JPH025710B2 - - Google Patents
Info
- Publication number
- JPH025710B2 JPH025710B2 JP60292559A JP29255985A JPH025710B2 JP H025710 B2 JPH025710 B2 JP H025710B2 JP 60292559 A JP60292559 A JP 60292559A JP 29255985 A JP29255985 A JP 29255985A JP H025710 B2 JPH025710 B2 JP H025710B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon fiber
- composite material
- carbon composite
- phosphorus compound
- resin
- 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
- 229910052799 carbon Inorganic materials 0.000 claims description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 57
- 239000002131 composite material Substances 0.000 claims description 35
- 229920005989 resin Polymers 0.000 claims description 16
- 239000011347 resin Substances 0.000 claims description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 15
- 150000002903 organophosphorus compounds Chemical class 0.000 claims description 13
- 229920001187 thermosetting polymer Polymers 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000007849 furan resin Substances 0.000 claims description 2
- 229920001721 polyimide Polymers 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims 1
- 229920000647 polyepoxide Polymers 0.000 claims 1
- 239000009719 polyimide resin Substances 0.000 claims 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 11
- 239000004917 carbon fiber Substances 0.000 description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000000835 fiber Substances 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 238000010000 carbonizing Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- -1 phosphorus compound Chemical class 0.000 description 4
- 239000002783 friction material Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 150000001721 carbon Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229920003987 resole Polymers 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011825 aerospace material Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は炭素繊維強化炭素複合材料の製造法に
関するものである。更に詳しくは、宇宙航空用構
造材料、耐熱構造部材或はブレーキ摩擦材料に利
用可能な耐熱酸化性の優れた炭素繊維強化炭素複
合材料の製造法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing carbon fiber reinforced carbon composite materials. More specifically, the present invention relates to a method for producing a carbon fiber-reinforced carbon composite material that has excellent heat oxidation resistance and can be used as a structural material for aerospace, a heat-resistant structural member, or a brake friction material.
従来、炭素繊維強化炭素複合材料は、その耐熱
性、高強度、高弾性、耐薬品性及び軽量性故に宇
宙航空材料、耐熱構造材料等に広く利用されてい
る。しかしながら、炭素繊維強化炭素複合材料は
空気等の酸化性雰囲気中では、酸化消耗が著しく
その利用範囲で限られていた。
Conventionally, carbon fiber-reinforced carbon composite materials have been widely used as aerospace materials, heat-resistant structural materials, etc. due to their heat resistance, high strength, high elasticity, chemical resistance, and light weight. However, carbon fiber-reinforced carbon composite materials suffer from oxidative wear and tear in oxidizing atmospheres such as air, which limits their range of use.
この耐熱酸化性を改良するために、リン酸或は
有機リン化合物を炭素繊維強化炭素複合材料に含
浸或は塗布することが行われていた（特開昭56−
16575号公報、米国特許第2868672号明細書）。 In order to improve this thermal oxidation resistance, carbon fiber-reinforced carbon composite materials have been impregnated or coated with phosphoric acid or organic phosphorus compounds (Japanese Patent Application Laid-Open No. 1983-1999).
16575, U.S. Pat. No. 2,868,672).
しかし、このリン酸等による処理では、炭素繊
維強化炭素複合材料がポーラスなために処理液が
非処理面に浸透して非処理面を汚染し、摩擦材等
においては、その摩擦特性を劣化させることがあ
り、摩擦材の耐熱酸化処理としては適当ではなか
つた。 However, in this treatment with phosphoric acid, etc., since the carbon fiber-reinforced carbon composite material is porous, the treatment liquid penetrates into the untreated surface and contaminates the untreated surface, causing the friction properties of friction materials to deteriorate. Therefore, it was not suitable as a heat-resistant oxidation treatment for friction materials.
本発明の目的は、炭素繊維強化炭素複合材料の
耐熱酸化性を改良するために、これにリン化合物
を付与する際、炭素繊維強化炭素複合材料の内部
への浸透を抑え、非処理部を汚染することなく、
耐熱酸化処理を行うことにある。
The purpose of the present invention is to suppress the penetration into the interior of the carbon fiber-reinforced carbon composite material and contaminate untreated parts when adding a phosphorus compound to the carbon fiber-reinforced carbon composite material in order to improve its thermal oxidation resistance. without doing,
The purpose is to perform heat-resistant oxidation treatment.
すなわち、本発明は、炭素繊維強化炭素複合材
料の外表面の一部或は全部に熱硬化性樹脂と有機
リン化合物の混合物を付与した後、該混合物を硬
化及び炭素化処理することを特徴とする耐熱酸化
性に優れた炭素繊維強化炭素複合材料の製造法で
ある。
That is, the present invention is characterized by applying a mixture of a thermosetting resin and an organic phosphorus compound to part or all of the outer surface of a carbon fiber-reinforced carbon composite material, and then curing and carbonizing the mixture. This is a method for producing carbon fiber-reinforced carbon composite materials with excellent thermal oxidation resistance.
本発明において炭素繊維強化炭素複合材料の強
化材とする炭素繊維は、レーヨン、ポリアクリロ
ニトリル、ピツチ等の繊維を夫々既知の方法で炭
素化した繊維、或は、それらを更に高温で熱処理
した黒鉛化繊維である。 In the present invention, the carbon fibers used as the reinforcing material of the carbon fiber-reinforced carbon composite material are fibers obtained by carbonizing fibers such as rayon, polyacrylonitrile, and pitucci by known methods, or graphitized fibers obtained by further heat-treating them at high temperatures. It is a fiber.
本発明における炭素繊維強化炭素複合材料の製
造は、炭素繊維にフエノール、フラン或はエポキ
シ等の熱硬化性樹脂を含浸し、所望の形状に成形
後、不活性雰囲気中で炭素化、或は必要により黒
鉛化処理して炭素繊維強化炭素複合材料とする。
又、必要により熱硬化性樹脂或はピツチ等を該炭
素繊維強化炭素複合材料に含浸させた後、炭素化
或は黒鉛化処理する、いわゆる緻密化処理を、所
要の機械的強度が得られるまで繰り返してもよ
い。この緻密化処理は高温に保持した該炭素繊維
強化炭素複合材料或は所定の形状に保持した炭素
繊維や黒鉛繊維に炭化水素ガスを加熱分解して炭
素を蒸着する、いわゆるケミカル・ベーパー・デ
イポジシヨン法（CVD法）によつて行つてもよ
い。 The production of carbon fiber-reinforced carbon composite materials in the present invention involves impregnating carbon fibers with a thermosetting resin such as phenol, furan, or epoxy, molding them into a desired shape, and then carbonizing them in an inert atmosphere, or by carbonizing them as necessary. The material is graphitized and made into a carbon fiber reinforced carbon composite material.
In addition, if necessary, after impregnating the carbon fiber reinforced carbon composite material with thermosetting resin or pitch, carbonization or graphitization treatment, so-called densification treatment, is performed until the required mechanical strength is obtained. May be repeated. This densification treatment is a so-called chemical vapor deposition method in which carbon is deposited by thermally decomposing hydrocarbon gas onto the carbon fiber-reinforced carbon composite material held at high temperature or carbon fibers or graphite fibers held in a predetermined shape. (CVD method).
又、本発明において使用される炭素繊維強化炭
素複合材料は、その製造工程において800〜3000
℃の熱処理を受けていることが望ましい。 In addition, the carbon fiber reinforced carbon composite material used in the present invention has a
It is desirable that the material has undergone heat treatment at ℃.
本発明において使用される有機リン化合物は、
リン酸或は亜リン酸のモノ、ジ或はトリアルキル
エステルが好ましい。又、アルキルホスフイン、
アルキルハロゲンホスフイン、酸化アルキルホス
フイン、アリールホスフイン、アリールリン酸、
アリール亜リン酸等も使用できる。 The organic phosphorus compound used in the present invention is
Mono-, di- or trialkyl esters of phosphoric acid or phosphorous acid are preferred. Also, alkylphosphine,
Alkylhalogenphosphine, alkylphosphine oxide, arylphosphine, aryl phosphoric acid,
Aryl phosphorous acids and the like can also be used.
本発明において有機リン化合物と混合して使用
される熱硬化性樹脂は、フエノール、フラン、エ
ポキシ、ポリイミド等の熱硬化性樹脂である。 The thermosetting resin used in combination with the organic phosphorus compound in the present invention is a thermosetting resin such as phenol, furan, epoxy, or polyimide.
熱硬化性樹脂と有機リン化合物との混合比は
１：0.2ないし１：1.4であることが望ましく、有
機リン化合物が0.2より小であると耐熱酸化性が
不足し、1.4より大であると硬化が困難になる。
有機リン化合物と熱硬化性樹脂が相溶性のある組
合せからなるほうが混合及び付与時に処理しやす
い。又、必要により溶剤或は硬化剤等を混合して
もよい。該混合物の粘度が低い場合には硬化剤の
添加、或は／及び加熱等の処理により粘度を上げ
ておくほうがよい。又、その後の硬化時におい
て、付与した面以外を汚染させないために硬化時
において著しく粘度の下がる樹脂は好ましくな
い。 The mixing ratio of the thermosetting resin and the organic phosphorus compound is preferably 1:0.2 to 1:1.4. If the ratio of the organic phosphorus compound is less than 0.2, thermal oxidation resistance will be insufficient, and if it is more than 1.4, hardening will occur. becomes difficult.
Compatible combinations of organic phosphorus compounds and thermosetting resins are easier to process during mixing and application. Further, a solvent, a curing agent, etc. may be mixed if necessary. If the viscosity of the mixture is low, it is better to increase the viscosity by adding a curing agent and/or by heating or the like. Furthermore, in order to avoid contaminating surfaces other than those to which it is applied during subsequent curing, resins whose viscosity decreases significantly during curing are not preferred.
炭素繊維強化炭素複合材料に対する有機リン化
合物と熱硬化性樹脂の混合物の付与は、該混合物
を炭素繊維強化炭素複合材料の表面の処理を必要
とする部分に対して行われる。次いで、加熱して
該混合物を硬化させ、更に窒素等の不活性雰囲気
中で500〜1500℃に加熱して混合物中の有機物を
炭素化させる。 The mixture of an organic phosphorus compound and a thermosetting resin is applied to the carbon fiber-reinforced carbon composite material on a portion of the surface of the carbon fiber-reinforced carbon composite material that requires treatment. Next, the mixture is cured by heating, and further heated to 500 to 1500° C. in an inert atmosphere such as nitrogen to carbonize the organic matter in the mixture.
本発明によると、有機リン化合物と熱硬化性樹
脂との併用によつて、炭素繊維強化炭素複合材料
の非処理部でのリン化合物による汚染を防止し、
しかも炭素繊維強化炭素複合材料の表面の内、必
要とする部分に耐熱酸化性の優れた層を形成せし
めることができる。
According to the present invention, by using an organic phosphorus compound and a thermosetting resin in combination, contamination by the phosphorus compound in the untreated portion of the carbon fiber reinforced carbon composite material is prevented,
Moreover, a layer with excellent thermal oxidation resistance can be formed on the surface of the carbon fiber reinforced carbon composite material at a necessary portion.
実施例
東邦レーヨン(株)製ベスフアイト織物3101にレゾ
ール系フエノール樹脂を含浸して樹脂含有率38％
のプリプレグを作成し、積層後、加熱加圧硬化さ
せて、繊維体積含有率50％の炭素繊維強化炭素複
合材料（CFRP）とした。次いで、該複合材料を
窒素雰囲気中1000℃で炭素化した後、ピツチ含
浸・再炭素化の緻密化工程及び不活性雰囲気中
2400℃での処理を繰り返して嵩密度1.6ｇ／cm3の
炭素繊維強化炭素複合材料（CFRC）を得た。
Example: Besuphite fabric 3101 manufactured by Toho Rayon Co., Ltd. is impregnated with resol-based phenolic resin to obtain a resin content of 38%.
prepreg was created, laminated, and cured under heat and pressure to create a carbon fiber-reinforced carbon composite material (CFRP) with a fiber volume content of 50%. Next, the composite material was carbonized at 1000°C in a nitrogen atmosphere, followed by a densification process of pitch impregnation and recarbonization, and an inert atmosphere.
The treatment at 2400°C was repeated to obtain a carbon fiber reinforced carbon composite material (CFRC) with a bulk density of 1.6 g/cm 3 .
この炭素繊維強化炭素複合材料よりブレーキテ
スト用試料を切りだし、ダイナモメータにより動
摩擦特性を吸収エネルギー300Kgｆ・ｍ／cm2、初
速度30ｍ／sec、押付圧力10Kgｆ／cm2で測定した
ところ、摩擦係数0.3で安定していたが、摩耗量
は８×10-3mm／回／面であつた。 A brake test sample was cut from this carbon fiber-reinforced carbon composite material, and its dynamic friction characteristics were measured using a dynamometer at an absorbed energy of 300 Kgf・m/cm 2 , an initial velocity of 30 m/sec, and a pressing pressure of 10 Kgf/cm 2 . It was stable at 0.3, but the amount of wear was 8 x 10 -3 mm/time/surface.
該炭素繊維強化炭素複合材料の外表面の一部に
フラン樹脂とリン酸トリ−ｎ−ブチルの混合物
（重量比１：１）を塗布し、170℃にて３時間加熱
硬化させた。次に、不活性雰囲気中1000℃で処理
して本発明の炭素繊維強化炭素複合材料を得た。 A mixture of furan resin and tri-n-butyl phosphate (weight ratio 1:1) was applied to a part of the outer surface of the carbon fiber-reinforced carbon composite material and cured by heating at 170°C for 3 hours. Next, the carbon fiber-reinforced carbon composite material of the present invention was obtained by processing at 1000° C. in an inert atmosphere.
このようにして得られた炭素繊維強化炭素複合
材料の諸特性は下記の通りである。 The properties of the carbon fiber-reinforced carbon composite material thus obtained are as follows.
（リンの付着状況）
前記混合物を塗布した外表面、塗布しない外表
面及び切削により塗布した面の１mm下の面を
EDXA（Energy Diffractive Ｘ−ray
Analysis：Philips社製装置）により、リンの付
着状況を調べたところ、処理した外表面以外では
リンは検出されなかつた。(Status of adhesion of phosphorus) The outer surface to which the mixture was applied, the outer surface to which it was not applied, and the surface 1 mm below the surface to which it was applied by cutting.
EDXA (Energy Diffractive X-ray
Analysis: When the adhesion status of phosphorus was investigated using a Philips device, no phosphorus was detected on any areas other than the treated outer surface.
（耐熱酸化性）
前記混合物を塗布した外表面及び塗布しない外
表面より約40mgの試料を、炭素繊維強化炭素複合
材料から切りだし、TGA（Thermo Gravimetric
Analysis）にて昇温速度10℃／min、空気流量
100ml／minで測定したところ、重量減少10％時
の温度は塗布面の方が約50℃高かつた。(Thermal oxidation resistance) Approximately 40 mg of samples were cut from the carbon fiber-reinforced carbon composite material from the outer surface coated with the above mixture and the outer surface not coated.
Analysis), heating rate 10℃/min, air flow rate
When measured at 100ml/min, the temperature at 10% weight loss was approximately 50°C higher on the coated surface.
（動摩擦特性）
前記混合物を塗布した面が非摺動面になるよう
にブレーキテスト用試料を、炭素繊維強化炭素複
合材料から切りだし、ダイナモメータにより動摩
擦特性を測定した。吸収エネルギー300Kgｆ・
ｍ／cm2、初速度30ｍ／sec、押付圧力10Kgｆ／cm2
で測定したところ、摩擦係数0.3で安定しており、
摩耗量10-3mm／回／面であり、摩擦特性は非常に
良好であつた。(Dynamic Frictional Characteristics) A brake test sample was cut out from a carbon fiber-reinforced carbon composite material so that the surface coated with the mixture was a non-sliding surface, and its dynamic frictional characteristics were measured using a dynamometer. Absorbed energy 300Kgf・
m/cm 2 , initial speed 30m/sec, pressing pressure 10Kgf/cm 2
When measured, the friction coefficient was stable at 0.3.
The amount of wear was 10 -3 mm/time/surface, and the friction characteristics were very good.
比較例
東邦レーヨン(株)製ベスフアイト織物3101にレゾ
ール系フエノール樹脂を含浸して樹脂含有率38％
のプリプレグを作成し、積層後、加熱加圧硬化さ
せて、繊維体積含有率50％の炭素繊維強化樹脂複
合材料（CFRP）を得た。該複合材料を窒素雰囲
気中1000℃で炭素化した後、ピツチ含浸・再炭素
化の緻密化工程及び不活性雰囲気中2400℃での処
理を繰り返して嵩密度1.6ｇ／cm3の炭素繊維強化
炭素複合材料（CFRC）を得た。Comparative example: Besuphite fabric 3101 manufactured by Toho Rayon Co., Ltd. is impregnated with resol-based phenolic resin, resulting in a resin content of 38%.
prepreg was created, laminated, and cured under heat and pressure to obtain a carbon fiber reinforced resin composite material (CFRP) with a fiber volume content of 50%. After carbonizing the composite material at 1000°C in a nitrogen atmosphere, the densification process of pitch impregnation and recarbonization and treatment at 2400°C in an inert atmosphere were repeated to obtain carbon fiber-reinforced carbon with a bulk density of 1.6 g/ cm3. A composite material (CFRC) was obtained.
この炭素繊維強化炭素複合材料に10重量％のリ
ン酸水溶液を外表面の一部に塗布した後、不活性
雰囲気中1000mmで処理した。リン酸を塗布した外
表面、塗布しない外表面及び切削により塗布した
面の１mm下の面をEDXAにより、リンの付着状
況を調べたところ、全ての面でリンが検出され
た。該複合材料よりリン酸を塗布した面が非摺動
面になるようにブレーキテスト用試料を切りだ
し、実施例と同一の条件でダイナモメータにより
動摩擦特性を測定したところ、摩擦係数は0.02〜
0.2で不安定であつた。 After applying a 10% by weight aqueous phosphoric acid solution to a part of the outer surface of this carbon fiber-reinforced carbon composite material, it was treated at 1000 mm in an inert atmosphere. When the state of phosphorus adhesion was examined using EDXA on the outer surface coated with phosphoric acid, the outer surface without coating, and the surface 1 mm below the surface coated by cutting, phosphorus was detected on all surfaces. A brake test sample was cut from the composite material so that the surface coated with phosphoric acid was a non-sliding surface, and the dynamic friction characteristics were measured using a dynamometer under the same conditions as in the example, and the friction coefficient was 0.02 ~
It was unstable at 0.2.
Claims (1)
は全部に熱硬化性樹脂と有機リン化合物の混合物
を付与した後、該混合物を硬化及び炭素化処理す
ることを特徴とする耐熱酸化性に優れた炭素繊維
強化炭素複合材料の製造法。 ２ 有機リン化合物がリン酸或は亜リン酸のモ
ノ、ジ或はトリアルキルエステルである特許請求
の範囲１記載の製造法。 ３ 熱硬化性樹脂と有機リン化合物の混合比が
１：0.2ないし１：1.4である特許請求の範囲１記
載の製造法。 ４ 熱硬化性樹脂がフラン樹脂、フエノール樹
脂、エポキシ樹脂、ポリイミド樹脂である特許請
求の範囲１記載の製造法。 ５ 熱硬化性樹脂と有機リン化合物が互いに相溶
性のある組合せからなる特許請求の範囲１記載の
製造法。[Claims] 1. A mixture of a thermosetting resin and an organic phosphorus compound is applied to part or all of the outer surface of a carbon fiber-reinforced carbon composite material, and then the mixture is cured and carbonized. A method for producing carbon fiber-reinforced carbon composite materials with excellent heat and oxidation resistance. 2. The production method according to claim 1, wherein the organic phosphorus compound is a mono-, di-, or trialkyl ester of phosphoric acid or phosphorous acid. 3. The manufacturing method according to claim 1, wherein the mixing ratio of the thermosetting resin and the organic phosphorus compound is 1:0.2 to 1:1.4. 4. The manufacturing method according to claim 1, wherein the thermosetting resin is a furan resin, a phenol resin, an epoxy resin, or a polyimide resin. 5. The manufacturing method according to claim 1, wherein the thermosetting resin and the organic phosphorus compound are a mutually compatible combination.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60292559A JPS62153164A (en) | 1985-12-27 | 1985-12-27 | Manufacture of carbon fiber reinforced carbon composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60292559A JPS62153164A (en) | 1985-12-27 | 1985-12-27 | Manufacture of carbon fiber reinforced carbon composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62153164A JPS62153164A (en) | 1987-07-08 |
| JPH025710B2 true JPH025710B2 (en) | 1990-02-05 |
Family
ID=17783332
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60292559A Granted JPS62153164A (en) | 1985-12-27 | 1985-12-27 | Manufacture of carbon fiber reinforced carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62153164A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6126002B2 (en) * | 2011-06-30 | 2017-05-10 | エドワーズ株式会社 | Manufacturing method of cylindrical body and manufacturing method of vacuum pump |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2868672A (en) * | 1956-03-27 | 1959-01-13 | Union Carbide Corp | Oxidation resistant carbon and graphite bodies |
| JPS5616575A (en) * | 1979-07-18 | 1981-02-17 | Toho Rayon Co Ltd | Friction material and its preparation |
| JPS5617311A (en) * | 1979-07-20 | 1981-02-19 | Hitachi Cable Ltd | Manufacture of image guide |
-
1985
- 1985-12-27 JP JP60292559A patent/JPS62153164A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2868672A (en) * | 1956-03-27 | 1959-01-13 | Union Carbide Corp | Oxidation resistant carbon and graphite bodies |
| JPS5616575A (en) * | 1979-07-18 | 1981-02-17 | Toho Rayon Co Ltd | Friction material and its preparation |
| JPS5617311A (en) * | 1979-07-20 | 1981-02-19 | Hitachi Cable Ltd | Manufacture of image guide |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62153164A (en) | 1987-07-08 |
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