JPH0986937A - Method for manufacturing synthetic quartz glass member - Google Patents
Method for manufacturing synthetic quartz glass memberInfo
- Publication number
- JPH0986937A JPH0986937A JP27049795A JP27049795A JPH0986937A JP H0986937 A JPH0986937 A JP H0986937A JP 27049795 A JP27049795 A JP 27049795A JP 27049795 A JP27049795 A JP 27049795A JP H0986937 A JPH0986937 A JP H0986937A
- Authority
- JP
- Japan
- Prior art keywords
- glass member
- quartz glass
- synthetic quartz
- gas
- hydrogen
- 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
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1415—Reactant delivery systems
- C03B19/1423—Reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
- C03B2207/32—Non-halide
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/36—Fuel or oxidant details, e.g. flow rate, flow rate ratio, fuel additives
- C03B2207/38—Fuel combinations or non-standard fuels, e.g. H2+CH4, ethane
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は合成石英ガラス部材の製
造方法に関する。さらに詳しくは、ケイ素化合物を酸水
素火炎中で燃焼分解又は加水分解してシリカ微粒子を生
成させ、これを直接透明な合成石英ガラスにする、いわ
ゆる直接法火炎法による合成石英ガラス部材の製造方法
に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a synthetic quartz glass member. More specifically, the present invention relates to a method for producing a synthetic quartz glass member by a so-called direct flame method, in which a silicon compound is burned or decomposed in an oxyhydrogen flame to produce silica fine particles, which is directly converted into transparent synthetic quartz glass. It is a thing.
【0002】[0002]
【従来の技術】合成石英ガラス部材の製造方法として
は、主原料としての四塩化ケイ素を酸水素火炎中で気相
加水分解させて微細なシリカ粉を発生させ、これを耐熱
性基体上に堆積させると同時にその顕熱で溶融ガラス化
して合成石英ガラスとする方法が知られている(米国特
許第2,272,342号明細書参照)。2. Description of the Related Art As a method for producing a synthetic quartz glass member, silicon tetrachloride as a main raw material is subjected to gas phase hydrolysis in an oxyhydrogen flame to generate fine silica powder, which is then deposited on a heat resistant substrate. A method is known in which a synthetic quartz glass is formed by melting and vitrifying it by sensible heat at the same time as it is deposited (see US Pat. No. 2,272,342).
【0003】また、使用する原料としてのケイ素化合物
は、四塩化ケイ素以外に、一般式RnSiX4-n(Rは水
素原子、メチル基又はエチル基、Xはハロゲン原子、メ
トキシ基又はエトキシ基、nは0〜4の整数を表す。)
で表されるケイ素化合物、例えばメチルトリクロロシラ
ン、メチルトリメトキシシラン等のシラン化合物が既に
使用されている。In addition to silicon tetrachloride, the silicon compound used as a raw material has the general formula R n SiX 4-n (R is a hydrogen atom, a methyl group or an ethyl group, X is a halogen atom, a methoxy group or an ethoxy group). , N represents an integer of 0 to 4.)
A silicon compound represented by, for example, a silane compound such as methyltrichlorosilane and methyltrimethoxysilane has already been used.
【0007】[0007]
【発明が解決しようとする課題】これらの製法において
は、火炎を形成する燃焼源として一般的に水素が使用さ
れるが、合成石英ガラス部材の生産量の増加やサイズの
大口径化に伴い、使用する水素の原単位が増加し、コス
トの増加を招いている。また、水素の原単位の増加に伴
って絶対量も多くなるため、それに対応した設備が必要
となり、さらに経費の増大を招くという不利を生じてい
る。In these manufacturing methods, hydrogen is generally used as a combustion source for forming a flame, but with the increase in the production amount of synthetic quartz glass members and the increase in size, The basic unit of hydrogen used increases, which causes an increase in cost. Further, since the absolute amount of hydrogen increases as the basic unit of hydrogen increases, equipment corresponding to the increase is required, which causes a disadvantage of further increase in cost.
【0008】そこで本発明は、水素の原単位を減少させ
た合成石英ガラス部材の製造方法を提供することを目的
とする。Therefore, an object of the present invention is to provide a method of manufacturing a synthetic quartz glass member in which the unit consumption of hydrogen is reduced.
【0009】[0009]
【課題を解決するための手段】本願の請求項1記載の発
明は、一般式RnSiX4-n(Rは水素原子、メチル基又
はエチル基、Xはハロゲン原子、メトキシ基又はエトキ
シ基、nは0〜4の整数を表す。)で表されるケイ素化
合物を酸水素火炎中で燃焼分解又は加水分解させてシリ
カ微粒子を生成させ、これを回転する耐熱性担体上に堆
積させると同時にその顕熱によって溶融ガラス化させる
合成石英ガラス部材の製造方法において、ケイ素化合物
を燃焼反応させる酸水素火炎の水素ガス中に、アルカン
類から選択される少なくとも一種又は二種を混合させる
ことを特徴とする合成石英ガラス部材の製造方法を提供
する。The invention according to claim 1 of the present application provides a compound represented by the general formula R n SiX 4-n (R is a hydrogen atom, a methyl group or an ethyl group, X is a halogen atom, a methoxy group or an ethoxy group, n represents an integer of 0 to 4) is decomposed or hydrolyzed in an oxyhydrogen flame to generate silica fine particles, which are deposited on a rotating heat-resistant carrier and at the same time. In a method for producing a synthetic quartz glass member that melts and vitrifies by sensible heat, at least one kind or two kinds selected from alkanes is mixed in hydrogen gas of an oxyhydrogen flame in which a silicon compound is burnt and reacted. A method of manufacturing a synthetic quartz glass member is provided.
【0010】本願の請求項2記載の発明は、水素ガスに
対する前記アルカン類から選択される少なくとも一種又
は二種の混合比を、流量比で少なくとも1.5倍混合さ
せることを特徴とする請求項1記載の合成石英ガラス部
材の製造方法を提供する。The invention according to claim 2 of the present application is characterized in that the mixing ratio of at least one kind or two kinds selected from the alkanes to hydrogen gas is mixed at a flow rate ratio of at least 1.5 times. 1. A method for manufacturing the synthetic quartz glass member according to 1 is provided.
【0011】本願の請求項3記載の発明は、前記アルカ
ン類がメタン又はプロパンである請求項1又は2記載の
合成石英ガラス部材の製造方法を提供する。The invention according to claim 3 of the present application provides the method for producing the synthetic quartz glass member according to claim 1 or 2, wherein the alkane is methane or propane.
【0012】次に、本発明をさらに詳細に説明する。Next, the present invention will be described in more detail.
【0013】本発明者らは、合成石英ガラス部材の製造
方法において、水素原単位を低減させる方法として種々
検討した結果、使用する水素ガス中に、燃焼ガスとして
アルカン類から選択される少なくとも一種又は二種を混
合させ、その混合比を特定することによって、本発明の
目的である水素原単位の低減を図ることができ、本発明
を完成させた。アルカン類としてはメタン、エタン、プ
ロパン、ブタン等が例示されるが、メタン(CH4)又
はプロパン(C3H8)若しくはこれらの混合ガスが好ま
しく用いられる。The inventors of the present invention have conducted various studies as a method of reducing the hydrogen consumption rate in the method for producing a synthetic quartz glass member, and as a result, have found that at least one selected from alkanes as a combustion gas in the hydrogen gas to be used, or By mixing two kinds and specifying the mixing ratio, it is possible to reduce the hydrogen consumption rate, which is the object of the present invention, and the present invention has been completed. Examples of alkanes include methane, ethane, propane, butane and the like, but methane (CH 4 ) or propane (C 3 H 8 ) or a mixed gas thereof is preferably used.
【0013】本発明の方法に使用される原料ガスとして
のケイ素化合物は、前記した一般式RnSiX4-nで表さ
れる。ここで、Rは水素原子、メチル基又はエチル基、
Xはハロゲン原子、メトキシ基又はエトキシ基、nは0
〜4の整数を表す。このケイ素化合物としては、例えば
SiH4、H2SiCl2、HSiCl3、SiCl4、S
iF4、CH3SiCl3、(CH3)2SiCl2、Si
(CH3)4、Si(OCH3)4、CH3Si(OCH3)
3、HSi(OCH3)3、Si(OC2H5)4、CH3S
i(OC2H5)3などが例示される。The silicon compound as a raw material gas used in the method of the present invention is represented by the above general formula R n SiX 4-n . Here, R is a hydrogen atom, a methyl group or an ethyl group,
X is a halogen atom, a methoxy group or an ethoxy group, n is 0
Represents an integer of 4; Examples of the silicon compound include SiH 4 , H 2 SiCl 2 , HSiCl 3 , SiCl 4 , and S.
iF 4 , CH 3 SiCl 3 , (CH 3 ) 2 SiCl 2 , Si
(CH 3 ) 4 , Si (OCH 3 ) 4 , CH 3 Si (OCH 3 )
3 , HSi (OCH 3 ) 3 , Si (OC 2 H 5 ) 4 , CH 3 S
i (OC 2 H 5 ) 3 and the like are exemplified.
【0014】上記のうち、工業的には、安価で容易に入
手することができ、危険性が少なく、揮発性に富み、排
ガス処理も容易であるという点で、SiCl4、Si
(OCH3)4、CH3Si(OCH3)3、CH3SiCl
3が好ましい。Among the above, SiCl 4 and Si are industrially available in that they are inexpensive, easily available, less dangerous, rich in volatility, and easy to treat exhaust gas.
(OCH 3 ) 4 , CH 3 Si (OCH 3 ) 3 , CH 3 SiCl
3 is preferred.
【0015】[0015]
【実施例】次に、本発明を実施例を挙げてさらに詳細に
説明する。EXAMPLES Next, the present invention will be described in more detail with reference to examples.
【0016】本発明の方法について、CH3SiCl3を
原料ガスとして使用する場合を例として説明する。図1
は、CH3SiCl3を使用した場合の装置の概略図を示
す。図において、蒸発器1内に収容されている原料物質
としてのCH3SiCl3は、供給部(A)からのキャリ
アガスaでバブリングされ、図示しない加熱器で加熱さ
れて気化し、バーナー2に送られる。The method of the present invention will be described with reference to the case where CH 3 SiCl 3 is used as a source gas. FIG.
Shows a schematic diagram of an apparatus when CH 3 SiCl 3 is used. In the figure, CH 3 SiCl 3 as a raw material contained in the evaporator 1 is bubbled with a carrier gas a from a supply part (A), heated by a heater (not shown) to be vaporized, and then burner 2 Sent.
【0017】このバーナー2のノズルは、図2に示すよ
うに、径の異なる複数のノズルA、B、C及びEが断面
同心円状に配列されるとともに、ノズルCの外側でノズ
ルD内に、比較的系の小さい複数のノズルDが、前記ノ
ズルA、B、C及びEの断面中心を共有する複数の同心
円上に配置されている。As shown in FIG. 2, the nozzle of the burner 2 has a plurality of nozzles A, B, C and E having different diameters arranged concentrically in cross section, and inside the nozzle D outside the nozzle C. A plurality of nozzles D having a relatively small system are arranged on a plurality of concentric circles sharing the cross-sectional centers of the nozzles A, B, C and E.
【0018】そして、原料物質としてのCH3SiCl3
はキャリアガスaとともにバーナー2のノズルAに供給
される。また、燃焼ガスとしての酸素ガスが供給部
(B)からノズルBに、水素及びメタンがそれぞれ供給
部(C1)及び(C2)からノズルCに、酸素等の支燃性
ガスが供給部(D)からノズルDに、水素及びメタンが
それぞれ供給部(E1)及び(E2)からノズルEに供給
される。Then, CH 3 SiCl 3 as a raw material
Is supplied to the nozzle A of the burner 2 together with the carrier gas a. Further, oxygen gas as a combustion gas is supplied from the supply unit (B) to the nozzle B, hydrogen and methane are supplied from the supply units (C 1 ) and (C 2 ) to the nozzle C, and a combustion-supporting gas such as oxygen is supplied to the supply unit. From (D), hydrogen and methane are supplied to the nozzle D from the supply units (E 1 ) and (E 2 ) respectively.
【0019】これらの混合ガスがバーナー2から火炎と
して合成石英ガラス基体3に照射され、ここに発生した
シリカの溶融成長によって合成石英ガラスインゴット4
が形成される。なお、図1では合成石英ガラス部材の成
長方向を水平方向として示したが、水平方向とするか又
は垂直方向とするかは任意である。The mixed gas is irradiated from the burner 2 as a flame onto the synthetic quartz glass substrate 3, and the synthetic quartz glass ingot 4 is produced by the melt growth of silica generated therein.
Is formed. In addition, in FIG. 1, the growth direction of the synthetic quartz glass member is shown as a horizontal direction, but it is arbitrary whether the growth direction is the horizontal direction or the vertical direction.
【0020】供給する水素とメタンとの混合比は、流量
比で水素流量の少なくとも1.5倍量のメタンを混合さ
せるのが好ましい。これにより、これまでの酸素と水素
のみを用いた火炎により製造した合成石英ガラス部材と
同等品質が得られ、且つ生産性を上げることが可能にな
る。混合比が1.5倍未満であると、目的とする水素原
単位を50%以下に低減することが困難となる可能性が
ある。As for the mixing ratio of hydrogen and methane to be supplied, it is preferable that methane is mixed at a flow ratio of at least 1.5 times the flow rate of hydrogen. This makes it possible to obtain the same quality as the conventional synthetic quartz glass member manufactured by a flame using only oxygen and hydrogen, and to improve the productivity. If the mixing ratio is less than 1.5 times, it may be difficult to reduce the target hydrogen consumption rate to 50% or less.
【0021】なお、バーナー2のノズルDの本数は少な
くとも30本以上あるのが好ましく、1本のノズル内径
は1.0〜2.0mmφであるのが好ましい。ノズルD
の本数が30本より少ない場合あるいはノズル径が2.
0mmより大きい場合は、メタンの燃焼効率が低下して
不完全燃焼を引き起こし、赤炎を伴うことがある。この
結果、シリカ微粒子が堆積し、溶融面にカーボン(C)
が析出してインクルージョンになってしまうことがあ
る。また、ノズルDの径が1.0mmφより小さい場合
は、酸素ガスの噴き出し線速が増加して火炎を乱すこと
がある。この結果、SiO2の固定率を低下させて生産
性を悪化させてしまう。The number of nozzles D of the burner 2 is preferably at least 30 or more, and the inner diameter of one nozzle is preferably 1.0 to 2.0 mmφ. Nozzle D
If the number is less than 30, or if the nozzle diameter is 2.
If it is larger than 0 mm, the combustion efficiency of methane decreases, causing incomplete combustion, which may be accompanied by a red flame. As a result, silica particles are deposited and carbon (C) is deposited on the melting surface.
May be deposited and become an inclusion. Further, when the diameter of the nozzle D is smaller than 1.0 mmφ, the ejection linear velocity of oxygen gas may increase and disturb the flame. As a result, the fixing rate of SiO 2 is lowered and productivity is deteriorated.
【0022】次に、図1に示した装置構成で、原料ガス
としてのメチルトリクロロシラン(CH3SiCl3)を
キャリアガスとしてのアルゴンガス、酸素ガスの混合ガ
スとともに図2に示したノズル構成を有するバーナーに
供給し、各ノズルから表1に示す流量比で各ガスを流し
て火炎を発生させ、直径100mmの合成石英ガラス基
体に照射するとともに、この基体上に成長した合成石英
素塊を得た。メタンガスを含む各ガスのガス量比と水素
の原単位をメタンを混焼させない場合の水素原単位を
「1」にした時の各実施例及び比較例の比率を表1に示
した。Next, in the apparatus structure shown in FIG. 1, the nozzle structure shown in FIG. 2 is used together with a mixed gas of methyltrichlorosilane (CH 3 SiCl 3 ) as a source gas as a carrier gas and an oxygen gas. The gas is supplied to the burner, and each gas is caused to flow from each nozzle at the flow rate ratio shown in Table 1 to generate a flame, which is irradiated to a synthetic quartz glass substrate having a diameter of 100 mm, and synthetic quartz ingots grown on this substrate are obtained. It was Table 1 shows the gas amount ratio of each gas containing methane gas and the ratio of each example and comparative example when the hydrogen basic unit was set to "1" when the hydrogen basic unit was not co-firing methane.
【0023】[0023]
【表1】 [Table 1]
【0024】表1から分かるように、水素に対するメタ
ンの混合比(流量比)が1.2倍の場合でもメタンを全
く混合させない場合より水素原単位を僅かながら減少さ
せることができるが、混合比が1.67倍及び2.0倍
の場合は水素原単位を大幅に減少させることができた。As can be seen from Table 1, even when the mixing ratio (flow ratio) of methane to hydrogen is 1.2 times, the hydrogen basic unit can be slightly reduced as compared with the case where methane is not mixed at all. Of 1.67 times and 2.0 times, it was possible to significantly reduce the hydrogen consumption rate.
【0025】[0025]
【発明の効果】以上説明した通り本発明によれば、合成
石英ガラス部材を製造するに際し、水素の原単位を大幅
に減少することができる。As described above, according to the present invention, it is possible to greatly reduce the unit consumption of hydrogen when manufacturing a synthetic quartz glass member.
【図1】本発明の方法を実施する際に用いる装置構成の
一例を示す説明図である。FIG. 1 is an explanatory diagram showing an example of an apparatus configuration used when carrying out a method of the present invention.
【図2】本発明の方法で用いるバーナーのノズル部分を
示す断面図である。FIG. 2 is a sectional view showing a nozzle portion of a burner used in the method of the present invention.
1 蒸発器 2 バーナー 3 合成石英ガラス基体 4 合成石英ガラスインゴット A,B,C,D,E ノズル 1 Evaporator 2 Burner 3 Synthetic quartz glass substrate 4 Synthetic quartz glass ingot A, B, C, D, E Nozzle
Claims (3)
チル基又はエチル基、Xはハロゲン原子、メトキシ基又
はエトキシ基、nは0〜4の整数を表す。)で表される
ケイ素化合物を酸水素火炎中で燃焼分解又は加水分解さ
せてシリカ微粒子を発生させ、これを回転する耐熱性担
体上に堆積させると同時にその顕熱によって溶融ガラス
化させる合成石英ガラス部材の製造方法において、 ケイ素化合物を燃焼反応させる酸水素火炎の水素ガス中
に、アルカン類から選択される少なくとも一種又は二種
を混合させることを特徴とする合成石英ガラス部材の製
造方法。1. A compound represented by the general formula R n SiX 4-n (R represents a hydrogen atom, a methyl group or an ethyl group, X represents a halogen atom, a methoxy group or an ethoxy group, and n represents an integer of 0 to 4). A method for producing a synthetic quartz glass member in which a silicon compound is decomposed by combustion or hydrolyzed in an oxyhydrogen flame to generate silica fine particles, which are deposited on a rotating heat-resistant carrier and, at the same time, melted and vitrified by the sensible heat thereof. 2. A method for producing a synthetic quartz glass member, wherein at least one kind or two kinds selected from alkanes is mixed with hydrogen gas of an oxyhydrogen flame in which a silicon compound is burned and reacted.
択される少なくとも一種又は二種の混合比を、流量比で
少なくとも1.5倍混合させることを特徴とする請求項
1記載の合成石英ガラス部材の製造方法。2. The synthetic quartz glass member according to claim 1, wherein the mixing ratio of at least one kind or two kinds selected from the alkanes to hydrogen gas is mixed at a ratio of at least 1.5. Production method.
ある請求項1又は2記載の合成石英ガラス部材の製造方
法。3. The method for producing a synthetic quartz glass member according to claim 1, wherein the alkane is methane or propane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27049795A JPH0986937A (en) | 1995-09-25 | 1995-09-25 | Method for manufacturing synthetic quartz glass member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27049795A JPH0986937A (en) | 1995-09-25 | 1995-09-25 | Method for manufacturing synthetic quartz glass member |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0986937A true JPH0986937A (en) | 1997-03-31 |
Family
ID=17487101
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27049795A Pending JPH0986937A (en) | 1995-09-25 | 1995-09-25 | Method for manufacturing synthetic quartz glass member |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0986937A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0878451A1 (en) * | 1997-05-14 | 1998-11-18 | Nikon Corporation | Synthetic silica glass optical member and method of manufacturing the same |
| JP2002080239A (en) * | 2000-09-06 | 2002-03-19 | Sumitomo Metal Ind Ltd | Synthetic quartz glass for optical member and method for producing synthetic quartz glass |
| WO2002090258A3 (en) * | 2001-05-04 | 2008-01-17 | Corning Inc | Method for making doped silica glass by vapour deposition |
-
1995
- 1995-09-25 JP JP27049795A patent/JPH0986937A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0878451A1 (en) * | 1997-05-14 | 1998-11-18 | Nikon Corporation | Synthetic silica glass optical member and method of manufacturing the same |
| JP2002080239A (en) * | 2000-09-06 | 2002-03-19 | Sumitomo Metal Ind Ltd | Synthetic quartz glass for optical member and method for producing synthetic quartz glass |
| WO2002090258A3 (en) * | 2001-05-04 | 2008-01-17 | Corning Inc | Method for making doped silica glass by vapour deposition |
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