JP4663501B2 - Manufacturing method of quartz glass base material - Google Patents
Manufacturing method of quartz glass base material Download PDFInfo
- Publication number
- JP4663501B2 JP4663501B2 JP2005351651A JP2005351651A JP4663501B2 JP 4663501 B2 JP4663501 B2 JP 4663501B2 JP 2005351651 A JP2005351651 A JP 2005351651A JP 2005351651 A JP2005351651 A JP 2005351651A JP 4663501 B2 JP4663501 B2 JP 4663501B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- base material
- glass rod
- rod
- optical fiber
- 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.)
- Active
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 134
- 239000000463 material Substances 0.000 title claims description 59
- 238000004519 manufacturing process Methods 0.000 title claims description 19
- 239000011521 glass Substances 0.000 claims description 35
- 239000013307 optical fiber Substances 0.000 claims description 30
- 239000010419 fine particle Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 230000001678 irradiating effect Effects 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 230000007547 defect Effects 0.000 description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 235000019441 ethanol Nutrition 0.000 description 12
- 238000009987 spinning Methods 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 230000002093 peripheral effect Effects 0.000 description 10
- 238000000151 deposition Methods 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
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]
- C03B37/01486—Means for supporting, rotating or translating the preforms being formed, e.g. lathes
- C03B37/01493—Deposition substrates, e.g. targets, mandrels, start rods or tubes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Description
本発明は、光ファイバなどの光学部材の製造に好適に用いられる石英ガラス母材の製造方法に関する。 The present invention relates to a method for producing a quartz glass base material suitably used for producing an optical member such as an optical fiber.
光ファイバなどに用いられる石英ガラス母材は、光ファイバ用のコア部を含む石英ガラスロッド上に石英ガラス微粒子を堆積させて石英ガラス多孔質体を作製した後、該石英ガラス多孔質体を焼結炉に入れて透明ガラス化し、石英ガラス母材とする製造方法が用いられる。このようにして得られた石英ガラス母材を観察すると、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近に欠陥が生じる場合がある。ここで言う欠陥は、気泡、金属や無機物の微粒子などの異物が残留したものなどである。これは、雰囲気中に浮遊している不純物が石英ガラスロッド上に付着した影響と考えられている。石英ガラスロッド上に異物が付着した状態で、石英ガラス微粒子を堆積させた場合、一部は火炎に焙られて揮発するが、一部は残存しガラス中の異物となる。石英ガラス母材中の欠陥は、紡糸工程における断線やファイバの強度低下を招く等好ましくない。そのため、石英ガラスロッド上に付着する異物を低減することが重要である。 A quartz glass base material used for an optical fiber or the like is prepared by depositing quartz glass fine particles on a quartz glass rod including a core portion for an optical fiber to produce a quartz glass porous body, and then firing the quartz glass porous body. A manufacturing method is used in which the glass is made into a transparent glass by being put into a furnace and used as a quartz glass base material. When the quartz glass base material obtained in this way is observed, a defect may occur in the vicinity of the interface between the quartz glass rod, which is the starting base material, and the outer peripheral glass. The defects referred to here are bubbles, foreign matters such as metal and inorganic fine particles remaining, and the like. This is considered to be the effect of the impurities floating in the atmosphere adhering to the quartz glass rod. When the silica glass fine particles are deposited in a state where foreign matter is adhered on the quartz glass rod, a part of the silica glass is roasted and volatilized by a flame, but a part remains and becomes a foreign matter in the glass. Defects in the quartz glass base material are not preferable because they cause breakage in the spinning process and decrease in fiber strength. For this reason, it is important to reduce foreign substances adhering to the quartz glass rod.
従来、石英ガラス母材に含まれる欠陥を低減するための方法として、例えば、特許文献１，２に開示された方法が提案されている。 Conventionally, as a method for reducing defects contained in a quartz glass base material, for example, methods disclosed in Patent Documents 1 and 2 have been proposed.
特許文献１には、石英系ガラスロッドの外周面にガラス層を形成することにより新たなガラスロッドを得る工程を有する光ファイバ母材の製造方法において、該ガラス層が形成される前のガラスロッドをその外周面の最大粗さが０．５μｍ以下となるように機械的手段で処理し、次いで前記外周面を洗浄した後に前記ガラス層を形成することを特徴とする光ファイバ母材の製造方法が記載されている。この特許文献１では、石英ガラスロッド表面を機械的に研削し、ある表面粗さ以下とした後、洗浄することが、気泡の低減に効果があるとしている。 Patent Document 1 discloses a method of manufacturing an optical fiber preform having a step of obtaining a new glass rod by forming a glass layer on the outer peripheral surface of a silica-based glass rod, and the glass rod before the glass layer is formed. Is processed by a mechanical means so that the maximum roughness of the outer peripheral surface is 0.5 μm or less, and then the outer peripheral surface is washed, and then the glass layer is formed. Is described. In this patent document 1, it is said that cleaning after the surface of the quartz glass rod is mechanically ground to a certain surface roughness or less and then cleaned is effective.
特許文献２には、少なくとも光伝搬部を含む光ファイバ用ガラスロッドに、光ファイバ原料の微粉末を堆積させた後、これを加熱して透明ガラス化する光ファイバ用母材の製造方法において、前記光ファイバ用ガラスロッド上に光ファイバ原料の微粉末を堆積させる前に、前記光ファイバ用ガラスロッドの表面を洗浄剤、高純度水にて順次洗浄し、その後前記光ファイバ用ガラスロッドを５００ｒｐｍ以上で回転させ、付着している高純度水の水滴を切ることを特徴とする光ファイバ用母材の製造方法が記載されている。この特許文献２では、光ファイバ用ガラスロッドを水酸化アンモニウム溶液及び高純度水で洗浄後、該ガラスロッドを回転させて乾燥することでガラス表面の乾燥むら（水滴痕）を無くすことができ、気泡低減に効果があるとしている。
しかしながら、特許文献１に記載の方法は、以下の点で問題がある。機械研削によって表面状態を均一にすることはできるが、石英ガラスロッド表面に歪みを発生させる可能性がある。歪みが残った状態の石英ガラスロッドを酸水素火炎で焙ると、割れなどを生じる恐れがある。
また研削加工時に、砥粒の大きい粒子が混入すると、石英ガラスロッド表面に深い傷が発生する場合がある。傷が残った状態で石英ガラスロッド上に石英ガラス微粒子を堆積させると、却って気泡などの欠陥の原因となる。そのため再研削の必要が生じる等、工程管理に手間が掛かる可能性がある。
また光ファイバを製造する場合、光ファイバの接続損失を低下させるため、コア部の偏心量を小さくする必要がある。しかし、長さ１０００ｍｍ以上の石英ガラス母材を研削する場合は、母材の曲がりの影響も受けやすく、クラッド部が片削りになる可能性が高い。そのためコア部の偏心量が大きくなり、結果として得られた光ファイバの接続損失等が大きくなるため、好ましくない。
However, the method described in Patent Document 1 has problems in the following points. Although the surface state can be made uniform by mechanical grinding, there is a possibility of generating distortion on the surface of the quartz glass rod. If a quartz glass rod with strain remaining is roasted with an oxyhydrogen flame, cracking or the like may occur.
In addition, when large abrasive particles are mixed during grinding, deep scratches may occur on the surface of the quartz glass rod. If quartz glass fine particles are deposited on the quartz glass rod with scratches remaining, it causes defects such as bubbles. Therefore, there is a possibility that it takes time and effort to manage the process, such as the need for regrinding.
Moreover, when manufacturing an optical fiber, in order to reduce the connection loss of an optical fiber, it is necessary to make small the eccentric amount of a core part. However, when a quartz glass base material having a length of 1000 mm or more is ground, it is easily affected by the bending of the base material, and the cladding portion is likely to be cut away. For this reason, the amount of eccentricity of the core portion is increased, and the resulting connection loss of the optical fiber is increased, which is not preferable.
また特許文献２に記載の方法は、アルカリ溶液を用いているため、確かに石英ガラスロッド表面の洗浄効果は高い。しかし、乾燥時に母材を高速で回転させる必要があるため、ガラスが破損する恐れもある。また洗浄に用いるアルカリ溶液の廃液処理などに余分なコストがかかるなどの問題があった。 Moreover, since the method described in Patent Document 2 uses an alkaline solution, the cleaning effect on the surface of the quartz glass rod is certainly high. However, since it is necessary to rotate the base material at high speed during drying, the glass may be damaged. In addition, there is a problem that extra cost is required for the waste liquid treatment of the alkaline solution used for cleaning.
本発明は、前記事情に鑑みてなされ、石英ガラス母材に含まれる欠陥を低減することができ、歩留まり良く光ファイバを紡糸でき、低コストで光ファイバを提供できる石英ガラス母材の製造方法の提供を目的とする。 The present invention has been made in view of the above circumstances, and is a method for producing a quartz glass preform that can reduce defects contained in a quartz glass preform, spin an optical fiber with a high yield, and provide an optical fiber at a low cost. For the purpose of provision.
