JPH01242499A - Method of decreasing dislocation of znse single crystal - Google Patents
Method of decreasing dislocation of znse single crystalInfo
- Publication number
- JPH01242499A JPH01242499A JP7119388A JP7119388A JPH01242499A JP H01242499 A JPH01242499 A JP H01242499A JP 7119388 A JP7119388 A JP 7119388A JP 7119388 A JP7119388 A JP 7119388A JP H01242499 A JPH01242499 A JP H01242499A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- crystal
- znse
- znse single
- heat treatment
- 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 47
- 238000000034 method Methods 0.000 title claims abstract description 9
- 230000003247 decreasing effect Effects 0.000 title abstract 2
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000012298 atmosphere Substances 0.000 abstract description 7
- 239000011261 inert gas Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000859 sublimation Methods 0.000 abstract description 4
- 230000008022 sublimation Effects 0.000 abstract description 4
- 230000002542 deteriorative effect Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Substances OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000007704 transition Effects 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〕
本願発明はＺｎＳｅ単結晶の転位減少法に関し、特に高
温熱処理によるＺｎＳｅ単結晶の転位減少法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for reducing dislocations in a ZnSe single crystal, and particularly to a method for reducing dislocations in a ZnSe single crystal by high-temperature heat treatment.
ＺｎＳｅ結晶は、従来種々の結晶をエピタキシャル成長
させるための基板用材料等として使用されている。該エ
ピタキシャル成長の基板材料としては、基板の結晶性（
例えば転移等）に反映した結晶が該基板上に成長するた
め、結晶性の良いものが望まれていた。ZnSe crystals have conventionally been used as substrate materials for epitaxial growth of various crystals. As the substrate material for epitaxial growth, the crystallinity of the substrate (
For example, since crystals reflecting transitions (for example, dislocations, etc.) grow on the substrate, a material with good crystallinity has been desired.
しかしながらＺｎＳｅ等の単結晶作製においては通常転
位等の欠陥が発生しやすく、特にＺｎＳｅ結晶における
無転位結晶はいまだ得られていない。However, in the production of single crystals such as ZnSe, defects such as dislocations are usually likely to occur, and in particular, dislocation-free ZnSe crystals have not yet been obtained.
−旦作製された単結晶中の欠陥は、恒温焼鈍、熱サイク
ル焼鈍等の方法によって減少させることができ、より良
質な単結晶を作製するために利用されている。例えばｍ
−ｖ族化合物結晶、特にＧａＡｓ結晶に対しても高温状
態に保持することが転位減少に効果があることが知られ
ている。（例えばＭａｔｅｒａｌｓ Ｌｅｔｔｅｒ ５
＋ １９６ ）しかしながら上記ＺｎＳｅ単結晶につい
て上記恒温焼鈍、熱サイクル焼鈍等の手段によって単結
晶中の転移を減少させる試みは今だ行なわれておらず、
又この様な手段によってＺｎＳｅ単結晶中の欠陥を減少
することができたという報告は今だなされていない。- Defects in single crystals once produced can be reduced by methods such as constant temperature annealing and thermal cycle annealing, which are used to produce higher quality single crystals. For example m
It is known that maintaining a -V group compound crystal, especially a GaAs crystal, at a high temperature is effective in reducing dislocations. (For example, Materials Letter 5
+196) However, no attempt has been made to reduce the dislocations in the single crystal of ZnSe by means of constant temperature annealing, thermal cycle annealing, etc.
Furthermore, there has been no report that defects in ZnSe single crystals can be reduced by such means.
本発明は、従来知られていないＺｎＳｅ単結晶の転位減
少法を提供するものであって、転位密度の小さい良質の
ＺｎＳｅ単結晶の製造を可能とするものである。The present invention provides a conventionally unknown method for reducing dislocations in ZnSe single crystals, and makes it possible to produce high-quality ZnSe single crystals with low dislocation density.
本発明は、ＺｎＳｅ単結晶を不活性ガス雰囲気下の６０
０〜８００℃で１０時間以上保持するＺｎＳｅ単結晶の
転位密度の減少法である。In the present invention, ZnSe single crystal is grown at 60°C under an inert gas atmosphere.
This is a method of reducing the dislocation density of a ZnSe single crystal by holding it at 0 to 800°C for 10 hours or more.
