JPH01145331A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPH01145331A JPH01145331A JP30534687A JP30534687A JPH01145331A JP H01145331 A JPH01145331 A JP H01145331A JP 30534687 A JP30534687 A JP 30534687A JP 30534687 A JP30534687 A JP 30534687A JP H01145331 A JPH01145331 A JP H01145331A
- Authority
- JP
- Japan
- Prior art keywords
- sol
- glass
- gel
- sintering
- prescribed
- 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 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000011240 wet gel Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000003980 solgel method Methods 0.000 claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 150000004703 alkoxides Chemical class 0.000 claims abstract 4
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract 2
- 150000004706 metal oxides Chemical class 0.000 claims abstract 2
- 238000000034 method Methods 0.000 abstract description 11
- 239000000499 gel Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 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)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ゾル−ゲ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 a sol-gel method.
従来のゾル−ゲル法によるガラスの製造においては、目
的ガラス成分組成の液状ゾルをゲル化させウェットゲル
を作製した後の、乾燥と焼結とは別々の装置にて行なっ
ていた。すなわち乾燥機中で加熱乾燥し、−旦室温付近
まで降温し、乾燥ゲルを取シ出し、再び焼結炉に投入し
、加熱焼結する方法であった。 −
〔発明が解決しようとする問題点〕
しかし、前述の従来技術では、乾燥ゲルを作製した後、
降温し、乾燥機から取）出す際に、空気中の水分が該乾
燥ゲルに吸着する、この水分による応力腐食を受け、部
分的に８１−０結合が切断されてしまう、このため、加
熱焼結する際にクラックが生じ易く、大型ガラスの作製
が困難であるという問題点を有する。In the conventional production of glass by the sol-gel method, a wet gel is produced by gelling a liquid sol having a desired glass component composition, and then drying and sintering are performed in separate apparatuses. That is, the method was to dry the gel by heating in a dryer, then lower the temperature to around room temperature, take out the dried gel, put it into the sintering furnace again, and heat and sinter it. - [Problems to be solved by the invention] However, in the above-mentioned conventional technology, after producing a dry gel,
When the gel is cooled down and removed from the dryer, moisture in the air is adsorbed onto the dried gel.This moisture causes stress corrosion and partially breaks the 81-0 bond. The problem is that cracks are likely to occur when bonding, making it difficult to produce large-sized glass.
そこで、本発明の目的は、ウェットゲルを熱処理しガラ
ス化する工程を改善し、大型ガラスの作製を容易にする
方法を提供するところにある。SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a method that improves the process of vitrifying wet gel by heat treatment and facilitates the production of large-sized glass.
本発明のゾル−ゲル法によるガラスの製造方法は、金属
アルフキシトあるいは、金属アルフキシトおよび金Ｆ［
化物の微粒子を主原料として、目的ガラス成分組成の液
状ゾルを調製し、該液状ゾルを所望形状の密閉容器中に
てゲル化させウェットゲルを作製した後、該ウェットゲ
ルを、乾燥。The method for producing glass by the sol-gel method of the present invention is based on metal alphoxide or metal alphoxide and gold F[
A liquid sol having the desired glass component composition is prepared using fine particles of the compound as a main raw material, and the liquid sol is gelled in a sealed container of a desired shape to produce a wet gel.The wet gel is then dried.
焼結する製造方法において、乾燥から焼結までの熱処理
を同一装置内にて継続して行なうことを特徴とする。The manufacturing method for sintering is characterized in that the heat treatment from drying to sintering is performed continuously in the same apparatus.
本発明によれば、ウェットゲルの熱処理を同一装置内で
連続して行ないガラス化するために、工程途中での水の
再吸着が生じない。したがって、熱処理におけるクラッ
クの発生原因の一つである水による応力腐食の影響がな
くなり、大型ガラスの作製を容易にするものである。According to the present invention, since the wet gel is continuously heat-treated and vitrified in the same apparatus, re-adsorption of water during the process does not occur. Therefore, the influence of stress corrosion due to water, which is one of the causes of cracks during heat treatment, is eliminated, making it easier to manufacture large glasses.
１）エチルシリケート（５ｉ（ＯＥｔ）４）、１五２ｔ
、［ＬＯＩ Ｎ−ＨＣ／、Ｉ ＣＬ８ ｔｔおよび超微
粒子シリカ（商品名：アエロジル０ｘ５０（デグサ社）
）４．５ＫＰを混合、攪拌し、エチルシリケートの加水
分解反応を行ない、更に、充分に超微粒子シリカを分散
させ、＊ｇｉなゾルを調製した。1) Ethyl silicate (5i(OEt)4), 152t
, [LOI N-HC/, I CL8 tt and ultrafine silica (product name: Aerosil 0x50 (Degussa)
) 4.5KP were mixed and stirred to carry out a hydrolysis reaction of ethyl silicate, and further, ultrafine silica particles were sufficiently dispersed to prepare a *gi sol.
