JPH085736B2 - Method and apparatus for growing silicon single crystal - Google Patents

Method and apparatus for growing silicon single crystal

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Publication number
JPH085736B2
JPH085736B2 JP13798487A JP13798487A JPH085736B2 JP H085736 B2 JPH085736 B2 JP H085736B2 JP 13798487 A JP13798487 A JP 13798487A JP 13798487 A JP13798487 A JP 13798487A JP H085736 B2 JPH085736 B2 JP H085736B2
Authority
JP
Japan
Prior art keywords
single crystal
quartz crucible
silicon
growing
silicon single
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.)
Expired - Lifetime
Application number
JP13798487A
Other languages
Japanese (ja)
Other versions
JPS63303893A (en
Inventor
道夫 喜田
健彰 佐平
治郎 梶原
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Priority to JP13798487A priority Critical patent/JPH085736B2/en
Publication of JPS63303893A publication Critical patent/JPS63303893A/en
Publication of JPH085736B2 publication Critical patent/JPH085736B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、多重構造の石英ルツボを用いて、半導体素
子および太陽電池用のシリコン単結晶を引上げ育成する
と同時に、育成単結晶と同量の原料シリコンを石英ルツ
ボ内に連続的に供給するシリコン単結晶育成方法及び装
置に関する。
DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention uses a quartz crucible having a multiple structure to pull and grow a silicon single crystal for a semiconductor device and a solar cell, and at the same time, to grow the same amount of the grown single crystal. The present invention relates to a silicon single crystal growing method and apparatus for continuously supplying raw material silicon into a quartz crucible.

〔従来の技術〕[Conventional technology]

従来から、チョクラルスキー法によるシリコン単結晶
製造方法として、石英ルツボ内のシリコン融液に原料シ
リコンを連続的に補給することにより、シリンコン融液
量を一定に保ったまま単結晶を引き上げる単結晶連続製
造方法が各種提案されている(例えば、特開昭57−1833
92号,特開昭58−130195号,USP−2892739号)。
Conventionally, as a method for producing a silicon single crystal by the Czochralski method, a single crystal is pulled up while the silicon melt in a quartz crucible is continuously replenished with raw material silicon, while keeping the amount of sillcon melt constant. Various continuous manufacturing methods have been proposed (see, for example, JP-A-57-1833).
92, JP-A-58-130195, USP-2892739).

〔発明が解決しようとする問題点〕[Problems to be solved by the invention]

ところで、シリコン単結晶を育成している最中に、シ
リコン融液と接触している石英ルツボの表面の一部が劣
化し、さらには剥離するという現象がたびたび生じてい
る。この剥離した石英の小片は、シリコン融液より比重
が小さいため、シリコン融液面上を浮遊し、ついには育
成中の単結晶に付着し、そこから転位を発生させ、シリ
コン単結晶を多結晶化するという問題を生じさせる。そ
して、この石英小片の剥離という現象は、第4図に示す
ように、グラファイトサセプタ1に支持された石英ルツ
ボ2がシリコン融液3の表面4と接触している部分5に
おいて最も生じ易い。なぜなら、この部分5が、固相
(石英ルツボ2)−液相(シリコン融液3)−気相(Si
Oベーパー6)の3相界面で最も反応が激しいからであ
る。
By the way, during the growth of a silicon single crystal, a part of the surface of the quartz crucible which is in contact with the silicon melt is deteriorated, and further, a phenomenon of peeling frequently occurs. Since this exfoliated piece of quartz has a smaller specific gravity than the silicon melt, it floats on the surface of the silicon melt and eventually adheres to the growing single crystal, causing dislocations from it and causing the silicon single crystal to become polycrystalline. Causes the problem of becoming The phenomenon of the exfoliation of the quartz pieces is most likely to occur in the portion 5 where the quartz crucible 2 supported by the graphite susceptor 1 is in contact with the surface 4 of the silicon melt 3, as shown in FIG. Because this part 5 is solid phase (quartz crucible 2) -liquid phase (silicon melt 3) -gas phase (Si
This is because the reaction is most intense at the three-phase interface of O vapor 6).

この点において、バッチ式のシリコン単結晶育成方法
では、シリコン融液表面の位置が単結晶育成とともに石
英ルツボに対して相対的に下降するから、石英小片の剥
離によって育成中の単結晶に転位が導入されるというこ
とは比較的少なく、実際上問題にならない。これに対し
て、上述した単結晶連続製造方法にあっては、本発明者
が鋭意研究した結果、石英ルツボ内の融液表面の位置が
変化しないため、上記三相界面5での石英の劣化および
剥離が激しく生じ、長時間の単結晶連続育成が困難であ
ることがわかった。この問題を解決するための1つの方
法として、上記単結晶連続製造方法においても、単結晶
の育成量と原料の供給量を一致せずに、石英ルツボ内の
融液表面の位置を徐々に変化させることが考えられる。
そして、この方法によれば、石英の剥離による単結晶育
成の阻害という問題は回避できるが、単結晶連続育成方
法における大きな特徴であるルツボ内融液量の一定化に
よる単結晶品質の均質化という長所が失われる。
In this respect, in the batch type silicon single crystal growing method, the position of the silicon melt surface is relatively lowered with respect to the quartz crucible as the single crystal is grown, and therefore, dislocation of the quartz small pieces causes dislocation in the growing single crystal. It is relatively rare that it will be introduced, and it is not a problem in practice. On the other hand, in the above-described continuous single crystal production method, as a result of intensive studies by the present inventors, the position of the melt surface in the quartz crucible does not change, and therefore the deterioration of quartz at the three-phase interface 5 is caused. Further, it was found that peeling occurred violently and continuous growth of single crystal for a long time was difficult. As one method for solving this problem, even in the above-described single crystal continuous manufacturing method, the position of the melt surface in the quartz crucible is gradually changed without the growth amount of the single crystal and the supply amount of the raw materials being matched. It is possible to make it.
According to this method, the problem of inhibiting single crystal growth due to exfoliation of quartz can be avoided, but the major feature of the single crystal continuous growth method is homogenization of single crystal quality by making the melt amount in the crucible constant. Loss of strength.

本発明は、上記事情に鑑みてなれたもので、その目的
とするところは、単結晶品質の均質化を損うことなく、
石英ルツボの三相界面部からの石英の劣化及び剥離を極
力防止できて、単結晶の多結晶化を未然に防ぐことがで
きるシリコン単結晶育成方法及び装置を提供することに
ある。
The present invention has been made in view of the above circumstances, and an object thereof is to maintain homogenization of single crystal quality,
It is an object of the present invention to provide a method and an apparatus for growing a silicon single crystal capable of preventing the deterioration and peeling of quartz from the three-phase interface of a quartz crucible as much as possible and preventing the polycrystallization of a single crystal.

〔問題点を解決するための手段〕[Means for solving problems]

上記目的を達成するために、本発明の方法は、単結晶
引上げ育成時に、多重構造の石英ルツボの最も内側の収
容体をシリコン融液表面に対して連続的に昇降させるも
のである。
In order to achieve the above object, the method of the present invention continuously raises and lowers the innermost container of the quartz crucible having a multiple structure with respect to the surface of the silicon melt during pulling and growing the single crystal.

また、本発明の装置は、多重構造の石英ルツボの内側
収容体を支持する支持体を、回転自在な外側収容体の外
周に、昇降自在にかつこの外側収容体とともに回転可能
に設ける一方、前記支持体に、この支持体と係合して支
持体を昇降させる昇降機構を設けたものである。
Further, in the apparatus of the present invention, a support for supporting the inner container of the multi-structured quartz crucible is provided on the outer periphery of the rotatable outer container so as to be vertically movable and rotatable together with the outer container. The supporting body is provided with an elevating mechanism that engages with the supporting body and elevates the supporting body.

〔作用〕 本発明のシリコン単結晶育成方法及び装置にあって
は、単結晶を引上げ育成するに際して、多重構造の石英
ルツボの最も内側の収容体をシリコン融液表面に対して
連続的に昇降させ、この収容体とシリコン融液の表面と
の位置関係を連続的に変化させる。
[Operation] In the method and apparatus for growing a silicon single crystal of the present invention, when pulling and growing a single crystal, the innermost container of the quartz crucible having a multiple structure is continuously moved up and down with respect to the surface of the silicon melt. The positional relationship between this container and the surface of the silicon melt is continuously changed.

ここで、二重あるいは三重以上の石英ルツボ構造を用
いて、単結晶の連続育成を行なう場合に、融液量が一定
による石英小片の剥離の現象が問題となるのは、育成単
結晶を包む最も内側の収容体だけである。なぜなら、外
側の収容体から石英小片が剥離しても、内側の収容体が
遮蔽板となって、育成単結晶へ付着することが防げるか
らである。従って、石英ルツボの最も内側の収容体だけ
が単結晶育成とともに融液表面に対して上昇または下降
すればよい。
Here, when a single crystal is continuously grown by using a double or triple or more quartz crucible structure, the phenomenon of the exfoliation of quartz pieces due to a constant melt amount is a problem. Only the innermost containment. This is because even if the small quartz pieces are peeled off from the outer container, the inner container serves as a shielding plate and can be prevented from adhering to the grown single crystal. Therefore, only the innermost container of the quartz crucible needs to rise or fall with respect to the melt surface as the single crystal grows.

〔実施例〕〔Example〕

以下、第1図ないし第3図に基づいて本発明の実施例
を説明する。
An embodiment of the present invention will be described below with reference to FIGS.

第1図は本発明のシリコン単結晶育成方法を実施する
ための装置の一例を示すもので、図中符号10は石英ルツ
ボ11の外側収容体である。この外側収容体10の中央部が
深く形成されていると供に、外周部をグラファイトサセ
プタ12に支持されている。また、外側収容体10内には、
シリコン融液13が保持されていると供に、円筒状の内側
収容体14が、昇降機構15に上下移動自在に支持された状
態で装入されている。さらに、外側収容体10の縁部上方
には、粉末,塊状,あるいは顆粒状の原料16を供給する
原料供給管17が配置されている。
FIG. 1 shows an example of an apparatus for carrying out the method for growing a silicon single crystal according to the present invention, in which reference numeral 10 is an outer container of a quartz crucible 11. The outer peripheral portion is supported by the graphite susceptor 12 while the central portion of the outer container 10 is deeply formed. In addition, in the outer container 10,
While the silicon melt 13 is held, a cylindrical inner container 14 is inserted in a state of being supported by an elevating mechanism 15 so as to be vertically movable. Further, a raw material supply pipe 17 for supplying the raw material 16 in the form of powder, lumps, or granules is arranged above the edge of the outer container 10.

上記のように構成されたシリコン単結晶育成装置を用
いて本発明の方法を実施する場合には、まず、石英ルツ
ボ11内に多結晶シリコンを充填し、炉内をアルゴンガス
で置換した後に、抵抗加熱ヒータに通電して炉内を昇温
する。そして、充填した原料シリコンが溶解した後に、
液温を結晶育成に適した温度とする。次いで、従来公知
のダッシュ(DASH)の方法で種結晶を無転位化し、ネッ
ク部,肩部を形成し所望の太さにする。所望の太さにな
った時点で成長速度及び液温を調整して一定の直径の単
結晶18の直胴部を育成する。この際、石英ルツボ11の内
側収容体14と外側収容体10との間に、粉末,塊状,ある
いは顆粒状の原料16を単結晶18の育成量と同量だけ原料
供給管17から供給すると共に、内側収容体14を、昇降機
構15によって連続的に下降(または上昇)させる。
When performing the method of the present invention using the silicon single crystal growth apparatus configured as described above, first, the polycrystalline silicon in the quartz crucible 11 is filled, after the furnace is replaced with argon gas, The resistance heater is energized to raise the temperature inside the furnace. Then, after the raw material silicon filled is melted,
The liquid temperature is set to a temperature suitable for crystal growth. Then, the seed crystal is made dislocation-free by a conventionally known method of DASH to form a neck portion and a shoulder portion to have a desired thickness. When the desired thickness is reached, the growth rate and liquid temperature are adjusted to grow the straight body of the single crystal 18 having a constant diameter. At this time, the powder, lump, or granular raw material 16 is supplied from the raw material supply pipe 17 between the inner container 14 and the outer container 10 of the quartz crucible 11 in the same amount as the growth amount of the single crystal 18. The inner container 14 is continuously lowered (or raised) by the lifting mechanism 15.

このようにして、内側収容体14を連続的に昇降させる
ことにより、内側収容体14の内面の決まった部位だけが
3相界面になることがなく、長時間にわたって運転して
も石英の一部が剥離することなく、単結晶育成を阻害す
ることがない。しかも、融液量を一定に保ったまま品質
の均一な単結晶を得ることが可能となった。
In this way, by continuously moving the inner container 14 up and down, only a fixed part of the inner surface of the inner container 14 does not become a three-phase interface, and even if it is operated for a long time, a part of the quartz is not formed. Does not peel off and does not hinder single crystal growth. Moreover, it became possible to obtain a single crystal of uniform quality while keeping the melt volume constant.

また、第2図と第3図は本発明のシリコン単結晶育成
装置の一例を示すものであり、これらの図において、上
記第1図に示す装置と同様の構成の部分については同符
号を付けて説明を省略する。
2 and 3 show an example of the silicon single crystal growing apparatus of the present invention. In these figures, the same components as those of the apparatus shown in FIG. And the description is omitted.

第2図と第3図において符号20は、石英ルツボ11の外
側収容体10を支持するグラファイトサセプタであり、こ
のグラファイトサセプタ20の外周には、その軸線方向に
4つの溝20aが等間隔に形成されている。一方、外側収
容体10内に装入されている内側収容体14には、連続部材
21を介して筒状の支持体22が連結されており、この支持
体22の内周には、上記グラファイトサセプタ20の各溝20
aに嵌入する4本の突条22aが形成されている。これによ
り、支持体22はグラファイトサセプタ20に対して上下方
向に移動可能に構成されている。
2 and 3, reference numeral 20 is a graphite susceptor that supports the outer container 10 of the quartz crucible 11, and four grooves 20a are formed on the outer periphery of the graphite susceptor 20 at equal intervals in the axial direction. Has been done. On the other hand, the inner container 14 loaded in the outer container 10 has a continuous member.
A cylindrical support 22 is connected via 21 and each groove 20 of the graphite susceptor 20 is provided on the inner periphery of the support 22.
Four ridges 22a that fit into a are formed. As a result, the support 22 is configured to be vertically movable with respect to the graphite susceptor 20.

さらに、上記支持体22の外周下部には、ネジ部22bが
形成されており、このネジ部22bには、昇降機構23が係
合されている。そして、上記外側収容体10,グラファイ
トサセプタ20が回転すると、それに伴い支持体22が回転
しながら下降(あるいは上昇)するようになっている。
Further, a screw portion 22b is formed on the lower portion of the outer periphery of the support body 22, and an elevating mechanism 23 is engaged with the screw portion 22b. When the outer container 10 and the graphite susceptor 20 rotate, the support 22 rotates and descends (or rises) accordingly.

上記のように構成されたシリコン単結晶育成装置を用
いて本発明の方法を実施する場合には、上述した方法と
同様にして、石英ルツボ11内に多結晶シリコンを充填
し、かつ炉内をアルゴンガスで置換した後に、ヒータに
よって多結晶シリコンを溶解する。次いで、シリコン融
液を結晶育成に適した温度にした後、種結晶を浸漬し、
引上げて、単結晶18のネック部,肩部,直胴部を順次育
成する。この際、石英ルツボ11の内側収容体14と外側収
容体10との間に原料16を単結晶18育成量と同量だけ供給
して、シリコン融液13の液面を一定に保つ。また、同時
に、グラファイトサセプタ20を外側収容体10とともに回
転させることにより、グラファイトサセプタ20の外周に
嵌め込まれた支持体22が回転するが、このとき、この支
持体22の外周下部のネジ部22bには固定状態の昇降機構2
3が係合されているから、上記支持体22の回転に伴い、
昇降機構23がネジ部22bの螺旋に沿って移動することに
より、支持体22が下降(または上昇)する。この結果、
上述した実施例と同様の効果を奏することができる。
When performing the method of the present invention using the silicon single crystal growth apparatus configured as described above, in the same manner as the above-mentioned method, the quartz crucible 11 is filled with polycrystalline silicon, and the inside of the furnace is After replacing with argon gas, the polycrystalline silicon is melted by a heater. Then, after bringing the silicon melt to a temperature suitable for crystal growth, soaking the seed crystal,
By pulling up, the neck portion, the shoulder portion, and the straight body portion of the single crystal 18 are sequentially grown. At this time, the raw material 16 is supplied between the inner container 14 and the outer container 10 of the quartz crucible 11 in the same amount as the growth amount of the single crystal 18 to keep the liquid surface of the silicon melt 13 constant. At the same time, by rotating the graphite susceptor 20 together with the outer accommodating body 10, the support body 22 fitted on the outer periphery of the graphite susceptor 20 rotates, but at this time, the support portion 22 has a screw portion 22b at the lower outer periphery thereof. Is a lifting mechanism in a fixed state 2
Since 3 is engaged, with the rotation of the support 22,
The support mechanism 22 descends (or rises) as the elevating mechanism 23 moves along the spiral of the screw portion 22b. As a result,
The same effect as that of the above-described embodiment can be obtained.

〔発明の効果〕〔The invention's effect〕

以上説明したように、本発明は、単結晶を引上げ育成
するに際して、多重構造の石英ルツボの最も内側の収容
体をシリコン融液表面に対して連続的に昇降させ、この
収容体とシリコン融液の表面との位置関係を連続的に変
化させることにより、シリコン融液量の一定化による単
結晶の品質の均一化を損うことがなく、石英ルツボの三
相界面部が絶えず変化することにより石英の劣化及び剥
離を極力防止できて、単結晶の多結晶化を防止できると
いう優れた効果を有する。
As described above, in the present invention, when pulling and growing a single crystal, the innermost container of the quartz crucible having a multiple structure is continuously moved up and down with respect to the surface of the silicon melt, and the container and the silicon melt. By continuously changing the positional relationship with the surface of the quartz crucible, the three-phase interface of the quartz crucible is constantly changing without impairing the homogenization of the quality of the single crystal due to the constant amount of silicon melt. It has an excellent effect that the deterioration and peeling of quartz can be prevented as much as possible and the polycrystallization of a single crystal can be prevented.

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

第1図は本発明の一実施例を示す概略構成図、第2図と
第3図は本発明の他の一実施例を示すもので、第2図は
概略構成図、第3図は平面図、第4図は従来の石英ルツ
ボを示す説明図である。 10……外側収容体、11…石英ルツボ、13……シリコン融
液、14……内側収容体、15……昇降機構、16……原料、
18……単結晶、20……グラファイトサセプタ、22……支
持体、23……昇降機構、20a……溝、22a……突条、22b
……ネジ部。
FIG. 1 is a schematic configuration diagram showing one embodiment of the present invention, FIGS. 2 and 3 show another embodiment of the present invention, FIG. 2 is a schematic configuration diagram, and FIG. 3 is a plan view. FIG. 4 and FIG. 4 are explanatory views showing a conventional quartz crucible. 10 ... Outer container, 11 ... Quartz crucible, 13 ... Silicon melt, 14 ... Inner container, 15 ... Elevating mechanism, 16 ... Raw material,
18 …… single crystal, 20 …… graphite susceptor, 22 …… support, 23 …… elevating mechanism, 20a …… groove, 22a …… projection, 22b
...... Screw part.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】多重構造の石英ルツボを用いて、シリコン
単結晶の引上げ育成を行うと同時に、育成単結晶と同量
の原料シリコンを連続的に石英ルツボ内に供給するシリ
コン単結晶育成方法において、単結晶引上げ育成時に、
前記石英ルツボの最も内側の収容体をシリコン融液表面
に対して連続的に昇降させることを特徴とするシリコン
単結晶育成方法。
1. A method for growing a silicon single crystal in which a silicon single crystal is pulled up and grown by using a quartz crucible having a multiple structure, and at the same time, the same amount of raw material silicon as the grown single crystal is continuously fed into the quartz crucible. , During single crystal pull-up growth,
A method for growing a silicon single crystal, wherein the innermost container of the quartz crucible is continuously moved up and down with respect to the surface of the silicon melt.
【請求項2】多重構造の石英ルツボを用いて、シリコン
単結晶の引上げ育成を行なうと同時に、育成単結晶と同
量の原料シリコンを連続的に石英ルツボ内に供給するシ
リコン単結晶育成装置において、石英ルツボの内側収容
体を支持する支持体が、回転自在な外側収容体の外周
に、昇降自在にかつこの外側収容体とともに回転可能に
設けられる一方、前記支持体に、この支持体と係合して
支持体を昇降させる昇降機構が設けられたことを特徴と
するシリコン単結晶育成装置。
2. A silicon single crystal growing apparatus for simultaneously pulling and growing a silicon single crystal by using a quartz crucible having a multi-structure and simultaneously supplying the same amount of raw material silicon as the grown single crystal into the quartz crucible. A support for supporting the inner container of the quartz crucible is provided on the outer periphery of the rotatable outer container so as to be vertically movable and rotatable together with the outer container, while the support is engaged with the support. An apparatus for growing a silicon single crystal, characterized in that an elevating mechanism for elevating and lowering a support is provided.
JP13798487A 1987-06-01 1987-06-01 Method and apparatus for growing silicon single crystal Expired - Lifetime JPH085736B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13798487A JPH085736B2 (en) 1987-06-01 1987-06-01 Method and apparatus for growing silicon single crystal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13798487A JPH085736B2 (en) 1987-06-01 1987-06-01 Method and apparatus for growing silicon single crystal

Publications (2)

Publication Number Publication Date
JPS63303893A JPS63303893A (en) 1988-12-12
JPH085736B2 true JPH085736B2 (en) 1996-01-24

Family

ID=15211338

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13798487A Expired - Lifetime JPH085736B2 (en) 1987-06-01 1987-06-01 Method and apparatus for growing silicon single crystal

Country Status (1)

Country Link
JP (1) JPH085736B2 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02243587A (en) * 1989-03-17 1990-09-27 Kawasaki Steel Corp Pulling up single crystal and device therefor
JPH0791147B2 (en) * 1989-10-04 1995-10-04 川崎製鉄株式会社 Method of growing polycrystalline ingot
JP5439353B2 (en) * 2010-12-27 2014-03-12 新日鐵住金株式会社 SiC single crystal manufacturing apparatus and crucible used therefor

Also Published As

Publication number Publication date
JPS63303893A (en) 1988-12-12

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