JP2018168001A - Iii族窒化物半導体基板、及び、iii族窒化物半導体基板の製造方法 - Google Patents
Iii族窒化物半導体基板、及び、iii族窒化物半導体基板の製造方法 Download PDFInfo
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- JP2018168001A JP2018168001A JP2017064486A JP2017064486A JP2018168001A JP 2018168001 A JP2018168001 A JP 2018168001A JP 2017064486 A JP2017064486 A JP 2017064486A JP 2017064486 A JP2017064486 A JP 2017064486A JP 2018168001 A JP2018168001 A JP 2018168001A
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- Prior art keywords
- group iii
- nitride semiconductor
- iii nitride
- growth
- substrate
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- 239000000758 substrate Substances 0.000 title claims abstract description 171
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 155
- 239000004065 semiconductor Substances 0.000 title claims abstract description 155
- 238000000034 method Methods 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims description 26
- 239000013078 crystal Substances 0.000 claims abstract description 66
- 229910052594 sapphire Inorganic materials 0.000 claims description 57
- 239000010980 sapphire Substances 0.000 claims description 57
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000002248 hydride vapour-phase epitaxy Methods 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 239000012159 carrier gas Substances 0.000 description 24
- 238000005121 nitriding Methods 0.000 description 12
- 238000011156 evaluation Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 8
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 3
- CAVCGVPGBKGDTG-UHFFFAOYSA-N alumanylidynemethyl(alumanylidynemethylalumanylidenemethylidene)alumane Chemical compound [Al]#C[Al]=C=[Al]C#[Al] CAVCGVPGBKGDTG-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910026551 ZrC Inorganic materials 0.000 description 2
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- WHJFNYXPKGDKBB-UHFFFAOYSA-N hafnium;methane Chemical compound C.[Hf] WHJFNYXPKGDKBB-UHFFFAOYSA-N 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 2
- 125000002524 organometallic group Chemical group 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910003468 tantalcarbide Inorganic materials 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- RVOMEIZTHYMDKM-UHFFFAOYSA-N triethylalumane;trimethylalumane Chemical compound C[Al](C)C.CC[Al](CC)CC RVOMEIZTHYMDKM-UHFFFAOYSA-N 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
III族窒化物半導体結晶で構成され、厚さが300μm以上1000μm以下であり、表裏の関係にある露出した第1及び第2の主面はいずれも半極性面であり、前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のm軸に平行に入射し測定したXRC(X-ray Rocking Curve)の半値幅の差が、500arcsec以下であるIII族窒化物半導体基板が提供される。
サファイア基板を準備する基板準備工程と、
前記基板準備工程の後、前記サファイア基板に対して熱処理を行う熱処理工程と、
前記熱処理工程の後、前記サファイア基板上に金属含有ガスを供給する先流し工程と、
前記先流し工程の後、前記サファイア基板上に、成長温度:800℃以上950℃以下、圧力:30torr以上200torr以下の成長条件で、バッファ層を形成するバッファ層形成工程と、
前記バッファ層形成工程の後、前記バッファ層の上に、MOCVD法で、成長温度:800℃以上1025℃以下、圧力:30torr以上200torr以下、成長速度:10μm/h以上の成長条件で、III族窒化物半導体を成長させることで、第1の成長層を形成する第1の成長工程と、
前記第1の成長工程の後、前記第1の成長層の上に、HVPE法でIII族窒化物半導体を成長させることで、第2の成長層を形成する第2の成長工程と、
を有するIII族窒化物半導体基板の製造方法が提供される。
圧力:30torr以上760torr以下
熱処理時間:5分以上20分以下
キャリアガス:H2、又は、H2とN2(H2比率0〜100%)
キャリアガス供給量:3slm以上50slm以下(ただし、成長装置のサイズにより供給量は変動する為、これに限定されない。)
圧力:30torr以上200torr以下
トリメチルアルミニウム供給量、供給時間:20ccm以上500ccm以下、1秒以上60秒以下
キャリアガス:H2、又は、H2とN2(H2比率0〜100%)
キャリアガス供給量:3slm以上50slm以下(ただしガスの供給量は成長装置のサイズや構成により変動する為、これに限定されない。)
成長温度:800℃以上950℃以下
圧力:30torr以上200torr以下
トリメチルアルミニウム供給量:20ccm以上500ccm以下
NH3供給量:0.5slm以上10slm以下
キャリアガス:H2、又は、H2とN2(H2比率0〜100%)
キャリアガス供給量:3slm以上50slm以下(ただしガスの供給量は成長装置のサイズや構成により変動する為、これに限定されない。)
成長温度:800℃以上1025℃以下
圧力:30torr以上200torr以下
TMGa供給量:25sccm以上1000sccm以下
NH3供給量:1slm以上20slm以下
キャリアガス:H2、又は、H2とN2(H2比率0〜100%)
キャリアガス供給量:3slm以上50slm以下(ただしガスの供給量は成長装置のサイズや構成により変動する為、これに限定されない。)
成長速度:10μm/h以上
成長温度:900℃以上1100℃以下
成長時間:1時間以上
V/III比:1以上20以下
成長膜厚:1.0mm以上
第1のステップでIII族窒化物半導体層を形成後、一旦冷却すると、当該III族窒化物半導体層にクラックが発生する。これにより、内部応力が緩和される。その後、クラックを有するIII族窒化物半導体層の上にIII族窒化物半導体をエピタキシャル成長させると、クラックを挟んで分かれた結晶どうしは成長にしたがい互いに会合する。そして、上記冷却により内部応力が緩和されているため、厚膜化してもバルク結晶に割れが生じにくい。
<第1の評価>
第1の評価では、上述した「III族窒化物半導体層の成長面の面方位を、N極性側の面とするための複数の要素」のすべてを満たすことで、III族窒化物半導体層の成長面の面方位をN極性側の面にできることを確認する。また、上述した「III族窒化物半導体層の成長面の面方位を、N極性側の面とするための複数の要素」の中の少なくとも1つを満たさなかった場合、III族窒化物半導体層の成長面の面方位がGa極性側の面になることを確認する。
圧力:100torr
キャリアガス:H2、N2
熱処理時間:10分または15分
キャリアガス供給量:15slm
圧力:100torr
トリメチルアルミニウム供給量、供給時間:90sccm、10秒
キャリアガス:H2、N2
キャリアガス供給量:15slm
成長温度:800〜930℃
圧力:100torr
トリメチルアルミニウム供給量:90sccm
NH3供給量:5slm
キャリアガス:H2、N2
キャリアガス供給量:15slm
圧力:100torr
TMGa供給量:50〜500sccm(連続変化)
NH3供給量:5〜10slm(連続変化)
キャリアガス:H2、N2
キャリアガス供給量:15slm
成長速度:10μm/h以上
第2の評価では、上述した「III族窒化物半導体層の成長面の面方位を調整するための複数の要素」を調整することで、III族窒化物半導体層の成長面の面方位を調整できることを確認する。
圧力:200torr
熱処理時間:10分
キャリアガス:H2、N2
キャリアガス供給量:15slm
圧力:100torr
トリメチルアルミニウム供給量、供給時間:90sccm、10秒
キャリアガス:H2、N2
キャリアガス供給量:15slm
圧力:100torr
V/III比:5184
TMAl供給量:90ccm
NH3供給量:5slm
キャリアガス:H2、N2
キャリアガス供給量:15slm
成長温度:900〜1100℃
圧力:100torr
V/III比:321
TMGa供給量:50〜500ccm(ランプアップ)
NH3供給量:5〜10slm(ランプアップ)
キャリアガス:H2、N2
キャリアガス供給量:15slm
第3の評価では、XRCの半値幅で自立基板30の結晶性を評価する。
まず、MOCVD法で、a面方向に2°のオフ角を有するm面サファイア基板上に、バッファ層を介して、GaN層(第1の成長層23)を形成した。第1の成長層23の主面(露出面)は、N極性側の半極性面({−1−12−4}面(オフ角+α°))であった。また、第1の成長層23の厚さは約15μmであった。
MOCVD法で、just m面サファイア基板上に、バッファ層を介してGaN層を形成した。GaN層の主面(露出面)は、Ga極性側の半極性面((11−22)面)であった。また、GaN層の厚さは約1μmであった。
次に、本実施形態の製造方法により、半極性面を主面とし、最大径が50mm以上4インチ以下と大口径の自立基板30を得られることを確認する。
成長時間:15時間
V/III比:10
成長膜厚:4.4mm
成長時間:14時間
V/III比:10
成長膜厚:3.0mm(第2の成長層25ののべ膜厚は7.4mm)
1. III族窒化物半導体結晶で構成され、厚さが300μm以上1000μm以下であり、表裏の関係にある露出した第1及び第2の主面はいずれも半極性面であり、前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のm軸に平行に入射し測定したXRCの半値幅の差が、500arcsec以下であるIII族窒化物半導体基板。
2. 1に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のm軸に平行に入射し測定したXRCの半値幅の差が、300arcsec以下であるIII族窒化物半導体基板。
3. 1又は2に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面は、いずれも、X線をIII族窒化物半導体結晶のm軸に平行に入射し測定したXRCの半値幅が500arcsec以下であるIII族窒化物半導体基板。
4. 1から3のいずれかに記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅の差が、500arcsec以下であるIII族窒化物半導体基板。
5. 4に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅の差が、300arcsec以下であるIII族窒化物半導体基板。
6. 4又は5に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面は、いずれも、X線をIII族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅が500arcsec以下であるIII族窒化物半導体基板。
7. サファイア基板を準備する基板準備工程と、
前記基板準備工程の後、前記サファイア基板に対して熱処理を行う熱処理工程と、
前記熱処理工程の後、前記サファイア基板上に金属含有ガスを供給する先流し工程と、
前記先流し工程の後、前記サファイア基板上に、成長温度:800℃以上950℃以下、圧力:30torr以上200torr以下の成長条件で、バッファ層を形成するバッファ層形成工程と、
前記バッファ層形成工程の後、前記バッファ層の上に、MOCVD法で、成長温度:800℃以上1025℃以下、圧力:30torr以上200torr以下、成長速度:10μm/h以上の成長条件で、III族窒化物半導体を成長させることで、第1の成長層を形成する第1の成長工程と、
前記第1の成長工程の後、前記第1の成長層の上に、HVPE法でIII族窒化物半導体を成長させることで、第2の成長層を形成する第2の成長工程と、
を有するIII族窒化物半導体基板の製造方法。
8. 7に記載のIII族窒化物半導体基板の製造方法において、
前記第1の成長層及び前記第2の成長層を含むバルク結晶から、III族窒化物半導体基板を切り出す切出工程をさらに有するIII族窒化物半導体基板の製造方法。
9. 8に記載のIII族窒化物半導体基板の製造方法において、
前記切出工程では、前記バルク結晶の内の成長厚さ3mm以上の部分から、前記III族窒化物半導体基板を切り出すIII族窒化物半導体基板の製造方法。
20 テンプレート基板
21 サファイア基板
22 バッファ層
23 第1の成長層
24 成長面
25 第2の成長層
30 自立基板
Claims (9)
- III族窒化物半導体結晶で構成され、厚さが300μm以上1000μm以下であり、表裏の関係にある露出した第1及び第2の主面はいずれも半極性面であり、前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のm軸に平行に入射し測定したXRC(X-ray Rocking Curve)の半値幅の差が、500arcsec以下であるIII族窒化物半導体基板。
- 請求項1に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のm軸に平行に入射し測定したXRCの半値幅の差が、300arcsec以下であるIII族窒化物半導体基板。 - 請求項1又は2に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面は、いずれも、X線をIII族窒化物半導体結晶のm軸に平行に入射し測定したXRCの半値幅が500arcsec以下であるIII族窒化物半導体基板。 - 請求項1から3のいずれか1項に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅の差が、500arcsec以下であるIII族窒化物半導体基板。 - 請求項4に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面各々に対してX線を前記III族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅の差が、300arcsec以下であるIII族窒化物半導体基板。 - 請求項4又は5に記載のIII族窒化物半導体基板において、
前記第1及び第2の主面は、いずれも、X線をIII族窒化物半導体結晶のc軸の投影軸に平行に入射し測定したXRCの半値幅が500arcsec以下であるIII族窒化物半導体基板。 - サファイア基板を準備する基板準備工程と、
前記基板準備工程の後、前記サファイア基板に対して熱処理を行う熱処理工程と、
前記熱処理工程の後、前記サファイア基板上に金属含有ガスを供給する先流し工程と、
前記先流し工程の後、前記サファイア基板上に、成長温度:800℃以上950℃以下、圧力:30torr以上200torr以下の成長条件で、バッファ層を形成するバッファ層形成工程と、
前記バッファ層形成工程の後、前記バッファ層の上に、MOCVD(metal organic chemical vapor deposition)法で、成長温度:800℃以上1025℃以下、圧力:30torr以上200torr以下、成長速度:10μm/h以上の成長条件で、III族窒化物半導体を成長させることで、第1の成長層を形成する第1の成長工程と、
前記第1の成長工程の後、前記第1の成長層の上に、HVPE法でIII族窒化物半導体を成長させることで、第2の成長層を形成する第2の成長工程と、
を有するIII族窒化物半導体基板の製造方法。 - 請求項7に記載のIII族窒化物半導体基板の製造方法において、
前記第1の成長層及び前記第2の成長層を含むバルク結晶から、III族窒化物半導体基板を切り出す切出工程をさらに有するIII族窒化物半導体基板の製造方法。 - 請求項8に記載のIII族窒化物半導体基板の製造方法において、
前記切出工程では、前記バルク結晶の内の成長厚さ3mm以上の部分から、前記III族窒化物半導体基板を切り出すIII族窒化物半導体基板の製造方法。
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WO2015160903A1 (en) * | 2014-04-16 | 2015-10-22 | Yale University | Nitrogen-polar semipolar gan layers and devices on sapphire substrates |
JP2017030984A (ja) * | 2015-07-29 | 2017-02-09 | 国立大学法人山口大学 | 半導体基板の製造方法 |
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EP3604632A1 (en) | 2020-02-05 |
TW201903183A (zh) | 2019-01-16 |
KR102605845B1 (ko) | 2023-11-23 |
US20200032418A1 (en) | 2020-01-30 |
TWI755508B (zh) | 2022-02-21 |
JP7055595B2 (ja) | 2022-04-18 |
CN110462113A (zh) | 2019-11-15 |
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