JPS63291822A - Production of large-sized glass block - Google Patents
Production of large-sized glass blockInfo
- Publication number
- JPS63291822A JPS63291822A JP12541287A JP12541287A JPS63291822A JP S63291822 A JPS63291822 A JP S63291822A JP 12541287 A JP12541287 A JP 12541287A JP 12541287 A JP12541287 A JP 12541287A JP S63291822 A JPS63291822 A JP S63291822A
- Authority
- JP
- Japan
- Prior art keywords
- gel
- sol
- wet gel
- glass
- solvent
- 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 15
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000011240 wet gel Substances 0.000 claims abstract description 19
- 239000000499 gel Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000011282 treatment Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 abstract description 11
- 238000005245 sintering Methods 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000003756 stirring Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005816 glass manufacturing process Methods 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
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000758 substrate 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】
〔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、ウ
ェットゲルに対しては、特に処理を施さずに、次工程の
乾燥を行なっていた。In the conventional glass manufacturing process using the sol-gel method, the wet gel is subjected to the next step of drying without being subjected to any particular treatment.
しかし、前述の従来技術では、大型塊状のガラスを作製
する場合、乾燥゛工程においで、ウェットゲル内部に存
在する水のゲル表面への拡散速度および蒸発速度が著し
く遅いため、乾燥終了までに非常に長時間を要するとい
う問題点を存する。However, with the above-mentioned conventional technology, when producing a large lump of glass, during the drying process, the diffusion rate and evaporation rate of water present inside the wet gel to the gel surface are extremely slow, so it takes a very long time to complete the drying process. The problem is that it takes a long time.
そこで、本発明は、前述の問題点を解決するもので、そ
の目的とするところは、ゾル−ゲル法により大型塊状ガ
ラスを容易に短時間で製造する方法を提供するととろに
ある。SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and its purpose is to provide a method for easily producing large lump glass in a short time using a sol-gel method.
（問題点を解決するための手段〕
本発明の大型塊状ガラスの製造方法は、金属アルコキシ
ドを主原料として、液状ゾルを調製し、これをゲル化さ
せてウェットゲルを作製した後、乾燥、焼結するゾル−
ゲル法によるガラスの製造においで、ウェットゲル作製
の際、該ウェットゲルを、アルコール等の揮発性の高い
溶剤中に少なくとも１日以上浸漬し取り出し、次に更に
水等の不揮発性の溶剤中に１時間から１０日間浸漬した
後、乾燥することを特徴とする。(Means for Solving the Problems) The method for producing large lump glass of the present invention involves preparing a liquid sol using metal alkoxide as the main raw material, gelling it to produce a wet gel, and then drying and baking it. The sol that binds
In the production of glass by the gel method, when producing a wet gel, the wet gel is immersed in a highly volatile solvent such as alcohol for at least one day, taken out, and then further immersed in a non-volatile solvent such as water. It is characterized by being soaked for 1 hour to 10 days and then dried.
本発明によれば、ウェットゲルの状態で、先ずウェット
ゲル中の水をアルコール等の揮発性の溶剤にて置換する
ため、乾燥時のゲル内部からの溶媒の拡散、蒸発速度が
早（なり、乾燥が短時間にて終了する。しかし、この処
理だけでは、乾燥初期におけるウェットゲル表面付近の
乾燥速度が著しく早いため割れ易い。そこで、更に水等
の不揮発性の溶剤にて、表面付近のみを置換することで
乾燥初期の割れを防止する。したがって、本発明の方法
によれば、大型塊状ガラスの前駆体である乾燥ゲルを、
短時間で容易に作製できることになる。According to the present invention, since the water in the wet gel is first replaced with a volatile solvent such as alcohol in the wet gel state, the diffusion and evaporation rate of the solvent from inside the gel during drying is fast. Drying is completed in a short time. However, if this treatment alone is used, the drying speed near the surface of the wet gel is extremely fast in the early stage of drying, making it prone to cracking. This replacement prevents cracking during the initial stage of drying.Therefore, according to the method of the present invention, the dried gel, which is a precursor of large lump glass, is
This means that it can be easily produced in a short time.
〔実施例〕
１） 市販ノエチルシリケー） （Ｓｉ （ＯＥｔ ）
、’）７．３１０．０ＩＮ−ＨＣｌ２．５１を混合撹拌
し、エチルシリケートの加水分解反応を行なった。該反
応液に撹拌しながら、超微粒子シリカ（商品名＝７エロ
ジルー０Ｘ５０ （デグサ社））２．７０ｋｇを混合し
た。この後、分散性を向上させるため、該分散液に対し
、超音波照射（撹拌併用）を３時間行なった。なお、こ
の際、超音波照射による該ゾル温度上昇を防ぎ、一定に
保持した。[Example] 1) Commercially available noethyl silica) (Si (OEt)
,')7.310.0 IN-HCl2.51 was mixed and stirred to perform a hydrolysis reaction of ethyl silicate. 2.70 kg of ultrafine particle silica (trade name: 7 Erogilu 0X50 (Degussa)) was mixed into the reaction solution while stirring. Thereafter, in order to improve dispersibility, the dispersion liquid was subjected to ultrasonic irradiation (combined with stirring) for 3 hours. At this time, the temperature of the sol was prevented from increasing due to ultrasonic irradiation and kept constant.
次工程として、該ゾル中の半ゲル化ゼリー状物や、不純
物含育粗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（３，０００ｒｐｍｓ ３０ｒｒ＋
ｉｎ）を加え、さらに濾過し、ゾルの精製を行なった。As the next step, the sol is subjected to centrifugation treatment (3,000 rpms 30rr +
in) was added and further filtered to purify the sol.
次に、該ゾルを撹拌しながら０．ＩＮ−アンモニア水を
滴下し、ｐＨ値を３〜６に調整した。この後、再遠心分
離、濾過などの処理を施し、内径２０Ｘ２０Ｘ、４０ｃ
ｍの容器に８１．同２０ｃｍφＸ４０ｃｍの容器に６．
５１それぞれ注入し、フタをして密閉状態にてゲル化さ
せた。 ゲル化後、ある程度まで収縮した時点で容器か
ら取り出し、エタノール中に浸漬し、１５日間静置した
・この後、さらに水中に１２時間浸漬させた後、乾燥機
に投入し、８０〜９０”Ｃにて乾燥し、７日間で、１４
．２Ｘ１４．２Ｘ１４．１ｃｍと、１４゜３ｃｍφＸ１
４．５ｃｍの乾燥ゲルを得た。Next, while stirring the sol, IN-aqueous ammonia was added dropwise to adjust the pH value to 3-6. After this, it is subjected to treatments such as recentrifugation and filtration, and the inner diameter is 20X20X, 40cm.
81.m in a container. 6. In the same 20cmφX40cm container.
No. 51 was injected into each well, the lid was closed, and gelation was allowed to occur. After gelation, when it had shrunk to a certain extent, it was taken out of the container, immersed in ethanol, and left to stand for 15 days.After this, it was further immersed in water for 12 hours, and then placed in a dryer at 80 to 90"C. Dry in 7 days, 14
．． 2X14.2X14.1cm and 14゜3cmφX1
4.5 cm of dry gel was obtained.
これらの乾燥ゲルを焼結炉に投入し、 加熱焼結し、そ
れぞれ１０．ｌＸｌ０．ｌＸｌ０．０ｃｍ５１０．２ｃ
ｍφＸ１０．３ｃｍの、塊状のガラスを得た。These dried gels were put into a sintering furnace, heated and sintered, and then heated and sintered for 10. lXl0. lXl0.0cm510.2c
A block of glass with mφ×10.3 cm was obtained.
以上のようにして得られたガラスに関する諸物性の分析
を行なったところ、ビッカース硬度、比重、赤外吸収ス
ベクシル、近−赤外吸収スペクトル屈折率など、はぼ市
販されている石英ガラスと一致した。When various physical properties of the glass obtained as described above were analyzed, it was found that the Vickers hardness, specific gravity, infrared absorption spectrum, refractive index of near-infrared absorption spectrum, etc. matched those of commercially available quartz glass. .
このように、本発明では、ウェットゲルに処理を施すこ
とで、乾燥ゲルの作製が非常に容易になる。したがって
これまでゾル−ゲル法による大型塊状ガラス作製の最大
の問題点であった乾燥ゲル作製方法は解決された。よっ
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、■Ｃ用フォトマスク基板、光フアイバー用母
材、レンズなど、種々の用途に応用されるものと考えら
れる。さらにゾル調整時に、Ａｌｓ Ｔｉｓ Ｇｅ。As described above, in the present invention, by processing a wet gel, it becomes very easy to produce a dry gel. Therefore, the method of producing dry gel, which has hitherto been the biggest problem in producing large lump glass by the sol-gel method, has been solved. Therefore, it is thought that it will be applied not only to fields where quartz glass has been used up until now, but also to various uses such as photomask substrates for C, optical fiber base materials, and lenses. Furthermore, when preparing the sol, Als Tis Ge.
Ｎａｓ Ｃａｓ Ｍｇｓ Ｌｉｓ Ｔｅｓなどの諸元素
を所定量添加することにより様々な特性をもつ多成分系
の高品質なガラスの作製も容易である。By adding predetermined amounts of various elements such as Nas Cas Mgs Lis Tes, it is easy to produce high quality multi-component glass having various properties.
また、石英ガラスに関しては、 他の製造方法（溶融法
、ＣＶＤ法など）に比べ、低コストにて作製可能である
。Furthermore, quartz glass can be manufactured at a lower cost than other manufacturing methods (melting method, CVD method, etc.).
以 上that's all
Claims (1)
し、これをゲル化させて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
スの製造においで、ウェットゲル作製の工程にて以下の
処理を施すことを特徴とする大型塊状ガラスの製造方法
。 ａ）ウェットゲルを、アルコール等の揮発性の高い溶剤
中に少なくとも１日以上浸漬する。 ｂ）前記ウェットゲルと溶剤中から取り出した後、更に
水等の不揮発性の溶剤中に１時間〜１０日間浸漬する。[Claims] 1) Glass production by a sol-gel method in which a liquid sol is prepared using a metal alkoxide as the main raw material, this is gelled to produce a wet gel, and then the wet gel is dried and sintered. A method for producing a large lump of glass, characterized in that the following treatment is performed in the process of producing a wet gel. a) The wet gel is immersed in a highly volatile solvent such as alcohol for at least one day. b) After removing the wet gel from the solvent, the gel is further immersed in a non-volatile solvent such as water for 1 hour to 10 days.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12541287A JPS63291822A (en) | 1987-05-22 | 1987-05-22 | Production of large-sized glass block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12541287A JPS63291822A (en) | 1987-05-22 | 1987-05-22 | Production of large-sized glass block |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63291822A true JPS63291822A (en) | 1988-11-29 |
Family
ID=14909466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12541287A Pending JPS63291822A (en) | 1987-05-22 | 1987-05-22 | Production of large-sized glass block |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63291822A (en) |
-
1987
- 1987-05-22 JP JP12541287A patent/JPS63291822A/en active Pending
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