JPS63195134A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPS63195134A JPS63195134A JP2780387A JP2780387A JPS63195134A JP S63195134 A JPS63195134 A JP S63195134A JP 2780387 A JP2780387 A JP 2780387A JP 2780387 A JP2780387 A JP 2780387A JP S63195134 A JPS63195134 A JP S63195134A
- Authority
- JP
- Japan
- Prior art keywords
- wet gel
- glass
- gel
- drying
- aging
- 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
- 239000011521 glass Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000011240 wet gel Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 9
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 8
- 239000000499 gel Substances 0.000 claims abstract description 8
- 239000002184 metal Substances 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 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 claims description 8
- 238000003980 solgel method Methods 0.000 claims description 5
- 239000000758 substrate Substances 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract 1
- 230000003247 decreasing effect Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011882 ultra-fine particle Substances 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)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
CIll m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 FIELD OF APPLICATION ON CIll m 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i!Iinにおいて
は、金属アルフキシトあるいは゛、金属アルコキシドお
よび金l14111!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
fil形吠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、該つ、ブトゲルを、」;紀容器中あるいは
、底面の平滑な容器にて乾燥し、乾燥ゲルを作製する方
法であった。i! of glass by conventional sol-gel method! In Iin, metal alkoxides or metal alkoxides and gold l14111! A liquid sol with the desired glass component composition is prepared using fine particles of the compound as the main raw material, and the liquid sol is gelled in a sealed container with a filtration shape to produce a wet gel. ; The method was to prepare a dry gel by drying in a container or a container with a smooth bottom.
しかし、前述・の従来技術では、ウェットゲルが大型に
なった場合、特にFJさが大きくなった場合には、つ、
ブトゲルの熟成中ウェットゲルのmmとウェットゲルの
構造的な強度とのバランスが崩れ容器との接触面からク
ラックが生じたり、乾燥においては、乾燥の進行に伴な
いウェットゲルが収縮するため、この収縮力が容器の接
触面との摩擦力よりも、小さくなり、クラックが化しる
などのため、大型化(特に厚さの大きなもの)は、困難
であるという問題点をイ丁する。However, in the conventional technology mentioned above, when the wet gel becomes large, especially when the FJ becomes large,
During maturation of butogel, the balance between the wet gel mm and the structural strength of the wet gel is lost, and cracks occur from the contact surface with the container, and during drying, the wet gel shrinks as the drying process progresses. The problem is that it is difficult to increase the size (particularly thick ones) because the shrinkage force is smaller than the frictional force with the contact surface of the container, which can lead to cracks.
そこで、本発明の目的は、ウェットゲルの熟成、乾燥方
法を改良することにより、熟成、乾燥の際のクラックを
防ぎ、大型ガラスの作製を容易にするゾル−ゲル法によ
るガラスの製造方法を提供するところにある。Therefore, an object of the present invention is to provide a method for manufacturing glass using the sol-gel method, which prevents cracks during aging and drying and facilitates the production of large glasses by improving the aging and drying method of wet gel. It's there to do.
本発明のゾル−ゲル法によるガラスのa!!遣方法は、
金属アルコキシドあるいは、金属アルコキシドおよび金
J1酸化物の微粒子を主原料として、旧的ガラス成分組
成の液状ゾルを調製し、該液状ゾルを所f71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ガラスの製造において、該
ウェットゲルを海綿状の下1k l−にて、熟成、乾燥
することを特徴とする。a! of glass produced by the sol-gel method of the present invention! ! The method of sending is
A liquid sol with a conventional glass component composition is prepared using metal alkoxide or fine particles of metal alkoxide and gold J1 oxide as main raw materials, and the liquid sol is gelled in an F71-shaped sealed container to produce a wet gel. After that, in the production of glass by drying and sintering the wet gel, the wet gel is aged and dried in a cavernous atmosphere of 1kl.
