JPH0797225A - Quartz glass jig and its production - Google Patents
Quartz glass jig and its productionInfo
- Publication number
- JPH0797225A JPH0797225A JP26403993A JP26403993A JPH0797225A JP H0797225 A JPH0797225 A JP H0797225A JP 26403993 A JP26403993 A JP 26403993A JP 26403993 A JP26403993 A JP 26403993A JP H0797225 A JPH0797225 A JP H0797225A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- jig
- temperature
- cleaning
- glass 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.)
- Granted
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
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
- Weting (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、耐エッチング性に優れ
た石英ガラス治具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 quartz glass jig excellent in etching resistance and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】従来、石英ガラスは高純度でしかも耐化
学薬品性に優れているところから、シリコンウエハ−の
ＲＣＡ洗浄等の洗浄治具、例えば槽、容器、キャリア−
等として使用されてきた。石英ガラスには天然溶融石英
ガラスや合成シリカガラスがあるが、合成シリカガラス
は高価なところから、洗浄治具用には専ら天然溶融石英
ガラスが用いられていた。ところが、天然溶融石英ガラ
ス中にはアルカリ金属元素、アルカリ土類金属元素また
は遷移金属元素などの不純物が含まれており、それが洗
浄溶液中に溶出してシリコンウエハ−を汚染したり、あ
るいは洗浄溶液のエッチング作用により洗浄槽壁自体が
減少し洗浄槽の寿命を短くし洗浄コストを高くする等の
欠点があった。2. Description of the Related Art Conventionally, since quartz glass has a high purity and is excellent in chemical resistance, cleaning jigs such as RCA cleaning of silicon wafers, for example, tanks, containers, carriers.
And so on. Quartz glass includes natural fused silica glass and synthetic silica glass, but synthetic fused silica glass is expensive, and therefore natural fused quartz glass has been used exclusively for cleaning jigs. However, natural fused silica glass contains impurities such as alkali metal elements, alkaline earth metal elements or transition metal elements, which are eluted into the cleaning solution to contaminate the silicon wafer or to clean the wafer. Due to the etching action of the solution, the wall of the cleaning tank itself is reduced, which shortens the life of the cleaning tank and increases the cleaning cost.
【０００３】[0003]
【発明が解決しようとする課題】そこで、本発明者等は
上記問題点を解決すべく鋭意研究を重ねた結果、洗浄溶
液のエッチング作用が石英ガラスの仮想温度により影響
され、この仮想温度が１２００℃以下である石英ガラス
からなる治具は各種酸またはアルカリ溶液によるエッチ
ングに対して高い抵抗を示すことを見出し、本発明を完
成したものである。The inventors of the present invention have conducted extensive studies to solve the above problems, and as a result, the etching action of the cleaning solution is affected by the fictive temperature of the quartz glass, and the fictive temperature is 1200. It was found that a jig made of quartz glass having a temperature of not higher than 0 ° C. has a high resistance to etching by various acid or alkali solutions, and completed the present invention.
【０００４】本発明は、仮想温度が１２００℃以下で耐
エッチング性に優れた石英ガラス治具を提供することを
目的とする。An object of the present invention is to provide a quartz glass jig having a fictive temperature of 1200 ° C. or lower and excellent in etching resistance.
【０００５】また、本発明は、耐エッチング性の高い洗
浄用石英ガラス治具を提供することを目的とする。Another object of the present invention is to provide a quartz glass jig for cleaning which has high etching resistance.
【０００６】さらに、本発明は、石英ガラス製板材を溶
接して形成した治具を加熱処理して仮想温度を１２００
℃以下にした石英ガラス治具の製造方法を提供すること
を目的とする。Further, according to the present invention, a jig formed by welding a quartz glass plate material is heat-treated to obtain a virtual temperature of 1200.
It is an object of the present invention to provide a method for manufacturing a quartz glass jig whose temperature is below ℃.
