at about 1 GPa and 1000$$^{circ}$$C was investigated by in-situ X-ray radiography. When the low-pressure liquid was compressed, dark and round objects appeared in the radiograph. X-ray diffraction measurements confirmed that these objects were the high-pressure liquid. The drops grew and eventually filled the sample space. Decompressing caused the reverse process. The macroscopic phase separation supported the view that it was a first-order liquid-liquid phase transition. X-ray absorption measurements revealed that the change in density at the transition is about 40 % of the density of the high-pressure liquid.

Journal Articles

X-ray magnetic circular dichroism at the U $$N_{4,5}$$ edges of uranium monochalcogenides US, USe and UTe

Okane, Tetsuo; Okamoto, Jun; Mamiya, Kazutoshi; Fujimori, Shinichi; Saito, Yuji; Muramatsu, Yasuji; Fujimori, Atsushi; Ochiai, Akira*

Physica B; Condensed Matter, 345(1-4), p.221 - 224, 2004/03

 Times Cited Count:4 Percentile:25.79(Physics, Condensed Matter)

Magnetic circular dichroism (MCD) has been measured at the U $$N_{4,5}$$ absorption edges of ferromagnetic uranium monochalcogenides US, USe and UTe. The MCD signals are weaker in US than in USe and UTe. Both the spin and orbital moments are increased in going from US to USe, and then reduced from USe to UTe.

Journal Articles

Characterization of carbon films on the Japanese smoked roof tile "Ibushi-Kawara" by high-resolution soft X-ray spectroscopy

Muramatsu, Yasuji; Motoyama, Muneyuki*; Denlinger, J. D.*; Gullikson, E. M.*; Perera, R. C. C.*

Japanese Journal of Applied Physics, Part 1, 42(10), p.6551 - 6555, 2003/10

 Times Cited Count:6 Percentile:28.82(Physics, Applied)

Carbon films on Japanese smoked roof tile "Ibushi-Kawara" were characterized by high-resolution soft X-ray spectroscopy using synchrotron radiation. By comparing the soft X-ray emission and absorption spectra of Kawara with the reference carbon compounds, it was determined that the carbon films on Kawara consist of mostly carbon-black-like sp2 carbon atoms and that the surface also contains polyethylene-like sp3 carbon atoms. The take-off/incident-angle dependence on the X-ray emission/absorption spectra of Kawara implies that the carbon-black-like sp2 carbon atoms partially form a layer structure parallel to the basal clay plane. From the take-off-angle dependence of the p/s-peak intensity ratio in the X-ray emission spectra, the layer ordering of the carbon films is estimated to be 50% of highly oriented pyrolytic graphite (HOPG). Therefore, the metallic oxidized color and durability are due to the layer structure and the random structure that connects the layer-structured clusters, respectively.

38 (Records 1-20 displayed on this page)