JPS63277526A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPS63277526A JPS63277526A JP11122387A JP11122387A JPS63277526A JP S63277526 A JPS63277526 A JP S63277526A JP 11122387 A JP11122387 A JP 11122387A JP 11122387 A JP11122387 A JP 11122387A JP S63277526 A JPS63277526 A JP S63277526A
- Authority
- JP
- Japan
- Prior art keywords
- added
- sol
- liquid sol
- liquid gel
- glass
- 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 20
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 239000011882 ultra-fine particle Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000000654 additive Substances 0.000 claims description 9
- 230000000996 additive effect Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000004017 vitrification Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 4
- 239000000499 gel Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (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.
従来のガラス中への微量の異元素の添加方法は、原料粉
体中に添加元素粉末を混合した後、溶融する方法、添加
元素を含む気体原料を主原料と共に反応させるＯＶＤ法
などであった。Conventional methods for adding trace amounts of different elements into glass include mixing the additive element powder into raw material powder and then melting it, and the OVD method in which a gaseous raw material containing the additive element is reacted with the main raw material. .
しかし、前述の従来技術では、溶融法においては、ガラ
ス中で添加元素の濃度分布が生じ、均質なガラスを得る
のは、困難であり、ＯＶＤ法においては、プロセス的に
高コストであり、ガラスが高価なものになってしまうと
いう問題点を有するそこで本発明はこのような問題点を
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、微量の異元素の添加を容易にし、低コストで
所望ガラスを製造する方法を提供するところにある。However, in the above-mentioned conventional technology, in the melting method, the concentration distribution of additive elements occurs in the glass, making it difficult to obtain homogeneous glass, and in the OVD method, the process cost is high, and the glass The present invention has the problem of being expensive, and the purpose of the present invention is to facilitate the addition of trace amounts of foreign elements using the sol-gel method. The purpose of the present invention is to provide a method for manufacturing desired glass at low cost.
少なくとも、金属アルコキシドあるいは、金属酸化物超
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、これをゲル化、乾燥、焼結するゾル−ゲル法に
よるガラスの製造において、ａｍの異元素の添加方法と
して、α）添加元素を含む易溶性の化合物（塩化物、各
種の塩など）を溶剤（水、アルコールなど）中に溶解さ
せ、これの所定量を液状ゾルに添加する。ｂ）添加元素
を含む化合物として金属アルコキシドを用い、これのア
ルコール溶液を、液状ゾルに添加する。At least, in the production of glass by the sol-gel method, in which a liquid sol with the desired glass component composition is prepared using metal alkoxide or metal oxide ultrafine particles as the main raw material, and this is gelled, dried, and sintered, different elements such as am are used. As a method for adding α), a readily soluble compound (chloride, various salts, etc.) containing the additive element is dissolved in a solvent (water, alcohol, etc.), and a predetermined amount of this is added to the liquid sol. b) A metal alkoxide is used as a compound containing an additive element, and an alcohol solution thereof is added to the liquid sol.
Ｃ）添加元素の酸化物超微粒子を所定量、液状ゾルに添
加する９以上のいずれかによることを特徴とする。C) It is characterized by adding a predetermined amount of ultrafine oxide particles of the additive element to the liquid sol.
本発明によれば、他成分元素の添加を液状ゾルの段階で
行なうため、濃度分布を生じない均質なガラスが得られ
ると共に、添加量の制御が容易であるため、種々の添加
量のガラスを、安価で作製できるものである。According to the present invention, since other component elements are added at the stage of liquid sol, a homogeneous glass without concentration distribution can be obtained, and the amount of addition can be easily controlled, so that glass with various addition amounts can be obtained. , which can be manufactured at low cost.
〔実施例〕
１）液状ゾルの調製
α）市販のエチルシリケート（５ｉ（ＯＥｃ）４）６１
０ｄ、 ＣＬＯＩ Ｍ−Ｎｆｔ ５４０ＩＬｌを混合
攪拌し、エチルシリケートの加水分解反応を行なった、
該反応液に攪拌しながら超微粒子シリカ２２５１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（攪拌併用）を３時間行なった。なお、こ
の際、超音波照射による該ゾ／Ｌ’温度の上昇を防ぐた
め、水浴中で行ない、ゾル温度をほぼ一定に保持した０
次工程として、該ゾル中の半ゲル化ゼリー状物やゴミな
どを除去するため、該ゾルに対し遠心分離、濾過により
精製し、液状ゾルを調製した。[Example] 1) Preparation of liquid sol α) Commercially available ethyl silicate (5i (OEc) 4) 61
0d, CLOI M-Nft 540ILl were mixed and stirred to perform a hydrolysis reaction of ethyl silicate.
Ultrafine particle silica 2251 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, in order to prevent the sol/L' temperature from increasing due to ultrasonic irradiation, the sol temperature was kept almost constant by being carried out in a water bath.
In the next step, in order to remove semi-gelled jelly-like substances and dust from the sol, the sol was purified by centrifugation and filtration to prepare a liquid sol.
ｂ）市販のエチルシリケート６００ｊｔエチルアルコー
ル（Ｃ！２Ｈ５ＯＨ） ９００ ｍ 、アンモニア水（
２９％）１５ｄおよび水２００ｄを混合攪拌し、シリカ
微粒子の分散液を調製し、１０時間程度静置した後、水
を２００ｄ添加し、濃縮を行ない２５０１Ｌｔのシリカ
微粒子分散液とした。更に、該分散液に２Ｎ−ＨＣｌを
滴下しＰＨ値を２０ｄ度に調整し、エチルシリケー）２
６０ｄを添加、攪拌し加水分解反応を行ない、均一な液
状ゾルを調製した。b) Commercially available ethyl silicate 600jt ethyl alcohol (C!2H5OH) 900 m, ammonia water (
29%) 15d) and 200d of water were mixed and stirred to prepare a dispersion of silica fine particles.After standing for about 10 hours, 200d of water was added and concentrated to obtain a 2501Lt silica fine particle dispersion. Furthermore, 2N-HCl was added dropwise to the dispersion to adjust the pH value to 20 degrees, and ethyl silicate) 2
60d was added and stirred to carry out a hydrolysis reaction to prepare a uniform liquid sol.
２）他成分元素の添加
α）Ｎａの添加
ＮａＣｔ を水に溶解させ、ガラス化時に５ＰＰｍとな
るように所定量を該液状ゾル中に添加した。2) Addition of other component elements α) Addition of Na NaCt was dissolved in water, and a predetermined amount was added to the liquid sol to give a concentration of 5 PPm during vitrification.
またＮａｏｃｚＨｓのエタノール溶液を上記同様に、ガ
ラス化時に５ ＰＰ、ＩＸとなるように所定量を該液状
ゾル中に添加した。Further, in the same manner as above, a predetermined amount of an ethanol solution of NaoczHs was added to the liquid sol so that 5 PP, IX was obtained during vitrification.
、６）Ｔｉの添加
ＴｉＯ４４を水に溶解させ、ガラス化時に５ＰＰｍとな
るように所定量を該液状ゾル中に添加した。, 6) Addition of Ti TiO44 was dissolved in water, and a predetermined amount was added to the liquid sol so as to give 5 PPm during vitrification.
またＴｉ（ｉｓｏ −０ｓＨｒＯ）４のイソプロハ／
−ルｆｌ液を上記同様に、ガラス化時に５ＰＰｍとなる
ように所定量を該液状ゾル中に添加した。Also, isoproha of Ti(iso -0sHrO)4/
In the same manner as above, a predetermined amount of the sol fl liquid was added to the liquid sol so that the concentration was 5 PPm during vitrification.
超微粒子チタニアを水に分散させ、この分散液を、ガラ
ス化時５ ＰＰｍとなるように所定量、該液状ゾル中に
添加し、均一に分散させた。Ultrafine titania particles were dispersed in water, and a predetermined amount of this dispersion liquid was added to the liquid sol so as to have a concentration of 5 PPm during vitrification, and was uniformly dispersed.
Ｃ）Ａｔの添加
ムｔａｔｓと水に溶解させ゛、ガラス化時に１０ ＰＰ
ｍとなるように所定量を液状ゾル中に添加した。C) Addition of Atts and dissolve in water to give 10 PP during vitrification.
A predetermined amount was added to the liquid sol so that m.
また）ｔ（０ｃｚＨｓ ） ｓ のエタノール溶液を
上記同様にガラス化時１’ＯＦＰｍとなるように所定−
を該液状ゾル中に添加した。Furthermore, an ethanol solution of t(0czHs) s was prepared in the same way as above so that it would be 1'OFPm during vitrification.
was added into the liquid sol.
超微粒子アルミナを水に分散させ、この分散液を、ガラ
ス化時１１０ＰＰとなるように所定量、該液状ゾル中に
添加し、均一に分散させた。Ultrafine particle alumina was dispersed in water, and a predetermined amount of this dispersion liquid was added to the liquid sol so as to have a PP of 110 PP during vitrification, and was uniformly dispersed.
以上のようにして、他成分元素の添加を行なったゾルに
アンモニア水を滴下しＰＨ値を３〜６程度に調整し、密
閉容器中でゲル化させた後、該ウェットゲルが脱水重縮
合反応の進行に伴ないある程度収縮した時点で、容器を
多少、開放し、乾燥機に投入し、７０℃にて乾燥し５日
間で乾燥が終了し、白色の乾燥ゲルを得た。As described above, ammonia water is added dropwise to the sol to which other component elements have been added, the pH value is adjusted to about 3 to 6, and the gel is formed in a closed container. When the container had shrunk to some extent as the process progressed, the container was opened a little, put into a dryer, and dried at 70°C. Drying was completed in 5 days to obtain a white dry gel.
ここで得られた種々の乾燥ゲルを焼結炉に投入し加熱焼
結し、１１００〜１３００℃にて透明なガラス体を得た
。The various dried gels obtained here were put into a sintering furnace and heated and sintered to obtain transparent glass bodies at 1100 to 1300°C.
このようにして作製したガラスの純度分析を行なったと
ころ、はぼ、予定通りの添加量であることが判明した。When the purity of the glass thus produced was analyzed, it was found that the amount added was exactly as expected.
このようにして本発明によれば、ガラス中へのｗｉｔの
他成分元素の添加が容易であるため、製造工程において
は、焼結温度の制御Ｃ低温化あるいは高温化）、優れた
特性（耐アルカリ、耐酸性。In this way, according to the present invention, it is easy to add other component elements of wit into the glass, so in the manufacturing process, it is possible to control the sintering temperature (lower or higher temperature), and have excellent properties (durability). Alkali and acid resistant.
高強度、耐熱性２強磁性、イオン伝導性など）の付加な
どが可能となる。It becomes possible to add properties such as high strength, heat resistance, ferromagnetism, and ionic conductivity.
したがって、これまで添加が困難であった元素の添加に
より種々の高機能を持つガラスの製造が可能となり、そ
の応用は広範囲になると考える。Therefore, by adding elements that have been difficult to add until now, it will become possible to manufacture glasses with various high functions, and we believe that their applications will be wide-ranging.
Claims (1)
化物超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、これをゲル化させた後、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、微量
の異元素を以下の方法にて添加することを特徴とするガ
ラスの製造方法。 ａ）添加元素を含む易溶性の化合物（塩化物、各種の塩
など）を溶剤（水、アルコールなど）中に溶解させ、こ
れの所定量を液状ゾルに添加するｂ）添加元素を含む化
合物として金属アルコキシドを用い、これのアルコール
溶液を、液状ゾルに添加する。 ｃ）添加元素の酸化物超微粒子を所定量、液状ゾルに添
加する。(1) At least, a liquid sol with the desired glass component composition is prepared using metal alkoxide or metal oxide ultrafine particles as the main raw material, and after gelling the liquid sol, it is dried and sintered. A method for producing glass, characterized in that a trace amount of a different element is added by the following method. a) A readily soluble compound (chloride, various salts, etc.) containing an additive element is dissolved in a solvent (water, alcohol, etc.) and a predetermined amount of this is added to the liquid sol b) As a compound containing an additive element A metal alkoxide is used and its alcohol solution is added to the liquid sol. c) Adding a predetermined amount of ultrafine oxide particles as an additive element to the liquid sol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11122387A JPS63277526A (en) | 1987-05-07 | 1987-05-07 | Production of glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11122387A JPS63277526A (en) | 1987-05-07 | 1987-05-07 | Production of glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63277526A true JPS63277526A (en) | 1988-11-15 |
Family
ID=14555659
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11122387A Pending JPS63277526A (en) | 1987-05-07 | 1987-05-07 | Production of glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63277526A (en) |
-
1987
- 1987-05-07 JP JP11122387A patent/JPS63277526A/en active Pending
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