【０００７】[0007]
【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、石英ガラスの仮想温度が１２００℃以下であるこ
とを特徴とする石英ガラス治具およびその製造方法に係
る。The present invention for achieving the above object relates to a quartz glass jig and a method for producing the same, wherein the fictive temperature of the quartz glass is 1200 ° C. or less.
【０００８】上記仮想温度とは、室温の石英ガラスの物
性が、そのガラスの熱履歴によって異なった値をとり、
それらの物性値が設定された温度をいう（Ｒ．Ｂｒｕｃ
ｋｎｅｒ（１９７０）Ｊｏｕｒｎａｌ ｏｆ Ｎｏｎ−
Ｃｒｙｓｔａｌｌｉｎｅ Ｓｏｌｉｄｓ ｖｏｌ．５
ｐｐ１２３〜１７５）。例えば、天然石英を電気溶融し
て得た石英ガラスは約１５００℃の仮想温度を有する
が、この石英ガラスを１５００℃に長時間保持した後水
中に投入して急冷却すると、その石英ガラスの仮想温度
は１５００℃となりその温度特有の物性を示す。ところ
が、１５００℃に長時間保持した石英ガラスを徐冷却す
ると、１５００℃より低い仮想温度を有するようにな
る。このように、石英ガラスの仮想温度は熱処理時の保
持温度と時間および冷却速度を調整することにより容易
に制御することができる。The fictive temperature means that the physical properties of quartz glass at room temperature have different values depending on the thermal history of the glass,
The temperature at which those physical properties are set (R. Bruc
kner (1970) Journal of Non-
Crystalline Solids vol. 5
pp123-175). For example, quartz glass obtained by electromelting natural quartz has a fictive temperature of about 1500 ° C., but if this quartz glass is kept at 1500 ° C. for a long time and then put into water and rapidly cooled, the fictitious glass The temperature is 1500 ° C., which shows the physical properties peculiar to that temperature. However, when the quartz glass kept at 1500 ° C. for a long time is gradually cooled, it has a fictive temperature lower than 1500 ° C. As described above, the fictive temperature of the quartz glass can be easily controlled by adjusting the holding temperature during heat treatment, the time, and the cooling rate.
【０００９】通常、石英ガラス治具はファイア−ポリシ
ュした石英ガラス製板材を溶接して容器に形成したのち
１１３０℃程度の温度でアニ−リング処理して作成され
ているが、該石英ガラス治具は、前記溶接時の熱履歴等
によりその仮想温度は１４００℃〜１５００℃であっ
た。本発明者等の研究によると、前記石英ガラス治具を
１０００〜１２００℃の温度範囲で１時間以上加熱した
後、徐冷するとその治具の仮想温度は１０００℃〜１２
００℃となること、特に重要なのは１０００〜１２００
℃の温度での加熱時間であり、１２００℃では１時間、
１１００℃では５時間加熱することにより仮想温度を１
２００℃以下に設定できることがわかった。そして、前
記仮想温度を有する石英ガラス治具は、フッ化水素酸、
塩酸、硫酸、りん酸等の酸性溶液やアンモニア、カセイ
ソ−ダ、カセイカリ等のアルカリ溶液に対する耐エッチ
ング性が著しく改善された。しかしながら、前記温度お
よび処理時間の範囲以外の熱処理では石英ガラスの仮想
温度は１２００℃以下とならず、耐エッチング性に改善
がみられない。また、降温速度が速くなると、石英ガラ
ス治具に歪みが発生し、問題となるので徐冷が必要であ
る。Usually, the quartz glass jig is made by welding a fire-polished quartz glass plate material to a container and then annealing it at a temperature of about 1130 ° C. Had a fictive temperature of 1400 ° C to 1500 ° C due to the heat history during the welding. According to the study by the present inventors, when the quartz glass jig is heated in the temperature range of 1000 to 1200 ° C. for 1 hour or more and then gradually cooled, the virtual temperature of the jig is 1000 ° C. to 12 ° C.
A temperature of 00 ° C, particularly important is 1000 to 1200
Heating time at a temperature of ℃, 1 hour at 1200 ℃,
At 1100 ° C, the fictive temperature becomes 1 by heating for 5 hours.
It was found that the temperature could be set to 200 ° C or lower. Then, the quartz glass jig having the virtual temperature is hydrofluoric acid,
The etching resistance to acidic solutions such as hydrochloric acid, sulfuric acid, phosphoric acid, etc. and alkaline solutions such as ammonia, caseisode, caustica, etc. was remarkably improved. However, the fictive temperature of the quartz glass does not become 1200 ° C. or lower by heat treatment outside the above range of temperature and treatment time, and no improvement in etching resistance is observed. Further, if the temperature lowering rate becomes faster, the quartz glass jig will be distorted, which becomes a problem, and therefore slow cooling is required.
【００１０】上記仮想温度の測定は、ラマン散乱分光光
度法（Ｆｒａｎｋ Ｌ．Ｇａｌｅｎｅｅｒ（１９８２）
Ｊｏｕｒｎａｌ ｏｆ Ｎｏｎ−Ｃｒｙｓｔａｌｌｉｎ
ｅＳｏｌｉｄｓ ｖｏｌ．４９ ｐｐ５３〜６２。Ａ．
Ｃｈｍｅｌ ａｎｄ Ｇ．Ｍ．Ｓｏｃｈｉｖｋｉｎ（１
９８６）Ｓｏｌｉｄ Ｓｔａｔｅ Ｃｏｍｍｕｎｉｃａ
ｔｉｏｎｓ ｖｏｌ．５８、Ｎｏ．６ ＰＰ３６３〜３
６５．）により行われる。The virtual temperature is measured by Raman scattering spectrophotometry (Frank L. Galeneer (1982).
Journal of Non-Crystallin
eSolids vol. 49 pp53-62. A.
Chmel and G.D. M. Sochivkin (1
986) Solid State Communica
tions vol. 58, No. 6 PP363-3
65. ).
【００１１】以下に実施例で本発明をさらに詳しく説明
するが、本発明はこれらの実施例に限定されるものでは
ない。Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to these Examples.
【００１２】[0012]
実施例１ 天然溶融石英ガラス板材を溶接して洗浄槽を作成した。
この洗浄槽を加熱炉に入れ１１５０℃で２時間保持した
後、３℃／分の降温速度で徐冷した。処理済洗浄槽の仮
想温度を測定したところ１２００℃であった。該洗浄槽
を２８％のＮＨ4ＯＨ溶液で４００時間室温でエッチン
グしたところ、４μｇ／ｃｍ2の損失があった。Example 1 A cleaning tank was prepared by welding a natural fused silica glass plate material.
This cleaning tank was placed in a heating furnace and kept at 1150 ° C. for 2 hours, and then gradually cooled at a temperature decreasing rate of 3 ° C./min. When the fictive temperature of the treated cleaning tank was measured, it was 1200 ° C. When the cleaning bath was etched with a 28% NH 4 OH solution for 400 hours at room temperature, there was a loss of 4 μg / cm 2 .
【００１３】比較例１ 実施例１と同様に天然溶融石英ガラスで洗浄槽を作成
し、１１５０℃の加熱炉に入れ３０分間保持した後、１
０℃／分の降温速度で室温まで徐冷した。該石英ガラス
槽の仮想温度を測定したところ１３５０℃であった。そ
こで、前記洗浄槽を２８％のＮＨ4ＯＨ溶液で４００時
間室温でエッチングしたとところ、７μｇ／ｃｍ2の損
失があった。Comparative Example 1 A cleaning tank was prepared from natural fused silica glass in the same manner as in Example 1, put in a heating furnace at 1150 ° C. and held for 30 minutes, and then 1
It was gradually cooled to room temperature at a temperature decreasing rate of 0 ° C / min. When the fictive temperature of the quartz glass tank was measured, it was 1350 ° C. Then, when the cleaning bath was etched with a 28% NH 4 OH solution at room temperature for 400 hours, there was a loss of 7 μg / cm 2 .
【００１４】実施例２ 天然溶融石英ガラス片を加熱炉に入れ、保持温度および
保持時間を変えて仮想温度１４００℃、１２００℃、１
１００℃の試料を作製した。これらの試料を１７％弗酸
溶液で６０分エッチング処理したところ、損失量はそれ
ぞれ２．１８ｍｇ／ｃｍ2、１．９１ｍｇ／ｃｍ2、１．
７８ｍｇ／ｃｍ2であった。以上のことから、１２００
℃、１１００℃の仮想温度を有する石英ガラス治具はエ
ッチング処理による損失量が少ないことがわかる。Example 2 A piece of natural fused silica glass was placed in a heating furnace, and the fictive temperature was 1400 ° C., 1200 ° C., 1 with changing the holding temperature and the holding time.
A sample at 100 ° C. was prepared. When these samples were etched with a 17% hydrofluoric acid solution for 60 minutes, the loss amounts were 2.18 mg / cm 2 , 1.91 mg / cm 2 , and 1.
It was 78 mg / cm 2 . From the above, 1200
It can be seen that the quartz glass jig having a fictive temperature of 1100 ° C. has a small amount of loss due to the etching process.
【００１５】[0015]
【発明の効果】本発明は、耐エッチングが高く、汚染物
質の溶出が少ない石英ガラス治具である。そして、例え
ば洗浄用治具とした時その寿命は長く、洗浄コストを大
幅に下げることができる。The present invention is a quartz glass jig having high etching resistance and less elution of contaminants. And, for example, when it is used as a cleaning jig, its life is long and the cleaning cost can be significantly reduced.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 瀬川 徹 福島県郡山市田村町金屋字川久保88 信越 石英株式会社石英技術研究所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Toru Segawa 88 Kawakubo, Kanaya, Tamura Town, Koriyama City, Fukushima Prefecture Shin-Etsu Quartz Co., Ltd.
Claims (3)
であることを特徴とする石英ガラス治具。1. A quartz glass jig, characterized in that the fictive temperature of quartz glass is 1200 ° C. or lower.
を特徴とする請求項１記載の石英ガラス治具2. The quartz glass jig according to claim 1, wherein the quartz glass jig is a cleaning jig.
ラス治具を１０００℃〜１２００℃の温度で１時間以上
加熱した後、徐冷することを特徴とする石英ガラス治具
の製造方法。3. A method of manufacturing a quartz glass jig, which comprises heating a quartz glass jig formed by welding a quartz glass plate at a temperature of 1000 ° C. to 1200 ° C. for 1 hour or more and then gradually cooling the quartz glass jig.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05264039A JP3117591B2 (en) | 1993-09-29 | 1993-09-29 | Quartz glass jig and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05264039A JP3117591B2 (en) | 1993-09-29 | 1993-09-29 | Quartz glass jig and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0797225A true JPH0797225A (en) | 1995-04-11 |
| JP3117591B2 JP3117591B2 (en) | 2000-12-18 |
Family
ID=17397706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05264039A Expired - Lifetime JP3117591B2 (en) | 1993-09-29 | 1993-09-29 | Quartz glass jig and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3117591B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302610A (en) * | 2020-02-21 | 2020-06-19 | 连云港国伦石英制品有限公司 | Annealing method of large-size quartz tube |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007101523A (en) | 2005-09-06 | 2007-04-19 | Nisshinbo Ind Inc | Corrosion-resistant member |
-
1993
- 1993-09-29 JP JP05264039A patent/JP3117591B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111302610A (en) * | 2020-02-21 | 2020-06-19 | 连云港国伦石英制品有限公司 | Annealing method of large-size quartz tube |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3117591B2 (en) | 2000-12-18 |
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