JP2008105903A - Method for manufacturing titania-silica glass - Google Patents

Method for manufacturing titania-silica glass Download PDF

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JP2008105903A
JP2008105903A JP2006290877A JP2006290877A JP2008105903A JP 2008105903 A JP2008105903 A JP 2008105903A JP 2006290877 A JP2006290877 A JP 2006290877A JP 2006290877 A JP2006290877 A JP 2006290877A JP 2008105903 A JP2008105903 A JP 2008105903A
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titania
silica
silica glass
glass
heat
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Shinji Kawabata
真司 河端
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Coorstek KK
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Covalent Materials Corp
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    • 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
    • C03B2201/00—Type of glass produced
    • C03B2201/06—Doped silica-based glasses
    • C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
    • C03B2201/40—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn
    • C03B2201/42—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with transition metals other than rare earth metals, e.g. Zr, Nb, Ta or Zn doped with titanium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for effectively manufacturing titania-silica glass which is practically free from bubbles and is transparent and which can be suitably used as an optical member such as a mask, a mirror material or the like in extreme-ultraviolet light lithography. <P>SOLUTION: The titania-silica glass is manufactured by heat-treating a porous titania-silica containing 1-10 wt.% of titania produced by the VAD method, to prepare a calcined titania-silica body and subjecting the calcined titania-silica body to a treatment for making it transparent under a vacuum atmosphere, at 1,600-1,800°C and at 0.1-1 MPa using a carbon mold. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

本発明は、チタニアを含むシリカガラスに関し、特に、半導体・液晶等の製造工程において、超紫外光リソグラフィ（以下、ＥＵＶリソグラフィという。）のフォトマスクまたはミラー材等の光学用部材として好適に使用されるチタニア−シリカガラスの製造方法に関する。   The present invention relates to silica glass containing titania, and is particularly suitably used as an optical member such as a photomask or mirror material for extreme ultraviolet lithography (hereinafter referred to as EUV lithography) in the manufacturing process of semiconductors and liquid crystals. The present invention relates to a method for producing titania-silica glass.

近年の半導体集積回路の高集積化において、微細加工技術は、最も重要な役割を担っている。半導体集積回路のさらなる微細化に伴い、光リソグラフィ技術の開発も進んでおり、その一つとして、露光光源にＥＵＶ光を用いたＥＵＶリソグラフィが注目されている。
このＥＵＶ光は、波長が１３．５ｎｍ以下で高エネルギーを有することから、あらゆる材料に吸収されるため、反射光学系のリソグラフィシステムが採用されている。 The microfabrication technology plays the most important role in the recent high integration of semiconductor integrated circuits. With further miniaturization of semiconductor integrated circuits, development of optical lithography technology is also progressing. As one of them, EUV lithography using EUV light as an exposure light source has attracted attention.
Since this EUV light has a high energy at a wavelength of 13.5 nm or less, it is absorbed by any material, and therefore a reflection optical lithography system is employed.

ＥＵＶリソグラフィにおいては、フォトマスク基板には、高出力レーザが照射されるため、サブナノメータオーダーでの熱的安定性が要求される。
したがって、フォトマスク基板の材料としては、従来のフォトリソグラフィに用いられていたシリカガラスよりも、低熱膨張のガラスが必要となる。 In EUV lithography, since the photomask substrate is irradiated with a high-power laser, thermal stability on the sub-nanometer order is required.
Therefore, as a material for the photomask substrate, a glass having a low thermal expansion is required as compared with silica glass used in conventional photolithography.

このような低熱膨張ガラスとしては、例えば、チタニア−シリカガラスが知られている。このチタニア−シリカガラスは、従来は、例えば、特許文献１に記載されているように、シリカ前駆体およびチタニア前駆体を火炎加水分解して得られた多孔質ガラス体を昇温して透明化し、成形後、アニール処理することにより製造されていた。   For example, titania-silica glass is known as such a low thermal expansion glass. This titania-silica glass has been conventionally made transparent by elevating the temperature of a porous glass body obtained by flame hydrolysis of a silica precursor and a titania precursor, as described in Patent Document 1, for example. It was manufactured by annealing after molding.

また、合成シリカガラスの製造方法としては、特許文献２に記載されているような高周波誘導発熱体を用いたゾーンシンター方式による製造方法が提案されている。
特開２００５−２２９５４号公報 特開２００４−３５９５２０号公報 Moreover, as a manufacturing method of synthetic silica glass, the manufacturing method by the zone sintering system using the high frequency induction heating body as described in patent document 2 is proposed.
JP 2005-22594 A JP 2004-359520 A

上記特許文献１に記載されているような従来のチタニア−シリカガラスの製造方法は、熱源に接触する方式ではなく、高温に長時間曝さなければならず、実質的に無気泡のチタニア−シリカガラスを効率的に得ることは困難であった。   The conventional method for producing titania-silica glass described in Patent Document 1 is not a method of contacting a heat source, but must be exposed to a high temperature for a long time, and is substantially bubble-free titania-silica glass. It was difficult to obtain the above efficiently.

そこで、本発明者は、上記特許文献２に記載されているようなゾーンシンター方式による透明化技術に着目し、真空雰囲気下での透明化処理により無気泡化を図ることを試みた。
具体的には、ＶＡＤ（Vapor-phase Axial Desposition）法により作製したチタニア−シリカ多孔体を高周波誘導発熱体であるカーボン筒状体内に配置し、真空雰囲気下で誘導加熱する方法により、透明化処理を試みた。 In view of this, the inventor of the present invention has focused on the transparency technique using the zone sinter method as described in Patent Document 2 described above, and has attempted to eliminate bubbles by a transparency treatment in a vacuum atmosphere.
Specifically, a titania-silica porous body produced by a VAD (Vapor-phase Axial Desposition) method is placed in a carbon cylindrical body, which is a high-frequency induction heating element, and transparentized by a method of induction heating in a vacuum atmosphere. Tried.

しかしながら、上記透明化処理においては、カーボンが高温真空下に曝されることにより、実質的に還元性ガス雰囲気となるため、チタニア−シリカ多孔体の表面が還元され、金属チタン等のチタニアの還元物の析出が生じた。
このため、前記チタニア−シリカ多孔体の表面を覆う金属チタン等によって輻射光が反射され、チタニア−シリカ多孔体の内部にまで熱が十分に伝わらず、内部はガラス転移温度に達せず、仮焼体のままの状態となり、得られるガラス体は熱膨張が大きくなるという課題を有していた。 However, in the above-described clearing treatment, the carbon is exposed to a high temperature vacuum, so that a substantially reducing gas atmosphere is formed. Therefore, the surface of the titania-silica porous body is reduced, and titania such as titanium metal is reduced. Precipitation occurred.
For this reason, radiant light is reflected by the titanium metal etc. which covers the surface of the titania-silica porous body, heat is not sufficiently transferred to the inside of the titania-silica porous body, the inside does not reach the glass transition temperature, and calcining is performed. The resulting glass body has a problem that thermal expansion is increased.

したがって、ＥＵＶリソグラフィにおけるフォトマスク材として使用される低熱膨張ガラスである２成分系のチタニア−シリカガラスにおいて、無気泡の透明なガラスを効率的に得ることができる製造方法が求められていた。   Accordingly, there has been a demand for a production method capable of efficiently obtaining a bubble-free transparent glass in a two-component titania-silica glass which is a low thermal expansion glass used as a photomask material in EUV lithography.

本発明は、上記技術的課題を解決するためになされたものであり、ＥＵＶリソグラフィにおけるフォトマスクまたはミラー材等の光学用部材として好適に使用することができる、実質的に無気泡の透明なチタニア−シリカガラスを効率的に製造する方法を提供することを目的とするものである。   The present invention has been made to solve the above technical problem, and is a substantially bubble-free transparent titania that can be suitably used as an optical member such as a photomask or a mirror material in EUV lithography. -It aims at providing the method of manufacturing a silica glass efficiently.

本発明に係るチタニア−シリカガラスの製造方法は、ＶＡＤ法で作製したチタニア１〜１０重量％を含むチタニア−シリカ多孔体を、加熱処理してチタニア−シリカ仮焼体とし、前記チタニア−シリカ仮焼体を、カーボン製型を用いて、真空雰囲気下、１６００〜１８００℃、０．１〜１ＭＰａで透明化処理を行うことを特徴とする。
上記製造方法によれば、チタニア−シリカ多孔体の仮焼体を、蓄熱体または熱源となるカーボン製型に接触させて、ホットプレス法にて透明化処理するため、前記仮焼体の内部にまで十分に熱が伝わり、低膨張かつ実質的に無気泡の透明チタニア−シリカガラスを効率的に得ることができる。 The titania-silica glass manufacturing method according to the present invention is a titania-silica calcined body obtained by heat-treating a titania-silica porous body containing 1 to 10% by weight of titania prepared by the VAD method. The sintered body is subjected to a transparentization treatment at 1600 to 1800 ° C. and 0.1 to 1 MPa in a vacuum atmosphere using a carbon mold.
According to the above manufacturing method, the calcined body of the titania-silica porous body is brought into contact with a carbon mold serving as a heat storage body or a heat source and subjected to a transparent treatment by a hot press method. Thus, heat can be sufficiently transferred to the transparent titania-silica glass with low expansion and substantially no bubbles.

前記仮焼体は、ゾーンシンター方式による熱処理によって得ることが好ましい。
このような加熱方式を採用して仮焼体を得ることにより、より気泡の少ない透明チタニア−シリカガラスを得ることができる。 The calcined body is preferably obtained by heat treatment by a zone sintering method.
By employing such a heating method to obtain a calcined body, a transparent titania-silica glass with fewer bubbles can be obtained.

上述したとおり、本発明に係る製造方法によれば、実質的に無気泡の透明チタニア−シリカガラスを効率的に製造することができる。
したがって、前記チタニア−シリカガラスは、フォトマスクまたはミラー材等の光学用部材として好適に用いることができ、特に、半導体・液晶等の製造工程におけるＥＵＶリソグラフィにおいて、好適に使用することができ、ひいては、半導体・液晶等の各種処理工程における歩留の向上に寄与し得る。 As described above, according to the production method of the present invention, a substantially bubble-free transparent titania-silica glass can be produced efficiently.
Therefore, the titania-silica glass can be suitably used as an optical member such as a photomask or a mirror material, and in particular, can be suitably used in EUV lithography in a manufacturing process of a semiconductor / liquid crystal, etc. In addition, it can contribute to the improvement of the yield in various processing steps such as semiconductor and liquid crystal.

以下、本発明について、より詳細に説明する。
本発明に係るチタニア−シリカガラスの製造方法は、ＶＡＤ法で作製したチタニア１〜１０重量％を含むチタニア−シリカ多孔体を、加熱処理してチタニア−シリカ仮焼体とし、前記チタニア−シリカ仮焼体を、カーボン製型を用いて、真空雰囲気下、１６００〜１８００℃、０．１〜１ＭＰａで透明化処理を行うものである。
上記方法においては、透明化処理において、カーボン製型が蓄熱体または熱源となり得るため、熱支配要因が伝導伝熱であり、接触するチタニア−シリカ仮焼体の内部にまで十分に熱を伝えることができ、気泡を実質的に含まない透明なチタニア−シリカガラスを効率的に得ることができる。 Hereinafter, the present invention will be described in more detail.
The titania-silica glass manufacturing method according to the present invention is a titania-silica calcined body obtained by heat-treating a titania-silica porous body containing 1 to 10% by weight of titania prepared by the VAD method. The fired body is subjected to a transparent treatment at 1600 to 1800 ° C. and 0.1 to 1 MPa in a vacuum atmosphere using a carbon mold.
In the above method, since the carbon mold can be a heat storage body or a heat source in the clearing treatment, the heat-dominating factor is conduction heat transfer, and the heat is sufficiently transferred to the inside of the contacted titania-silica calcined body. Thus, a transparent titania-silica glass substantially free of bubbles can be efficiently obtained.

具体的には、まず、ＶＡＤ法によりチタニア１〜１０重量％を含むチタニア−シリカ多孔体を得る。
チタニアの含有量が１重量％未満である場合、得られるチタニア−シリカガラスの熱膨張係数が大きくなり、好ましくない。一方、チタニアの含有量が１０重量％を超える場合は、０〜１００℃の温度範囲において、熱収縮が大きくなる。 Specifically, first, a titania-silica porous body containing 1 to 10% by weight of titania is obtained by the VAD method.
When the titania content is less than 1% by weight, the resulting titania-silica glass has a large thermal expansion coefficient, which is not preferable. On the other hand, when the titania content exceeds 10% by weight, thermal shrinkage increases in a temperature range of 0 to 100 ° C.

前記ＶＡＤ法においては、例えば、チタニア源、シリカ源としては、それぞれ、塩化物である四塩化チタン、四塩化ケイ素を用い、酸水素火炎中での加水分解によって、チタニアを１〜１０重量％含むチタニア−シリカ多孔体（スート体）が得られる。   In the VAD method, for example, as titania source and silica source, titanium tetrachloride and silicon tetrachloride which are chlorides are used, respectively, and 1 to 10% by weight of titania is contained by hydrolysis in an oxyhydrogen flame. A titania-silica porous body (soot body) is obtained.

次に、このスート体を熱処理して仮焼体とする。
この仮焼体を得るための熱処理は、通常、高周波炉内で行われるが、特に、ゾーンシンター方式にて加熱することが好ましい。
このような加熱方式を採用することにより、スート体の下方から順次加熱されるため、スート体上方から適切にガス抜きが行われ、前記スート体中の細孔を、ほとんど残存させることなく除去することができ、より気泡の少ない、無気泡の透明チタニア−シリカガラスを得ることができる。 Next, this soot body is heat-treated to form a calcined body.
The heat treatment for obtaining this calcined body is usually performed in a high-frequency furnace, but it is particularly preferable to heat by a zone sintering method.
By adopting such a heating method, the soot body is sequentially heated from below, so that the gas is appropriately degassed from above the soot body, and the pores in the soot body are removed almost without remaining. It is possible to obtain a bubble-free transparent titania-silica glass with fewer bubbles.

そして、上記により得られた仮焼体をカーボン製型に入れ、真空雰囲気下、０．１〜１ＭＰａの加圧下で、１６００〜１８００℃で透明化処理を施す。
すなわち、上記方法は、ホットプレス法を用いて透明化処理することにより、無気泡のチタニア−シリカガラスを得るものである。
この透明化処理においては、カーボン製型にチタニア−シリカ仮焼体が直接接触するため、従来の輻射伝導と異なり、伝熱伝導によって前記仮焼体に熱を伝えることができる。このため、仮焼体の内部にまでガラス化に十分な熱が伝わり、無気泡の透明チタニア−シリカガラスを得ることができる。 And the calcined body obtained by the above is put into a carbon mold and subjected to a transparent treatment at 1600 to 1800 ° C. under a vacuum atmosphere and under a pressure of 0.1 to 1 MPa.
That is, in the above method, a bubble-free titania-silica glass is obtained by performing a transparent treatment using a hot press method.
In this clearing treatment, since the titania-silica calcined body is in direct contact with the carbon mold, heat can be transferred to the calcined body by heat conduction, unlike conventional radiation conduction. For this reason, heat sufficient for vitrification is transmitted to the inside of the calcined body, and a bubble-free transparent titania-silica glass can be obtained.

前記透明化処理の際の圧力が０．１ＭＰａ未満である場合は、伝熱効果が十分に得られず、前記仮焼体の内部まで十分なガラス化がなされない。一方、前記圧力が１．０ＭＰａを超える場合は、ガラス体に亀裂が発生しやすくなる。
前記圧力は、０．１〜０．８ＭＰａであることがより好ましい。 When the pressure at the time of the transparentization treatment is less than 0.1 MPa, the heat transfer effect is not sufficiently obtained, and sufficient vitrification is not performed up to the inside of the calcined body. On the other hand, when the pressure exceeds 1.0 MPa, the glass body tends to crack.
The pressure is more preferably 0.1 to 0.8 MPa.

また、前記処理温度が１６００℃未満である場合は、前記仮焼体がカーボン製型内に十分に広がらず、成型性が不十分となる。一方、前記処理温度が１８００℃を超える場合は、ＳｉＯxガスが発生し、真空雰囲気が損なわれ、透明化が困難となる。 On the other hand, when the treatment temperature is less than 1600 ° C., the calcined body does not sufficiently spread in the carbon mold, and the moldability becomes insufficient. On the other hand, when the processing temperature exceeds 1800 ° C., SiO x gas is generated, the vacuum atmosphere is impaired, and transparency becomes difficult.

