JP2002293696A - METHOD OF MANUFACTURING CaN SINGLE CRYSTAL - Google Patents
METHOD OF MANUFACTURING CaN SINGLE CRYSTALInfo
- Publication number
- JP2002293696A JP2002293696A JP2001097551A JP2001097551A JP2002293696A JP 2002293696 A JP2002293696 A JP 2002293696A JP 2001097551 A JP2001097551 A JP 2001097551A JP 2001097551 A JP2001097551 A JP 2001097551A JP 2002293696 A JP2002293696 A JP 2002293696A
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- Japan
- Prior art keywords
- single crystal
- ammonia
- gan
- crystal
- gallium
- 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.)
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】この出願の発明は、ＧａＮ単
結晶の製造方法に関するものである。さらに詳しくは、
この出願の発明は、ＧａＮバルク単結晶の製造におい
て、成長速度を向上させることのできる高効率なＧａＮ
単結晶の製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a GaN single crystal. For more information,
The invention of this application provides a highly efficient GaN that can improve the growth rate in the production of a GaN bulk single crystal.
The present invention relates to a method for producing a single crystal.
【０００２】[0002]
【従来の技術と発明の課題】窒化ガリウム：ＧａＮは、
青色発光素子の材料として注目されている。BACKGROUND OF THE INVENTION Gallium nitride: GaN is
It is attracting attention as a material for blue light emitting devices.
【０００３】そして、窒化ガリウムは、エピタキシャル
成長による薄膜として、例えば、サファイア基板を用い
たヘテロエピタキシャル成長によるものが知られてい
る。[0003] Gallium nitride is known as a thin film formed by epitaxial growth, for example, formed by heteroepitaxial growth using a sapphire substrate.
【０００４】しかしながら、このような薄膜としての窒
化ガリウムには、基板と薄膜との格子定数差（１３．８
％）、熱膨張係数差（２５．５％）、および、壁開面の
違いがネックとなり、基板との整合性が悪いことから、
充分な結晶性を得ることが難しいという問題がある。However, gallium nitride as such a thin film has a lattice constant difference (13.8) between the substrate and the thin film.
%), The difference in thermal expansion coefficient (25.5%), and the difference in the wall open surface become a bottleneck, and the consistency with the substrate is poor.
There is a problem that it is difficult to obtain sufficient crystallinity.
【０００５】このような問題点を考慮して、窒化ガリウ
ム単結晶基板上にホモエピタキシャル成長によるデバイ
スを作製する方法が検討されており、その基板となるバ
ルク状窒化ガリウム単結晶の実現が重要な課題となって
いる。In consideration of such problems, a method of manufacturing a device by homoepitaxial growth on a gallium nitride single crystal substrate has been studied, and it is important to realize a bulk gallium nitride single crystal serving as the substrate. It has become.
【０００６】従来、ＧａＮ、ＡｌＮなどの窒化物バルク
結晶は、融点における窒素の平衡蒸気圧が１万気圧以上
であるため、ＧａＮの融液成長では１２００℃、８００
０気圧、ＡｌＮではそれ以上の高温・高圧を必要とする
という問題があった。このような状況において、Ｎａを
フラックスに用いることで、温度７５０℃・窒素ガス５
０気圧という比較的低温・低圧でＧａＮを合成できるこ
とが見出された。だが一方で、この方法の場合には、結
晶の成長速度が遅いという問題があった。Conventionally, bulk nitride crystals such as GaN and AlN have an equilibrium vapor pressure of nitrogen at the melting point of 10,000 atm or more.
In the case of 0 atm and AlN, there is a problem that a higher temperature and a higher pressure are required. In such a situation, by using Na for the flux, the temperature is 750 ° C. and the nitrogen gas 5
It has been found that GaN can be synthesized at a relatively low temperature and low pressure of 0 atm. On the other hand, however, this method has a problem that the crystal growth rate is low.
【０００７】そこで、この出願の発明は、成長速度を向
上させて、核発生数、結晶サイズ、そしてトータルの結
晶収量をより増大させることのできる、改良された新し
いバルクＧａＮ単結晶の製造方法を提供することを課題
としている。Accordingly, the invention of this application is to provide an improved new bulk GaN single crystal manufacturing method capable of increasing the growth rate and further increasing the number of nuclei generated, the crystal size, and the total crystal yield. The task is to provide.
【０００８】[0008]
【課題を解決するための手段】この出願の発明は、前記
の課題を解決するものとして、ガリウム原料物質をナト
リウム物質およびカリウム物質の少なくともいずれかの
存在下に窒素ガス加圧雰囲気下に反応させてＧａＮ単結
晶を製造する方法において、雰囲気窒素ガスの少なくと
も一部をアンモニアで置換して加圧反応させることを特
徴とするＧａＮ単結晶の製造方法を提供する。According to the invention of the present application, a gallium raw material is reacted under a nitrogen gas pressurized atmosphere in the presence of at least one of a sodium substance and a potassium substance. In the method for producing a GaN single crystal, a method of producing a GaN single crystal, characterized in that at least a part of an atmospheric nitrogen gas is replaced with ammonia and a pressure reaction is performed.
【０００９】また、この出願の発明は、第２には、ガリ
ウム原料物質は金属ガリウムであって、ナトリウム物質
とカリウム物質は、金属のナトリウムとカリウムである
ことを特徴とするＧａＮ単結晶の製造方法を提供し、第
３にはアンモニアを２０体積％以下に混合することを特
徴とするＧａＮ単結晶の製造方法を、第４には、窒素ガ
スとアンモニアの混合ガスの圧力を１０〜１００ａｔｍ
とすることを特徴とするＧａＮ単結晶の製造方法を提供
する。Secondly, the invention of this application is characterized in that the gallium raw material is metallic gallium, and the sodium and potassium substances are metallic sodium and potassium. Third, a method for producing a GaN single crystal characterized by mixing ammonia to 20% by volume or less, and fourth, a pressure of a mixed gas of nitrogen gas and ammonia of 10 to 100 atm.
A method for producing a GaN single crystal is provided.
【００１０】[0010]
【発明の実施の形態】この出願の発明は前記のとおりの
特徴をもつものであるが、以下にその実施の形態につい
て説明する。BEST MODE FOR CARRYING OUT THE INVENTION The invention of this application has the features as described above, and embodiments thereof will be described below.
【００１１】まず、この出願の発明においては、ガリウ
ム原料物質としては、単体金属、合金、化合物の各種の
ものでよいが、なかでもガリウムの単体金属の使用が取
扱いの上からも好適である。一方、この発明では、フラ
ックスとして、ナトリウム物質とカリウム物質のいずれ
か一方もしくはその両者を用いるが、これらの物質は、
単体金属、あるいは金属化合物の各種のものであってよ
い。なかでも、単体金属としてのナトリウム、カリウム
を用いるのが好適である。First, in the invention of this application, as the gallium raw material, various kinds of simple metals, alloys and compounds may be used, but the use of a simple metal of gallium is preferable from the viewpoint of handling. On the other hand, in the present invention, one or both of a sodium substance and a potassium substance are used as a flux.
It may be a single metal or various kinds of metal compounds. Among them, it is preferable to use sodium or potassium as a simple metal.
【００１２】ガリウム原料物質と、これらのナトリウ
ム、カリウム物質との使用割合は、適宜であってよい
が、一般的には、Ｇａ過剰量を用いることが考慮され
る。もちろん、このことは限定的ではない。The proportions of the gallium raw material and these sodium and potassium substances may be arbitrary, but generally, the use of an excess of Ga is considered. Of course, this is not limiting.
【００１３】反応は、ステンレス容器等の耐熱、耐圧
性、そして非反応性の容器内において行うことができ
る。反応温度は、通常は６００℃〜１０００℃の範囲で
よく、雰囲気圧力は、５００ａｔｍ程度まで考慮される
が、実際的には、窒素ガスのアンモニアによる置換の度
合い、つまりアンモニアの混合の度合いと、反応温度と
を考慮して決めることができる。この際には、温度が低
い場合にはアンモニアの液化によって圧力の上昇が難し
くなることが当然のこととして考慮される。The reaction can be carried out in a heat-resistant, pressure-resistant and non-reactive container such as a stainless steel container. The reaction temperature may be usually in the range of 600 ° C. to 1000 ° C., and the atmospheric pressure is considered up to about 500 atm. In practice, however, the degree of substitution of ammonia by nitrogen gas, that is, the degree of mixing of ammonia, It can be determined in consideration of the reaction temperature. At this time, it is naturally considered that when the temperature is low, it is difficult to increase the pressure due to liquefaction of ammonia.
【００１４】たとえば、圧力については、限定的ではな
いが目安として、１０〜１００ａｔｍとすることができ
る。そして、この発明の特徴として、加圧雰囲気のガス
については、窒素（Ｎ2）ガスの少なくとも一部をアン
モニアにより置換した混合ガスを用いる。For example, the pressure is not limited, but may be 10 to 100 atm as a guide. As a feature of the present invention, as a gas in a pressurized atmosphere, a mixed gas in which at least a part of a nitrogen (N 2 ) gas is replaced by ammonia is used.
【００１５】アンモニアは窒素に比べて自由エネルギー
が大きく、反応性が窒素に比べて大きいことから、アン
モニアの置換混合によって、ＧａＮ単結晶の成長速度
は、窒素ガス単体の場合に比べて、顕著に向上し、より
低い温度と、より低い圧力下でも、高品質のＧａＮ単結
晶が効率的に育成されることになる。アンモニアによる
置換については、この発明では、窒素ガスの全てをアン
モニアで置換した状態のアンモニアガスを反応に用いて
もよいし、一部をアンモニアにより置換した混合ガスで
あってもよい。混合ガスにおける混合の割合も、反応温
度と圧力を考慮して適宜に決めることができる。たとえ
ば５０体積％以下、さらに実際的には、２０体積％以下
程度とすることも考慮される。Since ammonia has a higher free energy than nitrogen and a higher reactivity than nitrogen, the substitution rate of ammonia causes the growth rate of a GaN single crystal to be significantly higher than that of nitrogen gas alone. Improved, higher quality GaN single crystals will be grown efficiently even at lower temperatures and lower pressures. Regarding the replacement with ammonia, in the present invention, ammonia gas in which all of the nitrogen gas has been replaced with ammonia may be used for the reaction, or a mixed gas in which a part of the nitrogen gas has been replaced with ammonia may be used. The mixing ratio in the mixed gas can also be appropriately determined in consideration of the reaction temperature and pressure. For example, 50% by volume or less, and more practically, about 20% by volume or less are also considered.
【００１６】この出願の発明により、結晶の核発生数、
結晶サイズ、トータルな結晶収量ともに窒素ガスのみの
場合よりも優れたものとなり、成長速度は大きく向上す
る。According to the invention of this application, the number of crystal nuclei generated,
Both the crystal size and the total crystal yield are superior to those using only nitrogen gas, and the growth rate is greatly improved.
【００１７】そこで以下に実施例を示し、さらに詳しく
この発明について説明する。The present invention will be described in more detail with reference to the following examples.
【００１８】[0018]
【実施例】金属のＧａとＮａを装入したるつぼ内におけ
る結晶生成時の圧力を５０ａｔｍ、温度を８００℃と一
定にして、Ｎ2ガス１００％と、アンモニア４％希釈の
Ｎ2ガスを用いて４８時間と９６時間、結晶の生成を行
った。EXAMPLE In a crucible charged with metal Ga and Na, the pressure during crystal formation was kept constant at 50 atm, the temperature was kept at 800 ° C., and N 2 gas 100% and N 2 gas diluted with 4% ammonia were used. For 48 and 96 hours.
【００１９】この際の出発条件は、次の表１のとおりと
した。The starting conditions at this time are as shown in Table 1 below.
【００２０】[0020]
【表１】 [Table 1]
【００２１】結晶育成後、放冷し常温まで下がってから
るつぼを取り出し残留Ｎａをエタノール、蒸留水を用い
て処理し、るつぼを半分に割り光学顕微鏡で観測したと
ころ図１（ａ）（ｂ）（ｃ）のような光学顕微鏡による
写真観察の結果が得られた。After the crystal was grown, the crucible was allowed to cool to room temperature, the crucible was taken out, the remaining Na was treated with ethanol and distilled water, and the crucible was cut in half and observed with an optical microscope. The result of the photograph observation by the optical microscope as shown in (c) was obtained.
【００２２】これより、生成時間が４８時間で窒素ガス
のみで育成したサンプル（ａ）は光学顕微鏡を用いて評
価してもＸ線解析測定でもＧａＮの生成を確認すること
はできなかった。同じく生成時間が４８時間で窒素希釈
のアンモニア４％の混合ガスを用いて育成した（ｂ）
は、個々の結晶サイズは約０．１ｍｍ程度ではあるがＧ
ａＮの生成を光学顕微鏡を用いて確認することができ
た。次に生成時間が９６時間で４％アンモニアの窒素ガ
スで育成したサンプル（ｃ）では、肉眼でＧａＮの生成
が確認でき、最大結晶サイズ１．２ｍｍのＧａＮの生成
が確認された。As a result, the sample (a) grown for 48 hours and grown only with nitrogen gas could not confirm the generation of GaN by the evaluation using an optical microscope or the X-ray analysis measurement. Similarly, it was grown using a mixed gas of 4% ammonia diluted with nitrogen for 48 hours (b).
Means that although the individual crystal size is about 0.1 mm,
The generation of aN could be confirmed using an optical microscope. Next, in sample (c) grown for 96 hours with 4% ammonia nitrogen gas for 96 hours, generation of GaN was confirmed by the naked eye, and generation of GaN having a maximum crystal size of 1.2 mm was confirmed.
【００２３】結晶の核発生数、結晶サイズ、トータルな
結晶収量ともに窒素ガスのみの場合よりも優れたものと
なり、成長速度は大きく向上する。The number of crystal nuclei generated, the crystal size, and the total crystal yield are all superior to those obtained using only nitrogen gas, and the growth rate is greatly improved.
【００２４】[0024]
【発明の効果】以上詳しく説明したとおり、この出願の
発明によって、ＧａＮ単結晶の成長速度を向上させて、
核発生数、結晶サイズ、そしてトータルの結晶収量をよ
り増大させることができる。As described in detail above, according to the invention of this application, the growth rate of a GaN single crystal is improved,
The number of nuclei generated, the crystal size, and the total crystal yield can be further increased.
【図１】実施例の結果を例示した光学顕微鏡写真であ
る。FIG. 1 is an optical micrograph illustrating the results of an example.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G077 AA02 BE15 CC06 EA04 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G077 AA02 BE15 CC06 EA04
Claims (4)
びカリウム物質の少なくともいずれかの存在下に窒素ガ
ス加圧雰囲気下に反応させてＧａＮ単結晶を製造する方
法において、雰囲気窒素ガスの少なくとも一部をアンモ
ニアで置換して加圧反応させることを特徴とするＧａＮ
単結晶の製造方法。1. A method for producing a GaN single crystal by reacting a gallium raw material under a nitrogen gas pressurized atmosphere in the presence of at least one of a sodium material and a potassium material, wherein at least a part of the atmospheric nitrogen gas is ammonia Characterized by substituting with GaN and reacting under pressure
Single crystal production method.
て、ナトリウム物質とカリウム物質は、金属のナトリウ
ムとカリウムであることを特徴とする請求項１のＧａＮ
単結晶の製造方法。2. The GaN material according to claim 1, wherein the gallium source material is metallic gallium, and the sodium and potassium materials are metallic sodium and potassium.
Single crystal production method.
換することを特徴とする請求項１または２のＧａＮ単結
晶の製造方法。3. The method for producing a GaN single crystal according to claim 1, wherein ammonia is replaced by mixing at 20% by volume or less.
を１０〜１００ａｔｍとすることを特徴とする請求項１
ないし３のいずれかのＧａＮ単結晶の製造方法。4. The pressure of a mixed gas of nitrogen gas and ammonia is set to 10 to 100 atm.
3. The method for producing a GaN single crystal according to any one of items 1 to 3.
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|---|---|---|---|
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ID=18951324
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2001
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