JPH03257092A - Apparatus for producing high dissociation pressure single crystal - Google Patents

Apparatus for producing high dissociation pressure single crystal

Info

Publication number
JPH03257092A
JPH03257092A JP5163990A JP5163990A JPH03257092A JP H03257092 A JPH03257092 A JP H03257092A JP 5163990 A JP5163990 A JP 5163990A JP 5163990 A JP5163990 A JP 5163990A JP H03257092 A JPH03257092 A JP H03257092A
Authority
JP
Japan
Prior art keywords
single crystal
shaft
shafts
dissociation pressure
high dissociation
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
Application number
JP5163990A
Other languages
Japanese (ja)
Other versions
JP2830315B2 (en
Inventor
Tomohiro Kawase
智博 川瀬
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 Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries 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 Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to JP5163990A priority Critical patent/JP2830315B2/en
Publication of JPH03257092A publication Critical patent/JPH03257092A/en
Application granted granted Critical
Publication of JP2830315B2 publication Critical patent/JP2830315B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Crystals, And After-Treatments Of Crystals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)

Abstract

PURPOSE:To smooth the revolving and lifting of upper and lower shafts and to produce the high quality single crystal of a small defect density by constituting the sealing part where the upper shaft for pulling up the single crystal or the lower shaft for supporting a crucible penetrates a hermetic vessel of a material softer than the material of the shafts. CONSTITUTION:Only central aperture parts 23, 24 of receiving trays 11, 12 sliding with the upper shaft 2 and lower shaft 3 of the apparatus for producing the high-dissiciation pressure single crystal are constituted of the relatively soft material. The material quality of the receiving trays 11, 12 are of not a particular problem and the same hard material as the material of the shafts is usable. The exchange of only the aperture parts 23, 24 is possible as well. The generation of flaws on the shaft surface is prevented in this way and the revolving and lifting of the shafts are smoothed. The disturbance in the temp. distribution of the raw material melt occurring in the oscillation of the shafts and the disturbance in the diameter control of the pulled up crystal, etc., are prevented, by which the seizure of the shafts and the sealing part is prevented.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、GaAs、 GaP5InAs、 InP等
のm−v族化合物半導体、並びに、CdTe、HgCd
Te、 Zn5e等の■−■族化合物半導体などの高解
離圧単結晶を、高解離圧成分元素ガスを封入した気密容
器中でチョクラルスキー法により製造する装置に関する
Detailed Description of the Invention (Industrial Application Field) The present invention is applicable to m-v group compound semiconductors such as GaAs, GaP5InAs, and InP, as well as CdTe, HgCd
The present invention relates to an apparatus for producing a high dissociation pressure single crystal of a ■-■ group compound semiconductor such as Te or Zn5e by the Czochralski method in an airtight container sealed with a high dissociation pressure component element gas.

(従来の技術) 高解離圧成分元素ガス雰囲気中で単結晶を育成する方法
は、従来のチョクラルスキー法やLEC法とは異なり、
成長した高解離圧単結晶表面で分解反応が生じて結晶の
品質を悪化することもなく、低い欠陥密度の高均一性を
有する単結晶を製造することができる。
(Prior art) The method for growing single crystals in a high dissociation pressure component gas atmosphere is different from the conventional Czochralski method or LEC method.
A single crystal with low defect density and high uniformity can be produced without deteriorating the quality of the crystal due to decomposition reactions occurring on the surface of the grown high dissociation pressure single crystal.

