JP2004127958A - Apparatus and method for performing high pressure anneal steam treatment - Google Patents

Apparatus and method for performing high pressure anneal steam treatment Download PDF

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JP2004127958A
JP2004127958A JP2002285383A JP2002285383A JP2004127958A JP 2004127958 A JP2004127958 A JP 2004127958A JP 2002285383 A JP2002285383 A JP 2002285383A JP 2002285383 A JP2002285383 A JP 2002285383A JP 2004127958 A JP2004127958 A JP 2004127958A
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pressure
reaction vessel
oxygen
steam treatment
supply line
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Japanese (ja)
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Masaru Kawahara
河原　勝
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Kyoshin Engineering KK
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Kyoshin Engineering KK
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a high pressure anneal steam treatment apparatus and method in which generation of SiOH radicals is suppressed in a quartz tube, i.e. a reaction vessel 7. <P>SOLUTION: After steam treatment is performed up to a given time (t2), pressure in a reaction vessel 24 is reduced slightly and oxygen is supplied into the reaction vessel 24 through an oxygen supply line 44 in order to compensate for the pressure reduction. Oxygen supply is stopped when the pressure in the reaction vessel returns back to p1. Consequently, an initial pressure p1 is substantially held in the reaction vessel 24. During that interval, temperature in the reaction vessel 24 is sustained at an initial level d1. The pressure reduction and oxygen supply operations are repeated several times. Subsequently, an oxygen substitution action is performed and oxidation reaction is repeated several times up to a specified time (t3). Undesirable SiOH radicals react on oxygen through oxidation reaction and the majority thereof disappears. <P>COPYRIGHT: (C)2004,JPO

Description

【０００１】
【発明の属する技術分野】
本発明は、液晶用ガラス基板やシリコンウエーハ等を高圧アニール処理する方法及びそれを実施するための装置に関し、特に液晶用ガラス基板やシリコンウエーハ等を高圧アニール水蒸気処理するための新規な方法及び装置に関する。
【０００２】
【従来の技術】
液晶用ガラス基板やシリコンウエーハ等を高圧アニール処理する場合にはエキシマレーザーを使用する方法が広く知られている。このエキシマレーザーアニール方法は、液晶用ガラス基板やシリコンウエーハ等の表面を６００℃又はそれ以上の高温まで加熱し表面を酸化してそこに酸化膜を形成するというものである。しかしながら、この方法では、しばしば通常のソーダガラスのように軟化点が５００−６００℃程度のガラスはエキシマレーザーが発生する高熱に耐えることが出来ずガラス表面が溶解するという事故が発生した。そこで、多くの場合、エキシマレーザーを使用する場合には通常のソーダガラスの代わりに軟化点が１４００−１７００℃程度の石英ガラスを使用することが要求された。しかし、この石英ガラスは一般に高価であり経済的でない。この経済上の問題がネックとなり、エキシマレーザーの代替方法が真剣に検討された。
【０００３】
