JP5665463B2 - Iii族窒化物半導体素子製造用基板およびiii族窒化物半導体自立基板またはiii族窒化物半導体素子の製造方法 - Google Patents
Iii族窒化物半導体素子製造用基板およびiii族窒化物半導体自立基板またはiii族窒化物半導体素子の製造方法 Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims description 218
- 239000004065 semiconductor Substances 0.000 title claims description 151
- 150000004767 nitrides Chemical class 0.000 title claims description 143
- 238000004519 manufacturing process Methods 0.000 title claims description 68
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 claims description 99
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 85
- 229910052804 chromium Inorganic materials 0.000 claims description 84
- 239000011651 chromium Substances 0.000 claims description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 71
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 70
- 238000005121 nitriding Methods 0.000 claims description 63
- 239000013081 microcrystal Substances 0.000 claims description 60
- 230000015572 biosynthetic process Effects 0.000 claims description 56
- 238000000034 method Methods 0.000 claims description 48
- 239000013078 crystal Substances 0.000 claims description 41
- 239000007789 gas Substances 0.000 claims description 36
- 238000004544 sputter deposition Methods 0.000 claims description 34
- 239000012159 carrier gas Substances 0.000 claims description 28
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 23
- 238000000151 deposition Methods 0.000 claims description 23
- 230000008021 deposition Effects 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 6
- 238000003486 chemical etching Methods 0.000 claims description 4
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 claims 2
- 239000010408 film Substances 0.000 description 87
- 238000005755 formation reaction Methods 0.000 description 53
- 229910052594 sapphire Inorganic materials 0.000 description 46
- 239000010980 sapphire Substances 0.000 description 46
- 229910052751 metal Inorganic materials 0.000 description 37
- 239000002184 metal Substances 0.000 description 37
- 229910052757 nitrogen Inorganic materials 0.000 description 21
- 238000002441 X-ray diffraction Methods 0.000 description 20
- 230000008569 process Effects 0.000 description 18
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 17
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 description 15
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 14
- 238000001816 cooling Methods 0.000 description 14
- 239000001257 hydrogen Substances 0.000 description 14
- 229910052739 hydrogen Inorganic materials 0.000 description 14
- 229910021529 ammonia Inorganic materials 0.000 description 10
- 238000012545 processing Methods 0.000 description 9
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 8
- 238000001552 radio frequency sputter deposition Methods 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000005530 etching Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910002704 AlGaN Inorganic materials 0.000 description 3
- XOYLJNJLGBYDTH-UHFFFAOYSA-M chlorogallium Chemical compound [Ga]Cl XOYLJNJLGBYDTH-UHFFFAOYSA-M 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- -1 chrome nitride Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical compound [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Description
(1)成長用下地基板上に、クロム層を形成する成膜工程と、該クロム層を、所定の条件で窒化することによりクロム窒化物層とする窒化工程と、該クロム窒化物層上に、少なくとも1層のIII族窒化物半導体層をエピタキシャル成長させる結晶層成長工程とを具えるIII族窒化物半導体素子製造用基板の製造方法であって、前記クロム層は、スパッタリング法により、スパッタリング粒子飛程領域における成膜速度が7〜65Å/秒の範囲で、厚さが50〜300Åの範囲となるよう成膜され、前記クロム窒化物層は、炉内圧力6.666kPa以上66.66kPa以下の、温度1000℃以上のMOCVD成長炉内において、アンモニアガスを含むガス雰囲気中で形成され、前記ガス雰囲気中のアンモニアガス以外のガス成分は、窒素ガスおよび水素ガスからなるキャリアガスとし、該キャリアガスに占める窒素ガスの含有比率は60〜100体積%の範囲であることを特徴とするIII族窒化物半導体素子製造用基板の製造方法。
2NH3 ⇔ N2 + 3H2 ・・・(式1)
の式で表記されるが、アンモニアが解離した際には、一旦原子状窒素と原子状水素が形成され、原子状窒素が金属クロム層の窒化に支配的な影響を与えるものと考えられる。
(0001)サファイア //(111)CrN //(0001)III族窒化物半導体層
ならびに、
〔1-100〕サファイア //〔10-1〕CrN //〔11-20〕III族窒化物半導体層
となる。
(0001)六方晶 //(111)CrN //(0001)III族窒化物半導体層
ならびに、
〔11-20〕六方晶 //〔10-1〕CrN //〔11-20〕III族窒化物半導体層
となる。
前記に記載した手順で、2インチ口径のサファイア(0001)基板上にRFスパッタリング法により平均成膜速度4.5Å/秒(スパッタリング粒子飛程領域における成膜速度は29.7Å/秒)で、120Å厚みの金属クロム層を成膜したのち、MOCVD炉内で基板温度1080℃、10分間の窒化処理を行った。その際の、アンモニアガスの含有比率は25体積%で流量は6SLM、アンモニアガス以外のキャリアガスとして水素は含有比率が20体積%ならびに窒素は含有比率が55体積%(キャリアガス中の窒素ガスの比率は73.3体積%)とし、全圧力は26.664kPaとした。その後基板温度を900℃まで降温し、GaNバッファ層を約2.5μm成長した後、1050℃まで昇温してGaN層を約3μm成長した。なお、成長中の炉内の全圧力は86.658kPa、V族(アンモニア中のN)とIII族(Ga)の原料ガス組成比(通称V/III比)は約1000とした。成長終了後室温近傍まで冷却し、GaNエピタキシャル層を有するIII族窒化物半導体基板を得た。GaN層の(0002)回折および(10-12)回折のX線ロッキングカーブ(XRD)の半値幅によって結晶性を評価した結果、各々290arcsec、330arcsecであり結晶性は良好であった。(図12(a)までの工程に相当)
2インチ口径のサファイア(0001)基板上にRFスパッタリング法により平均成膜速度4.5Å/秒で、120Å厚みの金属クロム層を成膜した。当該試料をMOCVD炉内で基板温度1080℃、10分間の窒化処理を行った。その後基板温度を900℃まで降温し、GaNバッファ層を約2.5μm成長した後、1050℃まで昇温してGaN層を約4μm成長した。GaNバッファ層上のGaN層にはSi(シリコン)をn型ドーパントして添加し、キャリア濃度を2×1018cm-3とした。
2インチ口径のサファイア(0001)基板上に直接AlNエピタキシャル層を形成した、AlN(0001)テンプレート基板を準備した。AlN層の厚みは約1μmで、XRDの半値幅は(0002)回折、(10-12)回折で各々85arcsec、1283arcsecであった。当該試料にRFスパッタリング法で平均成膜速度4.5Å/秒の条件で金属クロム層を90Å成膜した。
サファイア(0001)基板上に、RFスパッタリング法により平均成膜速度0.5Å/秒、スパッタリング粒子飛程領域における成膜速度3.3Å/秒の条件で金属クロム層を120Å成膜した。実施例1と同様、MOCVD炉内で基板温度1080℃、10分間の窒化処理を行った。その後基板温度を900℃まで降温し、GaNバッファ層を約2.5μm成長した後、1050℃まで昇温してGaN層を約3μm成長した。成長終了後室温近傍まで冷却し、GaNエピタキシャル層を有する半導体基板を得た。
サファイア(0001)基板上に、RFスパッタリング法により平均成膜速度4.5Å/秒、スパッタリング粒子飛程領域における成膜速度29.7Å/秒の条件で金属クロム層を25Åならびに500Åの厚みで成膜した。この際、基板トレーの回転数は30rpmとした。実施例1と同様、MOCVD炉内で基板温度1080℃、10分間の窒化処理を行った。その後基板温度を900℃まで降温し、GaNバッファ層を約2.5μm成長したのち、1050℃まで昇温してGaN層を約3μm成長した。成長終了後室温近傍まで冷却し、GaNエピタキシャル層を有する半導体基板を得た。
10a 下地基板の上面側の表面
20 金属クロム層
30 クロム窒化物層
40 III族窒化物半導体バッファ層
50 III族窒化物半導体層
60 III族窒化物半導体層
70 電極
80 電極
90 III族窒化物半導体素子製造用基板
90a III族窒化物半導体素子製造用基板
110 成長用下地基板
120 スパッタリングターゲット
130 基板ホルダーもしくは基板トレー
140 スパッタリング粒子飛程領域
150a III族窒化物半導体自立基板
150b III族窒化物半導体自立基板
160 III族窒化物半導体素子
Claims (10)
- 成長用下地基板上に、クロム層を形成する成膜工程と、
該クロム層を、所定の条件で窒化することによりクロム窒化物層とする窒化工程と、
該クロム窒化物層上に、少なくとも1層のIII族窒化物半導体層をエピタキシャル成長させる結晶層成長工程と
を具えるIII族窒化物半導体素子製造用基板の製造方法であって、
前記クロム層は、スパッタリング法により、スパッタリング粒子飛程領域における成膜速度が7〜65Å/秒の範囲で、厚さが50〜300Åの範囲となるよう成膜され、
前記クロム窒化物層は、炉内圧力6.666kPa以上66.66kPa以下の、温度1000℃以上のMOCVD成長炉内において、アンモニアガスを含むガス雰囲気中で形成され、前記ガス雰囲気中のアンモニアガス以外のガス成分は、窒素ガスおよび水素ガスからなるキャリアガスとし、該キャリアガスに占める窒素ガスの含有比率は60〜100体積%の範囲であることを特徴とするIII族窒化物半導体素子製造用基板の製造方法。 - 前記クロム窒化物層表面の窒化クロム微結晶のうち、略三角錐形状を有する窒化クロム微結晶の占める面積比率が、70%以上である請求項1に記載のIII族窒化物半導体素子製造用基板の製造方法。
- 前記クロム層は、複数の成長用下地基板上に、それぞれ平均成膜速度が1〜10Å/秒の範囲となるよう間欠的に成膜される請求項1または2に記載のIII族窒化物半導体素子製造用基板の製造方法。
- 前記略三角錐形状の窒化クロム微結晶の底辺の方位が、前記III族窒化物半導体層の<11-20>方向(a軸方向)群に平行である請求項2に記載のIII族窒化物半導体素子製造用基板の製造方法。
- 前記成長用下地基板は、六方晶系または擬似六方晶系の結晶構造を有し、表面が(0001)面である請求項1〜4のいずれか一項に記載のIII族窒化物半導体素子製造用基板の製造方法。
- 成長用下地基板上に、クロム層を形成する成膜工程と、
該クロム層を、所定の条件で窒化することによりクロム窒化物層とする窒化工程と、
該クロム窒化物層上に、少なくとも1層のIII族窒化物半導体層をエピタキシャル成長させる結晶層成長工程と、
前記クロム窒化物層をケミカルエッチングで除去することにより、前記成長用下地基板と前記III族窒化物半導体とを分離させる分離工程と
を具えるIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法であって、
前記クロム層は、スパッタリング法により、スパッタリング粒子飛程領域における成膜速度が7〜65Å/秒の範囲で、厚さが50〜300Åの範囲となるよう成膜され、
前記クロム窒化物層は、炉内圧力6.666kPa以上66.66kPa以下の、温度1000℃以上のMOCVD成長炉内において、アンモニアガスを含むガス雰囲気中で形成され、前記ガス雰囲気中のアンモニアガス以外のガス成分は、窒素ガスおよび水素ガスからなるキャリアガスとし、該キャリアガスに占める窒素ガスの含有比率は60〜100体積%の範囲であることを特徴とするIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法。 - 前記クロム窒化物層表面の窒化クロム微結晶のうち、略三角錐形状を有する窒化クロム微結晶の占める面積比率が、70%以上であることを特徴とする、請求項6に記載のIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法。
- 前記クロム層は、複数の成長用下地基板上に、それぞれ平均成膜速度が1〜10Å/秒の範囲となるよう間欠的に成膜される請求項6または7に記載のIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法。
- 前記略三角錐形状の窒化クロム微結晶の底辺の方位が、前記III族窒化物半導体層の<11-20>方向(a軸方向)群に平行である請求項7に記載のIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法。
- 前記成長用下地基板は、六方晶系または擬似六方晶系の結晶構造を有し、表面が(0001)面である請求項6〜9のいずれか一項に記載のIII族窒化物半導体自立基板またはIII族窒化物半導体素子の製造方法。
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