JPS6257568B2 - - Google Patents
Info
- Publication number
- JPS6257568B2 JPS6257568B2 JP58008258A JP825883A JPS6257568B2 JP S6257568 B2 JPS6257568 B2 JP S6257568B2 JP 58008258 A JP58008258 A JP 58008258A JP 825883 A JP825883 A JP 825883A JP S6257568 B2 JPS6257568 B2 JP S6257568B2
- Authority
- JP
- Japan
- Prior art keywords
- powder
- plasma
- diamond
- polycrystalline diamond
- diaphragm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000000843 powder Substances 0.000 claims description 25
- 229910003460 diamond Inorganic materials 0.000 claims description 22
- 239000010432 diamond Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 16
- 229930195733 hydrocarbon Natural products 0.000 claims description 6
- 150000002430 hydrocarbons Chemical class 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000001556 precipitation Methods 0.000 description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- 238000009792 diffusion process Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000012495 reaction gas Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010297 mechanical methods and process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/442—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using fluidised bed process
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明は多結晶質ダイヤモンドの合成法に関す
る。更に詳しくはプラズマ空間で粉体を流動さ
せ、その粉体の表面にプラズマ化学反応によつて
多結晶質ダイヤモンドを析出させる方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for synthesizing polycrystalline diamond. More specifically, the present invention relates to a method of flowing powder in a plasma space and depositing polycrystalline diamond on the surface of the powder by a plasma chemical reaction.
本発明者はさきにプラズマ発生室内に基体を設
置し、該プラズマ発生室内を排気した後、これに
揮発性炭化水素と水素ガスの混合ガスを導入した
後、マイクロ波または高周波を入射してプラズマ
を誘発し、基体上に多結晶質ダイヤモンドを析出
させる方法を開発した。 The present inventor first installed a substrate in a plasma generation chamber, evacuated the plasma generation chamber, introduced a mixed gas of volatile hydrocarbon and hydrogen gas, and then applied microwave or high frequency waves to generate a plasma. We have developed a method to induce the precipitation of polycrystalline diamond on a substrate.
該方法によると、ダイヤモンドの析出速度が満
足すべき程度でない問題点があつた。 According to this method, there was a problem that the diamond precipitation rate was not satisfactory.
本発明はこの問題点を解決すべくなされたもの
で、ダイヤモンドの析出速度を高め、且つ微細な
結晶粒子よりなる緻密な多結晶質ダイヤモンドの
合成法を提供するにある。 The present invention was made to solve this problem, and the object is to provide a method for increasing the precipitation rate of diamond and synthesizing dense polycrystalline diamond made of fine crystal grains.
本発明者らはダイヤモンドの析出速度のおそい
原因について検討した結果、その析出の過程は加
熱した基体表面への反応物体の気体の輸送、加熱
した基体表面での化学反応による析出、化学反応
によつて副生した副成生成物の脱離、及び逆拡散
などの過程を経ている。従つて、加熱した基体と
反応ガスの境界に拡散層が形成され、この拡散層
の存在が反応ガスの基体表面への拡散速度を阻害
することに起因すること、そして析出速度を上昇
させるためには、この拡散層を破り、副生気体の
逆拡散を促進することが必要であり、そのために
は基体として粉体を用い、これをプラズマ中で流
動させると粉体間の衝突が生じ、その衝突の際に
拡散層が破られ、ダイヤモンドの析出速度が促進
されることが分つた。この究明事実に基いて本発
明を完成した。 The present inventors investigated the causes of the slow precipitation rate of diamond, and found that the precipitation process involves transport of a reactant gas to the heated substrate surface, precipitation due to a chemical reaction on the heated substrate surface, and precipitation due to a chemical reaction. This process involves desorption of by-products and back-diffusion. Therefore, a diffusion layer is formed at the boundary between the heated substrate and the reaction gas, and the existence of this diffusion layer inhibits the diffusion rate of the reaction gas to the substrate surface, and in order to increase the precipitation rate. It is necessary to break this diffusion layer and promote back-diffusion of by-product gases. To do this, powder is used as the substrate, and when it is flowed in the plasma, collisions between the powders occur, and the It was found that the diffusion layer was broken during the collision, accelerating the diamond precipitation rate. The present invention was completed based on this finding.
本発明の要旨は、揮発性炭化水素と水素との混
合ガスに高周波またはマイクロ波を入射してプラ
ズマを誘発させ、このプラズマ空間でダイヤモン
ド粉末または金属、非金属無機質粉末を振動板を
振動させることによつて分散浮遊させながら流動
させて、これら粉末の表面に多結晶質ダイヤモン
ドを被覆または粉末を核として粒状多結晶質ダイ
ヤモンドを合成することを特徴とする多結晶質ダ
イヤモンドの合成法にある。 The gist of the present invention is to induce plasma by injecting high frequency waves or microwaves into a mixed gas of volatile hydrocarbon and hydrogen, and to vibrate diamond powder or metal or nonmetal inorganic powder with a diaphragm in this plasma space. This method of synthesizing polycrystalline diamond is characterized by coating the surface of the powder with polycrystalline diamond or synthesizing granular polycrystalline diamond using the powder as a nucleus by making the powder flow while being dispersed and suspended.
本発明の方法を図面に基いて説明すると、第１
図は高周波プラズマを用い、粉末の流動を音波に
よつて振動板を振動させて行う方法、第２図はマ
イクロ波プラズマを用い、粉末の流動を機械的な
方法によつて振動板を振動させて行う方法の概要
図を示す。図中、１は低周波発振機、２は増幅
機、３は拡声器、４は振動板、５は高周波発振
機、６は同軸ケーブル、７は高周波コイル、８は
プラズマ発生室、９は粉体、１０はガス供給装
置、１１は混合ガス供給管、１２は排気装置、１
３，１４，１５，１６は調整弁、１７はマイクロ
波発振機、１８は導波管、１９は電磁石を示す。 The method of the present invention will be explained based on the drawings.
The figure shows a method using high-frequency plasma and vibrating a diaphragm using sound waves to cause the powder to flow. Figure 2 shows a method using microwave plasma and vibrating a diaphragm using a mechanical method to cause the powder to flow. A schematic diagram of the method is shown below. In the figure, 1 is a low frequency oscillator, 2 is an amplifier, 3 is a loudspeaker, 4 is a diaphragm, 5 is a high frequency oscillator, 6 is a coaxial cable, 7 is a high frequency coil, 8 is a plasma generation chamber, 9 is a powder 10 is a gas supply device, 11 is a mixed gas supply pipe, 12 is an exhaust device, 1
3, 14, 15, and 16 are regulating valves, 17 is a microwave oscillator, 18 is a waveguide, and 19 is an electromagnet.
先ず、プラズマ発生室８に粉体９を入れ、排気
装置１２を作動して装置内を減圧した後、調整弁
１３，１４，１５を調整してガス供給装置１０よ
り水素ガス、揮発性炭化水素との混合ガスを混合
ガス供給管１１を通じてプラズマ発生室８内に供
給して所定の圧力に保持する。次に低周波発振機
１、増幅機２を作動し、拡声器３または電磁石１
９により振動板４を振動させ、低周波発振機１の
周波数、増幅機２の出力を調整して粉体９を適切
な状態で流動させる。 First, the powder 9 is put into the plasma generation chamber 8, the exhaust device 12 is operated to reduce the pressure inside the device, and the regulating valves 13, 14, 15 are adjusted to supply hydrogen gas and volatile hydrocarbons from the gas supply device 10. A mixed gas of the above is supplied into the plasma generation chamber 8 through the mixed gas supply pipe 11 and maintained at a predetermined pressure. Next, activate the low frequency oscillator 1 and amplifier 2, and activate the loudspeaker 3 or electromagnet 1.
9 vibrates the diaphragm 4 and adjusts the frequency of the low frequency oscillator 1 and the output of the amplifier 2 to flow the powder 9 in an appropriate state.
第１図においては高周波発振機５を作動してそ
の出力を高周波コイル７に与え、流動層中にプラ
ズマを誘発する。第２図においてはマイクロ波発
振機１７を作動して、その出力を導波管１８を通
じてプラズマ発生室８内に入射し、流動層中にプ
ラズマを誘発する。 In FIG. 1, a high frequency oscillator 5 is activated and its output is applied to a high frequency coil 7 to induce plasma in the fluidized bed. In FIG. 2, the microwave oscillator 17 is activated and its output is input into the plasma generation chamber 8 through the waveguide 18 to induce plasma in the fluidized bed.
本発明に用いる揮発性炭化水素としては、例え
ば、メタン，エタン，アセチレン，ブタン等が挙
げられる。メタンは安価で入手し易い点で好まし
い。揮発性炭化水素と水素との割合は、20：
100，望ましくは５：100以下あること、また粉体
としては、ダイヤモンド，α−Al2O3，タンタ
ル，モリブデン等が基げられる。その粒度は300
μｍ以下であることが好ましい。 Examples of volatile hydrocarbons used in the present invention include methane, ethane, acetylene, and butane. Methane is preferred because it is cheap and easily available. The ratio of volatile hydrocarbons to hydrogen is 20:
100, preferably 5:100 or less, and the powder is based on diamond, α-Al 2 O 3 , tantalum, molybdenum, etc. Its particle size is 300
It is preferable that it is less than μm.
実施例 １
第１図の装置において、粉体としてダイヤモン
ド粉末（30μｍ）、反応ガスとして、メタンと水
素との混合ガスを使用した。排気装置１２を作動
してプラズマ発生室８内を充分排気した後、ガス
供給装置１０より調整弁１３，１４，１５，１６
を調整してメタンガス濃度３％の水素との混合ガ
スをプラズマ発生室８内に導入し、該プラズマ発
生室８内の圧力を0.06気圧になるように混合ガス
の流速50cm／minで供給した。次に低周波発振機
１，増幅機２を調整して拡声器３に80ヘルツ、
5Wの出力を与えて振動板４を振動させてダイヤ
モンド粉末９を流動させた。ついで、高周波発振
機５（13.56MHz）、800Wの出力を同軸ケーブル
６を通じて高周波コイル７に与え、流動層中にプ
ラズマを誘発させた。３時間析出を行つたとこ
ろ、粒径42μｍの粒状多結晶体ダイヤモンドが得
られた。Example 1 In the apparatus shown in FIG. 1, diamond powder (30 μm) was used as the powder, and a mixed gas of methane and hydrogen was used as the reaction gas. After operating the exhaust device 12 to sufficiently exhaust the inside of the plasma generation chamber 8, the gas supply device 10 operates the regulating valves 13, 14, 15, 16.
A mixed gas of methane and hydrogen having a concentration of 3% was introduced into the plasma generation chamber 8, and the mixed gas was supplied at a flow rate of 50 cm/min so that the pressure inside the plasma generation chamber 8 became 0.06 atmospheres. Next, adjust the low frequency oscillator 1 and amplifier 2 to output 80 Hz to the loudspeaker 3.
The diaphragm 4 was vibrated by applying an output of 5 W to cause the diamond powder 9 to flow. Next, an output of 800 W from the high frequency oscillator 5 (13.56 MHz) was applied to the high frequency coil 7 through the coaxial cable 6 to induce plasma in the fluidized bed. After 3 hours of precipitation, granular polycrystalline diamond with a grain size of 42 μm was obtained.
実施例 ２
実施例１と同様な条件でマイクロ波（2450M
Hz）、600Wの出力をプラズマ発生室８内に入射
し、流動層中にプラズマを誘発した。振動板４の
振動は低周波発振機１、及び増幅機２を作動し、
電磁石１９を作用させて行つた。３時間析出を行
つたところ、粒径50μｍの粒状多結晶体ダイヤモ
ンドが得られた。Example 2 Microwave (2450M
Hz) and a power of 600 W was input into the plasma generation chamber 8 to induce plasma in the fluidized bed. The vibration of the diaphragm 4 operates a low frequency oscillator 1 and an amplifier 2,
This was done by activating the electromagnet 19. After 3 hours of precipitation, granular polycrystalline diamond with a grain size of 50 μm was obtained.
実施例 ３
実施例１と同様な条件で粉体としてアルミナ
（20μｍ），タンタル（20μｍ）を使用した場合、
３時間析出を行つたところ各々、粒径30μｍ，35
μｍの多結晶体ダイヤモンドが得られた。Example 3 When alumina (20 μm) and tantalum (20 μm) were used as powder under the same conditions as Example 1,
After 3 hours of precipitation, the particle size was 30 μm and 35
A polycrystalline diamond of μm size was obtained.
本発明の方法によると、静止した板状の基体表
面に析出させる場合に比較してその成長速度を数
倍に上昇できる。また添加物を加えることなしに
粒状の多結晶体ダイヤモンドを合成することがで
きるなどの利点がある。 According to the method of the present invention, the growth rate can be increased several times compared to when depositing on the surface of a stationary plate-like substrate. Another advantage is that granular polycrystalline diamond can be synthesized without adding additives.
図面は本発明方法の実施態様を示すもので、第
１図は高周波プラズマを用い、粉末の流動を音波
によつて振動板を振動させて行う方法、第２図は
マイクロ波プラズマを用い、粉末の流動を機械的
な方法によつて振動板を振動させる方法の概要図
である。
１：増幅機、２：低周波発振機、３：拡声器、
４：振動板、５：高周波発振機、６：同軸ケーブ
ル、７：高周波コイル、８：プラズマ発生室、
９：粉体、１０：ガス供給装置、１１：混合ガス
供給管、１２：排気装置、１３，１４，１５，１
６：調整弁、１７：マイクロ波発振機、１８：導
波管、１９：電磁石。
The drawings show embodiments of the method of the present invention. Fig. 1 shows a method in which high-frequency plasma is used to flow powder by vibrating a diaphragm using sound waves, and Fig. 2 shows a method in which powder is flowed using microwave plasma by vibrating a diaphragm. FIG. 2 is a schematic diagram of a method of vibrating a diaphragm using a mechanical method to generate a flow of water. 1: Amplifier, 2: Low frequency oscillator, 3: Loudspeaker,
4: Vibration plate, 5: High frequency oscillator, 6: Coaxial cable, 7: High frequency coil, 8: Plasma generation chamber,
9: Powder, 10: Gas supply device, 11: Mixed gas supply pipe, 12: Exhaust device, 13, 14, 15, 1
6: Regulating valve, 17: Microwave oscillator, 18: Waveguide, 19: Electromagnet.
Claims (1)
またはマイクロ波を入射してプラズマを誘導さ
せ、このプラズマ空間で、ダイヤモンド粉末また
は金属、非金属無機質粉末を、振動板を振動させ
ることによつて分散浮遊させながら流動させて、
これら粉末の表面に多結晶質ダイヤモンドを合成
することを特徴とする多結晶質ダイヤモンドの合
成法。1. Plasma is induced by injecting high frequency waves or microwaves into a mixed gas of volatile hydrocarbon and hydrogen, and in this plasma space, diamond powder or metal or non-metallic inorganic powder is vibrated by a diaphragm. Flow while dispersing and floating.
A method for synthesizing polycrystalline diamond characterized by synthesizing polycrystalline diamond on the surface of these powders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58008258A JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58008258A JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59137311A JPS59137311A (en) | 1984-08-07 |
| JPS6257568B2 true JPS6257568B2 (en) | 1987-12-01 |
Family
ID=11688118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58008258A Granted JPS59137311A (en) | 1983-01-21 | 1983-01-21 | Method for synthesizing polycrystalline diamond |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59137311A (en) |
Families Citing this family (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0717479B2 (en) * | 1985-12-09 | 1995-03-01 | 京セラ株式会社 | Diamond film manufacturing method |
| DE3546113A1 (en) * | 1985-12-24 | 1987-06-25 | Santrade Ltd | COMPOSITE POWDER PARTICLES, COMPOSITE BODIES AND METHOD FOR THE PRODUCTION THEREOF |
| JPS63107898A (en) * | 1986-10-23 | 1988-05-12 | Natl Inst For Res In Inorg Mater | Method for synthesizing diamond with plasma |
| JPS63156009A (en) * | 1986-12-19 | 1988-06-29 | Natl Inst For Res In Inorg Mater | Synthesis of fine diamond powder |
| US5080975A (en) * | 1987-03-23 | 1992-01-14 | Showa Denko K. K. | Composite diamond granules |
| US4859493A (en) * | 1987-03-31 | 1989-08-22 | Lemelson Jerome H | Methods of forming synthetic diamond coatings on particles using microwaves |
| JPS63270394A (en) * | 1987-04-28 | 1988-11-08 | Showa Denko Kk | Flow type method for synthesizing diamond and apparatus therefor |
| JP2550103B2 (en) * | 1987-10-20 | 1996-11-06 | 洋一 広瀬 | Diamond composite grain |
| JPH0288497A (en) * | 1988-06-09 | 1990-03-28 | Toshiba Corp | Production of single crystal diamond grain |
| JP2639505B2 (en) * | 1988-10-20 | 1997-08-13 | 住友電気工業株式会社 | Synthesis method of granular diamond |
| US5028452A (en) * | 1989-09-15 | 1991-07-02 | Creative Systems Engineering, Inc. | Closed loop system and process for conversion of gaseous or vaporizable organic and/or organo-metallic compounds to inert solid matrix resistant to solvent extraction |
| EP0459425A1 (en) * | 1990-05-30 | 1991-12-04 | Idemitsu Petrochemical Company Limited | Process for the preparation of diamond |
| US5783335A (en) * | 1992-04-07 | 1998-07-21 | The Regents Of The University Of California, Office Of Technology Transfer | Fluidized bed deposition of diamond |
| US6015597A (en) * | 1997-11-26 | 2000-01-18 | 3M Innovative Properties Company | Method for coating diamond-like networks onto particles |
| US6265068B1 (en) | 1997-11-26 | 2001-07-24 | 3M Innovative Properties Company | Diamond-like carbon coatings on inorganic phosphors |
-
1983
- 1983-01-21 JP JP58008258A patent/JPS59137311A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59137311A (en) | 1984-08-07 |
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