JPH0416524A - Production of fluoride optical fiber - Google Patents
Production of fluoride optical fiberInfo
- Publication number
- JPH0416524A JPH0416524A JP11899990A JP11899990A JPH0416524A JP H0416524 A JPH0416524 A JP H0416524A JP 11899990 A JP11899990 A JP 11899990A JP 11899990 A JP11899990 A JP 11899990A JP H0416524 A JPH0416524 A JP H0416524A
- Authority
- JP
- Japan
- Prior art keywords
- fluoride
- optical fiber
- glass
- mol
- fluoride glass
- 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
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims abstract description 31
- 239000013307 optical fiber Substances 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000005383 fluoride glass Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 229920006356 Teflon™ FEP Polymers 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 28
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 16
- 229910052731 fluorine Inorganic materials 0.000 claims description 16
- 239000011737 fluorine Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011521 glass Substances 0.000 abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 6
- 239000012298 atmosphere Substances 0.000 abstract description 4
- 238000005266 casting Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 2
- 229910006213 ZrOCl2 Inorganic materials 0.000 abstract 1
- 239000008246 gaseous mixture Substances 0.000 abstract 1
- 239000006060 molten glass Substances 0.000 abstract 1
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 13
- 230000005540 biological transmission Effects 0.000 description 12
- 239000000835 fiber Substances 0.000 description 12
- 238000010521 absorption reaction Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000005253 cladding Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- 229910001632 barium fluoride Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000156 glass melt Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000003746 surface roughness Effects 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
- C03B37/01265—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt
-
- 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
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/80—Non-oxide glasses or glass-type compositions
- C03B2201/82—Fluoride glasses, e.g. ZBLAN glass
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明はフッ化物光ファイバの製造方法、さらに詳細に
は低損失かつ高強度のフッ化物光ファイバの製造方法に
関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method of manufacturing a fluoride optical fiber, and more particularly to a method of manufacturing a fluoride optical fiber with low loss and high strength.
（従来の技術）
フッ化物光ファイバは石英系を凌ぐ１Ｏ−２ｄＢ／ｋｍ
以下の伝送損失が期待されており、長距離無中継が可能
な伝送媒体として有望視されている。(Conventional technology) Fluoride optical fiber has a 1O-2 dB/km performance that exceeds that of quartz fiber.
The following transmission loss is expected, and it is seen as a promising transmission medium capable of long-distance non-relaying.
しかし、フッ化物ガラスは空気中の水分と反応し、表面
に吸収損失の原因となるＯＨ基が生成しやすく、また線
引き時の加熱によりＯＨ基の脱水縮合により散乱損失の
原因となる酸化物結晶が生成し伝送特性が劣化するとい
う欠点があった。さらに酸化物結晶の生成によりファイ
バの強度が著しく低下するという欠点もあった。However, fluoride glass reacts with moisture in the air, easily producing OH groups on its surface that cause absorption loss, and oxide crystals that cause scattering loss due to dehydration and condensation of OH groups during heating during drawing. This has the disadvantage that the transmission characteristics are deteriorated due to the generation of Furthermore, there was also the disadvantage that the strength of the fiber was significantly reduced due to the formation of oxide crystals.
これまで母材の表面処理法としては、研磨後の母材をオ
キシ塩化ジルコニウムの塩酸溶液中で表面をケミカルエ
ツチングした後、不活性ガス中で乾燥する方法または乾
燥後に含フッ素ガスを放電ガスとするプラズマ中で表面
処理する方法が取られていた。Up until now, the surface treatment methods for the base material include chemical etching the surface of the base material after polishing in a hydrochloric acid solution of zirconium oxychloride, and then drying it in an inert gas, or using a fluorine-containing gas as a discharge gas after drying. A method of surface treatment in plasma was used.
（発明が解決する問題点）
しかし、不活性ガス中での乾燥では表面ＯＨ基を効率よ
く除去することはできず、脱水縮合による酸素不純物の
残留が生じ、その後の線引きでの酸化物結晶の生成を抑
制することはできなかった。(Problems to be Solved by the Invention) However, drying in an inert gas cannot efficiently remove surface OH groups, and oxygen impurities remain due to dehydration condensation. It was not possible to suppress the production.
一方、プラズマ処理では高エネルギの粒子にガラス表面
がさらされるため°、イオンによる表面のスパッタリン
グが生じ表面あれの原因となったり、吸収損失の原因と
なる欠陥が生じるなどの問題があった。On the other hand, plasma treatment exposes the glass surface to high-energy particles, which causes problems such as sputtering of the surface by ions, which causes surface roughness, and defects that cause absorption loss.
（発明の目的）
本発明の目的は、上記欠点を解決した低損失かつ高強度
のフッ化物光ファイバの製造方法を提供することにある
。(Object of the Invention) An object of the present invention is to provide a method for manufacturing a fluoride optical fiber with low loss and high strength, which solves the above-mentioned drawbacks.
（問題点を解決するための手段）
上記問題点を解決するために、本発明にょるフッ化物光
ファイバの製造方法は、フッ化物ガラス母材を線引きし
てフッ化物光ファイバを作製する工程およびフッ化物ガ
ラス母材まなはコア組成のフッ化物ガラスロッドをフッ
化物ガラスまたはテフロンＦＥＰのパイプの中に挿入し
線引きすることによりフッ化物光ファイバを作製する工
程において、該フッ化物ガラス母材、該フッ化物ガラス
ロッド、該フッ化物ガラスパイプの一部または全部を含
フッ素ガス中で加熱処理した後、線引きすることを特徴
とするものである。(Means for Solving the Problems) In order to solve the above problems, the method for producing a fluoride optical fiber according to the present invention includes a step of drawing a fluoride glass base material to produce a fluoride optical fiber; In the process of producing a fluoride optical fiber by inserting a fluoride glass rod having a fluoride glass base material or core composition into a fluoride glass or Teflon FEP pipe and drawing it, the fluoride glass base material, the The method is characterized in that a part or all of the fluoride glass rod and the fluoride glass pipe are heated in a fluorine-containing gas and then drawn.
すなわち、ケミカルエツチングを施し不活性ガス中また
は減圧下で乾燥した母材またはガラスチューブの表面を
含フッ素ガス中で加熱処理することを特徴とする。That is, it is characterized in that the surface of the base material or glass tube, which has been chemically etched and dried in an inert gas or under reduced pressure, is heat-treated in a fluorine-containing gas.
本発明をさらに詳しく説明する。The present invention will be explained in more detail.
本発明によれば、前述のように、フッ化物ガラス母材、
フッ化物ガラスロッド、フッ化物ガラスパイプの一部又
は全部をフッ化物ガスで加熱処理するものであるが、こ
のフッ化物ガスは表面ＯＨ基が除去できるようなフッ化
物ガスであれば、本発明において基本的に限定されるも
のではない。According to the present invention, as described above, a fluoride glass base material,
A part or all of the fluoride glass rod or fluoride glass pipe is heat-treated with fluoride gas, and in the present invention, as long as the fluoride gas is a fluoride gas that can remove surface OH groups, Basically, it is not limited.
たとえば、含フッ素ガスがフッ素かまたは水素、炭素、
ホウ素、窒素、塩素、臭素、ヨウ素、イオウのうち少な
くともいずれが１つとフッ素の化合物のガスであり、該
含フッ素ガスのいずれが１つまたは２つ以上の混合ガス
であることができる。For example, if the fluorine-containing gas is fluorine, hydrogen, carbon,
The gas is a compound of fluorine and at least one of boron, nitrogen, chlorine, bromine, iodine, and sulfur, and any one of the fluorine-containing gases can be a mixed gas of two or more.
具体例部しては、たとえばＨＦ、ＣＦ４、ＮＦ３、ＳＦ
ｂ、ＢＦ３、Ｆ２などの一種以上を挙げることができる
。Specific examples include HF, CF4, NF3, SF
b, BF3, F2, and the like.
さらに、含フッ化物ガスでの処理温度は、０〜４００℃
であるのが好ましい、０℃未満であると、温度が低すぎ
て含フッ化物ガスが活性化しない恐れがあり、４００℃
を越えると処理されるフッ化物ガラスが結晶化する恐れ
がある６
（実施例）
以下、本発明を実施例によって詳細に説明するが、本発
明はこれにより何等限定されるものではない。Furthermore, the treatment temperature with fluoride-containing gas is 0 to 400°C.
If the temperature is less than 0°C, the fluoride-containing gas may not be activated because the temperature is too low;
If the fluoride glass is exceeded, there is a risk that the fluoride glass to be treated may crystallize.6 (Example) The present invention will be explained in detail below with reference to Examples, but the present invention is not limited thereto in any way.
（実施例１）
ガラス融液を円筒状の鋳型にキャスティングし急冷する
ことにより作製したコア組成（４９モル％ＺｒＦ４−２
５モル％ＢａＦ２−３．５モル％ＬａＦ３−２モル％Ｙ
Ｆ３−２．５モル％ＡｌＦ３−１８モル％ＬｉＦ）を有
するガラスロッド（直径６ｍｍ、１５０ｍｍ長）および
ローテイシラナルキャスティング法（Ｄ、Ｃ，Ｔｒａｎ
ｅｔ、 ａｔ。(Example 1) Core composition (49 mol% ZrF4-2) produced by casting a glass melt into a cylindrical mold and rapidly cooling it
5 mol% BaF2-3.5 mol%LaF3-2 mol%Y
A glass rod (diameter 6 mm, 150 mm length) with F3-2.5 mol% AlF3-18 mol% LiF) and a rotary silanal casting method (D, C, Tran
et, at.
Ｅｌｅｃｔｒｏｎ、 Ｌｅｔｔ ｖｏｌ １ｇ、 Ｐ、
５９． （１９８２） ）で作製したクラッド組成（
４７，５モル％ＺｒＦ４−２３．５モル％ＢａＦ２−２
．５モル％ＬａＦ３−２モル％ＹＦ３−４．５モル％Ａ
ＩＦ−２０モル％ＬｉＦ）を有するガラスチューブ（外
径１２ｍｍ、内径６ｍｍ、１５０ｍｍ長）をオキシ塩化
ジルコニウムの塩酸溶液でエツチングし水洗後減圧乾燥
した。これらのロッドおよびガラスチューブをＨＦ （
５０ｖｏ １％） Ｈｅ （５０ｖｏ １％）雰囲気
（１１／ｍ１ｎ）で２００℃に加熱し１０時間保持した
。その後、雰囲気をＡｒガスに置換し室温まで炉冷した
。このようにして処理した母材を窒素雰囲気下でガラス
チューブ内に挿入しテフロンＦＥＰを被覆材に用い線引
きし、７００ｍのフッ化物光ファイバを得た。得られた
ファイバの伝送損失特性の測定結果を第１図に示す。な
お、比較のために、ＨＦガス処理を行わなかった以外は
、本実施例と同様の方法で作製したフッ化物光ファイバ
の損失特性も併記した。この図で明らかなように、従来
法で作製したファイバには２．９μｍ付近にＯＨ基によ
る大きい吸収ピークが見られ、また波長に依存しない散
乱損失が顕著である。Electron, Lett vol 1g, P,
59. (1982)) cladding composition (
47.5 mol% ZrF4-23.5 mol% BaF2-2
．． 5 mol%LaF3-2 mol%YF3-4.5 mol%A
A glass tube (outer diameter 12 mm, inner diameter 6 mm, length 150 mm) containing IF-20 mol % LiF) was etched with a hydrochloric acid solution of zirconium oxychloride, washed with water, and then dried under reduced pressure. These rods and glass tubes were heated in HF (
50vo 1%) He (50vo 1%) atmosphere (11/m1n) was heated to 200° C. and held for 10 hours. Thereafter, the atmosphere was replaced with Ar gas and the furnace was cooled to room temperature. The base material treated in this manner was inserted into a glass tube under a nitrogen atmosphere, and was drawn using Teflon FEP as a coating material to obtain a 700 m fluoride optical fiber. Figure 1 shows the measurement results of the transmission loss characteristics of the obtained fiber. For comparison, the loss characteristics of a fluoride optical fiber produced in the same manner as in this example except that no HF gas treatment was performed are also shown. As is clear from this figure, the fiber produced by the conventional method has a large absorption peak due to OH groups near 2.9 μm, and also has significant wavelength-independent scattering loss.
このＯＨ基はコアロッド表面およびガラスチューブ内面
に吸着しているＯＨ基が残留した結果であり、また波長
に依存しない散乱損失はこれらＯＨ基の一部が脱水縮合
して生成した酸化物結晶によるものである０本実施例で
作製したファイバは、ＯＨ基による吸収ピークが大幅に
低減されており、さらに波長に依存しない散乱損失も低
減されていることから、ＨＦガス処理により表面に吸着
している水、ＯＨ基などの酸素不純物が除去できること
がわかる。さらに、得られたファイバをゲージ長１ｍ、
引っ張り速度５９ｍ、ｍ／ｍ ｉ ｎ、試料数５０本で
引っ張り試験を行った。引っ張り強度の平均値は１．０
ＧＰａで、従来法で作製したファイバの４００ＭＰａに
比べ大幅に向上した。This OH group is the result of residual OH groups adsorbed on the core rod surface and the inner surface of the glass tube, and the wavelength-independent scattering loss is due to oxide crystals generated by dehydration and condensation of some of these OH groups. In the fiber produced in this example, the absorption peak due to OH groups is significantly reduced, and the wavelength-independent scattering loss is also reduced. It can be seen that oxygen impurities such as water and OH groups can be removed. Furthermore, the obtained fiber was given a gauge length of 1 m,
A tensile test was conducted at a tensile speed of 59 m, m/min, and 50 samples. The average value of tensile strength is 1.0
The GPa was significantly improved compared to the 400 MPa of the fiber produced using the conventional method.
この方法において、ＨＦガスの代わりにＣＦ４、ＮＦ３
、ＳＦ６、ＢＦ３を用いてもＨＦガスと同様の効果が得
られた。In this method, CF4, NF3 is used instead of HF gas.
, SF6, and BF3 also produced similar effects to those of HF gas.
（実施例２）
コア／クラッド構造を有する（コア組成＝４９モル％Ｚ
ｒＦ４−２５モル％ＢａＦ２−３．５モル％ＬａＦ３−
２モル％ＹＦ３−２．５モル％ＡｌＦ３−１８モル％Ｌ
ｉＦ、クラッド組成＝４７．５モル％ＺｒＦ４−２３．
５モル％Ｂａ、Ｆ２−２．５モル％ＬａＦ３−２モル％
ＹＦ３−４．５モル％ＡｌＦ３−２０モル％ＮａＦ）直
径６ｍｍ、１５０ｍｍ長の母材を用い、含フッ素ガスと
してＡｒで希釈したＦ２ガス（Ｆ２ （５０ＶＯ１％）
−Ａｒ （５０ｖｏ １％））を用い、処理温度を冷却
により０℃とした以外は実施例１と同様の方法でフッ化
物光ファイバを作製した０作製したファイバの伝送損失
特性を第２図に示す０作製したファイバは最低損失０．
７ｄＢ／ｋｍであり、フッ素処理により酸素不純物の除
去が可能であることが明らかになった。引っ張り試験に
より得られた平均値は１．ＩＧＰａでありこの方法によ
り高強度のファイバが得られた。(Example 2) Having a core/clad structure (core composition = 49 mol% Z
rF4-25 mol% BaF2-3.5 mol% LaF3-
2 mol% YF3-2.5 mol% AlF3-18 mol%L
iF, cladding composition = 47.5 mol% ZrF4-23.
5 mol%Ba, F2-2.5 mol%LaF3-2 mol%
Using a base material with a diameter of 6 mm and a length of 150 mm, F2 gas (F2 (50 VO 1%) diluted with Ar as a fluorine-containing gas) was used.
A fluoride optical fiber was fabricated in the same manner as in Example 1, except that the treatment temperature was 0°C by cooling. The transmission loss characteristics of the fabricated fiber are shown in Figure 2. The fabricated fiber shown below has a minimum loss of 0.
7 dB/km, indicating that oxygen impurities can be removed by fluorine treatment. The average value obtained by the tensile test was 1. IGPa, and a high-strength fiber was obtained by this method.
（実施例３）
５３モル％ＺｒＦ４−２０モル％ＢａＦ２−４モル％Ｌ
ａＦ３−３モル％ＡＩＦ−２０モル％ＮａＦの組成の直
径８ｍｍのガラスロッドをコア、テフロンＦＥＰをクラ
ッドとし、含フッ素ガスとしてＨＦ （５０ｖｏ １％
） Ｆ２（５０ｖｏ１％）、処理温度として１００
℃とした以外は実施例１の方法と同様の方法で３００ｍ
のフッ化物光ファイバを作製した０作製したファイバの
伝送損失特性を第３図に示す、この図から明らかなよう
に、２．９μｍ付近のＯＨ基の吸収が大幅に低減できた
。また、ＨＦとＦ２を混合することにより、単独のガス
で処理する場合に比べ低温でも効率よく酸素不純物を除
去できた。(Example 3) 53 mol% ZrF4-20 mol%BaF2-4 mol%L
aF3-3 mol% AIF-20 mol% NaF glass rod with a diameter of 8 mm was used as the core, Teflon FEP was used as the cladding, and HF (50vo 1%) was used as the fluorine-containing gas.
) F2 (50vo1%), 100 as processing temperature
300 m in the same manner as in Example 1 except that the temperature was
Figure 3 shows the transmission loss characteristics of the fabricated fluoride optical fiber.As is clear from this figure, the absorption of OH groups around 2.9 μm was significantly reduced. Furthermore, by mixing HF and F2, oxygen impurities could be removed more efficiently even at lower temperatures than when treating with a single gas.
この方法において、コアガラスをＨｆＦ４−ＢａＦ２を
主成分とするフッ化物ガラスとしても上記実施例と同様
にＯＨ基による吸収損失、酸化物による散乱損失および
強度低下を大幅に低減することができた。In this method, absorption loss due to OH groups, scattering loss due to oxides, and strength reduction were able to be significantly reduced even when the core glass was a fluoride glass mainly composed of HfF4-BaF2, as in the above example.
（実施例４）
組成２２モル％ＢａＦ２−２２モル％ＣａＦ２−１６モ
ル％ＹＦ３−４０モル％ＡｌＦ３の直径８ｍｍのガラス
ロッドをコア、テフロンＦＥＰをクラッドとし、含フッ
素ガスとしてＳＦ６、処理温度として４００℃とした以
外は実施例１と同様の方法でフッ化物光ファイバを作製
した。作製したファイバの伝送特性を第４図に示す。こ
の図から明らかなように、２．９μｍ付近のＯＨ基によ
る吸収が大幅に低減でき、波長に依存しない散乱損失も
低減されていることがわかる。このファイバの引っ張り
強度は１．０ＧＰａであり、本実施例の方法により低損
失かつ高強度のフッ化物光ファイバが得られた。(Example 4) Composition 22 mol% BaF2 - 22 mol% CaF2 - 16 mol% YF3 - 40 mol% AlF3 glass rod with a diameter of 8 mm was used as the core, Teflon FEP was used as the cladding, SF6 was used as the fluorine-containing gas, and the processing temperature was 400°C. A fluoride optical fiber was produced in the same manner as in Example 1 except that the temperature was changed to .degree. Figure 4 shows the transmission characteristics of the fabricated fiber. As is clear from this figure, absorption by OH groups near 2.9 μm can be significantly reduced, and scattering loss independent of wavelength is also reduced. The tensile strength of this fiber was 1.0 GPa, and a low-loss, high-strength fluoride optical fiber was obtained by the method of this example.
（発明の効果）
以上の実施例に示したように、本発明の方法を用いるこ
とにより、母材表面およびジャケットとして使用するガ
ラスチューブ表面に吸着した酸素不純物を除去すること
ができるため従来は困難であった低損失かつ高強度のフ
ッ化物光ファイバを作製できる利点がある。(Effects of the Invention) As shown in the above examples, by using the method of the present invention, oxygen impurities adsorbed on the surface of the base material and the surface of the glass tube used as a jacket can be removed, which is difficult to do in the past. This method has the advantage of being able to produce a fluoride optical fiber with low loss and high strength.
第１図は実施例１で作製したフ・ン化物光ファイバの伝
送損失特性、第２図は実施例２で作製したフッ化物光フ
ァイバの伝送損失特性、第３図は実施例３で作製したフ
ッ化物光ファイバの伝送損失特性、第４図は実施例４で
作製したフ・ン化物光ファイバの伝送損失特性である。Figure 1 shows the transmission loss characteristics of the fluoride optical fiber manufactured in Example 1, Figure 2 shows the transmission loss characteristics of the fluoride optical fiber manufactured in Example 2, and Figure 3 shows the transmission loss characteristics of the fluoride optical fiber manufactured in Example 3. Transmission Loss Characteristics of Fluoride Optical Fiber FIG. 4 shows the transmission loss characteristics of the fluoride optical fiber produced in Example 4.
Claims (3)
イバを作製する工程およびフッ化物ガラス母材またはコ
ア組成のフッ化物ガラスロッドをフッ化物ガラスまたは
テフロンＦＥＰのパイプの中に挿入し線引きすることに
よりフッ化物光ファイバを作製する工程において、該フ
ッ化物ガラス母材、該フッ化物ガラスロッド、該フッ化
物ガラスパイプの一部または全部を含フッ素ガス中で加
熱処理した後、線引きすることを特徴とするフッ化物光
ファイバの製造方法。(1) Step of drawing a fluoride glass base material to produce a fluoride optical fiber, and inserting a fluoride glass base material or a fluoride glass rod having a core composition into a fluoride glass or Teflon FEP pipe and drawing it. In the step of producing a fluoride optical fiber, a part or all of the fluoride glass base material, the fluoride glass rod, and the fluoride glass pipe are heated in a fluorine-containing gas and then drawn. A method for manufacturing a fluoride optical fiber.
素、窒素、塩素、臭素、ヨウ素、イオウのうち少なくと
もいずれか１つとフッ素の化合物のガスであり、該含フ
ッ素ガスのいずれか１つまたは２つ以上の混合ガスであ
ることを特徴とする特許請求の範囲第１項記載のフッ化
物光ファイバの製造方法。(2) The fluorine-containing gas is fluorine or a gas of a compound of fluorine and at least one of hydrogen, carbon, boron, nitrogen, chlorine, bromine, iodine, and sulfur, and any one of the fluorine-containing gases or The method for manufacturing a fluoride optical fiber according to claim 1, characterized in that the mixed gas is a mixture of two or more gases.
とを特徴とする特許請求の範囲第１項または第２項に記
載のフッ化物光ファイバの製造方法。(3) The method for manufacturing a fluoride optical fiber according to claim 1 or 2, wherein the heat treatment temperature is in the range of 0°C to 400°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11899990A JPH0416524A (en) | 1990-05-09 | 1990-05-09 | Production of fluoride optical fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11899990A JPH0416524A (en) | 1990-05-09 | 1990-05-09 | Production of fluoride optical fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0416524A true JPH0416524A (en) | 1992-01-21 |
Family
ID=14750496
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11899990A Pending JPH0416524A (en) | 1990-05-09 | 1990-05-09 | Production of fluoride optical fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0416524A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0672628A1 (en) * | 1994-03-16 | 1995-09-20 | CSELT Centro Studi e Laboratori Telecomunicazioni S.p.A. | Method for the fabrication of fluoride glass single mode optical fibres |
| CN115650575A (en) * | 2022-09-26 | 2023-01-31 | 中国科学院上海光学精密机械研究所 | Preparation method of fluoride optical fiber precursor glass |
-
1990
- 1990-05-09 JP JP11899990A patent/JPH0416524A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0672628A1 (en) * | 1994-03-16 | 1995-09-20 | CSELT Centro Studi e Laboratori Telecomunicazioni S.p.A. | Method for the fabrication of fluoride glass single mode optical fibres |
| CN115650575A (en) * | 2022-09-26 | 2023-01-31 | 中国科学院上海光学精密机械研究所 | Preparation method of fluoride optical fiber precursor glass |
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