JPH0774114B2 - Inner shield for single crystal pulling equipment - Google Patents
Inner shield for single crystal pulling equipmentInfo
- Publication number
- JPH0774114B2 JPH0774114B2 JP3278247A JP27824791A JPH0774114B2 JP H0774114 B2 JPH0774114 B2 JP H0774114B2 JP 3278247 A JP3278247 A JP 3278247A JP 27824791 A JP27824791 A JP 27824791A JP H0774114 B2 JPH0774114 B2 JP H0774114B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- porosity
- crystal pulling
- shield
- less
- 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
- 239000013078 crystal Substances 0.000 title claims description 12
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 13
- 239000011148 porous material Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 4
- 239000007789 gas Substances 0.000 description 11
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000011347 resin Substances 0.000 description 8
- 229920005989 resin Polymers 0.000 description 8
- 239000002912 waste gas Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 3
- 230000002093 peripheral effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007849 furan resin Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Ceramic Products (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、チョクラルスキー（Ｃ
Ｚ）法による単結晶引上装置においてヒーター等を同心
状に囲繞する円筒状のインナーシールド（保温筒）に関
する。BACKGROUND OF THE INVENTION The present invention relates to Czochralski (C
The present invention relates to a cylindrical inner shield (heat retaining cylinder) that concentrically surrounds a heater and the like in a single crystal pulling apparatus by the Z) method.
【０００２】[0002]
【従来の技術】従来、この種の単結晶引上装置のインナ
ーシールドは、ヒーターとの間に形成される廃ガスの流
路の所要空断面積を確保するため、内外周に機械加工を
施して所要寸法とした円筒状の黒鉛材から形成されてい
る。2. Description of the Related Art Conventionally, the inner shield of a single crystal pulling apparatus of this kind has been machined on its inner and outer circumferences in order to secure a required empty cross-sectional area of a waste gas flow path formed between it and a heater. It is made of a cylindrical graphite material with the required dimensions.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、上記従
来の単結晶引上装置のインナーシールドにおいては、黒
鉛材が多孔質で吸蔵ガスを有しているため、その放出に
よりチャンバー内の雰囲気を汚染するおそれがあると共
に、廃ガスの流れがスムースに行われず、かつパーティ
クルが発生する問題がある。However, in the inner shield of the above-mentioned conventional single crystal pulling apparatus, since the graphite material is porous and has a stored gas, its release pollutes the atmosphere in the chamber. There is a possibility that the waste gas may not flow smoothly and particles may be generated.
【０００４】そこで、本発明は、吸蔵ガスの発生がなく
チャンバー内の雰囲気が汚染されることがないと共に、
廃ガスの流れがスムースとなり、かつパーティクルが発
生することのない単結晶引上装置のインナーシールドの
提供を目的とする。Therefore, according to the present invention, the atmosphere in the chamber is not polluted because the stored gas is not generated, and
An object is to provide an inner shield of a single crystal pulling apparatus in which the flow of waste gas is smooth and particles are not generated.
【０００５】[0005]
【課題を解決するための手段】前記課題を解決するた
め、本発明の単結晶引上装置のインナーシールドは、気
孔率が５〜１０％で不純物含有率が５ｐｐｍ以下のガラ
ス状カーボンからなる円筒状のシールド本体の表面に、
最大径が１μｍ以下の独立閉気孔のみを有しかつこれに
よる気孔率が０．３％以下で不純物含有率が５ｐｐｍ以
下のガラス状カーボンの被模を形成したものである。Means for Solving the Problems] To solve the above problems, the inner shield of the single crystal pulling apparatus of the present invention, the gas
On the surface of a cylindrical shield body made of glassy carbon having a porosity of 5 to 10% and an impurity content of 5 ppm or less ,
Only has independent closed pores with a maximum diameter of 1 μm or less
Porosity is less than 0.3% and impurity content is less than 5ppm
The lower glassy carbon is formed.
【０００６】[0006]
【作用】上記手段においては、インナーシールドの全て
が高純度のガラス状カーボンのみからなって、熱伝導率
が極めて低くなると共に、熱履歴に伴ってシールド本体
と被膜に作用する熱応力が相互に緩衝され、かつその寸
法精度が高く表面が緻密で平滑となる。ガラス状カーボ
ンの不純物含有率が、５ｐｐｍを超えるとチャンバー内
の雰囲気を汚染するおそれがある。シールド本体の気孔
率（表面の凹部も含む）の気孔率が、５％未満であると
シールド本体にクラックを生じ、１０％を超えるとガス
の放出量が多くなる。 又、被膜の気孔率が、１％を超え
ると廃ガスの流れがスムースとならなくなる一方、その
独立閉気孔の最大径が、１μｍを超えるとパーティクル
の発生が多くなる。 [Action] In the above means, all of the inner shield consists of only the glass-like carbon of a high purity, thermal conductivity is very low Rutotomoni, with the heat history shield body
Thermal stress acting on the coating is buffered in each other and, and dimensions thereof
The method accuracy is high and the surface is dense and smooth. Impurity content of the glassy carbon and contaminate the atmosphere in the chamber exceeds 5 ppm. Porosity of shield body
Porosity (including surface recesses) of less than 5%
Cracks occur in the shield body and gas exceeds 10%
Will be released more. Also, the porosity of the coating exceeds 1%
Then the flow of waste gas will not be smooth, while
Particles when the maximum diameter of the closed closed pores exceeds 1 μm
Will occur more frequently.
【０００７】ガラス状カーボンの被膜は、５００〜１０
００μｍの厚さが好ましい。５００μｍ未満であると凹
部が完全に被われずパーティクルの発生源となり、１０
００μｍを超えるとシールド本体にクラックを発生す
る。The glassy carbon film has a thickness of 500 to 10
A thickness of 00 μm is preferred. If the thickness is less than 500 μm, the concave portions are not completely covered, and a particle generation source is generated.
If it exceeds 00 μm, cracks occur in the shield body.
【０００８】[0008]
【実施例】以下、本発明の実施例について詳細に説明す
る。先ず、液状の熱硬化性樹脂、例えばフラン樹脂、フ
ェノール樹脂等に有機スルホン酸を少量ずつ添加して常
温で重合させる操作を繰り返して行い、重合液を、内径
５００ｍｍ、外径６００ｍｍ、高さ８００ｍｍの円筒状
の型穴を有する成形型に注入して乾燥器内に納置して乾
燥後、脱型して樹脂円筒を得た。EXAMPLES Examples of the present invention will be described in detail below. First, the operation of adding organic sulfonic acid little by little to liquid thermosetting resin such as furan resin and phenol resin and polymerizing at room temperature is repeated, and the polymerization liquid is 500 mm in inner diameter, 600 mm in outer diameter, and 800 mm in height. Was poured into a molding die having a cylindrical mold hole, placed in a drier and dried, and then demolded to obtain a resin cylinder.
【０００９】この樹脂円筒を焼成収縮後に所要寸法とな
るように、内周面、外周面及び端面に旋削加工等の機械
加工を施して焼成炭化後にシールド本体となるシールド
素体とした。この機械加工によってシールド素体中の独
立閉気孔が開口され、表面に球面状の凹部が形成され
た。The resin cylinder was machined such as turning so as to have the required dimensions after firing shrinkage, and the inner peripheral surface, the outer peripheral surface and the end surface were machined to obtain a shield element body which becomes a shield body after firing and carbonization. By this machining, the independent closed pores in the shield body were opened, and the spherical concave portion was formed on the surface.
【００１０】次に、上記シールド素体の表面を平滑にす
るため、内外周面及び端面に前述した重合液を充填し、
その乾燥後に更に重合液を全表面に塗布して乾燥炉中に
おいて１０℃／ｈの昇温速度で８０〜１００℃まで昇温
し、この温度で１０ｈ保持し乾燥させて樹脂膜を形成さ
せて樹脂円筒を得た。Next, in order to make the surface of the shield element smooth, the inner and outer peripheral surfaces and the end surfaces are filled with the above-mentioned polymerization liquid,
After the drying, the polymerization solution is further applied to the entire surface, the temperature is raised to 80 to 100 ° C. at a heating rate of 10 ° C./h in a drying furnace, and the temperature is held for 10 h to dry to form a resin film. A resin cylinder was obtained.
【００１１】その後、上記樹脂円筒を非酸化性雰囲気中
において、２〜３℃／ｈの昇温速度で１０００℃まで昇
温して焼成炭化し、三次元網目状のガラス構造とした
後、ハロゲンガス雰囲気中において２０００℃の温度で
純化処理を施してガラス状カーボンのインナーシールド
を得た。After that, the resin cylinder is heated in a non-oxidizing atmosphere at a heating rate of 2 to 3 ° C./h to 1000 ° C. to be fired and carbonized to form a three-dimensional mesh-like glass structure, and then halogen. Purification was performed at a temperature of 2000 ° C. in a gas atmosphere to obtain a glassy carbon inner shield.
【００１２】ここで、ガス放出量の測定を行うために、
次の試料（６×６×１２ｍｍ）を作製した。 気孔率（表面の凹部も含む）７％のガラス状カーボン
に、気孔率０．２％、膜厚６００μｍのガラス状カーボ
ンのコーティングを施したもの。 気孔率１１％のガラス状カーボンに、気孔率０．２
％、膜厚６００μｍのガラス状カーボンのコーティング
を施したもの。 気孔率１２％の一般的な等方性カーボンに、気孔率
０．２％、膜厚６００μｍのガラス状カーボンのコーテ
ィングを施したもの。 上記各試料について、９００℃で加熱処理した際のガス
（Ｈ ２ ，Ｈ ２ Ｏ，ＣＯ，ＣＯ ２ ，Ｏ ２ その他）の放出量
（１００ｇ換算）の測定を行ったところ、次のようにな
った。 試料：１．１ｍｌ／１００ｇ 試料：２．０ｍｌ／１００ｇ 試料：２．９ｍｌ／１００ｇ よって、シールド本体の気孔率が１０％を越えるとガス
の放出量が多くなることがわかる。 一方、シールド本体
の気孔率が５％未満であると、チャンバー内で発生する
ＳｉＯ，Ｓｉガスにより、表面珪化が起こり、この珪化
がシールド本体の表面から５０〜１００μｍの深さまで
進行すると、両者の熱膨張差により珪化膜からシールド
本体内部までクラックが生じる。 従って、シールド本体
の気孔率は、５〜１０％であることが好ましい。 又、被
膜は、気孔率が０．３％以下で、かつ独立閉気孔の最大
径が１μｍ以下であることが好ましい。気孔率が１％を
超えると、廃ガスの流れがスムースとならなくなり、
又、独立閉気孔の最大径が１μｍを超えると、パーティ
クルの発生が多くなる。 Here, in order to measure the amount of gas released,
The following sample (6 × 6 × 12 mm) was prepared. Glassy carbon with 7% porosity (including concave portions on the surface)
In addition, a glass-like carb having a porosity of 0.2% and a film thickness of 600 μm
The one with a coating. 0.2% porosity on glassy carbon with 11% porosity
%, Glassy carbon coating with a thickness of 600 μm
Those that have been subjected to. General isotropic carbon with 12% porosity
0.2% glassy carbon coating with a thickness of 600 μm
It has been winged. Gas for each sample above when heat-treated at 900 ℃
Emissions of (H 2 , H 2 O, CO, CO 2 , O 2 and others)
The measurement of (100g conversion) was as follows.
It was. Sample: 1.1 ml / 100 g Sample: 2.0 ml / 100 g Sample: 2.9 ml / 100 g Therefore, gas is generated when the porosity of the shield body exceeds 10%.
It can be seen that the release amount of is increased. On the other hand, the shield body
Porosity of less than 5% occurs in the chamber
Surface silicification occurs due to SiO and Si gas, and this silicification
From the surface of the shield body to a depth of 50-100 μm
As it progresses, the thermal expansion difference between the two shields it from the silicide film.
Cracks occur inside the body. Therefore, the shield body
The porosity of is preferably 5 to 10%. Further, the coating film preferably has a porosity of 0.3% or less and a maximum diameter of the independent closed pores of 1 μm or less. If the porosity exceeds 1%, the flow of waste gas will not be smooth,
If the maximum diameter of the closed closed pores exceeds 1 μm, the number of particles is increased.
【００１３】次に、熱伝導率の測定を行うために、上記
，，の試料に加えて、次の試料（６×６×１２ｍ
ｍ）を作製した。 気孔率１２％の等方性カーボン 上記各試料について、熱伝導率の測定を行ったところ、
次のようになった。 試料：７ｗ／ｍ・ｋ 試料：９ｗ／ｍ・ｋ 試料：８０ｗ／ｍ・ｋ 試料：１００ｗ／ｍ・ｋ 従って、本発明品は、熱伝導率が極めて低いことがわか
る。 Next, in order to measure the thermal conductivity, the above
,,, and the next sample (6 x 6 x 12 m
m) was prepared. Isotropic carbon having a porosity of 12% When the thermal conductivity of each of the above samples was measured,
It became like this. Specimen: 7 w / m · k Specimen: 9 w / m · k Specimen: 80 w / m · k Specimen: 100 w / m · k Therefore, it can be seen that the product of the present invention has extremely low thermal conductivity.
It
【００１４】なお、シールド素体の全表面に対する重合
液の塗布は、１回に限定されることはなく、２回以上の
塗布と乾燥を繰り返してもよく、このようにすることに
より、ガラス状カーボンの被膜の厚さを厚くすることが
可能となる。ガラス状カーボンの被膜は、シールド素体
との熱膨張差がないので厚くなってもよいが、５００〜
１０００μｍであることが好ましい。５００μｍ未満で
あると凹部が完全に被われずパーティクルの発生源とな
り、１０００μｍを超えるとシールド本体にクラックを
発生することとなる。[001 4] The polymerization solution of the coating to the total surface of the shield body is not limited to one, may be repeated drying of more than two applications, by doing so, the glass It is possible to increase the thickness of the carbon film. The glassy carbon coating may have a thicker thickness because it has no difference in thermal expansion from the shield element,
It is preferably 1000 μm. 50 0 is less than μm recess becomes a particle generation source is not completely covered, so that the cracks in the shield body exceeds 1000 .mu.m.
【００１５】又は、シールド素体の凹部への充填は、そ
の独立閉気孔が小さい場合は行わなくよもよいが、シー
ルド素体が液状の熱硬化性樹脂に同種の樹脂粉末の添加
等によって独立閉気孔径が大きくなった場合には充填す
ることが好ましい。[001 5] or, filling of the concave portion of the shield body, the independent closed pores. However Restaurant good not performed smaller, by addition of a same type of resin powder shield body is in a liquid thermosetting resin It is preferable to fill when the size of the independent closed pores becomes large.
【００１６】ここで、上述したインナーシールドを備え
た単結晶引上装置を用いてシリコン単結晶を引き上げた
ところ、従来の黒鉛材からなる同一寸法のインナーシー
ルドを備えた単結晶引上装置を用いた場合に比べ、吸蔵
ガスの放出がなくなってシリコンインゴット単結晶が汚
染されることがなく、その歩留りが１５％向上すると共
に、ヒーターとの間に形成される廃ガス流路の廃ガスの
流れがスムースになり、かつパーティクルの発生が大幅
に滅少した。[001 6] Here, when a silicon single crystal is pulled using a single crystal pulling apparatus having an inner shield as described above, the single crystal pulling apparatus equipped with inner shield of the same dimensions made of conventional graphite materials Compared to the case where it is used, the silicon ingot single crystal is not contaminated due to the release of the occluded gas, the yield is improved by 15%, and the waste gas in the waste gas flow path formed between the heater and The flow became smooth and the generation of particles was greatly reduced.
