JPH04292425A - Production of silica glass - Google Patents
Production of silica glassInfo
- Publication number
- JPH04292425A JPH04292425A JP5439391A JP5439391A JPH04292425A JP H04292425 A JPH04292425 A JP H04292425A JP 5439391 A JP5439391 A JP 5439391A JP 5439391 A JP5439391 A JP 5439391A JP H04292425 A JPH04292425 A JP H04292425A
- Authority
- JP
- Japan
- Prior art keywords
- silica glass
- sol
- gel
- production
- dried
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- -1 silicon alkoxide Chemical class 0.000 claims abstract description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000010703 silicon Substances 0.000 claims abstract description 5
- 238000010304 firing Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 239000012298 atmosphere Substances 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 abstract description 2
- 229960001231 choline Drugs 0.000 abstract description 2
- 239000001307 helium Substances 0.000 abstract description 2
- 229910052734 helium Inorganic materials 0.000 abstract description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- CRNJBCMSTRNIOX-UHFFFAOYSA-N methanolate silicon(4+) Chemical compound [Si+4].[O-]C.[O-]C.[O-]C.[O-]C CRNJBCMSTRNIOX-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は光学用、半導体工業用、
電子工業用、理工学用等に使用されるシリカガラスを製
造する方法に関する。[Industrial Application Field] The present invention is applicable to optics, semiconductor industry,
This invention relates to a method for manufacturing silica glass used in the electronic industry, science and engineering, etc.
【０００２】0002
【従来の技術】シリカガラスは耐熱性、耐蝕性及び光学
的性質に優れていることから、半導体製造に欠かせない
重要な材料であり、さらには光ファイバやＩＣ製造用フ
ォトマスク基板、ＴＦＴ基板などに使用され、その用途
はますます拡大している。従来のシリカガラスの製造法
には、天然石英を電気炉又は酸水素炎により溶解する方
法、あるいは四塩化ケイ素を酸水素炎又はプラズマ炎中
で高温酸化し溶解する方法があるが、いずれの方法も製
造工程に２０００℃あるいはそれ以上の高温を要するた
め大量のエネルギーを消費し、また製造時にそのような
高温に耐える材料が必要なうえ、更に高純度のものが得
られにくい等、経済的、品質的にいくつかの問題点をも
っている。[Prior Art] Silica glass has excellent heat resistance, corrosion resistance, and optical properties, so it is an important material indispensable for semiconductor manufacturing, and is also used for optical fibers, photomask substrates for IC manufacturing, and TFT substrates. It is used for various purposes, and its applications are expanding more and more. Conventional methods for producing silica glass include a method in which natural quartz is melted in an electric furnace or an oxyhydrogen flame, or a method in which silicon tetrachloride is oxidized and melted at high temperature in an oxyhydrogen flame or a plasma flame. However, the manufacturing process requires high temperatures of 2000°C or higher, consuming a large amount of energy.In addition, materials that can withstand such high temperatures are required during manufacturing, and it is difficult to obtain high-purity materials, making it economical. There are some quality issues.
【０００３】これに対し、近年ゾル−ゲル法と呼ばれる
シリカガラスを低温で合成する方法が注目されている。
その概要を簡単に述べる。シリコンアルコキシドに水を
加え加水分解し、シリカヒドロゾルとする。この時、シ
リコンアルコキシドと水が均一な系となるように、溶媒
に通常、適当なアルコールが添加される。このシリカゾ
ルを静置、昇温、ゲル化剤の添加等によってゲル化させ
る。その後、ゲルから溶媒、水分を蒸発させたのち、こ
れを乾燥することにより乾燥ゲルとする。この乾燥ゲル
を通常、鏡面を研磨したシリカガラス板上に載せ、適当
な雰囲気中で焼成することによりシリカガラスを得る。On the other hand, in recent years, a method called the sol-gel method for synthesizing silica glass at low temperatures has been attracting attention. The outline will be briefly described below. Add water to silicon alkoxide and hydrolyze it to form silica hydrosol. At this time, an appropriate alcohol is usually added to the solvent so that the silicon alkoxide and water form a homogeneous system. This silica sol is gelled by standing still, increasing the temperature, adding a gelling agent, etc. Thereafter, after evaporating the solvent and water from the gel, this is dried to obtain a dry gel. This dried gel is usually placed on a mirror-polished silica glass plate and fired in an appropriate atmosphere to obtain silica glass.
