JP2002241135A - Method for producing opaque synthetic quartz glass - Google Patents
Method for producing opaque synthetic quartz glassInfo
- Publication number
- JP2002241135A JP2002241135A JP2001033726A JP2001033726A JP2002241135A JP 2002241135 A JP2002241135 A JP 2002241135A JP 2001033726 A JP2001033726 A JP 2001033726A JP 2001033726 A JP2001033726 A JP 2001033726A JP 2002241135 A JP2002241135 A JP 2002241135A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- quartz glass
- synthetic quartz
- opaque synthetic
- temperature
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
- C03B2207/24—Multiple flame type, e.g. double-concentric flame
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体製造プロセ
スの熱処理工程において使用されるフランジや炉芯管、
ダミーウェーハ等を形成する不透明合成石英ガラスの製
造方法に関する。BACKGROUND OF THE INVENTION The present invention relates to a flange or a furnace core tube used in a heat treatment step of a semiconductor manufacturing process,
The present invention relates to a method for manufacturing an opaque synthetic quartz glass for forming a dummy wafer or the like.
【０００２】[0002]
【従来の技術】一般に、フランジや炉芯管、ダミーウェ
ーハ等を形成する合成石英ガラスには、高純度であるこ
と、断熱性や耐熱性（高温強度）に優れていることが求
められる。従来、上記合成石英ガラスの製造方法として
は、特公平８−５６８３号公報記載の耐熱性及び加工性
の優れた合成石英ガラス部材の製造方法が知られてい
る。この製造方法は、精製された揮発性珪素化合物を酸
水素火炎中で加水分解して得られた多孔質ガラス母材を
加熱条件下で、窒素化材と反応させて、該ガラス母材に
窒素を含有させる方法である。そして、上記製造方法に
よって得られる合成石英ガラス部材は、耐熱性及び加工
性に優れ、アルカリ金属等の不純物を実質的に含まない
というものである。2. Description of the Related Art In general, synthetic quartz glass for forming a flange, a furnace core tube, a dummy wafer, and the like is required to have high purity, and excellent heat insulation and heat resistance (high-temperature strength). Conventionally, as a method of manufacturing the synthetic quartz glass, a method of manufacturing a synthetic quartz glass member excellent in heat resistance and workability described in Japanese Patent Publication No. 8-5683 is known. In this production method, a porous glass base material obtained by hydrolyzing a purified volatile silicon compound in an oxyhydrogen flame is reacted with a nitrogenation material under heating conditions, and nitrogen is added to the glass base material. It is a method of containing. And the synthetic quartz glass member obtained by the above-mentioned manufacturing method is excellent in heat resistance and workability, and does not substantially contain impurities such as alkali metals.
【発明が解決しようとする課題】しかし、従来の合成石
英ガラスの製造方法では、Ｓｉ−Ｏ結合よりも結合強度
が高いＳｉ−Ｎ結合を構造中に含有させ、粘性を高めて
シリカ多孔質体の耐熱性を向上し得るものの、シルカ多
孔質体に存在するＳｉ−ＯＨ結合等の欠陥をＳｉ−Ｎ結
合に置換する方法であるので、本質的に窒素含有量、す
なわち、Ｓｉ−Ｎ結合を多くできず、耐熱性が十分とは
いえない不具合がある。However, according to the conventional method for producing synthetic quartz glass, a porous silica material containing Si—N bonds having a bonding strength higher than that of Si—O bonds in the structure to increase the viscosity is used. Although it is a method of replacing defects such as Si—OH bonds existing in the porous silica material with Si—N bonds, the nitrogen content, that is, the Si—N bonds can be essentially improved. There is a problem that the heat resistance is not sufficient and the heat resistance is not sufficient.
【０００３】そこで、本発明は、純度及び断熱性を従来
と同様に保持しつつ、耐熱性を格段に高め得る不透明合
成石英ガラスの製造方法を提供することを目的とする。[0003] Accordingly, an object of the present invention is to provide a method for producing opaque synthetic quartz glass capable of significantly improving heat resistance while maintaining purity and heat insulating properties as in the past.
