JPH09295826A - Production of high-purity transparent silica glass - Google Patents
Production of high-purity transparent silica glassInfo
- Publication number
- JPH09295826A JPH09295826A JP10904596A JP10904596A JPH09295826A JP H09295826 A JPH09295826 A JP H09295826A JP 10904596 A JP10904596 A JP 10904596A JP 10904596 A JP10904596 A JP 10904596A JP H09295826 A JPH09295826 A JP H09295826A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- bubbles
- temperature
- transparent silica
- silica glass
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/02—Pure silica glass, e.g. pure fused quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2203/00—Production processes
- C03C2203/20—Wet processes, e.g. sol-gel process
- C03C2203/24—Wet processes, e.g. sol-gel process using alkali silicate solutions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2203/00—Production processes
- C03C2203/50—After-treatment
- C03C2203/52—Heat-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Compositions (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は気泡を消滅させた高
純度透明シリカガラスの製造方法に関する。光透過性を
利用する各種光学材料、高温型液晶基板などの材料とし
て利用できる。TECHNICAL FIELD The present invention relates to a method for producing high-purity transparent silica glass in which bubbles are eliminated. It can be used as various optical materials that utilize optical transparency, materials for high-temperature liquid crystal substrates, and the like.
【０００２】[0002]
【従来の技術】各種合成シリカ粉末を減圧雰囲気中で１
８００〜１９００℃に加熱し、透明シリカガラスとする
製造方法が従来から知られている。たとえば、特開平３
−３７１２０、特開平３−５３２９、特開平２−２２９
７３５には、アルコキシシランを加水分解したゲルを焼
成することにより得たシリカ粉末を減圧雰囲気下１５０
０〜２２００℃に加熱して透明シリカガラスとする製法
が開示されている。2. Description of the Related Art Various synthetic silica powders are mixed under reduced pressure atmosphere.
A method for producing a transparent silica glass by heating to 800 to 1900 ° C. has been conventionally known. For example, JP
-37120, JP-A-3-5329, JP-A-2-229
In 735, silica powder obtained by calcining a gel obtained by hydrolyzing alkoxysilane is mixed under reduced pressure atmosphere for 150 minutes.
A method for producing a transparent silica glass by heating to 0 to 2200 ° C. is disclosed.
【０００３】上記製法によれば、純度の高い透明シリカ
ガラスが比較的簡単に得られるが、得られたガラスには
気泡が含まれる。気泡の形態は１０〜１００μｍの微小
気泡が散在する場合や０．５〜２ｍｍの大きい気泡が点
在する場合など製法により様々である。また、こうした
ガラスを１２００〜１５００℃に長時間保持すると気泡
周辺部が結晶化してくるという現象も伴う。According to the above-mentioned manufacturing method, a highly pure transparent silica glass can be obtained relatively easily, but the obtained glass contains bubbles. The form of the bubbles varies depending on the manufacturing method, such as the case where fine bubbles of 10 to 100 μm are scattered or the case where large bubbles of 0.5 to 2 mm are scattered. Further, when such glass is kept at 1200 to 1500 ° C. for a long time, there is a phenomenon that the periphery of bubbles is crystallized.
【０００４】従って、光透過性を利用する各種光学材
料、高温型液晶基板などの用途、また高温で長時間使用
する半導体製造用治具などの用途には適さないという課
題があった。Therefore, there is a problem that it is not suitable for various optical materials utilizing light transmittance, high temperature type liquid crystal substrates and the like, and semiconductor manufacturing jigs which are used at high temperature for a long time.
【０００５】[0005]
【発明が解決しようとする課題】本発明の目的は、光透
過性を利用する各種光学材料、高温型液晶基板などの用
途、また高温で長時間使用する半導体製造用治具などの
用途に適する気泡の存在しない高純度透明シリカガラス
の製造方法を提供することにある。SUMMARY OF THE INVENTION The object of the present invention is suitable for various optical materials utilizing optical transparency, high temperature type liquid crystal substrates and the like, and semiconductor manufacturing jigs which are used at high temperature for a long time. It is an object of the present invention to provide a method for producing a high-purity transparent silica glass having no bubbles.
