JPH04265297A - Method and structure for sealing in treating device of high-dissociation-pressure compound semiconductor crystal - Google Patents
Method and structure for sealing in treating device of high-dissociation-pressure compound semiconductor crystalInfo
- Publication number
- JPH04265297A JPH04265297A JP6217491A JP6217491A JPH04265297A JP H04265297 A JPH04265297 A JP H04265297A JP 6217491 A JP6217491 A JP 6217491A JP 6217491 A JP6217491 A JP 6217491A JP H04265297 A JPH04265297 A JP H04265297A
- Authority
- JP
- Japan
- Prior art keywords
- sealing material
- joint
- sealing
- container
- airtight container
- 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.)
- Withdrawn
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 94
- 239000004065 semiconductor Substances 0.000 title claims abstract description 32
- 238000007789 sealing Methods 0.000 title claims description 52
- 150000001875 compounds Chemical class 0.000 title claims description 28
- 238000000034 method Methods 0.000 title claims description 15
- 239000003566 sealing material Substances 0.000 claims abstract description 135
- 229910052738 indium Inorganic materials 0.000 claims abstract description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010494 dissociation reaction Methods 0.000 claims description 41
- 230000005593 dissociations Effects 0.000 claims description 41
- 239000002994 raw material Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000470 constituent Substances 0.000 claims description 9
- 230000000452 restraining effect Effects 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000008595 infiltration Effects 0.000 abstract 1
- 238000001764 infiltration Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 24
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 22
- 239000007787 solid Substances 0.000 description 21
- 229910000673 Indium arsenide Inorganic materials 0.000 description 20
- 239000000463 material Substances 0.000 description 13
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 12
- 230000003139 buffering effect Effects 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000000565 sealant Substances 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 9
- 238000002844 melting Methods 0.000 description 9
- 230000008018 melting Effects 0.000 description 9
- 238000003825 pressing Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000011109 contamination Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910021478 group 5 element Inorganic materials 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 943°C Chemical compound 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- QYHNIMDZIYANJH-UHFFFAOYSA-N diindium Chemical compound [In]#[In] QYHNIMDZIYANJH-UHFFFAOYSA-N 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Sealing Material Composition (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は、レーザー用あるいはＩ
Ｃ用基板として有用なＧａＡｓ等の高解離圧化合物半導
体結晶を処理する高解離圧化合物半導体結晶処理装置に
おけるシール方法およびシール構造に係わり、特に半導
体の製造に適する高純度な高解離圧成分ガス雰囲気を気
密性よく閉じ込めるためのシール方法およびシール構造
の改良に関するものである。[Industrial Application Field] The present invention is applicable to laser or I
A high-purity high-dissociation-pressure component gas atmosphere particularly suitable for the manufacture of semiconductors, related to the sealing method and seal structure in a high-dissociation-pressure compound semiconductor crystal processing apparatus for processing high-dissociation-pressure compound semiconductor crystals such as GaAs useful as substrates for carbon. This invention relates to improvements in sealing methods and seal structures for airtightly confining.
【０００２】0002
【従来の技術】ＧａＡｓやＩｎＰ等の高解離圧化合物半
導体の結晶成長を行う場合には、化合物からの高解離圧
成分（Ａｓ，Ｐ等）の飛散を防ぐとともに結晶組成を制
御する目的で、処理温度での結晶の解離圧と平衡する高
解離圧成分ガス雰囲気中で処理を行う方法が採られてい
る。[Prior Art] When growing crystals of high dissociation pressure compound semiconductors such as GaAs and InP, in order to prevent high dissociation pressure components (As, P, etc.) from scattering from the compound and to control the crystal composition, A method is adopted in which the treatment is carried out in a high dissociation pressure component gas atmosphere that is in equilibrium with the dissociation pressure of the crystal at the treatment temperature.
【０００３】このような方法に用いられる処理装置とし
て、ＧａＡｓ単結晶の処理装置の一例を図１に示す。こ
の処理装置は特許１４９０６６９号に記載されたもので
、気密容器１は上部容器２および下部容器３より構成さ
れて外部容器４内に配置されており、これら上部容器２
と下部容器３の接合部にはシール材５が介装されていて
、下部容器３の押上げ下軸６に設けられた応力緩衝装置
７によって適正応力で接合されている。気密容器１の内
部にはサセプタ８に支持されてルツボ９が置かれ、サセ
プタ下軸８ａによって回転されるとともに、ヒータ１０
，１０で気密容器１ごと加熱される。また上部容器２に
は蒸気圧制御部１１が設けられており、これに設置され
たヒータ１１ａによってこの部分の温度を気密容器１内
で最も低いかつ適切な一定温度に制御し、高解離圧成分
固体をこの部分にのみ凝縮することによって気密容器内
の圧力を制御して、この蒸気圧と高解離圧成分の解離圧
とを平衡させることで原料融液Ｙの組成を制御する。
そして上部容器２の上部より挿通された引上軸１２の下
端に種結晶を固定し、これを原料融液Ｙに浸漬して回転
させながら引き上げることによって単結晶Ｔの成長を行
う。なお、符号１３は観察窓、符号１４は液体Ｂ２Ｏ３
等の液体シール材１５を満たした軸シール部である。こ
の処理装置では、気密容器１の分割および再使用が可能
で、大口径単結晶インゴットの製造が容易に行えるとい
う利点を有する。FIG. 1 shows an example of a GaAs single crystal processing apparatus used in such a method. This processing apparatus is described in Japanese Patent No. 1490669, and an airtight container 1 is composed of an upper container 2 and a lower container 3, and is arranged inside an outer container 4.
A sealing material 5 is interposed at the joint between the lower container 3 and the lower container 3, and the lower container 3 is joined with an appropriate stress by a stress buffer device 7 provided on the lower shaft 6 of the lower container 3. A crucible 9 is placed inside the airtight container 1 supported by a susceptor 8, rotated by a susceptor lower shaft 8a, and rotated by a heater 10.
, 10, the entire airtight container 1 is heated. In addition, the upper container 2 is provided with a vapor pressure control section 11, and a heater 11a installed in this section controls the temperature of this section to the lowest and appropriate constant temperature in the airtight container 1, and controls the high dissociation pressure components. By condensing the solid only in this portion, the pressure within the airtight container is controlled, and the composition of the raw material melt Y is controlled by balancing this vapor pressure with the dissociation pressure of the high dissociation pressure component. A seed crystal is fixed to the lower end of a pulling shaft 12 inserted through the upper part of the upper container 2, and a single crystal T is grown by immersing the seed crystal in the raw material melt Y and pulling it up while rotating. In addition, the reference numeral 13 is an observation window, and the reference numeral 14 is a liquid B2O3.
This is a shaft seal portion filled with a liquid sealing material 15 such as. This processing apparatus has the advantage that the airtight container 1 can be divided and reused, and large-diameter single crystal ingots can be easily produced.
【０００４】ところで、このような処理装置において良
好な単結晶を生成するには、高純度の高解離圧成分ガス
雰囲気を気密性よく閉じ込めることが重要である。この
雰囲気ガスが不純であるとそれは直ちに原料融液に取り
込まれ、結晶の不純物濃度を高めて電気的特性を劣化さ
せる。そして、このような気密容器の接合部に用いられ
るシール材としては容器に対して破壊的でなく、工業用
装置として十分操作性に優れること、またシール材自身
が高純度であって汚染の原因にならないことが必要であ
る。従来、このようなシール材としてはＢ２Ｏ３やＧａ
のような液体シール材、あるいは可撓性カーボンのよう
な固体シール材が用いられていた。By the way, in order to produce a good single crystal in such a processing apparatus, it is important to confine a high-purity, high-dissociation-pressure component gas atmosphere with good airtightness. If this atmospheric gas is impure, it is immediately incorporated into the raw material melt, increasing the impurity concentration of the crystal and deteriorating its electrical characteristics. The sealing material used for the joints of such airtight containers must not be destructive to the container and have sufficient operability as industrial equipment, and the sealing material itself must be of high purity and free from sources of contamination. It is necessary not to become Conventionally, such sealing materials include B2O3 and Ga.
Liquid sealants such as , or solid sealants such as flexible carbon were used.
【０００５】[0005]
【発明が解決しようとする課題】しかしながら、このよ
うな処理装置の上部容器と下部容器との接合部に用いら
れているシール材としては、Ｂ２Ｏ３は純度の点では問
題はないが、気密容器を構成するｐＢＮやＡｌＮに対し
て濡れ性が強く、かつ凝固後の熱収縮率が大きいため、
これらの材料を破壊してしまう危険性を有している。ま
た、Ｇａは成分元素なので高純度物質であるといえるが
、常温では通常液体であるためにチャージの際の取り扱
いが不便であるのと、高解離圧成分ガスと反応してでき
る化合物の融点がＧａＡｓでは１２３８℃、ＧａＰでは
１４６５℃であって使用温度の約１０００℃以下では軟
化せずにシール性を劣化させるおそれがある。[Problems to be Solved by the Invention] However, as a sealing material used at the joint between the upper container and the lower container of such processing equipment, B2O3 has no problem in terms of purity, but it is difficult to maintain an airtight container. It has strong wettability to the constituent pBN and AlN, and has a high thermal shrinkage rate after solidification.
There is a risk of destroying these materials. In addition, Ga is a component element and can be said to be a highly pure substance, but it is usually liquid at room temperature, making it inconvenient to handle when charging, and the melting point of the compound formed by reacting with a high dissociation pressure component gas is low. The temperature is 1238° C. for GaAs and 1465° C. for GaP, which is the operating temperature of about 1000° C. or lower, which may not soften the sealing performance and deteriorate the sealing performance.
【０００６】さらに、固体シール材として用いられる可
撓性カーボンは操作性には優れているが、気密容器内の
雰囲気ガスに材料自体に起因する不純物が混入する可能
性を有する。さらにまた、可撓性カーボンをシール材と
して用いる場合には、気密容器の接合部に密封性を高め
るためにシール材を押さえる微細なエッジ部を形成する
必要がある。Furthermore, although flexible carbon used as a solid sealing material has excellent operability, there is a possibility that impurities caused by the material itself may be mixed into the atmospheric gas inside the airtight container. Furthermore, when flexible carbon is used as a sealing material, it is necessary to form a fine edge portion that presses the sealing material at the joint of the airtight container in order to improve the sealing performance.
【０００７】ところで、このような気密容器の材料とし
ては前述のように不純物の混入を防ぐためにｐＢＮやＡ
ｌＮ等のＩＩＩ族とＶ族の元素からなる物質のセラミッ
クス材が使用されるが、このようなセラミックスからな
る気密容器の接合では上部容器または下部容器の接合部
にエッジを形成するとこの部分が脆く壊れやすくなるた
め高価な気密容器の寿命を短くし、ひいては製品の価格
を高めてしまうという欠点がある。By the way, as mentioned above, the material for such an airtight container is pBN or A to prevent contamination with impurities.
Ceramic materials made of substances of group III and group V elements such as lN are used, but when joining airtight containers made of such ceramics, if an edge is formed at the joint of the upper or lower container, this part becomes brittle. This has the disadvantage of shortening the lifespan of expensive airtight containers because they become fragile, which in turn increases the price of the product.
【０００８】[0008]
【課題を解決するための手段】本発明は前記の課題を解
決するためになされたもので、請求項１の高解離圧化合
物半導体結晶処理装置におけるシール方法は、分割可能
な構成部材よりなる気密容器の内部に高解離圧化合物半
導体結晶の原料を保持し、高解離圧成分蒸気の蒸気圧を
制御して高解離圧化合物半導体を成長せしめる高解離圧
化合物半導体結晶処理装置における分割部のシール方法
において、気密容器を構成する構成部材の少なくとも一
の接合部にＩｎ（インジウム）よりなるシール材を介装
するとともに、この接合部にて接合される構成部材をシ
ール材を圧縮する方向に付勢しつつ高解離圧化合物半導
体結晶を成長せしめることを特徴とする。[Means for Solving the Problems] The present invention has been made to solve the above-mentioned problems, and a sealing method in a high dissociation pressure compound semiconductor crystal processing apparatus according to claim 1 provides an airtight sealing method using divisible structural members. A method for sealing a divided part in a high dissociation pressure compound semiconductor crystal processing apparatus that holds raw materials for a high dissociation pressure compound semiconductor crystal inside a container and grows a high dissociation pressure compound semiconductor by controlling the vapor pressure of the high dissociation pressure component vapor. A sealing material made of In (indium) is interposed in at least one joint of the structural members constituting the airtight container, and the structural members joined at this joint are urged in a direction that compresses the sealing material. It is characterized by growing a high dissociation pressure compound semiconductor crystal while
【０００９】また、請求項２の高解離圧化合物半導体結
晶処理装置におけるシール構造は、請求項１記載の高解
離圧化合物半導体結晶処理装置におけるシール方法に用
いられる高解離圧化合物半導体結晶処理装置におけるシ
ール構造であって、前記接合部にて接合される前記構成
部材の少なくとも一つには、前記シール材の移動を拘束
する凹部が形成されていることを特徴とする。Further, the sealing structure in the high dissociation pressure compound semiconductor crystal processing apparatus according to claim 2 is a seal structure in the high dissociation pressure compound semiconductor crystal processing apparatus used in the sealing method in the high dissociation pressure compound semiconductor crystal processing apparatus according to claim 1. The sealing structure is characterized in that at least one of the constituent members joined at the joint portion is formed with a recessed portion that restricts movement of the sealing material.
【００１０】さらに、請求項３の高解離圧化合物半導体
結晶処理装置におけるシール方法およびシール構造は、
シール材が介装される前記構成部材の接合部の、このシ
ール材よりも気密容器の外部側に、Ｉｎ（インジウム）
とは異なる組成の第二のシール材が介装されていること
を特徴とする。なお、この第二のシール材の材質として
は例えば可撓性を有するカーボン等が適当である。Furthermore, the sealing method and sealing structure in the high dissociation pressure compound semiconductor crystal processing apparatus according to claim 3,
In the joint portion of the structural members where the sealing material is interposed, In (indium) is placed on the outside of the airtight container from the sealing material.
A second sealing material having a composition different from that of the second sealing material is interposed. Note that, as the material of this second sealing material, for example, flexible carbon or the like is suitable.
【００１１】[0011]
【作用】本発明において、シール材に用いられるＩｎ（
インジウム）は常温では適度な可撓性を有する固体であ
って、気密容器を構成する構成部材の接合部にこのよう
なシール材を介装し、該接合部において接合される構成
部材を、シール材を圧縮する方向に付勢してシール材に
適正な応力を与えることによってシール材は潰されてこ
の部分を密封する。次に、気密容器の温度を上げるとＩ
ｎはその融点１５６℃で液体となり、前記応力によって
さらに潰されて薄い膜となり、気密性を増す。そして、
例えばＧａＡｓ単結晶の成長の場合には気密容器の温度
を上げてＡｓ蒸気圧を徐々に高めると、このＩｎ膜はそ
の容器内側の部分からＡｓを吸収してＩｎＡｓとなる。
この反応の容器外側への進行は温度が低い間は極めてゆ
っくりと起こる。ここでシール材のＩｎＡｓとなった部
分は膨張しようとするが、構成部材を前記方向に付勢し
て接合部に常に応力を付与しておくことにより、固体Ｉ
ｎＡｓは接合部の形状に従って変形して該接合部に係合
した形状となるので、気密性が損なわれるようなことは
ない。また、このシール材のＩｎＡｓとなった部分の気
密容器外部側には、Ａｓと反応していない液状のＩｎが
存在していて気密性を一層確実に確保することができる
。[Operation] In the present invention, In(
Indium (indium) is a solid with moderate flexibility at room temperature, and such a sealing material is inserted at the joint of the constituent members that make up the airtight container, and the constituent members joined at the joint are sealed. By applying appropriate stress to the sealing material by urging the material in a compressive direction, the sealing material is crushed and seals the area. Next, when the temperature of the airtight container is increased, I
n becomes a liquid at its melting point of 156° C., and is further crushed by the stress to form a thin film, increasing airtightness. and,
For example, in the case of growing a GaAs single crystal, when the temperature of an airtight container is raised to gradually increase the As vapor pressure, the In film absorbs As from the inner part of the container and becomes InAs. This reaction progresses to the outside of the vessel very slowly while the temperature is low. At this point, the InAs portion of the sealing material tries to expand, but by urging the constituent members in the above direction and constantly applying stress to the joint, the solid I
Since nAs deforms according to the shape of the joint and assumes a shape that engages with the joint, airtightness is not impaired. In addition, liquid In that has not reacted with As exists on the outside of the airtight container in the InAs portion of the sealing material, so that airtightness can be ensured even more reliably.
【００１２】次いで気密容器の温度がさらに７００〜１
０００℃に上昇し、ＩｎＡｓの融点９４３℃に極めて近
いか、あるいはそれ以上の温度になると反応は急速に進
行する。しかし、シール材のすべてのＩｎがＩｎＡｓに
なったとしても、この温度ではＩｎＡｓは可撓性を有す
る固体か、あるいは液体であり、いずれにしても構成部
材を前記方向に付勢することによって接合部の形状に従
った形状を保持していて、このため接合部のシール性が
劣化するようなことはない。こうして結晶成長が終了し
、気密容器が徐冷されるに伴い接合部の温度も下がって
シール材の温度が７００℃以下になるとＩｎＡｓは剛性
が高まって可撓性を失うことになる。しかしながら、こ
の時点ではシール材の形状は高温時に成形された接合部
に係合した形状のままであるので、実用上十分な気密性
が維持される。また、この段階では結晶成長はすでに終
わっているので、仮に気密性の劣化のために気密容器内
のＡｓ蒸気圧が低下したとしても成長された半導体結晶
の組成に対する影響は無視できるものとなる。Next, the temperature of the airtight container is further increased to 700-1
As the temperature increases to 000°C, which is very close to or even higher than the melting point of InAs, 943°C, the reaction proceeds rapidly. However, even if all the In in the sealing material becomes InAs, InAs is a flexible solid or liquid at this temperature, and in any case, the components can be joined by urging them in the above direction. The shape is maintained according to the shape of the joint, so the sealing performance of the joint does not deteriorate. When the crystal growth is thus completed and the airtight container is slowly cooled, the temperature of the joint also decreases and the temperature of the sealing material becomes 700° C. or less, and the InAs increases in rigidity and loses its flexibility. However, at this point, the shape of the sealing material remains in the shape that engaged with the joint formed at high temperature, so that practically sufficient airtightness is maintained. Furthermore, since the crystal growth has already finished at this stage, even if the As vapor pressure in the airtight container were to drop due to deterioration of airtightness, the effect on the composition of the grown semiconductor crystal would be negligible.