【０００４】[0004]
【課題を解決するための手段】前記課題を解決するため
の、本発明の第１の不透明合成石英ガラスの製造方法
は、高純度の珪素化合物と窒素化合物を酸水素火炎中で
加水分解して円柱状のシリカ多孔質体を作製し、このシ
リカ多孔質体をＨ2ガスを含むガス雰囲気において１２
００〜１３００℃の温度で熱処理した後、Ｎ2ガス、Ｏ2
ガス又はＡｒガス以上の分子量を持つ希ガス、ＣＯガ
ス、ＣＯ2ガス及びそれらの任意の混合ガスのいずれか
のガス雰囲気において１４００〜１６００℃の温度で熱
処理することを特徴とする。第２の不透明合成石英ガラ
スの製造方法は、高純度の珪素化合物と窒素化合物を酸
水素火炎中で加水分解して円柱状のシリカ多孔質体を作
製し、このシリカ多孔質体をＨ2ガスを含むガス雰囲気
において１２００〜１３００℃の温度で熱処理した後、
Ｎ2ガス、Ｏ2ガス又はＡｒガス以上の分子量を持つ希ガ
ス、ＣＯガス、ＣＯ2ガス及びそれらの任意の混合ガス
のいずれかのガス雰囲気において１４００〜１６００℃
の温度で熱処理し、しかる後に、１７００〜１８５０℃
の温度で成型することを特徴とする。In order to solve the above-mentioned problems, a first method for producing opaque synthetic quartz glass according to the present invention comprises hydrolyzing a high-purity silicon compound and a nitrogen compound in an oxyhydrogen flame. A columnar silica porous body was prepared, and this silica porous body was subjected to a gaseous atmosphere containing H 2 gas for 12 hours.
After heat treatment at a temperature of 00 to 1300 ° C., N 2 gas, O 2
The heat treatment is performed at a temperature of 1400 to 1600 ° C. in a gas atmosphere of any one of a gas or a rare gas having a molecular weight equal to or higher than an Ar gas, a CO gas, a CO 2 gas, and an arbitrary mixed gas thereof. In the second method for producing opaque synthetic quartz glass, a high-purity silicon compound and a nitrogen compound are hydrolyzed in an oxyhydrogen flame to produce a columnar porous silica, and this porous silica is made of H 2 gas. After heat treatment at a temperature of 1200 to 1300 ° C. in a gas atmosphere containing
1400 to 1600 ° C. in a gas atmosphere of any one of a rare gas, a CO gas, a CO 2 gas and a mixed gas thereof having a molecular weight of N 2 gas, O 2 gas or Ar gas or more.
Heat treatment at a temperature of 1700-1850 ° C.
Molding at a temperature of
【０００５】第３の不透明合成石英ガラスの製造方法
は、第１又は第２の方法において、前記円柱状のシリカ
多孔質体を作製した後、それを切り出して板状のシリカ
多孔質体とすることを特徴とする。又、第４の不透明合
成石英ガラスの製造方法は、第１又は第２の方法におい
て、前記Ｈ2ガスを含むガス雰囲気において１２００〜
１３００℃の温度で熱処理した後、円柱状のシリカ多孔
質体を切り出して板状のシリカ多孔質体とすることを特
徴とする。[0005] A third method for producing opaque synthetic quartz glass is that, in the first or second method, after the columnar silica porous body is produced, it is cut out into a plate-like porous silica body. It is characterized by the following. Further, the fourth method for producing opaque synthetic quartz glass is the same as the first or second method, except that the opaque synthetic quartz glass is produced in a gas atmosphere containing the H 2 gas in a range of 1200 to 1200.
After heat treatment at a temperature of 1300 ° C., a columnar porous silica material is cut out to obtain a plate-like porous silica material.
