JPH01119527A - Production of silica glass - Google Patents
Production of silica glassInfo
- Publication number
- JPH01119527A JPH01119527A JP27645987A JP27645987A JPH01119527A JP H01119527 A JPH01119527 A JP H01119527A JP 27645987 A JP27645987 A JP 27645987A JP 27645987 A JP27645987 A JP 27645987A JP H01119527 A JPH01119527 A JP H01119527A
- Authority
- JP
- Japan
- Prior art keywords
- gel
- silica glass
- sol
- silica
- silicon alkoxide
- 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.)
- Granted
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 description 12
- -1 Silicon alkoxide Chemical class 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 229920013821 hydroxy alkyl cellulose Polymers 0.000 claims abstract description 12
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 3
- 238000003980 solgel method Methods 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000001879 gelation Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229920002153 Hydroxypropyl cellulose Polymers 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 3
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 2
- 229960001231 choline Drugs 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor 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
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel 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
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
Landscapes
- Glass Melting And Manufacturing (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
（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、理化学用
等に使用されるシリカガラスを製造する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field of Application) The present invention produces silica glass used for optics, semiconductor industry, electronic industry, physics and chemistry, etc.
（従来の技術）
シリカガラスは耐熱性、耐蚤性およ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、ＴＰＴ基板などに使用され、その用途はますます
拡大されている。(Prior technology) Silica glass has excellent heat resistance, flea 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 TPT. It is used for substrates, etc., and its applications are expanding more and more.
従来のシリカガラスの製造法には、天然石英を電気炉ま
た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２，０００℃あ
るいはそれ以上の高温を必要と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
が必要であり、また高純度のものが得にくいなど経済的
９品質的にいくつかの問題点をもっている。Conventional methods for manufacturing silica glass include melting natural quartz in an electric furnace or oxyhydrogen flame, or oxidizing and melting silicon tetrachloride at high temperature in an oxyhydrogen flame or plasma flame. However, the manufacturing process requires high temperatures of 2,000°C or higher, which consumes a large amount of energy, and materials that can withstand such high temperatures are required during manufacturing, and it is difficult to obtain high-purity materials, making it economically difficult. 9. There are some quality problems.
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。On the other hand, in recent years, a method of synthesizing silica glass at low temperature called the sol-gel method has been attracting attention. The outline will be briefly described below.
一般式Ｓ ｉ （ＯＲ） ａ （Ｒ：アルキル基）で
表わされるシリコンアルキシド（本発明に於いては、そ
の重縮合物を含む）９例えば（ＲＯ）３３ ｉ ・（Ｏ
３１（ＯＲ）ｚｌ−・Ｏ３１（ＯＲ）３． （ｎ＝０
〜８．Ｒ：アルキル基）に水（アルカリまたは酸でｐ）
［を調整してもよい）を加え、加水分解し、シリカヒド
ロシル（本発明に於いてはシリカゾルという）とする。Silicon alkoxide (including its polycondensate in the present invention) represented by the general formula S i (OR) a (R: alkyl group) 9 For example, (RO)33 i ・(O
31(OR)zl-・O31(OR)3. (n=0
~8. R: alkyl group) to water (alkali or acid p)
[may be adjusted] and hydrolyzed to obtain silica hydrosil (referred to as silica sol in the present invention).
この時、シリコンアルコキシドと水が均一な系となる様
、一般には溶媒として適当なアルコールが添加されてい
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。その後ゲルを蒸発乾燥することに
よりシリカ乾燥ゲルとする。この乾燥ゲルを適当な雰囲
気中な焼結することによりシリカガラスを得る。At this time, an appropriate alcohol is generally added as a 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, the gel is evaporated to dryness to obtain a dry silica gel. Silica glass is obtained by sintering this dried gel in a suitable atmosphere.
（発明が解決しようとする問題点）
しかし、ゾル−ゲル法によるシリカガラスの製造にはま
だ未解決の問題が残されている。(Problems to be Solved by the Invention) However, there are still unresolved problems in the production of silica glass by the sol-gel method.
特にゲルを乾燥していく過程でゲルにクランクや割れが
発生し易（、クランクや割れのないモノリシックな大形
の乾燥ゲルを歩留り良く製造することが困難となること
である。In particular, during the process of drying the gel, cracks and cracks are likely to occur in the gel (this makes it difficult to produce a monolithic large-sized dried gel without cracks and cracks with a good yield).
本発明はクランクや割れの発生することのないシリカガ
ラスの製造法を提供するものである。The present invention provides a method for manufacturing silica glass that does not cause cracks or cracks.