前記目的を達成するため、本発明は、光ファイバ用のコア部を含む石英ガラスロッド上に石英ガラス微粒子を堆積させて石英ガラス多孔質体とした後、該石英ガラス多孔質体を焼結して透明ガラス化し、石英ガラス母材を得る製造方法において、石英ガラス微粒子を堆積させる前の石英ガラスロッド表面の水に対する接触角が１０°以下であることを特徴とする石英ガラス母材の製造方法を提供する。 In order to achieve the above object, the present invention provides a quartz glass porous body by depositing quartz glass fine particles on a quartz glass rod including a core portion for an optical fiber, and then sintering the quartz glass porous body. The method for producing a quartz glass preform, wherein the quartz glass rod has a contact angle with water of 10 ° or less before the quartz glass fine particles are deposited in the production method for obtaining a quartz glass preform by converting into transparent glass. I will provide a.
本発明の石英ガラス母材の製造方法において、前記石英ガラスロッドに石英ガラス微粒子を堆積させる前に、石英ガラスロッド表面を有機溶媒で洗浄する第１の工程と、その後、石英ガラスロッド表面に紫外線を照射する第２の工程を行うことが好ましい。 In the method for producing a quartz glass base material of the present invention, the first step of washing the quartz glass rod surface with an organic solvent before depositing the quartz glass fine particles on the quartz glass rod, and then the ultraviolet ray on the quartz glass rod surface. It is preferable to perform the 2nd process of irradiating.
本発明の石英ガラス母材の製造方法において、前記第１の工程で用いる有機溶媒が炭素数３以下のアルコールから選択される１種又は２種以上であることが好ましい。 In the method for producing a quartz glass base material of the present invention, the organic solvent used in the first step is preferably one or more selected from alcohols having 3 or less carbon atoms.
本発明の石英ガラス母材の製造方法は、石英ガラス微粒子を堆積させる前の表面の水に対する接触角が１０°以下である石英ガラスロッドを用い、この表面に石英ガラス微粒子を堆積させて石英ガラス多孔質体を作製することによって、石英ガラス母材に含まれる欠陥を低減することができ、歩留まり良く光ファイバを紡糸でき、低コストで光ファイバを提供することができる。 The method for producing a quartz glass base material of the present invention uses a quartz glass rod having a contact angle with water of 10 ° or less on the surface before the quartz glass fine particles are deposited, and deposits the quartz glass fine particles on this surface to produce the quartz glass. By producing the porous body, defects contained in the quartz glass base material can be reduced, the optical fiber can be spun with a high yield, and the optical fiber can be provided at low cost.
本発明者らは、石英ガラスロッドとその外周部のガラスとの界面付近に発生する気泡や異物等の欠陥の元素分析を実施した。その結果、異物を構成する元素として、主にＮａやＣａ、炭素（Ｃ）などが検出されたことから、この異物はＮａやＣａを含む無機物と、何らかの有機物であることが分かった。これらの異物は、石英ガラス微粒子を堆積する前の石英ガラスロッドに付着し、石英ガラス微粒子を堆積し透明ガラス化後まで残留して欠陥となる。そのため、石英ガラス微粒子を堆積させる前に、石英ガラスロッド表面に付着した不純物を、あらかじめ除去する必要がある。 The present inventors conducted elemental analysis of defects such as bubbles and foreign matters generated near the interface between the quartz glass rod and the glass on the outer periphery thereof. As a result, Na, Ca, carbon (C), and the like were mainly detected as elements constituting the foreign matter, and it was found that the foreign matter was an inorganic substance containing Na or Ca and some organic substance. These foreign substances adhere to the quartz glass rod before the quartz glass fine particles are deposited, and the quartz glass fine particles are deposited and remain until transparent glass is formed to become defects. For this reason, it is necessary to remove impurities adhering to the surface of the quartz glass rod in advance before depositing the quartz glass fine particles.
本発明者らは、ガラス表面の清浄度の指標として、水に対する接触角に着目し、この接触角を小さくすることが重要であると考えた。
そのためには、石英ガラス微粒子を堆積させる前に、石英ガラスロッド表面をアルコールなどの有機溶媒で洗浄する第１の工程と、紫外線を照射する第２の工程を行うことで、石英ガラスロッド表面の水に対する接触角を小さくする効果が高いことがわかった。
The present inventors paid attention to the contact angle with water as an index of the cleanliness of the glass surface, and thought it was important to reduce this contact angle.
For that purpose, before depositing the quartz glass fine particles, the first step of washing the quartz glass rod surface with an organic solvent such as alcohol and the second step of irradiating ultraviolet rays are performed, thereby It was found that the effect of reducing the contact angle with water is high.
なお、本発明において「接触角」とは、図１に示すように、石英ガラスロッド１の表面に水滴２を滴下した際の、水滴の盛り上がり角度を測定し、これを接触角θとしている。接触角が小さいほど表面の異物が少ないことを意味する。一般に、表面に付着している物質が単分子層以下になると、接触角が４°になるとされている。 In the present invention, as shown in FIG. 1, the “contact angle” refers to the contact angle θ obtained by measuring the rising angle of the water droplet 2 when the water droplet 2 is dropped on the surface of the quartz glass rod 1. A smaller contact angle means less surface foreign matter. Generally, when the substance adhering to the surface becomes a monomolecular layer or less, the contact angle is assumed to be 4 °.
各種検討を行った結果、石英微粒子を堆積させる前の石英ガラスロッド表面の水に対する接触角を１０°以下とすることで、出発母材である石英ガラスロッドとその外周に形成されるガラスとの界面付近に欠陥が無い石英ガラス母材を得ることができた。この際、界面付近に存在する０．１ｍｍ以上の欠陥が、石英ガラス母材長で１ｍ当たり２個以下であれば、紡糸中に影響を及ぼすことはほぼ無くなる。実際には、以下の式で表す断線頻度について、１回／３００ｋｍ以下であれば、良好と判断できる。
断線頻度＝紡糸工程での断線頻度（回）／１母材の紡糸長（ｋｍ）
As a result of various studies, by setting the contact angle of water on the surface of the quartz glass rod before depositing the quartz fine particles to 10 ° or less, the quartz glass rod which is the starting base material and the glass formed on the outer periphery thereof are formed. A quartz glass base material having no defects near the interface was obtained. At this time, if the defects of 0.1 mm or more existing in the vicinity of the interface are two or less per 1 m in the length of the quartz glass base material, there is almost no influence during spinning. Actually, it can be determined that the disconnection frequency represented by the following formula is good if it is 1 time / 300 km or less.
Disconnection frequency = Disconnection frequency in spinning process (times) / 1 Spin length of base material (km)
第１の工程の有機溶媒による洗浄において、有機溶媒としては、メチルアルコール、エチルアルコール、イソプロピルアルコールなどのアルコール、アセトン、メチルエチルケトンなどのケトンなどを用いることができ、その中でも炭素数が３以下のアルコールから選択される１種または２種以上のアルコールが好ましく、とりわけエチルアルコールやイソプロピルアルコールが好ましい。この工程では、主にガラスロッド表面に付着している粒子径が０．５ｍｍ以上の有機物や無機物を除去できる。アルコール等の有機溶媒による洗浄は、発塵量の少ない不織布に有機溶媒を塗布し、直接石英ガラスロッドを拭くことでも可能であるが、石英ガラスロッドを有機溶媒中に浸漬して超音波洗浄する方法の方が、微粒子の除去効果が大きいため、望ましい。何れも場合も、液滴痕が残らないように乾燥させることが重要である。このためには、不織布で拭き取る際のスピードを遅くする。石英ガラスロッドを事前に保温しておくと液滴痕が残り難くなる。なお、一部液滴が残る場合もあるが、その多くは粒子径の小さい有機物であり、第２の工程で除去可能であるため問題はない。 In the washing with the organic solvent in the first step, as the organic solvent, alcohols such as methyl alcohol, ethyl alcohol and isopropyl alcohol, ketones such as acetone and methyl ethyl ketone, etc. can be used, among which alcohols having 3 or less carbon atoms. 1 type or 2 types or more of alcohol selected from these are preferable, and especially ethyl alcohol and isopropyl alcohol are preferable. In this step, organic substances and inorganic substances having a particle diameter of 0.5 mm or more mainly attached to the glass rod surface can be removed. Washing with an organic solvent such as alcohol can be done by applying the organic solvent to a non-woven fabric with a small amount of dust and wiping the quartz glass rod directly. However, the quartz glass rod is immersed in the organic solvent and cleaned ultrasonically. The method is desirable because it has a greater effect of removing fine particles. In either case, it is important to dry so as not to leave droplet marks. For this purpose, the speed when wiping with a non-woven fabric is reduced. If the quartz glass rod is kept warm in advance, the droplet traces are difficult to remain. Although some droplets may remain, most of them are organic substances having a small particle diameter, and there is no problem because they can be removed in the second step.
第２の工程は、第１の工程で除去できなかった粒子径の小さい有機物を除去することが目的である。この工程で使用する紫外線ランプは、紫外線が持つエネルギーによって、直接有機物を分解する効果がある。また、空気中の酸素（Ｏ２）からオゾン（Ｏ３）を生成し、そのオゾンから生成した活性酸素が有機物と反応し、ＣＯ２やＨ２Ｏ等を生成し、揮発除去するとされている。紫外線照射による有機物の分解除去の概要を図２に示す。 The purpose of the second step is to remove organic substances having a small particle diameter that could not be removed in the first step. The ultraviolet lamp used in this process has an effect of directly decomposing organic substances by the energy of ultraviolet rays. In addition, ozone (O 3 ) is generated from oxygen (O 2 ) in the air, and active oxygen generated from the ozone reacts with organic matter to generate CO 2 , H 2 O, etc., and is volatilized and removed. . An outline of decomposition and removal of organic substances by ultraviolet irradiation is shown in FIG.
照射する紫外線は、波長が短いほどエネルギーが高く、石英ガラスロッド表面と表面に付着した有機物との結合を切りやすい。実用的に用いられる紫外線ランプとしては、低圧水銀灯（波長１８５ｎｍ、波長２５４ｎｍ）、キセノンエキシマ光（波長１７２ｎｍ）などがある。
The shorter the wavelength, the higher the energy of the irradiated ultraviolet light, and the bond between the quartz glass rod surface and the organic matter attached to the surface is easy to break. Examples of ultraviolet lamps that are practically used include a low-pressure mercury lamp (
このように石英ガラスロッド表面の異物を除去することによって、石英ガラス微粒子を堆積させる前の石英ガラスロッド表面の水に対する接触角を小さくすることができる。その結果、この接触角を１０°以下とすることができれば、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近に気泡や異物等の欠陥は発生せず、良好な状態であることがわかった。 Thus, by removing the foreign matter on the surface of the quartz glass rod, the contact angle with respect to the water on the surface of the quartz glass rod before the quartz glass fine particles are deposited can be reduced. As a result, if this contact angle can be set to 10 ° or less, defects such as bubbles and foreign matters do not occur in the vicinity of the interface between the quartz glass rod, which is the starting base material, and the outer peripheral glass, and in a good state. I found out.
本発明の石英ガラス母材の製造方法は、石英ガラス微粒子を堆積させる前の表面の水に対する接触角が１０°以下である石英ガラスロッドを用い、この表面に石英ガラス微粒子を堆積させて石英ガラス多孔質体を作製することによって、石英ガラス母材に含まれる欠陥を低減することができ、歩留まり良く光ファイバを紡糸でき、低コストで光ファイバを提供することができる。
以下、実施例により本発明の効果を実証する。
The method for producing a quartz glass base material of the present invention uses a quartz glass rod having a contact angle with water of 10 ° or less on the surface before depositing the quartz glass fine particles, and deposits the quartz glass fine particles on this surface to produce the quartz glass. By producing the porous body, defects contained in the quartz glass base material can be reduced, the optical fiber can be spun with a high yield, and the optical fiber can be provided at low cost.
Hereinafter, the effects of the present invention will be demonstrated by examples.
［実施例１］
ＳｉＣｌ４流量：５．５〜７．５ＳＬＭ、水素ガス流量：４０〜１００ＳＬＭ、酸素ガス流量１５〜４０ＳＬＭ、シールガスとしてアルゴンガスを１ＳＬＭ、それぞれバーナに供給し、酸水素火炎中で石英ガラス微粒子を生成させ、火炎と共にバーナから噴出させた。
出発母材である石英ガラスロッドは、外径３５ｍｍの丸棒状のガラスロッドを用いた。石英ガラスロッドは、微粒子堆積前にエチルアルコールに浸漬し、超音波洗浄装置で洗浄後、紫外線ランプを３００秒照射した。このときの紫外線照射量は、石英ガラスロッド表面で１０ｍＷ／ｃｍ２であった。処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は９°であった。
その後、複数のバーナを用いて、経時的に石英ガラス微粒子を石英ガラスロッド上に堆積させ、外径２３０ｍｍ×長さ１８００ｍｍの石英ガラス多孔質母材を作製した。石英ガラス多孔質母材作製後、焼結炉に投入し、透明ガラス化して石英ガラス母材とした。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は０個であり、良好な結果が得られた。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は０．５回／３００ｋｍであり、良好であった。
[Example 1]
SiCl 4 flow rate: 5.5 to 7.5 SLM, hydrogen gas flow rate: 40 to 100 SLM, oxygen gas flow rate 15 to 40 SLM, argon gas 1 SLM as seal gas, each supplied to burner, quartz glass fine particles in oxyhydrogen flame It was generated and ejected from the burner along with the flame.
A quartz glass rod as a starting base material was a round rod-shaped glass rod having an outer diameter of 35 mm. The quartz glass rod was immersed in ethyl alcohol before depositing the fine particles, cleaned with an ultrasonic cleaning device, and then irradiated with an ultraviolet lamp for 300 seconds. The amount of ultraviolet irradiation at this time was 10 mW / cm 2 on the surface of the quartz glass rod. As a result of measuring the contact angle on the surface of the quartz glass rod after the treatment, the contact angle was 9 °.
Thereafter, using a plurality of burners, quartz glass fine particles were deposited over time on a quartz glass rod to produce a porous silica glass base material having an outer diameter of 230 mm × length of 1800 mm. After the production of the quartz glass porous base material, it was put into a sintering furnace and converted into a transparent glass to obtain a quartz glass base material.
About the obtained quartz glass base material, when the number of defects near the interface between the quartz glass rod as the starting base material and the glass at the outer peripheral portion thereof was confirmed, the number of defects per 1 m of the base material length was 0, which was favorable. Results were obtained.
This quartz glass base material was set in an optical fiber spinning device and spun. As a result, the disconnection frequency was 0.5 times / 300 km, which was good.
［実施例２］
紫外線ランプの照射時間を３６０秒としたこと以外は、実施例１と同様の方法で、石英ガラス母材を製造した。
処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は８°であった。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は１個であり、良好な結果が得られた。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は０．６回／３００ｋｍであり、良好であった。
[Example 2]
A quartz glass base material was produced in the same manner as in Example 1 except that the irradiation time of the ultraviolet lamp was set to 360 seconds.
As a result of measuring the contact angle on the surface of the quartz glass rod after the treatment, the contact angle was 8 °.
About the obtained quartz glass base material, when the number of defects in the vicinity of the interface between the quartz glass rod as the starting base material and the outer peripheral portion of the glass was confirmed, the number of defects per 1 m of the base material length was 1 and good. Results were obtained.
The quartz glass base material was set in an optical fiber spinning device and spun. As a result, the disconnection frequency was 0.6 times / 300 km, which was favorable.
［実施例３］
石英ガラスロッドのアルコール洗浄を、不織布にアルコールを塗布して拭き取り洗浄としたこと以外は、実施例１と同様の方法で、石英ガラス母材を製造した。
処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は１０°であった。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は２個であり、良好な結果が得られた。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は０．８回／３００ｋｍであり、良好であった。
[Example 3]
A quartz glass base material was produced in the same manner as in Example 1 except that the quartz glass rod was washed with alcohol by wiping the nonwoven fabric with alcohol.
As a result of measuring the contact angle on the surface of the quartz glass rod after the treatment, the contact angle was 10 °.
About the obtained quartz glass base material, when the number of defects in the vicinity of the interface between the quartz glass rod as the starting base material and the glass on the outer peripheral portion thereof was confirmed, the number of defects per 1 m of the base material length was 2 and good. Results were obtained.
This quartz glass base material was set in an optical fiber spinning device and spun. As a result, the disconnection frequency was 0.8 times / 300 km, which was good.
［比較例１］
石英ガラスロッドのアルコール洗浄を行わなかったこと以外は、実施例１と同様の方法で、石英ガラス母材を製造した。
処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は２２°であった。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は６個であった。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は３．２回／３００ｋｍであり、歩留まりが低下した。
[Comparative Example 1]
A quartz glass base material was produced in the same manner as in Example 1 except that the quartz glass rod was not washed with alcohol.
As a result of measuring the contact angle on the surface of the quartz glass rod after the treatment, the contact angle was 22 °.
When the number of defects in the vicinity of the interface between the quartz glass rod, which is the starting base material, and the glass at the outer peripheral portion of the obtained silica glass base material was confirmed, the number of defects per 1 m of the base material length was 6.
As a result of setting and spinning this quartz glass base material in an optical fiber spinning device, the frequency of disconnection was 3.2 times / 300 km, and the yield decreased.
［比較例２］
紫外線ランプの照射時間を２４０秒としたこと以外は、実施例１と同様の方法で、石英ガラス母材を製造した。
処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は１３°であった。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は４個であった。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は１．５回／３００ｋｍであり、歩留まりが低下した。
[Comparative Example 2]
A quartz glass base material was produced in the same manner as in Example 1 except that the irradiation time of the ultraviolet lamp was 240 seconds.
As a result of measuring the contact angle on the surface of the quartz glass rod after the treatment, the contact angle was 13 °.
When the number of defects in the vicinity of the interface between the quartz glass rod, which is the starting base material, and the glass at the outer periphery thereof was confirmed for the obtained quartz glass base material, the number of defects per meter length of the base material was four.
As a result of setting and spinning this quartz glass base material in an optical fiber spinning device, the frequency of disconnection was 1.5 times / 300 km, and the yield decreased.
［比較例３］
紫外線ランプの照射時間を６０秒としたこと以外は、実施例１と同様の方法で、石英ガラス母材を製造した。
処理後の石英ガラスロッド表面の接触角を測定した結果、接触角は１９°であった。
得られた石英ガラス母材について、出発母材である石英ガラスロッドとその外周部のガラスとの界面付近の欠陥数を確認したところ、母材長１ｍ当たり欠陥数は５個であった。その内１個は、０．３ｍｍ以上の大きい欠陥であった。
この石英ガラス母材を光ファイバ紡糸装置にセットし、紡糸した結果、断線頻度は２．２回／３００ｋｍであり、歩留まりが低下した。
[Comparative Example 3]
A quartz glass base material was produced in the same manner as in Example 1 except that the irradiation time of the ultraviolet lamp was set to 60 seconds.
As a result of measuring the contact angle of the quartz glass rod surface after the treatment, the contact angle was 19 °.
When the number of defects in the vicinity of the interface between the quartz glass rod, which is the starting base material, and the glass on the outer peripheral portion of the obtained quartz glass base material was confirmed, the number of defects per meter length of the base material was 5. One of them was a large defect of 0.3 mm or more.
As a result of setting and spinning this quartz glass base material in an optical fiber spinning device, the frequency of disconnection was 2.2 times / 300 km, and the yield was lowered.
１…石英ガラスロッド、２…水滴。
1 ... quartz glass rod, 2 ... water droplets.
Claims (3)
石英ガラス微粒子を堆積させる前の石英ガラスロッド表面の水に対する接触角が１０°以下であることを特徴とする石英ガラス母材の製造方法。 Silica glass fine particles are deposited on a quartz glass rod including a core portion for an optical fiber to form a quartz glass porous body, and then the quartz glass porous body is sintered to form a transparent glass to obtain a quartz glass base material. In the manufacturing method,
A method for producing a quartz glass base material, characterized in that the contact angle of water on the surface of the quartz glass rod before the quartz glass fine particles are deposited is 10 ° or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005351651A JP4663501B2 (en) | 2005-12-06 | 2005-12-06 | Manufacturing method of quartz glass base material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005351651A JP4663501B2 (en) | 2005-12-06 | 2005-12-06 | Manufacturing method of quartz glass base material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2007153679A JP2007153679A (en) | 2007-06-21 |
| JP4663501B2 true JP4663501B2 (en) | 2011-04-06 |
Family
ID=38238494
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2005351651A Active JP4663501B2 (en) | 2005-12-06 | 2005-12-06 | Manufacturing method of quartz glass base material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP4663501B2 (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58145643A (en) * | 1982-02-24 | 1983-08-30 | Sharp Corp | Cleaning of indium-tin glass plate |
| JPS62132737A (en) * | 1985-12-04 | 1987-06-16 | Mitsubishi Cable Ind Ltd | Production of multiple optical fiber |
| JPH05323131A (en) * | 1992-05-20 | 1993-12-07 | Furukawa Electric Co Ltd:The | Production of optical fiber base material |
| JPH09194226A (en) * | 1996-01-19 | 1997-07-29 | Furukawa Electric Co Ltd:The | Production of optical fiber preform |
| JP2001293442A (en) * | 2000-04-17 | 2001-10-23 | Canon Inc | Method for cleaning optical device |
| JP2001342041A (en) * | 2000-05-31 | 2001-12-11 | Asahi Glass Co Ltd | Optical part and its cleansing method |
| JP2003024891A (en) * | 2001-07-17 | 2003-01-28 | Canon Inc | Method and apparatus for cleaning material for optical device |
| JP2003073139A (en) * | 2001-09-04 | 2003-03-12 | Furukawa Electric Co Ltd:The | Method for producing optical fiber preform |
| JP2003300028A (en) * | 2002-04-09 | 2003-10-21 | Japan Storage Battery Co Ltd | Method and apparatus for manufacturing clean substrate |
| JP2004315290A (en) * | 2003-04-16 | 2004-11-11 | Shin Etsu Chem Co Ltd | Method for manufacturing glass rod |
-
2005
- 2005-12-06 JP JP2005351651A patent/JP4663501B2/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58145643A (en) * | 1982-02-24 | 1983-08-30 | Sharp Corp | Cleaning of indium-tin glass plate |
| JPS62132737A (en) * | 1985-12-04 | 1987-06-16 | Mitsubishi Cable Ind Ltd | Production of multiple optical fiber |
| JPH05323131A (en) * | 1992-05-20 | 1993-12-07 | Furukawa Electric Co Ltd:The | Production of optical fiber base material |
| JPH09194226A (en) * | 1996-01-19 | 1997-07-29 | Furukawa Electric Co Ltd:The | Production of optical fiber preform |
| JP2001293442A (en) * | 2000-04-17 | 2001-10-23 | Canon Inc | Method for cleaning optical device |
| JP2001342041A (en) * | 2000-05-31 | 2001-12-11 | Asahi Glass Co Ltd | Optical part and its cleansing method |
| JP2003024891A (en) * | 2001-07-17 | 2003-01-28 | Canon Inc | Method and apparatus for cleaning material for optical device |
| JP2003073139A (en) * | 2001-09-04 | 2003-03-12 | Furukawa Electric Co Ltd:The | Method for producing optical fiber preform |
| JP2003300028A (en) * | 2002-04-09 | 2003-10-21 | Japan Storage Battery Co Ltd | Method and apparatus for manufacturing clean substrate |
| JP2004315290A (en) * | 2003-04-16 | 2004-11-11 | Shin Etsu Chem Co Ltd | Method for manufacturing glass rod |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2007153679A (en) | 2007-06-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1107031C (en) | Process for producing glass preform for optical fiber | |
| JP4663501B2 (en) | Manufacturing method of quartz glass base material | |
| TWI608997B (en) | Nanoimprint mold-forming synthetic quartz glass and making method | |
| JP3023849B2 (en) | Method and apparatus for producing erbium-doped optical fiber | |
| KR100445046B1 (en) | Core glass for a preform for an optical fiber, preform made from the core glass, and method for making the core glass and an optical fiber | |
| JP5523465B2 (en) | Method for producing tubular semi-finished product made of quartz glass, method for producing optical components using the semi-finished product, and semi-finished product comprising fluorine-doped quartz glass | |
| JP3551006B2 (en) | Method for producing porous preform for optical fiber | |
| JP4297320B2 (en) | Cleaning method for optical fiber preform | |
| TW564242B (en) | Porous optical fiber base materials, optical fiber base materials and methods for producing them | |
| JP4494325B2 (en) | Manufacturing method of glass preform for optical fiber | |
| JP5995646B2 (en) | Manufacturing method of optical fiber preform and manufacturing method of hole structure optical fiber | |
| JP4107905B2 (en) | Synthetic silica glass optical material for YAG laser harmonics | |
| JP2006327858A (en) | Method of treating quartz glass base material and method of manufacturing optical fiber preform | |
| JP5380018B2 (en) | Optical fiber preform manufacturing method | |
| JP4663487B2 (en) | Manufacturing method of glass preform for optical fiber | |
| JP4536385B2 (en) | Photocatalyst-supporting optical fiber manufacturing method and photocatalyst-supporting optical fiber manufacturing apparatus | |
| JP2003212550A (en) | Method of manufacturing glass tube and target rod for the same | |
| JP2985667B2 (en) | Method for producing glass preform for optical fiber | |
| JP5204194B2 (en) | Formation of microstructured fiber preforms by porous glass deposition | |
| JP2005029399A (en) | Method for manufacturing glass particulate deposit | |
| JP2002020135A (en) | Method for manufacturing optical fiber | |
| JP2001294440A (en) | Method for manufacturing preform ingot for optical fiber and preform for optical fiber obtained by processing this preform ingot | |
| JP2004345902A (en) | Method for manufacturing quartz glass, quartz glass, optic component and optical fiber | |
| JP3051393B1 (en) | Manufacturing method of optical fiber preform | |
| JP2006321694A (en) | Method of manufacturing optical fiber preform |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20080528 |
|
| A977 | Report on retrieval |
Free format text: JAPANESE INTERMEDIATE CODE: A971007 Effective date: 20091118 |
|
| A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20091208 |
|
| A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20100208 |
|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20101220 |
|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20110105 |
|
| R151 | Written notification of patent or utility model registration |
Ref document number: 4663501 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R151 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20140114 Year of fee payment: 3 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |