JPS6054891B2 - Preform manufacturing method - Google Patents
Preform manufacturing methodInfo
- Publication number
- JPS6054891B2 JPS6054891B2 JP3653679A JP3653679A JPS6054891B2 JP S6054891 B2 JPS6054891 B2 JP S6054891B2 JP 3653679 A JP3653679 A JP 3653679A JP 3653679 A JP3653679 A JP 3653679A JP S6054891 B2 JPS6054891 B2 JP S6054891B2
- Authority
- JP
- Japan
- Prior art keywords
- porous glass
- rod
- glass rod
- block
- center
- 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.)
- Expired
Links
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
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01262—Depositing additional preform material as liquids or solutions, e.g. solution doping of preform tubes or rods
-
- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/50—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with alkali metals
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth 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)
Description
【発明の詳細な説明】
本発明は、光通信に用いられる光伝送線路又はレンズ的
な機能を持つ棒状ガラスの製造の基となるプレフオーム
の製造方法に関するものてある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a preform that is the basis for manufacturing a rod-shaped glass having a lens-like function or an optical transmission line used in optical communication.
これらプレフオームに於いては、半径方向に所定の屈折
率分布をなし(例えばステップ型や放物線型の屈折率分
布)を持ち、かつ長手方向に均一(棒状ガラスの場合は
目的によつては屈折率を変えることもある。)な屈折率
になるように屈折率を調整したものが、伝送信号の歪を
小さくする点や伝送エネルギーのパワー分布を整えて結
合損失を小さくする点等から要求されてくる。これら所
定の屈折率分布を持つプレフオームの作り方としては、
イオン交換を利用したセルフォック(商品名)以外に、
特開昭50−28339、51−135915、51−
126207、53−102324に示されるところの
分子充チッ法がある。この方法では、分相性ガラス(例
えばNa2O一に。These preforms have a predetermined refractive index distribution in the radial direction (for example, a step-shaped or parabolic refractive index distribution) and are uniform in the longitudinal direction (in the case of rod-shaped glass, depending on the purpose, the refractive index distribution may be uniform). The refractive index is adjusted to achieve a refractive index of come. How to make a preform with a predetermined refractive index distribution is as follows:
In addition to SELFOC (product name), which uses ion exchange,
JP 50-28339, 51-135915, 51-
126207, 53-102324. In this method, a phase splitting glass (for example, Na2O-1) is used.
O−B。O。−SiO。)の棒を引上げた後熱処理、溶
出、洗浄にB。03を若干含むSiO2ガラスからなる
多孔質ガラス棒をまず作り、屈折率を変えるドーパント
を微細孔の内表面に所定の濃度で析出させ(例えば95
℃の飽W■、sNO。O-B. O. -SiO. B) for heat treatment, elution, and washing after pulling up the rod. First, a porous glass rod made of SiO2 glass containing a small amount of
℃'s saturation W■, sNO.
の水溶液中に多孔質ガラス棒を入れ、微細孔中にCsN
O、水溶液を充テンした後、0℃の水に311r入れて
析出そして外側から微細孔中のCSNO3を除去した後
、さらに30%H2O−70%CH3OHにてさらに析
出そして外側の微細孔中のCSNO3を除去した後、乾
燥する、しかる後加熱してゆくとCSNO3はCS2O
となつてCS2Oが所定の濃度分布で微細孔内表面に析
出する)、さらに高温加熱して熱固化して透明のガラス
棒とする。しかし、この方法に於いては引上げ棒を分相
熱処理し、酸溶出を施して多孔質ガラス棒を作る為に、
酸溶出時に生じるストレスが生じながら(溶出されてる
部分が出来てくると、未溶出の時歪のバランスが取れて
いた2相(Na2O−K2O−B,O3の軟相とB2O
3−SjO2の硬相)のうち軟相の部分が酸と置換され
てくる為、歪のバランスがくずれ残留歪が生じる。A porous glass rod is placed in an aqueous solution of CsN in the micropores.
After filling with O, aqueous solution, put it in 0℃ water for 311r to precipitate, remove CSNO3 in the micropores from the outside, further precipitate in 30% H2O-70% CH3OH, and remove the CSNO3 in the outer micropores. After removing CSNO3, it is dried and then heated, and CSNO3 becomes CS2O.
As a result, CS2O is precipitated on the inner surface of the micropores in a predetermined concentration distribution), and then heated to a high temperature and thermally solidified to form a transparent glass rod. However, in this method, the pulling rod is subjected to phase separation heat treatment and acid elution is performed to create a porous glass rod.
While stress occurs during acid elution (when the eluted part is formed, the two phases (Na2O-K2O-B, O3 soft phase and B2O
Since the soft phase portion of the hard phase of 3-SjO2 is replaced with acid, the strain balance is lost and residual strain occurs.
これらの部分の歪が未溶出のガラスの部分にかかつてく
る。)、酸溶出の進行面が棒表面から中心に向つて行く
が、行き先で進行が止まるという特異点が中心にある。
理由は明確に判面していないが、いずれにしても棒の中
心の特異点近傍では酸溶出後の微細孔の孔の大きさはそ
の周辺より中心に向うに従つて大きくなつている(又は
小さくなることもある)ことが、電子顕微鏡観察により
確認することが出来た。その結果を図で示すと第1図a
のようになる。The strain in these areas is applied to the undissolved glass area. ), the surface of acid elution progresses from the rod surface toward the center, but there is a singular point at the center where the progress stops at the destination.
The reason is not clearly known, but in any case, near the singular point at the center of the rod, the size of the micropores after acid elution becomes larger toward the center than at the periphery (or This was confirmed by electron microscopy. The results are shown in Figure 1a.
become that way.
即ち多孔質ガラス棒11の中心では、12に示される如
き微細孔の大きさの分布になつている。このような多孔
質ガラス棒を出発部材に用いると、プレフォームを作る
場合、例えばステップ型の場合、第1図bに示すように
コア13の中心にはよ.り多くのドーパントが析出する
為、中心のもり上つた屈折率分布15のプレフォームに
なり、例えば放物線状屈折率分布型の場合、第1図Cに
示すように中心16にはより多くのドーパントが析出す
る為、中心のもり上つた屈折率分布17のプレjフォー
ムが得られる。このように中心に不整点のあるプレフォ
ームから作つた光伝送線路或は棒レンズに於いては、信
号歪が大きくなること或はエネルギーの分布が乱れ結合
損失が大きくなるという欠点があり、実用上大問題とな
つている。本発明は、これらの欠点を解決する為に、中
心に異状な微細孔を有しない多孔質ガラス棒を準備する
方法を提供し、それによつて中心点に不整点のないプレ
フォームを製造する方法を提供するものである。本発明
では、これら異状の微細孔を生じる部分が酸溶出の終り
端に相当する部分にのみ生じるという及び多孔質ガラス
の切削は容易であるという発見に基き、これの異状部分
を除いた多孔質ガラスの部分を有効に利用することによ
つて、不整点のないプレフォームを製造する方法を特徴
とするものである。That is, at the center of the porous glass rod 11, the size distribution of micropores is as shown by 12. When such a porous glass rod is used as a starting member, when making a preform, for example a step type, a hole is formed in the center of the core 13 as shown in FIG. 1b. Since more dopants are precipitated, the preform has a refractive index profile 15 that rises at the center. For example, in the case of a parabolic index profile, more dopants are deposited at the center 16 as shown in FIG. 1C. is precipitated, so that a pre-j form with a refractive index distribution 17 with an upward slope at the center is obtained. Optical transmission lines or rod lenses made from preforms with irregular points in the center have the disadvantage of increased signal distortion or disordered energy distribution, resulting in increased coupling loss, making them impractical for practical use. It has become a major problem. In order to solve these drawbacks, the present invention provides a method for preparing a porous glass rod without irregular micropores in the center, thereby producing a preform without irregularities in the center. It provides: In the present invention, based on the discovery that the part where these abnormal micropores are formed only occurs in the part corresponding to the end of acid elution and that cutting of porous glass is easy, we have developed a porous glass with the abnormal part removed. The present invention is characterized by a method of manufacturing a preform without irregularities by effectively utilizing the glass portion.
以下、本発明について詳細を述べる。The present invention will be described in detail below.
分相性ガラスとしては、例えば、Na2O−B2O3−
SlO2,Na2O−K2O−SlO2Na2O−K2
O−B2O3一SiO2の系のガラスで限定された組成
のガラス(これらは前述の特許やVycOr特許にある
)を用い、出発部材として棒又は管又は板を作る。As the phase splitting glass, for example, Na2O-B2O3-
SlO2, Na2O-K2O-SlO2Na2O-K2
Glasses of the O--B2O3-SiO2 system with defined compositions (these are found in the aforementioned patents and the VycOr patent) are used to make rods or tubes or plates as starting parts.
(特に変つた方法を用いず一般的な方法で作る。)次に
これを分相熱処理(この温度、時間条件は組成によつて
異る)し、さらに高温の酸(例えば100℃3NHC1
)に浸すと軟相が溶け出してくる。これを溶出の終端に
沿つて切削することによつて角柱を作る。この切削は溶
出後水洗浄を施した後又はそれを乾そうした後でもよい
。例えば第2図aに示すような板21の場合、溶出の終
端22に沿つて金鋸切りで切り、さらに細く切つて例え
ば角柱23のようなものを切り出す。角柱23の断面は
例えば第2図bの23″のような正方形にする。(It is made by a general method without using any special method.) Next, it is subjected to a phase separation heat treatment (this temperature and time conditions vary depending on the composition), and then a high temperature acid (for example, 100℃ 3NHC1
), the soft phase begins to dissolve. A prism is made by cutting this along the end of the elution. This cutting may be performed after washing with water after elution or after drying. For example, in the case of a plate 21 as shown in FIG. 2a, it is cut with a hacksaw along the end 22 of the elution, and then cut into thin pieces, such as a prism 23. The cross section of the prism 23 is, for example, a square like 23'' in FIG. 2b.
棒の場合は中心軸に沿つて4等分し、管の場合には、厚
みのムの面に沿つて切り出して行く必要がある。In the case of a rod, it is necessary to divide it into four equal parts along the central axis, and in the case of a tube, it is necessary to cut it out along the plane of the thickness.
このように切り出した棒23″は、次に通常の研まによ
り24,25のように角を取つてゆき、最終的には26
のように丸棒にする。The bar 23'' cut out in this way is then polished in the usual way to get the corners like 24 and 25, and finally becomes 26.
Make it into a round bar like this.
次にこれを酸洗、水洗して切削クズや汚れを除去するこ
とにより、全体に一様な微細孔を有する多孔質ガラス棒
を作ることが出来る。Next, by pickling and washing with water to remove cutting debris and dirt, a porous glass rod having uniform micropores throughout can be produced.
このようにして作つた多孔質ガラス棒を出発部材として
分る充テン法によりプレフォームを作ると、例えばステ
ップ型の場合、第3図aのコア31の中心の屈折率分布
32には不整点のないプレフォーム例えば放物線状屈折
率分布型の場合、第3図bの中心33には異常の見られ
ない屈折率分布34には不整点のないプレフォームが得
られる。When a preform is made by the filling method using the porous glass rod thus made as a starting material, for example, in the case of a step type, there are irregularities in the refractive index distribution 32 at the center of the core 31 in FIG. 3a. For example, in the case of a parabolic refractive index distribution type preform, a preform with no irregularities in the refractive index distribution 34 with no abnormality at the center 33 in FIG. 3b is obtained.
以下本発明の一実施例について説明する。An embodiment of the present invention will be described below.
しかしこれらの実施例に限定されるものではない。4%
Na2O−3%K2O−36%B2O3−57%SiO
2からなるガラスを白金るつぼで1500′Cにて溶解
し、このガラスをカーボンの鋳型(125?×125W
f&×25TI0ntの凹)の中に流し込んだ。However, the invention is not limited to these examples. 4%
Na2O-3%K2O-36%B2O3-57%SiO
The glass consisting of
It was poured into a f&×25TI0nt concave).
クラックの入らなかつた5h×5−X25順tの部分を
切り出した。次にこの板を550℃×6F1r熱処理し
た後、100℃3NHC1に浸して9ea!f間放置し
たところ完全に溶出は終つていた。これを水洗浄した後
、次にこれから第2図のようにした。8.5T!n×4
5Tfr1nIの四角柱を薄刃の金鋸で切り出し、次に
研ま機で#400を用いて角取りを行つた後、回転モー
ターに取り付けて回転させ#600,800,#100
0,#1500セロツクスという粉末で研まして丸棒と
した。A 5h x 5 - x 25 t portion with no cracks was cut out. Next, this board was heat treated at 550°C x 6F1r, and then immersed in 3NHC1 at 100°C to give 9ea! When the solution was allowed to stand for a period of f, the elution was completely completed. After washing this with water, it was then prepared as shown in Fig. 2. 8.5T! n×4
Cut out a 5Tfr1nI square prism with a thin-blade hacksaw, then use a #400 sharpening machine to cut the corners, and then attach it to a rotary motor and rotate it using #600, 800, and #100.
0, I polished it with #1500 Serox powder and made it into a round bar.
次にこれを3NHN03水にて充分洗浄した後、純水洗
浄を行い8TWLφ×40wrmIの多孔質ガラス棒と
した。Next, this was thoroughly washed with 3NHN03 water, and then washed with pure water to obtain a porous glass rod of 8TWLφ×40wrmI.
(これを試料Aとする)、一方同じ組成の8朗φのガラ
ス棒を引上げ、同じ分相熱処理、溶出処理、水洗浄3N
F[NO3水洗浄、純水洗浄を施し多孔質ガラス棒を作
つた。(これを試料Bとする)次に、これらを105℃
のCSNO3の水溶液に4hr浸漬した後、20゜Cに
冷やして311r洗い(この時始め析出してその後しだ
いに外側の部分が溶かし出されて透明になつてくる)、
その後チルルアルコール100%で1hr放置して外側
の部分の溶解CSNO3を析出させ、その後さらにこの
外側の部分の析出CSNO3をエチルアルコール80%
一水20%で48hr洗い外側のCSNO3の濃度を下
げた。次にこれらをC3H7OHでソーキングし、ゆつ
くり真空乾そうしながら850℃まで加熱していつたと
ころA,Bとも透明ガラス棒(6.4TnInφ×30
Tnm1)になつた。これらの屈折率分布を調べたとこ
ろAには中心点で屈折率の異常に高い点は無かつたが、
Bには中心点で分相性の異常に高い点が見られた。(This is referred to as sample A). On the other hand, a glass rod of 8 dia.
F[NO3 water washing and pure water washing were performed to prepare a porous glass rod. (This will be referred to as sample B) Next, heat these to 105°C.
After being immersed in an aqueous solution of CSNO3 for 4 hours, cooled to 20°C and washed at 311r (at this time, precipitation begins, and then the outer part gradually dissolves and becomes transparent).
After that, the dissolved CSNO3 in the outer part was allowed to precipitate by leaving it for 1 hour in 100% ethyl alcohol, and then the precipitated CSNO3 in the outer part was further dissolved in 80% ethyl alcohol.
Washed with 20% water for 48 hours to reduce the concentration of CSNO3 on the outside. Next, these were soaked in C3H7OH and heated to 850℃ while slowly vacuum drying.
Tnm1). When we investigated these refractive index distributions, we found that there was no point with an abnormally high refractive index at the center of A.
In B, a point with abnormally high phase separation was observed at the central point.
本発明によれば、半径方向に所定の屈折率分布をなし、
長手方向にも所定の屈折率分布を持つような屈折率点に
異常のないプレフォームが安いコストで得られる。この
プレフォームからは、光信号歪の小さいファイバーが得
られる。According to the present invention, a predetermined refractive index distribution is formed in the radial direction,
A preform having a predetermined refractive index distribution also in the longitudinal direction and having no abnormality in refractive index points can be obtained at a low cost. This preform yields a fiber with low optical signal distortion.
またエネルギーのパワー分布を整える棒状レンズをこの
プレフォームから作ることが出来る。A rod-shaped lens that adjusts the power distribution of energy can also be made from this preform.
第1図aは中心に異状な微細孔を有する多孔質ガラス棒
を示し、第1図B,cはそれら多孔質ガラス棒を用いた
場合、得られるステップ型、放物線型のプレフォームの
屈折率分布を示す。
第2図A,bは本発明を説明する為の図である。第3図
A,bは本発明の多孔質ガラス棒を用いた場合得られる
ステップ型、放物線型のプレフォームの屈折率分布を示
す。12は孔の大きさの分布、15,16は中心部の屈
折率分布、23は角柱、26は丸棒を示す。Figure 1a shows a porous glass rod with an unusual micropore in the center, and Figures 1B and c show the refractive index of the step-shaped and parabolic preforms obtained when these porous glass rods are used. Show the distribution. FIGS. 2A and 2B are diagrams for explaining the present invention. FIGS. 3A and 3B show the refractive index distributions of step-type and parabolic preforms obtained when using the porous glass rod of the present invention. Reference numeral 12 indicates a hole size distribution, 15 and 16 indicate a refractive index distribution at the center, 23 indicates a square column, and 26 indicates a round bar.
Claims (1)
を施し、酸溶出を必要により洗浄をも行い多孔質ガラス
・ブロックを作り、該多孔質ガラスブロックから中心部
を外して棒状のブロックを切り出し、該多孔質ガラス棒
を研摩して、円柱状の多孔質ガラス棒を準備し、この円
柱状多孔質ガラス棒の微細孔の内表面に所定の濃度分布
にドーパントを析出し、しかる後熱固化することによつ
て中心に不整点のない半径方向に所定の屈折率分布を有
するガラス棒を作ることを特徴とするプレフオームの製
造方法。 2 板状の単純な形状の分相性ガラスのブロックを熱処
理し、酸溶出し、多孔質ガラスとし、それから長手方向
に中心面を通るようにスライスして正四角柱を作り、該
正四角柱を角を取りながら丸めるように研磨し、必要に
よつてはフッ酸洗浄をも行い最後に純水で洗浄して円柱
状の多孔質ガラス棒を準備することを特徴とする特許請
求の範囲第1項記載のプレフオームの製造方法。[Claims] 1. A block of phase-splitting glass is made, a phase-splitting heat treatment is applied to it, acid elution is performed and washing is performed as necessary to make a porous glass block, and the center portion is removed from the porous glass block. A rod-shaped block is cut out, the porous glass rod is polished to prepare a cylindrical porous glass rod, and a dopant is precipitated in a predetermined concentration distribution on the inner surface of the micropores of this cylindrical porous glass rod. . A method for manufacturing a preform, characterized in that a glass rod having a predetermined refractive index distribution in the radial direction without an irregular point at the center is produced by thermally solidifying the glass rod. 2 Heat-treat a block of phase-splitting glass with a simple plate shape, elute it with acid, make it porous glass, then slice it longitudinally through the center plane to make a square prism, and cut the corners of the square prism. Claim 1 is characterized in that a cylindrical porous glass rod is prepared by polishing it in a rounded manner while taking it, and if necessary, washing it with hydrofluoric acid and finally washing it with pure water. Preform manufacturing method.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3653679A JPS6054891B2 (en) | 1979-03-27 | 1979-03-27 | Preform manufacturing method |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3653679A JPS6054891B2 (en) | 1979-03-27 | 1979-03-27 | Preform manufacturing method |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS55130830A JPS55130830A (en) | 1980-10-11 |
JPS6054891B2 true JPS6054891B2 (en) | 1985-12-02 |
Family
ID=12472498
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3653679A Expired JPS6054891B2 (en) | 1979-03-27 | 1979-03-27 | Preform manufacturing method |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS6054891B2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS6177629A (en) * | 1984-09-21 | 1986-04-21 | Hoya Corp | Production of spherical lens having refractive index distribution |
-
1979
- 1979-03-27 JP JP3653679A patent/JPS6054891B2/en not_active Expired
Also Published As
Publication number | Publication date |
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JPS55130830A (en) | 1980-10-11 |
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