JPH02289490A - Peephole in high temperature growth chamber and method for sealing the peephole - Google Patents
Peephole in high temperature growth chamber and method for sealing the peepholeInfo
- Publication number
- JPH02289490A JPH02289490A JP10577089A JP10577089A JPH02289490A JP H02289490 A JPH02289490 A JP H02289490A JP 10577089 A JP10577089 A JP 10577089A JP 10577089 A JP10577089 A JP 10577089A JP H02289490 A JPH02289490 A JP H02289490A
- Authority
- JP
- Japan
- Prior art keywords
- growth chamber
- viewing window
- growth
- chamber
- sealing
- 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
Links
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007789 sealing Methods 0.000 title claims description 11
- 239000013078 crystal Substances 0.000 claims abstract description 39
- 238000010494 dissociation reaction Methods 0.000 claims abstract description 20
- 230000005593 dissociations Effects 0.000 claims abstract description 20
- 239000003566 sealing material Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 239000000565 sealant Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000012768 molten material Substances 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- 239000003708 ampul Substances 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、高解離圧成分ガスを満たした高温成長室でチ
ョクラルスキー法により高解離圧化合物単結晶を製造す
る装置で、高温成長室に取り付ける覗き窓及び覗き窓の
シール方法に関する。Detailed Description of the Invention (Field of Industrial Application) The present invention is an apparatus for producing a single crystal of a high dissociation pressure compound by the Czochralski method in a high temperature growth chamber filled with a high dissociation pressure component gas. This invention relates to a viewing window installed in a vehicle and a method for sealing the viewing window.
（従来の技術）
第１図は、蒸気圧制御チヨクラルスキー法による単結晶
の製造装置の概念図である。この装置は、高温に保持さ
れた成長室に結晶の高解離圧成分ガスを閉じ込め、その
中でチョクラルスキ−法により単結晶を育成するための
ものである。不活性ガスを満たしたチャンバ１には、高
解離圧成分ガスを閉じ込める高温成長室２を置（。そし
て、種結晶４をに軸３で支持し、サセプタ６でるつぼ７
を支持して下軸５により、該成長室２内に配５置する。(Prior Art) FIG. 1 is a conceptual diagram of a single crystal manufacturing apparatus using the vapor pressure controlled Czyochralski method. This apparatus confines a high dissociation pressure component gas for crystals in a growth chamber maintained at a high temperature, and grows a single crystal therein by the Czochralski method. A high-temperature growth chamber 2 that confines a high dissociation pressure component gas is placed in a chamber 1 filled with an inert gas.
is supported and placed in the growth chamber 2 by the lower shaft 5.
上軸３と成長室２の接続部には液体封止剤１３を収容す
る液溜１２を、下軸５と成長室２の接合部には液体封止
剤１６を収容する液溜Ｉ５を設け、その周囲に配置した
ヒータＩ４及び１７で加熱する。−３方、るつぼ６には
、原料８及び液体封止剤９を収容し、ヒータ１１で加熱
融解し、かつ、原料融液の温度調節を行う。さらに、チ
ャンバ１の」二方で高温成長室２から離れた場所に、高
解離圧成分元素２０を収容するアンプル１９を設け、導
管１８により成長室２と連通させ、ヒータ２１でアンプ
ル１９を加熱し、高解離圧成分ガス圧を調節する。そし
て、ヒータ２２で導管１８を加熱することにより、高解
離圧成分ガスの凝縮を防止する。このように、成長室２
内の雰囲気ガス及び原料融液湯度を調節した後、」−軸
３を下降させて種結晶４を原料融液８に浸して十分なじ
ませてから、徐々に引き」二げることにより単結晶１０
を育成する。結晶育成の際には、引上結晶の直径を制御
するために随時結晶の形状を観察する必要がある。その
ため、ステンレスチャンバ１及び高温成長室２にそれぞ
れ覗き窓２４及び２３が取り付けられている。ステンレ
スチャンバの覗き窓２４の取り付け部には通常のＯリン
グが用いられる。高温に加熱される成長室２の覗き窓２
３には従来の０リングを用いることができないので、例
えば、第５図に示すようなシール方法が採用されている
。即ち、高温成長室２と覗き窓押さえ部材２６及び該部
材２６と覗き窓２５との間にカーボン製のフィルムを挟
みネジで締め付けることによりシールを完成するもので
ある。A liquid reservoir 12 containing a liquid sealant 13 is provided at the joint between the upper shaft 3 and the growth chamber 2, and a liquid reservoir I5 containing a liquid sealant 16 is provided at the joint between the lower shaft 5 and the growth chamber 2. , is heated by heaters I4 and 17 placed around it. - On the third side, a crucible 6 contains a raw material 8 and a liquid sealant 9, is heated and melted by a heater 11, and the temperature of the raw material melt is adjusted. Furthermore, an ampoule 19 containing a high dissociation pressure component element 20 is provided at a location away from the high-temperature growth chamber 2 on both sides of the chamber 1, communicated with the growth chamber 2 through a conduit 18, and the ampoule 19 is heated with a heater 21. and adjust the high dissociation pressure component gas pressure. By heating the conduit 18 with the heater 22, condensation of the high dissociation pressure component gas is prevented. In this way, growth chamber 2
After adjusting the atmospheric gas in the chamber and the temperature of the raw material melt, the shaft 3 is lowered to immerse the seed crystal 4 in the raw material melt 8 until it is sufficiently absorbed, and then the seed crystal 4 is gradually pulled out. crystal 10
Develop. During crystal growth, it is necessary to observe the shape of the crystal from time to time in order to control the diameter of the pulled crystal. Therefore, viewing windows 24 and 23 are installed in the stainless steel chamber 1 and the high temperature growth chamber 2, respectively. An ordinary O-ring is used for the attachment part of the observation window 24 of the stainless steel chamber. Peephole 2 of growth chamber 2 heated to high temperature
3, it is not possible to use a conventional O-ring, so a sealing method as shown in FIG. 5, for example, is adopted. That is, a carbon film is sandwiched between the high temperature growth chamber 2 and the viewing window holding member 26, and between the member 26 and the viewing window 25 and tightened with screws to complete the seal.
（発明が解決しようとする課題）
」〕記の装置では、カーボン製フィルム自体の材質に由
来する間隙があるために、締め付けを強めても完全にシ
ールすることはできず、成長室から高解離圧成分ガスの
漏れを防ぐことができなかった。(Problem to be Solved by the Invention) In the device described above, because there are gaps caused by the material of the carbon film itself, it is not possible to completely seal even if the tightening is tightened, and high dissociation is removed from the growth chamber. It was not possible to prevent the leakage of pressure component gas.
本発明は、かかる高温成長室の覗き窓のシールを改善し
、成長室からの高解離圧成分ガスの漏れを防止すること
のできる高温成長室の覗き窓及びそのシール方法を提供
しようとするものであり、さらに、このようなｔ１１結
晶５２造装置を用いることにより、原料融液の組成のズ
レを防ぎ、転位の発生を大幅に減少させることを１−ｉ
Ｊ能にしたものである。The present invention aims to improve the sealing of the viewing window of such a high-temperature growth chamber and to provide a viewing window for a high-temperature growth chamber and a method for sealing the same, which can prevent leakage of high dissociation pressure component gas from the growth chamber. Furthermore, by using such a T11 crystal production apparatus, it is possible to prevent deviations in the composition of the raw material melt and to significantly reduce the occurrence of dislocations.
This is a J-Noh version.
（課題を解決するための手段）
本発明は、（１）高解離圧成分ガスを満たした高温成長
室でチコクラルスキー法により単結晶を育成する高解離
圧化合物単結晶の製造装置で、高温成長室に取り付ける
覗き窓において、取り付け部にＩＩＩ Ｔ３族元索のシ
ール材を介在させたことを特徴とする覗き窓、及び、（
２）Ｊ−記（１）記載の覗き窓取り付け部のシール方法
において、成長結晶を構成するＩｎ ｎ族元素で作った
線状シール材を該取り付け部の周囲に挟み込み、単結晶
育成時の成長室加熱により、該シール材を溶融し、取り
付け部の隙間に浸透させてシールを完成させることを特
徴とする覗き窓取り付け部のシール方法である。(Means for Solving the Problems) The present invention provides (1) an apparatus for producing a single crystal of a high dissociation pressure compound, which grows a single crystal by the Cichochralski method in a high temperature growth chamber filled with a high dissociation pressure component gas; A viewing window attached to a growth chamber, characterized in that a sealing material of III T3 group original cable is interposed in the attachment part, and (
2) In the method for sealing the viewing window attachment part described in J-Note (1), a linear sealing material made of an In group element constituting the growing crystal is sandwiched around the attachment part to prevent growth during single crystal growth. This is a method of sealing a viewing window attachment part, characterized in that the sealing material is melted by room heating, and is allowed to penetrate into the gap in the attachment part to complete the seal.
（作用）
本発明は、第１図の１１１結晶製造装置等の高温成長室
の覗き窓の改良に係わり、第２図は、該覗き窓の拡大断
面図であり、第３図は、覗き窓のシール形成手順を示し
た説明図である。成長室２の開口に押さえ部材２６をネ
ジ山に沿って挿入し、また、透明セラミックス製の覗き
窓２５を該押さえ部材２６のネジ山に沿って挿入し、両
者のフランジの間に線状のインジウムシール材２７を挟
み込み、圧縮して固定する。シール材２７のズレを防止
するために、例えば、押さえ部材２６に図のような溝を
形成することが好ましい。(Function) The present invention relates to improvement of the observation window of a high temperature growth chamber such as the 111 crystal manufacturing apparatus shown in FIG. 1, FIG. 2 is an enlarged sectional view of the observation window, and FIG. FIG. 3 is an explanatory diagram showing a seal forming procedure. The holding member 26 is inserted into the opening of the growth chamber 2 along the screw thread, and the viewing window 25 made of transparent ceramics is inserted along the thread of the holding member 26, and a linear line is inserted between the flanges of both. Indium seal material 27 is sandwiched, compressed and fixed. In order to prevent the sealing material 27 from shifting, it is preferable to form a groove as shown in the figure in the holding member 26, for example.
次に、シールの形成手順を説明すると、第３図の（ａ）
は、シール材を挟んだ状態を示したもので、（Ｌ１）は
、これを圧縮して仮のシールを形成したものである。単
結晶製造装置の準備を総て整えて、ヒータを加熱し、成
長室を高／！シに加熱するときには、」−記シール材は
約８００℃に加熱されて溶融され、両者のフランジの隙
間に浸透して、（Ｃ）のようにシールを完成する。Next, to explain the procedure for forming the seal, see (a) in Figure 3.
(L1) shows the state in which the sealing material is sandwiched, and (L1) shows the state in which the sealing material is compressed to form a temporary seal. Make all preparations for the single crystal manufacturing equipment, heat the heater, and turn the growth chamber to high/! When the sealing material is heated to approximately 800° C., it is melted and penetrates into the gap between the flanges to complete the seal as shown in (C).
第４図は、第２図の覗き窓の変形であり、高温成長室２
と一体的に取り付けたフランジ２８に対して、覗き窓２
９を有するフランジ３ｏを市ね合わせ、両者の間に線状
インジウムシール材２７を挟み込み、ボルトナツトで締
め付けるものである。シール形成手順は、第２図の場合
と同じである。Figure 4 is a modification of the viewing window in Figure 2, and shows the high temperature growth chamber 2.
The viewing window 2 is attached to the flange 28 integrally attached to the
The flanges 3o having 9 are placed together, a linear indium sealing material 27 is sandwiched between them, and the flanges 3o are tightened with bolts and nuts. The seal forming procedure is the same as in FIG.
（実施例）
第４図のシール構造を採用した第１図の装置を用いて、
２インチ径のＩｎ１Ｊ１結晶を製造した。(Example) Using the device shown in Fig. 1 which adopts the seal structure shown in Fig. 4,
A 2 inch diameter In1J1 crystal was produced.
高温成長室及びアンプルはｌ）Ｂ Ｎコーティングのカ
ーボンで作製し、るつぼは４インチのｐＢＮ製のものを
用いた。るつぼには原料としてＩｎＰ多結晶］ ｋｇと
ドーパントのＮｅｏ、 ３ｇを、また、液体封ＩＩ“、
剤としてＢ 、 ０ 、３００ ｇを投入した。アンプ
ルには赤リン ５００ｇを投入した。覗き窓シール部の
溝には直径２■のインジウム線を配置した。The high temperature growth chamber and ampoule were made of l) BN coated carbon, and the crucible was a 4 inch pBN one. The crucible contains InP polycrystal] kg as the raw material, 3 g of Neo dopant, and liquid seal II",
300 g of B.0 was added as an agent. 500 g of red phosphorus was added to the ampoule. An indium wire with a diameter of 2 cm was placed in the groove of the viewing window seal.
単結晶の合成は、まず、成長室と」−下軸との接合部周
囲のヒータを加熱して、接合部の液体トＩ ＋ｌｘ剤を
溶融し、覗き窓のインジウムシール材も溶融して成長室
のシールを完成した。そして、アンプルを５５０℃以上
に加熱して、リン蒸気を成長室に供給した。成長室及び
導管はリン蒸気が凝縮しないようにアンプルの温度より
も高い温度に保持した。次いで、るつぼの周囲のヒータ
を加熱して原料及び液体封止剤を溶融し、雰囲気ガスと
原料融液を安定させた。種結晶を固定する」―軸を回転
数５ｒｐｍで回転し、るつぼを支持する下軸を回転数］
Ｏｒｐ＠で回転し、引」−速度を６ｍｍ／ｈｒとして単
結晶を引き」−げた。なお、成長室はアルゴンガスとリ
ン蒸気の混合ガスで全圧を３０ａｔｍ、 リンの分圧
を２０ａｔ−に調整した。また、高圧容器には約３０ａ
ｔ■のアルゴンガスを満たし、成長室内外の圧力バラン
スを保った。To synthesize a single crystal, first heat the heater around the junction between the growth chamber and the lower shaft to melt the liquid I + lx agent at the junction, and also melt the indium sealing material of the viewing window to grow. Completed the room seal. Then, the ampoule was heated to 550° C. or higher, and phosphorus vapor was supplied to the growth chamber. The growth chamber and conduits were kept at a temperature higher than that of the ampoule to prevent condensation of phosphorus vapor. Next, a heater around the crucible was heated to melt the raw material and the liquid sealant, thereby stabilizing the atmospheric gas and the raw material melt. Fix the seed crystal - rotate the shaft at a rotation speed of 5 rpm, and rotate the lower shaft that supports the crucible at a rotation speed]
It was rotated by Orp@ and the single crystal was pulled at a pulling speed of 6 mm/hr. In addition, the total pressure in the growth chamber was adjusted to 30 atm and the partial pressure of phosphorus to 20 atm using a mixed gas of argon gas and phosphorus vapor. In addition, the high pressure vessel has approximately 30a
The growth chamber was filled with argon gas to maintain a pressure balance inside and outside the growth chamber.
その結果、結晶成長過程で、種結晶の溶は落ちや成長室
の雰囲気ガス圧の低下は見られなか）た。また、得られ
たＩｎＰ単結晶は、直径が約６０−一で長さが約１２０
ｍ−であった。成長方向に垂直な而の転位密度分布は弱
いＷ型で、周辺の転位密度は５０００ｃｍ−”程度であ
り、平均すると約２００ＤＣ−１であった。As a result, during the crystal growth process, no drop in the dissolution of the seed crystal or a decrease in the atmospheric gas pressure in the growth chamber was observed. In addition, the obtained InP single crystal has a diameter of about 60 mm and a length of about 12 mm.
It was m-. The dislocation density distribution perpendicular to the growth direction was weak W-shaped, with a peripheral dislocation density of about 5000 cm-'' and an average of about 200 DC-1.
（発明の効果）
本発明は、」―記の構成を採用することにより、高温成
長室の覗き窓のシールを確実なものとすることができる
。このようなシール構造を採用した単結晶製造装置では
、結晶成長過程で高温成長室から高解離圧成分ガスの漏
出を防ぐことができ、原料融液の組成にズレを生ずるこ
ともなく、安定して結晶成長を行うことができるように
なり、低転位密度の単結晶を製造することができるよう
になった。(Effects of the Invention) The present invention can ensure reliable sealing of the viewing window of the high-temperature growth chamber by employing the configuration described in the following. Single crystal manufacturing equipment that employs such a sealing structure can prevent high dissociation pressure component gases from leaking from the high temperature growth chamber during the crystal growth process, and the composition of the raw material melt will not shift and will remain stable. It has now become possible to perform crystal growth using the same method, and it has become possible to produce single crystals with low dislocation density.
第１図は高解離圧化合物半導体単結晶の製造装置の概念
間、第２図及び第４図は本発明の高１、を成１に室の覗
き窓の断面図、第３図は本発明の覗き窓のシール形成手
順を説明するための図、第５図は従来装置の覗き窓の断
面図である。
１：チャンバ、２：高温成長室１３：上軸、４：種結晶
＋５：下軸、６：サセプタ、７：るつぼ、８゜原料融液
、 ９．１３及び１６：液体封止剤、１Ｇ：Ｊ）ｉ結晶
、 Ｉ＋、 １４． １７．２１及び２２：ヒータ
、１２及び１５：液溜め、Ｉ８：導管、Ｉ９：アンプル
、２０：高解離圧成分原料、２３：成長室覗き窓、２４
：チャンバ覗き窓、２５：覗き窓材、２６：押さえ部材
。
２７：インジウムシール材、２８；成長室の覗き窓取り
付け用フランジ、２９：覗き窓材、３０：覗き窓固定用
フランジ、３１：ボルトナット、３２：カーボンフィル
ム製シール材。
（ａ＞
第３図
（ｂ）
（Ｃ）
第４区
λFig. 1 is a conceptual diagram of a high dissociation pressure compound semiconductor single crystal manufacturing apparatus, Figs. 2 and 4 are cross-sectional views of a viewing window of a chamber in which the height 1 of the present invention is shown, and Fig. 3 is a cross-sectional view of a viewing window of a chamber according to the present invention. FIG. 5 is a cross-sectional view of the viewing window of the conventional device. 1: Chamber, 2: High temperature growth chamber 13: Upper axis, 4: Seed crystal + 5: Lower axis, 6: Susceptor, 7: Crucible, 8° raw material melt, 9.13 and 16: Liquid sealant, 1G: J) i crystal, I+, 14. 17.21 and 22: heater, 12 and 15: liquid reservoir, I8: conduit, I9: ampoule, 20: high dissociation pressure component raw material, 23: growth chamber observation window, 24
: Chamber viewing window, 25: Viewing window material, 26: Holding member. 27: indium sealing material, 28: flange for attaching the observation window of the growth chamber, 29: observation window material, 30: flange for fixing the observation window, 31: bolt nut, 32: carbon film sealing material. (a> Figure 3(b) (C) 4th section λ
Claims (2)
ラルスキー法により単結晶を育成する高解離圧化合物単
結晶の製造装置で、高温成長室に取り付ける覗き窓にお
いて、取り付け部にIIIＢ族元素のシール材を介在させ
たことを特徴とする覗き窓。(1) A high dissociation pressure compound single crystal manufacturing device that grows single crystals using the Czochralski method in a high temperature growth chamber filled with high dissociation pressure component gas. A viewing window characterized by interposing an elemental sealant.
法において、成長結晶を構成するIIIＢ族元素で作った
線状シール材を該取り付け部の周囲に挟み込み、単結晶
育成時の成長室加熱により、該シール材を溶融し、取り
付け部の隙間に浸透させてシールを完成させることを特
徴とする覗き窓取り付け部のシール方法。(2) In the method for sealing a viewing window attachment part according to claim (1), a linear sealing material made of a group IIIB element constituting a growing crystal is sandwiched around the attachment part, and a growth chamber during single crystal growth is provided. A method for sealing a viewing window mounting part, characterized in that the sealing material is melted by heating and permeated into a gap in the mounting part to complete the seal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10577089A JPH02289490A (en) | 1989-04-27 | 1989-04-27 | Peephole in high temperature growth chamber and method for sealing the peephole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10577089A JPH02289490A (en) | 1989-04-27 | 1989-04-27 | Peephole in high temperature growth chamber and method for sealing the peephole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02289490A true JPH02289490A (en) | 1990-11-29 |
Family
ID=14416403
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10577089A Pending JPH02289490A (en) | 1989-04-27 | 1989-04-27 | Peephole in high temperature growth chamber and method for sealing the peephole |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02289490A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0633962U (en) * | 1992-10-09 | 1994-05-06 | コマツ電子金属株式会社 | Semiconductor single crystal manufacturing equipment |
-
1989
- 1989-04-27 JP JP10577089A patent/JPH02289490A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0633962U (en) * | 1992-10-09 | 1994-05-06 | コマツ電子金属株式会社 | Semiconductor single crystal manufacturing equipment |
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