JPS632820A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPS632820A JPS632820A JP14737386A JP14737386A JPS632820A JP S632820 A JPS632820 A JP S632820A JP 14737386 A JP14737386 A JP 14737386A JP 14737386 A JP14737386 A JP 14737386A JP S632820 A JPS632820 A JP S632820A
- Authority
- JP
- Japan
- Prior art keywords
- liquid
- gel
- sol
- glass
- prepared
- 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
- 239000011521 glass Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000000499 gel Substances 0.000 claims abstract description 17
- 239000011240 wet gel Substances 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- -1 alkyl silicate Chemical compound 0.000 claims description 5
- 238000003980 solgel method Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000428 dust Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OWNRRUFOJXFKCU-UHFFFAOYSA-N Bromadiolone Chemical compound C=1C=C(C=2C=CC(Br)=CC=2)C=CC=1C(O)CC(C=1C(OC2=CC=CC=C2C=1O)=O)C1=CC=CC=C1 OWNRRUFOJXFKCU-UHFFFAOYSA-N 0.000 description 1
- 208000005156 Dehydration Diseases 0.000 description 1
- 101100528697 Helicobacter pylori (strain B128) rnaJ gene Proteins 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241001122767 Theaceae Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 238000006298 dechlorination reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
-
- 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)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はゾル−グル法によるガラスの製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing glass by the sol-glu method.
従来からゾル−ゲル法による石英ガラスの!!!造方法
は何列か報告されている。((1)計上、中容ら1oS
rnaJ of ’l1on−Crystalline
Bolids、 37 、191(1980)、(2
)ラビー1ビツヒら、 JolLrnaJ of Mo
n−Crystallixg 5olids、 47.
435(1982) + (3)土岐ら特願昭58−2
37577)
なかでも土岐らの方法は、金属アルコキシドの加水分解
溶液中に、超微粉末シリカを均一に分散させ、該分#!
i液のPH直を3〜6!F−調整したゾルを用いて作製
した多孔性のドライゲルを焼結するという工程を有して
おシ、池の2 gAJではP):!!困難な大型の石英
ガラス(EAUえば150×15(7)X O,5cm
)を歩留シよく作製でき、ゾル−ゲル法による石英ガ
ラスのIR造方法としては最もTぐれていると討える。Silica glass has been manufactured using the sol-gel method! ! ! Several construction methods have been reported. ((1) Recorded, Nakayo et al. 1oS
rnaJ of 'l1on-Crystalline
Bolids, 37, 191 (1980), (2
) Raby 1 Bituhi et al., JolLrnaJ of Mo
n-Crystallixg 5olids, 47.
435 (1982) + (3) Toki et al. patent application 1982-2
37577) Among them, the method of Toki et al. uniformly disperses ultrafine powdered silica in a hydrolyzed solution of metal alkoxide, and the corresponding #!
The pH of the i-liquid is 3-6! F-It has a step of sintering a porous dry gel prepared using the adjusted sol. ! Difficult to use large quartz glass (EAU: 150 x 15 (7) x O, 5 cm)
) can be produced with a high yield, and it can be said that this method is the best in terms of T as an IR manufacturing method of quartz glass using the sol-gel method.
さらKTf願昭60−237927にも記載されている
ように土岐らの方法から進めて肉厚ガラスの作製も可能
であシ、匝めで応用範囲の広ハ石英ガラスの製造方法で
ある。Further, as described in KTf Application No. 60-237927, it is possible to produce thick glass by proceeding from the method of Toki et al., and this is a method for producing silica glass that has a wide range of applications.
しかし、従来の土岐らの製造方法では、焼結後得られた
石英ガラス中に、分散させた超微粉末シリカの純度に起
因する金属イオン等の不純物、結晶、不定形状の異物が
含まれやすく1列えば光フアイバー用母材や工C用フォ
トマスク基板等の特に高品質を要求される用途に使用す
る場合は1品質的に問題があった。However, in the conventional manufacturing method of Toki et al., the silica glass obtained after sintering tends to contain impurities such as metal ions, crystals, and irregularly shaped foreign substances due to the purity of the dispersed ultrafine powder silica. In one line, when used in applications that require particularly high quality, such as base materials for optical fibers and photomask substrates for engineering C, there is a quality problem.
そこで、木兄8Aは従来のこのような品質上の問題点を
解決するもので、その目的とするところは。Therefore, Ki-en 8A is designed to solve these conventional quality problems, and what is its purpose?
金属イオン等の不純物、結晶、不定形状の異物の無い均
質で高品質な肉厚ガラスを製造する方法を提供するとこ
ろにある。The purpose of the present invention is to provide a method for producing homogeneous, high-quality, thick-walled glass that is free of impurities such as metal ions, crystals, and irregularly shaped foreign substances.
本発明のガラスの製造方法は、アルキルシリケートの塩
基性触媒下での加水分解反応生成物であるシリカ微粒子
が分散した窮l液と、アルキルシ、リケードの酸性触媒
による加水分解反応厄2液とを所定割合にて混合し調製
したゾルをゲル比させてウェットゲルを作製する工程、
前記ウェットゲルを乾燥してドライゲルを作製する工程
、および。The method for producing glass of the present invention uses a liquid containing fine silica particles dispersed therein, which is a product of the hydrolysis reaction of an alkyl silicate under a basic catalyst, and two liquids that undergo a hydrolysis reaction of an alkyl silicate under an acidic catalyst. A step of preparing a wet gel by comparing the sol prepared by mixing at a predetermined ratio to a gel;
a step of drying the wet gel to produce a dry gel;
前記ドライゲルを焼結し透明ガラス体を作製する工程か
らなるゾル−ゲル法によるガラスの製造方法の眞1液と
萬2液とを所定割合にて混合し調製したゾルをゲル化さ
せてウェットゲルを作製する工程において、調製したゾ
ルを2cm以上の厚さく仕込みゲル化させることtea
とする。A wet gel is produced by gelling a sol prepared by mixing the 1st liquid and the 2nd liquid in a predetermined ratio in the sol-gel glass manufacturing method, which comprises the step of sintering the dry gel to produce a transparent glass body. In the process of producing tea, prepare the prepared sol to a thickness of 2 cm or more and gel it.
shall be.
製造にあたりては以下の条件を有することが望ましい。It is desirable to have the following conditions during manufacturing.
α、窮工液および厄2液の原料は、蒸留、濾過等により
精製した高純度で微小なゴミ、異物のな^ものを使用す
る。The raw materials for α, Kukou liquid, and Yaku 2 liquid are highly pure, purified by distillation, filtration, etc., and are free of minute dust and foreign substances.
b、槙1液中のシリカ微粒子のモ均粒子径が、o、oo
s〜1.O#Lの範囲にあること。b. The average particle diameter of silica fine particles in Maki 1 liquid is o, oo
s~1. Must be within the O#L range.
6、IEl液と第2gを各液中のシリコン比で、o:i
oo〜100:Oの範囲、さらに好ましくは、20 :
80〜95:5 の範囲の所定割合にて混合すること
。6. IEl liquid and 2nd g with silicon ratio in each liquid, o:i
In the range of oo to 100:O, more preferably 20:
Mix at a predetermined ratio in the range of 80 to 95:5.
d、酵l液中のシリカ微粒子の@庇が0.051/rn
J以とであること。d, silica fine particles in the fermentation solution @ eave is 0.051/rn
Must be J or higher.
6、ゾル中の有効シリカ分が0 、10 f/mA以上
であること。6. The effective silica content in the sol is 0.10 f/mA or more.
f、ゾルのPEt値を3以上の直に14整した後ゲル化
させること。f. After adjusting the PEt value of the sol to 3 or more, gelation is performed.
またウェットゲルの乾燥にお^では、乾燥容器内でのゲ
ルを水子面から傾けて、ゲルの収量Kよる移動方向とゲ
ルの自重の収縮移動面方向への分力を同じ向きになるよ
り配置して行うことによフ乾燥時の割れが防止でき、歩
留シよくドライゲルを得ることができる。In addition, when drying a wet gel, the gel in the drying container is tilted from the water surface so that the moving direction due to the gel yield K and the component force of the gel's own weight toward the contraction moving surface are in the same direction. By arranging them, cracking during drying can be prevented, and a dry gel can be obtained with a high yield.
本発明によれば、原料として高純度な液体原料を選べる
ので金属イオン等の不純物や、ゴミ、チリ等の異物がな
く、本質的に高品質なガラスを作製することができる。According to the present invention, since a highly pure liquid raw material can be selected as a raw material, it is possible to produce essentially high-quality glass without impurities such as metal ions and foreign substances such as dust and dust.
〔実tN列1〕
■第1液の調製
蒸留精製したエチルシリケート、蒸留精製したエタノー
ル、蒸留精製した水、および孔径0.2μmのメンブラ
ンフィルタ−によシ濾過した市販電子工業用最高グレー
ドの29チアンモニア水、それぞれ%117 、16.
8J 、 3.8 J 、 0.457を温容し、4時
間激しく攪拌した後冷暗所にて一晩靜蟹しシリカ微粒子
を成長させた。とのシリカ微粒子分散液を濃縮し九後、
安定化のため、PH(直を4に調整し、孔径10#ys
のメングランフィルターによl’過し窮1液をlII
製した。光透過式の遠心沈降粒度分布″測定装置でシリ
カ微粒子のモ均粒径を測定したところ、 0.40尾で
あった。[Actual tN column 1] ■ Preparation of the first liquid Distilled purified ethyl silicate, distilled purified ethanol, distilled purified water, and commercially available highest grade 29 for the electronic industry, filtered through a membrane filter with a pore size of 0.2 μm. Thiammonia water, 117% and 16% respectively.
8 J, 3.8 J, and 0.457 were heated, stirred vigorously for 4 hours, and then incubated overnight in a cool, dark place to grow silica fine particles. After concentrating the silica fine particle dispersion with
For stabilization, adjust the pH to 4 and pore size to 10 #ys.
Pass the remaining liquid through the menglan filter.
Manufactured. When the average particle size of the silica fine particles was measured using a light transmission type centrifugal sedimentation particle size distribution measurement device, it was 0.40 particles.
■第2液のv4g
蒸留精製したエチルシリケート4.8!と孔径0.2μ
倶のメンブランフィルタ−によシ炉遇した0、02 規
定の塩酸6.157とを混合し、激しく攪拌し、加水分
解反応を行ない、第2液とした。■Second liquid v4g distilled purified ethyl silicate 4.8! and pore diameter 0.2μ
The mixture was mixed with 6.157% of 0.02N hydrochloric acid which had been filtered through the membrane filter, stirred vigorously, and subjected to a hydrolysis reaction to obtain a second liquid.
■ゾル調製
wcl液と窮2液を混合し、0.2μmのメンブランフ
ィルタ−によ)濾過した0、1規定のアンモニア水でP
H4,3に調整した。■Sol Preparation Mix the WCl solution and the 2nd solution, and use 0.1 N ammonia water filtered through a 0.2 μm membrane filter to prepare the solution.
Adjusted to H4.3.
■ゲル化〜乾燥
前記ゾル溶液をポリプロピレン製の容器(幅I備X 3
0 an X高さto cm ) K深さが9αになる
量を仕込み、密閉状態でゲル化させた。■Gelification ~ Drying The sol solution is placed in a polypropylene container (width I x 3).
0 an
得られたウェットゲルt−30’Cの恒温室内で5日間
熟成し、乾燥容器内でのゲルを水子面から傾けて設置し
て、乾燥容器K O,25チの開孔率を持った7タをし
て、55℃の乾燥室内で乾燥させた。乾燥終了までに約
2ケ月を要した。The obtained wet gel was aged for 5 days in a thermostatic chamber at t-30'C, and the gel was placed in a drying container so as to be tilted from the water surface, so that the drying container had a porosity of KO, 25 cm. It was dried in a drying room at 55°C. It took about two months to complete the drying process.
■焼結
該ドライゲルを焼結炉に投入し、昇温速度I℃/hrで
加℃から200℃まで加熱し、この温度にて5時間保持
した1、300℃まで加熱し5時間保持し脱吸着水処理
を行った。■Sintering The dry gel was placed in a sintering furnace, heated from ℃ to 200℃ at a temperature increase rate of 1℃/hr, held at this temperature for 5 hours, heated to 1,300℃, held for 5 hours, and desorbed. Adsorption water treatment was performed.
続いて昇温速度30 ’C1hr で300℃から7
00℃まで加熱し、との温度にて加持間保持した後。Then, from 300℃ to 7℃ at a heating rate of 30'C1hr.
After heating to 00°C and holding at a temperature of .
昇温速度30 ’C/hr で700℃から900℃
まで加熱し、この温良にて10時間保持し、昇温速[3
0’C/hrで900℃から1000℃まで加熱し、こ
の温度で10時間保持して脱炭素、脱塩化アンモニウム
処理、脱水縮合反応の促進処理を行った。From 700℃ to 900℃ at a heating rate of 30'C/hr
The heating rate was increased to 3.
It was heated from 900°C to 1000°C at 0'C/hr and held at this temperature for 10 hours to perform decarbonization, dechlorination ammonium treatment, and acceleration treatment of dehydration condensation reaction.
この後、炉内にH,ガスを流しながら昇温速度刃℃/h
rで1300℃まで加熱し、この温度で3時間保持して
閉孔化処理す行りた。After this, while flowing H and gas into the furnace, the temperature increase rate is ℃/h.
The sample was heated to 1,300° C. at R and held at this temperature for 3 hours to perform a pore-closing treatment.
そして、昇温速度ω℃/んrで1780℃まで加熱し、
この温度で30分間保持して無孔化し、透明ガラス体を
得た。Then, it was heated to 1780°C at a temperature increase rate of ω°C/mmr,
It was maintained at this temperature for 30 minutes to make it non-porous, and a transparent glass body was obtained.
得られたガラス体は、幅16.5m X 16.5α×
厚す4.9備の大きさであった。The obtained glass body has a width of 16.5m x 16.5α x
It was 4.9 mm thick.
本実施列で得られたガラス塊をスライス加工、研磨し、
6インチ角X O,12インチ厚の基板tmた。該石英
ガラス基板中には気泡等の異物はなく匝めて高品質であ
った。また紫外頭載での分光特性もよく、工C用フォト
マスク基板として十分使用できるものであった。The glass lump obtained in this implementation process was sliced and polished,
The board was 6 inches square, 12 inches thick. There were no foreign substances such as air bubbles in the quartz glass substrate, and the quality was high when it was inserted. In addition, the spectral properties under ultraviolet mount were good, and it could be sufficiently used as a photomask substrate for industrial C.
以上述へたよ5に本発明によれば、アルキシシリケート
の塩基性触媒下での加水分解反応生成物であるシリカ微
粒子が分散した溶液と、アルキルシリケートの酸性触媒
による加水分解反応浴敵とを所定割合にて混合し調整し
たゾルを2cm以上の肉厚にゲル化させてウェットゲル
を作製し、乾燥、焼結して透明ガラス体としたことくよ
シ、金属イオン等の不純物、結晶、不定形状の異物の無
い均質で高品質な肉厚ガラスを容易に作れるという効果
を有する。As mentioned above, according to the present invention, a solution in which fine silica particles, which are a product of a hydrolysis reaction of an alkoxysilicate under a basic catalyst, are dispersed, and a hydrolysis reaction bath for an alkylsilicate under an acidic catalyst are combined. A wet gel is prepared by mixing and adjusting the sol in a predetermined ratio to a thickness of 2 cm or more, and then drying and sintering it to form a transparent glass body. It has the effect of easily producing homogeneous, high-quality, thick glass without irregularly shaped foreign matter.
