JPS63210088A - Manufacture of thermally cracked carbon coated graphite material - Google Patents
Manufacture of thermally cracked carbon coated graphite materialInfo
- Publication number
- JPS63210088A JPS63210088A JP62042177A JP4217787A JPS63210088A JP S63210088 A JPS63210088 A JP S63210088A JP 62042177 A JP62042177 A JP 62042177A JP 4217787 A JP4217787 A JP 4217787A JP S63210088 A JPS63210088 A JP S63210088A
- Authority
- JP
- Japan
- Prior art keywords
- pyrolytic carbon
- coated graphite
- temperature
- graphite material
- graphite
- 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 11
- 239000007770 graphite material Substances 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 229910052799 carbon Inorganic materials 0.000 title 1
- 239000002296 pyrolytic carbon Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 description 16
- 238000007254 oxidation reaction Methods 0.000 description 16
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000008282 halocarbons Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- -1 furopane Chemical compound 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000000689 upper leg Anatomy 0.000 description 1
- 230000002747 voluntary effect Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は各種用途に用いられる寿命の長い熱分解炭素被
覆黒鉛材の製造法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing a long-life pyrolytic carbon-coated graphite material used in various applications.
（従来の技術）
熱分解炭素被覆黒鉛材の製造法は通常熱ＣＶＤ法であり
、その被覆温度は４００−２１００℃である。被覆され
る熱分解炭素の膜のかさ密度は１．４〜２．２ｇ／ｃｍ
”であり、結晶子の大きさＬＣ（００２）はｌＯ〜１５
０′にの範囲である。被覆温度の低い例としては特公昭
５６−３５６０３号公報に示されるハロゲン化炭化水素
を原料とし、４００−１０００℃で被覆する方法があり
、高い温度の例としては。(Prior Art) The method for producing pyrolytic carbon-coated graphite material is usually a thermal CVD method, and the coating temperature is 400-2100°C. The bulk density of the coated pyrolytic carbon film is 1.4 to 2.2 g/cm
”, and the crystallite size LC (002) is lO~15
0'. An example of a low coating temperature is a method disclosed in Japanese Patent Publication No. 56-35603 in which a halogenated hydrocarbon is used as a raw material and coating is carried out at 400-1000°C, and an example of a high temperature is a method of coating at a temperature of 400 to 1000°C.
特公昭４７−１００３号公報に示される初めに１１００
−１６００℃で９次いで１６００−２１００℃で被覆す
る方法がある。また熱分解黒鉛の製造法は熱分解炭素被
覆黒鉛材の製造法と類似しているが、熱分解黒鉛は膜を
厚くつけて基材から剥離させて製造するもので、膜が剥
離すると製品とならない被覆材とは本質的に異なるもの
である。1100 at the beginning shown in Special Publication No. 47-1003
There is a method of coating at -1600°C and then at 1600-2100°C. The manufacturing method for pyrolytic graphite is similar to the manufacturing method for pyrolytic carbon-coated graphite materials, but pyrolytic graphite is manufactured by applying a thick film and peeling it off from the base material. This is essentially different from a covering material that does not require a cladding.
（発明が解決しようとする問題点）
炭素材料は酸化に対して抵抗力が小さい欠点がある。炭
素材料に熱分解炭素を被覆すると耐酸化性は向上するが
、従来の４００〜２１００℃で熱分解炭素を被覆した黒
鉛材料ではその耐酸化性は不十分である。(Problems to be Solved by the Invention) Carbon materials have the disadvantage of low resistance to oxidation. Although oxidation resistance is improved when a carbon material is coated with pyrolytic carbon, the oxidation resistance of conventional graphite materials coated with pyrolytic carbon at 400 to 2100° C. is insufficient.
このため各種ヒータ、るつぼ、治具として使用した場合
、寿命が期待する程長くない問題点がある。Therefore, when used as various heaters, crucibles, and jigs, there is a problem that the lifespan is not as long as expected.
熱分解炭素は炭素材料であるため酸化を本質的に防止す
ることはできないが、耐酸化性をさらに向上させること
は可能である。また耐酸化性を向上させることにより稽
々の化学物質との反応性も同様に向上すると考えられる
。Since pyrolytic carbon is a carbon material, oxidation cannot be essentially prevented, but it is possible to further improve the oxidation resistance. Furthermore, it is thought that by improving the oxidation resistance, the reactivity with chemical substances will also be improved.
本発明は従来材のこのような問題点を改善し。The present invention improves these problems of conventional materials.
耐酸化性、耐反応性のさらに良好な熱分解炭素被覆黒鉛
材の製造法を提供することを目的とするものである。The object of the present invention is to provide a method for producing a pyrolytic carbon-coated graphite material that has even better oxidation resistance and reaction resistance.
（問題点を解決するための手段）
本発明者らは熱分解炭素の耐酸化性について研究を重ね
た結果、１６００−２２００℃の温度でＺＯｇ／ｃｍ”
以上のかさ密度を有する熱分解炭素を被覆した後、さら
に２５００℃以上の温度で熱処理することにより耐酸化
性を大幅に向上できることを見出ｌ１、た。゛
本発明は黒鉛基材に１６００−２２００℃の温度でＺＯ
ｇ／ｃｍ３以上のかさ密度を有する熱分解炭素を被ａ（
９次いで核熱分解炭素被覆黒鉛基材を２５００℃以上の
温度で熱処理する熱分解炭素被覆黒鉛材の製造法に関す
る。(Means for Solving the Problems) As a result of repeated research on the oxidation resistance of pyrolytic carbon, the inventors found that ZOg/cm"
It has been found that oxidation resistance can be significantly improved by further heat-treating at a temperature of 2500° C. or higher after coating with pyrolytic carbon having a bulk density above.゛The present invention applies ZO to a graphite base material at a temperature of 1600-2200℃.
Covered with pyrolytic carbon having a bulk density of g/cm3 or more
9. Next, the present invention relates to a method for producing a pyrolytic carbon-coated graphite material, in which a nuclear pyrolytic carbon-coated graphite substrate is heat-treated at a temperature of 2500° C. or higher.
本発明に用いられる黒鉛基材は通常の人造黒鉛であり、
このようなものとしては、たとえば等方性黒鉛材料をあ
げることができる。本発明に用いられる熱分解炭素の被
覆法は通常のＣＶＤ法であり、このようなものとしては
熱−ＣＶＤがあけられる。被覆温度を１６００℃以上と
したのは、 １６００℃未満では２５００℃以上で熱処
理した場合に膜が剥離しやすいためである。熱分解炭素
の膜のかさ密度を２．０ ｇ／ｃｍ３以上としたのは２
．０ｇ／ｃｍｊ未満では２５００℃以上で熱処理した場
合に多孔質な膜になりやすく、耐酸化性の向上効果が岬
いためである。また被徨温腿を２２００℃までと１．た
のは２２００℃を越えると煤が発生Ｌ５やすく、良好な
熱分解炭素膜を得るのが困難となるためである。The graphite base material used in the present invention is ordinary artificial graphite,
An example of such a material is an isotropic graphite material. The pyrolytic carbon coating method used in the present invention is a normal CVD method, and thermal CVD is an example of such a method. The reason why the coating temperature was set to 1,600°C or higher is that if the coating temperature is lower than 1,600°C, the film tends to peel off when heat-treated at 2,500°C or higher. The bulk density of the pyrolytic carbon film is 2.0 g/cm3 or more.
．． This is because if it is less than 0 g/cmj, the film tends to become porous when heat treated at 2500° C. or higher, and the effect of improving oxidation resistance is limited. In addition, the warm thighs can be heated up to 2200℃ and 1. This is because if the temperature exceeds 2200°C, soot is likely to be generated L5, making it difficult to obtain a good pyrolytic carbon film.
本発明では上記した熱分解炭素被接黒鉛基材を更に２５
００℃以上の温度で熱処理する。この熱処理工程を経な
いと耐酸化性向丘の効果があまりないためである。熱処
理温度の上限は特に制限はないが、黒鉛の耐酸化温度で
あるおよそ３２００℃程度である。経済的な点を考慮し
た最適上限は２８００℃程度である。In the present invention, the above-mentioned pyrolytic carbon-coated graphite base material is further added to 25
Heat treatment is performed at a temperature of 00°C or higher. This is because without this heat treatment step, the effect of the oxidation-resistant mucosa is not so great. The upper limit of the heat treatment temperature is not particularly limited, but is approximately 3200° C., which is the oxidation resistance temperature of graphite. The optimum upper limit considering economical points is about 2800°C.
本発明で使用される原料は炭素の化合物であり。The raw material used in the present invention is a carbon compound.
このようなものとしてはたとえば通常の炭化水素（メタ
ン、フロパン、ベンゼンなト）やハロゲン化炭化水素（
ジクａ口エチレン、トリクロロエタンなど）をあげるこ
とができる。These include, for example, ordinary hydrocarbons (such as methane, furopane, and benzene) and halogenated hydrocarbons (
Examples include dichloroethylene, trichloroethane, etc.
（実施例） 次に実施例により不発明の詳細な説明する。(Example) Next, the invention will be explained in detail with reference to examples.
通常の間接加熱減圧ＣＶＤ炉を使用り、、１０ｍｍ角×
厚さ２ｔｍＫ加工した等方性の黒鉛基材（日立化成工業
社製、ＰＤ−３２０）の全面に、原料としてベンゼンを
用い、炉内圧力を２０ ’ｒｏｒｒ以下に保ちつつ、第
１表に示す被覆温度で熱分解炭素の膜を４０μｍの厚さ
に被覆した。その後窒素ガス雰囲気中で２６００℃まで
昇温し２６００℃で３０分間熱処理を行った。その場合
の被膜の特性及び酸化速度の測定結果を第１表に示す。Using a normal indirect heating low pressure CVD furnace, 10mm square x
Benzene was used as a raw material on the entire surface of an isotropic graphite base material (manufactured by Hitachi Chemical Co., Ltd., PD-320) processed to a thickness of 2 tmK, and the pressure in the furnace was kept below 20'rorr as shown in Table 1. A film of pyrolytic carbon was applied to a thickness of 40 μm at the coating temperature. Thereafter, the temperature was raised to 2600°C in a nitrogen gas atmosphere, and heat treatment was performed at 2600°C for 30 minutes. Table 1 shows the measurement results of the film properties and oxidation rate in that case.
第１表における酸化速度は、７００℃に加熱された炉内
に試料を入れ、空気を通じて毎時１ｃが当りの重輩減を
求めたものである。第１表から実施例のものは、比較例
のものに較べて耐酸化性が著しく向上していることがわ
かる。The oxidation rate in Table 1 is determined by placing the sample in a furnace heated to 700° C. and determining the weight loss per hour by passing air through it. It can be seen from Table 1 that the oxidation resistance of the examples was significantly improved compared to that of the comparative examples.
（発明の効果）
本発明によれば、耐酸化性の優れた熱分解炭素被覆黒鉛
材が得らルる。該熱分解炭素被覆黒鉛材は耐熱性を要求
されるヒータ、るつぼ、治具に用いて好適であり、それ
らの寿命を延長できる。(Effects of the Invention) According to the present invention, a pyrolytic carbon-coated graphite material having excellent oxidation resistance can be obtained. The pyrolytic carbon-coated graphite material is suitable for use in heaters, crucibles, and jigs that require heat resistance, and can extend their service life.
代理人 弁理士 若 林 邦 彦 手続補正書（自発）Agent Patent Attorney Kunihiko Wakabayashi Procedural amendment (voluntary)
Claims (1)
／ｃｍ＾３以上のかさ密度を有する熱分解炭素を被覆し
、次いで該熱分解炭素黒鉛基材を２５００℃以上の温度
で熱処理することを特徴とする熱分解炭素被覆黒鉛材の
製造法。1. 2.0g on graphite base material at a temperature of 1600-2200℃
A method for producing a pyrolytic carbon-coated graphite material, which comprises coating pyrolytic carbon having a bulk density of /cm^3 or more, and then heat-treating the pyrolytic carbon graphite substrate at a temperature of 2500° C. or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62042177A JPH0717468B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing pyrolytic carbon-coated graphite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62042177A JPH0717468B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing pyrolytic carbon-coated graphite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63210088A true JPS63210088A (en) | 1988-08-31 |
| JPH0717468B2 JPH0717468B2 (en) | 1995-03-01 |
Family
ID=12628703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62042177A Expired - Lifetime JPH0717468B2 (en) | 1987-02-25 | 1987-02-25 | Method for producing pyrolytic carbon-coated graphite material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0717468B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0316994A (en) * | 1989-06-12 | 1991-01-24 | Nippon Mining Co Ltd | Growth of compound semiconductor single crystal |
| JP2016069230A (en) * | 2014-09-30 | 2016-05-09 | イビデン株式会社 | Production process for pyrolytic carbon-cladded graphite member |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61219708A (en) * | 1985-03-22 | 1986-09-30 | Hitachi Chem Co Ltd | Preparation of graphite article coated with pyrolytically prepared carbon |
| JPS61222914A (en) * | 1985-03-27 | 1986-10-03 | Hitachi Chem Co Ltd | Production of thermally decomposed carbon product |
| JPS61256909A (en) * | 1985-05-07 | 1986-11-14 | Hitachi Chem Co Ltd | Preparation of covering material for pyrolytic carbon |
| JPS61256993A (en) * | 1985-05-09 | 1986-11-14 | Toyo Tanso Kk | Graphite crucible and heater for silicon single crystal pulling device |
-
1987
- 1987-02-25 JP JP62042177A patent/JPH0717468B2/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61219708A (en) * | 1985-03-22 | 1986-09-30 | Hitachi Chem Co Ltd | Preparation of graphite article coated with pyrolytically prepared carbon |
| JPS61222914A (en) * | 1985-03-27 | 1986-10-03 | Hitachi Chem Co Ltd | Production of thermally decomposed carbon product |
| JPS61256909A (en) * | 1985-05-07 | 1986-11-14 | Hitachi Chem Co Ltd | Preparation of covering material for pyrolytic carbon |
| JPS61256993A (en) * | 1985-05-09 | 1986-11-14 | Toyo Tanso Kk | Graphite crucible and heater for silicon single crystal pulling device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0316994A (en) * | 1989-06-12 | 1991-01-24 | Nippon Mining Co Ltd | Growth of compound semiconductor single crystal |
| JP2016069230A (en) * | 2014-09-30 | 2016-05-09 | イビデン株式会社 | Production process for pyrolytic carbon-cladded graphite member |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0717468B2 (en) | 1995-03-01 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |