JPH05124828A - Production of glass - Google Patents
Production of glassInfo
- Publication number
- JPH05124828A JPH05124828A JP31189291A JP31189291A JPH05124828A JP H05124828 A JPH05124828 A JP H05124828A JP 31189291 A JP31189291 A JP 31189291A JP 31189291 A JP31189291 A JP 31189291A JP H05124828 A JPH05124828 A JP H05124828A
- Authority
- JP
- Japan
- Prior art keywords
- glass
- slurry
- produce
- particles
- binder
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/04—Other methods of shaping glass by centrifuging
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、例えば高温材料、光学
材料に適した単成分系の石英ガラス、耐熱材料等に適し
た複成分系ほうケイ酸ガラスのようなガラスの製造方法
に関し、また、板状、柱状の他、複雑な形状に対してニ
アネットシェイプで製造可能なガラスの製造方法に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing glass such as single-component quartz glass suitable for high-temperature materials and optical materials, and multi-component borosilicate glass suitable for heat-resistant materials. The present invention relates to a glass manufacturing method capable of manufacturing a plate shape, a column shape, and a near net shape for a complicated shape.
【0002】[0002]
【従来の技術】従来から、ガラスの製造は、主に粉体原
料の溶融により行われてきており、石英ガラスにおいて
は、水晶などの粉体の溶融の他に、例えば四塩化珪素な
どの液体原料の酸水素炎による加水分解溶融法、VAD
(Vapour Axial Deposittion)法等によっても製造され
ている。2. Description of the Related Art Conventionally, glass has been manufactured mainly by melting powder raw materials. In quartz glass, in addition to melting powder such as quartz, liquid such as silicon tetrachloride is used. Hydrolysis and melting method by oxyhydrogen flame of raw material, VAD
It is also manufactured by the (Vapour Axial Deposittion) method.
【0003】また、近年金属アルコキシドを原料とする
ゾルゲル法によりガラスを製造する試みもなされてい
る。In recent years, attempts have been made to manufacture glass by a sol-gel method using a metal alkoxide as a raw material.
【0004】その他、粉体を原料とするガラスの製造方
法としてホットプレス、スリップキャスト、CIP−H
IP(特開平1−119539)等が提案されている。In addition, hot pressing, slip casting, CIP-H are used as a method for producing glass using powder as a raw material.
IP (Japanese Patent Laid-Open No. 1-119539) and the like have been proposed.
【0005】[0005]
【発明が解決しようとする課題】しかしながら、溶融法
では1400℃以上の高温が必要であるし、特に石英ガ
ラスの製造においては、VAD法で1500℃以上、酸
水素炎加水分解溶融法では2000℃以上の高温度を必
要とするためエネルギーコストが高いという欠点があ
る。However, the melting method requires a high temperature of 1400 ° C. or higher, and particularly in the production of quartz glass, the VAD method is 1500 ° C. or higher, and the oxyhydrogen flame hydrolysis and melting method is 2000 ° C. Since the above high temperature is required, the energy cost is high.
【0006】また、ゾルゲル法では1300℃以下の比
較的低い温度でガラスを製造することができるが、ガラ
ス前駆体となるゲルが乾燥時に割れ易く、大型のガラス
を得ることが容易ではない。Although the sol-gel method can produce glass at a relatively low temperature of 1300 ° C. or lower, it is not easy to obtain a large glass because the gel as a glass precursor is easily broken during drying.
【0007】ゾルゲル法では、この他にゲルの乾燥を超
臨界乾燥によって行い、短時間で割れのないゲルを得る
ことができるが、大型の乾燥ゲルを得るためには大型の
高圧設備が必要であり、設備コストが極めて高くなると
いう欠点を有する。In the sol-gel method, in addition to this, gel drying can be performed by supercritical drying to obtain a gel without cracks in a short time, but a large high-pressure facility is required to obtain a large dried gel. However, there is a drawback that the equipment cost becomes extremely high.
【0008】ホットプレスを用いると、容易にガラスを
製造することができるが、プレス金型からの汚染が激し
く、しかも得られたガラスには多数の泡が内包されるた
め、低品質のものしか得られない。Glass can be easily produced by using a hot press, but since the contamination from the press die is severe and a large number of bubbles are included in the obtained glass, only a low quality glass is produced. I can't get it.
【0009】その他、粉体からのガラスの製造の試みと
して、スリップキャストによるガラスの製造が行われて
いるが、常圧キャストの場合は厚肉のガラスを得ること
ができないし、加圧キャストの場合、製造装置が複雑に
なるという欠点がある。In addition, as an attempt to manufacture glass from powders, glass is manufactured by slip casting, but in the case of normal pressure casting, thick glass cannot be obtained, and pressure casting In this case, there is a drawback that the manufacturing apparatus becomes complicated.
【0010】また、CIP−HIPによるガラスの製造
方法は、極めて高い圧力を必要とし、しかも大型のガラ
スを製造するためには設備コストが膨大となるため、ガ
ラスの製造には不利である。Further, the method for producing glass by CIP-HIP is extremely disadvantageous for producing glass because it requires extremely high pressure, and the equipment cost for producing large glass is enormous.
【0011】本発明の目的は前述のような問題点を解決
し、短時間でしかも安価に大型の、しかも高品質なガラ
スを製造する方法、所望の形状のガラスをニアネットシ
ェイプで製造する方法、あるいは多成分添加によって機
能性ガラスを製造する方法を提供することにある。An object of the present invention is to solve the above-mentioned problems, to produce a large glass of high quality in a short time and at low cost, and a method of producing a glass having a desired shape with a near net shape. Another object of the present invention is to provide a method for producing a functional glass by adding multiple components.
【0012】[0012]
【課題を解決するための手段】すなわち本発明は、ガラ
スの原料となる粒子をバインダーを添加した水あるいは
有機溶媒に分散させて均一なスラリーとし、該スラリー
を遠心鋳込み成形により固液分離し、成形後、該成形体
を乾燥、焼結、ガラス化することを特徴とするガラスの
製造方法である。Means for Solving the Problems That is, the present invention is to disperse particles, which are raw materials for glass, in water or an organic solvent to which a binder is added to obtain a uniform slurry, and the slurry is subjected to solid-liquid separation by centrifugal casting. After the molding, the molded body is dried, sintered, and vitrified, which is a method for producing glass.
【0013】本発明において、ガラス原料に用いる粒子
は金属、非金属を問わず、ガラスを形成する化合物であ
れば特に制限されないし、単成分に限らず複成分、多成
分でも利用可能である。主なガラスの原料としては、ケ
イ酸、ホウ酸、リン酸あるいはこれらのソーダ塩、カリ
塩などである。また、用いる粒子の形状は、真球状、亜
球状、凹凸状など種々のものが利用できるが、好ましく
は真球状がよく、しかも多分散よりも粒子径の揃った単
分散のものがさらに適当であり、結果として緻密な成形
体を得ることができるため、泡のない高品質なガラスを
製造することができる。また、用いる粒子の粒径は0.
01〜10μmの範囲が好ましい。In the present invention, the particles used for the glass raw material are not particularly limited as long as they are compounds that form glass, regardless of whether they are metals or non-metals, and they are not limited to a single component and may be a multi-component or a multi-component. The main raw materials for glass are silicic acid, boric acid, phosphoric acid, or their soda salts and potassium salts. Further, the shape of the particles to be used can be variously spherical, subspherical, uneven, etc., but preferably spherical, more preferably monodisperse with uniform particle size rather than polydisperse. Since, as a result, a dense molded body can be obtained, it is possible to manufacture high-quality glass without bubbles. The particle size of the particles used is 0.
The range of 01 to 10 μm is preferable.
【0014】原料粒子はバインダーを添加した水あるい
は有機溶媒等の溶液に分散して均一なスラリーとする
が、バインダーとしてはポリビニルアルコール等の有機
系高分子あるいは金属アルコキシド加水分解物を用い
る。The raw material particles are dispersed in a solution of a binder-added water or an organic solvent to form a uniform slurry, and an organic polymer such as polyvinyl alcohol or a metal alkoxide hydrolyzate is used as the binder.
【0015】また、必要により金属、非金属の添加剤を
用いることができる。例えば耐アルカリ性を付与するこ
とを目的とするジルコニウム塩、低熱膨張性を付与する
ことを目的とするチタニウム塩、紫外線透過率制御を目
的とするセリウム塩等を添加することができる。これら
は粉体としてスラリー中に添加されるか、又は溶液とし
てスラリーに混合して用いる。If desired, metallic or non-metallic additives can be used. For example, a zirconium salt for the purpose of imparting alkali resistance, a titanium salt for the purpose of imparting a low thermal expansion property, a cerium salt for the purpose of controlling the ultraviolet transmittance and the like can be added. These are added to the slurry as a powder or mixed with the slurry as a solution for use.
【0016】本発明は、遠心鋳込み成形によりスラリー
を固液分離し、成形を行う。遠心鋳込み成形に用いられ
る遠心鋳込み成形機は、遠心分離機と同様の構成であ
り、型となる容器にスラリーを投入し、遠心鋳込み成形
時に、その回転速度を高速にすることで大きな遠心力を
生ぜしめ、その遠心力でスラリーを固液分離して、成形
体を製造するため、回転速度は高いほうがより効果的で
あり、成形時の遠心力は3000G以上、好ましくは5
000G以上が必要である。According to the present invention, the slurry is subjected to solid-liquid separation by centrifugal casting to perform molding. The centrifugal cast molding machine used for centrifugal cast molding has the same configuration as the centrifugal separator, and puts the slurry into a container that becomes a mold, and at the time of centrifugal cast molding, a large centrifugal force is generated by increasing the rotation speed thereof. Since a slurry is produced and the slurry is solid-liquid separated by the centrifugal force to produce a molded body, a higher rotation speed is more effective, and the centrifugal force at the time of molding is 3000 G or more, preferably 5 G.
000G or more is required.
【0017】[0017]
【作用】本発明は、粉体の成形を遠心鋳込み成形により
行うために、極めて短時間でしかも容易に大型の成形体
を製造するとができる。また、得られた成形体に含まれ
る液量が少ないために、収縮が少なく、割れのない大型
の乾燥成形体を容易に製造することができるため、これ
を焼結することにより大型のガラスを製造することがで
きる。According to the present invention, since the powder is molded by centrifugal casting, it is possible to easily manufacture a large molded body in an extremely short time. Further, since the amount of liquid contained in the obtained molded product is small, it is possible to easily produce a large dry molded product with little shrinkage and no cracking. It can be manufactured.
【0018】[0018]
【実施例】以下に、本発明の実施例を示し、さらに詳し
く説明する。 実施例1 バインダーとしてポリビニルアルコールを0.5wt%
添加した水溶液に、平均粒径0.5μmの単分散微粒子
球状シリカを70wt%加え、十分に撹拌して分散さ
せ、均一なスラリーを調製した。次に、スラリーを縦7
cm、横25cm、高さ30cmの容器に高さ25cmまで注入
し密閉後、遠心鋳込み成形機にセットし、高速回転によ
り遠心力8000Gで固液分離を行い、縦7cm、横25
cm、高さ12cmの成形体を得た。得られた成形体を50
℃で3日間、さらに100℃で7日間乾燥を行い、クラ
ックのない乾燥体を製造した。EXAMPLES Examples of the present invention will be shown below and described in more detail. Example 1 0.5 wt% of polyvinyl alcohol as a binder
To the added aqueous solution, 70 wt% of monodisperse fine particle spherical silica having an average particle diameter of 0.5 μm was added, and sufficiently stirred to disperse the silica to prepare a uniform slurry. Next, the slurry is lengthwise 7
cm, width 25 cm, height 30 cm, filled up to a height of 25 cm, sealed, set on a centrifugal casting molding machine, and subjected to solid-liquid separation by centrifugal force 8000 G by high speed rotation, length 7 cm, width 25
A molded body having a height of 12 cm and a height of 12 cm was obtained. 50 to the obtained molded body
Drying was performed for 3 days at 100 ° C. and for 7 days at 100 ° C. to produce a crack-free dried body.
【0019】乾燥体を脱脂炉で、空気あるいは酸素など
の酸化性ガス気流中で800℃まで昇温速度25℃/hr
でか焼して脱炭を行い、次に減圧下で1300℃まで昇
温速度50℃/hrで焼結を行い、縦6cm、横21cm、高
さ10cmのサイズで無気泡の高品質な石英ガラスを製造
した。The dried product is heated in a degreasing furnace to 800 ° C. in a stream of oxidizing gas such as air or oxygen at a heating rate of 25 ° C./hr.
It is calcined to decarburize, then sintered under reduced pressure to a temperature of 1300 ° C at a heating rate of 50 ° C / hr, and has a length of 6 cm, a width of 21 cm and a height of 10 cm, and is a bubble-free high quality quartz The glass was manufactured.
【0020】実施例2 バインダーとしてポリビニルアルコールを0.5wt%
添加した水溶液に濃度10ppm となるように塩化セリウ
ム(7水和物)を溶解させた。次に、実施例1同様にし
て遠心鋳込み成形機を用いて成形、か焼、焼結によりシ
リカ−セリアガラスを製造した。 得られたガラスは波
長200nmの紫外線を70%透過する性質を有してい
た。Example 2 0.5 wt% of polyvinyl alcohol as a binder
Cerium chloride (heptahydrate) was dissolved in the added aqueous solution to a concentration of 10 ppm. Next, in the same manner as in Example 1, a silica-ceria glass was manufactured by molding using a centrifugal casting molding machine, calcination, and sintering. The obtained glass had a property of transmitting 70% of ultraviolet rays having a wavelength of 200 nm.
【0021】比較例1 バインダーを添加しない水を分散媒として、0.5μm
の微粒子球状シリカを70wt%加え、十分に撹拌し、
分散させて均一なスラリーを調製し、実施例1と同様に
遠心鋳込み成形機で成形体を製造した。Comparative Example 1 0.5 μm with water containing no binder as a dispersion medium
70% by weight of fine spherical silica particles, and thoroughly stirred,
A uniform slurry was prepared by dispersion, and a molded body was manufactured by a centrifugal casting molding machine in the same manner as in Example 1.
【0022】得られた成形体の乾燥を50℃で行ったと
ころ、乾燥途中で成形体にクラックが入り、割れのない
大型ガラスを得ることができなかった。When the obtained molded product was dried at 50 ° C., the molded product was cracked during the drying, and a large glass without cracks could not be obtained.
【0023】[0023]
【発明の効果】以上のように、本発明によれば、単成
分、多成分を問わず、大型、高品質でしかも種々のガラ
スを短時間で容易、かつ安価に製造することが可能であ
る。Industrial Applicability As described above, according to the present invention, it is possible to easily produce various types of glass of large size, high quality and various kinds, regardless of single component or multicomponent, in a short time and at low cost. ..
Claims (4)
加した水あるいは有機溶媒に分散させて均一なスラリー
とし、該スラリーを遠心鋳込み成形により固液分離し、
成形後、該成形体を乾燥、焼結、ガラス化することを特
徴とするガラスの製造方法。1. Particles, which are raw materials for glass, are dispersed in water or an organic solvent to which a binder is added to obtain a uniform slurry, and the slurry is subjected to centrifugal casting for solid-liquid separation.
After the molding, the molded body is dried, sintered, and vitrified, which is a method for producing glass.
属アルコキシド加水分解物を用いることを特徴とする請
求項1記載のガラスの製造方法。2. The method for producing glass according to claim 1, wherein an organic polymer or a metal alkoxide hydrolyzate is used as the binder.
属化合物を添加して多成分系とすることを特徴とする請
求項1記載のガラスの製造方法。3. The method for producing glass according to claim 1, wherein at least one metal or non-metal compound is added to form a multi-component system.
分散粒子であることを特徴とする請求項1記載のガラス
の製造方法。4. The method for producing glass according to claim 1, wherein the raw material particles of glass are monodisperse particles having a uniform particle size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31189291A JPH05124828A (en) | 1991-10-30 | 1991-10-30 | Production of glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31189291A JPH05124828A (en) | 1991-10-30 | 1991-10-30 | Production of glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05124828A true JPH05124828A (en) | 1993-05-21 |
Family
ID=18022673
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31189291A Pending JPH05124828A (en) | 1991-10-30 | 1991-10-30 | Production of glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05124828A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0775672A1 (en) * | 1995-11-25 | 1997-05-28 | Philips Patentverwaltung GmbH | Process for producing a flat, glasslike or ceramic shaped article of structured surface |
-
1991
- 1991-10-30 JP JP31189291A patent/JPH05124828A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0775672A1 (en) * | 1995-11-25 | 1997-05-28 | Philips Patentverwaltung GmbH | Process for producing a flat, glasslike or ceramic shaped article of structured surface |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A02 | Decision of refusal |
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