JP4860927B2 - エピタキシ用基板及びその製造方法 - Google Patents
エピタキシ用基板及びその製造方法 Download PDFInfo
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- JP4860927B2 JP4860927B2 JP2004558483A JP2004558483A JP4860927B2 JP 4860927 B2 JP4860927 B2 JP 4860927B2 JP 2004558483 A JP2004558483 A JP 2004558483A JP 2004558483 A JP2004558483 A JP 2004558483A JP 4860927 B2 JP4860927 B2 JP 4860927B2
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- nitride
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- gallium
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- 239000000758 substrate Substances 0.000 title claims abstract description 97
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 238000000407 epitaxy Methods 0.000 title abstract description 5
- 150000004767 nitrides Chemical class 0.000 claims abstract description 122
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims abstract description 25
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims abstract 3
- 229910052733 gallium Inorganic materials 0.000 claims description 118
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 108
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 91
- 238000000034 method Methods 0.000 claims description 87
- 229910052782 aluminium Inorganic materials 0.000 claims description 86
- 239000013078 crystal Substances 0.000 claims description 85
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- 239000002904 solvent Substances 0.000 claims description 33
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- 150000001340 alkali metals Chemical group 0.000 claims description 20
- 230000005693 optoelectronics Effects 0.000 claims description 12
- 239000012808 vapor phase Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 9
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
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- 150000003949 imides Chemical class 0.000 description 3
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- 229910052725 zinc Inorganic materials 0.000 description 3
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
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- 230000003287 optical effect Effects 0.000 description 2
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- ZFFBIQMNKOJDJE-UHFFFAOYSA-N 2-bromo-1,2-diphenylethanone Chemical compound C=1C=CC=CC=1C(Br)C(=O)C1=CC=CC=C1 ZFFBIQMNKOJDJE-UHFFFAOYSA-N 0.000 description 1
- 101150061900 Ambn gene Proteins 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001339 alkali metal compounds Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
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- 230000001010 compromised effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
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- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
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- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
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- C30B25/18—Epitaxial-layer growth characterised by the substrate
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30B29/403—AIII-nitrides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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Description
少なくとも1種のアルカリ金属を含有する超臨界アンモニア溶液中で窒化物の結晶化により形成した層A)の濃度よりも低い。アルカリ金属の濃度は、層B)またはC)及び層B1)及びB2)またはC1)及びC2)を形成する工程中に、層A)からの拡散を生じさせるからである。この場合、層B)、B1)、C)またはC1)はMOCVD法により形成でき、好ましくは厚さが0.1から3μmである。
(a)超臨界アンモニア含有溶液からシード上にガリウムまたはアルミニウム含有窒化物を結晶させて、アルカリ金属(I族元素、IUPAC 1989)の少なくとも1種を含有する窒化物バルク単結晶の層A)を基板のための膜厚をもたせて形成し、
(b)気相エピタキシャル成長法により、層A)のAlまたはGa極性面上に窒化物の層B)またはC)を形成し、
(c)基板A)から層B)またはC)を切り出し、100μm以上の膜厚をもたせ、主面が実質的にAlまたはGa極性面を有する基板を得る工程を備える。
a)化合物AmBn:AがH+および/または金属、好ましくはアルカリ、NH4+、Si、S、Pであり、Bがハロゲン、S、P、ならびにnとmが1以上の化学量論係数に相当する。
b)化学種のグループ:
−S4N4,S2N2,SN,S4N2,S11N2,P3N5、P4N6,PN
−PN2−,PN34−,PC47−,PN−,PN2−
−PNC12,P(NH)2NH2,P4S10,NP(SNH4)2,NPSNH4SH,NP(SH)2,PNS
ガリウム含有窒化物の結晶格子で形成される硫黄またはシリコン種をドナーとして機能させ;マグネシウム、亜鉛またはカドミウムをアクセプターとし;窒化ガリウム結晶格子において、マンガンまたはクロムといった添加物が磁性特性を付与し;蛍光体原子が窒素原子に対して等電子となり、エネルギーギャップは純粋なガリウム含有窒化物でのエネルギーギャップより狭くなる。これらの化学種は超臨界溶媒のアンモノ塩基性を損い、ガリウム含有窒化物の光学的、電気的、磁性的特性を変化させる。
アルミニウム含有フィードストックの溶解にも、類似の定義が適用される。
本発明の方法を行うにあたり、図3および図4に示す装置を用いるのが好ましい。詳細を以下に示す。
上記の方法および装置により、ガリウムまたはアルミニウム含有窒化物バルク単結晶を形成できる。バルク単結晶は低い欠陥密度を示す(バルクGaNの場合:104/cm2)バルク単結晶GaNは内径が1インチ以上、同時に、3mm以上(好ましくは5mm)の厚さを有することが重要である。単結晶をワイヤーソーでウエハに切断し、0.5mm厚のバルク単結晶基板を得る。バルク単結晶基板を後にシードとして用いることができる。n型導電性を改良するためには、気相成長中にSiをドープすることによりn型キャリア濃度を増加させるのが好ましい。ガリウムまたはアルミニウム含有窒化物を気相成長を用いて積層すれば、超臨界アンモニア中で形成するガリウムまたはアルミニウム含有窒化物がAlxGa1−xN(0≦x<1)を有するか、GaN上に積層したバルク単結晶AlxGa1−xN(0≦x<1)を用いるのが好ましい。ガリウムまたはアルミニウム含有窒化物の気相成長中にSiをドープすることにより、n型導電性を有するAlxGa1−x−yInyN、(0≦x≦1、0≦y<1、0≦x+y≦1)を形成でき、それを超臨界アンモニア中で、気相成長条件下でガリウムまたはアルミニウム含有窒化物上に結晶化させるので、高い結晶性及び105/cm2以下の欠陥密度を有するテンプレート型基板の形成に使用することができる。
本発明の方法においては、フィードストックの溶解工程と、超臨界溶液をより高温および/またはより低圧に輸送する工程とを分離でき、シードの表面にガリウムまたはアルミニウム含有窒化物の結晶化が生じる。さらに、該方法は、オートクレーブ中の異なる温度を有する少なくとも2つの領域を同時に形成する工程をそなえ、ガリウムまたはアルミニウム含有フィードストックをより低温の溶解領域に、シードをより高温の結晶化領域に配置する。溶解領域と結晶化領域間の温度差は1℃以上となるように制御し、超臨界溶液内での対流による化学輸送を確保する。超臨界アンモニア内で形成したガリウムまたはアルミニウム含有窒化物は、AlxGa1−xN、(0≦x<1)であり、ドナー型、アクセプター型、または磁気型の添加物を含有してもよく、一方、気相成長で形成したガリウムまたはアルミニウム含有窒化物は、AlxGa1−x−yInyN、(0≦x≦1、0≦y<1、0≦x+y≦1)である。
アルカリ金属イオンおよび/またはその誘導体を含んだアンモニアは超臨界溶媒として機能できる。フィードストックは主として、アジド類、イミド類、アミド−イミド類、アミド類、水素化物、金属間化合物およびガリウムまたはアルミニウム含有合金からなる群から選択されたガリウムまたはアルミニウム含有窒化物またはその前駆体と同様に、金属ガリウムからなる。シードは少なくともガリウムまたはアルミニウム含有窒化物または第XIII族(IUPAC, 1989)の他の元素の結晶層を備える。
半導体装置の適切な品質と寿命を確保できる。同時に、基板が導電性を有するので、n型パッド電極をその上に積層できる。
1)HVPE−GaNシード上に成長した5mmの単結晶の層を、加熱炉内に配置し、1〜5時間、600〜900℃、若干の酸素を含む窒素雰囲気で、アニール処理を行う。
2)次に、タカトリ(株)のワイヤーソーにサンプルを設置する。設置する際にはサンプルに結晶の主軸に適したオフ角を形成するため、1°以下傾けて設置する。その後ワイヤーソーを用いて5枚のウエハに切断し、0.05〜0.2度のオフ角のサンプルを得る。
3)次にサンプルを加熱炉内に設置し、1〜5時間、600〜900℃、若干の酸素を含む窒素雰囲気で、再度アニール処理を行う(以下、これをGaN基板と呼ぶ)。
4)次に、作業台上にGaN基板を載せ、ロジッテック社の研磨機にかけて、片面ずつ研磨する。研磨の行程においてはダイヤモンドツール及びシリカまたはアルミナスラリー溶液(pH3〜6またはpH9〜11)を用い、最終面10オングストローム以下の粗さに仕上げる。
5)その後、HVPE法またはMOCVD法にてGaN基板表面に(1〜数μm厚の)GaNまたはAlGaNの保護層を加え、テンプレート型基板を得る。
6)あるいは、上記保護層を備えるGaN基板上、または同保護層を備えないGaN基板上のいずれかに、3mm厚のGaN層を以下に示す一定条件の下でHVPE法により形成する。上記種々の方法を用いて切断、研磨した後、0.5mm厚のテンプレート型基板が形成され、オプトエレクトロニクス機器に使用される。HVPE条件は以下の通りである:反応温度:1050℃、反応圧力:気圧(0.1Mpa)、アンモニア分圧0.03Mpa、GaCl3分圧:100Pa、水素キャリアガス。
7)GaNまたはAlGaNにかわり、SiCまたはZnOからなる別の保護層をGaN基板上に形成でき、さらに3mm厚のGaN層をHVPE法を用いて形成できる。
Claims (14)
- オプトエレクトロニクスまたはエレクトロニクス機器のための基板の製造方法であって、
(a)超臨界アンモニア含有溶液からシード上にガリウムまたはアルミニウム含有窒化物を結晶させて、アルカリ金属(I族元素、IUPAC1989)の少なくとも1種を含有する窒化物バルク単結晶の層A)を、基板のための膜厚をもたせて形成する工程と、
(b)気相エピタキシャル成長法により、層A)のAlまたはGa極性面上に窒化物の層を100μm以上の厚さに形成する工程と、
(c)層A)から、工程(b)において形成した窒化物の層を100μm 以上の厚さに切り出し、主面が実質的にAl極性面またはGa極性面を有する基板を形成する工程と、を備えることを特徴とする製造方法。 - 前記工程(b)において、(b1)窒化物の第1層をMOCVD法またはMBE法により、層A)のAlまたはGa極性面上に形成し、(b2)窒化物の第2層をHVPE法により、100μm 以上の厚さに前記第1層上に形成することにより前記窒化物の層を形成し、
前記工程(c)において、 層A)から前記第2層を切り出すことを特徴とする請求項1記載の製造方法。 - 前記第1層がMOCVD法により形成され、膜厚が0.1から3μmであることを特徴とする請求項2記載の製造方法。
- 前記第2層の1つの表面を研磨し、気相エピタキシャル成長用の基板を得る工程をさらに備えることを特徴とする請求項3に記載の製造方法。
- 水素を含有しない空気中で、600℃ から1050℃ の温度で、工程(b)において形成した窒化物の層または第2層をアニーリング処理し、アニーリング処理前よりもより良好な結晶性を有する材料を製造する工程をさらに備えることを特徴とする請求項1から4のいずれかに記載の製造方法。
- 前記アニーリング処理を10から30Vol.%の酸素を添加した不活性ガスの空気中で行うことを特徴とする請求項5に記載の製造方法。
- 不純物(水素および/またはアンモニアまたは結晶および/またはアニーリング処理中に生じた不純物から形成されたイオン)が望ましいレベルに達するまで、アニーリング処理を単一工程または複数の工程で行うことを特徴とする請求項5に記載の製造方法。
- アンモニア含有溶媒、水または二酸化炭素の超臨界環境下に浸漬、またはガス状水素、窒素またはアンモニアの作用下に付し、窒化物バルク単結晶から不純物を除去する工程をさらに備えることを特徴とする請求項1から7のいずれかに記載の製造方法。
- 洗浄工程で超音波または電子ビーム照射を補助的に用いることを特徴とする請求項8に記載の製造方法。
- 前記(a)工程において、層A)はA軸成長されてC面からなる上面を有する請求項1から9のいずれかに記載の製造方法。
- 前記(c)工程で、切り出される基板の直径が1インチ以上である請求項1〜10のいずれかに記載の製造方法。
- 前記窒化物の層がAlxGa1−xN(0≦x≦1)で表わされる窒化物からなる請求項1から11のいずれかに記載の製造方法。
- 前記第2層がAlxGa1−xN(0≦x≦1)で表わされる窒化物からなる請求項1から12のいずれかに記載の製造方法。
- 前記(c)工程で、切り出される基板の厚さが150μm以上である請求項1から13いずれかに記載の製造方法。
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PL02357708A PL357708A1 (en) | 2002-12-11 | 2002-12-11 | Method of fabrication of epitaxial layer standardized substrate (template type substrates) from voluminal mono-crystalline aluminium nitride and nitride containing gallium for epitaxy of layers with high aluminium content as well as devices requiring efficient heat abstraction |
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PL357696A PL225423B1 (pl) | 2002-12-11 | 2002-12-11 | Sposób wytwarzania podłoża standaryzowanego warstwą epitaksjalną ( podłoża typu template), z objętościowego monokrystalicznego azotku zawierającego gal |
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PL357709A PL225425B1 (pl) | 2002-12-11 | 2002-12-11 | Sposób wytwarzania złożonego podłoża standaryzowanego warstwą epitaksjalną (podłoża typu template) z objętościowego monokrystalicznego azotku zawierającego gal |
PL357707A PL225424B1 (pl) | 2002-12-11 | 2002-12-11 | Sposób wytwarzania podłoża typu template z objętościowego monokrystalicznego azotku zawierającego gal |
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