JP2777858B2 - Silica glass tube for heat treatment of semiconductor and method for producing the same - Google Patents
Silica glass tube for heat treatment of semiconductor and method for producing the sameInfo
- Publication number
- JP2777858B2 JP2777858B2 JP4301628A JP30162892A JP2777858B2 JP 2777858 B2 JP2777858 B2 JP 2777858B2 JP 4301628 A JP4301628 A JP 4301628A JP 30162892 A JP30162892 A JP 30162892A JP 2777858 B2 JP2777858 B2 JP 2777858B2
- Authority
- JP
- Japan
- Prior art keywords
- silica glass
- glass tube
- heat treatment
- less
- semiconductor
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
- C03B2201/03—Impurity concentration specified
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Description
【0001】[0001]
【産業上の利用分野】本発明は、半導体熱処理用シリカ
ガラス管、特に短時間の空焼きで立上げができる電気溶
融して得たシリカガラス管、およびその製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a silica glass tube for heat treatment of semiconductors, and more particularly to a silica glass tube obtained by electromelting which can be started up in a short time baking, and a method for producing the same.
【0002】[0002]
【従来の技術】半導体製造に使用される機械、装置、容
器などは耐熱性とともに、化学的な高純度が要求され
る。そして、これら部材はどのような条件下でも、ウエ
ーハと反応したり、あるいは痕跡といえどもどのような
元素もウエーハに与えてはならない。こうした要求にこ
たえる材料として、従来、シリカガラスが用いられてき
た。シリカガラスには、結晶質石英を電気溶融法で溶融
しガラス化したシリカガラス(以下電気溶融シリカガラ
スという)、結晶質石英を酸水素火炎法で溶融しガラス
化したシリカガラス(以下酸水素火炎溶融シリカガラス
という)、およびゾルーゲル法やスート法で製造したシ
リカをガラス化した合成シリカガラス等がある。しかし
ながら、前記酸水素火炎溶融シリカガラスは多量のOH
基を含有するため、高温で長時間使用するとつぶれや変
形を起こすという欠点を有していた。また、合成シリカ
ガラスは結晶質石英粉から得られたシリカガラスに比較
して粘度が低く、かつ製造時の混入塩素および塩化水素
により気泡が発生し見栄が悪くなるという欠点を有して
いた。そのため、従来、半導体工業用治具として、特に
熱処理温度が1100℃以上のプロセスで用いる治具用
素材としては専ら電気溶融シリカガラスが用いられてき
た。2. Description of the Related Art Machines, devices, containers, and the like used in semiconductor manufacturing are required to have high heat resistance and high chemical purity. These components must not react with the wafer under any conditions or give any element, even traces, to the wafer. Conventionally, silica glass has been used as a material that meets such demands. Silica glass includes silica glass obtained by melting crystalline quartz by an electric melting method and vitrifying (hereinafter referred to as electrofused silica glass), and silica glass obtained by fusing and crystallizing crystalline quartz by an oxyhydrogen flame method (hereinafter referred to as oxyhydrogen flame). Fused silica glass), and synthetic silica glass obtained by vitrifying silica produced by a sol-gel method or a soot method. However, the oxyhydrogen flame fused silica glass has a large amount of OH.
Since it contains a group, it has a disadvantage that it is crushed or deformed when used for a long time at a high temperature. Further, the synthetic silica glass has a disadvantage that the viscosity is lower than that of the silica glass obtained from the crystalline quartz powder, and bubbles are generated by chlorine and hydrogen chloride mixed during the production, resulting in a poor appearance. For this reason, conventionally, electrofused silica glass has been exclusively used as a jig for semiconductor industry, particularly as a jig material used in a process in which a heat treatment temperature is 1100 ° C. or higher.
【0003】ところが、近年新しい評価法が開発され、
この評価法によりシリカガラスのウエーハへの影響を調
べたところ、電気溶融シリカガラス製品は、高純度にも
かかわらずウエーハの劣化をもたらすことがわかった。
この原因を調べるため電気溶融シリカガラス管と酸水素
火炎溶融シリカガラス管とを電気炉内にセットし同じ時
間空焼きをした後、ウエーハの酸化処理をおこなった。
すると、酸水素火炎溶融シリカガラス管の場合には規格
値以上のライフタイムを有するウエーハを得ることがで
きたが、電気溶融シリカガラスの場合には規格値領域が
少ないウエーハが得られるに過ぎなかった。このライフ
タイム低下の原因として、ウエーハの酸化膜中への金属
不純物元素の採り込みが考えられるが、その発生源が、
酸水素火炎溶融シリカガラス製品にライフタイム劣化が
少ないところから、電気溶融シリカガラス自体にあるも
のと考えられる。しかしながら、酸水素火炎溶融シリカ
ガラス製品は、1100℃以上の高温プロセスで変形が
起こり使用期間が短いところから、電気溶融シリカガラ
ス製品の改良が希求されていた。However, a new evaluation method has recently been developed,
When the effect of silica glass on the wafer was examined by this evaluation method, it was found that the electrofused silica glass product caused the deterioration of the wafer despite its high purity.
To investigate the cause, an electrofused silica glass tube and an oxyhydrogen flame fused silica glass tube were set in an electric furnace, baked for the same time, and then oxidized.
Then, in the case of the oxyhydrogen flame-fused silica glass tube, a wafer having a lifetime longer than the standard value could be obtained, but in the case of the electrofused silica glass, only a wafer having a small standard value region was obtained. Was. As a cause of the reduction in the lifetime, the incorporation of metal impurity elements into the oxide film of the wafer can be considered.
It is considered that the electrofused silica glass itself exists in the oxyhydrogen flame fused silica glass product since the life time degradation is small. However, since the oxyhydrogen flame fused silica glass product is deformed by a high temperature process of 1100 ° C. or higher and has a short service life, improvement of the electrofused silica glass product has been desired.
【0004】[0004]
【発明が解決しようとする課題】本発明者等は上記電気
溶融シリカガラス管の空焼き時間の短縮化について研究
していたところ、前記空焼きの短縮化に鉄元素および銅
元素の含有量が影響することがわかった。そのため先
ず、本発明者等は、シリカガラスバルク全体の鉄元素の
含有量の低減を検討したが、シリカガラス管の製造時や
加工時の汚染等のため現実的には実施化が困難であっ
た。さらに鋭意研究を続けたところ、内表面から100
μmまでの層中の鉄元素の含有量が100ppb以下で
銅元素の含有量が50ppb以下である電気溶融シリカ
ガラス管は、酸水素火炎溶融シリカガラス管と同程度の
空焼き時間で、ウエーハのライフタイムを規格値以上に
することを発見した。そこで、この鉄元素および銅元素
含有量の少ないシリカガラス層を電気溶融シリカガラス
管の内側に積層し、前記課題の解決を図ろうとしたが、
技術的に高度である上、コスト的にも高くなり好ましい
手段とはいえなかった。本発明者等は上記問題点を考慮
しつつさらに研究を重ねた結果、電気溶融シリカガラス
管を特定の条件下で雰囲気加熱処理することにより鉄元
素および銅元素含有量の少ない層を形成できることを発
見した。こうした知見に基づき本発明は完成したもので
ある。SUMMARY OF THE INVENTION The present inventors have been studying the shortening of the baking time of the above-mentioned electrofused silica glass tube. Turned out to affect. Therefore, the present inventors first examined the reduction of the iron element content in the entire silica glass bulk, but it was difficult to implement in practice due to contamination during the production and processing of the silica glass tube. Was. After further research, the inner surface was 100
An electrofused silica glass tube having a content of iron element of 100 ppb or less and a content of copper element of 50 ppb or less in a layer up to μm has a baking time similar to that of an oxyhydrogen flame fused silica glass tube, and has a wafer baking time. We found that the lifetime was over the standard value. Therefore, the silica glass layer having a low content of the iron element and the copper element was laminated on the inside of the electro-fused silica glass tube to solve the above problem.
It is technically advanced and costly, which is not a preferable means. The present inventors have conducted further studies in consideration of the above problems, and as a result, it has been found that a layer having a low content of iron and copper elements can be formed by subjecting the electrofused silica glass tube to an atmospheric heat treatment under specific conditions. discovered. The present invention has been completed based on these findings.
【0005】すなわち、本発明は、短時間の空焼きで立
上げができる新規な電気溶融シリカガラス管を提供する
ことを目的とする。[0005] That is, an object of the present invention is to provide a novel electro-fused silica glass tube which can be set up by baking in a short time.
【0006】また、本発明は、生産性のよいウエーハ熱
処理用電気溶融シリカガラス炉芯管を提供することを目
的とする。Another object of the present invention is to provide an electro-fused silica glass furnace core tube for wafer heat treatment with high productivity.
【0007】さらに、本発明は、電気溶融シリカガラス
管の内側に鉄元素および銅元素含有量の少ない層を形成
する新規な方法を提供することを目的とする。Another object of the present invention is to provide a novel method for forming a layer having a low content of iron and copper elements inside an electrofused silica glass tube.
【0008】[0008]
【課題を解決するための手段】上記目的を達成する本発
明は、結晶質石英粉を電気溶融して得たシリカガラス管
の内表面から少なくとも100μmまでの層中の鉄元素
含有量が100ppb以下で、銅含有量が50ppb以
下であることを特徴とするものである。Means for Solving the Problems The present invention for achieving the above object is to provide a silica glass tube obtained by electromelting a crystalline quartz powder, wherein the iron element content in the layer from the inner surface to at least 100 μm is 100 ppb or less. Wherein the copper content is 50 ppb or less.
【0009】また、本発明は、電気溶融シリカガラス管
を特定の条件下で雰囲気加熱処理することにより鉄元素
および銅元素含有量の少ない層を形成することを特徴と
するものである。Further, the present invention is characterized in that a layer having a small content of iron element and copper element is formed by subjecting an electrofused silica glass tube to an atmospheric heat treatment under specific conditions.
【0010】上記において、「結晶質石英粉」とは、水
晶等の天然の結晶質二酸化ケイ素を粉砕し精製して得た
ガラス原料粉を意味する。この結晶質石英粉の粒径は1
0〜1000μm、より好ましくは50〜500μmで
あり、粒径が10μm以下では石英粉が細か過ぎ気泡が
発生する。また、粒径が1000μm以上では純化が困
難で、不純物の混入が起こり易くなる。[0010] In the above description, "crystalline quartz powder" means glass raw material powder obtained by pulverizing and refining natural crystalline silicon dioxide such as quartz. The particle size of this crystalline quartz powder is 1
When the particle size is 10 μm or less, the quartz powder is too fine and bubbles are generated. On the other hand, when the particle size is 1000 μm or more, purification is difficult, and impurities are likely to be mixed.
【0011】また、上記において「空焼き」とは、炉芯
管を電気炉にセットし、ウエーハを挿入しない状態で、
加熱し、炉芯管内部の汚染や電気炉内のホコリを除去す
ることをいう。[0011] In the above description, "blank" means that the furnace core tube is set in an electric furnace, and no wafer is inserted.
Heating means removing contamination inside the furnace core tube and dust inside the electric furnace.
【0012】さらに、上記において「雰囲気加熱処理」
とは、酸素雰囲気、窒素雰囲気または塩素および塩化水
素雰囲気中で電気溶融シリカガラス管を加熱処理するこ
とをいう。Further, in the above, "atmosphere heat treatment"
This means that the electrofused silica glass tube is heat-treated in an oxygen atmosphere, a nitrogen atmosphere, or a chlorine and hydrogen chloride atmosphere.
【0013】上記電気溶融シリカガラス管において内表
面から100μmまでの層の鉄元素含有量が100pp
b以下で、銅含有量が50ppb以下であれば、酸水素
火炎溶融シリカガラス炉芯管と同じ空焼き時間で規格値
以上のウエーハを得ることができるが、より好ましくは
前記層の厚みが100μm以上1mm以下がよい。50
μm以下では効果がない。他方、層の厚みを1mm以上
に形成することは技術的に困難である。In the above electrofused silica glass tube, the iron element content of the layer from the inner surface to 100 μm is 100 pp.
b or less, if the copper content is 50 ppb or less, it is possible to obtain a wafer having a specified value or more in the same baking time as the oxyhydrogen flame fused silica glass furnace core tube, but more preferably the thickness of the layer is 100 μm It is preferably at least 1 mm. 50
There is no effect below μm. On the other hand, it is technically difficult to form a layer having a thickness of 1 mm or more.
【0014】電気溶融シリカガラス管の内層面から少な
くとも100μmの層の鉄元素含有量が100ppb以
下で、銅元素含有量が50ppb以下とするには、前記
電気溶融シリカガラス管を少なくとも1時間、雰囲気加
熱処理すればよい。前記加熱を長時間行なえば鉄元素お
よび銅元素の少ない層の厚さを大きくすることができる
がコスト的に高いものになり経済性に欠ける。In order to make the iron element content of the layer at least 100 μm from the inner layer surface of the electro-fused silica glass tube at 100 ppb or less and the copper element content at 50 ppb or less, the electro-fused silica glass tube is kept in the atmosphere for at least 1 hour. Heat treatment may be performed. If the heating is performed for a long time, the thickness of the layer containing less iron element and copper element can be increased, but the cost becomes high and the economy is lacking.
【0015】上記雰囲気加熱処理温度は900〜130
0℃の範囲がよい。処理温度が900℃以下では、鉄元
素および銅元素の除去に長時間を要し経済性に欠ける。
また1300℃以上ではガラス管自体が変形し好ましく
ない。The above-mentioned atmosphere heat treatment temperature is 900 to 130.
A range of 0 ° C. is preferred. When the treatment temperature is 900 ° C. or less, it takes a long time to remove the iron element and the copper element, which is not economical.
If the temperature is higher than 1300 ° C., the glass tube itself is undesirably deformed.
【0016】上記鉄含有量および銅含有量の少ない層以
外のシリカガラス層中には鉄元素の含有量は100pp
b以上でもかまわないが、200ppb以下が好まし
い。また、銅元素の含有量は50ppb以上でも構わな
いが、100ppb以下が好ましい。In the silica glass layers other than the layers having a low iron content and a low copper content, the iron element content is 100 pp.
Although it may be more than b, it is preferably 200 ppb or less. The content of the copper element may be 50 ppb or more, but is preferably 100 ppb or less.
【0017】以下に実施例を示しさらに本発明を詳細に
説明する。Hereinafter, the present invention will be described in detail with reference to Examples.
【0018】(ライフタイムの測定法)セミテックス製
LIFE TECHー88Rを使用してウエーハ面内の
ライフタイムをマップ測定する。(Method of Measuring Life Time) The life time in the wafer surface is measured by map using LIFE TECH-88R manufactured by Semitex.
【0019】(鉄元素および銅元素含有量の測定法)シ
リカガラスの内表面を、弗酸の蒸気で溶解し、この蒸気
を凝縮した後、前記弗酸溶液を原子吸光分光光度計にて
測定する。なお、溶解したシリカガラスの厚みについて
は、溶解後のシリカガラスの肉厚を測定し、溶解前との
差を計算し、厚みを確認した。(Measurement method of iron element and copper element content) The inner surface of silica glass is dissolved with hydrofluoric acid vapor, and after condensing this vapor, the hydrofluoric acid solution is measured with an atomic absorption spectrophotometer. I do. In addition, about the thickness of the melt | dissolved silica glass, the thickness of the silica glass after melt | dissolution was measured, the difference with before melt | dissolution was calculated, and the thickness was confirmed.
【0020】[0020]
【0021】 [0021]
【0022】得られたウエーハのライフタイムを測定し
たところ表1のとおりであった。Table 1 shows the measured lifetime of the obtained wafer.
【0023】[0023]
【表1】 [Table 1]
【0024】[0024]
【発明の効果】上記表1に示すように本発明の電気溶融
シリカガラス管は、酸水素溶融シリカガラス管と同じ空
焼き時間で、ほぼ同様の規格値のライフタイムを達成す
ることができる。しかもそのシリカガラスの粘度は未処
理電気溶融シリカガラスのそれとほとんど変わるところ
がない。このように、本発明のシリカガラス管は、熱処
理温度が1100℃と高温で行われる半導体の熱処理用
として優れたシリカガラス管である。As shown in the above Table 1, the electrofused silica glass tube of the present invention can achieve almost the same standardized lifetime with the same baking time as the oxyhydrogen fused silica glass tube. Moreover, the viscosity of the silica glass is almost the same as that of the untreated electrofused silica glass. Thus, the silica glass tube of the present invention is an excellent silica glass tube for heat treatment of semiconductors performed at a high heat treatment temperature of 1100 ° C.
【0025】他方、酸水素溶融シリカガラス炉芯管は確
かに鉄元素を多く含むにもかかわらずライフタイムの優
れたウエーハを得ることができるが、1100℃で使用
したとき、炉芯管の変形が起こり、その取替時間は前記
本発明の炉芯管の半分以下で行う必要があり、半導体熱
処理用としては不適なシリカガラス管である。On the other hand, the oxyhydrogen-fused silica glass furnace core tube can certainly provide a wafer having an excellent life time despite containing a large amount of iron element. The replacement time must be less than half that of the furnace core tube of the present invention, and is a silica glass tube unsuitable for semiconductor heat treatment.
フロントページの続き (58)調査した分野(Int.Cl.6,DB名) C03B 20/00 C03C 3/06 H01L 21/22 H01L 21/324Continuation of the front page (58) Field surveyed (Int. Cl. 6 , DB name) C03B 20/00 C03C 3/06 H01L 21/22 H01L 21/324
Claims (2)
ガラス管の内表面から少なくとも100μmの層の鉄元
素含有量が100ppb以下で、銅元素含有量が50p
pb以下であることを特徴とする半導体熱処理用シリカ
ガラス管。1. A layer of at least 100 μm from the inner surface of a silica glass tube obtained by electromelting crystalline quartz powder has an iron element content of 100 ppb or less and a copper element content of 50 pb or less.
A silica glass tube for heat-treating a semiconductor, which has a pb or less.
ガラス管を900〜1300℃で、雰囲気加熱処理を少
なくとも1時間行うことを特徴とする半導体熱処理用シ
リカガラス管の製造方法。2. A method for producing a silica glass tube for semiconductor heat treatment, comprising subjecting a silica glass tube obtained by electromelting crystalline quartz powder to heat treatment at 900 to 1300 ° C. for at least one hour.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4301628A JP2777858B2 (en) | 1992-10-15 | 1992-10-15 | Silica glass tube for heat treatment of semiconductor and method for producing the same |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP4301628A JP2777858B2 (en) | 1992-10-15 | 1992-10-15 | Silica glass tube for heat treatment of semiconductor and method for producing the same |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH06128100A JPH06128100A (en) | 1994-05-10 |
JP2777858B2 true JP2777858B2 (en) | 1998-07-23 |
Family
ID=17899237
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4301628A Expired - Fee Related JP2777858B2 (en) | 1992-10-15 | 1992-10-15 | Silica glass tube for heat treatment of semiconductor and method for producing the same |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2777858B2 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1988005505A1 (en) * | 1987-01-19 | 1988-07-28 | Kabushiki Kaisha Daikin Seisakusho | Damper disc |
JP4169325B2 (en) * | 2002-07-31 | 2008-10-22 | 信越石英株式会社 | Quartz glass jig and manufacturing method thereof |
-
1992
- 1992-10-15 JP JP4301628A patent/JP2777858B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JPH06128100A (en) | 1994-05-10 |
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