JPS6126592A - Crystal growing device - Google Patents
Crystal growing deviceInfo
- Publication number
- JPS6126592A JPS6126592A JP14910984A JP14910984A JPS6126592A JP S6126592 A JPS6126592 A JP S6126592A JP 14910984 A JP14910984 A JP 14910984A JP 14910984 A JP14910984 A JP 14910984A JP S6126592 A JPS6126592 A JP S6126592A
- Authority
- JP
- Japan
- Prior art keywords
- melt
- crystal
- substances
- replenishment
- supply
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は結晶成長中に枯渇しやすい成分を融液(もしく
は溶液)に補給する手段を具備する引き上げ式結晶成長
装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a pulling crystal growth apparatus equipped with means for replenishing a melt (or solution) with components that are easily depleted during crystal growth.
結晶成長中に、融液中の偏析係数の大きい成分が次第に
枯渇して、成長する結晶の組成変動を生じ、その結果結
晶の利用効率を著しく悪くする。During crystal growth, components with large segregation coefficients in the melt are gradually depleted, causing compositional fluctuations in the growing crystal, resulting in a significant decrease in the utilization efficiency of the crystal.
そのために該成分物質を補給する方法が種々試みられて
いる。For this purpose, various methods of replenishing the component substances have been attempted.
第3図は従来例による成分補給手段を具備する結晶成長
装置の断面図である。FIG. 3 is a sectional view of a crystal growth apparatus equipped with a conventional component supply means.
図示の装置は本発明者により提案された装置で、1はカ
ーボン等の導電性材料よりなる円筒状のルツボ側壁部、
2は窒化ボロン(PBN)等絶縁性材料よりなるルツボ
底部、3は融液、4は成長した結晶、4′は種結晶であ
る。The illustrated device is a device proposed by the present inventor, in which 1 is a cylindrical crucible side wall made of a conductive material such as carbon;
2 is a crucible bottom made of an insulating material such as boron nitride (PBN), 3 is a melt, 4 is a grown crystal, and 4' is a seed crystal.
補給すべき成分を含有し、゛かっ融点が成長用の融液よ
り高い補給物質5を融液3に接触させ、補給物質5ど融
液3の間に電流を流して補給すべき成分を融液3中に溶
は込ませる。A replenishment substance 5 containing the components to be replenished and having a higher melting point than the growth melt is brought into contact with the melt 3, and a current is passed between the replenishment substance 5 and the melt 3 to melt the components to be replenished. Let it dissolve in liquid 3.
そのために、補給物質5とルツボ側壁部1もしくは種結
晶4′間に、電源6を切換スイッチ7、電流検出部9を
介して接続する。For this purpose, a power source 6 is connected between the replenishment material 5 and the crucible side wall 1 or the seed crystal 4' via a changeover switch 7 and a current detection section 9.
電流検出部9より帰還回路10を経て駆動装置8を駆動
し、補給物質5を融液3中に押し出す。The drive device 8 is driven by the current detection unit 9 via the feedback circuit 10, and the replenishment substance 5 is pushed out into the melt 3.
以上のような装置では補給物質5が半導体結晶であるよ
うな場合、比抵抗等の電気的性質が局部的に異なること
により、ここを流れる電流に場所的な不均一を生じ、そ
の結果として補給物質5の溶は出しが場所的に一様でな
くなり、融液3にこ接する部分が非対称の凹凸のある形
状となり、そのため融液の対流に乱れを生じ、成長する
結晶が次第にゆがむとか、結晶に転位が入り易くなる等
の不都合を生ずることがあった。In the device described above, when the replenishment material 5 is a semiconductor crystal, local differences in electrical properties such as specific resistance cause local non-uniformity in the current flowing through the material, and as a result, the replenishment The melting of the substance 5 becomes uneven in places, and the part that comes in contact with the melt 3 has an asymmetrical uneven shape, which causes turbulence in the convection of the melt, causing the growing crystal to become gradually distorted, and the crystal to grow. This may cause problems such as the tendency for dislocations to occur.
補給物質の溶は込みの場所的な不均一による形状異常が
、融液中の対流に悪影響をおよぼし、均一な結晶が得ら
れ難い。Shape abnormalities due to local non-uniformity in the melting of the replenishing material adversely affect convection in the melt, making it difficult to obtain uniform crystals.
上記問題点の解決は、補給すべき成分を含有する補給物
質をルツボに対して相対的に移動できる機構と、該ルツ
ボに保持した融液もしくは溶液と該補給物質との間に電
流を流す手段を具備する結晶成長装置において、複数の
補給物質を有し、がつ各補給物質に流す電流と時間の積
が一定となるようにする電流切換手段を有する本発明に
よる結晶成長装置により達成される。The solution to the above problem is to provide a mechanism that can move the replenishment substance containing the components to be replenished relative to the crucible, and a means for passing an electric current between the melt or solution held in the crucible and the replenishment substance. This is achieved by the crystal growth apparatus according to the present invention, which has a plurality of replenishment substances and has current switching means for making the product of the current and time flowing through each replenishment substance constant. .
本発明は補給物質と融液間に電流を流したとき、融液に
溶は出す補給物質の量は電荷量に比例することと、補給
物質の寸法が小さくなればなるほど補給物質内の特性の
不均一の絶対量は小さくなるため、電流を流したときの
溶は出しによる補給物質の形状変化の絶対量は小さくな
ることに着目して、補給物質を複数に分は各の寸法を小
ざくして、これに流す電流と時間の積を一定にすること
により、各補給物質の形状変化の絶対量を減らすととも
に、各補給物質の融液と接触する部分の全体の形状が相
対的に一定となるようにして融液の対流を安定化するよ
うにしたものである。The present invention is based on the fact that when a current is passed between the replenishment material and the melt, the amount of the replenishment material dissolved into the melt is proportional to the amount of electric charge, and that the smaller the size of the replenishment material, the better the characteristics within the replenishment material. Since the absolute amount of non-uniformity is small, the absolute amount of change in the shape of the replenishment material due to dissolution when electric current is applied will be small. By making the product of the current applied to this and the time constant, the absolute amount of change in shape of each replenishment substance is reduced, and the overall shape of the part of each replenishment substance that comes into contact with the melt remains relatively constant. This is to stabilize the convection of the melt.
第2図は補給物質の寸法と変形量の関係を説明する図で
ある。FIG. 2 is a diagram illustrating the relationship between the dimensions of the replenishment material and the amount of deformation.
第2図(ajにおいて、単一の補給物質のときの、変形
の絶対量をdとする。FIG. 2 (in aj, let d be the absolute amount of deformation when a single supplementary substance is used.
第2図(blにおいて、上記単一の補給物質を1次元的
にn個に等分して先端を揃えたときの、変形の絶対量は
d / nになる。In FIG. 2 (bl), when the single replenishment substance is one-dimensionally divided into n pieces and the tips are aligned, the absolute amount of deformation is d/n.
第1図は本発明の実施例を示す成分補給手段を具備する
結晶成長装置の断面図と平面図である。FIG. 1 is a cross-sectional view and a plan view of a crystal growth apparatus equipped with component replenishment means, showing an embodiment of the present invention.
この装置はInAsNP I −XI Ga、lIn
1− XASI GaAs、lp、−X等の3元化合物
半導体結晶の引き上げに適する。This device is InAsNP I-XI Ga, lIn
1-XASI Suitable for pulling ternary compound semiconductor crystals such as GaAs, lp, -X, etc.
閏において、ルツボはカーボン等の導電性物質よりなる
円筒状側壁部1と、PBN等絶縁性材料よりなり、中心
部に結晶の回転軸に対して対称の位置に配置した7個の
貫通孔を有する底部2とを上下に重ねて構成される。In the crucible, the crucible has a cylindrical side wall 1 made of a conductive material such as carbon, and an insulating material such as PBN, and has seven through holes arranged symmetrically with respect to the axis of rotation of the crystal in the center. It is constructed by stacking the bottom part 2 with the bottom part 2 on top of the other.
各々の貫通孔に嵌合するように7個の補給物質5を挿入
し、これらは全体として駆動装置8により融液3中に押
し出され、またそれぞれ切換スイッチ11を通じて電源
6に接続されるようになっている。Seven replenishment substances 5 are inserted so as to fit into each through hole, and these are pushed out into the melt 3 by a drive device 8 as a whole, and are connected to a power source 6 through a changeover switch 11, respectively. It has become.
補給物質5はInAsxP+−xの場合はInP 。Replenishment substance 5 is InP in the case of InAsxP+-x.
Ga、In+4.ΔSの場合はGaAs、、GaASx
P+−xの場合はGaPを用いるとよい。Ga, In+4. For ΔS, GaAs, , GaASx
In the case of P+-x, GaP is preferably used.
成長にあたっては、まず補給物質5の代わりに同じ外形
のカーボンもしくはPBNの棒でルツボの底部2の貫通
孔を塞ぎ、ルツボ1,2に融液の材料をそれぞれ秤量し
て入れ、温度を上げて溶融する。For growth, first plug the through hole in the bottom 2 of the crucible with a rod of carbon or PBN of the same external shape instead of the replenishment material 5, weigh the melt materials into the crucibles 1 and 2, and raise the temperature. melt.
ここで一旦冷却しカーボンもしくはPBHの棒に代わり
、InPやGqAsあるいはGaPよりなる補給物質5
.を挿入し、再度温度を上げて溶融した後、種結晶4′
を融液3に浸け、回転しながら徐々に引き上げ結晶4を
大きく成長させる。Once cooled, a replenishing material 5 made of InP, GqAs, or GaP is added instead of the carbon or PBH rod.
.. Insert the seed crystal 4' and raise the temperature again to melt it.
is immersed in the melt 3 and gradually pulled up while rotating to grow the crystal 4 to a large size.
この場合補給物質5は融液より高い融点のものを用いる
ので、この時点で溶けてしまうことはない。In this case, the replenishment substance 5 used has a melting point higher than that of the melt, so it will not melt at this point.
結晶を引き上げるに従って、融液中の偏析係数の大きい
成分、例えば融液3がInAsxP+−xの場合はP
< GaJr++−xAsの場合はGa、、 GaAs
、P、−、の場合はPが枯渇してくるので、これを補う
ように電源6から補給物質5、融液3、第1のルツボl
もしくは結晶4の径路に電流を流して補給物質5を融液
3中へ溶は込ませるようにする。このとき複数の補給物
質5の各々に流れる電流と時間の積が等しくなるように
切換スイッチ11で切り換える。As the crystal is pulled up, components with large segregation coefficients in the melt, for example, P when melt 3 is InAsxP+-x,
< GaJr++-xAs, Ga, GaAs
, P, -, since P will be depleted, the supply material 5, melt 3, and first crucible l will be supplied from the power source 6 to compensate for this.
Alternatively, an electric current is passed through the path of the crystal 4 so that the replenishment substance 5 is dissolved into the melt 3. At this time, the changeover switch 11 is used to make the product of the current flowing through each of the plurality of replenishment substances 5 equal to the time.
電tA6に定電流源を用いれば、一定時間毎にスイッチ
を切り換えればよい。切り換えの時間は短いほど、各補
給物質5間の溶は出し量の時間的なバラツキが小さくな
る。If a constant current source is used for the voltage tA6, the switch may be changed over at regular intervals. The shorter the switching time, the smaller the temporal variation in the amount of elution between the replenishment substances 5.
溶は出した分だけ駆動装置8により、補給物質5を押し
出し、常にその先端がルツボの底面にくるようにすると
、融液3の形状が変わらないので、融液中の流れは一定
となり乱流を生ずることはない。If the replenishment material 5 is pushed out by the driving device 8 by the amount of melt released, and the tip is always placed at the bottom of the crucible, the shape of the melt 3 will not change, so the flow in the melt will be constant and turbulent. will not occur.
単一補給物質を使用していた従来例では、補給物質内の
ムラが甚だしい場合は、融液に乱流を生ずるだけでなく
ルツボ底部より融液が漏れだすこともあるが、本発明に
よる装置ではこのようなことはなく、安定した結晶成長
が行える。In the conventional example in which a single replenishment material was used, if there were severe unevenness in the replenishment material, it would not only cause turbulence in the melt but also cause the melt to leak from the bottom of the crucible. This does not occur and stable crystal growth can be achieved.
実施例では7木の丸棒状補給物質を用いたが、この数を
増やすほど効果は大きい。In the example, seven wooden round rod-shaped replenishment substances were used, but the greater the number, the greater the effect.
また実施例では補給物質5をルツボの底部2から融液に
接触させたが、融液表面より接触させてもよい。Further, in the embodiment, the replenishment substance 5 was brought into contact with the melt from the bottom 2 of the crucible, but it may be brought into contact from the surface of the melt.
また実施例では融液からの成長に適用したが、本発明は
溶液からの成長にも適用できる。Furthermore, although the embodiments have been applied to growth from a melt, the present invention can also be applied to growth from a solution.
以上詳細に説明したように本発明によれば、融液の対流
を乱すことなく、融液中で枯渇し易い成分を補給できる
ので、均一で良質の結晶を得ることができる。As described in detail above, according to the present invention, components that are easily depleted in the melt can be replenished without disturbing the convection of the melt, so that uniform and high-quality crystals can be obtained.
第1図は本発明の実施例を示す成分補給手段を具備する
結晶成長装置の断面図と平面図、第2図(a)および(
b)は補給物質の寸法と変形量の関係を説明する図、
第3図は従来例による成分補給手段を具備する結晶成長
装置の断面図である。
図において、
1はルツボ側壁部、 2はルツボ底部、3は融液、
4は成長した結晶、4′ば種結晶、 5は
補給物質、6は電源、 7.11は切換スイ
ッチ、8は駆動装置、 9は電流検出部、10は
帰還回路
を示す。
茅1 A
阜2珂
(幻 (b)FIG. 1 is a cross-sectional view and a plan view of a crystal growth apparatus equipped with component replenishment means showing an embodiment of the present invention, and FIGS. 2(a) and (
b) is a diagram illustrating the relationship between the dimensions of the replenishing material and the amount of deformation, and FIG. 3 is a sectional view of a crystal growth apparatus equipped with a conventional component replenishing means. In the figure, 1 is the crucible side wall, 2 is the crucible bottom, 3 is the melt,
4 is a grown crystal, 4' is a seed crystal, 5 is a supply substance, 6 is a power source, 7.11 is a changeover switch, 8 is a drive device, 9 is a current detection section, and 10 is a feedback circuit. Chi 1 A Fu 2 Ka (phantom (b)
Claims (2)
して相対的に移動できる機構と、該ルツボに保持した融
液もしくは溶液と該補給物質との間に電流を流す手段を
具備する結晶成長装置において、複数の補給物質を有し
、かつ各補給物質に流す電流と時間の積が一定となるよ
うにする電流切換手段を有することを特徴とする結晶成
長装置。(1) A crystal that is equipped with a mechanism that can move a replenishment substance containing the components to be replenished relative to a crucible, and a means for passing an electric current between the melt or solution held in the crucible and the replenishment substance. 1. A crystal growth apparatus comprising a plurality of replenishment substances and current switching means for making the product of current and time passed through each replenishment substance constant.
置に配置してなることを特徴とする特許請求の範囲第1
項記載の結晶成長装置。(2) Claim 1, characterized in that a plurality of replenishing substances are arranged at symmetrical positions with respect to the rotation axis of the crystal.
The crystal growth apparatus described in Section 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14910984A JPS6126592A (en) | 1984-07-18 | 1984-07-18 | Crystal growing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14910984A JPS6126592A (en) | 1984-07-18 | 1984-07-18 | Crystal growing device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6126592A true JPS6126592A (en) | 1986-02-05 |
Family
ID=15467895
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14910984A Pending JPS6126592A (en) | 1984-07-18 | 1984-07-18 | Crystal growing device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6126592A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0211166U (en) * | 1988-07-07 | 1990-01-24 |
-
1984
- 1984-07-18 JP JP14910984A patent/JPS6126592A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0211166U (en) * | 1988-07-07 | 1990-01-24 |
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