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Foreword

Based on the framework laid down by AIST (the Agency of Industrial Science and Technology) of

MITI (the Ministry of International Trade and Industry) for R&D in the areas of industrial science and

technology, frontier carbon technology (FCT) R&D project started in 1998. This project is entrusted

to the Japan Fine Ceramic Center (JFCC), a foundation in which 15 companies and 1 organization,

participate, under contract with the New Energy Development Organization (NEDO). At the same

time, JFCC made a joint research contract with National Institute of Materials and Chemical Research

(NIMC) and 2 other national research institutes to establish research scheme. In addition, joint

research contract is concluded with Osaka University, Tokyo Institute of Technology and Waseda

University, and cooperative research contract is made with Mie University, Osaka City University,

Kyoto University, University of Sussex, Techmical University of Vienna and Fraun hofer Institute.

This project has been promoted under the research scheme with the cooperation of industry,

government and universities.

This project has 2 main features. One of them is above-mentioned FCT research system. In

this system, the Research Promotion Council, which is composed of representatives from industry,

government and universities, adjust or steer the entire progress. The other feature is a system to carry

out intensive research and satellite research in parallel so as to increase efficiency of R&D. Intensive

research is made by research institutes of the Fine Ceramic Center in National Institute of Materials and

Chemical Research (Tsukuba) and Osaka University, while satellite research is conducted by 6

companies and 1 organization, members of the Fine Ceramic Center.

This report is results of research in 2000, R&D of frontier carbon technology (development of

High Function Control System for Power Generation).

Frontier Carbon Technology Research Organization

9F3EM3SX-M*Research grant & Evaluation cost Fund & Aid

Consignment

Central Research Lab. (NIMC) Central Research Lab. (Osaka.U.)

Joint

research

Joint

research

Reentrustment Reentrustment

Joint researchJoint research

NEDO

AIST

Universities Universities

NIMC Osaka Univ.

Overseas Organizations

Satellite research at

Private enterprises

JFCC

(V )

(NEDO^|t5fe: FCT9f%*S)

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(vi)

Frontier Carbon Technology Research Organization(NEDO entrustment to JFCC —FCT)

FCT R&D promoting comittee Comittee Sub-comittee

....................... ........ ...................... ........(Participating members) !Asahi Chemical Industry Co., Ltd. ;Ishikawajima-Harima Heavy Industries Co., Ltd. | Osaka Gas Co., Ltd. «Kawasaki Heavy Industries, Ltd. |Institute of Research and Innovation IShowa Denko K.K. ;Tokyo Gas Co., Ltd. IToshiba Corporation ;NEC CorporationJapan Fine Ceramics Center IMitsubishi Heavy Industries, Ltd. j

(Participating members)Kobe Steel, Ltd.Sumitomo Electric Industries, Ltd. Matsushita Electric Industries Co., Ltd.

(Participating members)Ion Engineering Research Institute Corporation Ishikawajima-Harima Heavy Industries Co., Ltd. Kawasaki Heavy Industries, Ltd.Sumitomo Electric Industries, Ltd.Mitsubishi Heavy Industries, Ltd.Mitsubishi Materials Corporation Applied Films Corporation

: The present R&D was carried outby the Organizations

New Materials Synthesis Technology

Reentrustment

Reentrustment

Reentrustment

Joint research

Reentrustment

Joint research

Joint research

Reentrustment

Osaka University

Mie University

Kyoto University

University of Sussex

Osaka-City University

Technical University of Vienna

Fraunhofer Institute

Waseda University

Tokyo Institute of Technology

Mechanically Functional Materials Processing Technology

Electrically Functional Materials Processing Technology

— Central Reseach Laboratry (Osaka University)________

Central Reseach Laboratry, NIMC (National Institute of Materials and Chemical Research),

MEL

Satellite laboratories (Kobe Steel,Ltd.)(Sumitomo Electric Industries,Ltd.)

— Satellite Laboratories(Ishikawajima-Harima Heavy Industries Co.,Ltd.) (Sumitomo Electric Industries,Ltd.)____________

Central Reseach Laboratry: NIMC (National Institute of Materials and Chemical Research), NIRIM

Satellite Laboratories (Showa Denko K.K.)(Toshiba Corporation)(NEC Corporation)(Japan Fine Ceramics Center)

Reentrustment

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^Frontier Carbon Technology Research organization^

Project Managing Group (PMG)

© Masanori Yoshikawa (JFCC., Tokyo Inst, of Technol. Professor emeritus)OShuzo Fujiwara (NIMC)OYoshinori Koga (NIMC) © Project leader□Akihiro Tanaka (MEL) O Sub-Project leader□Koji Kobashi (JFCC) □ Group leader

1. Development of Substance original production technologyMechanically high function materials

Research Center (NIMC)

Tamikuni Komatsu Mutsumasa Kyotani Hisashi Sawai Takeshi HasegawaTakazumi Kawai Akio Nishiyama Tsutomu Ikeda Fumio KokaiTakumi Kimura M. Liehr Shunji Kurooka Toshiki KomatsuM. Cedric Chiharu Yamaguchi Manabu Taniwaki Toshiya WatanabeKatsuhiro Sasaki Akefumi Ishikura Hiromichi Yoshikawa Junya KitamuraKoichiro Wazumi Chozo Inoue Sadao Fujii Masato BanHiroaki Yosida Akiko Goto M.Popov Kazuo TugawaS.P.Hong W.Zhang

Co - researcher

Hideyo Okushi (ETL)Kikuo Harigaya (ETL)

Satellite Lab. (Toshiba)

Naoshi Sakuma Tadashi Sakai Cyo

Satellite Lab. (JFCC)

Noriyoshi Shibata Michiko KusunokiTsukasa Hirayama Yukari TaniToshiki Shimizu Toshiyuki Suzuki

Satellite Lab. (NEC)

Osamu Sugino Yoshiyuki Miyamoto

(xi)

Satellite Lab. (Showa Denko)

Tatuyuki Yamamoto Sai Inoue Hajime Murakami Yoshihisa Sakamoto Toshio Morita

Satellite Lab. (IHI)

Tadashi Sassa kenji FuchigamiJoji Shinohara Tsumoru FujiiOsamu Harasaki Kazuo UematsuKatsumi Suzuki Masaaki HoriuchiYoshinori Kawasaki Kouji Takasima

Hajime Kuwahara

Joint Research(New Materials Synthesis Technology and Mechanically Functional Materials Processing Technolgy)

NIMC NIRIM MEL Tokyo Inst, of Technol. Waseda Univ.

Shuzo Fujiwara Yoshinori Koga Keiichiro Ishikawa Tsuguyori Ghana Yozo Kakudate Takako Nakamura Kazuhiro Yamamoto Shu UsubaHiroyuki YokoiMotoo Yumura Satoshi Oshima Kunio UchidaHiroki Gogo

Mutsukazu KamoHisao Kanda Satoshi Koizumi Noriyuki Teraji

Yuji Enomoto Akihiro Tanaka Yuko HibiKazuyuki Mizuhara

Atsushi Hirata Hiroshi Kawarada

Reentrustment(New Materials Synthesis Technology and Mechanically Functional Materials Processing Technolgy)

Mie Univ. Osaka-City Univ. Univ. of Sussex Vienna Univ.of Technol. Fraunhofer Inst.

Yahachi Saito Katsumi Tanigaki H. Kroto

M. Clark

W. Wru

R. HaubnerB. Lux

B. Momma

P. KoidlC. Klages

2. Electrically Functional Materials Processing Technolgy

Research Center (Osaka Univ.)

Koji Kobashi Takeshi Tachibana Yoshiki Nishibayashi Yutaka Ando Makoto Kitabatake Akihiko Watanabe Hirosi Huruta

Satellite Lab.(Kobe Steel,Ltd.)

Koji Kobashi Takeshi TachibanaKeniti Inoue Yosihiro YokotaKazusi Hayasi Nobuyuki Kawakami

Satellite LabXSumitomo Electric,Indus.)

Naoji Fujimori Yoshiyuki YamamotoShinichi Shikata Hirohisa SaitoTakahiro Imai Keiji IsibasiKeiitiro Tanabe

Joint Research & Reentrustment Research

Osaka Univ. Kyoto Univ.

Kenjiro Oura Shinichi Nakajima Junzo IshikawaTakashi Hirao Takeshi MatsuuraTakatomo Sasaki Kiichiro TsujiTakeshi Kobayashi Sadatoshi KumagaiMotoshi Iketani Hiroshi Yoshida

3. Genenal Research Comittee (JFCC)Evaluation Comittee Research Comittee

Chairman: Osamu Fukunaga Acetech Co.,Ltd.Member Takuo Takeshita Mitsubishi Materials

Mutsukazu Kamo NIRIMMasanori Yoshikawa JFCCKenichi Kondo Tokyo Inst, of Tech.

New Mateials Synthesis Technology

Chairman: Hidetoshi Saito Nagaoka Inst, of Tech.Member Tuneo Suzuki Nagaoka Inst, of Tech

Takahiro Imai Sumitomo Electric Indus.Takafumi Ishikura Tokyo Gas Co.,Ltd

Mechanically Functional Materials Processing Technology

Chairman: Naoto Ohtake Tokyo Inst, of Tech.Member Hidetoshi Kodera Kyoto-Gakuin Univ.

Tetuya Suzuki Keio Univ.Toshiyuki Yasuhara Tokyo Inst, of Tech.Koji Une Asahi Diamond Co.,Ltd.Yasushi Taniguchi Cannon Corp.Akio Nishiyama Mitsubishi MaterialsKunio Komaki New Diamond Forum

Chairman: Syuji Yazu Sumitomo Electric Indus.Member Takahiro Imai Sumitomo Electric Indus.

Atsuhito Sawabe Aoyama-Gakuin Univ.Takatosi Yamada Aoyama-Gakuin Univ.Tetuya Suzuki Keio Univ.Hidetoshi Kodera Kyoto-Gakuin Univ.Naoto Ohtake Tokyo Inst, of Tech.Toshiyuki Yasuhara

Tokyo Inst, of Tech.Syozou Kawano Tohoku Univ.Hidetoshi Saito

Nagaoka Inst, of Tech.Tuneo Suzuki

Nagaoka Inst, of Tech.Koji Une Asahi Diamond Co.,Ltd.Yasushi Taniguchi Cannon Corp.Kenichi Inoue Kobe Steel,Ltd.Manabu Sato Toshiba Tungaloy Co.,Ltd.Takafumi Ishikura Tokyo Gas Co.,LtdKazuhiro Baba NEC Corp.Masatoshi Kitagawa

Matsushita Electric Indus.Akio Nishiyama Mitsubishi MaterialsKunio Komaki New Diamond Forum

Electrically Functional Materials Processing Technology

Chairman: Hidetoshi SaitoNagaoka Inst, of Tech.

Member Takatosi Yamada Aoyama-Gakuin Univ.Syozou Kawano Tohoku Univ.Kenichi Inoue Kobe Steel,Ltd.Masatoshi Kitagawa

Matsushita Electric Indus.

(xi)

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(xvi)

Contents

(1) Foreword........................................................................................................................................ (iii)

(2) Organization Scheme of Frontier Carbon Technology......................................................... ( V )

(3) Organization of the Joint Research Consortium of Frontier Carbon Technology............. (vil)

(4) List of Members of the Joint Research Consortium of Frontier Carbon Technology........ (xi)

Chapter 1 Development of substance............................................................................................ 1

1.1 Synthesis and characterization of high temperature corrosion resistant materials........ 2

Chapter 2 Development of original production process technology for mechanically high

function materials............................................................................................................ 17

2.1 Composition gradient film forming techniques................................................................... 18

2.1.1 Development of high-temperature stable films............................................................. 18

2.2 Large area film forming technology..................................................................................... 29

2.2.1 Report of R&D system (Large diamond coater) for the fiscal year 1998................... 29

2.2.2 Research and development of large area diamond deposition technology.................... 43

2.3 Joint research and entrustment research............................................................................... 57

2.3.1 [Joint Research]

Microfabrication of high fanctional carbon ............................... Waseda Univ. • • • • 57

2.3.2 [Joint Research] Large-area high-rate deposition technique of diamond and related

carbon films.................................................................. Tokyo Inst.Tech. Univ. • • • • 69

2.3.3 [Entrustment Research] Large area diamond depositions and modification of

diamond film growth..................................................................................................... 78

Chapter 3 Combined research and Investigation......................................... JFCC (Tokyo) • • • • 88

3.1 Search on Fabrication Processes for Mechanically High-Performance

Materials ................................................................................................................................ 88

3.2 Overseas Investigation....................................................................................................... 153

3.3 Activity of R&D committee............................................................................................... 165

Chapter 4. Development of common base technology (platform) .......................................... 171

(Appendix) Publication list research report........................................................................... 173

Activity of R&D ................................................................................................. 190

(Insitute of Materials and Chcmuial Research) ................................................ 191

(Mechanical Engineering Laboratory).............................................................. 203

(National Institute for Research in Inorganic Materials)................................. 206

(xvi)

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Sputter cleaning condition

Treatment pressure 6.8 mPaApplied voltage for cleaning 1000 VTreatment time 300 sec

Deposition condition

Treatment pressure 13 mPaSubstrate temperature 773 KDeposition time 120 minApplied voltage for bombardment 300VDeposition rate of boron 1 nm/min

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-20-

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-27-

2 ^ C B^C C BN ^ ## f 6 2 & T FCT y o ^ h (7)—c

1) T. Komatsu, Y. Kakudate and S. Fujiwara, Rev. High Pressure Sci.Techol., 7 (1998) 983.

2) S. Kurooka, T. Ikeda, N. Iwamoto, Surface Engineering: In Material Science I,

Ed. by S. Seal et. al. TMS, Warrendale (2000) 357.

3) R. Geick and C. H. Perry, Phys. Rev., 146 (1966) 543.

4) A. Kolitsch, X. Wang, D. Manova, W. Fukarek, W. Moller and S. Oswald, Diam. Relat. Mater., 8

(1999) 386.

5) G. G. Stoney, Proc. Roy. Soc. A82 (1909) 172.

6) E. C. Critenden and Hoffman, Phys. Rev. 78 (1950) 349.

7) H. P. Murbach and Wilman, Proc. Soc. B66 (1953) 905.

8) C. Borse, TZ fur praktische Metallbearbeitung, 66 (1972) H. 1, S, 1/8.

9) I. L. Zagyansky and G. V. Samsonov, J. Appl. Chem. USSR, 25 (1952) 629.

10) C. G. Gofer and J. Economy, Carbon, 33, 4 (1995) 389.

11) L. E. Pechentkovskaya and T. N. Nazarchuk, Sov. Powder Metall., 7, 223 (1981) 83.

-28

2.2

2.2.1 T'fJDJS^TC V-fSM&'fa*4=9f 7 (7<H)

2.2.1.1 IntroductionThe second system delivered to the FCT project by LEYBOLD (now APPLIED FILM

CORPORATION) known as TruDi (standing for TRUe Diamond) is a large area coating system, see Figure 2.2.1-1. The plasma of TruDi is produced by eight parallel linear microwave-radiating structures located in fused silica tubes, which are used as atmosphere-to-vacuum interfaces. Driven by two 15 kW, 2.45 GHz magnetron tubes, eight individual plasma discharges form circumjacent the silica tubes. Care has been taken to properly design both the rectangular and coaxial waveguide sections since power levels of up to 15 kW c/w can easily cause high voltage arcs and also result in melting of the waveguide material. Therefore, the individual impedances of all transmission line elements and all passive circuits are fully matched to the generators so that operation without reflected power is possible. In the TruDi system, the process gases, mainly hydrogen, methane and carbon dioxide are dissociated and chemically activated by the plasma primarily on or near the outer surfaces of the fused silica tubes, since it is not possible to sustain a high pressure, contact free and flat discharge over areas much larger than the wavelength of the applied microwaves. The maximum operating gas pressure is currently in the range of 4 mbar. The maximum thermal load on the silica tubes limits the process pressure. The surface temperatures can easily exceed one thousand degrees centigrade even with airflow cooling on the inside surfaces of the silica tubes. The substrate can be oscillated during the deposition process to compensate for the non-uniform plasma densities inherent to discrete linear plasma sources. Since the overall thermal load from the plasma can be problematic particularly for dielectric substrates an efficient and homogeneous gas buffer substrate cooling system has been installed.

Figure 2.2.1-1 TruDi - the microwave PECVD system for diamond coatings on 300x300 mm2 substrates

-29-

The system has the following characteristics:• Equipped with one rotary pump a vacuum of 5T0"2 mbar can be reached within 90 seconds,

with a base pressure at 10'3 mbar.• For a better homogeneity, depositions can be done on a oscillating substrate oscillation speed

is variable. The substrate is insulated for the future use of biasing.• The plasma discharge can be sustained in a pressure ranging from 102 to 4 mbar (maximum

limit due to the thermal overload on the quartz tubes).• The position of the substrate has only a small influence on the plasma shape. But if the

substrate position is set too far away from the plasma region, the growth rate, the substrate temperature are considerably reduced.

• The temperature of the substrate can be measured with a pyrometer through the view port located in the top of the chamber.

• All of the deposition parameters are controlled from a visualization software connected to a stand-alone computer system.

• The process control and the measurement of the deposition parameters are achieved through a programmable logic controller (PLC) SIMATIC S7-300 from SIEMENS. The parameters are sent and read from a PC through a visualization software created for the system. Once the deposition parameters have been sent to the PLC, the process can run with all the safety interlocks even if the PC has been switched off. To record the parameters during the depositions, the PC needs to be on with the visualization software running.

Schematic representation of the system

Mobile armMFC

8 quartz tubes

I m "ilL- Plasma , X. Jr| region

Substrate

Figure 2.2.1-2 Schematic representation of the TruDi from the side

-30-

Water inlet outlet

Figure 2.2.1-3 Schematic layout of TruDi

Safety interlocksFor a safer use of the system, many safety interlocks have been built in the PLC. Modifications of the status of valves, motors or pumps have been blocked, if it was thought that this action might result in a danger either for the deposition in process or for the user. For example, the microwave generators can’t be switched on when the reactor door is opened, as well as when no gas is flowing through the chamber. When no cooling water is circulating through the system, or when the dilution gas at the exit of the vacuum pump isn’t open, processes can’t be run. The process will be stop if the cooling water flow is cut after that a visual and sound warning has been sent to the user. If the pressure in the chamber rises above 120 mbar (in case of fracture of a quartz tube, or another sudden vacuum leak of the reactor), the process will be shut down. Arc detectors automatically switch the microwave power generators off in case of an arc in one of the waveguide. The reflected power is monitored and the user can set a safety limit. When the reflected power becomes higher than this limit for a maximum of 15 seconds, the microwave power generators are turned off.

2.2.1.2 ExperimentsThe aim of the first depositions performed with TruDi was to prove that diamond could be deposited with this plasma source. Once this has been proved, the parameters were varied to observed their influence on the deposited materials. Many different analyzing techniques were used to characterize the layer: Raman spectra, AES, XRD and XPS. The microwave power, the process pressure and the methane concentration were varied. The typical deposition parameters are given in Table 2.2.1-1. The deposition conditions were chosen in a window that allows a safe and stable use of the system with a closed plasma over the whole substrate area.

-31-

Table 2.2.1-1 Nucleation and deposition parameters: The substrate temperature wasmeasured with a pyrometer through a view port of the top part of the reactor.

NucleationSubstrate distance from quartz tubes [mm] Oscillation speed [%]MW power [kW]Reflected power [W]H2 [seem]CH4 [seem]Pressure [mbar]Deposition time [h]Substrate temperature [°C]

Dry scratch with diamond powder 17 30 20 ~0

100010 (i.e. 1 %)

1-20-650

Effect of the process pressureStarting with the typical parameters given in Table 2.2.1-1, the pressure was varied between 0.7 and 2 mbar, while keeping all the other parameters constant.

MorphologyThe figure 2.2.1-4 shows the morphology of the grown films with TruDi while varying the process pressure. It was seen that at a pressure under 1.2 mbar, the grown film is difficult to observe by SEM. A film was grown but it is thought to be amorphous. At a pressure equal or higher than 1.2 mbar, well- defined crystals are seen. The morphology is similar to the one of film grown at higher pressure, but some amorphous-like phase can be seen between the crystals.

