JPS6374993A - Treatment of melt for crystal growth - Google Patents
Treatment of melt for crystal growthInfo
- Publication number
- JPS6374993A JPS6374993A JP22023186A JP22023186A JPS6374993A JP S6374993 A JPS6374993 A JP S6374993A JP 22023186 A JP22023186 A JP 22023186A JP 22023186 A JP22023186 A JP 22023186A JP S6374993 A JPS6374993 A JP S6374993A
- Authority
- JP
- Japan
- Prior art keywords
- melt
- gas
- crystal growth
- boat
- heat
- 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.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 29
- 238000011282 treatment Methods 0.000 title description 6
- 239000000155 melt Substances 0.000 claims abstract description 20
- 239000012535 impurity Substances 0.000 claims abstract description 13
- 239000010409 thin film Substances 0.000 claims abstract description 13
- 238000001451 molecular beam epitaxy Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- 230000008020 evaporation Effects 0.000 abstract description 15
- 238000001704 evaporation Methods 0.000 abstract description 15
- 239000010453 quartz Substances 0.000 abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910017009 AsCl3 Inorganic materials 0.000 abstract description 5
- OEYOHULQRFXULB-UHFFFAOYSA-N arsenic trichloride Chemical compound Cl[As](Cl)Cl OEYOHULQRFXULB-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 229910001218 Gallium arsenide Inorganic materials 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 9
- 238000007796 conventional method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、分子線エピタキシー法による結晶成長方法
に関し、特に半導体デバイスの材料である結晶成長用メ
ルトの処理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 crystals by molecular beam epitaxy, and particularly to a method for treating a melt for crystal growth, which is a material for semiconductor devices.
従来、分子線エピタキシー法による結晶成長方法におい
て、材料源となるＧａは固形のＧａを蒸発用るつぼに入
れ、高真空中で加熱処理するか、または第３図に示すよ
うに、別の石英管１中にＧａ４を収納したポート３を入
れ、加熱炉２によりＨ２ガス中で加熱処理することによ
り、Ｇａ４中の不純物の除去を行った後、蒸発用るつぼ
に入れ、結晶成長用の材料源として用いられていた。Conventionally, in the crystal growth method using molecular beam epitaxy, the Ga material source is obtained by placing solid Ga in an evaporation crucible and heat-treating it in a high vacuum, or as shown in Figure 3, using a separate quartz tube. A port 3 containing Ga4 is placed in a heating furnace 2 to remove impurities in the Ga4 by heat treatment in H2 gas, and then placed in an evaporation crucible to serve as a material source for crystal growth. It was used.
このような方法においては、例えば直接固形のＧａを蒸
発用るつぼに入れた場合、Ｇａは反応性が高く、蒸発用
るつぼに入れるまでに空気にさらされ、表面に酸化物が
生成する。In such a method, for example, when solid Ga is directly placed in an evaporation crucible, Ga is highly reactive and is exposed to air before being placed in the evaporation crucible, producing oxides on the surface.
また、第３図に示したように、加熱炉２中ではＨ２ガス
によりＧａ４を処理し、不純物を除去した場合において
も、加熱炉２からの取り出しや蒸発用るつぼに移し換え
るまでにＧａ４の表面が酸化されてしまう。Furthermore, as shown in FIG. 3, even when Ga4 is treated with H2 gas in the heating furnace 2 to remove impurities, the surface of Ga4 is becomes oxidized.
上記のように、従来方法では固形のＧａを直接蒸発用る
つぼに入れる方法や、Ｈ２ガス中における加熱処理を行
い、酸化物を除去しても蒸発用るつぼに移し換えるまで
にＧａの表面が酸化され、これらの酸化物などが原因と
なり、エピタキシー中において成長層の表面に粒状の欠
陥が生じたり、結晶の電気的特性を悪くする等の欠点が
あった。また、Ｇａ中に存在する金属不純物等は除去す
ることが難しく、したがって、結晶性のよい成長層を得
ることが難しいという問題点があった。As mentioned above, in conventional methods, solid Ga is directly placed in an evaporation crucible, or heat treatment is performed in H2 gas to remove oxides, but the surface of Ga is oxidized by the time it is transferred to an evaporation crucible. These oxides cause defects such as granular defects occurring on the surface of the grown layer during epitaxy and deterioration of the electrical characteristics of the crystal. Further, there is a problem in that it is difficult to remove metal impurities and the like existing in Ga, and therefore it is difficult to obtain a grown layer with good crystallinity.
この発明は、上記のような問題点を解消するためになさ
れたもので、結晶成長用メルト表面に生成している酸化
物を除去するとともに、その他の不純物をも除去するこ
とができる結晶成長用メルトの処理方法を得ることを目
的とするものである。This invention was made in order to solve the above-mentioned problems, and it is possible to remove oxides generated on the surface of a crystal growth melt as well as other impurities. The purpose of this study is to obtain a method for processing melt.
この発明に係る結晶成長用メルトの処理方法は、結晶成
長用メルトをＨ２ガス雰囲気中で加熱処理するとともに
、Ｈ２ガス中にＡＳＣＪ１３ガスを導入して処理を行い
、酸化物やその他の不純物を除去するとともに、結晶成
長用メルト表面に薄膜層を形成し、処理完了後に再び酸
化物が付着したとしても、蒸発用るつぼに混入すること
がないようにしたものである。The method for treating a melt for crystal growth according to the present invention heat-treats the melt for crystal growth in an H2 gas atmosphere, and also introduces ASCJ13 gas into the H2 gas to remove oxides and other impurities. At the same time, a thin film layer is formed on the surface of the crystal growth melt to prevent oxides from being mixed into the evaporation crucible even if they are attached again after the treatment is completed.
この発明においては、Ｈ２ガス中で加熱処理するととも
に、ＡｓＣｌ３ガスによる処理を行って酸化物や金属類
等の不純物の除去を行い、さらに、ポートに収納された
結晶成長用メルト表面に薄膜層を形成することから、表
面が酸化されたとしても薄膜層に覆われた内部の結晶成
長用メルトを蒸発用るつぼに移すことにより、酸化物の
混入は防止される。In this invention, in addition to heat treatment in H2 gas, impurities such as oxides and metals are removed by treatment with AsCl3 gas, and a thin film layer is further applied to the surface of the crystal growth melt stored in the port. Even if the surface is oxidized, the incorporation of oxides can be prevented by transferring the internal crystal growth melt covered with a thin film layer to the evaporation crucible.
第１図、第２図はこの発明の結晶成長用メルトの処理方
法の一実施例を説明するための図である。第１図におい
て、石英管１中にポート３に収納した結晶成長用メルト
、例えばＧａ４を入れ、Ｈ２ガスを導入しながら加熱炉
２で８００〜９００℃で１０〜２０時間加熱処理を行う
。次いで、Ｈ２ガスとＡＳＣｆＬ３ガスを石英管１に導
入しながら２〜５時間程度加熱処理を行う。このような
処理によってＧａ４に含まれる酸化物の除去を行うとと
もに、金属類等の不純物も同時に除去される。FIGS. 1 and 2 are diagrams for explaining an embodiment of the method for treating a crystal growth melt according to the present invention. In FIG. 1, a crystal growth melt, for example Ga4, housed in a port 3 is placed in a quartz tube 1, and heated in a heating furnace 2 at 800 to 900° C. for 10 to 20 hours while introducing H2 gas. Next, heat treatment is performed for about 2 to 5 hours while introducing H2 gas and ASCfL3 gas into the quartz tube 1. Through such treatment, oxides contained in Ga4 are removed, and impurities such as metals are also removed at the same time.
また、これらの処理を完了したＧａ４は、処理中におい
てＡｓＣｌ３ガス中のＡｓを吸収し、Ｇａ４の表面にＧ
ａＡｓの薄膜層５が形成される。したがって、この薄膜
層５により、Ｇａ４はポート３中に密封された状態とな
る。In addition, Ga4 that has undergone these treatments absorbs As in AsCl3 gas during the treatment, and G is deposited on the surface of Ga4.
A thin film layer 5 of aAs is formed. Therefore, Ga4 is sealed in the port 3 by this thin film layer 5.
次いで、第２図に示すように、この処理を完了したポー
ト３に入ったＧａ４を真空装置（分子線エピタキシー装
置）中に入れ、ポート３を傾けながらＧａ４がとける程
度に熱してやると、Ｇａ４の表面に形成されたＧａＡｓ
の薄膜層５の一部が破れ、その部分よりとけたＧａ４が
流れ出し、蒸発用るつぼ６中に充てんされる。なお、残
りの薄膜層５は固形のままポート３中に残るのでポート
３とともに取り出し、蒸発用るつぼ６に入ったＧａ４の
みを結晶成長用材料として用いる。Next, as shown in Fig. 2, the Ga4 that has entered port 3, which has completed this process, is placed in a vacuum device (molecular beam epitaxy device) and heated to the extent that Ga4 melts while tilting port 3. GaAs formed on the surface
A part of the thin film layer 5 is torn, and melted Ga4 flows out from that part and is filled into the evaporation crucible 6. Note that the remaining thin film layer 5 remains solid in the port 3, so it is taken out together with the port 3, and only the Ga4 that has entered the evaporation crucible 6 is used as a material for crystal growth.
また、従来方法でＨ２ガスのみで処理したＧａ４を、第
２図に示した方法で蒸発用るつぼ６中に充てんした場合
には表面に形成された薄い酸化物等も同時に蒸発用るつ
ぼ６中に混入してしまうが、この発明によれば、これら
の不純物の混入を防止できるのは明らかである。Furthermore, when Ga4 treated with only H2 gas in the conventional method is filled into the evaporation crucible 6 by the method shown in FIG. However, according to the present invention, it is clear that the incorporation of these impurities can be prevented.
この発明は以上説明したように、Ｈ２ガスによる加熱処
理と、Ｈ２ガスとＡｓＣｌ３ガスとにより、結晶成長用
メルト中に含まれる不純物を除去するとともに、結晶成
長用メルト表面に薄膜層を形成して結晶成長用メルト表
面を覆うことにより、内部の結晶成長用メルトは酸化さ
れず、例えばこの薄膜表面が酸化されたとしても蒸発る
つぼ中には不純物のない結晶成長用メルトのみが充てん
され、蒸発用るつぼへの酸化物の混入を防止する効果が
ある。As explained above, this invention removes impurities contained in the melt for crystal growth and forms a thin film layer on the surface of the melt for crystal growth by heat treatment with H2 gas and H2 gas and AsCl3 gas. By covering the surface of the crystal growth melt, the internal crystal growth melt will not be oxidized, and even if the surface of this thin film is oxidized, the evaporation crucible will be filled with only the crystal growth melt without impurities, and the evaporation This has the effect of preventing oxides from entering the crucible.
【図面の簡単な説明】
第１図、第２図はこの発明の結晶成長用メルトの処理方
法の一実施例を説明するための図、第３図は従来の結晶
成長用メルトの処理方法を説明するための図である。
図において、１は石英管、２は加熱炉、３はポート、４
はＧａ、５は薄膜層、６は蒸発用るつぼである。
なお、各図中の同一符号は同一または相当部分を示す。
代理人 大 岩 増 雄 （外２名）第１図
第３図
？[Brief Description of the Drawings] Figures 1 and 2 are diagrams for explaining an embodiment of the method for treating a melt for crystal growth according to the present invention, and Figure 3 is for explaining a conventional method for treating a melt for crystal growth. It is a figure for explaining. In the figure, 1 is a quartz tube, 2 is a heating furnace, 3 is a port, and 4
is Ga, 5 is a thin film layer, and 6 is an evaporation crucible. Note that the same reference numerals in each figure indicate the same or corresponding parts. Agent Masuo Oiwa (2 others) Figure 1 Figure 3?
Claims (1)
法において、前記結晶成長用メルトをＨ＿２ガス中で加
熱処理した後、前記Ｈ＿２ガス中にＡｓＣｌ＿３ガスを
導入して加熱処理を行い、前記結晶成長用メルト中の不
純物を除去するとともに、前記結晶成長用メルト表面に
薄膜層を形成することを特徴とする結晶成長用メルトの
処理方法。In a method for treating a melt for crystal growth using a molecular beam epitaxy method, the melt for crystal growth is heat-treated in H_2 gas, and then AsCl_3 gas is introduced into the H_2 gas and heat-treated, and the melt for crystal growth is heated. A method for treating a crystal growth melt, which comprises removing impurities therein and forming a thin film layer on the surface of the crystal growth melt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22023186A JPS6374993A (en) | 1986-09-17 | 1986-09-17 | Treatment of melt for crystal growth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22023186A JPS6374993A (en) | 1986-09-17 | 1986-09-17 | Treatment of melt for crystal growth |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6374993A true JPS6374993A (en) | 1988-04-05 |
| JPH0458435B2 JPH0458435B2 (en) | 1992-09-17 |
Family
ID=16747942
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22023186A Granted JPS6374993A (en) | 1986-09-17 | 1986-09-17 | Treatment of melt for crystal growth |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6374993A (en) |
-
1986
- 1986-09-17 JP JP22023186A patent/JPS6374993A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0458435B2 (en) | 1992-09-17 |
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