その結果考え出された方法としてレーザーアニール方法である。この方法は、ガラス表面だけを瞬間的に酸化させるものである。この方法によれば、通常のソーダガラスを使用した場合でも表面が溶けるということが無く、高価な石英ガラスの使用が不要となった。しかしながら、このレーザーアニール方法では別の問題点が発生した。それは、レーザーアニール方法では精度の高い酸化膜を形成することが困難であり所望の高精度なガラスの酸化膜加工が期待出来ないことが判明したのである。
【０００４】
そこで当業界において更に熱心な研究が継続された。その結果、今から約２０数年前の１９８０年代になって図３及び図４に示すような高圧アニール水蒸気処理装置が開発された。この装置は、エンドキャップ即ち下部内部容器１内にて加熱手段２、３（図３においては省略）によって加熱された高温の水蒸気４を、ガラス基板カセット５へ配置された被加工物（液晶用ガラス基板やシリコンウエーハ）６を配置したクオーツチューブ即ち反応容器７内へ供給して高圧アニール水蒸気処理を施すものである。このときクオーツチューブ即ち反応容器７が容器内方からの高温高圧によって破壊されるのを防止するため、当該クオーツチューブ即ち反応容器７全体を大きな圧力容器８内へ収容し、かつ当該圧力容器８とクオーツチューブ即ち反応容器７との間に画定される空間を加圧することで当該クオーツチューブ即ち反応容器７の内外圧力のバランスを取っている。更に、処理反応を迅速化しかつ高品質な酸化膜形成を可能とするため、当該圧力容器８とクオーツチューブ即ち反応容器７との間において被加工物６の周囲に第１付加的加熱ヒーター９を、更にクオーツチューブ即ち反応容器７の上方部分に更に第２付加的加熱ヒーター１０を設けて水蒸気を加熱するものである。
【０００５】
そして、この約２０数年前に開発された方式の具体例としては、図３に示すように装置全体を横方向に長く配置した形式のもの（例えば、非特許文献１参照）や、構造は全く同じであるが図４に示すように装置全体を縦方向に高く配置した形式のもの（例えば、非特許文献２及び特許文献１参照）がある。
【０００６】
【非特許文献１】
坪内夏朗及び平山誠著、「高圧酸化」「Ｓｅｍｉｃｏｎｄｕｃｔｏｒ　Ｗｏｒｌｄ」誌　プレスジャーナル出版、１９８２年９月号、ｐ．８２−８８
【非特許文献２】
カタログ「ＨＩＧＨ　ＰＲＥＳＳＵＲＥ　ＡＮＮＥＡＬ　ＳＹＳＴＥＭ」（高圧アニール装置ＨＰＡ）　石川島播磨重工業株式会社エネルギー事業本部　電子機器事業推進部　営業グループ　カタログ番号３６１１２−００４−１１−０１０３−５００ＭＲ　発行日不明
【特許文献１】
特開平１１−１５２５６７号公報（第１図）
【０００７】
【発明が解決しようとする課題】
高圧アニール水蒸気処理方法はこれまでの問題点の多くを解消し比較的高い酸化レートを得ることが出来たのである。しかしながら、この方法においては、高圧アニール水蒸気処理の際に、水蒸気とガラスとが一部反応してクオーツチューブ即ち反応容器７内にＳｉＯＨ基を発生するということが判明した。この僅かなＳｉＯＨ基はその後の作業において、ガラス表面の酸化膜の平滑度や酸化膜自体の性能上、有害な作用を提供し、製品の品質の均質化を阻害する要因となることが判明した。このため、ＳｉＯＨ基をクオーツチューブ即ち反応容器７内から除去することが望ましい。本発明は高圧アニール水蒸気処理方法において、クオーツチューブ即ち反応容器７内に発生する、このＳｉＯＨ基を減少させるための方法及び装置を提供する。
【０００８】
【課題を解決するための手段】
本発明は、水蒸気処理の際に高温加圧状態の水蒸気と薄板表面とが反応して発生する望ましくないＳｉＯＨ基を減少するために、水蒸気処理を所定時間（ｔ２）まで行なった後、反応容器２４内の圧力を僅かに減圧し、次いで、酸素供給ライン４４を介して反応容器２４内へ酸素を供給してその減圧分を補償する。酸素供給により反応容器内の圧力がｐ１に戻れば直ちに酸素供給を停止する。これにより実質的に反応容器２４内部の圧力は当初の圧力ｐ１を保持するようにする。この間中、反応容器２４内の温度は当初の温度ｄ１を維持するようにする。このような減圧及び酸素供給の動作を数回繰返す。これにより水蒸気と酸素とを置換する酸素置換作用を行ない、酸化反応を所定時間（ｔ３）まで数回繰返す。この酸化の酸化作用により好ましくないＳｉＯＨ基が酸素と反応を起こしその大部分を消滅させるのである。この酸素置換作用を３〜６回程度繰返すことでＳｉＯＨ基の少なくとも７０％以上が無くなる。
【０００９】
【発明の実施の形態】
図１は本発明の高圧アニール水蒸気処理方法を実施する装置の概略図である。この高圧アニール水蒸気処理装置２０は、圧力容器２２を有しており、圧力容器２２の内部には反応容器２４が収容されている。反応容器２４の内部には液晶用ガラス基板やシリコンウエーハ等の高圧アニール水蒸気処理されるべき薄板２６及びこれらの薄板２６を所定の間隔に保持するためのカセット２８が収容されている。この反応容器２４の下部はエンドキャップ３０により閉じられている。また、このエンドキャップ３０は圧力容器２２の内部を上下に封止分断している。
【００１０】
エンドキャップ３０の内部には反応容器２４内へ加熱水蒸気を供給するための加熱水蒸気供給装置３２が収容されている。この装置３２は、端部が純水等の給水源へ連結されている給水ライン３４と、給水ライン３４を開閉するための弁３６と、給水ライン３４により供給された水を収容するためタンク３８と、タンク３８から反応容器２４内へ連結し当該容器２４へ蒸気を提供する蒸気供給ライン４０と、加熱水蒸気供給装置３２全体を加熱するためのヒーター４２と、により構成されている。更に本発明においては、前記タンク３８へ対して、端部が例えば酸素ボンベ等へ接続され、そこから酸素を供給するための酸素供給ライン４４が接続されており、この酸素供給ライン４４には当該ライン４４を開閉するための弁４６が装着されている。
【００１１】
圧力容器２２と反応容器２４との間に画定される空所４８には、反応容器２４を取り囲むように複数のヒーター５０が配置されており、これらのヒーターは当該反応容器２４を介して薄板２６を加熱する作用をしている。また、圧力容器２２の外部からは、先端が反応容器２４内にて終わっている第１窒素供給ライン５２と、同様に先端が前記空所４８内にて終わっている第２窒素供給ライン５４と、が接続されており、これらのラインにはそれぞれ弁５６、５８が設けてある。
【００１２】
次に、本発明の高圧アニール水蒸気処理装置２０の動作について、図２を参照しながら述べる。図２は反応容器２４内の雰囲気の状態を示している作動グラフである。この図において、横軸は時間（Ｔ）を、縦軸は圧力（Ｐ）と温度（℃）とを示す。また、破線で示す曲線６０は、給水ライン３４を介して供給される水がヒーター４２によって加熱され、その後、蒸気供給ライン４０によって供給される水蒸気によって加熱される反応容器２４内の温度変化を示している。また、実線で示す曲線６２は加熱蒸気の導入により加圧される反応容器２４内の圧力変化を示している。
【００１３】
初め、反応容器２４内のカセット２８へ所定数の薄板２６を配置する。次いで、弁３６を開放し給水ライン３４を介してタンク３８内へ給水する。ここに溜められた水はヒーター４２によって加熱され、蒸気となって反応容器２４内へ供給される。即ち、給水ライン３４より供給された水は加熱水蒸気供給装置３２の作動により蒸気となって、反応容器２４内へ供給される。このため、反応容器２４内の温度は時間の経過に概ね比例した状態で次第に上昇する。同様に、蒸気の導入により反応容器２４内の圧力も時間の経過に概ね比例した状態で次第に上昇する。
【００１４】
反応容器２４内の圧力上昇に対抗するため、第２窒素供給ライン５４の弁５８を開放して当該ライン５４より当該圧力上昇に対応する圧力を提供するように窒素ガスをヒーター５０が作用している空所４８へ供給して、反応容器２４の破損を防止する。
【００１５】
一定時間（ｔ１）後に、反応容器２４内の温度及び圧力が高圧アニール水蒸気処理可能な状態（ｄ１及びｐ１）に達する。この雰囲気下で薄板２６へ対して所定の水蒸気処理が行なわれる。このとき、高温加圧状態の水蒸気と薄板表面とが反応して望ましくないＳｉＯＨ基を発生する。そこで水蒸気処理を所定時間（ｔ２）まで行なった後、反応容器２４内の圧力を図示していない公知の減圧手段によって僅かに減圧する。反応容器２４の内部が僅かに減圧したなら直ちに弁４６を開放して酸素供給ライン４４を介して反応容器２４内へ酸素を供給してその減圧分を補償する。酸素供給により反応容器内の圧力がｐ１に戻れば直ちに酸素供給を停止する。これにより実質的に反応容器２４内部の圧力は当初の圧力ｐ１を保持するようにする。
【００１６】
この間中、反応容器２４内の温度は当初の温度ｄ１を維持するようにする。このような減圧及び酸素供給の動作を数回繰返す。これにより水蒸気と酸素とを置換する酸素置換作用を行ない、酸化反応を所定時間（ｔ３）まで数回繰返す。この酸化の酸化作用により好ましくないＳｉＯＨ基が酸素と反応を起こしその大部分が消滅する。この酸素置換作用を３〜６回程度繰返すことでＳｉＯＨ基の少なくとも７０％以上が無くなることが実験の結果判明している。
【００１７】
その後、弁５６を開き第１窒素供給ライン５２から反応容器２４内へ窒素を供給しながら当該反応容器内の温度と圧力とを漸次低下させ、その後、高圧アニール水蒸気処理された薄板２６を取り出す。
【００１８】
【発明の効果】
本発明によれば、これまでの高圧アニール水蒸気処理装置において、高圧アニール水蒸気処理の際に液晶用ガラス基板やシリコンウエーハ等の製品の表面周辺に発生する好ましくないＳｉＯＨ基を簡単な装置及び動作により確実に減少させることが出来た。これにより液晶用ガラス基板やシリコンウエーハ等の製品の表面酸化膜の平滑度や酸化膜自体の性能が著しく上昇し、更に、それらの製品の品質の均質化が達成される。
【図面の簡単な説明】
【図１】本発明の実施例を示す概略図である。
【図２】本発明の反応容器内の雰囲気の状態を示している作動グラフである。
【図３】公知の高圧アニール水蒸気処理装置の例を示す図である。
【図４】別の公知の高圧アニール水蒸気処理装置の例を示す図である。
【符号の説明】
２０：高圧アニール水蒸気処理装置　２２：圧力容器
２４：反応容器　　　　　　　　　　２６：薄板
２８：カセット　　　　　　　　　　３０：エンドキャップ
３２：加熱水蒸気供給装置　　　　　３４：給水ライン
３６：弁　　　　　　　　　　　　　３８：タンク
４０：蒸気供給ライン　　　　　　　４２：ヒーター
４４：酸素供給ライン　　　　　　　４６：弁
４８：空所　　　　　　　　　　　　５０：ヒーター
５２：第１窒素供給ライン　　　　　５４：第２窒素供給ライン
５６、５８：弁　　　　　　　　　　６０、６２：曲線[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for high-pressure annealing of a glass substrate for liquid crystal or a silicon wafer, and an apparatus for performing the same, and in particular, a novel method and apparatus for high-pressure annealing steam processing of a glass substrate for liquid crystal, a silicon wafer, or the like. About.
[0002]
[Prior art]
A method using an excimer laser is widely known when high-pressure annealing is performed on a liquid crystal glass substrate, a silicon wafer, or the like. In this excimer laser annealing method, the surface of a liquid crystal glass substrate or a silicon wafer is heated to a high temperature of 600 ° C. or more to oxidize the surface to form an oxide film thereon. However, with this method, glass having a softening point of about 500 to 600 ° C., such as ordinary soda glass, often cannot withstand the high heat generated by the excimer laser, and the glass surface melts. Therefore, in many cases, when an excimer laser is used, it is required to use quartz glass having a softening point of about 1400 to 1700 ° C. instead of ordinary soda glass. However, this quartz glass is generally expensive and not economical. This economic problem was a bottleneck, and serious consideration was given to alternatives to excimer lasers.
[0003]
As a result, a laser annealing method has been devised. In this method, only the glass surface is instantaneously oxidized. According to this method, even when ordinary soda glass is used, the surface does not melt, and the use of expensive quartz glass is unnecessary. However, this laser annealing method has another problem. That is, it has been found that it is difficult to form a highly accurate oxide film by the laser annealing method, and it is not possible to expect a desired highly accurate glass oxide film processing.
[0004]
Therefore, more ardent research was continued in this industry. As a result, in the 1980s, about 20 years ago, a high-pressure annealing steam treatment apparatus as shown in FIGS. 3 and 4 was developed. In this apparatus, high-temperature steam 4 heated by heating means 2, 3 (omitted in FIG. 3) in an end cap or lower inner container 1 is applied to a workpiece (liquid crystal) disposed in a glass substrate cassette 5. It is supplied into a quartz tube, that is, a reaction vessel 7 on which a glass substrate or a silicon wafer 6 is disposed, and is subjected to high-pressure annealing steam treatment. At this time, in order to prevent the quartz tube or the reaction vessel 7 from being destroyed by the high temperature and high pressure from inside the vessel, the quartz tube or the reaction vessel 7 as a whole is accommodated in a large pressure vessel 8 and the quartz vessel or the reaction vessel 7 is By pressurizing a space defined between the quartz tube, ie, the reaction vessel 7, the pressure inside and outside the quartz tube, ie, the reaction vessel 7, is balanced. Furthermore, a first additional heater 9 is provided around the workpiece 6 between the pressure vessel 8 and the quartz tube or reaction vessel 7 in order to speed up the processing reaction and to form a high quality oxide film. Further, a second additional heater 10 is further provided in the upper portion of the quartz tube or the reaction vessel 7 to heat the steam.
