JPH0333062A - Oxidation-resistant carbon material and its manufacture - Google Patents
Oxidation-resistant carbon material and its manufactureInfo
- Publication number
- JPH0333062A JPH0333062A JP1164027A JP16402789A JPH0333062A JP H0333062 A JPH0333062 A JP H0333062A JP 1164027 A JP1164027 A JP 1164027A JP 16402789 A JP16402789 A JP 16402789A JP H0333062 A JPH0333062 A JP H0333062A
- Authority
- JP
- Japan
- Prior art keywords
- carbon material
- oxidation
- boron oxide
- sol
- boron
- 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
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 48
- 230000003647 oxidation Effects 0.000 title claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 4
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 13
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- -1 boron alkoxide Chemical class 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 3
- 229910052810 boron oxide Inorganic materials 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 5
- 230000003628 erosive effect Effects 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 17
- 239000011248 coating agent Substances 0.000 abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 125000000217 alkyl group Chemical group 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 150000001639 boron compounds Chemical class 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 238000003980 solgel method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000005470 impregnation Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OXMKQIVTFWEMRJ-UHFFFAOYSA-N [B+3].CCCC[O-].CCCC[O-].CCCC[O-] Chemical compound [B+3].CCCC[O-].CCCC[O-].CCCC[O-] OXMKQIVTFWEMRJ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007859 condensation product Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- WYXIGTJNYDDFFH-UHFFFAOYSA-Q triazanium;borate Chemical compound [NH4+].[NH4+].[NH4+].[O-]B([O-])[O-] WYXIGTJNYDDFFH-UHFFFAOYSA-Q 0.000 description 1
- LGQXXHMEBUOXRP-UHFFFAOYSA-N tributyl borate Chemical compound CCCCOB(OCCCC)OCCCC LGQXXHMEBUOXRP-UHFFFAOYSA-N 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〕
本発明は、酸化ホウ素を含む耐酸化性炭素材料に係り、
特に、宇宙往還機等の構成部品として好適な耐酸化性炭
素材料に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to an oxidation-resistant carbon material containing boron oxide,
In particular, the present invention relates to oxidation-resistant carbon materials suitable as components of spacecraft and the like.
これまで炭素材料に耐酸化性を付与した材料としては、
カーボン、第２２巻、６号（１９８４年）第５０７頁〜
第５１１頁（Ｃａｒｂｏｎ、 ｖｏ Ｑ ２２ 、 Ｎ
（１ｆ３ （１９８４）、ｐｐ５０７〜５１１）に記載
の材料がある。この材料は、炭素材料にアンモニウムボ
レイト（Ａｍｍｏｎｉｕｍ ｂｏｒａｔｅ）、 ｎ−ア
ミルボレイト（ｎ −ａ＋ｉｙｌ ｂｏｒａｔｅ）、
トリブチルボレイト（ｔｒｉ−ｂｕｔｈｙｌ ｂｏｒａ
ｔｅ）等の有機ホウ素化合物を含浸させたものである。Until now, materials that have added oxidation resistance to carbon materials include:
Carbon, Vol. 22, No. 6 (1984), p. 507~
Page 511 (Carbon, vo Q 22, N
(1f3 (1984), pp507-511). This material contains ammonium borate, n-amyl borate (n-a+iyl borate), and carbon material.
Tri-butyl borate
It is impregnated with an organic boron compound such as te).
しかし、上記技術は、有機ホウ素化合物を炭素材料上に
コーティングしたものであり、常温付近では、炭素材料
への耐酸化性付与に有効な酸化ホウ素は生成していない
。酸化ホウ素は、コーテイング材を温度上昇していく過
程で生成する。この際、有機ホウ素化合物上の有機置換
基が分解した後、酸素と反応し、酸化ホウ素が生成する
。しかし、表面被覆された有機ホウ素化合物より有機置
換基が分解離脱する際、被覆膜には無数のピンホール等
が生成し、表面コーティングの効果が低下する。このた
め、耐酸化性は空気中、８００℃での酸化耐食量が２．
ｌＸ１０−３ｇ／−・ｈと低いものであった。However, the above technique involves coating a carbon material with an organic boron compound, and boron oxide, which is effective in imparting oxidation resistance to the carbon material, is not produced at around room temperature. Boron oxide is produced during the process of increasing the temperature of the coating material. At this time, after the organic substituent on the organic boron compound is decomposed, it reacts with oxygen to generate boron oxide. However, when the organic substituent group decomposes and leaves the surface-coated organic boron compound, numerous pinholes and the like are generated in the coating film, reducing the effectiveness of the surface coating. Therefore, the oxidation resistance in air at 800°C is 2.
