JPH0130769B2 - - Google Patents
Info
- Publication number
- JPH0130769B2 JPH0130769B2 JP21060981A JP21060981A JPH0130769B2 JP H0130769 B2 JPH0130769 B2 JP H0130769B2 JP 21060981 A JP21060981 A JP 21060981A JP 21060981 A JP21060981 A JP 21060981A JP H0130769 B2 JPH0130769 B2 JP H0130769B2
- Authority
- JP
- Japan
- Prior art keywords
- porous body
- glass
- sintering
- film layer
- container
- 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
- 239000011521 glass Substances 0.000 claims description 29
- 238000005245 sintering Methods 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 5
- 239000005373 porous glass Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- RLOWWWKZYUNIDI-UHFFFAOYSA-N phosphinic chloride Chemical compound ClP=O RLOWWWKZYUNIDI-UHFFFAOYSA-N 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
Landscapes
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Description
【発明の詳細な説明】
本発明は多孔質体を焼結する際封入容器を用い
ずに該ガラス中に含まれる添加物の逃散を抑え、
かつ比較的低温でも加圧焼結を行うことのできる
焼結方法に関する。Detailed Description of the Invention The present invention suppresses escape of additives contained in the glass without using an enclosure when sintering a porous body,
The present invention also relates to a sintering method that allows pressure sintering to be performed even at relatively low temperatures.
従来多孔質体あるいは粒状物の集合体を焼結す
る方法として第１図に示す方法がある。これは、
多孔質体１０を圧力伝達用の容器１１に封入し、
これを加熱炉１２に装入して炉内に加圧流体を供
給し、この流体による静圧を加えながら容器ごと
多孔質体を加熱することにより焼結する方法であ
る。この手法は、(i)焼結の進み難い物質が比較的
低温かつ短時間で焼結が進み、高密度体が得られ
る。(ii)流体により静圧を加えると圧力を等方的に
印加できるため焼結前の形状がそのまま保持され
て焼結できるなどの長所があり有用である。一
方、この方法での難点は、流体により圧力を印加
させる際に必要となる圧力伝達用の容器に関する
問題である。この圧力伝達用容器としては、流体
分子を容器内部に通さず、高温に耐え、かつ加圧
に応じて容易に変形することが必要である。従来
この容器としては焼結条件、例えば温度、圧力、
被焼結体の材質などに応じて個々に特殊な金属
や、ガラス材などが使用されている。ところがこ
の容器を用いる方法においてはこの容器が被焼結
体を汚染し易く、汚染を避けるために特殊な材質
のものを用いる必要がある。また焼結後にこの容
器を除去する場合にその手間が煩雑であるなどの
欠点がある。更に上記容器と被焼結体との隙間が
大きいと、これらを加圧した際、被焼結体に圧力
が加わる時間的なずれが生じ、この加圧の部分的
なずれにより被焼結体が変形を受ける場合があ
る。 As a conventional method for sintering a porous body or an aggregate of granular materials, there is a method shown in FIG. this is,
The porous body 10 is enclosed in a pressure transmission container 11,
This is a method of sintering by charging the porous body into the heating furnace 12, supplying pressurized fluid into the furnace, and heating the porous body together with the container while applying static pressure due to the fluid. In this method, (i) materials that are difficult to sinter are sintered at relatively low temperatures and in a short period of time, resulting in a high-density body. (ii) When static pressure is applied using a fluid, the pressure can be applied isotropically, so the shape before sintering can be maintained as it is during sintering, which is useful. On the other hand, a difficulty with this method is the problem with the pressure transmission container required when applying pressure with a fluid. This pressure transmitting container must not allow fluid molecules to pass through the inside of the container, withstand high temperatures, and be easily deformed in response to pressurization. Traditionally, this container has been designed to meet the sintering conditions, such as temperature, pressure,
Depending on the material of the object to be sintered, special metals, glass materials, etc. are used. However, in the method using this container, the container tends to contaminate the object to be sintered, and it is necessary to use a special material to avoid contamination. Further, there is a drawback that it is troublesome to remove the container after sintering. Furthermore, if the gap between the container and the object to be sintered is large, when pressurizing them, there will be a time lag in applying pressure to the object to be sintered, and this partial deviation in pressure will cause the object to be sintered to may undergo deformation.
本発明は上記欠点を解消する焼結方法を提供す
るものであり、その構成は、多孔質体の表面にガ
ラス膜層を形成した後、該成形体を加熱炉に装入
し、加圧流体を該加熱炉に供給して上記多孔質体
をガラス膜層ごと熱間静圧成形下で焼結すること
を特徴とする。 The present invention provides a sintering method that eliminates the above-mentioned drawbacks, and its configuration is such that after forming a glass film layer on the surface of a porous body, the molded body is charged into a heating furnace, and pressurized fluid is applied to the formed body. is supplied to the heating furnace, and the porous body is sintered together with the glass film layer under hot isostatic pressing.
以下に本発明を図面を参照して詳細に説明す
る。 The present invention will be explained in detail below with reference to the drawings.
本発明の多孔質体としてはVAD法、外付法、
内付法などにより形成されたガラス微粒子体や、
分相を利用して形成された多孔質ガラス体を用い
ることができる。又、その他の多孔質体であつて
もよい。該多孔質体２０を容器２４内に挿入し、
容器内部にHeガスを供給して該多孔質体２０を
Heガス雰囲気中に保持する。上記Heガスの処理
により多孔質体２０の表面に吸着しているガスが
取除かれ、代りにHeガスが多孔質体２０の表面
に吸着される。Heガスは多孔質体２０に溶解し
拡散し易い反面、不活性なため多孔質体２０の成
分と反応しない。このためHeを吸着させた多孔
質体２０は熔融ガラス膜層２１を形成した後の加
圧処理中に気泡を生ずることがなく、高密度な焼
結体を得ることができる。次に上記Heガス処理
の後に多孔質体２０の表面にガラス膜層２１を形
成する。該ガラス膜層２１を形成するには第３図
に示すようにバーナ２２にH2ガス、O2ガスと共
にガラス原料であるSiCl4、POCl3、BBr3、
TiCl4、AlCl3、などを導き、高温の火炎加水分
解により上記原料ガスを熱焼させてSiO2、P2O5、
B2O3、TiO2、Al2O3などの微粒子を火炎中で形
成させると共にこの微粒子を上記多孔質体２０を
被うようにその表面に熔融ガラス状態で堆積させ
る。ここで上記ガラス膜層２１の材質としては、
多孔質ガラスの焼結の場合、該多孔質ガラスの焼
結温度に対応させ、POCl3、BBr3などの添加物
によりその性質を調整する。即ち、多孔質体の焼
結温度が低い場合には、P2O5、B2O3などのSiO2
ガラスを軟化させる添加剤を加えてガラス膜層の
焼結温度を内部の多孔質体に一致させ、又、多孔
質体の焼結温度が高い場合にはSiCl4、TiCl4、
AlCl3などを原料に加えより硬質なSiO2−TiO2−
Al2O3系ガラス等の膜層を多孔質体外面に形成す
る。尚、該ガラス膜層の厚さは多孔質体２０が径
50mmφ程度のガラス体である場合に約３mm程度で
よい。ガラス膜層２１を表面に設けた多孔質ガラ
ス体２０を加熱炉に装入し、所定の流圧を有する
加圧ガスを加熱炉に供給して、上記多孔質ガラス
体２０に静圧を加えながら炉内を高温に加熱して
該多孔質ガラス体２０を熱間焼結し、焼結ガラス
体２３を造る。 The porous body of the present invention includes VAD method, external method,
Glass particles formed by internal attachment method, etc.
A porous glass body formed using phase separation can be used. Also, other porous bodies may be used. Inserting the porous body 20 into a container 24,
The porous body 20 is heated by supplying He gas into the inside of the container.
Maintained in He gas atmosphere. By the He gas treatment described above, the gas adsorbed on the surface of the porous body 20 is removed, and He gas is adsorbed on the surface of the porous body 20 instead. Although He gas easily dissolves and diffuses in the porous body 20, it does not react with the components of the porous body 20 because it is inert. Therefore, the porous body 20 on which He is adsorbed does not generate bubbles during the pressure treatment after forming the molten glass film layer 21, and a high-density sintered body can be obtained. Next, after the He gas treatment, a glass film layer 21 is formed on the surface of the porous body 20. To form the glass film layer 21, as shown in FIG. 3, the burner 22 is filled with H 2 gas, O 2 gas, and glass raw materials SiCl 4 , POCl 3 , BBr 3 ,
TiCl 4 , AlCl 3 , etc. are introduced, and the above raw material gas is sintered by high-temperature flame hydrolysis to produce SiO 2 , P 2 O 5 , etc.
Fine particles of B 2 O 3 , TiO 2 , Al 2 O 3 and the like are formed in a flame and deposited in a molten glass state on the surface of the porous body 20 so as to cover it. Here, the material of the glass film layer 21 is as follows:
In the case of sintering porous glass, its properties are adjusted using additives such as POCl 3 and BBr 3 in accordance with the sintering temperature of the porous glass. That is, when the sintering temperature of the porous body is low, SiO 2 such as P 2 O 5 and B 2 O 3
An additive that softens the glass is added to match the sintering temperature of the glass membrane layer to that of the internal porous body, and if the sintering temperature of the porous body is high, SiCl 4 , TiCl 4 ,
By adding AlCl 3 etc. to the raw materials, harder SiO 2 −TiO 2 −
A film layer of Al 2 O 3 glass or the like is formed on the outer surface of the porous body. The thickness of the glass membrane layer is determined by the diameter of the porous body 20.
In the case of a glass body of about 50 mmφ, the thickness may be about 3 mm. A porous glass body 20 having a glass membrane layer 21 on its surface is placed in a heating furnace, and a pressurized gas having a predetermined flow pressure is supplied to the heating furnace to apply static pressure to the porous glass body 20. While heating the inside of the furnace to a high temperature, the porous glass body 20 is hot sintered to produce a sintered glass body 23.
次いで必要に応じ、焼結ガラス体２３を機械的
研削し、又はHF液を用いてエツチングすること
により上記ガラス膜層２１を除去する。尚、光フ
アイバ用ガラスを製造する際には上記ガラス膜層
２１を比較的厚く形成して該ガラス膜層２１をク
ラツドに代用させることも可能であり、勿論この
場合、膜層除去の後処理を施す必要はない。 Then, if necessary, the glass film layer 21 is removed by mechanically grinding the sintered glass body 23 or etching it using an HF solution. Incidentally, when manufacturing optical fiber glass, it is also possible to form the glass film layer 21 relatively thick and use the glass film layer 21 as a cladding.Of course, in this case, post-treatment for film layer removal is required. There is no need to apply
以上述べた本発明の焼結方法によれば、ガラス
膜層２１が多孔質ガラス体２０の表面を被うこと
から、従前の加圧焼結で用いていたような容器を
必要としない。このため焼結後に圧力伝達用容器
を除去するなどの手間が省ける。更に被焼結体が
圧力伝達用容器によつて汚染されることもない。
又本発明においては多孔質体の表面上にガラス膜
層を形成するため従前みられたような容器と被焼
結体との間の隙間に起因する変形歪み等も生ずる
ことがない。 According to the sintering method of the present invention described above, since the glass membrane layer 21 covers the surface of the porous glass body 20, there is no need for a container as used in conventional pressure sintering. This eliminates the need to remove the pressure transmission container after sintering. Furthermore, the body to be sintered is not contaminated by the pressure transmission vessel.
Further, in the present invention, since a glass film layer is formed on the surface of the porous body, deformation and strain caused by the gap between the container and the body to be sintered, which have been observed in the past, do not occur.
第１図は従来の加圧焼結方法の装置構成概略
図、第２図ないし第４図は本発明の焼結方法を示
す説明図であり、第２図は多孔質体のHeガス処
理、第３図はガラス膜層の形成、第４図は焼結工
程をそれぞれ示す。
図中１０，２０……多孔質体、１１……容器、
１２……加熱炉、１３……加圧流体、２１……ガ
ラス膜層、２２……バーナ、２３……焼結ガラス
体、２４……容器である。
Fig. 1 is a schematic diagram of the equipment configuration of a conventional pressure sintering method, Figs. 2 to 4 are explanatory diagrams showing the sintering method of the present invention, and Fig. 2 shows He gas treatment of a porous body, FIG. 3 shows the formation of the glass film layer, and FIG. 4 shows the sintering process. In the figure, 10, 20... porous body, 11... container,
12... Heating furnace, 13... Pressurized fluid, 21... Glass film layer, 22... Burner, 23... Sintered glass body, 24... Container.
Claims (1)
該成形体を加熱炉に装入し、加圧流体を該加熱炉
に供給して上記多孔質体をガラス膜層ごと熱間静
圧成形下で焼結することを特徴とする多孔質体の
焼結方法。 ２ 上記多孔質体をHe雰囲気に保持した後に該
多孔質体の表面にガラス膜層を形成することを特
徴とする特許請求の範囲第１項記載の多孔質体の
焼結方法。[Claims] 1. After forming a glass membrane layer on the surface of the porous body,
A porous body characterized in that the molded body is charged into a heating furnace, a pressurized fluid is supplied to the heating furnace, and the porous body is sintered together with the glass film layer under hot isostatic forming. Sintering method. 2. The method of sintering a porous body according to claim 1, wherein a glass film layer is formed on the surface of the porous body after the porous body is held in a He atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21060981A JPS58113232A (en) | 1981-12-26 | 1981-12-26 | Sintering of porous body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21060981A JPS58113232A (en) | 1981-12-26 | 1981-12-26 | Sintering of porous body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58113232A JPS58113232A (en) | 1983-07-06 |
| JPH0130769B2 true JPH0130769B2 (en) | 1989-06-21 |
Family
ID=16592152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21060981A Granted JPS58113232A (en) | 1981-12-26 | 1981-12-26 | Sintering of porous body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58113232A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6265947A (en) * | 1985-09-14 | 1987-03-25 | Tatsuta Electric Wire & Cable Co Ltd | Production of base material for optical fiber |
| JP4738163B2 (en) * | 2005-12-22 | 2011-08-03 | Ｎｏｋ株式会社 | Manufacturing method of inorganic composite hollow tube |
| JP4742852B2 (en) * | 2005-12-22 | 2011-08-10 | Ｎｏｋ株式会社 | Manufacturing method of inorganic composite hollow tube |
-
1981
- 1981-12-26 JP JP21060981A patent/JPS58113232A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58113232A (en) | 1983-07-06 |
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