JPS63270379A - Production of compound semiconductor single crystal and apparatus therefor - Google Patents
Production of compound semiconductor single crystal and apparatus thereforInfo
- Publication number
- JPS63270379A JPS63270379A JP10311587A JP10311587A JPS63270379A JP S63270379 A JPS63270379 A JP S63270379A JP 10311587 A JP10311587 A JP 10311587A JP 10311587 A JP10311587 A JP 10311587A JP S63270379 A JPS63270379 A JP S63270379A
- Authority
- JP
- Japan
- Prior art keywords
- crucible
- melt
- compound semiconductor
- seed crystal
- group
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 59
- 150000001875 compounds Chemical class 0.000 title claims abstract description 40
- 239000004065 semiconductor Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 239000000155 melt Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 12
- 229910021478 group 5 element Inorganic materials 0.000 claims abstract description 9
- 238000010899 nucleation Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 230000005484 gravity Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000001965 increasing effect Effects 0.000 abstract description 3
- 239000011261 inert gas Substances 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract 1
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
〔技術分野〕
本発明は、垂直凝固法による化合物半導体単結晶の製造
方法および装置に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Technical Field] The present invention relates to a method and apparatus for manufacturing a compound semiconductor single crystal by a vertical solidification method.
従来の垂直凝固法による化合物半導体単結晶の製造方法
は垂直温度勾配付き徐冷法によるものである （Ｊｏｕ
ｒｎａｌ ｏｆ ＣｒｙｓｔａＩ Ｇｒｏｗｔｈ ７４
（１９８６） ４９１〜５０６）。この方法は、原料と
して既に合成された多結晶を用い、それをルツボに入れ
て溶融させた後、融液をルツボ下端に配置した種子結晶
と接触させて種子付けを行い、下端より徐々に冷却して
上方に向かって化合物半導体単結晶を成長させていくと
いうものである。この方法では、原料の溶融、種子付け
の際、■族元素の事態による飛散を防止するため、ルツ
ボを収納した成長容器の下部低温帯に■族元素を配置し
、これを加熱して■族元素の蒸気圧を単離圧以上となる
ように調節しており、またこれにより融液組成のずれを
防止している。The conventional manufacturing method for compound semiconductor single crystals using the vertical solidification method is based on a slow cooling method with a vertical temperature gradient.
rnal of Crystal Growth 74
(1986) 491-506). This method uses polycrystals that have already been synthesized as raw materials, puts them in a crucible, melts them, and then seeds the melt by bringing it into contact with seed crystals placed at the bottom of the crucible, and gradually cools it from the bottom. The process involves growing a compound semiconductor single crystal upward. In this method, when melting raw materials and seeding, in order to prevent group Ⅰ elements from scattering due to situations, group Ⅰ elements are placed in the lower low temperature zone of the growth container that houses the crucible, and this is heated to prevent group Ⅰ elements from scattering. The vapor pressure of the elements is adjusted to be higher than the isolation pressure, and this also prevents deviations in the melt composition.
しかし従来の垂直凝固法による単結晶の製造方法は、原
料として化合物半導体多結晶を用いるものであるため、
多結晶を他の方法、例えば水平ブリッジマン法とか、高
圧容器内で液体封止剤を用いて直接合成する方法などに
より予め製造しておく必要がある。したがって単結晶を
得るには、別な装置で多結晶製造と単結晶製造の２段階
の工程を経なければならず、製造工程が煩雑で、不純物
混入の機会が増加する等の欠点がある。またこのため製
造コストが高くなる欠点がある。However, the conventional method for manufacturing single crystals using the vertical solidification method uses compound semiconductor polycrystals as raw materials, so
The polycrystals must be prepared in advance by other methods, such as the horizontal Bridgman method or direct synthesis using a liquid sealant in a high-pressure vessel. Therefore, in order to obtain a single crystal, it is necessary to go through a two-step process of polycrystal production and single crystal production using separate equipment, which has drawbacks such as a complicated manufacturing process and an increased chance of contamination with impurities. This also has the disadvantage of increasing manufacturing costs.
本発明は、上記のような従来技術の問題点を解決した垂
直凝固法による化合物半導体単結晶の製造方法を提供す
るもので、その方法は、垂直配置された成長容器内に、
下部に細い管状部を有する筒形のルツボを同軸配置し、
上記管状部に液止め栓と種子結晶を前者を上にして挿入
した状態で、上記ルツボ内で化合物半導体融液を合成し
、その後、上記種子結晶を下から押し上げ、液止め栓を
上記融液内に放出して融液面に浮上させることにより上
記種子結晶と融液を接触させ、種子付けを行った後、下
端より化合物半導体の単結晶を成長させることを特徴と
するものである。The present invention provides a method for manufacturing a compound semiconductor single crystal by a vertical solidification method that solves the problems of the prior art as described above.
A cylindrical crucible with a thin tubular part at the bottom is coaxially arranged,
A compound semiconductor melt is synthesized in the crucible with the liquid stopper and the seed crystal inserted into the tubular part with the former facing upward, and then the seed crystal is pushed up from below and the liquid stopper is inserted into the melt. The method is characterized in that the seed crystal is brought into contact with the melt by being ejected into the melt surface and floated on the surface of the melt, and after seeding, a single crystal of compound semiconductor is grown from the lower end.
液止め栓は、耐熱性があり、化合物半導体融液より比重
の小さいＢＮまたはＰＢＮなどの材料で作られる。この
ような液止め栓をルツボ下部の管状部に挿入することに
より液漏れを防止し、ルツボ内で化合物半導体融液の合
成を行えるようにする。融液合成後は、上記液止め栓を
その下部に挿入した種子結晶で融液中に押し出すと、液
止め栓が浮上し、種子結晶と融液が接触するから、種子
付けおよび結晶成長が行えることになる。The liquid stopper is made of a material such as BN or PBN that is heat resistant and has a lower specific gravity than the compound semiconductor melt. By inserting such a liquid stopper into the tubular portion at the lower part of the crucible, liquid leakage is prevented and a compound semiconductor melt can be synthesized within the crucible. After melt synthesis, when the liquid stopper is pushed into the melt using a seed crystal inserted under the liquid stopper, the liquid stopper floats up and the seed crystal comes into contact with the melt, allowing seeding and crystal growth. It turns out.
本発明はまた、上記製造方法の実施に好適な化合物半導
体単結晶の製造装置を提供するもので、その構成は、圧
力容器内に垂直配置された成長容器と、下部に液止め栓
および種子結晶が挿入される細い管状部を有する筒形の
ルツボと、このルツボを上記成長容器内の上部に垂直に
、かつ成長容器に対して相対的に上下動可能に支持する
支持体と、上記成長容器内の下部に垂直に設置され、上
端が上記ルツボの管状部に挿入される押し上げ棒とを備
え、上記ルツボを成長容器に対して相対的に下降させる
と、上記押し上げ棒が上記管状部内の液止め栓および種
子結晶を押し上げるようになっていることを特徴とする
ものである。The present invention also provides an apparatus for producing a compound semiconductor single crystal suitable for carrying out the above production method, and is composed of a growth vessel arranged vertically within a pressure vessel, a liquid stopper at the bottom, and a seed crystal. a cylindrical crucible having a thin tubular portion into which the crucible is inserted; a support that supports the crucible vertically in the upper part of the growth container and movable up and down relative to the growth container; and the growth container. A push-up rod is installed vertically in the lower part of the growth container and has an upper end inserted into the tubular part of the crucible, and when the crucible is lowered relative to the growth container, the push-up bar pushes up the liquid in the tubular part. It is characterized by a stopper and a device that pushes up the seed crystals.
この装置は、ルツボ下部の管状部に液止め栓および種子
結晶を挿入した状態で、化合物半導体融液の合成を行い
、その後、成長容器を静止させたままルツボを支持体と
共に下降させるか、またはその逆にルツボを支持体によ
って静止させたまま成長容器を上昇させると、押し上げ
棒により液止め栓が融液内に押し出され、種子結晶と融
液が接触するようになるので、この状態で種子付け、結
晶成長を行えるものである。This device synthesizes a compound semiconductor melt with a liquid stopper and a seed crystal inserted into the tubular part at the bottom of the crucible, and then lowers the crucible together with the support while keeping the growth container stationary, or Conversely, if the growth container is raised while the crucible is held stationary by the support, the liquid stopper will be pushed out into the melt by the push-up rod, and the seed crystals will come into contact with the melt. It is possible to attach and grow crystals.
以下、本発明の実施例を図面を参照して詳細に説明する
。Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.
第１図および第２図は本発明の一実施例を示す。1 and 2 show one embodiment of the invention.
図において、１１は圧力容器、１３はその中心に垂直に
配置された成長容器、１５はその中に同軸配置された筒
形のルツボである。ルツボ１５はＰＢＮ製で、その下部
は細い管状部１５ａとなっている。In the figure, 11 is a pressure vessel, 13 is a growth vessel arranged vertically at the center thereof, and 15 is a cylindrical crucible arranged coaxially therein. The crucible 15 is made of PBN, and its lower part is a thin tubular part 15a.
また１７は成長容器１３の上端開口部に擦り合わせ嵌合
された気密蓋、１９は成長容器１３の中間部に擦り合わ
せ嵌合されたルツボ支持台、２１はｆｉ１７にルツボ支
持台１９を吊り下げる吊り具である。吊り具２１はルツ
ボ１５のまわりに周方向に間隔をあけて多数設けられて
いる。ルツボ支持台１９は断熱材よりなるが、ポーラス
な材料で作るか、上下方向に穴をあける等して、上下方
向に通気性を持たせである。蓋１７は圧力容器１１の天
板を貫通する上部軸２３に支持されて上下動および回転
可能になっている。Further, 17 is an airtight lid that is fitted to the upper end opening of the growth container 13, 19 is a crucible support that is fitted to the middle part of the growth container 13, and 21 is a crucible support 19 suspended from the fi 17. It is a hanging device. A large number of hanging tools 21 are provided around the crucible 15 at intervals in the circumferential direction. The crucible support base 19 is made of a heat insulating material, but it is made of a porous material or has holes in the vertical direction to provide ventilation in the vertical direction. The lid 17 is supported by an upper shaft 23 passing through the top plate of the pressure vessel 11, and is vertically movable and rotatable.
また２５は成長容器１３内の底部に設置されたＶ族元素
収納用の下部容器、２７は下部容器２５の中心に垂直に
立設された押し上げ棒である。押し上げ棒２７の上端は
ルツボの管状部１５ａに挿入されるようになる。２９は
成長容器支持台で、これは圧力容器１１の底板を貫通す
る下部軸３１に支持されて上下動および回転可能になっ
ている。成長容器支持台２９の中には測温用のサーモカ
ンプル３３が設置されている。Further, 25 is a lower container for storing group V elements installed at the bottom of the growth container 13, and 27 is a push-up rod vertically installed in the center of the lower container 25. The upper end of the push-up rod 27 is inserted into the tubular portion 15a of the crucible. Reference numeral 29 denotes a growth vessel support stand, which is supported by a lower shaft 31 passing through the bottom plate of the pressure vessel 11 and is movable up and down and rotatable. A thermocample 33 for temperature measurement is installed inside the growth container support 29.
また３５は成長容器１３の外でルツボ１５を包囲するよ
うに設置された主加熱ヒーター、３７はその端子、３９
は給電用導体、４１は成長容器１３の外で下部容器２５
を包囲するように設置された副加りさヒーター、４３は
その端子、４５は給電用４体である。さらに４７は断熱
材、４９は圧力容器内面に配にした冷却管である。Further, 35 is a main heater installed outside the growth container 13 so as to surround the crucible 15, 37 is its terminal, and 39
41 is the power supply conductor, and 41 is the lower container 25 outside the growth container 13.
43 is a terminal thereof, and 45 is four units for power supply. Furthermore, 47 is a heat insulating material, and 49 is a cooling pipe arranged on the inner surface of the pressure vessel.
上記構成の装置による化合物半導体単結晶の製造は次の
ようにして行われる。まずルツボ下部の管状部１５ａに
液止め栓５１および種子結晶５３を前者が上になるよう
に挿入すると共に、ルツボ１５内に■族元素（ＧａＡｓ
の場合はＧａ） ５５を入れる。Manufacture of a compound semiconductor single crystal using the apparatus having the above configuration is performed as follows. First, the liquid stopper 51 and the seed crystal 53 are inserted into the tubular part 15a at the bottom of the crucible with the former facing upward, and the group
If , enter Ga) 55.
また下部容器２５内に■族元素（ＧａＡｓの場合はＡｓ
）５７を入れ、る。In addition, in the lower container 25, group Ⅰ elements (in the case of GaAs, As
) 57 and ru.
ルツボ１５内および圧力容器ｌｌ内の残留酸素を取り除
くため、上部軸２３を上昇させ、成長容器１３から蓋１
７を引き抜いた状態で、圧力容器１１内を真空引きする
。その後、不活性ガス（アルゴンまたは窒素）を充填し
、圧力容器１１内を３〜１００Ｋｇ／ｃｍ”の圧力にす
る０次いで上部軸２３を下降させ、第１図のように成長
容器１３に１ｉ１７を嵌合すると共に、種子結晶５３の
下端に押し上げ棒２７の上端が突き当たるようにする。In order to remove residual oxygen in the crucible 15 and pressure vessel 11, the upper shaft 23 is raised and the lid 1 is removed from the growth vessel 13.
7 is pulled out, the inside of the pressure vessel 11 is evacuated. After that, the inside of the pressure vessel 11 is filled with inert gas (argon or nitrogen) and the pressure is set to 3 to 100 kg/cm''.Then, the upper shaft 23 is lowered, and the growth vessel 13 is filled with 1i17 as shown in FIG. At the same time, the upper end of the push-up rod 27 is brought into contact with the lower end of the seed crystal 53.
次に、主加熱ヒーター３５を加熱し、■族元素５５を溶
融させ、ＧａＡｓ合成の場合であれば約１２３８℃に保
つ。また副加熱ヒーター４１も加熱し、Ｖ族元素５７を
約６１７℃にして、成長容器１３内のＶ族元素の蒸気圧
を１気圧以上にする。この状態で化合物半導体の合成反
応を進行させる。Next, the main heater 35 is heated to melt the group Ⅰ element 55, and in the case of GaAs synthesis, the temperature is maintained at about 1238°C. The auxiliary heater 41 is also heated to bring the V group element 57 to about 617° C., and the vapor pressure of the V group element in the growth container 13 to 1 atm or more. In this state, the compound semiconductor synthesis reaction is allowed to proceed.
化合物半導体の合成が終了したら、上部軸２３を徐々に
下降させる。すると、ルツボ１５が下降し、相対的に押
し上げ棒２７が種子結晶５３と液止め栓５１を押し上げ
るから、液止め栓５１が管状部１５ａから抜は出し、化
合物半導体融液中に放出される。液止め栓５１は化合物
半導体融液より比重が小さいので、第２図に示すように
液止め栓５１は化合物半導体融液５９の液面に浮上し、
融液５９と種子結晶５３の接触が得られることになる。When the synthesis of the compound semiconductor is completed, the upper shaft 23 is gradually lowered. Then, the crucible 15 descends and the push-up rod 27 relatively pushes up the seed crystal 53 and liquid stopper 51, so that the liquid stopper 51 is pulled out from the tubular portion 15a and discharged into the compound semiconductor melt. Since the liquid stopper 51 has a smaller specific gravity than the compound semiconductor melt, the liquid stopper 51 floats on the surface of the compound semiconductor melt 59 as shown in FIG.
Contact between the melt 59 and the seed crystal 53 is obtained.
このときの温度分布は、種子結晶５３と融液５９の接触
部で化合物半導体の融点となるようにし、それより上に
行くに従って徐々に高い温度となるようにしである。The temperature distribution at this time is such that the contact area between the seed crystal 53 and the melt 59 reaches the melting point of the compound semiconductor, and the temperature gradually increases as it goes above that point.
次に種子付けを行うため、上記接触部の温度を約１０℃
上げ、種子結晶５３の一部を再溶融させて融液５９にな
じませる。その後は、従来の垂直凝固法と同様で、上方
に向かって徐々に温度を低下させて行き、単結晶を成長
させる。冷却速度は３〜２０’Ｃ／ｈｒの範囲で制御さ
れる。成長方向の温度勾配は、種子結晶と融液の接触部
で２０〜ｂ肩部で２０〜１００℃／ｃｍ ％胴部で２〜
ｂるようにする。Next, in order to set seeds, the temperature of the above contact area is set to about 10℃.
Then, a part of the seed crystal 53 is remelted and blended into the melt 59. After that, the temperature is gradually lowered upwards to grow a single crystal, similar to the conventional vertical solidification method. The cooling rate is controlled in the range of 3-20'C/hr. The temperature gradient in the growth direction is 20°C/cm at the contact area between the seed crystal and the melt, 20°C/cm at the shoulder, and 2°C/cm at the body.
b.
以上のようにして本発明によれば、化合物半導体融液の
合成から単結晶の成長までを同一ルツボ内で行うことが
できる。なお上記の方法では単結晶成長の際、主加熱ヒ
ーターの温度分布を変化させたが、主加熱ヒーターの温
度分布は一定とし、ルツボ１５を成長容器１３と共に下
降させて行く方法も採用できる。As described above, according to the present invention, everything from synthesis of a compound semiconductor melt to growth of a single crystal can be performed in the same crucible. In the above method, the temperature distribution of the main heater is changed during single crystal growth, but a method may also be adopted in which the temperature distribution of the main heater is kept constant and the crucible 15 is lowered together with the growth container 13.
第３図は本発明の他の実施例を示す、同図において第１
図と同一部分には同一符号を付しである。FIG. 3 shows another embodiment of the present invention.
The same parts as in the figures are given the same reference numerals.
この実施例は、ルツボ１５内に■族元素５５と■族元素
５７を入れ、ルツボ１５内で直接合成反応により化合物
半導体多結晶原料を合成してから化合物半導体融液を作
るものである。In this embodiment, a group (1) element 55 and a group (2) element 57 are placed in a crucible 15, a compound semiconductor polycrystalline raw material is synthesized by a direct synthesis reaction in the crucible 15, and then a compound semiconductor melt is produced.
図示のようにルツボ１５内に■族元素５５とＶ族元素５
７を入れてから、内部の残留酸素を取り除くため前記実
施例と同様に真空引きしたあと、不活性ガスで置換し、
１００気圧程度に加圧する。As shown in the figure, in the crucible 15, a group II element 55 and a group V element 5 are placed.
7 and then evacuated in the same manner as in the previous example to remove residual oxygen inside, and then replaced with inert gas.
Pressurize to about 100 atmospheres.
まず始めに成長容器１３を１ｉ１７を嵌合させたまま下
降させ、ルツボ１５が主加熱ヒーター３５より下に位置
するようにする。この状態で主加熱ヒーター３５を加熱
し、ＧａＡｓの場合であれば８１７〜１２３８℃の範囲
内の一定の温度に保つ。その後、成長容器１３を上昇さ
せ、ルツボ１５を急速に主加熱ヒーター３５内に挿入す
る。これによってルツボ１５内の■族元素５５とＶ族元
素５７の反応が起こり、直接合成が進行する。このとき
未反応の■族元素が蒸散するのを抑えるため、下部容器
２５内に入れた■族元素５７を副加熱ヒーター４１によ
り加熱しくＧａＡｓの場合は６１７℃以上）、Ｖ族元素
の蒸気圧を保つようにする。直接合成反応は急激に行わ
せる。これによりルツボ１５内に化合物半導体多結晶が
生成される。その後、この多結晶原料を溶融するため、
融点＋１０℃程度の温度に加熱し、化合物半導体融液を
作成する。First, the growth container 13 is lowered with the 1i 17 fitted therein so that the crucible 15 is located below the main heater 35. In this state, the main heater 35 is heated and kept at a constant temperature within the range of 817 to 1238° C. in the case of GaAs. Thereafter, the growth container 13 is raised and the crucible 15 is rapidly inserted into the main heater 35. As a result, a reaction occurs between the Group I element 55 and the Group V element 57 in the crucible 15, and direct synthesis proceeds. At this time, in order to suppress the evaporation of the unreacted Group III element, the Group III element 57 placed in the lower container 25 is heated by the auxiliary heater 41 (617°C or higher in the case of GaAs), and the vapor pressure of the Group V element is heated. Try to keep it. Direct synthesis reactions are performed rapidly. As a result, a compound semiconductor polycrystal is produced within the crucible 15. Then, in order to melt this polycrystalline raw material,
It is heated to a temperature of about 10° C. above the melting point to create a compound semiconductor melt.
このあとはルツボ１５を下降させ、液止め栓５１を融液
中に押し出して種子付けを行うことになるが、これ以降
の工程は前記実施例と同じであるので説明を省略する。After this, the crucible 15 is lowered and the liquid stopper 51 is pushed out into the melt to perform seeding, but since the subsequent steps are the same as in the previous embodiment, the explanation will be omitted.
第４図は本発明のさらに他の実施例を示す。この実施例
は、化合物半導体融液５９と種子結晶５３を接触させた
後、単結晶の成長を行う際に、融液５９に垂直方向の磁
界を印加するようにしたものである。このため圧力容器
１１の外に同軸状に円筒コイル６１を設置し、ルツボ１
５内に垂直磁場を発生させる。なお圧力容器１１はステ
ンレス製とし、主加熱ヒーター３５は二重スパイラル巻
きの無誘導型として、垂直磁場を乱さないようにする。FIG. 4 shows yet another embodiment of the invention. In this embodiment, after bringing the compound semiconductor melt 59 into contact with the seed crystal 53, a vertical magnetic field is applied to the melt 59 when growing a single crystal. For this purpose, a cylindrical coil 61 is installed coaxially outside the pressure vessel 11, and the crucible 1
A vertical magnetic field is generated within 5. The pressure vessel 11 is made of stainless steel, and the main heater 35 is of a non-inductive type with double spiral winding so as not to disturb the vertical magnetic field.
磁界の強さは５００〜５０００Ｇａｕｓｓ程度とする。The strength of the magnetic field is approximately 500 to 5000 Gauss.
垂直磁界を印加すると、融液５９の流れは、磁界にクロ
スする方向つまり径方向の流れがローレンツ力により抑
制されるため、垂直方向の流れだけとなる。その結果、
熱移動は、径方向には熱伝導のみとなり、垂直方向には
熱対流による移動が存在するため、下方の低温部へ向け
ての熱移動が生じ易くなり、下端から熱が奪い去られる
ことになる。このため径方向の温度分布は、第５図に示
すようにＡ−Ａ’線の断面でみると、ヒーター３５に近
い外周面で温度が高く、中心に行くほど温度が低（なる
形となる。その結果、固液界面６３の形状は融液５９に
対して若干凸形となり、熱歪を抑制した状態で、低欠陥
高純度の化合物半導体単結晶を成長させることができる
。また融液の熱振動も抑制されるため、温度の揺らぎに
起因する成長縞の発生も抑制することができる。When a perpendicular magnetic field is applied, the melt 59 flows only in the vertical direction because the flow in the direction crossing the magnetic field, that is, the flow in the radial direction is suppressed by the Lorentz force. the result,
Heat transfer occurs only through conduction in the radial direction, and in the vertical direction there is movement due to thermal convection, so heat transfer tends to occur toward the lower low-temperature area, and heat is removed from the bottom end. Become. Therefore, the temperature distribution in the radial direction, when viewed in cross section along the line A-A' as shown in Figure 5, shows that the temperature is high on the outer peripheral surface near the heater 35, and the temperature is low as it goes toward the center. As a result, the shape of the solid-liquid interface 63 becomes slightly convex with respect to the melt 59, and it is possible to grow a compound semiconductor single crystal with low defects and high purity while suppressing thermal distortion. Since thermal vibrations are also suppressed, the occurrence of growth streaks caused by temperature fluctuations can also be suppressed.
なお上記各実施例では、種子結晶をルツボの管状部に裸
で挿入したが、種子結晶を押し上げ棒で押し上げる際、
種子結晶にキズが付かないようにするため、第６図に示
すように種子結晶５３は例えばＰＢＮ製の保護ケース７
１に入れた状態で管状部１５ａに挿入するとよい。In each of the above examples, the seed crystal was inserted naked into the tubular part of the crucible, but when pushing up the seed crystal with a push-up rod,
In order to prevent the seed crystal from being scratched, the seed crystal 53 is covered with a protective case 7 made of PBN, for example, as shown in FIG.
1 and insert it into the tubular part 15a.
以上説明したように本発明によれば、化合物半導体の合
成、種子付け、単結晶成長を同一装置内で一貫したプロ
セスで行うことができるから、工程が短縮され、生産性
が向上すると共に、不純物混入の機会が減り、高純度、
高品質の化合物半導体単結晶を製造できる利点がある。As explained above, according to the present invention, compound semiconductor synthesis, seeding, and single crystal growth can be performed in the same device in an integrated process, which shortens the process, improves productivity, and eliminates impurities. Reduced chance of contamination, high purity,
It has the advantage of producing high-quality compound semiconductor single crystals.
第１図は本発明の一実施例に係る化合物半導体製造装置
を示す断面図、第２図は同装置で種子付けを行う状態を
示す要部断面図、第３図および第４図はそれぞれ本発明
の他の実施例を示す断面図第５図は第４図の装置で化合
物半導体単結晶を成長させる過程を示す説明図、第６図
は種子結晶の挿入方法の一例を示す断面図である。
１１〜圧力容器、１３〜成長容器、１５〜ルツボ、１５
８〜管状部、１７〜蓋、１９〜ルツボ支持台、２１〜吊
り具、２５〜下部容器、２７〜押し上げ棒、２９〜成長
容器支持台、３５〜主加熱ヒーター、４１〜副加熱ヒー
ター、５１〜液止め栓、５３〜種子結晶、５５〜蓋族元
素、５７〜■族元素、５９〜化合物半導体融液、６１第
２図
第４図
第５図
第６図
手続主甫正書（自発）
昭和６３年 １月潟日FIG. 1 is a cross-sectional view showing a compound semiconductor manufacturing apparatus according to an embodiment of the present invention, FIG. 2 is a cross-sectional view of essential parts showing a state in which seeds are set in the same apparatus, and FIGS. 3 and 4 are in accordance with this invention. FIG. 5 is a cross-sectional view showing another embodiment of the invention. FIG. 5 is an explanatory view showing the process of growing a compound semiconductor single crystal using the apparatus shown in FIG. 4. FIG. 6 is a cross-sectional view showing an example of a method of inserting a seed crystal. . 11-pressure vessel, 13-growth container, 15-crucible, 15
8-tubular part, 17-lid, 19-crucible support stand, 21-hanger, 25-lower container, 27-push-up rod, 29-growth container support stand, 35-main heating heater, 41-sub-heating heater, 51 ~ Liquid stopper, 53 ~ Seed crystal, 55 ~ Lid group element, 57 ~ Group ■ element, 59 ~ Compound semiconductor melt, 61 Figure 2 Figure 4 Figure 5 Figure 6 Procedure master book (self-proposal) January Lagoon, 1986
Claims (4)
を有する筒形のルツボを同軸配置し、上記管状部に液止
め栓と種子結晶を前者を上にして挿入した状態で、上記
ルツボ内で化合物半導体融液を合成し、その後、上記種
子結晶を下から押し上げ、液止め栓を上記融液内に放出
して融液面に浮上させることにより上記種子結晶と融液
を接触させ、種子付けを行った後、下端より化合物半導
体の単結晶を成長させることを特徴とする化合物半導体
単結晶の製造方法。(1) A cylindrical crucible with a thin tubular part at the bottom is coaxially arranged in a vertically arranged growth container, and a liquid stopper and a seed crystal are inserted into the tubular part with the former facing upward. A compound semiconductor melt is synthesized in a crucible, and then the seed crystal is pushed up from below, and a liquid stopper is released into the melt to float on the surface of the melt, thereby bringing the seed crystal into contact with the melt. . A method for producing a compound semiconductor single crystal, which comprises growing a compound semiconductor single crystal from the lower end after seeding.
物半導体融液の合成は、ルツボ内にIII族元素を入れ、
成長容器下部にＶ族元素を配置して、ルツボ内で溶融し
たIII族元素に気化したＶ族元素を反応させることによ
り行うもの。(2) The method according to claim 1, in which the compound semiconductor melt is synthesized by placing a group III element in a crucible;
This is done by placing a group V element at the bottom of the growth container and causing the vaporized group V element to react with the group III element melted in the crucible.
物半導体融液の合成は、ルツボ内にIII族元素とＶ族元
素を入れ、加熱加圧して直接合成反応により化合物半導
体多結晶原料を作成し、その後、その多結晶原料を溶融
させることにより行うもの。(3) The method according to claim 1, in which the compound semiconductor melt is synthesized by placing a group III element and a group V element in a crucible, heating and pressurizing the compound semiconductor polycrystal through a direct synthesis reaction. This is done by creating a raw material and then melting the polycrystalline raw material.
