KR20190040480A - 주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착하는 방법 - Google Patents
주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착하는 방법 Download PDFInfo
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- KR20190040480A KR20190040480A KR1020180120767A KR20180120767A KR20190040480A KR 20190040480 A KR20190040480 A KR 20190040480A KR 1020180120767 A KR1020180120767 A KR 1020180120767A KR 20180120767 A KR20180120767 A KR 20180120767A KR 20190040480 A KR20190040480 A KR 20190040480A
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- tin
- metal
- deposition
- substrate
- atom
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 125
- 239000002184 metal Substances 0.000 title claims abstract description 125
- 238000000034 method Methods 0.000 title claims abstract description 98
- 239000000758 substrate Substances 0.000 title claims abstract description 87
- 238000000151 deposition Methods 0.000 title claims abstract description 78
- 230000008021 deposition Effects 0.000 title claims abstract description 56
- 239000000376 reactant Substances 0.000 claims abstract description 98
- 150000004770 chalcogenides Chemical class 0.000 claims abstract description 65
- 150000001787 chalcogens Chemical class 0.000 claims abstract description 58
- 229910052798 chalcogen Inorganic materials 0.000 claims abstract description 57
- 239000004065 semiconductor Substances 0.000 claims abstract description 13
- 239000012808 vapor phase Substances 0.000 claims abstract description 7
- 229910052718 tin Inorganic materials 0.000 claims description 73
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 54
- 125000004429 atom Chemical group 0.000 claims description 52
- 230000008569 process Effects 0.000 claims description 49
- ALRFTTOJSPMYSY-UHFFFAOYSA-N tin disulfide Chemical compound S=[Sn]=S ALRFTTOJSPMYSY-UHFFFAOYSA-N 0.000 claims description 41
- 239000007789 gas Substances 0.000 claims description 36
- 229910052760 oxygen Inorganic materials 0.000 claims description 30
- 239000001301 oxygen Substances 0.000 claims description 30
- 238000000231 atomic layer deposition Methods 0.000 claims description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 29
- 229910052799 carbon Inorganic materials 0.000 claims description 26
- 239000012071 phase Substances 0.000 claims description 26
- 239000000126 substance Substances 0.000 claims description 24
- 230000000737 periodic effect Effects 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000000137 annealing Methods 0.000 claims description 15
- 238000005229 chemical vapour deposition Methods 0.000 claims description 14
- 229910052732 germanium Inorganic materials 0.000 claims description 14
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 11
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 10
- 229910052711 selenium Inorganic materials 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 150000001721 carbon Chemical group 0.000 claims description 7
- 125000004122 cyclic group Chemical group 0.000 claims description 7
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 125000006527 (C1-C5) alkyl group Chemical group 0.000 claims description 5
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 5
- YJGJRYWNNHUESM-UHFFFAOYSA-J triacetyloxystannyl acetate Chemical compound [Sn+4].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O YJGJRYWNNHUESM-UHFFFAOYSA-J 0.000 claims description 5
- YMUZFVVKDBZHGP-UHFFFAOYSA-N dimethyl telluride Chemical compound C[Te]C YMUZFVVKDBZHGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002243 precursor Substances 0.000 description 126
- 239000010409 thin film Substances 0.000 description 53
- 239000010408 film Substances 0.000 description 42
- 239000000463 material Substances 0.000 description 39
- 239000003446 ligand Substances 0.000 description 25
- 238000010926 purge Methods 0.000 description 18
- 229910052739 hydrogen Inorganic materials 0.000 description 13
- 239000010410 layer Substances 0.000 description 13
- 150000002736 metal compounds Chemical class 0.000 description 13
- 239000002356 single layer Substances 0.000 description 13
- 238000005137 deposition process Methods 0.000 description 12
- 239000011669 selenium Substances 0.000 description 12
- 229930195733 hydrocarbon Natural products 0.000 description 10
- 150000002430 hydrocarbons Chemical class 0.000 description 10
- 150000003606 tin compounds Chemical class 0.000 description 10
- 239000004215 Carbon black (E152) Substances 0.000 description 9
- 238000001341 grazing-angle X-ray diffraction Methods 0.000 description 9
- 235000012431 wafers Nutrition 0.000 description 9
- 230000008901 benefit Effects 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 7
- 239000001257 hydrogen Substances 0.000 description 7
- 239000011261 inert gas Substances 0.000 description 7
- -1 transition metal chalcogenides Chemical class 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 125000000217 alkyl group Chemical group 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 229910052714 tellurium Inorganic materials 0.000 description 6
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 241000894007 species Species 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 125000005842 heteroatom Chemical group 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 238000001237 Raman spectrum Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 150000004820 halides Chemical group 0.000 description 3
- 238000000731 high angular annular dark-field scanning transmission electron microscopy Methods 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000579895 Chlorostilbon Species 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 125000005103 alkyl silyl group Chemical group 0.000 description 2
- 238000003877 atomic layer epitaxy Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000002178 crystalline material Substances 0.000 description 2
- 229910052876 emerald Inorganic materials 0.000 description 2
- 239000010976 emerald Substances 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- YIZVROFXIVWAAZ-UHFFFAOYSA-N germanium disulfide Chemical compound S=[Ge]=S YIZVROFXIVWAAZ-UHFFFAOYSA-N 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005019 vapor deposition process Methods 0.000 description 2
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- SDTMFDGELKWGFT-UHFFFAOYSA-N 2-methylpropan-2-olate Chemical compound CC(C)(C)[O-] SDTMFDGELKWGFT-UHFFFAOYSA-N 0.000 description 1
- OSXGKVOYAKRLCS-UHFFFAOYSA-N 2-methylpropan-2-olate;tin(4+) Chemical compound CC(C)(C)O[Sn](OC(C)(C)C)(OC(C)(C)C)OC(C)(C)C OSXGKVOYAKRLCS-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910005839 GeS 2 Inorganic materials 0.000 description 1
- 241000233805 Phoenix Species 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004871 chemical beam epitaxy Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000171 gas-source molecular beam epitaxy Methods 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000547 substituted alkyl group Chemical group 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 150000003573 thiols Chemical group 0.000 description 1
- TUTLDIXHQPSHHQ-UHFFFAOYSA-N tin(iv) sulfide Chemical compound [S-2].[S-2].[Sn+4] TUTLDIXHQPSHHQ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
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- 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
- C23C16/22—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 inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02568—Chalcogenide semiconducting materials not being oxides, e.g. ternary compounds
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- 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
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- 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
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- 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
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- 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
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- 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
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Abstract
주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착하는 방법이 개시된다. 방법은 기판을 적어도 하나의 금속 함유 기상 반응물과 접촉시키는 단계 및 기판을 적어도 하나의 칼코젠 함유 기상 반응물과 접촉시키는 단계를 포함할 수 있다. 본 개시의 방법에 의해 증착된 금속 칼코지나이드를 포함하는 반도체 소자 구조가 또한 제공된다.
Description
공동 연구 협약의 당사자
본원에 청구된 발명은 헬싱키 대학교와 ASM Microchemistry Oy 간의 공동 연구 협약에 의해, 또는 이를 대신하여, 그리고/또는 이와 관련하여 작성되었다. 상기 협약은 청구된 발명이 작성된 날짜 이전에 효력이 있었으며, 청구된 발명은 협약 범위 내에서 수행된 활동의 결과로서 작성되었다.
기술분야
본 개시는 일반적으로 주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착시키는 방법에 관한 것이며, 특히 이황화주석 또는 이황화 게르마늄의 주기적 증착에 관한 것이다. 또한 본 개시는 주기적 증착에 의해 형성된 금속 칼코지나이드를 포함하는 반도체 소자 구조에 관한 것이다.
2차원(2D) 재료에 대한 관심은 차세대 전자 소자의 성능 향상의 잠재력으로 인해 최근 몇 년 동안 극적으로 증가해 오고 있다. 예를 들어, 그래핀은 지금까지 가장 많이 연구된 2D 재료였고, 높은 이동도, 투과성, 기계적 강도 및 유연성을 나타낸다. 그러나 순수한 그래핀에서 밴드갭이 부족하면 트랜지스터와 같은 반도체 소자 구조에서 성능이 제한적이 되었다. 그래핀의 이러한 한계는 그래핀의 유사체인 2D 재료의 연구를 촉진해 오고 있다. 최근에, 전이금속 칼코지나이드, 특히 전이금속 디칼코지나이드가 그래핀의 대안으로서 상당한 연구 관심을 끌고 있다. 전이금속 디칼코지나이드는 MX2의 화학양론을 가질 수 있으며, 이는 칼코젠 원자의 두 층 사이에 샌드위치된 전이금속을 기술하며, 금속-칼코젠과 강한 면내(in-plane) 공유 결합 및 층간 약한 면외(out-of-plane) 반데르발스(Van der Walls) 결합을 갖는다.
그러나, 2D 재료를 생산하기 위한 확장 가능한 저온 방법은 거의 없다. 현재, 벌크 결정의 기계적 박리가 가장 일반적으로 사용되는 형성 방법이지만, 비록 이 방법이 우수한 품질의 결정을 생성하나, 이 방법은 연속막을 생산할 수 없으며, 매우 노동 집약적이어서 이러한 방법은 산업적 생산을 실행 가능하게 만들 수 없다. 화학 기상 증착(CVD)는 2D 재료를 증착하기 위해 사용되었지만, 현재 예를 들어, 이황화주석(SnS2)과 같은 금속 칼코지나이드용 CVD 공정은 600°C 이상의 온도에서 동작하고, 연속적이며 대면적 2D 재료를 제조할 수 없다. 따라서, 감소된 증착 온도 및 원자 수준의 막 두께 제어로 적절한 밴드 갭을 갖는 2D 재료를 생성할 수 있는 방법이 바람직하다.
본 발명의 내용은 선정된 개념을 단순화된 형태로 소개하기 위해 제공된다. 이들 개념은 하기의 본 발명의 예시적 구현예의 상세한 설명에 더 상세하게 기재되어 있다. 이러한 요약은 청구된 요지의 주된 특징 또는 필수적인 특징을 구분하려는 의도가 아니며 청구된 요지의 범주를 제한하기 위해 사용하려는 의도 또한 아니다.
일부 구현예에서, 주기적 증착에 의해 기판 상에 금속 칼코지나이드막을 증착하는 방법이 제공된다. 방법은 상기 기판을 화학 조성식 M-O-C(금속 원자는 하나의 산소(O) 원자에 결합되며, 상기 산소(O) 원자는 하나의 탄소(C) 원자에 결합됨)로 표시되는 부분 화학 구조를 포함하는 적어도 하나의 금속 함유 기상 반응물과 접촉시키는 단계; 및 상기 기판을 적어도 하나의 칼코젠 함유 기상 반응물과 접촉시키는 단계를 포함할 수 있다. 본 개시의 구현예는 본원에 기술된 방법에 의해 증착된 금속 칼코지나이드를 포함하는 반도체 소자 구조를 또한 제공한다.
본 발명 및 선행 기술에 대하여 달성되는 장점들을 요약하기 위한 목적으로, 본 발명의 특정 목적 및 장점들이 본원에 기술되었다. 물론, 모든 목적 및 장점들이 본 발명의 임의의 특별한 구현예에 따라 반드시 달성되는 것이 아니라는 것을 이해하여야 한다. 따라서, 예들 들어 당업자는, 본 발명이, 본원에 교시 또는 제안될 수 있는 다른 목적들 또는 장점들을 반드시 달성하지 않고서, 본원에 교시되거나 제시된 바와 같은 하나의 장점 또는 여러 장점들을 달성 또는 최적화 하는 방식으로 구현되거나 수행될 수 있다는 것을 인식할 것이다.
이들 구현예 모두 본원에 개시된 본 발명의 범주 내에 있도록 의도된다. 이들 및 다른 구현예들은 첨부된 도면들을 참조하는 특정 구현예들의 다음의 상세한 설명으로부터 당업자에게 쉽게 분명하게 될 것이고, 본 발명은 개시된 임의의 특정 구현예(들)에 한정되지 않는다.
본 명세서는 본 발명의 구현예로 간주되는 것을 특별히 지적하고 명백하게 주장하는 청구범위로 결론을 내지만, 본 개시의 구현예들의 장점들은 첨부한 도면들과 관련하여 읽을 때 본 개시의 구현예들의 특정 예의 설명으로부터 더욱 쉽게 확인될 수 있고, 도면들 중:
도 1은 본 개시의 구현예에 따른 예시적인 주기적 증착 방법을 도시하는 공정 흐름도이다.
도 2는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막에 대한 소각 x-선 회절(GIXRD) 데이터를 도시한다.
도 3은 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막에 대한 소각 x-선 회절(GIXRD) 데이터를 더 도시한다.
도 4는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 2D 재료를 포함하는 구조의 고각도 암시야 주사 투과 전자현미경(HAADF-STEM) 이미지이다.
도 5는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막으로부터 얻은 라만 스펙트럼을 도시한다.
도 6은 본 개시의 구현예에 따라 증착된 금속 칼코지나이드 박막을 포함하는 예시적인 반도체 소자 구조를 도시한다.
도 7은 본 개시의 구현예에 따라 금속 칼코지나이드 박막을 증착하기 위해 사용될 수 있는 예시적인 반응 시스템을 도시한다.
도 1은 본 개시의 구현예에 따른 예시적인 주기적 증착 방법을 도시하는 공정 흐름도이다.
도 2는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막에 대한 소각 x-선 회절(GIXRD) 데이터를 도시한다.
도 3은 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막에 대한 소각 x-선 회절(GIXRD) 데이터를 더 도시한다.
도 4는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 2D 재료를 포함하는 구조의 고각도 암시야 주사 투과 전자현미경(HAADF-STEM) 이미지이다.
도 5는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 박막으로부터 얻은 라만 스펙트럼을 도시한다.
도 6은 본 개시의 구현예에 따라 증착된 금속 칼코지나이드 박막을 포함하는 예시적인 반도체 소자 구조를 도시한다.
도 7은 본 개시의 구현예에 따라 금속 칼코지나이드 박막을 증착하기 위해 사용될 수 있는 예시적인 반응 시스템을 도시한다.
특정 구현예 및 실시예가 아래에 개시되었지만, 당업자는 본 발명이 구체적으로 개시된 구현예 및/또는 본 발명의 용도 및 이들의 명백한 변형 및 등가물 너머로 연장된다는 것을 이해할 것이다. 따라서, 개시된 발명의 범주는 후술되는 구체적인 개시된 구현예에 의해 제한되지 않도록 의도된다.
본원에 제시된 예시는 임의의 특정한 물질, 구조, 또는 소자의 실제 뷰를 의도하려 하는 것은 아니며, 단지 본 개시의 구현예를 설명하기 위해 사용되는 이상화된 표현이다.
본원에서 사용되는 바와 같이, 용어 "기판(substrate)"은, 사용될 수 있는, 또는 그 위에 소자, 회로, 또는 막이 형성될 수 있는, 임의의 하부 재료 또는 재료들을 지칭할 수 있다.
본원에서 사용되는 바와 같이, 용어 "주기적 증착(cyclic deposition)"은 반응 챔버 내로 전구체(반응물)를 순차적으로 도입시켜 기판 위에 막을 증착하는 것을 지칭할 수 있으며 원자층 증착 및 주기적 화학 기상 증착과 같은 증착 기술을 포함한다.
본원에서 사용되는 바와 같이, 용어 "원자층 증착"(ALD)은 증착 사이클, 바람직하게는, 복수의 연속 증착 사이클이 공정 챔버에서 수행되는 기상 증착 공정을 지칭할 수 있다. 일반적으로, 각각의 사이클 동안, 전구체는 증착 표면(예, 기판 표면, 또는 이전 ALD 주기로부터의 물질과 같은 이전에 증착된 하부 표면)에 화학 흡착되고, 추가적인 전구체와 쉽게 반응하지 않는(즉, 자기 제한적 반응) 단층 또는 서브 단층을 형성한다. 그 후 필요한 경우, 증착 표면 상에서 화학 흡착된 전구체를 원하는 재료로 전환시키는 용도로, 반응물(예, 다른 전구체 또는 반응 가스)이 후속해서 공정 챔버에 유입될 수 있다. 일반적으로, 이러한 반응물은 전구체와 더 반응할 수 있다. 각 사이클 동안 공정 챔버로부터 과잉의 전구체를 제거하고/하거나, 화학 흡착된 전구체의 변환 후 공정 챔버로부터 과잉의 반응물 및/또는 반응 부산물을 제거하기 위해 퍼징(purging) 단계들이 더 활용될 수도 있다. 추가로, 본원에서 사용된 용어 "원자층 증착(atomic layer deposition)"은 "화학적 기상 원자층 증착(chemical vapor atomic layer deposition)", "원자층 에피택시(atomic layer epitaxy)"(ALE), 분자 빔 에피택시(molecular beam epitaxy)(MBE), 가스 공급원 MBE, 또는 유기금속 MBE, 및 전구체 조성물(들), 반응 가스, 및 퍼지(예, 불활성 캐리어) 가스의 교번 펄스(alternating pulses)로 수행되는 경우의 화학적 빔 에피택시와 같은 관련 용어들에 의해 지정된 공정을 포함하는 것을 또한 의미한다.
본원에서 사용되는 바와 같이, 용어 "주기적 화학 기상 증착(cyclical chemical vapor deposition)"은 원하는 증착을 생성시키기 위해 기판 상에서 반응 및/또는 분해되는 둘 이상의 휘발성 전구체에 기판이 순차적으로 노출되는 임의의 공정을 지칭할 수 있다.
본원에서 사용된 바와 같이, 용어 "칼코젠 함유 기상 반응물(chalcogen containing vapor phase reactant)"은 칼코젠을 함유하는 반응물(전구체)을 지칭할 수 있으되, 칼코젠은 황, 셀레늄, 및 텔루륨을 포함하는 주기율표 VI족 원소이다.
본원에 사용된 바와 같이, 용어 "막(film)" 및 "박막(thin film)"은 본원에 개시된 방법에 의해 증착된 임의의 연속적인 또는 비연속적인 구조 및 재료를 지칭할 수 있다. 예컨대, "막" 및 "박막"은 2D 재료, 나노막대, 나노튜브 또는 나노입자 또는 심지어는 부분 또는 전체 분자층 또는 부분 또는 전체 원자층 또는 원자 및/또는 분자 클러스터를 포함할 수 있다. "막" 및 "박막"은 핀홀을 포함하는 재료 또는 층을 포함할 수 있지만 여전히 적어도 부분적으로 연속적일 수 있다.
본원에서 사용되는 바와 같이, 용어 "부분 화학 구조(partial chemical structure)"는 화학적 화합물의 일부의 화학 구조, 즉 전체 화학적 화합물보다 작은 화학 구조를 지칭할 수 있다.
본원에서 사용되는 바와 같이, 용어 "2D 재료(2D material)" 또는 2차원 재료(two-dimensional material)"은 나노미터 스케일의 결정질 재료, 하나 내지 세 개의 원자 두께를 지칭할 수 있다. 또한 "2D 재료" 또는 "2차원 재료"는 단일층당 약 세 개의 원자 두께를 갖는 결정질 재료의 다중 단층으로 구성된 나노미터 크기의 정렬된 결정 구조를 지칭할 수도 있다.
본 개시의 구현예는 주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착하는 방법, 특히 원자층 증착 공정에 의해 이황화주석(SnS2) 박막 또는 이황화게르마늄(GeS2) 박막을 증착하는 방법을 포함할 수 있다. 비제한적인 예로서, 이황화주석은 2D 결정 구조를 갖는 물질로 각광 받으며, 예를 들어 이황화몰리브덴(MoS2)과 같은 잘 알려진 전이금속 디칼코지나이드(TMDCs)와 유사하다. 가장 많이 연구된 2D 재료, 그래핀과 비교하여 이황화주석은 큰 밴드갭(벌크 ~1.8-2.2eV, 단층 2.8eV)을 가져서, 예를 들어 전계 효과 트랜지스터(FETs)와 같은 반도체 소자 구조에 많이 적합하게 만든다. FET 소자에서 채널 재료로서 이황화주석을 수반하는 초기 연구는 이황화몰리브덴과 비교할만한, 예를 들어 50-200cm2V-1s-1 및106 내지 108의 온/오프 비율뿐만 아니라, 100AW-1의 강한 광응답도와 같은 전기적 특성을 보여주고 있다. 이황화주석 박막에 대한 다른 가능한 응용 분야는 촉매 작용, 에너지 저장 및 광전지를 포함하나, 이에 제한되지 않는다.
이황화주석 박막을 형성하는 현재의 방법은 고품질의 등각성 저온박막을 형성하기에 적합하지 않다. 이황화주석 결정은 벌크 이황화주석 결정의 기계적 박리에 의해 형성될 수 있지만, 그러한 방법은 적합한 기판 상에 원자 수준의 두께 정확도로 이황화주석을 형성하기에 적합하지 않다. 또한, 이황화주석의 화학 기상 증착이 설명되었지만 그러한 공정은 높은 증착 온도(600°C 초과)에서 작동하고 나노 스케일의 등각성 박막을 생산하기에는 부적합하다.
주기적 화학 기상 증착 및 원자층 증착 기술과 같은 주기적 증착 방법은 본질적으로 확장 가능하며, 원주 수준에서 정확한 막 두께 제어를 제공하며, 이는 고품질의 2D 재료를 증착하는 데 결정적이다. 또한, 원자층 증착과 같은 주기적 증착 방법은 특징적으로 등각성(conformal)이고, 이로써 3차원 구조를 균일하게 코팅하는 능력을 제공한다. 이황화주석의 원자층 증착은 "Sn(NMe2)4 and H2S as the tin and chalcogenide precursors respectively", Ham et al., ACS Applied Material Interfaces, 5, (2013) 8880을 활용하여 설명되어 왔다. 그러나, 이황화주석을 형성하기 위한 그러한 종래 기술의 원자층 증착 공정은 문제가 될 수 있다. 예를 들어, 이황화주석은 좁은 온도 범위에 걸쳐 증착될 필요가 있을 수 있으며 이황화주석을 결정화하기 위해 증착후 어닐링 공정이 필요할 수 있다. 또한, Sn(NMe2)4 전구체는 다소 불안정할 수 있으며, 이는 예를 들어 200 mm 또는 300 mm 기판과 같은 대면적 기판 위에 열악한 품질의 막을 초래할 수 있다.
따라서, 원자 두께의 정확도를 갖고 저온에서 등각성으로 금속 디칼코지나이드막을 증착할 수 있는 방법이 바람직하다. 또한, 금속 디칼코지나이드막을 포함하는 반도체 소자 구조가 바람직하다.
주기적 증착 공정의 비제한적이고 예시적인 구현예는 ALD를 포함할 수 있으되, ALD는 일반적으로 자기 제한적 반응에 기반하고, 이에 의해 교대 순차적인 반응물 펄스가 증착 사이클당 약 하나의 원자(또는 분자) 단층을 증착하기 위해 사용된다. 증착 조건 및 전구체는 통상적으로 자기 포화 반응을 제공하도록 선택되어, 하나의 반응물의 흡착된 층이 동일한 반응물의 기상 반응물과 비반응성인 표면 종결부를 남긴다. 후속적으로 기판은 이전의 종결부와 반응하는 상이한 반응물과 접촉되어, 연속된 증착을 가능하게 한다. 따라서, 교번 펄스 반응물의 각각의 사이클은 통상적으로 원하는 재료를 약 단일층 이하로 남긴다. 그러나, 전술된 바와 같이, 당업자는 하나 이상의 ALD 사이클에서, 예를 들면 공정의 교번 특성에도 불구하고 일부 기상 반응이 발생하는 경우, 단일층보다 많은 재료가 증착될 수 있음을 인식할 것이다.
금속 칼코지나이드막의 증착을 위한 ALD형 공정에서, 하나의 증착 사이클은 기판을 제1 반응물에 노출시키고, 임의의 미반응된 제1 반응물 및 반응 부산물을 반응 공간으로부터 제거하고, 기판을 제2 반응물에 노출시키는 단계, 및 이어서 제2 제거 단계를 포함할 수 있다. 제1 반응물은 주석 또는 게르마늄 함유 전구체와 같은 금속 함유 전구체를 포함할 수 있고, 제2 반응물은 칼코젠 함유 전구체를 포함할 수 있다.
반응물 사이의 기상 반응을 방지하고 자기 포화 표면 반응을 가능하게 하도록, 전구체는 아르곤(Ar) 또는 질소(N2)와 같은 불활성 가스에 의해 분리될 수 있다. 그러나, 일부 구현예에서 기판은 제1 기상 반응물 및 제2 기상 반응물과 개별적으로 접촉되도록 이동될 수 있다. 반응은 자기 포화되기 때문에, 기판의 엄격한 온도 제어 및 전구체의 정확한 투여량 제어는 요구되지 않을 수 있다. 그러나, 기판 온도는 입사 가스종이 단층으로 응축되지 않거나 기판 표면 상에서 분해되지 않도록 하는 것이 바람직하다. 잉여 화학 물질 및 반응 부산물이 존재하는 경우, 기판이 다음 반응 화학 물질과 접촉하기 전에 이들은, 예를 들어 반응 공간을 퍼징하거나 기판을 이동함으로써 기판 표면으로부터 제거된다. 원하지 않는 가스 분자들은 불활성 퍼징 가스의 도움으로 반응 공간으로부터 효과적으로 방출될 수 있다. 진공 펌프는 퍼징 공정을 돕는 데 사용될 수 있다.
박막을 증착 또는 성장시키기 위해 사용될 수 있는 리액터들이 증착을 위해 사용될 수 있다. 이러한 리액터는 전구체를 제공하기 위한 적절한 장비 및 수단을 장착한 CVD 리액터뿐만 아니라 ALD 리액터를 포함한다. 일부 구현예에 따라, 샤워헤드 리액터가 사용될 수 있다.
사용될 수 있는 적합한 리액터의 예는 상업적으로 입수 가능한 단일 기판 (또는 단일 웨이퍼) 증착 설비, 예를 들면, 미국 애리조나주 피닉스 소재의 ASM America, Inc. 및 네덜란드 알메레 소재의 ASM Europe B.V로부터 입수 가능한 Pulsar® 리액터(예, Pulsar® 2000 및 Pulsar® 3000 및 Pulsar® XP ALD), 및 EmerALD® XP 및 EmerALD® 리액터를 포함한다. 다른 상업적으로 이용 가능한 리액터는 Eagle® XP 및 XP8의 상표명을 가진 ASM Japan K.K. (일본, 동경)사의 제품들을 포함한다. 일부 구현예에서 리액터는, 기판이 공정 동안 이동 또는 회전하는 공간 ALD 리액터이다.
일부 구현예에서, 배치식 리액터가 사용될 수 있다. 적합한 배치식 리액터는 A400 및 A412 PLUS라는 상표명으로 ASM Europe B.V(네덜란드, 알메르)사로부터 상업적으로 구매 가능한 Advance® 400 시리즈 리액터를 포함하나 이에 제한되지 않는다. 일부 구현예에서, 공정 처리 동안 보트가 회전하는 A412와 같은 수직형 배치식 리액터가 활용된다. 이처럼, 일부 구현예에서, 웨이퍼는 공정 처리 동안 회전한다. 다른 구현예에서, 배치식 리액터는 10개 이하의 웨이퍼, 8개 이하의 웨이퍼, 6개 이하의 웨이퍼, 4개 이하의 웨이퍼 또는 2개의 웨이퍼를 수용하도록 구성된 미니 배치식 리액터를 포함한다. 배치식 반응기가 사용되는 일부 구현예에서, 웨이퍼 대 웨이퍼의 불균일도는 3 %(1시그마) 미만, 2 % 미만, 1 % 미만, 또는 심지어 0.5 % 미만이다.
본원에서 설명되는 증착 공정은 클러스터 툴에 연결된 반응 챔버 또는 리액터에서 선택적으로 수행될 수 있다. 클러스터 툴에서, 각각의 반응 공간은 하나의 유형의 공정에 전용되기 때문에, 각 모듈 내의 반응 공간의 온도는 일정하게 유지될 수 있으며, 이는 각 공정 실행 전에 기판이 공정 온도로 가열되는 리액터에 비해 처리량을 향상시킨다. 추가적으로 클러스터 툴에서는, 기판들 사이의 원하는 공정 압력 레벨까지 반응 공간을 펌핑하는 시간이 줄어들 수 있다.
독립형 리액터는 로드-록(load-lock)이 장착될 수 있다. 이러한 경우, 각 공정 실행 사이에 반응 공간을 냉각할 필요가 없다. 일부 구현예에서, 금속 디칼코지나이드 박막을 포함하는 박막을 증착하기 위한 증착 공정은 복수의 증착 사이클, 예를 들면 ALD 사이클을 포함할 수 있다.
일부 구현예에서, 주기적 증착 공정은 금속막을 기판 상에 증착하는 데 사용되며, 주기적 증착 공정은 ALD 타입의 공정일 수 있다. 일부 구현예에서, 주기적 증착은 하이브리드 ALD/CVD 또는 주기적 CVD 공정일 수 있다. 예를 들어, 일부 구현예에서 ALD 공정의 증착 또는 성장 속도는 CVD 공정에 비해 낮을 수 있다. 성장 속도를 증가시키는 하나의 접근법은 ALD 공정에서 통상적으로 사용되는 것보다 높은 기판 온도에서 작동시켜, 화학 기상 증착 공정을 유발할 수 있으나, 전구체의 순차적 도입의 장점을 여전히 가지며, 이러한 공정을 주기적 CVD라고 지칭될 수 있다.
본 개시의 일부 구현예에 따라, ALD 공정은 집적 회로 피가공물과 같은 기판 상에 금속 칼코지나이드 박막을 형성하는 데 사용된다. 일부 구현예에서, 각각의 ALD 사이클은 두 개의 상이한 증착 스텝 또는 페이즈를 포함한다. 증착 사이클의 제1 페이즈("금속 페이즈")에서, 증착을 원하는 기판 표면은, 적어도 하나의 주석(Sn) 함유 기상 반응물 또는 적어도 하나의 게르마늄(Ge) 함유 기상 반응물을 포함하는 제1 기상 반응물과 접촉되어 기판 표면 상에 화학 흡착되어, 기판 표면 상에 반응물 종으로 이루어진 대략 하나의 단층만을 형성한다. 증착 사이클의 제2 페이즈("칼코젠 페이즈")에서, 증착을 원하는 기판 표면은 적어도 하나의 칼코젠 함유 기상 반응물 전구체를 포함하는 제2 기상 반응물과 접촉되어 이전의 화학 흡착 종과 반응하여 주석 디칼코지나이드 박막을 형성한다.
일부 구현예에서, 적어도 하나의 금속 함유 기상 반응물은 또한 "금속 화합물(metal compound)"로 여기에 지칭되며, 조성식으로 표시되는 부분 화학 구조를 포함할 수 있으되,
금속(M)은 하나의 산소(O) 원자에 결합되고, 상기 산소(O) 원자는 하나의 탄소(C) 원자와 결합된다. 일부 구현예에서, 원자 사이의 결합은 하나 이상의 단일 결합을 포함 할 수 있는 반면, 다른 구현예에서는 원자 사이의 결합은 하나 이상의 이중 결합을 포함할 수 있다. 본 개시의 일부 구현예에서, 금속 함유 기상 반응물은 주석(Sn) 함유 기상 반응물, 또는 게르마늄(Ge) 함유 기상 반응물 중 적어도 하나를 포함한다.
일부 구현예에서, 주석(Sn) 함유 기상 반응물 또는 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
주석(Sn) 원자는 하나의 산소(O) 원자에 결합되고, 상기 산소(O) 원자는 탄소(C) 원자에 결합되고, 개시된 원자들 사이의 결합은 단일 또는 이중 결합을 포함할 수 있다. 본 개시의 일부 구현예에서, 적어도 하나의 주석(Sn) 함유 기상 반응물은 화학 조성식 Sn(OR)x로 표시되며, R은 C1-C5 알킬기이거나 R은 OCCH3기이고 x는 2 내지 6의 정수값이다. 비제한적인 예로서, 일부 구현예에서 주석(Sn) 함유 기상 반응물은 주석(IV) 아세테이트(Sn(OAc)4)를 포함할 수 있다. 추가의 비제한적인 예로서, 일부 구현예에서 주석(Sn) 함유 기상 반응물은 주석(IV) tert-부톡사이드(Sn(OtBu)4)를 포함할 수 있다.
일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
주석(Sn) 원자는 두 개의 산소(O) 원자와 결합 또는 배위되고, 상기 산소(O) 원자는 하나의 단일 결합 및 하나의 이중 결합을 통해 하나의 탄소 원자(C)에 결합되고, R은 예를 들어 -CH3과 같은 C1-C3 알킬과 같은 치환 또는 미치환 탄화수소기일 수 있다.
일부 구현예에서, 주석(Sn) 전구체는 또한 여기서 "주석 화합물(tin compound)"로도 지칭되며 모노덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 또한 여기서 "주석 화합물(tin compound)"로도 지칭되며 바이덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 또한 여기서 "주석 화합물(tin compound)"로도 지칭되며 멀티덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 모노덴테이트 리간드를 포함할 수 없다. 일부 구현예에서, 주석(Sn) 전구체는 바이덴테이트 리간드로 이루어지지 않는다. 일부 구현예에서, 주석(Sn) 전구체는 아세틸아세토네이트(acac) 또는 2,2,6,6-테트라메틸-3,5-헵탄디오네이트(thd) 리간드와 같은 베타디케토네이트 리간드를 포함하지 않을 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 아세틸아세토네이트(acac) 또는 2,2,6,6-테트라메틸-3,5-헵탄디오네이트(thd) 리간드와 같은 베타디케토네이트 리간드를 두 개 이상 포함하지 않을 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 부가물 리간드를 포함하지 않을 수 있는 반면, 다른 구현예에서는 주석(Sn) 전구체는 하나 이상의 부가물 리간드를 포함할 수 있다. 일부 구현예에서, 주석(Sn) 전구체 내의 Sn은 산화수 +4를 가진다. 일부 구현예에서, 주석(Sn) 전구체 내의 Sn은 산화수 +2를 가진다. 일부 구현예에서, 주석(Sn) 전구체 내의 Sn은 산화수 +2를 갖지 않는다.
일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
주석(Sn) 원자는 두 개의 산소(O) 원자와 결합 또는 배위되고, 상기 산소(O) 원자는 하나의 단일 결합 및 하나의 이중 결합을 통해 하나의 탄소 원자(C)에 결합되고, R은 예를 들어 -CH3과 같은 C1-C3 알킬과 같은 치환 또는 미치환 탄화수소기일 수 있고, L은 알킬기와 같은 탄화수소기이며 상기 탄화수소는 이형원자(즉, C 또는 H와 다름)을 함유하거나 하지 않을 수 있다.
일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
주석(Sn) 원자는 하나의 산소(O) 원자에 결합 또는 배위되고, 상기 산소(O) 원자는 하나의 탄소 원자(C)에 결합되고, L은 알킬기와 같은 탄화수소기이며 상기 탄화수소는 이형원자(즉, C 또는 H와 다름)를 함유하거나 하지 않을 수 있다. 일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
X-Sn-L
X는 Cl과 같은 할라이드 또는 다른 탄화수소 함유 리간드이고, L은 알킬기와 같은 탄화수소기이며 상기 탄화수소는 이형원자(즉, C 또는 H와 다름)를 함유하거나 하지 않을 수 있다.
일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
Xy-Sn-Lw-y
X는 Cl과 같은 할라이드 또는 다른 탄화수소 함유 리간드이고, y는 0 내지 w 또는 1 내지 w-1이고, w는 2 내지 4이고, L은 알킬기와 같은 탄화수소기이며 상기 탄화수소는 이형원자(즉, C 또는 H와 다름)를 함유하거나 하지 않을 수 있다.
일부 구현예에서, 주석(Sn) 전구체는 또한 "주석 화합물(tin compound)"로도 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
Xy-Sn-L4-y
X는 Cl과 같은 할라이드 또는 다른 탄화수소 함유 리간드이고, y는 0 내지 4 또는 1 내지 3이고, L은 알킬기와 같은 탄화수소기이며 상기 탄화수소는 이형원자(즉, C 또는 H와 다름)를 함유하거나 하지 않을 수 있다.
일부 구현예에서, 금속 전구체는 또한 금속 화합물로 여기에 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 주석(Sn) 또는 게르마늄(Ge) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
-M-O-C-
금속 원자 M(Sn 또는 Ge)은 하나의 산소(O) 원자에 결합되고, 상기 산소(O) 원자는 하나의 탄소(C) 원자에 결합된다. 본원에서 간단히 하기 위해 Ge 전구체 또는 Ge는 "금속 화합물(metal compound)"또는 "금속(metal)"이라고도 부르나, 각각은 반금속 전구체 또는 반금속으로 간주될 수도 있다. 본 개시의 일부 구현예에서, 적어도 하나의 금속 함유 기상 반응물은 화학 조성식 M(OR)x로 표시되며, R은 C1-C5 알킬기이고 x는 2 내지 6의 정수값이고 M은 Ge 또는 Sn이다. 비제한적인 예로서, 일부 구현예에서 금속 함유 기상 반응물은 금속(IV) 아세테이트(M(OAc)4)를 포함할 수 있다. 추가의 비제한적인 예로서, 일부 구현예에서 금속 함유 기상 반응물은 금속(IV) tert-부톡사이드(M(OtBu)4)를 포함할 수 있다.
일부 구현예에서, 금속 전구체는 또한 금속 화합물로 여기에 지칭되며, 하기 조성식으로 표시되는 부분 화학 구조를 갖는 금속(Sn 또는 Ge) 함유 기상 반응물을 적어도 하나 포함할 수 있으되,
금속 원자 M(Sn, Ge)은 두 개의 산소(O) 원자와 결합 또는 배위되고, 상기 산소(O) 원자는 하나의 단일 결합 및 하나의 이중 결합을 통해 하나의 탄소 원자(C)에 결합되고, R은 예를 들어 -CH3과 같은 C1-C3 알킬과 같은 치환 또는 미치환 탄화수소기일 수 있다.
일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 모노덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 바이덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 멀티덴테이트 리간드를 포함할 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 모노덴테이트 리간드를 포함하지 않을 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 모노덴테이트 리간드로 이루어지지 않는다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 아세틸아세토네이트(acac) 또는 2,2,6,6-테트라메틸-3,5-헵탄디오네이트(thd) 리간드와 같은 베타디케토네이트 리간드를 포함하지 않을 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 아세틸아세토네이트(acac) 또는 2,2,6,6-테트라메틸-3,5-헵탄디오네이트(thd) 리간드와 같은 베타디케토네이트 리간드를 두 개 이상 포함하지 않을 수 있다. 일부 구현예에서, 금속 전구체는 또한 여기서 금속 화합물로도 지칭되며 부가물 리간드를 포함하지 않을 수 있는 반면, 다른 구현예에서 금속 화합물로도 지칭되는 금속 전구체는 하나 이상의 부가물 리간드를 포함할 수 있다. 일부 구현예에서, 금속 전구체 내의 Sn 또는 Ge는 산화수 +4를 가진다. 일부 구현예에서, 금속 전구체 내의 Sn 또는 Ge는 산화수 +2를 가진다. 일부 구현예에서, 금속 전구체 내의 Sn 또는 Ge는 산화수 +2를 갖지 않는다.