【０００６】[0006]
【課題を解決するための手段】本発明者らは、上記の課
題を解決するために鋭意検討を行った結果、アルカリケ
イ酸水溶液から得られた非晶質シリカ粉末を減圧雰囲気
中で１７１３℃以上の温度に加熱し、得られた透明シリ
カガラスに熱間静水圧プレス処理を施すことにより、ガ
ラス中の１ｍｍ未満の気泡が効果的に消滅することを見
出だし本発明に到達した。すなわち、本発明はアルカリ
金属ケイ酸水溶液と酸とを反応させて得たシリカを精製
することにより、Ｎａ，Ｋ，Ｍｇ，Ｃａ，Ｆｅ，Ａｌの
各不純物を１ｐｐｍ以下とした高純度非晶質シリカ粉末
を出発原料とし、これを１０torr以下の減圧雰囲気中で
クリストバライト溶融温度１７１３℃以上の温度にお
き、透明シリカガラスとする工程とこのガラスに熱間静
水圧プレス装置を用い、１２００〜１３５０℃の温度範
囲で１００〜２００ＭＰａのＡｒ又はＮ2ガス圧力を作
用させ、ガラス中の直径１ｍｍ未満の気泡を消滅させる
工程とからなる高純度シリカガラスの製造方法である。Means for Solving the Problems As a result of intensive studies to solve the above problems, the present inventors have found that an amorphous silica powder obtained from an aqueous solution of alkali silicic acid has a pressure of 1713 ° C. in a reduced pressure atmosphere. The present invention was found to be effective in eliminating bubbles of less than 1 mm in the glass by heating to the above temperature and subjecting the obtained transparent silica glass to hot isostatic pressing. That is, according to the present invention, by refining silica obtained by reacting an aqueous solution of an alkali metal silicic acid with an acid, high-purity amorphous containing each impurity of Na, K, Mg, Ca, Fe, and Al at 1 ppm or less. A silica powder is used as a starting material, and the temperature is set to a cristobalite melting temperature of 1713 ° C. or higher in a reduced pressure atmosphere of 10 torr or less to obtain transparent silica glass. This glass is subjected to a hot isostatic pressing apparatus at 1200 to 1350 ° C. In the temperature range of 100 to 200 MPa of Ar or N 2 gas pressure to eliminate bubbles having a diameter of less than 1 mm in the glass.
【０００７】以下、本発明をさらに詳細に説明する。Hereinafter, the present invention will be described in more detail.
【０００８】出発原料である非晶質シリカ粉末は、アル
カリケイ酸塩水溶液を酸処理し得られるシリカである。
この方法は例えば、特開昭６２−３０１１号、特開昭６
２−３０１２号、特開昭６２−２８３８０９号、特開昭
６２−２８３８１０号に記載されているが、粘性値が２
〜５００ポイズの範囲であるアルカリケイ酸塩水溶液を
孔径１ｍｍ以下のノズルを通して水混和性有機媒体また
は濃度４規定酸溶液からなる凝固浴中に押し出して凝固
し、得られた繊維状のゲルを酸を含む液で処理した後、
水洗して不純物を抽出除去し、さらに１０００℃以上で
加熱処理する方法によって、不純物Ｎａ，Ｋ，Ｍｇ，Ｃ
ａ，Ｆｅ，Ａｌがすべて１ｐｐｍ以下の非晶質シリカを
得ることができる。この粉末を耐熱性容器、例えば高純
度カ−ボンルツボに充填し、加熱処理を行うわけである
が、使用に際して粉末粒度を調製する必要がある。粒度
調製は、一般によく知られたボ−ルミルなどの乾式粉砕
によって行える。粒度範囲は３０〜５００μｍに調製す
ることが好ましい。さらに好ましい範囲は３０〜２００
μｍである。Amorphous silica powder as a starting material is silica obtained by acid treatment of an aqueous alkali silicate solution.
This method is described, for example, in JP-A-62-3011 and JP-A-6-301.
2-3012, JP-A-62-283809 and JP-A-62-283810, the viscosity value is 2
To 500 poises, an alkaline silicate aqueous solution is extruded through a nozzle having a pore size of 1 mm or less into a coagulation bath consisting of a water-miscible organic medium or a 4N acid solution having a concentration to coagulate the resulting fibrous gel. After treatment with a liquid containing
Impurities such as Na, K, Mg, and C were washed by washing with water to remove impurities, and then heat-treated at 1000 ° C. or higher.
Amorphous silica in which a, Fe, and Al are all 1 ppm or less can be obtained. This powder is filled in a heat resistant container, for example, a high-purity carbon crucible and subjected to heat treatment, but it is necessary to adjust the powder particle size before use. The particle size can be adjusted by dry grinding such as a well-known ball mill. The particle size range is preferably adjusted to 30 to 500 μm. A more preferable range is 30 to 200.
μm.
【０００９】透明シリカガラスとする工程は、耐熱容器
に充填したシリカ粉末を１０torr以下の減圧雰囲気下、
クリストバライト溶融温度１７１３℃以上の温度に加熱
することにより行う。加熱処理は通常、カ−ボン抵抗加
熱方式あるいは高周波加熱方式の真空電気炉により行え
る。減圧程度は低い方が好ましく、加熱中１０-1〜１０
-3torrを維持することが理想的であるが、温度上昇によ
りシリカの昇華が起こるため困難であり、１０torr以下
に抑制できればよい。加熱温度は、クリストバライト溶
融温度１７１３℃以上を必要とする。好ましい条件は１
８００〜１８５０℃で１０分間以上保持することであ
る。In the step of forming transparent silica glass, silica powder filled in a heat-resistant container is put under a reduced pressure atmosphere of 10 torr or less,
It is performed by heating to a temperature of 1713 ° C. or higher for the cristobalite melting temperature. The heat treatment is usually carried out in a vacuum electric furnace of carbon resistance heating type or high frequency heating type. It is preferable that the decompression degree is low, and 10 −1 to 10 during heating
It is ideal to maintain -3 torr, but it is difficult because the sublimation of silica occurs due to the temperature rise, and it is sufficient to suppress it to 10 torr or less. The heating temperature requires a cristobalite melting temperature of 1713 ° C. or higher. Preferred condition is 1
It is to hold at 800 to 1850 ° C. for 10 minutes or more.
【００１０】ここで得られる透明シリカガラスに要求さ
れる特性は、直径１ｍｍ以上の気泡が含まれないことで
ある。なぜなら、次の工程、熱間静水圧プレス処理で消
滅できる気泡径には臨界値があり、１ｍｍ以上の気泡を
消滅させることは困難となるからである。この要求特性
を達成するための焼成加熱条件は、減圧雰囲気下１８０
０〜１８５０℃の温度範囲で５分間以上保持し、ガラス
化を終えた後、温度を保持したままＮ2 ，Ａｒなどの不
活性ガスを加圧状態となるよう導入し、気泡を収縮させ
る操作を行うことである。ガス圧力は０．２ＭＰａ以上
とすることが好ましく、さらに好ましくは０．４〜１．
０ＭＰａの範囲である。The characteristic required for the transparent silica glass obtained here is that it does not contain bubbles having a diameter of 1 mm or more. This is because the bubble diameter that can be eliminated in the next step, hot isostatic pressing, has a critical value, and it is difficult to eliminate bubbles of 1 mm or more. The firing and heating conditions for achieving these required characteristics are 180 ° C. under a reduced pressure atmosphere.
An operation of holding the temperature in the temperature range of 0 to 1850 ° C. for 5 minutes or more to finish the vitrification, and then introducing an inert gas such as N 2 or Ar into a pressurized state while keeping the temperature to shrink the bubbles. Is to do. The gas pressure is preferably 0.2 MPa or more, more preferably 0.4 to 1.
