TW201346056A - 由金屬脒鹽前驅物製造介電膜的方法 - Google Patents
由金屬脒鹽前驅物製造介電膜的方法 Download PDFInfo
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- TW201346056A TW201346056A TW102114224A TW102114224A TW201346056A TW 201346056 A TW201346056 A TW 201346056A TW 102114224 A TW102114224 A TW 102114224A TW 102114224 A TW102114224 A TW 102114224A TW 201346056 A TW201346056 A TW 201346056A
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- 239000002243 precursor Substances 0.000 title claims abstract description 182
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 121
- 239000002184 metal Substances 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 79
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 68
- 229910003455 mixed metal oxide Inorganic materials 0.000 claims abstract description 48
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 38
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 17
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 16
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 13
- 230000015654 memory Effects 0.000 claims abstract description 11
- 239000003990 capacitor Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims description 67
- -1 alkyl decylamine Chemical compound 0.000 claims description 63
- 238000000151 deposition Methods 0.000 claims description 48
- 239000003446 ligand Substances 0.000 claims description 41
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 34
- 230000008021 deposition Effects 0.000 claims description 31
- 150000004714 phosphonium salts Chemical class 0.000 claims description 30
- 239000007800 oxidant agent Substances 0.000 claims description 29
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 21
- 230000001590 oxidative effect Effects 0.000 claims description 21
- 150000000703 Cerium Chemical class 0.000 claims description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 14
- 229910052707 ruthenium Inorganic materials 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 claims description 12
- 150000004703 alkoxides Chemical class 0.000 claims description 12
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 12
- 150000004820 halides Chemical class 0.000 claims description 12
- 150000004678 hydrides Chemical class 0.000 claims description 12
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 12
- 125000003342 alkenyl group Chemical group 0.000 claims description 11
- 125000000217 alkyl group Chemical group 0.000 claims description 11
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 125000000304 alkynyl group Chemical group 0.000 claims description 10
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- 125000004209 (C1-C8) alkyl group Chemical group 0.000 claims description 7
- 229910044991 metal oxide Inorganic materials 0.000 claims description 7
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- 125000004649 C2-C8 alkynyl group Chemical group 0.000 claims description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- 229930194542 Keto Natural products 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 6
- 150000001735 carboxylic acids Chemical class 0.000 claims description 6
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 6
- 125000000468 ketone group Chemical group 0.000 claims description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 150000002823 nitrates Chemical class 0.000 claims description 3
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- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 2
- 229910001482 mixed metal silicate Inorganic materials 0.000 claims 2
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- 239000012528 membrane Substances 0.000 claims 1
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- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 claims 1
- 229910052723 transition metal Inorganic materials 0.000 abstract description 21
- 150000003624 transition metals Chemical class 0.000 abstract description 21
- 238000000231 atomic layer deposition Methods 0.000 abstract description 18
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- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 79
- 239000000376 reactant Substances 0.000 description 50
- 230000008569 process Effects 0.000 description 29
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 238000000746 purification Methods 0.000 description 13
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- 229910002651 NO3 Inorganic materials 0.000 description 3
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- 230000015572 biosynthetic process Effects 0.000 description 3
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- 229910052754 neon Inorganic materials 0.000 description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 241000894007 species Species 0.000 description 3
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- 230000005641 tunneling Effects 0.000 description 3
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 2
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- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 2
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- 229920002098 polyfluorene Polymers 0.000 description 2
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- TVSBRLGQVHJIKT-UHFFFAOYSA-N propan-2-ylcyclopentane Chemical compound CC(C)C1CCCC1 TVSBRLGQVHJIKT-UHFFFAOYSA-N 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
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- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 1
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(iv) oxide Chemical compound O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
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- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910000311 lanthanide oxide Inorganic materials 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002052 molecular layer Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
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- 238000004151 rapid thermal annealing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000012713 reactive precursor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 159000000008 strontium salts Chemical class 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 239000006200 vaporizer Substances 0.000 description 1
Classifications
-
- 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
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
-
- 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
-
- 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
- C23C16/45531—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 specially adapted for making ternary or higher compositions
-
- 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
- H01L21/02172—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 at least one metal element, e.g. metal oxides, metal nitrides, metal oxynitrides or metal carbides
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Abstract
本案描述用於使用金屬脒鹽前驅物原子層沉積包含混合金屬氧化物之膜的方法。混合金屬氧化物膜可包含鑭系元素及諸如鉿、鋯及/或鈦之過渡金屬。此等混合金屬氧化物膜可用作以下各者中之介電層:電容器、電晶體、動態隨機存取記憶體單元、電阻式隨機存取記憶體單元、快閃記憶體單元及顯示面板。
Description
本發明之實施例大體而言係關於半導體製造製程及元件的領域,特定言之係關於沉積介電膜之方法及此等膜在電子元件中之使用。
微電子元件係製造於半導體基板上作為積體電路,其中各種導電層彼此互連以允許電子訊號在元件內傳播。此元件之實例為互補金氧半導體(complementary metal-oxide-semiconductor;CMOS)場效電晶體(field effect transistor;FET)或金氧半導體場效電晶體(metal-oxide-semiconductor field effect transistor;MOSFET)。
在過去的幾十年中,MOSFET已不斷按比例縮小尺寸且現代積體電路正併入具有小於0.1微米之通道長度的MOSFET。特徵尺寸之減少已導致某些挑戰,因為小的MOSFET與較大元件相比顯示較高的洩漏電流及較低輸出電阻。然而,較小的MOSFET由於若干原因是為人們所需要的。使電晶體更小之主要原因在於在給定晶片面積內填充越來越多元件,以降低每晶片之價格。另外,電晶體尺寸之縮減可
幫助增加速度。
因為小MOSFET幾何形狀的原因,必須降低可施加至閘極的電壓以維持可靠性。為維持效能,MOSFET之臨限電壓亦必須降低。當臨限電壓降低時,電晶體無法以可用之有限電壓擺動由完全斷開切換至完全接通。在過去忽略之次臨限值洩漏現在可對元件效能具有顯著影響。
閘極電極為積體電路之部分。舉例而言,CMOS電晶體包含安置在源極區與汲極區之間的閘極結構,該源極區及汲極區係形成在半導體基板中。閘極結構通常包含閘極電極及閘極介電質。閘極電極係安置在閘極介電質上方以控制載荷子在通道區內之流動,該通道區係形成在位於閘極介電質下方之汲極區與源極區之間。閘極介電質通常包含薄材料層(例如,諸如二氧化矽(SiO2)、氮氧化矽(SiON)及類似物之閘極氧化物),該薄材料層具有約4.0或更大的介電常數。當將矽CMOS元件之閘極長度定標為小於100nm時,新的高介電常數(K)材料將很可能取代氧化矽。另外,金屬閘極將很可能取代多晶矽(聚矽)閘極。舉例而言,在一些CMOS電晶體中,閘極電極可由以下之至少一者形成:金屬(例如,鈦(Ti)、鉭(Ta)、鎢(W)及類似物)及含金屬之導電化合物(例如,氮化鈦(TiN)、氮化鉭(TaN)、氮化鎢(WN)及類似物)。以金屬及含金屬之化合物取代作為閘極電極之傳統材料的聚矽降低了與聚矽空乏效應相關聯之非期望電壓降,以及增加CMOS電晶體之驅動電流效能及操作速度。
充當介於閘極與通道之間的絕緣體的閘極氧化物應
儘可能薄地製造,以在電晶體接通時增加通道導電性及效能且在電晶體斷開時降低次臨限值洩漏。然而,在具有約1.2nm厚度之當前閘極氧化物的情況下,電子穿隧之量子機械現象發生在閘極與通道之間,從而導致增加的功率消耗。
具有大於二氧化矽之介電常數的諸如二氧化鉿(HfO2)之高k介電質正被用來降低閘極洩漏。增加閘極介電質之介電常數允許較厚層,同時維持高電容。通常,較高的介電厚度降低通過介於閘極與通道之間的介電質的量子穿隧電流。然而,半導體與介電質在導電帶能方面的差異(及在價帶能量方面的相應差異)影響洩漏電流位準。對於傳統的閘極氧化物,二氧化矽,前阻障層為近似8eV。對於許多替代介電質,該值顯著較低,如此傾向於增加穿隧電流,而稍微否定較高介電常數之優點。
如上所述,已提出用作閘極介電材料之替代材料。儘管已藉由使用替代閘極金屬及閘極介電材料對半導體閘極電極進行改良,但期望進一步改良來改良積體電路元件之效能,例如以降低洩漏電流密度。
因此,在此技術領域中存在對於快速且有效地沉積介電膜之方法的持續需要。
本發明之一態樣係關於沉積膜之方法,該方法包含以下步驟:將基板之表面順序地暴露至第一金屬前驅物及氧化劑之交替脈衝以提供第一金屬氧化物膜;及將第一金屬氧化物膜順序地暴露至氧化劑及第二金屬前驅物之交替脈衝以
提供包含第一金屬及第二金屬之混合金屬氧化物之膜。在此態樣之實施例中,第一金屬為一或多個過渡金屬,諸如Hf、Zr或Ti。第二金屬前驅物可為鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物。根據一或多個實施例,鑭系元素為鈰。
第一金屬前驅物亦可為脒鹽前驅物或胍鹽前驅物,諸如具有化學式M1Ln之一者,其中M1係選自Hf、Zr及Ti,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至4的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物可具有藉由以下結構式表示之結構:
其中M2為鑭系元素,R、R'及R"每一者獨立地為氫、C1-8烷基、芳基、醯基、醛基、酮基、C2-4烯基、炔基、氮氣、氨基或CF3,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、
環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至3的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
根據一或多個實施例,包含混合金屬氧化物之膜為混合金屬氧化物膜、混合金屬氮氧化物膜、混合金屬矽酸鹽膜或氮化之混合金屬矽酸鹽膜。
基於在膜中之鑭系元素及過渡金屬的總莫耳,包含混合金屬氧化物之膜可包含1莫耳百分比至30莫耳百分比之鑭系元素。在一些實施例中,鑭系元素為鈰且過渡金屬為鉿。
氧化劑可包含以下各物質中之一或多者:H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、乙醇、羧酸、CO、CO2及HCOH。
在一些實施例中,包含混合金屬氧化物膜之膜可在沉積之後退火。
本發明之另一態樣係關於沉積膜之方法,該方法包含以下步驟:將基板之表面順序地暴露至氧化劑及前驅物混合物之交替脈衝以提供包含第一金屬及第二金屬之混合金屬氧化物的膜,該前驅物混合物包含第一金屬前驅物及第二金屬前驅物。在此態樣之實施例中,第一金屬為一或多個過渡金屬,諸如Hf、Zr或Ti。第二金屬前驅物可為鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物。根據一或多個實施例,鑭系元素為鈰。
第一金屬前驅物亦可為脒鹽前驅物或胍鹽前驅物,
諸如具有化學式M1Ln之一者,其中M1係選自Hf、Zr及Ti,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至4的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物可具有藉由以下結構式表示之結構:
其中M2為鑭系元素,R、R'及R"每一者獨立為氫、C1-8烷基、芳基、醯基、醛基、酮基、C2-4烯基、炔基、氮氣、氨基或CF3,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至3的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
根據此態樣之一或多個實施例,包含混合金屬氧化
物之膜為混合金屬氧化物膜、混合金屬氮氧化物膜、混合金屬矽酸鹽膜或氮化之混合金屬矽酸鹽膜。
第一金屬前驅物及第二金屬前驅物可在將第一金屬前驅物及第二金屬前驅物引入沉積腔室內之前混合,或前驅物可位於腔室本身中。在一些實施例中,第一金屬前驅物及第二金屬前驅物在前驅物混合物中之莫耳比係在自100:1至2:1之範圍內。
氧化劑可包含以下物質中之一或多者:H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、乙醇、羧酸、CO、CO2及HCOH。
本發明之又一態樣係關於沉積包含混合金屬氧化物之膜的方法,該方法包含以下步驟:控制第一金屬前驅物及第二金屬前驅物之流動以提供前驅物混合物;將基板之表面暴露至前驅物混合物;及將基板之表面暴露至氧化劑以提供包含第一金屬及第二金屬之混合金屬氧化物的膜。
在此態樣之實施例中,第一金屬為一或多個過渡金屬,諸如Hf、Zr或Ti。第二金屬前驅物可為鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物。根據一或多個實施例,鑭系元素為鈰。
第一金屬前驅物亦可為脒鹽前驅物或胍鹽前驅物,諸如具有化學式M1Ln之一者,其中M1係選自Hf、Zr及Ti,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒
鹽及胍鹽,n為自1至4的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物可具有藉由以下結構式表示之結構:
其中M2為鑭系元素,R、R'及R"每一者獨立為氫、C1-8烷基、芳基、醯基、醛基、酮基、C2-4烯基、炔基、氮氣、氨基或CF3,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至3的數字,且其中每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,一或多個L為另一脒鹽或胍鹽配位體。
根據此態樣之一或多個實施例,包含混合金屬氧化物之膜為混合金屬氧化物膜、混合金屬氮氧化物膜、混合金屬矽酸鹽膜或氮化之混合金屬矽酸鹽膜。
在一或多個實施例中,第一金屬前驅物及第二金屬前驅物之流動係經控制以基於在膜中之鑭系元素及第一金屬
的總莫耳而提供包含1莫耳百分比至30莫耳百分比之鑭系元素之混合金屬氧化物膜。
另一態樣係關於含有介電層之電子元件,該介電層包含根據本文描述之任何方法沉積之混合金屬氧化物膜。介電層可與導電層連通。在一些實施例中,電子元件可為電容器、電晶體、動態隨機存取記憶體單元、電阻式隨機存取記憶體單元、快閃記憶體單元或顯示面板。
前述內容已相當廣泛地概述了本發明之某些特徵及技術優勢。熟習此項技術者應瞭解,揭示之特定實施例可容易用作在本發明範疇內修改或設計其他結構或製程的基礎。熟習此項技術者亦應認識到,此等等效構造不脫離如在隨附申請專利範圍中所闡述之本發明之精神及範疇。
如本文所使用之「基板」係指任何基板或形成於基板上之材料表面,膜處理係在製造過程期間於該基板或材料表面上執行。舉例而言,取決於應用,可在其上執行處理之該基板表面包括各種材料,該等材料諸如矽、氧化矽、應變矽、絕緣層上矽(silicon on insulator;SOI)、碳摻雜氧化矽、氮化矽、摻雜矽、鍺、砷化鎵、玻璃、藍寶石,及任何其他材料,該任何其他材料諸如金屬、金屬氮化物、金屬合金及其他導電材料。基板包括且不限於半導體晶圓。可將基板暴露於預處理製程以研磨、蝕刻、還原、氧化、羥基化、退火
及/或烘烤基板表面。除直接在基板本身之表面上的膜處理之外,本發明中揭示之任何膜處理步驟亦可在如下文更詳細揭示的形成於基板上之下層上執行,且術語「基板表面」意欲包括如上下文指示之此下層。
根據本發明之各種實施例,提供了與沉積包含混合金屬氧化物之膜有關的方法。混合金屬氧化物膜包含鑭系元素及諸如鉿、鋯及/或鈦之過渡金屬。在一或多個實施例中,鑭系元素為鈰。一些實施例中,過渡金屬為鉿。
該等混合金屬氧化物可用作電晶體中之閘極介電質,或用作電容器、動態隨機存取記憶體單元、電阻式隨機存取記憶體單元、快閃記憶體單元及顯示面板中之介電質。
當前發明之一態樣提供藉由使用鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物沉積包含混合金屬氧化物之膜的方法。在此態樣之實施例中,該方法包含以下步驟:將基板之表面順序地暴露至第一金屬前驅物及氧化劑之交替脈衝以在基板表面上提供第一金屬氧化物膜;及將第一金屬氧化物膜順序地暴露至氧化劑及鑭系元素前驅物之交替脈衝。鑭系元素前驅物可為具有以下結構之鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物:
其中M2為鑭系元素,且R、R'及R"每一者獨立為氫、C1-8烷基、芳基、醯基、醛基、酮基、C2-4烯基、炔基、氮氣、氨基或CF3。Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至3的數字,且每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,每一L為相同的脒鹽配位體或胍鹽配位體以使得金屬錯合物為均配物。在其他實施例中,至少L與脒鹽配位體或胍鹽配位體不相同,且金屬錯合物為雜配物。根據一或多個實施例,鑭系元素包含鈰。
第一金屬可為過渡金屬,且在一些實施例中,第一金屬為鉿、鋯及鈦中之一或多者。類似鑭系元素前驅物,第一金屬前驅物亦可為脒鹽前驅物或胍鹽前驅物。在一些實施例中,第一金屬前驅物具有藉由M1Ln表示之化學式,其中M1係選自Hf、Zr及Ti,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、
鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至4的數字,且每一L獨立地為與另一L相同或不同的配位體。在一些實施例中,每一L為相同的脒鹽配位體或胍鹽配位體以使得金屬錯合物為均配物。在其他實施例中,至少L與脒鹽配位體或胍鹽配位體不相同,且金屬複合物為雜配物。根據一或多個實施例,過渡金屬包含鉿。
金屬脒鹽前驅物及金屬胍鹽前驅物可藉由鹽複分解反應製備,在該等鹽複分解反應中,金屬鹵化物係與脒或胍之相應鋰鹽反應。
用於過渡金屬氧化物及鑭系元素氧化物之氧化劑可為相同或不同。合適的氧化劑包括但不限於H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、乙醇、羧酸、CO、CO2及HCOH。為幫助滿足對於閘極介電質之遠低於1nm之等效氧化物厚度(equivalent oxide thickness;EOT)定標之嚴格要求,一些實施例中使用較不強的氧化劑。因此,在一些實施例中,氧化劑包含水。
包含混合金屬氧化物之膜可為含有過渡金屬、鑭系元素及氧之任何膜。在一些實施例中,包含混合金屬氧化物之膜可為混合金屬氧化物膜、混合金屬氮氧化物膜、混合金屬矽酸鹽膜或氮化之混合金屬矽酸鹽膜。
鑭系元素脒鹽及胍鹽前驅物可提供優於其他鑭系元素前驅物之許多優點。在本發明之前,缺乏可用之水反應化學,該等有效水反應化學在含鑭系元素之膜中留下低碳殘留物。同樣地,其他熟知的含鈰化合物,諸如四(2,2,6,6-四甲
基-3,5-己二酮)鈰(Ce(thd)4)及三(異丙基-環戊二烯基)鈰(Ce(iPrCp)3),具有低蒸氣壓力且需要大量加熱以提供待用於原子層沉積(ALD)或化學氣相沉積(CVD)處理中之化學品之充分蒸氣壓力。此加熱傾向於使前驅物過早分解,且因此致使該等源不適合於ALD或CVD處理。此外,與使用其他前驅物沉積之介電膜相比,使用鑭系元素脒鹽前驅物及胍鹽前驅物沉積之介電膜可具有降低之洩漏電流密度。舉例而言,與使用鈰之1-甲氧基-2-甲基-2-丙醇鹽(mmp)前驅物沉積之HfCeOx膜相比,使用鈰脒鹽前驅物沉積之HfCeOx膜顯示在電流密度上減少了10倍至60倍。
在一個實施例中,膜係使用原子層沉積(ALD)製程沉積。在ALD製程之示例性實施例中,將例如過渡金屬前驅物之第一化學前驅物(「A」)在第一半反應中脈衝輸送至基板表面。選擇第一化學前驅物「A」,以便該第一化學前驅物「A」與合適的下層物種(例如表面上之OH或NH官能基)反應以形成新的自飽和表面。然而,對於某些反應物而言,不一定需要表面官能基。過量的未使用反應物及反應副產物係通常藉由抽空泵及/或藉由流動惰性淨化氣體移除。隨後將例如氧化劑之共反應物「B」輸送至表面,其中第一半反應之先前反應的終止取代基或配位體係與來自「B」共反應物之新的配位體或取代基反應,如此生成交換副產物。「B」共反應物亦與下層反應物種形成自飽和鍵結以提供另一自限制及飽和的第二半反應。第二淨化時段係通常用於移除未使用反應物及反應副產物。
可隨後再次流動「A」前驅物、「B」共反應物及淨化氣體。持續交替暴露表面至反應物「A」及反應物「B」,直至達到期望厚度之膜為止。為併入第二金屬(亦即,鑭系元素),流動諸如鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物之第三化學前驅物「C」。隨後將例如氧化劑之共反應物「D」輸送至表面。「D」反應物可為與「B」反應物相同的氧化劑或「D」反應物可為不同的氧化劑。用於「A」氣體、「B」氣體、「C」氣體及「D」氣體之脈衝順序可取決於膜之期望組成而不同。將為A-B-C-D-A-B-C-D之一個示例性順序將會提供過渡金屬與鑭系元素之莫耳比為1:1的膜。其他示例性順序可為A-B-A-B-C-D-A-B、A-B-A-B-A-B-C-D-A-B等。
在一或多個實施例中,鑭系元素比係經選擇以增強K值或減少介電洩漏。鑭系元素比為鑭系元素之莫耳與鑭系元素及過渡金屬之莫耳總和的比率。一些實施例中,基於鑭系元素及過渡金屬之總莫耳,鑭系元素比為0.01至0.3,亦即,包含混合金屬氧化物之膜含有1%至30%的鑭系元素。
應理解,「A」氣體、「B」氣體、「C」氣體、「D」氣體及淨化氣體可同時流動,且基板及/或氣流噴嘴可振動以使得將基板如所期望地順序地暴露至A氣體、B氣體、C氣體、D氣體及淨化氣體。
前驅物及/或反應物可處於氣體、電漿、蒸汽的狀態或對氣相沉積製程有用之其他物質狀態。在淨化期間,通常將惰性氣體引入處理腔室內以淨化反應區,或以其他方式自反應區移除任何殘留反應化合物或副產物。或者,淨化氣體
可在整個沉積製程中連續地流動,以便僅淨化氣體在介於前驅物脈衝與共反應物脈衝之間的時間延遲期間流動。
因此,在一或多個實施例中,「A」前驅物及「B」共反應物之交替脈衝或流動可用以例如在脈衝化之前驅物及共反應物之多個循環之脈衝化輸送中沉積膜,例如,A脈衝、B共反應物脈衝、A前驅物脈衝、B共反應物脈衝、A前驅物脈衝、B共反應物脈衝、A前驅物脈衝、B共反應物脈衝。如上所說明,代替脈衝輸送反應物,氣體可自氣體輸送頭或噴嘴同時流動及/或可移動基板及/或氣體輸送頭以使得基板順序地暴露至氣體。
固然,上述ALD循環僅為多種ALD製程循環之示例性製程循環,在該等製程循環中,沉積層係藉由前驅物及共反應物的交替層而形成。儘管對作為過渡金屬前驅物之「A」反應物進行特定參考,但ALD循環中之第一反應物可為氧化劑或鑭系元素前驅物。
如本文所使用之沉積氣體或製程氣體係指單一氣體、多種氣體、含電漿之氣體、一或多種氣體及/或電漿之組合。沉積氣體可含有用於氣相沉積製程之至少一個反應化合物。反應化合物可在氣相沉積製程期間處於氣體、電漿、蒸汽的狀態。同樣地,製程可含有淨化氣體或載氣且不含有反應化合物。
根據本發明之各種實施例的膜可沉積在幾乎任何基板材料之上。當本文描述之ALD製程為低溫時,將該等製程用於熱不穩定之基板係尤其有利的。如本文所使用之「基板
表面」係指任何基板或形成於基板上之材料表面,膜處理係在製造過程期間於該基板或材料表面上執行。舉例而言,取決於應用,可在其上執行處理之該基板表面包括各種材料,該等材料諸如矽、氧化矽、應變矽、絕緣層上矽(SOI)、碳摻雜氧化矽、氮化矽、摻雜矽、鍺、砷化鎵、玻璃、藍寶石及任何其他材料,該任何其他材料諸如金屬、金屬氮化物、金屬合金及其他導電材料。基板表面上之阻障層、金屬或金屬氮化物包括鈦、氮化鈦、氮化鎢、鉭及氮化鉭、鋁、銅或對元件製造有用之任何其他導體或導電或非導電阻障層。基板可具有各種尺寸,諸如200mm或300mm直徑的晶圓以及矩形窗格或方形窗格。本發明之實施例在其上可能有用之該基板包括但不限於半導體晶圓,諸如晶態矽(例如,Si<100>或Si<111>)、氧化矽、應變矽、矽鍺、摻雜聚矽或未摻雜聚矽、摻雜矽晶圓或未摻雜矽晶圓、諸如GaAs、GaN、InP等之III-V族材料及圖案化晶圓或非圖案化晶圓。可將基板暴露於預處理製程以研磨、蝕刻、還原、氧化、羥基化、退火及/或烘烤基板表面。
因為本發明之實施例提供用於沉積或形成含有混合金屬氧化物之膜的方法,所以處理腔室經設置以在氣相沉積製程期間將基板暴露至一系列氣體及/或電漿。處理腔室將包括單獨供應A反應物及B反應物,或C反應物及D反應物,或所有的A反應物、B反應物、C反應物及D反應物。處理腔室亦將包括:載氣、淨化氣體及諸如氬氣及氮氣之惰性氣體的任何供應都與用於反應物及氣體中之每一者的氣體入口
流體連通。每一入口可藉由與中央處理單元(CPU)連通之諸如質量流量控制器或體積流量控制器之適當流量控制器控制,該流量控制器允許每一反應物流動至基板以執行如本文所述之ALD製程。中央處理單元可為一種任何形式的電腦處理器,該電腦處理器可用於工業設定中以控制各種腔室及子處理器。可將CPU耦接至記憶體,且CPU可為一或多個容易可用之記憶體,諸如隨機存取記憶體(RAM)、唯讀記憶體(ROM)、快閃記憶體、光碟、軟碟、硬碟或任何其他形式之本端或遠端數位儲存器。可將支援電路耦接至CPU來以習知方式支援CPU。該等電路包括快取記憶體、電源、時鐘電路、輸入/輸出電路系統、子系統及類似物。
共反應物通常係處於氣相形式或氣體形式。反應物可以載氣輸送。載氣、淨化氣體、沉積氣體或其他製程氣體可含有氮氣、氫氣、氬氣、氖氣、氦氣或前述氣體之組合。電漿可對本文描述之膜的沉積、形成、退火、處理或其他處理有用。本文描述之諸如氮氣電漿或惰性氣體電漿之各種電漿可由電漿共反應物氣體點燃及/或含有電漿共反應物氣體。
在一或多個實施例中,用於製程之各種氣體可自各種孔或出口經由氣體通道脈衝輸送至入口且至中央通道中。在一或多個實施例中,沉積氣體可順序地脈衝輸送至噴淋頭且通過噴淋頭。或者,如上所述,氣體可同時流動通過氣體供應噴嘴或氣體供應頭,且可移動基板及/或氣體供應頭以便將基板順序地暴露至氣體。
在另一實施例中,含有混合金屬氧化物之膜可在電
漿增強原子層沉積(plasma enhanced atomic layer deposition;PEALD)製程期間形成,該PEALD製程提供一或多個前驅物及電漿之順序脈衝。在特定實施例中,共反應物可涉及電漿。在涉及電漿使用之其他實施例中,在電漿步驟期間,試劑係通常在製程期間離子化,但此離子化可能僅在沉積腔室之上游發生以使得離子或其他高能物種或發光物種不與沉積膜直接接觸,此設置經常稱為遠端電漿。因此,在此類型之PEALD製程中,電漿係諸如藉由遠端電漿產生器系統自處理腔室外部產生。在PEALD製程期間,電漿可自微波(MW)頻率產生器或射頻(RF)產生器產生。儘管可在本文揭示之ALD製程期間使用電漿,但應注意,並非需要電漿。實際上,其他實施例係關於在無電漿的極溫和條件下的ALD。
因此,本發明之另一態樣係關於根據上述任何實施例用於在基板上沉積膜以執行製程的設備。在一個實施例中,設備包含用於在基板上原子層沉積膜之沉積腔室。腔室包含用於支撐基板之製程區域。設備包括與鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物之供應流體連通之前驅物入口。設備亦包括與氧化劑之供應流體連通之反應物氣體入口,如上所述。設備進一步包括與淨化氣體流體連通之淨化氣體入口。設備可進一步包括用於自沉積腔室移除氣體之真空埠。設備可進一步包括輔助氣體入口,用於供應諸如惰性氣體之一或多種輔助氣體至沉積腔室。沉積可進一步包括用於藉由輻射熱及/或電阻熱加熱基板之構件(means)。
在一些實施例中,可在本文所述之用於沉積或形成
光阻材料之方法期間使用的電漿系統及處理腔室或系統可在PRODUCER®系統、CENTURA®系統或ENDURA®系統中之任一者上執行,所有上述系統可購自位於Santa Clara,Calif之Applied Materials,Inc.。ALD處理腔室之詳細描述可見於共同讓渡之美國專利第6,878,206號、第6,916,398號及第7,780,785號中。
在ALD製程中,處理腔室或沉積腔室可在自約0.01托至約100托之範圍內的壓力下加壓,例如在自約0.1托至約10托的壓力下加壓。同樣地,根據一或多個實施例,可加熱腔室或基板,以使得沉積可發生在低於約300℃之溫度下。在其他實施例中,沉積可發生在低於約100℃之溫度下,且在其他實施例中,沉積可發生在甚至低至約室溫之溫度下。在一個實施例中,沉積係在約150℃至350℃之溫度範圍下進行。
基板可為上述任何類型的基板。可選製程步驟涉及藉由以電漿或其他合適的表面處理處理基板以在基板表面上提供活性部位而製備基板。合適活性部位之實例包括但不限於O-H終止表面、N-H終止表面或S-H終止表面。
「A」前驅物至基板表面之輸送
可將基板暴露於藉由使載氣(例如,氮氣或氬氣)通過前驅物之安瓿而形成之「A」前驅物氣體或蒸氣,該「A」前驅物氣體或蒸氣可處於液態形式。可加熱安瓿。或者,前驅物可溶於溶劑中且用於直接液體噴射及驟汽化。合適的溶劑包括烴類、烷基胺及醇類。當使用直接液體噴射及驟汽化時,在將液體傳輸至汽化器之前不必加熱前驅物溶液,此舉
改良前驅物溶液之存放期。
可在任何合適流動速率下輸送「A」前驅物氣體,該流動速率係在自約10sccm至約2000sccm之範圍內,例如,自約50sccm至約1000sccm,且在特定實施例中,該流動速率係在自約100sccm至約500sccm之範圍內,例如,約200sccm。可將基板暴露於含金屬之「A」前驅物氣體達一時間段,該時間段係在自約0.1秒至約10秒範圍內,例如,自約1秒至約5秒,且在特定實例中,該時間段達近似2秒。一旦前驅物已被吸附至基板表面上之所有反應表面部分上,就停止「A」前驅物氣體之流動。在理想進行之ALD製程中,容易以反應前驅物「A」使表面飽和,以使得額外暴露將不引起額外沉積(亦即,製程由於所有反應表面部分之消耗而自限制)。
第一淨化
在停止「A」前驅物氣體之流動之後,可將基板及腔室暴露至淨化步驟。可以一流動速率將淨化氣體供給至處理腔室內,該流動速率係在自約10sccm至約2000sccm之範圍內,例如,自約50sccm至約1000sccm,且在特定實施例中,該流動速率係在自約100sccm至約500sccm之範圍內,例如,約200sccm。淨化步驟移除處理腔室內之任何過量的前驅物、副產物及其他污染物。可進行淨化步驟達一時間段,該時間段係在自約0.1秒至約15秒範圍內,例如,自約1秒至約10秒,且在特定實例中,該時間段達約4秒。載氣、淨化氣體、沉積氣體或其他製程氣體可含有氮氣、氫氣、氬氣、
氖氣、氦氣或前述氣體之組合。在一個實例中,載氣包含氮氣。除淨化步驟外,可使用幫浦以增強抽空效率。
「B」共反應物至基板表面之輸送
在第一淨化之後,可將基板活性部位暴露於「B」共反應物氣體或蒸氣,該「B」共反應物氣體或蒸氣係藉由使載氣(例如,氮氣或氬氣)通過「B」共反應物之安瓿而形成。可加熱安瓿。可在任何合適流動速率下輸送「B」反應氣體,該流動速率係在自約10sccm至約2000sccm之範圍內,例如,自約50sccm至約1000sccm,且在特定實施例中,該流動速率為約200sccm。可將基板暴露於「B」反應氣體達一時間段,該時間段係在自約0.1秒至約8秒範圍內,例如,自約1秒至約5秒,且在特定實例中,該時間段達約2秒。一旦「B」已被吸附至先前步驟中沉積之「A」前驅物上且迅速地與「A」前驅物反應,則可停止「B」反應氣體之流動。
第二淨化
在停止「B」共反應物氣體之流動之後,可將基板及腔室暴露至淨化步驟。可以一流動速率將淨化氣體供給至處理腔室內,該流動速率係在自約10sccm至約2000sccm之範圍內,例如,自約50sccm至約1000sccm,且在特定實施例中,該流動速率係在自約100sccm至約500sccm之範圍內,例如,約200sccm。淨化步驟移除處理腔室內之任何過量的前驅物、副產物及其他污染物。可進行淨化步驟達一時間段,該時間段係在自約0.1秒至約8秒範圍內,例如,自約1秒至約5秒,且在特定實例中,該時間段達約4秒。載氣、淨化
氣體、沉積氣體或其他製程氣體可含有氮氣、氫氣、氬氣、氖氣、氦氣或前述氣體之組合。在一個實例中,載氣包含氮氣。「B」共反應物氣體亦可處於自製程腔室遠端產生之電漿的形式。除淨化步驟外,可使用幫浦以增強抽空效率。
可以與如上所述用於「A」反應物及「B」反應物相同的方式輸送「C」反應物及「D」反應物。
在已沉積含有混合金屬氧化物之膜之後,可將膜退火以使膜均勻化。退火條件可為在約200℃至1000℃之溫度範圍內,諸如300℃至800℃,且更特定言之為400℃至700℃,其中持續時間為0.1秒至60秒,諸如1秒至30秒,更特定言之2秒至10秒。包括尖波退火(亦即,短突退火(short abrupt anneal))之快速熱退火製程可為較佳的以最小化在金屬氧化物與基板之間的非期望界面氧化層成長。用於退火之周圍氣體可含有但不限於氮氣、氫氣、氬氣、氖氣、氦氣、成形氣體(H2/N2)H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、醇類、羧酸、CO、CO2及HCOH或前述各者之組合。在一或多個實施例中,載氣包含氮氣。
本發明之另一態樣係關於藉由使用前驅物混合物沉積含有混合金屬氧化物之膜的方法。在此態樣之一或多個實施例中,該方法包含將基板表面順序地暴露至氧化劑及前驅物混合物之交替脈衝。前驅物混合物包含諸如過渡金屬前驅物之第一金屬前驅物及諸如鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物之第二金屬前驅物。該等前驅物可為上文關於第一態樣描述之彼等前驅物中之任何者。
使前驅物混合物共同流動可具有優於在奈米層壓製程中分別沉積過渡金屬層及鑭系元素層之若干優勢。第一金屬與第二金屬在混合金屬氧化物膜中之比率可藉由控制兩個前驅物在混合物中之比率而控制。膜之最終組成將取決於兩個前驅物之比率以及兩個前驅物之相對反應性。根據一或多個實施例,過渡金屬前驅物與鑭系元素前驅物在前驅物混合物中之莫耳比係在自100:1至2:1或自20:1至5:1的範圍內。在一些實施例中,過渡金屬為鉿且鑭系元素為鈰,且鉿前驅物與鈰前驅物之莫耳比係自100:1至2:1或自20:1至5:1。
另一潛在優勢在於可直接沉積均勻混合金屬氧化物膜,此舉可減少對後沉積退火的需要或此舉可降低後沉積退火溫度。此外,可使用簡單的4步驟循環(前驅物混合物脈衝、淨化、氧化劑脈衝、淨化)代替具有8個或8個以上步驟(第一金屬前驅物脈衝、淨化、氧化劑脈衝、淨化、第二金屬前驅物脈衝、淨化、氧化劑脈衝、淨化)的更複雜沉積程序。
在一些實施例中,第一金屬前驅物之配位體及第二金屬前驅物之配位體係針對相容性而選擇以防止氣相反應。舉例而言,第一金屬前驅物及第二金屬前驅物兩者可為脒鹽前驅物或胍鹽前驅物。
前驅物可在混合之前引入沉積腔室內,或前驅物可在引入沉積腔室內之前混合。在一些實施例中,前驅物係在引入沉積腔室內之前混合以提供均勻前驅物混合物。
本發明之另一態樣係關於沉積包含混合金屬氧化物
之膜的方法,該方法包含:控制第一金屬前驅物及第二金屬前驅物之流動以提供前驅物混合物,且隨後將基板之表面暴露至前驅物混合物。在此態樣之實施例中,第一金屬為過渡金屬(諸如Hf、Zr及/或Ti),且第二金屬前驅物為鑭系元素脒鹽前驅物或鑭系元素胍鹽前驅物。亦將基板暴露至氧化劑以提供含有第一金屬及第二金屬之混合金屬氧化物的膜。
用於此態樣中之前驅物可為任何的上述前驅物。在一些實施例中,第一金屬前驅物亦為脒鹽前驅物或胍鹽前驅物。
本發明之又一態樣係關於電子元件,該等電子元件包含根據本文描述之任何方法沉積之混合金屬氧化物。混合金屬氧化物可用作該等電子元件中之介電質,且混合金屬氧化物可與元件中之導電層連通。其中可使用該等混合金屬氧化物膜之電子元件之實例為電容器、電晶體、動態隨機存取記憶體單元、電阻式隨機存取記憶體單元、快閃記憶體單元及顯示面板。
貫穿本說明書對「一個實施例」、「某些實施例」、「一或多個實施例」或「一實施例」之參考意謂:結合實施例描述之特定特徵、結構、材料或特性係包括於本發明之至少一個實施例中。因此,貫穿本說明書在各個位置中出現的諸如「在一或多個實施例中」、「在某些實施例中」、「在一個實施例中」或「在一實施例中」之用語未必指代本發明之相同實施例。此外,在一或多個實施例中,可以任何合適
方式組合特定特徵、結構、材料或特性。上述方法的描述次序不應視為限制,且該等方法可使用次序顛倒或具有遺漏或添加之所述操作。
應理解,上文描述意欲為說明性而非限制性。許多其他實施例將在一般技術者審閱上文描述後顯而易見。因此,本發明之範疇應參閱隨附申請專利範圍,連同該申請專利範圍所賦予之等效物之整體範疇一起來決定。
Claims (24)
- 一種沉積一膜之方法,該方法包含以下步驟:將一基板之一表面順序地暴露至一第一金屬前驅物及一氧化劑之交替脈衝以在該基板表面上提供一第一金屬氧化物膜,其中該第一金屬為Hf、Zr及Ti中之一或多者;以及將該第一金屬氧化物膜順序地暴露至一氧化劑及一前驅物之交替脈衝以提供包含該第一金屬及鈰之一混合金屬氧化物的一膜,該前驅物係選自鈰脒鹽前驅物及一鈰胍鹽前驅物。
- 如請求項1所述之方法,其中該第一金屬前驅物具有藉由M1Ln表示之一化學式,其中M1係選自Hf、Zr及Ti,Ln為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至4的一數字,且其中每一L獨立地為與另一L相同或不同的配位體;以及其中該鈰脒鹽前驅物或該鈰胍鹽前驅物具有藉由以下結構式表示之一結構:
- 如請求項2所述之方法,其中一或多個L為一脒鹽配位體或一胍鹽配位體。
- 如請求項1所述之方法,其中包含一混合金屬氧化物之該膜為一混合金屬氧化物膜、一混合金屬氮氧化物膜、一混合金屬矽酸鹽膜或一氮化之混合金屬矽酸鹽膜。
- 如請求項1所述之方法,其中該第一金屬包括Hf。
- 如請求項5所述之方法,其中該混合金屬氧化物膜基於鈰及鉿在該膜中之該總莫耳包含1莫耳百分比至30莫耳百分比的鈰。
- 如請求項1所述之方法,其中該氧化劑包含以下物質中之一或多者:H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、醇類、羧酸、CO、CO2及HCOH。
- 如請求項1所述之方法,進一步包含以下步驟:退火該混合金屬氧化物膜。
- 一種沉積一膜之方法,該方法包含以下步驟:將一基板之一表面順序地暴露至一氧化劑及一前驅物混合物之交替脈衝以提供包含該第一金屬及該第二金屬之一混合金屬氧化物之一膜,該前驅物混合物包含一第一金屬前驅物及一第二金屬前驅物,其中該第一金屬為Hf、Zr及Ti中之一或多者,且該第二金屬前驅物係選自一鑭系元素脒鹽前驅物及一鑭系元素胍鹽前驅物。
- 如請求項9所述之方法,其中該第一金屬前驅物包含該第一金屬之一脒鹽前驅物或一胍鹽前驅物。
- 如請求項9所述之方法,其中該第一金屬前驅物具有藉由M1Ln表示之一化學式,其中M1係選自Hf、Zr及Ti,Ln 為選自以下之一或多者的n個配位體:氫化物、烷基醯胺、二烷基醯胺、醇鹽、β-二酮基、酮亞胺鹽、環戊二烯基、C1-8烷基、C2-8烯基、C2-8炔基、CF3、鹵化物、咪唑、吡啶、脒鹽及胍鹽,n為自1至4的一數字,且其中每一L獨立地為與另一L相同或不同的配位體;以及其中該第二金屬前驅物具有藉由以下結構式表示之一結構:
- 如請求項11所述之方法,其中一或多個L為一脒鹽配位體或一胍鹽配位體。
- 如請求項9所述之方法,其中包含一混合金屬氧化物之該膜為一混合金屬氧化物膜、一混合金屬氮氧化物膜、一混合金屬矽酸鹽膜或一氮化之混合金屬矽酸鹽膜。
- 如請求項9所述之方法,其中該第一金屬包括Hf且該第二金屬包括Ce。
- 如請求項14所述之方法,其中該鉿前驅物與該鈰前驅物在該前驅物混合物中之該莫耳比係在自100:1至2:1之該範圍內。
- 如請求項8所述之方法,其中該氧化劑包含以下物質中之一或多者:H2O、H2O2、O2、O3、N2O、NO、NOx、硝酸鹽、醇類、羧酸、CO、CO2及HCOH。
- 如請求項8所述之方法,其中該第一金屬前驅物及該第二金屬前驅物係在將該第一金屬前驅物及該第二金屬前驅物引入一沉積腔室內之前混合,該沉積腔室用來沉積包含一混合金屬氧化物之該膜。
- 一種沉積包含一混合金屬氧化物之一膜的方法,該方法包含以下步驟:控制一第一金屬前驅物及一第二金屬前驅物之流動以提供一前驅物混合物,其中該第一金屬為Hf、Zr及Ti中之一 或多者,且該第二金屬前驅物為一鑭系元素脒鹽前驅物或一鑭系元素胍鹽前驅物;將一基板之一表面暴露至該前驅物混合物;以及將該基板之該表面暴露至一氧化劑以提供包含該第一金屬及該第二金屬之一混合金屬氧化物的一膜。
- 如請求項18所述之方法,其中該第一金屬前驅物包含該第一金屬之一脒鹽前驅物或一胍鹽前驅物。
- 如請求項18所述之方法,其中該第一金屬前驅物及該第二金屬前驅物之該等流動係經控制以基於在該膜中之鑭系元素及第一金屬的該總莫耳而提供包含1莫耳百分比至30莫耳百分比之鑭系元素之一混合金屬氧化物膜。
- 一種包含與一介電層連通之一導電層的電子元件,該介電層包含根據如請求項1所述之方法沉積之一混合金屬氧化物膜。
- 如請求項21所述之電子元件,其中該元件係選自:一電容器、一電晶體、一動態隨機存取記憶體單元、一電阻式隨機存取記憶體單元、一快閃記憶體單元及一顯示面板。
- 一種包含與一介電層連通之一導電層的電子元件,該介電層包含根據如請求項9所述之方法沉積之一混合金屬氧化物膜。
- 如請求項23所述之電子元件,其中該元件係選自:一電容器、一電晶體、一動態隨機存取記憶體單元、一電阻式隨機存取記憶體單元、一快閃記憶體單元及一顯示面板。
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US9269574B2 (en) | 2016-02-23 |
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