JPS63190726A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPS63190726A JPS63190726A JP2281687A JP2281687A JPS63190726A JP S63190726 A JPS63190726 A JP S63190726A JP 2281687 A JP2281687 A JP 2281687A JP 2281687 A JP2281687 A JP 2281687A JP S63190726 A JPS63190726 A JP S63190726A
- Authority
- JP
- Japan
- Prior art keywords
- vessel
- glass
- container
- sol
- air
- 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 30
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 15
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 230000005484 gravity Effects 0.000 claims abstract description 7
- 239000000919 ceramic Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims abstract description 5
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 239000005373 porous glass Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 8
- RVHSTXJKKZWWDQ-UHFFFAOYSA-N 1,1,1,2-tetrabromoethane Chemical compound BrCC(Br)(Br)Br RVHSTXJKKZWWDQ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000035699 permeability Effects 0.000 abstract description 3
- -1 Si(OC2H5)4 Chemical class 0.000 abstract description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract 1
- 238000007598 dipping method Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 19
- 239000000499 gel Substances 0.000 description 8
- 238000003980 solgel method Methods 0.000 description 5
- 238000005336 cracking Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N carbon tetrachloride Substances ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000007787 solid 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)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、金属アルコキシドを主原料としたゾル−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 Industrial Application] The present invention relates to a method for producing glass by a sol-gel method using metal alkoxide as a main raw material.
本発明は金属アルコキシドを主原料とするゾル溶液に対
して不溶性であり、かつ比重の大きな液体を入れた容器
内に、上記液体表面が少なくとも通気性容器内部底面よ
りも高くなるように少なくとも底部が通気性を持った通
気性容器を浸漬しこの通気性容器内に前記アルコキシド
を主原料とするゾル溶液を入れてゲル化した後、上記通
気性容器を前記液体より取り出してから本通気性容器内
で乾燥させて取り出し焼結することにより、このような
ブルーゲル法によるガラスの製造工程におけるワレ、ソ
リ、キレツ等を防ぐことを可能ならしむるものである。In the present invention, at least the bottom part is placed in a container containing a liquid that is insoluble in a sol solution containing a metal alkoxide as a main raw material and has a large specific gravity, so that the surface of the liquid is higher than the internal bottom surface of the breathable container. After immersing an air-permeable container into the air-permeable container and putting the sol solution containing the alkoxide as the main raw material into the air-permeable container and gelling it, the air-permeable container is removed from the liquid and then placed inside the air-permeable container. By drying the glass, taking it out and sintering it, it is possible to prevent cracks, warps, chips, etc. in the glass manufacturing process using the blue gel method.
従来から金属アルコキシドを主原料にしたゾル−ゲル法
によるガラスの製造方法は種々試みられている。ゾル−
ゲル法の利点として、今までガラスの製造方法は原料を
１５００℃〜２０００℃という高温で一度溶解した後結
晶ができないように凝固させる方法であったのが、この
ゾル−ゲル法を使用すれば１ｏｏｏ℃程度の低い温度で
製造することができることであり、したがってエネルギ
ーの節約にもなることである。また、低い温度で製造で
きるため耐熱性の低い金属と組み合わせたガラスを製造
できる。さらに高温で原料を熔かす従来の方法では溶か
した時に成分が均一に混ざり合わないことがあったが、
このゾル−ゲル法ではそのようなことはなく新しいガラ
スを製造する可能性がある、純度の高いガラスができる
、均質性が高い等のいくつかの利点があげられる。BACKGROUND ART Various methods for producing glass using a sol-gel method using metal alkoxide as the main raw material have been attempted. Sol-
An advantage of the gel method is that until now, the method for producing glass was to melt the raw materials at a high temperature of 1500°C to 2000°C and then solidify them to prevent crystals from forming. This means that it can be manufactured at a temperature as low as 100° C., thus saving energy. Additionally, since it can be manufactured at low temperatures, it is possible to manufacture glass in combination with metals that have low heat resistance. Furthermore, with the conventional method of melting raw materials at high temperatures, the ingredients sometimes did not mix uniformly when melted.
This sol-gel method does not have such problems, and has several advantages such as the possibility of producing new glass, the possibility of producing glass with high purity, and high homogeneity.
このように敗多くの利点を有しているゾル−ゲル法の一
般的な製造方法は、原料を水・アルコール（溶媒として
必要）と共に混合させて、加水分解をお、ニさせゲル状
にした後乾燥するとアルコールや水分が徐々に揮発し固
体状ゲルになりそれを焼結（過熱）することによりガラ
スを得てきた。The general manufacturing method of the sol-gel method, which has many advantages as described above, is to mix the raw materials with water and alcohol (required as a solvent) to slow down hydrolysis and form a gel. After drying, the alcohol and water gradually evaporate to form a solid gel, which is then sintered (overheated) to obtain glass.
しかしながら従来のゾル−ゲル法を用いたガラスの製造
方法では、乾燥・焼結中に表面全体にワレやキレツ、お
よびｍ ’ｆＩＱ・薄板を作製するときにソリが生ずる
という問題点を存していた。However, the conventional glass manufacturing method using the sol-gel method has problems such as cracks and chips on the entire surface during drying and sintering, and warping when manufacturing m'fIQ and thin plates. Ta.
本発明によるガラスの製造方法は、金属アルコキシドを
主原料とするゾル？ｆｉＷｉに対して不溶性であり、か
つ比重の大きな液体（以下この液体をフロート液と呼ぶ
）を入れた容器内に、上記フロート液表面が多孔質ガラ
ス、ハニカム構造セラミックス、多孔質ポリマーなどの
通気性容器内部底面よりも少な（とも高くなるように少
なくとも底部が通気性を持った通気性容器を漫清しこの
通気性容器内に前記アルコキシドを主原料とするゾル溶
液を入れてゲル化した後、上記通気性容器を前記フロー
ト液より取り出してから本通気性容器内で乾燥させて取
り出し焼結することによりワレ、ソリ、キレツ等のない
ガラスを製造することができ上記問題点を解決した。The method for producing glass according to the present invention is based on a sol whose main raw material is a metal alkoxide. In a container containing a liquid that is insoluble in fiWi and has a large specific gravity (hereinafter referred to as a float liquid), the surface of the float liquid is made of an air-permeable material such as porous glass, honeycomb structured ceramics, or porous polymer. After clearing an air-permeable container whose bottom has air permeability at least so that the amount is lower (or higher than the inside bottom surface of the container), and pouring the sol solution containing the alkoxide as the main raw material into the air-permeable container and gelling it, By taking out the air-permeable container from the float liquid, drying it in the air-permeable container, and then taking it out and sintering it, glass without cracks, warps, chips, etc. can be produced, and the above-mentioned problems have been solved.
以下の本発明によるガラスの製造方法を実施例に従って
図面を用いな、がら説明する０図は本発明によるガラス
の製造方法の工程図でありｆａ＋は出発工程、山）はゲ
ル化工程、ｆｃｌは乾燥工程、（ｄｌは焼結工程、（ｅ
）は完成工程を示している。また図中１はフロート液を
入れる容器、２は金属アルコキシドを主原料とするゾル
溶液、３は通気性容器、４は通気性容器内部底面、５は
フロート液、６はゲル化した原料である０図ｆａ＋に示
す出発工程においてまずガラスやテフロンなどからなる
フロート液を入れる容器１内に多孔質ガラス、ハニカム
構造セラミックス、多孔質ポリマー等の材料からなる通
気性容器３を入れ、テトラブロムエタンのような金属ア
ルコキシドを主原料とするゾル溶液に対し不溶性であり
かつ比重の大きなフロート液を液表面が通気性容器内部
底面より少なくとも高くなるまで入れた。なおこのとき
金属アルコキシドを主原料とするゾル溶液２の粘度が通
気性容器３をつくっている多孔性材料からしみ出ない程
度に大きい場合は通気性容器３全部を多孔性材料でつく
った方が良いが、そうでない場合は、通気性容器３の少
なくとも底部が多孔性材料でつくられていればよい。ま
た、通気性容器３の材料がハニカム構造セラミックであ
る場合は、ハニカムを構成している穴がフロート液に対
し適当な角度を持っていなければならない。そして通気
性容器３内に金属アルコキシドを主原料とするゾル溶液
２を入れ、通気性容器３に通気性のフタをして出発工程
＋８１は終了した。The method for producing glass according to the present invention will be explained below using the drawings in accordance with the examples. Figure 0 is a process diagram of the method for producing glass according to the present invention, where fa+ is the starting process, mountain) is the gelling process, and fcl is Drying process, (dl is sintering process, (e
) indicates the completion process. In addition, in the figure, 1 is a container containing the float liquid, 2 is a sol solution containing metal alkoxide as the main raw material, 3 is an air-permeable container, 4 is the inner bottom of the air-permeable container, 5 is the float liquid, and 6 is the gelled raw material. In the starting process shown in Figure 0fa+, first, an air-permeable container 3 made of a material such as porous glass, honeycomb structure ceramics, or porous polymer is placed in a container 1 made of glass or Teflon containing a float liquid. A float liquid which is insoluble in a sol solution containing a metal alkoxide as a main raw material and has a high specific gravity was poured into the air-permeable container until the surface of the liquid was at least higher than the inner bottom surface. At this time, if the viscosity of the sol solution 2 containing metal alkoxide as the main raw material is so large that it does not seep through the porous material that makes up the breathable container 3, it is better to make the entire breathable container 3 from a porous material. However, if this is not the case, at least the bottom of the breathable container 3 may be made of a porous material. Further, when the material of the breathable container 3 is a honeycomb structured ceramic, the holes forming the honeycomb must have an appropriate angle with respect to the float liquid. Then, the sol solution 2 containing metal alkoxide as the main raw material was put into the air-permeable container 3, and the air-permeable container 3 was covered with an air-permeable lid, and the starting step +81 was completed.
次に出発工程で作製した容器を適度な温度・湿度条件で
放置すると金属アルコキシドを主原料とするゾル溶液２
はゲル化した原料６となった。これがゲル化工程（ｂｌ
であるが、従来この工程においてワレ、ソリ、キレツが
多発していたが、本発明によるガラスの製造方法のゲル
化工程においてはワレ１ ソリ、キレツはほとんど見ら
れなかった。Next, when the container prepared in the starting process is left under moderate temperature and humidity conditions, a sol solution containing metal alkoxide as the main raw material 2
became gelled raw material 6. This is the gelation process (bl
However, conventionally, cracks, warps, and chips frequently occurred in this process, but hardly any cracks, warps, or chips were observed in the gelling step of the glass manufacturing method according to the present invention.
また、従来の方法に比べて薄い板状ゲルも容易に得られ
、最小板厚５０μｍのものまで得られた。In addition, thinner plate-shaped gels were easily obtained compared to conventional methods, and a minimum plate thickness of 50 μm was obtained.
次に、フロート液を入れる容器１から通気性容器３をと
り出し恒温槽内に入れ、ゲル化した原料６の溶媒を除去
する乾燥工程（Ｃ）に入る。その後乾燥したゲル原料を
通気性容器３から取り出して大気中で１０００℃程度で
焼結する焼結工程ｆｄ＋を経てガラスの製造を終わる。Next, the air-permeable container 3 is taken out from the container 1 containing the float liquid and placed in a constant temperature bath, and a drying step (C) is started in which the solvent of the gelled raw material 6 is removed. Thereafter, the dried gel raw material is taken out from the air-permeable container 3 and undergoes a sintering step fd+ in which it is sintered at about 1000° C. in the atmosphere, and glass production is completed.
また完成工程はガラス化した原料７を適当な形に加工す
る工程である。Further, the completion process is a process of processing the vitrified raw material 7 into a suitable shape.
本発明によるガラスの製造方法によって作製したガラス
は完成工程ｆｅｌにおける加工においてもワレのない加
工が可能であった。The glass produced by the glass production method of the present invention could be processed without cracking even in the finishing step fel.
実施例１
市販の５ｉ（ＯＣＪｓ）ａを５００ｍｊ！と０．０２Ｎ
−ＩＣＪを２００ｍｊ！とを混合したものを出発ゲルと
して、フロート液としてテトラブロムエタンを用い本発
明のガラスの製造方法に従ってＳｉＯ□ガラスを作製し
たところ、全くワレ、ソリ、キレンのないガラスができ
た。Example 1 500mj of commercially available 5i (OCJs)a! and 0.02N
-200 mj of ICJ! When SiO□ glass was produced according to the method for producing glass of the present invention using a mixture of the above as a starting gel and tetrabromoethane as a float liquid, a glass with no cracking, warping, or clearing was obtained.
実施例２
市販のＳｉ （ＯＣ２Ｈ５） ４をｌ Ｑ ｍ ｊ！と
０．００２Ｎ−１１Ｃｒｔをｍｌとを混合したものを出
発ゲルとして、フロート液としてテトラブロムエタンを
用い本発明のガラスの製造方法に従って厚み５０μｍの
５ｉＯｚＦｉｌ板を作製したところ全くワレ、ソリ、キ
レンは生じなかった。Example 2 Commercially available Si (OC2H5) 4 was added to l Q m j! When a 5iOzFil plate with a thickness of 50 μm was prepared according to the glass manufacturing method of the present invention using a mixture of 0.002N-11Crt and 0.002N-11Crt as a starting gel and tetrabromoethane as a float liquid, no cracks, warpage, or cracks were observed. It did not occur.
以上実施例を述べてきたが、フロート液としてはパーク
ロルエチレン、トリクロルエチレン、四塩化炭素などを
用いてもよい。Although the embodiments have been described above, perchloroethylene, trichlorethylene, carbon tetrachloride, etc. may also be used as the float liquid.
以上述べたように、本発明によるガラスの製造方法は、
金属アルコキシドを主原料とするゾル溶液に対して不溶
性であり、かつ比重の大きな液体を入れた容器内に、上
記液体表面が少なくとも通気性容器内部底面よりも高く
なるように少なくとも底部が通気性を持った通気性容器
を漫清しこの通気性容器内に前記アルコキシドを主原料
とするゾル溶液を入れてゲル化した後、上記通気性容器
を前記液体より取り出してから本通気性容器内で乾燥さ
せて取り出し焼結することにより、ワレ。As described above, the method for manufacturing glass according to the present invention includes:
In a container containing a liquid that is insoluble in a sol solution containing metal alkoxide as the main raw material and has a large specific gravity, at least the bottom part is made breathable so that the surface of the liquid is higher than the internal bottom of the breathable container. After thoroughly cleaning the breathable container held in the breathable container and putting the sol solution containing the alkoxide as the main raw material into the breathable container and gelling it, remove the breathable container from the liquid and dry it in the breathable container. By taking it out and sintering it, it becomes cracked.
ソリ、キレンのない高品質なガラスを安価に歩留り良く
製造することができるという効果を有する。It has the effect that high-quality glass without warping or cracking can be manufactured at low cost and with a high yield.
図は本発明によるガラスの製造方法の工程図でｔａｌ〜
ｆｄｌは側面図、（ｅ）は斜視図である。
＋ａｌ・・・出発工程
（ｂｌ・・・ゲル化工程
（ｃｌ・・・乾燥工程
（ｄｌ・・・焼結工程
ｔｅ＋・・・完成工程
１・・・フロート液を入れる容器
２・・・金属アルコキシドを主原料とするゾル溶液
３・・・通気性容器
４・・・通気性容器内部底面
５・・・フロート液
６・・・ゲル化した原料The figure is a process diagram of the glass manufacturing method according to the present invention.
fdl is a side view, and (e) is a perspective view. +al... Starting process (bl... Gelling process (cl... Drying process (dl... Sintering process te+... Completion process 1... Container for holding float liquid 2... Metal alkoxide Sol solution containing as main raw material 3... Breathable container 4... Inner bottom surface of breathable container 5... Float liquid 6... Gelled raw material
Claims (2)
て不溶性であり、かつ比重の大きいフロート液を入れた
容器内に、 少なくとも底部が通気性をもった通気性容器を前記フロ
ート液の表面がこの通気性容器内部底面よりも高くなる
ように浸漬し、 前記通気性容器内に前記ゾル溶液を入れてゲル化した後
、 前記通気性容器を前記フロート液より取り出して、この
通気性容器内でゲル原料を乾燥させ、この乾燥したゲル
原料を通気性容器から取り出して焼結することを特徴と
するガラスの製造方法。(1) In a container containing a float liquid that is insoluble in a sol solution containing metal alkoxide as the main raw material and has a high specific gravity, place an air-permeable container with at least a breathable bottom so that the surface of the float liquid is The sol solution is immersed in the air-permeable container so as to be higher than the inner bottom surface of the air-permeable container, and the sol solution is put into the air-permeable container and gelled. A method for producing glass, which comprises drying a gel raw material, taking out the dried gel raw material from an air-permeable container, and sintering it.
セラミックス、多孔質性ポリマーのいずれかであること
を特徴とする特許請求の範囲第１項記載のガラスの製造
方法。(2) The method for producing glass according to claim 1, wherein the material of the breathable container is porous glass, honeycomb structured ceramics, or porous polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2281687A JPS63190726A (en) | 1987-02-03 | 1987-02-03 | Production of glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2281687A JPS63190726A (en) | 1987-02-03 | 1987-02-03 | Production of glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63190726A true JPS63190726A (en) | 1988-08-08 |
Family
ID=12093212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2281687A Pending JPS63190726A (en) | 1987-02-03 | 1987-02-03 | Production of glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63190726A (en) |
-
1987
- 1987-02-03 JP JP2281687A patent/JPS63190726A/en active Pending
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