JPH02199037A - Production of quartz glass - Google Patents
Production of quartz glassInfo
- Publication number
- JPH02199037A JPH02199037A JP1918089A JP1918089A JPH02199037A JP H02199037 A JPH02199037 A JP H02199037A JP 1918089 A JP1918089 A JP 1918089A JP 1918089 A JP1918089 A JP 1918089A JP H02199037 A JPH02199037 A JP H02199037A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- quartz glass
- give
- gel
- silica gel
- 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 66
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000000843 powder Substances 0.000 claims abstract description 34
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 26
- -1 alkyl silicate Chemical compound 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 239000000741 silica gel Substances 0.000 claims abstract description 7
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 15
- 239000000499 gel Substances 0.000 abstract description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 239000011240 wet gel Substances 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract 2
- 238000010304 firing Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000010453 quartz Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000012643 polycondensation polymerization Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は石英ガラスの製造方法、特にはその０８基濃度
がコントロールされるので、エキシマレーザ−用などに
有用とされる石英ガラスの製造方法に関するものである
。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing quartz glass, and in particular, a method for producing quartz glass that is useful for excimer lasers, etc. because the concentration of 08 groups is controlled. It is related to.
［従来の技術］
四塩化けい素などのハロゲン化けい素を酸水素火炎中で
火炎加水分解させ、発生したシリカを担体上に堆積させ
て得た多孔質シリカ母材を加熱溶融してガラス化すると
いう方法で作られた合成石英ガラスは高純度であること
から各種用途に多用されており、これはエキシマレーザ
−用の光学用ガラス材料としても使用されている。[Prior art] A porous silica base material obtained by flame hydrolyzing silicon halide such as silicon tetrachloride in an oxyhydrogen flame and depositing the generated silica on a carrier is heated and melted to vitrify it. Synthetic quartz glass produced by this method is of high purity and is widely used for various purposes, and is also used as an optical glass material for excimer lasers.
しかし、この合成石英ガラスは始発材として四塩化けい
素などのハロゲン化けい素が使用されるために多量のハ
ロゲン元素を含有するものであるため、これにはハロゲ
ン元素を含有しないアルコキシシランを加水分解して、
シリカゾルを作り、これを脱水乾燥して得た湿式ゲルを
焼成ガラス化する、いわゆるゾル−ゲル法で作られたも
のを使用することも試みられている。However, this synthetic quartz glass contains a large amount of halogen elements because silicon halides such as silicon tetrachloride are used as the starting material. Take it apart and
Attempts have also been made to use a so-called sol-gel method, in which a silica sol is prepared, the resulting wet gel is fired and vitrified.
［解決されるべき課題］
しかし、特にエキシマレーザ−用に用いられる光学用石
英ガラスについてはレーザーの出力増加に伴なって耐レ
ーザー性が不足していてこの対策が問題となっており、
これには合成石英ガラスに含有されているＯＨ基濃度が
関係をもっていることが判っているが、上記した火炎加
水分解法、ゾル−ゲル法で得られた合成石英ガラスはそ
のＯＨ基濃度が不均一でかつその濃度範囲も一定でない
ために、このＯＨ基濃度が耐レーザー性にどれだけ関係
するかも正確には不明となっており、ＯＨ基量の制御さ
れた石英ガラスの提供が求められている。[Problems to be Solved] However, optical quartz glass used especially for excimer lasers lacks laser resistance as the laser output increases, and this problem has become a problem.
It is known that this is related to the concentration of OH groups contained in synthetic quartz glass, but synthetic silica glass obtained by the above-mentioned flame hydrolysis method or sol-gel method has an OH group concentration of Since it is uniform and its concentration range is not constant, it is unclear exactly how much this OH group concentration is related to laser resistance, and there is a need to provide quartz glass with a controlled amount of OH groups. There is.
［課題を解決するための手段］
本発明はこのように要求に応えることのできる制御され
たＯＨ基濃度をもつ合成石英ガラスの製造方法に関する
ものであり、これはアルキルシリケートを加水分解し、
縮重合させ、乾燥して得たシリカゲルを粉砕したのち、
通気性を保った炉内で焼成して得た石英ガラス粉を分級
し、つしＡで各分級粉別に例えば酸水素炎で分別溶融し
てＯＨ基濃度の制御された石英ガラスを得ることを特徴
とするものである。[Means for Solving the Problems] The present invention relates to a method for producing synthetic quartz glass having a controlled OH group concentration that can meet the above requirements, which involves hydrolyzing an alkyl silicate,
After pulverizing the silica gel obtained by condensation polymerization and drying,
The quartz glass powder obtained by firing in a furnace that maintains air permeability is classified, and each classified powder is melted separately with an oxyhydrogen flame, for example, to obtain quartz glass with a controlled OH group concentration. This is a characteristic feature.
すなわち、本発明者らはＯＨ基濃度の制御された石英ガ
ラスの製造方法について種々検討した結果、エチルシリ
ケートなどのようなアルキルシリケートを加水分解し、
縮重合させ、乾燥してゲルとしたのち粉砕し、焼成して
から少なくとも３分別以上になるように分級し、この各
分級粉末を各個に酸水素火炎で溶融し、得られた石英ガ
ラスのＯＨ基濃度をしらべたところ、このＯＨ基濃度は
この分級した粉末の粒径と相関があり、かつプラズマ溶
融品と異なり、得られた溶融体における塩素濃度が１
ｐｐｍ以下となるため、目的とする制御されたＯＨ基濃
度をもつ石英ガラスを得るためにはある特定の粒径をも
つ石英ガラス粉末をガラス化すればよいということを確
認して本発明を完成させた。That is, as a result of various studies by the present inventors regarding the manufacturing method of quartz glass with a controlled OH group concentration, the present inventors found that a method for producing quartz glass with a controlled OH group concentration was obtained by hydrolyzing an alkyl silicate such as ethyl silicate,
Condensation polymerization, drying to form a gel, pulverization, firing, and classification into at least 3 fractions, each of the classified powders is individually melted with an oxyhydrogen flame, and the OH of the obtained quartz glass is When we investigated the group concentration, we found that the OH group concentration was correlated with the particle size of the classified powder, and unlike plasma melted products, the chlorine concentration in the obtained melt was 1.
ppm or less, and completed the present invention by confirming that in order to obtain quartz glass with the desired controlled OH group concentration, it was sufficient to vitrify quartz glass powder with a specific particle size. I let it happen.
以下にこれをさらに詳述する。This will be explained in further detail below.
［作 用］
本発明による石英ガラスの製造はゾル−ゲル法によって
行なわれる。[Function] The quartz glass according to the present invention is produced by a sol-gel method.
したがって、本発明の方法はアルキルシリケートが始発
材とされるが、これはエチルシリケート、プロピルシリ
ケートなどのようなものとすればよい。Therefore, although the method of the present invention uses an alkyl silicate as the starting material, it may be ethyl silicate, propyl silicate, or the like.
このアルキルシリケートの加水分解は常法によってアル
キルシリケートにアルコール、水、塩酸のような酸性触
媒、またはアンモニアのような塩基性触媒を適当量加え
て加水分解すればよく、この加水分解で発生したシリカ
ゲルは縮重合させると塊状の、好ましくは径が２〜４ｍ
ｍの粒状物となる。This alkyl silicate can be hydrolyzed by a conventional method by adding an appropriate amount of alcohol, water, an acid catalyst such as hydrochloric acid, or a basic catalyst such as ammonia to the alkyl silicate, and the silica gel generated by this hydrolysis can be hydrolyzed. When subjected to condensation polymerization, it becomes a lump, preferably with a diameter of 2 to 4 m.
m granules.
この塊状物はついで加温し、ゲル化させて湿式ゲルとし
たのち、クリーンオーブンなどでよく乾燥してここに残
留しているアルコール分を除去して乾燥ゲルとし、つい
でロールミルなどを用いて粒径が１■以下に粉砕するの
であるが、この粉砕は粒度分布が５ＯＮ１，０００μｍ
１好ましくは１００〜７００μｍの範囲となるようにす
ればよく、好ましくはこの分布が平坦なものとなるよう
にすることがよい。This lump is then heated and gelled to form a wet gel, and then thoroughly dried in a clean oven to remove the remaining alcohol content to form a dry gel, and then granulated using a roll mill or the like. The particle size distribution of this grinding is 5ON1,000μm.
1. Preferably, the thickness may be in the range of 100 to 700 μm, and preferably, the distribution may be flat.
このようにして得られた乾燥ゲルは焼成して脱水するの
であるが、この焼成はこのゲルを石英ガラス容器に入れ
て石英炉芯管をもつ電気炉中で行なわせればよく、これ
は脱水ということから窒素ガスまたは酸素ガスのような
気流中で行なわせることが必要とされる。また、この焼
成は８００〜１゜２００℃で行えばよいが、最初から１
，２００ を以上の温度で焼成するとこのゲルが発泡し
て稠密な粉末が得られなくなるので、これは昇温速度を
ｔｏ’ｅ ／分として８００℃付近から数段階に分けて
数時間づつ焼成するようにすることがよく、好ましくは
窒素ガスまたは酸素ガスを１℃／分以上の量で流しなが
ら８００℃、 １，０００℃、 １，２００℃でそれぞ
れ５時間づつ焼成することがよいが、この焼成によって
ゲルは石英ガラス粉末とされる。The dried gel obtained in this way is dehydrated by firing, but this firing can be done by placing the gel in a quartz glass container and placing it in an electric furnace equipped with a quartz hearth tube, which is called dehydration. Therefore, it is necessary to carry out the process in a gas flow such as nitrogen gas or oxygen gas. Also, this firing can be carried out at 800-1°200°C, but
, 200, the gel will foam and it will not be possible to obtain a dense powder, so the heating rate is set to 800°C and the firing is divided into several stages for several hours at a time. It is preferable to bake at 800°C, 1,000°C, and 1,200°C for 5 hours each while flowing nitrogen gas or oxygen gas at a rate of 1°C/min or more. The gel is turned into quartz glass powder by firing.
なお、一般に原料アルキルシリケートを加水分解させて
シリカゲルを得る製造工程には塩素が含まれてくる問題
点があるが、本発明によれば焼成の工程が必須の要件と
されており、この焼成工程で塩素が除かれるので、上記
した塩素が入り込んでくるという問題点は解消され、得
られる石英ガラスへの塩素の混入が極力避けられるとい
う利点がある。Generally, there is a problem in that chlorine is included in the production process of hydrolyzing raw material alkyl silicate to obtain silica gel, but according to the present invention, the calcination process is an essential requirement. Since chlorine is removed, the above-mentioned problem of chlorine intrusion is solved, and there is an advantage that contamination of the resulting quartz glass with chlorine can be avoided as much as possible.
本発明の方法はこの石英ガラス粉末を分級し、この分級
された石英ガラス粉末を分級相別に分別溶融して石英ガ
ラスを得るのであるが、この分級は汚染防止のために、
ナイロンやテフロンなどのような合成樹脂製スクリーン
を用いて行なうことがよく、これはＪＩＳ標準篩で目の
開きが１０５〜７１０μｍの範囲となるように、好まし
くは１０５μｍ、１２５ μｍ、１４９ μｍ、１７７
μｍ、２１０μｍ、 ２５０ ｐｍ、 ２９７ ｐｍ
、 ３５０ ｐｍ、 ４２０μｍ、５００μｍ、５９０
μｍ、７１０μｍなどのような全ての篩を用いて行なう
ことが好ましい。分別溶融はこの谷筋で分別された石英
ガラス粉を各篩毎に採取し、これを酸素、水素の流量を
一定にした石英製の酸水素火炎バーナーからの火炎で溶
融させればよく、これによれば泡のない石英ガラスイン
ゴットが得られるが、この石英ガラスの０）１温源度を
しらべたところ、このＯＨ基濃度は溶融する前の石英ガ
ラス粉末の粒径と相関をもつもので、これは第１図に示
したように石英ガラス粉末が１０５μｍで最低となり、
これより小さくなるか大きくなるとＯＨ基濃度が増加す
るということが確認されたので、目的とするＯＨ基濃度
をもつ合成石英を得るにはこれに相当する粒径をもつ石
英ガラス粉末を溶融すればよい。In the method of the present invention, this quartz glass powder is classified, and the classified quartz glass powder is melted according to the classified phase to obtain quartz glass.This classification is performed to prevent contamination.
This is often carried out using a screen made of synthetic resin such as nylon or Teflon, and this is preferably a JIS standard sieve with a mesh size in the range of 105 to 710 μm, preferably 105 μm, 125 μm, 149 μm, or 177 μm.
μm, 210 μm, 250 pm, 297 pm
, 350 pm, 420 μm, 500 μm, 590
Preferably, all sieves such as .mu.m, 710 .mu.m etc. are used. Separate melting can be carried out by collecting the quartz glass powder separated by the valleys from each sieve and melting it with a flame from a quartz oxyhydrogen flame burner with a constant flow rate of oxygen and hydrogen. According to the method, a bubble-free quartz glass ingot can be obtained, but when the 0)1 temperature source temperature of this quartz glass was investigated, it was found that this OH group concentration has a correlation with the particle size of the quartz glass powder before melting. , as shown in Figure 1, the quartz glass powder reaches its minimum at 105 μm.
It has been confirmed that the OH group concentration increases when the particle size becomes smaller or larger than this, so in order to obtain synthetic quartz with the desired OH group concentration, it is necessary to melt silica glass powder with a particle size corresponding to this. good.
本発明の方法によるＯＨ基濃度の制御された石英ガラス
の製造は上記したようにゾル−ゲル法で得られた乾燥ゲ
ルを粉砕したのち、焼成、分級し、この篩分けで得られ
た石英ガラスを分別溶融するのであるが、希望するＯＨ
基温源をもつ石英ガラスを得るためにはこの分級を少な
くとも３フラクシヨン以上とすることが望ましい。分級
が２フラクシヨンもしくは末分級であると粗いガラス粉
末と細かいガラス粉末が混合して正確なＯＨ基濃度のコ
ントロールが難しくなるので、この分級は少なくとも３
フラクシヨン、好ましくは前記したＪＩＳ基準基準金て
用いることがよく、分別溶融で希望するＯＨ基濃度を得
るときには１段階上または１段階下の粉を配合するとこ
れが容易になり、これによれば希望するＯＨ基濃度に対
して±１０にの範囲で制御することが可能となる。ここ
に使用される石英ガラス粉末は粒径が７００μｍ以上の
もの、例えば７００−１．Ｏｎμｍのものはここに含有
されている水分が多く、したがって溶融するとＯＨ基濃
度が１．０００ｐｐｍ以上のものが得られるけれども、
このものは泡が多く発生し、光学材料には適しなくなる
ので、この石英ガラス粉末は粒径が７００μｍ以下のも
のとすることがよい。The production of quartz glass with a controlled OH group concentration by the method of the present invention involves pulverizing the dry gel obtained by the sol-gel method as described above, followed by firing and classifying the silica glass. The desired OH
In order to obtain quartz glass having a base temperature source, it is desirable that this classification be at least 3 fractions or more. If the classification is 2 fractions or final classification, coarse glass powder and fine glass powder will mix and it will be difficult to control the OH group concentration accurately, so this classification should be at least 3 fractions.
Fractions, preferably the JIS standard reference metals described above, are often used, and when obtaining the desired OH group concentration by fractional melting, it is easier to achieve the desired OH group concentration by blending a powder one step higher or one step lower. It becomes possible to control the OH group concentration within a range of ±10. The quartz glass powder used here has a particle size of 700 μm or more, for example, 700 μm or more. On μm ones contain a lot of water, so when melted, you can obtain one with an OH group concentration of 1.000 ppm or more.
Since this powder generates a lot of bubbles and is not suitable as an optical material, it is preferable that the particle size of the quartz glass powder be 700 μm or less.
なお、このようにして得られた石英ガラスは始発材が蒸
留精製されたアルキルシリケートであることから、ハロ
ゲン原子を含有しない高純度のものとなるし、ＯＨ基濃
度も制御されたものとなるので、各種用途に広く使用す
ることができるが、これは特には耐レーザー性研究のた
めのエキシマレーザ−用光学材料として利用することが
できる。In addition, since the starting material of the quartz glass obtained in this way is an alkyl silicate purified by distillation, it is highly pure and does not contain halogen atoms, and the OH group concentration is also controlled. , can be widely used for various applications, and in particular, it can be used as an optical material for excimer lasers for research on laser resistance.
［実施例］
つぎに本発明の実施例をあげるが、例中の部は重量部を
示したものである。[Example] Next, Examples of the present invention will be given, and parts in the examples indicate parts by weight.
実施例
２１のガラス製反応器にエチルシリケート１部、蒸留水
５部および０．ＩＮの塩酸５部を仕込み、攪拌しながら
エチルシリケートを加水分解させて粒状シリカゾルを生
成させた。Into the glass reactor of Example 21 were added 1 part of ethyl silicate, 5 parts of distilled water, and 0.5 parts of distilled water. 5 parts of IN hydrochloric acid was charged, and ethyl silicate was hydrolyzed while stirring to produce a granular silica sol.
ついでこのゾルを６０℃に加温して湿式ゲルとし、フリ
ーオーブンで２００℃で１０時間乾燥してアルコール分
を除去し、これをロールミルで粉砕して粒径が１０６〜
１，０００μｍの範囲の粉末とした。Next, this sol was heated to 60°C to form a wet gel, dried in a free oven at 200°C for 10 hours to remove the alcohol content, and ground in a roll mill to obtain particles with a particle size of 106 to 100°C.
It was made into a powder in the range of 1,000 μm.
つぎに、この粉末を石英ビーカーに入れ、石英炉芯管に
挿入し、これを窒素ガスが１９７分で流通している電気
炉中で昇温速度１０℃／分を保ちながら８００℃で５時
間、１ 、０００℃で５時間、１，２００℃で５時間焼
成したのち、冷却し、ＪＩＳ標準篩の目開きが１０５
ｐｍ、 １５０ μｍ、 ２１２ ｐｍ、 ３００μｍ
、５００μｍ、７００μｍであるナイロン族のスクリー
ンをもつ篩を用いて分級、篩別し、得られた粉末を酸素
ガス流量を２０１／分、水素ガス流量を５０ＩｔＺ分と
一定とした酸水素火炎バーナーを用いて溶融して各粒径
毎に３個の石英ガラスインゴットを作り、これらのＯＨ
基濃度をしらべたところ、第１表に示したとおりの結果
が得られた。Next, this powder was placed in a quartz beaker, inserted into a quartz furnace core tube, and heated to 800°C for 5 hours while maintaining a heating rate of 10°C/min in an electric furnace in which nitrogen gas was circulated every 197 minutes. After baking at 1,000℃ for 5 hours and 1,200℃ for 5 hours, it was cooled and the opening of the JIS standard sieve was 105.
pm, 150 μm, 212 pm, 300 μm
, 500 μm, and 700 μm using a sieve with a nylon screen, and the resulting powder was heated using an oxyhydrogen flame burner with a constant oxygen gas flow rate of 201/min and hydrogen gas flow rate of 50 ItZ min. These OH
When the base concentration was investigated, the results shown in Table 1 were obtained.
第
表
（ＯＨ基濃度ｐｐｍ）
比較例
実施例と同様にしてエチルシリケートを加水分解させ、
アルコール除去後、ロールミルで粉′砕して１０６μ■
〜１，０００μＩの範囲の粉末とし、同様の焼成を行い
、得られた石英ガラス粉末をＪＩＳ ｉ車重の目開きが
３００μＩのもので分級、篩別し、得られた粉末を酸水
素火炎バーナーで溶融し、各粒径毎に３個の石英ガラス
インゴットを作り、す、これらのＯＨ基濃度をしらべた
ところ、第２表に示したとおりの結果が得られ、この場
合には希望するＯＨ基濃度の石英ガラスの製造が困難で
あることが確認された。Table (OH group concentration ppm) Comparative Example Ethyl silicate was hydrolyzed in the same manner as in the example,
After removing alcohol, crush with a roll mill to 106μ■
A powder in the range of ~1,000 μI was prepared and fired in the same manner. The resulting quartz glass powder was classified and sieved using a JIS i vehicle weight aperture of 300 μI, and the resulting powder was heated in an oxyhydrogen flame burner. When three quartz glass ingots were made for each particle size and their OH group concentrations were examined, the results shown in Table 2 were obtained, and in this case, the desired OH It was confirmed that it is difficult to manufacture silica glass with a base concentration.
第 ２ 表 （ＯＨ基濃度ｐｐｍ）分けされた石英
ガラス粉末の粒径によって定まるので、制御されたＯＨ
基濃度をもつ石英ガラスを容易に、かつ安価に得ること
ができるという有利性が与えられる。Table 2 (OH group concentration ppm) Since it is determined by the particle size of the divided silica glass powder, the controlled OH
The advantage is that quartz glass with a base concentration can be obtained easily and inexpensively.
【図面の簡単な説明】
第１図は石英ガラス粉末の粒径とこれを溶融して得た石
英ガラスインゴットのＯＨ基濃度との関係を示したグラ
フである。
［発明の効果］BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the relationship between the particle size of quartz glass powder and the OH group concentration of a quartz glass ingot obtained by melting it. [Effect of the invention]
Claims (1)
シリカゲルを粉砕し、焼成したのち分級し、ついで各分
級粉別に溶融してＯＨ基濃度の制御された石英ガラスを
得ることを特徴とする石英ガラスの製造方法。 ２、前記の溶融手段が酸水素火炎加熱である請求項１に
記載の石英ガラスの製造方法。 ３、前記の分級が少なくとも３分別である請求項１に記
載の石英ガラスの製造方法。 ４、得られた石英ガラスの塩素含有量が１ｐｐｍ以下で
ある請求項１に記載の石英ガラスの製造方法。[Scope of Claims] 1. Silica gel obtained by hydrolyzing and polycondensing an alkyl silicate is crushed, fired and classified, and then each classified powder is melted to produce quartz glass with a controlled OH group concentration. A method for producing quartz glass characterized by obtaining. 2. The method for producing quartz glass according to claim 1, wherein the melting means is oxyhydrogen flame heating. 3. The method for producing quartz glass according to claim 1, wherein the classification is at least three classifications. 4. The method for producing quartz glass according to claim 1, wherein the chlorine content of the obtained quartz glass is 1 ppm or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1019180A JP2780799B2 (en) | 1989-01-27 | 1989-01-27 | Manufacturing method of quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1019180A JP2780799B2 (en) | 1989-01-27 | 1989-01-27 | Manufacturing method of quartz glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02199037A true JPH02199037A (en) | 1990-08-07 |
| JP2780799B2 JP2780799B2 (en) | 1998-07-30 |
Family
ID=11992146
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1019180A Expired - Fee Related JP2780799B2 (en) | 1989-01-27 | 1989-01-27 | Manufacturing method of quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2780799B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0803469A1 (en) * | 1995-01-12 | 1997-10-29 | Mitsubishi Chemical Corporation | Silica gel, synthetic quartz glass powder, quartz glass molding, and processes for producing these |
| JP2012508687A (en) * | 2008-11-13 | 2012-04-12 | コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ | Solar receiver used in solar energy concentrator |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6221708A (en) * | 1985-07-17 | 1987-01-30 | ヘレウス・クアルツシユメルツエ・ゲゼルシヤフト・ミツト・ベシユレンクタ−・ハフツング | Manufacture of products from granular synthetic high purity silicon dioxide |
-
1989
- 1989-01-27 JP JP1019180A patent/JP2780799B2/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6221708A (en) * | 1985-07-17 | 1987-01-30 | ヘレウス・クアルツシユメルツエ・ゲゼルシヤフト・ミツト・ベシユレンクタ−・ハフツング | Manufacture of products from granular synthetic high purity silicon dioxide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0803469A1 (en) * | 1995-01-12 | 1997-10-29 | Mitsubishi Chemical Corporation | Silica gel, synthetic quartz glass powder, quartz glass molding, and processes for producing these |
| EP0803469A4 (en) * | 1995-01-12 | 1997-11-19 | ||
| JP2012508687A (en) * | 2008-11-13 | 2012-04-12 | コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ | Solar receiver used in solar energy concentrator |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2780799B2 (en) | 1998-07-30 |
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