JPH03153544A - Production of rare earth element-dopoed glass - Google Patents
Production of rare earth element-dopoed glassInfo
- Publication number
- JPH03153544A JPH03153544A JP29425989A JP29425989A JPH03153544A JP H03153544 A JPH03153544 A JP H03153544A JP 29425989 A JP29425989 A JP 29425989A JP 29425989 A JP29425989 A JP 29425989A JP H03153544 A JPH03153544 A JP H03153544A
- Authority
- JP
- Japan
- Prior art keywords
- rare earth
- earth element
- soot body
- glass
- solution
- 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
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 57
- 239000011521 glass Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 13
- 239000004071 soot Substances 0.000 claims abstract description 57
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 238000011282 treatment Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 3
- 238000000151 deposition Methods 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 14
- 238000002791 soaking Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 239000013307 optical fiber Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002093 peripheral effect Effects 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
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 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
- C03B37/014—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]
- C03B37/01413—Reactant delivery systems
- C03B37/01433—Reactant delivery systems for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the porous glass preform
-
- 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
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野コ
この発明は、希土類元素ドープガラスの製造方法に関し
、特に希土類元素が均一にドープされたガラスを提供可
能としたものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing glass doped with a rare earth element, and in particular, it is possible to provide a glass uniformly doped with a rare earth element.
［従来の技術］
従来、希土類元素ドープガラスの製造方法として以下の
ような方法が用いられていた。[Prior Art] Conventionally, the following method has been used as a method for manufacturing rare earth element-doped glass.
まずＶＡＤ法等によりガラス微粒子が心棒の先端部に堆
積されてなるスート体を作成し、このスー４体を、希土
類元素が溶媒中に溶解されてなる溶液中に浸漬し、スー
ト体中に希土類元素を充分に含浸させる。ついで第２図
に示したような均熱炉２内で上記処理が施されたスート
体ｌに加熱乾燥処理を行う。さらにこの後に焼結処理を
施してスート体ｌを透明ガラス化し、かくして希土類元
素ドープガラスとすることができる。First, a soot body in which glass fine particles are deposited on the tip of a mandrel is created using the VAD method, etc., and the four soot bodies are immersed in a solution in which rare earth elements are dissolved in a solvent. Thoroughly impregnate the elements. Next, the soot body l subjected to the above treatment is subjected to a heat drying treatment in a soaking furnace 2 as shown in FIG. Furthermore, after this, a sintering treatment is performed to turn the soot body 1 into transparent glass, thus making it possible to obtain rare earth element-doped glass.
［発明が解決しようとする課題］
ところが上記従来方法においては、第２図に示したよう
に、希土類元素が含浸されたスート体■を鉛直方向に配
置して加熱乾燥処理を施すので、スート体１に含浸され
た希土類元素溶液か自重でスート体１の下部に集中する
。よってスート体ｌの下部の希土類元素の含浸濃度が高
くなり、希土類元素が長尺方向で均一濃度でドープされ
たガラスを得ることは困難であった。[Problems to be Solved by the Invention] However, in the above conventional method, as shown in FIG. The rare earth element solution impregnated in soot body 1 concentrates in the lower part of soot body 1 due to its own weight. Therefore, the impregnation concentration of the rare earth element in the lower part of the soot body 1 becomes high, and it is difficult to obtain a glass doped with the rare earth element at a uniform concentration in the longitudinal direction.
この発明は上記課題を解決するためになされたものであ
って、希土類元素が均一濃度でドープされたガラスが得
られる製造方法を提供することを目的としている。This invention was made to solve the above-mentioned problems, and an object of the invention is to provide a manufacturing method capable of obtaining glass doped with a rare earth element at a uniform concentration.
［課題を解決するだめの手段］
この発明の希土類元素添加ガラスの製造方法は、ガラス
微粒子を心棒の先端もしくは外周に堆積させてなるスー
ト体を、希土類元素を溶解してなる希土類元素溶液中に
浸漬して、上記スート体中に希土類元素溶液を含浸せし
めた後、加熱乾燥させ、ついで焼結処理を施して希土類
元素ドープガラスを製造する方法において、希土類元素
溶液が含浸されたスート体の心棒を水平に保ち、かつ上
記心棒を中心軸として回転さけつつ加熱乾燥処理を施す
ことを解決手段とした。[Means for Solving the Problems] The method for producing rare earth element-added glass of the present invention is to place a soot body formed by depositing glass fine particles on the tip or outer periphery of a mandrel into a rare earth element solution prepared by dissolving a rare earth element. A mandrel of a soot body impregnated with a rare earth element solution in a method of producing rare earth element doped glass by impregnating the soot body with a rare earth element solution, followed by heating and drying and then performing a sintering treatment. The solution was to perform the heat drying treatment while keeping the material horizontal and avoiding rotation about the mandrel as a central axis.
［作用］
希土類元素溶液が含浸されたスート体の心棒を平行に保
ち、かつその℃・棒を中心軸として回転させつつ加熱乾
燥処理を施すようにし、スート体の特定部分が下方を向
かないようにした。[Operation] The core of the soot body impregnated with the rare earth element solution is kept parallel and the heating drying process is performed while rotating the soot body around the center axis, so that specific parts of the soot body do not face downward. I made it.
よって加熱乾燥処理工程中に希土類元素溶液が自重で特
定部分に集中することがなくなり、均一に含浸された状
態で乾燥させることができる。Therefore, the rare earth element solution does not concentrate in a specific part due to its own weight during the heat drying process, and can be dried in a uniformly impregnated state.
以下、この発明の詳細な説明する。The present invention will be described in detail below.
まず通常のＶＡＤ法等により、スート体Ｉを作成する。First, a soot field I is created using a normal VAD method or the like.
すなわち酸水素火炎中に四塩化ケイ素等の原料ガスを供
給し、火炎加水分解反応および熱酸化反応によりガラス
微粒子を発生させ、このガラス微粒子を心棒４の軸方向
に沿って付着させることによりスート体１を得る。ここ
でスート体１とは、心棒４の先端部もしくは外周にガラ
ス微粒子が堆積された多孔質母材を指呼している。また
上記原料ガスとして、四塩化ケイ素とともに、四塩化ゲ
ルマニウム、ふっ素等の屈折率調整用の各種ドーパント
ガスを適宜供給してもよい。That is, a raw material gas such as silicon tetrachloride is supplied into an oxyhydrogen flame, glass particles are generated by a flame hydrolysis reaction and a thermal oxidation reaction, and the glass particles are attached along the axial direction of the mandrel 4 to form a soot body. Get 1. Here, the soot body 1 refers to a porous base material in which glass fine particles are deposited on the tip or outer periphery of the mandrel 4. Further, as the raw material gas, various dopant gases for adjusting the refractive index such as germanium tetrachloride and fluorine may be appropriately supplied together with silicon tetrachloride.
次に必要に応じて上記スート体ｌに加熱処理を施して、
スート体ｌの嵩密度を増加せしめても良い。加熱処理の
方法は特に限定されないが、たとえば均熱炉内にスート
体ｌを入れ、これを不活性ガス雰囲気中で回転させつつ
加熱する方法等を用いることができる。この加熱条件は
所望の嵩密度等に応じて適宜選択されるが、通常温度Ｉ
２８０〜１３２０℃、時間２〜６時間程度の条件で行い
、嵩密度０．４〜１．６ ｇ／ｃｍ’程度のスート体１
が得られる条件を選択することが好ましい。ここでスー
ト体Ｉの嵩密度を上記範囲に限定したのは、０ 、４
ｇ／ｃｏ＋’未満であると、スート体Ｉのクラックの発
生率が非常に高く、製品歩溜が低くなる不都合あり、ま
た１ 、 ６ ｇ／ｃｍ’を越えるとスート体１への希
土類元素溶液の含浸が困難あるいは不可能となる欠点が
あるためである。Next, if necessary, heat treatment is performed on the soot body l,
The bulk density of the soot body 1 may be increased. The method of heat treatment is not particularly limited, but for example, a method may be used in which the soot body I is placed in a soaking furnace and heated while rotating in an inert gas atmosphere. The heating conditions are appropriately selected depending on the desired bulk density, etc., but usually the temperature I
The soot body 1 having a bulk density of about 0.4 to 1.6 g/cm' was heated at 280 to 1320°C for about 2 to 6 hours
It is preferable to select conditions under which the following can be obtained. Here, the bulk density of the soot body I is limited to the above range because 0,4
If it is less than 1.6 g/cm', the rate of occurrence of cracks in soot body I will be very high and the product yield will be low, and if it exceeds 1.6 g/cm', the rare earth element solution will This is because there is a drawback that impregnation is difficult or impossible.
このようにスート体ｌの嵩密度を増加せしめると、希土
類元素溶液をスート体ｌに含浸させた後の乾燥工程にお
いて、クラック等の発生を減少させることができ、製品
歩溜を向上させることができる。By increasing the bulk density of the soot body 1 in this way, it is possible to reduce the occurrence of cracks, etc. in the drying process after impregnating the soot body 1 with the rare earth element solution, and it is possible to improve the product yield. can.
次に希土類元素溶液を用意する。希土類元素には、エル
ビウムの塩化物やネオジムの塩化物等を好適に用いるこ
とができるが、得られるガラスの目的、用途等に応じて
適宜選択される。溶媒としては水に塩酸を添加してなる
塩酸水溶液を好適に用いることができる。塩酸濃度は上
記希土類元素塩化物を完全に溶解可能であればよく、た
とえば水３００ｃＩＩｌｆｆに３５ｗＬ％塩酸を１〜５
Ｃ１１３程度添加してなる濃度である。またこの溶液中
の希土類元素塩化物の濃度は、ガラスへの高濃度ドープ
を可能とするように希土類元素塩化物が完全に溶解し得
る濃度であれば高い程良く、２〜１０ｗｔ％程度が好ま
しい。Next, a rare earth element solution is prepared. As the rare earth element, erbium chloride, neodymium chloride, etc. can be suitably used, and the rare earth element is appropriately selected depending on the purpose, use, etc. of the glass to be obtained. As the solvent, an aqueous hydrochloric acid solution prepared by adding hydrochloric acid to water can be suitably used. The concentration of hydrochloric acid may be as long as it can completely dissolve the rare earth element chloride.
This is the concentration obtained by adding about C113. The concentration of the rare earth element chloride in this solution is preferably as high as possible as long as the rare earth element chloride can be completely dissolved so as to enable high concentration doping into the glass, and is preferably about 2 to 10 wt%. .
この希土類元素溶液中に上記スート体Ｉを浸漬し、スー
ト体ｌ中に希土類元素溶液を含浸させる。The soot body I is immersed in this rare earth element solution to impregnate the soot body I with the rare earth element solution.
含浸は、温度２０〜２５℃で１０〜１００時間程度行い
、スート体１に溶液としてｌＯ〜２００ ｃｒａ３程度
含浸させる。ここで含浸された希土類元素は、塩化物あ
るいはイオンの形態をとっているものと考えられる。The impregnation is carried out at a temperature of 20 to 25° C. for about 10 to 100 hours, and the soot body 1 is impregnated with about 10 to 200 cr3 as a solution. The rare earth element impregnated here is considered to be in the form of chloride or ion.
次にこの含浸後のスート体ｌを乾燥させる。この乾燥工
程は第１図に示したような横型均熱炉３内で行なわれる
ことが好ましい。この横型均熱炉３は、加熱乾燥処理を
施すスート体１の心棒４を水・Ｌに収容し、かつスート
体１の心棒４を中心軸として回転させつつ加熱乾燥を行
うものである。Next, the soot body 1 after impregnation is dried. This drying step is preferably carried out in a horizontal soaking oven 3 as shown in FIG. This horizontal soaking furnace 3 houses the mandrel 4 of the soot body 1 to be heated and dried in water L, and performs heat drying while rotating the mandrel 4 of the soot body 1 as a central axis.
この横型均熱炉３内は、窒素またはアルゴン等の不活性
ガスにより満たされている。この加熱乾燥処理の条件は
特に限定されるものではないが、たとえば均熱炉３内へ
の乾燥窒素ガス流量２０Ｑ／分、温度１００℃、スート
体１の回転６ Ｑ ｒｐｍ、処理時間７２時間などとす
ることができる。The inside of this horizontal soaking furnace 3 is filled with an inert gas such as nitrogen or argon. The conditions for this heating drying treatment are not particularly limited, but include, for example, a flow rate of dry nitrogen gas into the soaking furnace 3 of 20Q/min, a temperature of 100°C, a rotation of the soot body 1 of 6Q rpm, a treatment time of 72 hours, etc. It can be done.
またスート体１の回転速度は１０〜Ｉ ＯＯｒｐｍ程度
が好ましい。ＩＯｒｐｍ未満であると、含浸された希土
類元素溶液が偏り、またＩ ＯＯｒｐｍより大きいと遠
心力により希土類元素溶液がスート体１の外周部分に偏
るためである。Further, the rotational speed of the soot body 1 is preferably about 10 to IOO rpm. If it is less than IOrpm, the impregnated rare earth element solution will be biased, and if it is larger than IOrpm, the rare earth element solution will be biased toward the outer peripheral portion of the soot body 1 due to centrifugal force.
上記加熱乾燥処理の後、ゾーン焼結炉内にてスート体１
の脱水および焼結を行い、スート体１を透明ガラス化す
る。まず脱水工程においては、ゾーン焼結炉内を０．２
％程度の濃度で塩素ガスを添加した不活性ガス雰囲気と
し、温度１０００℃程度で２〜３時間の処理とする。After the above heating and drying treatment, the soot body 1 is placed in a zone sintering furnace.
The soot body 1 is made into transparent glass by dehydration and sintering. First, in the dehydration process, the inside of the zone sintering furnace was
% concentration of chlorine gas added thereto, and the treatment is carried out at a temperature of about 1000° C. for 2 to 3 hours.
また焼結工程においては、上記脱水の後、ゾーン焼結炉
内への塩素ガスの供給を中止し、不活性ガス雰囲気中で
引き続き加熱を行う。炉内の温度は１５００〜１５５０
℃程度であり、スート体！が完全に透明ガラス化するま
で行う。In the sintering process, after the dehydration, the supply of chlorine gas into the zone sintering furnace is stopped, and heating is continued in an inert gas atmosphere. The temperature inside the furnace is 1500-1550
It is about ℃ and is a suit body! This is done until it becomes completely transparent and vitrified.
このような製造方法によれば、加熱乾燥処理工程におい
て希土類元素溶液が含浸されたスート体１の心棒４が水
平に保たれ、かつ心棒４を中心軸として回転されている
ので、スート体１の一定箇所が下方に固定されることが
なくなり、含浸された希土類元素溶液が自重で一箇所に
集中することがなくなる。よってガラス中に均一・濃度
で希土類元素をドープすることかできる。According to such a manufacturing method, the mandrel 4 of the soot body 1 impregnated with the rare earth element solution is kept horizontal and rotated about the mandrel 4 as a central axis in the heating drying process, so that the soot body 1 is heated and dried. A fixed location is no longer fixed downward, and the impregnated rare earth element solution is no longer concentrated in one location due to its own weight. Therefore, rare earth elements can be doped into the glass at a uniform concentration.
［実施例］
（実施例）
通常のＶＡＤ法により、純粋石英からなるスート体を作
成した。[Example] (Example) A soot body made of pure quartz was created by a normal VAD method.
ヘリウムガス雰囲気とされた均熱炉内に上記スート体を
入れ、１０００℃にて３時間の加熱処理を施した。この
加熱処理後のスート体の嵩密度は０ 、４５ ｇ／ｃｍ
’であった。The soot body was placed in a soaking furnace with a helium gas atmosphere, and heat treated at 1000° C. for 3 hours. The bulk density of the soot body after this heat treatment is 0.45 g/cm
'Met.
４．５ｇのＥ ｒＣ（！ｚ ” ０．５ Ｈｔｏと１
、８ ａｍ’のＨＣ（とを純水３００ ｃ＋ａ’中に溶
解せしめ、Ｅｒを含存した希土類元素溶液とした。この
希土類元素溶液中にＬ記スート体を１８時間浸漬させて
スート体中に希土類元素を充分に含浸させた。4.5 g of E rC (!z ” 0.5 Hto and 1
, 8 am' of HC (and) were dissolved in 300 c+a' of pure water to form a rare earth element solution containing Er.The soot body of L was immersed in this rare earth element solution for 18 hours to form a solution in the soot body. Thoroughly impregnated with rare earth elements.
ついで上記スート体を第１図に示したと同様の均熱炉内
に入れ、加熱乾燥処理を施した。この加熱乾燥処理条件
は温度１００℃、窒素供給１ｉ２０Ｑ／分、スート体の
回転速度６０ ｒｐｍ、処理時間７２時間とした。Next, the soot body was placed in a soaking furnace similar to that shown in FIG. 1, and subjected to a heat drying treatment. The heating drying treatment conditions were a temperature of 100° C., a nitrogen supply of 1i20 Q/min, a soot body rotation speed of 60 rpm, and a treatment time of 72 hours.
以上のような加熱乾燥処理が施されたスート体に、ＶＡ
Ｄ法で通常用いられる脱水、焼結処理を施して透明ガラ
ス化を行い、希土類元素ドープガラスとした。VA
It was subjected to dehydration and sintering treatments commonly used in Method D to make it transparent and glass doped with rare earth elements.
このようにして得られた希土類元素ドープガラスのｈｍ
および下部からそれぞれサンプルを採取し、Ｓ Ｉ Ｍ
Ｓにより各サンプルのＥ「のドープ量を調べたところ
、両者とらにｌ ＯＯｐｐｍであり、均一濃度でＥｒが
ドープされていることが確認できた。hm of the rare earth element-doped glass thus obtained
Samples were collected from the upper and lower parts of the S I M
When the doping amount of E'' in each sample was investigated using S, it was found that both samples were lOOppm, confirming that Er was doped at a uniform concentration.
（比較例）
加熱乾燥処理工程にて第２図に示したような均熱炉を用
いた以外は、上記実施例と全く同様にして希土類元素ド
ープガラスを製造した。(Comparative Example) A rare earth element-doped glass was produced in exactly the same manner as in the above example except that a soaking furnace as shown in FIG. 2 was used in the heating and drying process.
上記のようにして得られた希土類元素ドープガラスの上
部および下部からそれぞれサンプルを採取し、ＳＩＭＳ
により各サンプルのＥｒのドープ量を調べたところ、上
部のサンプルでは８０ｐｐｍ、下部のサンプルでは１２
０ ｐｐｍとなっており・Ｅｒのドープ濃度に分布が生
じた。Samples were taken from the upper and lower parts of the rare earth element-doped glass obtained as above, and SIMS
When the amount of Er doped in each sample was investigated, it was 80 ppm in the upper sample and 12 ppm in the lower sample.
0 ppm, and there was a distribution in the Er doping concentration.
［発明の効果］
以上説明したように、この発明の希土類元素添加ガラス
の製造方法は、希土類元素溶液が含浸されたスート体の
心棒を水平に保ち、かつ上記心棒を中心軸として回転さ
せつつ加熱乾燥処理を施すものであるので、スート体に
含浸された希土類元素溶液が加熱乾燥処理時に、自重に
より特定の一箇所に集中することがなくなり、希土類元
素のドープ濃度が均一なガラスを得ることができる。[Effects of the Invention] As explained above, the method for producing rare earth element-added glass of the present invention is to keep the mandrel of the soot body impregnated with the rare earth element solution horizontally, and to heat the soot body while rotating the mandrel as the central axis. Since the drying process is applied, the rare earth element solution impregnated into the soot body does not concentrate in one specific place due to its own weight during the heating drying process, making it possible to obtain glass with a uniform rare earth element doping concentration. can.
またこの発明の製造方法によって得られた希土類元素ド
ープガラスを光ファイバのコアとすれば、光ファイバの
長尺方向に沿って希土類元素が均一にドープされた希」
−類元素ドープ光ファイバを得ることができる。Furthermore, if the rare earth element-doped glass obtained by the manufacturing method of the present invention is used as the core of an optical fiber, the rare earth element can be uniformly doped along the longitudinal direction of the optical fiber.
- It is possible to obtain an optical fiber doped with a class element.
第１図はこの発明の製造方法において実施されるスート
体の加熱乾燥処理方法の一例を示す概略構成図であり、
第２図は従来のＶＡＤ法による製造方法において実施さ
れる加熱乾燥処理方法の例を示した概略構成図である。
ｌ・・スート体、
３ 横型均熱炉、
４・・・心棒。FIG. 1 is a schematic diagram showing an example of a heating drying treatment method for a soot body carried out in the manufacturing method of the present invention,
FIG. 2 is a schematic diagram showing an example of a heating drying treatment method carried out in a conventional manufacturing method using the VAD method. 1. Soot body, 3. Horizontal soaking furnace, 4. Mandrel.
Claims (1)
るスート体を、希土類元素を溶解してなる希土類元素溶
液中に浸漬して、上記スート体中に希土類元素溶液を含
浸せしめた後、加熱乾燥させ、ついで焼結処理を施して
希土類元素ドープガラスを製造する方法において、 希土類元素溶液が含浸されたスート体の心棒を水平に保
ち、かつ上記心棒を中心軸として回転させつつ加熱乾燥
処理を施すことを特徴とする希土類元素ドープガラスの
製造方法[Claims] A soot body formed by depositing glass particles on the tip or outer periphery of a mandrel is immersed in a rare earth element solution prepared by dissolving a rare earth element, so that the soot body is impregnated with the rare earth element solution. In the method of manufacturing rare earth element-doped glass by heating and drying and then performing a sintering treatment, the soot body is kept horizontally with a mandrel impregnated with a rare earth element solution and rotated about the mandrel as a central axis. A method for producing rare earth element-doped glass characterized by subjecting it to heating and drying treatment
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1294259A JP2828284B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing rare earth element doped glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1294259A JP2828284B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing rare earth element doped glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03153544A true JPH03153544A (en) | 1991-07-01 |
| JP2828284B2 JP2828284B2 (en) | 1998-11-25 |
Family
ID=17805402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1294259A Expired - Fee Related JP2828284B2 (en) | 1989-11-13 | 1989-11-13 | Method for producing rare earth element doped glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2828284B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8783906B2 (en) | 2010-04-16 | 2014-07-22 | Evolucia, Inc. | Solid state outdoor overhead lamp assembly |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6337469A (en) * | 1986-07-31 | 1988-02-18 | Sharp Corp | Statistical processing system |
| JPH0196021A (en) * | 1987-10-06 | 1989-04-14 | Mitsubishi Cable Ind Ltd | Production of base material for optical functional element |
-
1989
- 1989-11-13 JP JP1294259A patent/JP2828284B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6337469A (en) * | 1986-07-31 | 1988-02-18 | Sharp Corp | Statistical processing system |
| JPH0196021A (en) * | 1987-10-06 | 1989-04-14 | Mitsubishi Cable Ind Ltd | Production of base material for optical functional element |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8783906B2 (en) | 2010-04-16 | 2014-07-22 | Evolucia, Inc. | Solid state outdoor overhead lamp assembly |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2828284B2 (en) | 1998-11-25 |
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