JPH0569061B2 - - Google Patents
Info
- Publication number
- JPH0569061B2 JPH0569061B2 JP62081250A JP8125087A JPH0569061B2 JP H0569061 B2 JPH0569061 B2 JP H0569061B2 JP 62081250 A JP62081250 A JP 62081250A JP 8125087 A JP8125087 A JP 8125087A JP H0569061 B2 JPH0569061 B2 JP H0569061B2
- Authority
- JP
- Japan
- Prior art keywords
- pitch
- carbon
- fibers
- fiber
- composite material
- 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 - Lifetime
Links
- 239000000835 fiber Substances 0.000 claims description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 229910052799 carbon Inorganic materials 0.000 claims description 34
- 239000002131 composite material Substances 0.000 claims description 23
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 11
- 239000004917 carbon fiber Substances 0.000 claims description 11
- 238000003763 carbonization Methods 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000010030 laminating Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009987 spinning Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims 2
- 238000005096 rolling process Methods 0.000 claims 1
- 239000011295 pitch Substances 0.000 description 29
- 239000011159 matrix material Substances 0.000 description 7
- 239000011301 petroleum pitch Substances 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000002759 woven fabric Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000002074 melt spinning Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000011337 anisotropic pitch Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000009656 pre-carbonization Methods 0.000 description 2
- 239000003570 air Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011300 coal pitch Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、炭素／炭素複合材料の製造法に関す
る。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing carbon/carbon composite materials.
従来の技術および発明が解決しようとする問題点
炭素／炭素複合材料は、1000℃以上の高温にお
いても高強度、高弾性率を維持し、かつ熱膨張率
が小さい等の特異な性質を有する材料であり、航
空宇宙機器の部品、ブレーキ、炉材等への利用が
期待されている。炭素質ピツチは炭素／炭素複合
材料のマトリツクス用プリカーサとして用いられ
ているが、軟化点が低いものを用いれば、炭化収
率が低下し、また炭化時に発生する揮発性成分の
ためマトリツクス中に微細な気泡を生成する。一
方、軟化点が高いものを用いれば、炭素繊維束内
への均一な含浸が行いにくくなる。これらを避け
るため種々の工夫がなされているが、製造プロセ
スは複雑であり、かつ長い日数を要するためコス
トがかかつている。Conventional technology and problems to be solved by the invention Carbon/carbon composite materials are materials that have unique properties such as maintaining high strength and high modulus of elasticity even at high temperatures of 1000°C or higher, and having a small coefficient of thermal expansion. It is expected to be used in aerospace equipment parts, brakes, furnace materials, etc. Carbonaceous pitch is used as a matrix precursor for carbon/carbon composite materials, but if one with a low softening point is used, the carbonization yield will decrease, and volatile components generated during carbonization will cause fine particles to form in the matrix. Generates bubbles. On the other hand, if a material with a high softening point is used, uniform impregnation into the carbon fiber bundle becomes difficult. Various efforts have been made to avoid these problems, but the manufacturing process is complicated and takes a long time, resulting in high costs.
問題点を解決するための手段
本発明者らは、前記問題点を解決し、簡便な製
造プロセスを研究した結果、本発明の完成に至つ
た。Means for Solving the Problems The present inventors solved the above problems and researched a simple manufacturing process, and as a result, they completed the present invention.
本発明は炭素質ピツチを紡糸して得られるピツ
チ繊維、ピツチ繊維を不融化処理して得られる不
融化繊維および不融化繊維を不活性ガス雰囲気下
に400〜800℃で前炭化処理して得られる前炭化繊
維からなる群より選ばれる１種または２種以上の
繊維のトウとピツチ系炭素繊維のトウとを混織あ
るいは積層した後、これを加圧下あるいはプレス
下で炭化することを特徴とする炭素／炭素複合材
料の製造法に関する。 The present invention provides pitch fibers obtained by spinning carbonaceous pitch fibers, infusible fibers obtained by infusible treatment of pitch fibers, and pre-carbonization treatment of infusible fibers at 400 to 800°C in an inert gas atmosphere. The method is characterized in that after a tow of one or more types of fibers selected from the group consisting of pre-carbonized fibers and a tow of pitch-based carbon fibers are mixedly woven or laminated, this is carbonized under pressure or a press. The present invention relates to a method for producing a carbon/carbon composite material.
以下、本発明による炭素／炭素複合材料の製造
法について詳述する。 Hereinafter, the method for producing a carbon/carbon composite material according to the present invention will be described in detail.
本発明でいうピツチ繊維とは、炭素質ピツチを
公知の方法で溶融紡糸することにより得られる平
均直径５〜100μｍ、好ましくは７〜30μｍの繊維
である。ピツチ系炭素繊維の原料となる炭素質ピ
ツチとしては、軟化点100〜400℃、好ましくは
150〜300℃を有する石炭系あるいは石油系のピツ
チが用いられる。炭素質ピツチは、光学的に等方
性のピツチあるいは異方性のピツチのいずれも使
用できるが、光学的異方性相の含量が60〜100％
の光学的異方性ピツチが特に好ましく用いられ
る。 The pitch fiber as used in the present invention is a fiber having an average diameter of 5 to 100 μm, preferably 7 to 30 μm, obtained by melt spinning carbonaceous pitch by a known method. Carbonaceous pitch, which is a raw material for pitch-based carbon fiber, has a softening point of 100 to 400°C, preferably
A coal-based or petroleum-based pitch having a temperature of 150 to 300°C is used. The carbonaceous pitch can be either an optically isotropic pitch or an anisotropic pitch, but the content of the optically anisotropic phase is 60 to 100%.
An optically anisotropic pitch of 1 is particularly preferably used.
本発明でいう不融化繊維とは、前記ピツチ繊維
を不融化処理して得られる不融化繊維である。不
融化処理は、酸化性ガス雰囲気下、50〜400℃、
好ましくは100〜350℃で行うことができる。酸化
性ガスとしては、空気、酸素、窒素化合物、硫黄
化合物、ハロゲン、あるいはこれらの混合物が使
用できる。処理時間は10分〜20時間である。 The infusible fiber as used in the present invention is an infusible fiber obtained by subjecting the pitch fiber to an infusible treatment. Infusibility treatment is performed at 50 to 400℃ in an oxidizing gas atmosphere.
Preferably, it can be carried out at 100 to 350°C. As the oxidizing gas, air, oxygen, nitrogen compounds, sulfur compounds, halogens, or mixtures thereof can be used. Processing time is 10 minutes to 20 hours.
本発明でいう前炭化繊維とは、前記不融化繊維
をさらに前炭化処理して得られる繊維をいう。前
炭化処理は、不活性ガス雰囲気下、400〜800℃で
10分〜５時間実施する。 The pre-carbonized fiber in the present invention refers to a fiber obtained by further pre-carbonizing the infusible fiber. Pre-carbonization treatment is performed at 400-800℃ under an inert gas atmosphere.
Perform for 10 minutes to 5 hours.
本発明でいうピツチ系炭素繊維とは、炭素質ピ
ツチを溶融紡糸し、これを不融化、炭化および必
要に応じて黒鉛化することにより得られる繊維で
ある。ここでいう炭素質ピツチ、溶融紡糸、不融
化については、すでに述べたとおりであり、また
炭化処理および黒鉛化処理は、不活性ガス雰囲気
下でそれぞれ800〜2000℃および2000〜3000℃で
行うことができる。 The pitch-based carbon fiber as used in the present invention is a fiber obtained by melt-spinning carbonaceous pitch, making it infusible, carbonizing it, and graphitizing it if necessary. The carbonaceous pitch, melt spinning, and infusibility mentioned here are as described above, and the carbonization treatment and graphitization treatment are performed at 800 to 2000℃ and 2000 to 3000℃, respectively, in an inert gas atmosphere. I can do it.
ピツチ繊維、不融化繊維および前炭化繊維から
なる群から選ばれる１種または２種以上の繊維と
ピツチ系炭素繊維とを混織あるいは積層した後、
これを加圧下あるいはプレス下で炭化し、さらに
必要に応じて常圧下で炭化あるいは黒鉛化する。
混織あるいは積層の際に、各繊維を500〜10000本
のトウとする。 After blending or laminating one or more types of fibers selected from the group consisting of pitch fibers, infusible fibers, and pre-carbonized fibers and pitch carbon fibers,
This is carbonized under pressure or a press, and further carbonized or graphitized under normal pressure if necessary.
When blended or laminated, each fiber is made into 500 to 10,000 tows.
加圧下の炭化は、不活性ガスにより50〜10000
Kg／cm2に加圧し、400〜2000℃において実施する。
また、プレス下の炭化は、ホツトプレスにより10
〜500Kg／cm2圧力下、400〜2000℃において実施す
る。加圧下あるいはプレス下での炭化後、必要に
応じて行う常圧下の炭化あるいは黒鉛化は、不活
性ガス雰囲気下400〜3000℃において実施する。 Carbonization under pressure is 50~10000 by inert gas
Pressure is applied to Kg/cm 2 and the temperature is 400 to 2000°C.
In addition, carbonization under the press can be achieved by hot pressing.
Performed at 400-2000°C under ~500Kg/ cm2 pressure. After carbonization under pressure or a press, carbonization or graphitization under normal pressure, if necessary, is carried out at 400 to 3000° C. in an inert gas atmosphere.
複合材料におけるピツチ系炭素繊維の体積含有
率（Vf）は、目的によつて任意に決定されるが、
通常は５〜70％である。 The volume content (Vf) of pitch-based carbon fiber in a composite material is arbitrarily determined depending on the purpose, but
Usually it is 5-70%.
実施例
以下に実施例をあげ、本発明を具体的に説明す
る。EXAMPLES The present invention will be specifically explained with reference to Examples below.
実施例 １
軟化点280℃を有する光学的異方性の石油系ピ
ツチを溶融紡糸し、平均直径13μｍのピツチ繊維
を得た。このピツチ繊維2000本のトウと平均直径
10μｍのピツチ系炭素繊維2000本のトウとを平織
りし、織物とした。この織物を100層重ねたもの
を、ホツトプレスにより100Kg／cm2圧力下、600℃
においてプレス炭化した。さらにこの炭化物を窒
素雰囲気下1000℃で30分焼成し炭素／炭素複合材
料を製造した。得られた炭素／炭素複合材料は、
繊維の体積含有率は50％、複合材料の空隙率は10
％であつた。偏光顕微鏡あるいは電子顕微鏡を用
いた観察により、マトリツクスがきわめて均一に
分布していることも明らかとなつた。Example 1 Optically anisotropic petroleum pitch having a softening point of 280° C. was melt-spun to obtain pitch fibers with an average diameter of 13 μm. This pitch fiber has 2000 tows and average diameter
2000 tows of 10 μm pitch carbon fibers were plain woven into a woven fabric. 100 layers of this fabric are hot pressed at 600℃ under 100Kg/ cm2 pressure.
Press carbonized at Furthermore, this carbide was fired at 1000°C for 30 minutes in a nitrogen atmosphere to produce a carbon/carbon composite material. The obtained carbon/carbon composite material is
The volume content of fiber is 50%, the porosity of the composite is 10
It was %. Observation using a polarizing microscope or an electron microscope revealed that the matrix was extremely uniformly distributed.
比較例 １
軟化点280℃を有する光学的異方性の石油系ピ
ツチを粉砕し、平均直径10μｍのピツチ系炭素繊
維2000本のトウの平織物と交互に100層積層した。
この積層物を、ホツトプレスにより100Kg／cm2圧
力下、600℃においてプレス炭化した。この炭化
物を窒素雰囲気下1000℃で30分焼成し炭素／炭素
複合材料を製造した。得られた炭素／炭素複合材
料は、繊維の体積含有率は50％、複合材料の空隙
率は30％であつた。偏光顕微鏡あるいは電子顕微
鏡を用いて観察すると、マトリツクス中にピツチ
が均一に分布していないことが確認された。Comparative Example 1 An optically anisotropic petroleum-based pitch having a softening point of 280° C. was pulverized, and 100 layers were alternately laminated with a plain woven fabric of 2000 tow pitch-based carbon fibers having an average diameter of 10 μm.
This laminate was press carbonized at 600° C. under a pressure of 100 kg/cm 2 using a hot press. This carbide was fired at 1000°C for 30 minutes in a nitrogen atmosphere to produce a carbon/carbon composite material. The obtained carbon/carbon composite material had a fiber volume content of 50% and a porosity of the composite material of 30%. When observed using a polarizing microscope or an electron microscope, it was confirmed that the pitches were not uniformly distributed in the matrix.
実施例 ２
実施例１で得られた織物を100層重ねたものを、
不活性ガスにより200Kg／cm2に加圧し、550℃にお
いて１時間加圧炭化し、ついで常圧下、1300℃に
おいての炭化30分焼成し炭素／炭素複合材料を製
造した。得られた炭素／炭素複合材料は、繊維の
体積含有率は50％、複合材料の空隙率は10％であ
つた。偏光顕微鏡あるいは電子顕微鏡を用いた観
察により、マトリツクスがきわめて均一に分布し
ていることも明らかとなつた。Example 2 A layer of 100 layers of the fabric obtained in Example 1 was
The mixture was pressurized to 200 kg/cm 2 with an inert gas, carbonized under pressure at 550°C for 1 hour, and then carbonized and fired at 1300°C for 30 minutes under normal pressure to produce a carbon/carbon composite material. The obtained carbon/carbon composite material had a fiber volume content of 50% and a porosity of the composite material of 10%. Observation using a polarizing microscope or an electron microscope revealed that the matrix was extremely uniformly distributed.
実施例 ３
軟化点280℃を有する光学的異方性の石油系ピ
ツチを溶融紡糸し、平均直径13μｍのピツチ繊維
を得た。このピツチ繊維2000本のトウを空気中
300℃で１時間不融化処理し不融化繊維トウを得
た。この不融化繊維トウと平均直径10μｍのピツ
チ系炭素繊維2000本のトウとを平織りし、織物と
した。この織物を100層重ねたものを、ホツトプ
レスにより100Kg／cm2圧力下、600℃においてプレ
ス炭化した。この炭化物を窒素雰囲気下1200℃で
30分焼成し炭素／炭素複合材料を製造した。得ら
れた炭素／炭素複合材料は、繊維の体積含有率は
50％、複合材料の空隙率は５％未満であつた。偏
光顕微鏡あるいは電子顕微鏡を用いた観察によ
り、マトリツクスがきわめて均一に分布している
ことも明らかとなつた。Example 3 Optically anisotropic petroleum pitch having a softening point of 280° C. was melt-spun to obtain pitch fibers with an average diameter of 13 μm. 2000 tows of this pitch fiber are suspended in the air.
An infusible fiber tow was obtained by infusibility treatment at 300° C. for 1 hour. This infusible fiber tow and 2000 pitch carbon fiber tows having an average diameter of 10 μm were plain woven to form a woven fabric. A stack of 100 layers of this fabric was press carbonized at 600° C. under a pressure of 100 kg/cm 2 using a hot press. This carbide was heated at 1200℃ under nitrogen atmosphere.
A carbon/carbon composite material was produced by firing for 30 minutes. The obtained carbon/carbon composite material has a fiber volume content of
50%, and the porosity of the composite was less than 5%. Observation using a polarizing microscope or an electron microscope revealed that the matrix was extremely uniformly distributed.
実施例 ４
軟化点280℃を有する光学的異方性の石油系ピ
ツチを溶融紡糸し、平均直径13μｍのピツチ繊維
を得た。このピツチ繊維2000本のトウを空気中
300℃で１時間不融化処理した後、窒素中、600℃
で１時間処理して前炭化繊維トウを得た。この前
炭化繊維トウと平均直径10μｍのピツチ系炭素繊
維2000本のトウとを平織りし、織物とした。この
織物を100層重ねたものを、ホツトプレスにより
100Kg／cm2圧力下、600℃においてプレス炭化し
た。この炭化物を窒素雰囲気下1200℃で30分焼成
し炭素／炭素複合材料を製造した。得られた炭
素／炭素複合材料は、繊維の体積含有率は55％、
複合材料の空隙率は５％未満であつた。偏光顕微
鏡あるいは電子顕微鏡を用いた観察により、マト
リツクスがきわめて均一に分布していることも明
らかとなつた。Example 4 Optically anisotropic petroleum pitch having a softening point of 280° C. was melt-spun to obtain pitch fibers with an average diameter of 13 μm. 2000 tows of this pitch fiber are suspended in the air.
After infusibility treatment at 300℃ for 1 hour, 600℃ in nitrogen
A pre-carbonized fiber tow was obtained. This pre-carbonized fiber tow and 2000 pitch carbon fiber tows having an average diameter of 10 μm were plain woven to form a woven fabric. 100 layers of this fabric are made by hot pressing.
Press carbonization was performed at 600° C. under a pressure of 100 Kg/cm 2 . This carbide was fired at 1200°C for 30 minutes in a nitrogen atmosphere to produce a carbon/carbon composite material. The obtained carbon/carbon composite material has a fiber volume content of 55%,
The porosity of the composite material was less than 5%. Observation using a polarizing microscope or an electron microscope revealed that the matrix was extremely uniformly distributed.
Claims (1)
維、ピツチ繊維を不融化処理して得られる不融化
繊維および不融化繊維を不活性ガス雰囲気下に
400〜800℃で前炭化処理して得られる前炭化繊維
からなる群より選ばれる１種または２種以上の繊
維のトウとピツチ系炭素繊維のトウとを混織ある
いは積層した後、これを加圧下あるいはプレス下
で炭化することを特徴とする炭素／炭素複合材料
の製造法。 ２ 加圧下あるいはプレス下で炭化後、さらに炭
化あるいは黒鉛化することを特徴とする特許請求
の範囲第１項記載の炭素／炭素複合材料の製造
法。[Claims] 1. Pitch fibers obtained by spinning carbonaceous pitch fibers, infusible fibers obtained by infusible treatment of pitch fibers, and infusible fibers in an inert gas atmosphere.
After mixing or laminating a tow of one or more types of fibers selected from the group consisting of pre-carbonized fibers obtained by pre-carbonizing at 400 to 800°C and a tow of pitch carbon fiber, this is processed. A method for producing a carbon/carbon composite material characterized by carbonization under rolling or pressing. 2. The method for producing a carbon/carbon composite material according to claim 1, which comprises carbonizing under pressure or pressing and then further carbonizing or graphitizing.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62081250A JPS63248770A (en) | 1987-04-03 | 1987-04-03 | Manufacture of carbon/carbon composite material |
| EP88302963A EP0297695B1 (en) | 1987-04-03 | 1988-03-31 | Process for fabricating carbon/carbon fibre composite |
| DE88302963T DE3882452T2 (en) | 1987-04-03 | 1988-03-31 | Process for the manufacture of articles from carbon / carbon fibers. |
| US07/176,713 US4849200A (en) | 1987-04-03 | 1988-04-01 | Process for fabricating carbon/carbon composite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62081250A JPS63248770A (en) | 1987-04-03 | 1987-04-03 | Manufacture of carbon/carbon composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63248770A JPS63248770A (en) | 1988-10-17 |
| JPH0569061B2 true JPH0569061B2 (en) | 1993-09-30 |
Family
ID=13741143
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62081250A Granted JPS63248770A (en) | 1987-04-03 | 1987-04-03 | Manufacture of carbon/carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63248770A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH089822B2 (en) * | 1988-02-26 | 1996-01-31 | 株式会社ペトカ | Method for producing carbon fiber non-woven fabric |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5252912A (en) * | 1975-10-25 | 1977-04-28 | Nippon Carbon Co Ltd | Manufacture of carbon materials |
| JPS57209883A (en) * | 1981-06-16 | 1982-12-23 | Tokai Carbon Kk | Manufacture of carbon fiber reinforced carbon material |
| JPS5935841A (en) * | 1982-08-21 | 1984-02-27 | Nitto Shoko Kk | Wire straightener |
| JPS61111963A (en) * | 1984-11-05 | 1986-05-30 | 出光興産株式会社 | Manufacture of carbon formed body |
| JPS621969A (en) * | 1985-06-25 | 1987-01-07 | 松下電工株式会社 | Structure of under floor substrate |
-
1987
- 1987-04-03 JP JP62081250A patent/JPS63248770A/en active Granted
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5252912A (en) * | 1975-10-25 | 1977-04-28 | Nippon Carbon Co Ltd | Manufacture of carbon materials |
| JPS57209883A (en) * | 1981-06-16 | 1982-12-23 | Tokai Carbon Kk | Manufacture of carbon fiber reinforced carbon material |
| JPS5935841A (en) * | 1982-08-21 | 1984-02-27 | Nitto Shoko Kk | Wire straightener |
| JPS61111963A (en) * | 1984-11-05 | 1986-05-30 | 出光興産株式会社 | Manufacture of carbon formed body |
| JPS621969A (en) * | 1985-06-25 | 1987-01-07 | 松下電工株式会社 | Structure of under floor substrate |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63248770A (en) | 1988-10-17 |
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