JP4065055B2 - Method for growing gallium nitride compound semiconductor single crystal - Google Patents
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- gallium nitride
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Description
【０００１】
【発明の属する技術分野】
本発明は、光デバイス，電子デバイスなどの半導体デバイスの製造に用いられる窒化ガリウム系化合物半導体単結晶の製造方法に関するものである。
【０００２】
【従来の技術】
窒化ガリウム系化合物半導体（例えば、ＩｎxＧａyＡｌ1-x-yＮ）（０≦ｘ，ｙ；ｘ＋ｙ≦１；但し、ｘ＝１,ｙ＝０の場合は除く）は、禁制帯幅が広く、短波長発光素子，耐環境素子として期待され、広く研究されてきた。
【０００３】
しかしながら、この窒化ガリウム系化合物半導体においては、未だ大型のバルク結晶が得られないため、異種結晶（例えばサファイアα−Ａｌ2Ｏ3）上へのヘテロエピタキシーによってＧａＮ等の薄膜単結晶を形成したものが基板として用いられてきた。
【０００４】
ところが、サファイアに代表されるように、多くの場合、基板に用いられる異種結晶とその上に成膜される窒化ガリウム系化合物半導体薄膜との格子不整合性が大きく、欠陥や熱歪みなどが発生し易いため、窒化ガリウム系化合物半導体単結晶は品質的に問題を抱えるものであった。
【０００５】
そこで、本発明者等は、窒化ガリウム系化合物半導体をヘテロエピタキシーによって成長させる際に、種々の優れた特性を備える異種結晶基板の材料の一つとして希土類１３（３Ｂ）族ペロブスカイトを用いた窒化ガリウム系化合物半導体単結晶の成長方法および窒化ガリウム系化合物半導体装置を提案した（特願平７−５２６２３３号）。
【０００６】
この成長技術によれば、例えば希土類１３（３Ｂ）族ペロブスカイトの一種としてＮｄＧａＯ3を基板として用い、その基板上にＧａＮをエピタキシャル成長させる場合には、格子不整合を１．２％程度とすることができた。
【０００７】
この格子不整合性は、サファイアやその代替品として用いられるＳｉＣを基板とした場合と比較しても非常に小さく、窒化ガリウム系化合物半導体単結晶のヘテロエピタキシーに有効であると期待される。
【０００８】
また、その後の研究により、例えばＮｄＧａＯ3上にＧａＮをエピタキシャル成長させる場合に、低温でＧａＮの第１層を成長させた後に、高温で第２層を成長させるとより良質のＧａＮ単結晶を得ることができることが分かってきた。
【０００９】
【発明が解決しようとする課題】
しかし、一方で上述のようにＮｄＧａＯ3上に低温でＧａＮの第１層を成長させた後に高温で第２層を成長させるという成長方法をとる場合に、ＧａＮの第１層を成長後、第２層の成長温度までの熱処理工程を窒素源であるＮＨ3を流しながら行うと、第１層に生じたピンホールを通してＮＨ3がＮｄＧａＯ3の表面まで達し、基板が窒化する反応を起こし、その影響で基板面から第１層のＧａＮが剥がれてしまうという不具合を生じることが明らかとなってきた。
【００１０】
また、ＮｄＧａＯ3を基板としてＧａＮをエピタキシャル成長する場合、低温で成長するＧａＮの第１層は緩衝層としての役割を果たすほか、ＮｄＧａＯ3とＮＨ3が反応して不要な層が生成されるのを防ぐ保護膜としての機能を有しているが、ＧａＮの第１層を成長後、第２層の成長温度までの熱処理工程をＮＨ3の雰囲気で行うと、この保護膜としての機能が低下するという障害を生じることが分かってきた。
【００１１】
本発明は上述のような問題を解決すべく案出されたものであり、１または２種類以上の希土類元素を含む希土類１３（３Ｂ）族ペロブスカイトの単結晶基板上に良質の窒化ガリウム系化合物半導体単結晶を成長させることのできる方法を提供することを主目的とするものである。
【００１２】
【課題を解決するための手段】
上記目的を達成するために、本発明は、１または２種類以上の希土類元素を含む希土類１３（３Ｂ）族ペロブスカイトの単結晶を基板とする窒化ガリウム系化合物半導体単結晶の成長方法において、第１の温度条件下で上記基板上に第１の窒化ガリウム層を成長させる第１の成膜工程と、上記基板を不活性ガス雰囲気中で所定温度まで昇温させて熱処理を施す熱処理工程と、前熱処理温工程の終了後に、前記第１の温度条件より高温に設定される第２の温度条件下で前記第１の窒化ガリウム層の上に第２の窒化ガリウム層を成長させる第２の成膜工程とを少なくとも有するようにしたものである。
【００１３】
これにより、従来のように第１層のＧａＮが剥がれるという不具合を解消することができる。
【００１４】
なお、上記第１の成膜工程における第１の温度条件は、４００℃〜７５０℃、好ましくは５５０℃〜６５０℃、形成する第１の窒化ガリウム層の膜厚は、２０ｎｍ〜３５０ｎｍ、好ましくは８０ｎｍ〜１２０ｎｍとすることが望ましい。
【００１５】
ここで、４００℃未満ではＧａＮが成膜せず、８００℃を超えると基板と原料ガスが反応するため好ましくなく、又、８０ｎｍ未満だと基板を完全に被覆することができず、１２０ｎｍを超えると生成する膜質が悪くなるため好ましくない。
【００１６】
また、上記熱処理工程における所定温度は、８００℃〜１２００℃、好ましくは９５０℃〜１０５０℃とするとよい。この範囲外では，第１の窒化ガリウム層が緩衝層あるいは保護膜としての機能が低下するので好ましくない。
【００１７】
また、上記熱処理工程における不活性ガス雰囲気は、Ｎ2ガス雰囲気とすると効果的である。
【００１８】
また、上記第２の成膜工程における第２の温度条件は、８００℃〜１２００℃、好ましくは９５０℃〜１０５０℃とすることが望ましい。
【００１９】
ここで、８００℃未満では成長速度ｇは遅く、１２００℃を超えると生成する膜質が悪くなるため好ましくない。
【００２０】
さらに、上記１３（３Ｂ）族元素として、Ａｌ，Ｇａ，Ｉｎのうち少なくとも１種類を含むようにすることができる。
【００２１】
このようにして成長させた窒化ガリウム系化合物半導体単結晶を用いることにより、熱的，化学的に安定な高性能の青色発光ダイオードや半導体レーザ等の半導体装置を得ることが可能となる。
【００２２】
【発明の実施の形態】
ここで、本発明の実施形態の一例について説明する。
【００２３】
本実施形態では、希土類ガリウムペロブスカイトとしてＮｄＧａＯ3の単結晶基板の（００１）面上に窒化ガリウム系化合物半導体としてのＧａＮ単結晶を成長させる場合について述べる。
【００２４】
まず、厚さ３５０μｍの（００１）面ＮｄＧａＯ3単結晶基板を有機溶剤で洗浄した後に、ハイドライドＶＰＥ装置にセットした。
【００２５】
次いで、窒素ガスを流しながら、基板部の温度を６００℃に、Ｇａ原料の温度を８５０℃に昇温した。
【００２６】
そして、Ｇａ原料の上流側から窒素（Ｎ2）ガスで希釈されたＨＣｌガスを流し、同時にＧａ原料をバイパスして基板の直上にＮＨ3ガスを流して、基板上に第１のＧａＮ層の薄膜を１０分間成長させた。
【００２７】
これにより得られた第１のＧａＮ層の薄膜の厚さは約１００ｎｍであった。
【００２８】
続いて不活性ガスとしてのＮ2ガスの雰囲気中で基板部の温度を１０００℃まで昇温して熱処理を施した後、Ｇａ原料の上流側からＮ2ガスで希釈されたＨＣｌガスを流すと同時にＧａ原料をバイパスして基板の直上にＮＨ3ガスを流して、前記第１のＧａＮ層の上に第２のＧａＮ層を６０分間にわたって成長させた。
【００２９】
これにより、約２０μｍの厚さのＧａＮ厚膜を得ることができた。このＧａＮ層からなる厚膜を観察したところ、表面に異常成長が見られない平坦な鏡面状のエピタキシャル膜であった。
【００３０】
また、Ｘ線回折分析した結果、良質な膜質の（０００１）面の単結晶であることが確認された。
【００３１】
このように、本発明に係る成長方法によれば、希土類ガリウムペロブスカイトの（００１）面上に良質なＧａＮ単結晶を成長させ得ることが実験的に確かめられた。
【００３２】
よって、この良質なＧａＮ単結晶を用いることにより熱的，化学的に安定な高性能の青色発光ダイオードや半導体レーザ等の半導体装置を製造することが可能となる。
【００３３】
なお、本実施形態では、希土類ガリウムペロブスカイトとしてＮｄＧａＯ3単結晶基板を用い、ＧａＮ単結晶を成長させる場合について説明したが、これに限られるものではなく、その他の１または２種類以上の希土類元素を含む希土類１３（３Ｂ）族ペロブスカイトの単結晶基板上にＧａＮ以外の窒化ガリウム系化合物半導体単結晶を成長させる場合にも適用することができる。
【００３４】
また、本実施形態では、不活性ガスとしてＮ2ガスを用いる場合について述べたがこれに限定されずその他の不活性ガスを用いることも可能である。
【００３５】
【発明の効果】
本発明は、１または２種類以上の希土類元素を含む希土類１３（３Ｂ）族ペロブスカイトの単結晶を基板とする窒化ガリウム系化合物半導体単結晶の成長方法において、第１の温度条件下で上記基板上に第１の窒化ガリウム層を成長させる第１の成膜工程と、上記基板を不活性ガス雰囲気中で所定温度まで昇温させて熱処理を施す熱処理工程と、前記熱処理工程の終了後に、前記第１の温度条件より高温に設定される第２の温度条件下で前記第１の窒化ガリウム層の上に第２の窒化ガリウム層を成長させる第２の成膜工程とを少なくとも有するようにしたので、従来のように第１層のＧａＮが剥がれるなどの不具合を解消することができ、良質の窒化ガリウム系化合物半導体単結晶を得ることができるという優れた効果がある。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for manufacturing a gallium nitride-based compound semiconductor single crystal used for manufacturing semiconductor devices such as optical devices and electronic devices.
[0002]
[Prior art]
Gallium nitride compound semiconductors (for example, In x Ga y Al 1-xy N) (0 ≦ x, y; x + y ≦ 1; except when x = 1 and y = 0) have a wide forbidden band width Expected as a short wavelength light emitting element and an environment resistant element, it has been widely studied.
[0003]
However, in this gallium nitride compound semiconductor, since a large bulk crystal cannot be obtained yet, a thin film single crystal such as GaN is formed by heteroepitaxy on a different crystal (for example, sapphire α-Al 2 O 3 ). Have been used as substrates.
[0004]
However, as represented by sapphire, in many cases, the lattice mismatch between the dissimilar crystal used for the substrate and the gallium nitride compound semiconductor thin film formed thereon is large, and defects and thermal strain are generated. Therefore, the gallium nitride compound semiconductor single crystal has a quality problem.
[0005]
Accordingly, the present inventors have developed gallium nitride using rare earth 13 (3B) group perovskite as one of the materials of different crystal substrates having various excellent characteristics when growing gallium nitride compound semiconductors by heteroepitaxy. And a gallium nitride compound semiconductor device have been proposed (Japanese Patent Application No. 7-526233).
[0006]
According to this growth technique, for example, when NdGaO 3 is used as a substrate as a kind of rare earth 13 (3B) group perovskite and GaN is epitaxially grown on the substrate, the lattice mismatch may be about 1.2%. did it.
[0007]
This lattice mismatch is very small as compared with the case where sapphire or SiC used as an alternative is used as a substrate, and is expected to be effective for heteroepitaxy of a gallium nitride compound semiconductor single crystal.
[0008]
Further, by subsequent research, for example, when GaN is epitaxially grown on NdGaO 3 , if a first layer of GaN is grown at a low temperature and then a second layer is grown at a high temperature, a higher quality GaN single crystal can be obtained. I know that I can do it.
[0009]
[Problems to be solved by the invention]
However, on the other hand, when the growth method in which the second layer is grown at a high temperature after the first layer of GaN is grown on NdGaO 3 at a low temperature as described above, the first layer of GaN is grown after the first layer is grown. When the heat treatment process to the growth temperature of the second layer performs while flowing NH 3 as a nitrogen source, NH 3 through the pin hole occurs in the first layer reaches to the surface of NdGaO 3, reacts the substrate is nitrided, the It has become clear that the first layer of GaN peels off from the substrate surface due to the influence.
[0010]
In addition, when epitaxially growing GaN using NdGaO 3 as a substrate, the first layer of GaN grown at a low temperature serves as a buffer layer, and NdGaO 3 and NH 3 react to generate an unnecessary layer. Although the protective film functions as a protective film, if the heat treatment step up to the growth temperature of the second layer is performed in an NH 3 atmosphere after the growth of the first layer of GaN, the function as the protective film is reduced. It has been found that this causes a failure.
[0011]
The present invention has been devised to solve the above problems, and a high-quality gallium nitride compound semiconductor is formed on a single crystal substrate of a rare earth 13 (3B) group perovskite containing one or more rare earth elements. The main object is to provide a method capable of growing a single crystal.
[0012]
[Means for Solving the Problems]
To achieve the above object, the present invention provides a method for growing a gallium nitride compound semiconductor single crystal using a rare earth 13 (3B) group perovskite single crystal containing one or more rare earth elements as a substrate. A first film-forming step for growing a first gallium nitride layer on the substrate under the temperature conditions, a heat treatment step for heating the substrate to a predetermined temperature in an inert gas atmosphere, Second film formation for growing a second gallium nitride layer on the first gallium nitride layer under a second temperature condition set higher than the first temperature condition after completion of the heat treatment temperature step And at least a process.
[0013]
Thereby, the problem that the first layer of GaN peels off as in the conventional case can be solved.
[0014]
The first temperature condition in the first film formation step is 400 ° C. to 750 ° C., preferably 550 ° C. to 650 ° C., and the thickness of the first gallium nitride layer to be formed is 20 nm to 350 nm, preferably It is desirable to set it as 80 nm-120 nm.
[0015]
Here, if the temperature is lower than 400 ° C., GaN does not form a film, and if it exceeds 800 ° C., the substrate and the source gas react with each other, which is not preferable. Since the film quality to be produced deteriorates, it is not preferable.
[0016]
The predetermined temperature in the heat treatment step is 800 ° C. to 1200 ° C., preferably 950 ° C. to 1050 ° C. Outside this range, the function of the first gallium nitride layer as a buffer layer or a protective film is not preferable.
[0017]
Further, it is effective that the inert gas atmosphere in the heat treatment step is an N 2 gas atmosphere.
[0018]
The second temperature condition in the second film formation step is 800 ° C. to 1200 ° C., preferably 950 ° C. to 1050 ° C.
[0019]
Here, if it is less than 800 degreeC, the growth rate g is slow, and if it exceeds 1200 degreeC, the quality of the film | membrane produced will deteriorate, and it is not preferable.
[0020]
Furthermore, at least one of Al, Ga, and In can be included as the 13 (3B) group element.
[0021]
By using the gallium nitride compound semiconductor single crystal thus grown, it is possible to obtain a semiconductor device such as a high-performance blue light-emitting diode or semiconductor laser that is thermally and chemically stable.
[0022]
DETAILED DESCRIPTION OF THE INVENTION
Here, an example of the embodiment of the present invention will be described.
[0023]
In this embodiment, a case will be described in which a GaN single crystal as a gallium nitride compound semiconductor is grown on the (001) plane of a single crystal substrate of NdGaO 3 as a rare earth gallium perovskite.
[0024]
First, a (001) plane NdGaO 3 single crystal substrate having a thickness of 350 μm was washed with an organic solvent, and then set in a hydride VPE apparatus.
[0025]
Next, while flowing nitrogen gas, the temperature of the substrate portion was raised to 600 ° C., and the temperature of the Ga raw material was raised to 850 ° C.
[0026]
Then, HCl gas diluted with nitrogen (N 2 ) gas is flowed from the upstream side of the Ga raw material, and at the same time, NH 3 gas is flowed directly above the substrate, bypassing the Ga raw material, and the first GaN layer on the substrate. The thin film was grown for 10 minutes.
[0027]
The thickness of the first GaN layer thin film thus obtained was about 100 nm.
[0028]
Subsequently, when the temperature of the substrate portion is increased to 1000 ° C. in an atmosphere of N 2 gas as an inert gas and heat treatment is performed, HCl gas diluted with N 2 gas is flowed from the upstream side of the Ga raw material. At the same time, NH 3 gas was allowed to flow immediately above the substrate while bypassing the Ga material, and a second GaN layer was grown on the first GaN layer for 60 minutes.
[0029]
Thereby, a GaN thick film having a thickness of about 20 μm could be obtained. When the thick film composed of the GaN layer was observed, it was a flat mirror-like epitaxial film with no abnormal growth on the surface.
[0030]
Further, as a result of X-ray diffraction analysis, it was confirmed that the single crystal had a good quality (0001) plane.
[0031]
As described above, according to the growth method of the present invention, it has been experimentally confirmed that a high-quality GaN single crystal can be grown on the (001) plane of the rare earth gallium perovskite.
[0032]
Therefore, by using this high-quality GaN single crystal, it is possible to manufacture a semiconductor device such as a thermally and chemically stable high-performance blue light-emitting diode or semiconductor laser.
[0033]
In the present embodiment, the case where a NdGaO 3 single crystal substrate is used as a rare earth gallium perovskite and a GaN single crystal is grown has been described. However, the present invention is not limited to this, and one or more other rare earth elements are added. The present invention can also be applied to the case where a gallium nitride compound semiconductor single crystal other than GaN is grown on a rare earth 13 (3B) group perovskite single crystal substrate.
[0034]
In this embodiment, the case where N 2 gas is used as the inert gas has been described. However, the present invention is not limited to this, and other inert gases can also be used.
[0035]
【The invention's effect】
The present invention provides a method for growing a gallium nitride-based compound semiconductor single crystal using a single crystal of a rare earth 13 (3B) group perovskite containing one or more rare earth elements as a substrate, on the substrate under a first temperature condition. A first film-forming process for growing a first gallium nitride layer, a heat-treating process in which the substrate is heated to a predetermined temperature in an inert gas atmosphere, and after the heat-treating process, At least a second film-forming step for growing a second gallium nitride layer on the first gallium nitride layer under a second temperature condition set higher than the first temperature condition. Thus, it is possible to solve the problems such as the conventional peeling of the first layer of GaN and to obtain a good quality gallium nitride compound semiconductor single crystal.
Claims (6)
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|---|---|---|---|
| JP16719498A JP4065055B2 (en) | 1998-06-15 | 1998-06-15 | Method for growing gallium nitride compound semiconductor single crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16719498A JP4065055B2 (en) | 1998-06-15 | 1998-06-15 | Method for growing gallium nitride compound semiconductor single crystal |
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| JP2000004045A JP2000004045A (en) | 2000-01-07 |
| JP4065055B2 true JP4065055B2 (en) | 2008-03-19 |
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|---|---|---|---|---|
| JP4673514B2 (en) * | 2001-08-06 | 2011-04-20 | Ｊｘ日鉱日石金属株式会社 | GaN compound semiconductor crystal manufacturing method |
| JP2003218043A (en) * | 2002-01-28 | 2003-07-31 | Nikko Materials Co Ltd | METHOD OF MANUFACTURING GaN-BASED COMPOUND SEMICONDUCTOR CRYSTAL |
| JP4150527B2 (en) | 2002-02-27 | 2008-09-17 | 日鉱金属株式会社 | Crystal production method |
| CN113930745A (en) * | 2021-09-30 | 2022-01-14 | 北京工业大学 | Preparation method of high-crystallization GaN film |
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