JPH03275579A - Production of film coated with silicon carbide - Google Patents
Production of film coated with silicon carbideInfo
- Publication number
- JPH03275579A JPH03275579A JP7444890A JP7444890A JPH03275579A JP H03275579 A JPH03275579 A JP H03275579A JP 7444890 A JP7444890 A JP 7444890A JP 7444890 A JP7444890 A JP 7444890A JP H03275579 A JPH03275579 A JP H03275579A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- substrate
- organopolysiloxane
- base plate
- reduced pressure
- 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
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims description 46
- 229910010271 silicon carbide Inorganic materials 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 38
- 238000000576 coating method Methods 0.000 claims abstract description 38
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims description 61
- 239000012466 permeate Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 10
- 239000010439 graphite Substances 0.000 abstract description 10
- 229910002804 graphite Inorganic materials 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract description 5
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 abstract description 5
- 125000003342 alkenyl group Chemical group 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract description 3
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 abstract description 2
- 125000000217 alkyl group Chemical group 0.000 abstract description 2
- 125000003118 aryl group Chemical group 0.000 abstract description 2
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 abstract description 2
- 125000000725 trifluoropropyl group Chemical group [H]C([H])(*)C([H])([H])C(F)(F)F 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 125000004432 carbon atom Chemical group C* 0.000 abstract 1
- 125000001183 hydrocarbyl group Chemical group 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 229910052710 silicon Inorganic materials 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 239000010703 silicon Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 3
- -1 polysiloxane Polymers 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000005372 silanol group Chemical group 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Laminated Bodies (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
【発明の詳細な説明】
（ａ業上の利用分野）
本発明は炭化けい素被覆膜の製造方法、特には基材の表
面に炭化けい素被覆膜を設けてなる、半導体プロセス治
具として有用とされる炭化けい素被覆材料の製造方法に
関するものである。Detailed Description of the Invention (Field of Application in Industry A) The present invention relates to a method for manufacturing a silicon carbide coating film, and particularly to a semiconductor process jig in which a silicon carbide coating film is provided on the surface of a base material. The present invention relates to a method for producing a silicon carbide coating material that is useful as a silicon carbide coating material.
（従来の技術）
従来、半導体プロセス治具としては黒鉛などのような耐
熱性のすぐれた基板の表面に炭化けい素を被覆したもの
が多く使用されており、これを使用すれば１）基板材料
から発生する粉じんや不純物ガスによる汚染が防止され
る、２）このものがすぐれた耐酸化性、耐摩耗性、高温
強度性を有しているので長期間使用することができると
いう有利性が与えられる。(Prior art) Conventionally, semiconductor process jigs have often been made of graphite or other heat-resistant substrates coated with silicon carbide. 2) This product has the advantage of being able to be used for a long time because it has excellent oxidation resistance, abrasion resistance, and high temperature strength. It will be done.
（発明が解決しようとする！！題）
しかし、この基板に炭化けい素を被覆したものは、基板
と炭化けい素抜覆膜との熱膨張率が相違すること、また
基板と炭化けい素抜覆膜との密着性が不充分であるため
に、くり返して使用していると基板と炭化けい素抜覆膜
との境界にクラックや剥離が発生し、使用できなくなる
という不利がある。(Problem to be solved by the invention!!) However, when this substrate is coated with silicon carbide, the thermal expansion coefficients of the substrate and the silicon carbide-free coating film are different, and the substrate and the silicon carbide-free coating film are different. Since the adhesion with the coating film is insufficient, repeated use may cause cracks or peeling at the boundary between the substrate and the silicon carbide-free coating film, making it unusable.
（！Ｉ！！！を解決するための手段）
本発明はこのような不利を解決した炭化けい素抜覆膜の
製造方法（関するものであり、これは基材の表面にオル
ガノポリシロキサン層を設け、これを加熱して該基板上
に炭化けい素を被覆することを特徴とするものである。(Means for Solving !I!!!) The present invention relates to a method for producing a silicon carbide-free coating film that solves these disadvantages. The method is characterized in that silicon carbide is coated on the substrate by heating the silicon carbide.
すなわち、本発明者らは基材に炭化けい素抜覆膜を設け
た炭化けい素抜覆膜品における基材と炭化けい素抜覆膜
との境界面におけるクラック発生や剥離を防止する方法
について種々検討した結果、基材表面に予じめオルガノ
ポリシロキサン層を設け、このオルガノポリシロキサン
層を加熱分解し、該基板上に炭化けい素抜覆膜を設けれ
ば炭化けい素抜覆膜が基板とよく密着するので基板と炭
化けい素抜覆膜との境界におけるクラック発生や剥離が
なくなり、これを半導体プロセス治具として使用したと
きにくり返し使用することができるようになるというこ
とを見出し、ここに使用するオルガノポリシロキサンの
種類、使用量などについての研究を進めて本発明を完成
させた。That is, the present inventors have proposed a method for preventing cracking and peeling at the interface between the base material and the silicon carbide-free coating in a silicon carbide-free coating product in which a silicon carbide-free coating is provided on the base material. As a result of various studies, we found that if an organopolysiloxane layer is previously provided on the surface of a substrate, this organopolysiloxane layer is thermally decomposed, and a silicon carbide release coating is provided on the substrate, the silicon carbide release coating can be formed. It was discovered that since it adheres well to the substrate, there is no cracking or peeling at the boundary between the substrate and the silicon carbide-extracted coating film, and it becomes possible to use it repeatedly when used as a semiconductor process jig. The present invention was completed by conducting research on the type and amount of organopolysiloxane used here.
以下にこれをさらに詳述する。This will be explained in further detail below.
（作用）
本発明による炭化けい素板Ｎ膜の製造は、基板に予じめ
オルガノポリシロキサン層を設け、これを加熱して該基
板上に炭化けい素を被覆することによって行なわれる。(Function) The silicon carbide plate N film according to the present invention is manufactured by providing an organopolysiloxane layer on a substrate in advance and heating the layer to coat silicon carbide on the substrate.
本発明において使用される基板は耐熱性のすぐれたもの
とすることが必要とされるが、これは公知のものでよく
、したがってこれには黒鉛、炭化けい素、黒鉛と炭化け
い素との混合物、けい素と炭化けい素との混合物などで
作られたものとすればよい、また、この基板の形状は目
的に応じ任意のものとすればよく、したがって特に制限
はなく、これは例えばボート状、板状、円盤状とすれば
よいが、不純物による汚染防止ということかはできるだ
け高純度のものからなるものとすることがよい。The substrate used in the present invention is required to have excellent heat resistance, and may be of any known type, such as graphite, silicon carbide, or a mixture of graphite and silicon carbide. The substrate may be made of a mixture of silicon and silicon carbide, etc. The shape of this substrate may be arbitrary depending on the purpose, so there is no particular restriction, and it may be shaped like a boat, for example. , a plate shape, or a disk shape, but it is preferable to use a material with as high purity as possible to prevent contamination by impurities.
本発明においてはこの基板の上に予じめオルガノポリシ
ロキサン層が形成されるのであるが、これは一般式 Ｒ
ｎ５１０ユ で示されＲがメチル基、エチル基、プロピ
ル基、ブチル基などのアルキル基、ビニル基、アリル基
などのアルケニル基、フェニル基、トリル基などのアリ
ール基、この炭素原子に結合している水素原子の一部ま
たは全部をハロゲン原子、シアノ基などで置換したクロ
ロメチル基、トルフルオロプロピル基、シアノエチル基
などから選択される同一または異種の非置換または置換
１価炭化水素基、ｎが４以下の正の数であるものとすれ
ばよく、この分子鎖は直鎖状だけでなく、分枝鎖をもつ
ものであってもよいが、コストの面からは直鎮状のジメ
チルポリシロキサンとすることが有利とされる。In the present invention, an organopolysiloxane layer is formed on this substrate in advance, and this layer has the general formula R
n510U, and R is an alkyl group such as a methyl group, ethyl group, propyl group, or butyl group, an alkenyl group such as a vinyl group or an allyl group, an aryl group such as a phenyl group or a tolyl group, and is bonded to this carbon atom. the same or different unsubstituted or substituted monovalent hydrocarbon groups selected from chloromethyl groups, trifluoropropyl groups, cyanoethyl groups, etc. in which some or all of the hydrogen atoms in the group are substituted with halogen atoms, cyano groups, etc., where n is It may be a positive number of 4 or less, and the molecular chain may be not only linear but also branched, but from the cost perspective, linear dimethylpolysiloxane is preferable. It is considered advantageous to do so.
また、このオルガノポリシロキサンの粘度には特に制限
はないが、２５℃における粘度が１００ｃＰ未渦のもの
はこれを基板に塗布すると浸透速度が大きすぎて、後述
する炭化けい素抜覆形成後の炭化けい素抜覆の膜厚の制
御が困難となるので１０ＤｃＰ以上のものとすることが
よく、これは特に１．０００，０００ｃＰ〜生ゴム状の
ものをトルエンやキシレンなどの有機溶剤に溶解して粘
度を１００〜１０．０００ｃＰになるようにしたものと
することがよい。There is no particular limit to the viscosity of this organopolysiloxane, but if the viscosity at 25°C is 100 cP without vortex, the permeation rate will be too high when applied to a substrate, and after forming silicon carbide as described below. Since it is difficult to control the film thickness for silicon carbide removal, it is best to use a film of 10 DcP or more. It is preferable to set the viscosity to 100 to 10.000 cP.
なお、このオルガノポリシロキサンは特に架橋（硬化）
反応させる必要はないが、これを硬化させる場合にはこ
れに有機過酸化物を添加して基板Ｃ塗布後に１５０〜２
５０℃に加熱してオルガノポリシロキサンを架橋させる
か、あるいはこのオルガノポリシロキサンを分子中にア
ルケニル基を含有するオルガノポリシロキサンと分子中
にけい素原子に直接結合している水素原子（−ＳＩＨ）
を有するオルガノハイドロジエンポリシロキサンとの混
合物とし、これに触媒としての白金系化合物を添加した
ものを基板に塗布後、１００〜２００℃に加熱し付加反
応させて硬化させる方法、さらにはこのオルガノボリシ
ロキサンを分子鎖末端にシラノール基を有するオルガノ
ポリシロキサンと分子中に前記したＳｉＨ基を有するオ
ルガノハイドロジエンポリシロキサンとの混合物とし、
これに触媒としての有機すず化合物などを添加したもの
を基板に塗布後に１００〜２００℃に加熱し縮合反応に
よって硬化させるようにしてもよい。In addition, this organopolysiloxane is particularly suitable for crosslinking (curing).
It is not necessary to react, but if you want to cure it, add an organic peroxide to it and after coating the substrate C,
Either cross-link the organopolysiloxane by heating to 50°C, or combine this organopolysiloxane with an organopolysiloxane containing an alkenyl group in the molecule and a hydrogen atom (-SIH) directly bonded to a silicon atom in the molecule.
A method in which a mixture of organohydrodiene polysiloxane having The siloxane is a mixture of an organopolysiloxane having a silanol group at the end of the molecular chain and an organohydrodiene polysiloxane having the aforementioned SiH group in the molecule,
An organic tin compound or the like as a catalyst may be added to this, and after being applied to the substrate, it may be heated to 100 to 200°C and cured by a condensation reaction.
このオルガノポリシロキサンの基板への塗布はドクター
ブレード法、ディッピング法、スプレー法、スピンナー
法など任意の方法で行なえばよいが、このオルガノポリ
シロキサンの塗布量は得られる炭化けい葉液覆膜が所定
の厚みになるように調整する。一般には炭化けい葉液覆
膜の厚みは５０〜３００μｍである。したがってここに
塗布するオルガノポリシロキサンの厚みは有ｓ！溶剤を
除去した固形量で基板へのしみ込みや反応による減量を
勘案して７５〜４５０μｍを目安とするような量とすれ
ばよい。このようにして基板上に塗布されたオルガノポ
リシロキサンは塗布後５〜６０分間そのまま静置してオ
ルガノポリシロキサンを基板表面より内部に浸透させる
ことがよく、そのためには基板を減圧下においてオルガ
ノポリシロキサンの内部浸透を促進させるようにしても
よい、なお、基板上に塗布されたオルガノポリシロキサ
ンは架橋（硬化）させてもよく、この場合にはこのオル
ガノポリシロキサンに添加される硬化用触媒の種類に応
じた前記した温度にこれを加熱して架橋（硬化）させれ
ばよい。This organopolysiloxane may be applied to the substrate by any method such as a doctor blade method, dipping method, spray method, or spinner method. Adjust so that the thickness is as follows. Generally, the thickness of the carbonized silica leaf liquid coating film is 50 to 300 μm. Therefore, the thickness of the organopolysiloxane applied here is very important! The solid amount from which the solvent has been removed may be determined to be approximately 75 to 450 μm, taking into consideration penetration into the substrate and weight loss due to reaction. The organopolysiloxane coated on the substrate in this way is often left undisturbed for 5 to 60 minutes after application to allow the organopolysiloxane to penetrate from the surface of the substrate into the interior. In addition, the organopolysiloxane coated on the substrate may be crosslinked (cured), and in this case, the curing catalyst added to the organopolysiloxane may be This may be crosslinked (cured) by heating to the above-mentioned temperature depending on the type.
このようにしてオルガノポリシロキサン層を設けた基板
は、ついでこれを加熱分解して該基板上に炭化けい素を
被覆するのであるが、これらの場合における反応条件は
反応装置内を１〜１００）−ルに減圧して１，１００〜
１，５００ ℃に加熱するようにし、この加熱時間はオ
ルガノポリシロキサンの分解と形成した炭化けい素を熟
成させるということから３０分〜３時間程度とすればよ
く、これによれば炭化けい素が５０〜３００μｍの厚さ
で被覆されたものを得ることができ、この炭化けい素被
膜が基板上に良好な密着性をもって形成されるので、炭
化けい素被膜が基板との界面でクラックを発生したり、
剥離することがなくなり、これをくり返し使用すること
ができるとう有利性が与えられる。The substrate provided with the organopolysiloxane layer in this way is then thermally decomposed to coat silicon carbide on the substrate, and the reaction conditions in these cases are as follows: - Reduce the pressure to 1,100 ~
The heating time should be about 30 minutes to 3 hours to decompose the organopolysiloxane and age the formed silicon carbide. It is possible to obtain a coating with a thickness of 50 to 300 μm, and this silicon carbide coating is formed on the substrate with good adhesion, so that cracks do not occur at the interface between the silicon carbide coating and the substrate. Or,
There is no peeling, giving the advantage that it can be used repeatedly.
（実施例）
つぎに本発明の実施例、比較例をあげるが、例中の部は
重量部を、粘度は２５℃での測定値を示したものである
。(Example) Next, Examples and Comparative Examples of the present invention will be given. In the examples, parts are parts by weight, and viscosity is a value measured at 25°C.
実施例１
基板として５０Ｘ １５０ Ｘ ５ ａｍの黒鉛基板を
使用し、これに生ゴム状のジメチルポリシロキサンをト
ルエンに５０部濃度に溶解した粘度が１５．０００ｃＰ
の溶液をドクターブレードを用いて厚さ２００μｍに塗
布したのち、室温下に１時間放置してトルエンを蒸発さ
せた。Example 1 A graphite substrate of 50 x 150 x 5 am was used as a substrate, and raw rubber-like dimethylpolysiloxane was dissolved in toluene at a concentration of 50 parts to give a viscosity of 15.000 cP.
The solution was applied to a thickness of 200 μm using a doctor blade, and then left at room temperature for 1 hour to evaporate the toluene.
ついでこれを内径１５０ｍｍ 、長さ１，５００ｍｍの
合成石英管を反応管とする加熱炉に入れ、５ｍｍトール
の減圧下に温度を常温から１，３００℃まで３０分間で
昇温きせて２時間保持したところ、ジメチルポリシロキ
サンが炭化けい素となり、基板上に炭化けい素が７８μ
ｍで被覆されたものが得られたので、室温にまで自然冷
却したのち、これを取り出した。This was then placed in a heating furnace using a synthetic quartz tube with an inner diameter of 150 mm and a length of 1,500 mm as a reaction tube, and the temperature was raised from room temperature to 1,300°C in 30 minutes under reduced pressure of 5 mm Torr and held for 2 hours. As a result, dimethylpolysiloxane turned into silicon carbide, and 78 μm of silicon carbide was deposited on the substrate.
Since a product coated with m was obtained, it was naturally cooled to room temperature and then taken out.
なお、このようにして得られた炭化けい素抜種基板は均
一な表面状態を有しており、１，２００℃から室温まで
１分間で冷却するという急冷を行なっても基板のそりや
、クランク、剥離などの発生が認められず、基板と炭化
けい葉液覆膜とがすぐれた密着性をもって密着している
ことが確認された。The silicon carbide-extracted substrate obtained in this way has a uniform surface condition, and even after rapid cooling from 1,200°C to room temperature in 1 minute, the substrate does not warp or crack. No peeling was observed, and it was confirmed that the substrate and the silicon carbide leaf liquid coating film were in close contact with each other with excellent adhesion.
実施例２
実施例１と同じ黒鉛基板に、分子鎖両末端にシラノール
基を有する、粘度が２．０００ｃｐのジメチルポリシロ
キサン１００部と式
で示されるメチルハイドロジエンポリシロキサン５部お
よびジブチルすずジアセテート１部とからなるシロキサ
ン組成物をトルエン２０部に溶解した溶液を実施例１と
同じ方法で塗布したのち、室温下で３０分間放置後、１
８０℃で２０分間加熱したところ、このオルガノポリシ
ロキサンは架橋されて硬化した。Example 2 On the same graphite substrate as in Example 1, 100 parts of dimethylpolysiloxane with a viscosity of 2.000 cp, which has silanol groups at both ends of the molecular chain, 5 parts of methylhydrodiene polysiloxane represented by the formula, and dibutyltin diacetate were placed. A solution of 1 part of siloxane composition dissolved in 20 parts of toluene was applied in the same manner as in Example 1, and after being left at room temperature for 30 minutes, 1 part of siloxane composition was dissolved in 20 parts of toluene.
When heated at 80° C. for 20 minutes, the organopolysiloxane was crosslinked and cured.
ついで、このものを実施例１と同じ合成石英反応管に入
れ、５ｍｍトールの減圧下に１，３００℃に２時間加熱
し基板上に炭化けい素を被覆した。炭化けい素が厚さ１
４０μｍに被覆されたものが得られたので、室温まで冷
却してからこれを取り出した。Next, this product was placed in the same synthetic quartz reaction tube as in Example 1, and heated at 1,300° C. for 2 hours under a reduced pressure of 5 mm Torr to coat silicon carbide on the substrate. Silicon carbide has a thickness of 1
A product coated with a thickness of 40 μm was obtained, which was cooled to room temperature and then taken out.
このようにして得られた炭化けい素被覆基板は均一な表
面を有するもので、実施例１と同様に急冷しても基板に
そりやクラック、剥離などの発生はなく、基板と炭化け
い素抜覆膜はよく密着していた。The silicon carbide coated substrate obtained in this way has a uniform surface, and as in Example 1, even when rapidly cooled, there is no warping, cracking, or peeling of the substrate, and the silicon carbide is removed from the substrate. The covering film adhered well.
実施例３
実施例１と同じ黒鉛基板に主成分がＣＨ３５ｉＯｓｚａ
からなるシリコーンワニス・ＫＲ２５１［信越化学工業
（株）製、商品名、シリコーン分３０％】をドクターブ
レードを用いて厚さ２００μｍに塗布したのち、室温下
に１時間放置して溶剤を蒸発させた。Example 3 The main component was CH35iOsza on the same graphite substrate as Example 1.
Silicone varnish KR251 [manufactured by Shin-Etsu Chemical Co., Ltd., trade name, silicone content 30%] was applied to a thickness of 200 μm using a doctor blade, and then left at room temperature for 1 hour to evaporate the solvent. .
ついでこのものを実施例１と同じ合成石英反応管に入れ
、ｌ Ｇｅｍトールの減圧下に１，２５０℃の温度で２
時間加熱したところ、基板上に厚さ４８μｍの炭化けい
素抜覆膜が得られた。This product was then placed in the same synthetic quartz reaction tube as in Example 1, and heated at a temperature of 1,250°C under a reduced pressure of 1 Gem Torr.
When heated for a period of time, a silicon carbide-free coating film with a thickness of 48 μm was obtained on the substrate.
この炭化けい素抜覆膜は均一な表面を有しており、実施
例１と同様に急冷しても基板にそりやクラック、剥離な
どの発生はなく、基板と炭化けい素抜覆膜はよく密着し
ていた。This silicon carbide release coating has a uniform surface, and even when rapidly cooled as in Example 1, there is no warping, cracking, or peeling on the substrate, and the substrate and silicon carbide release coating are bonded well. They were in close contact.
比較例
実施例１と同じ黒鉛基板を加熱炉に入れ、この反応室内
に四塩化けい素（ＳＩＣ１１４）６００ＣＣ／分と炭化
水素化合物Ｃ，Ｈ，２００ｃｃ／分を供給し、２０ｍｍ
トールの減圧下に１，３００℃に加熱し、ＣＶＤ法で基
板の上に炭化けい素を１００μ園の厚さに被覆して炭化
けい素被覆基板を作った。Comparative Example The same graphite substrate as in Example 1 was placed in a heating furnace, and 600 cc/min of silicon tetrachloride (SIC114) and 200 cc/min of hydrocarbon compounds C, H were supplied into the reaction chamber.
The substrate was heated to 1,300° C. under a vacuum of Torr, and silicon carbide was coated on the substrate to a thickness of 100 μm using the CVD method to produce a silicon carbide-coated substrate.
ついで、このものを実施例１と同様に急冷したところ、
このものは黒鉛基板と炭化けい素被覆との境界面にクラ
ックが発生したので、黒鉛基板と炭化けい素被覆とは密
着性が不充分なものであることが確認された。Then, when this material was rapidly cooled in the same manner as in Example 1,
In this case, cracks occurred at the interface between the graphite substrate and the silicon carbide coating, so it was confirmed that the adhesion between the graphite substrate and the silicon carbide coating was insufficient.
（発明の効果）
本発明は炭化けい素抜覆膜の製造方法に関するもので、
これは前記したように基板の表面にオルガノポリシロキ
サン層を設け、これを加熱して該基板上に炭化けい素を
形成し、被覆することを特徴とするものであるが、これ
によれば炭化けい素抜覆膜が基板に均一に、かつよく密
着したものが得られ、このものは例えば１，２００℃か
ら常温まで１分間で急冷させても基板にそりが発生した
り、基板と炭化けい素抜覆膜との境界にクラックが発生
し、炭化けい素抜覆膜が基板から剥離するということも
ないので、半導体製造用の治具として、また各種物品の
高温下での使用材料としたときにくり返し使用すること
ができるという有利性が与えられる。(Effects of the Invention) The present invention relates to a method for producing a silicon carbide removal coating,
As described above, this method is characterized by providing an organopolysiloxane layer on the surface of a substrate and heating it to form silicon carbide on the substrate to cover it. A silicon-free coating film that adheres uniformly and well to the substrate can be obtained, and even if this film is rapidly cooled from 1,200°C to room temperature in 1 minute, the substrate will not warp or the silicon carbide will bond to the substrate. Since cracks do not occur at the boundary with the bare coating film and the silicon carbide coating film does not peel off from the substrate, it is used as a jig for semiconductor manufacturing and as a material for use in various products at high temperatures. It sometimes has the advantage of being able to be used repeatedly.
Claims (1)
を加熱して該基板上に炭化けい素を被覆することを特徴
とする炭化けい素被覆膜の製造方法。 ２、加熱が１〜１００トールにおいて１，１００〜１，
５００℃で行なわれる請求項１に記載した炭化けい素被
覆膜の製造方法。 ３、基板表面にオルガノポリシロキサンを塗布して該オ
ルガノポリシロキサンを基板内に均一に浸透させた後、
減圧下に加熱して炭化けい素被覆を形成させる請求項１
に記載した炭化けい素被覆膜の製造方法。 ４、基板表面にオルガノポリシロキサンを塗布して該オ
ルガノポリシロキサンを基板内に均一に浸透させたのち
該オルガノポリシロキサンを硬化させ、減圧下に加熱し
て炭化けい素被覆を形成させる請求項１に記載した炭化
けい素被覆を膜の製造方法。[Claims] 1. A method for producing a silicon carbide coating film, which comprises providing an organopolysiloxane on the surface of a substrate and heating the organopolysiloxane to coat the substrate with silicon carbide. 2. Heating is 1,100-1, at 1-100 Torr.
The method for producing a silicon carbide coating film according to claim 1, which is carried out at 500°C. 3. After coating the surface of the substrate with organopolysiloxane and uniformly permeating the organopolysiloxane into the substrate,
Claim 1: Forming a silicon carbide coating by heating under reduced pressure.
A method for producing a silicon carbide coating film described in . 4. The organopolysiloxane is applied to the surface of the substrate so that the organopolysiloxane permeates uniformly into the substrate, and then the organopolysiloxane is cured and heated under reduced pressure to form a silicon carbide coating. A method of manufacturing a silicon carbide coating described in .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2074448A JP2866435B2 (en) | 1990-03-23 | 1990-03-23 | Method for producing silicon carbide coating film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2074448A JP2866435B2 (en) | 1990-03-23 | 1990-03-23 | Method for producing silicon carbide coating film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03275579A true JPH03275579A (en) | 1991-12-06 |
| JP2866435B2 JP2866435B2 (en) | 1999-03-08 |
Family
ID=13547529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2074448A Expired - Fee Related JP2866435B2 (en) | 1990-03-23 | 1990-03-23 | Method for producing silicon carbide coating film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2866435B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011043427A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Method for densifying porous silicon carbide base |
| WO2011043426A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Silicon carbide joined body and method for joining silicon carbide members |
| WO2011043428A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Method for producing carbon material coated with silicon carbide |
| WO2011043425A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Process for production of silicon carbide molded article |
| JP2011079725A (en) * | 2009-10-09 | 2011-04-21 | Shin-Etsu Chemical Co Ltd | Silicon carbide impregnated carbon material |
| JP2015107896A (en) * | 2013-12-05 | 2015-06-11 | 信越半導体株式会社 | Manufacturing method of silicon carbide-coated graphite member, silicon carbide coated graphite member, and manufacturing method of silicon crystal |
| JP2021049770A (en) * | 2019-09-17 | 2021-04-01 | 株式会社巴川製紙所 | Heat-resistant coating sheet and fixture included therein |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4633449B2 (en) * | 2004-11-25 | 2011-02-16 | 日本碍子株式会社 | Silicon carbide based porous material and method for producing the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS526714A (en) * | 1975-07-05 | 1977-01-19 | Tohoku Daigaku Kinzoku Zairyo | Manufacture of carbon products coated with silicon carbide |
| JPS5428309A (en) * | 1977-08-03 | 1979-03-02 | Tokushiyu Muki Zairiyou Kenkiy | Method of making heattresistant ceramic sintered body |
-
1990
- 1990-03-23 JP JP2074448A patent/JP2866435B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS526714A (en) * | 1975-07-05 | 1977-01-19 | Tohoku Daigaku Kinzoku Zairyo | Manufacture of carbon products coated with silicon carbide |
| JPS5428309A (en) * | 1977-08-03 | 1979-03-02 | Tokushiyu Muki Zairiyou Kenkiy | Method of making heattresistant ceramic sintered body |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011043427A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Method for densifying porous silicon carbide base |
| WO2011043426A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Silicon carbide joined body and method for joining silicon carbide members |
| WO2011043428A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Method for producing carbon material coated with silicon carbide |
| WO2011043425A1 (en) * | 2009-10-09 | 2011-04-14 | 信越化学工業株式会社 | Process for production of silicon carbide molded article |
| JP2011079725A (en) * | 2009-10-09 | 2011-04-21 | Shin-Etsu Chemical Co Ltd | Silicon carbide impregnated carbon material |
| CN102686538A (en) * | 2009-10-09 | 2012-09-19 | 信越化学工业株式会社 | Method for densifying porous silicon carbide base |
| JPWO2011043425A1 (en) * | 2009-10-09 | 2013-03-04 | 信越化学工業株式会社 | Method for producing silicon carbide molded body |
| JPWO2011043427A1 (en) * | 2009-10-09 | 2013-03-04 | 信越化学工業株式会社 | Method for densifying porous silicon carbide substrate |
| JPWO2011043426A1 (en) * | 2009-10-09 | 2013-03-04 | 信越化学工業株式会社 | Silicon carbide bonded body and silicon carbide member bonding method |
| JP5488607B2 (en) * | 2009-10-09 | 2014-05-14 | 信越化学工業株式会社 | Method for producing silicon carbide-coated carbon material |
| JP2015107896A (en) * | 2013-12-05 | 2015-06-11 | 信越半導体株式会社 | Manufacturing method of silicon carbide-coated graphite member, silicon carbide coated graphite member, and manufacturing method of silicon crystal |
| JP2021049770A (en) * | 2019-09-17 | 2021-04-01 | 株式会社巴川製紙所 | Heat-resistant coating sheet and fixture included therein |
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| Publication number | Publication date |
|---|---|
| JP2866435B2 (en) | 1999-03-08 |
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