JP2553389B2 - Carbon jig for CVD equipment - Google Patents
Carbon jig for CVD equipmentInfo
- Publication number
- JP2553389B2 JP2553389B2 JP63328587A JP32858788A JP2553389B2 JP 2553389 B2 JP2553389 B2 JP 2553389B2 JP 63328587 A JP63328587 A JP 63328587A JP 32858788 A JP32858788 A JP 32858788A JP 2553389 B2 JP2553389 B2 JP 2553389B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- film
- coating
- jig
- carbon jig
- 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.)
- Expired - Fee Related
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 43
- 229910052799 carbon Inorganic materials 0.000 title claims description 43
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 3
- 239000010408 film Substances 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 17
- 238000000576 coating method Methods 0.000 description 17
- 239000011148 porous material Substances 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 238000005268 plasma chemical vapour deposition Methods 0.000 description 3
- 239000002296 pyrolytic carbon Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、CVD装置用カーボン治具に係り、特に半導
体デバイス用シリコンウェーハに対して薄膜を形成する
ホットウォール形プラズマCVD装置等に用いられるカー
ボンプレート若しくはカーボンディスク電極又は電極間
の連結部材等のCVD装置用カーボン治具に関する。Description: TECHNICAL FIELD The present invention relates to a carbon jig for a CVD apparatus, and is particularly used for a hot wall type plasma CVD apparatus for forming a thin film on a silicon wafer for semiconductor devices. The present invention relates to a carbon jig for a CVD device such as a carbon plate or a carbon disk electrode or a connecting member between electrodes.
従来、この種のカーボン治具は、コークスを粉砕して
粉末状のカーボン材料を作製する工程、粉末状のカーボ
ン材料に適宣のバインダを添加して混練する工程、混練
材料を成形して成形素体を作製する工程、成形素体を焼
成する工程、及び焼成素体を熱処理によって黒鉛化する
工程を経て作製されていた。Conventionally, this kind of carbon jig is a step of crushing coke to produce a powdery carbon material, a step of adding an appropriate binder to the powdery carbon material and kneading, and a step of molding and kneading the kneading material. It was produced through a step of producing an element body, a step of firing a molded element body, and a step of graphitizing the fired element body by heat treatment.
カーボン治具は、半導体デバイス用シリコンウェーハ
が載置され、ホットウォール形のプラズマCVD装置内に
挿入された状態で、半導体デバイス用シリコンウェーハ
に対し適宣の熱処理を施すために電極として使用されて
いた。従って、カーボン治具上にも窒化物あるいは酸化
物が付着され、使用回数を重ねるに従って次第にプラズ
マが安定して発生しにくくなり、ひいては半導体デバイ
ス用シリコンウェーハ上に均一なCVD膜が形成されにく
くなっていたので、付着された窒化物あるいは酸化物を
取り除く必要があり、フレオンガス等を用いて定期的に
カーボン治具を洗浄していた。The carbon jig is used as an electrode to appropriately heat-treat a silicon wafer for a semiconductor device with the silicon wafer for a semiconductor device placed and inserted in a hot-wall type plasma CVD device. It was Therefore, nitride or oxide is attached to the carbon jig, and it becomes difficult for plasma to be stably generated gradually as the number of times of use is increased, and it is difficult to form a uniform CVD film on the silicon wafer for semiconductor devices. Therefore, it is necessary to remove the attached nitride or oxide, and the carbon jig is regularly cleaned using freon gas or the like.
この定期的な洗浄に伴ってカーボン治具からカーボン
粒子が脱落し易くなり、プラズマCVD処理中に脱落して
半導体デバイス用シリコンウェーハに付着するおそれが
あった。これを防止するため、カーボン治具の表面にガ
ラス状カーボン膜、熱分解炭素膜を形成したものであっ
た。With this regular cleaning, carbon particles are likely to fall off from the carbon jig, and there is a risk that they may fall off during the plasma CVD process and adhere to the silicon wafer for semiconductor devices. In order to prevent this, a glassy carbon film and a pyrolytic carbon film were formed on the surface of the carbon jig.
これは、先の問題に対処するため、第３図に示すよう
に、カーボン基材11の表面にガラス状カーボンあるいは
熱分解炭素の被膜12を形成してなるカーボン治具であ
る。図中13は開気孔である。In order to deal with the above problem, this is a carbon jig in which a coating 12 of glassy carbon or pyrolytic carbon is formed on the surface of a carbon base material 11, as shown in FIG. In the figure, 13 is an open pore.
しかしながら、上記従来のCVD装置用カーボン治具に
おいては、炭素基材の表面にガラス状カーボンあるいは
熱分解炭素の被膜が単にのっているだけの状態であり、
被膜自体の機械的強度が十分でなく、問題解決の要求を
十分に満足するものではなかった。一方、被膜の強度を
高めるため、膜厚を厚くしようとすると被膜生成の際の
熱処理工程で熱膨張の差などにより、被膜にクラックや
剥離が生じてしまい、厚い被膜（５μｍ以上）を形成す
ることが困難であった。However, in the above-mentioned conventional carbon jig for a CVD device, a coating of glassy carbon or pyrolytic carbon is simply deposited on the surface of the carbon substrate,
The mechanical strength of the coating itself was not sufficient, and the demand for solving the problem was not sufficiently satisfied. On the other hand, if an attempt is made to increase the film thickness in order to increase the strength of the film, cracks and peeling will occur in the film due to the difference in thermal expansion during the heat treatment process for forming the film, thus forming a thick film (5 μm or more). Was difficult.
そこで、本発明は、ガラス状カーボンの被膜の膜厚を
増して機械的強度を向上させ、ひいては耐薬品性、耐酸
化性及びライフを大幅に向上し得るCVD装置用カーボン
治具の提供を目的とする。Therefore, the present invention aims to provide a carbon jig for a CVD apparatus capable of improving the mechanical strength by increasing the film thickness of the glassy carbon coating, and thus significantly improving chemical resistance, oxidation resistance and life. And
前記課題を解決するため、本発明は、カサ密度1.50〜
1.90g/cm3のカーボン基材中の開気孔にガラス状カーボ
ンが充填率60％以上に充填され、かつこのカーボン素材
の表面に開気孔率0.1〜1.0％のガラス状のカーボンの被
膜が形成されているものである。In order to solve the above problems, the present invention provides a bulk density of 1.50 to
Glass-like carbon is filled in the open pores of a carbon substrate of 1.90 g / cm 3 at a filling rate of 60% or more, and a glassy carbon film with an open-pore rate of 0.1 to 1.0% is formed on the surface of this carbon material. It has been done.
被膜の膜圧は、２μｍ〜1mmとるとよい。 The film pressure of the film is preferably 2 μm to 1 mm.
上記手段においては、カーボン基材中の開気孔がガラ
ス状カーボンの充填によって減少し、カーボン基材中に
満たされる気体又は液体の量が減少する一方、充填され
たガラス状カーボンの同種の被膜のアンカーとなる。In the above means, the open pores in the carbon substrate are reduced by the filling of the glassy carbon, the amount of gas or liquid filled in the carbon substrate is reduced, while the same kind of coating of the glassy carbon filled Become an anchor.
カーボン基材のカサ密度が1.50g/cm3未満であると機
械的強度が低下する一方、カサ密度が1.90g/cm3を超え
るとコスト高になる。While bulk density of the carbon substrate is lowered mechanical strength is less than 1.50 g / cm 3, bulk density increases costs exceeds 1.90 g / cm 3.
開気孔に対するガラス状カーボンの充填率が60％未満
であるとカーボン基材中に満たされる気体や液体によっ
て被膜にクラックや剥離が生じると共に、被膜を保持す
る力が小さくなる。If the filling ratio of the glassy carbon with respect to the open pores is less than 60%, the film and the liquid filled with the carbon crack or crack, and the force for holding the film becomes small.
被膜の膜厚が２μｍ未満であると被膜としても効果が
生ぜず、1mmを超えると被膜形成の熱処理の過程におい
てその収縮からクラックや剥離を生じる。If the film thickness is less than 2 μm, no effect is produced as a film, and if it exceeds 1 mm, cracking or peeling occurs due to the shrinkage during the heat treatment for forming the film.
被膜の開気孔率が0.1％未満であると使用時の昇降温
の際に、カーボン基材中に存在する気体又は液体によ
り、被膜にクラックや剥離等が生じてライフが著しく低
下し望ましくない。When the open porosity of the coating is less than 0.1%, the gas or liquid present in the carbon substrate causes cracks or peeling of the coating during temperature raising / lowering during use, which is not desirable because the life is significantly reduced.
以下、本発明の一実施例を第１図と共に説明する。 An embodiment of the present invention will be described below with reference to FIG.
各種のカーボン基材に熱硬化性樹脂（例えばフェノー
ル樹脂やフラン樹脂）を減圧含浸した後、80℃の温度で
１日保持して半硬化状態にし、そこに更に同種の熱硬化
性樹脂をカーボン基材１の表面にコーティングし、その
後に200℃の温度に１時間保持して熱硬化性樹脂を硬化
させた後、不活性雰囲気中において2000℃の温度で熱処
理して熱硬化性樹脂をガラス状カーボンに転換し、第１
図に示すように、カーボン基材１の開気孔２にガラス状
カーボン３が充填され、かつこのカーボン基材１の表面
にガラス状カーボンの被膜４が形成されたCVD装置用カ
ーボン治具を得た。After thermosetting resin (for example, phenol resin or furan resin) is impregnated into various carbon base materials under reduced pressure, it is kept at 80 ° C for 1 day to be in semi-cured state. After coating the surface of the base material 1 and holding the temperature at 200 ° C for 1 hour to cure the thermosetting resin, the thermosetting resin is heat-treated at a temperature of 2000 ° C in an inert atmosphere to make the thermosetting resin glass. First converted to carbon-like carbon
As shown in the figure, a carbon jig for a CVD apparatus in which glassy carbon 3 is filled in the open pores 2 of the carbon substrate 1 and a glassy carbon coating 4 is formed on the surface of the carbon substrate 1 is obtained. It was
各カーボン治具のカサ密度、気孔率、曲げ強度及びラ
イフは、比較例を併記した第１表に示すようになった。The bulk density, porosity, bending strength, and life of each carbon jig were as shown in Table 1 which also shows a comparative example.
従って、カーボン基材のカサ密度を1.50〜1.90g/cm3
とし、かつ被膜の気孔率を0.1〜1.0％とすることにより
曲げ強度及びライフを向上し得ることがわかる。 Therefore, the bulk density of the carbon substrate is 1.50 to 1.90 g / cm 3
It is understood that the bending strength and the life can be improved by setting the porosity of the coating to 0.1 to 1.0%.
そして、開気孔に対するガラス状カーボンの充填率
は、60％以上が好ましく、かつ被膜の膜厚は、２μｍ〜
1mmの範囲が好ましかった。The filling rate of glassy carbon with respect to open pores is preferably 60% or more, and the film thickness of the coating is 2 μm to
The 1 mm range was preferred.
又、上記実施例及び従来例のカーボン治具並びに被膜
を形成しない未処理のカーボン治具に、酸化消耗試験
（800℃の温度の空気中に放置）を施したところ、第２
図に示すようになった。Further, the carbon jigs of the above-mentioned example and the conventional example and the untreated carbon jigs on which the coating is not formed were subjected to an oxidative wear test (left in the air at a temperature of 800 ° C.),
It came to be shown in the figure.
従って、本発明品は、60分後でも重量減少率が低く、
耐酸化性に著しく優れていることがわかる反面、未処理
品は、60分でほとんど形状がなくなり、又、従来品は、
30分を過ぎたあたりから重量減少率が高くなり、耐酸化
性が劣るようになることがわかる。これは、ガラス状カ
ーボンの被膜が酸化されて劣化すると共に、開気孔中の
気体の膨張により被膜にクラックが発生したため、剥離
が生じてカーボン基材が直接酸化の影響を受けたためで
ある。Therefore, the product of the present invention has a low weight loss rate even after 60 minutes,
It can be seen that the oxidation resistance is remarkably excellent, but the untreated product loses its shape in 60 minutes, and the conventional product is
It can be seen that after 30 minutes, the weight reduction rate becomes high and the oxidation resistance becomes poor. This is because the glass-like carbon coating film was oxidized and deteriorated, and the coating film was cracked due to the expansion of the gas in the open pores, so that the carbon substrate was directly affected by the oxidation due to peeling.
以上のように本発明によれば、カーボン基材中の開気
孔がガラス状カーボンの充填によって減少し、カーボン
基材中に満たされる気体又は液体の量が減少する一方、
充填されたガラス状カーボンが同種の被膜のアンカーと
なるので、被膜の膜厚を増して機械的強度を向上させる
ことができ、ひいては耐薬品性、耐酸化性及びライフを
大幅に向上することができる。As described above, according to the present invention, the open pores in the carbon substrate are reduced by the glassy carbon filling, while the amount of gas or liquid filled in the carbon substrate is reduced,
Since the filled glassy carbon serves as an anchor for the same kind of coating, it is possible to increase the thickness of the coating and improve the mechanical strength, which in turn greatly improves chemical resistance, oxidation resistance and life. it can.
第１図は本発明の一実施例を示すCVD装置用カーボン治
具の断面図、第２図はその酸化消耗試験結果の説明図、
第３図は従来のCVD装置用カーボン治具の説明図であ
る。 １……カーボン基材、２……開気孔 ３……ガラス状カーボン、４……被膜FIG. 1 is a sectional view of a carbon jig for a CVD apparatus showing an embodiment of the present invention, FIG.
FIG. 3 is an explanatory view of a conventional carbon jig for a CVD apparatus. 1 ... Carbon substrate, 2 ... Open pores 3 ... Glassy carbon, 4 ... Coating
───────────────────────────────────────────────────── フロントページの続き (72)発明者 井村 浩一 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (72)発明者 笠原 雅寿 山形県西置賜郡小国町大字小国町378番 地 東芝セラミックス株式会社小国製造 所内 (56)参考文献 特開 昭62−270491（ＪＰ，Ａ) 特開 昭63−89490（ＪＰ，Ａ) 特開 昭62−205278（ＪＰ，Ａ) 特公 昭52−39684（ＪＰ，Ｂ２) 特公 昭47−1003（ＪＰ，Ｂ２) 特公 昭63−26194（ＪＰ，Ｂ２) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Koichi Imura Koichi Imura, Oguni Town, Oguni Town, Yamagata Prefecture, 378 Oguni Town, Oguni Manufacturing Co., Ltd. (72) Masato Kasahara Oguni Town, Oguni Town, Yamagata Prefecture No. 378 Toshiba Ceramics Co., Ltd. Oguni Factory (56) Reference JP 62-270491 (JP, A) JP 63-89490 (JP, A) JP 62-205278 (JP, A) JP 52-39684 (JP, B2) JP47-1003 (JP, B2) JP63-26194 (JP, B2)
Claims (1)
中の開気孔にガラス状カーボンが充填率60％以上に充填
され、かつこのカーボン基材の表面に開気孔率0.1〜1.0
％のガラス状のカーボンの被膜が形成されていることを
特徴とするCVD装置用カーボン治具。1. A glass substrate having a bulk density of 1.50 to 1.90 g / cm 3 is filled with glassy carbon at a filling rate of 60% or more, and the surface of the carbon substrate has an open porosity of 0.1 to 1.0.
% Carbon glass film is formed on the carbon jig for a CVD device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63328587A JP2553389B2 (en) | 1988-12-26 | 1988-12-26 | Carbon jig for CVD equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63328587A JP2553389B2 (en) | 1988-12-26 | 1988-12-26 | Carbon jig for CVD equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02173269A JPH02173269A (en) | 1990-07-04 |
| JP2553389B2 true JP2553389B2 (en) | 1996-11-13 |
Family
ID=18211940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63328587A Expired - Fee Related JP2553389B2 (en) | 1988-12-26 | 1988-12-26 | Carbon jig for CVD equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2553389B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3454333B2 (en) * | 1996-04-22 | 2003-10-06 | 日清紡績株式会社 | Plasma etching electrode |
| CA2207878A1 (en) * | 1996-06-20 | 1997-12-20 | Qqc, Inc. | Glassy carbon coatings having water repellant and corrosion-, erosion-, and wear-resistant characteristics |
| JPH11322427A (en) | 1998-05-19 | 1999-11-24 | Toshiba Mach Co Ltd | Production of vitreous carbon member |
| JP6888463B2 (en) * | 2017-07-28 | 2021-06-16 | トヨタ自動車株式会社 | Film removal method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3995045A (en) * | 1975-09-25 | 1976-11-30 | E. R. Squibb & Sons, Inc. | 2'-[(3,6-Dihydro-phenyl-1(2H)pyridinyl)alkylaminocarbonyl][1,1'-biphenyl]-2-carboxylic acids |
| JPS62270491A (en) * | 1986-05-15 | 1987-11-24 | Seitetsu Kagaku Co Ltd | Production of susceptor |
-
1988
- 1988-12-26 JP JP63328587A patent/JP2553389B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02173269A (en) | 1990-07-04 |
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