일부 구현예에서, 기판을 적어도 하나의 금속 함유 기상 반응물에 노출시키는 단계는 금속 전구체를 약 0.01 초 내지 약 60 초 사이, 약 0.05 초 내지 약 10 초 사이, 약 0.1 초 내지 약 5.0 초 사이의 시간 동안 기판 위로 펄싱하는 단계를 포함할 수 있다. 또한, 금속 전구체를 기판 상으로 펄싱하는 동안 금속 전구체의 유량은 2000 sccm 미만, 또는 500 sccm 미만, 또는 심지어 100 sccm 미만일 수 있다. 또한, 기판 위로 금속 전구체를 펄스화하는 동안, 금속 전구체의 유속은 약 1 내지 2000 sccm, 약 5 내지 1000 sccm, 또는 약 10 내지 약 500 sccm 범위일 수 있다.
예를 들어, 주석(Sn)과 같은 과잉의 금속 전구체 및 반응 부산물(있는 경우)은 예를 들어, 불활성 가스로 펌핑함으로써 기판 표면으로부터 제거될 수 있다. 예를 들어, 본 개시의 일부 구현예에서 방법은 기판 표면이 대략 2.0 초 미만의 시간 동안 퍼징되는 퍼지 사이클을 포함할 수 있다. 과잉의 금속 전구체 및 임의의 반응 부산물은 펌핑 시스템에 의해 생성된 진공의 도움으로 제거될 수 있다.
증착 사이클의 제2 페이즈("칼코젠 페이즈")에서, 기판은 적어도 하나의 칼코젠 함유 기상 반응물을 포함하는 제2 기상 반응물과 접촉된다. 본 개시의 일부 구현예에 있어서, 적어도 하나의 칼코젠 함유 기상 반응물은 황화수소(H2S), 셀렌화수소(H2Se), 디메틸 설파이드((CH3)2S), 또는 디메틸 텔루라이드((CH3)2Te)를 포함할 수 있다.
임의의 수의 칼코젠 전구체가 본원에 개시된 주기적 증착 공정에 사용될 수 있음이 당업자에 의해 이해될 것이다. 일부 구현예에서, 칼코젠 전구체는 다음의 리스트로부터 선택된다: H2S, H2Se, H2Te, (CH3)2S, (NH4)2S, 디메틸술폭시드((CH3)2SO), (CH3)2Se, (CH3)2Te, 원소 또는 원자 S, Se, Te, (H2S2, H2Se2, H2Te2와 같은) 기타 전구체 함유 칼코젠-수소 결합, 또는 조성식 R-Y-H를 갖는 칼코제놀(여기서 R은 치환 또는 비치환 탄화수소, 바람직하게는 C1-C8 알킬 또는 (알킬실릴기와 같은) 치환 알킬, 보다 바람직하게는 선형 또는 가지형 C1-C5 알킬기일 수 있고, Y는 S, Se, 또는 Te일 수 있음). 일부 구현예에서, 칼코젠 전구체는 조성식 R-S-H를 갖는 티올이며 R은 치환 또는 비치환 탄화수소, 바람직하게는 C1-C8 알킬기, 보다 바람직하게는 선형 또는 가지형 C1-C5 알킬기일 수 있다. 일부 구현예에서, 칼코젠 전구체는 조성식 (R3Si)2Y를 가지며 R3Si는 알킬실릴기이고 Y는 Se 또는 Te일 수 있다. 일부 구현예에서, 칼코젠 전구체는 S 또는 Se를 포함한다. 바람직한 구현예에서, 칼코겐 전구체는 S를 포함한다. 일부 구현예에서, 칼코젠 전구체는 원소 황과 같은 원소 칼코젠을 포함할 수 있다. 일부 구현예에서, 칼코젠 전구체는 Te를 포함하지 않는다. 일부 구현예에서, 칼코젠 전구체는 Se를 포함한다. 일부 구현예에서, 칼코젠 전구체는 S, Se, 또는 Te를 포함하는 전구체로부터 선택된다. 일부 구현예에서, 칼코젠 전구체는 H2Sn을 포함하며 n은 4 내지 10이다.
적절한 칼코젠 전구체는 이들이 적어도 하나의 칼코젠-산소 결합을 포함하는 한, 임의의 수의 칼코젠-함유 화합물을 포함할 수 있다. 일부 구현예에서, 칼코젠 전구체는 칼코젠 플라즈마, 칼코젠 원자 또는 칼코젠 라디칼을 포함할 수 있다. 일부 구현예에서, 에너지화된 칼코젠 전구체가 바람직하며, 플라즈마는 반응 챔버에서 또는 반응 챔버의 상단 유동부에서 생성될 수 있다. 일부 구현예에서, 칼코젠 전구체는 플라즈마, 원자, 또는 라디칼과 같이, 에너지화된 칼코젠 전구체를 포함하지 않는다. 일부 구현예에서, 칼코젠 전구체는 H2S와 같은 칼코젠-수소 결합을 포함하는 칼코젠 전구체로부터 형성된 칼코젠 플라즈마, 칼코젠 원자 또는 칼코젠 라디칼을 포함할 수 있다. 일부 구현예에서, 칼코젠 전구체는 황, 셀레늄 또는 텔루륨을 포함하는 플라즈마 바람직하게는 황을 포함하는 플라즈마와 같은 칼코젠 플라즈마, 칼코젠 원자 또는 칼코젠 라디칼을 포함할 수 있다. 일부 구현예에서, 플라즈마, 원자 또는 라디칼은 텔루륨을 포함한다. 일부 구현예에서, 플라즈마, 원자 또는 라디칼은 셀레늄을 포함한다. 일부 구현예에서, 칼코젠 전구체는 텔루륨 전구체를 포함하지 않는다.
일부 구현예에서, 기판을 칼코젠 함유 기상 반응물에 노출시키는 단계는 칼코젠 전구체(예, 수소 황화물)를 기판 위에 0.1 초 내지 2.0 초, 또는 약 0.01 초 내지 약 10 초, 또는 약 20 초 미만, 약 10 초 미만 또는 약 5 초 미만의 시간 동안 펄싱하는 단계를 포함할 수 있다. 칼코젠 전구체를 기판 위에 펄싱하는 동안, 치환 칼코젠 전구체의 유속은 50 sccm 미만, 또는 25 sccm 미만, 또는 15 sccm 미만, 또는 심지어 10 sccm 미만일 수 있다.
칼코젠 함유 전구체를 포함하는 제2 기상 반응물은 기판 상에 남아 있는 금속 함유 분자와 반응할 수 있다. 일부 구현예에서, 제2 상 칼코젠 전구체는 수소 황화물을 포함할 수 있고, 반응은 기판의 표면 상에 금속 디설파이드를 증착할 수 있다.
과잉의 제2 공급원 화학물질 및 반응 부산물이 존재하는 경우, 이들은 예를 들어 퍼징 가스 펄스 및/또는 진공(펌핑 시스템에 의해 발생됨)에 의해 기판 표면으로부터 제거될 수 있다. 퍼징 가스는 임의의 불활성 가스, 예를 들어 아르곤(Ar), 질소(N2) 또는 헬륨(He)인 것이 바람직하며 이들로 제한되지는 않는다. 퍼지(즉, 퍼징 가스 펄스) 또는 다른 반응물 제거 단계가 개재되는 경우, 하나의 페이즈는 일반적으로 다른 페이즈를 바로 따르는 것으로 간주된다.
기판이 제1 기상 반응물(즉, 금속 함유 전구체) 및 제2 기상 반응물(즉, 칼코젠 함유 전구체)과 교대로 접촉되는 증착 사이클은 원하는 두께의 선택적 금속막이 증착될 때까지 2회 이상 반복될 수 있다. 본 개시의 일부 구현예에서, 기판이 제1 기상 반응물 및 제2 기상 반응물과 접촉하는 순서는, 기판이 제2 기상 반응물과 먼저 접촉하고 이어서 제1 기상 반응물과 접촉하는 순서일 수 있는 것으로 이해되어야 한다. 추가적으로, 일부 구현예에서, 주기적 증착 공정은 기판이 제1 기상 반응물(즉, 금속 함유 전구체)과 1회 이상 접촉하고 이어서 기판이 제2 기상 반응물(즉, 칼코젠 함유 전구체)과 1회 이상 접촉하는 것을 포함할 수 있으며, 유사하게 대안적으로 기판이 제2 기상 반응물과 1회 이상 접촉하고 이어서 기판이 제1 기상 반응물과 1회 이상 접촉하는 것을 포함할 수 있다. 또한, 본 개시의 일부 구현예는 비-플라즈마 반응물을 포함할 수 있으며, 즉 제1 기상 반응물 및 제2 기상 반응물은 이온화된 반응성 종이 실질적으로 없다. 일부 구현예에서, 제1 기상 반응물 및 제2 기상 반응물은 이온화된 반응성 종, 여기된 종 또는 라디칼 종이 실질적으로 없다. 예를 들어, 제1 기상 반응물 및 제2 기상 반응물은 모두 비-플라즈마 반응물을 포함할 수 있어서 하부 기판의 이온화 손상 및 이로 인해 발생하는 관련 결함을 방지한다.
금속 함유 전구체 및 칼코젠 함유 전구체를 활용하여 금속 칼코지나이드 박막을 형성하는, 본원에 기술된 주기적 증착 공정은 가열된 기판을 갖는 ALD 또는 CVD 증착 시스템에서 수행될 수 있다. 예를 들어, 일부 구현예에서, 방법은 기판을 약 80℃ 내지 약 150℃ 사이의 온도로 가열하는 단계, 또는 심지어 기판을 대략 80℃ 내지 약 120℃ 사이의 온도로 가열하는 단계를 포함할 수 있다. 물론, 임의의 주어진 주기적 증착 공정의 적합한 온도 범위, 예를 들어 ALD 반응과 같은 적절한 온도 범위는 관련된 표면 종결부 및 반응물 종에 의존할 것이다. 본원에서, 온도는 사용되는 전구체에 따라 변하며, 일반적으로 약 700℃ 이하이다. 일부 구현예에서 증착 온도는 기상 증착 공정에서 일반적으로 약 100℃ 이상이고, 일부 구현예에서 증착 온도는 약 100℃ 내지 약 250℃ 사이이고, 일부 구현예에서 증착 온도는 약 120℃ 내지 약 200℃ 사이이다. 일부 구현예에서 증착 온도는 약 500℃ 미만, 약 400℃ 미만 또는 약 300℃ 미만이다. 일부 예에서 예를 들어 추가 반응물 또는 환원제가 공정에 사용되는 경우 증착 온도는 약 200℃ 미만, 약 150℃ 미만 또는 약 100℃ 미만일 수 있다. 일부 예에서, 증착 온도는 약 20℃ 이상, 약 50℃ 이상 및 약 75℃ 이상일 수 있다. 본 개시의 일부 구현예에서 증착 온도, 즉 증착하는 동안 기판의 온도는 약 150℃이다.
일부 구현예에서, 금속 칼코지나이드 박막의 성장 속도는 약 0.005 Å/사이클 내지 약 5 Å/사이클, 약 0.01 Å/사이클 내지 약 2.0 Å/사이클이다. 일부 구현예에서, 막의 성장 속도는 약 0.05 Å/사이클 초과, 약 0.1 Å/사이클 초과, 약 0.15 Å/사이클 초과, 약 0.20 Å/사이클 초과, 약 0.25 Å/사이클 초과, 약 0.3 Å/사이클 초과이다. 일부 구현예에서, 금속막의 성장 속도는 약 2.0 Å/사이클 미만, 약 1.0 Å/사이클 미만, 약 0.75 Å/사이클 미만, 약 0.5 Å/사이클 미만 또는 약 0.2 Å/사이클 미만이다. 본 개시의 일부 구현예에서 금속 칼코지나이드의 성장 속도는 대략 0.18 Å/사이클이다.
본 개시의 구현예는 도 1의 방법(100)에 의해 보다 상세하게 도시 될 수 있는 주기적 증착을 포함할 수 있다. 방법(100)은 기판을 반응 챔버 내에 제공하고 기판을 증착 온도로 가열하는 단계를 포함하는 공정 블록(110)으로 시작될 수 있으며, 예를 들어 기판은 벌크 실리콘 기판을 포함할 수 있고, 반응 챔버는 원자층 증착 반응 챔버를 포함할 수 있고 기판은 약 150 ℃의 증착 온도로 가열 될 수 있다. 방법(100)은 기판을 금속 함유 기상 반응물과 접촉시키는 단계를 포함하는 공정 블록(120)으로 계속될 수 있으며, 예를 들어 기판은 주석(IV) 아세테이트(Sn(OAc)4)와 약 1 초의 시간 동안 접촉될 수 있다. 기판을 금속 함유 전구체와 접촉시, 과잉의 금속 함유 전구체 및 임의의 부산물은 퍼지/펌프 공정에 의해 반응 챔버로부터 제거될 수 있다. 방법(100)은 기판을 칼코젠 함유 기상 반응물과 접촉시키는 단계를 포함하는 공정 블록(130)으로 계속될 수 있으며, 예를 들어 기판은 황화수소(H2S)와 약 4 초의 시간 동안 접촉될 수 있다. 기판을 칼코젠 함유 전구체와 접촉시, 과잉의 칼코젠 함유 전구체 및 임의의 부산물은 퍼지/펌프 공정에 의해 반응 챔버로부터 제거될 수 있다.
기판이 상기 적어도 금속 함유 기상 반응물 및 상기 적어도 하나의 칼코젠 함유 기상 반응물과 교대 순차적으로 접촉되는 방법이 하나의 증착 사이클을 구성한다. 본 개시의 일부 구현예에서, 금속 칼코지나이드(예, 금속 디칼코지나이드)를 증착하는 방법은 증착 사이클을 2회 이상 반복하는 단계를 포함할 수 있다. 예를 들어, 방법(100)은 결정 게이트(140)로 진행될 수 있는데, 여기서 결정 게이트는 방법(100)이 계속되거나 종료되는지를 판단한다. 블록 (140)의 결정 게이트는 증착된 금속 칼코지나이드막의 두께에 기반하여 결정되고, 예를 들어 금속 칼코지나이드막의 두께가 원하는 소자 구조에 대해 불충분한 경우, 그 다음에 방법(100)은 공정 블록(120)으로 다시 돌아갈 수 있고 기판을 금속 함유 기상 반응물과 접촉시키고 기판을 칼코젠 함유 기상 반응물과 접촉시키는 공정이 2회 이상 반복될 수 있다. 일단 금속 칼코지나이드막이 원하는 두께로 증착되면, 방법은 종료(150)될 수 있고, 금속 칼코지나이드막은 소자 구조를 형성하기 위한 부가적인 공정을 받을 수 있다.
본 개시의 일부 구현예에서, 증착시 금속 칼코지나이드 박막은 적어도 부분적으로 결정질일 수 있다. 예를 들어, 도 2는 주석 함유 전구체로서 주석(IV) 아세테이트(Sn(OAc)4)와 칼코젠 함유 전구체로서 황화수소(H2S)를 사용하고 약 150°C의 온도에서 본원내에 개시된 원자층 증착을 활용하여 증착된 이황화주석 세(3) 개의 비 제한적 예에 대한 소각 x-선 회절(GIXRD) 데이터를 도시한다. 도 2에 도시된 GIXRD 데이터는 다른 Sn(OAc)4 펄스 시간을 갖는 이황화주석 박막을 설명하는데, 예를 들어 202로 라벨링된 데이터는 0.2 초의 Sn(OAc)4 펄스 시간을 갖는 이황화주석 박막을 도시하고, 204로 라벨링된 데이터는 1 초의 Sn(OAc)4 펄스 시간을 갖는 이황화주석 박막을 도시하고, 206으로 라벨링된 데이터는 2 초의 Sn(OAc)4 펄스 시간을 갖는 이황화주석 박막을 도시한다. 세(3) 개의 이황화주석 박막에 대한 GIXRD 데이터의 피크는 (001) 결정학적 방향에 대응한다. 따라서, 본 개시의 일부 구현예에서, 이황화주석 박막을 증착하는 단계는 현저한 (001) 결정학적 방향을 갖는 이황화주석 박막을 증착하는 단계를 포함한다.
도 3은 주석 함유 전구체로서 주석(IV) 아세테이트(Sn(OAc)4)와 칼코젠 함유 전구체로서 황화수소(H2S)를 사용하고 약 150°C의 온도에서 본원 내에 개시된 원자층 증착을 활용하여 증착된 이황화주석 세(3) 개의 비 제한적 예에 대한 GIXRD 데이터를 도시한다. 도 3에 도시된 GIXRD 데이터는 다른 H2S 펄스 시간을 갖는 이황화주석 박막을 설명하는데, 예를 들어 302로 라벨링된 데이터는 8 초의 H2S 펄스 시간을 갖는 이황화주석 박막을 도시하고, 304로 라벨링된 데이터는 4 초의 H2S 펄스 시간을 갖는 이황화주석 박막을 도시하고, 306으로 라벨링된 데이터는 2 초의 H2S 펄스 시간을 갖는 이황화주석 박막을 도시한다. 이전에 설명한 바와 같이, 세(3) 개의 이황화주석 박막에 대한 GIXRD 데이터의 피크는 (001) 결정학적 방향에 대응한다. 또한, H2S 펄스 시간이 증가함에 따라 GIXRD에서의 피크 세기가 증가하는데, H2S 펄스 시간이 증가함에 따라 이황화주석 박막의 결정성이 증가함을 설명한다. 따라서, 본 개시의 일부 구현예에서 이황화주석 박막의 증착은 칼코젠 함유 전구체(예, H2S)를 약 2 초 초과, 또는 약 4 초 초과, 또는 심지어 약 8 초 초과하는 시간 동안 펄싱하는 단계를 포함한다.
비록 증착시 금속 칼코지나이드 박막은 적어도 부분적으로 결정질일 수 있으나, 금속 칼코지나이드 박막의 결정화가 증착 공정 동안 천천히 진행될 수 있어서 얇은 막은 두꺼운 막보다 덜 결정질이 된다. 이것은 금속 칼코지나이드 박막이 약 10 나노미터 미만의 두께를 갖는 2D 재료를 포함할 때 문제가 될 수 있다. 따라서, 본 개시의 일부 구현예에서 증착된 금속 칼코지나이드 박막은 금속 칼코지나이드 박막의 결정성을 개선하기 위한 증착후 어닐링 공정을 받을 수 있다. 예를 들어, 일부 구현예에서, 금속 칼코지나이드를 증착시키는 방법은 약 150℃ 내지 약 300℃ 사이의 온도에서 금속 칼코지나이드의 증착후 어닐링을 더 포함할 수 있다. 일부 구현예에서, 금속 칼코지나이드의 어닐링은 약 800℃ 미만, 또는 약 600℃ 미만, 또는 약 500℃ 미만, 또는 심지어 약 400℃ 미만의 온도로 금속 칼코지나이드를 가열하는 단계를 포함할 수 있다. 일부 구현예에서, 금속 칼코지나이드 박막의 증착후 어닐링은 칼코젠을 포함하는 분위기에서 수행될 수 있으며, 예를 들어 증착후 어닐링 공정은 칼코지나이드 화합물을 포함하는, 예를 들어 황화수소(H2S) 분위기와 같은 황 화합물 분위기에서 수행될 수 있다. 일부 구현예에서, 금속 칼코지나이드 박막의 증착후 어닐링은 1시간 미만, 또는 30분 미만, 또는 15분 미만, 또는 심지어 5분 미만의 시간 동안 수행될 수 있다. 일부 구현예에서, 이황화주석 박막과 같은 금속 칼코지나이드 박막의 증착후 어닐링은 S, Se, 또는 Te과 같은 칼코젠을 포함하지 않는 분위기에서 수행될 수 있으며, 예를 들어 N2와 같은 비활성 가스, 또는 (Ar 또는 He과 같은) 희귀 가스 분위기, 또는 (H2 또는 H2/N2 분위기와 같은) 수소 함유 분위기에서 수행된다.
