JP2507375B2 - Method and apparatus for pressurizing and enclosing container - Google Patents
Method and apparatus for pressurizing and enclosing containerInfo
- Publication number
- JP2507375B2 JP2507375B2 JP18887A JP18887A JP2507375B2 JP 2507375 B2 JP2507375 B2 JP 2507375B2 JP 18887 A JP18887 A JP 18887A JP 18887 A JP18887 A JP 18887A JP 2507375 B2 JP2507375 B2 JP 2507375B2
- Authority
- JP
- Japan
- Prior art keywords
- container
- stopper
- tapered hole
- tubular inlet
- pressure
- 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 - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は容器の加圧封入方法及び装置に関し、特に、
結晶原料を石英管等に加圧封入して結晶を製造するに適
したものである。TECHNICAL FIELD The present invention relates to a method and a device for pressurizing and enclosing a container, and in particular,
It is suitable for producing crystals by pressure-sealing the crystal raw material in a quartz tube or the like.
従来、結晶原料等を収容した石英管に石英の栓を入
れ、管の端部を真空に引きながら、栓の部分を外側から
酸水素バーナーで加熱溶融して真空封入、若しくは減圧
封入が行われていた。Conventionally, a quartz stopper was placed in a quartz tube containing a crystal raw material and the like, and the end portion of the tube was evacuated, while the stopper was heated and melted from the outside with an oxyhydrogen burner to perform vacuum sealing or vacuum sealing. Was there.
このように封入された原料を加熱して結晶成長を行う
ときには、原料中の揮発性成分が揮発し、原料融液の組
成を調整することが困難であつた。When the thus-encapsulated raw material is heated to grow crystals, the volatile components in the raw material are volatilized, and it is difficult to adjust the composition of the raw material melt.
そこで、管内を予じめ加圧して封入することが考えら
れるが、石英管を酸水素バーナーで加熱溶融するときに
管内の圧力により石英管が膨れて封入できなかつた。Therefore, it is conceivable to pre-pressurize the inside of the tube and seal it, but when the quartz tube was heated and melted by an oxyhydrogen burner, the quartz tube swelled due to the pressure in the tube and could not be sealed.
本発明は従来不可能であつた容器の加圧封入を可能に
した封入方法及び封入装置を提供しようとするものであ
り、揮発性成分を含有する被処理物を加圧封入し、被処
理物の組成制御を容易にするものである。The present invention is intended to provide an encapsulation method and an encapsulation device that enable pressure encapsulation of a container, which has been impossible in the past, and encapsulates an object to be treated containing a volatile component under pressure, It facilitates the control of the composition.
本発明は、 （１） 容器を加圧封入する方法において、被処理物等
を容器に収容し、テーパー状の穴を有する第１の栓と該
テーパー状の穴に密着可能な第２の栓を容器の管状入口
に挿入し、容器の管状入口端を真空手段と接続して容器
内を真空に保ちながら、第１の栓の挿入位置を容器外か
ら加熱して第１の栓を容器に融着し、次いで、真空手段
を加圧ガス源に流路を切換えて容器内を加圧状態に保
ち、第２の栓をマニピユレーターで第１の栓に挿入した
後加圧力を高めて密着させ第２の栓の裏に付設したマイ
クロヒーターに通電して第２の栓を第１の栓と融着する
ことを特徴とする容器の加圧封入方法、 （２） 容器を加圧封入する装置において、被処理物等
を収容するための管状入口を有する容器と、テーパー状
の穴を有し、かつ、容器の管状入口に内接する第１の栓
と、テーパー状の穴に密着可能な第２の栓と、第２の栓
の裏に付設するマイクロヒーターと、第２の栓を操作す
るマニユピレーターと、容器の管状入口端を気密にする
蓋と、該蓋に設けた開口と真空装置及び加圧ガス源とを
弁を介して接続する導管と、第１の栓を容器の管状入口
に融着するための加熱装置とを有することを特徴とする
容器の加圧封入装置である。The present invention provides: (1) In a method of pressure-sealing a container, a first plug having a tapered hole for accommodating an object to be treated and the like, and a second plug capable of closely contacting the tapered hole. Is inserted into the tubular inlet of the container, the tubular inlet end of the container is connected to a vacuum means to maintain the inside of the container under vacuum, and the insertion position of the first stopper is heated from outside the container to put the first stopper into the container. Fusing, and then switching the flow path of the vacuum means to the pressurized gas source to keep the inside of the container pressurized, insert the second stopper into the first stopper with the manipulator, and then increase the pressure. A method of pressurizing and encapsulating a container, characterized in that a micro heater attached to the back of the second cap and energized to fuse the second cap with the first cap, (2) pressurizing and encapsulating the container In the device, a container having a tubular inlet for accommodating an object to be treated and the like, and a tapered hole, and A first stopper inscribed in the tubular inlet, a second stopper capable of adhering to a tapered hole, a micro heater attached to the back of the second stopper, a manipulator for operating the second stopper, and a container A lid for hermetically sealing the tubular inlet end, a conduit for connecting the opening provided in the lid with a vacuum device and a pressurized gas source via a valve, and a first stopper for fusing the tubular inlet of the container It is a pressurizing and enclosing device for a container, which has a heating device.
なお、容器と第１の栓、第２の栓を石英で構成すると
融着が容易となる。また、接合面を予じめスリガラス状
にしておくと、融着時に透明になるので接合面の安全な
融着を確認することが容易となる。If the container, the first stopper, and the second stopper are made of quartz, fusion can be facilitated. Further, if the joint surface is preliminarily ground glass, it becomes transparent at the time of fusion, so that it becomes easy to confirm the safe fusion of the joint surface.
第１図は、本発明の１つの具体例である加圧封入装置
の概念図である。一端を封じた石英管１の中に原料10を
収容し、テーパーの穴を有する第１の栓２と該穴に密着
する円錐形の第２の栓３を挿入する。次に、真空装置７
により石英管内を真空に保ちながら酸水素バーナー11で
第１の栓２を石英管１に融着させる。それから、加圧ガ
ス源８からの加圧ガスを石英管１内に満し、マニユピレ
ーター５で第２の栓３を第１の栓のテーパー状穴に密着
させる。その後、第２の栓の裏に付設するマイクロヒー
ター４に電源６から通電して第２の栓３を第１の栓と融
着させる。なお、石英管１と真空装置７、加圧ガス源８
との間にチヤンバー９を設けた。また、チヤンバー９の
上方には、リークバルブを介して、大気に連通する導管
を設けた。FIG. 1 is a conceptual diagram of a pressure sealing device which is one specific example of the present invention. A raw material 10 is housed in a quartz tube 1 having one end sealed, and a first plug 2 having a tapered hole and a second conical plug 3 closely contacting the hole are inserted. Next, the vacuum device 7
Thus, the first stopper 2 is fused to the quartz tube 1 by the oxyhydrogen burner 11 while keeping the inside of the quartz tube in vacuum. Then, the pressurized gas from the pressurized gas source 8 is filled in the quartz tube 1, and the second stopper 3 is brought into close contact with the tapered hole of the first stopper by the manipulator 5. Then, the micro heater 4 attached to the back of the second plug is energized from the power source 6 to fuse the second plug 3 with the first plug. The quartz tube 1, the vacuum device 7, and the pressurized gas source 8
A chamber 9 is installed between Further, a conduit communicating with the atmosphere via a leak valve is provided above the chamber 9.
第１図の装置を用いて、InとAs及びB2O3を封入し、In
As多結晶の合成を行なつた。石英管は内径17.5mmφのも
のを用いた。第１の栓は外径が17mmφで長さ10mmL、テ
ーパー状穴の最大径を5mmφとした。第２の栓は第１の
栓のテーパー状穴に現物合わせしたもので、第１の栓及
び第２の栓を分離した状態で石英管内に挿入した。Encapsulating In, As, and B 2 O 3 using the device shown in FIG.
As polycrystal was synthesized. The quartz tube used had an inner diameter of 17.5 mmφ. The first plug had an outer diameter of 17 mmφ and a length of 10 mmL, and the maximum diameter of the tapered hole was 5 mmφ. The second stopper was actually matched with the tapered hole of the first stopper, and was inserted into the quartz tube in a state where the first stopper and the second stopper were separated.
まず、真空装置を用いて石英管内を10-6torrまで減圧
し、酸水素バーナーで管外から加熱して第１の栓を石英
管に融着した。次いで、加圧ガスとしてHeを用い石英管
内を5atmに加圧した後マニユピレーターを用いて第２の
栓を第１の栓のテーパー状穴に挿入し、次いで圧力を10
atmに上昇して第２の栓を密着させた。それから、マイ
クロヒーターに通電し、第２の栓を第１の栓と融着し
た。なお、マニユピレーターはアルミナ製で、マイクロ
ヒーターはアルミナに白金線を高密度に巻いたものを用
いた。First, the inside of the quartz tube was depressurized to 10 −6 torr using a vacuum device, and the first stopper was fused to the quartz tube by heating from outside the tube with an oxyhydrogen burner. Then, using He as a pressurized gas and pressurizing the inside of the quartz tube to 5 atm, the second stopper was inserted into the tapered hole of the first stopper using a manipulator, and then the pressure was adjusted to 10 atm.
Ascended to atm and brought the second stopper into close contact. Then, the micro heater was energized to fuse the second plug with the first plug. The manipulator was made of alumina, and the microheater was made by winding platinum wire at high density on alumina.
このようにして、InとAs、B2O3を5atmのHeとともに封
入したアンプルを作ることができた。In this way, an ampoule in which In, As, and B 2 O 3 were enclosed together with 5 atm of He could be made.
このアンプルを1000℃の電気炉中で５時間加熱保持し
た。このとき原料融液は20atmのHeガスにより加圧され
るためにAsが揮発することはなかつた。その後急冷して
InAsの多結晶体を得た。The ampoule was heated and held in an electric furnace at 1000 ° C. for 5 hours. At this time, since the raw material melt was pressurized by 20 atm of He gas, As did not evaporate. Then quench
A polycrystalline InAs was obtained.
この多結晶体をスライスしてその表面を観察すると気
泡は全く見い出せず、また、成分組成もストイキオメト
リツクが保たれており、電気特性も良いことが判つた。When slicing this polycrystal and observing its surface, it was found that no bubbles were found, the composition of the composition was stoichiometric, and the electrical characteristics were good.
一方、同量の原料を真空封入した後結晶合成をすると
石英管の上面に多くのAsが蒸着した。また、得られた多
結晶体スライス面を観察すると気泡だらけであつた。On the other hand, a large amount of As was deposited on the upper surface of the quartz tube when crystal synthesis was performed after vacuum-sealing the same amount of raw material. In addition, when observing the sliced surface of the obtained polycrystal, it was found to be full of bubbles.
本発明は、上記構成を採用することにより、加圧封入
を可能とし、InAs、GaAs等飛散し易い成分を含む物質の
合成を容易にし、かつ得られる物質の組成比を確実に制
御することができるようになつた。By adopting the above-mentioned configuration, the present invention enables pressure encapsulation, facilitates the synthesis of a substance containing easily scattered components such as InAs and GaAs, and reliably controls the composition ratio of the obtained substance. I was able to do it.
第１図は、本発明の一具体例である加圧封入装置の概念
図である。FIG. 1 is a conceptual diagram of a pressure sealing device which is one specific example of the present invention.
Claims (4)
物等を容器に収容し、テーパー状の穴を有する第１の栓
と該テーパー状の穴に密着可能な第２の栓を容器の管状
入口に挿入し、容器の管状入口端を真空手段と接続して
容器内を真空に保ちながら、第１の栓の挿入位置を容器
外から加熱して第１の栓を容器に融着し、次いで、真空
手段を加圧ガス源に流路を切換えて容器内を加圧状態に
保ち、第２の栓をマニピユレーターで第１の栓に挿入し
た後加圧力を高めて密着させ第２の栓の裏に付設したマ
イクロヒーターに通電して第２の栓を第１の栓と融着す
ることを特徴とする容器の加圧封入方法。1. A method of pressure-sealing a container, in which an object to be treated is housed in the container, and a first stopper having a tapered hole and a second stopper capable of closely contacting the tapered hole are provided. The first inlet of the container is heated from the outside of the container while the inside of the container is kept in a vacuum by connecting the tubular inlet end of the container to a vacuum means, and the first stopper is fused to the container. Then, switch the flow path of the vacuum means to the pressurized gas source to keep the inside of the container pressurized, insert the second stopper into the first stopper with a manipulator, and then increase the pressure to bring it into close contact. A method for pressurizing and enclosing a container, comprising energizing a micro-heater attached to the back of the second stopper to fuse the second stopper with the first stopper.
物等を収容するための管状入口を有する容器と、テーパ
ー状の穴を有し、かつ、容器の管状入口に内接する第１
の栓と、テーパー状の穴に密着可能な第２の栓と、第２
の栓の裏に付設するマイクロヒーターと、第２の栓を操
作するマニユピレーターと、容器の管状入口端を気密に
する蓋と、該蓋に設けた開口と真空装置及び加圧ガス源
とを弁を介して接続する導管と、第１の栓を容器の管状
入口に融着するための加熱装置とを有することを特徴と
する容器の加圧封入装置。2. A container for pressurizing and enclosing a container, wherein the container has a tubular inlet for accommodating an object to be treated and the like, a tapered hole, and a first inscribed in the tubular inlet of the container.
The second plug, which can be closely attached to the tapered hole, and the second
A micro heater attached to the back of the stopper, a manipulator for operating the second stopper, a lid for making the tubular inlet end of the container airtight, an opening provided in the lid, a vacuum device and a pressurized gas source. And a heating device for fusing the first stopper to the tubular inlet of the container.
することを特徴とする特許請求の範囲第２項記載の容器
の加圧封入装置。3. The pressure encapsulating device for a container according to claim 2, wherein the container, the first stopper and the second stopper are made of quartz.
ガラス状とすることを特徴とする特許請求の範囲第３項
記載の容器の加圧封入装置。4. The pressure encapsulating device for a container according to claim 3, wherein the joint surfaces of the first stopper and the second stopper have a ground glass shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18887A JP2507375B2 (en) | 1987-01-06 | 1987-01-06 | Method and apparatus for pressurizing and enclosing container |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18887A JP2507375B2 (en) | 1987-01-06 | 1987-01-06 | Method and apparatus for pressurizing and enclosing container |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63170295A JPS63170295A (en) | 1988-07-14 |
| JP2507375B2 true JP2507375B2 (en) | 1996-06-12 |
Family
ID=11467018
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18887A Expired - Lifetime JP2507375B2 (en) | 1987-01-06 | 1987-01-06 | Method and apparatus for pressurizing and enclosing container |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2507375B2 (en) |
-
1987
- 1987-01-06 JP JP18887A patent/JP2507375B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63170295A (en) | 1988-07-14 |
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