It was as low as 1×10−3 g/−·h.
本発明の目的は、炭素材料上への酸化ホウ素の表面被覆
効果を高め、耐酸化性の良好な炭素材料を得ることにあ
る。また、耐酸化性の良好な宇宙往還機用表面タイルを
得ることにある。An object of the present invention is to enhance the surface coating effect of boron oxide on a carbon material and to obtain a carbon material with good oxidation resistance. Another object of the present invention is to obtain a surface tile for a spacecraft with good oxidation resistance.
本発明は、上記目的をゾル・ゲル法を用いて酸化ホウ素
を合成し、炭素材料に含浸被覆し、炭素材料上への酸化
ホウ素の表面被覆効果を高めることにより遠戚したもの
である。本発明により空気中、８００℃での酸化浸食量
が１．８ Ｘ １０−３ｇ／ａ（−ｈ以下の炭素材料を
得ることができる。この炭素材料の作製方法は、ボロン
アルコキシドを加水分解する工程を含み、ゾル・ゲル法
によって合成されたゾル溶液中に炭素材料を真空中で含
浸した後、乾燥するという工程で処理することを特徴と
するものである。これにより、酸化ホウ素の炭素材料上
への表面被覆率を９５％以上としたものである。また、
上記製法により作製した炭素材料を宇宙往還機用表面タ
イルとしたものである。The present invention is a distant relative of the above object by synthesizing boron oxide using a sol-gel method, impregnating and coating it on a carbon material, and enhancing the surface coating effect of boron oxide on the carbon material. According to the present invention, it is possible to obtain a carbon material with an oxidative erosion amount of 1.8 x 10-3 g/a (-h or less) in air at 800°C.The method for producing this carbon material involves hydrolyzing boron alkoxide. It is characterized by a process of impregnating a carbon material in a sol solution synthesized by the sol-gel method in a vacuum and then drying it.Thus, the carbon material of boron oxide The upper surface coverage is 95% or more.Also,
The carbon material produced by the above method was used as a surface tile for a spacecraft.
本発明に用いられるボロンアルコキシドは一般弐Ｂ （
ＯＲ）３（Ｒ：アルキル基）で表わされる化合物である
。ボロンアルコキシドは、水の存在下に速やかに加水分
解して（ＲＯｈＢＯＨで表わされるアルコキシ基の一部
が水酸基で置換された構造を持つ化合物を生成する。こ
のように部分的に加水分解して生成した中間体は、さら
に、他のボロンアルコキシド分子と反応し、
なる酸化ホウ素の縮合生成物となって成長していく。本
発明はこのような縮合生成物を炭素材料に含浸被覆する
ことにより耐酸化性炭素材料を得るものである。The boron alkoxide used in the present invention is general 2B (
OR) 3 (R: alkyl group). Boron alkoxide rapidly hydrolyzes in the presence of water (ROhBOH), producing a compound with a structure in which a portion of the alkoxy group is substituted with a hydroxyl group. The intermediate further reacts with other boron alkoxide molecules and grows into a condensation product of boron oxide.The present invention provides acid-resistant coating by impregnating a carbon material with such a condensation product. This is to obtain a carbonaceous material.
ここで酸化ホウ素を用いると耐酸化性向上に効果がある
のは次のように説明される。通常、炭素材料には表面に
結合が欠けているダングリングボンドが存在する。この
ダングリングボンドは反応活性であり酸素と反応し易い
。このため、炭素材料を空気中で熱すると燃焼し、ＣＯ
ｚとＣＯが生成してしまう。酸化ホウ素は、このダング
リングボンド間の距離とほぼ等しい間隔を持つホウ素結
合酸素を持つため、炭素材料上に表面被覆した時、この
ダングリングボンドを押え、ａ索との反応を抑制するこ
とができる（第１図）。The reason why boron oxide is effective in improving oxidation resistance is explained as follows. Usually, carbon materials have dangling bonds, which are missing bonds on the surface. This dangling bond is reactive and easily reacts with oxygen. For this reason, when carbon materials are heated in the air, they burn and CO
z and CO will be generated. Since boron oxide has boron-bonded oxygen with a distance approximately equal to the distance between these dangling bonds, when it is coated on the surface of a carbon material, it can hold down these dangling bonds and suppress the reaction with a-cords. Yes (Figure 1).
また、ゾル・ゲル法によって作製した酸化ホウ素のゾル
溶液はすでに溶液中に酸化ホウ素の無機重合体を含むた
め、炭素材料上に、直接、酸化ホウ素の被覆膜を作製す
ることができる。このため、有機ホウ素化合物を被覆し
た場合と異なり、ホウ素結合有機物が温度上昇の過程で
分解飛散することもないため、被覆膜上のピンホール等
を減少させ表面コーティング効果を増加させることがで
きる。Furthermore, since the sol solution of boron oxide prepared by the sol-gel method already contains an inorganic polymer of boron oxide in the solution, a coating film of boron oxide can be directly formed on the carbon material. Therefore, unlike when coating with an organic boron compound, the boron-bonded organic substance does not decompose and scatter during the temperature rise process, reducing pinholes on the coating film and increasing the surface coating effect. .
ゾル溶液を被覆する際、真空含浸、乾燥の工程をくり返
すことにより、特に酸化ホウ素の表面被覆率をより高め
ることができる。これによって、得られた炭素材料への
酸化ホウ素の表面被覆率は９５％以上になる。こうして
１作製した炭素材料は、空気中、８００℃での酸化浸食
量が１．８×１０−３ｇ／ａＪ−ｈ以下のものを作製す
ることができる。従って１本炭素材料は宇宙往還機等の
軽量。When coating with a sol solution, by repeating the steps of vacuum impregnation and drying, it is possible to further increase the surface coverage, especially of boron oxide. As a result, the surface coverage of boron oxide on the obtained carbon material becomes 95% or more. One carbon material thus produced can have an oxidative erosion amount of 1.8×10 −3 g/aJ−h or less at 800° C. in air. Therefore, a single carbon material is lightweight for spacecraft, etc.
高強度表面タイルとして好適である。Suitable as a high-strength surface tile.
従来の有機ホウ素化合物を被覆したものでは、被覆を繰
り返す過程で熱処理が必要なため、下地の炭素材料の酸
化侵食が進んでしまう。従って、被覆を繰り返して被覆
率を増加させることはできない。Conventional materials coated with organic boron compounds require heat treatment during the repeated coating process, resulting in accelerated oxidation erosion of the underlying carbon material. Therefore, it is not possible to increase the coverage by repeating coating.
以下、本発明を実施例を用いて説明する。 The present invention will be explained below using examples.
〈実施例１〉
ボロンブトキシドの１ｍｏＱ／１１ エタノール溶液
を作製した。この溶液２００ｍｆｌに水の１．５ｒａｏ
Ｑ／Ｑのエタノール溶液２００ｍＱを三時間かけて添加
した。ついで、この溶液を７０℃で三時間、反応撹拌し
た。得られたこの溶液中に立方体形に作製した炭素材料
ブロック（１ｏ Ｘ １０ Ｘ１０ｍ）を入れ、真空デ
シケータ中で真空含浸を行なった。ついでこの炭素材料
を取り出し、１００℃で乾燥した。この真空含浸、乾燥
の工程を十回くり返した。この材料の空気中、８００℃
での耐酸化性試験結果を第１図に示す。本材料の酸化浸
食量は１．６ Ｘ １０−３ｇ／ｃＪ−ｈと有機ホウ素
化合物を含浸したもの（２，↓Ｘ １０−”ｇ ／ａＪ
−ｈ ） 。<Example 1> A 1moQ/11 ethanol solution of boron butoxide was prepared. 1.5 rao of water to 200 mfl of this solution
200 mQ of Q/Q ethanol solution was added over 3 hours. This solution was then reacted and stirred at 70°C for 3 hours. A cube-shaped carbon material block (10 x 10 x 10 m) was placed in the resulting solution, and vacuum impregnation was performed in a vacuum desiccator. This carbon material was then taken out and dried at 100°C. This process of vacuum impregnation and drying was repeated ten times. This material in air at 800℃
The results of the oxidation resistance test are shown in Figure 1. The amount of oxidative erosion of this material is 1.6 x 10-3g/cJ-h and that of the material impregnated with an organic boron compound (2,↓X 10-”g/aJ-h)
-h).
及び、コーティングしないもの（２８Ｘ １０−’ｇ／
ｃｒｊ−１１）に比べ、耐酸化性が向上している。and uncoated (28X 10-'g/
oxidation resistance is improved compared to crj-11).
ゾル・ゲル法で酸化ホウ素を炭素材料上に表面被瑣した
材料の酸化ホウ素の表面被覆率は９６％であった６一方
、有機ホウ素化合物を表面被覆した材料では、酸化ホウ
素の表面被覆率は４０％程度であった。ゾル・ゲル法で
作製した耐酸化性炭素材料は、酸化ホウ素の表面波ｒｒ
Ｉ率が高いため、有機ホウ素化合物を含浸したものより
も耐酸化性が向上したと考えられる。The surface coverage of boron oxide in a material whose surface was coated with boron oxide on a carbon material using the sol-gel method was 96%.6 On the other hand, in the case of a material whose surface was coated with an organic boron compound, the surface coverage of boron oxide was 96%. It was about 40%. The oxidation-resistant carbon material produced by the sol-gel method has surface waves of boron oxide.
It is thought that because the I ratio is high, the oxidation resistance is improved compared to that impregnated with an organic boron compound.
〈実施例２〉
ボロンブトキシド１ｍｏＱ／Ｑのエタノール溶液を作製
した。この溶液２００ｍＱに水の１．５ｍｏＱ／ａのエ
タノール溶液２００ｍｆｆを三時間かけて添加した。つ
いでこの溶液を７０℃で三時間反応撹拌した。得られた
この溶液をパレット（４００Ｘ４００Ｘ３０ｍ）に移し
、この中に直方体形炭素材料（３００ｘ３００ＸＩＯｎ
ｎ）を入れ、直空デシケータ中で真空含浸を行なった。<Example 2> An ethanol solution of 1 moQ/Q of boron butoxide was prepared. To 200 mQ of this solution, 200 mff of an ethanol solution containing 1.5 moQ/a of water was added over 3 hours. This solution was then reacted and stirred at 70°C for 3 hours. The obtained solution was transferred to a pallet (400 x 400 x 30 m), and a rectangular parallelepiped carbon material (300 x 300 x ION
n) and vacuum impregnation was performed in a direct air desiccator.
ついで、この炭素材料を取り出し、１００℃で３０分間
乾燥させた。この真空含浸、乾燥の工程を十回くり返し
て得られた炭素材料は実施例１で示したものと同様な性
質を示し、宇宙柱ｉ！！ｎ用表面タイルとして好適であ
る。Then, this carbon material was taken out and dried at 100° C. for 30 minutes. The carbon material obtained by repeating this vacuum impregnation and drying process ten times exhibited properties similar to those shown in Example 1, and the space column i! ! Suitable as a surface tile for n.
本発明によれば、ゾル・ゲル法を用いて酸化ホウ素の炭
素材料への表面被覆率９５％以上の耐酸化性炭素材料を
作製す′ることかできる。本炭素材料は、宇宙往還機等
に使用される軽量、高強度な表面タイルに好適である。According to the present invention, it is possible to produce an oxidation-resistant carbon material having a surface coverage of 95% or more of boron oxide on the carbon material using the sol-gel method. This carbon material is suitable for lightweight, high-strength surface tiles used in spacecraft and the like.
第１図は、酸化ホウ素を含浸させた炭素材料の耐酸化性
試験結果（空気中、８００℃）を示す特性図、第２図は
、炭素材料上への酸化ホウ素の被覆の説明図である。
将
第
図
ＣＡ）
／θFigure 1 is a characteristic diagram showing the oxidation resistance test results (in air, 800°C) of a carbon material impregnated with boron oxide, and Figure 2 is an explanatory diagram of the coating of boron oxide on the carbon material. . General chart CA) /θ
Claims (5)
量が１．８×１０＾−＾３ｇ／ｃｍ＾２・ｈ以下である
ことを特徴とする耐酸化性炭素材料。1. An oxidation-resistant carbon material containing boron oxide and having an oxidative erosion amount of 1.8 x 10^-^3 g/cm^2.h or less at 800°C in air.
ことを特徴とする耐酸化性炭素材料。2. An oxidation-resistant carbon material characterized by containing boron oxide produced using a sol-gel reaction.
ホウ素の炭素材料への表面被覆率が９５％以上であるこ
とを特徴とする耐酸化性炭素材料。3. An oxidation-resistant carbon material containing boron oxide, characterized in that the surface coverage of boron oxide on the carbon material is 95% or more.
作製したゾル溶液を炭素材料に真空中で含浸、ついで乾
燥する工程とを含むことを特徴とする耐酸化性炭素材料
の製造方法。4. A method for producing an oxidation-resistant carbon material, comprising a step of hydrolyzing boron alkoxide, a step of impregnating a carbon material with the sol solution prepared thereby in a vacuum, and then drying the material.
性材料を含むことを特徴とする宇宙往還機用表面タイル
。5. A surface tile for a spacecraft, comprising the oxidation-resistant material according to claim 1, 2, or 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1164027A JPH0333062A (en) | 1989-06-28 | 1989-06-28 | Oxidation-resistant carbon material and its manufacture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1164027A JPH0333062A (en) | 1989-06-28 | 1989-06-28 | Oxidation-resistant carbon material and its manufacture |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0333062A true JPH0333062A (en) | 1991-02-13 |
Family
ID=15785412
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1164027A Pending JPH0333062A (en) | 1989-06-28 | 1989-06-28 | Oxidation-resistant carbon material and its manufacture |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0333062A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2681064A1 (en) * | 1991-09-06 | 1993-03-12 | Daimler Benz Ag | PROCESS FOR IMPREGNATING POROUS CARBON PARTS TO PROTECT THEM AGAINST OXIDATION |
| JPH06249997A (en) * | 1993-02-27 | 1994-09-09 | Kenzo Ishida | Neutron capturing body and building |
| EP0633234A1 (en) * | 1993-07-08 | 1995-01-11 | Societe Des Terres Refractaires Du Boulonnais | Agent for protecting carbon containing refractories against oxidation, comprising a mixture of a borate compound and an amine derivative as well as process of manufacturing of said refractories |
-
1989
- 1989-06-28 JP JP1164027A patent/JPH0333062A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2681064A1 (en) * | 1991-09-06 | 1993-03-12 | Daimler Benz Ag | PROCESS FOR IMPREGNATING POROUS CARBON PARTS TO PROTECT THEM AGAINST OXIDATION |
| JPH06249997A (en) * | 1993-02-27 | 1994-09-09 | Kenzo Ishida | Neutron capturing body and building |
| EP0633234A1 (en) * | 1993-07-08 | 1995-01-11 | Societe Des Terres Refractaires Du Boulonnais | Agent for protecting carbon containing refractories against oxidation, comprising a mixture of a borate compound and an amine derivative as well as process of manufacturing of said refractories |
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