【０００４】0004
【発明が解決しようとする課題】しかし、上記のゾル−
ゲル法によるシリカガラスの製造法には次の問題がある
。すなわち、乾燥ゲルを焼成する際に、敷板のシリカガ
ラスが変形するので、得られるシリカガラスも変形する
。また、敷板として、耐熱性がシリカガラスよりも優れ
たアルミナや炭化ケイ素から成るセラミック板を用いた
場合は高純度で大形のシリカガラスは得られにくいこと
である。本発明は、上記問題点を解決し、高純度で大形
のシリカガラスを製造する方法を提供するものである。[Problem to be solved by the invention] However, the above sol
The gel method for producing silica glass has the following problems. That is, when the dry gel is fired, the silica glass of the base plate is deformed, so the obtained silica glass is also deformed. Furthermore, when a ceramic plate made of alumina or silicon carbide, which has better heat resistance than silica glass, is used as the bottom plate, it is difficult to obtain a high-purity, large-sized silica glass. The present invention solves the above-mentioned problems and provides a method for producing high-purity, large-sized silica glass.
【０００５】[0005]
【課題を解決するための手段】本発明は、シリコンアル
コキシドを加水分解してシリカゾルとし、これをゲル化
し、乾燥して乾燥ゲルとしたのち焼成するシリカガラス
の製造法において、乾燥ゲルを焼成する段階で、乾燥ゲ
ルをカーボンから成る敷板に載せ、焼成することを特徴
とするシリカガラスの製造法に関するものである。[Means for Solving the Problems] The present invention provides a method for producing silica glass in which silicon alkoxide is hydrolyzed to produce silica sol, this is gelled, dried to form a dry gel, and then fired, in which the dried gel is fired. The present invention relates to a method for producing silica glass characterized in that, in the step, a dried gel is placed on a base plate made of carbon and fired.
【０００６】本発明で用いる敷板は、カーボンから成る
敷板である。カーボンから成る敷板としては、例えば、
コークス、ピッチ等の炭素材料を混練、粉砕、成形した
のち不活性ガス雰囲気下で焼成したもの、あるいは熱硬
化性樹脂を成形、硬化したのち不活性ガス雰囲気下で焼
成したもの、又はメタン、ベンゼン等の炭化水素を出発
材料としてＣＶＤ法でつくったもの等がある。これらは
、いずれも原料の組成及び炭化の熱処理条件により、種
々の気孔率及び黒鉛結晶化率をもつものが得られるが、
本発明では焼成時の温度で変形しない程度の強度をもつ
ものであれば気孔率及び黒鉛結晶化率は特に限定するも
のではない。敷板の形状は、面が平らで操作時に割れな
い程度の厚みをもった板状がよい。これらのカーボンか
ら成る板は市販品を入手することも容易である。[0006] The bottom plate used in the present invention is a bottom plate made of carbon. For example, as a floor plate made of carbon,
Carbon materials such as coke and pitch are kneaded, crushed, molded and then fired in an inert gas atmosphere, or thermosetting resins are molded and hardened and then fired in an inert gas atmosphere, or methane, benzene, etc. There are products made by the CVD method using hydrocarbons such as the following as starting materials. All of these can be obtained with various porosity and graphite crystallinity depending on the composition of the raw material and the heat treatment conditions for carbonization.
In the present invention, the porosity and graphite crystallization rate are not particularly limited as long as the material has enough strength not to be deformed at the firing temperature. The shape of the bottom plate is preferably a plate with a flat surface and a thickness that does not break during operation. These plates made of carbon are easily available commercially.
