JP4811082B2 - N-type AlN crystal and manufacturing method thereof - Google Patents
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Description
本発明は、ワイドバンドギャップ半導体として開発が進められている、低抵抗ｎ型ＡｌＮ結晶及びその製造方法に関するものである。 The present invention relates to a low-resistance n-type AlN crystal being developed as a wide band gap semiconductor and a method for manufacturing the same.
ＡｌＮ（窒化アルミニウム）は、バンドギャップが大きい（６．５ｅＶ）のに加え、高い熱伝導率（３２０Ｗ／ｍＫ）や耐熱性等多くの優れた特性を有することから、高密度記録に必要な短波長発光素子やパワーデバイスへの利用が期待されている。これらの用途に用いられるためには、ドーピングによってｐ，ｎ型結晶を合成する必要があり、多方面で検討が行われている。 AlN (aluminum nitride) has many excellent characteristics such as high thermal conductivity (320 W / mK) and heat resistance, in addition to a large band gap (6.5 eV), and therefore it is a short necessary for high-density recording. Use in wavelength light emitting devices and power devices is expected. In order to be used for these applications, it is necessary to synthesize p-type and n-type crystals by doping, and various studies have been conducted.
例えば、原子状のビームを用いて、Ｃ原子とＯ原子を同時ドーピングしたＡｌＮ結晶を合成し、Ｃ，Ｏの比率によってｐ型やｎ型の半導体を得た事例（特許文献１参照）や、ＭＯＣＶＤを用いたＡｌＮ合成時にＳｉを導入し、キャリア濃度が約１０17cm-3のｎ型ＡｌＮ結晶を得た事例（非特許文献１参照）が報告されている。しかし、これらの方法では、生産性やキャリア濃度が十分ではないという問題があった。本発明は、これらの問題を解決するためになされた。
従来の技術において不十分であった生産性やキャリア濃度という問題を解決し、低抵抗ｎ型ＡｌＮ半導体結晶を提供し、もって短波長発光素子やパワーデバイスを実現することを目的とする。 An object of the present invention is to solve the problems of productivity and carrier concentration, which are insufficient in the prior art, to provide a low resistance n-type AlN semiconductor crystal, and to realize a short wavelength light emitting element and a power device.
本発明は、上記課題を解決するために以下の構成が採用された。
（１）本発明は、ＡｌＮ結晶のＡｌ原子の一部をＩＩＩａ族元素又は／及びＩＩＩｂ族元素で置換し、隣接するＮ原子のうち１原子をＯ原子で同時に置換した構造のｎ型ＡｌＮ結晶であって、前記ＩＩＩａ族元素又は／及びＩＩＩｂ族元素は、Ｙ、Ｓｃ、Ｌａ、Ｃｅ、及びＧａよりなる群から選ばれる１種以上の元素であることを特徴とするｎ型ＡｌＮ結晶である。
（２）本発明は、ＩＩＩａ族元素又は／及びＩＩＩｂ族元素の合計濃度（Ｃ３Ａ）が１×１０１８ｃｍ−３以上であり、Ｏ濃度（ＣＯ）が、０．０１Ｃ３Ａ＜ＣＯ＜１．５Ｃ３Ａであることを特徴とする、請求項１記載のｎ型ＡｌＮ結晶である。
The present invention employs the following configuration in order to solve the above problems.
(1) The present invention, a part of Al atoms in the AlN crystal was replaced with IIIa group element and / or IIIb group elements, n-type AlN crystal simultaneously having a structure resulting from substitution of the one atom in O atom of the adjacent N atom The group IIIa element and / or group IIIb element is an n-type AlN crystal characterized by being one or more elements selected from the group consisting of Y, Sc, La, Ce, and Ga. .
(2) In the present invention, the total concentration (C 3A ) of group IIIa elements and / or group IIIb elements is 1 × 10 18 cm −3 or more, and the O concentration (C O ) is 0.01C 3A <C O The n-type AlN crystal according to claim 1, characterized in that it is <1.5C 3A .
（３）本発明は、ＣＶＤ法又はＭＢＥ法を用いてＡｌＮ結晶を合成する際、IIIａ族元素
又は／及びIIIｂ族元素含有化合物及び酸素（Ｏ) 含有化合物を添加することを特徴とす
る、請求項１又は２記載のｎ型ＡｌＮ結晶の製造方法である。
（４）本発明は、昇華法を用いてＡｌＮ結晶を合成する際、IIIａ族元素又は／及びIIIｂ族元素含有化合物及び酸素（Ｏ) 含有化合物を添加することを特徴とする、請求項１又は２記載のｎ型ＡｌＮ結晶の製造方法である。
（５）本発明は、合成したＡｌＮ結晶を、不活性雰囲気において熱処理することを特徴とする、請求項１又は２記載のｎ型ＡｌＮ結晶の製造方法である。
すなわち本発明によれば、ＡｌＮ結晶のＡｌ原子を、IIIａ族元素又は／及びIIIｂ族元素（以下「III族元素」と略記）で置換し、隣接する窒素（Ｎ）１原子を酸素（Ｏ）原子
で置換することにより、浅い不純物準位が形成され、低抵抗ｎ型ＡｌＮ結晶を得ることが
できる。ここで、IIIａ族元素とは、Ｓｃ，Ｙの他ランタン系及びアクチニウム系の希土
類元素を、IIIｂ族元素とは、Ｂ，Ｇａ，Ｉｎ，Ｔｌを意味する。
(3) The present invention is characterized in that when an AlN crystal is synthesized using a CVD method or an MBE method, a IIIa group element or / and a IIIb group element-containing compound and an oxygen (O) -containing compound are added. Item 3. A method for producing an n-type AlN crystal according to Item 1 or 2.
(4) The present invention is characterized in that when an AlN crystal is synthesized using a sublimation method, a group IIIa element or / and a group IIIb element-containing compound and an oxygen (O) -containing compound are added. 2. A method for producing an n-type AlN crystal according to 2.
(5) The present invention is the method for producing an n-type AlN crystal according to claim 1 or 2, wherein the synthesized AlN crystal is heat-treated in an inert atmosphere.
That is, according to the present invention, an Al atom of an AlN crystal is substituted with a group IIIa element or / and a group IIIb element (hereinafter abbreviated as “group III element”), and one adjacent nitrogen (N) atom is oxygen (O). By substituting with atoms, shallow impurity levels are formed, and a low-resistance n-type AlN crystal can be obtained. Here, the group IIIa element means Sc, Y, lanthanum and actinium rare earth elements, and the group IIIb element means B, Ga, In, Tl.
より具体的には、ＣＶＤ法や昇華法等によってＡｌＮ結晶を合成する際に、III族元素
化合物及び酸素（Ｏ) 含有化合物を添加することによって、これらの元素を含有する結晶を合成し、必要に応じて熱処理（拡散処理）することにより、前述の「Ｍ−Ｏ構造」（ＭはIII族元素）を形成して、浅い不純物準位を有するｎ型半導体を得ることができる。こ
の際、III族元素及び酸素（Ｏ)が単一の化合物中に含有される場合には、必ずしも、複数の化合物を用いる必要はない。
前述のＭ−Ｏ構造形成とその導電性を向上させる効果については、第一原理計算による解析等から、次のような要因があると推定される。
More specifically, when an AlN crystal is synthesized by a CVD method, a sublimation method, or the like, a crystal containing these elements is synthesized by adding a group III element compound and an oxygen (O) -containing compound. By performing heat treatment (diffusion treatment) according to the above, the above-described “MO structure” (M is a group III element) can be formed, and an n-type semiconductor having a shallow impurity level can be obtained. At this time, when the group III element and oxygen (O) are contained in a single compound, it is not always necessary to use a plurality of compounds.
About the effect which improves the above-mentioned MO structure formation and its electroconductivity, it is estimated from the analysis etc. by the first principle calculation that there are the following factors.
構造形成については、Ｍ−Ｏ構造では、格子の歪みが小さく、Ｍ−Ｏ結合エネルギーが極めて強いことも相まって、単独置換する場合に比較してエネルギー的に極めて有利となる。このため、結晶成長中や熱処理中において、Ｍ，Ｏは隣接サイトに選択的に導入されると推定される。この隣接サイト選択置換効果は、Ｍ−Ｏ結合エネルギーが大きいIIIａ
族元素でより顕著である。
Regarding the structure formation, in the MO structure, the lattice distortion is small and the MO bond energy is extremely strong, which is extremely advantageous in terms of energy compared to the case of single substitution. For this reason, it is estimated that M and O are selectively introduced into adjacent sites during crystal growth and heat treatment. This adjacent site selective substitution effect is caused by IIIa having a large MO bond energy.
It is more prominent among group elements.
この構造の効果については、Ｍ−Ｏ結合により、Ｏの結合形態が変化するためと考えている。酸素は、ＡｌＮに相当量（約１０００ｐｐｍ）固溶することが古くから知られており、「ｎ型半導体」となるが、深い不純物準位（３５０〜７００ｍｅＶ）を形成するため、現実には絶縁体的な挙動を示す。この原因は、ＯがＮサイトで偏心するため、非結合手が生じるためと考えられている。III族元素で隣接位置を置換することによって偏心が解
消され、不純物準位が浅くなり、導電性が向上すると推定される。
The effect of this structure is considered to be due to the change of the O bond form due to the M—O bond. It has long been known that oxygen is dissolved in a considerable amount (about 1000 ppm) in AlN, and becomes an “n-type semiconductor”. However, since it forms a deep impurity level (350 to 700 meV), it is actually insulated. Shows physical behavior. This is thought to be because non-bonded hands are generated because O is eccentric at the N site. By substituting the adjacent position with a group III element, the eccentricity is eliminated, the impurity level becomes shallow, and the conductivity is estimated to be improved.
上述の同時ドーピングにおいて、ドープ元素濃度の比率は重要である。Ｏ／Ｍが０．０１以下の場合には、Ｍの単独置換サイト（電荷中立）が多数形成されて結晶構造が乱れる効果が大きく、ｎ型半導体としての機能が十分ではなくなる。一方、Ｏ／Ｍが１．５以上の場合には、Ｏの単独置換サイトが多く形成されて、深い不純物準位の影響が主体的となり、導電率が低下する。 In the above-described co-doping, the ratio of the doping element concentration is important. When O / M is 0.01 or less, many single substitution sites (charge neutrality) of M are formed and the crystal structure is disturbed, and the function as an n-type semiconductor is not sufficient. On the other hand, when O / M is 1.5 or more, a large number of single substitution sites for O are formed, the influence of deep impurity levels becomes dominant, and the conductivity decreases.
以上の様に、本発明によれば、低抵抗ｎ型ＡｌＮ半導体結晶を得ることができ、短波長発光素子やパワーデバイスを実現することができる。 As described above, according to the present invention, a low-resistance n-type AlN semiconductor crystal can be obtained, and a short wavelength light emitting element and a power device can be realized.
以下、実施例に基づいて本発明を具体的に説明する。 Hereinafter, the present invention will be specifically described based on examples.
ＡｌＮ単結晶板（１ｍｍ×５ｍｍ×１ｍｍ）に、III族元素及びＯの濃度が表１の濃度
になるよう、イオン注入法を用いてドープを行い、不活性雰囲気中１５００℃で１０分間熱処理して試料を作製し、１２０℃で導電率を測定した。結果を表１に併記した。
An AlN single crystal plate (1 mm × 5 mm × 1 mm) is doped using an ion implantation method so that the concentrations of Group III elements and O are the concentrations shown in Table 1, and heat-treated at 1500 ° C. for 10 minutes in an inert atmosphere. A sample was prepared, and the conductivity was measured at 120 ° C. The results are also shown in Table 1.
昇華法により、ＳｉＣ基板上に成長したＡｌＮ（０００１）を基板としてエピタキシャル成長をＭＯＣＶＤ法により行った。トリメチルアルミニウムとアンモニアからドーパントを含まないＡｌＮエピタキシャル層を約０．５μｍに成長させた後、装置内にトリメチルアルミニウム、アンモニアとは別系統で基板ホルダー直上に設置したノズルから、エチルアルコールとビスシクロペンタディエニルイットリウムを導入しながら０．２μｍのエピタキシャル層を成長させた。成長後、不活性ガス雰囲気下で１１５０℃にてアニール処理を行った。その結果、シート抵抗２ｋΩ、またホール測定によりｎ型の導電性を示すことが確認された。 Epitaxial growth was performed by MOCVD using AlN (0001) grown on a SiC substrate by a sublimation method. After growing an AlN epitaxial layer containing no dopant from trimethylaluminum and ammonia to about 0.5 μm, ethyl alcohol and biscyclopenta were introduced from a nozzle installed directly above the substrate holder in a separate system from trimethylaluminum and ammonia. An epitaxial layer of 0.2 μm was grown while introducing dienyl yttrium. After the growth, annealing was performed at 1150 ° C. in an inert gas atmosphere. As a result, it was confirmed that the sheet resistance was 2 kΩ and n-type conductivity was shown by hole measurement.
高さが２００ｍｍの炭素（グラファイト）製ヒータの内部に、ＣｅＯ2粉末（２wt％）
を混合したＡｌＮ粉末を入れたＢＮ製のルツボを設置し、ケースの上部にはＡｌＮの種結晶を固定して、１気圧の窒素雰囲気中、ルツボ下部の温度が２２００℃，上部が２１００℃となるよう２０時間加熱し、ＡｌＮ結晶を成長させた。得られた結晶の比抵抗を１５０℃で測定した結果、５Ω・cmであった。
Inside a carbon (graphite) heater with a height of 200 mm, CeO 2 powder (2 wt%)
A crucible made of BN containing AlN powder mixed with the above was installed, and the seed crystal of AlN was fixed to the upper part of the case, and the temperature at the bottom of the crucible was 2200 ° C. and the upper part was 2100 ° C. It was heated for 20 hours to grow an AlN crystal. As a result of measuring the specific resistance of the obtained crystal at 150 ° C., it was 5 Ω · cm.
サファイア（０００１）を基板として、ＡｌＮエピタキシャル成長をＨＶＰＥ法により行った。
石英管中にＡｌＣｌ3とＮＨ3を別系統で導入して基板上で反応させ、さらに別系統からＬａＣｌ3と酸素を導入した。圧力は常圧、温度は１０００℃とし、１０時間結晶成長さ
せた後、不活性ガス雰囲気下、１２００℃でアニール処理を行った。得られた試料の導電性を測定した結果、シート抵抗は１．５ｋΩであり、ホール測定によりｎ型の電気伝導を示すことが確認された。
AlN epitaxial growth was performed by HVPE using sapphire (0001) as a substrate.
Into the quartz tube, AlCl 3 and NH 3 were introduced in different systems and reacted on the substrate, and LaCl 3 and oxygen were introduced from another system. The pressure was normal pressure, the temperature was 1000 ° C., and the crystal was grown for 10 hours, and then annealed at 1200 ° C. in an inert gas atmosphere. As a result of measuring the conductivity of the obtained sample, the sheet resistance was 1.5 kΩ, and it was confirmed by hole measurement that n-type electric conduction was exhibited.
ＳｉＣを基板として、ＡｌＮエピタキシャル成長をＭＢＥ法により行った。
Ｇａ源として金属Ｇａ、Ｎ源として窒素分子（Ｎ2）を用い、Ｎ2をＲＦプラズマにより活性化した。
ＳｉＣ基板上に、低温ＡｌＮバッファ層を堆積させた後、Ｙ金属（４００ｐｐｍ）を含むＧａ源と共にＯ（Ｏ2，Ｈ2Ｏとして）を１００ｐｐｍ含むＮ源として用い、１０時間結晶成長させた後、窒素雰囲気下、１１００℃で１時間アニール処理を行った。得られた試料の導電性を１００℃で測定した結果、シート抵抗は５ｋΩであり、ホール測定によりｎ型の電気伝導を示すことが確認された。
AlN epitaxial growth was performed by the MBE method using SiC as a substrate.
Metal Ga was used as the Ga source, nitrogen molecules (N 2 ) were used as the N source, and N 2 was activated by RF plasma.
After depositing a low-temperature AlN buffer layer on a SiC substrate, using a Ga source containing Y metal (400 ppm) and an N source containing 100 ppm of O (as O 2 , H 2 O), after crystal growth for 10 hours Annealing treatment was performed at 1100 ° C. for 1 hour in a nitrogen atmosphere. As a result of measuring the conductivity of the obtained sample at 100 ° C., the sheet resistance was 5 kΩ, and it was confirmed by hole measurement to show n-type electrical conduction.
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