前記透明化処理においては、高周波加熱炉内の雰囲気を、真空からヘリウム等の不活性ガス雰囲気に変えて行ってもよい。
このような不活性ガスの存在は、伝熱媒体の役割を果たし、前記仮焼体の内部にまで、より熱を伝えやすくすることができるため好ましい。 In the transparentization treatment, the atmosphere in the high-frequency heating furnace may be changed from a vacuum to an inert gas atmosphere such as helium.
The presence of such an inert gas is preferable because it serves as a heat transfer medium and can more easily transfer heat to the inside of the calcined body.

また、前記透明化処理においては、前記仮焼体に加える圧力を変化させ、カーボン製型との接触面積を大きくすることにより、高温状態での保持時間を短縮することができる。
このようなホットプレス法による透明化処理は、透明化および成型時に発生する酸化物の揮発量を抑制することができる点でも有利な方法である。 Moreover, in the said transparentization process, the holding time in a high temperature state can be shortened by changing the pressure applied to the said calcined body, and enlarging a contact area with a carbon mold.
Such a transparent treatment by the hot press method is also advantageous in that it can suppress the volatilization amount of the oxide generated during the transparency and molding.

以下、本発明を実施例に基づきさらに具体的に説明するが、本発明は下記の実施例により制限されるものではない。
［実施例１］
ＶＡＤ法によりチタニア含有量５重量％のチタニア−シリカ多孔体を作製し、高周波炉内で、１２００〜１５００℃で仮焼体を作製した。
これを、カーボン製型に入れ、高周波加熱方式のホットプレスを用いて、真空雰囲気下、１７００℃、０．５ＭＰａで３０分間熱処理し、５０ｍｍ×５０ｍｍのチタニア−シリカガラスを得た。
得られたガラス体は、カーボン製型に接触している表面部分には、還元反応が見受けられたが、内部は、実質的に無気泡（１個／ｃｍ3以下）の透明ガラスであった。 EXAMPLES Hereinafter, although this invention is demonstrated more concretely based on an Example, this invention is not restrict | limited by the following Example.
[Example 1]
A titania-silica porous body having a titania content of 5% by weight was produced by the VAD method, and a calcined body was produced at 1200 to 1500 ° C. in a high frequency furnace.
This was put into a carbon mold and heat-treated at 1700 ° C. and 0.5 MPa for 30 minutes in a vacuum atmosphere using a high-frequency heating hot press to obtain a 50 mm × 50 mm titania-silica glass.
In the obtained glass body, a reduction reaction was observed on the surface portion in contact with the carbon mold, but the inside was a transparent glass substantially free of bubbles (1 piece / cm 3 or less). .

［実施例２］
チタニア−シリカ多孔質体のチタニア含有量を８重量％とし、それ以外については、実施１と同様にして、チタニア−シリカガラスを作製した。
得られたガラス体は、カーボン製型に接触している表面部分には、還元反応が見受けられたが、内部は、実質的に無気泡（１個／ｃｍ3以下）の透明ガラスであった。 [Example 2]
A titania-silica glass was prepared in the same manner as in Example 1 except that the titania content of the titania-silica porous body was 8% by weight.
In the obtained glass body, a reduction reaction was observed on the surface portion in contact with the carbon mold, but the inside was a transparent glass substantially free of bubbles (1 piece / cm 3 or less). .

［実施例３］
仮焼体の作製を、抵抗発熱体を用いたゾーンシンター方式にて、コイル上昇速度０．２ｍｍ／ｍｉｎで、１２００〜１５００℃で行い、それ以外については、実施例１と同様にして、チタニア−シリカガラスを作製した。
得られたガラス体は、カーボン製型に接触している表面部分には、還元反応が見受けられたが、内部は、無気泡の透明ガラスであった。 [Example 3]
The calcined body was produced by a zone sintering method using a resistance heating element at a coil rising speed of 0.2 mm / min at 1200 to 1500 ° C., and the rest was performed in the same manner as in Example 1 except for titania. -Silica glass was prepared.
In the obtained glass body, a reduction reaction was observed on the surface portion in contact with the carbon mold, but the inside was a bubble-free transparent glass.

