JPS61215292A - Apparatus for producing compound semiconductor single crystal - Google Patents

Apparatus for producing compound semiconductor single crystal

Info

Publication number
JPS61215292A
JPS61215292A JP5433285A JP5433285A JPS61215292A JP S61215292 A JPS61215292 A JP S61215292A JP 5433285 A JP5433285 A JP 5433285A JP 5433285 A JP5433285 A JP 5433285A JP S61215292 A JPS61215292 A JP S61215292A
Authority
JP
Japan
Prior art keywords
compound semiconductor
crucible
single crystal
semiconductor single
pulling
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
JP5433285A
Other languages
Japanese (ja)
Inventor
Joshi Nishio
譲司 西尾
Satao Yashiro
八代 佐多夫
Shoichi Washitsuka
鷲塚 章一
Masayuki Watanabe
正幸 渡辺
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.)
Toshiba Corp
Original Assignee
Toshiba Corp
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 Toshiba Corp filed Critical Toshiba Corp
Priority to JP5433285A priority Critical patent/JPS61215292A/en
Publication of JPS61215292A publication Critical patent/JPS61215292A/en
Pending 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 produce a compound semiconductor crystal having high purity and low dislocation density, in high yield, by using sintered aluminum nitride as a material of a heat-shielding plate placed above the crucible to decrease the temperature gradient in the molten raw material and the encapsulant along the direction of the pulling-up axis. CONSTITUTION:The crucible 3 is charged with Ga and As as starting raw materials and then with B2O3 as encapsulant, and is placed in a high-pressure vessel 1. The space in the high-pressure vessel 1 is pressurized with Ar gas, and the crucible 3 is heated with the heater 2 to obtain molten liquid of Ga-As 7. The liquid is pulled up with the pulling-up shaft 5 to produce a compound semiconductor single crystal. In the above process, a sintered aluminum nitride is used as a material of a heat-shielding plate 10 placed above the crucible 3 to decrease the temperature gradient in the molten raw material 7 along the direction of the pulling-up axis.

Description

【発明の詳細な説明】 〔発明の技術分野〕 本発明は、化合物半導体単結晶の製造装置の改良に関す
るものである。
DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to an improvement in a compound semiconductor single crystal manufacturing apparatus.

〔発明の技術的背景とその問題点〕[Technical background of the invention and its problems]

化合物半導体単結晶は光デバイス、電子デバイス用基板
材料として用いられており、高品質なものが要求されて
いる。たとえば超高速IC用基板となるGaAs単結晶
では、アンドープで熱変成が無く、均一性良好な半絶縁
性基板が必要である。
Compound semiconductor single crystals are used as substrate materials for optical devices and electronic devices, and high quality is required. For example, GaAs single crystal, which is used as a substrate for ultra-high-speed ICs, requires a semi-insulating substrate that is undoped, does not undergo thermal transformation, and has good uniformity.

ところが、化合物半導体単結晶を製造する高圧容器内の
炉材には、従来グラファイト製品が使用されておシ、炉
材からの炭素汚染があり、化合物半導体単結晶基板の電
気特性の均一性に悪影響を及ぼすという問題があった。
However, graphite products have traditionally been used for the furnace material in the high-pressure vessel used to manufacture compound semiconductor single crystals, and carbon contamination from the furnace material has an adverse effect on the uniformity of the electrical properties of compound semiconductor single crystal substrates. There was a problem that it caused

ところで、化合物半導体単結晶の製造装置では、第3図
に示すように上部熱しゃへい板10もグラファイト製で
あシ、熱伝導率が窒化アルミニウムの焼結体より1桁以
上大きく、単結晶育成時に結晶内部から上部への熱の逃
げが大きくなシ、熱環境を緩く設定することが困離なた
め、転位密度が1000as  以下の低転位結晶を歩
留り良く製造することは非常に困離で6つ之。
By the way, in the compound semiconductor single crystal production equipment, the upper heat shield plate 10 is also made of graphite, as shown in Fig. 3, and the thermal conductivity is more than one order of magnitude higher than that of the aluminum nitride sintered body, so that it can be easily used during single crystal growth. It is extremely difficult to produce low-dislocation crystals with a dislocation density of 1000 as or less with good yield because heat escapes from the inside of the crystal to the top is large and it is difficult to set a gentle thermal environment. this.

またパイロリティック窒化ボロン製の上部熱し中へい板
を用いる例もあるが(特開昭59−57992号公報)
、単結晶化歩留りが低く、また封止剤の付着による劣化
が激しいという問題があった。
There is also an example of using an upper heating inner plate made of pyrolytic boron nitride (Japanese Patent Application Laid-Open No. 59-57992).
However, there were problems in that the single crystallization yield was low and the deterioration due to the adhesion of the sealant was severe.

〔発明の目的〕[Purpose of the invention]

本発明の目的は、上述した問題点を解決し、高純度で低
転位密度の化合物半導体単結晶を歩留シ良く製造できる
装置を提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems and to provide an apparatus capable of manufacturing compound semiconductor single crystals of high purity and low dislocation density with a high yield.

〔発明の概要〕[Summary of the invention]

即ち、本発明は、るつは上部に設けられる熱しゃへい板
を窒化アルミニウムからなる焼結体で構成したものでち
る。
That is, in the present invention, the heat shield plate provided on the upper part of the crucible is made of a sintered body made of aluminum nitride.

本発明の窒化アルミニウムの焼結体より成る上部熱し中
へい板は、熱伝導率がグラファイトに比べて1桁以上小
さく、また、ふく対重も小さいため、ふく射、対流によ
る熱損失が少ない。すなわちグラファイトに比べ、よシ
大きな熱しゃへい効果が得られる特徴がある。また、封
止剤に対しても化学的に安定であるので、結晶中の炭素
濃度を低く、また熱環境を緩く設定できるため、歩留り
良く低転位、化炭素濃度の結晶育成が行なえる。
The upper heat shield plate made of a sintered body of aluminum nitride according to the present invention has a thermal conductivity that is more than one order of magnitude lower than that of graphite, and also has a smaller weight per layer, so there is less heat loss due to radiation and convection. In other words, it has the characteristic of providing a greater heat shielding effect than graphite. Furthermore, since it is chemically stable against sealants, the carbon concentration in the crystal can be kept low and the thermal environment can be set loosely, so that crystals with low dislocations and carbon dioxide concentration can be grown with high yield.

〔発明の効果〕〔Effect of the invention〕

以上説明したように本発明の装置によれば、上部熱しゃ
へい板から育成結晶中への炭素汚染を低減し、かつ結晶
内部から上部への熱の流れを適正化できるので、熱環境
を緩く設定でき、歩留り良く低転位結晶を育成すること
が可能になる。
As explained above, according to the apparatus of the present invention, it is possible to reduce carbon contamination from the upper heat shield plate into the grown crystal, and to optimize the flow of heat from the inside of the crystal to the upper part, so the thermal environment can be set loosely. This makes it possible to grow low-dislocation crystals with good yield.

〔発明の実施例〕[Embodiments of the invention]

以下、本発明の一実施例を図面を参照しながら説明する
。第1図は本発明の化合物半導体単結晶の製造装置の一
例である。
An embodiment of the present invention will be described below with reference to the drawings. FIG. 1 shows an example of a compound semiconductor single crystal manufacturing apparatus of the present invention.

第1図において1は高圧容器、2はヒータ、3はるつぼ
、4はサセプタ、5は引上げ軸、6は種結晶、7はGa
 A s融液、8はB2O3融液、9はるつぼ回転軸、
10は上部熱し中へい板である。
In Fig. 1, 1 is a high pressure vessel, 2 is a heater, 3 is a crucible, 4 is a susceptor, 5 is a pulling shaft, 6 is a seed crystal, and 7 is Ga
A s melt, 8 is B2O3 melt, 9 is crucible rotation axis,
10 is an upper heated inner plate.

ここで上部熱しゃへい板10は窒化アルミニウムの焼結
体を成型したものである。
Here, the upper heat shield plate 10 is formed from a sintered body of aluminum nitride.

