JPS58185443A - Preparation of quartz glass powder - Google Patents
Preparation of quartz glass powderInfo
- Publication number
- JPS58185443A JPS58185443A JP6813782A JP6813782A JPS58185443A JP S58185443 A JPS58185443 A JP S58185443A JP 6813782 A JP6813782 A JP 6813782A JP 6813782 A JP6813782 A JP 6813782A JP S58185443 A JPS58185443 A JP S58185443A
- Authority
- JP
- Japan
- Prior art keywords
- water
- quartz glass
- glass powder
- gel
- vol
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/106—Forming solid beads by chemical vapour deposition; by liquid phase reaction
- C03B19/1065—Forming solid beads by chemical vapour deposition; by liquid phase reaction by liquid phase reactions, e.g. by means of a gel phase
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
本発Ｉ＃は石英ガラス粉末の製造法の改良に関する。さ
らに−しくは、主として＾わゆる多成分系オプティカル
ファイバーｌ１ｉｉｉＩｉ用の基幹＃科％時に元通偏向
けのオプテイ）ル７ア、づバー用として高純度の石英ガ
ラス粉末並びに半導体素子の封止材用光Ｉ１４物として
の石英ガラス粉末を高収率で製造することを可能ならし
める石英ガラス粉末の製造法ｔこ関する。DETAILED DESCRIPTION OF THE INVENTION The present invention I# relates to an improvement in the manufacturing method of quartz glass powder. Furthermore, we mainly use high-purity quartz glass powder for so-called multi-component optical fibers, optical fibers for optical fibers, and encapsulating materials for semiconductor devices. The present invention relates to a method for producing quartz glass powder that makes it possible to produce quartz glass powder as a product at a high yield.
オプティカルファイバーは石英ガラス粉末と酸化ホウ素
、炭酸ソーダ等を混合熔融してホウ珪酸ガラス等の一体
とし、二重のルツボから相１１に尚い尤屈折率を呈する
組成のガラスが中心軸（コア）に位＋１するように、二
種の組成のガラス一体を同軸状に引き出してＭＥする。Optical fibers are made by mixing and melting quartz glass powder, boron oxide, soda carbonate, etc. to form a single body such as borosilicate glass, and the glass having a composition that exhibits a typical refractive index of phase 11 from a double crucible forms the central axis (core). Two pieces of glass with different compositions are pulled out coaxially and ME is performed so that the position increases by +1.
石英ガラスとしては４移址楓か不純物として含まれる場
合ＶｃＦｉ光吸収を惹起するため、高純度であることが
望まれまた曲の成分との混合上粉粒体であることｆ：Ｊ
Ｗ！する。As quartz glass, if it is included as an impurity, it will cause VcFi light absorption, so it is desirable to have high purity, and it must be a granular material when mixed with the components of the song f: J
W! do.
一方、半４捧累子の封止用としては例えばエボキンｍ脂
中に石英ガラス扮ｔ−混ぜ込んだ複合体が用いられるが
、ｄ年素子の嶋密度化に伴い、在米の石英ガラス粉中に
混在すると考えられるウラン。On the other hand, for the sealing of half-fourth graders, for example, a composite of quartz glass mixed with Evokin resin is used. Uranium is thought to be mixed in.
トリウム等からの放射−が素子の作動に支障をきたすこ
とが明らかになり、高純度の石英ガラス粉末が要望され
ている。It has become clear that radiation from thorium and the like interferes with the operation of devices, and there is a demand for high-purity silica glass powder.
さらに、半導体単結晶の高品質化のため高＃１ｌＩＩの
石英ガラスルツボが必要となっており、高純度の原料粉
末が要望されている。従来１石英ガラス粉末としては天
然水晶を粉砕したものがあるが。Furthermore, in order to improve the quality of semiconductor single crystals, a quartz glass crucible with a high #1lII is required, and a raw material powder with high purity is desired. Conventionally, 1 quartz glass powder is made by crushing natural quartz.
天然水晶にはもともと？！ｒ１１の不純物が含まれてお
り、酸洗等の方法では不４４物の除去が出来ないばかり
でなく、＃砕工根でさらに不純−の混入がまぬかれない
ため、前記のごとき高純ＦＸ’ｔ＊する目的の場合には
不適当であるー
一万、常法としては知られていなかが、四塩化珪素の酸
水素炎酸化４＃釦より製造される高４４直の石英ガラス
塊を粉砕して粉体を得ることも考えられるが、粉砕に伴
う汚染のため、高純度品が得られない上、粉砕により必
然的に生成する微粉末が粉砕ならびにハンドリングの通
根でダストとして角数し、環境衛生上大きな問題となる
。What does natural crystal have originally? ! It contains impurities of R11, and not only can impurities not be removed by methods such as pickling, but also impurities cannot be removed by crushing, so high purity FX such as the one described above cannot be used. It is unsuitable for the purpose of 't* - 10,000, although it is not known as a conventional method, a quartz glass block with a height of 44 straight is manufactured from oxyhydrogen flame oxidation of silicon tetrachloride. It is possible to obtain powder by grinding, but it is not possible to obtain a high-purity product due to the contamination that accompanies grinding, and the fine powder that is inevitably generated by grinding is crushed as dust during grinding and handling. This poses a major environmental health problem.
さらに、４溜等による高純度化の可能な珪酸エステルの
加水分解により得られるゲルの塊を砕いて焼成する方法
も試みたが、°ダーストの角数が甚しく実用的でになか
った。Furthermore, a method of crushing and firing a gel mass obtained by hydrolyzing a silicate ester, which can be highly purified using a four-distillation method, was also attempted, but the number of squares of the dust was too large to be practical.
このように１問題の多い粉砕工程を経由することなく、
尚純度の石英ガラス粉末を製造する新規なり法として。In this way, without going through the problematic grinding process,
As a new method to produce high purity quartz glass powder.
＋１１ 珪酸エチルに所定範囲量の水と触媒を加えて
加熱しなから激しく攪拌して粉粒状のゲルｔ′−［威さ
せ、この粉粒状グルｔ−ｍ成する方法。+11 A method of adding a predetermined amount of water and a catalyst to ethyl silicate, heating and stirring vigorously to form a powdery gel t'-[t-m].
（２） ｔ！：酸エステルと所定範囲量の水と所定量
以ドのアルコールとの混合溶液をドデカン等の皺混台Ｓ
漱と実簀的に相溶しない分散媒中に撹拌等の操作によっ
て、細粒のｇ滴として懸濁させてゲル化し、舟られた粉
粒状ゲルを焼成する方法、
が提楽されているが、（１）の方法では使用した珪酸エ
チルの３０ ％に＆ぶ盪が該粉状ゲルの生成反応後の母
液中にｆＡ留し、該母液中の刷生エチルアルコールから
分離、回収しなければならない癩点が残されており、ま
た（２）の方法ではハンドリングロスｔ−砿けば使用し
た珪酸エステルはほとんど全量が石英ガラス粉氷となる
筈であり、実際Ｋ１４い収率が優られているが、多量の
分散媒を使用しなければならない欠点がある。(2) t! : A mixed solution of an acid ester, a predetermined amount of water, and a predetermined amount of alcohol is mixed with dodecane, etc.
A method has been proposed in which fine particles of g droplets are suspended in a dispersion medium that is practically incompatible with sodium to form a gel, and the suspended powdery gel is fired. In method (1), 30% of the ethyl silicate used must be distilled into the mother liquor after the reaction to form the powdered gel, and must be separated and recovered from the raw ethyl alcohol in the mother liquor. In addition, in method (2), almost all of the silicate ester used would have turned into quartz glass powder ice if the handling loss had occurred, so the yield of K14 was actually excellent. However, it has the disadvantage that a large amount of dispersion medium must be used.
さらに１両方法ともに粉末ゲルの生成に長時間を要し、
実際上回分操作を採用せざるを慢ず、従って生産性に不
満が残されている。Furthermore, both methods require a long time to produce powder gel;
In reality, they have no choice but to adopt fractional operations, and as a result, productivity remains unsatisfactory.
本発明者らは上記の従来技術の欠点を解決し、問題の多
い粉砕工程を必要とすることなく、高純度の石英ガラス
粉末を高収率でＩｌｉ！造することｔ可能ならしめる石
英ガラス粉末のＩ１１！造法を提供すべく検討した結果
、珪酸エステルと水単味とよりなる混合溶液、あるいは
珪酸エステルと水とアルコールとよりなる混合溶液を強
熱すると、温ＫＫよる反応速度の増大と該混合溶液中の
アルコールないし水の蒸発促進とくより、Ｍ混合溶液の
ゲル化が急速く進み、特に？ｌｌ１合浴液を噴繕状にし
た場合（は表面積の増大により両効果かさらに顕着くな
ることを見出し、本発明に到達した。The present inventors have solved the above-mentioned drawbacks of the prior art and produced high-purity quartz glass powder in high yield without the need for a problematic grinding process. I11 of quartz glass powder that makes it possible to produce! As a result of studying to provide a manufacturing method, it was found that when a mixed solution of a silicate ester and water alone, or a mixed solution of a silicate ester, water, and alcohol is ignited, the reaction rate increases due to warm KK and the mixed solution Due to the promotion of evaporation of the alcohol or water in the mixture, the gelation of the M mixed solution progresses rapidly. The present invention was achieved by discovering that when the ll1 combined bathing liquid is made into a foam, both effects become even more pronounced due to an increase in the surface area.
すなわち１本発明の要旨とするところは％珪酸エステル
１００容量と水５０〜４００容瞳とよりなる混合溶敵會
、温１ｆ９°０°Ｃ以上の気体中に噴霧して粉状ケルを
生成させ、該粉状ゲルを分離、焼成することを特値とす
る石英ガラス粉末の製造法。That is, 1. The gist of the present invention is to form a powdery Kel by spraying it into a gas having a temperature of 1f9°0°C or higher using a mixed melting mixture consisting of 100% silicate ester and 50-400% water. , a method for producing quartz glass powder, which features separation and firing of the powdered gel.
ＶＣある。There is a VC.
本発明ではさらに、上ｍｌの唖鍍エステル１００谷縦と
水単味の５０容菫以上４００容蓋以下とからなる混合浴
液の代りに、珪酸ニスデル１００答緻と水５０谷献以上
４００谷量以下と疎水との含量が４００容ｔを越えない
範囲のアルコールとからなる混片浴液を使用することが
できる。これは珪酸エステルと水単味との組合せでは混
合溶液の刺合に時間がかかるが、珪酸エステルと水とに
上記範Ｈのアルコールを加えると、混合？！液の調合が
看しく容易となり促進されるからである。Furthermore, in the present invention, instead of a mixed bath solution consisting of 100 ml of Nisdel silicate and 50 ml or more of pure water and 50 ml or more of 400 ml of plain water, It is possible to use a mixed bath solution consisting of alcohol with a hydrophobic content not exceeding 400 vol/t. This is because when a silicate ester and water are combined, it takes time to mix the mixed solution, but when the alcohol in the range H above is added to the silicate ester and water, it becomes possible to mix the mixture. ! This is because the preparation of the liquid is visually easy and promoted.
次に、本発明による石英ガラス粉の製造工ｍＫついて詳
述する。Next, the quartz glass powder manufacturing process mK according to the present invention will be described in detail.
１１Ｊ 混合浴液の調合王権
混合溶液ｒｉ珪酸エステル１００容量と水５ｏ容量以上
４００ｓｔ以ドの水とをａｌｉＶ合した−のであるが。11J Preparation of mixed bath liquid 100 volumes of royal mixed solution ri silicate ester and water of 50 volumes or more and 400 sts or more were combined.
上述したように、６１Ｊ合を促進するためＫは上記範囲
のアルコールを加えればよい。As mentioned above, in order to promote the 61J combination, an alcohol within the above range may be added to K.
珪酸エステル１００谷緻当りの水の配＆緻が５０容緻未
満では該珪酸エステルの加水分解によるゲル化が十分に
進行せず、次工輸で加熱気流中で４発して損失ｔもたら
し、一方畦酸エステル１００容量当りの水の配合量、あ
るいは水とアルコールの合一が４００容ｔ′ｔ−越える
と、欠工根で噴霧により生成した粉状ゲルが軟弱で、捕
喫恢程子同士が結合して凝塊状となり、粉砕なしでは石
英ガラス粉は得られない。If the distribution and concentration of water per 100 pores of silicate ester is less than 50 pores, the gelation due to hydrolysis of the silicate ester will not progress sufficiently, and in the next process, it will be exposed to 4 shots in a heated air stream, resulting in a loss of t. If the amount of water mixed per 100 volumes of silicic acid ester or the combination of water and alcohol exceeds 400 volumes t't-, the powdery gel produced by spraying with the cutting root will be soft and the particles will not be able to absorb each other. They combine to form an agglomerate, and quartz glass powder cannot be obtained without crushing.
（２）粉状ゲルの生成１梅
該混合溶液を温度９０°Ｃ以上、好ましくは１２００Ｃ
以上の気体中にＩｎＪｊ弱し、生成する粉状ゲルを沈降
、サイクロン等により捕集する。(2) Generation of powder gel
InJj is added to the above gas, and the resulting powdery gel is collected by sedimentation, cyclone, or the like.
Ｂ気体の温度が９０°Ｃ未満でｒｉ懺赫された該混合＃
液のゲル化が十分圧進行せず、捕集４根ないし補！Ｓ後
１粒子同士が凝結して塊状となり、好ましくない０次工
程の焼成により石英ガラス粉ｔ−得るに適した粉状ゲル
を得るためには該気体１ｉｆｔ９０’Ｃ以上、好ましく
ｖま１２０°Ｃ以上に保つことが必要である。The mixture # is heated at a temperature of B gas below 90°C.
The gelation of the liquid does not proceed under sufficient pressure, and the collection 4 roots or supplements! After S, each particle coagulates and becomes a lump, and in order to obtain a powder gel suitable for obtaining quartz glass powder by firing in the undesirable 0-th step, the gas is heated at 90'C or higher, preferably at 120°C. It is necessary to maintain the above level.
（３）粉状ゲルの焼成［描
ト記粉状ゲルを、ａ常のいわゆるゾルゲル法による６鵠
ガラスの合）戊における焼成と同様Ｋ １ 、００００
Ｃ乃至１，３００°Ｃの温度で焼成すれば石英ガラス粉
が１→られる・
仄に１本発明を実梱列によりさらに具体的に説ゆＪ「る
が１本発明はその要ｄ倉越えない限り以下の−Ａ！禰丙
に上って限“逆されるものでない。(3) Firing of the powdered gel [The powdered gel described above was mixed with 6-glass glass by the usual so-called sol-gel method] K 1,0000, similar to the firing in the process.
If fired at a temperature of C to 1,300°C, silica glass powder can be produced. Unless otherwise specified, the following shall not be reversed.
喪＠例１
噴楊乾様４を用い、珪酸メチル１００容緻と水４００容
１とからなる混合浴液ｔ１５ｍ／＋の速度で２５分間、
２００°Ｃの加熱空気流（６ｔ／分）中に噴霧し、ナイ
フロン式［集４に粉状ゲルを捕集した。この粉状グルを
アルミナボートに畝せて電気炉中１５０°Ｃ／時で昇温
し、１，０５０°Ｃで１時間焼成し、得らｔＬだ粉末は
比１２．１９６ 、 Ｓ ｉｏｎ分９９．９優で石英ガ
ラス粉であることが確献された。その収率は９７％であ
った。なお、該粉末の粒子は１μｍ〜ｌＯμｍの球状を
呈していた。Mourning@Example 1 A mixed bath solution consisting of 100 volumes of methyl silicate and 400 volumes of water was mixed for 25 minutes at a speed of t15m/+ using a 4-way dryer.
The gel was sprayed into a heated air stream (6 t/min) at 200°C, and the powdered gel was collected in a Nifron type [Collection 4]. This powdered glue was ridged on an alumina boat, heated at 150°C/hour in an electric furnace, and fired at 1,050°C for 1 hour. It was confirmed that it was quartz glass powder with a score of .9. The yield was 97%. The particles of the powder had a spherical shape with a size of 1 μm to 10 μm.
夷九例２〜７
噴霧乾燥器を用い、第１表に下す各種配合組成の混合溶
液を、１０ａ／／分の連（で２５分間、渠ｌ嫌に示す温
度の加熱窒素気流＜３．５ｔ１分）中忙噴鐸し、サイク
ロン式捕ＩＩ器に粉末ゲルを補集した。Examples 2 to 7 Using a spray dryer, mixed solutions of the various compositions shown in Table 1 were heated in a stream of heated nitrogen at a temperature of <3.5t1 for 25 minutes at 10a/min. 1) The powder gel was collected in a cyclone collector II.
この粉状ゲルを実ＲｊＡ例１と同じ条件で処理し、石英
ガラス粉末ｆ：得たので、その収本金第１表にツバ丁、
いずれも高収率である。This powdered gel was treated under the same conditions as in Actual RjA Example 1 to obtain quartz glass powder f.
Both have high yields.
第１表
比較例１〜４
噴霧乾燥器を用い、請２責に示す谷橿配合ｍ或の１合＃
１％［を１ｏ４／分の導度で２５分間幕２次に！Ｆ −
ｒ’ Ｉｎ Ｉｔの加熱望素気流Ｃ３，５ｔ／分）中忙
噴繕し。Table 1 Comparative Examples 1 to 4 Using a spray dryer, make a 1/1 cup of the taniko blend m or 1 cup as shown in Example 2.
1% [25 minutes at a conductivity of 1o4/min! F-
r' In It's heated airflow C3,5t/min) during busy repair.
サイクロノ式捕１１！４に粉状ゲルを捕集した。この粉
状グルを１．０５０’ｃで焼成して得られた石英ガラス
扮末ｔｆ′ｉｔｉ酸エステル１００容皺当り水の配合量
が５０谷１未４面の比較ガｌでは収率が６４嘩と代く、
また疎水の配合量ある（／′１は該水と該アルコールの
配合量の合一が４００容１ｉｉｔ越えた比較例３．４な
らびに加熱気流の温度が９０’ｔｌ’より低い比較例２
では上Ｂｔｔ昆片浴孜の噴霧粒は十分な強度のゲルにな
らず、核補楽器内で凝結して塊状となり、ケ砕［慢なく
しＣは石英ガラス粉が優られず。The powdered gel was collected in a cyclone trap 11!4. A comparative glass containing 50 troughs, 1 and 4 sides of water per 100 volumes of tf'iti acid ester obtained by firing this powdered glue at 1.050'c had a yield of 64 Instead of a fight,
In addition, there is a hydrophobic blending amount (/'1 is Comparative Example 3.4 where the combined blending amount of water and alcohol exceeds 400 volumes 1iit and Comparative Example 2 where the temperature of the heated air stream is lower than 90'tl'
In this case, the spray particles of the above Btt kelp bath did not form a gel of sufficient strength, and condensed in the nuclear instrument, forming a lump, and pulverizing.
いｔ’ｒＬも不１檜当な条件範囲になることが確認され
た。It was confirmed that t'rL also falls within an inappropriate range of conditions.
濃ｊす４dark jsu 4
Claims (1)
００容置以下とからなる混合層液を、温（９０°Ｃ以上
の気体中に噴−して粉状ゲルを生成さ（、該粉状ゲルを
４分喝、ｍ成すること管４１＋愼とする石英ガラス粉末
の製造法。 （２）４ｍエステル１００谷綾と水５０谷緻以上４０θ
容量以下と咳水との合量が４００谷重會−えない軸回の
アルコールとからなる混合Ｓａｔ、ｎ度９υ０Ｃ以上の
気体中に噴−して粉状グルを生成させ、咳粉状ゲルを分
離、ｓｉ成すること１−＊＊とする石英ガラス粉末の製
造法。[Claims] +1) 100 volumes of 4-acid ester and 50 volumes or more of water 4
A mixed layer liquid consisting of 0.00 ml or less is injected into a gas at a temperature of 90° C. or higher to produce a powdered gel. (2) 4m ester with 100 valleys and water with 50 valleys and more than 40θ
A mixed Sat consisting of alcohol with a total volume of less than 400 degrees and cough water is injected into a gas of n degree 9υ0C or more to produce a powdery gel. A method for producing quartz glass powder, which involves separating and forming 1-**.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6813782A JPS58185443A (en) | 1982-04-23 | 1982-04-23 | Preparation of quartz glass powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6813782A JPS58185443A (en) | 1982-04-23 | 1982-04-23 | Preparation of quartz glass powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58185443A true JPS58185443A (en) | 1983-10-29 |
| JPS615657B2 JPS615657B2 (en) | 1986-02-20 |
Family
ID=13365056
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6813782A Granted JPS58185443A (en) | 1982-04-23 | 1982-04-23 | Preparation of quartz glass powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58185443A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63215525A (en) * | 1986-12-11 | 1988-09-08 | エイ・ティ・アンド・ティ・コーポレーション | Manufacture of product containing high silica glass body |
| JP2009071296A (en) * | 2007-08-20 | 2009-04-02 | Chem Art Technol:Kk | Etching solution reproducing apparatus |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6233662A (en) * | 1985-08-08 | 1987-02-13 | Alps Electric Co Ltd | Control system of motor for printer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1459786A (en) * | 1973-08-01 | 1976-12-31 | Zirconal Processes Ltd | Preparation of hydrolysates of alkyl silicates |
-
1982
- 1982-04-23 JP JP6813782A patent/JPS58185443A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1459786A (en) * | 1973-08-01 | 1976-12-31 | Zirconal Processes Ltd | Preparation of hydrolysates of alkyl silicates |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63215525A (en) * | 1986-12-11 | 1988-09-08 | エイ・ティ・アンド・ティ・コーポレーション | Manufacture of product containing high silica glass body |
| JP2009071296A (en) * | 2007-08-20 | 2009-04-02 | Chem Art Technol:Kk | Etching solution reproducing apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS615657B2 (en) | 1986-02-20 |
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