JP2007204319A - Nitride-based semiconductor substrate, its producing method and nitride-based semiconductor light-emitting element - Google Patents

Nitride-based semiconductor substrate, its producing method and nitride-based semiconductor light-emitting element Download PDF

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JP2007204319A
JP2007204319A JP2006025656A JP2006025656A JP2007204319A JP 2007204319 A JP2007204319 A JP 2007204319A JP 2006025656 A JP2006025656 A JP 2006025656A JP 2006025656 A JP2006025656 A JP 2006025656A JP 2007204319 A JP2007204319 A JP 2007204319A
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JP4609334B2 (en
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Takamasa Suzuki
貴征 鈴木
Takeshi Meguro
健 目黒
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Hitachi Cable Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a nitride-based semiconductor substrate with a low dislocation density, its producing method at a low cost and with high productivity and a nitride-based semiconductor light-emitting element having high light-emitting output and being formed by using the above substrate. <P>SOLUTION: After a primary GaN layer is grown on a sapphire substrate to be a film thickness of 10 μm or more at a growing velocity of 500 μm/hr or less, a secondary GaN layer is grown on the primary GaN layer at a growing velocity of 600 μm/hr or more and then the nitride-based semiconductor substrate is produced. The nitride-based semiconductor light-emitting element is produced by using the substrate. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、窒化物系半導体基板の製造方法、窒化物系半導体基板、及び窒化物系半導体発光素子に係り、特に、転位密度が低い窒化物系半導体基板を安価かつ生産性良く製造する方法、及び低転位密度の窒化物系半導体基板、並びに当該基板を用いて形成した発光出力の高い窒化物系半導体発光素子に関するものである。   The present invention relates to a method for producing a nitride semiconductor substrate, a nitride semiconductor substrate, and a nitride semiconductor light emitting device, and in particular, a method for producing a nitride semiconductor substrate having a low dislocation density at low cost and high productivity, The present invention also relates to a nitride semiconductor substrate having a low dislocation density, and a nitride semiconductor light emitting device having a high light emission output formed using the substrate.

窒化ガリウム（ＧａＮ）、窒化インジウムガリウム（ＩｎＧａＮ）、窒化ガリウムアルミニウム（ＡｌＧａＮ）等のＧａＮ系化合物半導体は、青色発光ダイオード（ＬＥＤ）やレーザーダイオ−ド（ＬＤ）用材料として、現在脚光を浴びているが、さらに、耐熱性や耐環境性が良いという特徴を活かして、電子デバイス用素子への応用開発も始まっている。   GaN-based compound semiconductors such as gallium nitride (GaN), indium gallium nitride (InGaN), and gallium aluminum nitride (AlGaN) are currently in the limelight as materials for blue light emitting diodes (LEDs) and laser diodes (LDs). However, taking advantage of its good heat resistance and environmental resistance, application development for electronic device elements has also begun.

ＧａＮ系化合物半導体を成長させるための基板としては、これまで、単結晶サファイア基板が利用されてきた。   A single crystal sapphire substrate has been used as a substrate for growing a GaN-based compound semiconductor.

しかしながら、サファイア基板はＧａＮと格子定数が異なるため、サファイア基板上に直接ＧａＮを成長させたのではＧａＮの単結晶膜を得ることができない。このため、サファイア基板上に一旦低温でＡｌＮやＧａＮのバッファ層を成長させ、この低温成長バッファ層で格子の歪みを緩和させてからその上にＧａＮを成長させる方法が考案されている（例えば、特許文献１参照）。   However, since the sapphire substrate has a lattice constant different from that of GaN, a single crystal film of GaN cannot be obtained by directly growing GaN on the sapphire substrate. For this reason, a method has been devised in which an AlN or GaN buffer layer is once grown on a sapphire substrate at a low temperature, and lattice distortion is relaxed in the low temperature growth buffer layer, and then GaN is grown thereon (for example, Patent Document 1).

この低温成長窒化物層をバッファ層として用いることで、ＧａＮの単結晶エピタキシャル成長は可能になったが、この方法でも、やはり基板と結晶の格子のずれは如何ともし難く、成長後のＧａＮは無数の欠陥を有している。この欠陥は、ＧａＮ系ＬＤや高輝度ＬＥＤを製作する上で障害となることが予想される。   By using this low-temperature grown nitride layer as a buffer layer, single-crystal epitaxial growth of GaN has become possible, but even with this method, the deviation between the lattice of the substrate and the crystal is still difficult, and innumerable GaN after growth Have defects. This defect is expected to be an obstacle in manufacturing GaN-based LDs and high-brightness LEDs.

上記のような理由から、基板と結晶との格子のずれが生じないＧａＮ自立基板が切望されている。ＧａＮ自立基板は、ＧａＮがＳｉやＧａＡｓのように融液から大型のインゴットを引き上げて製造することが困難なため、例えば、サファイア基板やガリウム砒素などの異種基板上にＨＶＰＥ(ハイドライド気相成長法：Hydride Vapor Phase Epitaxy)法等によりＧａＮ層を成長した後、ＧａＮ層のみを残すように下地基板を除去することにより得られる。通常は、生産性を上げるため、サファイア基板やガリウム砒素などの異種基板上に、窒化物半導体層を６００μｍ／時以上の速度で成長させる。
特開平４−２９７０２３号公報 For the reasons described above, a GaN free-standing substrate that does not cause a lattice shift between the substrate and the crystal is desired. Since a GaN free-standing substrate is difficult to manufacture by pulling a large ingot from a melt such as Si or GaAs, for example, HVPE (hydride vapor phase epitaxy) is formed on a dissimilar substrate such as a sapphire substrate or gallium arsenide. Obtained by removing the base substrate so as to leave only the GaN layer after the GaN layer is grown by a method such as (Hydride Vapor Phase Epitaxy). Usually, in order to increase productivity, a nitride semiconductor layer is grown at a rate of 600 μm / hour or more on a dissimilar substrate such as a sapphire substrate or gallium arsenide.
Japanese Patent Laid-Open No. 4-297003

しかしながら、上記の方法においても、サファイアなどの格子不整合の大きい異種基板上にＧａＮ層をエピタキシャル成長させるため、通常、異種基板とＧａＮ成長層界面から高密度の転位が発生する。この高密度の転位はＧａＮ層中を貫通する、いわゆる貫通転位となって表面まで達するため、下地基板を除去してＧａＮ自立基板としても、その上に形成する発光素子構造中にも転位が伝播してしまう。この転位は非発光中心となり、デバイス性能を劣化させる原因となる。   However, also in the above method, since a GaN layer is epitaxially grown on a heterogeneous substrate having a large lattice mismatch, such as sapphire, usually high-density dislocations are generated from the interface between the heterogeneous substrate and the GaN growth layer. Since this high-density dislocation penetrates the GaN layer and reaches the surface as a so-called threading dislocation, the dislocation propagates in the light-emitting element structure formed on the GaN free-standing substrate by removing the base substrate. Resulting in. This dislocation becomes a non-light-emitting center and causes deterioration in device performance.

転位密度を低減するためには、異種基板上にＧａＮ層を形成する際、成長初期に形成される成長核の発生密度を少なくしなければならない。成長核の発生密度を少なくするためには、基板に到達した原料が次々に核形成しないように、表面マイグレーションを促進すべく、ＧａＮ層の成長速度を遅くする必要がある。   In order to reduce the dislocation density, when a GaN layer is formed on a heterogeneous substrate, the generation density of growth nuclei formed at the initial stage of growth must be reduced. In order to reduce the generation density of growth nuclei, it is necessary to slow down the growth rate of the GaN layer so as to promote surface migration so that the raw materials reaching the substrate do not nucleate one after another.

しかしながら、単純に成長速度を遅くすると、同じ厚さを作るのにも非常に時間がかかるため、生産効率が低下し、コスト面で不利になってしまう。   However, if the growth rate is simply slowed down, it takes a very long time to produce the same thickness, resulting in a decrease in production efficiency and a disadvantage in cost.

従って、本発明の目的は、上述の問題を解決し、転位密度が低い窒化物系半導体基板を安価かつ生産性良く製造する方法、及び低転位密度の窒化物系半導体基板、並びに当該基板を用いて形成した発光出力の高い窒化物系半導体発光素子を提供することにある。   Accordingly, an object of the present invention is to solve the above-mentioned problems, to use a method for manufacturing a nitride semiconductor substrate having a low dislocation density at low cost and with high productivity, a nitride semiconductor substrate having a low dislocation density, and the substrate. It is an object of the present invention to provide a nitride-based semiconductor light-emitting device having a high light emission output.

上記目的を達成するため、本発明の窒化物系半導体基板の製造方法は、異種基板上に、第１の窒化物系半導体層を成長させる工程と、前記第１の窒化物系半導体層上に、第２の窒化物系半導体層を成長させる工程とを備え、前記第１の窒化物系半導体層の成長速度を、前記第２の窒化物系半導体層の成長速度よりも遅くしたことを特徴とする。   In order to achieve the above object, a method for producing a nitride-based semiconductor substrate according to the present invention includes a step of growing a first nitride-based semiconductor layer on a dissimilar substrate, and a step of growing on the first nitride-based semiconductor layer. And a step of growing a second nitride-based semiconductor layer, wherein the growth rate of the first nitride-based semiconductor layer is made slower than the growth rate of the second nitride-based semiconductor layer. And

前記第１の窒化物系半導体層の成長速度が５００μｍ／時以下であり、前記第２の窒化物系半導体層の成長速度が６００μｍ／時以上であることが好ましい。   The growth rate of the first nitride-based semiconductor layer is preferably 500 μm / hour or less, and the growth rate of the second nitride-based semiconductor layer is preferably 600 μm / hour or more.

更に、前記第１の窒化物系半導体層の成長速度が３００μｍ／時以下であり、前記第２の窒化物系半導体層の成長速度が６００μｍ／時以上であることがより好ましい。   Furthermore, it is more preferable that the growth rate of the first nitride-based semiconductor layer is 300 μm / hour or less and the growth rate of the second nitride-based semiconductor layer is 600 μm / hour or more.

前記第１の窒化物系半導体層及び前記第２の窒化物系半導体層をＧａＮ層、前記異種基板をサファイアとすることができる。   The first nitride semiconductor layer and the second nitride semiconductor layer may be GaN layers, and the dissimilar substrate may be sapphire.

前記第１の窒化物系半導体層を成長させる工程及び前記第２の窒化物系半導体層を成長させる工程は、ハイドライド気相成長法により行うことが好ましい。   The step of growing the first nitride-based semiconductor layer and the step of growing the second nitride-based semiconductor layer are preferably performed by a hydride vapor phase growth method.

前記第１の窒化物系半導体層を膜厚が１０μｍ以上になるように成長させることが好ましく、２５μｍ以上になるように成長させることがより好ましい。   The first nitride-based semiconductor layer is preferably grown so as to have a thickness of 10 μm or more, and more preferably grown so as to have a thickness of 25 μm or more.

また、本発明の窒化物系半導体基板の製造方法は、サファイア基板上に、第１のＧａＮ層を成長速度が５００μｍ／時以下で膜厚が１０μｍ以上になるように成長させる工程と、前記第１のＧａＮ層上に、第２のＧａＮ層を成長速度が６００μｍ／時以上で成長させる工程とを備えることを特徴とする。   The method for producing a nitride-based semiconductor substrate according to the present invention includes a step of growing a first GaN layer on a sapphire substrate so that the growth rate is 500 μm / hour or less and the film thickness is 10 μm or more. And a step of growing a second GaN layer on the first GaN layer at a growth rate of 600 μm / hour or more.

前記第１のＧａＮ層の成長速度が３００μｍ／時以下であることが好ましく、前記第１のＧａＮ層の膜厚が２５μｍ以上であることが望ましい。   The growth rate of the first GaN layer is preferably 300 μm / hour or less, and the film thickness of the first GaN layer is preferably 25 μm or more.

また、上記目的を達成するため、本発明の窒化物系半導体基板は、表面のピット数が１平方ｃｍ当たり１００個以下であることを特徴とする。   In order to achieve the above object, the nitride semiconductor substrate of the present invention is characterized in that the number of pits on the surface is 100 or less per square centimeter.

更に、前記窒化物系半導体基板の製造方法により得られた窒化物系半導体基板上に、少なくとも窒化物系半導体からなる発光層を成長させて窒化物系半導体発光素子を作製することができる。   Furthermore, a nitride-based semiconductor light-emitting device can be manufactured by growing a light-emitting layer made of at least a nitride-based semiconductor on the nitride-based semiconductor substrate obtained by the method for manufacturing a nitride-based semiconductor substrate.

本発明の窒化物系半導体基板の製造方法によれば、転位密度が低い窒化物系半導体基板を安価かつ生産性良く製造することができる。従って、この窒化物系半導体基板上にＬＥＤなどの半導体発光素子を作製すれば、発光出力を飛躍的に向上させることができる。   According to the method for producing a nitride semiconductor substrate of the present invention, a nitride semiconductor substrate having a low dislocation density can be produced at low cost and with high productivity. Therefore, if a semiconductor light emitting element such as an LED is fabricated on the nitride semiconductor substrate, the light emission output can be drastically improved.

以下、本発明の実施形態に係るＧａＮ自立基板の製造方法について説明する。
図１に、本実施形態の製造方法で使用するＨＶＰＥ反応炉の例を示す。
このＨＶＰＥ反応炉１０は、横長の石英反応管１の外側にヒータ２を設けて加熱するホットウォール式であり、石英反応管１の図面左側（上流側）には、Ｖ族原料となるＮＨ３ガスを導入するＮＨ３導入管３と、III族原料となるＧａＣｌを形成するためのＨＣｌガスを導入するＨＣｌ導入管４と、導電性制御のためのドーパントガスを導入するドーピング管５とを備えている。また、ＨＣｌ導入管４は、途中が拡径されてメタルボード６が形成されており、Ｇａメタル７を収容できるようになっている。一方、石英反応管１内の図面右側（下流側）には、下地基板８を配置した基板ホルダ９が回転昇降自在に設けられている。 Hereinafter, a method for manufacturing a GaN free-standing substrate according to an embodiment of the present invention will be described.
In FIG. 1, the example of the HVPE reactor used with the manufacturing method of this embodiment is shown.
This HVPE reaction furnace 10 is a hot wall type in which a heater 2 is provided outside the horizontally long quartz reaction tube 1 to heat it, and NH 3 serving as a group V material is shown on the left side (upstream side) of the quartz reaction tube 1 in the drawing. NH 3 introduction tube 3 for introducing gas, HCl introduction tube 4 for introducing HCl gas for forming GaCl as a group III material, and doping tube 5 for introducing a dopant gas for conductivity control are provided. ing. Further, the HCl introduction pipe 4 is enlarged in diameter in the middle to form a metal board 6 so that Ga metal 7 can be accommodated. On the other hand, on the right side (downstream side) of the quartz reaction tube 1 in the drawing, a substrate holder 9 on which a base substrate 8 is arranged is provided so as to be rotatable up and down.

このＨＶＰＥ反応炉１０を用いてＧａＮを成長させるには、まず、メタルボード６をＧａの融点以上の温度に加熱してＧａメタル７を溶解し、Ｇａ融液を形成する。次に、ＮＨ３導入管３からＶ族原料となるＮＨ３ガスを、ＨＣｌ導入管４からIII族原料となるＨＣｌガスを、ドーピング管５からドーパント成分を含むガスを導入する。なお、反応性の制御の点から、原料ガスであるＨＣｌガス及びＮＨ３ガスは、Ｈ２ガスなどのキャリアガスと混合して用いられる。 In order to grow GaN using the HVPE reactor 10, first, the metal board 6 is heated to a temperature equal to or higher than the melting point of Ga to dissolve the Ga metal 7, thereby forming a Ga melt. Next, an NH 3 gas as a group V material is introduced from the NH 3 introduction tube 3, an HCl gas as a group III material is introduced from the HCl introduction tube 4, and a gas containing a dopant component is introduced from the doping tube 5. From the viewpoint of controlling the reactivity, HCl gas and NH 3 gas, which are raw material gases, are used by being mixed with a carrier gas such as H 2 gas.

ＨＣｌ導入管４では、途中で、ＨＣｌガスがＧａ融液と接触して、Ｇａ＋ＨＣｌ→ＧａＣｌ＋（１／２）Ｈ２という反応が起こり塩化ガリウムＧａＣｌを生成する。 In the HCl introduction tube 4, HCl gas comes into contact with the Ga melt and a reaction of Ga + HCl → GaCl + (1/2) H 2 occurs to generate gallium chloride GaCl.

このＧａＣｌガスとキャリアガスＨ２の混合ガス、及びアンモニアＮＨ３とキャリアガスＨ２の混合ガスが石英反応管１内の空間内を矢印方向に運ばれ、基板ホルダ９に設けられた下地基板８上で、ＧａＣｌ＋ＮＨ３→ＧａＮ＋ＨＣｌ＋Ｈ２の反応が起こり、下地基板８上にＧａＮが堆積される。なお、ＨＶＰＥ法においては、雰囲気温度を８００℃〜１０５０℃程度の高温にしてＧａＮ単結晶をエピタキシャル成長させる。なお、排ガスは図示しない排ガス出口から排出される。 The mixed gas of this GaCl gas and carrier gas H 2 and the mixed gas of ammonia NH 3 and carrier gas H 2 are carried in the space in the quartz reaction tube 1 in the direction of the arrow, and the base substrate 8 provided on the substrate holder 9. Above, a reaction of GaCl + NH 3 → GaN + HCl + H 2 occurs, and GaN is deposited on the base substrate 8. In the HVPE method, the GaN single crystal is epitaxially grown at an atmospheric temperature of about 800 ° C. to 1050 ° C. The exhaust gas is discharged from an exhaust gas outlet (not shown).

図１に示すＨＶＰＥ反応炉１０を用い、以下のようにしてＧａＮ自立基板を製造した。
まず、基板ホルダ９に下地基板８として２インチφのサファイア基板を固定し、石英からなるメタルボード６にＧａメタル７を配置した。次に、Ｇａメタル７のメタルボート６を９００℃に、基板ホルダ９を５１０℃に加熱した。さらに、ＨＣｌ導入管４から水素キャリアガスと共にＨＣｌガスを導入する一方、ＮＨ３導入管３から窒素キャリアガスと共にアンモニアガスを導入した。そして、ＨＣｌ導入管４内でＨＣｌガスとＧａを反応させてＧａＣｌを生成させ、このＧａＣｌとアンモニアガスとをサファイア基板上で反応させてＧａＮよりなるバッファ層を３０ｎｍの膜厚で成長させた。 Using the HVPE reactor 10 shown in FIG. 1, a GaN free-standing substrate was manufactured as follows.
First, a 2 inch φ sapphire substrate was fixed to the substrate holder 9 as the base substrate 8, and the Ga metal 7 was disposed on the metal board 6 made of quartz. Next, the metal boat 6 of Ga metal 7 was heated to 900 ° C., and the substrate holder 9 was heated to 510 ° C. Further, HCl gas was introduced from the HCl introduction pipe 4 together with hydrogen carrier gas, while ammonia gas was introduced from the NH 3 introduction pipe 3 together with nitrogen carrier gas. Then, HCl gas and Ga were reacted in the HCl introduction tube 4 to generate GaCl, and this GaCl and ammonia gas were reacted on the sapphire substrate to grow a buffer layer made of GaN with a film thickness of 30 nm.

バッファ層成長後、サファイア基板側の温度を１０５０℃に上昇させ、第１のＧａＮ層を成長速度５０〜６００μｍ／時の範囲内で０.１〜２.４時間成長させ、厚さが１２０μｍになるように形成した。その後、第１のＧａＮ層と同じ温度で第１のＧａＮ層上に第２のＧａＮ層を成長速度６００μｍ／時で成長させた。第１のＧａＮ層と第２のＧａＮ層との総膜厚は、およそ５００μｍになるようにした。   After growing the buffer layer, the temperature on the sapphire substrate side is raised to 1050 ° C., and the first GaN layer is grown for 0.1 to 2.4 hours at a growth rate of 50 to 600 μm / hour to a thickness of 120 μm. It formed so that it might become. Thereafter, a second GaN layer was grown on the first GaN layer at the same temperature as the first GaN layer at a growth rate of 600 μm / hour. The total film thickness of the first GaN layer and the second GaN layer was about 500 μm.

第２のＧａＮ層が成長した後、作製したウェーハをＨＶＰＥ反応炉１０から取り出して研磨装置に移送し、ダイヤモンド研磨剤を用いてサファイア基板側をラッピングし、サファイア基板とバッファ層とを除去した。続いて、さらに細かいダイヤモンド研磨剤を用いてポリシングして、膜厚４００μｍのＧａＮ自立基板を得た。   After the growth of the second GaN layer, the produced wafer was taken out from the HVPE reactor 10 and transferred to a polishing apparatus, and the sapphire substrate side was lapped with a diamond abrasive to remove the sapphire substrate and the buffer layer. Subsequently, polishing was performed using a finer diamond abrasive to obtain a GaN free-standing substrate having a thickness of 400 μm.

以上のような製造方法により得られたＧａＮ自立基板について、成長速度を５０〜６００μｍ／時の範囲で変化させた場合の第２のＧａＮ層の表面の転位密度について調べた。   Regarding the GaN free-standing substrate obtained by the above manufacturing method, the dislocation density on the surface of the second GaN layer when the growth rate was changed in the range of 50 to 600 μm / hour was examined.

表１及び図２に、成長速度と転位密度の関係を示す。   Table 1 and FIG. 2 show the relationship between the growth rate and the dislocation density.

Figure 2007204319
Figure 2007204319

表１及び図２の結果より、転位密度は、成長速度の低下に伴って減少し、成長速度を５０μｍ／時にした時に最も転位密度が低くなっていることが分かる。これは、第１のＧａＮ層の成長速度を第２のＧａＮ層の成長速度よりも遅くしたことにより、成長初期に形成される核密度が少なくなったため、核の融合時における転位の発生が減った結果、転位密度が低くなったと考えられる。他方、第１のＧａＮ層の成長速度が６００μｍ／時の場合は、転位密度が極端に高くなっている。これは、上述の理由とは逆に、核密度が増えて転位密度も増えたためと考えられる。   From the results of Table 1 and FIG. 2, it can be seen that the dislocation density decreases as the growth rate decreases, and the dislocation density is the lowest when the growth rate is 50 μm / hour. This is because the growth rate of the first GaN layer is slower than the growth rate of the second GaN layer, so that the density of nuclei formed at the initial stage of growth is reduced, so that the generation of dislocations during fusion of nuclei is reduced. As a result, it is considered that the dislocation density was lowered. On the other hand, when the growth rate of the first GaN layer is 600 μm / hour, the dislocation density is extremely high. This is thought to be because, contrary to the above reasons, the nuclear density increased and the dislocation density also increased.

次に、図１に示すＨＶＰＥ反応炉を用いて、実施例１と同様にＧａＮ自立基板を製造した。この際、第１のＧａＮ層の成長速度を５０μｍ／時と一定にして、成長時間を変化させ、第１のＧａＮ層の膜厚を５〜１００μｍの範囲で変化させた場合の第２のＧａＮ層の表面の転位密度について調べた。   Next, a GaN free-standing substrate was manufactured in the same manner as in Example 1 using the HVPE reactor shown in FIG. At this time, the growth rate of the first GaN layer is kept constant at 50 μm / hour, the growth time is changed, and the second GaN when the film thickness of the first GaN layer is changed in the range of 5 to 100 μm. The dislocation density on the surface of the layer was investigated.

表２及び図３に、成長速度と転位密度の関係を示す。   Table 2 and FIG. 3 show the relationship between the growth rate and the dislocation density.

Figure 2007204319
Figure 2007204319

表２及び図３の結果より、第１のＧａＮ層の膜厚が５μｍの時は転位密度が極端に高くなったが、２５μｍになると大幅に減少し、転位密度は１００μｍまで減少した。これは、第１のＧａＮ層の膜厚が薄いと、核が全面を埋め尽くす前に第２のＧａＮ層の成長に移ってしまい、その結果、成長の初期から成長速度を速くして成長させているのと同じ状態になり、核密度が増えて転位密度が高くなったと考えられる。   From the results shown in Table 2 and FIG. 3, the dislocation density was extremely high when the film thickness of the first GaN layer was 5 μm, but it decreased significantly when the film thickness was 25 μm, and the dislocation density decreased to 100 μm. This is because if the film thickness of the first GaN layer is small, the growth proceeds to the growth of the second GaN layer before the nuclei fill the entire surface. As a result, the growth rate is increased from the initial stage of the growth. It is considered that the dislocation density increased as the nuclear density increased.

実施例１及び実施例２で作成したＧａＮ自立基板を用いて、窒化物系半導体発光素子を製造した。
図４は、実施例３で製造した窒化物系半導体発光素子を示す構造断面図である。
この窒化物系半導体発光素子２０は、ＧａＮ自立基板１１上に、順に、ｎ−ＧａＮ層１２、ＩｎＧａＮ井戸層１４とＧａＮ障壁層１５とを交互に形成した多重量子井戸構造１３、ｐ−ＡｌＧａＮクラッド層１６、ｐ−ＧａＮコンタクト層１７を設け、ＧａＮ自立基板１１側に負電極１８、ｐ−ＧａＮコンタクト層１７側に正電極１９を形成したものである。 Using the GaN free-standing substrate created in Example 1 and Example 2, a nitride-based semiconductor light emitting device was manufactured.
4 is a structural cross-sectional view showing the nitride-based semiconductor light-emitting device manufactured in Example 3. FIG.
The nitride-based semiconductor light-emitting device 20 includes a multiple quantum well structure 13 in which n-GaN layers 12, InGaN well layers 14 and GaN barrier layers 15 are alternately formed on a GaN free-standing substrate 11, and a p-AlGaN cladding. The layer 16 and the p-GaN contact layer 17 are provided, the negative electrode 18 is formed on the GaN free-standing substrate 11 side, and the positive electrode 19 is formed on the p-GaN contact layer 17 side.

この窒化物系半導体発光素子２０を有機金属気相成長（ＭＯＣＶＤ）法により以下のようにして製造した。
まず、周知の有機金属原料として、トリメチルガリウム（ＴＭＧ），トリメチルアルミニウム（ＴＭＡ），トリメチルインジウム（ＴＭＩ），ビスシクロペンタジエニルマグネシウム（Ｃｐ２Ｍｇ）を用いた。ガス原料として、アンモニア（ＮＨ３），シラン（ＳｉＨ４）を用いた。また、キャリアガスとして、水素及び窒素を用いた。
上記の原料及びキャリアガスを用いて、実施例１及び実施例２で得られたＧａＮ自立基板１１上に、１０５０℃にて、Ｓｉを１×１０１９ｃｍ−３ドープしたｎ型ＧａＮ層１２を４μｍの膜厚で成長させた。
次に、活性層として、厚さ３ｎｍのアンドープＩｎ０．１Ｇａ０．９Ｎ井戸層１４を３層、厚さ１０ｎｍのアンドープＧａＮ障壁層１５を４層交互に形成した多重量子井戸構造（ＭＱＷ）１３を有するアンドープＩｎＧａＮ系活性層を８００℃で成長させた。
更に、その上に、ｐ型Ａｌ０．１Ｇａ０．９Ｎクラッド層１６、ｐ型ＧａＮコンタクト層１７を順に形成し、最後に、ＧａＮ自立基板１１側に負電極１８、ｐ−ＧａＮコンタクト層１７側に正電極１９を形成した。 This nitride-based semiconductor light emitting device 20 was manufactured by the metal organic chemical vapor deposition (MOCVD) method as follows.
First, trimethylgallium (TMG), trimethylaluminum (TMA), trimethylindium (TMI), and biscyclopentadienylmagnesium (Cp 2 Mg) were used as known organometallic raw materials. Ammonia (NH 3 ) and silane (SiH 4 ) were used as gas raw materials. Moreover, hydrogen and nitrogen were used as carrier gas.
An n-type GaN layer 12 doped with Si at 1 × 10 19 cm −3 at 1050 ° C. is formed on the GaN free-standing substrate 11 obtained in Example 1 and Example 2 using the above raw materials and carrier gas. The film was grown with a thickness of 4 μm.
Next, as an active layer, a multiple quantum well structure (MQW) in which three undoped In 0.1 Ga 0.9 N well layers 14 having a thickness of 3 nm and four undoped GaN barrier layers 15 having a thickness of 10 nm are alternately formed. ) 13 was grown at 800 ° C.
Further, a p-type Al 0.1 Ga 0.9 N clad layer 16 and a p-type GaN contact layer 17 are sequentially formed thereon, and finally, a negative electrode 18 and a p-GaN contact layer are formed on the GaN free-standing substrate 11 side. A positive electrode 19 was formed on the 17 side.

表３及び図５に、実施例１及び２で作製したＧａＮ自立基板の条件Ｎｏ１〜９と、実施例３で作製した発光素子の発光出力との関係を示す。   Table 3 and FIG. 5 show the relationship between the condition Nos. 1 to 9 of the GaN free-standing substrate produced in Examples 1 and 2 and the light emission output of the light emitting device produced in Example 3.

Figure 2007204319
Figure 2007204319

表３及び図５の結果、成長速度を５０〜３００μｍ／時とした条件Ｎｏ．１〜３、及び成長膜厚を２５〜１００μｍとした条件Ｎｏ．６〜９のＧａＮ自立基板を用いて製造した窒化物系半導体発光素子２０の発光出力は全て４ｍＷ以上と発光出力が良好な値となった。
これに対して、第１のＧａＮ層の成長速度を６００μｍ／時として作製したＧａＮ自立基板（条件Ｎｏ.４）、及び、第１のＧａＮ層の膜厚を５μｍとして作製したＧａＮ自立基板（条件Ｎｏ.５）を用いて製造した窒化物系半導体発光素子２０の発光出力は約２ｍＷ程度となり、大幅に低下した。
また、窒化物系半導体発光素子２０の発光出力はおよそＧａＮ自立基板の転位密度と相関関係があり、転位密度が低いほど発光出力が上がっていることが分かる。 As a result of Table 3 and FIG. 1 to 3 and the growth film thickness is 25 to 100 μm. All of the light emission outputs of the nitride-based semiconductor light-emitting elements 20 manufactured using 6 to 9 GaN free-standing substrates were 4 mW or more, and the light emission output was a good value.
In contrast, a GaN free-standing substrate (condition No. 4) manufactured with a growth rate of the first GaN layer of 600 μm / hour and a GaN free-standing substrate manufactured with a thickness of the first GaN layer of 5 μm (conditions) The light emission output of the nitride-based semiconductor light-emitting element 20 manufactured using No. 5) was about 2 mW, which was greatly reduced.
Further, it can be seen that the light emission output of the nitride-based semiconductor light-emitting element 20 has a correlation with the dislocation density of the GaN free-standing substrate, and the light emission output increases as the dislocation density decreases.

図１に示すＨＶＰＥ反応炉１０を用い、実施例１と同様にしてＧａＮ自立基板を製造した。
まず、基板ホルダ９に下地基板８として２インチφのサファイア基板を固定し、石英からなるメタルボード６にＧａメタル７を配置した。次に、Ｇａメタル７のメタルボート６を９００℃に、基板ホルダ９を５１０℃に加熱した。さらに、ＨＣｌ導入管４から水素キャリアガスと共にＨＣｌガスを導入する一方、ＮＨ３導入管３から窒素キャリアガスと共にアンモニアガスを導入した。そして、ＨＣｌ導入管４内でＨＣｌガスとＧａを反応させてＧａＣｌを生成させ、このＧａＣｌとアンモニアガスとをサファイア基板上で反応させてＧａＮよりなるバッファ層を３０ｎｍの膜厚で成長させた。 A GaN free-standing substrate was manufactured in the same manner as in Example 1 using the HVPE reactor 10 shown in FIG.
First, a 2 inch φ sapphire substrate was fixed to the substrate holder 9 as the base substrate 8, and the Ga metal 7 was disposed on the metal board 6 made of quartz. Next, the metal boat 6 of Ga metal 7 was heated to 900 ° C., and the substrate holder 9 was heated to 510 ° C. Further, HCl gas was introduced from the HCl introduction pipe 4 together with hydrogen carrier gas, while ammonia gas was introduced from the NH 3 introduction pipe 3 together with nitrogen carrier gas. Then, HCl gas and Ga were reacted in the HCl introduction tube 4 to generate GaCl, and this GaCl and ammonia gas were reacted on the sapphire substrate to grow a buffer layer made of GaN with a film thickness of 30 nm.

バッファ層成長後、サファイア基板側の温度を１０５０℃に上昇させ、成長速度１００μｍ／時で３時間成長を行い、厚さ３００μｍのＧａＮ基板を得た。
成長後、作製したウェーハをＨＶＰＥ反応炉１０から取り出し、ウェーハを研磨装置に移送し、ダイヤモンド研磨剤を用いて、サファイア基板側をラッピングし、サファイア基板とバッファ層とを除去した。続いて、さらに細かいダイヤモンド研磨剤を用いてポリシングして、膜厚２７０μｍのＧａＮ自立基板を得た。 After the growth of the buffer layer, the temperature on the sapphire substrate side was raised to 1050 ° C., and growth was performed for 3 hours at a growth rate of 100 μm / hour to obtain a GaN substrate having a thickness of 300 μm.
After the growth, the produced wafer was taken out from the HVPE reactor 10, the wafer was transferred to a polishing apparatus, the sapphire substrate side was lapped using a diamond abrasive, and the sapphire substrate and the buffer layer were removed. Subsequently, polishing was performed using a finer diamond abrasive to obtain a GaN free-standing substrate having a thickness of 270 μm.

以上のようにして得られたＧａＮ自立基板において、表面のピット数と研磨により発生したクラックの発生頻度との関係を調べた。なお、表面のピット数は、光学顕微鏡を用いて確認した。
図６に、表面のピット数とクラックの発生頻度との関係を示す。
図６の結果より、表面のピット数を１００個／ｃｍ２以下とすることにより、クラックの発生頻度が大幅に低下していることが分かった。 In the GaN free-standing substrate obtained as described above, the relationship between the number of pits on the surface and the occurrence frequency of cracks generated by polishing was investigated. The number of pits on the surface was confirmed using an optical microscope.
FIG. 6 shows the relationship between the number of pits on the surface and the occurrence frequency of cracks.
From the results of FIG. 6, it was found that the occurrence frequency of cracks was greatly reduced by setting the number of pits on the surface to 100 pieces / cm 2 or less.

［他の応用例、変形例］
以上述べた実施例においてはアンドープＧａＮ自立基板の例について説明したが、これには限定されず、Ｓｉ等をドープしたｎ型ＧａＮ自立基板やＭｇ等をドープしたｐ型ＧａＮ自立基板、更には、窒化アルミニウムガリウム（ＡｌＧａＮ）や窒化ガリウムインジウム（ＩｎＧａＮ）等の３元混晶の窒化物系単結晶自立基板についても同様に適用することができる。これらの窒化物半導体基板は、自立できハンドリングに不便がないようなものとするため、異種基板上に成長させる第１の窒化物系半導体層と第２の窒化物系半導体層との総膜厚は１００μｍ以上とすることが好ましい。また、ｎ型またはｐ型とする場合には、キャリア密度が１×１０２０ｃｍ−３以下の範囲であることが望ましい。 [Other application examples and modifications]
In the embodiment described above, an example of an undoped GaN free-standing substrate has been described. However, the present invention is not limited to this. An n-type GaN free-standing substrate doped with Si or the like, a p-type GaN free-standing substrate doped with Mg or the like, The present invention can be similarly applied to a ternary mixed crystal nitride single crystal free-standing substrate such as aluminum gallium nitride (AlGaN) or gallium indium nitride (InGaN). Since these nitride semiconductor substrates are self-supporting and have no inconvenience in handling, the total film thickness of the first nitride-based semiconductor layer and the second nitride-based semiconductor layer grown on a different substrate Is preferably 100 μm or more. In the case of n-type or p-type, the carrier density is desirably in the range of 1 × 10 20 cm −3 or less.

また、自立基板の製造のみならず、サファイア等の異種基板上がついたままのものについても適用可能である。また、異種基板としては、サファイア（Ａｌ２Ｏ３）の他に、炭化ケイ素、シリコン、ガリウム砒素など従来から窒化物半導体のエピタキシャル成長に用いられていて、高品質な窒化物半導体が得られている基板や、窒化物半導体の格子定数に近いものを用いることができる。あるいは、基板上に窒化物半導体層を形成した複合基板であってもよい。これら基板は、研磨、溶解（ウェットエッチング）、ドライエッチング、あるいは自然剥離等の手段で除去することができる。 Further, the present invention can be applied not only to the production of a self-supporting substrate, but also to a substrate with a dissimilar substrate such as sapphire attached. Further, as foreign substrate, in addition to a sapphire (Al 2 O 3), silicon carbide, silicon, and the like conventionally gallium arsenide have been used in the nitride semiconductor epitaxial growth, and high-quality nitride semiconductor can be obtained A substrate or a material close to the lattice constant of a nitride semiconductor can be used. Alternatively, a composite substrate in which a nitride semiconductor layer is formed on the substrate may be used. These substrates can be removed by means such as polishing, dissolution (wet etching), dry etching, or natural peeling.

また、実施例では自立基板の製造方法において、ＨＶＰＥ法による成長法のみについて言及したが、他に、昇華法、有機金属気相成長法、液相成長法またはそれらの成長法の２つ以上を組み合わせたもののいずれであってもよい。   In the examples, only the HVPE growth method is referred to in the method for manufacturing a self-supporting substrate, but in addition, a sublimation method, a metal organic vapor phase growth method, a liquid phase growth method, or two or more growth methods thereof are used. Any of the combinations may be used.

実施例で使用するＨＶＰＥ反応炉の概略図である。It is the schematic of the HVPE reactor used in an Example. 第１のＧａＮ層の成長速度とＧａＮ自立基板表面の転位密度との関係を示すグラフである。It is a graph which shows the relationship between the growth rate of a 1st GaN layer, and the dislocation density of the GaN self-supporting substrate surface. 第１のＧａＮ層の成長膜厚とＧａＮ自立基板の表面の転位密度との関係を示すグラフである。It is a graph which shows the relationship between the growth film thickness of a 1st GaN layer, and the dislocation density of the surface of a GaN self-supporting substrate. 実施例３において製造した窒化物系半導体発光素子の断面構造を示す概略図である。6 is a schematic view showing a cross-sectional structure of a nitride-based semiconductor light-emitting element manufactured in Example 3. FIG. 実施例１及び２で作製したＧａＮ自立基板の条件Ｎｏ１〜９と、実施例３で作製した窒化物系半導体発光素子の発光出力との関係を示すグラフである。6 is a graph showing a relationship between conditions No. 1 to 9 of the GaN free-standing substrate manufactured in Examples 1 and 2 and the light emission output of the nitride-based semiconductor light-emitting element manufactured in Example 3. 表面のピット数とクラックの発生頻度との関係を示すグラフである。It is a graph which shows the relationship between the number of pits on the surface and the occurrence frequency of cracks.

符号の説明Explanation of symbols

１ 石英反応管
２ ヒータ
３ ＮＨ３導入管
４ ＨＣｌ導入管
５ ドーピング管
６ メタルボード
７ Ｇａメタル
８ 下地基板
９ 基板ホルダ
１０ ＨＶＰＥ反応炉
１１ ＧａＮ自立基板
１２ ｎ−ＧａＮ層
１３ 多重量子井戸構造
１４ ＩｎＧａＮ井戸層
１５ ＧａＮ障壁層
１６ ｐ−ＡｌＧａＮクラッド層
１７ ｐ−ＧａＮコンタクト層
１８ 負電極
１９ 正電極
２０ 窒化物系半導体発光素子 2 heater 1 quartz reaction tube 3 NH 3 inlet tube 4 HCl inlet tube 5 doping tube 6 metal board 7 Ga metal 8 underlying substrate 9 substrate holder 10 HVPE reactor 11 GaN free-standing substrate 12 n-GaN layer 13 multiple quantum well structure 14 InGaN Well layer 15 GaN barrier layer 16 p-AlGaN cladding layer 17 p-GaN contact layer 18 negative electrode 19 positive electrode 20 nitride semiconductor light emitting device

Claims (12)

異種基板上に、第１の窒化物系半導体層を成長させる工程と、
前記第１の窒化物系半導体層上に、第２の窒化物系半導体層を成長させる工程とを備え、
前記第１の窒化物系半導体層の成長速度を、前記第２の窒化物系半導体層の成長速度よりも遅くしたことを特徴とする窒化物系半導体基板の製造方法。 Growing a first nitride-based semiconductor layer on a heterogeneous substrate;
Growing a second nitride-based semiconductor layer on the first nitride-based semiconductor layer,
A method for producing a nitride-based semiconductor substrate, wherein the growth rate of the first nitride-based semiconductor layer is made slower than the growth rate of the second nitride-based semiconductor layer. 前記第１の窒化物系半導体層の成長速度が５００μｍ／時以下であり、前記第２の窒化物系半導体層の成長速度が６００μｍ／時以上であることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The nitriding according to claim 1, wherein the growth rate of the first nitride-based semiconductor layer is 500 μm / hour or less, and the growth rate of the second nitride-based semiconductor layer is 600 μm / hour or more. A method for manufacturing a physical semiconductor substrate. 前記第１の窒化物系半導体層の成長速度が３００μｍ／時以下であり、前記第２の窒化物系半導体層の成長速度が６００μｍ／時以上であることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The nitriding according to claim 1, wherein the growth rate of the first nitride-based semiconductor layer is 300 μm / hour or less, and the growth rate of the second nitride-based semiconductor layer is 600 μm / hour or more. A method for manufacturing a physical semiconductor substrate. 前記第１の窒化物系半導体層及び前記第２の窒化物系半導体層がＧａＮ層であり、前記異種基板がサファイアであることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The method of manufacturing a nitride semiconductor substrate according to claim 1, wherein the first nitride semiconductor layer and the second nitride semiconductor layer are GaN layers, and the heterogeneous substrate is sapphire. . 前記第１の窒化物系半導体層を成長させる工程及び前記第２の窒化物系半導体層を成長させる工程は、ハイドライド気相成長法により行われることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The nitride system according to claim 1, wherein the step of growing the first nitride-based semiconductor layer and the step of growing the second nitride-based semiconductor layer are performed by hydride vapor phase epitaxy. A method for manufacturing a semiconductor substrate. 前記第１の窒化物系半導体層を膜厚が１０μｍ以上になるように成長させることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The method of manufacturing a nitride semiconductor substrate according to claim 1, wherein the first nitride semiconductor layer is grown to have a thickness of 10 [mu] m or more. 前記第１の窒化物系半導体層を膜厚が２５μｍ以上になるように成長させることを特徴とする請求項１記載の窒化物系半導体基板の製造方法。   2. The method for manufacturing a nitride semiconductor substrate according to claim 1, wherein the first nitride semiconductor layer is grown to have a thickness of 25 [mu] m or more. サファイア基板上に、第１のＧａＮ層を成長速度が５００μｍ／時以下で膜厚が１０μｍ以上になるように成長させる工程と、
前記第１のＧａＮ層上に、第２のＧａＮ層を成長速度が６００μｍ／時以上で成長させる工程とを備えることを特徴とする窒化物系半導体基板の製造方法。 Growing the first GaN layer on the sapphire substrate so that the growth rate is 500 μm / hour or less and the film thickness is 10 μm or more;
And a step of growing a second GaN layer on the first GaN layer at a growth rate of 600 μm / hour or more. 前記第１のＧａＮ層の成長速度が３００μｍ／時以下であることを特徴とする請求項８記載の窒化物系半導体基板の製造方法。   9. The method for producing a nitride-based semiconductor substrate according to claim 8, wherein the growth rate of the first GaN layer is 300 μm / hour or less. 前記第１のＧａＮ層の膜厚が２５μｍ以上であることを特徴とする請求項８記載の窒化物系半導体基板の製造方法。   9. The method for manufacturing a nitride-based semiconductor substrate according to claim 8, wherein the first GaN layer has a thickness of 25 μm or more. 表面のピット数が１平方ｃｍ当たり１００個以下であることを特徴とする窒化物系半導体基板。   A nitride semiconductor substrate characterized in that the number of pits on the surface is 100 or less per square centimeter. 請求項１〜１０のいずれか１項記載の窒化物系半導体基板の製造方法により得られた窒化物系半導体基板上に、少なくとも窒化物系半導体からなる発光層を成長させたことを特徴とする窒化物系半導体発光素子。   A light emitting layer made of at least a nitride-based semiconductor is grown on the nitride-based semiconductor substrate obtained by the method for manufacturing a nitride-based semiconductor substrate according to claim 1. Nitride semiconductor light emitting device.
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