液止め栓および種子結晶が挿入される細い管状部を有す
る筒形のルツボと、このルツボを上記成長容器内の上部
に垂直に、かつ成長容器に対して相対的に上下動可能に
支持する支持体と、上記成長容器内の下部に垂直に設置
され、上端が上記ルツボの管状部に挿入される押し上げ
棒とを備え、上記ルツボを成長容器に対して相対的に下
降させると、上記押し上げ棒が上記管状部内の液止め栓
および種子結晶を押し上げるようになっていることを特
徴とする化合物半導体単結晶の製造装置。(4) A growth container arranged vertically within a pressure vessel, a cylindrical crucible having a thin tubular part in the lower part into which a liquid stopper and a seed crystal are inserted, and this crucible arranged vertically in the upper part of the growth container. , and a support member that supports the growth container so as to be movable up and down relative to the growth container; and a push-up rod that is installed vertically in the lower part of the growth container and whose upper end is inserted into the tubular part of the crucible, An apparatus for manufacturing a compound semiconductor single crystal, characterized in that when the crucible is lowered relative to the growth container, the push-up rod pushes up a liquid stopper and a seed crystal in the tubular part.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10311587A JPS63270379A (en) | 1987-04-28 | 1987-04-28 | Production of compound semiconductor single crystal and apparatus therefor |
| US07/185,476 US4904336A (en) | 1987-04-28 | 1988-04-25 | Method of manufacturing a single crystal of compound semiconductor and apparatus for the same |
| GB8809809A GB2205087B (en) | 1987-04-28 | 1988-04-26 | Method of manufacturing a single crystal of compound semiconductor and apparatus for the same |
| DE3814259A DE3814259A1 (en) | 1987-04-28 | 1988-04-27 | METHOD AND DEVICE FOR PRODUCING A SINGLE CRYSTAL OF A CONNECTION SEMICONDUCTOR |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10311587A JPS63270379A (en) | 1987-04-28 | 1987-04-28 | Production of compound semiconductor single crystal and apparatus therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63270379A true JPS63270379A (en) | 1988-11-08 |
Family
ID=14345596
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10311587A Pending JPS63270379A (en) | 1987-04-28 | 1987-04-28 | Production of compound semiconductor single crystal and apparatus therefor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63270379A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278490A (en) * | 1988-04-28 | 1989-11-08 | Nippon Telegr & Teleph Corp <Ntt> | Growth of crystal and crucible therefor |
| JPH0380181A (en) * | 1989-08-24 | 1991-04-04 | Mitsubishi Monsanto Chem Co | Device for producing single crystal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6374990A (en) * | 1986-09-16 | 1988-04-05 | Nippon Telegr & Teleph Corp <Ntt> | Production of single crystal of compound semiconductor and production device therefor |
-
1987
- 1987-04-28 JP JP10311587A patent/JPS63270379A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6374990A (en) * | 1986-09-16 | 1988-04-05 | Nippon Telegr & Teleph Corp <Ntt> | Production of single crystal of compound semiconductor and production device therefor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01278490A (en) * | 1988-04-28 | 1989-11-08 | Nippon Telegr & Teleph Corp <Ntt> | Growth of crystal and crucible therefor |
| JPH0380181A (en) * | 1989-08-24 | 1991-04-04 | Mitsubishi Monsanto Chem Co | Device for producing single crystal |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0068021B1 (en) | The method and apparatus for forming and growing a single crystal of a semiconductor compound | |
| JP4810346B2 (en) | Method for producing sapphire single crystal | |
| EP1571240B1 (en) | Method for producing compound semiconductor single crystal | |
| US3173765A (en) | Method of making crystalline silicon semiconductor material | |
| US4904336A (en) | Method of manufacturing a single crystal of compound semiconductor and apparatus for the same | |
| CN111809229A (en) | Preparation method and device of indium antimonide single crystal | |
| US5047113A (en) | Method for directional solidification of single crystals | |
| JPS63270379A (en) | Production of compound semiconductor single crystal and apparatus therefor | |
| JP3152971B2 (en) | Manufacturing method of high purity copper single crystal ingot | |
| JPS63285183A (en) | Production of compound semiconductor single crystal | |
| JP2690419B2 (en) | Single crystal growing method and apparatus | |
| JPS63270378A (en) | Production of single crystal of compound semiconductor | |
| JPS63274684A (en) | Production of compound semiconductor single crystal | |
| JP4117813B2 (en) | Method for producing compound semiconductor single crystal | |
| JP2758038B2 (en) | Single crystal manufacturing equipment | |
| CN217922421U (en) | Crystal pulling device | |
| JPS6090897A (en) | Method and apparatus for manufacturing compound semiconductor single crystal | |
| JPH08119784A (en) | Production of compound single crystal and production device therefor | |
| JPH02229791A (en) | Apparatus for producing compound semiconductor single crystal | |
| JP2022146327A (en) | MANUFACTURING METHOD OF FeGa ALLOY SINGLE CRYSTAL | |
| JP3654314B2 (en) | Manufacturing method of AlGaAs single crystal by flux method and manufacturing apparatus used therefor | |
| JPH08104591A (en) | Apparatus for growing single crystal | |
| JPH061692A (en) | Device for producing compound semiconductor single crystal | |
| JPS60122793A (en) | Device for growing single crystal of compound semiconductor | |
| JPS60122791A (en) | Pulling up method of crystal under liquid sealing |