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JPH10226596A - Device for synthesizing compound and method therefor - Google Patents

Device for synthesizing compound and method therefor

Info

Publication number
JPH10226596A
JPH10226596A JP2818297A JP2818297A JPH10226596A JP H10226596 A JPH10226596 A JP H10226596A JP 2818297 A JP2818297 A JP 2818297A JP 2818297 A JP2818297 A JP 2818297A JP H10226596 A JPH10226596 A JP H10226596A
Authority
JP
Japan
Prior art keywords
pressure
vessel
compound
synthesis
synthesizing
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
JP2818297A
Other languages
Japanese (ja)
Inventor
Yoshihiro Okabe
良宏 岡部
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.)
Sumitomo Metal Mining Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
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 Sumitomo Metal Mining Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Priority to JP2818297A priority Critical patent/JPH10226596A/en
Publication of JPH10226596A publication Critical patent/JPH10226596A/en
Pending legal-status Critical Current

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  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a device and a method for synthesizing a compound which can be repeatedly used, requires no process such as vacuum sealing, leaks no vapor of group V elements from a synthesizing vessel to a pressure vessel and is low in running cost. SOLUTION: While controlling vapor pressure by vapor of the group V element raw material 3 having higher dissociation pressure among component elements constituting the compound, heating of a crucible 2 bottom part, heating of a crucible 2 upper part and heating of a reservoir 4 for controlling vapor pressure are controlled and the group V element raw material 3 is moved into the crucible 2 to synthesize the compound. A vent hole 7 is provided at the synthesizing vessel 5 in order to communicate the inside of the synthesizing vessel 5 with the inside of the pressure vessel 6 and further a sealant 8 capable of opening and closing from outside of the pressure vessel 6 is provided at the air hole 7 in order to hermetically seal the space in the synthesizing vessel 5. Thus, after the pressure vessel 6 and the synthesizing vessel 5 are simultaneously evacuated to vacuum, the vent hole 7 is closed and heating is applied thereto to equalize vapor pressure of the group V element raw material 3 in the synthesizing vessel 5 and pressure of an inert gas in the pressure vessel 6.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、GaP、GaA
s、InPなどの化合物を合成する装置および方法に関
する。
TECHNICAL FIELD The present invention relates to GaP, GaAs
The present invention relates to an apparatus and a method for synthesizing a compound such as s and InP.

【0002】[0002]

【従来の技術】GaP、GaAs、InPなどの化合物
の合成方法では、V族元素(Ga、P)の蒸気圧が高い
ため、合成中のV族元素の解離を抑制する方策、あるい
は積極的にV族元素の蒸気圧を印加制御する方策が採ら
れる。
2. Description of the Related Art In a method for synthesizing a compound such as GaP, GaAs or InP, since the vapor pressure of a group V element (Ga, P) is high, measures for suppressing dissociation of the group V element during synthesis or aggressively. A measure is taken to control the application of the vapor pressure of the group V element.

【0003】前者のV族元素の解離を制御する方策で
は、III 族元素原料とV族元素原料とを同一のルツボ内
に装填し、この上にB2 3 などの液体封止剤を載せ、
V族元素の蒸気圧以上の気圧の不活性ガスを印加する。
このV族元素の解離を抑制する方策を伴う化合物の合成
方法に使用される合成装置の構成は、シンプルである。
しかし、V族元素原料から飛散する量を皆無にすること
は困難であるため、飛散する量を予めV族元素原料に加
えておく。ところが、飛散する量にばらつきが生じるた
め、合成した化合物の組成にもばらつきが生じることに
なる。また、この方法では、化合物の合成中に飛散した
V族元素が圧力容器内に付着し固化するため、化合物の
合成後に圧力容器内に固化したV族元素の除去作業(ク
リーニング)が必要となる。
In the former method of controlling the dissociation of a group V element, a group III element raw material and a group V element raw material are loaded in the same crucible, and a liquid sealant such as B 2 O 3 is placed thereon. ,
An inert gas having a pressure higher than the vapor pressure of the group V element is applied.
The configuration of a synthesis apparatus used in a method for synthesizing a compound with a measure for suppressing the dissociation of a group V element is simple.
However, since it is difficult to eliminate the amount scattered from the group V element raw material, the amount scattered is added to the group V element raw material in advance. However, since the scattering amount varies, the composition of the synthesized compound also varies. Further, in this method, since the group V element scattered during the synthesis of the compound adheres to the pressure vessel and solidifies, it is necessary to remove (solidify) the group V element solidified in the pressure vessel after the synthesis of the compound. .

【0004】後者の蒸気圧を印加制御する方策では、蒸
気圧が低いIII 族元素原料を装填した合成用ルツボとは
別に、蒸気圧制御用リザーバを設け、該蒸気圧制御用リ
ザーバ内に蒸気圧が高いV族元素原料を装填し、該蒸気
圧制御用リザーバの温度を制御する。この蒸気圧を印加
制御する方策を伴う化合物の合成方法では、蒸気圧制御
用リザーバの温度制御により、化合物の組成制御を行う
ため、化合物のロット毎に生じる組成のばらつきが小さ
い。しかし、ルツボと蒸気圧制御用リザーバとを収納
し、蒸気圧を制御する空間を構成する容器(以下合成容
器と呼ぶ)と、ルツボと蒸気圧制御用リザーバの温度を
独立して制御するヒーターとが必要となる。そのため、
前記のV族元素の解離を抑制する方策を伴う合成方法に
よる合成装置に比べて、蒸気圧を印加制御する方策を伴
う化合物の合成方法による合成装置は複雑となる。
In the latter method of controlling the application of the vapor pressure, a reservoir for controlling the vapor pressure is provided separately from a crucible for synthesis loaded with a Group III element raw material having a low vapor pressure, and the vapor pressure is stored in the reservoir for controlling the vapor pressure. Is loaded with a high V group element material, and the temperature of the vapor pressure control reservoir is controlled. In the method of synthesizing a compound with a method of controlling the application of the vapor pressure, the composition of the compound is controlled by controlling the temperature of the reservoir for controlling the vapor pressure. However, a container (hereinafter, referred to as a synthesis container) that houses a crucible and a vapor pressure control reservoir and forms a space for controlling the vapor pressure, and a heater that independently controls the temperature of the crucible and the vapor pressure control reservoir are provided. Is required. for that reason,
As compared with the above-described synthesis apparatus that employs a method of suppressing dissociation of a group V element, a synthesis apparatus that employs a compound synthesis method that includes a method of applying and controlling a vapor pressure is more complicated.