【０００６】前記珪素化合物と窒素化合物の割合は、珪
素元素１００に対して窒素元素５０〜１５００であるこ
とが好ましい。前記珪素化合物は、ＳｉＨnＣｌ4-n（ｎ
＝０〜４）、テトラメトキシシラン及びテトラエトキシ
シランのいずれかであり、窒素化合物は、ＮＨ3ガス、
ＮＯガス及びそれらの混合ガスのいずれかであることが
好ましい。又、前記Ｈ2ガスを含むガス雰囲気が、１Ｖ
ｏｌ．％以上のＨ2ガスを含むＮ2ガス、Ａｒガス及び両
者の混合ガスのいずれかであることが好ましい。It is preferable that the ratio of the silicon compound to the nitrogen compound is 50 to 1500 nitrogen elements with respect to 100 silicon elements. The silicon compound is SiH n Cl 4-n (n
= 0 to 4), one of tetramethoxysilane and tetraethoxysilane, and the nitrogen compound is NH 3 gas,
It is preferable to use any one of NO gas and a mixed gas thereof. The gas atmosphere containing the H 2 gas is 1 V
ol. % Of H 2 gas or more, and it is preferable to use any one of N 2 gas, Ar gas and a mixed gas of both.
【０００７】[0007]
【作用】第１の方法においては、円柱状のシリカ多孔質
体が、Ｓｉ−ＯＨ結合等の欠陥数に関係なく、あらかじ
め結合強度の高いＳｉ−Ｎ結合を所要数構造中に含むも
のとなり、かつ開気孔を保持した状態でＯＨ基及びＣｌ
基を除去された後、閉気孔のみを有するものとなる。第
２の方法においては、円柱状のシリカ多孔質体が、Ｓｉ
−ＯＨ結合等の欠陥数に関係なく、あらかじめ結合強度
の高いＳｉ−Ｎ結合を所要数構造中に含むものとなり、
かつ、開気孔を保持した状態でＯＨ基及びＣｌ基を除去
された後、閉気孔のみを有するものとなり、しかる後
に、所望の形状に成形される。In the first method, the columnar porous silica body contains Si—N bonds having a high bond strength in a required number of structures in advance regardless of the number of defects such as Si—OH bonds. OH groups and Cl while maintaining open pores
After removal of the group, it will have only closed pores. In the second method, the columnar porous silica is made of Si.
Regardless of the number of defects such as -OH bonds, the required number of structures include Si-N bonds having high bond strength in advance,
In addition, after the OH group and the Cl group are removed while maintaining the open pores, only the closed pores are obtained, and thereafter, it is formed into a desired shape.
【０００８】第３の方法においては、円柱状のシリカ多
孔質体が、Ｓｉ−ＯＨ結合等の欠陥数に関係なく、あら
かじめ結合強度の高いＳｉ−Ｎ結合を所要数構造中に含
むものとなった後、板状のシリカ多孔質体とされ、この
板状のシリカ多孔質体が、開気孔を保持した状態でＯＨ
基及びＣｌ基を除去された後、閉気孔のみを有する板状
のものとされ、又は更に所望の板形状にされる。又、第
４の方法においては、円柱状のシリカ多孔質体が、Ｓｉ
−ＯＨ結合等の欠陥数に関係なく、あらかじめ結合強度
の高いＳｉ−Ｎ結合を所要数構造中に含むものとなり、
かつ、開気孔を保持した状態でＯＨ基及びＣｌ基が除去
された後、板状のシリカ多孔質体とされ、この板状のシ
リカ多孔質体が、閉気孔のみを有する板状のものとさ
れ、又は更に所望の板形状とされる。[0008] In the third method, a columnar porous silica material contains Si—N bonds having high bond strength in a required number of structures in advance regardless of the number of defects such as Si—OH bonds. After that, a plate-shaped porous silica material is formed, and the plate-shaped porous silica material is
After the group and Cl group are removed, the plate is made into a plate having only closed pores, or further into a desired plate. In the fourth method, the columnar silica porous body is made of Si.
Regardless of the number of defects such as -OH bonds, the required number of structures include Si-N bonds having high bond strength in advance,
And, after the OH group and the Cl group are removed while maintaining the open pores, a plate-like porous silica is formed, and the plate-like porous silica is a plate-like porous body having only closed pores. Or a desired plate shape.
【０００９】Ｈ2 （水素）ガスを含むガス雰囲気におけ
る熱処理の温度が、１２００℃未満であると、シリカ多
孔質体（石英ガラス）とＨ2ガスとの反応が十分に進ま
なく、ＯＨ（水酸）基及びＣｌ（ハロゲン）基の除去効
果が低い。一方、１３００℃を超えると、シリカ多孔質
体に閉気孔が一部生成し、ＯＨ基及びＣｌ基がシリカ多
孔質体に残留してしまう。If the temperature of the heat treatment in a gas atmosphere containing H 2 (hydrogen) gas is lower than 1200 ° C., the reaction between the porous silica (quartz glass) and H 2 gas does not proceed sufficiently, and OH (water) The effect of removing (acid) groups and Cl (halogen) groups is low. On the other hand, when the temperature exceeds 1300 ° C., some closed pores are generated in the porous silica material, and OH groups and Cl groups remain in the porous silica material.
【００１０】所要の分子量を持つ希ガス等のガス雰囲気
における熱処理の温度が、１４００℃未満であると、焼
成が十分に進まない、一方、１６００℃を超えると、異
常発泡する確率が高くなり、好ましくない。好ましい熱
処理温度は、１４５０〜１５５０℃である。If the temperature of the heat treatment in a gas atmosphere of a rare gas or the like having a required molecular weight is less than 1400 ° C., the sintering does not proceed sufficiently. On the other hand, if it exceeds 1600 ° C., the probability of abnormal foaming increases. Not preferred. A preferred heat treatment temperature is 1450-1550 ° C.
【００１１】又、１４００〜１６００℃の温度での熱処
理のガス雰囲気が、Ｎ2（窒素）ガス、Ｏ2（酸素）ガス
又はＡｒ（アルゴン）ガス以上の分子量を持つ希ガス、
ＣＯ（一酸化炭素）ガス、ＣＯ2（二酸化炭素）ガス及
びそれらの任意の混合ガス以外のガスを用いると、焼成
体が部分的に透明化するなど、所望の不透明合成石英ガ
ラスを得ることができなくなるおそれがある。A gas atmosphere for the heat treatment at a temperature of 1400 to 1600 ° C. is a rare gas having a molecular weight equal to or higher than N 2 (nitrogen) gas, O 2 (oxygen) gas or Ar (argon) gas.
If a gas other than CO (carbon monoxide) gas, CO 2 (carbon dioxide) gas and any mixed gas thereof is used, it is possible to obtain a desired opaque synthetic quartz glass such that the fired body becomes partially transparent. It may not be possible.
【００１２】成型温度が、１７００℃未満であると、石
英ガラスの粘性流動が起き難いため、成型に時間がかか
り、スループットが低下する。一方、１８５０℃を超え
ると、石英ガラスの昇華が起き易くなるため、歩留まり
が低下すると共に、装置へのＳｉＯ（一酸化珪素）付着
等が激しくなり、メンテナンス性が悪くなる。好ましい
熱処理温度は、１７００〜１８００℃である。If the molding temperature is lower than 1700 ° C., viscous flow of the quartz glass hardly occurs, so that it takes a long time for molding and the throughput is reduced. On the other hand, when the temperature exceeds 1850 ° C., sublimation of the quartz glass is apt to occur, so that the yield is lowered and the attachment of SiO (silicon monoxide) to the device becomes severe, which deteriorates the maintainability. A preferred heat treatment temperature is 1700 to 1800 ° C.
【００１３】珪素化合物と窒素化合物の割合が、珪素元
素１００に対して窒素元素５０未満であると、石英ガラ
ス中のＳｉ−Ｎ結合の導入数が少なく、所望の特性を得
ることができなくなる。一方、珪素元素１００に対して
窒素元素１５００を超えると、成型時の異常発泡の原因
となる。より好ましい珪素化合物と窒素化合物の割合
は、珪素元素１００に対して窒素元素１００〜１２００
である。If the ratio of the silicon compound to the nitrogen compound is less than 50 for the nitrogen element with respect to 100 for the silicon element, the number of Si—N bonds introduced into the quartz glass is small, and desired characteristics cannot be obtained. On the other hand, if the nitrogen element exceeds 1500 with respect to the silicon element 100, it causes abnormal foaming during molding. A more preferable ratio of the silicon compound and the nitrogen compound is 100 to 1200 elemental nitrogen for 100 elemental silicon.
It is.
【００１４】１２００〜１３００℃の温度での熱処理の
ガス雰囲気に含まれるＨ2ガスが１Ｖｏｌ．％未満であ
ると、シリカ多孔質体（石英ガラス）とＨ2ガスとの反
応が不十分となる。Ｈ2ガスは、５０〜１００Ｖｏｌ．
％がより好ましい。又、Ｈ2ガスと混合されるガスが、
Ｎガス、Ａｒガス及び両者の混合ガス以外であると、Ｏ
Ｈ基及びＣｌ基の除去効果が低くなる。H 2 gas contained in the gas atmosphere of the heat treatment at a temperature of 1200 to 1300 ° C. is 1 Vol. %, The reaction between the porous silica (quartz glass) and the H 2 gas becomes insufficient. H 2 gas, 50~100Vol.
% Is more preferred. Also, the gas mixed with the H 2 gas is
If it is other than N gas, Ar gas and a mixed gas of both, O
The effect of removing H groups and Cl groups is reduced.
【００１５】[0015]
【発明の実施の形態】以下、本発明の実施の形態につい
て具体的な実施例及び比較例を参照して説明する。 実施例１，２ 先ず、ＶＡＤ(Vapor-phase Axial Deposition ：気相軸
付）法により、表１に示す種類と割合の高純度の珪素化
合物と窒素化合物を酸水素火炎中で加水分解して円柱状
（直径２５０ｍｍ，長さ５００ｍｍ）のシリカ多孔質体
をそれぞれ作製した。次に、各シリカ多孔質体を、表１
に示す割合でＨ2ガスを含む表１に示す種類のガス雰囲
気において、表１に示す温度で熱処理した。次いで、各
シリカ多孔質体を、表１に示すガス雰囲気において、表
１に示す温度で熱処理して不透明合成石英ガラスを得
た。DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to specific examples and comparative examples. Examples 1 and 2 First, by the VAD (Vapor-phase Axial Deposition: with a gas phase shaft) method, a high purity silicon compound and nitrogen compound of the kind and ratio shown in Table 1 were hydrolyzed in an oxyhydrogen flame to obtain a circle. Columnar (diameter 250 mm, length 500 mm) silica porous bodies were produced. Next, each of the porous silica materials is shown in Table 1.
The heat treatment was performed at the temperature shown in Table 1 in a gas atmosphere of the type shown in Table 1 containing H 2 gas at the ratio shown in Table 1. Next, each porous silica was heat-treated at a temperature shown in Table 1 in a gas atmosphere shown in Table 1 to obtain an opaque synthetic quartz glass.
【００１６】[0016]
【表１】 [Table 1]
【００１７】得られた各不透明合成石英ガラスの純度
（ＯＨ基濃度、Ｃｌ基濃度）、断熱性及び耐熱性（粘
度）は、それぞれ表２に示すようになったThe purity (OH group concentration, Cl group concentration), heat insulation and heat resistance (viscosity) of each of the obtained opaque synthetic quartz glasses are as shown in Table 2.
【００１８】[0018]
【表２】 [Table 2]
【００１９】比較例 先ず、ＶＡＤ法により、高純度の珪素化合物（ＳｉＣｌ
4）を酸水素火炎中で加水分解して円柱状（直径２５０
ｍｍ，長さ５００ｍｍ）のシリカ多孔質体を作製した。
次に、シリカ多孔質体をＮＨ3（アンモニア）：Ｎ2＝５
０：５０Ｖｏｌ．％の混合ガス雰囲気において８５０℃
の温度で４時間加熱処理した後、ＮＨ3ガスのみ供給を
停止し、Ｎ2ガス単独の雰囲気においてそのままの温度
を保って１時間熱処理した。次いで、Ｏ2ガスを５０Ｖ
ｏｌ．％混合したガス雰囲気において同温度を保持して
１時間加熱処理して不透明合成石英ガラスを得た。得ら
れた不透明合成石英ガラスの純度、断熱性及び耐熱性
は、表２に示すようになった。Comparative Example First, a high purity silicon compound (SiCl
4 ) is hydrolyzed in an oxyhydrogen flame to obtain a columnar shape (250 mm diameter).
(mm, 500 mm in length).
Next, the silica porous material was subjected to NH 3 (ammonia): N 2 = 5.
0:50 Vol. 850 ° C in a mixed gas atmosphere of
After the heat treatment at a temperature of 4 hours, supply of only NH 3 gas was stopped, and heat treatment was performed for 1 hour in an atmosphere of N 2 gas alone while maintaining the temperature as it was. Next, the O 2 gas is supplied to 50 V
ol. %, And heat-treated for 1 hour while maintaining the same temperature in an atmosphere of mixed gas to obtain opaque synthetic quartz glass. Table 2 shows the purity, heat insulation and heat resistance of the obtained opaque synthetic quartz glass.
【００２０】なお、実施例１と同様にして得られた不透
明合成石英ガラスを１７００〜１８５０°の温度で成型
することによって所望の形状に成形することができた。Incidentally, the opaque synthetic quartz glass obtained in the same manner as in Example 1 was formed at a temperature of 1700 to 1850 ° to obtain a desired shape.
【００２１】[0021]
【発明の効果】以上説明したように、本発明の第１の不
透明合成石英ガラスの製造方法によれば、円柱状のシリ
カ多孔質体が、Ｓｉ−ＯＨ結合等の欠陥数に関係なく、
あらかじめ結合強度の高いＳｉ−Ｎ結合を所要数構造中
に含むものとなり、かつ、開気孔を保持した状態でＯＨ
基及びＣｌ基を除去された後、閉気孔のみを有するもの
となるので、従来と同様の純度と断熱性を保持しつつ、
耐熱性を格段に高めた不透明合成石英ガラスを得ること
ができる。第２の不透明合成石英ガラスの製造方法によ
れば、円柱状のシリカ多孔質体が、Ｓｉ−ＯＨ結合等の
欠陥数に関係なく、あらかじめ結合強度の高いＳｉ−Ｎ
結合を所要数構造中に含むものとなり、かつ、開気孔を
保持した状態でＯＨ基及びＣｌ基を除去された後、閉気
孔のみを有するものとなり、しかる後に、所望の形状に
成形されるので、従来と同様の純度と断熱性を保持しつ
つ、耐熱性を格段に高めた所望形状の不透明合成石英ガ
ラスを得ることができる。As described above, according to the first method for producing opaque synthetic quartz glass of the present invention, the columnar porous silica can be produced regardless of the number of defects such as Si-OH bonds.
In the required number of structures, Si—N bonds having a high bond strength are contained in advance, and OH
After removing the group and Cl group, it will have only closed pores, while maintaining the same purity and heat insulation as before,
An opaque synthetic quartz glass with significantly improved heat resistance can be obtained. According to the second method for producing an opaque synthetic quartz glass, a columnar silica porous body is made of Si—N having a high bond strength in advance regardless of the number of defects such as Si—OH bonds.
The bond is included in the required number of structures, and after the OH group and the Cl group are removed while maintaining the open pores, the structure has only closed pores, and thereafter, it is formed into a desired shape. Thus, it is possible to obtain an opaque synthetic quartz glass having a desired shape with significantly improved heat resistance while maintaining the same purity and heat insulating properties as those of the related art.
【００２２】第３の不透明合成石英ガラスの製造方法に
よれば、円柱状のシリカ多孔質体が、Ｓｉ−ＯＨ結合等
の欠陥数に関係なく、あらかじめ結合強度の高いＳｉ−
Ｎ結合を所要数構造中に含むものとなった後、板状のシ
リカ多孔質体とされ、この板状のシリカ多孔質体が、開
気孔を保持した状態でＯＨ基及びＣｌ基を除去された
後、閉気孔のみを有する板状のものとなり、又は更に所
望の板形状となるので、従来と同様の純度と断熱性を保
持しつつ、耐熱性を格段に高めた板状又は所望板形状の
不透明合成石英ガラスを得ることができる。又第４の不
透明合成石英ガラスの製造方法によれば、円柱状のシリ
カ多孔質体が、Ｓｉ−ＯＨ結合等の欠陥数に関係なく、
あらかじめ結合強度の高いＳｉ−Ｎ結合を所要数構造中
に含むものとなり、かつ、開気孔を保持した状態でＯＨ
基及びＣｌ基が除去された後、板状のシリカ多孔質体と
され、この板状のシリカ多孔質体が閉気孔のみを有する
板状のものとされ、又は更に所望の板形状とされるの
で、従来と同様の純度と断熱性を保持しつつ、耐熱性を
格段に高めた板状又は所望板形状の不透明合成石英ガラ
スを得ることができる。According to the third method for producing opaque synthetic quartz glass, a columnar porous silica material has a high bonding strength in advance of Si—OH regardless of the number of defects such as Si—OH bonds.
