JPS62158106A - Production of graphite material for coating silicon carbide - Google Patents
Production of graphite material for coating silicon carbideInfo
- Publication number
- JPS62158106A JPS62158106A JP60297269A JP29726985A JPS62158106A JP S62158106 A JPS62158106 A JP S62158106A JP 60297269 A JP60297269 A JP 60297269A JP 29726985 A JP29726985 A JP 29726985A JP S62158106 A JPS62158106 A JP S62158106A
- Authority
- JP
- Japan
- Prior art keywords
- coke
- graphite material
- thermal expansion
- crushing
- sic
- 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.)
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- 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ＳｉＣ被覆用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 graphite material for SiC coating.
（従来の技術）
一般の黒鉛材は２例えば製鋼用電極のように熱膨張係数
を少さくして（２Ｘ １０−’／’Ｃ）耐熱衝撃性の大
きくしたものが用いられるが、ガラス封着用治具、シリ
コンウエノ１−のエピタキシャル処理用のサセプタ等に
用いられるＳｉＣ被覆用の黒鉛材は、 ５ｉＣＯ熱膨張
係数より大きくしないとＳｉＣ被膜に亀裂が入汎その寿
命を短くする。５ｉＣＯ熱膨張係数は５．０〜５．ｌＸ
１０／℃であるから、黒鉛材の熱膨張係数は５． Ｉ
Ｘ １０−’／’Ｃ以上あることが必要であり、更に等
方性であることが望まれる。(Prior art) General graphite materials with a low coefficient of thermal expansion (2X 10-'/'C) and high thermal shock resistance are used, for example, in electrodes for steel manufacturing, but they are not suitable for glass sealing. Graphite materials for SiC coating used in susceptors for epitaxial processing of silicon urethane, etc. must have a coefficient of thermal expansion greater than 5iCO, otherwise cracks will enter the SiC coating and shorten its life. 5iCO thermal expansion coefficient is 5.0-5. lX
10/℃, the thermal expansion coefficient of graphite material is 5. I
It is necessary that X 10-'/'C or more, and it is further desired that it is isotropic.
（発明が解決しようとする問題点） 黒鉛材の原料は一般的にコークスが用いられ。(Problem to be solved by the invention) Coke is generally used as the raw material for graphite material.
特にニードルコークスが多用されている。ニードルコー
クスを原料としたものは高温度の熱処理（黒鉛化処理）
により黒鉛の結晶が発達し易く。In particular, needle coke is widely used. Products made from needle coke are subjected to high temperature heat treatment (graphitization treatment)
This makes it easier for graphite crystals to develop.
結晶の熱膨張係数は六角網状の層平面方向（ａ軸方向）
ではＯに近く層間方向（Ｃ軸方向）では２８ Ｘ １０
−’／℃にも達することがあり異方性が極めて大きい。The thermal expansion coefficient of the crystal is in the plane direction of the hexagonal network layer (a-axis direction)
28 x 10 in the interlayer direction (C axis direction) near O
-'/°C, and the anisotropy is extremely large.
このためコークス粉の粒度を調整したシ、生コークス、
石炭等を添加したり、原料を特殊処理したものを用いる
等して成形粉を得、これを静水加圧成形する方法が採用
されている。このようにして得られた黒鉛材は１曲げ強
さ、電気比抵抗等の異方性は小さくなるが、熱膨張係数
はせいぜい４．５〜５． ＯＸ １０−６／℃程度であ
、りＳｉＣ被覆用の黒鉛材としては未だ不十分である。For this reason, raw coke, which has adjusted the particle size of coke powder,
A method has been adopted in which molding powder is obtained by adding coal or the like or using specially treated raw materials, and then isostatically press molding the powder. The graphite material thus obtained has a low bending strength and anisotropy such as electrical resistivity, but a thermal expansion coefficient of 4.5 to 5. OX is about 10-6/°C, which is still insufficient as a graphite material for SiC coating.
本発明は上記した問題点を解消し、熱膨張係数が５．５
Ｘ １０＝／℃以上のＳｉＣ被旋用の黒鉛材を提供す
ることを目的とする。The present invention solves the above problems and has a thermal expansion coefficient of 5.5.
The object of the present invention is to provide a graphite material for SiC turning with a temperature of X10=/°C or higher.
（問題点を解決するだめの手段）
本発明は、単位セルの大きさが３０μｍ以下のモザイク
コークスを平均粒径１５μｍ以下に粉砕し、結合材を加
えて混練し２次いで粉砕、静水加圧成形、焼成及び黒鉛
化することを特徴とするＳｉＣ被覆用黒鉛材の製造法に
関する。(Means for Solving the Problem) The present invention involves crushing mosaic coke with a unit cell size of 30 μm or less to an average particle size of 15 μm or less, adding a binder, kneading, and then crushing and isostatic pressing. , relates to a method for producing a graphite material for SiC coating, which is characterized by firing and graphitizing.
本発明において、モザイクコークスとは、コークス組織
の発達したニードル部分（針状部分）を含まず、コーク
ス組織の発達が特になされていない実質的にモザイク構
造だけからなるコークスであシ、原料のピッチにキノリ
ンネ溶分（ＱＩ酸成分゛を多く含むものを用いて得られ
るものである。In the present invention, mosaic coke refers to coke that does not contain needle parts (needle-shaped parts) with developed coke structures, and consists essentially only of mosaic structures without particularly developed coke structures, and is composed of coke made from raw material pitch. It is obtained by using a quinoline solution (containing a large amount of QI acid component).
ピッチからコークスを得る過程で熱処理され。Heat treated in the process of obtaining coke from pitch.
メソフェーズが生成し、これが多数個合体してコークス
の流れ模様の出来たものがニードルコークスであシ、メ
ソフェーズがＱＩ酸成分フリーカーボン等によって合体
するのを抑制され、そのまま炭化されたものがモザイク
コークスであると考えられる。Needle coke is produced when mesophase is generated and a large number of them coalesce to create a coke flow pattern, and mosaic coke is when mesophase is suppressed from coalescing by QI acid component-free carbon, etc. and is carbonized as it is. It is thought that.
モザイクコークスは、切断面を鏡面研磨して顕微鏡で観
察すると、第１図に示すように球状の枠１が見え、その
中に２本程度の気孔２が存在する。When the cut surface of mosaic coke is mirror-polished and observed under a microscope, a spherical frame 1 can be seen as shown in FIG. 1, and about two pores 2 are present within the spherical frame 1.
前記球状の枠１で囲まれた部分を本発明では単位セルと
呼称する。尚３はフリーカーボンの層である。この単位
セルの大きさが３０μｍを越えると平均粒径１５μｍ以
下のコークス粉を得ることが難しい。コークス粉が平均
粒径１５μｍを越えるとＳｉＣ被覆用黒鉛材として充分
な密度及び強度が得られず、ピッチ含浸等の工程追加が
必要となる。In the present invention, the portion surrounded by the spherical frame 1 is referred to as a unit cell. Note that 3 is a free carbon layer. If the size of this unit cell exceeds 30 μm, it is difficult to obtain coke powder with an average particle size of 15 μm or less. If the average particle size of the coke powder exceeds 15 μm, sufficient density and strength will not be obtained as a graphite material for SiC coating, and additional steps such as pitch impregnation will be required.
上記黒鉛材の密度は１．８０ ｇ／ａｍ３以上及び強度
は曲げ強さとして５００ ｋｇ／ｃ−以上あることが好
ましい。又、コークスは黒鉛化等の工程で気孔が増大し
ないように灰分等の不純物は出来るだけ少ないこと（０
，５重量％以下）が好ましい。黒鉛材の気孔は熱膨張を
吸収するからである。The graphite material preferably has a density of 1.80 g/am3 or more and a bending strength of 500 kg/c- or more. In addition, impurities such as ash should be as low as possible in coke to prevent pores from increasing during processes such as graphitization (0
, 5% by weight or less) is preferred. This is because the pores of the graphite material absorb thermal expansion.
結合材は公知のタールピッチ、コールタール等を用いる
。コークス粉等の骨材と結合材との混練及び成形粉を得
るための粉砕は公知の方法による。As the binding material, known tar pitch, coal tar, etc. are used. Kneading of aggregate such as coke powder and binder and pulverization to obtain molded powder are performed by known methods.
成形は静水加圧成形により黒鉛結晶のＣ軸方向をランダ
ムに分布させ、配向性を小さくする。焼成及び黒鉛化は
公知の方法による。The forming is carried out by hydrostatic pressing to randomly distribute the C-axis direction of the graphite crystals, thereby reducing the orientation. Firing and graphitization are performed by known methods.
（作用）
上記のように構成すると黒鉛結晶のＣ軸方向は黒鉛材の
中でランダムに分布し、熱膨張係数はどの方向でも５．
５ Ｘ １０””／℃以上になり、 ８ｉＣ被覆の際及
び被覆後の繰返しの使用においてＳｉＣ被膜に亀裂を入
り難くする。(Function) With the above structure, the C-axis direction of the graphite crystal is randomly distributed in the graphite material, and the coefficient of thermal expansion is 5.5 in any direction.
5 x 10''/°C or higher, making it difficult for the SiC coating to crack during coating with 8iC and during repeated use after coating.
（実施例） 以下、実施例及び比較例を説明する。(Example) Examples and comparative examples will be described below.
ニードルコークス及び単位セルの大きさが第１表に示す
値のモザイクコークスを用意した。まずこれらコークス
を２８００℃で黒鉛化処理して黒鉛の結晶子の大きさく
Ｌｃ ）をＸ線回折法で求めたところ第１表に示す値と
なり、モザイクコークスはＬｃが小さく配向性が小さい
ことが示される。Needle coke and mosaic coke having unit cell sizes shown in Table 1 were prepared. First, these cokes were graphitized at 2800°C and the size of graphite crystallites (Lc) was determined by X-ray diffraction method, and the values shown in Table 1 were obtained, indicating that mosaic coke has a small Lc and low orientation. shown.
次に黒鉛化しないコークスを衝撃粉砕機で粉砕して第１
表に示す平均粒径のコークス粉を得た。Next, the non-graphitized coke is crushed using an impact crusher and
Coke powder having the average particle size shown in the table was obtained.
第１表
上記コークス粉に結合材としてタールピッチ（ＪＩＳ
Ｋ ２４３９．一般用、中ピツチ〕を加え。Table 1 Tar pitch (JIS
K 2439. General purpose, medium pitch] added.
それぞれワーナー型埠和機で加熱混練し、冷却後粉砕し
て成形粉を得、該成形粉をゴム型に入れ静水加圧成形し
２次いで焼成炉で１０００℃に焼成し、電気炉で２８０
０℃で黒鉛化した。得られた黒鉛材の物理特性を第２表
に示す。Each was heated and kneaded in a Warner-type mixing machine, cooled and pulverized to obtain a molded powder.The molded powder was placed in a rubber mold and subjected to isostatic pressure molding.Then, it was fired in a kiln to 1000°C, and then in an electric furnace to 280°C.
It was graphitized at 0°C. Table 2 shows the physical properties of the graphite material obtained.
以ｒ’ 、−、”１
第２表
第２表中ＣＴＣは熱膨張係数であシ実施例の黒鉛材は５
．５ Ｘ １０−’／℃以上の値を示す。又実施例の黒
鉛材は比較例の黒鉛材よシかさ密度及び曲げ強さが大き
く、異方性比が小さいことが示される。Hereinafter, r', -, "1 In Table 2, CTC is the coefficient of thermal expansion, and the graphite material in the example is 5.
．． Indicates a value of 5 x 10-'/°C or more. It is also shown that the graphite material of the example has higher bulk density and bending strength than the graphite material of the comparative example, and has a lower anisotropy ratio.
次に上記黒鉛材をそれぞれ３００謳φＸ１０ｍｍｔの円
板に加工し、ＣＶＤ炉に入れてキャリアガスのＨ２を毎
分２００１の速度で通じながら、濃度が１、 ＯＸ １
０”−３ｍｏｌ ／ ｌ ” Ｈ２のＣＨａＳｉＣ１ｓ
ガスを通じ。Next, each of the above-mentioned graphite materials was processed into a disk of 300 mm φ x 10 mm, and placed in a CVD furnace while passing H2 as a carrier gas at a rate of 200 mm per minute until the concentration was 1 and OX 1.
CHaSiC1s of 0”-3mol/l”H2
Through gas.
黒鉛材を１５００℃に加熱して表面に４０μｍのＳｉＣ
被膜を形成した。このＳｉＣ被覆黒鉛材のＳｉＣ被覆直
後におけるＳｉＣ被膜のキレツ発生の有無及び１５００
℃−室温の冷熱サイクル試験における耐用回数（ＳｉＣ
被膜に亀裂が発生するまでの回数）を求めた結果を第３
表に示す。Graphite material is heated to 1500℃ and 40μm SiC is applied to the surface.
A film was formed. The presence or absence of cracks in the SiC coating of this SiC-coated graphite material immediately after coating with SiC, and the
℃-room temperature thermal cycle test (SiC
The results of determining the number of times it takes for cracks to occur in the coating are shown in the third
Shown in the table.
第３表
第３表から明らかなように、モザイクコークスを用いた
ものはＳｉＣ被覆直後に亀裂が発生することはなく、実
施例のものは耐用回数が大きいことが示される。Table 3 As is clear from Table 3, the products using mosaic coke did not develop cracks immediately after coating with SiC, indicating that the products of Examples had a long service life.
（発明の効果）
本発明によれば、熱膨張係数が５．５ Ｘ １０−’／
’Ｃ以上でかつかさ密度及び曲げ強さが大きく等方性の
ＳｉＣ被覆用黒鉛材が得られ、エピタキシャル成長用の
サセプタ等に用いてその寿命を延長することが可能にな
る。(Effect of the invention) According to the invention, the coefficient of thermal expansion is 5.5 x 10-'/
It is possible to obtain an isotropic graphite material for SiC coating, which has a temperature of C or more and has a large bulk density and bending strength, and can be used as a susceptor for epitaxial growth to extend its life.
第１図は本発明に用いるモザイクコークスの粒子構造の
モデルを示す図である。
符号の説明
１・・・枠 ２・・・気孔３・・・フ
リーカーボン
代理人 弁理士 若 林 邦 彦
手続補正書（自発）
昭和 ６１年 ２ ｎ２７日
特ｌｌν庁長官殿 ・くし１、コド
件の表示
昭和６０年特許願第２９７２６９号
２、発明の名称
ＳｉＣ被覆用黒鉛材の製造法
３、補正をする者
小ｆ↑との関係 特許出願人
名 称 （４４５） 日立化成工業株式会社５、補正の
対象
１５Ｘ１０”’／’Ｃであり、」と訂正します。
手続補正書（自発）
昭ｔａ ６１年 （３Ｊ１１２ Ｇ
、〆一
■、小事件表示
昭和６０年特許願第２９７２６９号
２、発明の名称
ＳｉＣ被覆用黒鉛材の製造法
３、補正をする者
Ｉｃ件との関係 特許出願人
名 称 ＋４４５１ 日立化成工業株式会社５、補正の
ヌｊ象FIG. 1 is a diagram showing a model of the particle structure of mosaic coke used in the present invention. Explanation of symbols 1... Frame 2... Pore 3... Free carbon agent Patent attorney Kunihiko Wakabayashi Procedural amendment (voluntary) 2/27/1988 To the Commissioner of the Special Agency - Comb 1, Kodo matter Indication of 1985 Patent Application No. 297269 2, Name of the invention Process for manufacturing graphite material for SiC coating 3, Relationship with the person making the amendment Small f↑ Patent applicant name (445) Hitachi Chemical Co., Ltd. 5, Amendment The target is 15X10''/'C,'' and am corrected. Procedural amendment (voluntary) Showa 1961 (3J112 G, 〆1■, Small case indication 1985 Patent Application No. 297269 2, Title of invention Method for manufacturing graphite material for SiC coating 3, Person making the amendment Ic matter Relationship with Patent Applicant Name +4451 Hitachi Chemical Co., Ltd. 5, Amendment Nuj
Claims (1)
スを平均粒径１５μｍ以下に粉砕し、結合材を加えて混
練し、次いで粉砕、静水加圧成形、焼成及び黒鉛化する
ことを特徴とするＳｉＣ被覆用黒鉛材の製造法。1. SiC characterized by pulverizing mosaic coke with a unit cell size of 30 μm or less to an average particle size of 15 μm or less, adding a binder and kneading, followed by crushing, isostatic pressing, sintering, and graphitization. Manufacturing method of graphite material for coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60297269A JPS62158106A (en) | 1985-12-30 | 1985-12-30 | Production of graphite material for coating silicon carbide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60297269A JPS62158106A (en) | 1985-12-30 | 1985-12-30 | Production of graphite material for coating silicon carbide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62158106A true JPS62158106A (en) | 1987-07-14 |
| JPH0580405B2 JPH0580405B2 (en) | 1993-11-09 |
Family
ID=17844331
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60297269A Granted JPS62158106A (en) | 1985-12-30 | 1985-12-30 | Production of graphite material for coating silicon carbide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62158106A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9677430B2 (en) | 2011-03-01 | 2017-06-13 | General Electric Technology Gmbh | Combined cycle power plant |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5358496A (en) * | 1976-11-05 | 1978-05-26 | Agency Of Ind Science & Technol | Production of graphite substrate for oxidation resistant coating |
| JPS605523A (en) * | 1983-06-23 | 1985-01-12 | Fujitsu Ltd | Correction for mask |
-
1985
- 1985-12-30 JP JP60297269A patent/JPS62158106A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5358496A (en) * | 1976-11-05 | 1978-05-26 | Agency Of Ind Science & Technol | Production of graphite substrate for oxidation resistant coating |
| JPS605523A (en) * | 1983-06-23 | 1985-01-12 | Fujitsu Ltd | Correction for mask |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9677430B2 (en) | 2011-03-01 | 2017-06-13 | General Electric Technology Gmbh | Combined cycle power plant |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0580405B2 (en) | 1993-11-09 |
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