JPS62260728A - Production of glass preform for optical transmission - Google Patents
Production of glass preform for optical transmissionInfo
- Publication number
- JPS62260728A JPS62260728A JP9596386A JP9596386A JPS62260728A JP S62260728 A JPS62260728 A JP S62260728A JP 9596386 A JP9596386 A JP 9596386A JP 9596386 A JP9596386 A JP 9596386A JP S62260728 A JPS62260728 A JP S62260728A
- Authority
- JP
- Japan
- Prior art keywords
- fluorine
- silicon
- deposit
- glass
- base material
- 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
- 239000011521 glass Substances 0.000 title claims abstract description 27
- 230000005540 biological transmission Effects 0.000 title claims description 12
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 230000003287 optical effect Effects 0.000 title claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- OJCDKHXKHLJDOT-UHFFFAOYSA-N fluoro hypofluorite;silicon Chemical compound [Si].FOF OJCDKHXKHLJDOT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000003377 silicon compounds Chemical class 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 16
- 229910052731 fluorine Inorganic materials 0.000 abstract description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011737 fluorine Substances 0.000 abstract description 12
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000002019 doping agent Substances 0.000 description 7
- -1 fluorine compound Chemical class 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 150000002222 fluorine compounds Chemical class 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000004017 vitrification Methods 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 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 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JZUFKLXOESDKRF-UHFFFAOYSA-N Chlorothiazide Chemical compound C1=C(Cl)C(S(=O)(=O)N)=CC2=C1NCNS2(=O)=O JZUFKLXOESDKRF-UHFFFAOYSA-N 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical group F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- ARBIYISMVFAYHV-UHFFFAOYSA-N trifluoro(trifluorosilyloxy)silane Chemical compound F[Si](F)(F)O[Si](F)(F)F ARBIYISMVFAYHV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
- C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Glass Compositions (AREA)
Abstract
Description
【発明の詳細な説明】
3 発明の評や◆1な説明
+t!p2上の利用分野)
本発明は元伝送用ガラス母材の製造方法、待(二1;ド
ーパントとしてフッ素原子を含有する元伝送用ガラス母
材のり造方法f二閏するものである。[Detailed description of the invention] 3. Review of the invention and ◆1 explanation +t! The present invention relates to a method for manufacturing a glass base material for transmission, and a method for manufacturing a glass base material for transmission containing a fluorine atom as a dopant.
(従来の技術)
元伝送用ガラス母材としての石英材が四塩化けい素など
のけい素化合物の火炎加水分解により生成したりリカ微
粉末を支持体上に堆積六七、こ\(二得られた多孔質の
りリカ堆積体の加熱溶融(=よる透明ガラス化C二よっ
て得られることは丁でによく知られたところである。(Prior art) Quartz material, which is the original transmission glass base material, is produced by flame hydrolysis of silicon compounds such as silicon tetrachloride, and fine powder of silica is deposited on a support. It is well known that transparent vitrification can be obtained by heating and melting a porous glue deposit.
しかして、この光伝送用ガラス母材は通常、中心部を光
が通る高屈折率のコアと呼ばれろ部分とし、外周部を他
極折率のクラッドと呼ばれる部分としたものとされるの
で、屈折率を高めるためにンリ力堆積JT−を作ると六
にけい素化合物にCre(’E1などを添n口し、Ge
Q□をドーパントと下る方法が採られているが、これC
:はOeCl 、などが高価で資源面にもBIJりのあ
る工)のであるということからクラッド四となるガラス
母材を低屈折諷のものと下る方法も採用されている。こ
のカラス母材のiF%率をイ氏下さセろためのドーパン
トとしてはほう素とフッ素が知られているが、はう素は
長波長域で赤外吸収性をもっているので好ましいもので
はなく、フッ素が好ましいものとされているが、上記し
たけい素化合物にOF4. eel、F、 、 SiF
、などのフッ素化合物を混入してシリカ#:積体を作ろ
うとしてもフッ素がりリカ堆積体に含有される量が極め
て少なくなるためこの方法は実用的には問題がある。However, this optical transmission glass base material usually has a central part called a core with a high refractive index through which light passes, and an outer peripheral part called a cladding with a different polar refractive index. In order to increase the refractive index, when a JT layer is made by force deposition, Cre ('E1, etc.) is added to the silicon compound in order to increase the refractive index.
A method of lowering Q□ with a dopant has been adopted, but this
Since OeCl (OeCl, etc.) is expensive and resource-intensive, a method of using a low-refractive material as the glass base material for the cladding has also been adopted. Boron and fluorine are known as dopants to reduce the iF% ratio of the glass base material, but boron is not preferable because it has infrared absorption in the long wavelength range. Although fluorine is preferred, OF4. eel, F, , SiF
Even if an attempt is made to make a silica stack by mixing a fluorine compound such as fluorine compound, the amount contained in the fluorine-containing silica deposit will be extremely small, so this method is problematic in practice.
他方、ガラス母材のドーピングについてはけい素化合物
の火災加水分解で得たりリカ堆積体の透明ガラス化の際
f二上記したようなドーパントを加え、その熱処理時に
ドープとするという方法も知られているが、この場合に
は目11”l ’:t C対して大過軸のドーパントを
除服する必要が、あり、このドーパントとしてフッ素化
合物を便用Tろとfirユはガラス成分がSiF4 と
して体数したり、フッ素化合物中に存在する炭素原子【
二よってガラス成分としてのSiO□が5ill二還元
されて揮散し、さらにはこの炭素原子C二よって酸素欠
陥が生じるという不利がある。On the other hand, regarding doping of the glass base material, it is also known to obtain dopants obtained by fire hydrolysis of silicon compounds or to add dopants such as those mentioned above during the transparent vitrification of liquefied deposits, and to dope them during heat treatment. However, in this case, it is necessary to remove the dopant that has a large overaxis with respect to 11"l':tC, and when using a fluorine compound as the dopant, the glass component is SiF4. carbon atoms present in fluorine compounds [
Therefore, there is a disadvantage that SiO□ as a glass component is reduced by 5ill and volatilized, and furthermore, oxygen defects are generated by this carbon atom C2.
(弁明Q)々が成)
本つi明はこのよつl不利を解法したフッ素でドープさ
れた元伝送用ガラス母材の製造に関Tるものであり、こ
れはけい素化合物の火炎加水+f解で生成したりリカa
程子を堆積させて多孔質のシリカ堆楯体を形1戊さセた
のち、これをオキシフッ化けい素を含む※囲気で、また
はオキシフッ化けい票券囲気にさらしたり)ち、nD熱
溶融して透明かラス化することを特徴とてるものである
。(Explanation Q) The present article is concerned with the production of a fluorine-doped glass base material for transmission that solves this disadvantage, and this is a method for producing a glass base material for transmission by flame hydration of a silicon compound. Generate with +f solution or Rika a
After depositing the powder and forming a porous silica shell into a shape, it is heated in an atmosphere containing silicon oxyfluoride (or exposed to an atmosphere containing silicon oxyfluoride), and is then thermally melted. It is characterized by being transparent or lathed.
Tなわち、本発四者らはけい素化合物から得られた多孔
laのりリカ堆積体からフッ素ドープされた光伝送用ガ
ラス母材を製造する方法について枠中(:そのま\取り
込まれ易く、ガラス中1:フッ素を効率よく添加するこ
とかで★、高いフッ素収率を得ることができることから
、結果において効率よくフッ素ドープされたガラス母材
を得ることができることを見出下と共(二、このオキシ
フッ化けい素化合物は高純度品として製造し得るもので
あることから炭素などの不純物の存在(二よる不利を避
けることがでまろということを確認し、こ\に使用Tる
オキシフッ化けい素化合物の種類、除服量などについて
の研゛究を進めて本発明を完成させた。In other words, the present inventors have described a method for producing a fluorine-doped optical transmission glass base material from a porous LA glue deposit obtained from a silicon compound. In glass 1: By efficiently adding fluorine, a high fluorine yield can be obtained, and as a result, a glass base material doped with fluorine can be obtained efficiently. Since this silicon oxyfluoride compound can be manufactured as a high-purity product, we confirmed that it is possible to avoid the presence of impurities such as carbon (two disadvantages). The present invention was completed by conducting research on the types of silicon compounds and the amount to be removed.
本発明の方法における多孔″fiシリカ唯梼休の体造は
公刊の方法で行えはよい。したがってこれには一般式
RmSlx4−mで示され、Rはメチル基、エチル基、
プロピル基などのような1価炭化水素基、χは塩素、フ
ッ素などのハロゲン原子5艷まメトキン基、エトキシ基
などのアルコキシ基、mはO〜4の整智とされるけい≠
化合物、例えば5iC1,、8i、(i’4. H81
C1,、5iF(4,C)(,5iC1,。The structure of the porous silica structure in the method of the present invention can be carried out by the published method. Therefore, the general formula
RmSlx4-m, R is a methyl group, an ethyl group,
A monovalent hydrocarbon group such as a propyl group, χ is a halogen atom such as chlorine or fluorine, an alkoxy group such as a methquine group or an ethoxy group, and m is an atom of O to 4.
Compounds such as 5iC1,, 8i, (i'4. H81
C1,,5iF(4,C)(,5iC1,.
CH,51(OCH,+、、 5itOOH,+4.
5i(OC,H,+4などを主成分とするガラス1皇
科を酸水異炎などの火炎中に供給して火炎110水分解
反応させ、この反応によって生成したりリカ微粉末を支
持体上に堆積させればよい。このシリカ堆積4本の製法
は1山常、[可転している支持体上にシリカ微粉末を堆
積させろと共にこれを搭勅さセて、このL仲Fα体を軸
方向(二l戊慎させる軸付i’lQによって行7にねれ
るが、これは石グLまたはカーホン質からなる]耐熱性
の支持体の外周(こJく−カーを往復運動させながら、
シリカ微粒子を堆積させる外付法で行jjつてもよい。CH,51(OCH,+,, 5itOOH,+4.
Glasses containing 5i (OC, H, +4, etc. as main components) are fed into a flame such as an acidic water flame to cause a flame 110 water decomposition reaction. The manufacturing method for these four silica deposits is as follows: [Deposit fine silica powder on a rotatable support, and then use it to deposit this L-nof-Fα form. The outer periphery of the heat-resistant support in the axial direction (which is twisted in row 7 by the shaft attached to it, which is made of stone or carbonaceous material) (while the car is reciprocating) ,
It may also be performed by an external method of depositing fine silica particles.
このようにして得られた・7リ力惟積体は密IWがQ、
1〜Q、−1p/Cこの多孔′に体であり、これは反
l、iゞ1、時に生成下る水分、水酸基、塩素を吸着ま
たシま結合したちの、この支持体として元伝送用のコア
となる石英棒を便用下ることにより、元伝送母材用素し
とTることつ;でまる。The density IW of the 7-reforced product obtained in this way is Q,
1~Q, -1p/C This porous body absorbs and bonds moisture, hydroxyl groups, and chlorine that sometimes occur, and serves as a support for original transmission. By removing the quartz rod that forms the core of the quartz rod, it becomes the base material for the original transmission base material.
本発明の方法はこのようにして得た多孔質のりリカ堆積
体をオキシフッ素けい素化合物の存在下で加熱溶融して
元伝送用ガラス母材と下るのであるが、この処pHl二
当ってはシリカ堆積イ本をオキシフッ化けい素化倚′P
Aを含む雰囲気中で予じめ1.000〜1,300℃の
温度で処理してから1.300−1.600℃で溶融し
て透明ガラス化してもよいし、シリカ堆梼体をオネジフ
ッ化けい素化合物を含む≧メ囲気中で1,300〜1.
600℃に770熱し溶融して透明ガラス化してもよい
が、一般刊には後者のほうが透明ガラス化時のフッ素の
揮散が/plいので高1kKのドープには好ましい。こ
の透明ガラス化はオキシフッ化けい素化合物の存在下で
行なわれるので、これによればフッ素によろドープと同
時(二悦水反応も行なわれるという有利性も与えられる
。この処理におけるオキシフッ化けい素化合物を含む雰
曲気シばヘリウム、アルゴン、窒素、#素などのガス中
にオキシフッ化けい素化合物を拡散させたものとすれば
よいが、このfl’J Iす:が低下ぎるとフッ素ドー
プC:よろ属折謁の低下効果が不充分とIEす、高Tぎ
ると残イI気泡がガラス母材中に残るようにγ2るので
、このJUjは0.01〜10モル%の悦曲、好ましく
はQ、1〜5モル%の軸弁と下ることがよく、この処f
!’! 8% F:’+Jは!Iη常1〜3時ttnと
丁ればよい。In the method of the present invention, the porous glue deposit thus obtained is heated and melted in the presence of an oxyfluorosilicon compound to form the original transmission glass base material. The silica deposits are converted to oxyfluoride silicon.
Alternatively, the silica pellet may be treated in advance at a temperature of 1,000 to 1,300°C in an atmosphere containing A, and then melted at 1,300 to 1,600°C to form transparent glass. 1,300-1.
Although it may be heated to 600° C. for 770°C to melt and form transparent glass, the latter method is preferred for high 1 kK doping because the volatilization of fluorine during transparent vitrification is less per pl. Since this transparent vitrification is carried out in the presence of a silicon oxyfluoride compound, it also provides the advantage that the fluorine doping and simultaneous reaction (also known as Eryu water reaction) are carried out. The atmosphere containing the compound may be one in which a silicon oxyfluoride compound is diffused in a gas such as helium, argon, nitrogen, # element, etc., but if this fl'J I: is too low, fluorine doped C : The effect of lowering the elasticity is insufficient, and if the temperature is too high, γ2 will remain so that bubbles remain in the glass base material, so this JUj is preferably 0.01 to 10 mol%. Q, 1 to 5 mol% of the shaft valve is often found, and this process f
! '! 8% F:'+J is! Iη should always be 1 to 3 o'clock ttn.
こ\に使用されるオー1−シフッ化けい素化合物は一#
Q式5inOn−、F2n+2で示され、nは1〜10
のV数と六れるもの、さらにはこのFの1部がclで置
換されたものとネれるか、これについては沸点カ低く
精動も′8易であるヘキぜ)口ロシ、ンロキ−+ ンS
i、OF、 、オクタフロロトリゾロキ+ySi、O,
F、 、デカフロロテトラシロキチンs1t’s”+。The O-1-silicon fluoride compound used for this is 1#
Q formula 5inOn-, represented by F2n+2, where n is 1 to 10
If the number of V is six, and if a part of this F is replaced with Cl, the boiling point is low.
The spirit is also '8 easy.
i, OF, , octafluorotrizoloki+ySi, O,
F, Decafluorotetrasilochitin s1t's"+.
が好ましいものとされろ。be preferred.
な3、これらのオキシフッ化けい素化合物は例えばエチ
ルエーテルと水の胛、合液−で四瑠化けい素を部分n0
水分解する方a (J、 Az、 chem、 Soc
、 。3.These silicon oxyfluoride compounds can be prepared by converting silicon tetraruride into partial n0 with a mixture of ethyl ether and water, for example.
Water splitting method a (J, Az, chem, Soc
, .
72 、3178(1950年〕参照〕、クロロシロキ
チン類を5bC1sを触媒としてSbF、でフ゛l素化
する方法[J、 Am、 Cbem、 Soc、 、
h7.1092 (1945年]釡照〕でり造Tること
かで七、Si、 OF、は5i20CI、 をフッ素
化下ることによって得ることができるが、このフッ素化
工程でl1M1l I’tE Tる5L20 F2O3
,、Si、OF1”1なども本発明に使用Tることがで
夫るが、これらは蒸留などの手段で容易に高紳変のもの
が得られる。72, 3178 (1950)], a method for fluorination of chlorosilochitins with SbF using 5bC1s as a catalyst [J, Am, Cbem, Soc,
h7.1092 (1945) [Kateru] Derizo T. 7, Si, OF, can be obtained by fluorinating 5i20CI, but in this fluorination process, l1M1l I'tE T 5L20 F2O3
, Si, OF1''1, etc. can also be used in the present invention, but they can be easily obtained in high grade by distillation or other means.
ツキ(二本イ1〉明の実施(yjlをあげろ。Tsuki (two i1) Akira's implementation (raise yjl.
実施例1
万乗製の四11−管バーナー(二5il14430m1
1分、8210g/分、02161/分ン供給して酸水
素火炎を形す又さセ、こ\(=生成したシリカ微粉末を
回転している妬純度石英ガラス製の支持体上に堆漬六せ
て多孔0シリ力惟噴体を!成長さ仕た。Example 1 Manjo 411-tube burner (25il14430m1
1 minute, 8210 g/min, 02161/min to form an oxyhydrogen flame. In addition, a porous 0-silicon blowing body was grown!
つぎにこの多孔質S/リカ年積体を13モル%のへキ斗
フロロジー/ロキサンS1□OF、を含むヘリウムガス
雰卵気下に1.200℃で2時間加熱したのち、ヘリウ
ムガスのみからなる不活性ガス雰呼気に1.500℃で
111−:p間加熱し溶飼へセて透明ガラス化したとこ
ろ、OH基含有F・Iが50ppbで石英ガラスの屈折
率に対して0.3%低い屈に率をちり石英、ガラヌカ1
得られ、このときのガラスl申:孜率は2%ときわめて
低い値であった。Next, this porous S/liquid volume was heated at 1.200°C for 2 hours in a helium gas atmosphere containing 13 mol % of hekitofluorology/roxane S1□OF, and then heated from helium gas alone. When heated for 111-:p in an inert gas atmosphere at 1.500°C and melted to form transparent glass, the OH group-containing F/I was 50 ppb and the refractive index was 0.3 compared to that of silica glass. % low yield rate quartz, Galanuka 1
The glass filtration ratio at this time was an extremely low value of 2%.
なお、上記におけるヘキサフロロジシロキサンのe度を
0〜8モル%にかえて上記と同じ方法で石英ガラスを作
り、得られた石英ガラスの屈折率を測定したところ、躬
1図に示したような結果か得られた。In addition, when quartz glass was made in the same manner as above except that the e degree of hexafluorodisiloxane was changed to 0 to 8 mol%, and the refractive index of the obtained quartz glass was measured, it was as shown in Figure 1. I got some good results.
1;良:;1mi 例2
実施例1の方法で得られた多孔Gシリカ上口へ体を5モ
ル%のオクタフロロトリゾロキサンSi、 0. Fs
を会むヘリウムガス写卵気の慟気炉に入れ、1.000
−Cから1,500’Cまでを5”07分のノ←涌工・
μ曳で110熱し約2b間熱・処理し2ところ、14i
1月fご石英ガラス母材が得られ、このものに−j、O
H含有借が30 ppbで石英ガラヌC二効してQ、6
%低い屈折率をもつものであり、このと傘のガラス揮散
率は3%で、Flつた。1; Good: ;1mi Example 2 The porous G silica obtained by the method of Example 1 was loaded with 5 mol% of octafluorotrisoloxane Si, 0. Fs
Put the helium gas into the gas furnace, and 1.000
- From C to 1,500'C 5"07 minutes ← Wakuko・
Heat it to 110℃ with a μ pull, heat and treat for about 2b, then 14i.
A quartz glass matrix was obtained in January, and −j, O
H content is 30 ppb and quartz galanu C has two effects, Q, 6
% low refractive index, and the glass volatilization rate of this umbrella was 3%, which was less than Fl.
男1図は実施例1(−おけるヘキサフロロシシロキチン
のモル%と石英ガラス管の屈折率との関係をボ丁グラフ
を示したものである。
時計出願人 信越化学工業株式会社
代理人 弁理士 山 本 売 −
第1図
0 5
1゜S:20F6彷し%
〜・1Figure 1 is a box graph showing the relationship between the mole percent of hexafluorocysilochitin and the refractive index of the quartz glass tube in Example 1 (-). Applicant Shin-Etsu Chemical Co., Ltd. Agent Patent attorney Mr. Yamamoto Sales - Figure 1 0 5
1゜S: 20F6 Wandering% ~・1
Claims (1)
子を堆積させて多孔質のシリカ堆積体を形成させたのち
、これをオキシフッ化けい素を含む雰囲気中で、または
オキシフッ化けい素雰囲気にさらしたのち、加熱溶融し
て透明ガラス化することを特徴とする光伝送用ガラス母
材の製造方法。1. After depositing silica particles produced by flame hydrolysis of a silicon compound to form a porous silica deposit, this is exposed to an atmosphere containing silicon oxyfluoride or to a silicon oxyfluoride atmosphere. A method for producing a glass base material for optical transmission, which is then heated and melted to form transparent glass.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9596386A JPS62260728A (en) | 1986-04-25 | 1986-04-25 | Production of glass preform for optical transmission |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP9596386A JPS62260728A (en) | 1986-04-25 | 1986-04-25 | Production of glass preform for optical transmission |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS62260728A true JPS62260728A (en) | 1987-11-13 |
JPH0460056B2 JPH0460056B2 (en) | 1992-09-25 |
Family
ID=14151866
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP9596386A Granted JPS62260728A (en) | 1986-04-25 | 1986-04-25 | Production of glass preform for optical transmission |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS62260728A (en) |
Cited By (2)
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US20220041488A1 (en) * | 2020-08-06 | 2022-02-10 | Heraeus Quarzglas Gmbh & Co. Kg | Process for the preparation of fluorinated quartz glass |
JP2022031249A (en) * | 2020-08-06 | 2022-02-18 | ヘレウス・クアルツグラース・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツング・ウント・コンパニー・コマンディット・ゲゼルシャフト | Alternative fluorination agent for manufacturing fluorinated quartz glass |
-
1986
- 1986-04-25 JP JP9596386A patent/JPS62260728A/en active Granted
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20220041488A1 (en) * | 2020-08-06 | 2022-02-10 | Heraeus Quarzglas Gmbh & Co. Kg | Process for the preparation of fluorinated quartz glass |
KR20220018442A (en) * | 2020-08-06 | 2022-02-15 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | Process for the preparation of fluorinated quartz glass |
JP2022031249A (en) * | 2020-08-06 | 2022-02-18 | ヘレウス・クアルツグラース・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツング・ウント・コンパニー・コマンディット・ゲゼルシャフト | Alternative fluorination agent for manufacturing fluorinated quartz glass |
JP2022033708A (en) * | 2020-08-06 | 2022-03-02 | ヘレウス・クアルツグラース・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツング・ウント・コンパニー・コマンディット・ゲゼルシャフト | Method for manufacturing fluorinated quartz glass |
US11884571B2 (en) | 2020-08-06 | 2024-01-30 | Heraeus Quarzglas Gmbh & Co. Kg | Alternative fluorinating agents for the production of fluorinated quartz glass |
US11952302B2 (en) * | 2020-08-06 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Process for the preparation of fluorinated quartz glass |
Also Published As
Publication number | Publication date |
---|---|
JPH0460056B2 (en) | 1992-09-25 |
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