After the N-bonds are included in the required number of structures, a plate-shaped porous silica is formed, and the OH group and the Cl group are removed while maintaining the open pores. After that, it becomes a plate having only closed pores or a more desired plate shape, so that while maintaining the same purity and heat insulation as before, a plate shape or a desired plate shape with significantly improved heat resistance Opaque synthetic quartz glass can be obtained. In addition, according to the fourth method for producing opaque synthetic quartz glass, a columnar silica porous body can be formed regardless of the number of defects such as Si-OH bonds.
In the required number of structures, Si—N bonds having a high bond strength are contained in advance, and OH
After the group and Cl group are removed, a plate-shaped porous silica is formed, and the plate-shaped porous silica is formed into a plate having only closed pores, or further formed into a desired plate shape. Therefore, it is possible to obtain an opaque synthetic quartz glass having a plate shape or a desired plate shape with significantly improved heat resistance while maintaining the same purity and heat insulating properties as in the related art.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 生野 浩人 山口県徳山市大字徳山字江口開作8231−５ 徳山東芝セラミックス株式会社内 (72)発明者 周 忠華 神奈川県秦野市曽屋30番地 東芝セラミッ クス株式会社開発研究所内 Ｆターム(参考） 4G014 AH12 AH14 AH15 AH21 AH23 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Hiroto Ikuno 8231-5, Eguchi Kaisaku, Tokuyama, Tokuyama-shi, Yamaguchi Prefecture Inside Tokuyama Toshiba Ceramics Co., Ltd. 4G014 AH12 AH14 AH15 AH21 AH23
Claims (7)
素火炎中で加水分解して、円柱状のシリカ多孔質体を作
製し、このシリカ多孔質体をＨ2ガスを含むガス雰囲気
において１２００〜１３００℃の温度で熱処理した後、
Ｎ2ガス、Ｏ2ガス又はＡｒガス以上の分子量を持つ希ガ
ス、ＣＯガス、ＣＯ2ガス及びそれらの任意の混合ガス
のいずれかのガス雰囲気において１４００〜１６００℃
の温度で熱処理することを特徴とする不透明合成石英ガ
ラスの製造方法。1. A high-purity silicon compound and nitrogen compound are hydrolyzed in an oxyhydrogen flame to produce a columnar silica porous body, and this silica porous body is subjected to a 1200 ppm gas atmosphere containing H 2 gas. After heat treatment at a temperature of ~ 1300 ° C,
1400 to 1600 ° C. in a gas atmosphere of any one of a rare gas, a CO gas, a CO 2 gas and a mixed gas thereof having a molecular weight of at least N 2 gas, O 2 gas or Ar gas.
A method for producing opaque synthetic quartz glass, comprising heat-treating at an ambient temperature.
素火炎中で加水分解して、円柱状のシリカ多孔質体を作
製し、このシリカ多孔質体をＨ2ガスを含むガス雰囲気
において１２００〜１３００℃の温度で熱処理した後、
Ｎ2ガス、Ｏ2ガス又はＡｒガス以上の分子量を持つ希ガ
ス、ＣＯガス、ＣＯ2ガス及びそれらの任意の混合ガス
のいずれかのガス雰囲気において１４００〜１６００℃
の温度で熱処理し、しかる後に、１７００〜１８５０℃
の温度で成型することを特徴とする不透明合成石英ガラ
スの製造方法。2. A high-purity silicon compound and a nitrogen compound are hydrolyzed in an oxyhydrogen flame to produce a columnar porous silica, and this porous silica is subjected to a 1200 ppm gas atmosphere containing H 2 gas. After heat treatment at a temperature of ~ 1300 ° C,
1400 to 1600 ° C. in a gas atmosphere of any one of a rare gas, a CO gas, a CO 2 gas and a mixed gas thereof having a molecular weight of at least N 2 gas, O 2 gas or Ar gas.
Heat treatment at a temperature of 1700-1850 ° C.
A method for producing opaque synthetic quartz glass, characterized by molding at a temperature of
後、それを切り出して板状のシリカ多孔質体とすること
を特徴とする請求項１又は２記載の不透明合成石英ガラ
スの製造方法。3. The method for producing an opaque synthetic quartz glass according to claim 1, wherein the columnar silica porous body is prepared and then cut out to obtain a plate-like porous silica body. .
１２００〜１３００℃の温度で熱処理した後、円柱状の
シリカ多孔質体を切り出して板状のシリカ多孔質体とす
ることを特徴とする請求項１又は２記載の不透明合成石
英ガラスの製造方法。4. A heat treatment at a temperature of 1200 to 1300 ° C. in a gas atmosphere containing the H 2 gas, and then a columnar porous silica is cut out to obtain a plate-like porous silica. Item 3. The method for producing an opaque synthetic quartz glass according to Item 1 or 2.
珪素元素１００に対して窒素元素５０〜１５００である
ことを特徴とする請求項１、２、３又は４記載の不透明
合成石英ガラスの製造方法。5. The method according to claim 1, wherein the ratio of the silicon compound to the nitrogen compound is
5. The method for producing opaque synthetic quartz glass according to claim 1, wherein the nitrogen element is 50 to 1500 with respect to 100 silicon elements.
〜４）、テトラメトキシシラン及びテトラエトキシシラ
ンのいずれかであり、窒素化合物がＮＨ3ガス、ＮＯガ
ス及びそれらの混合ガスのいずれかであることを特徴と
する請求項１、２、３、４又は５記載の不透明合成石英
ガラスの製造方法。6. The method according to claim 1, wherein the silicon compound is SiH n Cl 4-n (= 0
4), any one of tetramethoxysilane and tetraethoxysilane, and the nitrogen compound is any one of NH 3 gas, NO gas, and a mixed gas thereof. Or a method for producing an opaque synthetic quartz glass according to 5.
ｏｌ．％以上のＨ2ガスを含むＮ2ガス、Ａｒガス及び両
者の混合ガスのいずれかであることを特徴とする請求項
１、２、３、４、５又は６記載の不透明合成石英ガラス
の製造方法。7. A gas atmosphere containing H 2 gas is 1 V
ol. The opaque synthetic quartz glass according to any one of claims 1, 2, 3, 4, 5, and 6, wherein the gas is any one of N 2 gas, Ar gas, and a mixed gas containing both H 2 gas and H 2 %. Method.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001033726A JP2002241135A (en) | 2001-02-09 | 2001-02-09 | Method for producing opaque synthetic quartz glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001033726A JP2002241135A (en) | 2001-02-09 | 2001-02-09 | Method for producing opaque synthetic quartz glass |
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| Publication Number | Publication Date |
|---|---|
| JP2002241135A true JP2002241135A (en) | 2002-08-28 |
Family
ID=18897432
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007238419A (en) * | 2006-03-13 | 2007-09-20 | Tosoh Quartz Corp | Opaque sintered compact |
| KR100845506B1 (en) | 2005-11-14 | 2008-07-10 | 세이코 엡슨 가부시키가이샤 | Semiconductor device fabrication method and electronic device fabrication method |
-
2001
- 2001-02-09 JP JP2001033726A patent/JP2002241135A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100845506B1 (en) | 2005-11-14 | 2008-07-10 | 세이코 엡슨 가부시키가이샤 | Semiconductor device fabrication method and electronic device fabrication method |
| JP2007238419A (en) * | 2006-03-13 | 2007-09-20 | Tosoh Quartz Corp | Opaque sintered compact |
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