［比較例１］
仮焼していないチタニア−シリカ多孔体をカーボン製型に入れ、高周波炉内で、真空雰囲気下、１７００℃で３０分間熱処理し、チタニア−シリカガラスを作製した。
得られたガラス体は、気泡が多く残存していた。また、熱処理時に加圧しなかったため、型との接触面積が小さく、伝導伝熱効果が十分に得られず、内部までは十分にガラス化していなかった。 [Comparative Example 1]
A titania-silica porous body that was not calcined was placed in a carbon mold and heat-treated in a high-frequency furnace at 1700 ° C. for 30 minutes in a high-frequency furnace to produce titania-silica glass.
The obtained glass body had many bubbles remaining. In addition, since no pressure was applied during the heat treatment, the contact area with the mold was small, a sufficient conductive heat transfer effect was not obtained, and the interior was not sufficiently vitrified.

［比較例２］
熱処理時の圧力を３０ＭＰａとし、それ以外については、実施例３と同様にして、チタニア−シリカガラスを作製した。
得られたガラス体は、高圧のため、亀裂が発生した。 [Comparative Example 2]
Titania-silica glass was produced in the same manner as in Example 3 except that the pressure during the heat treatment was 30 MPa.
The obtained glass body was cracked due to high pressure.

［比較例３］
ＶＡＤ法によりチタニア含有量５重量％のチタニア−シリカ多孔体を作製し、仮焼せずに、高周波炉内でゾーンシンター方式にて、真空雰囲気下、最高到達温度１８００℃で熱処理した。
得られたガラス体の表面部分は、還元反応により金属チタンが析出し、内部は、ガラス化まで至らず、仮焼体に止まった。
表面に析出した金属チタンが、輻射光を反射し、内部にまで輻射伝導が及ばなかったことが原因であると考えられる。 [Comparative Example 3]
A titania-silica porous body having a titania content of 5% by weight was prepared by the VAD method, and was heat-treated at a maximum reached temperature of 1800 ° C. in a vacuum atmosphere in a high-frequency furnace by a zone sintering method without calcining.
On the surface portion of the obtained glass body, metal titanium was deposited by a reduction reaction, and the inside did not reach vitrification, but remained as a calcined body.
It is thought that this is because the titanium metal deposited on the surface reflects radiation light and does not reach the inside.

Claims (2)

ＶＡＤ法で作製したチタニア１〜１０重量％を含むチタニア−シリカ多孔体を、熱処理してチタニア−シリカ仮焼体とし、前記チタニア−シリカ仮焼体を、カーボン製型を用いて、真空雰囲気下、１６００〜１８００℃、０．１〜１ＭＰａで透明化処理を行うことを特徴とするチタニア−シリカガラスの製造方法。   A titania-silica porous body containing 1 to 10% by weight of titania prepared by the VAD method is heat-treated to form a titania-silica calcined body, and the titania-silica calcined body is subjected to a vacuum atmosphere using a carbon mold. , 1600-1800 ° C., 0.1-1 MPa, a titania-silica glass production method characterized by performing a transparentization treatment. 前記仮焼体をゾーンシンター方式による熱処理によって得ることを特徴とする請求項１記載のチタニア−シリカガラスの製造方法。   The method for producing a titania-silica glass according to claim 1, wherein the calcined body is obtained by heat treatment by a zone sintering method.
JP2006290877A 2006-10-26 2006-10-26 Method for manufacturing titania-silica glass Pending JP2008105903A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004359520A (en) * 2003-06-06 2004-12-24 Toshiba Ceramics Co Ltd Method and apparatus for manufacturing synthetic silica glass
JP2005298322A (en) * 2004-03-18 2005-10-27 Shinetsu Quartz Prod Co Ltd Large size synthetic quartz glass plate for excimer uv lamp device
JP2006103988A (en) * 2004-10-01 2006-04-20 Asahi Glass Co Ltd MANUFACTURING METHOD OF SILICA GLASS CONTAINING TiO2

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004359520A (en) * 2003-06-06 2004-12-24 Toshiba Ceramics Co Ltd Method and apparatus for manufacturing synthetic silica glass
JP2005298322A (en) * 2004-03-18 2005-10-27 Shinetsu Quartz Prod Co Ltd Large size synthetic quartz glass plate for excimer uv lamp device
JP2006103988A (en) * 2004-10-01 2006-04-20 Asahi Glass Co Ltd MANUFACTURING METHOD OF SILICA GLASS CONTAINING TiO2

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