【0005】GaAs結晶を液体封止引上法により製造
する場合の化合物の合成には、引上機内で解離を抑制す
る方策を伴う化合物の合成方法を採用する。しかし、G
aAs結晶を他の製造方法で製造する場合の化合物の合
成や、Pを含む化合物結晶(GaP、InP)を製造す
る場合の化合物の合成には、蒸気圧を印加制御する方策
を伴う化合物の合成方法を採用する。
[0005] When a GaAs crystal is produced by a liquid sealing pulling method, a compound synthesizing method involving a measure for suppressing dissociation in a pulling machine is employed. But G
In the synthesis of a compound in the case of manufacturing an aAs crystal by another manufacturing method or in the synthesis of a compound in the case of manufacturing a compound crystal containing P (GaP, InP), a synthesis of a compound accompanied by a measure of controlling the vapor pressure is applied. Adopt the method.

【0006】以下、V族元素の蒸気圧を印加制御する方
策を伴う化合物の合成装置とその合成方法について、図
4と図5に基づき説明する。
Hereinafter, a compound synthesizing apparatus and a method for synthesizing the compound with a measure for applying and controlling the vapor pressure of a group V element will be described with reference to FIGS. 4 and 5.

【0007】III 族元素原料1を装填したルツボ2と、
V族元素原料3を装填した蒸気圧制御用リザーバ4は合
成容器5内に収められ、この合成容器5は圧力容器6内
に収めて、加熱され昇温する。III 族元素原料1の底部
の温度を、合成する化合物の融点とし、III 族元素原料
1の上部の温度を該融点より10〜30℃高くしてお
く。蒸気圧制御用リザーバ4は合成容器5内で最も温度
が低い部位に配置され、該部位に温度が一定となる領域
(均熱帯)を設け、該蒸気圧制御用リザーバ4の温度制
御によって蒸気圧制御が行われる。この蒸気圧制御と
は、化合物の合成において、V族元素原料3の蒸気圧が
III 族元素原料1の解離圧に等しくなる温度に制御する
ことである。これらの温度制御を実現するために、ルツ
ボ2の上部と下部と蒸気圧制御用リザーバ4は互いに独
立して温度制御されなければならず、ルツボ2の上部と
下部と蒸気圧制御用リザーバ4の加熱のために、それぞ
れヒーター15が配置される。
A crucible 2 loaded with a group III element raw material 1,
The vapor pressure control reservoir 4 loaded with the group V element raw material 3 is housed in a synthesis vessel 5, and the synthesis vessel 5 is housed in a pressure vessel 6, heated and heated. The temperature at the bottom of Group III element raw material 1 is the melting point of the compound to be synthesized, and the temperature at the top of Group III element raw material 1 is 10 to 30 ° C. higher than the melting point. The vapor pressure control reservoir 4 is disposed in the lowest temperature part in the synthesis vessel 5, and a region where the temperature is constant (uniform tropics) is provided in the part, and the vapor pressure is controlled by the temperature control of the vapor pressure control reservoir 4. Control is performed. This vapor pressure control means that in the synthesis of the compound, the vapor pressure of the group V element raw material 3 is increased.
That is, the temperature is controlled to be equal to the dissociation pressure of the group III element raw material 1. In order to realize these temperature controls, the upper and lower portions of the crucible 2 and the vapor pressure control reservoir 4 must be temperature controlled independently of each other, and the upper and lower portions of the crucible 2 and the vapor pressure control reservoir 4 A heater 15 is provided for each heating.

【0008】化合物の合成では、上記温度分布を実現
し、V族元素を蒸気にして蒸気圧制御用リザーバ4から
ルツボ2へと移動させ、ルツボ2のみを徐々に降温する
ことによって、ルツボ2の底部から上方へと化合物を固
化させる。固化の終了時点では、化合物の最上部が化合
物の融点である。固化完了まで、V族元素原料3の蒸気
圧は一定に制御される。その後、ルツボ2と蒸気圧制御
用リザーバ4とを室温まで冷却して終了する。昇温開始
から冷却終了までの間、圧力容器6は合成容器5の内圧
にバランスする気圧の不活性ガスで満たされる。
[0008] In the synthesis of the compound, the above temperature distribution is realized, the V-group element is vaporized and moved from the vapor pressure control reservoir 4 to the crucible 2, and only the crucible 2 is gradually cooled. The compound solidifies from the bottom up. At the end of solidification, the top of the compound is the melting point of the compound. Until the solidification is completed, the vapor pressure of the group V element raw material 3 is controlled to be constant. After that, the crucible 2 and the vapor pressure control reservoir 4 are cooled down to room temperature, and the process ends. During the period from the start of heating up to the end of cooling, the pressure vessel 6 is filled with an inert gas having a pressure balanced with the internal pressure of the synthesis vessel 5.

【0009】蒸気圧が制御される空間を構成する合成容
器5は、石英製の封管などの様に密閉容器であることが
望ましいが、熱分解炭素、ガラス状炭素、炭化珪素など
の通気性の無い材料を被覆したグラファイト製や、窒化
ホウ素製の、密閉性が劣る容器(以後セミシールド容器
と呼ぶ)が用いられることもある。
The synthetic vessel 5 constituting the space where the vapor pressure is controlled is desirably a closed vessel such as a sealed tube made of quartz or the like, but is preferably made of a gas permeable material such as pyrolytic carbon, glassy carbon, or silicon carbide. In some cases, a container made of graphite or boron nitride coated with a material having no seal and having poor sealing properties (hereinafter referred to as a semi-shielded container) may be used.

【0010】合成温度が石英の軟化点を超えるGaPの
様な化合物を、石英製の封管を使用して合成するために
は、高周波加熱方式を選択しなければならず、抵抗加熱
方式を採用するためには、合成容器5にセミシールド容
器を使用しなければならない。GaAsやInPなどの
化合物を合成する場合は、高周波加熱方式と抵抗加熱方
式のいずれも採用でき、密閉容器、セミシールド容器の
いずれも使用できる。一般的には、石英製の封管と高周
波加熱方式の組み合わせが採用されることが多い。
In order to synthesize a compound such as GaP whose synthesis temperature exceeds the softening point of quartz using a sealed tube made of quartz, a high-frequency heating method must be selected, and a resistance heating method is adopted. To do so, a semi-shielded container must be used for the synthesis container 5. When synthesizing a compound such as GaAs or InP, either a high-frequency heating method or a resistance heating method can be adopted, and either a closed container or a semi-shielded container can be used. Generally, a combination of a sealed tube made of quartz and a high-frequency heating method is often used.

【0011】[0011]

【発明が解決しようとする課題】しかしながら、石英製
の封管を使用し、高周波加熱方式による合成方法および
合成装置では、以下の問題がある。
However, there are the following problems in the synthesis method and the synthesis apparatus using a quartz sealed tube and using a high-frequency heating method.

【0012】合成容器を圧力容器内に装着するプロセス
の前に、III 族元素原料を装填したルツボとV族元素原
料を装填した蒸気圧制御用リザーバとを合成容器(石英
製アンプル)内に収め、該石英製アンプルを真空封止す
るプロセスが必要となり、該石英製アンプルは繰り返し
使用できない。また、高周波加熱方式では、抵抗加熱方
式に比べると装置価格が高くなり、メンテナンスも煩雑
である。いずれも、化合物の合成の製造コストを上昇さ
せるといった問題がある。さらに、合成する化合物のサ
イズが大きくなると、充分な強度を持つ石英製アンプル
の設計と、それを真空封止する作業とが難しくなるとい
った問題もある。
Prior to the process of mounting the synthesis vessel in the pressure vessel, the crucible loaded with the group III element raw material and the vapor pressure control reservoir loaded with the group V element raw material are placed in a synthesis vessel (quartz ampule). In addition, a process of vacuum-sealing the quartz ampule is required, and the quartz ampule cannot be used repeatedly. Further, in the high-frequency heating method, the device price is higher than in the resistance heating method, and the maintenance is complicated. In any case, there is a problem that the production cost of the synthesis of the compound is increased. Further, when the size of the compound to be synthesized is increased, there is a problem that it is difficult to design a quartz ampoule having sufficient strength and to vacuum seal the ampoule.

【0013】一方、合成容器をセミシールド容器とした
場合には、繰り返し使用可能で、真空封止などのプロセ
スを必要としない。しかし、制御するV族元素の蒸気
が、合成容器から圧力容器へと漏れ出すという問題があ
る。漏れ出す量は、セミシールド容器の構造と外圧(圧
力容器内不活性ガス圧)の印加の仕方次第である。漏れ
出た蒸気は、圧力容器内の温度の低い部位に付着し、固
化する。GaPやInPの化合物の合成では、発火し易
い白燐や赤燐が付着し、GaAsの合成では、毒物であ
るAsが付着する。これらの付着物のために、化合物を
化合する毎にホットゾーン(ヒーター、断熱材などの炉
材)や圧力容器のクリーニング作業を行わなければなら
ない。従って、製造効率を下げるという問題がある。
On the other hand, when the synthesis container is a semi-shield container, it can be used repeatedly and does not require a process such as vacuum sealing. However, there is a problem that the vapor of the group V element to be controlled leaks from the synthesis vessel to the pressure vessel. The amount of leakage depends on the structure of the semi-shielded container and the manner of applying the external pressure (inert gas pressure in the pressure container). The leaked steam adheres to a low-temperature portion in the pressure vessel and solidifies. In the synthesis of GaP or InP compounds, white phosphorus or red phosphorus, which easily ignites, adheres, and in the synthesis of GaAs, toxic As adheres. Due to these deposits, the hot zone (furnace material such as a heater and a heat insulating material) and the cleaning operation of the pressure vessel must be performed each time the compound is compounded. Therefore, there is a problem that manufacturing efficiency is reduced.

【0014】本発明の目的は、繰り返し使用可能で、真
空封止などのプロセスを必要とせず、かつV族元素の蒸
気が合成容器から圧力容器へと漏れ出さない合成容器を
提供し、低ランニングコストの化合物の合成装置および
方法を実現することである。
An object of the present invention is to provide a synthesis vessel which can be used repeatedly, does not require a process such as vacuum sealing, and does not leak vapor of a group V element from a synthesis vessel to a pressure vessel. It is to realize an apparatus and method for synthesizing a compound at low cost.

【0015】[0015]

【課題を解決するための手段】本発明による化合物の合
成装置は、化合物を構成する成分元素の内の解離圧の高
い成分元素の蒸気で蒸気圧を制御しつつ、該化合物の高
解離圧の成分元素を収容可能な蒸気圧制御用リザーバ
と、該化合物の他の成分元素を収容可能なルツボと、該
蒸気圧制御用リザーバと該ルツボとを収め蒸気を満たす
空間を有する合成容器と、該合成容器の外部から該ルツ
ボ底部を加熱するヒーターと、該合成容器の外部から該
ルツボ上部を加熱するヒーターと、該合成容器の外部か
ら該蒸気圧制御用リザーバを加熱するヒーターと、該合
成容器と前記3種のヒーターを内部に収める圧力容器と
を有し、合成容器内の空間と圧力容器の内部とを連通す
るために通気口を合成容器に設け、かつ合成容器内の空
間を密閉するために圧力容器の外部から開閉可能なシー
ル材を前記通気口に設ける。
The apparatus for synthesizing a compound according to the present invention controls the vapor pressure with the vapor of a component element having a high dissociation pressure among the component elements constituting the compound, and at the same time controls the vapor pressure of the compound at a high dissociation pressure. A vapor pressure control reservoir capable of accommodating the component elements, a crucible capable of accommodating other component elements of the compound, a synthesis vessel having a space for accommodating the vapor pressure control reservoir and the crucible and filling the vapor, A heater for heating the crucible bottom from outside the synthesis vessel, a heater for heating the crucible top from outside the synthesis vessel, a heater for heating the vapor pressure control reservoir from outside the synthesis vessel, and the synthesis vessel And a pressure vessel for accommodating the three types of heaters therein. A ventilation port is provided in the synthesis vessel to communicate the space in the synthesis vessel with the inside of the pressure vessel, and the space in the synthesis vessel is sealed. for The openable sealing member from external forces container provided to the vent.

【0016】好ましくは、前記合成容器を熱分解炭素、
ガラス状炭素、炭化珪素よりなる群から選択した1種ま
たは2種以上の材料を被覆したグラファイトで形成す
る。また、前記通気口が合成容器内側で小さい内径を有
し外側で大きい内径を有する構造とする。さらに、シー
ル材が開閉棒からなり、合成容器外側で通気口の内壁部
と同材質の被覆を施した前記開閉棒が滑動することで通
気口を開閉させる。前記開閉棒に連なる押し棒を設け、
該押し棒が前記圧力容器に取り付けたシャフト内で滑動
可能で、該押し棒を駆動する機構を備える。
Preferably, the synthesis vessel is made of pyrolytic carbon,
It is formed of graphite coated with one or more materials selected from the group consisting of glassy carbon and silicon carbide. Further, the vent has a structure having a small inside diameter inside the synthesis container and a large inside diameter outside. Further, the sealing member is made of an opening / closing rod, and the opening / closing rod, which is coated with the same material as the inner wall portion of the ventilation hole, slides on the outside of the synthetic container to open and close the ventilation hole. Providing a push rod connected to the opening and closing rod,
The push rod is slidable within a shaft attached to the pressure vessel and includes a mechanism for driving the push rod.

【0017】以上の構造を有する合成装置を用いて、昇
温、化合物の合成、および冷却の工程は、合成容器と圧
力容器との連通を遮断し、それ以外の工程では合成容器
と圧力容器とを連通する操作を該圧力容器の外部から行
い化合物を合成する。
Using the synthesis apparatus having the above structure, the steps of raising the temperature, synthesizing the compound, and cooling shut off the communication between the synthesis vessel and the pressure vessel. Is conducted from the outside of the pressure vessel to synthesize a compound.

【0018】[0018]

【発明の実施の形態】上記目的を達成するため種々の検
討を行った結果、到達した本発明の装置構成を図1から
図4に基づき説明する。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS As a result of various studies to achieve the above object, the structure of the apparatus of the present invention which has been reached will be described with reference to FIGS.

【0019】本発明の化合物の合成装置の特徴は、蒸気
を満たす空間を構成する合成容器5に圧力容器6外から
開閉可能な通気口7を設けたことである。通気口7は合
成容器5の内側で小さい内径を有し、外側で大きい内径
を有する構造であり、合成容器5の外側で、開閉棒8が
滑動することで通気口7が開閉される。合成容器ベース
13の外側から突合して、通気口7を塞ぐ開閉棒8が設
けられている。すなわち、図2(b)のように、開閉棒
8を通気口7に突き合わせることで、通気口7が閉じ
て、図2(a)のように開閉棒8を通気口7から離すこ
とで通気口7が開く。
A feature of the compound synthesizing apparatus of the present invention resides in that a vent 7 which can be opened and closed from the outside of the pressure vessel 6 is provided in the synthesis vessel 5 constituting a space filled with steam. The vent 7 has a small inside diameter inside the synthetic container 5 and a large inside diameter outside the synthetic container 5. The opening and closing rod 8 slides outside the synthetic container 5 to open and close the vent 7. An opening / closing rod 8 that abuts from the outside of the synthesis container base 13 to close the ventilation port 7 is provided. That is, as shown in FIG. 2 (b), the opening / closing rod 8 is closed by bringing the opening / closing rod 8 into contact with the ventilation port 7, and the opening / closing rod 8 is separated from the ventilation port 7 as shown in FIG. 2 (a). The vent 7 opens.

【0020】合成容器5と開閉棒8はグラファイト製で
あるが、熱分解炭素、ガラス状炭素、炭化珪素よりなる
群から選択した1種または2種以上の材料を被覆し、通
気性がない。なお、通気口7と開閉棒8とは同材質の被
覆が施され、被覆膜の反応が起きず繰り返し使用可能な
ものである。また、合成容器5の接合部はねじ締めによ
る封止構造とし、ねじを締めることにより、シール材
(グラフォイル、カーボンシート)を圧壊し、気密性を
確保する。なお、このねじ締めによる封止部分は、III
族元素原料1とV族元素原料3とを装填した後は、合成
多結晶を取り出すまで閉じたままである。
The synthesis vessel 5 and the opening and closing rod 8 are made of graphite, but are coated with one or more materials selected from the group consisting of pyrolytic carbon, glassy carbon, and silicon carbide, and have no air permeability. The ventilation port 7 and the opening / closing rod 8 are coated with the same material, and can be used repeatedly without reaction of the coating film. In addition, the joint portion of the synthesis container 5 has a sealing structure by screw tightening, and by tightening the screw, the sealing material (Grafoil, carbon sheet) is crushed and airtightness is secured. In addition, the sealing part by this screw tightening is III
After loading the group 1 element raw material 1 and the group V element raw material 3, it remains closed until the synthetic polycrystal is taken out.

【0021】開閉棒8には連なる押し棒9を設け、押し
棒9にはO−リング10が取り付けられて、圧力容器6
は気密性を保つ。この押し棒9を駆動することにより開
閉棒8が滑動し通気口7を開閉する。押し棒9の駆動機
構としては、図3に示したように、押しねじ11を回す
ことにより開閉方向に駆動する。また、押し棒9の圧力
容器6の外側に出た部分をモーター駆動する機構(図示
せず。)でもよい。
The open / close rod 8 is provided with a continuous push rod 9, and the push rod 9 is provided with an O-ring 10.
Keeps hermetic. By driving the push rod 9, the open / close rod 8 slides to open and close the vent 7. As shown in FIG. 3, the drive mechanism of the push rod 9 is driven in the opening and closing direction by turning the push screw 11. Further, a mechanism (not shown) for driving the portion of the push rod 9 outside the pressure vessel 6 by a motor may be used.

【0022】押し棒9を内装するのは、圧力容器6のい
ずれの場所であっても基本的には変わらないが、ホット
ゾーン(ヒーター、断熱材などの炉材)の構成や強度な
どから、合成容器ベース13の底部か合成容器5の上部
が望ましい。さらに、圧力容器6内に突き出たシャフト
12内に押し棒9を内装し、シャフト12に合成容器5
と合成容器ベース13を固定することで、開閉棒8を駆
動する際に通気口7の開閉を容易にするので好ましい。
もちろん、開閉棒8の駆動に際し、合成容器5と合成容
器ベース13を固定するシャフト12を設けず、別途合
成容器5と合成容器ベース13を圧力容器6に対して固
定する構造を設けたものでもよい。
Although the push rod 9 is basically provided in any place of the pressure vessel 6, the push rod 9 is not changed. However, due to the structure and strength of the hot zone (furnace material such as a heater and a heat insulating material), The bottom of the synthesis vessel base 13 or the top of the synthesis vessel 5 is desirable. Further, a push rod 9 is provided inside a shaft 12 protruding into the pressure vessel 6, and the shaft 12 is
It is preferable to fix the synthesis container base 13 because the opening and closing of the vent 7 is facilitated when the opening and closing rod 8 is driven.
Of course, when the opening / closing rod 8 is driven, the shaft 12 for fixing the synthesis container 5 and the synthesis container base 13 is not provided, and a structure for separately fixing the synthesis container 5 and the synthesis container base 13 to the pressure container 6 may be provided. Good.

【0023】圧力容器6内で合成容器5と合成容器ベー
ス13を移動しながら合成を行う方法では、押し棒9を
内装し合成容器ベース13を固定するシャフト12を駆
動することで可能となる。
In the method of performing the synthesis while moving the synthesis vessel 5 and the synthesis vessel base 13 in the pressure vessel 6, it is possible to drive the shaft 12 in which the push rod 9 is provided and the synthesis vessel base 13 is fixed.

【0024】III 族元素原料1を装填したルツボ2とV
族元素原料3を装填した蒸気圧制御用リザーバ4が収め
られた合成容器5と合成容器ベース13を圧力容器6内
に取り付け、圧力容器6内を真空排気する際に通気口7
を開けておき、合成容器5と合成容器ベース13の内部
も同時に真空排気する。真空排気終了後に、開閉棒9を
駆動して通気口7を閉め、合成容器5と合成容器ベース
13を密閉する。この後の昇温では、合成容器5と合成
容器ベース13の内部のV族元素原料3の蒸気圧に等し
い圧力となるように、不活性ガスを圧力容器6内に供給
する。昇温、化合物合成、冷却過程を通じて、合成容器
5と合成容器ベース13は密閉であり、内外に圧力差が
無いため、V族元素の蒸気は合成容器5と合成容器ベー
ス13から漏れ出てこない。V族元素原料3の蒸気圧が
十分に小さくなってから、あるいは冷却が終了した後
に、通気口7を開け、合成容器5と合成容器ベース13
の内圧と圧力容器6の内圧とを大気圧に戻し、合成容器
5と合成容器ベース13から化合物を取り出す。真空封
止を必要としない合成容器5と合成容器ベース13は、
繰り返し使用が可能である。
Crucible 2 loaded with Group III element material 1 and V
The synthesis vessel 5 containing the vapor pressure control reservoir 4 loaded with the group 3 element raw material 3 and the synthesis vessel base 13 are mounted in the pressure vessel 6.
Is opened, and the insides of the synthesis vessel 5 and the synthesis vessel base 13 are simultaneously evacuated. After the evacuation is completed, the opening / closing rod 9 is driven to close the ventilation port 7, and the synthesis container 5 and the synthesis container base 13 are hermetically closed. In the subsequent temperature increase, an inert gas is supplied into the pressure vessel 6 so that the pressure becomes equal to the vapor pressure of the group V element raw material 3 inside the synthesis vessel 5 and the synthesis vessel base 13. During the process of raising the temperature, synthesizing the compound, and cooling, the synthesis vessel 5 and the synthesis vessel base 13 are hermetically closed, and there is no pressure difference between the inside and outside, so that the vapor of the group V element does not leak out of the synthesis vessel 5 and the synthesis vessel base 13. . After the vapor pressure of the group V element raw material 3 becomes sufficiently low or after cooling is completed, the vent 7 is opened, and the synthesis vessel 5 and the synthesis vessel base 13 are opened.
And the internal pressure of the pressure vessel 6 are returned to the atmospheric pressure, and the compound is taken out of the synthesis vessel 5 and the synthesis vessel base 13. The synthesis container 5 and the synthesis container base 13 that do not require vacuum sealing are:
It can be used repeatedly.

【0025】[0025]

【実施例】以下にGaPの合成に使用する合成装置と方
法を、図1から図4に基づいて説明すると以下の通りで
ある。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A synthesizing apparatus and method used for synthesizing GaP will be described below with reference to FIGS.

【0026】圧力容器6の底部中心に設けられたシャフ
ト12に合成容器ベース13を取り付け、この上に35
0gの赤燐を入れた蒸気圧制御用リザーバ4を載せ、そ
の上方に700gのGa原料を装填した内径95mmの
PBNルツボ2を配置し、合成容器5を被せた。合成容
器5と合成容器ベース13はグラファイトに熱分解炭素
を被覆して用いた。合成容器ベース13の中心部は蒸気
圧制御用リザーバ4内の温度をモニタするための熱電対
14を配置し、その隣に通気口7が設けられた。通気口
7は合成容器ベース13の内側で内径が1mm、外側で
内径が6mmとした。開閉棒8は、合成容器ベース13
内に収められ、シャフト12に内装された押し棒9と一
直線上に配置される。押し棒9はO−リング10でシー
ルされ、押し棒9を駆動する押しねじ11は、シャフト
12の下部のフランジ19に取り付けられる。
The synthetic vessel base 13 is attached to the shaft 12 provided at the center of the bottom of the pressure vessel 6, and 35
A vapor pressure control reservoir 4 containing 0 g of red phosphorus was placed thereon, and a PBN crucible 2 having an inner diameter of 95 mm loaded with 700 g of Ga raw material was placed above the reservoir 4, and the synthesis vessel 5 was covered. The synthesis vessel 5 and the synthesis vessel base 13 were used by coating graphite with pyrolytic carbon. A thermocouple 14 for monitoring the temperature in the vapor pressure control reservoir 4 was arranged at the center of the synthesis vessel base 13, and the vent 7 was provided next to the thermocouple 14. The inside diameter of the vent 7 was 1 mm inside the synthetic container base 13 and 6 mm inside the outside. The opening / closing rod 8 is a synthetic container base 13.
It is housed inside and is arranged in line with the push rod 9 provided inside the shaft 12. The push rod 9 is sealed with an O-ring 10, and a set screw 11 for driving the push rod 9 is attached to a lower flange 19 of the shaft 12.

【0027】合成容器5と合成容器ベース13を加熱す
るヒーター15はグラファイト製で、円筒型で同径のも
のを同軸上に3段重ねた。上の2つのヒーター15をル
ツボ加熱用に、下の1つのヒーターを蒸気圧制御用リザ
ーバの加熱用とし、その間と外周および合成容器5の上
部と、合成容器ベース13の下部とは断熱材で構成し
た。
The heater 15 for heating the synthesis vessel 5 and the synthesis vessel base 13 is made of graphite, and three cylindrical cylinders having the same diameter are stacked coaxially. The upper two heaters 15 are used for crucible heating, and the lower one heater is used for heating the vapor pressure control reservoir, and the space between the heater, the outer periphery, the upper part of the synthesis vessel 5 and the lower part of the synthesis vessel base 13 are made of heat insulating material. Configured.

【0028】合成容器5と合成容器ベース13とホット
ゾーンとをセットした後、圧力容器6を閉め真空排気を
開始した。この時、通気口7は開けておき、合成容器5
と合成容器ベース13の内部も真空排気した。約2時間
真空排気した後、合成容器5と合成容器ベース13を加
熱して、昇温を開始した。蒸気圧制御用リザーバ4内の
温度が300℃となった時点で、押しねじ11を回して
押し棒9を上げて開閉棒8で通気口7を閉め、合成容器
5と合成容器ベース13を密閉容器とした。真空排気を
止め、Arガスを圧力容器6内に供給した。以後は、蒸
気圧制御用の赤燐3の温度を蒸気圧制御用リザーバ4内
に配置した熱電対14で測定し、この温度から赤燐3の
蒸気圧(合成容器5と合成容器ベース13の内圧)を求
め、これに圧力容器6の内圧(合成容器5と合成容器ベ
ース13の外圧)が等しくなるようにArガスを供給し
ていった。
After setting the synthesis vessel 5, the synthesis vessel base 13, and the hot zone, the pressure vessel 6 was closed and the evacuation was started. At this time, the ventilation port 7 is opened, and the synthetic container 5 is opened.
The inside of the synthesis container base 13 was also evacuated. After evacuating for about 2 hours, the synthesis vessel 5 and the synthesis vessel base 13 were heated to start raising the temperature. When the temperature in the vapor pressure control reservoir 4 reaches 300 ° C., turn the push screw 11 to raise the push rod 9, close the vent 7 with the open / close rod 8, and seal the synthesis container 5 and the synthesis container base 13. It was a container. The evacuation was stopped, and Ar gas was supplied into the pressure vessel 6. Thereafter, the temperature of the red phosphorus 3 for controlling the vapor pressure is measured by a thermocouple 14 disposed in the reservoir 4 for controlling the vapor pressure, and the vapor pressure of the red phosphorus 3 (from the synthesis vessel 5 and the base 13 of the synthesis vessel 13) is measured based on this temperature. The internal pressure) was obtained, and Ar gas was supplied thereto so that the internal pressure of the pressure vessel 6 (the external pressure of the synthesis vessel 5 and the synthesis vessel base 13) became equal.

【0029】昇温開始から約4時間後、蒸気圧制御用リ
ザーバ4側のヒーター15の制御温度を595℃として
保持した。この時の蒸気圧制御用リザーバ4内の温度は
578℃であり、合成容器5と合成容器ベース13の内
部の燐の蒸気圧は35kg/cm2 、圧力容器6内のA
rガス圧(合成容器5と合成容器ベース13の外圧)も
35kg/cm2 である。この約20分間後、ルツボ2
側の2つのヒーター15の制御温度を上からそれぞれ1
520℃、1450℃として昇温を終了した。この状態
は別途行った温度分布を測定した結果から、ルツボ2の
底部の温度がGaPの融点の1465℃となり、上が高
く、下が低い温度分布となり、ルツボ2の上部の温度は
1485℃である。この状態を約20分間保持した後、
上部2つのヒーター15の制御温度を25℃/hで1時
間下げ、化合物の合成を行った。この間、蒸気圧制御用
リザーバ4内の温度を578℃(合成容器5と合成容器
ベース13の内部の燐の蒸気圧は35kg/cm2 )に
保持した。
About four hours after the start of the temperature rise, the control temperature of the heater 15 on the vapor pressure control reservoir 4 side was maintained at 595 ° C. At this time, the temperature in the vapor pressure control reservoir 4 is 578 ° C., the vapor pressure of phosphorus inside the synthesis vessel 5 and the synthesis vessel base 13 is 35 kg / cm 2 , and A in the pressure vessel 6
The r gas pressure (external pressure of the synthesis vessel 5 and the synthesis vessel base 13) is also 35 kg / cm 2 . After about 20 minutes, crucible 2
The control temperature of the two heaters 15 on the
The heating was completed at 520 ° C. and 1450 ° C. In this state, the temperature at the bottom of the crucible 2 was 1465 ° C., which is the melting point of GaP, the temperature at the top was low, and the temperature at the bottom was low, and the temperature at the top of the crucible 2 was 1485 ° C. is there. After holding this state for about 20 minutes,
The control temperature of the upper two heaters 15 was lowered at 25 ° C./h for 1 hour to synthesize a compound. During this time, the temperature in the vapor pressure control reservoir 4 was maintained at 578 ° C. (the vapor pressure of phosphorus in the synthesis vessel 5 and the synthesis vessel base 13 was 35 kg / cm 2 ).

【0030】その後、約2時間で、上部2つのヒーター
15の制御温度を800℃まで、蒸気圧制御用リザーバ
4側のヒーター15の制御温度を440℃まで下げて、
全体を冷却した。この間は昇温時と同様に、圧力容器6
の内圧(合成容器5と合成容器ベース13の外圧)が合
成容器5と合成容器ベース13の内圧の燐の蒸気圧に等
しくなるように圧力容器6内のArガスを排気した。圧
力容器6の内圧が2kg/cm2 となった時点で、Ar
ガスの排気を止め、さらに室温まで、約3時間で冷却し
た。
Thereafter, in about two hours, the control temperature of the upper two heaters 15 was lowered to 800 ° C. and the control temperature of the heater 15 on the vapor pressure control reservoir 4 side was lowered to 440 ° C.
The whole was cooled. During this time, the pressure vessel 6
The Ar gas in the pressure vessel 6 was evacuated so that the internal pressure (the external pressure of the synthesis vessel 5 and the synthesis vessel base 13) became equal to the vapor pressure of phosphorus as the internal pressure of the synthesis vessel 5 and the synthesis vessel base 13. When the internal pressure of the pressure vessel 6 becomes 2 kg / cm 2 , Ar
The evacuation of the gas was stopped, and the system was further cooled to room temperature in about 3 hours.

【0031】冷却終了後、通気口7を開け、合成容器5
と合成容器ベース13の内圧と、圧力容器6の内圧とを
大気圧に戻し、圧力容器6から合成容器5と合成容器ベ
ース13を取り出し、化合物を得た。
After the cooling, the vent 7 is opened, and the synthesis vessel 5
Then, the internal pressure of the synthesis vessel base 13 and the internal pressure of the pressure vessel 6 were returned to the atmospheric pressure, and the synthesis vessel 5 and the synthesis vessel base 13 were taken out of the pressure vessel 6 to obtain a compound.

【0032】直径95mm、長さ34mmで質量が1k
gのGaP化合物が得られた。合成容器5と合成容器ベ
ース13の内部には、燐が付着していたが、圧力容器6
内には燐が漏れ出していなかった。合成容器5と合成容
器ベース13は、付着した燐を取り除くだけで繰り返し
使用でき、圧力容器6はそのまま次の化合物の製造に使
用することができた。
The diameter is 95 mm, the length is 34 mm and the mass is 1 k.
g of GaP compound were obtained. Phosphorous adhered to the interior of the synthesis vessel 5 and the synthesis vessel base 13, but the pressure vessel 6
No phosphorus had leaked inside. The synthesis vessel 5 and the synthesis vessel base 13 could be used repeatedly only by removing the attached phosphorus, and the pressure vessel 6 could be used as it was for the production of the next compound.

【0033】[0033]

【発明の効果】本発明により、合成容器を繰り返し使用
でき、かつ真空封止などのプロセスを必要とせず、化合
物の成分であるV族元素の蒸気が合成容器から漏れ出さ
ないため、ホットゾーン(ヒーター、断熱材などの炉
材)や圧力容器のクリーニング作業を毎回必要としない
化合物の合成装置および方法が実現でき、低ランニング
コストで化合物を製造することができるようになった。
According to the present invention, the synthesis vessel can be used repeatedly, a process such as vacuum sealing is not required, and the vapor of the group V element which is a component of the compound does not leak out of the synthesis vessel. A compound synthesizing apparatus and method can be realized which do not require a cleaning operation of a furnace material such as a heater and a heat insulating material) and a pressure vessel each time, and the compound can be manufactured at low running cost.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の合成容器の構成断面図である。FIG. 1 is a sectional view showing the configuration of a synthesis container according to the present invention.

【図2】図1の通気口の拡大図である。FIG. 2 is an enlarged view of a vent of FIG.

【図3】図1の押しねじ部の拡大図である。FIG. 3 is an enlarged view of a push screw portion of FIG. 1;

【図4】化合物の合成装置全体の構成断面図である。FIG. 4 is a cross-sectional view of the overall configuration of a compound synthesizing apparatus.

【図5】従来の技術における合成容器の構成断面図であ
る。
FIG. 5 is a cross-sectional view of a configuration of a synthesis container according to a conventional technique.

【符号の説明】[Explanation of symbols]

1 III 族元素原料 2 ルツボ 3 V族元素原料 4 蒸気圧制御用リザーバ 5 合成容器 6 圧力容器 7 通気口 8 開閉棒 9 押し棒 10 O−リング 11 押しねじ 12 シャフト 13 合成容器ベース 14 熱電対 15 ヒーター 16 断熱材 18 不活性ガス供給口 19 フランジ DESCRIPTION OF SYMBOLS 1 Group III element raw material 2 Crucible 3 Group V element raw material 4 Reservoir for vapor pressure control 5 Synthetic container 6 Pressure container 7 Vent 8 Opening / closing rod 9 Push rod 10 O-ring 11 Push screw 12 Shaft 13 Synthetic container base 14 Thermocouple 15 Heater 16 Insulation material 18 Inert gas supply port 19 Flange

Claims (10)

【特許請求の範囲】[Claims] 【請求項1】 複数の成分元素の反応により化合物を生
成する第1空間を有する合成容器と、該合成容器を包
囲、収容する圧力容器と、反応時における該合成容器の
中の圧力に見合う圧力を、該圧力容器内に生じさせる機
構とを有する化合物の合成装置。
1. A synthesis vessel having a first space for producing a compound by the reaction of a plurality of component elements, a pressure vessel surrounding and containing the synthesis vessel, and a pressure corresponding to the pressure in the synthesis vessel during the reaction. For producing a compound in the pressure vessel.
【請求項2】 化合物を反応により生成する成分元素を
配置する複数の収納部と、該収納部に前記成分元素を入
れる機構と、前記収納部を加熱する加熱装置と、前記反
応を生じさせる反応空間とを有する密封型合成容器、お
よび該合成容器を収容する包囲空間を有する圧力容器か
らなる化合物の合成装置において、前記合成容器の反応
空間と圧力容器の包囲空間とに連通する通気口と、該通
気口の開閉部材を合成容器に設け、該開閉部材の作動を
外部から行うための開閉装置が、圧力容器に設けられて
いることを特徴とする化合物の合成装置。
2. A plurality of storage sections for disposing component elements for producing a compound by a reaction, a mechanism for putting the component elements into the storage sections, a heating device for heating the storage section, and a reaction for causing the reaction. A sealed synthetic container having a space, and a compound synthesizing apparatus comprising a pressure vessel having an enclosed space for accommodating the synthetic container, wherein a vent communicating with the reaction space of the synthetic container and the enclosed space of the pressure vessel, An apparatus for synthesizing a compound, wherein an opening / closing member for the vent is provided in a synthesis container, and an opening / closing device for externally operating the opening / closing member is provided in the pressure vessel.
【請求項3】 化合物の合成装置において、該化合物の
高解離圧の成分元素を収容可能な蒸気圧制御用リザーバ
と、該化合物の他の成分元素を収容可能なルツボと、該
蒸気圧制御用リザーバと該ルツボとを収め蒸気を満たす
空間を有する合成容器と、該合成容器を内部に収める圧
力容器とを有し、合成容器内の空間と圧力容器の内部と
を連通するために通気口を合成容器に設け、かつ合成容
器内の空間を密閉するために圧力容器の外部から開閉可
能なシール材を前記通気口に設けたことを特徴とする化
合物の合成装置。
3. A compound synthesizing apparatus, comprising: a vapor pressure control reservoir capable of accommodating a component element having a high dissociation pressure of the compound; a crucible accommodating another component element of the compound; A synthesis container having a space for storing the reservoir and the crucible and filling with steam, and a pressure container for housing the synthesis container therein, wherein a vent is provided for communicating the space in the synthesis container with the inside of the pressure container. An apparatus for synthesizing a compound, wherein a sealing member provided in the synthesis vessel and capable of being opened and closed from the outside of the pressure vessel to seal a space inside the synthesis vessel is provided in the vent.
【請求項4】 前記ルツボと前記蒸気圧制御用リザーバ
とを加熱するヒーターを有する構造であることを特徴と
する請求項3に記載の化合物の合成装置。
4. The compound synthesizing apparatus according to claim 3, wherein the apparatus has a heater for heating the crucible and the vapor pressure control reservoir.
【請求項5】 前記合成容器が熱分解炭素、ガラス状炭
素、炭化珪素よりなる群から選択した1種または2種以
上の材料を被覆したグラファイトで形成されることを特
徴とする請求項3と4のいずれかに記載の化合物の合成
装置。
5. The method according to claim 3, wherein the synthesis vessel is made of graphite coated with one or more materials selected from the group consisting of pyrolytic carbon, glassy carbon, and silicon carbide. 5. An apparatus for synthesizing the compound according to any one of 4.
【請求項6】 前記通気口が合成容器内側で小さい内径
を有し外側で大きい内径を有する構造であることを特徴
とする請求項3から5のいずれかに記載の化合物の合成
装置。
6. The compound synthesizing apparatus according to claim 3, wherein the vent has a structure having a small inside diameter inside the synthesis vessel and a large inside diameter outside.
【請求項7】 前記シール材が開閉棒からなり、前記通
気口の内壁部と同材質の被覆を施した該開閉棒が、合成
容器外側で滑動することで通気口が開閉することを特徴
とする請求項3から6のいずれかに記載の化合物の合成
装置。
7. The opening and closing rod is characterized in that the sealing member is made of an opening and closing rod, and the opening and closing rod coated with the same material as the inner wall portion of the ventilation opening slides outside the synthesis container to open and close the ventilation opening. An apparatus for synthesizing the compound according to claim 3.
【請求項8】 前記開閉棒に連なる押し棒を設け、該押
し棒が前記圧力容器に取り付けたシャフト内で滑動可能
で、該押し棒を駆動する機構があることを特徴とする請
求項3から7のいずれかに記載の化合物の合成装置。
8. A push rod connected to the open / close rod is provided, and the push rod is slidable in a shaft attached to the pressure vessel, and a mechanism for driving the push rod is provided. 8. An apparatus for synthesizing the compound according to any one of the above items 7.
【請求項9】 次の各工程からなる化合物の合成方法。 (1)高解離圧の成分元素を蒸気圧制御用リザーバに収
容し、他の成分元素をルツボに収容し、該ルツボと該蒸
気圧制御用リザーバとを合成容器に収納し、該合成容器
を圧力容器に収納し、前記通気口を開け、合成容器と圧
力容器の内部を同時に真空排気してから、前記通気口を
閉じる第1工程。 (2)合成容器の内部の前記高解離圧の成分元素の蒸気
圧と等しい気圧で、圧力容器の内部に不活性ガスを供給
しつつ、該合成容器の外部から該ルツボ底部を加熱する
ヒーターと、該合成容器の外部から該ルツボ上部を加熱
するヒーターと、該合成容器の外部から該蒸気圧制御用
リザーバを加熱するヒーターとで、合成容器を加熱し、
ルツボの底部を化合物の融点に温度制御し、ルツボ上部
は該融点よりも高い温度に制御し、ルツボ内の成分元素
の該融点における解離圧と、蒸気圧制御用リザーバ内の
前記高解離圧成分元素の蒸気圧が等しくなるように、蒸
気圧制御用リザーバの温度を制御する第2工程。 (3)合成容器の内部の前記高解離圧の成分元素の蒸気
圧と等しい気圧で、圧力容器の内部に不活性ガスを供給
しつつ、前記ルツボの底部の温度とルツボ上部の温度を
徐々に降温し、蒸気圧制御用リザーバ内の成分元素の温
度は第2工程の温度を維持する制御を行う第3工程。 (4)合成装置全体を室温にまで冷却し、化合物を取り
出す第4工程。
9. A method for synthesizing a compound comprising the following steps: (1) A component element having a high dissociation pressure is contained in a vapor pressure control reservoir, another component element is contained in a crucible, and the crucible and the vapor pressure control reservoir are contained in a synthesis vessel. A first step of storing in a pressure vessel, opening the vent, evacuating the interior of the synthesis vessel and the pressure vessel simultaneously, and then closing the vent. (2) a heater for heating the bottom of the crucible from outside the synthesis vessel while supplying an inert gas to the interior of the pressure vessel at a pressure equal to the vapor pressure of the high dissociation pressure component element inside the synthesis vessel; Heating the synthesis vessel with a heater that heats the crucible top from outside the synthesis vessel and a heater that heats the vapor pressure control reservoir from outside the synthesis vessel;
The bottom of the crucible is temperature controlled to the melting point of the compound, the top of the crucible is controlled to a temperature higher than the melting point, the dissociation pressure of the component elements in the crucible at the melting point, and the high dissociation pressure component in the vapor pressure control reservoir. A second step of controlling the temperature of the vapor pressure control reservoir so that the vapor pressures of the elements are equal. (3) The temperature at the bottom of the crucible and the temperature at the top of the crucible are gradually increased while supplying an inert gas into the pressure vessel at a pressure equal to the vapor pressure of the high dissociation pressure component element inside the synthesis vessel. The third step of lowering the temperature and controlling the temperature of the component elements in the vapor pressure control reservoir to maintain the temperature of the second step. (4) The fourth step of cooling the whole synthesis apparatus to room temperature and taking out the compound.
【請求項10】 化合物を構成する成分元素の内の解離
圧の高い成分元素の蒸気で蒸気圧制御を行いつつ、その
他の成分元素を該化合物の融点に加熱し、該融点から徐
々に冷却して前記解離圧の高い成分元素の蒸気を移動さ
せる化合物の合成方法において、該蒸気の蒸気圧を制御
する密閉空間の周囲に圧力空間を設け、該密閉空間にお
ける少なくとも昇温、化合物の合成、冷却の工程は、該
密閉空間と圧力空間との連通を遮断し、それ以外の工程
では該密閉空間と圧力空間とを連通する操作を該圧力空
間の外部からから行うようにしたことを特徴とする化合
物の合成方法。
10. While controlling the vapor pressure with the vapor of the component element having a high dissociation pressure among the component elements constituting the compound, the other component elements are heated to the melting point of the compound, and gradually cooled from the melting point. In the method for synthesizing a compound for transferring a vapor of a component element having a high dissociation pressure, a pressure space is provided around an enclosed space for controlling the vapor pressure of the vapor, and at least the temperature in the enclosed space is increased, and the compound is synthesized and cooled. The step is characterized in that the communication between the closed space and the pressure space is cut off, and in the other steps, the operation of connecting the closed space and the pressure space is performed from outside the pressure space. A method for synthesizing a compound.
JP2818297A 1997-02-12 1997-02-12 Device for synthesizing compound and method therefor Pending JPH10226596A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2818297A JPH10226596A (en) 1997-02-12 1997-02-12 Device for synthesizing compound and method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2818297A JPH10226596A (en) 1997-02-12 1997-02-12 Device for synthesizing compound and method therefor

Publications (1)

Publication Number Publication Date
JPH10226596A true JPH10226596A (en) 1998-08-25

Family

ID=12241580

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2818297A Pending JPH10226596A (en) 1997-02-12 1997-02-12 Device for synthesizing compound and method therefor

Country Status (1)

Country Link
JP (1) JPH10226596A (en)

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