JPH04170366A - Production of carbon fiber-reinforced carbon composite material - Google Patents
Production of carbon fiber-reinforced carbon composite materialInfo
- Publication number
- JPH04170366A JPH04170366A JP2298627A JP29862790A JPH04170366A JP H04170366 A JPH04170366 A JP H04170366A JP 2298627 A JP2298627 A JP 2298627A JP 29862790 A JP29862790 A JP 29862790A JP H04170366 A JPH04170366 A JP H04170366A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- carbon fiber
- carbon
- base material
- 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.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 70
- 239000004917 carbon fiber Substances 0.000 claims abstract description 56
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229920005989 resin Polymers 0.000 claims abstract description 54
- 239000011347 resin Substances 0.000 claims abstract description 54
- 239000000843 powder Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 31
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 9
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 41
- 239000000839 emulsion Substances 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 13
- 239000002759 woven fabric Substances 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 8
- 229920000877 Melamine resin Polymers 0.000 claims description 7
- 239000003822 epoxy resin Substances 0.000 claims description 7
- 229920000647 polyepoxide Polymers 0.000 claims description 7
- 239000004640 Melamine resin Substances 0.000 claims description 6
- 229920005992 thermoplastic resin Polymers 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- XQUPVDVFXZDTLT-UHFFFAOYSA-N 1-[4-[[4-(2,5-dioxopyrrol-1-yl)phenyl]methyl]phenyl]pyrrole-2,5-dione Chemical compound O=C1C=CC(=O)N1C(C=C1)=CC=C1CC1=CC=C(N2C(C=CC2=O)=O)C=C1 XQUPVDVFXZDTLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004962 Polyamide-imide Substances 0.000 claims description 2
- 238000010000 carbonizing Methods 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 239000004745 nonwoven fabric Substances 0.000 claims description 2
- 239000000123 paper Substances 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920003192 poly(bis maleimide) Polymers 0.000 claims description 2
- 229920006122 polyamide resin Polymers 0.000 claims description 2
- 229920002312 polyamide-imide Polymers 0.000 claims description 2
- 229920013716 polyethylene resin Polymers 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- 239000009719 polyimide resin Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 abstract description 24
- 238000004070 electrodeposition Methods 0.000 abstract description 18
- 238000005245 sintering Methods 0.000 abstract description 16
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 10
- 239000010935 stainless steel Substances 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002904 solvent Substances 0.000 abstract description 7
- 239000012298 atmosphere Substances 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000001652 electrophoretic deposition Methods 0.000 abstract description 4
- 239000002659 electrodeposit Substances 0.000 abstract 1
- 238000010030 laminating Methods 0.000 abstract 1
- 229920001169 thermoplastic Polymers 0.000 abstract 1
- 239000004416 thermosoftening plastic Substances 0.000 abstract 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 14
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 14
- 239000000969 carrier Substances 0.000 description 12
- 125000000129 anionic group Chemical group 0.000 description 9
- 239000003973 paint Substances 0.000 description 9
- 238000005470 impregnation Methods 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野コ
この発明は、炭素繊維強化炭素複合材料の製造方法に関
するものであり、特に、電気泳動沈積を利用して炭素繊
維強化炭素複合材料を製造する方法に関するものである
。[Detailed Description of the Invention] [Industrial Field of Application] This invention relates to a method for producing carbon fiber-reinforced carbon composite materials, and in particular, to a method for producing carbon fiber-reinforced carbon composite materials using electrophoretic deposition. It is about the method.
［従来の技術］
炭素繊維強化炭素複合材料は、炭素繊維基材上に炭素を
付着さす、それを炭化焼成することにより、製造する。[Prior Art] Carbon fiber-reinforced carbon composite materials are manufactured by depositing carbon onto a carbon fiber base material and carbonizing and firing it.
炭素繊維基材上に炭素を付着する方法として、従来は主
に、ＣＶＤ法、液相含浸法を用いていた。Conventionally, CVD methods and liquid phase impregnation methods have been mainly used as methods for attaching carbon onto carbon fiber substrates.
ＣＶＤ法は、減圧条件下、高温に熱した炭素繊維基材上
に炭化水素ガスを接触させ、炭素原子を炭素繊維基材上
に堆積させる方法である。The CVD method is a method in which a carbon fiber base material heated to a high temperature is brought into contact with a hydrocarbon gas under reduced pressure conditions to deposit carbon atoms on the carbon fiber base material.
液相含浸法は、炭素繊維基材に液状レジン、溶融ピッチ
等のマトリックス材料を含浸させる方法である。液相含
浸法を用いて炭素繊維基材上に炭素を付着させた場合、
炭化焼成する際に、マトリックス材料中の揮発成分が抜
けることにより、炭素繊維強化炭素複合材料中に微細な
空孔を生じる。The liquid phase impregnation method is a method in which a carbon fiber base material is impregnated with a matrix material such as liquid resin or molten pitch. When carbon is attached onto a carbon fiber base material using a liquid phase impregnation method,
During carbonization and firing, volatile components in the matrix material escape, creating fine pores in the carbon fiber-reinforced carbon composite material.
したがって、材料強度を上げるために、液相含浸法を用
いた場合は、含浸焼成を繰り返す必要がある。Therefore, in order to increase material strength, when a liquid phase impregnation method is used, it is necessary to repeat impregnation and firing.
ＣＶＤ法、液相含浸法は、いずれも、複雑な方法である
。また、炭素繊維基材に炭素を付着させるのに長時間か
かる。これらのことは、炭素繊維強化炭素複合材料が高
価格となっている原因の１つとなっている。したがって
、炭素繊維強化炭素複合材料は、材料特性（高温強度、
化学的安定性等）が優れているにもかかわらず、現在実
用化されている分野は限られている。Both the CVD method and the liquid phase impregnation method are complicated methods. Further, it takes a long time to attach carbon to the carbon fiber base material. These factors are one of the reasons why carbon fiber-reinforced carbon composite materials are expensive. Therefore, carbon fiber reinforced carbon composite materials have material properties (high temperature strength,
Despite its excellent chemical stability, etc., the fields in which it is currently put into practical use are limited.
一方、最近繊維強化を行なわない通常の炭素材料の製造
方法として、炭素質粉末を炭化焼成することにより製造
する方法が行なわれている。この方法は、既に熱処理を
行なったマトリックス材料を用いている。熱処理を行な
ったマトリックス材料は、揮発分が少ないため、高密度
の炭素材料を短時間に得ることができる。On the other hand, recently, as a conventional method for producing carbon materials without fiber reinforcement, a method has been used in which carbonaceous powder is carbonized and fired. This method uses a matrix material that has already been heat treated. Since the heat-treated matrix material has a low volatile content, a high-density carbon material can be obtained in a short time.
この方法で用いる炭素質粉末を炭素繊維基材上に付着さ
せて焼成すれば、短時間で炭素繊維強化炭素複合材料を
製造することができる。しかし、炭素繊維基材上に炭素
粉末を付着させる方法としては次の２つの方法が考えら
れるが、これらの方法には問題があった。By depositing the carbonaceous powder used in this method on a carbon fiber base material and firing it, a carbon fiber-reinforced carbon composite material can be produced in a short time. However, the following two methods can be considered as a method for attaching carbon powder onto a carbon fiber base material, but these methods have problems.
１つは、炭素繊維基材と炭素粉末とを混ぜ合わせる方法
である。しかしこの方法においては、炭素粉末が炭素繊
維基材を傷付けるおそれがある。One method is to mix a carbon fiber base material and carbon powder. However, in this method, there is a risk that the carbon powder may damage the carbon fiber base material.
他の１つは、炭素粉末を水に混ぜ、スラリー状（どろっ
とした液状）にし、その液に炭素繊維基材をつける方法
である。しかし、この方法においては、所望量の炭素粉
末を、炭素繊維基材上にしかも均一に付着させることが
困難である。Another method is to mix carbon powder with water to form a slurry (thick liquid) and apply the carbon fiber base material to the slurry. However, in this method, it is difficult to uniformly deposit a desired amount of carbon powder onto the carbon fiber substrate.
炭素繊維基材上に、炭素粉末を定量的に均一に付着させ
る方法として、いわゆる電気泳動沈積法がある。この方
法は、本願出願人と同一出願人がした特開昭６０−５４
９７４号公報に開示されている。この方法を簡単に説明
する。まず、担体が付着した炭素質粉末が分散している
液体を準備する。この液体に、炭素繊維基材と電極部材
とを浸漬する。担体は電気泳動性を有する。したがって
、炭素繊維基材と電極部材との間に直流電圧を印加する
と、担体は、炭素繊維基材に付着する。担体には、炭素
質粉末が付着しているので、炭素繊維基材上に炭素質粉
末を付着させることができる。As a method for quantitatively and uniformly depositing carbon powder on a carbon fiber base material, there is a so-called electrophoretic deposition method. This method is based on Japanese Patent Application Laid-Open No. 60-54 filed by the same applicant as the present applicant.
It is disclosed in Japanese Patent No. 974. This method will be briefly explained. First, a liquid in which carbonaceous powder to which a carrier is attached is dispersed is prepared. The carbon fiber base material and the electrode member are immersed in this liquid. The carrier has electrophoretic properties. Therefore, when a DC voltage is applied between the carbon fiber base material and the electrode member, the carrier adheres to the carbon fiber base material. Since the carbonaceous powder is attached to the carrier, the carbonaceous powder can be attached onto the carbon fiber base material.
さらに、担体として熱硬化性樹脂を用いる方法がある。Furthermore, there is a method of using a thermosetting resin as a carrier.
この方法は、本願出願人と同一出願人がした特開昭６１
−２１９７３号公報に開示されている。熱硬化性樹脂は
、焼成すると炭素となるので、この方法によれば、さら
に、高密度な炭素繊維強化炭素複合材料を得られる。This method is based on the patent application published in Japanese Patent Application Laid-Open No. 61, published by the same applicant as the present applicant.
It is disclosed in Japanese Patent No.-21973. Since the thermosetting resin becomes carbon when fired, a carbon fiber-reinforced carbon composite material with even higher density can be obtained by this method.
電気泳動沈積法を用いた場合、担体の数を少なくすると
、炭素繊維基材上に炭素粉末を短時間で析出させること
ができる。しかし、担体の数が少ないと、炭素繊維基材
の場所によって、炭素粉末の付着量に差が生じ、むらの
ある炭素繊維強化炭素複合材料となってしまう。When electrophoretic deposition is used, carbon powder can be deposited on a carbon fiber substrate in a short time by reducing the number of carriers. However, if the number of carriers is small, the amount of carbon powder deposited will vary depending on the location on the carbon fiber base material, resulting in an uneven carbon fiber reinforced carbon composite material.
一方、担体の数を多くすると、炭素繊維基材上に炭素粉
末を付着させるのに長時間を要する。しかし、担体の数
が多いと、炭素繊維基材上に均一に炭素粉末を付着させ
ることができ、均一な炭素繊維強化炭素複合材料を得ら
れる。このことを、具体的に説明していく。On the other hand, when the number of carriers is increased, it takes a long time to adhere the carbon powder onto the carbon fiber base material. However, when the number of carriers is large, carbon powder can be uniformly deposited on the carbon fiber base material, and a uniform carbon fiber reinforced carbon composite material can be obtained. This will be explained in detail.
たとえば、１０個の炭素質粉末を２個の担体で析出させ
る場合と、１０個の炭素質粉末を５個の担体で析出する
場合とを比較してみる。単位時間に炭素繊維基材上に付
着する担体の量は決まっている。担体が２個の場合は、
１個の担体で５個の炭素質粉末を運ぶ。担体が５個の場
合は、１個の担体で２個の炭素質粉末を運ぶ。したがっ
て、担体の数が少ない方が、短時間で、炭素繊維基材上
に炭素質粉末を析出させることができる。For example, let us compare the case where 10 carbonaceous powders are precipitated using two carriers and the case where 10 carbonaceous powders are precipitated using 5 carriers. The amount of carrier deposited on the carbon fiber substrate per unit time is fixed. If there are two carriers,
One carrier carries 5 pieces of carbonaceous powder. When there are five carriers, one carrier carries two carbonaceous powders. Therefore, the smaller the number of carriers, the faster the carbonaceous powder can be deposited on the carbon fiber base material.
担体が炭素繊維基材上に析出すると、担体は絶縁物に変
わる。このため、担体が析出した箇所には、さらに担体
または炭素質粉末が析出するということはない。一方、
炭素は導電性を有するので、炭素質粉末が析出したた箇
所には、さらに担体または炭素質粉末が析出する。した
がって、担体の数が少ないと、炭素繊維基材上に炭素質
粉末を均一に析出させることができない。When the carrier is deposited on the carbon fiber substrate, the carrier turns into an insulator. Therefore, no further carrier or carbonaceous powder is deposited at the location where the carrier is deposited. on the other hand,
Since carbon has conductivity, a carrier or carbonaceous powder is further precipitated at the location where the carbonaceous powder has been precipitated. Therefore, if the number of carriers is small, carbonaceous powder cannot be uniformly deposited on the carbon fiber base material.
［発明が解決しようとする課題］
炭素繊維強化炭素複合材料としては、当然、均一なもの
が好ましい。したがって、従来は担体の量を多くして、
炭素繊維基材上に炭素質粉末を析出させていた。しかし
、先はど説明したように、担体の量が多くなると、炭素
繊維基材上に炭素質粉末を析出させるのに長時間を要す
る。これにより、炭素繊維強化炭素複合材料の製造時間
が長くなる。[Problems to be Solved by the Invention] Naturally, it is preferable that the carbon fiber reinforced carbon composite material be uniform. Therefore, conventionally, the amount of carrier was increased,
Carbonaceous powder was deposited on the carbon fiber base material. However, as explained earlier, when the amount of carrier increases, it takes a long time to deposit the carbonaceous powder on the carbon fiber substrate. This increases the manufacturing time of the carbon fiber reinforced carbon composite material.
この発明はかかる従来の問題点を解決するためになされ
たものである。この発明の目的は、炭素繊維基材上に炭
素質粉末を均一に析出させることができ、かつ炭素繊維
基材上に炭素質粉末を短時間で析出させることができる
、炭素繊維強化炭素複合材料の製造方法を提供すること
である。This invention has been made to solve these conventional problems. An object of the present invention is to create a carbon fiber-reinforced carbon composite material that can deposit carbonaceous powder uniformly on a carbon fiber base material and that can deposit carbonaceous powder on a carbon fiber base material in a short time. An object of the present invention is to provide a manufacturing method.
［課題を解決するための手段］
この発明に従った炭素繊維強化炭素複合材料の製造方法
は以下の工程を備える。 、液体中でイオン化するこ
とにより担体となる物質とエマルジョンタイプの樹脂と
が吸着している炭素質の粉末が分散している液体を作製
する。[Means for Solving the Problems] A method for manufacturing a carbon fiber-reinforced carbon composite material according to the present invention includes the following steps. By ionizing in the liquid, a liquid is prepared in which carbonaceous powder in which a carrier substance and an emulsion type resin are adsorbed is dispersed.
次に、液体に、炭素繊維基材と電極部材とを浸漬する。Next, the carbon fiber base material and the electrode member are immersed in the liquid.
次に、炭素繊維基材と電極部材との間に直流電圧を印加
し、担体の電気泳動性を利用して、炭素繊維基材上に、
担体とエマルジョンタイプの樹脂とが吸着している炭素
質の粉末を、析出させる。Next, a DC voltage is applied between the carbon fiber base material and the electrode member, and using the electrophoretic properties of the carrier, the carbon fiber base material is
Carbonaceous powder to which the carrier and emulsion type resin are adsorbed is precipitated.
次に、炭素質の粉末が析出している炭素繊維基材を炭化
焼成する。Next, the carbon fiber base material on which the carbonaceous powder has been precipitated is carbonized and fired.
エマルジョンタイプ樹脂としては、親水基をもつ界面活
性剤を吸着させた熱可塑性樹脂、または、親水基をもつ
界面活性剤を吸着させた熱硬化性樹脂のうち、少なくと
もいずれか一方がある。The emulsion type resin includes at least one of a thermoplastic resin on which a surfactant having a hydrophilic group is adsorbed, and a thermosetting resin on which a surfactant having a hydrophilic group is adsorbed.
熱可塑性樹脂としては、ポリアミド樹脂又はポリエチレ
ン樹脂があり、熱硬化性樹脂としては、メラミン樹脂、
エポキシ樹脂、フラン樹脂、フェノール樹脂、ポリイミ
ド樹脂、ポリアミドイミド樹脂およびビスマレイミド樹
脂を含む群から選ばれた少なくとも１種以上がある。Thermoplastic resins include polyamide resins and polyethylene resins, and thermosetting resins include melamine resins,
There is at least one kind selected from the group including epoxy resin, furan resin, phenol resin, polyimide resin, polyamideimide resin, and bismaleimide resin.
担体となる物質としては、熱可塑性樹脂誘導体を改質し
電気泳動性を持たせたものまたは、熱硬化性樹脂誘導体
を改質し電気泳動性を持たせたもの、のうち少なくとも
いずれか一方がある。The carrier material may be at least one of a thermoplastic resin derivative modified to have electrophoretic properties or a thermosetting resin derivative modified to have electrophoretic properties. be.
炭素繊維基材としては、短繊維、長繊維、長繊維を束ね
た紐状のもの、織布、ペーパーおよび不織布を含む群か
ら選ばれた少なくとも１種以上がある。As the carbon fiber base material, there is at least one kind selected from the group including short fibers, long fibers, string-like materials made by bundling long fibers, woven fabrics, paper, and nonwoven fabrics.
［作用］ エマルジョンタイプの樹脂は、絶縁性を有する。[Effect] Emulsion type resin has insulation properties.
このため、炭素質粉末にエマルジョンタイプの樹脂を吸
着させて、炭素繊維基材上に析出させると、その箇所に
は、新たに炭素質粉末は析出しない。Therefore, when an emulsion type resin is adsorbed to carbonaceous powder and deposited on the carbon fiber base material, no new carbonaceous powder is deposited at that location.
したがって、担体の量を少なくしても、炭素繊維基材上
に炭素質粉末を均一に析出させることができる。先はど
説明したように、担体の量が少ないと、炭素繊維基材上
に炭素質粉末を析出せさる時間を短くすることができる
。Therefore, even if the amount of carrier is reduced, the carbonaceous powder can be uniformly deposited on the carbon fiber base material. As explained earlier, when the amount of carrier is small, the time for depositing the carbonaceous powder on the carbon fiber substrate can be shortened.
樹脂のうちエマルジョンタイプの樹脂としたのは、エマ
ルジョンタイプの樹脂に水溶性があるからである。エマ
ルジョンタイプの樹脂を炭素粉末に付着させると、炭素
質粉末は液体中に均一に分散する。したがって、炭素質
粉末にエマルジョンタイプの樹脂を吸着させた場合は、
液体中の炭素質粉末を沈澱しにく（させる効果がある。Among the resins, the emulsion type resin was selected because emulsion type resins are water-soluble. When an emulsion type resin is attached to carbon powder, the carbonaceous powder is uniformly dispersed in the liquid. Therefore, when emulsion type resin is adsorbed on carbonaceous powder,
It has the effect of making it difficult for the carbonaceous powder in the liquid to settle.
［実施例］
（実施例１）
■ 自己焼結性炭素粉末とエマルジョンタイプのメラミ
ン樹脂を重量比で３＝１の割合で混合した。これにより
、自己焼結性炭素粉末にエマルジョンタイプのメラミン
樹脂が吸着する。[Examples] (Example 1) (1) Self-sintering carbon powder and emulsion type melamine resin were mixed in a weight ratio of 3=1. As a result, the emulsion type melamine resin is adsorbed onto the self-sintering carbon powder.
■ 上記粉末を、ポリアクリロニトリル系ｔｌＦ用樹脂
（電着用樹脂とは、電気泳動性を持たせた樹脂のことで
ある）および溶剤とよ（混練りした後、水に分散させ、
いわゆるアニオン系塗料分散状態とした。この状態で炭
素質粉末（エマルジョンタイプのメラミン樹脂を含む）
と電着用樹脂との比率を重量比で４＝１とした。■ The above powder is mixed with a polyacrylonitrile TIF resin (electrodeposition resin is a resin that has electrophoretic properties) and a solvent (after kneading, it is dispersed in water,
It was in a so-called anionic paint dispersion state. In this state, carbonaceous powder (including emulsion type melamine resin)
The weight ratio of the electrodepositing resin and the electrodepositing resin was 4=1.
■ このアニオン系塗料に、ＰＡＮ系炭素炭素繊維織布
テンレス鋼板とを浸漬させた。ＰＡＮ系炭素炭素繊維織
布極とし、ステンレス鋼板を陰極とし、ＰＡＮ系炭素炭
素繊維織布テンレス鋼板との間に直流電圧を印加し、ア
ニオン系塗料を撹拌しながらＰＡＮ系炭素炭素繊維織布
上己焼結性炭素粉末、エマルジョンタイプのメラミン樹
脂、ポリアクリロニトリル系電着用樹脂を析出させた。(2) A PAN-based carbon carbon fiber woven stainless steel plate was immersed in this anionic paint. A PAN-based carbon carbon fiber woven fabric is used as an electrode, a stainless steel plate is used as a cathode, and a DC voltage is applied between the PAN-based carbon carbon fiber woven fabric and the stainless steel plate, and while stirring the anionic paint, the PAN-based carbon carbon fiber woven fabric is coated. Self-sintering carbon powder, emulsion type melamine resin, and polyacrylonitrile electrodeposition resin were deposited.
ＰＡＮ系炭素炭素繊維織布覆物（自己焼結性炭素粉末、
エマルジョンタイプのメラミン樹脂、ポリアクリロニト
リル系電着用樹脂）との重量比が１０＝１２となるよう
にした。電圧は、約５０Ｖにした。電着時間は、２分間
であった。PAN-based carbon carbon fiber woven covering (self-sintering carbon powder,
The weight ratio of emulsion type melamine resin and polyacrylonitrile electrodepositing resin was 10=12. The voltage was approximately 50V. The electrodeposition time was 2 minutes.
■ 上記電着体を２００枚積層した。そして、温度２５
０℃、面圧カフ５ｋｇ／ｃｍ２、時間５０分で加圧成形
した。(2) 200 sheets of the above electrodeposited bodies were laminated. And temperature 25
Pressure molding was carried out at 0°C, surface pressure cuff 5 kg/cm2, and time 50 minutes.
■ この成形体の厚みを保持しながら３５０℃で９時間
加熱した。(2) The molded body was heated at 350° C. for 9 hours while maintaining its thickness.
■ この後、この成形体を不活性雰囲気中で昇温させな
がら加圧し炭素繊維強化炭素複合材料を得た。面圧力は
、６００ｋｇ／ｃｍ２であった。(2) Thereafter, this molded body was heated and pressed in an inert atmosphere to obtain a carbon fiber-reinforced carbon composite material. The surface pressure was 600 kg/cm2.
昇温速度は、１０００℃までが３０℃／ ｈ ｒで、２
０００℃までが１００℃／ ｈ ｒであった。The temperature increase rate is 30℃/hr up to 1000℃, 2
The temperature up to 000°C was 100°C/hr.
■ 電着に要した時間は、合計で６時間４０分であった
。なぜなら、１枚につき電着時間が２分かかるのを、２
００枚電着したからである。■ The total time required for electrodeposition was 6 hours and 40 minutes. This is because it takes 2 minutes for electrodeposition per sheet.
This is because 00 sheets were electrodeposited.
（実施例２）
■ 自己焼結性炭素粉末とエマルジョンタイプのエポキ
シ樹脂を重量比で５：２の割合で混合した。これにより
自己焼結性炭素粉末にエマルジョンタイプのエポキシ樹
脂が吸着する。(Example 2) (2) Self-sintering carbon powder and emulsion type epoxy resin were mixed at a weight ratio of 5:2. As a result, the emulsion type epoxy resin is adsorbed onto the self-sintering carbon powder.
■ 上記粉末をポリアクリロニトリル系電着用樹脂およ
び溶剤とよく混練りした後、水に分散させ、いわゆるア
ニオン系塗料分散状態とした。この状態で炭素質粉末（
エマルジョンタイプのエポキシ樹脂を含む）と電着用樹
脂との比率を重量比で４：１とした。(2) The above powder was thoroughly kneaded with a polyacrylonitrile electrodeposition resin and a solvent, and then dispersed in water to form a so-called anionic paint dispersion state. In this state, carbonaceous powder (
(including emulsion type epoxy resin) and the electrodepositing resin was set at a weight ratio of 4:1.
■ このアニオン系塗料に、ＰＡＮ系炭素炭素繊維織布
テンレス鋼板とを浸漬した。ＰＡＮ系炭素炭素繊維織布
極とし、ステンレス鋼板を陰極とし、ＰＡＮ系炭素炭素
繊維織布テンレス鋼板との間に直流電圧を印加し、アニ
オン系塗料を撹拌しながらＰＡＮ系炭素炭素繊維織布上
己焼結性炭素粉末、エマルジョンタイプのエポキシ樹脂
、ポリアクリロニトリル系電着用樹脂を析出させた。Ｐ
ＡＮ系炭素炭素繊維織布覆物（自己焼結性炭素粉末、エ
マルジョンタイプのエポキシ樹脂、ポリアクリロニトリ
ル系電着用樹脂）との重量比が１０＝１２となるように
した。電圧は約５０Ｖにした。(2) A PAN-based carbon carbon fiber woven stainless steel plate was immersed in this anionic paint. A PAN-based carbon carbon fiber woven fabric is used as an electrode, a stainless steel plate is used as a cathode, and a DC voltage is applied between the PAN-based carbon carbon fiber woven fabric and the stainless steel plate, and while stirring the anionic paint, the PAN-based carbon carbon fiber woven fabric is coated. Self-sintering carbon powder, emulsion type epoxy resin, and polyacrylonitrile electrodeposition resin were deposited. P
The weight ratio with the AN-based carbon carbon fiber woven fabric covering (self-sintering carbon powder, emulsion type epoxy resin, polyacrylonitrile electrodepositing resin) was adjusted to 10=12. The voltage was approximately 50V.
電着時間は、２分１０秒間であった。The electrodeposition time was 2 minutes and 10 seconds.
■ 上記電着体を２００枚積層した。そして、温度２５
０℃、面圧カフ５ｋｇ／ｃｍ２、時間５０分で加圧成形
した。(2) 200 sheets of the above electrodeposited bodies were laminated. And temperature 25
Pressure molding was carried out at 0°C, surface pressure cuff 5 kg/cm2, and time 50 minutes.
■ この成形体の厚みを保持しながら３５０℃で９時間
加熱した。(2) The molded body was heated at 350° C. for 9 hours while maintaining its thickness.
■ この後、この成形体を不活性雰囲気中で昇温させな
がら加圧し、炭素繊維強化炭素複合材料を得た。面圧力
は、６００ｋｇ／ｃｍ２であった。(2) Thereafter, this molded body was heated and pressed in an inert atmosphere to obtain a carbon fiber-reinforced carbon composite material. The surface pressure was 600 kg/cm2.
昇温速度は、１０００℃までが３０℃／ ｈ ｒで、２
０００℃までが１００℃／ｈｒであった。The temperature increase rate is 30℃/hr up to 1000℃, 2
The rate was 100°C/hr up to 000°C.
■ 電着に要した時間は、合計７時間１３分２０秒であ
った。なぜなら、１枚につき電着時間が２分１０秒かか
るるのを、２００枚電着したからである。■ The total time required for electrodeposition was 7 hours, 13 minutes, and 20 seconds. This is because 200 sheets were electrodeposited, although it took 2 minutes and 10 seconds for each sheet.
（比較例）
■ 自己焼結性炭素粉末をポリアクリロニトリル系電着
用樹脂および溶剤とよく混練りした後、水に分散させ、
いわゆるアニオン系塗料分散状態とした。この状態で炭
素質粉末と電着用樹脂との比率を重量比で１＝１とした
。(Comparative example) ■ After thoroughly kneading self-sintering carbon powder with polyacrylonitrile electrodepositing resin and solvent, dispersing it in water,
It was in a so-called anionic paint dispersion state. In this state, the weight ratio of the carbonaceous powder to the electrodepositing resin was set to 1=1.
■ このアニオン系塗料中に、ＰＡＮ系炭素炭素繊維織
布テンレス鋼板とを浸漬した。ＰＡＮ系炭素炭素繊維織
布極とし、ステンレス鋼板を陰極とし、ＰＡＮ系炭素炭
素繊維織布テンレス鋼板との間に直流電圧を印加し、ア
ニオン系塗料を撹拌しながら、ＰＡＮ系炭素炭素繊維織
布上己焼結性炭素粉末、ポリアクリロニトリル系電着用
樹脂を析出させた。ＰＡＮ系炭素炭素繊維織布覆物（自
己焼結性炭素粉末、ポリアクリロニトリル系電着用樹脂
）との重量比が１０ ：１２となるようにした。電圧は
約５０Ｖにした。電着時間は、１５分間であった。(2) A PAN-based carbon fiber woven stainless steel plate was immersed in this anionic paint. A PAN-based carbon carbon fiber woven fabric is used as an electrode, a stainless steel plate is used as a cathode, and a DC voltage is applied between the PAN-based carbon carbon fiber woven fabric and the stainless steel plate, and while stirring the anionic paint, the PAN-based carbon carbon fiber woven fabric is A self-sintering carbon powder and a polyacrylonitrile electrodepositing resin were deposited. The weight ratio with the PAN-based carbon carbon fiber woven fabric covering (self-sintering carbon powder, polyacrylonitrile-based electrodepositing resin) was adjusted to 10:12. The voltage was approximately 50V. Electrodeposition time was 15 minutes.
■ 上記電着体を２００枚積層した。そして、温度２５
０℃、面圧カフ ５ ｋ ｇ ／ ｃ ｍ ２、時間５
０分で加圧成形した。(2) 200 sheets of the above electrodeposited bodies were laminated. And temperature 25
0℃, surface pressure cuff 5 kg/cm2, time 5
Pressure molding was performed in 0 minutes.
■ この成形体の厚みを保持しながら３５０℃で９時間
加熱した。(2) The molded body was heated at 350° C. for 9 hours while maintaining its thickness.
■ この後、この成形体を不活性雰囲気中で不活性雰囲
気を昇温させながら加圧し、炭素繊維強化炭素複合材料
を得た。面圧力は、６００ｋｇ／Ｃｍ２であった。昇温
速度は、１０００℃までが３０℃／ｈｒで、２０００℃
までが１００℃／ｈｒであった。(2) Thereafter, this molded body was pressurized in an inert atmosphere while increasing the temperature of the inert atmosphere to obtain a carbon fiber-reinforced carbon composite material. The surface pressure was 600 kg/Cm2. The temperature increase rate is 30℃/hr up to 1000℃, and 2000℃
up to 100°C/hr.
■ 電着に要した時間は、合計５０時間であった。なぜ
なら、１枚につき電着時間が１５分かかるのを２００枚
電着したからである。■ The total time required for electrodeposition was 50 hours. This is because 200 sheets were electrodeposited, although each sheet required 15 minutes for electrodeposition.
実施例１、実施例２、比較例における電着時間を比較す
ればわかるように、実施例１および実施例２は、比較例
と比べ、電着時間を大幅に短縮することができる。した
がって、実施例１、実施例２を用いて炭素繊維強化炭素
複合材料を製造すれば、製造時間を短縮することができ
る。As can be seen by comparing the electrodeposition times in Example 1, Example 2, and Comparative Example, Example 1 and Example 2 can significantly shorten the electrodeposition time compared to the Comparative Example. Therefore, if a carbon fiber-reinforced carbon composite material is manufactured using Examples 1 and 2, manufacturing time can be shortened.
実施例１、実施例２によれば、自己焼結性炭素粉末、エ
マルジョンタイプの樹脂、電着用樹脂、溶剤を混練りし
たものを、水に分散させている。According to Examples 1 and 2, a mixture of self-sintering carbon powder, emulsion type resin, electrodepositing resin, and solvent was dispersed in water.
しかしながら、この発明においてはこれに限定されるわ
けではなく、水辺外の溶媒に分散させてもよい。この場
合、エマルジョンタイプの樹脂は、この溶媒中に分散す
るものでなければならない。However, the present invention is not limited to this, and may be dispersed in a solvent outside the water. In this case, the emulsion type resin must be one that is dispersed in this solvent.
実施例１、実施例２によれば、自己焼結性炭素粉末とエ
マルジョンタイプの樹脂とを混合した後、水に分散させ
ている。しかしながら、この発明においてはこれに限定
されるわけではなく、水に自己焼結性炭素粉末とエマル
ジョンタイプの樹脂と電着用樹脂とを入れ、撹拌するこ
とにより、電着液を作製してもよい。According to Examples 1 and 2, the self-sintering carbon powder and the emulsion type resin are mixed and then dispersed in water. However, the present invention is not limited to this, and the electrodeposition liquid may be prepared by adding self-sintering carbon powder, emulsion type resin, and electrodeposition resin to water and stirring the mixture. .
実施例１、実施例２によれば、炭素質の粉末として自己
焼結性炭素粉末を用いている。しかしながら、この発明
においてはこれに限定されるわけではなく、黒鉛粉末、
カーボン粉末を用いてもよい。According to Examples 1 and 2, self-sintering carbon powder is used as the carbonaceous powder. However, the present invention is not limited to this, and graphite powder,
Carbon powder may also be used.
［効果コ
この発明に従った炭素繊維強化炭素複合材料の製造方法
においては、炭素質粉末にエマルジョンタイプの樹脂を
吸着させている。したがって担体の数を少なくしても炭
素繊維基材上に炭素質粉末を均一に析出させることがで
きる。担体の数を少なくすると炭素質粉末を析出させる
時間が短くなるので、炭素繊維強化炭素複合材料の製造
時間を短くすることができる。[Effects] In the method for producing a carbon fiber-reinforced carbon composite material according to the present invention, an emulsion type resin is adsorbed onto carbonaceous powder. Therefore, even if the number of carriers is reduced, the carbonaceous powder can be uniformly deposited on the carbon fiber base material. When the number of carriers is reduced, the time for precipitating the carbonaceous powder is shortened, so that the manufacturing time of the carbon fiber reinforced carbon composite material can be shortened.
Claims (5)
とエマルジョンタイプの樹脂とが吸着している炭素質の
粉末が分散している液体を作製する工程と、 前記液体に、炭素繊維基材と電極部材とを浸漬する工程
と、 前記炭素繊維基材と前記電極部材との間に直流電圧を印
加し、前記担体の電気泳動性を利用して、前記炭素繊維
基材上に、前記担体と前記エマルジョンタイプの樹脂と
が吸着している前記炭素質の粉末を、析出させる工程と
、 前記炭素質の粉末が析出している前記炭素繊維基材を炭
化焼成する工程と、 を備えた、炭素繊維強化炭素複合材料の製造方法。(1) A step of producing a liquid in which carbonaceous powder in which a carrier substance and an emulsion type resin are adsorbed by ionization in the liquid is dispersed, and adding a carbon fiber base material to the liquid. applying a DC voltage between the carbon fiber base material and the electrode member, and utilizing the electrophoretic properties of the carrier to coat the carbon fiber base material with the carrier and the electrode member; a step of precipitating the carbonaceous powder to which the emulsion type resin is adsorbed; and a step of carbonizing and firing the carbon fiber base material on which the carbonaceous powder is precipitated. Method for manufacturing fiber reinforced carbon composite material.
界面活性剤を吸着させた熱可塑性樹脂または、親水基を
もつ界面活性剤を吸着させた熱硬化性樹脂のうち、少な
くともいずれか一方である、請求項１に記載の炭素繊維
強化炭素複合材料の製造方法。(2) The emulsion type resin is at least one of a thermoplastic resin on which a surfactant having a hydrophilic group is adsorbed, and a thermosetting resin on which a surfactant having a hydrophilic group is adsorbed. A method for producing a carbon fiber reinforced carbon composite material according to claim 1.
チレン樹脂であり、 前記熱硬化性樹脂は、メラミン樹脂、エポキシ樹脂、フ
ラン樹脂、フェノール樹脂、ポリイミド樹脂、ポリアミ
ドイミド樹脂およびビスマレイミド樹脂を含む群から選
ばれた少なくとも１種以上である、請求項２に記載の炭
素繊維強化炭素複合材料の製造方法。(3) The thermoplastic resin is a polyamide resin or a polyethylene resin, and the thermosetting resin is selected from the group including melamine resin, epoxy resin, furan resin, phenol resin, polyimide resin, polyamide-imide resin, and bismaleimide resin. The method for producing a carbon fiber-reinforced carbon composite material according to claim 2, wherein the carbon fiber-reinforced carbon composite material is at least one selected type.
動性を持たせたもの、または熱硬化性樹脂誘導体を改質
し、電気泳動性を持たせたもの、のうち少なくともいず
れか一方である、請求項１に記載の炭素繊維強化炭素複
合材料の製造方法。(4) The substance is at least one of a thermoplastic resin derivative modified to have electrophoretic properties, or a thermosetting resin derivative modified to have electrophoretic properties. The method for producing a carbon fiber reinforced carbon composite material according to claim 1.
束ねた紐状のもの、織布、ペーパーおよび不織布を含む
群から選ばれた少なくとも１種以上である、請求項１に
記載の炭素繊維強化炭素複合材料の製造方法。(5) The carbon fiber base material is at least one type selected from the group consisting of short fibers, long fibers, string-like materials made by bundling long fibers, woven fabric, paper, and non-woven fabric. The method for manufacturing the carbon fiber reinforced carbon composite material described above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2298627A JPH04170366A (en) | 1990-11-02 | 1990-11-02 | Production of carbon fiber-reinforced carbon composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2298627A JPH04170366A (en) | 1990-11-02 | 1990-11-02 | Production of carbon fiber-reinforced carbon composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04170366A true JPH04170366A (en) | 1992-06-18 |
Family
ID=17862183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2298627A Pending JPH04170366A (en) | 1990-11-02 | 1990-11-02 | Production of carbon fiber-reinforced carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04170366A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880494A (en) * | 2016-09-30 | 2018-04-06 | 比亚迪股份有限公司 | A kind of carbon fibre initial rinse fabric and preparation method thereof and metal fiber composite |
-
1990
- 1990-11-02 JP JP2298627A patent/JPH04170366A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880494A (en) * | 2016-09-30 | 2018-04-06 | 比亚迪股份有限公司 | A kind of carbon fibre initial rinse fabric and preparation method thereof and metal fiber composite |
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