本発明によれば、熟成および乾燥の際、つ、ットゲルを
1f4綿伏の下敷」;に置くため、ウェットゲルの自i
n IIkが、熟成の際のつ、フトゲル強度および!π
燥の際の収縮力に及ぼず負荷が軽減される。According to the present invention, during ripening and drying, the wet gel is placed under a 1F4 cotton cloth.
n IIk during aging, soft gel strength and! π
The shrinkage force during drying is not as strong and the load is reduced.
したがって、ウェットゲルには、クラックが生じ難くな
り、大型ガラスの作製が容易となるものである。Therefore, cracks are less likely to occur in the wet gel, making it easier to manufacture large glasses.
l)市販のエチルミリケート(S i (OEi )、
)132ρ、0.0IN−IICβ108β、および超
微粒子シリカ(商品名:アエロジル0X50(デグサ社
) 45 k gを混合し、M1拌分散装置にて811
↑を3時間行ない、エチルシリケートの加水分解反応を
行なうと共に超微粒子シリカのある程1α分散したゾル
を調製した。この後、さらに分散性を向、l二させるた
め、1に分散液に対し、超音波を11り(射(撹拌併用
)を5時par行なった。なお、この際、超音波II(
(射による該ゾル温度の」−昇を防ぐため、冷却装置に
より該ゾル温度を一定に保tηした。l) Commercially available ethyl millicate (S i (OEi),
) 132ρ, 0.0IN-IICβ108β, and 45 kg of ultrafine particle silica (trade name: Aerosil 0X50 (Degussa)) were mixed and 811
The above procedure was carried out for 3 hours to carry out the hydrolysis reaction of ethyl silicate and to prepare a sol in which ultrafine silica particles were dispersed to a certain degree. After this, in order to further improve the dispersibility, the dispersion liquid was irradiated with ultrasonic waves (combined with stirring) for 5 o'clock at 5 o'clock.
(In order to prevent the sol temperature from increasing due to radiation, the sol temperature was kept constant by a cooling device.
次工程として、該ゾル中の半ゲル化ゼリー状物不純物含
イr fil大粒子およびゴミなどを除去するため該ゾ
ルに対し遠心分離処理(3,00Orpm1C)OmI
n)を加えた、さらに濾過し、ゾルの精製を行なった。As a next step, the sol was subjected to centrifugation treatment (3,00 Orpm 1C) to remove semi-gelled jelly-like impurity-containing large particles and dust.
n) was added, and the sol was further purified by filtration.
次に該ゾルを撹拌しながら0.IN−アンモニア水を滴
下し、pTI値を3〜0に調製した。この後、再遠心分
離、濾過などの処理を施し大きさ30X30X20 (
cm)のポリプロピレン製の容器に10ρ、7.5J2
.5β、2.5βの6量をそれぞれ6個、注入しフタを
して書閉吠態でゲル化させウェットゲルを作製した。こ
こで作製したウェットゲルを各注入fL1に対して次の
ような、3種類の方法で乾燥した。(1) 容器はその
ままでフタを5%の開孔率のものにした。Next, while stirring the sol, IN-ammonia water was added dropwise to adjust the pTI value to 3-0. After this, it is subjected to treatments such as recentrifugation and filtration, and the size is 30X30X20 (
cm) in a polypropylene container with 10ρ, 7.5J2
.. Six doses each of 5β and 2.5β were injected, the lids were closed, and the gels were formed in a closed state to prepare wet gels. The wet gel prepared here was dried for each injection fL1 using the following three methods. (1) The container was kept as it was, but the lid had a 5% porosity.
(2) ウェットゲルの下に厚さIcmのスポンジを入
れ、フタを5%の開孔率のものにした。(2) A sponge with a thickness of I cm was placed under the wet gel, and the lid had a porosity of 5%.
(3) ウェットゲルの下に厚さ4cmのスポンジを
入れ、フタを5%の開孔率のものにした。(3) A 4 cm thick sponge was placed under the wet gel, and the lid had a 5% porosity.
これらを乾燥機に投入し、70@Cにて乾燥した。乾燥
ゲルの作製状況を表1に示す。These were put into a dryer and dried at 70@C. Table 1 shows the preparation status of the dried gel.
表1 乾燥吠況
表1に示したように、本発明の方法でなければ厚い乾燥
ゲルの作製は困難であった。Table 1 Drying condition As shown in Table 1, it was difficult to produce a thick dry gel without the method of the present invention.
このようにして得られた乾燥ゲルを焼結炉に投入し、加
熱焼結し、1350@Cにて透明なガラス体を得た。こ
れらガラスの大きさは、ゾル注入1it2.5ρで15
X15X1.3 (am)、同5βで15X15X2.
8 (cm)、同?、5j2で15X 15X3.0
(cm)、同10.12で15X15X5.’3 (a
m)であった、また、ことで得られたガラスの諸物性は
、ビッカース[Il’、比重;熱膨張係数、赤外吸収ス
ペクトル、近赤外吸収スペクトル、屈折率など、石英ガ
ラスと一致した。The dry gel thus obtained was placed in a sintering furnace and sintered by heating to obtain a transparent glass body at 1350@C. The size of these glasses is 15
X15X1.3 (am), 15X15X2.
8 (cm), same? , 15X 15X3.0 in 5j2
(cm), same 10.12 and 15X15X5. '3 (a
m), and the physical properties of the glass thus obtained were consistent with those of silica glass, including Vickers [Il', specific gravity, coefficient of thermal expansion, infrared absorption spectrum, near-infrared absorption spectrum, and refractive index. .
以」−のように、本発明の方法によれば、熟成、乾燥の
際のクラックの発生を抑制でき、大型ガラスの作製が容
易となる。As described below, according to the method of the present invention, the generation of cracks during aging and drying can be suppressed, and large-sized glass can be easily produced.
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、IC用フォトマスク基板、光フアイ
バー9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, it is thought that the application will expand to various fields such as photomask substrates for IC, optical fiber 9 materials, and optics, as well as fields where quartz glass has been used up until now.
また、ゾル調製1稈において、Tis Ges Na、
Cas f、is Aρ% Tas Z rs Crs
など種々の元素と添加することにより、種々の多成分系
のガラスおよび填存ルn成以外のガラスの製造も容易で
ある。In addition, in one culm of sol preparation, Tis Ges Na,
Cas f, is Aρ% Tas Z rs Crs
By adding various elements such as, it is easy to manufacture various multi-component glasses and glasses other than filled glass.
以 上that's all
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、焼結するゾルーゲル法によるガラ
スの製造方法において、該ウェットゲルを海綿状の下敷
上にて、熟成、乾燥することを特徴とするガラスの製造
方法。(1) Using metal alkoxide or fine particles of metal alkoxide and metal oxide as main raw materials, prepare a liquid sol with the desired glass component composition, and gel the liquid sol in a sealed container of 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, the method comprising aging and drying the wet gel on a spongy underlayment.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2780387A JPH0751445B2 (en) | 1987-02-09 | 1987-02-09 | Glass manufacturing method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2780387A JPH0751445B2 (en) | 1987-02-09 | 1987-02-09 | Glass manufacturing method |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63195134A true JPS63195134A (en) | 1988-08-12 |
JPH0751445B2 JPH0751445B2 (en) | 1995-06-05 |
Family
ID=12231134
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2780387A Expired - Fee Related JPH0751445B2 (en) | 1987-02-09 | 1987-02-09 | Glass manufacturing method |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0751445B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0719735A1 (en) * | 1994-12-29 | 1996-07-03 | AT&T Corp. | Fabrication of a thin sheet by a sol-gel process |
-
1987
- 1987-02-09 JP JP2780387A patent/JPH0751445B2/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0719735A1 (en) * | 1994-12-29 | 1996-07-03 | AT&T Corp. | Fabrication of a thin sheet by a sol-gel process |
Also Published As
Publication number | Publication date |
---|---|
JPH0751445B2 (en) | 1995-06-05 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
LAPS | Cancellation because of no payment of annual fees |