【００１３】ところで、結晶成長中でシール材が液体の
状態にあっては前記応力緩衝装置による付勢によってシ
ール材が押圧され、この押圧力によって液状のシール材
が接合部を移動して該接合部より逸脱してしまい、シー
ル性が失われてしまうおそれがある。そこで、これに対
してシール材を介装する気密容器構成部材の接合部にシ
ール材を配設する部位に沿って、該シール材の移動を拘
束する凹部を形成することにより、液状シール材が前記
押圧力によってこの凹部に圧入されてその移動が阻止さ
れ、シール材が接合部より逸脱するような事態を防止し
てシール性を維持することができる。また結晶成長前あ
るいは成長初期のシール材が個体の状態の時には前記応
力によってシール材が前記溝に圧入され、該溝に係合す
る形状に成形されるのでシール性をより一層向上させる
ことができ、さらにＩｎシール材が気密容器内のＡｓ蒸
気と反応して固体のＩｎＡｓとなった場合にもシール材
は該溝に係合した形状に固化し、このままの状態で結晶
成長終了にまで至るのでシール性をより確実に維持する
ことができる。By the way, when the sealing material is in a liquid state during crystal growth, the sealing material is pressed by the force exerted by the stress buffering device, and this pressing force causes the liquid sealing material to move through the joint, thereby damaging the joint. There is a risk that the seal may deviate from the part and the sealing performance may be lost. Therefore, by forming a recess that restricts the movement of the sealant along the joint portion of the airtight container component in which the sealant is disposed, a recess is formed to restrict the movement of the sealant. The pressing force presses the sealing material into the recess and prevents its movement, thereby preventing the sealant from coming off the joint and maintaining sealing performance. Furthermore, when the sealing material is in a solid state before crystal growth or in the initial stage of growth, the stress causes the sealing material to be press-fitted into the groove and is formed into a shape that engages with the groove, so that the sealing performance can be further improved. Furthermore, even if the In sealing material reacts with the As vapor in the airtight container and becomes solid InAs, the sealing material will solidify into a shape that engages with the groove, and the crystal growth will end in this state. Sealing performance can be maintained more reliably.
【００１４】さらにまた、シール材が介装される構成部
材の接合部の該シール材よりも気密容器の外部側に、例
えば可撓性を有するカーボン等のＩｎとは異なる組成の
第二のシール材を介装することにより、これだけでも接
合部は略過不足ない気密性を持つことになる。このため
気密容器内外の圧力差が大きくなったときでも結晶成長
中に液状となったＩｎシール材の移動が阻止されるため
、前述のような液状シール材が接合部から失われるよう
な事態をより確実に防止することができる。[0014] Furthermore, a second seal having a composition different from In, such as flexible carbon, is placed on the outside of the airtight container from the sealing material at the joint of the structural members in which the sealing material is interposed. By interposing the material, the joint will have almost the same airtightness. For this reason, even when the pressure difference between the inside and outside of the airtight container becomes large, the movement of the In sealant that has become liquid during crystal growth is prevented, thereby preventing the situation where the liquid sealant is lost from the joint as described above. This can be prevented more reliably.
【００１５】ここでシール材としてＩｎを使用した場合
には、このようなＩｎシール材は前記接合部の接合面に
あまりによく馴染む結果、接合部への押圧力が強すぎる
と引き上げ終了後も接合部がくっついて分割できなくな
るいう事態が生じるおそれがあり、このような事態とな
ると気密容器の破壊、または結晶の破壊といった新たな
問題につながることになる。ところがこのような事態も
、接合部に前記第二のシール材を介装することによって
解決することができる。即ち、Ｉｎシール材がまだＩｎ
Ａｓにならない流動性を有する段階では、前述のように
第二のシール材によって気密性が得られ、その一方でこ
の第二のシール材の存在によって、Ｉｎシール材に対す
る押圧力が減少される。次いでＩｎが反応してＩｎＡｓ
に変わる際の自然の膨張によって該接合部の気密性が向
上し、最終的かつ完全な気密性を得ることができる。
これより、Ｉｎが直接前記接合面に馴染んで接着されて
しまうといった事態を防ぐことができ、結果的に引上げ
終了後の前記トラブルを解決する事ができる。また、Ｉ
ｎシール材がこの第二のシール材より気密容器内部側に
配設されるため、第二のシール材による気密容器内の汚
染の危険性はなく、従って第二のシール材の材質はその
使用条件等によって広い範囲から選択することができる
。そしてＩｎシール材と、Ｉｎとは異なる組成の第二の
シール材とを二重に配置することにより、個々の使用条
件に応じてシール性の向上を図ることが可能となる。[0015] When In is used as the sealing material, such In sealing material blends very well with the joint surface of the joint, and as a result, if the pressing force on the joint is too strong, the joint will continue even after the pulling is completed. There is a risk that the parts will stick together and cannot be divided, and such a situation will lead to new problems such as destruction of the airtight container or destruction of the crystal. However, such a situation can also be solved by interposing the second sealing material in the joint. That is, the In seal material is still In.
At the stage where the material has fluidity that does not result in As, airtightness is obtained by the second sealing material as described above, and on the other hand, the presence of this second sealing material reduces the pressing force against the In sealing material. Then In reacts to form InAs
The natural expansion during the transition improves the airtightness of the joint, resulting in final and complete airtightness. This can prevent a situation where In directly adapts to the bonding surface and adheres to it, and as a result, the above-mentioned trouble after the pulling is completed can be solved. Also, I
Since the sealing material is placed inside the airtight container from the second sealing material, there is no risk of contamination inside the airtight container due to the second sealing material, and therefore the material of the second sealing material is It can be selected from a wide range depending on conditions etc. By arranging the In sealing material and the second sealing material having a composition different from In in duplicate, it is possible to improve the sealing performance according to individual usage conditions.
【００１６】[0016]
【実施例】以下に、本発明を図１に示した処理装置の上
部容器２と下部容器３との接合部に使用した場合の一実
施例を、図１ないし図５を用いて説明する。なお、図２
ないし図５においては、図中右側を気密容器１の内部側
とする。DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment in which the present invention is applied to a joint between an upper container 2 and a lower container 3 of the processing apparatus shown in FIG. 1 will be described below with reference to FIGS. 1 to 5. In addition, Figure 2
5 through 5, the right side in the figure is the inside of the airtight container 1.
【００１７】気密容器１は、外部容器４内に配置され、
天板付円筒状の上部容器２と有底円筒状の下部容器３か
ら構成されている。これら上部容器２と下部容器３の内
面および接合部には、ＩＩＩ族とＶ族元素からなるｐＢ
ＮやＡｌＮ等のセラミックスのうちバインダーを含まな
い、いわゆるＣＶＤ法によって形成されたものがコーテ
ィングされている。下部容器３の接合部には周方向に溝
３ａが形成されており、これに対して上部容器２の接合
部には周方向に、この溝３ａの深さより高い突条２ａが
形成されている。なお、下部容器３をその軸方向にさら
に２分割し、円筒状の中間容器と有底円筒状あるいはフ
ランジ状の下部容器として、気密容器１全体を３つの部
分で構成するようにしてもよい。この場合には、接合部
は上部容器と中間容器との接合部、および中間容器と下
部容器との接合部の２ヶ所となる。[0017] The airtight container 1 is placed inside the outer container 4,
It consists of a cylindrical upper container 2 with a top plate and a cylindrical lower container 3 with a bottom. The inner surfaces and joints of the upper container 2 and the lower container 3 contain pB, which is made of group III and group V elements.
The coating is made of ceramics such as N and AlN that do not contain a binder and are formed by a so-called CVD method. A groove 3a is formed in the circumferential direction at the joint part of the lower container 3, whereas a protrusion 2a is formed in the circumferential direction at the joint part of the upper container 2, which is higher than the depth of this groove 3a. . Note that the lower container 3 may be further divided into two parts in the axial direction to form a cylindrical intermediate container and a bottomed cylindrical or flange-shaped lower container, so that the entire airtight container 1 is composed of three parts. In this case, there are two joints: the joint between the upper container and the intermediate container, and the joint between the intermediate container and the lower container.
【００１８】この下部容器３は応力緩衝装置７を介して
押上げ下軸６に連結されており、また底部にはサセプタ
８の下軸８ａが挿通されていて、このサセプタ８上には
ルツボ９が配置されている。ここで、この応力緩衝装置
７は例えば押上げ下軸６に同心状に配設されたスプリン
グ等により、下部容器３を上部容器２側に、両者の接合
部に一定の応力が生じるように付勢する構造となってい
る。一方、上部容器２の上部には蒸気圧制御部１１が設
けられており、また上方からは引上軸１２が挿通されて
いる。なお、引上軸１２およびサセプタ８の下軸８ａの
気密容器１への挿通部にはＢ２Ｏ３等の液体シール材１
５を保持する軸シール部１４が設けられている。また、
この上部容器２には石英やサファイア製の観察窓１３が
挿通されている。This lower container 3 is connected to a push-up lower shaft 6 via a stress buffering device 7, and a lower shaft 8a of a susceptor 8 is inserted through the bottom, and a crucible 9 is placed on the susceptor 8. is located. Here, this stress buffering device 7 is configured to attach the lower container 3 to the upper container 2 side using, for example, a spring disposed concentrically on the lower push-up shaft 6 so that a certain stress is generated at the joint between the two. It has a strong structure. On the other hand, a vapor pressure control section 11 is provided in the upper part of the upper container 2, and a pulling shaft 12 is inserted from above. In addition, a liquid sealing material such as B2O3 is applied to the insertion portion of the pulling shaft 12 and the lower shaft 8a of the susceptor 8 into the airtight container 1.
A shaft seal portion 14 for holding the shaft 5 is provided. Also,
An observation window 13 made of quartz or sapphire is inserted into the upper container 2.
【００１９】そして、この気密容器１の上部容器２と下
部容器３との接合部には紐状のＩｎからなるシール材５
が無端状に連結され、下部容器３の接合部に形成された
溝３ａの幅方向略中央に配置されている。なお、この紐
状のＩｎシール材５を無端状にするには端部を重ねて押
し付けるだけでよい。A string-like sealing material 5 made of In is attached to the joint between the upper container 2 and the lower container 3 of the airtight container 1.
are connected in an endless manner and are arranged approximately at the center in the width direction of the groove 3a formed in the joint portion of the lower container 3. Note that in order to make the string-shaped In sealing material 5 endless, it is only necessary to press the ends together.
【００２０】このような構成の処理装置を用いて例えば
ＧａＡｓの単結晶の成長を行うには、まず下部容器３の
底部にＡｓ原料を、ルツボ９内にＧａ原料を、引上軸１
２下端部にＧａＡｓ種結晶をそれぞれ配置し、外部容器
４内を真空排気した後、押上げ下軸６を押し上げて下部
容器３を上部容器２に当接せしめ、さらに応力緩衝装置
７によって下部容器３を上部容器２側に付勢して気密容
器１を密封する。この時点ではＩｎシール材５は可撓性
を有する固体であり、前記応力緩衝装置７による付勢に
よって生じた応力により、図２に示すように上部容器２
の突条２ａと下部容器３の溝３ａとの間で潰されてこれ
ら両者の接合部をシールする。しかる後、ヒータ１０，
１０によって気密容器１を昇温するとＩｎシール材５は
その融点１５６℃で液体となるが、押上げ下軸６に設け
られた応力緩衝装置７によって下部容器３は常に上部容
器２側に付勢されているので、図３に示すように液状の
Ｉｎシール材５はさらに潰れて薄い膜となる。To grow, for example, a single crystal of GaAs using a processing apparatus having such a configuration, first, an As raw material is placed in the bottom of the lower container 3, a Ga raw material is placed in the crucible 9, and the pulling shaft 1 is
After evacuating the inside of the outer container 4, the lower push-up shaft 6 is pushed up to bring the lower container 3 into contact with the upper container 2, and the stress buffer device 7 is used to lower the lower container 3. 3 toward the upper container 2 side to seal the airtight container 1. At this point, the In sealing material 5 is a flexible solid, and due to the stress generated by the biasing force of the stress buffering device 7, as shown in FIG.
is crushed between the protrusion 2a and the groove 3a of the lower container 3 to seal the joint between them. After that, the heater 10,
When the temperature of the airtight container 1 is increased by 10, the In sealing material 5 becomes liquid at its melting point of 156° C., but the lower container 3 is always urged toward the upper container 2 by the stress buffer device 7 provided on the lower push-up shaft 6. Therefore, as shown in FIG. 3, the liquid In sealing material 5 is further crushed into a thin film.
【００２１】さらに気密容器１を徐々に加熱し、ルツボ
９内Ｇａ原料をＧａＡｓの融点（１２３８℃）以上の温
度、例えば１３００℃程度に、また気密容器１の底部の
温度を５５０〜６５０℃に上昇させると気密容器１内の
Ａｓ蒸気圧が高まり、ルツボ９内のＧａと反応してＧａ
Ａｓ原料融液Ｙが合成される。この合成に当たって、Ａ
ｓ蒸気圧が徐々に高まると、液状となったＩｎシール材
５は図４に示すように、その気密容器１内部側の部分５
ａからＡｓを吸収してこの温度では固体であるＩｎＡｓ
となる。この反応の気密容器１外部側への進行は既に反
応してできた固体のＩｎＡｓの薄い膜中の拡散に支配さ
れて起こるので、温度が低い間は極めてゆっくりと起こ
る。ここで、シール材５のＩｎＡｓとなった部分５ａは
膨張しようとするが、前述のように応力緩衝装置７によ
って下部容器３が上部容器２側に付勢されて両者の接合
部には常に応力が付加されているため、固体となったＩ
ｎＡｓ部分５はこの接合部の形状に従って変形し、該接
合部に係合した形状に成形されてそのシール性を維持す
る。また、この固体ＩｎＡｓ部分５ａの気密容器１外部
側にはシール材５の液状部分５ｂが存在するのでシール
性が劣化することはない。なお、この合成の最中は外部
容器４内に不活性ガスを導入し、気密容器１内外の圧力
バランスをとる。Further, the airtight container 1 is gradually heated to bring the Ga raw material in the crucible 9 to a temperature above the melting point of GaAs (1238°C), for example, about 1300°C, and the temperature at the bottom of the airtight container 1 to 550 to 650°C. As it rises, the As vapor pressure in the airtight container 1 increases, reacts with Ga in the crucible 9, and Ga
As raw material melt Y is synthesized. In this synthesis, A
s As the vapor pressure gradually increases, the liquid In sealing material 5 melts into the inner part 5 of the airtight container 1, as shown in FIG.
InAs absorbs As from a and is solid at this temperature.
becomes. Since this reaction progresses to the outside of the airtight container 1, it occurs under the control of diffusion in the thin film of solid InAs that has already been reacted, and therefore occurs extremely slowly while the temperature is low. Here, the portion 5a of the sealing material 5 that has become InAs tries to expand, but as mentioned above, the lower container 3 is urged toward the upper container 2 by the stress buffering device 7, and the joint between the two is constantly stressed. I becomes a solid because of the addition of
The nAs portion 5 deforms according to the shape of this joint, is molded into a shape that engages with the joint, and maintains its sealing properties. Moreover, since the liquid portion 5b of the sealing material 5 exists on the outside of the airtight container 1 of the solid InAs portion 5a, the sealing performance is not deteriorated. Note that during this synthesis, an inert gas is introduced into the external container 4 to balance the pressure inside and outside the airtight container 1.
【００２２】こうしてＧａＡｓ原料融液Ｙが合成された
なら引上軸１２を降下させてその先端部に取り付けられ
た種結晶を原料融液Ｙに浸漬し、しかる後、引上軸１２
を回転しつつ観察窓１３よりその成長状態を観察しなが
ら単結晶Ｔを引上げる。また、この時にはＡｓ蒸気圧制
御部１１の温度を気密容器１の内部で最も低い一定温度
（例えば６１５℃）に保ち、ここにＡｓ蒸気を凝縮させ
て固化せしめることによって気密容器１内のＡｓ蒸気圧
を制御する。ここで、この成長操作に移る時にはシール
材５は７００〜１０００℃の温度下に置かれる。この温
度はＩｎＡｓの融点９４３℃に極めて近いか、あるいは
それ以上の温度であり、ＩｎがＡｓを吸収してＩｎＡｓ
になる反応は急速に進行するが、図５に示すようにＩｎ
シール材５がすべてＩｎＡｓ部分５ａになってもこの温
度ではＩｎＡｓは可撓性を有する固体か液体であり、い
ずれにしても前記応力緩衝装置７によって生じた応力に
より、接合部に従った形状になっていてシール材として
十分機能する。After the GaAs raw material melt Y has been synthesized in this way, the pulling shaft 12 is lowered and the seed crystal attached to its tip is immersed in the raw material melt Y.
The single crystal T is pulled up while rotating and observing its growth state through the observation window 13. At this time, the temperature of the As vapor pressure control unit 11 is maintained at the lowest constant temperature (for example, 615° C.) inside the airtight container 1, and the As vapor inside the airtight container 1 is condensed and solidified. Control pressure. Here, when moving on to this growth operation, the sealing material 5 is placed at a temperature of 700 to 1000°C. This temperature is extremely close to or higher than the melting point of InAs, 943°C, and InAs absorbs As and becomes InAs.
The reaction proceeds rapidly, but as shown in Figure 5, In
Even if the sealing material 5 is entirely InAs portion 5a, InAs is a flexible solid or liquid at this temperature, and in any case, due to the stress generated by the stress buffer device 7, the shape conforms to the joint. It functions well as a sealing material.
【００２３】最後に単結晶Ｔの成長が終わると気密容器
１は徐冷される。そしてこれに伴って接合部の温度も下
がって７００℃以下になると、すべてがＩｎＡｓ部分５
ａとなったシール材５は剛性が高まり可撓性が失われる
が、シール材５は前述のように接合部に係合した形状に
成形されており、また応力緩衝装置７によって付勢され
た下部容器３により上部容器２側に押圧されるため、実
用上十分なシール性を保つことができる。また、仮にこ
の段階でシール性が劣化してＡｓ蒸気圧が十分でなくな
ったとしても、単結晶の成長は既に終了しているので結
晶の組成に対する影響は無視することができる。Finally, when the growth of the single crystal T is finished, the airtight container 1 is slowly cooled. When the temperature of the junction decreases to below 700°C, all the InAs parts 5
Although the sealing material 5 that has become a increases in rigidity and loses its flexibility, the sealing material 5 is formed into a shape that engages with the joint as described above, and is also biased by the stress buffer device 7. Since it is pressed against the upper container 2 side by the lower container 3, practically sufficient sealing performance can be maintained. Furthermore, even if the sealing performance deteriorates and the As vapor pressure becomes insufficient at this stage, the effect on the composition of the crystal can be ignored since the growth of the single crystal has already been completed.
【００２４】以上説明したように、Ｉｎよりなるシール
材５は常温下の気密容器１の構成段階では可撓性を有す
る固体であり、気密容器１を加熱してＩｎの融点を超え
た時点で液体となり、さらに原料融液Ｙの合成および単
結晶Ｔの成長段階では高解離圧成分ガスと反応して再び
可撓性を持つ固体となる。そして結晶成長が終了して装
置が徐冷されると高解離圧成分と反応したシール材５は
固化して可撓性を失うが、高温下において接合部に係合
した形状に成形されているのでシール性は維持すること
ができる。As explained above, the sealing material 5 made of In is a flexible solid when the airtight container 1 is constructed at room temperature, and when the airtight container 1 is heated to exceed the melting point of In. It becomes a liquid, and then reacts with the high dissociation pressure component gas during the synthesis of the raw material melt Y and the growth stage of the single crystal T, and becomes a flexible solid again. When the crystal growth is finished and the device is slowly cooled, the sealing material 5 that has reacted with the high dissociation pressure component solidifies and loses its flexibility, but is still formed into a shape that engages the joint at high temperatures. Therefore, the sealing performance can be maintained.
【００２５】また、結晶成長のすべての段階を通じて応
力緩衝装置７によって下部容器３がシール材５を圧縮す
る方向、すなわち上部容器２側に付勢されており、これ
によって上部容器２と下部容器３との接合部に介装され
るシール材５には常に一定の応力が作用する。このため
、シール材５が固体状態にある時にはこれを押圧してシ
ール性を確保し、また気密容器１の昇温に伴ってシール
材５が液化した際にはさらにこれを押圧して薄膜状とし
、接合部に間隙が生じることを防いでシール性を維持す
る。さらに結晶成長の進行に伴ってシール材５を構成す
るＩｎが高解離圧成分と反応して固化する際にも、前記
応力が作用しているためにシール材５は前記接合部に係
合した形状に固化・成形され、その上この段階から結晶
成長が終了して気密容器１が徐冷されるに至るまでも応
力緩衝装置７による付勢によって下部容器３がシール材
５を押圧してシール性を保持する。Further, throughout all stages of crystal growth, the lower container 3 is biased by the stress buffering device 7 in a direction that compresses the sealing material 5, that is, toward the upper container 2, and as a result, the upper container 2 and the lower container 3 A constant stress is always applied to the sealing material 5 interposed at the joint portion. Therefore, when the sealing material 5 is in a solid state, it is pressed to ensure sealing performance, and when the sealing material 5 liquefies as the temperature of the airtight container 1 increases, it is further pressed to form a thin film. This prevents gaps from forming at the joint and maintains sealing performance. Furthermore, as the crystal growth progresses, when the In that constitutes the sealing material 5 reacts with the high dissociation pressure component and solidifies, the stress acts, so that the sealing material 5 engages with the joint. The lower container 3 presses the sealing material 5 due to the force exerted by the stress buffer 7 until the crystal growth ends and the airtight container 1 is slowly cooled. Retain your sexuality.
【００２６】このように、本発明によれば結晶成長の全
段階でＩｎシール材がその状態を変化しつつも応力を受
けて変形し、その状態に適した形態で接合部をシールす
るため、一連の結晶成長段階すべてを通じて安定的かつ
高いシール性を維持することができる。特に、原料融液
生成から結晶成長時の高温下においてシール材が液化し
ても気密容器の構成部材が常にシール材を圧縮する方向
に付勢されており、このため接合部に間隙を生じてシー
ル性を失うようなことがないので、気密容器１内の高解
離圧成分ガスの蒸気圧を正確に制御して当初の設定通り
の半導体結晶を成長させることが可能である。また、全
段階を通じてのシール性の高さから、気密容器内に混入
する不純物の濃度を極めて低く抑えることができ、この
ため高純度で電気的特性等の良好な半導体結晶を得るこ
とが可能である。また、ＩｎおよびＩｎと高解離圧成分
ガスの反応物は常温では固体であるから、単結晶の成長
前に接合部に介装する際には紐状に形成されたＩｎシー
ル材を配置すればよく、また成長後に再び固化したシー
ル材を除去する場合でも、接合部から容易に剥離するの
で気密容器を破損することがなく、取り扱いが非常に簡
単になる。さらに本発明ではシール材をＩｎに置き換え
ただけであり、装置そのものは従来のものを流用するこ
とができるから、その実施が容易であるという利点を有
する。As described above, according to the present invention, the In sealing material changes its state during all stages of crystal growth, deforms under stress, and seals the joint in a form suitable for the state. Stable and high sealing performance can be maintained throughout a series of crystal growth stages. In particular, even if the sealing material liquefies at high temperatures during the generation of raw material melt and crystal growth, the constituent members of the airtight container are always biased in a direction that compresses the sealing material, which creates gaps at the joints. Since there is no loss of sealing performance, it is possible to accurately control the vapor pressure of the high dissociation pressure component gas in the airtight container 1 and grow the semiconductor crystal as originally set. In addition, due to the high sealing performance throughout all stages, the concentration of impurities that enter the airtight container can be kept extremely low, making it possible to obtain semiconductor crystals with high purity and good electrical properties. be. In addition, since In and the reaction product of In and high dissociation pressure component gas are solid at room temperature, it is necessary to place an In sealing material formed in a string shape when interposing it at the joint before growing the single crystal. Moreover, even when the sealing material that has solidified again after growth is removed, it is easily peeled off from the joint, so the airtight container is not damaged, and handling becomes very easy. Furthermore, in the present invention, the sealing material is simply replaced with In, and since the conventional device itself can be used, it has the advantage of being easy to implement.
【００２７】ところで、本実施例では気密容器１の接合
部において上部容器２に突条２ａを、下部容器３に溝３
ａをそれぞれ形成してこの溝３ａにＩｎシール材５を配
置したが、図６および図７に示すように気密容器の接合
部にこのような突条や溝がなくても構わない。この場合
、Ｉｎシール材５は図６に示すように上部容器２と下部
容器３との接合部の互いに対向する端面の略中央に配置
され、応力緩衝装置７による付勢によって図７に示すよ
うに潰されて接合部をシールする。その後の過程は前記
実施例と同様であり、結晶成長のすべての段階で十分な
シール性を発揮する。By the way, in this embodiment, at the joint of the airtight container 1, the upper container 2 is provided with a protrusion 2a, and the lower container 3 is provided with a groove 3.
Although the In sealing material 5 is arranged in the grooves 3a by forming grooves 3a, it is not necessary for the joint portion of the airtight container to have such protrusions or grooves, as shown in FIGS. 6 and 7. In this case, the In sealing material 5 is placed approximately at the center of the opposing end surfaces of the joint between the upper container 2 and the lower container 3, as shown in FIG. crushed to seal the joint. The subsequent process is similar to that of the previous example, and sufficient sealing performance is exhibited at all stages of crystal growth.
【００２８】また前記実施例では本発明を気密容器１を
構成する上部容器２と下部容器３の接合部に使用したが
、これ以外の気密容器１の接合部に用いても構わない。
例えば図８はこのＩｎシール材５を上部容器２と観察窓
１３との接合部に使用した場合の一実施例を示す、観察
窓１３の挿通部の拡大図である。この実施例では観察窓
１３の中途部に円環状の凸部１３ａが形成されており、
また上部容器２の観察窓１３が挿通される部分には筒状
の保持部２ｂが形成されていて、この凸部１３ａの下端
面と保持部２ｂの上端面との間にＩｎシール材５が介装
されている。一方、観察窓１３の上端部は外部容器４に
設けられた筒状の凸部１６を貫通して外部に露出してお
り、この凸部１６の上端より気密容器１内での結晶の成
長状態を目視によって観察することができる。また、こ
の観察窓１３の上端側には外周にＯリング１７が嵌装さ
れた円筒状のシール部１８が設けられていて、このＯリ
ング１７が前記凸部１６の内面に摺接することにより、
この部分のシール性が保持される。さらにこのシール部
１８の上部にはコイルスプリング１９が観察窓１３に同
軸的に緩挿されており、このコイルスプリング１９の下
端は前記シール部１８の上端面に当接せしめられている
とともに、その上端は前記凸部１６の上端に螺嵌された
穴付きの袋ナット２０の裏面に当接せしめられている。
そして、このコイルスプリング１９によって観察窓１３
は下向きに付勢されており、これによって上部容器２の
保持部２ｂと観察窓１３の凸部１３ａとの間に介装され
たＩｎシール材５には該凸部１３ａを介して常に一定の
応力が与えられている。すなわち本実施例では、前記凸
部１６、Ｏリング１７、シール部１８、コイルスプリン
グ１９、および袋ナット２０等により観察窓応力付与機
構が構成されている。Further, in the embodiment described above, the present invention was used at the joint between the upper container 2 and the lower container 3 constituting the airtight container 1, but it may be used at other joints of the airtight container 1. For example, FIG. 8 is an enlarged view of the insertion portion of the observation window 13, showing an example in which the In sealing material 5 is used at the joint between the upper container 2 and the observation window 13. In this embodiment, an annular convex portion 13a is formed in the middle of the observation window 13,
Further, a cylindrical holding portion 2b is formed in the portion of the upper container 2 through which the observation window 13 is inserted, and an In sealing material 5 is placed between the lower end surface of the convex portion 13a and the upper end surface of the holding portion 2b. It has been intervened. On the other hand, the upper end of the observation window 13 passes through a cylindrical protrusion 16 provided on the outer container 4 and is exposed to the outside, and the upper end of the protrusion 16 allows the state of crystal growth within the airtight container 1 to be observed. can be observed visually. Further, a cylindrical seal portion 18 having an O-ring 17 fitted around the outer periphery is provided on the upper end side of the observation window 13, and as this O-ring 17 comes into sliding contact with the inner surface of the convex portion 16,
The sealing properties of this part are maintained. Further, a coil spring 19 is coaxially loosely inserted into the observation window 13 in the upper part of the seal part 18, and the lower end of this coil spring 19 is brought into contact with the upper end surface of the seal part 18, and its lower end is brought into contact with the upper end surface of the seal part 18. The upper end is brought into contact with the back surface of a cap nut 20 with a hole screwed into the upper end of the convex portion 16. The coil spring 19 allows the observation window 13 to
is biased downward, and as a result, the In sealing material 5 interposed between the holding part 2b of the upper container 2 and the convex part 13a of the observation window 13 is always supplied with a constant amount of air through the convex part 13a. Stress is applied. That is, in this embodiment, the observation window stress applying mechanism is constituted by the convex portion 16, the O-ring 17, the seal portion 18, the coil spring 19, the cap nut 20, and the like.
【００２９】このような構成によれば、気密容器１を構
成する上部容器２と観察窓１３との接合部にはＩｎシー
ル材５が介装され、かつコイルスプリング１９によって
観察窓１３の凸部１３ａが上部容器２の保持部２ｂ側に
向かって付勢されてＩｎシール材５に一定の応力が作用
しているため、前記実施例と同様の効果を得ることがで
きる。すなわち、結晶成長前および成長初期の段階では
Ｉｎシール材５は可撓性を有する固体であって前記凸部
１３ａに押圧されてこの接合部をシールし、原料融液生
成から結晶成長段階においては液化して膜状となって該
接合部をシールし、さらに結晶成長終了後から徐冷の段
階においては気密容器１内の高解離圧成分と反応し、か
つ前記コイルスプリング１９による付勢によって該接合
部に係合した形状の固体となってこの接合部のシール性
を保持することができる。従って結晶成長の全段階を通
して良好なシール性を維持することが可能であり、電気
的性能等に優れた結晶を安定的に成長せしめることがで
きる。According to this configuration, the In sealing material 5 is interposed at the joint between the upper container 2 and the observation window 13 constituting the airtight container 1, and the convex portion of the observation window 13 is held by the coil spring 19. 13a is urged toward the holding portion 2b of the upper container 2, and a certain stress is applied to the In sealing material 5, so that the same effect as in the embodiment described above can be obtained. That is, before crystal growth and at the initial stage of growth, the In sealing material 5 is a flexible solid and is pressed against the convex portion 13a to seal this joint, and from the raw material melt generation to the crystal growth stage. It liquefies into a film form and seals the joint, and further reacts with the high dissociation pressure component in the airtight container 1 during the slow cooling stage after the completion of crystal growth, and is biased by the coil spring 19. It becomes a solid shape that engages with the joint and can maintain the sealing properties of this joint. Therefore, it is possible to maintain good sealing properties throughout all stages of crystal growth, and it is possible to stably grow crystals with excellent electrical performance and the like.
【００３０】ところで前述したように、ＧａＡｓの原料
融液の合成に伴って気密容器１を昇温させると上部容器
２と下部容器３との接合部に介装されたＩｎシール材５
は溶融して液状となり、流動性を有することになる。し
かし、この間もＩｎシール材５は応力緩衝装置７による
付勢によって押圧力を受けており、この結果液化して流
動性を持ったシール材５は前記押圧力によって押し出さ
れて接合部より逸脱してしまい、接合部のシール性が失
われてしまうおそれがある。そこで、このような場合に
は該接合部のシール構造を、シール材５の移動を拘束す
るような構造とすることが好ましい。図９ないし図１２
は、このような事情を鑑みてなされた本発明のシール構
造の一実施例を示す上部容器２と下部容器３の接合部の
拡大図である。なおこれらの図において、図２ないし図
５に示した実施例と同じ部分には同一の符号を配して説
明を簡略化するものとし、また図中右側を気密容器１の
内部側とする。By the way, as mentioned above, when the temperature of the airtight container 1 is increased during the synthesis of the GaAs raw material melt, the In sealing material 5 interposed at the joint between the upper container 2 and the lower container 3 is heated.
is melted to become liquid and has fluidity. However, even during this time, the In sealing material 5 is being subjected to a pressing force by the stress buffering device 7, and as a result, the sealing material 5, which has liquefied and has fluidity, is pushed out by the pressing force and deviates from the joint. There is a risk that the sealing properties of the joint may be lost. Therefore, in such a case, it is preferable that the sealing structure of the joint is configured to restrict the movement of the sealing material 5. Figures 9 to 12
1 is an enlarged view of a joint between an upper container 2 and a lower container 3, showing an embodiment of the seal structure of the present invention, which was made in view of the above circumstances. In these figures, the same parts as those in the embodiment shown in FIGS. 2 to 5 are given the same reference numerals to simplify the explanation, and the right side in the figures is the inside of the airtight container 1.
【００３１】本実施例では、下部容器３の上部容器２と
の接合部に形成された溝３ａの底面の幅方向中央に、下
部容器３の周方向に沿ってさらに断面Ｖ字型の凹溝３ｂ
が形成されていることを特徴とするものである。以下、
このようなシール構造を有する高解離圧化合物半導体処
理装置においてＩｎシール材５を用いてＧａＡｓ単結晶
を成長させる場合について説明する。まず前記実施例同
様、図９に示すように紐状のＩｎシール材５を前記凹溝
３ｂ上に配置して気密容器１を構成する。この際、前記
実施例と同様に応力緩衝装置７によって下部容器３を上
部容器２側に付勢することにより、シール材５は押圧さ
れて上部容器２と下部容器３との接合部をシールする。
そしてこの時、押圧されたシール材５の一部は図１０に
示すように凹溝３ｂ内に圧入されて該凹溝３ｂに係合し
た形状になる。In this embodiment, a concave groove having a V-shaped cross section is further formed along the circumferential direction of the lower container 3 in the widthwise center of the bottom surface of the groove 3a formed at the joint of the lower container 3 with the upper container 2. 3b
It is characterized by the formation of below,
A case will be described in which a GaAs single crystal is grown using the In seal material 5 in a high dissociation pressure compound semiconductor processing apparatus having such a seal structure. First, as in the embodiment described above, as shown in FIG. 9, a string-shaped In sealing material 5 is placed on the groove 3b to form an airtight container 1. At this time, by urging the lower container 3 toward the upper container 2 side by the stress buffering device 7 as in the previous embodiment, the sealing material 5 is pressed and seals the joint between the upper container 2 and the lower container 3. . At this time, a part of the pressed sealing material 5 is press-fitted into the groove 3b and has a shape engaged with the groove 3b, as shown in FIG.
【００３２】次いで気密容器１を昇温させて原料融液を
合成する段階では、Ｉｎシール材５はその融点１５６℃
を超えると溶融して液状となり、前記応力緩衝装置７に
よる付勢によってさらに押し潰されて薄膜状になって該
接合部をシールする。この時液化して流動性を有するに
至ったシール材５は下部容器３に押圧されて接合部を溝
３ａの幅方向に移動しようとするが、前記凹溝３ｂ内に
圧入された部分は図１０に示した状態のまま液化して該
凹溝３ｂ内に保持されるため、その移動は阻止される。
さらに原料融液の合成が進行して気密容器１内が高解離
圧成分であるＡｓ蒸気で満たされると、Ｉｎシール材５
は図１１に示すようにその気密容器１内部側の部分５ａ
から反応してＩｎＡｓとなり、固化して該接合部に係合
する形状に成形される。この時、前記凹溝３ｂ内に保持
されたＩｎシール材５もこの凹溝３ｂに係合した形状に
固化・成形される。そして結晶成長が終了して気密容器
１が徐冷されると、これに伴ってＩｎＡｓとなったシー
ル材５も冷却されて高温時の可撓性を失うが、図１２に
示すように接合部および凹溝３ｂに係合する形状に成形
され、かつ応力緩衝装置７による付勢によって押圧され
ているためにシール性が劣化することはない。また、こ
の段階では結晶成長は既に終了しているので、万一シー
ル性が損なわれても結晶組成への影響は最小限に抑えら
れる。Next, in the step of raising the temperature of the airtight container 1 to synthesize the raw material melt, the In sealing material 5 has a melting point of 156°C.
When the temperature exceeds the limit, it melts into a liquid state, and is further crushed by the force applied by the stress buffering device 7 to become a thin film to seal the joint. At this time, the sealing material 5, which has become liquefied and has fluidity, is pressed by the lower container 3 and tries to move the joint part in the width direction of the groove 3a, but the part press-fitted into the groove 3b is Since it is liquefied and held in the groove 3b in the state shown in 10, its movement is prevented. When the synthesis of the raw material melt further progresses and the inside of the airtight container 1 is filled with As vapor, which is a high dissociation pressure component, the In sealing material 5
is the inner part 5a of the airtight container 1 as shown in FIG.
It reacts to become InAs, which solidifies and is molded into a shape that engages with the joint. At this time, the In sealing material 5 held in the groove 3b is also solidified and molded into a shape that engages with the groove 3b. When the crystal growth is finished and the airtight container 1 is slowly cooled, the sealing material 5, which has become InAs, is also cooled and loses its flexibility at high temperatures, but as shown in FIG. Since it is molded into a shape that engages with the concave groove 3b and is pressed by the stress buffering device 7, the sealing performance will not deteriorate. Furthermore, since crystal growth has already been completed at this stage, even if the sealing performance is impaired, the effect on the crystal composition can be minimized.
【００３３】このように本実施例では、図１０および図
１１に示したようなシール材５が液状の場合には前記凹
溝３ｂによって液状シール材５が保持されてその移動が
拘束されるため、応力緩衝装置７の付勢による押圧力に
よってシール材５が該接合部から逸脱してシール性が損
なわれる様な事態を未然に防止することができる。また
、図９や図１２に示したようなシール材５が固化した状
態ではシール材５はこの凹溝３ｂにも係合する形状とな
るため、気密容器１の内部と外部とがより確実に隔絶さ
れ、シール性の向上を図ることができるという利点を有
する。なお、本実施例では下部容器３の溝３ａの底面に
Ｖ字型断面の凹溝３ｂを一条形成して液状のＩｎシール
材５の移動を拘束したが、これ以外にも例えば下部容器
３の接合部の周方向に延びる比較的浅い溝を径方向に多
数形成してもよい。また、前記接合部の接合面に粗面を
形成するような構成としてもよい。As described above, in this embodiment, when the sealing material 5 is in a liquid state as shown in FIGS. 10 and 11, the liquid sealing material 5 is held by the groove 3b and its movement is restricted. It is possible to prevent a situation in which the sealing material 5 deviates from the joint portion due to the pressing force caused by the biasing force of the stress buffering device 7 and the sealing performance is impaired. In addition, in the solidified state of the sealing material 5 as shown in FIGS. 9 and 12, the sealing material 5 has a shape that also engages with this groove 3b, so that the inside and outside of the airtight container 1 are more securely connected. It has the advantage of being isolated and improving sealing performance. In this embodiment, a groove 3b having a V-shaped cross section is formed on the bottom surface of the groove 3a of the lower container 3 to restrain the movement of the liquid In sealant 5. A large number of relatively shallow grooves extending in the circumferential direction of the joint portion may be formed in the radial direction. Further, a structure may be adopted in which a rough surface is formed on the joint surface of the joint portion.
【００３４】次に、図１３ないし図１６は本発明のその
他の実施例を示すものであり、図２ないし図５および図
９ないし図１２に示した実施例と同じ部分には同一の符
号を配してある。この実施例では図９ないし図１２に示
した実施例において、接合部の前記Ｖ字型断面の凹溝３
ｂの気密容器１外部側に、可撓性を有するカーボンより
なるガスケット状の第二のシール材２１が介装されてい
ることを特徴とするものである。このような構成とする
ことにより、気密容器１の昇温に伴って液化したＩｎシ
ール材５は溝３ｂの中に保持されるとともに前記応力緩
衝装置７による付勢によって押圧され、かつ気密容器１
は第二のシール材２１で略気密に保持されるので、気密
容器１の内外に圧力差があっても、Ｉｎシール材５が前
記外部側から接合部より逸脱してしまうことはなく、接
合部のシール性を確実に維持することが可能となる。ま
た本実施例では、Ｉｎシール材５が第二のシール材２１
より気密容器１の内部側に配設されるため、カーボンよ
りなる第二のシール材２１によって気密容器１内部のＡ
ｓ雰囲気が汚染されるような危険性はない。従って本実
施例では第二のシール材２１としてカーボンを用いたが
、これ以外の材質をその使用条件等によって広い範囲か
ら選択することもでき、個々の使用条件に適した材質を
使用することによって効果的に接合部のシール性の向上
を図ることが可能であるという利点を有する。さらに本
実施例では、第二のシール材２１を介装することによっ
て、Ｉｎシール材５に対する押圧力を結果的に減らすこ
とができるので、このようなＩｎシール材５が気密容器
１の構成部材の接合面に過度に馴染んでしまうことを抑
えることができ、結晶引上げ終了後の気密容器１の分割
やシール材５の剥離に有利となる。Next, FIGS. 13 to 16 show other embodiments of the present invention, and the same parts as in the embodiments shown in FIGS. 2 to 5 and 9 to 12 are designated by the same reference numerals. It is arranged. In this embodiment, in the embodiment shown in FIGS. 9 to 12, the concave groove 3 of the V-shaped cross section of the joint part is
A gasket-shaped second sealing material 21 made of flexible carbon is interposed on the outside of the airtight container 1 of b. With this configuration, the In sealing material 5 liquefied as the temperature of the airtight container 1 rises is held in the groove 3b and is pressed by the stress buffering device 7, and
is held substantially airtight by the second sealing material 21, so even if there is a pressure difference between the inside and outside of the airtight container 1, the In sealing material 5 will not deviate from the joint from the outside side, and the joining will be completed. This makes it possible to reliably maintain the sealing properties of the parts. Further, in this embodiment, the In sealing material 5 is the second sealing material 21.
Since it is disposed closer to the inside of the airtight container 1, the second sealing material 21 made of carbon seals the inside of the airtight container 1.
s There is no risk of contamination of the atmosphere. Therefore, in this embodiment, carbon is used as the second sealing material 21, but other materials may be selected from a wide range depending on the usage conditions, etc., and by using a material suitable for each usage condition, This has the advantage that it is possible to effectively improve the sealing performance of the joint. Furthermore, in this embodiment, by interposing the second sealing material 21, the pressing force on the In sealing material 5 can be reduced as a result, so that such In sealing material 5 can be used as a component of the airtight container 1. It is possible to suppress excessive adhesion to the joint surfaces of the crystals, which is advantageous for dividing the airtight container 1 and peeling off the sealing material 5 after crystal pulling is completed.
【００３５】なお、前述したすべての実施例ではＧａＡ
ｓの結晶成長の場合を例として示したが、本発明はこの
他の高解離圧化合物半導体、例えばＧａＰの単結晶成長
のような場合にも同じように実施することができる。こ
の場合、Ｉｎシール材はＰ雰囲気によってＩｎＰとなる
が、このＩｎＰの融点は１０６２℃であるので７００〜
１０００℃のＧａＰ単結晶の成長温度で良好なシール材
として機能する。さらに、これらの実施例では単結晶の
引上げによる処理装置に本発明を用いた場合について説
明したが、気密容器中に高解離圧成分ガスを封じ込める
他の処理装置、例えば図１７に示すような縦型ブリッジ
マン結晶成長装置や単結晶熱処理装置にも応用すること
ができる。なお、図１７において図１に示した結晶処理
装置と同じ部分には同一の符号を配して説明を省略する
。また、符号２２はｐＢＮルツボ９を支持する支持台で
あり、符号Ｓは種結晶である。[0035] In all the above-mentioned embodiments, GaA
Although the case of crystal growth of s is shown as an example, the present invention can be implemented in the same way in the case of single crystal growth of other high dissociation pressure compound semiconductors, for example, GaP. In this case, the In sealing material becomes InP due to the P atmosphere, but since the melting point of this InP is 1062°C,
It functions as a good sealing material at the GaP single crystal growth temperature of 1000°C. Further, in these Examples, the case where the present invention is applied to a processing apparatus for pulling a single crystal has been described, but it can also be applied to other processing apparatuses that confine a high dissociation pressure component gas in an airtight container, such as the vertical one shown in FIG. It can also be applied to Bridgman type crystal growth equipment and single crystal heat treatment equipment. Note that in FIG. 17, the same parts as those in the crystal processing apparatus shown in FIG. Further, the reference numeral 22 is a support stand that supports the pBN crucible 9, and the reference numeral S is a seed crystal.
【００３６】次に、図１の結晶処理装置に本発明を用い
てＧａＡｓ単結晶を成長させ、その電気的特性を測定す
る実験を行った。ただしこの実験では、気密容器にｐＢ
Ｎをコートしたグラファイト、観察窓に石英を用い、そ
れぞれの接合部に直径１ｍｍの紐状Ｉｎをシール材とし
て介装した。そしてルツボにＧａ２ｋｇを、下部容器の
底部にＡｓ２．３ｋｇを配置して図２ないし図５に示し
た実施例の通りにＧａＡｓ単結晶の成長を行った。なお
、この時応力緩衝装置による付勢によって接合部に掛け
られた押圧力は１０ｋｇ／ｃｍ２程度であった。この実
験によって直径８０ｍｍ、長さ１００ｍｍの単結晶を得
ることができた。この単結晶のホール測定による抵抗率
、電子移動度の値はそれぞれシード端部においては１．
３×１０７Ωｃｍ，７３００ｃｍ２／Ｖｓ、テイル部に
おいては１．１×１０７Ωｃｍ，７０００ｃｍ２／Ｖｓ
であった。また、不純物濃度に関しては、ＳＩＭＳ分析
によって、Ｓｉ，Ｓ濃度はそれぞれ３×１０１４ｃｍ−
３，３×１０１４ｃｍ−３であり、さらにＦＴＩＲ分析
によるＣ濃度は８×１０１４ｃｍ−３であった。これら
の特性は得られた結晶の純度が十分高いことを示してい
る。また、操作中のＡｓの損失は約５０ｇ であったが
、これは気密容器接合部の密封性が十分高いことを示す
ものである。また、気密容器を常温に戻した後、押上げ
下軸を下げて再び接合部を分割したが、シール材のＩｎ
Ａｓ膜は、接合部から簡単に剥がれ、接合面を破損する
ようなことはなかった。Next, an experiment was conducted in which a GaAs single crystal was grown using the present invention in the crystal processing apparatus shown in FIG. 1, and its electrical characteristics were measured. However, in this experiment, pB was stored in an airtight container.
Graphite coated with N and quartz were used for the observation window, and a string of In with a diameter of 1 mm was interposed at each joint as a sealing material. Then, 2 kg of Ga was placed in the crucible and 2.3 kg of As was placed at the bottom of the lower container, and a GaAs single crystal was grown as in the example shown in FIGS. 2 to 5. Note that at this time, the pressing force applied to the joint portion by the urging force by the stress buffer device was about 10 kg/cm 2 . Through this experiment, a single crystal with a diameter of 80 mm and a length of 100 mm could be obtained. The resistivity and electron mobility values of this single crystal measured by Hall are 1.1 at the seed end, respectively.
3×107Ωcm, 7300cm2/Vs, 1.1×107Ωcm, 7000cm2/Vs at the tail part
Met. Regarding the impurity concentration, SIMS analysis revealed that the Si and S concentrations were each 3 x 1014 cm-
The C concentration was 3.3 x 1014 cm-3, and the C concentration by FTIR analysis was 8 x 1014 cm-3. These characteristics indicate that the purity of the obtained crystals is sufficiently high. Furthermore, the loss of As during the operation was approximately 50 g, which indicates that the sealing performance of the joint of the airtight container was sufficiently high. In addition, after returning the airtight container to room temperature, the lower push-up shaft was lowered and the joint was divided again, but the sealant's In
The As film was easily peeled off from the bonded portion and did not damage the bonded surface.
【００３７】[0037]
【発明の効果】以上説明したように、本発明によれば単
結晶生成のすべての段階でＩｎシール材がその形態を変
化させつつ気密容器をシールし、特に単結晶成長時の高
温下においてもシール効果を失うことがなく、不純物の
混入を防ぐことができるので、高純度で高品質の半導体
結晶を成長せしめることが可能となる。またシール材と
して使用されるＩｎ、およびこのＩｎと高解離圧成分ガ
スとの反応物は常温においては固体であるので、気密容
器の接合部への介装や除去が容易であり、取り扱いが簡
便になるという利点を有する。さらに、本発明はシール
材をＩｎに置き換えることで簡単に実施でき、装置その
ものは従来のものを流用することが可能である。As explained above, according to the present invention, the In sealing material changes its form and seals the airtight container at all stages of single crystal growth, and even under high temperatures during single crystal growth. Since the sealing effect is not lost and the contamination of impurities can be prevented, it is possible to grow highly pure and high quality semiconductor crystals. In addition, since the In used as the sealing material and the reaction product of this In and the high dissociation pressure component gas are solid at room temperature, they can be easily inserted into and removed from the joints of the airtight container, making them easy to handle. It has the advantage of being Furthermore, the present invention can be easily implemented by replacing the sealing material with In, and the conventional device itself can be used.
【００３８】また前記接合部に凹部を形成した上でＩｎ
シール材を介装することにより、結晶成長中の液状とな
ったＩｎシール材の移動が拘束され、接合部から該シー
ル材が逸脱するような事態を未然に防ぐことができ、よ
り確実に接合部のシール性を維持することが可能となる
。あるいはこのＩｎシール材よりも気密容器の外部側に
第二のシール材を配設することにより、昇温時に気密容
器内外の圧力差によってＩｎシール材が移動して失われ
るのを防ぐことができ、また、引上げ終了後のＩｎシー
ル材の剥離を容易にすることが可能となる。[0038] Further, after forming a recess in the joint part, In
By interposing the sealing material, the movement of the liquid In sealing material during crystal growth is restrained, and it is possible to prevent the sealing material from deviating from the joint, making it possible to join more reliably. This makes it possible to maintain the sealing properties of the parts. Alternatively, by arranging a second sealing material on the outside of the airtight container rather than this In sealing material, it is possible to prevent the In sealing material from moving and being lost due to the pressure difference inside and outside the airtight container when the temperature rises. Moreover, it becomes possible to easily peel off the In sealing material after the pulling is completed.
【図１】本発明に係わる高解離圧化合物半導体結晶処理
装置の一例を示す断面図である。FIG. 1 is a sectional view showing an example of a high dissociation pressure compound semiconductor crystal processing apparatus according to the present invention.
【図２】本発明の一実施例を示す気密容器１の接合部の
断面図である。FIG. 2 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the present invention.
【図３】本発明の一実施例を示す気密容器１の接合部の
断面図である。FIG. 3 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the present invention.
【図４】本発明の一実施例を示す気密容器１の接合部の
断面図である。FIG. 4 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the present invention.
【図５】本発明の一実施例を示す気密容器１の接合部の
断面図である。FIG. 5 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the present invention.
【図６】本発明の他の実施例を示す気密容器１の接合部
の断面図である。FIG. 6 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図７】本発明の他の実施例を示す気密容器１の接合部
の断面図である。FIG. 7 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図８】本発明を気密容器１と観察窓１３の接合部に用
いた場合の例を示す断面図である。FIG. 8 is a cross-sectional view showing an example in which the present invention is applied to a joint between the airtight container 1 and the observation window 13.
【図９】本発明のシール構造の一実施例を示す気密容器
１の接合部の断面図である。FIG. 9 is a sectional view of a joint portion of the airtight container 1 showing an embodiment of the seal structure of the present invention.
【図１０】本発明のシール構造の一実施例を示す気密容
器１の接合部の断面図である。FIG. 10 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the seal structure of the present invention.
【図１１】本発明のシール構造の一実施例を示す気密容
器１の接合部の断面図である。FIG. 11 is a sectional view of a joint portion of an airtight container 1 showing an embodiment of the seal structure of the present invention.
【図１２】本発明のシール構造の一実施例を示す気密容
器１の接合部の断面図である。FIG. 12 is a sectional view of a joint portion of the airtight container 1 showing an embodiment of the seal structure of the present invention.
【図１３】本発明のその他の実施例を示す気密容器１の
接合部の断面図である。FIG. 13 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図１４】本発明のその他の実施例を示す気密容器１の
接合部の断面図である。FIG. 14 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図１５】本発明のその他の実施例を示す気密容器１の
接合部の断面図である。FIG. 15 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図１６】本発明のその他の実施例を示す気密容器１の
接合部の断面図である。FIG. 16 is a sectional view of a joint portion of an airtight container 1 showing another embodiment of the present invention.
【図１７】本発明を縦型ブリッジマン結晶成長装置に用
いた場合の一例を示す断面図である。FIG. 17 is a cross-sectional view showing an example of the case where the present invention is applied to a vertical Bridgman crystal growth apparatus.
１ 気密容器 ２ 上部容器 ２ａ 接合部突条 ２ｂ 保持部 ３ 下部容器 ３ａ 接合部溝 ３ｂ 凹溝 ４ 外部容器 ５ シール材 ５ａ ＩｎＡｓ部分 ５ｂ Ｉｎ部分 ６ 押上げ下軸 ７ 応力緩衝装置 １１ 蒸気圧制御部 １２ 引上軸 １３ 観察窓 １３ａ 凸部 １６ 凸部 １７ Ｏリング １８ シール部 １９ コイルスプリング ２０ 袋ナット ２１ 第二のシール材 ２２ ルツボ支持台 Ｙ 原料融液 Ｔ 単結晶 Ｓ 種結晶 1 Airtight container 2 Upper container 2a Joint protrusion 2b Holding part 3 Lower container 3a Joint groove 3b Concave groove 4 External container 5 Seal material 5a InAs part 5b In part 6 Push-up lower shaft 7 Stress buffer device 11 Steam pressure control section 12 Pulling axis 13 Observation window 13a Convex part 16 Convex part 17 O-ring 18 Seal part 19 Coil spring 20 Cap nut 21 Second sealing material 22 Crucible support stand Y Raw material melt T Single crystal S seed crystal
Claims (3)
の内部に高解離圧化合物半導体結晶の原料を保持し、高
解離圧成分蒸気の蒸気圧を制御して前記高解離圧化合物
半導体を成長せしめる高解離圧化合物半導体結晶処理装
置における分割部のシール方法において、前記気密容器
を構成する構成部材の少なくとも一の接合部に、Ｉｎ（
インジウム）よりなるシール材を介装するとともに、該
接合部にて接合される前記構成部材を前記シール材を圧
縮する方向に付勢しつつ、前記高解離圧化合物半導体結
晶を成長せしめることを特徴とする高解離圧化合物半導
体結晶処理装置におけるシール方法。1. A raw material for a high dissociation pressure compound semiconductor crystal is held inside an airtight container made of divisible structural members, and the high dissociation pressure compound semiconductor is grown by controlling the vapor pressure of the high dissociation pressure component vapor. In a method for sealing a divided portion in a high dissociation pressure compound semiconductor crystal processing apparatus, at least one joint portion of the constituent members constituting the airtight container is coated with In(
The high dissociation pressure compound semiconductor crystal is grown while interposing a sealing material made of (indium) and urging the constituent members joined at the joint in a direction that compresses the sealing material. A sealing method for high dissociation pressure compound semiconductor crystal processing equipment.
結晶処理装置におけるシール方法に用いられる高解離圧
化合物半導体処理装置におけるシール構造であって、前
記接合部にて接合される前記構成部材の少なくとも一つ
には、前記シール材の移動を拘束する凹部が形成されて
いることを特徴とする高解離圧化合物半導体結晶処理装
置におけるシール構造。2. A sealing structure in a high dissociation pressure compound semiconductor processing apparatus used in the sealing method in the high dissociation pressure compound semiconductor crystal processing apparatus according to claim 1, wherein the constituent members joined at the joint portion A sealing structure for a high dissociation pressure compound semiconductor crystal processing apparatus, characterized in that at least one of the sealing members is formed with a recessed portion for restraining movement of the sealing material.
接合部の該シール材よりも前記気密容器外部側に、Ｉｎ
（インジウム）とは異なる組成の第二のシール材が介装
されていることを特徴とする請求項１記載の高解離圧化
合物半導体結晶処理装置におけるシール方法、および請
求項２記載の高解離圧化合物半導体結晶処理装置におけ
るシール構造。3. In a joint portion of the structural member in which the sealing material is interposed, an In
The sealing method in a high dissociation pressure compound semiconductor crystal processing apparatus according to claim 1, characterized in that a second sealing material having a composition different from (indium) is interposed, and the high dissociation pressure according to claim 2. Seal structure in compound semiconductor crystal processing equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6217491A JPH04265297A (en) | 1990-03-30 | 1991-03-26 | Method and structure for sealing in treating device of high-dissociation-pressure compound semiconductor crystal |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2-83741 | 1990-03-30 | ||
| JP8374190 | 1990-03-30 | ||
| JP6217491A JPH04265297A (en) | 1990-03-30 | 1991-03-26 | Method and structure for sealing in treating device of high-dissociation-pressure compound semiconductor crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04265297A true JPH04265297A (en) | 1992-09-21 |
Family
ID=26403234
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6217491A Withdrawn JPH04265297A (en) | 1990-03-30 | 1991-03-26 | Method and structure for sealing in treating device of high-dissociation-pressure compound semiconductor crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04265297A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012126644A (en) * | 2001-07-05 | 2012-07-05 | Axt Inc | Method and apparatus for growing semiconductor crystal with a rigid support with carbon doping, resistivity control and thermal gradient control |
| JP2016148702A (en) * | 2015-02-10 | 2016-08-18 | 株式会社リコー | Housing structure, optical scanner, and image forming apparatus |
-
1991
- 1991-03-26 JP JP6217491A patent/JPH04265297A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012126644A (en) * | 2001-07-05 | 2012-07-05 | Axt Inc | Method and apparatus for growing semiconductor crystal with a rigid support with carbon doping, resistivity control and thermal gradient control |
| JP2016148702A (en) * | 2015-02-10 | 2016-08-18 | 株式会社リコー | Housing structure, optical scanner, and image forming apparatus |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Application deemed to be withdrawn because no request for examination was validly filed |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19980514 |