It is in the range of 0 MPa.
【００１１】得られたガラスの熱間静水圧プレス処理
は、１２００〜１３５０℃の温度範囲で１００〜２００
ＭＰａのＡｒ又はＮ2 ガス圧力を作用させて行う。温度
範囲を１２００〜１３５０℃に規定した理由は、１２０
０℃以下では２００ＭＰａの圧力を掛けても０．１ｍｍ
以上の気泡を消滅させることができず、また１３５０℃
以上では、気泡は１００ＭＰａの圧力でも効果的に消滅
できるものの、ガラスの結晶化が著しくなるからであ
る。The hot isostatic pressing process of the obtained glass is carried out at a temperature range of 1200 to 1350 ° C. for 100 to 200.
It is performed by applying Ar or N 2 gas pressure of MPa. The reason for defining the temperature range from 1200 to 1350 ° C. is 120
0.1 mm even if a pressure of 200 MPa is applied at 0 ° C or lower
The above bubbles cannot be extinguished, and 1350 ° C
In the above, the bubbles can be effectively extinguished even at a pressure of 100 MPa, but the crystallization of the glass becomes remarkable.
【００１２】気泡を消滅させるには１００ＭＰａ以上の
圧力が必要であり、圧力媒体としてはＡｒガスが最も一
般的であるが、Ｎ2 ガスを利用することも可能である。
熱間静水圧プレスによる気泡の消滅速度は、気泡径、圧
力、ガラスの粘性に依存する。気泡径が大きく、ガラス
の粘性が高いほど、消滅速度は遅くなる。ガラスの粘性
が１２００℃で１０13〜１０13.3ポイズの本発明の高純
度透明シリカガラスの場合、好ましい処理条件は、１３
００℃、１５０ＭＰａ、１〜４時間である。A pressure of 100 MPa or more is required to extinguish bubbles, and Ar gas is the most common pressure medium, but N 2 gas can also be used.
The bubble disappearance rate by hot isostatic pressing depends on the bubble diameter, pressure, and glass viscosity. The larger the bubble diameter and the higher the viscosity of the glass, the slower the extinction rate. In the case of the high-purity transparent silica glass of the present invention having a glass viscosity of 10 13 to 10 13.3 poise at 1200 ° C., preferable treatment conditions are 13
00 ° C., 150 MPa, 1 to 4 hours.
【００１３】熱間静水圧プレス処理したガラスは、未処
理ガラスより密度が約０．６％高くなり、２．２１２〜
２．２２８ｇ／ｃｍ3の値を示す。１１５０〜１２５０
℃で再加熱することにより、もとの密度２．２０〜２．
２１ｇ／ｃｍ3に戻すことができる。The glass subjected to the hot isostatic pressing has a density of about 0.6% higher than that of the untreated glass, which is 2.212 to
A value of 2.228 g / cm 3 is shown. 1150-1250
The original density of 2.20 to 2.
It can be returned to 21 g / cm 3 .
【００１４】以下、実施例によって、本発明をさらに説
明するが、本発明は実施例に限定されるものではない。The present invention will be further described below with reference to examples, but the present invention is not limited to the examples.
【００１５】[0015]
【実施例】 実施例１ アルカリケイ酸塩水溶液を酸処理し、水洗して不純物を
抽出除去し、１２００℃で焼成したシリカをナイロンポ
ット、ナイロンボ−ルを用い粉砕し、平均粒径１００μ
ｍとなるように調製した。得られた粉末を化学分析した
結果は表１の通りであった。Example 1 An alkaline silicate aqueous solution was treated with an acid, washed with water to remove impurities, and the silica calcined at 1200 ° C. was pulverized using a nylon pot and nylon ball to obtain an average particle size of 100 μm.
It was prepared so that m. The results of chemical analysis of the obtained powder are shown in Table 1.
【００１６】[0016]
【表１】 [Table 1]
【００１７】この粉末を高純度処理したカ−ボン容器に
充填し、カ−ボン抵抗加熱炉に設置し、真空度を１０-3
torrまで減圧し、３００℃／ｈｒで１８５０℃まで昇温
し、５分間保持した後、減圧を解除し、窒素ガスを４ｋ
ｇｆ／ｃｍ2 となるまで導入し、さらに５分間保持し
た。保持中の真空度は１torrであった。冷却はガス圧を
かけたまま、放冷した。得られた透明シリカガラスの密
度は２．２１０ｇ／cm3 であった。This powder was filled in a carbon container subjected to high-purity treatment, placed in a carbon resistance heating furnace, and the degree of vacuum was 10 -3.
The pressure was reduced to torr, the temperature was raised to 1850 ° C. at 300 ° C./hr, and the temperature was maintained for 5 minutes.
It was introduced until it reached gf / cm 2, and held for another 5 minutes. The degree of vacuum during holding was 1 torr. Cooling was allowed to cool with the gas pressure applied. The density of the transparent silica glass obtained was 2.210g / cm 3.
【００１８】次に、このガラスを熱間静水圧プレス装置
に入れ、Ａｒガスを圧力媒体とし、６００℃／ｈｒで１
３００℃まで上げ、圧力１５０ＭＰａをかけた状態で１
ｈｒ保持した。Next, this glass was placed in a hot isostatic press, and Ar gas was used as a pressure medium, at 600 ° C./hr for 1 hour.
Raise to 300 ° C and apply pressure of 150MPa 1
It was held for hr.
【００１９】得られたガラスの密度を測定したところ、
２．２２２ｇ／ｃｍ3 であった。When the density of the obtained glass was measured,
It was 2.222 g / cm 3 .
【００２０】熱間静水圧プレス処理前後におけるガラス
中の気泡量は表２に示す通りであり、処理によって無気
泡となったことが判った。The amount of bubbles in the glass before and after the hot isostatic pressing treatment is as shown in Table 2, and it was found that the treatment resulted in no bubbles.
【００２１】[0021]
【表２】 [Table 2]
【００２２】実施例２ 実施例１と同様の製法で得られた粉末をさらに粉砕し、
平均粒径５０μｍとなるように調製した。この粉末を実
施例１と同様の方法で透明シリカガラスとし、熱間静水
圧プレス処理をＡｒを圧力媒体とし１２５０℃、１５０
ＭＰａ、４時間で行った。Example 2 The powder obtained by the same production method as in Example 1 was further pulverized,
The average particle size was adjusted to 50 μm. This powder was made into transparent silica glass by the same method as in Example 1, and hot isostatic pressing was performed at 1250 ° C. and 150 ° C. using Ar as a pressure medium.
It was performed at 4 MPa for 4 hours.
【００２３】熱間静水圧プレス処理前後のガラスの気泡
量、密度、ＯＨ量を測定し、表３に示す結果を得た。The amount of bubbles, the density and the amount of OH of the glass before and after the hot isostatic pressing were measured and the results shown in Table 3 were obtained.
【００２４】[0024]
【表３】 [Table 3]
【００２５】表３から明らかなように、処理により無気
泡となったことが判った。As is clear from Table 3, it was found that the treatment resulted in no bubbles.
【００２６】実施例３ 実施例１で得られた無気泡ガラスの一部を大気炉に入
れ、１２００℃で１０時間保持した。取り出したガラス
に外見上の変化はなかった。密度を測定したところ、
２．２１０ｇ／ｃｍ3 であり、熱間静水圧プレス処理前
に戻ることが判った。また、ガラス内部に気泡の再発生
もまったく見られなかった。Example 3 Part of the bubble-free glass obtained in Example 1 was placed in an atmospheric furnace and kept at 1200 ° C. for 10 hours. There was no apparent change in the glass taken out. When I measured the density,
It was 2.210 g / cm 3 and was found to return to the value before the hot isostatic pressing treatment. In addition, no re-generation of bubbles was observed inside the glass.
【００２７】[0027]
【発明の効果】本発明の製造方法によれば、高純度粉末
を溶融して得たシリカガラスを熱間静水圧プレス処理に
より、無気泡とすることができる。従って、気泡のため
に従来利用できなかった光透過性を必要とする用途、例
えば高温型液晶基板、プリズム、レンズなど各種光学材
料として利用できる。また、気泡周辺の結晶化のために
使用できなかった用途、例えば半導体製造用の各種治工
具類の材料としても利用できる。According to the manufacturing method of the present invention, the silica glass obtained by melting the high-purity powder can be made bubble-free by hot isostatic pressing. Therefore, it can be used for applications requiring light transmittance which has not been conventionally available due to bubbles, for example, various optical materials such as high-temperature liquid crystal substrates, prisms, and lenses. It can also be used as a material that could not be used due to crystallization around bubbles, for example, as a material for various jigs and tools for semiconductor manufacturing.
Claims (1)
せて得たシリカを精製することにより、Ｎａ，Ｋ，Ｍ
ｇ，Ｃａ，Ｆｅ，Ａｌの各不純物を１ｐｐｍ以下とした
高純度非晶質シリカ粉末を出発原料とし、これを１０to
rr以下の減圧雰囲気中でクリストバライト溶融温度１７
１３℃以上の温度におき、直径１ｍｍ以上の気泡を消滅
させた透明シリカガラスとする工程とこのガラスに熱間
静水圧プレス装置を用い、１２００〜１３５０℃の温度
範囲で１００〜２００ＭＰａのＡｒ又はＮ2ガス圧力を
作用させ、ガラス中の直径１ｍｍ未満の気泡を消滅させ
る工程とからなる高純度透明シリカガラスの製造方法。1. A silica obtained by reacting an aqueous solution of an alkali metal silicic acid with an acid is refined to obtain Na, K, M.
A high-purity amorphous silica powder in which each impurity of g, Ca, Fe, and Al is 1 ppm or less is used as a starting material.
Cristobalite melting temperature 17 in a reduced pressure atmosphere of rr or less
The temperature is set to 13 ° C. or higher, and a step of forming a transparent silica glass in which bubbles having a diameter of 1 mm or more are extinguished, and a hot isostatic pressing device is used for this glass, and Ar of 100 to 200 MPa in a temperature range of 1200 to 1350 ° C. or A process for producing high-purity transparent silica glass, which comprises applying N 2 gas pressure to eliminate bubbles having a diameter of less than 1 mm in the glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10904596A JPH09295826A (en) | 1996-04-30 | 1996-04-30 | Production of high-purity transparent silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10904596A JPH09295826A (en) | 1996-04-30 | 1996-04-30 | Production of high-purity transparent silica glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09295826A true JPH09295826A (en) | 1997-11-18 |
Family
ID=14500218
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10904596A Pending JPH09295826A (en) | 1996-04-30 | 1996-04-30 | Production of high-purity transparent silica glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH09295826A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11209132A (en) * | 1998-01-23 | 1999-08-03 | Tosoh Corp | Production of high purity transparent silica glass |
| WO2003070652A1 (en) * | 2002-02-20 | 2003-08-28 | Fujikura Ltd. | Optical glass and method for producing the same |
| WO2007107709A1 (en) * | 2006-03-17 | 2007-09-27 | Saint-Gobain Quartz Plc | Manufacture of large articles in synthetic vitreous silica |
-
1996
- 1996-04-30 JP JP10904596A patent/JPH09295826A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11209132A (en) * | 1998-01-23 | 1999-08-03 | Tosoh Corp | Production of high purity transparent silica glass |
| WO2003070652A1 (en) * | 2002-02-20 | 2003-08-28 | Fujikura Ltd. | Optical glass and method for producing the same |
| US7437893B2 (en) | 2002-02-20 | 2008-10-21 | Fujikura Ltd. | Method for producing optical glass |
| WO2007107709A1 (en) * | 2006-03-17 | 2007-09-27 | Saint-Gobain Quartz Plc | Manufacture of large articles in synthetic vitreous silica |
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