JPH03261699A - Growth method of ZnSe single crystal - Google Patents
Growth method of ZnSe single crystalInfo
- Publication number
- JPH03261699A JPH03261699A JP5881290A JP5881290A JPH03261699A JP H03261699 A JPH03261699 A JP H03261699A JP 5881290 A JP5881290 A JP 5881290A JP 5881290 A JP5881290 A JP 5881290A JP H03261699 A JPH03261699 A JP H03261699A
- Authority
- JP
- Japan
- Prior art keywords
- znse
- single crystal
- polycrystal
- tip
- temperature
- 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
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000013078 crystal Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000000137 annealing Methods 0.000 abstract description 2
- 239000002775 capsule Substances 0.000 description 15
- 239000010453 quartz Substances 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000007796 conventional method Methods 0.000 description 8
- 239000000725 suspension Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
この発明は、ＺｎＳｅのバルク単結晶の成長方法に関し
、特に、青色発光素子（発光ダイオードおよび半導体レ
ーザなど）用の基板として良質なバルクＺｎＳｅ単結晶
を育成する方法に関するものである。Detailed Description of the Invention [Industrial Application Field] The present invention relates to a method for growing a bulk single crystal of ZnSe, and in particular, to a method for growing bulk single crystals of ZnSe, particularly for growing high quality bulk single crystals of ZnSe as a substrate for blue light emitting devices (light emitting diodes, semiconductor lasers, etc.). This invention relates to a method for growing crystals.
［従来の技術］
ＺｎＳｅのバルク単結晶を成長させる従来の方法として
、本出願人が特装車１−１９２．７９９に開示した方法
を挙げることができる。この方法は、ＣＶＤ法により合
成した多結晶ＺｎＳｅをゾーン４乙
アニーリングすることにより、ＺｎＳｅ単結ｔて行なう
方法である。この方法は、たとえば第３Ａ図に示される
ような装置を用い、ＺｎＳｅ多結晶を第３Ｂ図に示され
る温度分布の中にゆっくりと移動させてい（ものである
。第３Ａ図および第３Ｂ図を参照しながら、以下に簡単
にこの従来の方法について述べていく。[Prior Art] As a conventional method for growing a bulk single crystal of ZnSe, there is a method disclosed by the present applicant in Tokokusha 1-192.799. In this method, polycrystalline ZnSe synthesized by CVD is subjected to zone 4 annealing to form a single ZnSe bond. This method uses, for example, the apparatus shown in FIG. 3A, and slowly moves the ZnSe polycrystal into the temperature distribution shown in FIG. 3B. This conventional method will be briefly described below with reference to the following.
この装置において、棒状のＺｎＳｅ多結晶３１は、０．
１〜１００ＴｏｒｒのＡ「雰囲気３４にされた、石英カ
プセル３２内に収められている。In this device, the rod-shaped ZnSe polycrystal 31 has a diameter of 0.
It is housed in a quartz capsule 32 in an atmosphere 34 of 1 to 100 Torr.
この石英カプセル３２は、上下移動可能な懸架装置３３
に吊下げられ、図に示す矢印の方向に移動させられる。This quartz capsule 32 is mounted on a suspension device 33 that can be moved up and down.
and is moved in the direction of the arrow shown in the figure.
石英カプセル３２か移動する下方には、ヒータ３５が設
けられており、石英カプセル３２を周囲から加熱するよ
うになっている。従来の方法は、このような装置を一例
として用い、石英カプセル３２内のＺｎＳｅ多結晶３１
をその先端から加熱していき、単結晶に変えていくもの
である。このように単結晶に変えていくに際し、ＺｎＳ
ｅ多結晶３１は、第３Ｂ図に示すような温度分布中に移
動させられる。第３Ｂ図に示される温度分布は、室温〜
１００℃の低温部ＡＢから始まり、温度勾配が５０℃／
Ｃｍ〜２００℃／ ｃ ｍである昇温部ＢＣ１温度か７
００°Ｃ〜９００℃である高温部ＣＤ、温度勾配か一り
００℃／ ｃ ｍ〜−５０℃／ ｃ ｍである降温部Ｄ
Ｅおよびそれに続く室温〜１００℃の低温部ＥＦとから
構成されている。石英カプセル３２中のＺｎＳｅ多結晶
３１は、このような温度分布中を、ＡＢから順次矢印の
方向に従って、０．０５ｍｍ／ｄａｙ 〜５ｍｍ／ｄａ
ｙの速度で、移動させられる。移動によって、ＺｎＳｅ
多結晶３１は、固相を保ちながら単結晶に変化していく
。A heater 35 is provided below where the quartz capsule 32 moves, and heats the quartz capsule 32 from its surroundings. The conventional method uses such a device as an example, and the ZnSe polycrystal 31 inside the quartz capsule 32 is
The material is heated from its tip, turning it into a single crystal. When converting to single crystal in this way, ZnS
The e-polycrystal 31 is moved through a temperature distribution as shown in FIG. 3B. The temperature distribution shown in Figure 3B is from room temperature to
Starting from the low temperature part AB at 100℃, the temperature gradient is 50℃/
Cm ~ 200℃/cm Temperature rising part BC1 temperature or 7
High temperature part CD is 00°C to 900°C, and cooling part D is temperature gradient 00°C/cm to -50°C/cm.
E and a subsequent low temperature section EF ranging from room temperature to 100°C. The ZnSe polycrystal 31 in the quartz capsule 32 has a temperature distribution of 0.05 mm/day to 5 mm/day sequentially from AB in the direction of the arrow.
It is moved at a speed of y. By moving, ZnSe
The polycrystal 31 changes into a single crystal while maintaining its solid phase.
［発明か解決しようとする課題］
上述した従来の方法において、棒状のＺｎＳｅ多結晶の
形状は、特に強調されるところではなかった。[Problem to be Solved by the Invention] In the conventional method described above, the shape of the rod-shaped ZnSe polycrystal is not particularly emphasized.
従来の方法において、その具体例に従い、角柱形または
円柱形の多結晶を用い、単結晶の育成を行なったところ
、用いた多結晶の先端部で複数の核から単結晶の成長が
起こり、完全な単結晶か得られない場合が起こった。In the conventional method, when a single crystal was grown using a prismatic or cylindrical polycrystal according to the specific example, single crystal growth occurred from multiple nuclei at the tip of the polycrystal used, and it was not completely completed. There were cases where it was not possible to obtain a single crystal.
この発明の目的は、上述した問題点を解決し、再現性良
く単結晶を育成するＺｎＳｅ単結晶の育成方法を提供す
ることにある。An object of the present invention is to provide a method for growing a ZnSe single crystal that solves the above-mentioned problems and grows a single crystal with good reproducibility.
［課題を解決するための手段］
この発明のＺｎＳｅ単結晶の育成方法は、棒状のＺｎＳ
ｅ多結晶を加熱部を通過させていくことにより部分的に
アニーリングして、単結晶に変化させていくＺｎＳｅ単
結晶の育成方法において、棒状のＺｎＳｅ多結晶の先端
部が、略錐形であることを特徴としている。[Means for Solving the Problems] The method for growing ZnSe single crystals of the present invention includes rod-shaped ZnS
e In a method for growing a ZnSe single crystal in which polycrystal is partially annealed by passing through a heating section and transformed into a single crystal, the tip of the rod-shaped ZnSe polycrystal is approximately pyramid-shaped. It is characterized by
上記略錐形として、たとえば、略円錐形および略角錐形
を挙げることができる。また、略錐形の頂点の角度か６
０゛以内であれば、発明の目的をより効果的に達成する
ことができる。Examples of the above-mentioned substantially conical shape include a substantially conical shape and a substantially pyramidal shape. Also, the angle of the apex of the approximately conical shape is 6
If it is within 0, the purpose of the invention can be achieved more effectively.
［作用コ
この発明において、棒状のＺｎＳｅ多結晶の先端部を略
錐形にすることで、その先端を尖ったものにすれば、先
端から核が成長していくので、成長核を確実に１つとす
ることができる。したがって、従来のように複数の核か
ら単結晶が成長するおそれかなくなり、再現性良く単結
晶を育成できるようになる。[Operation] In this invention, if the tip of the rod-shaped ZnSe polycrystal is made into a substantially conical shape and the tip is made sharp, the nucleus will grow from the tip, so it is possible to ensure that the growth nucleus is only one. It can be done as one. Therefore, there is no fear that a single crystal will grow from a plurality of nuclei as in the conventional method, and it becomes possible to grow a single crystal with good reproducibility.
［実施例］
第１図に、この発明に従う棒状のＺｎＳｅ多結晶の形状
について、その−例を示す。このＺｎＳｅ多結晶１０は
、ＣＶＤ法で合成したものを、寸注か５ｍｍＸ５ｍｍＸ
５０ｍｍの直方形に切り出した後、その先端を加工した
ものである。また、その結晶粒径は、数１０μｍであっ
た。ＺｎＳｅ多結晶１０の先端部１１は、図に示すよう
に円錐形に加工され、その先端のテーバ角は６０゛にさ
れている。[Example] FIG. 1 shows an example of the shape of a rod-shaped ZnSe polycrystal according to the present invention. This ZnSe polycrystal 10 was synthesized by CVD method and was poured into a 5mm x 5mm x
After cutting into a 50 mm rectangular shape, the tip was processed. Moreover, the crystal grain size was several tens of micrometers. The tip 11 of the ZnSe polycrystal 10 is processed into a conical shape as shown in the figure, and the Taber angle of the tip is set to 60°.
以上のような形状のＺｎＳｅ多結晶を第２Ａ図に示すよ
うな装置を用い、単結晶に変えていった。The ZnSe polycrystal having the shape described above was converted into a single crystal using an apparatus as shown in FIG. 2A.
第２Ａ図に示す装置において、上述したＺｎＳｅ多結晶
１０は、石英カプセル１２内に収められている。また、
石英カプセル１２内は、０．１〜１００Ｔｏ ｒ ｒの
Ａｒ雰囲気１４にされている。図に示すようにＺｎＳｅ
多結晶１０が収められた石英カプセル１２は、上下移動
可能な懸架装置１３に吊下げられ、図に示す矢印の方向
に移動させられる。さらに、石英カプセル１２が移動す
る下方には、ヒータ１５が設けられており、石英カプセ
ル１２を周囲から加熱するようになっている。In the apparatus shown in FIG. 2A, the above-mentioned ZnSe polycrystal 10 is housed in a quartz capsule 12. Also,
Inside the quartz capsule 12, an Ar atmosphere 14 of 0.1 to 100 Torr is created. As shown in the figure, ZnSe
A quartz capsule 12 containing a polycrystal 10 is suspended from a vertically movable suspension device 13, and is moved in the direction of the arrow shown in the figure. Further, a heater 15 is provided below where the quartz capsule 12 moves, and heats the quartz capsule 12 from its surroundings.
このような装置を用い、石英カプセル１２内のＺｎＳｅ
多結晶１０を加熱していく際の温度分布は、第２Ｂ図に
示すようなものであった。すなわち、温度分布は、室ｌ
Ａ〜１００℃の低温部Ａ、 Ｂ、を始まりとし、温度勾
配が１５０°Ｃ／ｃｍの昇温部Ｂ、Ｃ，、温度が９００
℃である高温部Ｃ４Ｄ１、温度勾配か−１５０”Ｃ／
ｃ ｍである降温部り、Ｅ、およびそれに続く室温〜１
００℃の低温部Ｅ、Ｆ、とから構成されていた。Using such a device, ZnSe in the quartz capsule 12 is
The temperature distribution during heating of the polycrystal 10 was as shown in FIG. 2B. That is, the temperature distribution is
Starting from the low-temperature parts A and B with a temperature gradient of 150°C/cm, and the temperature rising parts B and C with a temperature gradient of 150°C/cm, the temperature is 900°C.
℃, high temperature part C4D1, temperature gradient -150"C/
The temperature drop zone, E, which is cm, and the subsequent room temperature ~1
It consisted of low-temperature parts E and F at 00°C.
このような温度分布中をＡ、Ｂ、を始まりとして移動さ
せていくにあたり、石英カプセル１２の降下速度は、２
．０ｍｍ／ｄａｙとした。When moving through such a temperature distribution starting from A and B, the descending speed of the quartz capsule 12 is 2.
．． It was set to 0 mm/day.
石英カプセル１２を降下させて、上記温度分布中を移動
させることにより単結晶化を行なった結果、ＺｎＳｅ単
結晶か再現性良く得られた。Single crystallization was performed by lowering the quartz capsule 12 and moving it through the above temperature distribution, and as a result, a ZnSe single crystal was obtained with good reproducibility.
［発明の効果］
以上説明したように、この発明に従って大型のＺｎＳｅ
単結晶を再現性良く形成することかできる。したかって
この発明は、特に、青色発光ダイオードおよび青色半導
体レーザ等の材料として強く期待されるＺｎＳｅ単結晶
の作成に非常に効果的である。[Effect of the invention] As explained above, according to this invention, large-sized ZnSe
Single crystals can be formed with good reproducibility. Therefore, the present invention is particularly effective in producing ZnSe single crystals, which are highly expected to be used as materials for blue light emitting diodes, blue semiconductor lasers, and the like.
第１図は、この発明に従う棒状のＺｎＳｅ多結晶の形状
について、その−例を示す斜視図である。
第２Ａ図は、この発明を実施するにあたり、用いられた
装置の一例を示す断面図である。
第２Ｂ図は、この発明を実施するにあたり、ＺｎＳｅ多
結晶を加熱して単結晶に移行させる際の温度分布を示す
図である。
第３Ａ図は、従来の方法に用いられる装置の一例を示す
断面図である。
第３Ｂ図は、従来の方法に用いられる温度分布を示す図
である。
図において、１０および３１はＺｎＳｅ多結晶、１１は
先端部、１２および３２は石英カプセル、１３および３
３は懸架装置、１４および３４はＡｒ雰囲気、１５およ
び３５はヒータを示す。FIG. 1 is a perspective view showing an example of the shape of a rod-shaped ZnSe polycrystal according to the present invention. FIG. 2A is a sectional view showing an example of an apparatus used in carrying out the present invention. FIG. 2B is a diagram showing the temperature distribution when ZnSe polycrystal is heated to transform it into a single crystal in carrying out the present invention. FIG. 3A is a cross-sectional view showing an example of an apparatus used in the conventional method. FIG. 3B is a diagram showing the temperature distribution used in the conventional method. In the figure, 10 and 31 are ZnSe polycrystals, 11 is the tip, 12 and 32 are quartz capsules, 13 and 3
3 is a suspension device, 14 and 34 are Ar atmospheres, and 15 and 35 are heaters.
Claims (1)
により部分的にアニーリングして、単結晶に変化させて
いくＺｎＳｅ単結晶の育成方法において、 前記棒状のＺｎＳｅ多結晶の先端部が、略錐形であるこ
とを特徴とするＺｎＳｅ単結晶の育成方法。[Claims] A method for growing a ZnSe single crystal in which a rod-shaped ZnSe polycrystal is partially annealed by passing through a heating section to transform it into a single crystal, comprising: A method for growing a ZnSe single crystal, characterized in that the tip has a substantially pyramidal shape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5881290A JPH03261699A (en) | 1990-03-09 | 1990-03-09 | Growth method of ZnSe single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5881290A JPH03261699A (en) | 1990-03-09 | 1990-03-09 | Growth method of ZnSe single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03261699A true JPH03261699A (en) | 1991-11-21 |
Family
ID=13095023
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5881290A Pending JPH03261699A (en) | 1990-03-09 | 1990-03-09 | Growth method of ZnSe single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03261699A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1345480A2 (en) | 2002-03-15 | 2003-09-17 | Dowa Mining Co., Ltd. | Ceramic circuit board and power module |
| CN103194802A (en) * | 2012-01-05 | 2013-07-10 | 昆山中辰矽晶有限公司 | Tempering method of crystal bar surface, and crystal bar |
-
1990
- 1990-03-09 JP JP5881290A patent/JPH03261699A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1345480A2 (en) | 2002-03-15 | 2003-09-17 | Dowa Mining Co., Ltd. | Ceramic circuit board and power module |
| CN103194802A (en) * | 2012-01-05 | 2013-07-10 | 昆山中辰矽晶有限公司 | Tempering method of crystal bar surface, and crystal bar |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH0637354B2 (en) | Method and apparatus for growing silicon carbide single crystal | |
| JPH03261699A (en) | Growth method of ZnSe single crystal | |
| US3360405A (en) | Apparatus and method of producing semiconductor rods by pulling the same from a melt | |
| JPH04104988A (en) | Growth of single crystal | |
| JPH0748200A (en) | Single crystal manufacturing method | |
| JP2574618B2 (en) | Crystal growth method and crucible for crystal growth | |
| JP2004203721A (en) | Apparatus and method for growing single crystal | |
| JP2542434B2 (en) | Compound semiconductor crystal manufacturing method and manufacturing apparatus | |
| JP2733898B2 (en) | Method for manufacturing compound semiconductor single crystal | |
| JP2622274B2 (en) | Single crystal growth method | |
| JPH11274537A (en) | Manufacture of polycrystalline silicon of large grain size | |
| JPH0648898A (en) | Production of silicon carbide single crystal | |
| JPH0259485A (en) | Growing method for crystal | |
| JPS60226495A (en) | Method for growing lanthanum hexaboride single crystal | |
| JP2810975B2 (en) | Single crystal manufacturing method | |
| JPH05262596A (en) | Production of single crystal of lithium tetraborate | |
| JPH10251099A (en) | Production of lithium tetraborate single crystal | |
| JPH0341440B2 (en) | ||
| JPH042683A (en) | Production of rutile single crystal | |
| JPH0710674A (en) | Method for growing inorganic compound signal crystal | |
| JPH06199600A (en) | Method for growing beta-barium borate single crystal | |
| JPS60118700A (en) | Production of semiconductor crystal | |
| JPH0867593A (en) | Single crystal growth method | |
| JPS6027677A (en) | Production of solid solution single crystal by floating zone melting method | |
| JPH0369880B2 (en) |