（問題点を解決するための手段）
本発明は、ゾル−ゲル法によるシリカガラスの製造法に
於て、ゾル調整時に、２％（重量％）水溶液の２０℃で
の粘度が１００−１００００センチボイズであるヒドロ
キソアルキルセルロースを、シリコンアルコキシド１０
０重量部に対し０．１〜５．０重量添加することを特徴
とするものである。(Means for Solving the Problems) The present invention provides a method for producing silica glass using a sol-gel method, in which the viscosity of a 2% (wt%) aqueous solution at 20°C is 100 to 10,000 centivoise during sol preparation. silicon alkoxide 10
It is characterized by adding 0.1 to 5.0 parts by weight relative to 0 parts by weight.
本発明において、シリコンアルコキシドのアルキル基に
ついて、特に制限はないが、加水分解のし易さ、ゲル化
時間の点から、メチル基、エチル基、プロピル基、ブチ
ル店を有するシリコンアルコキシドを使用することが好
ましい、シリコンアルコキシドに水又は水とアルコール
の混合溶液を加えて加水分解してシリカゾルを生成させ
る際、水、アルコール、又は水とアルコールの混合溶液
にあらかじめヒドロキソアルキルセルロースヲ添加。In the present invention, there are no particular restrictions on the alkyl group of silicon alkoxide, but from the viewpoint of ease of hydrolysis and gelation time, silicon alkoxide having a methyl group, ethyl group, propyl group, or butyl group is used. Preferably, when adding water or a mixed solution of water and alcohol to silicon alkoxide and hydrolyzing it to generate silica sol, hydroxoalkyl cellulose is added in advance to water, alcohol, or a mixed solution of water and alcohol.
均一に溶解させておく。Let it dissolve evenly.
添加するヒドロキシアルキルセルロースの分子量は、２
％水溶液の２０℃での粘度が１００〜１００００センチ
ボイスのもの、好ましくは５ｏｏｏ〜８０００センチポ
イズ。The molecular weight of the hydroxyalkylcellulose to be added is 2
% aqueous solution with a viscosity of 100 to 10,000 centipoise at 20°C, preferably 500 to 8,000 centipoise.
最も好ましくは１０００〜６０００センチボイズの範囲
のものが使用でき、これらは単独でも混合物でもよい。Most preferably, those having a range of 1,000 to 6,000 centivoids can be used, and these may be used alone or as a mixture.
ヒドロキシアルキルセルロースの分子量が２％水溶液の
２０℃での粘度で１００センチボイズ未満であると、有
効な効果を得るためには、かなりの量を系内に加える必
要があり。When the molecular weight of hydroxyalkyl cellulose is less than 100 centivoise in terms of the viscosity of a 2% aqueous solution at 20°C, a considerable amount must be added to the system in order to obtain an effective effect.
後のゲルの焼結ガラス化工程でクラックや割れが発生し
易くなる。一方１分子量が２％水溶液の２０℃での粘度
で１００００センチボイズを越えると、著しいゲル化促
進効果のため、均一なゲルを得ることは非常に困難とな
るはかりでなく、ゲルの乾燥過程でゲル中に析出した高
分子量のヒドロキシアルキルセルロースが後の焼成過程
に於いて分解、燃焼する結果、ゲル中に大きな空隙が生
じ、ガラス中に欠陥として残留し易くなる。Cracks and fractures are likely to occur during the subsequent gel sintering and vitrification process. On the other hand, if the viscosity of a 2% aqueous solution at 20°C exceeds 10,000 centivoise, it will be extremely difficult to obtain a uniform gel due to the significant gelation promoting effect. The high molecular weight hydroxyalkyl cellulose precipitated therein decomposes and burns during the subsequent firing process, resulting in large voids in the gel, which tend to remain as defects in the glass.
ヒドロキシアルキルセルロースとしては。As hydroxyalkyl cellulose.
ヒドロキシメチルセルロース、ヒドロキエチルセルロー
ス、ヒドロキシプロピルセルロース、ヒドロキシブチル
セルロース等が使用しうる。Hydroxymethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, hydroxybutylcellulose, etc. can be used.
添加するヒドロ・キシアルキルセルロースの量はヒドロ
キシアルキルセルロースの分子量によって１選択される
べきである。比較的低分子量のヒドロキシアルキルセル
ロースの場合、シリコンアルコキシド１００重量部に対
して、０．１重量部未満の添加では、はとんど効果はな
い、一方、比較的高分子量のヒドロキシアルキルセルロ
ースの場合、シリコンアルコキシド１００重量部に対し
て５．０重里部を越える添加では、著しいゲル化促進効
果のため、均一なゲルを得ることは非常に困難となる。The amount of hydroxyalkylcellulose added should be selected depending on the molecular weight of the hydroxyalkylcellulose. In the case of relatively low molecular weight hydroxyalkylcellulose, adding less than 0.1 part by weight to 100 parts by weight of silicon alkoxide will have little effect; on the other hand, in the case of relatively high molecular weight hydroxyalkylcellulose If the amount exceeds 5.0 parts by weight per 100 parts by weight of silicon alkoxide, it becomes extremely difficult to obtain a uniform gel due to the significant effect of promoting gelation.