従ってスライス加工、研磨することくよシ薄板ガラスは
勿論のこと、あらゆる厚さのガラス、各種形状ガラスへ
の適用が可能となシ、ゾル−ゲル法ではバルクガラスは
できな^という一般的欠点を克服することができた。Therefore, it can be applied not only to thin glass, which requires slicing and polishing, but also to glass of all thicknesses and various shapes.The general drawback is that the sol-gel method cannot produce bulk glass. was able to overcome.
以 とMore and more
Claims (1)
成物であるシリカ微粒子が分散した溶液(以後第1液と
記す)と、アルキルシリケートの酸性触媒による加水分
解反応溶液(以後第2液と記す)とを所定割合にて混合
し調製したゾルをゲル化させてウェットゲルを作製する
工程、前記ウェットゲルを乾燥してドライゲルを作製す
る工程、および、前記ドライゲルを焼結し透明ガラス体
を作製する工程からなるゾル−ゲル法によるガラスの製
造方法の第1液と第2液とを所定割合にて混合し調製し
たゾルをゲル化させてウェットゲルを作製する工程にお
いて、調製したゾルを2cm以上の厚さに仕込みゲル化
させることを特徴とするガラスの製造方法。A solution in which fine silica particles are dispersed, which is a product of the hydrolysis reaction of an alkyl silicate under a basic catalyst (hereinafter referred to as the first liquid), and a solution of the hydrolysis reaction of an alkyl silicate under an acidic catalyst (hereinafter referred to as the second liquid). A step of preparing a wet gel by gelling a sol prepared by mixing the sol in a predetermined ratio, a step of drying the wet gel to prepare a dry gel, and a step of sintering the dry gel to prepare a transparent glass body. In the step of producing a wet gel by gelling the sol prepared by mixing the first liquid and the second liquid at a predetermined ratio in the method for manufacturing glass by the sol-gel method, the prepared sol is heated to a thickness of 2 cm or more. 1. A method for producing glass, which is characterized by preparing glass to a thickness of .
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14737386A JPS632820A (en) | 1986-06-24 | 1986-06-24 | Production of glass |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP14737386A JPS632820A (en) | 1986-06-24 | 1986-06-24 | Production of glass |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS632820A true JPS632820A (en) | 1988-01-07 |
Family
ID=15428766
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP14737386A Pending JPS632820A (en) | 1986-06-24 | 1986-06-24 | Production of glass |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS632820A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02107535U (en) * | 1989-02-14 | 1990-08-27 |
-
1986
- 1986-06-24 JP JP14737386A patent/JPS632820A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH02107535U (en) * | 1989-02-14 | 1990-08-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JPS59116135A (en) | Manufacture of quartz glass | |
JPS632820A (en) | Production of glass | |
JPH0582331B2 (en) | ||
JPS63297226A (en) | Production of short-wavelength laser beam transmitting quartz glass | |
JPS62246827A (en) | Production of glass | |
JPH0258214B2 (en) | ||
JPS643812B2 (en) | ||
JPS6065735A (en) | Production of quartz glass | |
JPH0114177B2 (en) | ||
JPH02145442A (en) | Production of glass | |
JPH03285833A (en) | Manufacture of porous glass | |
JP3582093B2 (en) | Method for producing silica glass | |
JPS6054929A (en) | Production of quartz glass | |
JPS63291824A (en) | Production of quartz glass transmitting short wavelength laser light | |
JPS6126525A (en) | Production of quartz glass | |
JPS62123029A (en) | Production of glass | |
JPS62113737A (en) | Production of quartz glass | |
JPH0755836B2 (en) | Glass manufacturing method | |
JPH01119531A (en) | Production of glass | |
JPS6330330A (en) | Production of glass | |
JPS61186227A (en) | Production of quartz glass | |
JPS6158818A (en) | Manufacture of quartz glass | |
JPS6140825A (en) | Preparation of quartz glass | |
JPS62288122A (en) | Production of glass body by sol-gel method | |
JPS643814B2 (en) |