第2図は、高解離圧成分元素ガスを封入した気密容器中
で高解離圧単結晶をチョクラルスキー法で製造する従来
装置の断面図である。チャンバー1内には、高解離圧成
分元素ガスを密閉するための気密容器10が配置されて
おり、種結晶9を下端に取り付けて単結晶8を引き上げ
る上軸2、及び、サセプタ4で支持されたるつぼ5をそ
の上端で支持する下軸3は、チャンバー1及び気密容器
10を貫通し、該るつぼ5内には原料融液6と液体封止
剤7を収容し、気密容器1oの貫通部分に°液体封止剤
13並びに14を収容する受皿11並びに12を設け、
該受皿11並びに12の中央開口部は上軸2並びに下軸
3とそれぞれ摺動して、該軸を回転昇降可能として、か
つ、液体封止剤の流下を防止する構造を育している。気
密容器10の上方には、高解離圧成分元素17を収容す
るアンプル18を導管22を介して気密容器1oと接続
し、気密容器10内に所定の高解離圧成分元素ガス分圧
を確保するためのヒータ21をアンプル18の周囲に配
置し、上軸貫通部の液体封止剤13並びに下軸貫通部の
液体封止剤14を溶融させるためのヒータ19並びに2
0を配置し、るっぽ5の周囲にはヒータ15及び16を
配置する。
FIG. 2 is a sectional view of a conventional apparatus for producing a high dissociation pressure single crystal by the Czochralski method in an airtight container filled with a high dissociation pressure component gas. An airtight container 10 for sealing a high dissociation pressure component element gas is disposed in the chamber 1, and is supported by an upper shaft 2 and a susceptor 4 for pulling up a single crystal 8 with a seed crystal 9 attached to the lower end. The lower shaft 3 supporting the crucible 5 at its upper end passes through the chamber 1 and the airtight container 10, contains the raw material melt 6 and the liquid sealant 7 in the crucible 5, and the penetrating portion of the airtight container 1o. , provided with saucers 11 and 12 for accommodating liquid sealants 13 and 14;
The central openings of the saucers 11 and 12 slide on the upper shaft 2 and the lower shaft 3, respectively, to allow the shafts to rotate up and down and to prevent the liquid sealant from flowing down. Above the airtight container 10, an ampoule 18 containing the high dissociation pressure component element 17 is connected to the airtight container 1o via a conduit 22 to ensure a predetermined high dissociation pressure component gas partial pressure in the airtight container 10. Heaters 19 and 2 are arranged around the ampoule 18 to melt the liquid sealant 13 in the upper shaft penetration part and the liquid sealant 14 in the lower shaft penetration part.
0 is placed, and heaters 15 and 16 are placed around the Ruppo 5.

まず、原料、液体封止剤及び高解離圧成分元素を所定の
場所に挿入し、チャンバー1内を一旦真空に排気した後
、ヒータエ9及び20を加熱して液体封止剤13及び1
4を溶融し、気密容器10を密封し、次いで、ヒータ2
1を加熱して、単結晶8及び原料融液6の分解反応を抑
制するように、気密容器10内の高解離圧成分元素ガス
の分圧を調整し、同時に、これに見合う不活性ガスをチ
ャンバー1内に満たし、次いで、ヒータ15及び16を
加熱して原料融液6及び液体封止剤7の温度を調整し、
かつ、気密容器1oの壁面を加熱して高解離圧成分元素
の析出を防止することにより高解離圧成分元素ガスの分
圧を維持した状態で、上軸2を降下して種結晶9を原料
融液6に十分になじませて種付けし、直径を制御しなが
ら単結晶8を引き上げる。なお、気密容器10内に十分
高い高解離圧成分元素ガス分圧が得られる場合は、るつ
ぼ6内の液体封止剤7を省略してもよい。
First, the raw materials, liquid sealant, and high dissociation pressure component elements are inserted into predetermined locations, and the inside of the chamber 1 is once evacuated to vacuum, and then the heaters 9 and 20 are heated to
4 is melted, the airtight container 10 is sealed, and then the heater 2
1 to adjust the partial pressure of the high dissociation pressure component element gas in the airtight container 10 so as to suppress the decomposition reaction of the single crystal 8 and the raw material melt 6, and at the same time supply an inert gas corresponding to this. filling the chamber 1, then heating the heaters 15 and 16 to adjust the temperature of the raw material melt 6 and the liquid sealant 7,
In addition, while maintaining the partial pressure of the high dissociation pressure component gas by heating the wall surface of the airtight container 1o to prevent precipitation of the high dissociation pressure component element, the upper shaft 2 is lowered to feed the seed crystal 9 as a raw material. The single crystal 8 is thoroughly blended into the melt 6 and seeded, and the single crystal 8 is pulled up while controlling the diameter. Note that if a sufficiently high partial pressure of the high dissociation pressure component element gas is obtained in the airtight container 10, the liquid sealant 7 in the crucible 6 may be omitted.

従来、この種の装置では、気密容器1o、アンプル18
及び導管22は、石英、カーボン、pBN、SiC,気
密質のカーボン、カーボンにpBNをコーティングした
もの、カーボンに気密質カーボンをコーティングしたも
の、カーボンにSiCをコーティングしたもの、モリブ
デン、ステンレス等の材料で作られ、上下軸2,3及び
気密部分の受皿11゜12はモリブデン又はステンレス
で作られていた。
Conventionally, in this type of device, an airtight container 1o, an ampoule 18
The conduit 22 is made of materials such as quartz, carbon, pBN, SiC, airtight carbon, carbon coated with pBN, carbon coated with airtight carbon, carbon coated with SiC, molybdenum, stainless steel, etc. The upper and lower shafts 2, 3 and the airtight parts 11 and 12 were made of molybdenum or stainless steel.