Figure 2.2.1-4 SEM pictures of the films deposited with TruDi with various process pressure [0.7-2 mbar]. Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 jL/m grains); depositions with 2x10 kW, 1 % CH4 in 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%; a) 0.7 mbar; b) 1.2 mbar; and c) 2 mbar.

-32-

Raman spectraFrom the number of different peaks it can be assumed that the film is formed of many different kinds of bonds, see Fig. 2.2.1-5. It can be seen that the film isn’t only composed of sp3, sp2 bonds but also of trans-polyacetylene (trans-PA). The broad peak around 1470 cm'1 is assigned to C=C double-bond stretching vibration (vl), and that around 1150 cm'1 is due to the mixed vibrations (v3) of C-C single bond stretching and CH in-plane bending. The presence of trans-PA had been often reported to be present in bad quality diamond CVD films that are grown at too low a substrate temperature or with too high a methane content. It is therefore possible that trans-PA is also formed at low pressure. The intensity of the G band decreased with increasing process pressure. The D band is rather broad, between 1300 and 1360 cm'1. The signal/noise ratio is rather high for the film deposited at 0.7 mbar; because of the film thickness, which is very thin.

G band0.7 mbar 1.2 mbar

D band

2 mbar

Trans-PA v1

Trans-PA v3

Raman shift [cm'1]

Figure 2.2.1-5. Effect of the process pressure [0.7-2 mbar] on the Raman spectra of the deposited films Nucleation: scratched with dry diamond powder (nanopower mixed with 0.25 ^m grains); depositions with 2x10 kW, 1% CH4 in 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%.

For comparison with green light Raman (514 nm), UV (244 nm) Raman was used to analyse the sample grown with 2 mbar. Figure 2.2.1-6 shows a comparison of both spectra. With the UV Raman, the D band intensity is increased while the trans-PA peaks don’t appear. UV Raman analysis proved that film with a high content of sp3 was deposited in the film. The XPS analysis of this sample gave the following atomic concentration: Cls 90.59%; Ols 8.33% and Si2p 1.08%. A fair amount of oxygen was still detected but this could be attributed to exposure to air. Detailed analysis performed in the range of 280-290 eV showed that C-C (sp3) bonds accounted for 93% of the overall carbon bonds. The oxygen present in the film is either bonded with Si (Si02; 48%) or present as O-H (contamination from air; 52%). The silicon atoms are either bonded to O (Si02; 63%) or C (SiC; 37%).

33

Trans-PAv1Green (514 nm) UV (244 nm)

D band

G band

Trans-PA v3

1100 1300Raman shift [cm-1]

Figure 2.2.1-6 Raman spectra of the sample grown with 2 mbar, once with UV Raman and once with green light Raman.

XRD spectraAs expected after the UV Raman analysis, the XRD measurements (Fig. 2.2.1-7) showed that diamond was effectively grown at pressure higher or equal to 1.2 mbar. The film grown at 0.7 mbar didn’t show any diamond peak, unlike for the 2 other samples. The pSiC peaks was seen and it intensity was higher at lower pressure. It is thought that the interlayer between the film and the substrate is mostly formed of pSiC. When the pressure was low, the growth rate was lower and as the deposition times were kept the same, the film thickness decreased with the process pressure. This could explain why the interlayer signal is larger at lower pressure.

-34-

0.7 mbar

2 mbar !

2e n

Figure 2.2.1-7 Effect of the process pressure [0.7-2 mbar] on the XRD spectra of the deposited films. Nucleation: scratched with dry diamond powder (nanopower mixed with 0.25 pm grains); depositions with 2x10 kW, 1% CH4 in 1000 seem H2 for 20±2 hours with a substrate oscillation of 30%.

ConclusionDepositions are a pressure lower than 1.2 mbar didn’t lead to the growth of diamond; moreover the plasma etched locally the substrate. When the pressure is high enough, growth of diamond was observed. UV Raman XPS and XRD analysis proved that the grown films were mostly composed of sp3 bonds.

Effect of the microwave powerStarting with the typical parameters given in Table 2.2.1-1, the microwave power was varied between 16 and 20 kW, while keeping all the other parameters constant.

MorphologyThe figure 2.2.1-8 shows the morphology of the grown films with TruDi at two different microwave power levels. It was seen that with 16 kW (see figure 2.2.1-8 a), the morphology of the grown film is rather different from the standard polycrystalline diamond film. The larger crystals grew mostly in the scratch lines, with smaller crystals forming a closed film between the larger crystals.

-35-

Figure 2.2.1-8 SEM pictures of the films deposited with TruDi with various microwave power [16-20 kW]. Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 grains); depositions with 1 mbar, 1% CH4 in 1000 seem H2 for 19±3 hours with a substrate oscillation of 30%; a) 16 kW; b) 20 kW.

Raman spectraThe measured Raman spectra (see Fig. 2.2.1-9) were rather similar, but some differences could be pointed out. The G band intensity decreased with increasing microwave power. The D was split in 2 bands are lower microwave power level and formed a broad peak at 20 kW. Beside that another broad peak was seen at 1240 cm"1 at high power. Its origin couldn’t be explained.

D band2x8 kWG band2x10 kW

Si 2nd order

Trans-PAv1

Trans-PA v3

Raman shift [cm"1]

Figure 2.2.1-9 Effect of the microwave power level [16-20 kW] on the Raman spectra of the deposited films. Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 jum grains); depositions with 1 mbar, 1% CH4 in 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%;

-36

XRD spectraThe XRD analysis confirmed one more time what the SEM observations of the samples showed us. Both measured spectra are shown in Fig. 2.2.1-10. The grown film with 16 kW didn’t show any diamond peak, but only a broad peak for pSiC at 35.60°. With 20 kW, beside the large |3SiC peak, the 3 main peaks for diamond were clearly seen.

3

si&</>c0)

20 30 40 50 602 6[°]

70 80 90 100

Figure 2.2.1-10 Effect of the microwave power level [16-20 kW] on the XRD spectra of the deposited films. Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 A/m grains); depositions with 1 mbar, 1% CH4 in 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%;

ConclusionThe film deposited with only 16 kW didn’t show the expected characteristic of diamond films. A D band was however observed. From these samples, it appears that 20 kW is the minimal power needed to grow reasonable quality diamond.

Effect of methane concentrationStarting with the typical parameters given in Table 2.2.1-1, the methane concentration was varied between 0.5 and 2 %, while keeping all the other parameters constant.

MorphologyThe figure 2.2.1-11 shows the morphology of the grown films with TruDi with three different methane concentrations. It was seen that with 0.5 % methane, the crystals edged were very smooth, but quite a number of faces showed steps. Doubling the methane fraction, the faces became smoothers, but some amorphous phase was observed between the crystals. With a methane concentration of 2%, the crystals didn’t exhibit smooth faces neither edges. The average crystal size was slightly smaller for the film grown with 0.5% methane. As the films were grown during the same time period (20 hr.) such a difference is expected. The morphology of these crystals showed us that the grown films were very similar to diamond as many (111) faces were seen.

-37-

Figure 2.2.1-11 SEM pictures of the films deposited with TruDi with various methane concentration [0.5-2%]. Nucleation: scratched with dry diamond powder (nanopower mixed with 0.25 jum grains); depositions with 2x10 kW, 1 mbar, 1000 seem H2 for 20±2 hours with a substrate oscillation of 30%; a) 0.5%; b) 1%; and c) 2%.

Raman spectraThe Raman spectra for these three samples are shown in Figure 2.2.1-12. The D band was particularly seen for the films grown with 1 and 2% methane. While the trans-PA peaks were the highest for the deposition done with 0.5% CH4. As this film was probably thinner than the other ones, could explain why the trans-PA signals appeared with more intensity. The film grown with 1% methane seemed to have the lower graphite content, as its G band was much lower compared the other peaks. With the 2% CH4, the trans-PA peaks weren’t so important compared to the D and G bands.

-38-

D band0.5% I G band

Trans-PA v1

Trans-PAv3

Raman shift [cm'1]

Figure 2.2.1-12 Effect of the methane concentration [0.5-2 %] on the Raman spectra of the deposited films Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 /vm grains); depositions with 2x10 kW, 1 mbar, 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%.

XRD spectraThe XRD spectra measured on the three samples are shown in Figure 2.2.1-13. The diamond peaks were distinctly seen for the samples grown with 1 and 2 % methane. Only the (220) diamond peak was observed for the film deposited with 0.5% CH4. This was rather surprising as the intensity of the (111) diamond peak should normally be almost 4 times higher and it was not observed. The (BSiC peaks were detected on the film grown with the lowest methane contents. It is assumed that the interface between the film and the substrate is formed of pSiC and when the film was thinner, the importance of the interface region became larger. The peaks seen at 42° and 71° were probably ghost peaks due to a problem of the X-ray apparatus.

-39-

0.5 %

Q G,<*

20 n

Figure 2.2.1-13 Effect of the methane concentration [0.5-2 %] on the XRD spectra of the deposited films Nucleation: scratched with dry diamond powder (nano-power mixed with 0.25 pm grains); depositions with 2x10 kW, 1 mbar, 1000 seem H2 for 20±1 hours with a substrate oscillation of 30%.

ConclusionOver the whole range of methane concentrations, diamond was grown. When the methane concentration was low, the growth rate was smaller and longer deposition times would probably show similar XRD spectra.

2.2.1.3 Problems and solutionsSince the installation of TruDi in Tsukuba, many problems arose. The following paragraphs explain the most important problems and the found solutions.

Tuning of the magnetronsIn order to be able to stable emission of the microwaves at the designated frequency, a perfect setting of parameters controlling microwave emission by the magnetron is obligatory. These parameters are Imagnet, the current for the electro-magnet, and 2 upper-limits of the high-voltage (between the anode and the cathode) in the magnetron; one during start of the magnetron: Umagne,ron(Start); and one while running: Umagnetron(Run). Looking at the emission spectra of the magnetron (what it is the frequency of the microwaves, ideally 2.45 GHz), it’s possible to tune all these parameters in order to a have small emission range of ± 1 MHz. The parameters are dependant of the microwave power; for example, the Imagnet has to be increased proportionally with the microwave power level. Figure 2.2.1-14 shows the dependence of these parameters with the microwave power.

-40-

Upper limit of the high-voltage around 12-12.5 kV

Minimum Maximum

15 MW power [kW]

Figure 2.2.1-14 Evolution of the anode current depending on the controlled variation of the electro magnet current for different microwave power in a 15 kW magnetron

Oil in the compressed airArcs often melted various parts of the systems. The occurrence of the arcs wasn’t understood until oil was found in the compressed air circuit. As the air is used to cool the inside to the quartz tubes, the oil accumulated along the antennas or in the power divider. The presence of oil increased the occurrence of arc destroying some antennas and shield (See pictures in Fig. 2.2.1-15). To solve this problem, oil filters were added between the compressor and the system.

Figure 2.2.1-15 Damages that occurred due to the oil mist in the cooling air circuit: Left:melting of an antenna; Right: Al shield that melted due to an arc along the quartz ring used as support.

-41-

Arcing in the power divider of MW2During various tests to increase the power to level higher than 20 kW, arcs occurred between the inner and outer conductors at the end of the last division in the power divider of MW2, where the quartz rings are situated, see Fig. 2.2.1-16. The power divider was taken apart and the damage parts were “repaired” by polishing them with sandpaper. The inner power divider was inverted (division to antenna #1 became the one for #8, #2 for #7 and so on). Arcing in the power divider no longer occurred. Another solution was thought of in case of the further occurrence of arcs in this location. As the quartz rings enhanced the occurrence of such arcs along it surface the metallic inner and outer conductor could be further insulated using a 30 mm long quartz tube between the inner conductor and the quartz ring, moving the shortest way for an arc to occur away from the quartz ring.

Figure 2.2.1-16 Pictures of the last division of the inner power divider where arcs occurred along the quartz ring used as support.

Failure of the power supplies for the electro-magnetsTo emit the microwave, a powerful electromagnet is situated around the magnetron. The current circulating through this electromagnet Imagnet is one of the main parameters controlling the emission of the microwaves, see paragraph about the tunning of the magnetrons. At the end of February, the transformer (400V to 30 V) used in the power supply for the electro-magnet which is situated in the power generator MW2 broke down, a new transformer was sent by Aixcon and replaced. 2 weeks later, the same transformer but in power generator MW1 broke down as well. Both power supplies were then send to Aixcon for revision and upgrade. They are expected to return to Tsukuba before the end of March.

2.2.1.4 ConclusionsIt was shown that diamond could be deposited with TruDi. It appeared that the best film, in term of diamond quality, was grown with 20 kW, 1% CH4 in 2 mbar. At microwave power up to 2x10 kW, the system runs smoothly without arcing occurring anymore for deposition times up to 22 hrs.

2.2.1.5 Future plansThe use of shields to limit the plasma under the quartz tubes will be investigated. It is thought that the use of these shields will allow deposition at higher pressure. A better homogeneity of the growth rate over the whole surface will be inquired. To achieve this deposition at lower pressure will be investigated. The growth rate will be even lower, but in order to gain in deposition homogeneity, some concessions must be made.

42-

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51

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54—

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[1] D. Zhou, D. M. Gruen, L. C. Qin, T.G. McCauley, A. R. Krauss, J. Appl. Phy., Vol.84(4),

(1998)1981.

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[3] S.P. Hong, C. Morel, ^#$d, # 103

#, (2001,3)289.

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Mater.,4,4,261(1995)

[9] S.P. Hong, C. Morel, ^ 102

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-56-

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(1) S.Shikata et al., 2nd International Conference on the Applications of

Diamond Films and Related Materials. Tokyo, 377 (1993).

(2) NEW DIAMOND Vol.13 No.4, 28 (1997).

(3) ^###, 220 (2000).

(4) K.Ohtsuka et al.,Jpn.J.Appl.Phys. 35,1072(1996).

(5) T.Tsubota et al.,Diamond Relat. Mater. 9, 1380 (2000).

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substrates using antenna-edge type microwave plasma assisted chemical vapor deposition ,

12th European Conference on Diamond,Diamond-Like Materials,Carbon Nanotubes,Nitrides

& Silicon Carbide , Hungary (2001 ¥ 9 fj

• M.Tachiki et al., “Heteroepitaxial diamond thin film growth on Ir(001)/Mg0(001) substrate by

antenna-edge plasma assisted chemical vapor deposition” (submitted to Appl. Phys. Lett.).

• K.Tanabe et al., "Reactive ion etching of diamond using 02 and CHF3” , (#,#[#).

• K.Nakazawa et al., “Reactive ion etching of diamond by inductively coupled plasma” (#1

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2) R.J. Waltman et al., in: C.S. Bhatia (Ed.), Interface Tribology towards 100 Gbits/in2, ASME,

(1999).

77-

2.3.3 [SSEffi%]

Introduction

In the present project, free-standing diamond wafers and heteroepitaxial diamond films will be prepared for assessment of their structural and physical properties.

Within the period from April 2000 to March 2001 emphasis was on the assessment of high purity free-standing CVD-diamond layers and epitaxial diamond grown on 13-SiC. These materials have successfully been applied for FET processing.

In addition to our ellipsoidal microwave-Plasma-CVD systems, a novel plasma-CVD system, the CAP-reactor (CAP: circumferential antenna plasma) has been designed and built. It offers good potential for the large area deposition of CVD-diamond and epitaxial films.

CVD-Diamond for Electronic Applications

Large area diamond wafers have been prepared in our ellipsoidal microwave-Plasma- CVD system. The structural and physical properties have been measured and topographically mapped, as described in the previous report [1]. High quality polycrystalline diamond wafers of 250 pm thickness with thermal conductivities over 18 W/cmK were shown by IR-Raman spectroscopy to be of high phase purity. The wafers were diced into small chips. They were used by H. Kawarada et al. for the processing of surface channel field effect transistors (FETs) with gate lengths down to 1 pm. Transconductance values of 15 to 20 mS/mm have been obtained, which is more than an order of magnitude better than that of the best previous poly-diamond FETs [2]. Also, heteroepitaxial diamond films deposited on B-SiC in a tubular microwave-plasma CVD reactor have been assessed in cooperation with H. Kawarada et al. by processing of FETs. Transistor properties comparable to homoepitaxial diamond FETs have been demonstrated with our heteroepitaxial films [3],

The Circumferential Antenna Plasma (CAP) reactor

Our plasma CVD reactor with ellipsoidal cavity is well suited for the deposition of homogeneous large area CVD diamond films and wafers. The system is very stable and therefore very well suited for the long term deposition of thick layers. In order to get better direct access to the plasma discharge, e.g. for diagnostic in situ techniques, we have designed a novel plasma CVD-reactor, the CAP-reactor. Here, microwave is introduced into a metal chamber by radially expanding a coaxial waveguide. The central conductor is connected with the cover pfate of the reactor and the microwave is guided to an annular quartz window which forms a circumferential antenna. The two concepts are compared in Figures 1 and 2.

-78

AntennaWaveguide,

Ellipsoid

Plasma

Substrate

MicrowaveRadiation

CoaxialWaveguide

Plasma

SubstrateHolderQuartz Ring

(Window)

Cavity Z ReactorCooling Cooling \ Water water \Outlet Inlet Gas

Outlet

Fig. 1: Ellipsoidal-Reactor Fig. 2: CAP-Reactor(Circumferential Antenna Plasma-Reactor)

The electric field and plasma distribution of the CAP-reactor have been calculated on the basis of finite element simulations with an algorithm as described in [4], The geometrical dimensions to generate a central plasma ball in contact with the substrate holder have been deduced from these simulations, and a CAP reactor powered with 6 kW microwave of 2.45 GHz has been built. Fig. 3 shows the experimental system.

-79

In order to verify the calculations of the microwave field distribution, spatially resolved field measurements have been performed. For these measurements a muniature field sensor based on a Schottky diode, low pass RC filters and a high resistance cable has been constructed (Fig. 4). This sensor can be inserted in the reactor through small orifices, without disturbing the microwave-field. Herewith a calibration can be performed.

Fig. 4: Schottky diode based microwave field probe

The distribution of the electric field has been experimentally measured and compared to the theoretical results. Since the CAP reactor is radially symmetric, radial scans in the field measurements were performed. Scans in the expanded antenna and above the substrate plane were made. A perfect agreement between measured and calculated values was demonstrated, as shown in Fig. 5.The CAP reactor shows great promise for the deposition of CVD-diamond. It offers good access to the plasma region e.g. for in situ probe measurements. In addition, bias enhanced deposition is facilitated. The CAP reactor will be used within the FCT project for the deposition of diamond films and wafers. A first publication about the CAP reactor is planned at the ADC/FCT 2001 conference in August 2001 [5].

-HO-

Symmetry Axis

Radial Position (mm)

Symmetry AxisSimulation

• Measurement8000-

6000-

4000-

2000-


12000— Simulation 240° Measurement 250°260°270°280°290°300° i310° /

10000 -

8000-

6000-

4000-

2000-


Fig. 5: Simulated microwave field distribution in CAP reactor and comparison of measured and simulated electric field.

-81-

Acknowledgement

This work was supported by NEDO and JFCC as part of the Frontier Carbon Technology (FCT) project promoted by AIST, MITI, Japan. Partial support of CeramOptec GmbH is acknowledged; H. Kawarada is thanked for his cooperation in qualifying CVD-diamond by FET applications.

References

[1 ] E. Worner, E. Pleuler, M. Jehle, W. Muller-Sebert, C. Wild, P. Koidl Proc. 1st Symposium on Frontier Carbon Technology,Japan Fine Ceramics Center (2000), p. 79

[2] N.Fujihara, T.Arima, H.Umezawa, C.Wild, P.Koidl, and H.Kawarada „High performance polycrystalline diamond MISFET"to be presented at Diamond 2001, Budapest, 02 - 07 Sep 2001

[3] S. Kono, T. Goto, T. Abukawa, C. Wild, P. Koidl, H. Kawarada „Surface order evaluation of heteroepitaxial diamond films grown on inclined B-SiC(001)"Jpn. J. Appl. Phys. 39, 4372 (2000)

[4] M. Funer, C. Wild, P. Koidl Simulation and development of optimized microwave plasma reactors for diamond deposition" Surface Coatings Technol. 116-119. 853 (1999)

[5] C. Wild, E. Pleuler, P. Koidl „Numerical simulation and realisation of novel microwave plasma reactors for diamond CVD"to be presented at ADC/FCT 2001, Auburn (USA), 6-10 August 2001

-82-

1. Introduction

During the last two years the modification of diamond film growth by ion bombardment of different energy ranges at different substrate temperatures in microwave plasma chemical vapour deposition (MWCVD) has been investigated [1]. The film structures were studied by SEM and Raman spectrometry. The film stress was characterized in-situ by using the bending beam method [2,3].

By ion bombardment at a negative bias voltage above 80 V the grain size of the films begins to decrease and a nano-diamond film can be obtained at a bias voltage of 140 V. Raman spectroscopy confirmed the diamond phase. Due to ion subplantation the prepared nanocrystalline diamond films were under high intrinsic compressive stress. The prepared nanocrystalline films show improved electron emission properties [4,5].

In this report period highly boron doped nanocrystalline diamond films were prepared in a MWCVD process by ion bombardment at different substrate bias voltages. Doping with levels higher than 1000 ppm was carried out in-situ using gaseous trimethylborane/hydrogen mixture as doping source. The boron incorporation was studied using secondary ion mass spectrometry (SIMS), the film morphology by scanning electron microscopy (SEM) and the phase quality by Raman spectroscopy (RS). Much attention was paid to the influences of film structure and boron incorporation on the field emission properties.

2. Experimental

Mirror-polished n-type Si (001) wafers with a diameter of 50 mm and thickness of 300 pm were used as substrates. All nucleation experiments were performed using an Astex 1.5 kW microwave CVD reactor (see report 1999), 840 °C substrate temperature, 5 % CH4 in hydrogen and 900 W microwave power. For achieving a nucleation density higher than 1010 cm'2 a dc bias of -150 V was applied to the substrate for about 17 min. The growth step was performed at different bias voltages from 0 V to -200 V and a substrate temperature of 780 ± 50 °C.

The 1 pm thick films were grown. For achieving boron doping gaseous hydrogen/trimethylborane mixture (0.1 %) was added into the gas phase by keeping a constant boron content relative to the methane content at 0.3%. During deposition, the electrical potential was kept constant at the substrate so that the substrate surface would be continuously bombarded by energetic ions. The typical deposition parameters are given in Table 1.

TABLE 1: Experimental conditions used for the boron dopingSubstrate (001)-oriented Si-wafersProcess gas 0.5% CH/99.5%H,Doping gas 0.1 % trimethylborane in H2Pressure 25 mbarSubstrate temperature 780 °CMicrowave power 800 WSubstrate bias 0 to -200VProcess duration 6 h

-83-

3. Results and discussion

A. Film morphology and phase propertiesFigure 1 shows the SEM images of films prepared at different bias voltages. Figure

1(a) is an image of a film deposited at 0 V. It displays randomly oriented diamond crystallites with the average grain size of about 0.3 pm at a thickness of 1 pm and a relatively rough surface. This is a typical micro-crystalline film which should present columnar structure if a long term deposition process was performed. With increasing bias voltage a morphology change occurs firstly at a negative voltage of -160 V due to the onset of secondary nucleation. The average grain size, which is plotted in Fig. 2 as a function of negative bias voltage, rapidly decreases from 250 nm at -100 V to 80 nm at -160 V [Fig. 1(b)]. At -200 V a film with grain size of 20 nm was prepared.

For a comparison a SEM picture and the curve of grain size of the films prepared without doping are shown in Figs. 1d and 2, respectively. The phenomenon that a slight increase in grain size occurs at low bias voltages due to the ion-induced (001)-textured growth effect can not be repeated with boron doping. On the other hand a shift of the bias voltage for the deposition of nanodiamond films to a larger value is found for the presence of boron.

FIG. 1: SEM morphologies of the films prepared under different substrate bias voltages, (a) Vb = 0 V, boron doped; (b) Vb = -160 V, boron doped; (c) Vb = -180 V, boron doped;(d) Vb = -140 V, undoped.

To further characterize the films, micro-Raman spectroscopy was performed. The Raman spectra shown in Fig.3 were obtained with a laser spot size of approximately 20 |im in diameter on the samples. For the film deposited without biasing the substrate, a

-84-

peak at 1300 cm'1, which is the phonon fingerprint of diamond, was observed. A strong broad signal at 1200 cm 1 which is a characteristic signal for heavily doped diamond [6] and a low broad signal from 1400 to 1600 cm1 caused by sp2-bonded carbon were also detected. With increasing substrate bias, a broadening of the diamond peak at 1331 cm'1 and lower intensities for the broad peak at 1200 cm'1 can be observed. Both peaks are shifted to a higher frequency. The amorphous carbon signal at first decreases up to -120 V and then increases. It is interesting to be noticed that for the film prepared without bias a shift of the diamond phonon from 1332 to 1300 cm'1 happens, which is obviously caused by a tensile film stress. For increasing substrate bias, this diamond feature shifts back to a higher frequency, indicating a release of the tensile film stress. The feature at around 1140 cm'1 which was suggested to be characteristic for nanocrystalline diamond films could not be observed for the boron doped nanodiamond films, possibly due the boron-induced broad peak around 1200 cm'1.

FIG. 2: Grain size vs substrate bias voltage.

Raman shift (cm )

FIG. 3: Raman spectra of diamond films.

B. Electron emission propertiesThe electron emission properties of the boron doped films prepared under

different substrate bias voltages were studied. In Figure 4(a) the current densities are plotted as functions of the applied electric field. Clearly the field emissions of different films exhibit a significant decrease in emission threshold and a stronger increase in emission current if the bias voltage during film preparation is increased to -180 V. The reasons for these improvements might be attributed to the decreased grain size and therefore the increased density of grain boundaries. The irregular behavior of the film at 200 V is possibly due to the porous film structure.

-85-

-180 Bias

-160 Bias 0 Bias-200 Bias

1.5

applied electric field (V/pm)

« 2e-5

time (min.)

beforeconditioning

after j conditioning !

applied electric field (V/pm) time (min.)

FIG. 4: Emission characteristics of 1 pm thick diamond films deposited on Si substrates under different bias voltages, (a) The effect of bias on J-E (current density vs electric field) characteristics of boron-doped nano-crystalline diamond films; (b) Effect of sample conditioning and l-E plot of boron-doped nanodiamond film deposited under -180 V bias; (c) Stability test of field emission of a sample prepared at-160 V.

After conditioning the sample deposited under -180V bias voltage shows a lower threshold and a steep increase of the emission current. The stability of emission after conditioning increases. The stability test shows a current fluctuation at starting point [first several tens min., Fig. 4(b)]. Then the current density stabilized at certain value for a time up to 900 min. [Fig. 4(c)].

-86

4. Conclusions

Nanocrystalline boron-doped diamond films were prepared using MWCVD process assisted by a continuous ion bombardment. Investigations about the dependencies of grain size and phase purity on the process parameters and boron incorporation were performed. By a ion bombardment at bias voltage first above 120 V the grain size of the films begins to decrease, which is much higher than those prepared without doping, and a nano-diamond film can be obtained at a bias voltage of > 160 V. Raman spectroscopy confirmed the diamond phase. Due to boron incorporation the prepared nanocrystalline diamond films show a lowered intrinsic compressive stress which is due to an interesting compensation effect between the boron doping-induced tensile stress and the ion subplantation-induced compressive stress. The prepared nanocrystalline films show improved electron emission properties.

Acknowledgement

This work was supported by NEDO and JFCC as part of the Frontier Carbon Technology (FCT) project promoted by AI ST, MITI, Japan

References

1 X. Jiang, W.J. Zhang, and C.-P. Klages, Rhys. Rev. B 58, 7064 (1998).

2 X. Jiang, W.J. Zhang, M. Paul and C.-P. Klages, Appl. Phys. Lett. 68, 1927 (1996).

3 X. Jiang, C.Z. Gu, L. Schafer, and C.-P. Klages, Proc. of 5th International Conference on the Application of Diamond Films and Related Materials & 1st International Conference on Frontier Carbon Technology, August 31- September 3, 1999, Tsukuba, Japan.

4 C.Z. Gu and X. Jiang, J. Appl. Phys. 88, 1788 (2000).

5 X. Jiang, C.Z. Gu, L. Schager, and C.-P. Klages, FCT report of the year 1999.

6 K. Ushizawa et al., Diamond Rel. Mater. 7, 1719 (1998).

87-

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HI 3.1.2-5 Effect of hydrogen flow rate on hardness of BCN film.

HI 3.1.2-6 SEM photograph of BCN film.

(a) H2 flow rate 0 cmVmin (b) H2 flow rate 10 cm3/min[El 3.1.2-7 AFM images of BCN film deposited without hydrogen (a)

and deposited with hydrogen (b).

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3.1.2-2 Change in thickness of BCN films by annealing.

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300%: 200nm 200nm

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3.1.2.2.4

*

1) 59(2000)15.

2) A. Grill: Surf. Coat. Technol., 94-95(1997) 507.

3) C. Bonnet,: Surf. Coat. Technol., 100-101(1998)180.

4) 55(1999)38.

5) 57(2000)38.

6) S. Aisenberg and R. Chabot: J. Appl. Phys., 42*7(1971) 2953.

7) .6IC #;ilIH^:#1±(h))IIT., 413(1995)593.

-96-

8) S. Watanabe, S. Miyake J. Kim and M. Murakawa- New Diamond and Frontier

Carbon Technol., 10-4(2000) 191.

9) Y.*K. Yap, M. Yoshimura, Y Mori and T. Sasaki- New Diamond and Frontier Carbon

Technol., 10 4(2000) 201.

10) K. Yamamoto, M. Kuenecke and K. Bewilogua: New Diamond and Frontier Carbon

Technol., 10 4(2000) 225.

3.1.2.3

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* #W3tii*

1) Wu, Weng Jin. Hon, Min-Hsiung. Effect of silicon on thermal stability and wear

behavior of diamond like carbon films Materials Research Society Symposium

Proceedings, v 555 1999. p 339.

2 Camargo, S S Jr. Santos, R A. Neto, A L Baia. Carius, R. Finger, F. Structural

modifications and temperature stability of silicon incorporated diamond like a-C-H

films Thin Solid Films, v 332 n 1*2 Nov 2 1998. p 130.

3) Camargo, S S , Jr. Neto, ALB. Santos, R A. Freire, F L , Jr. Carius, R. Finger, F.

Improved high temperature stability of Si incorporated a C=H films Diamond &

Related Materials, v 7 n 8 Aug 1998. p 1155.

4) Wang, W J. Wang, T M. Chen, B L. Hydrogen release from diamondlike carbon films

due to thermal annealing in vacuum Nuclear Instruments & Methods in Physics

Research Section BBeam Interactions with Materials & Atoms, v 117 n 12 Aug 1

1996. p 140.

-98-

5) Parmeter, John E. Tallant, David R. Siegal, Michael P. Thermal stability studies of

diamond Tike carbon films Novel Forms of Carbon Materials Research Society

Symposium Proceedings, v 349 1994. Materials Research Society, Pittsburgh, PA,

USA. p 513.

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CCD camera

H] 3.1.3.1-1 Arrangement of dual-beam

speckle interferometry.

(a) Photograph of displacement measurement system.

column

(b) Side view of displacement measurement system.

HI 3.1.3.1-2 Displacement measurement system using dual-beam speckle interferometry.

6.

s = A/2 sin 0

(|X| 3.1.3.13(b), (c)#j!(1).

-106-

(a) Speckle fringe pattern of gage (b) Histogram of fringe pattern (c) Averaged histogram portion of stainless specimen along gage portion direction of fringe pattern

1E1 3.1.3.1-3 Method of extraction of speckle fringe displacement.

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gage portion of 1 st test gage portion of 2nd test

E, ,t.

(d) Determination of Young’s modulus of thin film by rule of mixture

IH3.1.3.1-4 Flow of micro tensile.

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(c) Photograph of attachment system

HH 3.1.3.1-7 Attachment with slide system.

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-111-

3.1.3.1-1 Characteristics of Attachment system

Element Error (%)Parallelism between load direction and specimen plane 0.25

Perpendicularity between specimen plane and observation direction

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El 3.1.3.1-8 Load vs. output voltage of developed El 3.1.3.1-9 Load vs. output voltage of two

load measurement system. type calibration method.

-112

3.1.3.1-2 Characteristics of developed load measurement system

Parameter Value

Calibration constant 0.701 N/VNonlinearity 0.5%ROHystereisis 0.2%RO

Load capacity 3N

3.1.3.1-3 Tensile test of stainless steel substrate

Parameter Value

Averaged Young’s modulus 211.3±0.6GPaYoung’s modulus in loading 211.1GPa

Young’s modulus in unloading 211.4GPaDispersion of Young’s modulus in each specimen 2 %

Strain speed 15 ps/sec.

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IE] 3.1.3.1-10 Measured strain-stress curve of

stainless steel specimen.

113-

3.1.3.1.5

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3.1.3.1-4 Conditions for depositing

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3.1.3.1-12 1:^7. El 3.1.3.1-12

Parameters Conditions

Evaporated gas CeHe

Substrate bias -2 kV

Gas flow rate 30 SCCM

Gas pressure 1.8 X 10 1 Pa

Substratetemperature

200T:

El 3.1.3.1-11 SEM image of cross section of DLC films on stainless steel substrate.

ID 3.1.3.1-12 Apparent measured strain- stress curve of DLC-coat stainless steel specimen.

-114-

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1 >~0~ :>X f At£f/tf H it^ http 7/pharaoh.cda.ics.saitama-u.ac.jp/ChemSensor

>'+t ;>X x — A^\—V Last update: Aug 02, 1999 Access Count:

4176 MENU

#PN#

2 MEMS-based Microvalve http://www.eng.tohoku.ac.jp/eng/souzou/groups/Lhtml

MEMS-based Microvalve | "7 7 v7 □ V :> >Sf/|ij (C <L <5 V 7 7 P A' 11/7 | Group Resources

Members Message Board 170^%^ h#g

3 http://www.ims.tsukuba.ac.jp/lab/suzuki

m/Mb##m^tfryXf-A(p-TAS)(7)#^^ffoTW^f-o T</7

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4 Laboratrv page of enviroircherrrsec http://www.onri.so.ip/Labo/environ

XXlI/^ — ‘ TEL:0727-51-9659 FAX:0727 51 9629

[email protected] English Version jtîESr B : 2000 ^ 8 H 11 0 4i

5 ^7 y http7/www.scr news.co.jp/news/200009/120915.htm

^12^9^ isa^

(Gso

6 The Micro Total Analysis Systems project at Mikroelektronik Centret

http://www.mic.dtu.dk/research/microtas/microtas.htm 2000/12/13

Micro Total Analysis Systems project About the project Publications Project members

Vacant positions (Master/PhD/PostDoc) micro TAS related links About the project

General Introd

-125-

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> X £0 B £ fl- ik t Z Ml ^ -5 CD *i' R Bt| £ Jg £> tl -5. 1 2 3

1) K.L.Mittal, J.Adhesion, Sci. and Technol. 1. (1987) 247.

2) AIM#. XS 37 (1994) 379.

3) T.Suzuki and Y.Ikuhara, in Crystal Growth and Heteroepitaxy, La Jolla Press (2001)

in press.

-136-

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Tensile strength [MPa] 43

Bending strength [MPa] 54Heating transformation

74temperature [°C]Specific gravity 1.05

L, VGCF 0.4, 2.0, 6.0, 10wt%(D4@#(D#m^:#m##^f#MLô

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Mixing volume [cm3] 50Mixing speed [rpm] 50Melt temperature [°C] 220

Mixing time [s] 300

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Diameter of screw [mm] 26Maximum injection pressure [MPa] 173.5

Maximum injection rate [cm3/s] 27Mold clumping force [ton] 30

Maximum stroke [mm] 250

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Injection pressure [MPa] 7.2, 72Injection rate [mm3/s] 6.8

Injection time [s] 2.0Cooling time [s] 15

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— : not tested

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14) S.A.Gordeyev, F.J.Macedo, J.A.Ferreira, F.W.J. van Hattum, C.A. Bernardo,

7%ysfcaB 279, 33 (2000).

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Materials Processing Technology, 92 93 , 151 (1999).

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6. A^*#

(1) “Diameter grouping in bulk samples of single-walled carbon nanotubes from optical absorption

spectroscopy" , O. lost et al. Appl. Phys. Lett. 75, 2217 (1999).

(2) “ Gas-dynamic consideration of the laser evaporation synthesis of single-wall carbon

nanotubes” , A. A. Gorbunov et al. Appl. Phys. A 69 [Suppl], S593 (2000).

(3) “Nanopatterning by biological templating and laser direct writing in thin laser deposition films”,

A. A. Gorbunov et al. Appl. Surf. Sci. 109, 621 (1997).

(4) “Features of the thin-growth conditions by cross-beam pulsed-laser deposition”, A. Tselev et al.

Appl. Phys. A 69, 353 (1999).

(5) “Thin film mixtures synthesized by cross-beam PLD , A. A. Gorbunov et al. Appl. Phys. A 69

[Suppl], S463 (2000).

(6) IFW Dresden Annual Report 1999.

(7) “Localized and delocalized electronic states in single-wall carbon nanotubes” , T. Pichler et al.

Phys. Rev. Lett. 80, 4729 (1998).

(8) “Potassium intercalated bundles of single-wall carbon nanotubes: electronic structure and

optical properties” T. Pichler et al. Solid State Commu. 109, 721 (1999).

(9) “On-ball doping of fullerenes: The electronic structure of C59N dimmers from experimental

and theory” , Phys. Rev. Lett. 78, 4749 (1997).

(10) “Mott-Hubbard-like behavior of the energy gap of A4C60 (A=Na, K, Rb, Cs) and NalOC6” ,

M. Knupfer and J. Fink, Phys. Rev. Lett. 79, 2714 (1997).

2000 ^9^118

PJr S ttk Freiberg University of Mining and Technology

Brennhausgasse 14, D 09599 Freiberg, Germany

Tel:+49 (3731)39-2666

Fax:+49 (3731)39-3129

-161

pfj 9l%'\: Prof.Dr.Robert B.Heimann(Chair of Technical Mineralogy)

Dr. Werner Klemm, associate professor of geochemistry

Dr.Jens-Uwe Goetze, research associate, technical mineralogy

Ms.Margitta Hengst, M.Sc. (chemistry)

Mr.Michael Scheel, M.Sc. (mineralogy)

i.

langasite (LGS) La3Ga5Si014, langanite (LGN) La3Ga5.5Nb0.5O14, langataite(LGT)

La3Ga5.5Ta0.5O14 LT V^„

0 , [00.1] (crystallographic c-axis and electric Z-axis)# t:E1f t:^c# L/Co

(ii) ad (i4) ii, 5ô3^<,

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(1) List of Publication of Prof.Dr.R.B.Heimann(July 12,2000)

(2) "Czochralski growth and charactrerization of piezoelectric single crystals with langasite

structure:La3Ga5Si014(LGS), La3Ga5.5Nb0.5O14(LGN) and La3Ga5.5Ta0.O14(LGT) Part

I",J.Bohm,R.B.Heimann, M.Hengst, R.RRoewer, J.Schindler J.Cryst.Growth 204(1999)128

(3) "Czochralski growth and charactrerization of piezoelectric single crystals with langasite

structure:La3Ga5Si014(LGS), La3Ga5.5Nb0.5O14(LGN) and La3Ga5.5Ta0.O14(LGT) Part

ll",J.Bohm,E.Chilla, C.Flannery, H.J.Frohlich, T.Hauke, R.B.Heimann, M.Hengst, U.Straube

J.Cryst.Growth 216(2000)293

(4) "Recent trends towards improved plasma-sprayed advanced bioceramic coatings on Ti6A14V

implants", R.B.Heimann Mat.-wiss.u. Werkstoffeetech.30 (1999)775

-162-

(5) "Compositional and microstructual changes of engineered plasma-sparayed hydroxyapatite

coatings on Ti6A14V substrates during incubation in protein-free simulated body fluid",

O.Grassmann, R.B.Heimann J.Biomed. Mater. Res., Appl. Biomaterial (in press)

OFraunhofer Institut Electronenstrahl und Plasmatechnik

0^8 0# 2000^9^12 8 4:#

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Director Plsama) (D —AC:@ALA = Prof. Dr. Brauer RA <0 , IEP#^BrO#E#,

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(##) (2000.4-2001.3)

2000.4.3 S# SFI, AS. SS.#

2000.4. 5

2000.4.12 /j# M5M IE%. SH Time-resolved emission spectroscopic studies of laser ablat ion of born nitride and carbide

Japan Laser Processing Society

2000.6.14 ~ 16

2000.4.20 # AS f (D# 2000.8.1

2000.4.20 # AS. SM2000.5. 15 mm 2000.7

2000.5.16 m. mm . a#s* mm # ms 2000.9.3

2000.5.17 J F C C (#)3 $ ZL%A—>/ 3 >%

2000.5

2000.5.17 IS AS j pee 2000.3.31

2000.5.29 m i EFCTSx>^^Â ## 2000.6.6

2000.5.30 s* ms #E,fflS Triborogical properties of diamond-like carbon films synthe sizedby plasma based ion implantation

2000. 10. 30

2000.5.31 sm mumFCTS/^Â 2000.6.6

2000.5.31 AS. SmUM ^11 Amorphous Carbon Structure for Injection Enhancement into Diamond

DIAMQND2000 ## 2000.9.3

2000.5.31 fii. (/F^ mN. Rupesinghe , G. Amaralunga) Carbon-based Vacuum Microelectronic Power Switch Device: Its

Possibilities and RequirementsDIAMOND2000 2000.9.3

2000.6.1 ^0 #%, s* mgfflS -cm### 2000.9.4

2000.6.1 A# jes. mm w. mm #s. mm ms 2000.9.3-7

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2001.2.8 E&L Eg S AW#f(7)M% WE## 2000.7

2001.2.8 M.1shihara,K,Yamamoto,F.Kokai,Y.koga

Aluminum nitride thin films prepared by radical-assited pulsed laser deposition

Vacuum59,649-656(2000) 2000.11

2001.2.8 M. Popov, M. Kyotani, Y.koga,R. J.Nemanich

Polymerized nano tubes:Bir t h of a new class of superhard materials

Phys.Rev #7: 2000.11.1

2001.2.14 mm #is

Carbon nanotubes and carbon nanofibers synthesized by sublimating decomposition of silicon carbide with catalysts

ADC/FCT 2001 2001.8. 10

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2001.2.16 7 — zff 77 7 f a — ~f 0#I#EM EM 2001.2.16

187

2001.2.16 2001.2. 1 6

2001.2.19 CURRENT STATUS OF R&D IN FRONTIER CARBON TECHNOLOGY (FCT)PROJECT • ELECTRICALLY FUNCTIONAL MATERIALS

ADC/FCT 2001.8

2001.2.19 ^ a:#,# ftuS, Ji|± imZ.

R&D OF DIAMOND FILMS IN KOBE STEEL ADC/FCT 2001.8

2001.2. 19 pmim. iiuu'i MICROFABRICATION OF VARIOUS EMITTERS ON SINGLE CRYSTAL DIAM OND

ADC/FCT 2001.8

2001.2.19 #m. m#, /j\m#

Morphological control of diamond films using a 60 kW mi crow ave plasma CVD reactor

ADC/FCT 2001.8

2001.2.22 %a >

2001.4. 1

2001.2.23 *7®)

2000.12

2001.2.28 /j# em #. sm a** #^2

Deposition of boron carbide thin films and their hardnesses Auburn University, JFCC 2001.8.6~ 10

2001.2.28 Takeshi Hasegawa,Kazuhiro Yamamoto,Yozo Kakudate

Synthesis of B-C-N thin films by electron beam excited pi as maCVD

Diamond 2001 2001.9.2

2001.3.1 %lil A# m$ff

2001.3. 1 (## : /J\# Smooth and high-rate reactive Ion Etching of Diamond Elsevier Science in association with Diamond and Related Materials

2001.9.2

2001.3. 1 (## : Large Area Deposition of<100>-Textured Diamond Films byA60 KW Microwave Plasma CVD Reactor

Elsevier Science in association with Diamond and Related Materials

2001.9.2

2001.3.5 # $ii./i# ±$

Field Emission and Electrical Characteristics of Ion-implan ledHomoepitaxial CVD Diamond

ELSEVIER SCIENSE 2001.3.5

2001.3.6 'I'K S% The first syntesis and characterization of cyameluric high polymers

Macromol chem phyo 2000.10.19

2001.3.6 K am, f#BS, Ci-fTfE/h' 7^-;A 2001.9.2

2001.3.6 Sung-Pill Hong, Hironiichi Yoshikawa, K oichiro Waztimi and Yoshinori Koga

Synthesis and Tribological Characteristics of Nanocrystal 1i neDiamond Film using CH,/H: Microwave Plasmas

Diamond 2001 2001.9.2-9. 7

188

2001.3.6 #^x em i#urn f'L /]#

Synthesis of High Quality Homoepitaxial Diamond using High Pow erMicrowave Plasma CVD system

ELSEVIER SCIENCE 2001.9.3

2001.3.12 #jn îi*

2001.5. 10

2001.3.13 iVn1 Akt. AA tnA. # Al'tufi 11}lit. ilil l r A.r. tktl- \:k. Ah!

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2001.5.23

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2001.3.31

2001.3. 13 mm#, mof#. Nano-structural Properties of Carbon Materials obtained fro m Organic Compounds

ADC/FCT 2001Conference

2001.8.6- 8.10

2001.3.15 meig &]. &#ni m^x ##

FIELD EMISSION CHARACTERISTICS OF ION IMPLANED CVD DIAMOND JFCC fill 2001.8.6

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Synthesis of Amorphous Carbon Films by Plasma-Based Ion Imp lantation using ECR Plasma with a mirror fierd

CNRS,Eurupian Commision and

Governmental Institutions

2001.6.26

2001.3. 16 mm mm. a* #9Ax mefflf

Formation of a-C thin films by plasma-based ion implantatio n

NED,JFCC.NDF 2001.8.6

2001.3. 1 6 mm ##x a* %sAx #Efflf SB

Formation of a-C thin films by plasma-based ion implantatio n

Elsevier 2001.2.15

2001.3.16 m Isotope effects of CH-i in synthesis of single-walled and mult i-walled carbon nanotube by thermal chemical vapor deposition

Nanotube 2001 2001.7.22-7.25

2001.3. 19 /j\# ^c*x em #xem mm. ^ ms

Effect of laser fluence on the deposition and hardness of b oroncarbide thin films

Springer 2001.3.19

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Carbonization of Polyacetyrene by Pyrolysis Auburn University 2001.8.6

2001.3.22 B#, A# #x mm

#11Gas-phase Synthesis of Single-wall Carbon Nanotubes from Co lloidal Solution of Metal Nanoparticles

Chemical Physics Letters 2001.2.27

189

2001.3.22 Ab-initio investigation of physisorption of moleclar hydrog en on planar and crved graphenes

Journal of ChemicalPhysics B

2000.9. 2

2001.3.23 mo ?#. mm. mm

2001.3.23 mo mm. mm

2001.3.23 Field Emission and structure of Aligned Carbon Nanofibers deposited by ECR-CVD Plasma method

SAMC 2000Organizing Comittee

2000.9.1

2001.3.23 Y.Koga Field Emission of Carbon Nanofibers Elsevier Science 2000. 9. 5

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(1) T.Nakamura,K.Ishikawa,A.Goto,M.Ishihara,T.Ohana,Y.Koga,"BN substitution reaction of

fullerene using an excimer laser irradiation",Diamond Relat.Mater.(in press)

(2) M.Ishihara,K.Yamamoto,F.Kokai,Y.Koga,"Aluminum nitride thin films prepared

byradical-assited pulsed laser deposition",Vacuum 59,649(2000)

(3) M.Ishihara,K.Yamamoto,F.Kokai,Y.Koga,"Effect of laser wavelength for surface morphology

of aluminum nitride thin films by nitrogen radical-assited" Jpn.J.Appl.Phys.(in press)

(4) SMiE&L "SAW#f(D^^",#### 20,28(2000)

(5) T.Kawai,Y.Miyamoto,O.Sugino,Y.Koga,"Graphite ribbons without hydrogen-termination:

Electronic structures and stabilities",Phys. Rev.B62,Rl6349(2000)

(6) F.Hoshi,K.Tsugawa,A.Goto,T.Ishikura,S.Yamashita,M.Yumura,T.Hirao,K.Oura, Y.Koga,"Field

emission and structure of aligned carbon nanofibers deposited by ECR-CVD plasma

method",Diamond Relat.Mater.(in press)

0 5#%#

(1) T.Nakamura,K.Ishikawa,A.Goto,T.Ohana,Y.Koga,"BN substitution reaction of Fulleren using

an exicimer laser irradiation",Diamond 2000(4 Sept.2000)

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(5) Y.Koga,"Field emission and structure of aligned carbon nanofibers deposited by ECR-CVD

plasma method",SMAC2000(Montovi)(l Sept.2000)

(6) Y.Koga,"Field emission of aligned nanofibers",Diamond 2000(5 Sept.2000)

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(1) K.Yamamoto,Y.Koga,S.Fujiwara,"Binding Energies of amorphous CN and SiCN films on

X-ray photoelectron spectroscopy ",Jpn.J.Appl.Phys.,40,LI 23(2001)

(2) T.Kimura,T.Nakamura,K.Ishikawa,F.Kokai,YKoga,"Time of flight mass spectroscopic studies

of positive ionic species generated by laser ablation of silicon carbide",Chem.

Phys.Lett.(2001)(in press)

(3 F.Kokai,M.Taniwaki,K.Takahashi,M.Ishihara,K.Yamamoto,Y.Koga,"Laser ablation of boron

carbide:thin film deposition and plume analysis"Diamond Relat.Mater.(in press)

(4) T.Ohana,A.Goto,K.Yamamoto,T.Nakamura,A.Tanaka,Y.Koga,"The structure and tribological

property of amorphous carbon and carbon nitride films prepared by ECR plasma sputtering

method"Diamond Relat.Mater.(in press)

(5) F.Kokai,K.Yamamoto,Y.Koga,"Time-of-flight mass spectrometric studies on laser ablation

dynamics of graphite: correlation to diamond-like carbon film deposition",SPIE

3885,193,(2000)

(6) #M#&E, "7/Û77;l/7X'tt>H"NewDiamond, 59, 29

(2000)

(1) Y.Yamamoto,T.Watanabe,K.Wazumi,F.Kokai,Y.Koga,S.Fujiwara,"The sp3 bond fraction in

carbon films prepared by mass-separated ion beam deposition",Diamond2000(Porto, 4

Sept.2000)

(2)

(3)

(4)

(5)

H.Yoshikawa,S.Hong,M.Cedric,Y.Koga,H.Kawarada,"Synthesis of transparent and continuous

diamond film on glass by microwave plasma CVD",Diamond2000(Porto, 4 Sept.2000)

T.Ohana,A.Goto,K.Yamamoto,T.Nakamura,A.Tanaka,Y.Koga,"The structure and tribological

property of amorphous carbon and carbon nitride films prepared by ECR plasma sputtering

method",Diamond 2000(Porto,7 Sept.2000)

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K.Yamamoto,Y.Koga,S.Fujiwara,"XPS studies of amorphous SiCN thin films prepared by

nitrogen assisted pulsed laser deposition of SiC target", 7th International Conference on New

— 199 —

Diamond Science & Technology,(Hong Kong)(25 July 2000)

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WC-Co by physical vaper deposition method, EBtkSfn, '017X' XX' XX (IX jS, Surface and

Coatings Technology , 133-134 (2000), p.455 -459

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1) The effect of humidity on the tribological behavior of diamond-like carbon film coated on

WC-Co by physical vapor deposition method, (1141 Siri, T 11/77' tk X' k >, A# iS,

International Conference on Metallurgical Coatings and Thin Films, 3kEl,2000. 4

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EE 2000.9

6) Friction and Wear of Si-Containing DLC Films under Different Humidity Conditions, EE X ##.

X TTX XX X > > Xl# iS, International Tribology Conference Nagasaki 2000, 2000.10

7) HUMIDITY DEPENDENCY OF TRIBOLOGY OF DLC FILM SYNTHESIZED ON WC-Co

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1) S. Koizumi, T. Teraji, and H. Kanda, "Phosphorus doped chemical vapor deposition of

diamond" Diamond Relat. Mater.9 (2000) 935-940.

2) E. Gheeraert , S. Koizumi, T. Teraji, H. Kanda and M. Nesladek , "Electronic states of

phosphorus in diamond"Diamond Relat. Mater.9 (2000) 948-951.

3) K. Haenen , K. Meykens, M. Nesladek, G. Knuyt, L. M. Stals,T. Teraji, S. Koizumi and E.

Gheeraert , "Electronic states of phosphorus in diamond" Diamond Relat. Mater.9 (2000)

952-955.

4) T. Teraji, S. Koizumi, and H. Kanda; "Ga Ohmic Contacts for n-type Diamond by Ion

Implantation" Appl. Phys. Lett., vol. 76, No. 10, (2000) 1303-1305.

5) E.Gheeraert, S.Koizumi, T.Teraji and H.Kanda, "Electronic transitions of electrons bound to

phosphorus donors in diamond" Solid State Com. 113(2000)577-580

6) A.T.Collins, H.Kanda and H.Kitawaki, " Colour changes produced in natural brown diamonds

by high pressure, high tempearature treatment " Diamond Relat.Mater. 9 (2000) 113-122

7) K.Thonke,R.Schliesing, N.Teofilov, H.Zacharias, R.Sauer, A.M.Zaitsev, H.Kanda and

-207-

T.R.Anthony, "Electron-Hole Drops in Synthetic Diamond" Diamond Relat. Mater. 9 (2000)

428-431

8) A.J.Neves, R. Pereira, N.A.Sobolev, M.H.Nazare, W.Gchlhoff, "New paramagnetic centers in

annealed high-pressure synthetic diamond" Diamond Relat. Mater. 9 (2000) 1057-60

9) G.Davies, H.Smith and H.Kanda, "The self-interstitial in diamond" Phys.Rcv. B 62 (2000)

1528-31

10) S.Yamaoka, M.D.Shaji Kumar, M.Akaishi and H.Kanda, "Reaction between carbon and water

under diamond-stable high pressure and high temperature conditions" Diamond Relat. Mater.

9 (2000) 1480-1486

11) M.Akaishi, M.D.S.Kumar, H.Kanda, S.Yamaoka, "Formation process of diamond from

supercritical H20-C02 fluid under high pressure and high temperature conditions" Diamond

Relat. Mater. 9(2000) 1945-1950

12) T.Kawashima, S.Sueno and H.Kanda, "Preparation of diamond and graphite from super-cooled

molten metal inNi-C system under HPHT conditions, New Diamond and Frontier Carbon Tech.

10 (2000) 283-289

13) H.Kanda and T.Sekine, High temperature high pressure synthesis of single crystal diamond, in

Properties, growth and applications of diamond ed. by M.H.Nazare and A.J.Neves, INSPEC

Pub. 2001 UK, pp.247-255

14) S.Koizumi, T.Teraji and H.Kanda," Ohmic contacts for phosphorus-doped n-type diamond"

phys.stat.sol. 181, 129 (2000)

15) O.A.Loutchev, Y.Sato, H.Kanda, "Postnucleation surface transport-kinetical phenomena and

morphological instability in film deposition from vapor" J.Appl.Phys. 89 (2001) 2151-59

16) H.Kanda, X.Jia, "Change of luminescence character of lb diamonds with HPHT treatment"

Diamond Relat. Mater, in press 1 2 3

1) S. Koizumi, T. Teraji, H. Kanda, "Growth of P-doped {100} homoepitaxial diamond films"

11th European Conference on Diamond, Diamond-Like Materials, Carbon Nanotubes, Nitrides

and Silicon Carbide,

2) K. Haenen, K. Meykens, M. Nesladek, G. Knuyt, L. M. Stals, T. Teraji, S. Koizumi,

"Phonon-assisted electronic transitions in phosphorus-doped n-type CVD diamond films" 11th

European Conference on Diamond, Diamond-Like Materials, Carbon Nanotubes, Nitrides and

Silicon Carbide,

3) E.Gheeraert, N.Casanova, S.Koizumi, T.Teraji and H. Kanda "Low temperature excitation

spectrum of phosphorus in diamond" 11th European Conference on Diamond, Diamond-Like

Materials, Carbon Nanotubes, Nitrides and Silicon Carbide,

-208-

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7) tffli-s. mmmm. m. mem # nj > k^--S#$BS-F%7t®E#J IS HEiiy-f t€> KAAdUÂ,

8) rhSE KB, ilxiSWm, ilkt-WW.#, Ft1 EH t\ fk "Diamond pn junction UV-LED"

IS 14 05'®!' tk> Kx >#'>*'!7 A,

9) S.Koizumi "Formation of diamond pn junction and its optical emission characteristics" The

3rd International Symposium on Diamond Electronic Devices,

10) M.Hasegawa, T.Teraji and S.Koizumi "Lattice location of phosphorus in n-type homoepitaxial

diamond grown by chemical vapor deposition" The 3rd International Symposium on Diamond

Electronic Devices,

11) S. Koizumi, K. Watanabe, M. Hasegawa, H. Kanda "Formation of diamond pn junction and its

optical emission characteristics" Surface and Bulk Defects in CVD Diamond Films, VI,

12) N. Casanova, E. Gheeraert, E. Bustarret, S. Koizumi, T. Teraji, H. Kanda, J. Zeman "Effect of

magnetic field on phosphorus center in diamond" Surface and Bulk Defects in CVD Diamond

Films, VI,

13) T. Yamada, A. Sawabe, S. Koizumi, J. Itoh, K. Okano, "The effect of sp2/sp3 ratio on electron

emission properties of nitrogen doped diamond electron emitter" Surface and Bulk Defects in

CVD Diamond Films, VI,

14) fflHZSBI, Jfc* m, #, JWSEBff, E u > K-AX Vt > K1343

15) Yigang Chen, M. Hasegawa, D. Takeuchi, H. Okushi, S. Koizumi, "Properties of

metal/diamond interface (I) Graphitic electrode for n-type diamond" # 48 0 Af|!550'

i6) zj># m, sasfri, witiiiMt ry-itt> h pn#48® A

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-209-

20) H.Kanda " Colored synthetic diamonds made under high pressure conditions" 14th

International Conference on Defects in Insulating Materials

21) H.Kanda and X.Jia, "Change of luminescence character of lb and Ha HPHT diamonds with

HPHT treatment" 7th International Conference on New Diamond Science and Technology

22) mwi smiiis. ffl'iiiiXife.ffrJ m 41 im A ft Mm A

23) #•*«-. Sffl3Et2

$j 35 41 WifiEr-ISSS

24) M.D.Shaji Kumar, H20-C02 6 ® #''-1'"V ^

> Kro£6£S@8J IS I4 0y-fjr;t>25) ga*S|. 4r:E> Hto/O HSICjotj-^fg

TtWttJ S 14 @j'"4'-V:E>

26) H.Kanda "Influence of HPHT treatment on luminescence of diamond" Proceedings of the 8th

NIRIM International Symposium on Advanced Materials(ISAM2001)

27) M.Akaishi, M.D.S.Kumar, H.Kanda, S.Yamaoka "Formation of diamond from C-O-H fluid

under HP-HT conditions" Proceedings of the 8th NIRIM International Symposium on

Advanced Materials(ISAM2001)

28) O.Fukunaga, T.Sugano, H.Kanda "Epitaxial growth of B-doped diamond single crystal by

limited growth space" Proceedings of the 8th NIRIM International Symposium on Advanced

Materials(ISAM2001)

29) S.Satoh, Y.Takigawa, H.Kanda, Y.Yasutomi " Observation of natural carbonados by EBSD and

CL" Proceedings of the 8th NIRIM International Symposium on Advanced

Materials(ISAM2001)

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mmmA - OSTI.GOV

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