【０００７】[0007]
【実施例】シリコンテトラメトキシド（Ｓｉ（ＯＣＨ３
）４）の重縮合物とメタノールを１：３のモル比となる
ように量りとり、この溶液に１０ｍＭのコリン水溶液を
シリコンテトラメトキシド１モルに対し水が２．５モル
となるように加え、充分混合してシリカゾルを得た。
得られたゾルをポリフッ化エチレンでコーティングした
直径２００ｍｍのガラスシャーレに深さ１０ｍｍまで入
れ、密封して室温でゲル化した。ゲル化したのち、ガラ
スシャーレの蓋を、穴のある蓋に代えて６０℃で１００
日間乾燥し、その後１５０℃まで３０℃／日の昇温速度
で加温し、乾燥ゲルを得た。この乾燥ゲルをシリカガラ
ス板の上に載せ、焼成炉中、空気雰囲気下で８００℃ま
で５０℃／時間の昇温速度で加熱し、その後、シリカガ
ラス板の敷板の代わりにカーボンの敷板（厚さ５ｍｍ）
の上に載せ、焼成炉中、ヘリウム雰囲気下で１４００℃
まで１００℃／時間の昇温速度で加熱し、シリカガラス
を得た。得られたシリカガラスは反りや変形はみられな
かった。[Example] Silicon tetramethoxide (Si(OCH3)
) Weigh out the polycondensate from 4) and methanol at a molar ratio of 1:3, and add 10 mM choline aqueous solution to this solution so that the ratio of water to 1 mole of silicon tetramethoxide is 2.5 moles. and thoroughly mixed to obtain silica sol. The obtained sol was placed in a glass Petri dish with a diameter of 200 mm coated with polyfluoroethylene to a depth of 10 mm, sealed, and gelatinized at room temperature. After gelatinization, replace the lid of the glass petri dish with a lid with holes and heat at 60℃ for 100 minutes.
The gel was dried for several days, and then heated to 150° C. at a rate of 30° C./day to obtain a dry gel. This dry gel was placed on a silica glass plate and heated to 800°C in an air atmosphere at a heating rate of 50°C/hour in a firing furnace. 5mm)
1400℃ in a helium atmosphere in a firing furnace.
Silica glass was obtained by heating at a temperature increase rate of 100° C./hour. The obtained silica glass showed no warping or deformation.
【０００８】[0008]
【発明の効果】本発明により、ゾル−ゲル法で大形の高
純度シリカガラスの製造が可能となる。[Effects of the Invention] According to the present invention, it is possible to produce large-sized, high-purity silica glass by the sol-gel method.
Claims (1)
カゾルとし、これをゲル化し、乾燥して乾燥ゲルとした
のち焼成するシリカガラスの製造法において、乾燥ゲル
を焼成する段階で、乾燥ゲルをカーボンから成る敷板に
載せ、焼成することを特徴とするシリカガラスの製造法
。Claim 1: In a method for producing silica glass in which silicon alkoxide is hydrolyzed to produce silica sol, this is gelled, dried to form a dry gel, and then fired, in the step of firing the dry gel, the dry gel is separated from carbon. A method for manufacturing silica glass characterized by placing it on a base plate made of silica glass and firing it.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5439391A JPH04292425A (en) | 1991-03-19 | 1991-03-19 | Production of silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5439391A JPH04292425A (en) | 1991-03-19 | 1991-03-19 | Production of silica glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04292425A true JPH04292425A (en) | 1992-10-16 |
Family
ID=12969442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5439391A Pending JPH04292425A (en) | 1991-03-19 | 1991-03-19 | Production of silica glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04292425A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8163382B2 (en) | 2006-03-27 | 2012-04-24 | 3M Innovative Properties Company | Glass ceramic self-supporting film and process for its production |
| US8464552B2 (en) | 2006-03-27 | 2013-06-18 | 3M Innovative Properties Company | Production of a self-supporting glass film |
-
1991
- 1991-03-19 JP JP5439391A patent/JPH04292425A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8163382B2 (en) | 2006-03-27 | 2012-04-24 | 3M Innovative Properties Company | Glass ceramic self-supporting film and process for its production |
| US8464552B2 (en) | 2006-03-27 | 2013-06-18 | 3M Innovative Properties Company | Production of a self-supporting glass film |
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