次に、この窒化アルミニウムの焼結体よ構成る上部熱し
中へい板10を用いた具体的な実施例を詳細に説明する
Next, a specific example using the upper heat shield plate 10 made of the sintered body of aluminum nitride will be described in detail.

るつぼ3の中に出発原料であるGaとAsを充填した後
、封止剤としてB2O3を充填した。次にるつぼ3を高
圧容器1内に収納し、高圧容器内を人rガスで加圧した
後、加熱を開始した。約600℃で82038が軟化し
、原料が完全に覆われたので、さらに加熱を続け、Ga
とA3を反応させてGa A s融液7を侵た。引き続
いて引上げ圧力、ここでは20atmに減圧し、温度の
安定を待ってから種付けを行ない、その後引上げを開始
した。
After filling the crucible 3 with Ga and As as starting materials, it was filled with B2O3 as a sealant. Next, the crucible 3 was housed in the high-pressure container 1, and after pressurizing the inside of the high-pressure container with human gas, heating was started. 82038 softened at about 600°C and the raw material was completely covered, so heating was continued and Ga
and A3 were reacted to invade the GaAs melt 7. Subsequently, the pulling pressure was reduced to 20 atm, and after waiting for the temperature to stabilize, seeding was performed, and then pulling was started.

Ga入入線融液7中よびB2O3融液8中の熱環境を非
常に緩く設定したが、双晶または多結晶化することなく
直径80φ重量約2.5麺の(100) GaAs単結
晶が得られた。このようにして得られた単結晶は従来の
グラファイト製上部熱し中へい板を用いて育成した単結
晶に比べ、結晶中の炭素濃度はi以下と低くなカ、また
転位密度は10003  以下であった。
Although the thermal environments in the Ga incoming wire melt 7 and the B2O3 melt 8 were set very loosely, a (100) GaAs single crystal with a diameter of 80φ and a weight of about 2.5 mm was obtained without twinning or polycrystalization. It was done. The single crystal thus obtained has a lower carbon concentration of less than i, and a dislocation density of less than 10003, compared to a single crystal grown using a conventional graphite heating plate. Ta.

〔発明の他の実施例〕[Other embodiments of the invention]

本発明の他の実施例を図面を参照しながら説明する。第
2図は本発明の化合物半導体単結晶の製造装置の一例で
ある。
Other embodiments of the invention will be described with reference to the drawings. FIG. 2 shows an example of the compound semiconductor single crystal manufacturing apparatus of the present invention.

第2図において、1は高圧容器、2はヒータ、3はるつ
ぼ、4はサセプタ、5は引上げ軸、6は種結晶、7はG
aAs融液、8はB2O3融液、9はるつぼ回転軸、1
0は上部熱し中へい板である。
In Fig. 2, 1 is a high pressure vessel, 2 is a heater, 3 is a crucible, 4 is a susceptor, 5 is a pulling shaft, 6 is a seed crystal, and 7 is a G
aAs melt, 8 B2O3 melt, 9 crucible rotation axis, 1
0 is the upper heated inner plate.

ここで上部熱し中へい板10は窒化アルミニウムの焼結
体を成型したものである。
Here, the upper heated inner partition plate 10 is formed from a sintered body of aluminum nitride.

上記した本発明の一実施例で述べたのと同様の操作を行
ない、直径55φ重量約80ofの(100)Ga A
 s単結晶が得られた。このようにして得られた単結晶
は、従来のグラファイト製上部熱しゃへい板を用いて育
成した単結晶に比べ、結晶中の炭素濃度は低く、また転
位密度は10100O”以下でsb、一部無転位領域も
見られた。
The same operation as described in the above embodiment of the present invention was carried out to prepare (100) Ga A with a diameter of 55φ and a weight of about 80of.
s single crystal was obtained. The single crystal thus obtained has a lower carbon concentration than a single crystal grown using a conventional graphite upper heat shield plate, and has a dislocation density of 10,100 O" or less, with sb and some parts free. Dislocation regions were also observed.

以上のように本発明の単結晶の製造装置によれば、低炭
素濃度、低転位密度の単結晶を育成することができる。
As described above, according to the single crystal manufacturing apparatus of the present invention, a single crystal with low carbon concentration and low dislocation density can be grown.

また、封止剤が付着しても劣化は全く見られていない。Furthermore, no deterioration was observed even when the sealant was attached.

更には、液体封止引上げ法によるGaP 、 IuP等
、他のI−V族化合物半導体単結晶の製造にも適応する
ことができ、得られる効果も大きい。
Furthermore, it can be applied to the production of other group IV compound semiconductor single crystals such as GaP, IuP, etc. by the liquid seal pulling method, and the obtained effects are great.

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

第1図は本発明の化合物半導体単結晶の製造装置の一実
施例を示す構成図、第2図は本発明の化合物半導体単結
晶の製造装置の他の実施例を示す構成図、第3図は従来
の化合物半導体単結晶の製造装置の構成図である。 1:高圧容器、2:ヒータ、3:るつぼ、4:サセプタ
、5:引上げ軸、6:種結晶、7 : GaAs融液、
8:B2O3融液、9:るつぼ回転軸、10:上部熱し
中へい板。 代理人弁理士 則近憲佑 (ほか1名)第1図 第  2  図 第  3  図
FIG. 1 is a block diagram showing one embodiment of the compound semiconductor single crystal production apparatus of the present invention, FIG. 2 is a block diagram showing another embodiment of the compound semiconductor single crystal production apparatus of the present invention, and FIG. 1 is a configuration diagram of a conventional compound semiconductor single crystal manufacturing apparatus. 1: High pressure container, 2: Heater, 3: Crucible, 4: Susceptor, 5: Pulling shaft, 6: Seed crystal, 7: GaAs melt,
8: B2O3 melt, 9: Crucible rotating shaft, 10: Upper heating medium plate. Representative Patent Attorney Kensuke Norichika (and 1 other person) Figure 1 Figure 2 Figure 3

Claims (1)

【特許請求の範囲】[Claims] 化合物半導体単結晶を液体封止引上げ法により製造する
装置において、原料融液中、および封止剤中の引上げ軸
方向温度勾配を低減させるためにるつぼ上部に設けられ
る熱しゃへい板を、窒化アルミニウムからなる焼結体で
構成したことを特徴とする化合物半導体単結晶の製造装
置。
In an apparatus for manufacturing compound semiconductor single crystals by the liquid-sealed pulling method, a heat shield plate provided at the top of the crucible is made of aluminum nitride in order to reduce the temperature gradient in the pulling axis direction in the raw material melt and in the sealant. 1. An apparatus for manufacturing a compound semiconductor single crystal, characterized in that it is constructed of a sintered body.
JP5433285A 1985-03-20 1985-03-20 Apparatus for producing compound semiconductor single crystal Pending JPS61215292A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5433285A JPS61215292A (en) 1985-03-20 1985-03-20 Apparatus for producing compound semiconductor single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5433285A JPS61215292A (en) 1985-03-20 1985-03-20 Apparatus for producing compound semiconductor single crystal

Publications (1)

Publication Number Publication Date
JPS61215292A true JPS61215292A (en) 1986-09-25

Family

ID=12967639

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5433285A Pending JPS61215292A (en) 1985-03-20 1985-03-20 Apparatus for producing compound semiconductor single crystal

Country Status (1)

Country Link
JP (1) JPS61215292A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01145395A (en) * 1987-11-30 1989-06-07 Nippon Mining Co Ltd Production of compound semiconductor single crystal
JPH02180794A (en) * 1988-12-29 1990-07-13 Toshiba Corp Apparatus for producing iii-v compound semiconductor single crystal

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01145395A (en) * 1987-11-30 1989-06-07 Nippon Mining Co Ltd Production of compound semiconductor single crystal
JPH02180794A (en) * 1988-12-29 1990-07-13 Toshiba Corp Apparatus for producing iii-v compound semiconductor single crystal

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