【００１７】[0017]
【発明の効果】以上説明したように本発明の単結晶引上
装置のインナーシールドによれば、インナーシールドの
全てが高純度のガラス状カーボンのみからなって、熱伝
導率が極めて低くなるので、従来のものと同等の肉厚で
あれば従来のものより格段に高い保温性を有し、電力量
を節約できる一方、肉厚を薄くしたとしても、熱伝導的
に支障なく、十分な軽量化を図ることができる。又、熱
履歴に伴ってシールド本体と被膜に作用する熱応力が相
互に緩衝されるので、シールド本体の強度が比較的高い
ことも相俟ってシールド本体及び被膜にクラックが生じ
ることなく、チャンバー内の雰囲気が従来のように吸蔵
ガスの放出によって汚染されることがないと共に、パー
ティクルの発生頻度を極めて低下させることができる。
更に、その寸法精度が高く表面が緻密で平滑となるの
で、廃ガスの流れがスムースになるという効果を有す
る。As described above, according to the inner shield of the single crystal pulling apparatus of the present invention, all of the inner shield is made of only high-purity glassy carbon and the thermal conductivity is extremely low. If the wall thickness is the same as the conventional one, it has much higher heat retention than the conventional one and can save the amount of electric power. On the other hand, even if the wall thickness is thin, there is no problem in heat conduction and sufficient weight reduction. Can be achieved. Also, heat
The thermal stress acting on the shield body and the coating changes with the history.
The strength of the shield body is relatively high because they are buffered by each other
This also causes cracks in the shield body and coating.
Without Rukoto, the never atmosphere in the chamber is contaminated by the release of occluded gases as in the prior art, par
The frequency of tickle generation can be extremely reduced.
Furthermore, its dimensional accuracy is high and the surface is dense and smooth.
This has the effect of smoothing the flow of waste gas.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 蒔田 律郎 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 外谷 栄一 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 (56)参考文献 特開 昭64−18986（ＪＰ，Ａ) 特開 昭62−297293（ＪＰ，Ａ) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Ritsuro Makita 378, Oguni-machi, Oguni-cho, Nishiokitama-gun, Yamagata Prefecture Oguni Factory, Toshiba Ceramics Co., Ltd. No. 378 Toshiba Ceramics Co., Ltd. Oguni Factory (56) Reference JP-A 64-18986 (JP, A) JP-A 62-297293 (JP, A)
Claims (1)
ｐｐｍ以下のガラス状カーボンからなる円筒状のシール
ド本体の表面に、最大径が１μｍ以下の独立閉気孔のみ
を有しかつこれによる気孔率が０．３％以下で不純物含
有率が５ｐｐｍ以下のガラス状カーボンの被膜を形成し
たことを特徴とする単結晶引上装置のインナーシール
ド。1. A porosity of 5 to 10% and an impurity content of 5
Only independent closed pores with a maximum diameter of 1 μm or less on the surface of a cylindrical shield body made of glassy carbon of less than ppm
And has a porosity of 0.3% or less.
An inner shield for a single crystal pulling apparatus, characterized in that a glassy carbon film having a content of 5 ppm or less is formed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3278247A JPH0774114B2 (en) | 1991-09-30 | 1991-09-30 | Inner shield for single crystal pulling equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3278247A JPH0774114B2 (en) | 1991-09-30 | 1991-09-30 | Inner shield for single crystal pulling equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0585884A JPH0585884A (en) | 1993-04-06 |
| JPH0774114B2 true JPH0774114B2 (en) | 1995-08-09 |
Family
ID=17594675
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3278247A Expired - Fee Related JPH0774114B2 (en) | 1991-09-30 | 1991-09-30 | Inner shield for single crystal pulling equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0774114B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4600703B2 (en) * | 1999-10-25 | 2010-12-15 | 日立化成工業株式会社 | Method for producing glassy carbon |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62297293A (en) * | 1986-06-16 | 1987-12-24 | Ibiden Co Ltd | Insulating foam material of single crystal-pulling up system |
| JPH062637B2 (en) * | 1987-07-13 | 1994-01-12 | 東洋炭素株式会社 | Single crystal pulling device |
-
1991
- 1991-09-30 JP JP3278247A patent/JPH0774114B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0585884A (en) | 1993-04-06 |
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