JP2003183076A - Method for manufacturing pyrolytic carbon or graphite- coated carbon material - Google Patents
Method for manufacturing pyrolytic carbon or graphite- coated carbon materialInfo
- Publication number
- JP2003183076A JP2003183076A JP2001382813A JP2001382813A JP2003183076A JP 2003183076 A JP2003183076 A JP 2003183076A JP 2001382813 A JP2001382813 A JP 2001382813A JP 2001382813 A JP2001382813 A JP 2001382813A JP 2003183076 A JP2003183076 A JP 2003183076A
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- gas
- graphite
- carbon material
- pyrolytic
- 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
Abstract
Description
【０００１】[0001]
【技術分野】本発明は、熱分解炭素または黒鉛被覆炭素
材料の製造方法に関し、より詳しくは炭素材料に熱分解
炭素を被覆する工程において、原料ガスである炭化水素
ガスとキヤリアガスである水素ガスとともに塩化水素ガ
スを流入することにより、高純度でガスシ−ル性に優れ
た熱分解炭素または黒鉛被覆炭素材料を安価に得ること
ができる製造方法に関する。TECHNICAL FIELD The present invention relates to a method for producing a pyrolytic carbon or a graphite-coated carbon material, and more particularly, in the step of coating a carbon material with a pyrolytic carbon, together with a hydrocarbon gas as a raw material gas and a hydrogen gas as a carrier gas. The present invention relates to a method for producing a pyrolytic carbon or graphite-coated carbon material having high purity and excellent gas sealability at low cost by introducing hydrogen chloride gas.
【０００２】[0002]
【従来の技術】熱分解炭素または熱分解黒鉛（以下熱分
解炭素という）は、通常の炭素材料の持つ耐熱性、低反
応性、耐薬品性等に優れるばかりでなく、結晶性が高
く、熱伝導性の良好な優れた材料である。2. Description of the Related Art Pyrolytic carbon or pyrolytic graphite (hereinafter referred to as pyrolytic carbon) is not only excellent in heat resistance, low reactivity, chemical resistance and the like of ordinary carbon materials, but also high in crystallinity. It is an excellent material with good conductivity.
【０００３】更に、熱分解炭素はガス透過性が著しく低
い材料のため、各種のガスのシ−ル性に優れた効果を発
揮する。Further, since pyrolytic carbon is a material having extremely low gas permeability, it exerts an excellent effect on the sealing property of various gases.
【０００４】このため、通常多孔質である炭素材料の表
面に熱分解炭素を被覆することにより、炭素材料へのガ
スの侵入を抑制できるので、熱分解炭素被覆炭素材料の
ガスシ−ル性に着目した用途への使用が期待されてい
る。Therefore, by coating the surface of the carbon material, which is usually porous, with pyrolytic carbon, it is possible to suppress the invasion of gas into the carbon material. Therefore, pay attention to the gas sealing property of the carbon material coated with pyrolytic carbon. It is expected to be used for such purposes.
【０００５】特に近年、シリコン単結晶引き上げ装置
（ＣＺ炉）におけるルツボやヒ−タ−等の各種の部材に
おける優れた効果が期待されている。Particularly, in recent years, excellent effects have been expected on various members such as crucibles and heaters in a silicon single crystal pulling apparatus (CZ furnace).
【０００６】即ち、ＣＺ炉においては揮発性の一酸化シ
リコン（ＳｉＯガス）が多量に発生する。このＳｉＯは
多孔質である炭素材料内に侵入し、炭素材料を珪化す
る。その結果、炭素材料は劣化、消耗するため、この炭
素材料を用いたルツボやヒ−タ−等は、寿命が非常に短
くなる問題がある。That is, a large amount of volatile silicon monoxide (SiO gas) is generated in the CZ furnace. This SiO penetrates into the porous carbon material and silicifies the carbon material. As a result, since the carbon material deteriorates and is consumed, there is a problem that the crucible, the heater and the like using this carbon material have a very short life.
【０００７】そこで、多孔質の炭素材料の表面にガスシ
−ル性に優れた熱分解炭素の皮膜を被覆すると、炭素材
料へのＳｉＯの侵入を抑制でき、炭素材料とＳｉＯの反
応の進行を表面のみにとどめ、炭素材料の内部の珪化に
よる劣化や消耗を有効に防ぐことができる。このような
熱分解炭素被覆炭素材料を用いたルツボやヒ−タ−は、
その寿命を大幅に延長できるメリットがある。Therefore, by coating the surface of the porous carbon material with a film of pyrolytic carbon having an excellent gas sealing property, the penetration of SiO into the carbon material can be suppressed, and the progress of the reaction between the carbon material and SiO can be prevented. However, it is possible to effectively prevent deterioration and consumption due to silicidation inside the carbon material. Crucibles and heaters using such pyrolytic carbon-coated carbon material,
There is a merit that the life can be greatly extended.
【０００８】しかしながら、熱分解炭素を被覆した直後
の炭素材料は、充分に高純度ではなく、コンタミを嫌う
用途では、熱分解炭素で被覆した後に、ハロゲンガス等
で純化する必要がある。例えば、特開平１０−４５４７
４号には、黒鉛基材に熱分解炭素を被覆した後、純化の
ためハロゲンガス雰囲気中で１５００〜２５００℃の温
度で熱処理し純度の高い熱分解炭素被覆黒鉛材を製造す
る方法が記載されているが、被覆後の純化処理のためコ
スト高にならざるを得ない。このように、高純度の熱分
解炭素被覆炭素材料の製造はコスト面で難があり、安価
に製造できる方法が望まれている。However, the carbon material immediately after being coated with pyrolytic carbon is not sufficiently high in purity, and for applications where contamination is disliked, it is necessary to purify with a halogen gas or the like after coating with pyrolytic carbon. For example, JP-A-10-4547.
No. 4 describes a method of producing a highly pure pyrolytic carbon-coated graphite material by coating a pyrolyzed carbon on a graphite base material and then heat-treating at a temperature of 1500 to 2500 ° C. in a halogen gas atmosphere for purification. However, the cost is inevitably high due to the purification treatment after coating. As described above, the production of a high-purity pyrolytic carbon-coated carbon material is difficult in terms of cost, and a method that can be produced inexpensively is desired.
【０００９】[0009]
【発明の課題】上記のような状況に鑑み、本発明者は高
純度でガスシ−ル性に優れた熱分解炭素被覆炭素材料を
安価に製造できる方法を提供する。In view of the above situation, the present inventor provides a method for inexpensively producing a pyrolytic carbon-coated carbon material having high purity and excellent gas sealability.
【００１０】[0010]
【課題解決の手段】上記のような課題を解決するため
に、本発明者が提案するのは、減圧下、１２００℃以上
の雰囲気で、炭素材料に原料ガスである炭化水素ガス、
キヤリアガスである水素ガスと同時に塩化水素ガスを流
入させ、熱分解炭素または黒鉛を炭素材料に被覆させる
ことを特徴とする熱分解炭素または黒鉛被覆炭素材料の
製造方法である。In order to solve the above problems, the present inventor proposes that a hydrocarbon gas, which is a raw material gas, is added to a carbon material under reduced pressure in an atmosphere of 1200 ° C. or higher,
A method for producing a pyrolytic carbon- or graphite-coated carbon material, characterized in that hydrogen chloride gas is introduced at the same time as hydrogen gas as a carrier gas to coat the carbon material with pyrolytic carbon or graphite.
【００１１】以下に本発明を詳細に説明する。The present invention will be described in detail below.
【００１２】まず、基材となる炭素材料は、炭素質、黒
鉛質のいずれの材料も使用され、一般の炭素材料、黒鉛
材料、炭素繊維強化炭素材料（Ｃ／Ｃ）、炭素繊維成形
断熱材等の各種の炭素材料を使用できる。First, as the carbon material as the base material, any of carbonaceous material and graphite material is used, and general carbon material, graphite material, carbon fiber reinforced carbon material (C / C), carbon fiber molded heat insulating material. Various carbon materials such as
【００１３】本発明では、基材の炭素材料をまずルツ
ボ、ヒ−タ−等の製品形状に加工して、ハロゲンガス雰
囲気中、１５００℃以上で熱処理して純化する。In the present invention, the carbon material of the base material is first processed into a product shape such as a crucible or a heater, and heat-treated at 1500 ° C. or higher in a halogen gas atmosphere for purification.
【００１４】上記のように加工、純化した炭素材料に熱
分解炭素を被覆する。被覆には、原料ガスにメタン、エ
タン、プロパン、ブタン等から選ばれる炭化水素ガスを
使用し、キャリアガスとして水素ガスを使用するが、本
発明で特徴となるのは、同時に塩化水素ガスを流入させ
ることである。この塩化水素ガスを炭化水素ガス、水素
ガスと同時に流入することにより、高純度の熱分解炭素
を被覆することができる。The carbon material processed and purified as described above is coated with pyrolytic carbon. For the coating, a hydrocarbon gas selected from methane, ethane, propane, butane, etc. is used as a raw material gas, and hydrogen gas is used as a carrier gas. The feature of the present invention is that hydrogen chloride gas is introduced at the same time. It is to let. By inflowing this hydrogen chloride gas at the same time as the hydrocarbon gas and the hydrogen gas, high-purity pyrolytic carbon can be coated.
【００１５】塩化水素ガスの流入量は炭化水素ガスに対
して５容量％以上とする。５容量％未満では、熱分解炭
素被覆炭素材料の純度を改善できない。The inflow amount of hydrogen chloride gas is 5% by volume or more with respect to the hydrocarbon gas. If it is less than 5% by volume, the purity of the pyrolytic carbon-coated carbon material cannot be improved.
【００１６】被覆の条件は、減圧下において１２００℃
以上で熱処理するものとする。熱処理の温度が１２００
℃未満では、熱分解炭素の皮膜が多孔質化し、ガスシ−
ル性が不良となる。The coating conditions are 1200 ° C. under reduced pressure.
The heat treatment is performed as described above. Heat treatment temperature is 1200
If the temperature is lower than ℃, the pyrolytic carbon film becomes porous and gas seal
Poor quality.
【００１７】本発明における熱分解炭素は、炭素質、黒
鉛質いずれも含むもので、被覆の熱処理温度を２０００
〜３０００℃の高温とした場合は、黒鉛質の熱分解黒鉛
となる。上記のような方法により、熱分解炭素を炭素材
料に被覆した後に高純度化処理をすることなく、高純度
の熱分解炭素被覆炭素材料を得ることができる。The pyrolytic carbon in the present invention includes both carbonaceous and graphitic substances, and the coating heat treatment temperature is 2000.
When the temperature is set to a high temperature of up to 3000 ° C, it becomes a pyrolytic graphite of graphite. By the method as described above, a high-purity pyrolytic carbon-coated carbon material can be obtained without performing a high-purification treatment after coating the pyrolytic carbon on the carbon material.
【００１８】[0018]
【発明の効果】本発明によれば、高純度でガスシ−ル性
にすぐれた熱分解炭素被覆炭素材料を安価に製造するこ
とができる。特にシリコン単結晶引き上げ装置のルツボ
等に優れた効果を発揮する熱分解炭素被覆炭素材料を安
価に提供でき工業上有用なものである。According to the present invention, a pyrolytic carbon-coated carbon material having high purity and excellent gas sealability can be manufactured at a low cost. In particular, a pyrolytic carbon-coated carbon material exhibiting an excellent effect on a crucible of a silicon single crystal pulling apparatus can be provided at low cost and is industrially useful.
【００１９】[0019]
【実施例１】直径５００ｍｍ、高さ４００ｍｍのルツボ
形状に加工した黒鉛材料（材料名：ＥＧＦ−２６２ 日
本カ−ボン（株）製）を塩化水素ガス雰囲気中、２００
０℃で純化処理し、高純度の黒鉛ルツボを得た。この黒
鉛ルツボに、１４００℃、減圧５０ｔｏｒｒにおいて、
プロパン流量に対して１０容量％の塩化水素と水素ガス
を３時間流入させ、熱分解炭素被覆黒鉛ルツボを得た。
得られた熱分解炭素の純度をグロ−放電質量分析で測定
した結果、検出限界の範囲内では、不純物は検出されな
かった。尚、グロ−放電質量分析の検出限界は、鉄、ニ
ッケル、銅いずれも１０ｐｐｂ以下である。Example 1 A graphite material (material name: EGF-262 manufactured by Nippon Carbon Co., Ltd.) processed into a crucible shape having a diameter of 500 mm and a height of 400 mm was used in a hydrogen chloride gas atmosphere at 200
Purification treatment was performed at 0 ° C. to obtain a high-purity graphite crucible. In this graphite crucible, at 1400 ° C. and a reduced pressure of 50 torr,
Hydrogen chloride and hydrogen gas of 10% by volume with respect to the flow rate of propane were introduced for 3 hours to obtain a pyrolytic carbon-coated graphite crucible.
As a result of measuring the purity of the obtained pyrolytic carbon by glow-discharge mass spectrometry, impurities were not detected within the detection limit range. The detection limit of the glow discharge mass spectrometry is 10 ppb or less for all of iron, nickel and copper.
【００２０】[0020]
【比較例１】実施例１における塩化水素の量を１％とす
る以外は、全て実施例１と同様にして熱分解炭素被覆黒
鉛ルツボを得た。実施例１と同様にして熱分解炭素の純
度を測定した結果、不純物として、鉄３．１ｐｐｍ，ニ
ッケル４１ｐｐｂ，銅１．１ｐｐｍが検出された。Comparative Example 1 A pyrolytic carbon-coated graphite crucible was obtained in the same manner as in Example 1, except that the amount of hydrogen chloride in Example 1 was 1%. As a result of measuring the purity of the pyrolytic carbon in the same manner as in Example 1, iron 3.1 ppm, nickel 41 ppb, and copper 1.1 ppm were detected as impurities.
【００２１】[0021]
【実施例２】直径８００ｍｍ、高さ５００ｍｍのルツボ
形状に加工した炭素繊維強化炭素材料（製品名称：ＣＣ
Ｍ−１９０Ｃ 日本カ−ボン（株）製）を実施例１と同
様に処理して高純度の炭素繊維強化炭素ルツボを得た。
この炭素繊維強化炭素ルツボに、１５００℃，減圧３０
ｔｏｒｒにおいて、プロパン流量に対し２０容量％の塩
化水素と水素を流入させ、熱分解炭素被覆炭素繊維強化
炭素ルツボを得た。これを実施例１と同様にして分析
し、測定した結果、検出限界の範囲内では検出されなか
った。Example 2 Carbon fiber reinforced carbon material (product name: CC) processed into a crucible shape with a diameter of 800 mm and a height of 500 mm
M-190C manufactured by Nippon Carbon Co., Ltd. was treated in the same manner as in Example 1 to obtain a high-purity carbon fiber reinforced carbon crucible.
In this carbon fiber reinforced carbon crucible, 1500 ℃, reduced pressure 30
At torr, 20% by volume of hydrogen chloride and hydrogen with respect to the flow rate of propane was introduced to obtain a pyrolytic carbon-coated carbon fiber-reinforced carbon crucible. As a result of analyzing and measuring this in the same manner as in Example 1, it was not detected within the detection limit range.
Claims (3)
雰囲気で、原料ガスである炭化水素ガス、キャリアガス
である水素ガスと同時に塩化水素ガスを流入させ、熱分
解炭素または黒鉛を炭素材料に被覆させることを特徴と
する熱分解炭素または黒鉛被覆炭素材料の製造方法。1. A pyrolysis carbon or graphite is made into a carbon material by inflowing a hydrocarbon gas, which is a raw material gas, and a hydrogen gas, which is a carrier gas, into a carbon material at a temperature of 1200 ° C. or more under reduced pressure. A method for producing a pyrolytic carbon or a graphite-coated carbon material, which comprises coating the carbonaceous material on the surface.
る前に、炭素材料を製品形状に加工し、ハロゲンガス雰
囲気中、１５００℃以上の温度で熱処理して純化する熱
分解炭素または黒鉛被覆炭素材料の製造方法。2. The pyrolytic carbon or graphite-coated carbon obtained by processing a carbon material into a product shape and heat-treating at a temperature of 1500 ° C. or higher in a halogen gas atmosphere to purify the carbon material before coating with the pyrolytic carbon according to claim 1. Material manufacturing method.
化水素ガスの量を炭化水素ガスに対して５容量％以上と
する熱分解炭素または黒鉛被覆炭素材料の製造方法。3. The method for producing a pyrolytic carbon or graphite-coated carbon material according to claim 1, wherein the amount of hydrogen chloride gas is 5% by volume or more with respect to the hydrocarbon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001382813A JP2003183076A (en) | 2001-12-17 | 2001-12-17 | Method for manufacturing pyrolytic carbon or graphite- coated carbon material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001382813A JP2003183076A (en) | 2001-12-17 | 2001-12-17 | Method for manufacturing pyrolytic carbon or graphite- coated carbon material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003183076A true JP2003183076A (en) | 2003-07-03 |
Family
ID=27593040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001382813A Pending JP2003183076A (en) | 2001-12-17 | 2001-12-17 | Method for manufacturing pyrolytic carbon or graphite- coated carbon material |
Country Status (1)
| Country | Link |
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| JP (1) | JP2003183076A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008222456A (en) * | 2007-03-08 | 2008-09-25 | Ibiden Co Ltd | Carbon composite member |
| JP2014084264A (en) * | 2012-10-26 | 2014-05-12 | Shin Etsu Chem Co Ltd | Member for silicon oxide production device, silicon oxide production device and method of forming coat |
| KR20210007905A (en) * | 2019-07-12 | 2021-01-20 | 이비덴 가부시키가이샤 | Carbon composite material |
| CN115231930A (en) * | 2022-07-21 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | C/C composite material anti-oxidation coating process and coating |
-
2001
- 2001-12-17 JP JP2001382813A patent/JP2003183076A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008222456A (en) * | 2007-03-08 | 2008-09-25 | Ibiden Co Ltd | Carbon composite member |
| JP2014084264A (en) * | 2012-10-26 | 2014-05-12 | Shin Etsu Chem Co Ltd | Member for silicon oxide production device, silicon oxide production device and method of forming coat |
| KR20210007905A (en) * | 2019-07-12 | 2021-01-20 | 이비덴 가부시키가이샤 | Carbon composite material |
| KR102406281B1 (en) | 2019-07-12 | 2022-06-10 | 이비덴 가부시키가이샤 | Carbon composite material |
| CN115231930A (en) * | 2022-07-21 | 2022-10-25 | 青岛晶易新材料科技股份有限公司 | C/C composite material anti-oxidation coating process and coating |
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