JP2560354B2 - Defoaming method of quartz glass - Google Patents
Defoaming method of quartz glassInfo
- Publication number
- JP2560354B2 JP2560354B2 JP28840487A JP28840487A JP2560354B2 JP 2560354 B2 JP2560354 B2 JP 2560354B2 JP 28840487 A JP28840487 A JP 28840487A JP 28840487 A JP28840487 A JP 28840487A JP 2560354 B2 JP2560354 B2 JP 2560354B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- glass
- metal
- defoaming
- powder
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Melting And Manufacturing (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、泡を含有する石英ガラスの脱泡方法に関す
るものであり、この石英ガラスは光学用部品（窓，レン
ズ，プリズム等）及びマスク用基板等に使用できる。Description: TECHNICAL FIELD The present invention relates to a method for defoaming quartz glass containing bubbles, which is used for optical parts (windows, lenses, prisms, etc.) and masks. It can be used for substrates.
［従来の技術］ 光学用部品（窓，レンズ，プリズム等）及びマスク用
基板等に使用する石英ガラスインゴットは従来 （１）天然水晶を粉砕し原料粉末とした溶融石英法 （２）四塩化硅素の燃焼による合成石英法 で作製されている。[Prior Art] Conventional quartz glass ingots used for optical parts (windows, lenses, prisms, etc.) and mask substrates are (1) a fused silica method in which natural quartz is crushed into a raw material powder (2) silicon tetrachloride It is made by the synthetic quartz method by burning of.
通常のガラスは、融点が低いため、再溶解をすること
である程度脱泡が可能であるが、石英ガラスの場合、軟
化させるのに1500℃以上が必要な上、石英ガラスの粘性
が高いため、ガスがガラス中に取込まれると容易に除去
できず、それが泡となって残ってしまう。Since ordinary glass has a low melting point, it can be defoamed to some extent by remelting, but in the case of quartz glass, 1500 ° C. or higher is required to soften it, and the viscosity of quartz glass is high. Once the gas is entrapped in the glass it cannot be easily removed and it remains as bubbles.
脱泡方法として、泡を含む石英ガラスを真空溶融する
方法が考えられるが、これは酸化硅素の蒸発が生じる上
に溶融して初期形状が変型してしまい、製品にするため
には再度切出しが必要になり、工程が大幅に増えるため
あまりメリットがない。As a defoaming method, a method of vacuum melting quartz glass containing bubbles is conceivable, but this causes evaporation of silicon oxide and melting and the initial shape is deformed. It is necessary, and there is not much merit because the number of steps increases significantly.
また、特開昭57−34031号公報に報告されている熱間
静水圧プレス（以下、HIPとする）による脱泡は有効な
手段ではあるが、圧力媒体となるガスの混入があり前述
した用途での使用には大きな問題となる。Further, although defoaming by a hot isostatic press (hereinafter referred to as HIP) reported in Japanese Patent Laid-Open No. 57-34031 is an effective means, there is a mixture of a gas serving as a pressure medium and the above-mentioned applications. It becomes a big problem to use it.
現状では、泡の混入している石英ガラスは前に述べた
用途には使用不可能であるため、泡の存在しない部分を
切出して製品としていることから、製品歩留が非常に低
いという問題を抱えている。At present, quartz glass containing bubbles cannot be used for the above-mentioned applications.Therefore, since the product is cut out from the part where no bubbles are present, the product yield is extremely low. I'm holding.
［発明が解決しようとする問題点］ 本発明は従来、泡が存在するために使用されていなか
った石英ガラスを、形状の変化なしに容易に短時間で脱
泡を行い、製品歩留を飛躍的に向上することが出来る石
英ガラスの脱泡方法を提供するものである。[Problems to be Solved by the Invention] In the present invention, silica glass, which has not been used in the past due to the presence of bubbles, is easily defoamed in a short time without changing the shape, and the product yield is increased. The present invention provides a method for defoaming quartz glass that can be improved.
［問題点を解決するための手段及び作用］ 本発明者らは上記問題点を解決するため鋭意検討を重
ねた結果、本発明に到達した。すなわち本発明は、泡を
含む石英ガラスを金属またはガラスで覆い、HIPを使用
し、1200℃以上の温度に加熱し、かつ1MPa以上に加圧す
ることを特徴とする石英ガラスの脱泡方法である。[Means and Actions for Solving Problems] The present inventors have arrived at the present invention as a result of intensive studies to solve the above problems. That is, the present invention is a method for defoaming quartz glass, characterized in that the quartz glass containing bubbles is covered with metal or glass, HIP is used, the temperature is raised to 1200 ° C. or higher, and the pressure is increased to 1 MPa or higher. .
本発明に使用する石英ガラスは、泡を含むものであれ
ばその石英ガラスの製法に制限はなく、いかなる方法で
作製したものでも良い。形状、大きさ等にも制限はなく
ルツボの中に挿入できればいかなる形状でも良いが、あ
らかじめ、ほぼ、製品寸法にされているものが好まし
い。The quartz glass used in the present invention is not limited in the method for producing the quartz glass as long as it contains bubbles, and may be produced by any method. The shape and size are not limited, and any shape may be used as long as it can be inserted into the crucible, but it is preferable that the size of the product is set in advance.
この石英ガラスを金属またはガラスで覆い、HIPを使
用し1200℃以上に加熱し、かつ1MPa以上に加圧して脱泡
する。高圧で処理するため、比較的温度を下げても泡は
流動する。したがって、このときの温度は、1200℃以上
であれば充分であるが、短時間で脱泡するには約1500℃
以上が好ましい。This quartz glass is covered with metal or glass, heated to 1200 ° C. or higher using HIP, and pressurized to 1 MPa or higher to defoam. Since the treatment is performed at a high pressure, the bubbles flow even when the temperature is relatively low. Therefore, the temperature at this time is sufficient if it is 1200 ° C or higher, but about 1500 ° C for defoaming in a short time.
The above is preferable.
圧力は、軟化させておけば相対的に小さくできるが、
少なくとも1MPa以上の圧力で処理する必要がある。The pressure can be made relatively small by softening it,
It is necessary to process at a pressure of at least 1 MPa or higher.
石英ガラスを覆うのに金属を用いる場合、例えばモリ
ブデン，タングステン等の高融点金属で石英ガラスの形
状に近い容器をつくり、その中に該石英ガラスを入れ、
真空下、該金属のふたで密封すればよい。When a metal is used to cover the quartz glass, for example, a container having a shape close to that of the quartz glass is made of a high melting point metal such as molybdenum or tungsten, and the quartz glass is put therein.
It may be sealed with the metal lid under vacuum.
また石英ガラスを用いて覆う場合、そのガラスの種類
には特に限定はないが、ホウケイ酸ガラス，石英ガラス
を用いるのが好ましい。この場合は、一端を閉じたガラ
スチューブに該石英ガラスを入れ、真空下、加熱するこ
とによって、ガラスチューブの他端を閉じればよい。In the case of covering with quartz glass, the kind of the glass is not particularly limited, but it is preferable to use borosilicate glass or quartz glass. In this case, the quartz glass may be placed in a glass tube whose one end is closed and heated under vacuum to close the other end of the glass tube.
これら金属またはガラスの覆いは、該石英ガラスをHI
P処理後、簡単に除去することができる。These metal or glass covers make the quartz glass HI
It can be easily removed after P treatment.
石英ガラスを金属またはガラスで覆う理由は、圧力媒
体としてのガスが石英ガラスに混入すると石英ガラスが
着色したり、歪を生じる恐れがあるため、ガスとの接触
を避ける為である。The reason why the quartz glass is covered with metal or glass is to avoid contact with the gas, because if the gas as the pressure medium is mixed into the quartz glass, the quartz glass may be colored or distorted.
石英ガラスを金属またはガラスで覆ったものの周囲に
粉末を充填し、HIP処理してもよい。粉末は覆った金属
またはガラスと反応しない粉末、例えば炭素,ZrC,SiCな
どの粉末を使用する。また、これらの粉末を充填するこ
とでより完全に初期形状を保つことが出来る。ここで使
用する粉末の粒度は約50μｍ〜5mmが好ましい。5mmを越
えると、流動性のある石英ガラスを脱泡処理前の形状に
保持することが難しく、50μｍ未満では粉末が焼結しす
ぎて強固になりすぎ石英ガラスの取り出しが面倒になる
ためである。これらの約50μｍ〜5mmの粉末は完全には
焼結しないので、石英ガラスの取り出しが比較的容易で
ある。The powder may be filled around the quartz glass covered with metal or glass and subjected to HIP treatment. As the powder, a powder which does not react with the covered metal or glass, for example, powder of carbon, ZrC, SiC or the like is used. Moreover, the initial shape can be more completely maintained by filling these powders. The particle size of the powder used here is preferably about 50 μm to 5 mm. If it exceeds 5 mm, it is difficult to maintain the flowable quartz glass in the shape before defoaming treatment, and if it is less than 50 μm, the powder is sintered too hard and becomes too strong, and it becomes difficult to take out the quartz glass. . Since these powders of about 50 μm to 5 mm are not completely sintered, the quartz glass can be taken out relatively easily.
この粉末充填によってより形状の変化なしで高温処理
することが出来、短時間化が可能となった。By this powder filling, it was possible to perform high temperature treatment without changing the shape, and it was possible to shorten the time.
以上のような脱泡処理を行うための簡便な装置として
本発明ではHIPを用いる。In the present invention, HIP is used as a simple device for performing the above defoaming treatment.
これらの脱泡処理によると、石英ガラス中に含有され
る泡は石英ガラスの流動により徐々に外部へ押出されて
行き、完全に泡は除去される。According to these defoaming treatments, the bubbles contained in the quartz glass are gradually extruded to the outside due to the flow of the quartz glass, and the bubbles are completely removed.
次に、本発明を図面にもとづき説明するが、一例を示
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 described with reference to the drawings, but it is merely an example and the present invention is not limited thereto.
第１図は本発明の実施状況の一例を示す概念図であ
る。泡を含有す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、金属またはガラスで覆い、覆っ
た金属またはガラスと反応しない粉末の中にうめこん
でカーボンルツボにセットし、高温、高圧処理をして
脱泡を行う。FIG. 1 is a conceptual diagram showing an example of the implementation status of the present invention. Quartz glass containing bubbles is processed into a shape close to the product in advance, covered with metal or glass, embedded in powder that does not react with the covered metal or glass, set in a carbon crucible, and treated at high temperature and high pressure. To defoam.
以上のような方法により容易に脱泡を行うことが出来
る。Defoaming can be easily performed by the above method.
［実施例］ 次に、本発明を実施例により更に詳細に説明するが、
一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。EXAMPLES Next, the present invention will be described in more detail with reference to Examples.
However, the present invention is not limited to these examples.
（実施例１） 一辺が50mmの立方体で泡が約100mm3/100mlの泡を含む
石英ガラスを該石英ガラスの形状に近いモリブデン製容
器で覆い、真空下、モリブデン製のふたで密封し、覆と
した。これを第１図に示すようにHIP処理用カーボンル
ツボ内にセットした。この時、充填粉末は炭素粉末（粒
径１〜2mm）を使用した。HIP処理の温度を1200℃、圧力
を60MPa、処理時間を２時間、圧力媒体にArガスを使用
し、昇温、降温の速度を200℃/Hrで、処理をした後、モ
リブデンによる覆いを除去した。その結果、石英ガラス
中に直径が10μｍ以上の泡の存在は、ピンホール法およ
び顕微鏡では、認められず、またArガスの石英ガラスへ
の混入も、EPMA（電子線マイクロアナライザー）では、
認められなかった。(Example 1) side covers the quartz glass containing bubbles cube foam about 100 mm 3/100 ml of 50mm molybdenum steel container close to the shape of the quartz glass, under vacuum, sealed with molybdenum lid, covering And This was set in a carbon crucible for HIP treatment as shown in FIG. At this time, as the filling powder, carbon powder (particle diameter 1 to 2 mm) was used. HIP treatment temperature is 1200 ° C, pressure is 60MPa, treatment time is 2 hours, Ar gas is used as pressure medium, and the temperature rising / falling rate is 200 ° C / Hr. After treatment, molybdenum cover is removed. did. As a result, the presence of bubbles having a diameter of 10 μm or more in the quartz glass was not recognized by the pinhole method or the microscope, and the mixing of Ar gas into the quartz glass was confirmed by EPMA (electron beam microanalyzer).
I was not able to admit.
［発明の効果］ 本発明のように泡を含む石英ガラスを金属またはガラ
スで覆い、HIPを使用し、1200℃以上に加熱し、かつ1MP
a以上に加圧することにより、 ・初期形状を変形させず ・短時間に ・ガスの混入なしに ・石英ガラス中に含有する泡を完全に除去でき ・保留を飛躍的に向上できる。[Effect of the invention] As in the present invention, the quartz glass containing bubbles is covered with metal or glass, HIP is used, and the temperature is raised to 1200 ° C or higher, and 1MP
By applying more than a pressure, the initial shape is not deformed. In a short time. No gas is mixed. Bubbles contained in the quartz glass can be completely removed. Retention can be dramatically improved.
第１図は、本発明の実施状況の一例を示す概念図であ
る。 ……泡を含む石英ガラス ……金属またはガラス ……粉末 ……カーボンルツボFIG. 1 is a conceptual diagram showing an example of the implementation status of the present invention. ...... Fused quartz glass ...... Metal or glass ...... Powder ...... Carbon crucible
Claims (3)
覆い、熱間静水圧プレスを使用し、1200℃以上に加熱
し、かつ1MPa以上に加圧することを特徴とする石英ガラ
スの脱泡方法。1. A method of defoaming quartz glass, characterized in that the quartz glass containing bubbles is covered with metal or glass, heated to 1200 ° C. or higher, and pressurized to 1 MPa or higher using a hot isostatic press. .
方法において、石英ガラスを金属またはガラスで覆った
ものの周囲に覆った金属またはガラスと反応しない粉末
を充填する石英ガラスの脱泡方法。2. The defoaming method for quartz glass according to claim 1, wherein the quartz glass is covered with a metal or glass, and the quartz glass is defoamed with a powder which does not react with the metal or glass. Method.
方法において、石英ガラスを金属またはガラスで覆った
ものの周囲に充填する粉末の粒度が、50μｍ〜5mmであ
る石英ガラスの脱泡方法。3. The defoaming method of quartz glass according to claim 2, wherein the particle size of the powder filled around the quartz glass covered with metal or glass is 50 μm to 5 mm. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28840487A JP2560354B2 (en) | 1987-11-17 | 1987-11-17 | Defoaming method of quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28840487A JP2560354B2 (en) | 1987-11-17 | 1987-11-17 | Defoaming method of quartz glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01131032A JPH01131032A (en) | 1989-05-23 |
| JP2560354B2 true JP2560354B2 (en) | 1996-12-04 |
Family
ID=17729770
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28840487A Expired - Fee Related JP2560354B2 (en) | 1987-11-17 | 1987-11-17 | Defoaming method of quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2560354B2 (en) |
-
1987
- 1987-11-17 JP JP28840487A patent/JP2560354B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01131032A (en) | 1989-05-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |