JPWO2012056928A1 - 光学素子の製造方法 - Google Patents
光学素子の製造方法 Download PDFInfo
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- JPWO2012056928A1 JPWO2012056928A1 JP2012540780A JP2012540780A JPWO2012056928A1 JP WO2012056928 A1 JPWO2012056928 A1 JP WO2012056928A1 JP 2012540780 A JP2012540780 A JP 2012540780A JP 2012540780 A JP2012540780 A JP 2012540780A JP WO2012056928 A1 JPWO2012056928 A1 JP WO2012056928A1
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- aluminum nitride
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- 230000003287 optical effect Effects 0.000 title claims abstract description 91
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 141
- 239000013078 crystal Substances 0.000 claims abstract description 120
- 239000000758 substrate Substances 0.000 claims abstract description 112
- 238000005229 chemical vapour deposition Methods 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 36
- 238000002834 transmittance Methods 0.000 abstract description 8
- 239000010410 layer Substances 0.000 description 143
- 150000004767 nitrides Chemical class 0.000 description 39
- 239000004065 semiconductor Substances 0.000 description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 239000007789 gas Substances 0.000 description 15
- 238000005498 polishing Methods 0.000 description 11
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 9
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000010409 thin film Substances 0.000 description 7
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 7
- 239000012535 impurity Substances 0.000 description 5
- QBJCZLXULXFYCK-UHFFFAOYSA-N magnesium;cyclopenta-1,3-diene Chemical compound [Mg+2].C1C=CC=[C-]1.C1C=CC=[C-]1 QBJCZLXULXFYCK-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 229910052594 sapphire Inorganic materials 0.000 description 3
- 239000010980 sapphire Substances 0.000 description 3
- 238000005092 sublimation method Methods 0.000 description 3
- VCZQFJFZMMALHB-UHFFFAOYSA-N tetraethylsilane Chemical compound CC[Si](CC)(CC)CC VCZQFJFZMMALHB-UHFFFAOYSA-N 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910021478 group 5 element Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- RGGPNXQUMRMPRA-UHFFFAOYSA-N triethylgallium Chemical compound CC[Ga](CC)CC RGGPNXQUMRMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000001039 wet etching Methods 0.000 description 1
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Abstract
Description
(1)最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板上に、化学気相成長法により窒化アルミニウム単結晶層を形成する第1の工程と、
前記窒化アルミニウム単結晶層上に、光学素子層を形成して光学素子用積層体を得る第2の工程と、
前記光学素子用積層体から前記窒化アルミニウム種基板を除去する第3の工程と
を含む光学素子の製造方法。
(2) 前記第1の工程における前記窒化アルミニウム単結晶層の厚みは50μm以上である(1)に記載の光学素子の製造方法。
(3) 前記第2の工程における前記光学素子層はLED素子層であることを特徴とする(1)または(2)に記載の光学素子の製造方法。
(4) 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板と、
前記窒化アルミニウム種基板上に形成された窒化アルミニウム単結晶層と、
前記窒化アルミニウム単結晶層上に形成された光学素子層と、を有する光学素子用積層体。
(5) 前記窒化アルミニウム単結晶層の波長240nmから300nmにおける吸収係数が30cm−1以下である(4)に記載の光学素子用積層体。
(6) 前記窒化アルミニウム単結晶層の転位密度が109cm−2以下である(4)または(5)に記載の光学素子用積層体。
本発明の第1の工程では、同種基板である窒化アルミニウム種基板11上に、化学気相成長法により窒化アルミニウム単結晶層12を形成して第1の積層体(自立基板)1を得る。
本発明の第2の工程では、第1の工程で得られた、第1の積層体(自立基板)1上に光学素子層20を形成して、第2の積層体、すなわち光学素子用積層体2を得る。
本発明の第3の工程では、第2の工程で得られた光学素子用積層体2から窒化アルミニウム種基板11を除去して、光学素子22を得る。
窒化アルミニウム種基板11は、WO2009/090821に記載の方法により作製した。この窒化アルミニウム種基板11は、窒化アルミニウム単結晶面11aを構成する窒化アルミニウム単結晶薄膜層の厚みが200nmであって、その下の窒化アルミニウム非単結晶層(窒化アルミニウム多結晶層)の厚みが300μmである積層体を用いた。また、この窒化アルミニウム種基板11は、8mm角のものを2枚準備した。
2枚の前記窒化アルミニウム種基板11を窒化アルミニウム単結晶面11aが最表面となるようにHVPE装置内のサセプター上に設置した後、水素を10slm、アンモニアを200sccmの流量で流しながら、該窒化アルミニウム種基板11を1450℃に加熱し、20分間保持することにより表面クリーニングを行った。次いで、500℃に加熱した金属アルミニウムと塩化水素ガスを反応させて得られる三塩化アルミニウムガス5sccm、アンモニアガス15sccm、キャリアガスとして窒素1500sccm、水素5000sccmを窒化アルミニウム種基板11上に供給し、窒化アルミニウム単結晶層12を150μm成長させた。
次いで、上記窒化アルミニウム単結晶層12の表面をCMP(Chemical Mechanical Polishing)研磨によって、RMS値が1nm以下になるまで研磨し、第1の積層体1(自立基板1)を得た。
次いで、第1の積層体1(自立基板1)の1枚を、研磨された窒化アルミニウム単結晶層12表面が最表面となるようにMOCVD装置内のサセプター上に設置した。その後、水素を13slmの流量で流しながら、該自立基板1を1250℃まで加熱し、10分間保持することで表面クリーニングを行った。
前記光学素子用積層体2の裏面の窒化アルミニウム非単結晶層(窒化アルミニウム多結晶層)を機械研磨により除去し、その後CMP研磨によってRMS値が5nm以下になるまで研磨して、光学素子22を作製した。なお、この光学素子22の厚みは、約100μmであった。この光学素子22を光学素子用積層体2と同様の方法で発光測定を行ったところ、発光波長265nmのシングルピーク発光であり、この光学素子22の発光ピーク強度は、光学素子用積層体2の強度よりも10倍以上であることが確認された。
1 第1の積層体(自立基板)
11 窒化アルミニウム種基板
11a 窒化アルミニウム単結晶面
12 窒化アルミニウム単結晶層
20 光学素子層
22 光学素子
Claims (6)
- 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板上に、化学気相成長法により窒化アルミニウム単結晶層を形成する第1の工程と、
前記窒化アルミニウム単結晶層上に、光学素子層を形成して光学素子用積層体を得る第2の工程と、
前記光学素子用積層体から前記窒化アルミニウム種基板を除去する第3の工程と
を含む光学素子の製造方法。 - 前記第1の工程における前記窒化アルミニウム単結晶層の厚みは50μm以上である請求項1に記載の光学素子の製造方法。
- 前記第2の工程における前記光学素子層はLED素子層であることを特徴とする請求項1または2に記載の光学素子の製造方法。
- 最表面が窒化アルミニウム単結晶面である窒化アルミニウム種基板と、
前記窒化アルミニウム種基板上に形成された窒化アルミニウム単結晶層と、
前記窒化アルミニウム単結晶層上に形成された光学素子層と、を有する光学素子用積層体。 - 前記窒化アルミニウム単結晶層の240nmから300nmにおける吸収係数が30cm−1以下である請求項4に記載の光学素子用積層体。
- 前記窒化アルミニウム単結晶層の転位密度が109cm−2未満である請求項4または5に記載の光学素子用積層体。
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DE112021004184T5 (de) | 2020-08-04 | 2023-05-17 | Tokuyama Corporation | Verfahren zum waschen von einem aluminiumnitrid-einkristall-substrat, verfahren zur herstellung von einem aluminiumnitrid-einkristall-schichtkörper, und verfahren zur herstellung von einem aluminiumnitrid-einkristall-substrat, und ein aluminiumnitrid-einkristall-substrat |
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