(発明が解決しようとする課題) この種の装置では、上軸2及び下軸3が気密容器10を
貫通する気密部分が高温にさらされるため、ゴム製のO
リングを使用することができないので、軸及び受皿の材
料は、高温で強度を有し、耐腐食性の優れたモリブデン
又はステンレスを使用していた。これらの軸は回転及び
昇降を行うため、受皿の開口部とは非接触で一定の隙間
を設けることが望ましいが、液体封止剤の流下を防止す
るためには、この隙間は必要最小限にされている。
(Problem to be Solved by the Invention) In this type of device, the airtight portion where the upper shaft 2 and the lower shaft 3 penetrate the airtight container 10 is exposed to high temperature, so the rubber O
Since a ring cannot be used, molybdenum or stainless steel, which is strong at high temperatures and has excellent corrosion resistance, has been used for the shaft and saucer. Since these shafts rotate and move up and down, it is desirable to have a certain gap between them and the opening of the saucer, but in order to prevent the liquid sealant from flowing down, this gap should be kept to the minimum necessary. has been done.

しかし、軸と受皿の軸芯を一致させることが難しく、完
全な非接触を維持することは困難である。
However, it is difficult to align the axes of the shaft and the saucer, and it is difficult to maintain complete non-contact.

軸と受皿の接触は、軸の表面をキズ付けて軸の円滑な回
転を妨げることになり、その振動が原料融液の温度分布
を乱して双晶の発生や多結晶化をもたらしたり、単結晶
の直径制御を妨げたりする原因ともなり、さらには、両
者の焼き付けを起こして単結晶の引き上げを不可能にす
る場合もある。
Contact between the shaft and the saucer scratches the surface of the shaft and prevents it from rotating smoothly, and the vibrations disturb the temperature distribution of the raw material melt, resulting in the generation of twins and polycrystals. This may interfere with the diameter control of the single crystal, and furthermore, it may cause burning of both, making it impossible to pull the single crystal.

本発明は、上記の欠点を解消し、上下軸のキズの発生を
防止し、軸の回転と昇降を円滑に行うことができる高解
離圧単結晶の製造装置を提供しようとするものである。
The present invention aims to eliminate the above-mentioned drawbacks, to provide an apparatus for producing a high dissociation pressure single crystal that can prevent the occurrence of scratches on the upper and lower shafts, and can smoothly rotate and move the shafts up and down.

(課題を解決するための手段) 本発明は、高解離圧成分元素ガスを封入した気密容器中
でチョクラルスキー法により高解離圧単結晶を製造する
装置において、単結晶を引き上げる上軸及び又はるつぼ
を支持する下軸が上記気密容器を貫通するシール部を、
該軸より軟質の材料で構成したことを特徴とする高解離
圧単結晶の製造装置である。
(Means for Solving the Problems) The present invention provides an apparatus for producing a high dissociation pressure single crystal by the Czochralski method in an airtight container filled with a high dissociation pressure component gas. A seal portion where the lower shaft supporting the crucible passes through the airtight container,
This is an apparatus for producing a high dissociation pressure single crystal, characterized in that it is made of a material softer than the axis.

なお、上軸及び又は下軸をモリブデン又はステンレスで
構成し、受皿全体もしくは、受皿の開口部を石英、カー
ボン、I)BN% SiC,気密質のカーボン、カーボ
ンにpBNをコーティングしたもの、カーボンに気密質
カーボンをコーティングしたもの、カーボンにSiCを
コーティングしたもの、ステンレス等の材料で構成する
ことが好ましい。また、前記シール部は、液体封止剤を
収容する受皿として構成することが好ましい。
The upper and/or lower shafts are made of molybdenum or stainless steel, and the entire saucer or the opening of the saucer is made of quartz, carbon, I) BN% SiC, airtight carbon, carbon coated with pBN, or carbon. It is preferable to use materials such as those coated with airtight carbon, carbon coated with SiC, and stainless steel. Further, it is preferable that the seal portion is configured as a saucer that accommodates the liquid sealant.

(作用) 本発明は、高解離圧成分元素ガスを封入した気密容器中
でチョクラルスキー法により高解離圧単結晶を製造する
装置の、上軸と下軸が上記気密容器を貫通するシール部
を該軸より軟らい材質で構成したことを特徴とするもの
であり、このような構成を採用することによ′す、軸表
面のキズの発生を防止し、軸の回転と昇降を円滑にし、
軸の振動に起因する原料融液の温度分布の乱れや引き上
げ結晶の直径制御の乱れ等を防止し、軸とシール部の焼
き付けを防止したものである。
(Function) The present invention provides a seal portion of an apparatus for producing a high dissociation pressure single crystal by the Czochralski method in an airtight container sealed with a high dissociation pressure component elemental gas, in which the upper shaft and the lower shaft pass through the airtight container. The shaft is made of a material that is softer than the shaft, and by adopting this structure, it is possible to prevent the occurrence of scratches on the shaft surface and to make the rotation and elevation of the shaft smooth. ,
This prevents disturbances in the temperature distribution of the raw material melt and disturbances in the diameter control of the pulled crystal caused by vibrations of the shaft, and prevents seizure of the shaft and seal portion.

このように、本発明は軸の材質とシール部の材質の組み
合わせに特徴がある。それ故、従来の高解離圧単結晶の
製造装置として説明した第2図の装置も、その上下軸2
.3を比較的硬質の材質で構成し、シール部の受皿12
.13を比較的軟質の材質で構成するときには、本発明
の1具体例となる。第1図は、軸2.3と摺動する受皿
12.13の中央の開口部分24.25のみを比較的軟
質の材質で構成したもので、この場合は受皿12.13
の材質は特別問題にされることはなく、軸と同じ硬質の
ものも使用することができるし、この開口部分のみを交
換することも可能である。そして、受皿以外の装置構成
は、第2図と総て同じであるから、説明を省略する。
As described above, the present invention is characterized by the combination of the material of the shaft and the material of the seal portion. Therefore, the apparatus shown in FIG. 2, which was explained as a conventional high dissociation pressure single crystal manufacturing apparatus, also has a vertical axis 2.
.. 3 is made of a relatively hard material, and the saucer 12 of the seal portion is made of a relatively hard material.
.. When 13 is made of a relatively soft material, this is a specific example of the present invention. In FIG. 1, only the central opening 24.25 of the saucer 12.13 that slides on the shaft 2.3 is made of a relatively soft material; in this case, the saucer 12.13
There is no particular problem with the material of the shaft, and it is possible to use the same hard material as the shaft, and it is also possible to replace only this opening part. The configuration of the device other than the saucer is entirely the same as that shown in FIG. 2, so a description thereof will be omitted.

(実施例) 第1図の装置を用いて、ノンドープGaAs単結晶を育
成した。モリブデン製の上下軸を用い、気密容器、アン
プル及び導管は材質pBNをコーティングしたカーボン
で作り、受皿は材質モリブデンで作り、受皿の中央の開
口部分は気密性カーボンでコーティングしたカーボン製
とした。6インチのpBN製るつぼには、ノンドープG
aAs多結晶原料4.0Kg及びB、03液体封止剤3
00gをチャージした。上下軸の受皿にもB、03液体
封止剤を収容した。また、アンプルにはヒ素500gを
収容した。単結晶育成時には、アンプルは615℃以上
に加熱して、気密容器にヒ素ガスを供給してヒ素と窒素
の混合ガスで気密容器内を15Kg/cm”に加圧した
。そして、上軸の回転速度を5rpm、下軸の回転速度
を2Orpm。
(Example) A non-doped GaAs single crystal was grown using the apparatus shown in FIG. Using a molybdenum upper and lower shaft, the airtight container, ampoule, and conduit were made of carbon coated with pBN, the saucer was made of molybdenum, and the opening in the center of the saucer was made of carbon coated with airtight carbon. The 6-inch pBN crucible contains non-doped G.
aAs polycrystalline raw material 4.0Kg and B, 03 liquid sealant 3
00g was charged. B, 03 liquid sealant was also contained in the trays of the upper and lower shafts. The ampoule also contained 500 g of arsenic. During single crystal growth, the ampoule was heated to 615°C or higher, arsenic gas was supplied to the airtight container, and the inside of the airtight container was pressurized to 15 kg/cm'' with a mixed gas of arsenic and nitrogen.Then, the upper shaft was rotated. The speed is 5 rpm, and the rotation speed of the lower shaft is 2 Orpm.

引上速度を6mm/hrとして、重さ3.5Kg、直径
8oII!1、長さ150■の単結晶を育成した。この
間、軸の回転及び引き上げは円滑であり、焼き付けを起
こすことはなかった。結晶育成後、上下軸を調べたが、
キズは全く観察されなかった。得られた単結晶の直径制
御は良好であり、転位密度は、従来のLEC法で育成し
た単結晶と比較すると、およそ20分の1で、1000
cv−”と低(、電気特性の面内均一性も極めて良好で
あった。
At a pulling speed of 6mm/hr, the weight is 3.5Kg and the diameter is 8oII! 1. A single crystal with a length of 150 cm was grown. During this time, the shaft was rotated and pulled up smoothly, and no seizure occurred. After crystal growth, we examined the vertical axis, but
No scratches were observed. The diameter of the obtained single crystal was well controlled, and the dislocation density was approximately 1/20th that of a single crystal grown by the conventional LEC method, and the dislocation density was 1000.
The in-plane uniformity of the electrical properties was also very good.

(発明の効果) 本発明は、上記の構成を採用することにより、上下軸と
シール部の焼き付けを防止し、上下軸表面のキズの発生
を防止し、上下軸の回転と昇降を円滑にして、軸の振動
に起因する原料融液の温度分布の乱れや引き上げ結晶の
直径制御の乱れ等を未然に防止することができ、その結
果、双晶の発生や多結晶化を防止することができるので
、欠陥密度の少ない、均一な電気特性を有する高品質の
単結晶を高い歩留まりで製造することができるようにな
った。
(Effects of the Invention) By adopting the above configuration, the present invention prevents the vertical shaft and the seal portion from being burned, prevents the occurrence of scratches on the surface of the vertical shaft, and smoothes the rotation and elevation of the vertical shaft. , it is possible to prevent disturbances in the temperature distribution of the raw material melt and disturbances in the diameter control of the pulled crystal caused by shaft vibration, and as a result, the generation of twins and polycrystalization can be prevented. Therefore, it has become possible to produce high-quality single crystals with low defect density and uniform electrical properties at high yields.

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

第1図は本発明の1具体例である高解離圧単結晶の製造
装置の断面図、第2図は従来の高解離圧単結晶の製造装
置の断面図である。
FIG. 1 is a sectional view of an apparatus for producing a high dissociation pressure single crystal, which is a specific example of the present invention, and FIG. 2 is a sectional view of a conventional apparatus for producing a high dissociation pressure single crystal.

Claims (3)

【特許請求の範囲】[Claims] (1)高解離圧成分元素ガスを封入した気密容器中でチ
ョクラルスキー法により高解離圧単結晶を製造する装置
において、単結晶を引き上げる上軸及び又はるつぼを支
持する下軸が上記気密容器を貫通するシール部を、該軸
より軟質の材料で構成したことを特徴とする高解離圧単
結晶の製造装置。
(1) In an apparatus for producing a high dissociation pressure single crystal by the Czochralski method in an airtight container filled with a high dissociation pressure component element gas, the upper shaft for pulling up the single crystal and/or the lower shaft for supporting the crucible are connected to the airtight container. 1. An apparatus for producing a high dissociation pressure single crystal, characterized in that a seal portion passing through the shaft is made of a material softer than the shaft.
(2)前記シール部を、液体封止剤を収容する受皿とし
たことを特徴とする請求項(1)記載の高解離圧単結晶
の製造装置。
(2) The apparatus for producing a high dissociation pressure single crystal according to claim (1), wherein the seal portion is a receiving tray that accommodates a liquid sealant.
(3)上軸及び又は下軸の材料をモリブデン又はステン
レスとし、シール部の材料をカーボン、気密質のカーボ
ン又は気密質のカーボンをコーティングしたカーボンと
したことを特徴とする請求項(1)又は(2)記載の高
解離圧単結晶の製造装置。
(3) Claim (1) characterized in that the material of the upper shaft and/or the lower shaft is molybdenum or stainless steel, and the material of the seal portion is carbon, airtight carbon, or carbon coated with airtight carbon. (2) The apparatus for producing a high dissociation pressure single crystal as described in (2).
JP5163990A 1990-03-05 1990-03-05 High dissociation pressure single crystal manufacturing equipment Expired - Lifetime JP2830315B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5163990A JP2830315B2 (en) 1990-03-05 1990-03-05 High dissociation pressure single crystal manufacturing equipment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5163990A JP2830315B2 (en) 1990-03-05 1990-03-05 High dissociation pressure single crystal manufacturing equipment

Publications (2)

Publication Number Publication Date
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003060202A1 (en) * 2002-01-11 2003-07-24 Nikko Materials Co., Ltd. Single crystal growth system and single crystal growth method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003060202A1 (en) * 2002-01-11 2003-07-24 Nikko Materials Co., Ltd. Single crystal growth system and single crystal growth method

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