[0005]
As a specific example of the method developed about 20 years ago, as shown in FIG. 3, a device in which the entire device is arranged long in the horizontal direction (for example, see Non-Patent Document 1), There is a type in which the entire device is arranged vertically high as shown in FIG. 4 (for example, see Non-Patent Document 2 and Patent Document 1).
[0006]
[Non-patent document 1]
Natsuro Tsubouchi and Makoto Hirayama, "High Pressure Oxidation", "Semiconductor World", Press Journal, September 1982, p. 82-88
[Non-patent document 2]
Catalog "HIGH PRESSURE anneal system" (high-pressure annealing equipment HPA) Ishikawajima-Harima Heavy Industries, Ltd.
JP-A-11-152567 (FIG. 1)
[0007]
[Problems to be solved by the invention]
The high-pressure annealing steam treatment method solved many of the problems so far and was able to obtain a relatively high oxidation rate. However, it has been found that in this method, during the high-pressure annealing steam treatment, the steam and glass partially react to generate SiOH groups in the quartz tube, that is, the reaction vessel 7. It has been found that this slight SiOH group provides a detrimental effect on the smoothness of the oxide film on the glass surface and the performance of the oxide film itself in the subsequent work, and is a factor that hinders homogenization of product quality. . For this reason, it is desirable to remove the SiOH groups from the quartz tube, that is, the reaction vessel 7. The present invention provides a method and an apparatus for reducing the SiOH groups generated in a quartz tube or the reaction vessel 7 in the high-pressure annealing steam treatment method.
[0008]
[Means for Solving the Problems]
In order to reduce undesirable SiOH groups generated by the reaction between the steam under high pressure and the thin plate surface during the steam treatment, the steam treatment is performed until a predetermined time (t2). The pressure in the chamber 24 is slightly reduced, and then oxygen is supplied into the reaction vessel 24 through the oxygen supply line 44 to compensate for the reduced pressure. As soon as the pressure in the reaction vessel returns to p1 by the supply of oxygen, the supply of oxygen is stopped. Thereby, the pressure inside the reaction vessel 24 is substantially maintained at the initial pressure p1. During this time, the temperature in the reaction vessel 24 is maintained at the initial temperature d1. Such an operation of reducing pressure and supplying oxygen is repeated several times. Thus, an oxygen substitution action for replacing water vapor with oxygen is performed, and the oxidation reaction is repeated several times until a predetermined time (t3). Undesired SiOH groups react with oxygen due to the oxidizing action of this oxidation, and most of them are extinguished. By repeating this oxygen substitution action about 3 to 6 times, at least 70% or more of the SiOH groups are eliminated.
[0009]
BEST MODE FOR CARRYING OUT THE INVENTION
FIG. 1 is a schematic view of an apparatus for performing the high-pressure annealing steam treatment method of the present invention. The high-pressure annealing steam treatment device 20 has a pressure vessel 22, and a reaction vessel 24 is housed inside the pressure vessel 22. Inside the reaction container 24, thin plates 26 to be subjected to high-pressure annealing steam treatment, such as a glass substrate for liquid crystal and silicon wafer, and a cassette 28 for holding these thin plates 26 at predetermined intervals are accommodated. The lower part of the reaction vessel 24 is closed by an end cap 30. Further, the end cap 30 vertically seals and separates the inside of the pressure vessel 22.
[0010]
Inside the end cap 30, a heated steam supply device 32 for supplying heated steam into the reaction vessel 24 is accommodated. The device 32 includes a water supply line 34 having an end connected to a water supply source such as pure water, a valve 36 for opening and closing the water supply line 34, and a tank 38 for containing water supplied by the water supply line 34. And a steam supply line 40 connected from the tank 38 to the inside of the reaction vessel 24 to supply steam to the vessel 24, and a heater 42 for heating the entire heated steam supply device 32. Further, in the present invention, an end of the tank 38 is connected to, for example, an oxygen cylinder or the like, and an oxygen supply line 44 for supplying oxygen from the end is connected to the oxygen supply line 44. A valve 46 for opening and closing the line 44 is mounted.
[0011]
In a space 48 defined between the pressure vessel 22 and the reaction vessel 24, a plurality of heaters 50 are arranged so as to surround the reaction vessel 24, and these heaters are connected to the thin plate 26 via the reaction vessel 24. Has the effect of heating. Also, from the outside of the pressure vessel 22, a first nitrogen supply line 52 whose tip ends in the reaction vessel 24, and a second nitrogen supply line 54 which similarly ends in the cavity 48. , And these lines are provided with valves 56 and 58, respectively.
[0012]
Next, the operation of the high-pressure annealing steam treatment apparatus 20 of the present invention will be described with reference to FIG. FIG. 2 is an operation graph showing the state of the atmosphere in the reaction vessel 24. In this figure, the horizontal axis represents time (T), and the vertical axis represents pressure (P) and temperature (° C.). A curve 60 indicated by a broken line indicates a temperature change in the reaction vessel 24 in which the water supplied through the water supply line 34 is heated by the heater 42 and then heated by the steam supplied by the steam supply line 40. ing. A curve 62 shown by a solid line indicates a pressure change in the reaction vessel 24 which is pressurized by the introduction of the heating steam.
[0013]
First, a predetermined number of thin plates 26 are arranged in a cassette 28 in the reaction container 24. Next, the valve 36 is opened to supply water into the tank 38 via the water supply line 34. The water stored here is heated by the heater 42 and is supplied into the reaction vessel 24 as steam. That is, the water supplied from the water supply line 34 is turned into steam by the operation of the heating steam supply device 32 and is supplied into the reaction vessel 24. For this reason, the temperature in the reaction vessel 24 gradually increases in a state substantially proportional to the passage of time. Similarly, the introduction of steam causes the pressure in the reaction vessel 24 to gradually increase in a state substantially proportional to the passage of time.
[0014]
In order to counter the pressure increase in the reaction vessel 24, the valve 50 of the second nitrogen supply line 54 is opened, and the heater 50 acts on the nitrogen gas so as to provide a pressure corresponding to the pressure increase from the line 54. Is supplied to the empty space 48 to prevent the reaction vessel 24 from being damaged.
[0015]
After a certain time (t1), the temperature and pressure in the reaction vessel 24 reach a state (d1 and p1) where high-pressure annealing steam treatment is possible. Under this atmosphere, the thin plate 26 is subjected to a predetermined steam treatment. At this time, the steam under the high temperature and pressurized state reacts with the surface of the thin plate to generate undesired SiOH groups. Therefore, after performing the steam treatment for a predetermined time (t2), the pressure in the reaction vessel 24 is slightly reduced by a known pressure reducing means (not shown). As soon as the pressure inside the reaction vessel 24 is slightly reduced, the valve 46 is opened and oxygen is supplied into the reaction vessel 24 via the oxygen supply line 44 to compensate for the reduced pressure. As soon as the pressure in the reaction vessel returns to p1 by the supply of oxygen, the supply of oxygen is stopped. Thereby, the pressure inside the reaction vessel 24 is substantially maintained at the initial pressure p1.
[0016]
During this time, the temperature in the reaction vessel 24 is maintained at the initial temperature d1. Such an operation of reducing pressure and supplying oxygen is repeated several times. Thus, an oxygen substitution action for replacing water vapor with oxygen is performed, and the oxidation reaction is repeated several times until a predetermined time (t3). Due to the oxidizing action of this oxidation, undesirable SiOH groups react with oxygen and most of them disappear. Experiments have shown that at least 70% or more of the SiOH groups are eliminated by repeating this oxygen substitution action about 3 to 6 times.
[0017]
Thereafter, the valve 56 is opened to gradually decrease the temperature and pressure in the reaction vessel while supplying nitrogen from the first nitrogen supply line 52 into the reaction vessel 24, and then the high-pressure annealed steam-treated thin plate 26 is taken out.
[0018]
【The invention's effect】
According to the present invention, in a conventional high-pressure annealing steam treatment apparatus, undesired SiOH groups generated around the surface of a product such as a liquid crystal glass substrate or a silicon wafer during high-pressure annealing steam treatment can be reduced by a simple apparatus and operation. It was able to be surely reduced. As a result, the smoothness of the surface oxide film of a product such as a glass substrate for a liquid crystal or a silicon wafer and the performance of the oxide film itself are remarkably improved, and the quality of the product is homogenized.
[Brief description of the drawings]
FIG. 1 is a schematic diagram showing an embodiment of the present invention.
FIG. 2 is an operation graph showing a state of an atmosphere in a reaction vessel of the present invention.
FIG. 3 is a diagram showing an example of a known high-pressure annealing steam treatment apparatus.
FIG. 4 is a diagram showing an example of another known high-pressure annealing steam processing apparatus.
[Explanation of symbols]
20: High pressure annealing steam treatment device 22: Pressure vessel 24: Reaction vessel 26: Thin plate 28: Cassette 30: End cap 32: Heated steam supply device 34: Water supply line 36: Valve 38: Tank 40: Steam supply line 42: Heater 44 : Oxygen supply line 46: Valve 48: Void 50: Heater 52: First nitrogen supply line 54: Second nitrogen supply line 56, 58: Valve 60, 62: Curve

Claims (7)

液晶用ガラス基板やシリコンウエーハ等の薄板２６を高圧アニール水蒸気処理する装置２０であって、圧力容器２２と、圧力容器２２の内部に収容されている反応容器２４と、反応容器２４の内部に収容されている薄板２６及びこれらの薄板２６を所定の間隔に保持するためのカセット２８と、圧力容器２２内部において反応容器２４の下部を閉じておりかつ圧力容器２２の内部を上下に封止分断しているエンドキャップ３０と、エンドキャップ３０と圧力容器２２との間にあり反応容器２４内へ加熱水蒸気を供給するための加熱水蒸気供給装置３２と、を有しており、
加熱水蒸気供給装置３２が、端部が給水源へ連結されている給水ライン３４と、給水ライン３４を開閉するための弁３６と、給水ライン３４により供給された水を収容するためタンク３８と、タンク３８から反応容器２４内へ連結し当該容器２４へ蒸気を提供する蒸気供給ライン４０と、加熱水蒸気供給装置３２全体を加熱するためのヒーター４２と、により構成されており、
圧力容器２２と反応容器２４との間には空所４８が画定されており、この空所４８には、反応容器２４を取り囲むように複数のヒーター５０が配置され、
圧力容器２２の外部からは、先端が反応容器２４内にて終わっている第１窒素供給ライン５２と、同様に先端が前記空所４８内にて終わっている第２窒素供給ライン５４と、が接続されており、これらのラインにはそれぞれ弁５６、５８が設けてある高圧アニール水蒸気処理装置において、
前記反応容器２４へ対して、酸素を供給するための酸素供給ライン４４が接続されていることを特徴とする高圧アニール水蒸気処理装置。An apparatus 20 for subjecting a thin plate 26 such as a liquid crystal glass substrate or a silicon wafer to high-pressure annealing steam treatment, comprising a pressure vessel 22, a reaction vessel 24 contained in the pressure vessel 22, and a reaction vessel 24 contained in the reaction vessel 24. And a cassette 28 for holding the thin plates 26 at predetermined intervals, a lower portion of the reaction container 24 being closed inside the pressure container 22 and the inside of the pressure container 22 being vertically sealed and divided. An end cap 30, and a heated steam supply device 32 between the end cap 30 and the pressure vessel 22 for supplying heated steam into the reaction vessel 24.
A heated water vapor supply device 32 having a water supply line 34 having an end connected to a water supply source, a valve 36 for opening and closing the water supply line 34, a tank 38 for containing water supplied by the water supply line 34, A steam supply line 40 connected from the tank 38 to the inside of the reaction vessel 24 to supply steam to the vessel 24, and a heater 42 for heating the entire heated steam supply device 32;
A space 48 is defined between the pressure vessel 22 and the reaction vessel 24, and a plurality of heaters 50 are arranged in the space 48 so as to surround the reaction vessel 24,
From the outside of the pressure vessel 22, a first nitrogen supply line 52 whose end terminates in the reaction vessel 24, and a second nitrogen supply line 54 which similarly terminates in the cavity 48. Are connected, and these lines are provided with valves 56 and 58, respectively, in a high pressure annealing steam treatment apparatus,
An oxygen supply line 44 for supplying oxygen to the reaction vessel 24 is connected to the high-pressure annealing steam treatment apparatus. 酸素供給ラインが前記タンク３８へ連結されていることを特徴とする請求項１に記載の高圧アニール水蒸気処理装置。The high pressure annealing steam treatment apparatus according to claim 1, wherein an oxygen supply line is connected to the tank (38). 酸素供給ラインの端部が酸素ボンベへ連結されかつ開閉弁４６を有していることを特徴とする請求項１又は２に記載の高圧アニール水蒸気処理装置。The high-pressure annealing steam treatment apparatus according to claim 1 or 2, wherein an end of the oxygen supply line is connected to the oxygen cylinder and has an on-off valve (46). 液晶用ガラス基板やシリコンウエーハ等の薄板２６を高圧アニール水蒸気処理する方法であって、
反応容器２４内のカセット２８へ所定数の薄板２６を配置すること、
給水ライン３４より供給された水を加熱水蒸気供給装置３２により蒸気とし、この蒸気を反応容器２４内へ供給し、反応容器２４内の温度と圧力を上昇すること、
反応容器２４内の圧力上昇に対抗するため、第２窒素供給ライン５４より圧力を提供すること、
一定時間（ｔ１）後に、反応容器２４内の温度及び圧力を高圧アニール水蒸気処理可能な状態（ｄ１及びｐ１）とし、この雰囲気下で所定の水蒸気処理を行なうこと、より成る高圧アニール水蒸気処理方法において、
水蒸気処理を所定時間（ｔ２）まで行なった後、反応容器２４内の圧力を僅かに減圧すること、
反応容器２４の内部が僅かに減圧されたなら直ちに酸素供給ライン４４から反応容器２４内へ酸素を供給してその減圧分を補償し、酸素供給によって反応容器内の圧力がｐ１に戻れば直ちに酸素供給を停止すること、
このような反応容器２４内の減圧及び酸素供給の動作を数回繰返し、これにより水蒸気と酸素とを置換する酸素置換作用を行なうこと、
酸素置換作業中、反応容器２４内の温度を当初の温度ｄ１に維持すること、
酸素置換作用によって置換された酸素により酸化反応を行なうこと、
その後、反応容器内の温度と圧力とを漸次低下させること、
の諸工程により水蒸気処理の際に発生するＳｉＯＨ基を減少することをことを特徴とする高圧アニール水蒸気処理方法。A method for subjecting a thin plate 26 such as a liquid crystal glass substrate or a silicon wafer to high-pressure annealing steam treatment,
Disposing a predetermined number of thin plates 26 in a cassette 28 in the reaction vessel 24;
Converting the water supplied from the water supply line 34 into steam by the heated steam supply device 32, supplying the steam into the reaction vessel 24, and increasing the temperature and pressure in the reaction vessel 24;
Providing pressure from the second nitrogen supply line 54 to counter the pressure increase in the reaction vessel 24;
After a certain time (t1), the temperature and pressure in the reaction vessel 24 are set to a state (d1 and p1) in which high-pressure annealing steam treatment is possible, and a predetermined steam treatment is performed in this atmosphere. ,
After performing the steaming for a predetermined time (t2), the pressure in the reaction vessel 24 is slightly reduced,
As soon as the pressure inside the reaction vessel 24 is slightly reduced, oxygen is supplied from the oxygen supply line 44 into the reaction vessel 24 to compensate for the reduced pressure. Stopping the supply,
Such an operation of reducing the pressure and supplying oxygen in the reaction vessel 24 is repeated several times, thereby performing an oxygen replacement action for replacing steam with oxygen.
Maintaining the temperature inside the reaction vessel 24 at the initial temperature d1 during the oxygen displacement operation;
Performing an oxidation reaction with oxygen replaced by oxygen displacement action,
Thereafter, gradually reducing the temperature and pressure in the reaction vessel,
A high pressure annealing steam treatment method characterized by reducing SiOH groups generated during steam treatment by the various steps. 前記酸素置換作用を３〜６回程度繰返すことを特徴とする請求項４に記載の高圧アニール水蒸気処理方法。The high-pressure annealing steam treatment method according to claim 4, wherein the oxygen substitution action is repeated about 3 to 6 times. 酸素置換の間中、反応容器内の圧力を実質的に当初圧力ｐ１に保持していることを特徴とする請求項４又は５に記載の高圧アニール水蒸気処理方法。The high pressure annealing steam treatment method according to claim 4 or 5, wherein the pressure in the reaction vessel is substantially maintained at the initial pressure p1 during the oxygen substitution. 反応容器内での減圧及び酸素供給による酸素置換作用を３〜６回程度繰返すことを特徴とする請求項４、５又は６に記載の高圧アニール水蒸気処理方法。7. The high pressure annealing steam treatment method according to claim 4, wherein the oxygen replacement action by reducing the pressure and supplying oxygen in the reaction vessel is repeated about 3 to 6 times.
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