JPH0345568A - Carbon fiber reinforced composite material - Google Patents
Carbon fiber reinforced composite materialInfo
- Publication number
- JPH0345568A JPH0345568A JP1182314A JP18231489A JPH0345568A JP H0345568 A JPH0345568 A JP H0345568A JP 1182314 A JP1182314 A JP 1182314A JP 18231489 A JP18231489 A JP 18231489A JP H0345568 A JPH0345568 A JP H0345568A
- Authority
- JP
- Japan
- Prior art keywords
- composite material
- oxidation
- carbon fiber
- carbon
- matrix
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 18
- 239000004917 carbon fiber Substances 0.000 title claims description 18
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title description 16
- 239000011208 reinforced composite material Substances 0.000 title description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 27
- 239000000919 ceramic Substances 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 13
- 239000012779 reinforcing material Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000003733 fiber-reinforced composite Substances 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 239000000843 powder Substances 0.000 abstract description 5
- 238000001962 electrophoresis Methods 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 4
- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 238000005245 sintering Methods 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 abstract 3
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 abstract 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000005452 bending Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000011812 mixed powder Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 239000002759 woven fabric Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000013001 point bending Methods 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
Landscapes
- Ceramic Products (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、耐酸化性に優れた炭素繊維強化複合材料に関
する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a carbon fiber reinforced composite material with excellent oxidation resistance.
炭素のマ） ＩＪラックス中強化材として炭素繊維を含
む炭素繊維強化炭素複合材料（所謂Ｃ／Ｃフンポジット
）は、１００ＯＣ”以上の高温下で優れた比強度及び比
剛性を示すことから、宇宙往還機等の断熱材料への適用
が検討されている。Carbon fiber-reinforced carbon composite material (so-called C/C composite), which contains carbon fiber as a reinforcing material in IJ Lux, exhibits excellent specific strength and specific stiffness at high temperatures of 100 OC" or higher, and is therefore used for space travel. Application to insulation materials for machines, etc. is being considered.
しかしながら、炭素繊維強化炭素複合材料は、炭素を原
料としているため高温での耐酸化性に欠ける欠点がある
。この欠点を補うため、高温下で優れた耐酸化性を有す
るセラミックスを化学蒸着法等により表面被覆した被覆
複合材料が提案されている。However, carbon fiber-reinforced carbon composite materials have the drawback of lacking oxidation resistance at high temperatures because they use carbon as a raw material. In order to compensate for this drawback, a coated composite material has been proposed in which the surface is coated with a ceramic material having excellent oxidation resistance at high temperatures by chemical vapor deposition or the like.
ところが、このような被覆複合材料はマトリックスであ
る炭素と表面部分のセラミックスとの熱膨張係数に差が
あるため、加熱と冷却の熱サイクル下で両者の界面に熱
応力による亀裂が発生して、セラミックス被覆が剥離し
たり、強度が著しく低下するという欠点があった。However, in such coated composite materials, there is a difference in the coefficient of thermal expansion between the carbon matrix and the ceramic surface, so cracks occur at the interface between the two due to thermal stress during thermal cycles of heating and cooling. There were drawbacks such as the ceramic coating peeling off and the strength significantly decreasing.
又、マトリックスとして炭素の代りにセラミックスを用
いた炭素繊維強化セラミックス複合材料も検討されてい
るが、耐酸化性に優れる反面、曲げ強度が著しく低下す
る欠点があった。Also, carbon fiber reinforced ceramic composite materials using ceramics instead of carbon as a matrix have been considered, but although they have excellent oxidation resistance, they have the drawback of significantly lower bending strength.
本発明はかかる従来の事情に鑑み、優れた耐酸化性、耐
熱衝撃性及び強度特性を兼ね備えた炭素繊維強化複合材
料を提供することを目的とする。In view of the conventional circumstances, the present invention aims to provide a carbon fiber reinforced composite material that has excellent oxidation resistance, thermal shock resistance, and strength characteristics.