本発明においては、ＺｎＳｅ単結晶を不活性ガス中で加
熱しているが、例えば０２等の活性ガス雰囲気下で加熱
するとＺｎＳｅ表面に酸化物等の不純物を形成し、Ｚｎ
Ｓｅ単結晶の品質を低下させることになる。In the present invention, the ZnSe single crystal is heated in an inert gas, but when heated in an active gas atmosphere such as 02, impurities such as oxides are formed on the ZnSe surface, and the ZnSe single crystal is heated in an inert gas atmosphere.
This will reduce the quality of the Se single crystal.
又加熱温度は６００〜８００℃であるが、該温度が６０
０°Ｃより低いと転位密度を減少させる効果がなく、又
８００℃より高いと昇華により単結晶が欠なわれていく
様になる。The heating temperature is 600 to 800°C, but if the temperature is 60°C
If it is lower than 0°C, there is no effect of reducing the dislocation density, and if it is higher than 800°C, single crystals will be lost due to sublimation.
又該温度における保持時間は１０時間以上とすることが
必要である。転位密度を減少させられる処理時間は、結
晶の完全性、処理温度、結晶の大きさ等によって変化す
るが、６００〜８００°Ｃの温度で処理を行なう本発明
においては１０時間以上保持しないと本発明の効果は現
れない。Further, it is necessary that the holding time at this temperature be 10 hours or more. The treatment time required to reduce the dislocation density varies depending on the completeness of the crystal, the treatment temperature, the size of the crystal, etc., but in the present invention, where the treatment is carried out at a temperature of 600 to 800°C, it is necessary to hold the treatment for more than 10 hours. The effect of the invention does not appear.
上記熱処理を行なったＺｎＳｅ単結晶は、室温に冷却さ
れて切断石層等を行なって前記エピタキシャル成長用基
板等に加工されるが、該室温への冷却は３°Ｃ／ｍｉｎ
以下の冷却速度で冷却することが好ましい。該冷却速度
が３’Ｃ／ｍｉｎより速くなると、冷却時の熱歪に基づ
いてせっかく転位密度を減少させたＺｎＳｅ単結晶中に
転移を形成するおそれがある。The ZnSe single crystal subjected to the above heat treatment is cooled to room temperature and processed into the epitaxial growth substrate etc. by cutting a stone layer, etc., but the cooling to room temperature is performed at a rate of 3°C/min.
It is preferable to cool at the following cooling rate. If the cooling rate is faster than 3'C/min, there is a risk that dislocations will be formed in the ZnSe single crystal whose dislocation density has been reduced due to thermal strain during cooling.
本発明によれば、不活性ガス雰囲気下で加熱を行なって
いるため、ＺｎＳｅ単結晶を変質させることなく、又昇
華等が激しくなることなく熱処理が行なえる。又６００
〜８００℃の温度で１０時間以上熱処理を行なうことに
よって結晶中の歪を緩和し、それにともなって転位密度
の低下および均一化が行なわれる。According to the present invention, since heating is performed under an inert gas atmosphere, heat treatment can be performed without altering the ZnSe single crystal or causing severe sublimation. 600 again
By performing heat treatment at a temperature of ~800° C. for 10 hours or more, strain in the crystal is relaxed, and dislocation density is accordingly reduced and made uniform.
ＺｎＳｅ（１１１）ウェハについて実施した例について
記載する。成長結晶から（１１１）面に対して平行に任
意の厚さに切り出したものを成形し、ラッピング、ポリ
ッシングを行ない、最後に加工歪を臭、素−メタノール
液等で取り除いた。また、不活性ガスとしては窒素を用
いた。該結晶を洗浄済みの石英ボートにのせ窒素雰囲気
炉に入れ徐々に温度を上げ７００°Ｃまで昇温した。こ
のときの窒素流量は１００ｃｃ／ｍｉｎ程度である。An example performed on a ZnSe (111) wafer will be described. The grown crystal was cut parallel to the (111) plane to a desired thickness, then molded, lapped and polished, and finally, processing distortion was removed using an odor, base-methanol solution, or the like. Further, nitrogen was used as the inert gas. The crystals were placed on a cleaned quartz boat and placed in a nitrogen atmosphere furnace to gradually raise the temperature to 700°C. The nitrogen flow rate at this time is about 100 cc/min.
この条件下で２３時間置き、その後３℃／ｍｉｎの降温
速度で室温まで冷却した。It was left under these conditions for 23 hours, and then cooled to room temperature at a rate of 3° C./min.
この結晶の処理前と処理後の結晶性を比較したものが、
第１表である。その評価法としてはエッチピットデンシ
ティ、Ｘ線２結晶回折法による、強度曲線全半値幅を用
いた。A comparison of the crystallinity of this crystal before and after treatment is as follows.
This is Table 1. As the evaluation method, etch pit density and full width at half maximum of the intensity curve by X-ray two-crystal diffraction method were used.
第１表より明らかに熱処理をほどこしたものはエッチピ
ットデンシティ、Ｘ線の半値幅が変化しており、結晶性
が向上していることがわかる。From Table 1, it is clear that the etch pit density and X-ray half width of the heat-treated samples change, indicating that the crystallinity is improved.
第 １ 表
〔発明の効果〕
本発明によれば、実施例からもあきらかな通り、ＺｎＳ
ｅ単結晶の転位密度を十分減少させることができ、より
高品質のＺｎＳｅ単結晶を作製することができる。又本
発明によって処理したＺｎＳｅ車結晶をエピタキシャル
成長用基板として用いれば、欠陥の少ない各種結晶を得
ることができ、高性能のデバイスを作製することができ
る。Table 1 [Effects of the invention] According to the present invention, as is clear from the examples, ZnS
The dislocation density of the e single crystal can be sufficiently reduced, and a higher quality ZnSe single crystal can be produced. Furthermore, if the ZnSe wheel crystal treated according to the present invention is used as a substrate for epitaxial growth, various crystals with few defects can be obtained, and high-performance devices can be manufactured.
Claims (2)
８００℃で１０時間以上保持するＺｎＳｅ単結晶の転位
減少法。(1) ZnSe single crystal was heated to 600 ~
A method for reducing dislocations in a ZnSe single crystal held at 800°C for 10 hours or more.
以下の速度で降温する請求項１項記載のＺｎＳｅ単結晶
の転位減少法。(2) 3℃/min from a heat treatment temperature of 600 to 800℃
A method for reducing dislocations in a ZnSe single crystal according to claim 1, wherein the temperature is lowered at a rate of:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7119388A JPH01242499A (en) | 1988-03-25 | 1988-03-25 | Method of decreasing dislocation of znse single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7119388A JPH01242499A (en) | 1988-03-25 | 1988-03-25 | Method of decreasing dislocation of znse single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01242499A true JPH01242499A (en) | 1989-09-27 |
Family
ID=13453587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7119388A Pending JPH01242499A (en) | 1988-03-25 | 1988-03-25 | Method of decreasing dislocation of znse single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01242499A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980018445A (en) * | 1996-08-12 | 1998-06-05 | 구라우치 노리타카 | Heat treatment method of YSN crystal |
| JP2007204324A (en) * | 2006-02-02 | 2007-08-16 | Tokyo Denpa Co Ltd | Manufacturing method of high purity zinc oxide single crystal, and high purity zinc oxide single crystal |
| CN103590112A (en) * | 2013-11-18 | 2014-02-19 | 北京雷生强式科技有限责任公司 | Post-processing method of iron-doped zinc selenide laser crystal |
-
1988
- 1988-03-25 JP JP7119388A patent/JPH01242499A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980018445A (en) * | 1996-08-12 | 1998-06-05 | 구라우치 노리타카 | Heat treatment method of YSN crystal |
| JP2007204324A (en) * | 2006-02-02 | 2007-08-16 | Tokyo Denpa Co Ltd | Manufacturing method of high purity zinc oxide single crystal, and high purity zinc oxide single crystal |
| CN103590112A (en) * | 2013-11-18 | 2014-02-19 | 北京雷生强式科技有限责任公司 | Post-processing method of iron-doped zinc selenide laser crystal |
| CN103590112B (en) * | 2013-11-18 | 2016-03-30 | 北京雷生强式科技有限责任公司 | A kind of post-treating method of iron-doped zinc selenide laser crystals |
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