예를 들어 본원에 기재된 구현예들 중 일부에 따라 증착된 이황화주석 박막과 같은 금속 칼코지나이드막을 포함하는 박막은 2D 재료를 포함하는 연속적인 박막일 수 있다. 일부 구현예에서, 본원에 기재된 구현예들 중 일부에 따라 증착된 금속 칼코지나이드막을 포함하는 박막은 약 100 nm 미만, 약 60 nm 미만, 약 50 nm 미만, 약 40 nm 미만, 약 30 nm 미만, 약 25 nm 미만, 또는 약 20 nm 미만 또는 약 15 nm 미만 또는 약 10 nm 미만 또는 약 5 nm 미만 또는 그 이하의 두께에서 연속성일 수 있다. 본원에서 지칭하는 연속성(continuity)은 물리적으로 연속성이거나 전기적으로 연속성일 수 있다. 일부 구현예에서, 막이 물리적으로 연속성일 수 있는 두께는 막이 전기적으로 연속성인 두께와 동일하지 않을 수 있으며, 막이 전기적으로 연속성일 수 있는 두께는 막이 물리적으로 연속성인 두께와 동일하지 않을 수 있다.
도 4는 본 개시의 구현예에 따라 증착된 주석 디칼코지나이드 2D 재료를 포함하는 구조의 단면적 고각도 암시야 주사 투과 전자현미경(HAADF-STEM) 이미지를 도시한다. HAADF-STEM 이미지는 실리콘 기판, 실리콘 기한 위에 배치된 이산화규소, 이산화규소(SiO2) 위에 배치된 이황화주석 2D 재료를 포함하는 구조를 도시한다. 구조는 이황화주석 위에 배치된 탄소(C)층을 더 포함하며 상기 탄소(C)층은 이미징 과정의 부분으로서 적용된다. 도 4는 2D 결정 구조 및 약 8 나노미터 미만의 두께를 갖는 결정질 이황화주석(SnS2) 2D 재료를 명확히 설명한다.
본 개시의 구현예에 의해 증착된 주석 디칼코지나이드 박막은 이황화주석을 포함할 수 있고 SnSx 형태를 취할 수 있으며 상기 x는 약 0.75 내지 약 2.8, 또는 상기 x는 약 0.8 내지 약 2.5, 또는 상기 x는 0.9 내지 약 2.3, 또는 대안적으로 상기 x는 약 0.95 내지 약 2.2 범위 일 수 있다. SnSx 에 대한 원소 조성 범위는, 약 30 원자% 내지 약 60 원자%, 또는 약 35 원자% 내지 약 55 원자%, 또는 심지어 약 40 원자% 내지 약 50 원자%의 Sn을 포함할 수 있다. 대안적으로, SnSx 에 대한 원소 조성 범위는 약 25 원자% 내지 약 75 원자%의 S, 약 30 원자% 내지 약 60 원자%의 S, 또는 심지어 약 35 원자% 내지 약 55 원자%의 S를 포함할 수 있다.
본 개시의 일부 구현예에서 금속 칼코지나이드, 예를 들어 이황화주석의 상은 라만 분광기를 활용하여 결정될 수 있다. 예를 들어, 도 5는 250℃의 온도에서 어닐링한 후, 7 나노미터 두께의 이황화주석 박막을 325 나노미터 레이저로 측정한 라만 스펙트럼을 도시한다. 도 5에서 도시된 라만 스펙트럼은 명확히 SnS2 피크에 해당하는 313cm-1에서 피크 세기를 보인다. 측정에서 SnS 또는 Sn2S3과 같이 다른 SnSx 상으로부터의 피크는 검출되지 않았다. 따라서, 본 개시의 일부 구현예에서, 주석 디칼코지나이드를 증착하는 단계는 SnS2로 주어지는 화학양론을 갖는 이황화주석 박막을 증착하는 단계를 포함한다.
추가적인 구현예에서, SnSx는 약 20 원자% 미만의 산소, 약 10 원자% 미만의 산소, 약 5 원자% 미만의 산소, 또는 심지어 약 2 원자% 미만의 산소를 포함할 수 있다. 다른 구현예에서, SnSx는 약 10 원자% 미만의 수소, 약 5 원자% 미만의 수소, 또는 약 2 원자% 미만의 수소, 또는 심지어 약 1 원자% 미만의 수소를 포함할 수 있다. 또 다른 구현예에서, SnSx는 약 10 원자% 미만의 탄소, 약 5 원자% 미만의 탄소, 또는 약 2 원자% 미만의 탄소, 또는 약 1 원자% 미만의 탄소, 또는 심지어 약 0.5 원자% 미만의 탄소를 포함할 수 있다. 본원에 개요된 구현예에서, 원소의 원자 농도는 러더퍼드 후방 산란(RBS)을 활용하여 결정될 수 있다.
본 개시의 구현예에 따라 금속 칼코지나이드 박막은 3차원 구조 상에 증착될 수 있다. 일부 구현예에서, 금속 칼코지나이드 박막의 스텝 커버리지는, 약 2 초과, 5 초과, 약 10 초과, 약 25 초과, 약 50 초과, 또는 심지어 약 100 초과의 종횡비(높이/폭)를 갖는 구조에서 약 50 % 이상, 약 80 % 이상, 약 90 % 이상, 약 95 % 이상, 약 98 % 이상 또는 약 99 % 이상일 수 있다.
일부 구현에서, 본원에 기술된 구현예 중 일부에 따라 증착된 주석 및 칼코젠을 포함하는 주석 디칼코지나이드 박막과 같은 금속 칼코지나이드 박막은 결정질 또는 다결정질일 수 있다. 일부 구현예에서, 본원에 기재된 구현예 중 일부에 따라 증착된 금속 칼코지나이드 박막은 약 20 nm 내지 약 100 nm의 두께를 가질 수 있다. 일부 구현예에서, 본원에 기재된 구현예 중 일부에 따라 증착된 금속 칼코지나이드 박막은 약 20 nm 내지 약 60 nm의 두께를 가질 수 있다. 일부 구현예에서, 본원에 기재된 구현예 중 일부에 따라 증착된 금속 칼코지나이드 박막은 약 20 초과, 약 30 nm 초과, 약 40 nm 초과, 약 50 nm 초과, 약 60 nm 초과, 약 100 nm 초과, 약 250 nm 초과, 약 500 nm 초과, 또는 그 이상의 두께를 가질 수 있다. 일부 구현예에서, 본원에 기재된 구현예 중 일부에 따라 증착된 금속 칼코지나이드 박막은 약 50 nm 미만, 약 30 nm 미만, 약 20 nm 미만, 약 15 nm 미만, 약 10 nm 미만, 약 5 nm 미만, 약 3 nm 미만, 약 2 nm 미만, 또는 심지어 약 1 nm 미만의 두께를 가질 수 있다.
일부 구현예에서, 본원에 기재된 구현예 중 일부에 따라 증착된 주석 또는 게르마늄 디칼코지나이드 박막과 같은 금속 칼코지나이드 박막은 금속 칼코지나이드 재료의 약 10개 이하의 단층 두께, 금속 칼코지나이드 재료의 약 7개 이하의 단층 두께, 금속 칼코지나이드 재료의 약 5개 이하의 단층 두께, 금속 칼코지나이드 재료의 약 4개 이하의 단층 두께, 금속 칼코지나이드 재료의 약 3개 이하의 단층 두께, 금속 칼코지나이드 재료의 약 2개 이하의 단층 두께 또는 심지어 금속 칼코지나이드 재료의 약 1개 이하의 단층 두께를 포함할 수 있다.
본원에 개시된 주기적 증착 공정에 의해 증착된 금속 칼코지나이드막은 반도체 소자 구조의 형성과 같은 다양한 상황에 활용될 수 있다. 당업자는 본원에 설명된 공정이 트랜지스터의 제조를 포함하며 많은 상황에 적용 가능하다는 것을 인식할 것이다.
비제한적 예로서 도 6을 참조로 반도체 소자 구조(600)는 실리콘 기판(602)와 상기 실리콘 기판(602) 위에 배치된 이산화규소(SiO2)층(604)을 포함할 수 있는 전계 효과 트랜지스터(FET)를 포함할 수 있다. 반도체 소자 구조(600)은 소스 영역(606)과 드레인 영역(608)을 더 포함할 수 있다. 소스 및 드레인 영역 사이에는 본 개시의 구현예에 따라 증착된 금속 칼코지나이드(610)의 박막이 배치된다. 금속 칼코지나이드 박막은 이황화주석의 얇은 층을 포함할 수 있고 FET 구조의 채널 영역으로 이루어질 수 있다. 본 개시의 일부 구현예에 따라, 이황화주석의 얇은 층은 10 nm 미만, 또는 5 nm 미만, 또는 1 nm 미만의 두께를 가질 수 있다. 반도체 소자 구조(600)는 이황화주석 박막 위에 배치된 게이트 유전체층(612)을 더 포함할 수 있으며 상기 게이트 유전체층(612)은 이산화하프늄(HfO2)을 포함할 수 있다. 반도체 소자 구조(600)는 이황화주석(610)의 얇은 층 위에 배치된 게이트 전극(614)을 더 포함할 수 있다.
본 개시의 구현예는 본 개시의 금속 칼코지나이드막을 형성하도록 구성된 반응 시스템을 또한 포함할 수 있다. 보다 상세하게, 도 7은 소정의 압력, 온도, 및 주변 조건 하에 기판(미도시)을 유지하고, 다양한 가스에 기판을 선택적으로 노출시키기 위한 메커니즘을 더 포함하는 반응 챔버(702)를 포함하는 반응 시스템(700)을 개략적으로 도시한다. 전구체 반응물 공급원(704)은 도관 또는 다른 적절한 수단(704A)에 의해 반응 챔버(702)에 결합될 수 있고, 매니폴드, 밸브 제어 시스템, 질량 유량 제어 시스템, 또는 전구체 반응물 공급원(704)으로부터 유래된 기상 전구체를 제어하기 위한 메커니즘에 추가로 결합될 수 있다. 전구체 반응물 공급원(704)에 의해 공급된 전구체(미도시)인 반응물(미도시)은 실온 및 표준 대기압 조건하에서 액체 또는 고체일 수 있다. 이러한 전구체는, 전구체 공급원 챔버 내에서의 기화 온도 또는 그 이상으로 유지될 수 있는 반응물 공급원 진공 용기 내에서 기화될 수 있다. 이러한 구현예에서, 기화된 전구체는 캐리어 가스(예컨대, 비활성 또는 불활성 가스)와 함께 운반된 다음 도관(704A)을 통해 반응 챔버(702) 내로 공급될 수 있다. 다른 구현예에서, 전구체는 표준 조건 하의 증기일 수 있다. 이러한 구현예에서, 전구체는 기화될 필요가 없으며, 캐리어 가스를 필요로 하지 않을 수 있다. 예를 들어, 일 구현예에서, 전구체는 가스 실린더 내에 저장될 수 있다. 반응 시스템(700)은 또한 추가적인 전구체 반응물 공급원을 또한 포함할 수 있는데, 이러한 전구체 반응물 공급원(706)은 또한 전술한 바와 같이 도관(706A)에 의해 반응 챔버에 결합될 수 있다.
퍼지 가스 공급원(708)은 도관(708A)을 통해 반응 챔버(702)에 결합될 수 있으며, 다양한 불활성 또는 비활성 가스를 반응 챔버(702)로 선택적으로 공급하여 반응 챔버로부터 전구체 가스 또는 폐가스의 제거를 돕는다. 공급될 수 있는 다양한 불활성 또는 비활성 가스는 고체, 액체 또는 저장된 기체 형태로부터 유래될 수 있다.
도 7의 반응 시스템(700)은 또한 선택적으로 어닐링 스테이션(712)을 포함할 수 있으며 금속 칼코지나이드는 성장후 어닐링 공정을 겪을 수 있다. 일부 구현예에서 성장후 어닐링 공정은 반응 챔버(702)에서 수행될 수 있는 반면에, 일부 구현예에서 금속 칼코지나이드 박막이 어닐링 스테이션(712)으로 이송될 수 있으며(예, 제어된 분위기 하에서) 상기 성장후 어닐링 공정은 원하는 가스 환경 하에서 수행될 수 있다.
도 7의 반응 시스템(700)은 반응 시스템(700)에 포함된 밸브, 매니폴드, 펌프 및 기타 설비를 선택적으로 작동시키기 위한 전자 회로 및 기계적 구성 요소를 제공하는 시스템 작동 및 제어 메커니즘(710)을 또한 포함할 수 있다. 이러한 회로 및 구성 요소는 전구체 공급원(704, 706) 및 퍼지 가스 공급원(708)으로부터 전구체, 퍼지 가스를 각각 도입하도록 작동한다. 시스템 작동 및 제어 메커니즘(710)은 가스 펄스 시퀀스의 시점, 기판과 반응 챔버의 온도, 반응 챔버의 압력, 및 반응 시스템(700)이 적절하게 작동하는데 필요한 다양한 기타 작동을 또한 제어한다. 작동 및 제어 메커니즘(710)은 반응 챔버(702) 내부 및 외부로의 전구체, 반응물 및 퍼지 가스의 유동을 제어하기 위한 제어 소프트웨어 및 전기적 또는 공기압 제어 밸브를 포함할 수 있다. 제어 시스템은 소프트웨어 또는 하드웨어 구성 요소, 예를 들어 특정 작업을 수행하는 FPGA 또는 ASIC과 같은 모듈을 포함할 수 있다. 유리하게는, 모듈은 제어 시스템의 어드레스 가능한 저장 매체에 탑재되어 하나 이상의 공정을 실행하도록 구성될 수 있다.
관련 기술분야의 당업자는, 상이한 수 및 종류의 전구체 반응물 공급원 및 퍼지 가스 공급원을 포함하여 본 반응 시스템의 다른 구성이 가능함을 이해한다. 또한, 당업자는 가스를 반응 챔버(702) 내로 선택적으로 공급하는 목적을 달성하는데 사용될 수 있는 밸브, 도관, 전구체 공급원, 퍼지 가스 공급원의 많은 배열이 존재함을 이해할 것이다. 또한, 반응 시스템을 개략적으로 표현하면서, 많은 구성 요소가 도면의 단순화를 위해 생략되었는데, 이러한 구성 요소는 예를 들면 다양한 밸브, 매니폴드, 정화기, 히터, 용기, 환기 장치, 및/또는 측관을 포함할 수 있다.
위에 설명된 본 개시의 예시적 구현예는 본 발명의 구현예의 예시일 뿐이기 때문에 이들 구현예는 첨부된 청구범위 및 그의 법적 등가물에 의해 정의되는 본 발명의 범주를 제한하지 않는다. 임의의 등가적인 구현예는 본 발명의 범주 내에 있도록 의도된다. 확실하게, 본원에 도시되고 기재된 것 외에도, 기재된 요소들의 선택적인 유용한 조합과 같은 본 발명의 다양한 변경은 설명으로부터 당업자에게 분명할 수 있다. 이러한 변경 및 구현예도 첨부된 청구범위의 범주 내에 있는 것으로 의도된다.
Claims (24)
- 주기적 증착에 의해 기판 상에 금속 칼코지나이드를 증착하는 방법으로서,
상기 기판을 조성식 M-O-C(금속(M) 원자는 하나의 산소(O) 원자에 결합되며, 상기 산소(O) 원자는 하나의 탄소(C) 원자에 결합됨)로 표시되는 부분 화학 구조를 포함하는 적어도 하나의 금속 함유 기상 반응물과 접촉시키는 단계; 및
상기 기판을 적어도 하나의 칼코젠 함유 기상 반응물과 접촉시키는 단계를 포함하는 방법. - 제1항에 있어서, 상기 금속 칼코지나이드는 금속 디칼코지나이드를 포함하는 방법.
- 제1항에 있어서, 상기 적어도 하나의 칼코젠 함유 기상 반응물은 S, Se, 또는 Te을 포함하는 방법.
- 제1항에 있어서, 상기 금속 칼코지나이드는 10 원자-% 미만의 산소(O) 함량을 포함하는 방법.
- 제1항에 있어서, 상기 주기적 증착은 원자층 증착을 포함하는 방법.
- 제1항에 있어서, 상기 주기적 증착은 주기적 화학 기상 증착을 포함하는 방법.
- 제1항에 있어서, 상기 금속 함유 기상 반응물은 주석(Sn) 함유 기상 반응물, 또는 게르마늄(Ge) 함유 기상 반응물 중 적어도 하나를 포함하는 방법.
- 제7항에 있어서, 상기 적어도 하나의 주석(Sn) 함유 기상 반응물은 화학 조성식 Sn(OR)x(R은 C1-C5 알킬기이고, x는 2 내지 6의 정수값임)로 표시되는 방법.
- 제7항에 있어서, 상기 적어도 하나의 주석(Sn) 함유 기상 반응물은 주석(IV) 아세테이트를 포함하는 방법.
- 제1항에 있어서, 상기 적어도 하나의 칼코젠 함유 기상 반응물은 황화수소(H2S), 셀렌화수소(H2Se), 디메틸 설파이드((CH3)2S), 또는 디메틸 텔루라이드((CH3)2Te)를 포함하는 방법.
- 제1항에 있어서, 상기 방법은 상기 기판이 상기 적어도 금속 함유 기상 반응물 및 상기 적어도 하나의 칼코젠 함유 기상 반응물과 교대 순차적으로 접촉되는 증착 사이클을 적어도 1회 포함하는 방법.
- 제14항에 있어서, 상기 증착 사이클은 2회 이상 반복되는 방법.
- 제1항에 있어서, 상기 기판을 약 150℃ 초과의 온도로 가열하는 단계를 더 포함하는 방법.
- 제16항에 있어서, 상기 기판을 약 500℃ 미만의 온도로 가열하는 단계를 더 포함하는 방법.
- 제1항에 있어서, 상기 금속 칼코지나이드는 이황화주석을 포함하는 방법.
- 제1항에 있어서, 상기 금속 칼코지나이드는 이황화게르마늄을 포함하는 방법.
- 제1항에 있어서, 약 150°C 내지 약 300°C의 온도에서 상기 금속 칼코지나이드의 증착후 어닐링을 더 포함하는 방법.
- 제20항에 있어서, 상기 금속 칼코지나이드의 상기 증착후 어닐링은 황화수소(H2S) 분위기에서 수행되는 방법.
- 제1항의 방법에 의해 증착된 금속 칼코지나이드를 포함하는 반도체 소자 구조.
- 제24항에 있어서, 상기 금속 칼코지나이드는 트랜지스터 구조 내 채널 영역의 적어도 일부를 포함하는 반도체 소자 구조.
- 제1항의 방법을 수행하도록 구성된 반응 시스템.
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US10734223B2 (en) | 2020-08-04 |
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