（課題を解決するための手段）
上記目的を達成するため、本発明の炭素繊維強化複合材
料は、炭素とセラミックスの複合物からなる板状のマト
リックスと、マトリックス中に強化材として含まれる炭
素繊維とからなり、当該マトリックスの両側の表面部分
が耐酸化性セラミックスからなり、両側の表面部分に対
する中心部分が炭素であって、中心部分から両側の表面
部分までの組成が炭素から耐酸化性セラミックスまでほ
ぼ連続的に変化していることを特徴とする。(Means for Solving the Problems) In order to achieve the above object, the carbon fiber reinforced composite material of the present invention comprises a plate-shaped matrix made of a composite of carbon and ceramics, and carbon fibers contained in the matrix as a reinforcing material. The surface portions on both sides of the matrix are made of oxidation-resistant ceramics, the center portions of the matrix on both sides are carbon, and the composition from the center portion to the surface portions on both sides ranges from carbon to oxidation-resistant ceramics. It is characterized by an almost continuous change.
本発明の炭素繊維強化複合材料では、マ） ＩＪラック
ス体が炭素と耐酸化性セラミックスとの複合した組成で
、しかも中心部分（炭素）から両側の表面部分（耐酸化
性セラミックス）までほぼ連続的に変化した傾斜組成に
なっている。In the carbon fiber reinforced composite material of the present invention, the IJ lux body has a composite composition of carbon and oxidation-resistant ceramics, and is almost continuous from the center portion (carbon) to the surface portions on both sides (oxidation-resistant ceramics). It has a gradient composition that has changed.
従って、外部に露出するマ） ＩＪラックス両側の表面
部分を構成する耐酸化性セラミックスが優れた耐酸化性
を付与し、同時にマ） リツクスの中心部分は炭素であ
るため優れた強度特性を示す。しかも、中心部分と両側
の表面部分の間は炭素から耐酸化性セラミックスまでほ
ぼ連続的に変化した傾斜組成となっているので、組成の
傾斜に伴なってマ） ＩＪラックス熱膨張係数が連続的
に変化し、熱サイクル下での熱応力の発生が緩和され、
耐熱衝撃性を改善向上させることが出来る。Therefore, the oxidation-resistant ceramics constituting the surface portions on both sides of the matrix IJ lux exposed to the outside provide excellent oxidation resistance, and at the same time, since the central portion of the matrix is carbon, it exhibits excellent strength characteristics. Moreover, between the center part and the surface parts on both sides, there is a gradient composition that changes almost continuously from carbon to oxidation-resistant ceramics, so as the composition gradient increases, the IJ Lux thermal expansion coefficient is continuous. , the occurrence of thermal stress under thermal cycles is alleviated,
Thermal shock resistance can be improved.
耐酸化性セラミックスは、耐熱性及び耐酸化性に優れた
炭化珪素（Ｓｉｎ） 、窒化珪素（ＳｉＮ）、炭化チタ
ン（ＴｉＣ）又は窒化硼素（ＥＮ）等が好ましい。The oxidation-resistant ceramics are preferably silicon carbide (Sin), silicon nitride (SiN), titanium carbide (TiC), or boron nitride (EN), which have excellent heat resistance and oxidation resistance.
（実施例）
実施例１
マトリックス成分として、平均粒径２μｍの炭素粉末と
、：３１Ｃ粉末を微量のＡｌＯ粉末と混合し、ＳｉＣ／
（Ｓｉ（１！＋Ｏ）を０１２０．４０．６０．８０．１
００ ｍｏ１％とした各混合粉末を準備した。各混合粉
末をアクリルアマイド系樹脂とよく混練し、電気泳動用
の浴液に夫々分散させた。これらの各浴液中に、陰極と
してＰＡＮ系炭素炭素繊維織布び陽極として炭素板を浸
漬し、よく攪拌しながら約２００ Ｖの電圧を印加して
１０分間通電した。電気泳動により各混合粉末粒子が炭
素繊維織布上に析出し、マ） ＩＪツクス戊成分ある上
記各ｓｔｃ／ ＜ｓｉａ＋ｃ ）組成の混合粉末と強化
材となる炭素繊維織布とから構成された複合体が得られ
た。(Example) Example 1 As matrix components, carbon powder with an average particle size of 2 μm and :31C powder were mixed with a trace amount of AlO powder, and SiC/
(Si(1!+O)0120.40.60.80.1
Each mixed powder having a concentration of 0.00 mo1% was prepared. Each mixed powder was thoroughly kneaded with an acrylamide resin and dispersed in a bath liquid for electrophoresis. A PAN-based carbon fiber woven fabric as a cathode and a carbon plate as an anode were immersed in each of these bath solutions, and while stirring well, a voltage of about 200 V was applied and electricity was applied for 10 minutes. By electrophoresis, each mixed powder particle is precipitated on a carbon fiber woven fabric, and a composite composed of a mixed powder having the above-mentioned stc/<sia+c) composition and a carbon fiber woven fabric serving as a reinforcing material is formed. I got a body.
次に、得られた各複合体を、マトリックス成分のＳｉｎ
／ （ＳｉＯ＋Ｃ）組成に基ずき第１表の如く組合せて
１１枚ずつ積層し、１００Ｃ’で一時間乾燥後、更に５
００Ｃで三時間加熱して揮発物を除去した。Next, each of the obtained composites was mixed with the matrix component Sin
/ (SiO+C) Based on the composition, 11 sheets were laminated in combination as shown in Table 1, and after drying at 100C' for 1 hour,
The volatiles were removed by heating at 00C for 3 hours.
この積層物を２０００ Ｃ’で二時間２００ ｋＶｆ−
♂の圧力で加圧焼結し、夫々厚さ３Ｎの炭素繊維強化複
合材料を得た。This laminate was heated at 2000 C' for 2 hours at 200 kVf-
Pressure sintering was performed at a pressure of ♂ to obtain carbon fiber reinforced composite materials each having a thickness of 3N.
第 １ 表
試料 積層順のマ）ＩＪツクス戊成分組成ＳｉＯｍｏ
１％）株 １００−８０−６０−４０−２０−０ （
０１００） −２０−４０−６０−８０−Ｚｏ。Table 1 Sample Lamination order Ma) IJTxX component composition SiOmo
1%) stock 100-80-60-40-20-0 (
0100) -20-40-60-80-Zo.
２ １００−１００−０−０−０−０−０−０−０
−１００−１００３ 全でＳｉＯ１００
４全で ｃ ｏ（ａｚｏｏ）
（注）※印は本発明例を示す（以下同じ）。2 100-100-0-0-0-0-0-0-0
-100-1003 SiO100 in total 4 in total co(azoo) (Note) *marks indicate examples of the present invention (the same applies below).
得られた各炭素繊維強化複合材料について、以下の耐酸
化試験と曲げ試験を行なった。耐酸化試験は、２５Ｘ２
５Ｘ３ｍｌＮの試料（四側面は大気と非接触）を大気中
で１５００ （’にて一時間加熱し、加熱前後の重量か
ら酸化による重量減少を求め、耐酸化性を評価した。又
、曲げ試験は４０Ｘ４Ｘ３ｆｉ の試料を３点曲げ試験
により行なった。The following oxidation resistance test and bending test were conducted on each of the obtained carbon fiber reinforced composite materials. Oxidation resistance test is 25X2
A 5 x 3 mlN sample (four sides not in contact with the atmosphere) was heated in the atmosphere at 1500°C for one hour, and the weight loss due to oxidation was determined from the weight before and after heating to evaluate the oxidation resistance. A 40X4X3fi sample was subjected to a three-point bending test.
結果を第２表に示した。The results are shown in Table 2.
第 ２ 表
本発明例の炭素繊維強化複合材料は、耐酸化性及び曲げ
強度とも優れていることが判る。Table 2 It can be seen that the carbon fiber reinforced composite materials of the examples of the present invention are excellent in both oxidation resistance and bending strength.
実施例２
実施例１と同様に作成した試料を、予め１３００Ｃに保
った炉内に入れて急加熱し、この温度に５分間保持した
後、液体窒素に投入して急冷するという熱サイクルを三
回繰り返し、その後実施例１と同様に曲げ強度を測定し
た。Example 2 A sample prepared in the same manner as in Example 1 was placed in a furnace previously maintained at 1300C, heated rapidly, held at this temperature for 5 minutes, and then placed in liquid nitrogen for rapid cooling. This was repeated twice, and then the bending strength was measured in the same manner as in Example 1.
上記熱サイクル後の曲げ強度は、本発明例の試料１が２
１１、試料２がｌＯ４、試料３が１０２、試料４が２１
２ ＭＰａであり、マトリックスが０−８ｉ（！無傾斜
組成の試料２は熱亀裂により強度が極度に低下したこと
が判る。The bending strength after the above thermal cycle was 2 for Sample 1 of the present invention example.
11, sample 2 is lO4, sample 3 is 102, sample 4 is 21
2 MPa, and the matrix was 0-8i (!) It can be seen that the strength of sample 2 with an ungraded composition was extremely reduced due to thermal cracking.
実施例３
セラミックスとしてＴｔＣを用いた以外は実施例１と同
様の方法により、積層順によるＴｉＯとＣのマ） ＩＪ
ツクス成分組組成第３表のようにした炭素繊維強化複合
材料を製造した。Example 3 The same method as Example 1 was used except that TtC was used as the ceramic, and TiO and C were stacked in the order of lamination.
A carbon fiber reinforced composite material having the composition shown in Table 3 was produced.
第 ３ 表
５※
１００−８０−６０−４０−２０−０ （ＯＺｏｏ）−
２０−４０−６０−８０−１００６１００−１００−０
−０−０−０−０−０−０−１００−１００７全てＴｉ
Ｏ１００
次に１
各試料を耐酸化試験用の２５Ｘ２５Ｘ３ｍ１１１Ｋ と
曲げ試験用の４０Ｘ４Ｘ３−に切断し、予め１０００
Ｃ’に保った炉内に入れて急加熱し、この温度に１０時
間保持した後、液体窒素に投入して急冷した。3rd Table 5* 100-80-60-40-20-0 (OZoo)-
20-40-60-80-1006100-100-0
-0-0-0-0-0-0-100-1007 All Ti
O100 Next, each sample was cut into 25X25X3m111K for oxidation resistance test and 40X4X3- for bending test.
It was placed in a furnace maintained at C' and rapidly heated, held at this temperature for 10 hours, and then placed in liquid nitrogen to be rapidly cooled.
その後、各試料について酸化重量減少と３点曲げ強度を
測定し、結果を第４表に示した。Thereafter, the oxidation weight loss and three-point bending strength of each sample were measured, and the results are shown in Table 4.
第 ４ 表
〔発明の効果〕
本発明によれば、比強度及び比剛性に優れると同時に、
耐熱性、耐酸化性及び耐熱衝撃性を兼ね備えた炭素繊維
強化複合材料を提供することができる。Table 4 [Effects of the Invention] According to the present invention, the specific strength and specific stiffness are excellent, and at the same time,
A carbon fiber reinforced composite material that has heat resistance, oxidation resistance, and thermal shock resistance can be provided.
この炭素繊維強化複合材料は高温での断熱性に優れ、超
音速航空機や宇宙往還機などの機体壁用断熱材として特
に有効である。This carbon fiber-reinforced composite material has excellent heat insulation properties at high temperatures and is particularly effective as a heat insulating material for the walls of supersonic aircraft and spacecraft.
手続補正書（自発） １゜ 事件の表示 平成 年 特 許 願 第１８２３１４ 号 ２発明の名称 炭素繊維強化複合材料 ３、 補正をする者 事件との関係Procedural amendment (voluntary) 1゜ Display of incidents Heisei Year Special permission wish No. 182314 issue 2. Name of the invention Carbon fiber reinforced composite material 3. Person making the amendment Relationship with the incident
Claims (1)
リツクスと、マトリツクス中に強化材として含まれる炭
素繊維とからなり、当該マトリツクスの両側の表面部分
が耐酸化性セラミツクスからなり、両側の表面部分に対
する中心部分が炭素であつて、中心部分から両側の表面
部分までの組成が炭素から耐酸化性セラミツクスまでほ
ぼ連続的に変化していることを特徴とする炭素繊維強化
複合材料。(1) It consists of a plate-shaped matrix made of a composite of carbon and ceramics, and carbon fibers contained in the matrix as a reinforcing material, and the surface portions on both sides of the matrix are made of oxidation-resistant ceramics, and the surface portions on both sides A carbon fiber-reinforced composite material characterized in that a central portion thereof is carbon, and the composition from the central portion to both surface portions changes almost continuously from carbon to oxidation-resistant ceramics.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1182314A JPH0345568A (en) | 1989-07-14 | 1989-07-14 | Carbon fiber reinforced composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1182314A JPH0345568A (en) | 1989-07-14 | 1989-07-14 | Carbon fiber reinforced composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0345568A true JPH0345568A (en) | 1991-02-27 |
Family
ID=16116139
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1182314A Pending JPH0345568A (en) | 1989-07-14 | 1989-07-14 | Carbon fiber reinforced composite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0345568A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05104506A (en) * | 1991-10-17 | 1993-04-27 | Toda Constr Co Ltd | Manufacture of carbon fiber reinforced inorganic composite |
-
1989
- 1989-07-14 JP JP1182314A patent/JPH0345568A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05104506A (en) * | 1991-10-17 | 1993-04-27 | Toda Constr Co Ltd | Manufacture of carbon fiber reinforced inorganic composite |
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