水と共に加える触媒は、塩基、酸等特に制限しないが、
ゲル化時間、また得られる乾燥ゲルの焼結のし易すさの
点から塩基の方が好ましい結果が得られる。水と共に加
えるアルコールについては特に制限しないが、水、アル
コキシドの両者に対する溶解性の点より。The catalyst added with water is not particularly limited, such as bases and acids, but
From the viewpoint of gelation time and ease of sintering of the resulting dry gel, a base gives more preferable results. There are no particular restrictions on the alcohol added together with water, but from the viewpoint of solubility in both water and alkoxide.
メチルアルコール、エチルアルコール、１−プロピルア
ルコール、２−プロピルアルコール等を使用するのが好
ましい。Preferably, methyl alcohol, ethyl alcohol, 1-propyl alcohol, 2-propyl alcohol, etc. are used.
シリカガラスは、上記のようにして調整したシリカゾル
をシャーレ等の容器に移し、室温〜７０℃に保って、ゲ
ル化し２次いで室温以上の温度で数週間乾燥して、乾燥
ゲルとし。Silica glass is obtained by transferring the silica sol prepared as described above to a container such as a petri dish, keeping it at room temperature to 70°C to gel it, and then drying it at a temperature above room temperature for several weeks to form a dry gel.
更に公知の方法１例えば、空気中で１０００〜１４００
℃に昇温しで焼結することにより得られる。Further known method 1, for example, 1000 to 1400 in air
It is obtained by sintering at elevated temperature to ℃.
（作用）
ヒドロキシアルキルセルロースの添加効果の原因につい
ては、詳細は不明であるが、ゾル中でのシリカ微粒子の
生成の制御、ゲル中でのこれらのシリカ微粒子間の結合
、乾燥過程でゲル中に発生する応力の緩和等に寄与し。(Effect) The details of the effects of adding hydroxyalkylcellulose are unknown, but they include control of the formation of silica particles in the sol, bonding between these silica particles in the gel, and formation of silica particles in the gel during the drying process. Contributes to alleviating the stress that occurs.
ゲルの大形化が可能となったものと考えられる。It is thought that this made it possible to increase the size of the gel.
実施例 １
３モルのメチルアルコールと３モルの水と０、０００５
モルのコリンを混合し、これに７．６ｇのヒドロキシプ
ロピルセルロース（２％水溶液の２０’Ｃ−での粘度で
４００センチポイズ）を添加し溶解させた。得られた溶
液を１モルのシリコメトキシド（Ｓｉ （ＯＣＨ３）
ａ）にゆっくりと加え、さらに充分混合しシリカゾルを
得た。これを直径１５０１１１Ｉ１１のテフロンでコー
ティングしたガラス製シャーレに入れ、アルミ箔で密封
し、室温でゲル化した。その後。Example 1 3 moles of methyl alcohol and 3 moles of water and 0,0005
7.6 g of hydroxypropylcellulose (2% aqueous solution with a viscosity of 400 centipoise at 20'C) was added and dissolved. The resulting solution was diluted with 1 mol of silicomethoxide (Si (OCH3)
It was slowly added to a) and mixed thoroughly to obtain a silica sol. This was placed in a Teflon-coated glass Petri dish with a diameter of 150111111, sealed with aluminum foil, and gelled at room temperature. after that.
蓋に孔を開け、５０℃の恒温槽中で２週間乾燥し、その
後１２０℃の恒温槽に移して１日乾燥して、直径約１２
０１１＋１の乾燥ゲルを得た。A hole was made in the lid and dried in a constant temperature bath at 50℃ for two weeks, then transferred to a constant temperature bath at 120℃ and dried for one day.
A dry gel of 011+1 was obtained.
こうして得られた乾燥ゲルのかさ密度は約０゜６ｇ／ａ
ａであり、クラックや割れは全くなかった。The bulk density of the dry gel thus obtained was approximately 0°6 g/a.
a, and there were no cracks or breaks at all.
得られたゲルを空気中１３００℃まで加熱焼結したとこ
ろ直径約８０ａ＋ｍ、厚さ５ｇ蒙のクランクや割れのな
い透明なシリカガラスが得られた。このシリカガラスは
分析の結果、そのシリカガラスと一致した。When the obtained gel was heated and sintered in air to 1300°C, a transparent silica glass with a diameter of about 80 m and a thickness of 5 g and no cracks or cracks was obtained. As a result of analysis, this silica glass matched that of the silica glass.
実施例 ２
２％水溶液の２０℃での粘度が４０００センチボイズの
ヒドロキシプロピルセルロース２．３ｇｔ−３モルのメ
チルアルコール、３モルの水、ｏ、ｏｏｏｓモルのコリ
ンとを混合した。Example 2 2.3 gt of hydroxypropyl cellulose having a viscosity of 4000 centivoids at 20° C. in a 2% aqueous solution was mixed with 3 moles of methyl alcohol, 3 moles of water, and o,oos moles of choline.
以下実施例１と同様の操作を行って乾燥ゲルを得た。得
られた乾燥ゲルにはクランクや割れは全くなかった。Thereafter, the same operation as in Example 1 was performed to obtain a dry gel. The dried gel obtained had no cracks or cracks.
実施例 ３
２％水溶液の２０℃での粘度が１４０００センチボイズ
のヒドロキシブチルセルロース１．２ｇを３モルのメチ
ルアルコール、３モル？−Ｊ
の水、０．０００５モルのコリン゛ざを混合した。Example 3 1.2 g of hydroxybutylcellulose, a 2% aqueous solution with a viscosity of 14,000 centivoids at 20°C, was mixed with 3 moles of methyl alcohol and 3 moles of methyl alcohol. -J of water and 0.0005 mol of choline were mixed.
以下実施例１と同様の操作を行って乾燥ゲルを得た。得
られた乾燥ゲルにはクラックや割れは全くなかった。Thereafter, the same operation as in Example 1 was performed to obtain a dry gel. The dried gel obtained had no cracks or breaks.
（発明の効果）
本発明によれば、クランクや割れのない大形のシリカガ
ラスをゾルケール法により容易に製造可能となる。その
大きさは基本的には制約がな（、形状も板状、棒状、管
状等のいずれでも製造できる。(Effects of the Invention) According to the present invention, large-sized silica glass without cranks or cracks can be easily produced by the Solcale method. There are basically no restrictions on its size (and it can be manufactured in any shape, such as a plate, rod, or tube).
また１本発明に・よればシリカガラスは従来より安価に
製造できるため、従来から使用されてきたＩＣ製造用フ
ォトマスク基材等の分野はもちろん、液晶表示用基材等
にも応用が拡大できる。In addition, according to the present invention, silica glass can be manufactured at a lower cost than before, so its application can be expanded not only to fields such as photomask substrates for IC manufacturing, which have been conventionally used, but also to substrates for liquid crystal displays, etc. .
代理人 弁理士 廣 瀬 章Agent Patent Attorney Akira Hirose
Claims (1)
し、次いで焼結するシリカガラスの製造法に於て、シリ
コンアルキシドを加水分解してシリカゾルとする段階で
、２％水溶液の２０℃での粘度が１００〜１００００セ
ンチポイズであるヒドロキシアルキルセルロースをシリ
コンアルコキシド１００重量部に対し０．１〜５．０重
量添加することを特徴とするシリカガラスの製造法。[Scope of Claims] 1. In a method for producing silica glass in which silicon alkoxide is hydrolyzed to form silica sol, this is gelled, dried to form a dry gel, and then sintered, silicon alkoxide is hydrolyzed. In the step of preparing a silica sol, 0.1 to 5.0 weight of hydroxyalkylcellulose having a 2% aqueous solution having a viscosity of 100 to 10,000 centipoise at 20°C is added to 100 parts by weight of silicon alkoxide. Glass manufacturing method.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27645987A JPH0717388B2 (en) | 1987-10-31 | 1987-10-31 | Silica glass manufacturing method |
| US07/262,803 US4943542A (en) | 1987-10-31 | 1988-10-26 | Process for producing silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27645987A JPH0717388B2 (en) | 1987-10-31 | 1987-10-31 | Silica glass manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01119527A true JPH01119527A (en) | 1989-05-11 |
| JPH0717388B2 JPH0717388B2 (en) | 1995-03-01 |
Family
ID=17569735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27645987A Expired - Lifetime JPH0717388B2 (en) | 1987-10-31 | 1987-10-31 | Silica glass manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0717388B2 (en) |
-
1987
- 1987-10-31 JP JP27645987A patent/JPH0717388B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0717388B2 (en) | 1995-03-01 |
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