JPS58104034A - Preparation of optical fiber having high strength - Google Patents
Preparation of optical fiber having high strengthInfo
- Publication number
- JPS58104034A JPS58104034A JP19998881A JP19998881A JPS58104034A JP S58104034 A JPS58104034 A JP S58104034A JP 19998881 A JP19998881 A JP 19998881A JP 19998881 A JP19998881 A JP 19998881A JP S58104034 A JPS58104034 A JP S58104034A
- Authority
- JP
- Japan
- Prior art keywords
- base material
- optical fiber
- hydrofluoric acid
- hikari
- high temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/66—Chemical treatment, e.g. leaching, acid or alkali treatment
- C03C25/68—Chemical treatment, e.g. leaching, acid or alkali treatment by etching
-
- 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
- C03B37/01225—Means for changing or stabilising the shape, e.g. diameter, of tubes or rods in general, e.g. collapsing
- C03B37/01228—Removal of preform material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
Abstract
Description
【発明の詳細な説明】 本発明は高強度の光ファイバを製造する方法に関する。[Detailed description of the invention] The present invention relates to a method of manufacturing high strength optical fiber.
光ツアイパは低損失で大容量の伝送媒体であ〉、かつ軽
量であるため無接続の長尺伝送路用媒体として有望であ
るが、その丸めには上記特性の他に強度が高いという特
性をも満たすことが必要である。Optical fibers are a low-loss, high-capacity transmission medium and are lightweight, making them promising as media for long, unconnected transmission lines. It is also necessary to satisfy the following requirements.
光ファイバの強度を劣化させる因子としては、光７アイ
パおよびその母材の内部の欠陥および表面に散在する傷
であるととが知られているが、とシわけ低強度の生える
要因は、光７アイパに線引する前の母材表面の傷および
汚濁にあることが実験的に明らかになっている。表面の
傷を除去して光７アイパの強度の改善をはかる方法とし
て、線引前の光フアイバ用母材を弗酸系溶液に浸漬した
彼に線引する方法が従来知られている（成瀬省著「ガラ
ス工学Ｊｐ２５５、共立出版社）。It is known that the factors that degrade the strength of optical fibers are defects inside the optical fiber and its base material, as well as scratches scattered on the surface. It has been experimentally revealed that this is caused by scratches and contamination on the surface of the base material before it is drawn into the 7-eye paper. As a method for removing surface scratches and improving the strength of Hikari 7 EyePa, it is known to immerse the pre-drawn optical fiber base material in a hydrofluoric acid solution and then draw it (Sei Naruse et al. Author: Glass Engineering JP255, Kyoritsu Shuppansha).
しかしながら、本発明者岬がこの弗酸系溶液による表面
処理を施した母材を線引してみたところ、強度の著しい
改善効果はみられず、一方、強度のバラツキが認められ
た。そこで本発明者等は、この従来法による母材表面処
理の欠点を解決して、高強度の光ファイバを提供すべく
研究を重ねた結果、上記の強旋のバラツキ、および強度
改善の不十分さは、弗酸系溶液による母、、・、：
材表面のエツチングが不均一であ）、またエツチングに
よシ異物や比較的”）ｚきい表面傷の除去は為される４
のの、一方で、小さいエッチビットが発゛生し九ことに
起因することをつきとめた。However, when Misaki, the inventor of the present invention, drew a base material that had been surface-treated with this hydrofluoric acid solution, no significant improvement in strength was observed, and on the other hand, variations in strength were observed. Therefore, the inventors of the present invention have conducted repeated research to solve the drawbacks of base material surface treatment using the conventional method and provide a high-strength optical fiber. However, etching with a hydrofluoric acid solution may result in non-uniform etching of the material surface, and foreign matter and relatively large surface scratches may be removed by etching4.
On the other hand, we found that this was caused by the occurrence of small etch bits.
本発明では弗酸系の溶液にて表面層をエツチング後の母
材を、高温に加熱することにより表面を平滑化して上記
のエッチビットの発生醇による不利益を解決し、強度の
改善を図るものである。本発明の表面平滑化における高
温加熱は、燃焼ガス例えば酸水素バーナー等による火炎
研磨、抵抗加熱炉による処理、高温プラズマ炎による火
炎研磨等種々０手段を用いることができ、母材表面を清
浄な高温雰囲気、好ましくはファイバ母材の表面が１５
００℃〜２３００℃となるような雰囲気に秦すことＫよ
〕、弗酸系溶液エツチングで派生した表置の凹凸の平滑
化が行なわれるものである。この高温加熱処理は１回だ
けでなく、それ以上行なって４よい。In the present invention, after etching the surface layer with a hydrofluoric acid solution, the base material is heated to a high temperature to smooth the surface, solve the disadvantages caused by the generation of etch bits, and improve the strength. It is something. The high-temperature heating in surface smoothing of the present invention can be carried out by various methods such as flame polishing using a combustion gas such as an oxyhydrogen burner, treatment using a resistance heating furnace, flame polishing using a high-temperature plasma flame, etc. High temperature atmosphere, preferably when the surface of the fiber matrix is 15
The surface irregularities resulting from etching with a hydrofluoric acid solution are smoothed. This high-temperature heat treatment may be performed not only once but more than once.
本発明で使用するフッ酸系溶液としては、７フ化水素（
ＨＦ 、’）、フッ硫酸（ＨＦ鳴ＳＱＩ ） 、フッ硝
酸（韮・掛へ）褌どが挙げられ、その濃度は５〜３０重
量％、浸漬時間はａ５〜５時間が好ましい。フッ酸系溶
液処理時に超音波洗浄を行うと、エツチングの均質化が
図られ、好ましい。The hydrofluoric acid solution used in the present invention is hydrogen heptafluoride (
Examples include HF, '), fluorosulfuric acid (HF-Ni SQI), and fluoronitric acid (Nira/Kakehe), and the concentration thereof is preferably 5 to 30% by weight, and the immersion time is preferably 5 to 5 hours. It is preferable to carry out ultrasonic cleaning during the hydrofluoric acid solution treatment, as this ensures homogenization of the etching.
本発明におけるフッ酸系溶液処理と高温加熱、高温加熱
と線引、各々の間の時間を短くすると、よ）効果が上夛
、その時間としては（１５時間程度が好ましい。In the present invention, shortening the time between the hydrofluoric acid solution treatment and high-temperature heating, and between high-temperature heating and drawing will increase the effect, and the preferred time is about 15 hours.
更に本発明者尋紘、母材表面のエツチングの不均一性は
母材表面に付着している有機物が弗酸系溶液による母材
表面の浸蝕を妨げていることにも起因すると考え、母材
表面を有機溶剤で清浄化した後に、上記弗酸系溶液処理
、加熱処理したところ、強度のバラツキおよび強度が更
に改善された。有機溶剤としては、エタノール、メタノ
ール、プロパツール、アセトン、メチルエチルケトン勢
が用いられ、これら解削に母材を浸漬して、超音波洗浄
を行うとより一層の効果が奏される。゛
次に本発明方法、および従来法による光ファイバの強度
を試験した結果を示す。Furthermore, the present inventor, Hirohiro, believes that the non-uniformity of etching on the surface of the base material is due to the fact that organic matter adhering to the surface of the base material prevents erosion of the surface of the base material by the hydrofluoric acid solution. After cleaning the surface with an organic solvent, the above-mentioned hydrofluoric acid solution treatment and heat treatment were performed, and the strength variation and strength were further improved. Ethanol, methanol, propatool, acetone, and methyl ethyl ketone are used as organic solvents, and the effect will be even greater if the base material is immersed in these demolition processes and then subjected to ultrasonic cleaning. Next, the results of testing the strength of optical fibers using the method of the present invention and the conventional method will be shown.
例１
ファイバの長さ１０１１１％７アイパ径１２５μ清、歪
速度５％／分における、破断荷重（横軸）Ｋ対するファ
イバの破断確率分布を第１図に示す。Example 1 Figure 1 shows the fiber breakage probability distribution with respect to the breakage load (horizontal axis) K when the fiber length is 10111%7, the eye diameter is 125μ, and the strain rate is 5%/min.
図中、曲線ａは表面処理を全く施こさずに線引したもの
である。曲線すは濃度１０チの弗酸に２時間浸漬した後
に線引し九ものである。ａ１ｂ両曲線から、従来Ｏ弗酸
処理によシ破断荀重１１ｃｆ以下の低強度の原因となる
表面の傷、無機物汚れ等を除去できるが、エツチングピ
ットが生じる丸め、ｓ’Ｈ以上の高強度部分の破断強度
は逆に劣化していると考えられる。In the figure, curve a is drawn without any surface treatment. The curved line was drawn after being immersed in hydrofluoric acid with a concentration of 10% for 2 hours. From the a1b curves, it is clear that conventional O-hydrofluoric acid treatment can remove surface scratches, inorganic stains, etc. that cause low strength at breakage weight of 11 cf or less; On the contrary, it is thought that the breaking strength of the part has deteriorated.
曲線Ｃは濃度１０チの弗酸に２時間浸漬したのち、水素
１５０１７分、酸素５０ｔ／分をノ（−チー外で燃焼さ
せた火炎によシ母材表面を火炎研磨して表面の平滑化処
理を施こし、次いで線引したもので、従来法によるファ
イバの破断強度と比較してその改善効果は明らかである
。Curve C shows that after 2 hours of immersion in hydrofluoric acid with a concentration of 10%, the surface of the base material was flame-polished using a flame that was burned outside of the base metal to make the surface smooth. The fiber was treated and then drawn, and the improvement in the breaking strength of the fiber by the conventional method is obvious.
曲線ｄはエタノールに母材を浸漬後、上記Ｃの弗酸処理
、火炎研磨、線引を行な−りたもので、有機物の除去に
より、弗酸によるエツチングの均質４ムを図った効果が
顕著に認められる。Curve d shows the result of immersing the base material in ethanol and then performing the hydrofluoric acid treatment, flame polishing, and line drawing as described in C above.The removal of organic matter has the effect of making the etching with hydrofluoric acid more homogeneous. Remarkably recognized.
なお、ｃ、ｄにおいて、上記酸水素炎以外の抵抗炉加燃
、高温プラズマ炎加熱でも同様の効果が奏される。In addition, in c and d, similar effects can be achieved by heating in a resistance furnace or heating with a high-temperature plasma flame other than the above-mentioned oxyhydrogen flame.
例２
第２図に、同一のファイバ母材を５分割し、各々イ：ア
ルコールによシ表面の汚れを除去、９２１５重量−のフ
ッ酸溶液に２．５時間浸漬したもの、ハ：ロを更に７ア
イパ母材の表面温１度ｚｏｏｏｔｌ：になるように酸水
素火炎研磨し丸もの、の処理を施した後、カーボン抵抗
炉で約２５００℃で線引した７アイパの引張強度を示す
。Example 2 In Figure 2, the same fiber base material is divided into 5 parts, each of which is divided into 5 parts: A: the surface of which was removed with alcohol, immersed for 2.5 hours in a 9215 wt hydrofluoric acid solution, and C: B: Furthermore, the tensile strength of 7 Eyepa was drawn at about 2500°C in a carbon resistance furnace after being subjected to oxyhydrogen flame polishing and round treatment so that the surface temperature of the 7 Eyepa base material was 1 degree zoootl:.
試料長は２０濁、歪速度はｌ１０５／分、ｎ ＝ ｓ０
０回である。Sample length is 20mm, strain rate is 1105/min, n = s0
0 times.
第２図から判るように７ツ酸処理のみの７アイパロは処
理なしイに比較してはるかに改善されているが、峻Ｏｍ
Ｘ ５００ ”＝ １０−での最低強度は６０麺／■
黛とまだ小さい。それに対しハ□
の本発明の７アイパは１０１ｍｆの最低強度が１５０麺
／■３ と非常に高いレベルにある。As can be seen from Figure 2, the 7 Eye Paro treated only with 7 acid is much improved compared to the non-treated A, but the sharp Om
The minimum strength at X 500” = 10- is 60 noodles/■
Mayuzumi is still small. On the other hand, the minimum strength of the 7-aipa of the present invention in HA□ is at a very high level of 150 noodles/■3 at 101 mf.
第１図および第２図は、本発明方法および従来法による
ファイバの破断確率分布および引張シ強度を各々示すグ
ラフである。
代理人 内 １） 明
代理人 荻 原 亮 −
巴・FIGS. 1 and 2 are graphs showing the fracture probability distribution and tensile strength of fibers according to the method of the present invention and the conventional method, respectively. Agents 1) Akira’s agent Ryo Ogihara − Tomoe・
Claims (1)
ツチングした後、骸母材を高温に加熱することＫよシ表
面を平滑化し、次いで線引することからなる光７アイパ
の製造方法。 ２ 光７アイパ用母材の表面を有機溶剤で処理俵、・弗
酸系の溶液にて母材の表面層をエツチングし、次いで該
母材を高温に加熱するととＫよシ表面を平滑化し、線引
することからなる光７アイパの製造方法。 五 燃焼ガスによシ該母材を高温に加熱する特許請求の
範囲１ま゛たは２記載の光ファイバの製造方法゛。′ 表 抵抗加熱炉によ）＃母材を高温に加熱す□る特許請
求の範囲１または２記載の光ファイバの製造方法。 翫 高温プラズマ炎によ〕該母材を高温に加熱する特許
請求の範囲１または２記載の光７アイバＯ製造方法。 ４ 線引き前の光フアイバ母材を５重量−から３０重量
−のフッ酸系溶液Ｋ（１５時間から５時間浸漬し、しか
る後、酸水素炎にて該ファイバ母材の表両温度が１５０
０℃かう２５００℃となるような火炎研磨を少なくとも
１回行ない、その後、線引きする特許請求の範囲１ｔｆ
ｌ：、ａ２記載の光７アイパの製造方法。[Claims] t After etching the surface layer of the base material for Hikari 7 Eyepa with a solution of hydrofluoric acid, the surface is smoothed by heating the shell base material to a high temperature, and then wire drawing is performed. A method for manufacturing Hikari 7 Eyepa, which comprises: 2. Treating the surface of the base material for Hikari 7 Eyepa with an organic solvent. When the surface layer of the base material is etched with a hydrofluoric acid solution, and then the base material is heated to a high temperature, the surface of the base material is smoothed. , a method for manufacturing Hikari 7-aipa, which comprises drawing a line. 5. The method for manufacturing an optical fiber according to claim 1 or 2, wherein the base material is heated to a high temperature by combustion gas. The method for manufacturing an optical fiber according to claim 1 or 2, wherein the base material is heated to a high temperature in a resistance heating furnace. The method for producing Hikari 7 Aiba O according to claim 1 or 2, wherein the base material is heated to a high temperature by a high-temperature plasma flame. 4. The optical fiber preform before drawing is immersed in a 5- to 30-weight hydrofluoric acid solution K (15 to 5 hours, and then heated to an oxyhydrogen flame until the temperature on both sides of the fiber is 150%.
Claim 1tf that flame polishing is performed at least once so that the temperature is between 0°C and 2500°C, and then a line is drawn.
1:, the method for manufacturing Hikari 7 Eyepa described in a2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19998881A JPS58104034A (en) | 1981-12-14 | 1981-12-14 | Preparation of optical fiber having high strength |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19998881A JPS58104034A (en) | 1981-12-14 | 1981-12-14 | Preparation of optical fiber having high strength |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58104034A true JPS58104034A (en) | 1983-06-21 |
| JPS6144820B2 JPS6144820B2 (en) | 1986-10-04 |
Family
ID=16416917
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19998881A Granted JPS58104034A (en) | 1981-12-14 | 1981-12-14 | Preparation of optical fiber having high strength |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58104034A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60246240A (en) * | 1984-05-07 | 1985-12-05 | ル ヴエール フリユオール エス ア | Manufacture of fluorine glass optical fiber and optical element and device for carrying out same |
| EP0519479A2 (en) * | 1991-06-20 | 1992-12-23 | Sumitomo Electric Industries, Ltd | Method for flame abrasion of glass preform |
| EP0630864A2 (en) * | 1993-05-24 | 1994-12-28 | Sumitomo Electric Industries, Ltd. | Fabrication process of polarization-maintaining optical fiber |
| JP2010013352A (en) * | 2009-09-07 | 2010-01-21 | Shin-Etsu Chemical Co Ltd | Method of processing glass preform |
| EP2481715A1 (en) * | 2011-01-26 | 2012-08-01 | Shin-Etsu Chemical Co., Ltd. | Optical fiber preform and method of manufacturing optical fiber preform |
| JP2014531567A (en) * | 2011-09-14 | 2014-11-27 | 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Ｈｅｒａｅｕｓ ＱｕａｒｚｇｌａｓＧｍｂＨ ＆ Ｃｏ． ＫＧ | Solar radiation receiver with quartz glass window and method of manufacturing window |
| CN109270612A (en) * | 2018-09-04 | 2019-01-25 | 安徽新恒辉反光材料有限公司 | A kind of tension reflective strip and preparation method thereof |
-
1981
- 1981-12-14 JP JP19998881A patent/JPS58104034A/en active Granted
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60246240A (en) * | 1984-05-07 | 1985-12-05 | ル ヴエール フリユオール エス ア | Manufacture of fluorine glass optical fiber and optical element and device for carrying out same |
| EP0519479A2 (en) * | 1991-06-20 | 1992-12-23 | Sumitomo Electric Industries, Ltd | Method for flame abrasion of glass preform |
| US5685889A (en) * | 1991-06-20 | 1997-11-11 | Sumitomo Electric Industries, Ltd. | Method for flame abrasion of glass preform |
| EP0630864A2 (en) * | 1993-05-24 | 1994-12-28 | Sumitomo Electric Industries, Ltd. | Fabrication process of polarization-maintaining optical fiber |
| EP0630864A3 (en) * | 1993-05-24 | 1995-05-24 | Sumitomo Electric Industries | Fabrication process of polarization-maintaining optical fiber. |
| JP2010013352A (en) * | 2009-09-07 | 2010-01-21 | Shin-Etsu Chemical Co Ltd | Method of processing glass preform |
| EP2481715A1 (en) * | 2011-01-26 | 2012-08-01 | Shin-Etsu Chemical Co., Ltd. | Optical fiber preform and method of manufacturing optical fiber preform |
| JP2014531567A (en) * | 2011-09-14 | 2014-11-27 | 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Ｈｅｒａｅｕｓ ＱｕａｒｚｇｌａｓＧｍｂＨ ＆ Ｃｏ． ＫＧ | Solar radiation receiver with quartz glass window and method of manufacturing window |
| US10024577B2 (en) | 2011-09-14 | 2018-07-17 | Heraeus Quarzglas Gmbh & Co. Kg | Solar radiation receiver having an entry window made of quartz glass and method for producing an entry window |
| CN109270612A (en) * | 2018-09-04 | 2019-01-25 | 安徽新恒辉反光材料有限公司 | A kind of tension reflective strip and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6144820B2 (en) | 1986-10-04 |
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