JPH0196098A - Production of carbonaceous whisker - Google Patents
Production of carbonaceous whiskerInfo
- Publication number
- JPH0196098A JPH0196098A JP25246687A JP25246687A JPH0196098A JP H0196098 A JPH0196098 A JP H0196098A JP 25246687 A JP25246687 A JP 25246687A JP 25246687 A JP25246687 A JP 25246687A JP H0196098 A JPH0196098 A JP H0196098A
- Authority
- JP
- Japan
- Prior art keywords
- carbonaceous
- compd
- compound
- molar ratio
- whisker
- 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.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 150000003961 organosilicon compounds Chemical class 0.000 claims abstract description 9
- 239000012159 carrier gas Substances 0.000 claims abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 150000003464 sulfur compounds Chemical class 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 8
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000012779 reinforcing material Substances 0.000 abstract description 3
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 abstract description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 2
- 229930195733 hydrocarbon Natural products 0.000 abstract description 2
- 239000011541 reaction mixture Substances 0.000 abstract description 2
- 150000003568 thioethers Chemical class 0.000 abstract description 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract 1
- 239000007792 gaseous phase Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 229910000077 silane Inorganic materials 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000002994 raw material Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 150000004756 silanes Chemical class 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- -1 siloxanes Chemical class 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- LJSQFQKUNVCTIA-UHFFFAOYSA-N diethyl sulfide Chemical compound CCSCC LJSQFQKUNVCTIA-UHFFFAOYSA-N 0.000 description 2
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- AQRLNPVMDITEJU-UHFFFAOYSA-N triethylsilane Chemical compound CC[SiH](CC)CC AQRLNPVMDITEJU-UHFFFAOYSA-N 0.000 description 2
- LXUNZSDDXMPKLP-UHFFFAOYSA-N 2-Methylbenzenethiol Chemical compound CC1=CC=CC=C1S LXUNZSDDXMPKLP-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-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
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000002898 organic sulfur compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000004819 silanols Chemical class 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical class [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- VCZQFJFZMMALHB-UHFFFAOYSA-N tetraethylsilane Chemical compound CC[Si](CC)(CC)CC VCZQFJFZMMALHB-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
主呈上皇肌里分駈
本発明は、炭素質ウィスカの製造方法に関し、と（に各
種複合材料用の補強材や導電材等として有用なウィスカ
の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing carbonaceous whiskers, and more particularly, to a method for producing whiskers useful as reinforcing materials, conductive materials, etc. for various composite materials.
腫］欽υ支青
炭素質ウィスカは高強度、高弾性を有するために、樹脂
材料、炭素材料あるいはセラミックス等と組合せて種々
の複合材料を製造することが行われている。また、炭素
質ウィスカを高温処理することにより黒鉛化物とし、あ
るいはまた、その黒鉛化物に対して種々の物質を結合さ
せて層間化合物とし、導電材料として用いることも知ら
れている。Because carbonaceous whiskers have high strength and high elasticity, they are combined with resin materials, carbon materials, ceramics, etc. to produce various composite materials. It is also known to process carbonaceous whiskers at high temperatures to form a graphitized material, or to combine various substances with the graphitized material to form an intercalation compound, which is then used as a conductive material.
かかる炭素質ウィスカを製造する方法としては、遷移金
属触媒の存在下に炭化水素を気相熱分解する方法（たと
えば特開昭５７−１１７６２２）が知られている。しか
し、このような方法においては触媒の調製や生成ウィス
カの回収等が面倒で手数がかかるほか、均質なウィスカ
を得に（いという問題があった。更にまた、この方法に
よって得られた炭素質ウィスカは、繊維軸方向に平行に
同心状の炭化六角網面が発達し、しかもその先端部分が
閉じているために、黒鉛層間化合物の生成が進みにくい
という欠点を有している。As a method for producing such carbonaceous whiskers, a method of gas-phase thermal decomposition of hydrocarbons in the presence of a transition metal catalyst (for example, Japanese Patent Laid-Open No. 117622/1983) is known. However, in this method, preparation of the catalyst and collection of generated whiskers are troublesome and time-consuming, and there are problems in obtaining homogeneous whiskers.Furthermore, the carbonaceous material obtained by this method Whiskers have a drawback in that the formation of graphite intercalation compounds is difficult to proceed because a concentric hexagonal carbonized network surface is developed parallel to the fiber axis direction and the tips thereof are closed.
解決ル〕ご＋、Ｔｈｔを肌社−嘉
そこで本発明は、均質な黒鉛層間化合物を容易に製造で
きてしかも複合材料に用いるに適した性状の炭素質ウィ
スカを、収率よく製造できる方法を提供することを目的
とした。Therefore, the present invention provides a method for easily producing a homogeneous graphite intercalation compound and for producing carbonaceous whiskers with properties suitable for use in composite materials with high yield. intended to provide.
、１′占を”ンするための′又
かかる目的を達成することができる本発明の炭素質ウィ
スカの製造方法は、有機ケイ素化合物または有機ケイ素
化合物と炭化水素化合物との混合物を、イオウ化合物を
含有する還元性または不活性のキャリヤガスの存在下に
高温で気相熱分解するに当り、系中のケイ素と炭素のモ
ル比を０．１未満０．００５以上とすることを特徴とす
るものであり、とくに熱分解温度を１１００〜１５００
℃とすることによって性状の好適な炭素質ウィスカが得
られる。The method for producing carbonaceous whiskers of the present invention, which can achieve this purpose, comprises adding an organosilicon compound or a mixture of an organosilicon compound and a hydrocarbon compound to a sulfur compound. In the gas phase pyrolysis at high temperature in the presence of a reducing or inert carrier gas, the molar ratio of silicon to carbon in the system is less than 0.1 and 0.005 or more. In particular, the thermal decomposition temperature is 1100 to 1500.
By adjusting the temperature to 0.degree. C., carbonaceous whiskers with suitable properties can be obtained.
本発明において原料として用いられる有機ケイ素化合物
は、ケイ素−炭素結合を有するシラン類またはシロキサ
ン類などが用いられる。このうちシラン類としてはトリ
エチルシラン、テトラエチルシラン、ヘギサメチルジシ
ラン等のアルキル置換シラン類、テトラメトキシシラン
、テトラエトキシシラン等のアルコキシ置換シラン類、
芳香族置換シラン類などがあげられ、またシロキサン類
としてはヘキサメチルジシロキサン、ジメチルポリシロ
キサン、メチルフェニルポリシロキサン等があげられる
。この他、トリメチルシラノールなどのシラノール類、
アルコキシ置換シロキサン類等も用いることができ、こ
れらの混合物または誘導体などもガス化が可能であれば
使用可能である。As the organosilicon compound used as a raw material in the present invention, silanes or siloxanes having a silicon-carbon bond are used. Among these, silanes include alkyl-substituted silanes such as triethylsilane, tetraethylsilane, and hegisamethyldisilane; alkoxy-substituted silanes such as tetramethoxysilane and tetraethoxysilane;
Examples include aromatic substituted silanes, and examples of siloxanes include hexamethyldisiloxane, dimethylpolysiloxane, and methylphenylpolysiloxane. In addition, silanols such as trimethylsilanol,
Alkoxy-substituted siloxanes and the like can also be used, and mixtures or derivatives thereof can also be used as long as they can be gasified.
本発明において有機ケイ素化合物と混合して原料として
用いられる炭化水素化合物は、メタン、エタン、プロパ
ン等の脂肪族炭化水素類、ベンゼン、トルエン等の芳香
族炭化水素類が用いられるが、少量であれば酸素などの
他種の元素を含んでいても差支えない。In the present invention, the hydrocarbon compound mixed with an organosilicon compound and used as a raw material includes aliphatic hydrocarbons such as methane, ethane, and propane, and aromatic hydrocarbons such as benzene and toluene. It may also contain other elements such as oxygen.
本発明において用いられるイオウ化合物は触媒として挙
動するもので、たとえば硫化水素、あるいはメチルメル
カプタン、エチルメルカプタン、トルエンチオール等の
メルカプタン類、またはジエチルスルフィド、チオフェ
ン等のチオエーテル類などが用いうる。イオウ化合物が
有機イオウ化合物であるときは、原料である前記の炭化
水素化合物の一部または全部に置き換えて用いることが
できる。また、イオウ化合物がケイ素を含む有機化合物
であるときは、原料である前記の有機ケイ素化合物の少
くとも一部に置き換えて用いることができ、このような
触媒の例としてたとえばδ−メルカプトプロピル・トリ
メトキシシランなどのメルカプト変性シラン類やメルカ
プト変性ポリシロキサンなどが挙げられる。The sulfur compound used in the present invention behaves as a catalyst, and for example, hydrogen sulfide, mercaptans such as methyl mercaptan, ethyl mercaptan, and toluenethiol, or thioethers such as diethyl sulfide and thiophene can be used. When the sulfur compound is an organic sulfur compound, it can be used in place of part or all of the aforementioned hydrocarbon compound as a raw material. Furthermore, when the sulfur compound is an organic compound containing silicon, it can be used in place of at least a part of the above-mentioned organosilicon compound as a raw material. Examples of such catalysts include δ-mercaptopropyl tritri Examples include mercapto-modified silanes such as methoxysilane and mercapto-modified polysiloxanes.
本発明において用いられるキャリヤガスは、還元性また
は不活性のガスであり、水素、窒素、アルゴン等が挙げ
られるが、中でも水素が好ましく用いられる。The carrier gas used in the present invention is a reducing or inert gas, and examples thereof include hydrogen, nitrogen, and argon, among which hydrogen is preferably used.
本発明においては、原料となる有機ケイ素化合物または
これと炭化水素化合物との混合物は、触媒と共にキャリ
ヤガスによって高温反応帯域に送られるが、この際、反
応ガス中に含まれるケイ素と炭素とのモル比が０．１未
満ｏ、 ｏ ｏ ｓ以上であることが必要である。すな
わち、モル比が０．１以上であるときは炭化ケイ素質ウ
ィスカが生成し、純度のよい炭素質ウィスカは得られな
い。またモル比がＯ，ＯＯ５より小さくなるとすすの生
成が多くなり、ウィスカの収率が低い。In the present invention, an organosilicon compound or a mixture of it and a hydrocarbon compound as a raw material is sent to a high temperature reaction zone together with a catalyst by a carrier gas, but at this time, the molar ratio of silicon and carbon contained in the reaction gas It is necessary that the ratio is less than 0.1 and greater than or equal to o o s. That is, when the molar ratio is 0.1 or more, silicon carbide whiskers are produced, and carbonaceous whiskers with good purity cannot be obtained. Furthermore, when the molar ratio is smaller than O, OO5, soot is produced in large quantities and the yield of whiskers is low.
また、触媒としてのイオウ化合物の使用量に関しては特
に制限はないが、多すぎては原料の濃度を制限すること
になるから、反応混合物中の１０容量％以下、好ましく
は５容量％以下の有効量を、キャリヤガスまたは原料と
共に送り込み、反応混合物中に均一に存在させるように
することが望ましい。There is no particular restriction on the amount of the sulfur compound used as a catalyst, but if it is too large, it will limit the concentration of the raw material, so the effective It is desirable to introduce the amount along with the carrier gas or feedstock so that it is uniformly present in the reaction mixture.
本発明における熱分解反応は１１００〜１５００℃、好
ましくは１２００〜１４００℃で実施される。そのため
の装置としては、たとえば横型電気炉中にアルミナ等の
耐熱性の反応管を設けたものを用いることができるが、
必ずしもこのような装置に限定されるものではない。The thermal decomposition reaction in the present invention is carried out at 1100-1500°C, preferably 1200-1400°C. As an apparatus for this purpose, for example, a horizontal electric furnace equipped with a heat-resistant reaction tube made of alumina or the like can be used.
The present invention is not necessarily limited to such a device.
災旙開上
内径７０ｍ■、長さ１０００ｎの反応管を装着した電気
炉に対し、触媒として３容量％の硫化水素を含有する水
素を２００ｃｃ／ｍｉｎの割合で供給し、また原料とし
てテトラメチルジシロキサンとベンゼンとをＳ ｉ ／
Ｃモル比が０．０３となるように混合し、これを１．
３ ｃｃ／ｈｒの割合で反応管の蒸発部（温度１５０℃
）へ供給した。こうしてキャリヤガスと混合された気化
原料は反応管内の１３００℃の部分で熱分解され、２時
間の反応の後、長さ１菖璽以下、平均径０．６μｍの炭
素質ウィスカＩｇが得られた。During the emergency period, hydrogen containing 3% by volume hydrogen sulfide was supplied as a catalyst to an electric furnace equipped with a reaction tube with an inner diameter of 70m and a length of 1000n at a rate of 200cc/min. Siloxane and benzene are Si/
They were mixed so that the C molar ratio was 0.03, and this was mixed so that the C molar ratio was 0.03.
The evaporation section of the reaction tube (temperature 150°C
). The vaporized raw material mixed with the carrier gas was thermally decomposed at a temperature of 1300°C in the reaction tube, and after 2 hours of reaction, carbonaceous whisker Ig with a length of less than 1 iris and an average diameter of 0.6 μm was obtained. .
夫膳斑主
実施例１と同じ装置を使用し、原料としてヘキサメチル
ジシラザンとベンゼンとをＳ ｉ ／ Ｃモル比が０．
０３となるように混合したものを用いたほかは実施例１
と同様に２時間反応させたところ、長さ１龍以下、平均
径１．０μｍの炭素質ウィスカ１．２ｇが得られた。Using the same equipment as in Example 1, hexamethyldisilazane and benzene were used as raw materials at a Si/C molar ratio of 0.
Example 1 except that a mixture of 0.03 and 0.03 was used.
When the reaction was carried out in the same manner as above for 2 hours, 1.2 g of carbonaceous whiskers with a length of less than 1 mm and an average diameter of 1.0 μm were obtained.
光凱皇肱果
本発明の炭素質ウィスカの製造方法によれば、複合材料
用の補強材や導電材として好適な炭素質ウィスカが効率
よく製造できる利点がある。According to the method for producing carbonaceous whiskers of the present invention, carbonaceous whiskers suitable as reinforcing materials and conductive materials for composite materials can be efficiently produced.
Claims (2)
水素化合物との混合物を、イオウ化合物を含有する還元
性または不活性のキャリヤガスの存在下に高温で気相熱
分解するに当り、系中のケイ素と炭素のモル比を０．１
未満０．００５以上とすることを特徴とする炭素質ウィ
スカの製造方法。(1) When performing gas phase pyrolysis of an organosilicon compound or a mixture of an organosilicon compound and a hydrocarbon compound at high temperature in the presence of a reducing or inert carrier gas containing a sulfur compound, silicon in the system and carbon molar ratio is 0.1
A method for producing a carbonaceous whisker, characterized in that the whisker is less than 0.005.
請求の範囲第１項記載の炭素質ウィスカの製造方法。(2) The method for producing carbonaceous whiskers according to claim 1, wherein the thermal decomposition temperature is 1100 to 1500°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62252466A JPH06680B2 (en) | 1987-10-08 | 1987-10-08 | Carbonaceous whisker manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62252466A JPH06680B2 (en) | 1987-10-08 | 1987-10-08 | Carbonaceous whisker manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0196098A true JPH0196098A (en) | 1989-04-14 |
| JPH06680B2 JPH06680B2 (en) | 1994-01-05 |
Family
ID=17237776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62252466A Expired - Lifetime JPH06680B2 (en) | 1987-10-08 | 1987-10-08 | Carbonaceous whisker manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06680B2 (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6054999A (en) * | 1983-09-06 | 1985-03-29 | Nikkiso Co Ltd | Production of carbon fiber grown in vapor phase |
-
1987
- 1987-10-08 JP JP62252466A patent/JPH06680B2/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6054999A (en) * | 1983-09-06 | 1985-03-29 | Nikkiso Co Ltd | Production of carbon fiber grown in vapor phase |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06680B2 (en) | 1994-01-05 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |