CN103012457A - 卤代有机氨基硅烷前体及包含该前体的薄膜沉积方法 - Google Patents
卤代有机氨基硅烷前体及包含该前体的薄膜沉积方法 Download PDFInfo
- Publication number
- CN103012457A CN103012457A CN2012103922079A CN201210392207A CN103012457A CN 103012457 A CN103012457 A CN 103012457A CN 2012103922079 A CN2012103922079 A CN 2012103922079A CN 201210392207 A CN201210392207 A CN 201210392207A CN 103012457 A CN103012457 A CN 103012457A
- Authority
- CN
- China
- Prior art keywords
- alkyl
- chlorosilane
- aryl
- alkynyl
- thiazolinyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002243 precursor Substances 0.000 title claims abstract description 196
- 238000000034 method Methods 0.000 title claims abstract description 123
- 238000000151 deposition Methods 0.000 title claims description 51
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 27
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 27
- 125000006711 (C2-C12) alkynyl group Chemical group 0.000 claims abstract description 25
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 25
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 108
- 229910000077 silane Inorganic materials 0.000 claims description 108
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 105
- 125000005843 halogen group Chemical group 0.000 claims description 86
- 239000000758 substrate Substances 0.000 claims description 75
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 65
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 53
- 239000000203 mixture Substances 0.000 claims description 52
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 49
- 238000006243 chemical reaction Methods 0.000 claims description 45
- SDGKUVSVPIIUCF-UHFFFAOYSA-N 2,6-dimethylpiperidine Chemical group CC1CCCC(C)N1 SDGKUVSVPIIUCF-UHFFFAOYSA-N 0.000 claims description 43
- 238000010926 purge Methods 0.000 claims description 41
- 229910052710 silicon Inorganic materials 0.000 claims description 40
- 239000010703 silicon Substances 0.000 claims description 40
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 38
- 239000001301 oxygen Substances 0.000 claims description 38
- 229910052760 oxygen Inorganic materials 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 35
- 238000005229 chemical vapour deposition Methods 0.000 claims description 32
- -1 cyclohexyl ethylamino chlorosilane Chemical compound 0.000 claims description 31
- 239000005046 Chlorosilane Substances 0.000 claims description 30
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 30
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 28
- 230000008021 deposition Effects 0.000 claims description 25
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims description 25
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 25
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 24
- 229910052736 halogen Inorganic materials 0.000 claims description 23
- 150000002367 halogens Chemical class 0.000 claims description 23
- 239000001257 hydrogen Substances 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 20
- 125000004122 cyclic group Chemical group 0.000 claims description 20
- 125000000217 alkyl group Chemical group 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 16
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical group N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 15
- 229910021529 ammonia Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000010408 sweeping Methods 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- VPZDAHBNTYZYHC-UHFFFAOYSA-N chlorosilylamine Chemical compound N[SiH2]Cl VPZDAHBNTYZYHC-UHFFFAOYSA-N 0.000 claims description 10
- 125000004429 atom Chemical group 0.000 claims description 7
- 238000005137 deposition process Methods 0.000 claims description 7
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 7
- 150000003512 tertiary amines Chemical class 0.000 claims description 7
- 238000009832 plasma treatment Methods 0.000 claims description 6
- 239000013049 sediment Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- UJOBWOGCFQCDNV-UHFFFAOYSA-N 9H-carbazole Chemical compound C1=CC=C2C3=CC=CC=C3NC2=C1 UJOBWOGCFQCDNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 3
- 150000002825 nitriles Chemical class 0.000 claims description 3
- SBOJXQVPLKSXOG-UHFFFAOYSA-N o-amino-hydroxylamine Chemical class NON SBOJXQVPLKSXOG-UHFFFAOYSA-N 0.000 claims description 3
- POTIYWUALSJREP-UHFFFAOYSA-N 1,2,3,4,4a,5,6,7,8,8a-decahydroquinoline Chemical compound N1CCCC2CCCCC21 POTIYWUALSJREP-UHFFFAOYSA-N 0.000 claims description 2
- 150000002475 indoles Chemical class 0.000 claims description 2
- 229940074386 skatole Drugs 0.000 claims description 2
- RVUTUEKLTCAHQU-UHFFFAOYSA-N N-[chloro(cyclohexyl)silyl]propan-2-amine Chemical compound CC(C)N[SiH](Cl)C1CCCCC1 RVUTUEKLTCAHQU-UHFFFAOYSA-N 0.000 claims 7
- NEHMKBQYUWJMIP-UHFFFAOYSA-N anhydrous methyl chloride Natural products ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims 7
- 125000004210 cyclohexylmethyl group Chemical group [H]C([H])(*)C1([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C1([H])[H] 0.000 claims 7
- 238000006884 silylation reaction Methods 0.000 claims 7
- 238000000231 atomic layer deposition Methods 0.000 claims 4
- 239000011261 inert gas Substances 0.000 claims 4
- 125000000041 C6-C10 aryl group Chemical group 0.000 abstract 3
- 125000000008 (C1-C10) alkyl group Chemical group 0.000 abstract 2
- 125000006165 cyclic alkyl group Chemical group 0.000 abstract 2
- 125000006710 (C2-C12) alkenyl group Chemical group 0.000 abstract 1
- 239000010408 film Substances 0.000 description 120
- 239000002585 base Substances 0.000 description 79
- 238000009835 boiling Methods 0.000 description 26
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 26
- 229910052751 metal Inorganic materials 0.000 description 20
- 239000002184 metal Substances 0.000 description 20
- 230000008569 process Effects 0.000 description 19
- 239000012686 silicon precursor Substances 0.000 description 19
- 239000000460 chlorine Substances 0.000 description 18
- 229910052799 carbon Inorganic materials 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 14
- 239000000377 silicon dioxide Substances 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 12
- 239000007788 liquid Substances 0.000 description 11
- 239000003153 chemical reaction reagent Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- 125000003545 alkoxy group Chemical group 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 230000002829 reductive effect Effects 0.000 description 9
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 8
- 238000012545 processing Methods 0.000 description 8
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 8
- 150000001412 amines Chemical class 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 7
- 230000007062 hydrolysis Effects 0.000 description 7
- 238000006460 hydrolysis reaction Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 239000005052 trichlorosilane Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 150000001721 carbon Chemical group 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 150000003335 secondary amines Chemical class 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- KVKAPJGOOSOFDJ-UHFFFAOYSA-N CN(C)[Ta] Chemical compound CN(C)[Ta] KVKAPJGOOSOFDJ-UHFFFAOYSA-N 0.000 description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 150000004696 coordination complex Chemical class 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 4
- 125000002769 thiazolinyl group Chemical group 0.000 description 4
- 239000006200 vaporizer Substances 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- MHMBUJVKUFAYFM-UHFFFAOYSA-N C(C)N(C)[Ta] Chemical compound C(C)N(C)[Ta] MHMBUJVKUFAYFM-UHFFFAOYSA-N 0.000 description 3
- OTSOGXNIABDRQR-UHFFFAOYSA-N C(C)N(CC)[Ta] Chemical compound C(C)N(CC)[Ta] OTSOGXNIABDRQR-UHFFFAOYSA-N 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- SKYWAOSWRWWISV-UHFFFAOYSA-N N-propan-2-yl-N-(2-silylethyl)propan-2-amine Chemical compound C(C)(C)N(C(C)C)CC[SiH3] SKYWAOSWRWWISV-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 125000000304 alkynyl group Chemical group 0.000 description 3
- 229910021417 amorphous silicon Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229910002091 carbon monoxide Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 125000000753 cycloalkyl group Chemical group 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 3
- 238000003618 dip coating Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 239000002019 doping agent Substances 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- 125000002524 organometallic group Chemical group 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000006557 surface reaction Methods 0.000 description 3
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- LBUJPTNKIBCYBY-UHFFFAOYSA-N 1,2,3,4-tetrahydroquinoline Chemical compound C1=CC=C2CCCNC2=C1 LBUJPTNKIBCYBY-UHFFFAOYSA-N 0.000 description 2
- PAMIQIKDUOTOBW-UHFFFAOYSA-N 1-methylpiperidine Chemical compound CN1CCCCC1 PAMIQIKDUOTOBW-UHFFFAOYSA-N 0.000 description 2
- FENFUOGYJVOCRY-UHFFFAOYSA-N 1-propoxypropan-2-ol Chemical compound CCCOCC(C)O FENFUOGYJVOCRY-UHFFFAOYSA-N 0.000 description 2
- RKMGAJGJIURJSJ-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidine Chemical compound CC1(C)CCCC(C)(C)N1 RKMGAJGJIURJSJ-UHFFFAOYSA-N 0.000 description 2
- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical class CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 2
- XLLIQLLCWZCATF-UHFFFAOYSA-N 2-methoxyethyl acetate Chemical compound COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 2
- WWUVJRULCWHUSA-UHFFFAOYSA-N 2-methyl-1-pentene Chemical compound CCCC(C)=C WWUVJRULCWHUSA-UHFFFAOYSA-N 0.000 description 2
- BHNHHSOHWZKFOX-UHFFFAOYSA-N 2-methyl-1H-indole Chemical compound C1=CC=C2NC(C)=CC2=C1 BHNHHSOHWZKFOX-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 2
- KTRLOZVAGCGQMN-UHFFFAOYSA-N CC(C)N([SiH3])C1CCCCC1 Chemical compound CC(C)N([SiH3])C1CCCCC1 KTRLOZVAGCGQMN-UHFFFAOYSA-N 0.000 description 2
- GXWVPPAINCVSEX-UHFFFAOYSA-N CCN(CC)[SiH2]Cl Chemical compound CCN(CC)[SiH2]Cl GXWVPPAINCVSEX-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical compound CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- FBIBVSMERHBWSW-UHFFFAOYSA-N N-cyclohexylsilylmethanamine Chemical compound C1(CCCCC1)[SiH2]NC FBIBVSMERHBWSW-UHFFFAOYSA-N 0.000 description 2
- LFDXRDGBAGSVFB-UHFFFAOYSA-N N-dichlorosilyl-N-ethylethanamine Chemical class CCN(CC)[SiH](Cl)Cl LFDXRDGBAGSVFB-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical class CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 125000004103 aminoalkyl group Chemical group 0.000 description 2
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 description 2
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical class B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 2
- 229910000085 borane Inorganic materials 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910052729 chemical element Inorganic materials 0.000 description 2
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 description 2
- KCWYOFZQRFCIIE-UHFFFAOYSA-N ethylsilane Chemical compound CC[SiH3] KCWYOFZQRFCIIE-UHFFFAOYSA-N 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
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- 125000000587 piperidin-1-yl group Chemical group [H]C1([H])N(*)C([H])([H])C([H])([H])C([H])([H])C1([H])[H] 0.000 description 1
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- WYVAMUWZEOHJOQ-UHFFFAOYSA-N propionic anhydride Chemical compound CCC(=O)OC(=O)CC WYVAMUWZEOHJOQ-UHFFFAOYSA-N 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 150000004874 silinanes Chemical class 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
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- 239000007921 spray Substances 0.000 description 1
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- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- MNWRORMXBIWXCI-UHFFFAOYSA-N tetrakis(dimethylamido)titanium Chemical compound CN(C)[Ti](N(C)C)(N(C)C)N(C)C MNWRORMXBIWXCI-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- 238000001149 thermolysis Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 230000001131 transforming effect Effects 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- 229940094989 trimethylsilane Drugs 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
-
- 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
- C23C16/22—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
-
- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/025—Silicon compounds without C-silicon linkages
-
- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
-
- 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
- C23C16/22—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
- C23C16/24—Deposition of silicon only
-
- 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
- C23C16/22—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
-
- 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
- C23C16/22—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
- C23C16/40—Oxides
- C23C16/401—Oxides containing silicon
- C23C16/402—Silicon dioxide
-
- 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
-
- 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]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45536—Use of plasma, radiation or electromagnetic fields
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
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- H—ELECTRICITY
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- 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
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
- H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
- H01L21/02219—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen
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Abstract
本发明描述了形成薄膜的前体和方法。在一个方面,提供了具有下式I的硅前体:XmR1 nHpSi(NR2R3)4-m-n-p I其中X选自C1、Br、I;R1选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且m+n+p小于4,其中R2和R3连接形成环或不连接。
Description
相关申请的交叉引用
本申请根据35U.S.C.119要求下列申请的优先权:2011年9月27日提交的U.S.临时申请号61/539,717,其所披露的内容整体以引用的方式并入本文。
背景技术
本文描述了可以用于沉积介电薄膜的前体,特别是卤代有机氨基硅烷前体,所述介电薄膜包括,但不限于,含硅薄膜诸如硅、无定形硅、晶体硅、微晶硅、多晶硅、氮化硅、氧化硅、碳掺杂的氧化硅、碳氮化硅和氧氮化硅薄膜。在又另一方面,本文描述了用于沉积含硅介电薄膜的卤代有机氨基硅烷前体在制造集成电路器件中的用途。在这些或其它的方面,卤代有机氨基硅烷前体可以用于多种基于气相的沉积工艺,包括,但不限于原子层沉积(“ALD”)、化学气相沉积(“CVD”)、循环化学气相沉积(“CCVD”)、等离子体增强化学气相沉积(“PECVD”)、低压化学气相沉积(“LPCVD”)和常压化学气相沉积(“APCVD”)或基于液体的沉积工艺,包括,但不限于旋涂、浸涂、气溶胶、喷墨、丝网印刷或喷射沉积或薄膜形成法。
几类化合物可用作含硅薄膜(例如,但不限于,氧化硅或氮化硅薄膜)的前体。适合用作前体的这些化合物的实例包括硅烷类、氯硅烷类、聚硅氮烷类、氨基硅烷类和叠氮基硅烷类。惰性载气或稀释剂(例如,但不限于,氦、氢、氮等)也用于输送前体到反应室中。
美国专利6,869,638描述了采用金属氨基化物和下式的氨基硅烷化合物在衬底上形成栅介电薄膜例如栅介电的、高介电常数金属氧化物和铁电金属氧化物的CVD方法:HxSiAy(NR1R2)4-x-y,其中H是氢;x为0至3;N是氮,各R1和R2相同或不同且独立地选自下组:H、芳基、全氟芳基、C1-C8烷基和C1-C8全氟烷基;且n为1-6。6,869,638号专利中描述的氨基硅烷前体的实例包括二(二乙基氨基)二氯硅烷和三(二乙基氨基)氯硅烷。
WO 2011/123792描述了由氨基-金属前体和卤代金属前体的组合形成含金属-氮化物的薄膜的低温的、基于热或等离子体的ALD方法,优选从氨基硅烷前体和氯硅烷前体的组合形成含SiN的薄膜。该WO 2011/12792申请中描述了包含氨基氯硅烷和氨基烷基硅烷前体的氨基硅烷前体,所述氨基氯硅烷具有式Cl4-xSi(NR’R”)x,其中x=2或3,R’和R”独立地选自H或烷基,且R和R”可以连接以形成环结构,所述氨基烷基硅烷前体具有式R’”4-xSi(NR’R”)x,其中x=1、2或3,R’和R”独立地选自H或烷基,R’和R”可以连接以形成环结构,且R’”是具有少于三个碳的烷基。
参考文献“Substitution of chlorine in silicon tetrachloride bydimethyl,diethylamino,and piperidino groups”,Breederveld等,Research(London)5:537-9(1952)描述了通过用二烷基氨基逐步替换SiCl4中的原子来合成二烷基氨基氯硅烷,从而产生一种或多种以下化合物:二乙基氨基三氯硅烷、二(二乙基氨基)二氯硅烷、三(二乙基氨基)氯硅烷或四(二乙基氨基)硅烷。类似的过程用于制备哌啶子基三氯硅烷和二哌啶子基二氯硅烷。
参考文献“Molecular structures of some(dimethylamino)halogenosilanes in the gas phase by electrondiffraction and the crystal and molecular structures on mono-anddi-chloro(dimethylamino)silane by x-ray diffraction at lowtemperatures”,Anderson等,J.Chem.Soc.,(1987)描述了(二甲基氨基)卤代硅烷SiH2X(NMe2),其中X=Cl、Br或I。
参考文献“Chloroaminosilanes.I.Preparation ofchloro(dimethylamino)hydrogen silanes”,Washburne等,Inorg.Nucl.Chem.,5(1):17-19(1969)描述了HSiCl2NMe2(I)、HSiCl(NMe2)2(II)和HSi(NMe2)3(III)的制备以及这些化合物的相关化学性质。
参考文献“Preparation of β-cyanoethyltrichlorosilane usingsilylamine catalysts”,Pike等,Journal of Organic Chemistry,27(6):21-90-92(1962)描述了(CH3)3SiNR2型甲硅烷基胺,其通过将三氯硅烷添加到丙烯腈上被证明是定向催化剂。该参考文献中描述的甲硅烷基胺的一个实例是(iPr2N)SiCl2H。
本领域需要提供可用于沉积含硅薄膜并提供一个或多个以下优点的前体:低的加工温度(例如,300℃或以下);相对良好的沉积速率;组成均匀性和/或高纯度。
发明简述
本文描述了卤代有机氨基硅烷前体和将其用于在衬底的至少一部分上形成包含硅的薄膜的方法,含硅薄膜诸如但不限于硅薄膜、氧化硅、碳掺杂的氧化硅、氮化硅、氧氮化硅、碳化硅、碳氮化硅及其组合。本文还公开了在待加工的物体(例如,举例来说,半导体晶片)上形成介电薄膜或涂层的方法。在本文所述方法的一个实施方式中,包含硅和氧的层在生成衬底上的氧化硅层的条件下,在沉积室中使用卤代有机氨基硅烷前体、任选的一种或多种另外的非卤代有机氨基硅烷前体和氧化剂而沉积到衬底上。在本文所述方法的另一个实施方式中,包含硅和氮的层在生成衬底上的氮化硅层的条件下,在沉积室中使用卤代前体、任选的一种或多种非卤代有机氨基硅烷前体和含氮前体而沉积到衬底上。在进一步的实施方式中,本文所述的卤代有机氨基硅烷前体也可以用作含金属薄膜(例如,但不限于,金属氧化物薄膜或金属氮化物薄膜)的掺杂剂。在本文所述方法中,本文所述的具有式I的卤代有机氨基硅烷用作至少一种含硅前体。
如本领域技术人员可理解的,在本文中所描述的式I中,在R2和R3连接在一起以形成环的情况下,R2包括用于与R3连接的键(而不是氢取代基),反之亦然。因此,在R2和R3连接在一起以形成环的情况下,R2选自直链或支链C1-C10亚烷基、C3-C12亚烯基、C3-C12亚炔基、C4-C10亚环烷基和C6-C10亚芳基;R3选自支链C3-C10亚烷基、C3-C12亚烯基、C3-C12亚炔基、C4-C10亚环烷基和C6-C10亚芳基。
在一个方面,本文所述的卤代有机氨基硅烷前体包含具有下式I的硅前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环。在某些实施方式中,式I中的R2和R3可以连接在一起以形成环。在其他实施方式中,式I中的R2和R3不连接在一起形成环。
在另一个方面,还提供了在衬底的至少一个表面上形成含硅薄膜的方法,其包括:
在反应室中提供所述衬底的该至少一个表面;和
通过选自化学气相沉积工艺和原子层沉积工艺的沉积工艺,使用具有下式I的卤代有机氨基硅烷前体在所述的至少一个表面上形成含硅薄膜:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环。在式I的一个具体实施方式中,R2和R3可以连接在一起以形成环。在式I的另一个实施方式中,R2和R3不连接在一起形成环。
在另一个方面,提供了通过原子层沉积工艺或循环化学气相沉积工艺形成氧化硅薄膜的方法,该方法包括以下步骤:
a.在反应器中提供衬底;
b.向反应器中引入选自由下式I表示的至少一种卤代有机氨基硅烷前体的至少一种硅前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
c.用吹扫气体吹扫反应器;
d.向反应器中引入氧源;
e.用吹扫气体吹扫反应器;和
重复步骤b至e直到获得希望的薄膜厚度。
在另外的方面,提供了使用CVD工艺在衬底的至少一个表面上形成氧化硅薄膜的方法,包括:
a.在反应器中提供衬底;
b.向反应器中引入由下式I表示的至少一种卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和
c.提供氧源以沉积氧化硅薄膜到该至少一个表面上。
在另一个方面,提供了通过原子层沉积工艺或循环化学气相沉积工艺形成氮化硅薄膜的方法,该方法包括以下步骤:
a.在反应器中提供衬底;
b.向反应器中引入由下式I表示的至少一种硅前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
c.用吹扫气体吹扫反应器;
d.向反应器中引入含氮源;
e.用吹扫气体吹扫反应器;和
重复步骤b至e直到获得希望的氮化硅薄膜厚度。
在另外的方面,提供了使用CVD工艺在衬底的至少一个表面上形成氮化硅薄膜的方法,包括:
a.在反应器中提供衬底;
b.向反应器中引入由下式I表示的至少一种有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和
c.提供含氮源,其中所述的至少一种有机氨基硅烷前体和含氮源反应以沉积含硅和氮的薄膜到所述的至少一个表面上。
在另一个方面,本文描述了用于沉积介电薄膜的容器,包含一种或多种具有式I的卤代有机氨基硅烷前体。在一个特别的实施方式中,所述容器包含至少一个配备有适当的阀和配件的可加压容器(优选由不锈钢制成),以允许输送一种或多种前体到用于CVD或ALD工艺的反应器中。
在又另一个方面,提供了用于沉积介电薄膜的组合物,其包含:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和选自下组的溶剂:醚、叔胺、腈、烷基烃、芳族烃、叔氨基醚或其混合物。
附图简要说明
图1提供了实施例3中描述的2,6-二甲基哌啶子基二氯硅烷的质谱(MS)图。
发明详述
卤代有机氨基硅烷用作形成化学计量的和非化学计量的含硅薄膜(例如,但不限于,硅、无定形硅、晶体硅、微晶硅、多晶硅、氧化硅、碳掺杂的氧化硅、氮化硅、氧氮化硅和氧碳氮化硅的薄膜)的前体。这些前体也可以用作例如用于含金属薄膜的掺杂剂。卤代有机氨基硅烷前体通常是高纯度的挥发性液体前体化学物质,其被蒸发并作为气体输送到沉积室或反应器中以通过用于半导体器件的CVD或ALD工艺沉积含硅薄膜。在其他实施方式中,所述卤代有机氨基硅烷可用于基于液体的沉积或薄膜形成方法中,例如,但不限于,旋涂、浸涂、气溶胶、喷墨、丝网印刷或喷射涂覆。用于沉积的前体材料的选择取决于希望产生的介电材料或薄膜。例如,前体材料可以基于其化学元素的含量、其化学元素的化学计量比和/或在CVD下形成的最终介电薄膜或涂层而进行选择。前体材料也可以对于各种其它特征如成本、非毒性、操作性能、在室温下保持液相的能力、挥发性、分子量和/或其它因素而进行选择。在某些实施方式中,本文描述的前体可以通过任何方式,优选使用配备有适当的阀和配件的可加压不锈钢容器输送到反应器系统,以允许将液相前体输送至沉积室或反应器。
据信,与非卤代有机氨基硅烷相比,本文所描述的卤代有机氨基硅烷前体可在化学气相沉积(特别是循环CVD沉积)或原子层沉积期间提供对于衬底表面的更好的反应性,以经由原位催化反应形成Si-N-Si键、Si-Si键、Si-O-Si键而释放有机胺和HCl,然后有机胺和HCl结合形成胺-盐酸盐。据信,与常规的硅前体例如四氯化硅或有机氨基硅烷相比,卤代有机氨基硅烷的一个特别的优点是在ALD或CCVD过程中卤素和有机氨基都可以与衬底表面上的Si-OH或SiNH2反应来锚定所述前体,从而促进含硅薄膜的沉积。除上述优点之外,在例如采用循环CVD、ALD或PEALD沉积方法来沉积氧化硅或氮化硅薄膜的某些实施方式中,本文描述的卤代有机氨基硅烷前体可能能够在相对低的沉积温度(例如,500℃或更低,400℃或更低或得300℃或更低)下沉积高密度的材料。在其他实施方式中,本文描述的前体例如可以用于在约500℃-约800℃的温度下的较高温度的沉积。
在一个方面,提供了由下式I表示的前体或卤代有机氨基硅烷:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环。在式I的卤代有机氨基硅烷的某些实施方式中,R2和R3可以连接在一起以形成环。在式I的卤代有机氨基硅烷的替代实施方式中,R2和R3不连接在一起形成环。
在式I-III中和在整个说明书中,术语“烷基”表示具有1-10个或1-4个碳原子的直链或支链官能团。示例性的烷基包括,但不限于,甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基、异戊基、叔戊基、己基、异己基和新己基。在某些实施方式中,烷基可以具有一个或多个与其连接的官能团,例如,但不限于,烷氧基、二烷基氨基或其组合。在其它实施方式中,烷基不具有与其连接的一个或多个官能团。
在式I-III中和在整个说明书中,术语“环烷基”表示具有3-12个或4-10个碳原子的环状官能团。示例性的环烷基包括,但不限于,环丁基、环戊基、环己基和环辛基。
在式I-III中和在整个说明书中,术语“芳基”表示具有6-12个碳原子的芳香族环状官能团。示例性的芳基包括,但不限于,苯基、苄基、氯代苄基、甲苯基和邻二甲苯基。
在式I-III中和在整个说明书中,术语“烯基”表示具有一个或多个碳-碳双键并具有2-12个或2-6个碳原子的基团。示例性的烯基包括,但不限于,乙烯基或烯丙基。
在式I-III中和在整个说明书中,术语“炔基”表示具有一个或多个碳-碳三键并具有2-12个或2-6个碳原子的基团。
在式I-III中和在整个说明书中,术语“烷氧基”表示连接至氧原子且可以具有1-12个或1-6个碳原子的烷基(例如,R-O)。示例性的烷氧基包括,但不限于,甲氧基(-OCH3)、乙氧基(-OCH2CH3)、正丙氧基(-OCH2CH2CH3)和异丙氧基(-OCHMe2)。
在某些实施方式中,式I-III中的烷基、烯基、炔基、烷氧基和/或芳基中的一个或多个基团可以被取代,或者具有替代例如氢原子的一个或多个原子或原子团。示例性的取代基包括,但不限于,氧、硫、卤素原子(例如,F、Cl、I或Br)、氮和磷。在其它实施方式中,式I中的烷基、烯基、炔基、烷氧基和/或芳基中的一个或多个可以是未取代的。
在某些实施方式中,取代基R2和R3在式I中连接以形成环结构。在其它实施方式中,取代基R2和R3在式I中不连接。
下表1提供了具有式I的有机氨基硅烷的某些实施方式的一些非限制性实例。
表1.示例性的具有式I的有机氨基硅烷
在某些实施方式中,式I的卤代有机氨基硅烷包含Cl作为X并选自ClH2Si(NR2R3)(其中m=1、n=0、p=2,R2选自直链或支链C3-C10烷基和C6-C10芳基,R3是支链C3-C10烷基或C6-C10芳基,且其中R2和R3可以形成环或烷基取代的环)和R1ClHSi(NR2R3)(其中m=1、n=1、p=1,R1是C1-C10烷基且R2和R3是直链或支链C3-C10烷基或C4-C10芳基,且其中R2和R3可以形成环或烷基取代的环)。
在某些实施方式中,具有式I的卤代有机氨基硅烷可在有机溶剂或溶剂混合物中通过使1摩尔当量的二氯硅烷(DCS)与1摩尔当量的仲胺或使三氯硅烷(TCS)和1或2摩尔当量的具有下式II的仲胺反应来制备,采用1或2摩尔当量的叔胺例如三乙胺或三丁胺来吸收副产物氯化氢,优选如以下实施例1和2所示采用叔胺。在某些实施方式中,叔胺被等摩尔当量的仲胺替代。可用于该实施方式中的所选择的仲胺具有下式II:
R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基,且其中R2和R3连接以形成环或R2和R3不连接形成环。在其中R2和/或R3是支链烷基、环烷基或芳族基团的实施方式中,由这些胺合成的卤代有机氨基硅烷的稳定性可极大提高,因为氨基和卤素原子的分子间取代交换反应被这种R2和/或R3基团的立体位阻所阻碍。具有式II的示例性仲胺包括,但不限于:二异丙胺、二异丁胺、二仲丁胺、异丙基甲基胺、异丙基乙基胺、环己基甲基胺、环丙基乙基胺、二环丙基胺、环己基异丙基胺、N-甲基苯胺(苯基甲基胺)、N-乙基苯胺(苯基乙基胺)、N-异丙基苯胺、N-丁基苯胺、N-烯丙基苯胺、N-乙基-间甲苯胺、N-甲基-邻甲苯胺、N-甲基-对甲苯胺、4-氟-N-甲基苯胺、4-氯-N-甲基苯胺、N-环己基苯胺、3-苯胺基丙腈或N-苯基氨基乙腈。
具有式II(其中R2和R3连接以形成环)的示例性的胺包括,但不限于2,6-二甲基哌啶、2-甲基哌啶、2-甲基吡咯烷、2,5-二甲基吡咯烷、2,2,6,6-四甲基哌啶、3-甲基吲哚、2-甲基吲哚、吲哚、十氢喹啉、8-甲基-1,2,3,4-四氢喹啉、3-吲哚乙腈、2-甲基二氢吲哚、2,3-二氢吲哚、5-甲基二氢吲哚、1,2,3,4-四氢喹啉、1,2,3,4-四氢-2-甲基喹啉、1,2,3,4-四氢-6-甲基喹啉、3,4-二氢-2H-1,4-苯并噁嗪、咔唑、2,6-二甲基吗啉和3,5-二甲基吗啉。
下面的反应式1、2和3提供了可以用于制备具有本文描述的式I的卤代有机氨基硅烷的反应流程或合成路线的实例。反应式1、2和3中的反应可以利用有机溶剂(例如,在有机溶剂存在的情况下)进行。在其中使用有机溶剂的实施方式中,合适的有机溶剂的例子包括,但不限于,烃(如己烷、辛烷、甲苯)和醚(如二乙醚和四氢呋喃(THF))。在这些实施方式或其它实施方式中,反应温度在大约-70℃至所采用溶剂(涉及溶剂的话)的沸点的范围内。所产生的有机氨基硅烷可以通过在除去所有副产物以及溶剂后的真空蒸馏进行纯化。反应式1-3是涉及二氯硅烷或三氯硅烷的反应的实施方式。涉及部分胺化反应的合成路线的实例在本文中以实施例1和3给出,而涉及可经由具有式II的胺与烷基金属的反应制得的金属氨基化物的反应式2在实施例2中给出。
反应式1
反应式2
反应式3
用于形成含硅介电薄膜或涂层的方法是沉积工艺。用于本文公开的方法的合适沉积工艺的例子包括,但不限于,循环CVD(CCVD)、MOCVD(金属有机CVD)、热化学气相沉积、等离子体增强化学气相沉积(“PECVD”)、高密度PECVD、光子辅助CVD、等离子体-光子辅助的化学气相沉积(“PPECVD”)、低温化学气相沉积、化学物质辅助的气相沉积、热丝化学气相沉积、液体聚合物前体的CVD、超临界流体的沉积和低能量CVD(LECVD)。在某些实施方式中,含金属的薄膜通过原子层沉积(ALD)、等离子体增强ALD(PEALD)或等离子体增强循环CVD(PECCVD)工艺沉积。如本文所用,术语“化学气相沉积工艺”指其中衬底暴露于一种或多种与衬底表面反应或在衬底表面上分解以产生希望的沉积的挥发性前体的任何工艺。如本文所用,术语“原子层沉积工艺”是指将材料的薄膜沉积到具有不同组成的衬底上的自限式(self-limiting)(例如,在各反应循环中沉积的薄膜材料的量是恒定的)顺序表面化学作用。虽然本文中使用的前体、试剂和源有时可以描述为“气态的”,但应理解该前体可以是通过直接蒸发、鼓泡或升华在利用或不利用惰性气体的条件下转运到反应器中的液体或固体。在一些情况中,蒸发的前体可以经过等离子体发生器。在一个实施方式中,使用ALD工艺沉积介电薄膜。在另一实施方式中,使用CCVD工艺沉积介电薄膜。在进一步的实施方式中,使用热CVD工艺沉积介电薄膜。本文使用的术语“反应器”包括,但不限于反应室或沉积室。
在某些实施方式中,本文公开的方法通过使用在引入反应器之前和/或过程中隔离前体的ALD或CCVD避免了前体的预反应。在这一方面,如ALD或CCVD工艺的沉积技术用于沉积介电薄膜。在一个实施方式中,通过将衬底表面交替地暴露于一种或多种含硅前体、氧源、含氮源或其它前体或试剂而经由ALD工艺沉积薄膜。薄膜生长通过表面反应的自限式控制、各前体或试剂的脉冲长度和沉积温度进行。但是,一旦衬底表面饱和,薄膜生长停止。
在某些实施方式中,本文描述的方法进一步包括除了具有上述式I的卤代有机氨基硅烷前体之外的一种或多种另外的含硅前体或非卤代前体。另外的含硅前体的例子包括,但不限于,有机硅化合物如硅氧烷类(例如,六甲基二硅氧烷(HMDSO)和二甲基硅氧烷(DMS0))、有机硅烷类(例如,甲基硅烷、二甲基硅烷、乙烯基三甲基硅烷、三甲基硅烷、四甲基硅烷、乙基硅烷、二甲硅烷基甲烷、2,4-二硅杂戊烷、1,4-二硅杂丁烷、2,5-二硅杂己烷、2,2-二甲硅烷基丙烷、1,3,5-三硅杂环己烷和这些化合物的氟化衍生物)、含苯基的有机硅化合物(例如,二甲基苯基硅烷和二苯基甲基硅烷)、含氧有机硅化合物,例如二甲基二甲氧基硅烷、1,3,5,7-四甲基环四硅氧烷、1,1,3,3-四甲基二硅氧烷、1,3,5,7-四硅杂-4-氧代-庚烷、2,4,6,8-四硅杂-3,7-二氧代-壬烷、2,2-二甲基-2,4,6,8-四硅杂-3,7-二氧代-壬烷、八甲基环四硅氧烷、[1,3,5,7,9]-五甲基环五硅氧烷、1,3,5,7-四硅杂-2,6-二氧代-环辛烷、六甲基环三硅氧烷、1,3-二甲基二硅氧烷、1,3,5,7,9-五甲基环五硅氧烷、六甲氧基二硅氧烷和这些化合物的氟化衍生物。
在本文所描述的方法的一个具体的实施方式中,所述非卤代含硅前体是具有下式III的化合物:
(R2R3N)SiH3(III)
其中R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基,且其中R2和R3连接以形成环或R2和R3不连接形成环。在式III的某些实施方式中,R2和R3可以结合以形成环状基团或环。在式III的其他实施方式中,R2和R3不结合形成环状基团或环。非卤代含硅前体的实例包括,但不限于:二-异丙基氨基硅烷、二-仲丁基氨基硅烷、苯基甲基氨基硅烷和2,6-二甲基哌啶子基硅烷。
取决于沉积方法,在某些实施方式中,一种或多种卤代或非卤代的含硅前体可以以预定的摩尔量(molar volume)或大约0.1-大约1000微摩尔引入反应器中。在这一实施方式或其它实施方式中,卤代或非卤代的有机氨基硅烷前体可以以预定的时间长度引入反应器中。在某些实施方式中,该时间长度为大约0.001-大约500秒。
在某些实施方式中,使用氧源、含氧的试剂或前体在氧的存在下形成使用本文描述的方法沉积的介电薄膜。氧源可以以至少一种氧源的形式引入反应器中和/或可以附带地存在于用于沉积工艺的其它前体中。合适的氧源气体可以包括,例如,水(H2O)(例如,去离子水、纯化水和/或蒸馏水)、氧(O2)、氧等离子体、臭氧(O3)、NO、NO2、一氧化碳(CO)、二氧化碳(CO2)及其组合。在某些实施方式中,氧源包含以大约1-大约2000标准立方厘米/分钟(squarecubic centimeter)(sccm)或大约1-大约1000sccm的流速引入反应器中的氧源气体。氧源可以引入大约0.1-大约100秒的时间。在一个特别的实施方式中,氧源包含具有10℃或更高的温度的水。在其中薄膜通过ALD或循环CVD工艺沉积的实施方式中,前体脉冲可以具有大于0.01秒的脉冲持续时间,且氧源可以具有小于0.01秒的脉冲持续时间,而水的脉冲持续时间可以具有小于0.01秒的脉冲持续时间。在再另一实施方式中,脉冲之间的吹扫持续时间可以低至0秒或没有脉冲之间的吹扫而连续地进行脉冲。氧源或试剂以低于与硅前体的1∶1比率的分子数量提供,从而至少一些碳保留在如此沉积的介电薄膜中。
在某些实施方式中,介电薄膜包含硅和氮。在这些实施方式中,使用本文描述的方法沉积的介电薄膜在含氮源的存在下形成。含氮源可以以至少一种氮源的形式引入反应器中和/或可以附带地存在于用于沉积工艺的其它前体中。合适的含氮源气体可以包括,例如,氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。在某些实施方式中,含氮源包含以大约1至大约2000标准立方厘米/分钟(sccm)或大约1至大约1000sccm的流速引入反应器中的氨等离子体或氢/氮等离子体源气体。含氮源可以引入大约0.1至大约100秒的时间。在其中薄膜通过ALD或循环CVD工艺沉积的实施方式中,前体脉冲可以具有大于0.01秒的脉冲持续时间,且含氮源可以具有小于0.01秒的脉冲持续时间,而水的脉冲持续时间可以具有小于0.01秒的脉冲持续时间。在再另一实施方式中,脉冲之间的吹扫持续时间可以低至0秒或没有脉冲之间的吹扫而连续地进行脉冲。
本文公开的沉积方法可以包括一种或多种吹扫气体。用于吹扫掉未消耗的反应物和/或反应副产物的吹扫气体是不与前体发生反应的惰性气体。示例性的吹扫气体包括,但不限于,氩(Ar)、氮(N2)、氦(He)、氖、氢(H2)及其混合物。在某些实施方式中,吹扫气体如Ar以大约10至大约2000sccm的流速供应到反应器中大约0.1-1000秒,从而吹扫可能残留在反应器中的未反应物质和任何副产物。
供应前体、氧源、含氮源和/或其它前体、源气体和/或试剂的相应步骤可以通过改变供应这些物质的时间来进行,以改变所获得的介电薄膜的化学计量组成。
能量供应给前体、含氮源、还原剂、其它前体或其组合中的至少一种以诱导反应和在衬底上形成介电薄膜或涂层。这种能量可以通过(但不限于)热、等离子体、脉冲等离子体、螺旋波等离子体(helicon plasma)、高密度等离子体、电感耦合等离子体、X射线、电子束、光子、远程等离子体方法及其组合提供。在某些实施方式中,第二RF射频源可以用于改变衬底表面处的等离子体特性。在其中沉积涉及到等离子体的实施方式中,等离子体发生方法可以包括直接等离子体发生方法(其中等离子体在反应器中直接发生)或可选地远程等离子体发生方法(其中等离子体在反应器外发生并供应到反应器中)。
有机氨基硅烷前体和/或其它含硅前体可以以多种方式输送到反应室如CVD或ALD反应器。在一个实施方式中,可以利用液体输送系统。在替代的实施方式中,可以采用综合的液体输送和闪蒸处理单元,例如,举例来说,由Shoreview,MN的MSP Corporation制造的涡轮蒸发器(turbo vaporizer),以使得低挥发性的物质能够定量地输送,这导致可重现的输送和沉积而没有前体的热分解。在液体输送方式中,本文描述的前体可以以纯液体形式输送,或者可选择地,可以以包含前体的溶剂制剂或组合物形式使用。因此,在某些实施方式中,当可能在给定的终端应用中希望和有利时,前体制剂可以包括具有适当特性的溶剂成分以在衬底上形成薄膜。
对于其中具有式I的卤代有机氨基硅烷前体用于包含溶剂和具有本文描述的式I的卤代有机氨基硅烷前体的组合物中的那些实施方式,所选择的溶剂或其混合物不与有机氨基硅烷反应。组合物中溶剂以重量百分比计的量的范围从0.5重量%到99.5重量%或者从10重量%到75重量%。在这一或其他实施方式中,所述的溶剂具有和式I的卤代有机氨基硅烷沸点(b.p.)相似的沸点或者溶剂的沸点和式I的卤代有机氨基硅烷的沸点之间的差异是40℃或更小、30℃或更小、20℃或更小或者10℃。或者,沸点之间的差异范围具有下面任意一个或多个端点:0、10、20、30或40℃。沸点差异的合适范围的实例包括,但不限于0-40℃、20-30℃或10-30℃。组合物中合适的溶剂的实例包括,但不限于:醚(例如1,4-二氧杂环己烷、二丁基醚)、叔胺(例如吡啶、1-甲基哌啶、1-乙基哌啶、N,N’-二甲基哌嗪、N,N,N’,N’-四甲基乙二胺)、腈(例如苯甲腈)、烷基烃(如辛烷、壬烷、十二烷、乙基环己烷)、芳族烃(例如甲苯、均三甲苯)、叔氨基醚(例如双(2-二甲基氨基乙基)醚)或者它们的混合物。一些非限制性的示例组合物包括,但不限于:包含二异丙基氨基硅烷(沸点约116℃)和辛烷(沸点125-126℃)的组合物、包含二异丙基氨基硅烷(沸点约116℃)和吡啶(沸点115℃)的组合物、包含二异丙基氨基硅烷(沸点约116℃)和甲苯(沸点110℃)的组合物、包含N-甲基环己基氨基硅烷(沸点约171℃)和癸烷(沸点174℃)的组合物、包含N-甲基环己基氨基硅烷(沸点约171℃)和二乙二醇二甲基醚(沸点162℃)的组合物、包含N-异丙基环己基氨基硅烷(沸点约199℃)和双(2-二甲基氨基乙基)醚(沸点189℃)的组合物、包含N-异丙基环己基氨基硅烷(沸点约199℃)和苯甲腈(沸点191℃)的组合物。
在另一实施方式中,本文描述了用于沉积介电薄膜的容器,其包含一种或多种具有式I的卤代有机氨基硅烷前体。在一个特别的实施方式中,容器包含至少一个配备有适当的阀和配件的可加压容器(优选由不锈钢制成),以允许一种或多种前体输送到用于CVD或ALD工艺的反应器。在这一实施方式或其它实施方式中,式I的卤代有机氨基硅烷前体在由不锈钢构成的可加压容器中提供,且前体的纯度为以重量计为98%或更高或者99.5%或更高,这适合于大多数的半导体应用。在某些实施方式中,这种容器也可以具有用于混合所述前体和一种或多种另外的前体(如果需要)的装置。在这些实施方式或其它实施方式中,容器的内容物可以与另外的前体预混合。可选择地,卤代有机氨基硅烷前体和/或其它前体可以保持在独立的容器中或在具有用于在储存期间保持有机氨基硅烷前体和其它前体隔离的分隔装置的单一容器中。在某些实施方式中,容器中具有式I的卤代有机氨基硅烷前体还包含回填气体(back fillgas),例如但不限于:氮气、惰性气体例如氦气或其组合。在替代的实施方式中,所述容器不包含回填气体。
如上所述,卤代有机氨基硅烷的纯度水平是足够高的,以足以为可靠的半导体生产所接受。在某些实施方式中,本文所述的卤代有机氨基硅烷前体包含少于2%重量、或少于1%重量或少于0.5%重量的一种或多种以下的杂质:游离胺、游离卤化物或卤素离子及高分子量物质。本文所述的有机氨基硅烷的较高纯度可以通过一种或多种下述过程获得:纯化、吸附和/或蒸馏。
在本文描述的方法的一个实施方式中,可以采用循环沉积工艺如CCVD、ALD或PEALD,其中采用选自具有式I的卤代有机氨基硅烷前体的至少一种含硅前体和任选地采用含氮源(例如,举例来说,氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体)。
在某些实施方式中,连接前体容器到反应室的气体管线根据工艺要求加热到一个或多个温度,且具有式I的卤代有机氨基硅烷前体的容器保持在一个或多个温度以进行鼓泡。在其它实施方式中,将包含至少一种具有式I的卤代有机氨基硅烷前体的溶液注入到蒸发器中,所述蒸发器保持在一个或多个温度下用于直接液体注射。
氩和/或其它气体的气流可以用作载气以在前体脉冲期间帮助输送该至少一种有机氨基硅烷前体的蒸气到反应室。在某些实施方式中,反应室工作压力为大约1Torr。
在典型的ALD或CCVD工艺中,衬底(如氧化硅衬底)在反应室中的加热台上加热,所述加热台初始暴露于该含硅前体以使得该复合物化学吸附到衬底表面上。
吹扫气体(如氩气)从处理室吹扫掉未吸附的过量复合物。在充分吹扫后,含氮源可以被引入反应室中以与吸附的表面反应,随后进行另一气体吹扫以从该室除去反应副产物。处理循环可以重复以获得希望的薄膜厚度。
在某些实施方式中,所述工艺使用还原剂。所述还原剂通常以气态形式引入。适当的还原剂的实例包括,但不限于:氢气、氢等离子体、远程氢等离子体(remote hydrogen plasma)、硅烷类(即二乙基硅烷、乙基硅烷、二甲基硅烷、苯基硅烷、硅烷、乙硅烷、氨基硅烷、氯硅烷)、硼烷类(即硼烷、乙硼烷)、铝烷类、锗烷类、肼类、氨或其混合物。在例如沉积无定形硅的一个特定实施方式中,使用还原剂。
在这一实施方式或其它实施方式中,可以理解,本文描述的方法的步骤可以以多种顺序进行,可以顺序地或同时地(例如,在另一步骤的至少一部分时间内)进行,和以上述方式的任何组合方式进行。供应前体和含氮源气体的相应步骤可以通过改变供应这些物质的时间长度来进行,以改变所产生的介电薄膜的化学计量组成。
在本文公开的方法的另一实施方式中,使用包括以下步骤的ALD沉积方法形成含硅和氮的薄膜:
在ALD反应器中提供衬底;
向ALD反应器中引入至少一种由下式I表示的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
化学吸附该至少一种卤代有机氨基硅烷前体到衬底上;
用吹扫气体吹扫掉未反应的该至少一种有机氨基硅烷前体;
向加热的衬底上的该有机氨基硅烷前体提供含氮源以与吸附的该至少一种有机氨基硅烷前体反应;和
任选地吹扫掉任何未反应的含氮源。
在本文公开的方法的另一实施方式中,使用包括以下步骤的ALD沉积方法形成介电薄膜:
在反应器中提供衬底;
向反应器中引入至少一种由下式I表示的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
化学吸附该至少一种有机氨基硅烷前体到衬底上;
用吹扫气体吹扫掉未反应的该至少一种有机氨基硅烷前体;
向加热的衬底上的该有机氨基硅烷前体提供氧源以与吸附的该至少一种有机氨基硅烷前体反应;和
任选地吹扫掉任何未反应的氧源。
上述步骤限定了用于本文描述的方法的一个循环,且该循环可以重复直到获得希望的介电薄膜厚度。在这一实施方式或其它实施方式中,可以理解,本文描述的方法的步骤可以以多种顺序进行,可以顺序地或同时地(例如,在另一步骤的至少一部分时间内)进行,和以上述方式的任何组合方式进行。供应前体和氧源的相应步骤可以通过改变供应这些物质的时间长度来进行,以改变所产生的介电薄膜的化学计量组成,虽然总是以低于相对于可用的硅的化学计量的量使用氧。
对于多成分介电薄膜,其它前体如含硅前体、含氮前体、还原剂或其它试剂可以交替地引入反应室中。
在本文描述的方法的进一步实施方式中,使用热CVD工艺沉积介电薄膜。在这一实施方式中,该方法包括:
将一个或多个衬底置于加热到从环境温度到大约700℃的温度并保持在1Torr或更低的压力下的反应器中;
引入具有下式I的至少一种卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和
向反应器中提供氧源以至少部分地与该至少一种有机氨基硅烷前体反应并沉积介电薄膜到该一个或多个衬底上。在该CVD方法的某些实施方式中,反应器在引入步骤过程中保持在100mTorr至600mTorr的压力下。
上述步骤限定了用于本文描述的方法的一个循环,且该循环可以重复直到获得希望的介电薄膜厚度。在这一实施方式或其它实施方式中,可以理解本文描述的方法的步骤可以以多种顺序进行,可以顺序地或同时地(例如,在另一步骤的至少一部分时间内)进行,和以上述方式的任何组合方式进行。供应前体和氧源的相应步骤可以通过改变供应这些物质的时间长度来进行,以改变所产生的介电薄膜的化学计量组成,虽然总是以低于相对于可用的硅的化学计量量使用氧。
对于多成分介电薄膜,其它前体如含硅前体、含氮前体、氧源、还原剂和/或其它试剂可以交替地引入反应室中。
在本文描述的方法的进一步实施方式中,使用热CVD工艺沉积介电薄膜。在这一实施方式中,该方法包括:
将一个或多个衬底置于加热到从环境温度到大约700℃的温度并保持在1Torr或更低的压力下的反应器中;
引入具有下式I的至少一种卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和
向反应器中提供含氮源以至少部分地与该至少一种有机氨基硅烷前体反应并沉积介电薄膜到该一个或多个衬底上。在该CVD方法的某些实施方式中,反应器在引入步骤过程中保持在100mTorr至600mTorr的压力下。
如上所述,本文描述的方法可用于采用超过一种前体(例如本文描述的具有式I的卤代有机氨基硅烷)与另外的前体(例如本文描述的具有式III的非卤代有机氨基硅烷前体)、含硅前体例如本文描述的那些和/或氯硅烷(例如,但不限于一氯硅烷(MCS)、二氯硅烷(DCS)、三氯硅烷或四氯化硅)和/或烷基氯硅烷(例如,但不限于甲基氯硅烷、乙基氯硅烷、甲基二氯硅烷、乙基二氯硅烷)来沉积薄膜。在这些实施方式中,取决于所使用的不同前体的数目,将一种或多种前体描述为第一前体、第二前体、第三前体等等。该方法例如可用于循环化学气相沉积或原子层沉积中。在这些或其他的实施方式中,所述前体可以以多种方式引入(例如,a)引入第一前体;b)吹扫;c)引入第二前体;d)吹扫;e)引入第三前体;f)吹扫等,或者,a)引入第一前体;b)吹扫;c)引入第二前体;d)吹扫;e)引入第二前体;等)。在一个特定的实施方式中,提供了沉积氧化硅薄膜或硅、碳和氧化物薄膜的方法,包括以下步骤:
a)使由第一前体产生的蒸汽与加热的衬底接触以化学吸附所述第一前体到加热的衬底上;
b)吹扫掉任何未吸附的前体;
c)向加热的衬底上引入氧源以与吸附的第一前体反应;
d)吹扫掉任何未反应的氧源;
e)使由与第一前体不同的第二前体产生的蒸汽与加热的衬底接触以化学吸附所述第二前体到加热的衬底上;
f)吹扫掉任何未吸附的前体;
g)向加热的衬底上引入氧源以与吸附的第一和第二前体反应;和
h)吹扫掉任何未反应的氧源,
其中重复步骤a)至h)直到达到希望的厚度。
在本文所描述的方法的再另一个实施方式中,提供了沉积氮化硅或碳氮化硅薄膜的方法,包括以下步骤:
a)使由第一前体产生的蒸汽与加热的衬底接触以化学吸附所述第一前体到加热的衬底上;
b)吹扫掉任何未吸附的前体;
c)向加热的衬底上引入氮源以与吸附的第一前体反应;
d)吹扫掉任何未反应的氮源;
e)使由与第一前体不同的第二前体产生的蒸汽与加热的衬底接触以化学吸附所述第二前体到加热的衬底上;
f)吹扫掉任何未吸附的第二前体;
g)向加热的衬底上引入氮源以与吸附的第二前体反应;和
h)吹扫掉任何未反应的氮源,
其中重复步骤a)至h)直到达到希望的厚度。
在进一步的实施方式中,本文所描述的是采用循环化学气相沉积(CCVD)或原子层沉积(ALD)技术例如但不限于等离子体增强ALD(PEALD)或等离子体增强CCVD(PECCVD)工艺来沉积含硅薄膜的方法。在这些实施方式中,沉积温度可以相对较高,或为约500℃-800℃,从而控制特定半导体应用中所需的薄膜性能的规格。在一个特定的实施方式中,所述方法包括以下步骤:使由具有式I的卤代有机氨基硅烷产生的蒸汽与加热的衬底接触以化学吸附所述前体到加热的衬底上;吹扫掉任何未吸附的前体;引入还原剂以还原吸附的前体;和吹扫掉任何未反应的还原剂。
在某些实施方式中,本文描述的具有式I的卤代有机氨基硅烷前体也可以用作含金属薄膜(例如,但不限于,金属氧化物薄膜或金属氮化物薄膜)的掺杂剂。在这些实施方式中,使用ALD或CVD工艺(如本文描述的那些工艺),利用金属醇盐、金属氨基化物或挥发性有机金属前体沉积含金属薄膜。可以用于本文描述的方法的合适金属醇盐前体的例子包括,但不限于,3-6族金属醇盐、具有烷氧基和烷基取代的环戊二烯基配体的3-6族金属络合物、具有烷氧基和烷基取代的吡咯基配体的3-6族金属络合物、具有烷氧基和二酮根(diketonate)配体的3-6族金属络合物、具有烷氧基和酮酯配体的3-6族金属络合物;可以用于本文描述的方法的合适金属氨基化物前体的例子包括,但不限于,四(二甲基氨基)锆(TDMAZ)、四(二乙基氨基)锆(TDEAZ)、四(乙基甲基氨基)锆(TEMAZ)、四(二甲基氨基)铪(TDMAH)、四(二乙基氨基)铪(TDEAH)和四(乙基甲基氨基)铪(TEMAH)、四(二甲基氨基)钛(TDMAT)、四(二乙基氨基)钛(TDEAT)、四(乙基甲基氨基)钛(TEMAT)、叔丁基亚氨基三(二乙基氨基)钽(TBTDET)、叔丁基亚氨基三(二甲基氨基)钽(TBTDMT)、叔丁基亚氨基三(乙基甲基氨基)钽(TBTEMT)、乙基亚氨基三(二乙基氨基)钽(EITDET)、乙基亚氨基三(二甲基氨基)钽(EITDMT)、乙基亚氨基三(乙基甲基氨基)钽(EITEMT)、叔戊基亚氨基三(二甲基氨基)钽(TAIMAT)、叔戊基亚氨基三(二乙基氨基)钽、五(二甲基氨基)钽、叔戊基亚氨基三(乙基甲基氨基)钽、二(叔丁基亚氨基)二(二甲基氨基)钨(BTBMW)、二(叔丁基亚氨基)二(二乙基氨基)钨、二(叔丁基亚氨基)二(乙基甲基氨基)钨及其组合。可以用于本文公开的方法的合适的有机金属前体的例子包括,但不限于,3族金属环戊二烯基化物或烷基环戊二烯基化物。本文的示例性3-6族金属包括,但不限于,Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Er、Yb、Lu、Ti、Hf、Zr、V、Nb、Ta、Cr、Mo和W。其他挥发性有机金属前体包括,但不限于金属烷基前体例如,但不限于三乙基铝(TEA)、三甲基铝(TEA)。
在某些实施方式中,所述卤代有机氨基硅烷可用于基于液体的沉积或薄膜形成方法,例如但不限于,旋涂、浸涂、气溶胶、喷墨、丝网印刷或喷射涂覆。在其中硅薄膜通过基于液体的沉积形成的实施方式中,复合薄膜由特别地包含作为二氧化硅来源的至少一种含硅前体例如本文所述的具有式I的卤代有机氨基硅烷、催化剂和水的组合物形成。所述组合物还可以包含溶剂和表面活性剂。简言之,将组合物分配在衬底上并蒸发溶剂和水可以形成薄膜。表面活性剂、剩余溶剂和水通常通过使涂覆的衬底与一种或多种能源接触足以生成含硅薄膜的时间来去除。在一些情况下,所述薄膜可预热从而基本上完成二氧化硅源的水解、继续交联过程并从薄膜中驱除任何剩余溶剂(如果存在)。
除了本文描述的具有式I的卤代有机氨基硅烷外,二氧化硅源的另一个实例可以包括在除去成孔材料时产生Si-H键的化合物。
该源的再进一步的实例见于例如参考文献Hay等,“Synthesis ofOrganic-Inorganic Hybrids via the Non-hydrolytic Sol-Gel Process”,Chem.Mater.,13,3396-3403(2001)或Hay等,“A Versatile Route toOrganically-Modified Silicas and Porous Silicas via the Non-HydrolyticSol-Gel Process”,J.Mater.Chem.,10,1811-1818(2000)中描述的非水解化学作用方法中。
二氧化硅源的又另一个实例可以包括胶体二氧化硅、煅制二氧化硅或硅酸起始材料。
二氧化硅源的再其他的实例包括倍半硅氧烷,例如氢倍半硅氧烷(HSQ、HSiO1.5)和甲基倍半硅氧烷(MSQ、RSiO1.5,其中R是甲基)。
在某些实施方式中,可以将二氧化硅源作为水解和缩合产物添加到混合物中。二氧化硅源的水解和缩合通过间歇地或连续地将水和催化剂添加至溶剂并同时添加二氧化硅源,并在通常为-30-100℃、优选20-100℃的温度下搅拌所述混合物0-24小时的同时进行水解和缩合反应而发生。可以调节所述组合物以通过在各制备步骤中进行浓缩或用溶剂稀释来提供希望的固体含量。此外,二氧化硅源可以是水解时产生乙酸的化合物。
二氧化硅源的水解和缩合可以发生在薄膜形成期间的任何一点,即,添加至混合物之前、添加到混合物之后、与至少一种能源接触之前和/或期间等。例如,在某些实施方式中,至少一种二氧化硅源在容器中与溶剂、水和表面活性剂混合,且将催化剂逐渐加入容器中并混合。预期在不脱离本发明精神的情况下可使用多种不同的顺序添加到混合物中。
适于本发明的催化剂包括在存在水的情况下可催化来自二氧化硅源的取代基水解和/或催化两种二氧化硅源的缩合以形成Si-O-Si桥的任何有机或无机酸或碱。催化剂可以是有机碱,例如但不限于季铵盐和氢氧化物,例如铵或四甲铵;胺类,例如伯胺、仲胺和叔胺;和氧化胺。催化剂也可以是酸,例如但不限于硝酸、马来酸、草酸、醋酸、甲酸、乙醇酸、乙醛酸或其混合物。在优选的实施方式中,所述催化剂包括硝酸。
适用于本发明的溶剂可以包括对试剂具有溶解性的任何溶剂。溶剂例如可以是醇溶剂、酮溶剂、酰胺溶剂或酯溶剂。在某些实施方式中,所述溶剂可以是超临界流体,例如二氧化碳、碳氟化合物、六氟化硫、烷烃及其他合适的多组分混合物等。在某些实施方式中,用于本发明的一种或多种溶剂具有相对较低的沸点,即,低于160℃。这些溶剂包括但不限于,四氢呋喃、丙酮、1,4-二噁烷、1,3-二氧戊环、乙酸乙酯和甲基乙基酮。可用于本发明但沸点超过160℃的其他溶剂包括二甲基甲酰胺、二甲基乙酰胺、N-甲基吡咯烷酮、碳酸乙二酯、碳酸丙二酯、甘油及衍生物、萘及取代形式、乙酸酐、丙酸和丙酸酐、二甲基砜、二苯甲酮、二苯砜、苯酚、间甲酚、二甲亚砜、二苯醚、三联苯等。优选的溶剂包括丙二醇丙醚(PGPE)、3-庚醇、2-甲基-1-戊醇、5-甲基-2-己醇、3-己醇、2-庚醇、2-己醇、2,3-二甲基-3-戊醇、丙二醇甲醚醋酸酯(PGMEA)、乙二醇正丁基醚、丙二醇正丁基醚(PGBE)、1-丁氧基-2-丙醇、2-甲基-3-戊醇、乙酸2-甲氧基乙酯、2-丁氧基乙醇、2-乙氧基乙基乙酰醋酸酯、1-戊醇和丙二醇甲醚。进一步的示例性溶剂包括乳酸酯、丙酮酸酯和二醇。进一步的示例性溶剂包括EP1,127,929中所列的那些溶剂。以上列举的溶剂可以单独使用或以两种或更多种溶剂的组合使用。
在某些实施方式中,组合物中的试剂反应从而在衬底上形成冷凝的可流动的薄膜。该薄膜流入缝隙中以用介电材料填充缝隙。然后该薄膜通过一种或多种不同技术转化为固体介电材料,所述技术包括热退火、紫外线(UV)照射、微波照射或暴露于氧化性等离子体。根据某些实施方式,所述薄膜通过包括(但不限于)交联所述前体从而生成固体材料和/或去除氢(--H)、羟基(--OH)或水(H2O)基团的机制转化为固体材料。在特定实施方式中,电感耦合等离子体用于转化该薄膜。
在某些实施方式中,所产生的介电薄膜或涂层可以进行沉积后处理,例如,但不限于,等离子体处理、化学处理、紫外光照射、电子束照射和/或影响薄膜的一种或多种性能的其它处理。
在某些实施方式中,本文描述的介电薄膜具有6或更低的介电常数。在这些实施方式或其它实施方式中,薄膜可以具有大约5或更低的或者大约4或更低的或者大约3.5或更低的介电常数。但是,可以构想的是,可以根据薄膜的预期终端用途形成具有其它介电常数(例如,更高或更低)的薄膜。使用本文描述的有机氨基硅烷前体和方法形成的含硅薄膜或介电薄膜具有式SixOyCzNvHw的一个实施方式中,其中Si的范围为大约10%至大约40%,O的范围为大约0%至大约65%,C的范围为大约0%至大约75%或大约0%至大约50%,N的范围为大约0%至大约75%或大约0%至大约50%,和H的范围为大约0%至大约50%,以上百分比为原子重量百分比,其中x+y+z+v+w=100原子重量百分比,如例如通过XPS或其它方法测定的。然而,具有不同配方的介电或含硅薄膜的其他实施方式可采用本文描述的卤代有机氨基硅烷前体来进行。
如前所述,本文描述的方法可以用于在衬底的至少一部分上沉积含硅薄膜。合适的衬底的例子包括,但不限于,硅、SiO2、Si3N4、OSG、FSG、碳化硅、氢化碳化硅、氮化硅、氢化氮化硅、碳氮化硅、氢化碳氮化硅、氮化硼(boronitride)、抗反射涂层、光致抗蚀剂、有机聚合物、多孔有机和无机材料、金属(如铜和铝)及扩散屏障层(例如,但不限于,TiN、Ti(C)N、TaN、Ta(C)N、Ta、W或WN)。薄膜与多种后续的处理步骤相容,例如,举例来说,化学机械抛光(CMP)和各向异性蚀刻处理。
沉积的薄膜具有包括,但不限于,计算机芯片、光学器件、磁信息存储、支撑材料或衬底上的涂层、微型机电系统(MEMS)、纳米机电系统、薄膜晶体管(TFT)和液晶显示器(LCD)的应用。
在权利要求中,字母用于标识所要求保护的步骤(例如(a)、(b)和(c))。这些字母用于帮助指称方法步骤,而不意图指示所要求保护的步骤执行的次序,除非且仅达到这种次序在权利要求中具体叙述的程度。
以下实施例举例说明了本文描述的制备卤代有机氨基硅烷前体的方法以及本文描述的沉积的含硅薄膜的方法,且不意图以任何方式限制本发明。
实施例
实施例1:合成2,6-二甲基哌啶子基氯硅烷
在2000ml配备有机械搅拌器和加料漏斗的3颈圆底烧瓶中添加1000ml己烷。采用干冰IPA冷浴将烧瓶冷却到-20℃,101g(1.0mol)二氯硅烷被冷凝并溶于己烷中。在搅拌下将113g(1.0mol)2,6-二甲基哌啶和111g(1.1mol)三乙胺的混合物滴加到烧瓶中。添加完成后,在-20℃搅拌反应混合物1小时,然后升温到室温。通过在手套袋中真空过滤去除HCl·Et3N的盐副产物沉淀,用N2吹扫以防止产物与空气中的水分反应。对滤液的GC/MS分析确认了产物2,6-二甲基哌啶子基氯硅烷,显示产物的分子离子质量为177以及M-CH3支持质量片段的质量为162。溶剂己烷通过蒸馏去除,且产物通过真空蒸馏分离。10torr下的沸点为60℃,收率为66%。
实施例2:2,6-二甲基哌啶子基氯硅烷的替代合成路线
-78℃下向7.55g(66.68mmol)顺式-2,6-二甲基哌啶于50mL THF中的溶液滴加28.00mL(70.02mmol)的正丁基锂的2.5M己烷溶液。析出沉淀并在搅拌下将反应混合物升温至室温。一小时后,在-40℃下将该混合物滴加至6.74g(66.68mmol)二氯硅烷于30mL二甲苯和70mL己烷的溶液中,并形成浅灰色沉淀。将反应混合物搅拌16小时,之后将其从析出的固体中倾析并在环境压力下进行蒸馏以去除挥发性物质。分离了3.16g所需产物,收率为27%。产物经GC/MS分析证实为2,6-二甲基哌啶子基氯硅烷。
实施例3:合成2,6-二甲基哌啶子基二氯硅烷
2,6-二甲基哌啶子基二氯硅烷的合成通过在70重量%的己烷溶液中以1份2,6-二甲基哌啶∶1份三乙胺∶1.1份三氯硅烷的摩尔比混合来制备。需要过量的三氯硅烷以防止双(2,6-二甲基哌啶子基)氯硅烷的形成。通过在手套袋中真空过滤去除HCl·Et3N盐副产物沉淀,用N2吹扫以防止产物与空气中的水分反应。对滤液的GC/MS分析(显示于图1中)确认生成了产物2,6-二甲基哌啶子基二氯硅烷,显示质量为211以及-CH3的支持质量片段质量为196。真空过滤后,总己烷量通过第一步骤中的简单蒸馏去除。第二步骤采用真空蒸馏技术,其中收集产物。由真空蒸馏测定18torr下的沸点为93℃,在5torr下的沸点为66℃,产率为64%。
实施例4:含硅薄膜的原子层沉积
使用以下前体:2,6-二甲基哌啶子基氯硅烷进行含硅薄膜的原子层沉积。在实验室规模的ALD处理设备上进行沉积。所有气体(例如,吹扫和反应气体或前体和氧源)预热到100℃,然后进入沉积区。气体和前体流速用具有高速致动的ALD隔膜阀控制。用于沉积的衬底是12英寸长的硅带,使热电偶附着在样品支架上以确认衬底温度。采用臭氧作为氧源气体进行沉积,且沉积的工艺参数提供于表II中:
表II:用臭氧进行含硅薄膜的原子层沉积的工艺
重复步骤b)到e)直到达到希望的厚度。表征所产生的含硅薄膜的沉积速率和折射率。通过将来自薄膜的反射数据与预设的物理模型(例如Lorentz Oscillator模型)拟合,使用FilmTek 2000SE椭率计测量薄膜的厚度和折射率。薄膜组成用X-射线光电子光谱(XPS)技术来分析。在配备有多通道板(MCD)和聚焦的Al单色X-射线源的PHI 5000VersaProbe分光计上进行X-射线光电子光谱实验。薄膜组成在薄膜中处测量以去除偶然的碳信号。测量的薄膜组成省略了氢(因为其不能用XPS检测到),并归一化至100%。
在所有样品上进行X-射线反射计测量(XRR)以确定薄膜密度。在0.2≤2≤0.65范围内采用0.001的步长和1s/步的计数时间来扫描样品。采用两层模型分析数据,其中将衬底定义为Si以及将薄膜定义为氧化硅。
如表III中总结的,以一秒的前体加料,采用2,6-二甲基哌啶子基氯硅烷在150-300℃的各种不同衬底温度下形成氧化硅薄膜:
表III:2,6-二甲基哌啶子基氯硅烷的工艺参数和结果的总结
如表IV中总结的,以可变的前体加料,采用2,6-二甲基哌啶子基氯硅烷在300℃的衬底温度下形成氧化硅薄膜:
表IV:2,6-二甲基哌啶子基氯硅烷的工艺参数和结果总结
氧化硅沉积显示随着前体加料增加的沉积速率饱和,表明类似于自限的原子层沉积(ALD)样行为。如通过X射线光电子光谱法(XPS)测定的,沉积薄膜具有33at.%的Si和67at.%的O。没有在薄膜中检测到碳、氮和氯。薄膜密度为1.9±0.05g/cc。
Claims (31)
1.由下式I表示的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n - p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环。
2.如权利要求1的卤代有机氨基硅烷前体,其中R1和R2相同。
3.如权利要求1的卤代有机氨基硅烷前体,其中R1和R2不同。
4.通过沉积工艺在衬底的至少一个表面上形成介电薄膜的方法,所述沉积工艺选自化学气相沉积工艺和原子层沉积工艺,该方法包括:
在反应室中提供所述衬底的该至少一个表面;
引入至少一种具有下式I的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环;
将含氮源引入反应器中,其中所述至少一种有机氨基硅烷前体和所述含氮源反应以在该至少一个表面上获得所述的介电薄膜。
5.如权利要求4的方法,其中所述至少一种有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
6.如权利要求4或5的方法,其中所述含氮源选自氨、肼、单烷基肼、二烷基肼、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。
7.如权利要求4-6任一项的方法,其中所述介电薄膜选自氮化硅和碳氮化硅。
8.通过原子层沉积(ALD)工艺形成介电薄膜的方法,该方法包括以下步骤:
a.在ALD反应器中提供衬底;
b.在所述ALD反应器中提供至少一种具有下式I的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
c.用惰性气体吹扫所述ALD反应器;
d.在所述ALD反应器中提供含氮源;
e.用惰性气体吹扫所述ALD反应器;和
重复步骤b至e直到获得希望的介电薄膜厚度。
9.如权利要求8的方法,其中所述至少一种卤代有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
10.如权利要求8或9的方法,其中所述含氮源选自氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。
11.如权利要求8-10中任一项的方法,其中所述介电薄膜选自氮化硅和碳氮化硅。
12.使用等离子体增强原子层沉积(PEALD)工艺在衬底的至少一个表面上形成介电薄膜的方法,该方法包括:
a.在ALD反应器中提供衬底;
b.在所述ALD反应器中提供至少一种具有下式I的卤代有机氨基硅烷前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
c.用惰性气体吹扫所述ALD反应器;
d.在所述ALD反应器中提供等离子体含氮源;
e.用惰性气体吹扫所述ALD反应器;和
重复步骤b至e直到获得希望的介电薄膜厚度。
13.如权利要求12的方法,其中所述至少一种卤代有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
14.如权利要求12或13的方法,其中所述含氮源选自氨、肼、单烷基肼、二烷基肼、氮、氮/氢、氨等离子体、氮等离子体、氮/氢等离子体及其混合物。
15.如权利要求12-14中任一项的方法,其中所述介电薄膜选自氮化硅和碳氮化硅。
16.在衬底上形成氧化硅薄膜的方法,包括:
在气相沉积工艺中使氧化剂与包含下式I表示的卤代有机氨基硅烷的前体反应以在所述衬底上形成氧化硅薄膜:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环。
17.如权利要求16的方法,其中所述气相沉积为选自化学气相沉积、低压气相沉积、等离子体增强化学气相沉积、循环化学气相沉积、等离子体增强循环化学气相沉积、原子层沉积和等离子体增强原子层沉积中的至少一种。
18.如权利要求16或17的方法,其中所述至少一种卤代有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
19.用于在衬底上形成氧化硅薄膜的方法,包括:
通过气相沉积由包含至少一种具有下式I的有机氨基硅烷前体和至少一种氧化剂的组合物在所述衬底上形成氧化硅薄膜:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环,
其中所述气相沉积为选自化学气相沉积、低压气相沉积、等离子体增强化学气相沉积、循环化学气相沉积、等离子体增强循环化学气相沉积、原子层沉积和等离子体增强原子层沉积中的至少一种。
20.如权利要求19的方法,其中所述至少一种卤代有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
21.用于在衬底上形成氧化硅薄膜的方法,包括:
向反应器中引入由下式I表示的卤代有机氨基硅烷:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;
向反应器中引入至少一种氧化剂,其中,该至少一种氧化剂与所述有机氨基硅烷反应以在所述衬底上提供氧化硅薄膜。
22.用于在衬底上形成具有一定厚度的氧化硅薄膜的方法,该方法包括:
a.向沉积室中引入至少一种由下式I表示的卤代有机氨基硅烷:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环;
b.化学吸附所述至少一种卤代有机氨基硅烷前体到所述衬底上;
c.使用吹扫气体吹扫掉未反应的所述至少一种卤代有机氨基硅烷前体;
d.向加热的衬底上的卤代有机氨基硅烷前体提供氧源以与所吸附的至少一种卤代有机氨基硅烷前体反应;和
e.任选地吹扫掉任何未反应的氧源。
23.根据权利要求22所述的方法,其中重复步骤a至d和任选的步骤e,直到达到所述的薄膜厚度。
24.如权利要求22或23的方法,其中所述至少一种有机氨基硅烷前体选自2,6-二甲基哌啶子基二氯硅烷、2,6-二甲基哌啶子基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷和环己基异丙基氨基氯硅烷,优选包括2,6-二甲基哌啶子基二氯硅烷和/或2,6-二甲基哌啶子基氯硅烷。
25.如权利要求22-24中任一项的方法,其是原子层沉积方法或等离子体增强循环化学气相沉积方法。
26.用于输送用于沉积含硅薄膜的前体的容器,该容器包含:
由下式I表示的前体:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环;和
其中所述前体的纯度为大约98%或更高。
27.如权利要求26的容器,其中所述容器由不锈钢构成。
28.卤代有机氨基硅烷前体,选自2,6-二甲基哌啶子基氯硅烷、2,6-二甲基哌啶子基二氯硅烷、二环己基氨基氯硅烷、环己基甲基氨基氯硅烷、环己基乙基氨基氯硅烷、环己基异丙基氨基氯硅烷、N-(氯甲硅烷基)十氢喹啉、苯基烯丙基氨基氯硅烷、间甲苯基甲基氨基氯硅烷、N-(氯甲硅烷基)咔唑、N-(氯甲硅烷基)-四氢喹啉、N-(氯甲硅烷基)吲哚、N-(氯甲硅烷基)-2-甲基吲哚、N-(氯甲硅烷基)-3-甲基吲哚和N-(氯甲硅烷基)-1,2,3,4-四氢-2-甲基喹啉。
29.具有下式的卤代有机氨基硅烷前体:
ClH2Si(NR2R3)
其中R2选自直链或支链C3-C10烷基和C6-C10芳基,和R3是支链C3-C10烷基或C6-C10芳基,且其中R2和R3可以形成环或烷基取代的环。
30.具有下式的卤代有机氨基硅烷前体:
R1ClHSi(NR2R3)
其中R1是C1-C10烷基,且R2和R3是直链或支链C3-C10烷基或C4-C10芳基,其中R2和R3可以形成环或烷基取代的环。
31.用于沉积介电薄膜的组合物,包含:
XmR1 nHpSi(NR2R3)4-m-n-p I
其中X是选自Cl、Br、I的卤素;R1独立地选自直链或支链C1-C10烷基、C2-C12烯基、C2-C12炔基、C4-C10环烷基和C6-C10芳基;R2选自直链或支链C1-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;R3选自支链C3-C10烷基、C3-C12烯基、C3-C12炔基、C4-C10环烷基和C6-C10芳基;m是1或2;n是0、1或2;p是0、1或2;且(m+n+p)的和小于4,且其中R2和R3连接以形成环或R2和R3不连接形成环;和
选自醚、叔胺、腈、烷基烃、芳族烃、叔氨基醚或其混合物的溶剂。
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JP5658214B2 (ja) | 2015-01-21 |
EP2574611B1 (en) | 2016-03-23 |
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JP6100743B2 (ja) | 2017-03-22 |
EP2574611A1 (en) | 2013-04-03 |
CN107312028B (zh) | 2023-04-14 |
JP6310018B2 (ja) | 2018-04-11 |
KR20130034001A (ko) | 2013-04-04 |
US20130078392A1 (en) | 2013-03-28 |
JP2015026849A (ja) | 2015-02-05 |
KR101506940B1 (ko) | 2015-03-31 |
TWI437005B (zh) | 2014-05-11 |
CN103012457B (zh) | 2018-02-09 |
CN107857774A (zh) | 2018-03-30 |
CN107312028A (zh) | 2017-11-03 |
TW201319077A (zh) | 2013-05-16 |
US8993072B2 (en) | 2015-03-31 |
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