次に、該ゾルにアンモニア水を添加し、ＰＨ値を５〜６
に調整し、大きさ３０Ｘ３０Ｘ２０（副〕のポリプロピ
レン製の容器に各１″Ｌ５ｔ、Ｌ５ｔ、計２．７タをし
て密閉状態でゲル化させ、ウェットゲルを作製した。該
ウェットゲルを以下に示す２種類の方法でガラス化した
。Next, ammonia water is added to the sol to adjust the pH value to 5-6.
A wet gel was prepared by gelling in a polypropylene container with a size of 30 x 30 x 20 (secondary), 1 inch L5 t, L 5 t each, and a total of 2.7 tahts in a sealed state.The wet gel was prepared as follows. It was vitrified using the two methods shown below.
方法（１）
該ウェットゲルを乾燥機に入れ、８０℃にて乾燥し、大
きさ２１Ｘ２１Ｘ１（Ｌ５（譚〕の乾燥ゲルを得た。乾
燥機内の温度を室温付近（２５℃前後）に下げ、乾燥ゲ
ルを取シ出し、電気炉に投入し、加熱焼結し、１２９０
℃にて、透明なガラス体を得た。しかしこのガラスには
、多数のクラックが生じていた。Method (1) The wet gel was placed in a dryer and dried at 80°C to obtain a dry gel with a size of 21×21×1 (L5).The temperature inside the dryer was lowered to around room temperature (around 25°C), The dried gel was taken out, put into an electric furnace, heated and sintered, and heated to 1290
A transparent glass body was obtained at °C. However, this glass had many cracks.
方法（２）
該ウェットゲルを、加熱装置に入れ、５０℃／ｈｒにて
８０℃まで昇温した後、１０日間保持した。この後再昇
温し、１２９０℃にて、透明なガラス体を得た。このガ
ラスは、大きさ１５Ｘ１５Ｘ ７．５ （ｃｍ ）で、
外観上クラックなどの発生は見られなかった。Method (2) The wet gel was placed in a heating device, heated to 80° C. at 50° C./hr, and then held for 10 days. Thereafter, the temperature was raised again to 1290°C to obtain a transparent glass body. This glass has a size of 15X15X 7.5 (cm),
No cracks or the like were observed in appearance.
また、ここで得られたガラスの諸物性は、ビッカース硬
度、比重、熱膨張係数、赤外および近赤外吸収スペクト
ル、屈折率など石英ガラスと一致していた。In addition, the physical properties of the glass obtained here matched those of silica glass, including Vickers hardness, specific gravity, coefficient of thermal expansion, infrared and near-infrared absorption spectra, and refractive index.
以上のように、本発明の方法によれば、加熱処理の際、
クラックの発生を抑制することが可能となるため、大型
ガラスの作製が容易である。。As described above, according to the method of the present invention, during heat treatment,
Since it is possible to suppress the occurrence of cracks, it is easy to produce large glass. .
したがって、これまで石英ガラスを使用していた分野で
はもちろんのこと、工Ｏ用フォトマスク基板、光ファイ
バー母材、光学用など種々の分野に応用が広がるものと
考える。Therefore, we believe that the application will expand not only to fields where quartz glass has been used up until now, but also to various fields such as optical photomask substrates, optical fiber base materials, and optical applications.
また、ゾル調製工程において、Ｔｉ、Ｇｅ、Ｎａ、Ｏａ
、Ｌｉ、ＡＡ、Ｔｏ、Ｚｒ、Ｏｓ、Ｎｄ、。In addition, in the sol preparation process, Ti, Ge, Na, Oa
, Li, AA, To, Zr, Os, Nd,.
Ｏｒ、など、種々の元素を添加することＫより、種々の
多成分系ガラスおよび既存組成以外のガラスの製造も容
易である。By adding various elements such as Or, it is easy to manufacture various multi-component glasses and glasses with compositions other than existing ones.
以上 出願人 セイコーエプソン株式会社that's all Applicant: Seiko Epson Corporation
Claims (1)
よび金属酸化物の微粒子を主原料として目的ガラス成分
組成の液状ゾルを調製し、該液状ゾルを所望形状の密閉
容器中にてゲル化させウェットゲルを作製した後、該ウ
ェットゲルを乾燥、焼結するゾル−ゲル法によるガラス
の製造方法において、乾燥から焼結までの熱処理を同一
装置内にて継続して行なうことを特徴とするガラスの製
造方法。(1) A liquid sol having the desired glass component composition was prepared using metal alkoxide or fine particles of metal alkoxide and metal oxide as main raw materials, and the liquid sol was gelled in a sealed container of a desired shape to produce a wet gel. A method for producing glass by a sol-gel method in which the wet gel is then dried and sintered, characterized in that the heat treatment from drying to sintering is performed continuously in the same apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30534687A JPH01145331A (en) | 1987-12-02 | 1987-12-02 | Production of glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30534687A JPH01145331A (en) | 1987-12-02 | 1987-12-02 | Production of glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01145331A true JPH01145331A (en) | 1989-06-07 |
Family
ID=17944006
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30534687A Pending JPH01145331A (en) | 1987-12-02 | 1987-12-02 | Production of glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01145331A (en) |
-
1987
- 1987-12-02 JP JP30534687A patent/JPH01145331A/en active Pending
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