JP7032781B2 - ガリウムを含有する薄膜の原子層堆積方法 - Google Patents
ガリウムを含有する薄膜の原子層堆積方法 Download PDFInfo
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- 238000000231 atomic layer deposition Methods 0.000 title claims description 32
- 238000000034 method Methods 0.000 title claims description 30
- 229910052733 gallium Inorganic materials 0.000 title claims description 21
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims description 19
- 239000010409 thin film Substances 0.000 title claims description 14
- 239000002243 precursor Substances 0.000 claims description 16
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 239000000758 substrate Substances 0.000 description 16
- 239000010408 film Substances 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 6
- 239000003446 ligand Substances 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 125000000217 alkyl group Chemical group 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 description 4
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- XCZXGTMEAKBVPV-UHFFFAOYSA-N trimethylgallium Chemical compound C[Ga](C)C XCZXGTMEAKBVPV-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- -1 plasma and ozone Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WXAXJIIKFAZYSN-UHFFFAOYSA-N (1,2,3,4,5-pentamethylcyclopenta-2,4-dien-1-yl)methylbenzene Chemical compound CC1=C(C)C(C)=C(C)C1(C)CC1=CC=CC=C1 WXAXJIIKFAZYSN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 150000002259 gallium compounds Chemical class 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45553—Atomic layer deposition [ALD] characterized by the use of precursors specially adapted for ALD
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/18—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metallo-organic compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/542—Controlling the film thickness or evaporation rate
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Description
本発明は、低温でも蒸気圧が高く、熱安定性の高いガリウム含有前駆体を用いて、プラズマやオゾンなどのラジカル種を用いない原子層堆積(ALD)によって、ガリウムを含有する薄膜を堆積する方法を提供することを課題とする。
前記一般式(1)において、R1~R5のうち4つが水素原子である場合、残りの1つは炭素原子数1~4のアルキル基が好ましく、R1~R5のうち4つがメチル基である場合、残りの1つはメチル基、ノルマルプロピル基又はイソプロピル基が好ましい。
なお、Cp*Gaは、前記方法に限られることなく、種々の方法により合成することができる。
さらに、本発明の前駆体は、一価のガリウムとシクロペンタジエニル配位子との化合物であり、ガリウムは三価やゼロ価(金属)になりやすいので、熱分解温度よりも低い温度領域での反応性が高く、ALDに好適である。本発明の前駆体に対する反応性ガスは限定されないが、酸化膜を形成させたいときには水が好ましく使用できる。プラズマによって活性化した酸素や、オゾンを反応性ガスとして使用することもできるが、本発明の原料は反応性が高いので、低温においてもラジカル種を含まない反応性ガスでもALD成膜が可能である。
非特許文献3に記載の方法と同様の手順でGa(C5(CH3)5)を合成した。Ga(C5(CH3)5)は光と熱に極めて敏感と予想されたため、合成は不活性ガス中で行った。
1H-NMRスペクトル(400MHz(C6D6))において、Cp*のメチル基に相当する1.928ppm(s,15H,Cp* メチル)のピークが、非特許文献4に記載の値(1.92ppm(s,15H,Cp* メチル)500.1MHz(C6D6))とほぼ一致することで、目的としているGa(C5(CH3)5)が合成できたことを確認した。
このGa(C5(CH3)5)について、Arフロー中で熱重量測定を行ったところ、図1のようになり、約40℃から蒸発し始めて、約190℃までに、熱分解することなく、ほぼ100%蒸発した。
また、このGa(C5(CH3)5)を大気に曝すと、白煙をともない発熱した。また、NMR測定のため、NMR用の重ベンゼンに溶解させた際に、この溶媒中のわずかな水分とも激しく反応して白煙を発した。このように、Ga(C5(CH3)5)は、室温でも水と激しく反応することが確認された。前記したようにGa(C5(CH3)5)は、約190℃までは熱的に安定なので、約140℃程度以下の低い温度でも好適にALDに使用できることが確認された。
実施例1におけるGa(C5(CH3)5)の代わりに、非特許文献1に記載のGa(OiPr)3について、実施例1と同様に熱重量測定を行ったところ、図2のようになり、約250℃まで熱分解することなく、ほぼ100%蒸発したが、このGa(OiPr)3は常温で固体であり、融解した後に蒸発し始めるのは、約150℃と比較的高めの温度であった。非特許文献1に示されているようにALDに好適な温度領域は150~250℃であり、下限温度はGa(C5(CH3)5)よりも高い。
Claims (1)
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JP2017179819A JP7032781B2 (ja) | 2017-09-20 | 2017-09-20 | ガリウムを含有する薄膜の原子層堆積方法 |
US16/194,835 US10752992B2 (en) | 2017-09-20 | 2018-11-19 | Atomic layer deposition method of metal-containing thin film |
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JP2017179819A JP7032781B2 (ja) | 2017-09-20 | 2017-09-20 | ガリウムを含有する薄膜の原子層堆積方法 |
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JP2019056133A JP2019056133A (ja) | 2019-04-11 |
JP7032781B2 true JP7032781B2 (ja) | 2022-03-09 |
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US20230160051A1 (en) * | 2020-05-26 | 2023-05-25 | Kojundo Chemical Laboratory Co., Ltd. | Method for manufacturing crystalline gallium nitride thin film |
Citations (1)
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US20070148350A1 (en) | 2005-10-27 | 2007-06-28 | Antti Rahtu | Enhanced thin film deposition |
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US8795771B2 (en) * | 2006-10-27 | 2014-08-05 | Sean T. Barry | ALD of metal-containing films using cyclopentadienyl compounds |
US9217200B2 (en) * | 2007-12-21 | 2015-12-22 | Asm International N.V. | Modification of nanoimprint lithography templates by atomic layer deposition |
EP2492273A1 (en) | 2011-02-23 | 2012-08-29 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Deposition of gallium containing thin films using gallium alkylamide precursor |
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US20070148350A1 (en) | 2005-10-27 | 2007-06-28 | Antti Rahtu | Enhanced thin film deposition |
Non-Patent Citations (2)
Title |
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J. W. Elam, et al.,Chemical Materials,2006年01月07日,vol.18,p.3571-3578 |
Peter Jutzi et al.,Organometallics,1998年02月28日,vol.17,p.1305-1314 |
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US20190203357A1 (en) | 2019-07-04 |
US10752992B2 (en) | 2020-08-25 |
JP2019056133A (ja) | 2019-04-11 |
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