JPH07268111A - Composite material using carbon fiber - Google Patents
Composite material using carbon fiberInfo
- Publication number
- JPH07268111A JPH07268111A JP20343994A JP20343994A JPH07268111A JP H07268111 A JPH07268111 A JP H07268111A JP 20343994 A JP20343994 A JP 20343994A JP 20343994 A JP20343994 A JP 20343994A JP H07268111 A JPH07268111 A JP H07268111A
- Authority
- JP
- Japan
- Prior art keywords
- composite material
- carbon fiber
- oxide
- matrix
- carbon fibers
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 48
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 29
- 239000011159 matrix material Substances 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 239000011247 coating layer Substances 0.000 claims abstract description 15
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims abstract description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 3
- 239000000084 colloidal system Substances 0.000 claims description 7
- 229910052752 metalloid Inorganic materials 0.000 claims description 6
- 150000002738 metalloids Chemical class 0.000 claims description 6
- 238000011282 treatment Methods 0.000 abstract description 9
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 229920005989 resin Polymers 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 239000004593 Epoxy Substances 0.000 abstract description 2
- 239000004952 Polyamide Substances 0.000 abstract description 2
- 229920002647 polyamide Polymers 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 21
- 239000000835 fiber Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 239000011295 pitch Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- -1 or electrolysis Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Inorganic Fibers (AREA)
- Reinforced Plastic Materials (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、表面に金属又は半金属
の酸化物のゲルが被覆された、マトリックスとの接着性
が改善された炭素繊維を使用した複合材に関するもので
ある。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composite material using a carbon fiber whose surface is coated with a gel of a metal or metalloid oxide and which has improved adhesion to a matrix.
【０００２】[0002]
【従来の技術】炭素繊維は、樹脂、金属、セラミック、
炭素等をマトリックスとする複合材の補強繊維として注
目されている。複合材においては、補強繊維が負荷され
た応力を主に担い、マトリックスは応力を個々の繊維に
均等に分担させる伝達の役割を担うといわれている。従
って、複合材としての性能を充分なものとするために
は、繊維がマトリックス中に均一に分布し、その繊維が
マトリックスで一様に囲まれており、更に、繊維とマト
リックスが充分に接着していて応力の伝達が円滑に行わ
れるようになっていることが重要である。2. Description of the Related Art Carbon fibers are used for resins, metals, ceramics,
It has been attracting attention as a reinforcing fiber for composite materials using carbon as a matrix. In the composite material, it is said that the reinforcing fibers mainly bear the stress applied thereto, and the matrix plays a role of transmitting the stress to the individual fibers evenly. Therefore, in order to obtain sufficient performance as a composite material, the fibers are uniformly distributed in the matrix, the fibers are uniformly surrounded by the matrix, and further, the fibers and the matrix are sufficiently adhered. However, it is important that the stress is transmitted smoothly.
【０００３】しかし、一般に、炭素繊維はマトリックス
との接着性が悪く、充分な性能を示す複合材が得にく
い。そこで、従来は、例えば、酸化性ガスや酸溶液、或
いは、電気分解等により炭素繊維の表面を活性化した
り、化学蒸着法（ＣＶＤ法）等により炭素繊維の表面に
金属の蒸着層を設けたりする等の方法が取られている。However, in general, carbon fibers have poor adhesion to the matrix, and it is difficult to obtain a composite material having sufficient performance. Therefore, conventionally, for example, the surface of the carbon fiber is activated by an oxidizing gas, an acid solution, or electrolysis, or a metal vapor deposition layer is provided on the surface of the carbon fiber by a chemical vapor deposition method (CVD method) or the like. The method such as doing is taken.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、これら
従来の方法は、製造工程が繁雑であったり、大規模の処
理装置を必要とする等工業的生産には必ずしも有利とは
いえなかった。また、補強繊維を比較的簡便に製造する
方法として、炭素繊維の表面にアルコキシアルミニウム
アセチレートの溶液を塗布し、それを焼成して酸化アル
ミニウム等の被膜を形成する方法が提案されている（特
開昭６０−７６３３５号公報）が、未だマトリックスと
の接着性が充分とはいえず、更に改良が望まれていた。However, these conventional methods have not always been advantageous for industrial production due to complicated manufacturing steps and the need for large-scale processing equipment. Further, as a method of relatively easily producing reinforcing fibers, a method of applying a solution of alkoxyaluminum acetylate on the surface of carbon fibers and firing the solution to form a coating film of aluminum oxide or the like has been proposed. However, it cannot be said that the adhesiveness with the matrix is still sufficient, and further improvement has been desired.
【０００５】[0005]
【課題を解決するための手段】そこで、本発明者は、か
かる課題を解決すべく、鋭意検討した結果、炭素繊維の
表面に金属又は半金属の酸化物のコロイド溶液を塗布
し、加熱処理して酸化物のゲルの被覆層を形成すれば炭
素繊維の表面に凹凸を有する被覆層とすることができる
結果、上述の如き課題が解決できることを見い出し本発
明に到達した。The inventors of the present invention have made extensive studies in order to solve the above-mentioned problems, and as a result, applied a colloidal solution of a metal or metalloid oxide to the surface of carbon fiber and heat-treated it. The present invention has been accomplished by finding that the above-mentioned problems can be solved as a result of forming a coating layer having an oxide gel on the surface of the carbon fiber to form a coating layer having irregularities.
【０００６】すなわち、本発明の目的は、簡便な方法
で、しかもマトリックスとの接着性が更に改善された補
強繊維を使用した複合材を提供することにある。そし
て、その目的は、補強繊維とマトリックスからなる複合
材において、該補強繊維が、表面に金属又は半金属の酸
化物のゲルの被覆層を有する炭素繊維であって、該被覆
層が炭素繊維表面に塗布された該酸化物のコロイド溶液
を加熱処理することによって形成されたものであること
を特徴とする複合材により容易に達成される。[0006] That is, an object of the present invention is to provide a composite material using a reinforcing fiber by a simple method and further having improved adhesion to a matrix. And the object is a composite material comprising a reinforcing fiber and a matrix, wherein the reinforcing fiber is a carbon fiber having a coating layer of a metal or semimetal oxide gel on the surface, and the coating layer is a carbon fiber surface. It is easily achieved by the composite material characterized in that it is formed by heat-treating the colloidal solution of the oxide applied to the.
【０００７】以下本発明を詳細に説明する。本発明で使
用する炭素繊維は、公知のポリアクリロニトリル系及び
ピッチ系炭素繊維が使用できるが、ピッチ系、特にメソ
フェーズピッチを紡糸して得られる炭素繊維、或いは、
気相熱分解法により得られる炭素繊維の様な表面活性の
低い炭素繊維において効果が大であるので好適である。The present invention will be described in detail below. The carbon fiber used in the present invention, known polyacrylonitrile-based and pitch-based carbon fiber can be used, pitch-based, especially carbon fiber obtained by spinning mesophase pitch, or,
It is suitable because it has a great effect on carbon fibers having a low surface activity such as carbon fibers obtained by a vapor phase pyrolysis method.
【０００８】これら炭素繊維は、予め陽極酸化等により
表面を酸化処理しておくことが本発明の被覆層を堅固に
固着することができるので好ましい。その際、酸化によ
り炭素繊維自体の性能が劣化されない程度の極く軽度な
酸化処理でよい。本発明においては、炭素繊維の表面に
金属又は半金属の酸化物のコロイド溶液を浸漬等の方法
によって塗布する。It is preferable that the surface of these carbon fibers is previously oxidized by anodic oxidation or the like so that the coating layer of the present invention can be firmly fixed. At that time, the oxidation treatment may be extremely mild to such an extent that the performance of the carbon fiber itself is not deteriorated by the oxidation. In the present invention, a colloidal solution of a metal or metalloid oxide is applied to the surface of the carbon fiber by a method such as dipping.
【０００９】本発明の金属又は半金属の酸化物として
は、コロイドを形成し得るものであればよく、例えば、
アルミニウム、チタニウム、クロム、鉄、銅、ジルコニ
ウム、トリウム、或いは、ケイ素等の酸化物が挙げられ
る。特に、アルミニウム、ケイ素の酸化物が好適であ
る。これら金属又は半金属の酸化物のコロイド溶液は常
法に従い、例えば、加水分解等によって調製すればよ
い。その際、コロイド状態の安定化を計るために、酢
酸、塩酸等の酸や水酸化ナトリウム、アンモニア水等の
アルカリ、或いは塩化ナトリウム、塩化カリウム等の塩
類を適宜添加してもよい。The metal or semi-metal oxide of the present invention may be any as long as it can form a colloid.
Examples of the oxide include aluminum, titanium, chromium, iron, copper, zirconium, thorium, and silicon. Particularly, oxides of aluminum and silicon are suitable. The colloidal solution of the oxide of these metals or semimetals may be prepared by a conventional method, for example, by hydrolysis. At that time, in order to stabilize the colloidal state, an acid such as acetic acid or hydrochloric acid, an alkali such as sodium hydroxide or ammonia water, or a salt such as sodium chloride or potassium chloride may be appropriately added.
【００１０】本発明においては、金属又は半金属の酸化
物のコロイドの粒径が、５〜３００ｍμの範囲のものを
使用するのがマトリックスとの接着性の点で好適であ
る。かかる金属又は半金属の酸化物のコロイド溶液を炭
素繊維に塗布する方法としては、コロイド溶液の満たさ
れた槽内を連続的に炭素繊維を走行させる方法が、処理
の効率、均一塗布の点から好ましい。また、この際に、
コロイド溶液の満たされた槽に１０〜５０ＫＨｚ程度の
超音波を作用させておくと、例えば、炭素繊維を束状で
処理した場合にも繊維間の気泡等による処理むらの影響
を防ぐことができるので好ましい。In the present invention, it is preferable to use a colloid of a metal or semimetal oxide having a particle size in the range of 5 to 300 mμ from the viewpoint of adhesion to the matrix. As a method of applying the colloidal solution of the metal or semimetal oxide to the carbon fibers, a method of continuously running the carbon fibers in a tank filled with the colloidal solution is effective from the viewpoint of treatment efficiency and uniform application. preferable. Also, at this time,
When ultrasonic waves of about 10 to 50 KHz are applied to the tank filled with the colloidal solution, for example, even when the carbon fibers are processed in a bundle, it is possible to prevent the effect of uneven processing due to bubbles between the fibers. Therefore, it is preferable.
【００１１】コロイド溶液を塗布した炭素繊維は、適宜
ローラー等を通すなどして余分な溶液を除き、その後加
熱処理を施される。コロイド溶液の塗布は、加熱処理後
の被覆厚さとして、１μｍ以下（被覆量で５％以下）と
なるように行う。本発明の加熱処理によって、金属又は
半金属の酸化物のコロイドはゲルの状態に変換される。
本発明におては、通常、１００〜８００℃、好ましく
は、１００〜４００℃の温度で、０．５〜１０時間、好
ましくは、１〜５時間加熱処理される。その際、炭素繊
維を加熱炉内を連続的に走行させるのが処理効率、繊維
同士のからみ及び固着防止の点から好ましい。The carbon fiber coated with the colloidal solution is appropriately passed through a roller or the like to remove excess solution, and then subjected to heat treatment. The application of the colloidal solution is performed so that the coating thickness after the heat treatment is 1 μm or less (the coating amount is 5% or less). By the heat treatment of the present invention, the colloid of metal or metalloid oxide is converted into a gel state.
In the present invention, heat treatment is usually carried out at a temperature of 100 to 800 ° C, preferably 100 to 400 ° C for 0.5 to 10 hours, preferably 1 to 5 hours. At that time, it is preferable that the carbon fibers are continuously run in the heating furnace from the viewpoints of treatment efficiency, entanglement of fibers and prevention of sticking.
【００１２】あまり高温、長時間処理すると炭素繊維に
付着したゲルの被覆層が、炭素繊維との熱収縮の差異に
より剥離してしまうので、上記範囲で加熱処理するのが
よい。加熱処理は、約４００℃以下で行う場合は空気中
で行ってもよいが、それ以上の温度で処理する場合は炭
素繊維の酸化により性能劣化を防ぐために不活性雰囲気
下で行う。If the treatment is carried out at an excessively high temperature for a long time, the gel coating layer adhered to the carbon fibers will be peeled off due to the difference in thermal contraction with the carbon fibers. Therefore, it is preferable to perform the heat treatment within the above range. The heat treatment may be carried out in air when it is carried out at about 400 ° C. or lower, but when it is carried out at a temperature higher than that, it is carried out in an inert atmosphere in order to prevent performance deterioration due to oxidation of carbon fibers.
【００１３】以上のようにして得られる炭素繊維は、そ
の表面に凹凸を有する金属又は半金属の酸化物のゲルの
被覆層が形成されている。この被覆層の持つ活性及びそ
の凹凸の効果によりマトリックスとの接着性が改善さ
れ、より優れた性能の複合材料の補強繊維として使用す
ることができる。また、本発明の複合材におけるマトリ
ックスの例示としては、例えば、エポキシやポリアミド
等の樹脂、アルミニウム、マグネシウム等の金属、Ｓｉ
Ｃ、ＢＮ等のセラミック、フェノール樹脂やピッチ類に
由来する炭素等、好ましくは、樹脂及び金属が挙げられ
る。The carbon fiber obtained as described above has a coating layer of a metal or semimetal oxide gel having irregularities formed on the surface thereof. The activity of this coating layer and the effect of its unevenness improve the adhesiveness to the matrix, and it can be used as a reinforcing fiber of a composite material having more excellent performance. Examples of the matrix in the composite material of the present invention include resins such as epoxy and polyamide, metals such as aluminum and magnesium, and Si.
Ceramics such as C and BN, carbon derived from phenol resins and pitches, and the like, preferably resins and metals are mentioned.
【００１４】本発明の複合材は、前述の炭素繊維を、こ
れらマトリックス中、通常、３０〜７０ｖｏｌ ％の範
囲となるように使用し、常法に従い成型することによっ
て、得ることができる。The composite material of the present invention can be obtained by using the above-mentioned carbon fibers in these matrices so as to be in the range of usually 30 to 70% by volume and molding them according to a conventional method.
【００１５】[0015]
【発明の効果】本発明によれば、金属又は半金属のコロ
イド溶液を炭素繊維の表面に塗布し、加熱処理するとい
う簡便な方法でマトリクッスとの接着性が更に改善され
た補強繊維を得ることができ、かかる補強繊維を使用す
ることにより高特性の複合材を得ることができる。EFFECTS OF THE INVENTION According to the present invention, a reinforcing fiber having further improved adhesiveness with a matrix can be obtained by a simple method of applying a colloidal solution of metal or metalloid to the surface of carbon fiber and heat-treating it. By using such reinforcing fibers, it is possible to obtain a composite material having high characteristics.
【００１６】以下、本発明を実施例を用いて、より具体
的に説明するが、本発明はその要旨をこえない限り下記
の実施例に限定されるものではない。Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples unless it exceeds the gist.
【００１７】[0017]
【実施例】 実施例１ ２０００℃で焼成したピッチ系炭素繊維束（３０００フ
ィラメント）を０．０５ｗｔ％水酸化ナトリウム水溶液
中を連続的に走行させながら繊維束を陽極として処理量
１ｃ／ｇ−炭素繊維となるように電解酸化し、次いで、
脱塩水の洗浄槽を通過させて洗浄し、更に複数のローラ
ーを通過させて水切りを行った。Example 1 Pitch-based carbon fiber bundles (3000 filaments) fired at 2000 ° C. were continuously run in a 0.05 wt% sodium hydroxide aqueous solution while using the fiber bundles as an anode, and the treatment amount was 1 c / g-carbon. Electrolytically oxidize to form fibers, then
It was passed through a washing tank of demineralized water for washing, and further passed through a plurality of rollers for draining.
【００１８】引続き、この繊維束を４５ＫＨｚ、１００
Ｗの超音波を作用させているアルミナコロイド溶液（日
産化学社製、アルミナゾル−２００を１ｗｔ％となるよ
うに脱塩水にて希釈）の満たされた槽内を走行させ、次
いで、複数のローラーを通過させた後、ドラムに巻取っ
た。この一連の処理における通糸速度は５ｍ／時であ
り、アルミナコロイド溶液の槽における繊維束の滞留時
間は２分間であった。Subsequently, this fiber bundle was placed at 45 KHz and 100
It is run in a tank filled with an alumina colloidal solution (Nissan Chemical Co., Inc., alumina sol-200 diluted with demineralized water so as to be 1 wt%) in which ultrasonic waves of W are applied, and then, a plurality of rollers are run. After passing, it was wound on a drum. The threading speed in this series of treatments was 5 m / hour, and the residence time of the fiber bundle in the tank of the alumina colloid solution was 2 minutes.
【００１９】アルミナコロイド溶液を塗布した炭素繊維
束は、次いで、全長０．３ｍ、中心部最高温度２００℃
の炉内を０．４５ｍ／時の速度で走行させて加熱処理を
行った。得られた炭素繊維束は、処理前に比べて２．５
％の重量増加があり、又、走査型電子顕微鏡で観察した
ところ、炭素繊維の表面に平均で約０．５μの厚さの凹
凸のあるゲルの被覆層が確認された。The carbon fiber bundle coated with the alumina colloid solution has a total length of 0.3 m and a maximum temperature of 200 ° C. at the center.
Heat treatment was carried out by traveling in the furnace at a speed of 0.45 m / hour. The obtained carbon fiber bundle is 2.5 compared to before treatment.
%, And when observed with a scanning electron microscope, a gel coating layer having irregularities with an average thickness of about 0.5 μ was confirmed on the surface of the carbon fiber.
【００２０】この炭素繊維束を使用してエポキシ樹脂を
マトリックスとする繊維含有率５０％ん２×１０×１２
ｍｍの成型体（硬化条件；１８０℃、２時間）を常法に
従い作成し、３点曲げ試験法（スパン間１０ｍｍ、歪速
度２ｍｍ／ｍｍ）により層間せん断強度を求めた結果、
４点の試験片の平均値として９．６ｋｇ／ｍｍ2 であっ
た。Using this carbon fiber bundle, the fiber content of the epoxy resin as a matrix is 50% and 2 × 10 × 12.
mm molded body (curing condition; 180 ° C., 2 hours) was prepared according to a conventional method, and the interlaminar shear strength was determined by the 3-point bending test method (span interval 10 mm, strain rate 2 mm / mm).
The average value of the four test pieces was 9.6 kg / mm 2 .
【００２１】実施例２ 実施例１において、アルミナコロイド溶液の代わりに酸
化ケイ素コロイド溶液（日産化学社製、商標スノーテッ
クφを１ｗｔ％となるように脱塩水で希釈し、更に酢酸
でｐＨ４に調整）を使用する外は、実施例１と同様にし
てコロイド溶液を塗布し、加熱処理した。Example 2 In Example 1, instead of the alumina colloidal solution, a silicon oxide colloidal solution (Nissan Chemical Co., Ltd., trademark Snow Tech φ was diluted with demineralized water to 1 wt% and further adjusted to pH 4 with acetic acid. ) Was used and the colloidal solution was applied and heat treated in the same manner as in Example 1.
【００２２】得られた炭素繊維束は、処理前に比べて
１．８％の重量増加があり、又、その表面に平均で約
０．３μの厚さの凹凸のあるゲルの被覆層が確認され
た。この炭素繊維束を使用して実施例１と同様に成型体
を作成し、層間せん断強度を求めたところ、８．４ｋｇ
／ｍｍ2 であった。The obtained carbon fiber bundle had a weight increase of 1.8% as compared with that before the treatment, and a gel coating layer having an irregularity of about 0.3 μm on average was confirmed on the surface thereof. Was done. A molded body was prepared using this carbon fiber bundle in the same manner as in Example 1, and the interlaminar shear strength was determined to be 8.4 kg.
/ Mm 2 .
【００２３】比較例１ 実施例１において、アルミナコロイド溶液塗布を行わな
かった以外は、実施例１と同様にして補強炭素繊維を得
た。そして、実施例１と同様にして作成した複合材料の
層間せん断強度を求めたところ、４．２ｋｇ／ｍｍ2 で
あった。Comparative Example 1 A reinforced carbon fiber was obtained in the same manner as in Example 1 except that the application of the alumina colloid solution was not performed. Then, the interlaminar shear strength of the composite material produced in the same manner as in Example 1 was determined to be 4.2 kg / mm 2 .
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 // Ｄ０６Ｍ 101:40 Continuation of front page (51) Int.Cl. 6 Identification number Office reference number FI technical display location // D06M 101: 40
Claims (6)
において、該補強繊維が、表面に金属又は半金属の酸化
物のゲルの被覆層を有する炭素繊維であって、該被覆層
が炭素繊維表面に塗布された該酸化物のコロイド溶液を
加熱処理することによって形成されたものであることを
特徴とする複合材。1. A composite material comprising a reinforcing fiber and a matrix, wherein the reinforcing fiber is a carbon fiber having a coating layer of a metal or semi-metal oxide gel on the surface, the coating layer being on the surface of the carbon fiber. A composite material, which is formed by heat-treating the applied colloidal solution of the oxide.
許請求項１記載の複合材。2. The composite material according to claim 1, wherein the carbon fiber is a pitch-based carbon fiber.
ものである特許請求項１又は２記載の複合材。3. The composite material according to claim 1, wherein the surface of the carbon fiber is anodized.
径が、５〜３００ｍμである特許請求１乃至３のいずれ
か記載の複合材。4. The composite material according to claim 1, wherein the colloid of the metal or semimetal oxide has a particle size of 5 to 300 mμ.
が、アルミナ又は酸化ケイ素のコロイド溶液である特許
請求項１乃至４のいずれかに記載の複合材。5. The composite material according to claim 1, wherein the colloidal solution of a metal or metalloid oxide is a colloidal solution of alumina or silicon oxide.
る特許請求項１乃至５のいずれかに記載の複合材。6. The composite material according to claim 1, wherein the heat treatment temperature is 100 to 800 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20343994A JPH0830122B2 (en) | 1994-08-29 | 1994-08-29 | Composite material using carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20343994A JPH0830122B2 (en) | 1994-08-29 | 1994-08-29 | Composite material using carbon fiber |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61153875A Division JPH0791780B2 (en) | 1986-06-30 | 1986-06-30 | Carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07268111A true JPH07268111A (en) | 1995-10-17 |
| JPH0830122B2 JPH0830122B2 (en) | 1996-03-27 |
Family
ID=16474126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20343994A Expired - Fee Related JPH0830122B2 (en) | 1994-08-29 | 1994-08-29 | Composite material using carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0830122B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002180370A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Carbon fiber for metal oxide coating and method for producing the same |
| JP2002180372A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Metal oxide-coated carbon fiber and method for producing the same |
| JP2007107151A (en) * | 2005-10-17 | 2007-04-26 | Showa Denko Kk | Silica-coated carbon fiber |
| KR101428423B1 (en) * | 2013-11-15 | 2014-08-08 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
| KR101482452B1 (en) * | 2013-11-15 | 2015-01-14 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
| CN113881191A (en) * | 2021-11-17 | 2022-01-04 | 湖南东映碳材料科技有限公司 | Asphalt-based carbon fiber/resin-based composite material and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109322162A (en) * | 2018-11-14 | 2019-02-12 | 罗莱生活科技股份有限公司 | A kind of preparation process of multifunctional fabric |
-
1994
- 1994-08-29 JP JP20343994A patent/JPH0830122B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002180370A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Carbon fiber for metal oxide coating and method for producing the same |
| JP2002180372A (en) * | 2000-12-15 | 2002-06-26 | Toho Tenax Co Ltd | Metal oxide-coated carbon fiber and method for producing the same |
| JP2007107151A (en) * | 2005-10-17 | 2007-04-26 | Showa Denko Kk | Silica-coated carbon fiber |
| KR101428423B1 (en) * | 2013-11-15 | 2014-08-08 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
| KR101482452B1 (en) * | 2013-11-15 | 2015-01-14 | 주식회사 포스코 | Manufacturing method of carbon fiber reinforced thermoplastic composite and the composite manufactured by the same |
| CN113881191A (en) * | 2021-11-17 | 2022-01-04 | 湖南东映碳材料科技有限公司 | Asphalt-based carbon fiber/resin-based composite material and preparation method thereof |
| CN113881191B (en) * | 2021-11-17 | 2024-05-17 | 湖南东映碳材料科技股份有限公司 | Asphalt-based carbon fiber/resin-based composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0830122B2 (en) | 1996-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPS6153418B2 (en) | ||
| Katzman | Fibre coatings for the fabrication of graphite-reinforced magnesium composites | |
| JPS59187622A (en) | Graphite filament having high electrical conductivity and its preparation | |
| JPH07268111A (en) | Composite material using carbon fiber | |
| US4131697A (en) | Method of coating carbon filaments with silicon carbide | |
| JPH0791780B2 (en) | Carbon fiber | |
| CN106957510A (en) | A kind of titanium dioxide nano-rod is modified the preparation method of carbon cloth reinforced resin based composites | |
| CN118290821B (en) | A method for improving interface bonding and wear resistance of basalt fiber composite materials | |
| JP2664047B2 (en) | Method for producing carbon fiber reinforced carbon composite material | |
| US4737382A (en) | Carbide coatings for fabrication of carbon-fiber-reinforced metal matrix composites | |
| JP3755255B2 (en) | Carbon fiber and method for producing the same | |
| JPH0544154A (en) | Surface treatment of carbon fiber | |
| JP2001176333A (en) | Overhead transmission line | |
| CN113896551B (en) | Preparation method of alkaline earth metal reinforced continuous aluminum silicate ceramic fiber | |
| JPS6126737A (en) | Manufacture of carbon fiber reinforced metallic composite body | |
| US3876444A (en) | Method of treating high strength carbon fibers | |
| RU2714650C1 (en) | Method of hardening composite materials based on carbon fiber | |
| JPS63107862A (en) | Manufacturing method of carbon fiber reinforced carbon composite material | |
| JPS6228411A (en) | Production of pitch carbon fiber | |
| JPH02167859A (en) | Production of carbon fiber-reinforced carbon composite material | |
| JPH06148474A (en) | Heat resistant coated glass fiber | |
| CN108329649A (en) | A kind of preparation method of titanium dioxide-silane coupling agent cooperative reinforcing carbon cloth reinforced resin base frication material | |
| JPH07138070A (en) | Method for producing glassy carbon-coated carbonaceous material | |
| CN110453495B (en) | A kind of method for plating boron carbide on carbon fiber surface | |
| JP2736428B2 (en) | Manufacturing method of ultra-high elasticity graphite fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |