JPS63265835A - Production of high-hardness quartz glass - Google Patents
Production of high-hardness quartz glassInfo
- Publication number
- JPS63265835A JPS63265835A JP9616787A JP9616787A JPS63265835A JP S63265835 A JPS63265835 A JP S63265835A JP 9616787 A JP9616787 A JP 9616787A JP 9616787 A JP9616787 A JP 9616787A JP S63265835 A JPS63265835 A JP S63265835A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- hardness
- glass
- translucency
- inert gas
- 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
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 238000007731 hot pressing Methods 0.000 abstract description 5
- 239000011521 glass Substances 0.000 description 20
- 238000000034 method Methods 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000002542 deteriorative effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000005345 chemically strengthened glass Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Glass Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、高硬度石英ガラスの製造方法に関するもので
あり、この方法で製造された高硬度石英ガラスは透明性
に優れ、かつ硬度が高く、光学部品（光学素子、光通信
用素子等）、構造材（繊維化し、複合材料の素材等とす
る）１時計、航空機。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing high-hardness quartz glass, and the high-hardness quartz glass produced by this method has excellent transparency and high hardness. , optical parts (optical elements, optical communication elements, etc.), structural materials (made into fibers and used as materials for composite materials, etc.)1 watches, aircraft.
高圧容器などの窓材などに使用出来る。Can be used as window material for high-pressure containers, etc.
［従来の技術］
純粋な石英ガラスは透光性に非常に優れておりかつ、比
較的硬度が高く、ビッカース硬度は５．８ＧＰａ〜８．
９ＧＰａである。石英ガラスの硬度をさらに向上させる
ために添加物を混入させたりするが、透光性が悪化する
のが普通である。[Prior Art] Pure silica glass has excellent translucency and relatively high hardness, with a Vickers hardness of 5.8 GPa to 8.8 GPa.
It is 9GPa. Additives are sometimes mixed in to further improve the hardness of quartz glass, but this usually results in poorer translucency.
また、高硬度化を目的とした以下のようなガラスが報告
されている。In addition, the following glasses aimed at increasing hardness have been reported.
１、結晶化ガラス
■、オキシナイトライドガラス
■、化学強化ガラス
これらの中で現在、硬度が最も高いガラスはオキシナイ
トライドガラスである。このガラスは窒素をガラス構造
中に取り入れ、硬度を向上させたものである。1. Crystallized glass ①, oxynitride glass ②, chemically strengthened glass Among these, oxynitride glass currently has the highest hardness. This glass incorporates nitrogen into the glass structure to improve its hardness.
オキシナイトライドガラスの製造方法には以下のような
方法がある。There are the following methods for manufacturing oxynitride glass.
（１）高温溶融体へのＮＨ３ガス吹込み（２）多孔質ガ
ラスのＮＨ，ガス高温処理法（３）窒化物原料使用の高
温溶融法
（４）窒化物原料使用の高温高圧溶融法しかし、以上の
ような方法によって製造されたオキシナイトライドガラ
スは透光性に優れたものがなかなかできないのが現状で
ある。現在報告されている中で透光性を有し、かつ高い
硬度を持つオキシナイトライドガラスの硬度の値を表１
に示す。(1) Injection of NH3 gas into high-temperature melt (2) High-temperature treatment of porous glass with NH gas (3) High-temperature melting method using nitride raw materials (4) High-temperature and high-pressure melting method using nitride raw materialsHowever, At present, it is difficult to produce oxynitride glasses with excellent translucency produced by the method described above. Table 1 shows the hardness values of oxynitride glasses that are currently reported to have translucency and high hardness.
Shown below.
表１
これらは、石英ガラスと比べてかなり硬度が向上してい
る。しかし、前述したような製造方法では、
（１）原材料が非常に高価である
（２）製造工程が非常に複雑である
（３）透光性に優れたものを製造するのに多くの専門的
技術が必要である
などの問題点があり、オキシナイトライドガラスは市販
に至っていない。そこで、透光性を有した高硬度のガラ
スを容易に製造する方法への要望が極めて強くなってい
る。Table 1 These have considerably improved hardness compared to quartz glass. However, with the manufacturing method described above, (1) the raw materials are extremely expensive, (2) the manufacturing process is extremely complex, and (3) it requires many specialized skills to manufacture products with excellent translucency. Oxynitride glass has not been commercially available due to problems such as the need for advanced technology. Therefore, there is an extremely strong demand for a method for easily manufacturing highly hard glass having translucency.
［発明が解決しようとする問題点］
本発明は、これらの問題点を解決するための透光性に優
れた高硬度の石英ガラスを容易に製造する方法を提供す
るものである。[Problems to be Solved by the Invention] The present invention provides a method for easily producing high-hardness quartz glass with excellent translucency in order to solve these problems.
［問題点を解決するための手段および作用］すなわち、
本発明は、石英ガラスを不活性ガス雰囲気内で、ホット
プレスにより１０００℃以上１５００℃未満に加熱し、
かつ１０ ＭＰａ以上に加圧することによって石英ガラ
スの透光性を実質的に劣化させずに、かつ、高硬度であ
る石英ガラスを製造する方法である。[Means and actions for solving the problem] That is,
The present invention heats quartz glass to 1000°C or more and less than 1500°C by hot pressing in an inert gas atmosphere,
In addition, this is a method for producing quartz glass that is highly hard without substantially deteriorating the translucency of the quartz glass by applying pressure to 10 MPa or more.
純粋な石英ガラスは透光性に非常に優れておりかつ、比
較的硬度が高くビッカース硬度は５．８ＧＰａ〜Ｂ、９
ＧＰａである。石英ガラスは一般に硬度の向上のために
添加物を混入させるが、透光性が悪化するのが普通であ
る。水洗は透光性を実質的に劣化させることなく、高硬
度化が実現することから非常に有効な手段である。Pure silica glass has excellent translucency and is relatively hard, with a Vickers hardness of 5.8 GPa to B, 9.
It is GPa. Additives are generally mixed into silica glass to improve its hardness, but this usually results in poor light transmittance. Washing with water is a very effective means because it can increase hardness without substantially deteriorating translucency.
ここで使用する石英ガラスはいかなる方法で製造したも
のでも良い。形状、大きさについては、操作性の点で２
０ｃ＋ｎ程度のあらかじめほぼ製品寸法に加工されてい
ることが好ましいが特に制限はないＯ
雰囲気は、不活性ガスを使用する。これは石英ガラスの
表面に結晶相が析出しないようにするためである。The quartz glass used here may be manufactured by any method. Regarding the shape and size, it is rated 2 in terms of operability.
It is preferable that the material is pre-processed to approximately the product size of about 0c+n, but there is no particular restriction.O 2 An inert gas is used as the atmosphere. This is to prevent a crystal phase from precipitating on the surface of the quartz glass.
処理温度は、１０００℃以上にすることによって、透光
性にすぐれた高硬度石英ガラスが得られる。By setting the treatment temperature to 1000° C. or higher, high hardness quartz glass with excellent translucency can be obtained.
また、ガラスの流動性を防ぎ初期形状を保つことができ
る１５００℃未満でなければならない。Further, the temperature must be lower than 1500°C, which can prevent the fluidity of the glass and maintain its initial shape.
圧力は、ガラスの大きさにもよるが、ガラス内に圧縮応
力を残すために１０ ＭＰａ以上を必要とする。Although the pressure depends on the size of the glass, a pressure of 10 MPa or more is required to leave compressive stress within the glass.
本発明により透光性に優れた高硬度石英ガラスが製造出
来る理由は、石英ガラスを原料とし、不活性ガス雰囲気
内で、ホットプレスにより１０００℃以上１５００℃未
満に加熱し、かつ１０ ＭＰａ以上に加圧することによ
りガラス中に圧縮応力が残り、それによって硬度があが
ると考えられる。また、ガラス中に入る圧縮応力は極微
量にしか入らない為その透光性に及ぼす影響は全くなく
、石英ガラス本来の非常に優れた透光性を保ったまま硬
度を向上することができるのである。The reason why high-hardness quartz glass with excellent translucency can be produced by the present invention is that quartz glass is used as a raw material, heated to 1000°C or more and less than 1500°C in an inert gas atmosphere by hot pressing, and heated to 10 MPa or more. It is thought that compressive stress remains in the glass by applying pressure, which increases the hardness. In addition, since only a very small amount of compressive stress enters the glass, it has no effect on its translucency, and the hardness can be improved while maintaining the excellent translucency inherent to quartz glass. be.
このようにして製造された透光性に優れた高硬度石英ガ
ラスは圧縮応力が入っているため加工性は比較的とぼし
く、また硬度測定の際にもクラックが入ってしまい正確
な測定は不可能である。そこで、このガラスを通常のガ
ラスの熱処理と同様な方法により処理すると圧縮応力が
多少緩和され、加工性が良好となり、かつ残′存する圧
縮応力によって高硬度な石英ガラスが得られる。熱処理
は大気雰囲気で１０００℃〜１２００℃の温度で行えば
よい。The high-hardness quartz glass manufactured in this way, which has excellent translucency, has compressive stress and therefore has relatively poor workability, and also cracks occur during hardness measurement, making accurate measurement impossible. It is. Therefore, if this glass is treated in a manner similar to the heat treatment of ordinary glass, the compressive stress will be alleviated to some extent, the workability will be improved, and quartz glass with high hardness will be obtained due to the remaining compressive stress. The heat treatment may be performed at a temperature of 1000°C to 1200°C in an air atmosphere.
しかし、この熱処理は必ずしも必要ということではなく
、初期形状において製品寸法に加工しておけば省略する
ことができる。However, this heat treatment is not necessarily necessary, and can be omitted if the initial shape is processed to the product dimensions.
次に、本発明を図面にもとづき説明するが、−例を示す
ものであり本発明はこれになんら限定されるものではな
い。Next, the present invention will be explained based on the drawings, but the present invention is not limited to these examples.
第１図は本発明の高硬度石英ガラスの製造方法の実施状
況の一例を示す概念図である。石英ガラス■をあらかじ
め製品に近い形状に加工しておきセットする。これをカ
ーボンバンチ■とカーボン押し型■により不活性ガス雰
囲気下、高温、高圧処理をして高硬度石英ガラスを製造
する。FIG. 1 is a conceptual diagram showing an example of the implementation status of the method for manufacturing high-hardness quartz glass of the present invention. The quartz glass■ is processed in advance into a shape similar to the product and then set. This is subjected to high-temperature, high-pressure treatment in an inert gas atmosphere using a carbon bunch (2) and a carbon press (2) to produce high-hardness quartz glass.
以上のような方法により容易に透光性に優れた高硬度石
英ガラスを製造することが出来る。High hardness quartz glass with excellent translucency can be easily produced by the method described above.
［実施例コ
次に、本発明を実施例により更に詳細に説明するが、−
例を示すものであり、本発明はこれらの実施例になんら
限定されるものではない。[Example] Next, the present invention will be explained in more detail with reference to Examples.
These examples are shown, and the present invention is not limited to these examples in any way.
（実施例１〜５）
直径７０ｍｍ５高さ７０ｍｍ、、ビッカース硬度８．８
８ＧＰａの石英ガラスを第１図に示すようにホットプレ
ス用カーボン押し型にセットした。ホットプレスの圧力
、雰囲気、時間はそれぞれ１０ ＭＰａｓ Ａｒ雰囲気
、１時間とし、温度を変化させ、得られた石英ガラスを
大気中、 １１５０℃、１時間の熱処理を行った後の石
英ガラスの硬度を表２に示した。ガラスの硬度はビッカ
ース硬度計を用いて荷重２５ｇで測定した。なお、ホッ
トプレスの昇温、降温の速度は２００℃／ｈｒとした。(Examples 1 to 5) Diameter 70 mm 5 Height 70 mm, Vickers hardness 8.8
A piece of 8 GPa quartz glass was set in a hot press carbon mold as shown in FIG. The pressure, atmosphere, and time of hot pressing were 10 MPas Ar atmosphere for 1 hour, and the temperature was varied.The obtained quartz glass was heat-treated in the air at 1150 °C for 1 hour.The hardness of the quartz glass was then determined. It is shown in Table 2. The hardness of the glass was measured using a Vickers hardness meter under a load of 25 g. Note that the rate of temperature increase and temperature decrease in the hot press was 200° C./hr.
表２
以上のガラスはすべて波長が０．１６μｍ〜４．８μｍ
の光を透過し、通常の石英ガラスの透光性と比べて遜色
なかった。Table 2 All of the above glasses have wavelengths of 0.16 μm to 4.8 μm.
of light, and its translucency was comparable to that of ordinary quartz glass.
【発明の効果］
本発明のように石英ガラスを不活性ガス雰囲気内で高温
、高圧でホットプレス処理することにより、（１）初期
形状をほぼ保ったまま
（２）安い製造コストで
（３）短時間で
（４）容易に
（５）透光性に優れた高硬度の石英ガラスが製造出来る
。[Effects of the Invention] By hot-pressing quartz glass at high temperature and high pressure in an inert gas atmosphere as in the present invention, (1) the initial shape is almost maintained (2) the manufacturing cost is low (3) Highly hard quartz glass with excellent translucency can be produced (4) easily and (5) in a short time.
第１図は本発明の高硬度石英ガラスの製造方法の実施状
況の一例を示す概念図である。
■・・・石英ガラス
■・９拳カーボンバンチ
■・・・カーボン押し型
特許出願人 東洋曹達工業株式会社
第 １ 図FIG. 1 is a conceptual diagram showing an example of the implementation status of the method for manufacturing high-hardness quartz glass of the present invention. ■...Quartz glass■・Nine fist carbon bunch■...Carbon stamping mold Patent applicant Toyo Soda Kogyo Co., Ltd. Figure 1
Claims (1)
り１０００℃以上１５００℃未満に加熱し、かつ１０Ｍ
Ｐａ以上に加圧することを特徴とする高硬度石英ガラス
の製造方法。Quartz glass is heated to 1000°C or more and less than 1500°C in an inert gas atmosphere using a hot press, and 10M
A method for producing high-hardness quartz glass, characterized by pressurizing it to a pressure of Pa or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62096167A JP2702478B2 (en) | 1987-04-21 | 1987-04-21 | Manufacturing method of high hardness quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62096167A JP2702478B2 (en) | 1987-04-21 | 1987-04-21 | Manufacturing method of high hardness quartz glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63265835A true JPS63265835A (en) | 1988-11-02 |
| JP2702478B2 JP2702478B2 (en) | 1998-01-21 |
Family
ID=14157776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62096167A Expired - Fee Related JP2702478B2 (en) | 1987-04-21 | 1987-04-21 | Manufacturing method of high hardness quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2702478B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1304313A1 (en) * | 2001-10-22 | 2003-04-23 | Degussa AG | Method for producing ultra-high purity, optical quality, glass articles |
| US7069746B2 (en) | 2001-10-22 | 2006-07-04 | Degussa Ag | Method for producing ultra-high purity, optical quality glass articles |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5734031A (en) * | 1980-08-07 | 1982-02-24 | Toshiba Ceramics Co Ltd | Method and apparatus for decreasing number of bubbles in formed quartz glass |
| JPS5934660A (en) * | 1982-08-21 | 1984-02-25 | Mitsubishi Electric Corp | Semiconductor device |
-
1987
- 1987-04-21 JP JP62096167A patent/JP2702478B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5734031A (en) * | 1980-08-07 | 1982-02-24 | Toshiba Ceramics Co Ltd | Method and apparatus for decreasing number of bubbles in formed quartz glass |
| JPS5934660A (en) * | 1982-08-21 | 1984-02-25 | Mitsubishi Electric Corp | Semiconductor device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1304313A1 (en) * | 2001-10-22 | 2003-04-23 | Degussa AG | Method for producing ultra-high purity, optical quality, glass articles |
| US7069746B2 (en) | 2001-10-22 | 2006-07-04 | Degussa Ag | Method for producing ultra-high purity, optical quality glass articles |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2702478B2 (en) | 1998-01-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |