JPS63206318A - Production of glass body for optical transmission - Google Patents

Production of glass body for optical transmission

Info

Publication number
JPS63206318A
JPS63206318A JP3520287A JP3520287A JPS63206318A JP S63206318 A JPS63206318 A JP S63206318A JP 3520287 A JP3520287 A JP 3520287A JP 3520287 A JP3520287 A JP 3520287A JP S63206318 A JPS63206318 A JP S63206318A
Authority
JP
Japan
Prior art keywords
glass body
dopant
distribution
sample
porous 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
Application number
JP3520287A
Other languages
Japanese (ja)
Inventor
Mikio Aoki
三喜男 青木
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Seiko Epson Corp
Original Assignee
Seiko Epson Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Seiko Epson Corp filed Critical Seiko Epson Corp
Priority to JP3520287A priority Critical patent/JPS63206318A/en
Publication of JPS63206318A publication Critical patent/JPS63206318A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture 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]
    • C03B37/01446Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2201/00Type of glass produced
    • C03B2201/06Doped silica-based glasses

Abstract

PURPOSE:To enable ready formation of a glass body for optical transmission having a constant dopant concentration gradient, by dipping porous glass homogeneously soaked with the dopant in hot water, taking out the porous glass, drying the porous glass at a specific temperature or above and sintering the dried porous glass. CONSTITUTION:A dopant is diffused into porous glass and the resultant sample is placed in a solvent to produce distribution in the dopant concentration. The dopant concentration is then fixed and the sample is subsequently passed through drying and sintering to provide a glass body having refractive index distribution which is a glass body for optical transmission. In the process for producing the glass body, the following method is used. That is distribution is formed in the sample homogeneously soaked with the dopant in hot water and the sample is directly dried at >=150 deg.C temperature in producing distribution of dopant concentration and fixing the distribution thereof.

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は光伝送用ガラス体の製造方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method of manufacturing a glass body for light transmission.

[従来の技術] 屈折率勾配を有するガラス体の製造方法としては、分子
スタッフィング法が知られている。この方法は多孔質ガ
ラス体内に!:゛−バント(屈折率修正成分)の濃度勾
配が形成されるようドーパントを多孔質ガラス体の細孔
内に充慎し、しかる後細孔を熱処理(焼成)によってつ
ぶす方法であって、特開昭51−12607’号公報に
は多孔質ガラス体内にドーパントの溶液を浸透させた後
そのガラス体内からドーパントの一部を溶出させて細孔
内に分布するドーパントに濃度勾配を形成させ、次にド
ーパントを細孔内に析出させてからそのガラス体を乾燥
し、しかる後これに焼成処理を施して細孔をつぶすこと
からなる屈折率勾配を有するガラス体の製造方法が教示
させている。
[Prior Art] A molecular stuffing method is known as a method for manufacturing a glass body having a refractive index gradient. This method works inside a porous glass body! : A method in which a dopant is filled into the pores of a porous glass body so that a concentration gradient of a band (refractive index modifying component) is formed, and then the pores are crushed by heat treatment (firing). Japanese Patent Publication No. 51-12607' discloses that after a dopant solution is infiltrated into a porous glass body, a part of the dopant is eluted from the glass body to form a concentration gradient in the dopant distributed in the pores, and then A method for producing a glass body with a refractive index gradient is taught, which comprises precipitating a dopant into the pores, drying the glass body, and then subjecting it to a firing treatment to collapse the pores.

[発明が解決しようとする問題点] しかし前述の従来技術では、多孔質ガラス体にドーパン
トを充慎させ、その後のドーパント溶液を溶出させドー
パントの濃度勾配を形成させた後乾燥する時点において
、−担固定した濃度が平均化してしまうといった現象が
生じ、望みの屈折率分布を有するガラス体が得られにく
い、そこで本発明はこのような問題点を解決するもので
、その目的とするところは、一定の濃度勾配を有する光
伝送用ガラス体を容易に製造することにある。
[Problems to be Solved by the Invention] However, in the above-mentioned prior art, at the time of filling a porous glass body with a dopant, eluting the dopant solution to form a dopant concentration gradient, and then drying - A phenomenon occurs in which the concentration of supported particles is averaged, making it difficult to obtain a glass body having a desired refractive index distribution.The present invention is intended to solve these problems, and its purpose is to: An object of the present invention is to easily manufacture a glass body for light transmission having a constant concentration gradient.

E問題点を解決するための手段] 本発明の光伝送用ガラス体の製造方法は多孔質ガラスに
ドーパントを拡散させた後、溶媒中に試料を入れドーパ
ントの濃度に分布を荏じさせ、その後ドーパントの′a
度分布を固定させ、乾燥、焼結を経て屈折率分布ガラス
体を得る光伝送用ガラス体の製造方法のドーパントの濃
度分布及び該分布の固体時において、ドーパントの一様
にしみ込んだ試料に湯中で分布を生じさせた後すぐに1
50℃以上の温度で乾燥することを@徴とする。
Means for Solving Problem E] The method for producing a glass body for optical transmission of the present invention is to diffuse a dopant into a porous glass, then place a sample in a solvent to create a uniform distribution of dopant concentration. dopant'a
The concentration distribution of the dopant in the manufacturing method of a glass body for optical transmission, in which the refractive index distribution is fixed and the refractive index distribution glass body is obtained through drying and sintering. 1 immediately after generating the distribution in
Drying at a temperature of 50°C or higher is the @ sign.

[作用] 多孔質ガラス体内にドーパントを十分に拡散させた後、
ドーパンI・の濃度に分布をつけるために該多孔質ガラ
スをアルコールと水の混合液等の溶媒に浸しドーパント
を溶出させる。この時点で、ドーパントの濃度は表面付
近から内部に向かって勾配がついている1次に該試料は
乾燥され、焼結されて透明ガラス体となるわけである。
[Function] After sufficiently diffusing the dopant into the porous glass body,
In order to distribute the concentration of Dopan I, the porous glass is immersed in a solvent such as a mixture of alcohol and water to dissolve the dopant. At this point, the primary sample, in which the concentration of dopant is graded from near the surface to the interior, is dried and sintered into a transparent glass body.

しかしこの乾燥時において、該試料内の溶媒が中心付近
から周囲に向かって移動し、それに伴って試料中のドー
パントも移動してしまう、結果濃度分布が緩和されたガ
ラスとなってしまう、ところが本発明のように、ドーパ
ントの一様にしみ込んだ試料を湯中にて分布つけると、
湯からとり出した後、試料の表面付近の水分は自然に蒸
発する。したがって、溶媒が中心付近にしか存在しない
ため、ドーパントが溶媒に溶けて移動する可能性が少な
くなる。またこの後、溶媒が周囲に向かって移動を開始
するが、この移動前に、150℃以上の高熱で乾燥を行
うことによりって、ドーパントの移動無しに溶媒を取り
除くことができる。結果として、きれいな濃度勾配を有
する多孔質ガラス体を得ることができ、これを焼結する
ことにより光伝達用ガラス体が得られる。
However, during this drying process, the solvent in the sample moves from near the center toward the periphery, and the dopants in the sample also move accordingly, resulting in a glass with a relaxed concentration distribution. As in the invention, if a sample uniformly impregnated with dopant is distributed in hot water,
After removing the sample from hot water, the water near the surface of the sample evaporates naturally. Therefore, since the solvent is present only near the center, there is less possibility that the dopant will dissolve in the solvent and move. Further, after this, the solvent starts to move toward the surroundings, but by drying at a high temperature of 150° C. or higher before this movement, the solvent can be removed without moving the dopant. As a result, a porous glass body having a clear concentration gradient can be obtained, and by sintering this, a glass body for light transmission can be obtained.

[実施例] 以下本発明について実施例に基づいて詳細に説明する。[Example] The present invention will be described in detail below based on examples.

実施例−1 エチルミリケート (S i  (OC2H5) 4 
)  1mol 、水 8.7molの比で混合した液
にINの塩酸を加え激しく攪拌し加水分解を行った後、
5i02微粒子を加え超音波照射を行い均質度の高いゾ
ルを得た。このゾルを内径10o+mΦのチューブの中
に流し込み30℃で保持したところ3日後に固まった。
Example-1 Ethyl millicate (S i (OC2H5) 4
) 1 mol of water and 8.7 mol of water, IN hydrochloric acid was added and stirred vigorously to perform hydrolysis.
5i02 fine particles were added and ultrasonic irradiation was performed to obtain a highly homogeneous sol. When this sol was poured into a tube with an inner diameter of 10°+mΦ and kept at 30°C, it solidified after 3 days.

その後60℃で5日間乾燥を行ない、一定のプログラム
のもとで1050℃まで焼結を行い外径61Φの多孔質
ガラスを得た。この多孔質ガラスには全体積の17%の
孔が存在している。
Thereafter, it was dried at 60°C for 5 days and sintered to 1050°C under a certain program to obtain a porous glass with an outer diameter of 61Φ. This porous glass has pores that account for 17% of the total volume.

この多孔質ガラスを80℃の硝酸セシウム飽和水溶液中
に数時間保持し、多孔質内に硝酸セシウムを十分に拡散
させた。この後95℃の湯中に該試料を5分間浸した。
This porous glass was held in a saturated aqueous solution of cesium nitrate at 80° C. for several hours to sufficiently diffuse cesium nitrate within the pores. After this, the sample was immersed in hot water at 95°C for 5 minutes.

5分後に試料を湯から取り出し、300℃の炉中で急激
に乾燥させた。この後該試料を一定プログラムで焼結を
行い閉孔化させ透明ガラス体を得た。この透明ガラス体
には第1図に示す様な濃度分布がついていた。
After 5 minutes, the sample was removed from the hot water and rapidly dried in an oven at 300°C. Thereafter, the sample was sintered according to a certain program to close the pores and obtain a transparent glass body. This transparent glass body had a concentration distribution as shown in FIG.

比較例−1 実施例−1と同様の方法で多孔質ガラス体内に硝酸セシ
ウムを十分に拡散させた試料をエタノールと水の体積比
1:1の40℃の溶液中に浸し濃度分布を生じさせたf
&該試才+1を60℃で乾燥した。
Comparative Example-1 A sample in which cesium nitrate was sufficiently diffused into a porous glass body in the same manner as in Example-1 was immersed in a solution of ethanol and water at a volume ratio of 1:1 at 40°C to generate a concentration distribution. ta f
& The sample +1 was dried at 60°C.

この後一定のプログラムのもとで閉孔化させ透明ガラス
体を得た。この透明ガラス体にはflS2図に示す様な
濃度分布がついていた。
Thereafter, the pores were closed under a certain program to obtain a transparent glass body. This transparent glass body had a concentration distribution as shown in the flS2 diagram.

以上のようにドーパントの一様にしに込んだ試ネ11に
湯中で分布を生じさせた後すぐに150″C以上の温度
で乾燥することにより、得られるガラス体の濃度分布が
明らかに向上していることがわかる。
As described above, the concentration distribution of the resulting glass body is clearly improved by immediately drying at a temperature of 150"C or more after creating a distribution in the sample 11 in which the dopant is uniformly soaked in hot water. I know what you're doing.

[発明の効果] 以上述べた様に本発明によれば、ドーパントの一様にし
み込んだ試p1に湯中で分布を生じさせた後すぐに15
0℃以上の温度で乾燥を行なうので−ta固定されたド
ーパントが溶媒の移動により緩和されるということがな
くなる。したがって該多孔質体を閉孔化することにより
その屈折率が二乗分布を有する透明ガラス体を得ること
ができる。
[Effects of the Invention] As described above, according to the present invention, immediately after causing distribution in sample P1 in which the dopant was uniformly soaked in hot water, 15
Since drying is performed at a temperature of 0° C. or higher, the -ta fixed dopant is not relaxed by movement of the solvent. Therefore, by making the porous body closed, a transparent glass body whose refractive index has a square distribution can be obtained.

こうして得られたガラス体の屈折率はきれいな二乗分布
を有しているため、エネルギー伝達用ガラスやセルフォ
ックレンズ、光フアイバー用母材等に応用できるもので
ある。
Since the refractive index of the glass body thus obtained has a clean square law distribution, it can be applied to energy transmission glasses, SELFOC lenses, optical fiber base materials, etc.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は実施例−1で得られたガラス体中のセシウムの
濃度分布図、第2図は比較例−1で得られたガラス体中
のセシウムの濃度分布を示す図。 以   上 (中1い        (4F馴 〔半径方向] 第1図
FIG. 1 is a diagram showing the concentration distribution of cesium in the glass body obtained in Example-1, and FIG. 2 is a diagram showing the concentration distribution of cesium in the glass body obtained in Comparative Example-1. Above (1st year of junior high school) (4F standard [radial direction] Fig. 1)

Claims (1)

【特許請求の範囲】[Claims] 多孔質ガラスにドーパントを拡散させた後、溶媒中に試
料を入れドーパントの濃度に分布を生じさせ、その後ド
ーパントの濃度分布を固定させ、乾燥、焼結を経て屈折
率分布ガラス体を得る光伝送用ガラス体の製造方法のド
ーパントの濃度分布及び該分布の固定時において、ドー
パントの一様にしみ込んだ試料に湯中で分布を生じさせ
た後すぐに150℃以上の温度で乾燥することを特徴と
する光伝送用ガラス体の製造方法。
After dopant is diffused into porous glass, a sample is placed in a solvent to create a dopant concentration distribution, and then the dopant concentration distribution is fixed, and a gradient index glass body is obtained through drying and sintering. Optical transmission. In the dopant concentration distribution and the fixing of the dopant concentration distribution in the method for producing a glass body for use, a sample uniformly impregnated with the dopant is made to have a distribution in hot water, and then immediately dried at a temperature of 150°C or higher. A method for manufacturing a glass body for optical transmission.
JP3520287A 1987-02-18 1987-02-18 Production of glass body for optical transmission Pending JPS63206318A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3520287A JPS63206318A (en) 1987-02-18 1987-02-18 Production of glass body for optical transmission

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3520287A JPS63206318A (en) 1987-02-18 1987-02-18 Production of glass body for optical transmission

Publications (1)

Publication Number Publication Date
JPS63206318A true JPS63206318A (en) 1988-08-25

Family

ID=12435274

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3520287A Pending JPS63206318A (en) 1987-02-18 1987-02-18 Production of glass body for optical transmission

Country Status (1)

Country Link
JP (1) JPS63206318A (en)

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