WO2013161772A1 - 成膜方法及び成膜装置 - Google Patents
成膜方法及び成膜装置 Download PDFInfo
- Publication number
- WO2013161772A1 WO2013161772A1 PCT/JP2013/061810 JP2013061810W WO2013161772A1 WO 2013161772 A1 WO2013161772 A1 WO 2013161772A1 JP 2013061810 W JP2013061810 W JP 2013061810W WO 2013161772 A1 WO2013161772 A1 WO 2013161772A1
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- WO
- WIPO (PCT)
- Prior art keywords
- film
- gas
- source gas
- film forming
- insulating film
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000010408 film Substances 0.000 claims abstract description 143
- 230000004888 barrier function Effects 0.000 claims abstract description 43
- 239000010409 thin film Substances 0.000 claims abstract description 20
- 229920000642 polymer Polymers 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 12
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 11
- 150000004985 diamines Chemical class 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims description 54
- 238000012545 processing Methods 0.000 claims description 44
- 230000008569 process Effects 0.000 claims description 38
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 13
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 6
- 150000008064 anhydrides Chemical class 0.000 claims description 4
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 4
- GHWVXCQZPNWFRO-UHFFFAOYSA-N butane-2,3-diamine Chemical compound CC(N)C(C)N GHWVXCQZPNWFRO-UHFFFAOYSA-N 0.000 claims description 3
- FHBXQJDYHHJCIF-UHFFFAOYSA-N (2,3-diaminophenyl)-phenylmethanone Chemical compound NC1=CC=CC(C(=O)C=2C=CC=CC=2)=C1N FHBXQJDYHHJCIF-UHFFFAOYSA-N 0.000 claims description 2
- PWGJDPKCLMLPJW-UHFFFAOYSA-N 1,8-diaminooctane Chemical compound NCCCCCCCCN PWGJDPKCLMLPJW-UHFFFAOYSA-N 0.000 claims description 2
- WRRQKFXVKRQPDB-UHFFFAOYSA-N 2-(2-aminophenyl)sulfanylaniline Chemical compound NC1=CC=CC=C1SC1=CC=CC=C1N WRRQKFXVKRQPDB-UHFFFAOYSA-N 0.000 claims description 2
- DLCQVSZPARLPHV-UHFFFAOYSA-N 4-(1,3-dioxo-2-benzofuran-4-carbonyl)-2-benzofuran-1,3-dione Chemical compound C=1C=CC=2C(=O)OC(=O)C=2C=1C(=O)C1=CC=CC2=C1C(=O)OC2=O DLCQVSZPARLPHV-UHFFFAOYSA-N 0.000 claims description 2
- AEJWKVGGBGUSOA-UHFFFAOYSA-N 4-[(1,3-dioxo-2-benzofuran-4-yl)sulfonyl]-2-benzofuran-1,3-dione Chemical compound O=C1OC(=O)C2=C1C=CC=C2S(=O)(=O)C1=CC=CC2=C1C(=O)OC2=O AEJWKVGGBGUSOA-UHFFFAOYSA-N 0.000 claims description 2
- YGYCECQIOXZODZ-UHFFFAOYSA-N 4415-87-6 Chemical compound O=C1OC(=O)C2C1C1C(=O)OC(=O)C12 YGYCECQIOXZODZ-UHFFFAOYSA-N 0.000 claims description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- XTUVJUMINZSXGF-UHFFFAOYSA-N N-methylcyclohexylamine Chemical compound CNC1CCCCC1 XTUVJUMINZSXGF-UHFFFAOYSA-N 0.000 claims description 2
- RZIPTXDCNDIINL-UHFFFAOYSA-N cyclohexane-1,1,2,2-tetracarboxylic acid Chemical compound OC(=O)C1(C(O)=O)CCCCC1(C(O)=O)C(O)=O RZIPTXDCNDIINL-UHFFFAOYSA-N 0.000 claims description 2
- OYOFUEDXAMRQBB-UHFFFAOYSA-N cyclohexylmethanediamine Chemical compound NC(N)C1CCCCC1 OYOFUEDXAMRQBB-UHFFFAOYSA-N 0.000 claims description 2
- STZIXLPVKZUAMV-UHFFFAOYSA-N cyclopentane-1,1,2,2-tetracarboxylic acid Chemical compound OC(=O)C1(C(O)=O)CCCC1(C(O)=O)C(O)=O STZIXLPVKZUAMV-UHFFFAOYSA-N 0.000 claims description 2
- OWEZJUPKTBEISC-UHFFFAOYSA-N decane-1,1-diamine Chemical compound CCCCCCCCCC(N)N OWEZJUPKTBEISC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- UYXJVBAGMQWSOS-UHFFFAOYSA-N hept-1-ene-1,1-diamine Chemical compound CCCCCC=C(N)N UYXJVBAGMQWSOS-UHFFFAOYSA-N 0.000 claims description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 2
- -1 hexazolopropane Chemical compound 0.000 claims description 2
- OLAKSHDLGIUUET-UHFFFAOYSA-N n-anilinosulfanylaniline Chemical compound C=1C=CC=CC=1NSNC1=CC=CC=C1 OLAKSHDLGIUUET-UHFFFAOYSA-N 0.000 claims description 2
- DDLUSQPEQUJVOY-UHFFFAOYSA-N nonane-1,1-diamine Chemical compound CCCCCCCCC(N)N DDLUSQPEQUJVOY-UHFFFAOYSA-N 0.000 claims description 2
- GPCKFIWBUTWTDH-UHFFFAOYSA-N pentane-3,3-diamine Chemical compound CCC(N)(N)CC GPCKFIWBUTWTDH-UHFFFAOYSA-N 0.000 claims description 2
- KQAYXXFFBQKDEP-UHFFFAOYSA-N undecane-6,6-diamine Chemical compound CCCCCC(N)(N)CCCCC KQAYXXFFBQKDEP-UHFFFAOYSA-N 0.000 claims description 2
- 125000006160 pyromellitic dianhydride group Chemical group 0.000 claims 1
- 229920001721 polyimide Polymers 0.000 abstract description 46
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- ANSXAPJVJOKRDJ-UHFFFAOYSA-N furo[3,4-f][2]benzofuran-1,3,5,7-tetrone Chemical compound C1=C2C(=O)OC(=O)C2=CC2=C1C(=O)OC2=O ANSXAPJVJOKRDJ-UHFFFAOYSA-N 0.000 abstract 2
- 238000002407 reforming Methods 0.000 abstract 2
- 230000001360 synchronised effect Effects 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 163
- 239000010949 copper Substances 0.000 description 41
- 239000000758 substrate Substances 0.000 description 26
- 238000003860 storage Methods 0.000 description 25
- 239000012159 carrier gas Substances 0.000 description 21
- 239000010410 layer Substances 0.000 description 20
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 19
- 239000010936 titanium Substances 0.000 description 17
- 238000009792 diffusion process Methods 0.000 description 15
- 239000004065 semiconductor Substances 0.000 description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 11
- 229910052802 copper Inorganic materials 0.000 description 11
- 239000006185 dispersion Substances 0.000 description 11
- 229910052710 silicon Inorganic materials 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000004048 modification Effects 0.000 description 8
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- 150000002500 ions Chemical group 0.000 description 7
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- 238000010926 purge Methods 0.000 description 7
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- 235000012239 silicon dioxide Nutrition 0.000 description 7
- 239000010453 quartz Substances 0.000 description 6
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- 238000010586 diagram Methods 0.000 description 3
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- 239000010935 stainless steel Substances 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000003708 ampul Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
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- 238000007789 sealing Methods 0.000 description 2
- 238000000992 sputter etching Methods 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004590 computer program Methods 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- JMLPVHXESHXUSV-UHFFFAOYSA-N dodecane-1,1-diamine Chemical compound CCCCCCCCCCCC(N)N JMLPVHXESHXUSV-UHFFFAOYSA-N 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011553 magnetic fluid Substances 0.000 description 1
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- 238000004544 sputter deposition Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Images
Classifications
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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
- H01L21/02118—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 carbon based polymeric organic or inorganic material, e.g. polyimides, poly cyclobutene or PVC
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/52—Controlling or regulating the coating process
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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
- H01L21/022—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 a laminate, i.e. composed of sublayers, e.g. stacks of alternating high-k metal oxides
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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
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
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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
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02337—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment by exposure to a gas or vapour
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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
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- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02318—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment
- H01L21/02359—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer post-treatment treatment to change the surface groups of the insulating layer
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- H—ELECTRICITY
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- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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- 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
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76801—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing
- H01L21/76829—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing characterised by the formation of thin functional dielectric layers, e.g. dielectric etch-stop, barrier, capping or liner layers
- H01L21/76831—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics characterised by the formation and the after-treatment of the dielectrics, e.g. smoothing characterised by the formation of thin functional dielectric layers, e.g. dielectric etch-stop, barrier, capping or liner layers in via holes or trenches, e.g. non-conductive sidewall liners
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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
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
- H01L21/768—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics
- H01L21/76898—Applying interconnections to be used for carrying current between separate components within a device comprising conductors and dielectrics formed through a semiconductor substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/36—Successively applying liquids or other fluent materials, e.g. without intermediate treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2490/00—Intermixed layers
- B05D2490/50—Intermixed layers compositions varying with a gradient perpendicular to the surface
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
Definitions
- the present invention relates to a film forming method and a film forming apparatus for forming an insulating film made of a polymer thin film.
- a desired device is manufactured by repeatedly performing various processes such as a film forming process, a patterning process, and a dry etching process on a substrate such as a semiconductor wafer.
- various processes such as a film forming process, a patterning process, and a dry etching process
- the line width and the hole diameter have been increasingly miniaturized due to the demand for further higher integration and miniaturization of semiconductor devices.
- the wiring layer has a multi-wiring structure such as an eight-layer structure.
- the wiring material and the embedding material there is a tendency to use copper which has a very low electric resistance and is inexpensive because it is necessary to reduce the electric resistance by miniaturizing various dimensions (for example, see Patent Document 1). .
- tantalum metal Ti
- titanium Ti
- tantalum nitride in consideration of adhesion to the lower layer and prevention of copper diffusion.
- a film (TaN), a titanium nitride film (TiN) or the like is interposed as a barrier layer.
- FIGS. 1A and 1B are views for explaining a part of a conventional embedding process of a concave portion of an object to be processed.
- FIG. 1A shows a part of a process in the middle of forming a TSV (Through Silicon Via) structure used when three-dimensionally mounting an integrated circuit.
- TSV Three Silicon Via
- a semiconductor element such as a transistor or a wiring layer thereof is formed on the surface of a substrate 4 made of a disk-shaped silicon substrate having a thickness of about 0.7 mm.
- the conductive layer 6 is formed, and the entire surface of the semiconductor element and the conductive layer 6 is covered with a protective insulating layer 8.
- the back surface side of the substrate 4 is polished (back grind) to reduce the thickness of the substrate 4 to about 0.1 mm, and this is turned upside down (reversely).
- a recess 10 is formed by etching or the like from the back side (upper side in the figure) to the conductive layer 6.
- the conductive layer 6 is exposed at the bottom of the recess 10.
- the recess 10 becomes a through hole for contact with the lead electrode of the semiconductor element, a via hole for connection between wiring layers, or the like.
- the concave portion 10 is filled with a copper film for conduction when a semiconductor element or the like is further formed on the upper surface side of the inverted substrate 4.
- an insulating film 12 is formed on the entire surface and the entire sidewall in the recess 10 in order to ensure insulation against the substrate 4.
- a barrier film 14 for preventing copper diffusion is formed.
- the recessed metal 10 is embedded by forming the embedded metal film 16.
- the insulating film 12 for example, SiO2 made of TEOS (tetraethylorthosilicate) is used. A membrane is used.
- Ti, Ta, nitride films thereof (TiN, TaN), or the like is used.
- a copper film is used as the buried metal film 16.
- One embodiment of the present invention is a film forming method and a film forming apparatus that can be applied to filling a recess with a high aspect ratio and that can provide a polymer thin film insulating film that also has a barrier property.
- a film forming method which includes a first source gas and an diamine made of an acid anhydride in a processing container that contains an object to be processed and is evacuated. And an insulating film made of a polymer thin film is formed on the surface of the object to be processed, and the supply of the second source gas into the processing container is stopped and the first source gas is stopped. One source gas is continuously supplied into the processing container, and the insulating film is modified to give the insulating film a barrier function.
- a film forming apparatus including a processing container that accommodates an object to be processed, a holding unit that holds the object to be processed in the processing container, A vacuum exhaust system for evacuating the inside of the processing vessel, a first gas supply means for supplying a first source gas made of acid anhydride into the processing vessel, and a second source gas made of diamine are supplied.
- a second gas supply unit ; a heating unit configured to heat the object to be processed; and an apparatus control unit configured to control the entire apparatus.
- the apparatus control unit supplies the first source gas from the first gas supply unit and also supplies the second source gas from the second source gas supply unit to supply the surface of the object to be processed.
- An insulating film made of a polymer thin film is formed, and then the first source gas is continuously supplied from the first gas supply means, and the second source gas is supplied from the second gas supply means. Control to stop the supply.
- the insulating film can be provided with a barrier function by modifying the insulating film. Accordingly, it is possible to form an insulating film of a polymer thin film that can be applied to filling a concave portion with a high aspect ratio and also has a barrier property.
- FIG. 2 is a longitudinal sectional view showing an example of a film forming apparatus according to the present invention
- FIG. 3 is a transverse sectional view showing a film forming apparatus (heating means is omitted).
- the film forming apparatus 20 includes a cylindrical inner cylinder 22 having a dome-shaped ceiling and a cylindrical outer cylinder 24 having a dome-shaped ceiling concentrically arranged on the outer side thereof. And a processing container 26 having a double cylinder structure. Both the inner cylinder 22 and the outer cylinder 24 are made of a heat-resistant material such as quartz. The lower end of the processing container 26 is connected to and supported by a cylindrical manifold 30 made of, for example, stainless steel via a seal member 28 such as an O-ring. The lower end portion of the inner cylinder 22 is supported on a support ring 32 attached to the inner wall of the manifold 30. There is also an apparatus in which a stainless-steel manifold 30 is not provided and the whole is formed of a cylindrical quartz processing vessel.
- the manifold 30 is formed in a cylindrical shape, and a quartz wafer boat 34 as a holding means on which a large number of disk-like objects 2 are placed in multiple stages from below the manifold 30 can be moved up and down. It is made removable. In the case of the present embodiment, for example, about 50 to 150 pieces of the object to be processed 2 having a diameter of 300 mm can be supported in multiple stages at substantially equal pitches on the support 34A of the wafer boat 34.
- the wafer boat 34 is placed on a table 38 via a quartz heat insulating cylinder 36, and the table 38 passes through a lid 40 made of, for example, stainless steel that opens and closes the lower end opening of the manifold 30. It is supported on the rotating shaft 42.
- a magnetic fluid seal 44 is interposed in the penetrating portion of the rotating shaft 42 and supports the rotating shaft 42 so as to be rotatable while hermetically sealing.
- a seal member 46 made of, for example, an O-ring is interposed between the peripheral portion of the lid portion 40 and the lower end portion of the manifold 30 to maintain the sealing performance in the processing container 26.
- the rotating shaft 42 is attached to the tip of an arm 47 supported by an elevating mechanism (not shown) such as a boat elevator, for example, and moves up and down integrally with the wafer boat 34 and the lid 40. 26 can be inserted and removed.
- the table 38 may be fixedly provided on the lid 40 side so that the object to be processed 2 can be processed without rotating the wafer boat 34.
- the processing vessel 26 is provided with a gas introduction part 48.
- the gas introduction part 48 has a plurality of, here two gas dispersion nozzles 50 and 52, each of which is made of a quartz tube that extends inwardly through the side wall of the manifold 30. ing.
- Each gas dispersion nozzle 50, 52 is formed with a plurality of (many) gas injection holes 50A, 52A at a predetermined interval along the length direction thereof, and the horizontal direction from each gas injection hole 50A, 52A. The gas can be injected almost uniformly toward the center.
- a nozzle accommodating recess 54 (see FIG. 3) is formed in a part of the side wall of the inner cylinder 22 of the processing container 26 along the height direction. Further, an exhaust port 56 for evacuating the internal atmosphere is provided on the opposite side of the processing container 26 facing the nozzle housing recess 54.
- the exhaust port 56 may be formed to be elongated by scraping in the vertical direction, for example, or a number of slits extending in the horizontal direction may be formed in the vertical direction.
- the nozzle accommodating recess 54 forms a vertically elongated opening 58 by scraping the side wall of the processing container 26 with a predetermined width along the vertical direction, and covers the opening 58 from the outside.
- the gas dispersion nozzles 50 and 52 are provided side by side in the nozzle housing recess 54.
- a gas outlet 62 communicating with the exhaust port 56 is formed on the side wall above the support ring 32 of the manifold 30, and the atmosphere in the inner cylinder 22 is communicated with the inner cylinder via the exhaust port 56.
- the gas is discharged into the gap between the outer cylinder 22 and the outer cylinder 24 and reaches the gas outlet 62.
- the gas outlet 62 is provided with an evacuation system 64.
- the evacuation system 64 has an exhaust passage 66 connected to the gas outlet 62, and a pressure adjustment valve 68 and a vacuum pump 70 are interposed in the exhaust passage 66, and the inside of the processing vessel 26 is passed through. While maintaining a predetermined pressure, a vacuum is drawn.
- the cylindrical heating means 72 which heats this process container 26 and this to-be-processed object 2 is provided so that the outer periphery of this process container 26 may be enclosed.
- a gas supply means 74 is provided for supplying the gas necessary for the film forming process to the processing container 26.
- a first source gas supply system 76 that supplies a first source gas
- a second source gas supply system 78 that supplies a second source gas
- a purge gas supply system 80 that supplies a purge gas
- the first source gas supply system 76 includes a first source storage tank 84 that stores a first source 82 made of an acid anhydride that is in a liquid state at room temperature.
- the first raw material storage tank 84 is also referred to as an ampoule or a reservoir.
- Examples of the acid anhydride that is the first raw material 82 include pyromellitic dianhydride, oxydiphthalic dianhydride, biphthalic anhydride, carbonyldiphthalic anhydride, diphthalic anhydride, and sulfonyldiphthalic anhydride.
- One or more materials selected from the group consisting of a product, cyclohexanetetracarboxylic dianhydride, cyclopentanetetracarboxylic dianhydride, and cyclobutanetetracarboxylic dianhydride can be used.
- pyromellitic dianhydride (PMDA) is used.
- the first raw material storage tank 84 is provided with a raw material heater 86 that forms a first raw material gas by heating and vaporizing the first raw material 82 within a range not thermally decomposing. For example, it is heated to about 200 to 260 ° C.
- the first raw material storage tank 84 includes a gas supply unit 88 that supplies a carrier gas that conveys the first raw material gas, and a gas outflow unit 90 that flows out the first raw material gas along with the carrier gas. Is provided.
- the gas supply unit 88 and the gas outflow unit 90 are both provided on the ceiling of the first raw material storage tank 84.
- a first source gas passage 92 is provided.
- An opening / closing valve 94 is interposed in the middle of the first raw material gas passage 92 to control the flow of the first raw material gas.
- the gas outlet on the upstream side of the first raw material gas passage 92 is positioned so as to face the upper space in the first raw material storage tank 84, and the first raw material gas generated here Can be discharged together with the carrier gas.
- the first source gas passage 92 is provided with a passage heater (not shown) such as a tape heater along the first source gas passage 92.
- the first source gas passage 92 is heated to about 260 to 300 ° C., for example. Thus, the first source gas is prevented from being liquefied or solidified.
- a carrier gas passage 96 for introducing a carrier gas into the first raw material storage tank 84 is connected to the gas supply unit 88 of the first raw material storage tank 84.
- the gas supply port of the gas supply unit 88 is located so as to face the upper space in the first raw material storage tank 84.
- a flow rate controller 98 such as a mass flow controller for controlling the gas flow rate from the upstream side toward the downstream side and an on-off valve 100 are sequentially provided.
- N 2 gas is used as the carrier gas.
- the present invention is not limited to this, and other rare gases such as He and Ar may be used.
- the second source gas supply system 78 has a second source storage tank 104 that stores the second source 102 made of diamine that is in a liquid state at room temperature.
- the second raw material storage tank 104 is also referred to as an ampoule or a reservoir.
- Examples of the diamine that is the second raw material 102 include oxydianiline, diaminodecane, ethylenediamine, diaminoundecane, trimethylenediamine, diaminododecane, diaminobutane, hexohesolopropane, diaminopentane, thiodianiline, aminophenyl sulfide, and the like.
- One or more materials selected from the group consisting of diaminohexane, diaminodiphenylsulfone, heptenediamine, diaminobenzophenone, diaminooctane, diaminononane, diaminocyclohexylmethane, and methylcyclohexylamine can be used.
- oxydianiline (ODA) is used.
- the second raw material storage tank 104 is provided with a raw material heater 106.
- the raw material heater 106 forms the second raw material gas by heating and vaporizing the second raw material 102 within a range not thermally decomposing.
- the raw material heater 106 is heated to about 130 to 220 ° C., for example.
- the second raw material storage tank 104 includes a gas supply unit 108 that supplies a carrier gas that conveys the second raw material gas, and a gas outflow unit 110 that discharges the second raw material gas along with the carrier gas. Is provided.
- both the gas supply unit 108 and the gas outflow unit 100 are provided on the ceiling of the first raw material storage tank 104.
- a second source gas passage 112 is provided.
- the first source gas passage 92 and the second source gas passage 112 are connected to each other on the downstream side and used as a common passage, and the first source gas and the second source gas are used in common. Gas is mixed on the way.
- An on-off valve 114 is interposed in the middle of the second source gas passage 112 so as to control the flow of the second source gas.
- the gas outlet on the upstream side of the second raw material gas passage 112 is positioned so as to face the upper space in the second raw material storage tank 104, and the second raw material gas generated here Can be discharged together with the carrier gas.
- the second source gas passage 112 is provided with a passage heater (not shown) such as a tape heater along the second source gas passage 112.
- the second source gas passage 112 is heated to about 260 to 300 ° C., for example. This prevents the second source gas from being liquefied.
- a carrier gas passage 116 for introducing a carrier gas into the second raw material storage tank 104 is connected to the gas supply unit 108 of the second raw material storage tank 104.
- the gas supply port of the gas supply unit 108 is positioned so as to face the upper space in the second raw material storage tank 104.
- a flow controller 118 such as a mass flow controller for controlling the gas flow rate from the upstream side to the downstream side and an on-off valve 120 are sequentially provided.
- N 2 gas is used as the carrier gas.
- the present invention is not limited to this, and other rare gases such as He and Ar may be used.
- the purge gas supply system 80 has a purge gas passage 122 connected to the remaining one gas dispersion nozzle 52.
- a flow rate controller 124 such as a mass flow controller and an opening / closing valve 126 are sequentially provided so that the purge gas can be supplied while controlling the flow rate as necessary.
- the purge gas for example, an inert gas such as N 2 gas is used.
- the first source gas and the second source gas are mixed in the middle, and this mixed gas is discharged from one gas dispersion nozzle 50.
- the present invention is not limited to this, and another gas dispersion nozzle is provided, and the first and second source gas passages 92 and 112 are individually connected to the two gas dispersion nozzles. Two source gases may be mixed in the processing container 26.
- the overall operation of the film forming apparatus 20 configured as described above is controlled by an apparatus control unit 128 including, for example, a computer.
- a computer program for performing this operation is stored in the storage medium 130.
- the storage medium 130 includes, for example, a flexible disk, a CD (Compact Disc), a hard disk, a flash memory, a DVD, or the like. Specifically, the start and stop of each gas, flow control, control of process temperature and process pressure, and the like are performed according to commands from the apparatus control unit 128.
- FIG. 4 is a process diagram showing a flow of the film forming method of the present invention
- FIGS. 5A to 5E are cross-sectional views showing a state of embedding the recesses of the object to be processed
- a polyimide film is formed as a polymer thin film by vapor deposition polymerization using PMDA as the first raw material 82 and ODA as the second raw material 102 will be described as an example.
- a polyimide film which is an insulating film having a barrier function, is formed by using PMDA as the acid anhydride that is the first raw material 82 and ODA as the diamine that is the second raw material 102. It is supposed to be.
- the first source 82 When supplying the first source gas, the first source 82 is vaporized by heating in the first source storage tank 84 in the first source gas supply system 76 and is saturated. .
- the saturated first raw material gas By supplying the carrier gas whose flow rate is controlled into the saturated first raw material reservoir 84, the saturated first raw material gas is accompanied by the carrier gas to the first raw material gas passage 92 side. leak. Then, the first source gas transported together with the carrier gas is ejected from the gas dispersion nozzle 50 provided in the processing container 26 and supplied into the processing container 26.
- the second source gas 102 When supplying the second source gas, the second source gas 102 is vaporized by heating in the second source storage tank 104 in the second source gas supply system 78 and becomes saturated. Yes.
- the carrier gas By supplying the carrier gas whose flow rate is controlled into the second raw material storage tank 104 in the saturated state, the second raw material gas in the saturated state is accompanied by the carrier gas to the second raw material gas passage 112 side. leak.
- the second source gas conveyed together with the carrier gas is injected from the gas dispersion nozzle 50 provided in the processing container 26 and supplied into the processing container 26.
- first and second source gas passages 92 and 112 are connected on the way, when the first source gas and the second source gas are flowing, both source gases are on the way.
- the mixed gas is supplied into the processing container 26 after being mixed.
- the gas supplied into the processing container 26 flows in the horizontal direction (horizontal direction) between the objects to be processed while being in contact with the object 2 accommodated therein, and the inner cylinder 22 through the exhaust port 56. And flows into the gap between the outer cylinder 24 and the outer cylinder 24. Further, the gas flows down in the gap and is discharged out of the container from the gas outlet 62 by the vacuum exhaust system 64.
- a wafer boat 34 on which a large number of normal-temperature pieces, for example, 50 to 150 300 mm-sized workpieces 2 are placed is placed in a processing container 26 that has been previously set at a predetermined temperature. Raise and load more.
- the inside of the container is sealed by closing the lower end opening of the manifold 30 with the lid 40.
- a recessed portion 10 for embedding is formed on the surface as shown in FIG. 5A.
- This object 2 is the same as that described above with reference to FIG. 1A. That is, in the object 2 to be processed, a conductive material such as a semiconductor element (not shown) such as a transistor or its wiring layer is formed on the surface of a substrate 4 made of a disk-shaped silicon substrate having a thickness of about 0.7 mm. The layer 6 is formed, and the entire surface of the semiconductor element and the conductive layer 6 is covered with a protective insulating layer 8.
- the back surface side of the substrate 4 is polished (back grind) to reduce the thickness of the substrate 4 to about 0.1 mm, and this is turned upside down (reversely) so that the back surface side of the substrate 4 (in the figure)
- the recess 10 is formed by etching or the like from the upper side to the conductive layer 6.
- the recess 10 has a high aspect ratio with a diameter of about 5 ⁇ m, a depth of about 50 ⁇ m, and an aspect ratio of about 10.
- the processing container 24 When the object 2 to be processed is accommodated in the processing container 26, the processing container 24 is evacuated and maintained within a range of about 0.1 to 1.0 torr, and the heating means 72 is supplied to the heating means 72. By increasing the supply power, the wafer temperature is raised and the process temperature in the processing chamber 26 is maintained within a range of 20 to 450 ° C. (polyimide heat resistance temperature), for example. Then, each gas is supplied from the first source gas supply system 76 and the second source gas supply system 104 of the gas supply means 74 as described above.
- the first step S1 and the second step S2 are sequentially performed as described above.
- the first raw material gas PMDA and the second raw material gas ODA are supplied and polymerized by a vapor polymerization method to form a polymer thin film as shown in FIG. 5B.
- An insulating film 140 is formed.
- This insulating film 140 is a polyimide film.
- the first source gas and the second source gas may be supplied simultaneously, or the first source gas and the second source gas may be supplied alternately and repeatedly. May be.
- the process proceeds to the second step S2.
- the supply of the ODA gas is stopped by closing the on-off valve 114 of the second source gas passage 112, and the PMDA gas is continuously supplied to reform the insulating film 140 as shown in FIG. 5C.
- the post-flow process is performed by stopping the supply of the ODA gas and continuously flowing the PMDA gas.
- the surface of the insulating film 140 is modified to have a PMDA termination, and the insulating film 140 having a barrier function is formed.
- the process temperature in the processing vessel 26 is in the range of 20 to 450 ° C. (polyimide heat resistance temperature), preferably in the range of 130 to 200 ° C. as described above, and the process pressure in the processing vessel 26. Is in the range of 0.1 to 1.0 Torr (13 to 133 Pa), preferably in the range of 0.2 to 0.4 Torr.
- the gas flow rate in the first step S1 and the second step S2, the flow rate of the carrier gas is in the range of 0.8 to 1.5 liters / min, respectively, here 0.9 liters / min.
- the flow rate is
- the process time is in the range of 5-30 min, preferably in the range of 5-15 min.
- each step is performed for about 10 minutes.
- the insulating film 140 is not sufficiently modified, and if it is longer than 30 minutes, the modification is not only saturated but also the modification time becomes too long. Throughput decreases.
- the film formation rate is in the range of 20 to 50 nm / min.
- the target film thickness of the insulating film 140 is in the range of 250 to 500 nm, thereby eliminating the need to form a conventionally used barrier layer.
- a conventionally used barrier film 142 is formed on the modified insulating film 140 as shown in FIG. 5E. Thereafter, the seed film may be formed as described above to form the embedded metal film 16 such as Cu. In this case, the barrier film 142 can be made thinner than the conventional case.
- the barrier film 142 a Ti film, a Ta film, or a nitride film thereof is used as described above.
- the acid anhydride is used in the film forming method for forming the insulating film 140 made of a polymer thin film on the surface of the object 2 to be processed in the evacuated processing container 26, the acid anhydride is used.
- An insulating film 140 is formed by supplying a first source gas and a second source gas made of diamine, and after the first step, the supply of the second source gas is stopped and the first source gas is supplied.
- the insulating film 140 has a barrier function.
- the insulating film 140 can be applied to burying a recess with a high aspect ratio and has a barrier property. Can be formed.
- FIG. 7 is a graph showing Cu diffusion resistance against the termination treatment of the polyimide film.
- a polyimide film which is a polymer thin film, was formed on the surface of a silicon substrate with a thickness of about 0.3 ⁇ m, and a Cu film was formed on the surface of the polyimide film.
- SIMS secondary ion mass spectrometry
- the Cu element in the polyimide film is 5 ⁇ 10 17 atoms. / Cm3 is lowered to about one digit less than the case of curves A and B.
- the diffusion of the Cu element can be suppressed as compared with the other curves A and B.
- FIGS. 8A and 8B are graphs showing the Cu diffusion resistance of the polyimide film when the barrier film is used.
- FIGS. 8A and 8B a schematic view of a laminated state of a thin film as a sample is shown.
- a Ti film as a barrier film, and a Cu film are sequentially laminated.
- a polyimide film polymer thin film, second process completed
- Ti as a barrier film A film and a Cu film are sequentially stacked.
- the thickness of the Ti barrier film is 5 nm, which is considerably thinner than the thickness of 50 to 200 nm of the barrier film generally used in the past.
- the horizontal axis represents depth
- the vertical axis represents secondary ion intensity.
- SIMS is used to measure the elements in the sample, and secondary ions generated by sputter etching from the substrate side are measured. Focusing on the Cu concentration, in the case shown in FIG. 8A, the Cu element passes through the Ti film, which is a barrier film, and SiO 2. It is understood that the film diffuses to a considerable depth, for example, about 300 nm, and the barrier property against Cu diffusion is not sufficient.
- the Cu element seems to diffuse to the polyimide film through the Ti film as a barrier film and reach a depth of about 250 nm. Is an error that occurs in the characteristics of the SIMS method in which a sample is sputter-etched with ions.
- the polyimide film is much softer than the silicon or Ti film, so when sputtering with sputter etching ions for measurement from the silicon substrate side (right side in the graph), sputter ions penetrate in the depth direction. As a result, the sputter ions partially reach the Ti film portion from the point of about 250 nm in depth indicated by the point P1, and the Ti element starts to be detected.
- the Cu element and the Ti element are starting to be detected almost simultaneously. This means that the diffusion of the Cu element stops at the boundary portion between the Ti film and the polyimide film and does not diffuse to the polyimide film. In other words, since the start of detection of the Ti element and the start of detection of the Cu element are almost simultaneous, the Cu element has diffused to reach the boundary between the Ti film and the polyimide film, but has not diffused to the polyimide film. It turns out that there is no.
- the polyimide film whose surface is modified according to the embodiment of the present invention in addition to the insulating property, it can also be used as a barrier function and used in combination with a very thin barrier film of only about 5 ⁇ m. It can be seen that a sufficiently high barrier property can be exhibited as a whole. That is, if the insulating film having the barrier function of the present invention is used, the conventionally used barrier film can be thinned.
- the present invention is not limited to this, and the present invention is also applicable to the case where a recess is embedded in an object having a recess such as a via hole or a through hole formed on the surface side of a normal semiconductor substrate having a thickness of about 0.7 mm. Inventive methods can also be applied.
- the recess to be filled is formed in, for example, an interlayer insulating film.
- the present invention includes not only a silicon substrate but also a compound semiconductor substrate such as GaAs, SiC, and GaN as a substrate on which an object to be processed is formed, and is not limited to these substrates, and is used for a liquid crystal display device.
- the present invention can also be applied to glass substrates, ceramic substrates, and the like.
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Abstract
Description
膜が用いられる。バリア膜14としてはTiやTaやこれらの窒化膜(TiN、TaN)等が用いられる。埋め込み金属膜16としては例えば銅膜が用いられる。
4 基板
6 導電層
20 成膜装置
26 処理容器
34 ウエハボート(保持手段)
64 真空排気系
74 ガス供給手段
76 第1の原料ガス供給系
78 第2の原料ガス供給系
82 第1の原料
102 第2の原料
128 装置制御部
140 絶縁膜
142 バリア膜
S1 第1の工程
S2 第2の工程
ここで、上記絶縁膜140であるポリイミド膜の界面(表面)の改質による変化ついて図6A及び6Bを参照して説明する。図6A及び6B中において”P”はPMDA分子を示し、”O”はODA分子を示す。まず、図6Aに示すように第1の工程S1でPMDAとODAとを供給して絶縁膜140であるポリイミド膜を形成した時点では、基板4上に蒸気重合法によって形成されるポリイミド膜は”P”で終端しているものと、”O”で終端しているものとが混在している。
次に、ポリイミド膜のCu拡散耐性について検討を行ったので、その結果について図7を参照して説明する。図7はポリイミド膜の終端処理に対するCu拡散耐性を示すグラフである。ここでは、試料としてシリコン基板の表面に高分子薄膜であるポリイミド膜を0.3μm程度の厚さで形成し、このポリイミド膜の表面にCu膜を形成した。
次に、バリア膜とポリイミド膜とを併用した時のCu拡散耐性について検討を行ったので、その評価結果について図8A及び8Bを参照して説明する。図8A及び8Bはバリア膜を用いた時のポリイミド膜のCu拡散耐性を示すグラフである。この図8A及び8Bには試料となる薄膜の積層状態の模式図が併記されている。
膜、バリア膜としてのTi膜及びCu膜を順次積層している。また、図8Bに示す場合には、シリコン基板の表面に本発明の一実施形態に係る方法で形成した絶縁膜であるポリイミド膜(高分子薄膜、第2の工程済み)、バリア膜としてのTi膜及びCu膜を順次積層している。ここでTiのバリア膜の厚さは5nmであり、従来のおいて一般的に用いられていたバリア膜の厚さ50~200nmよりもかなり薄く形成してある。
膜のかなりの深さ、例えば深さ300nm程度まで拡散しており、Cu拡散に対するバリア性が十分でないことが判る。
Claims (8)
- 成膜方法であって、
被処理体を収容し、真空引きされた処理容器内に酸無水物よりなる第1の原料ガスとジアミンよりなる第2の原料ガスとを供給し、前記被処理体の表面に高分子薄膜よりなる絶縁膜を形成し、
前記処理容器内への前記第2の原料ガスの供給を停止すると共に前記第1の原料ガスを前記処理容器内に引き続き供給し、前記絶縁膜を改質することにより前記絶縁膜にバリア機能を持たせる、成膜方法。 - 前記処理容器内におけるプロセス温度は20~450℃の範囲内である請求項1記載の成膜方法。
- 前記処理容器内におけるプロセス圧力は0.1~1.0Torrの範囲内である請求項1記載の成膜方法。
- 前記酸無水物は、ピロメリット酸二無水物とオキシジフタル酸二無水物とビフタル酸無水物とカルボニルジフタル酸無水物とジフタル酸無水物とスルホニルジフタル酸無水物とシクロヘキサンテトラカルボン酸二無水物とシクロペンタンテトラカルボン酸二無水物とシクロブタンテトラカルボン酸二無水物とよりなる群から選択される1以上の材料を含み、
前記ジアミンは、オキシジアニリンとジアミノデカンとエチレンジアミンとジアミノウンデカンとトリメチレンジアミンとジアミノドデカンとジアミノブタンとヘキヘサルオロプロパンとジアミノペンタンとチオジアニリンとアミノフェニルスルフィドとジアミノヘキサンとジアミノジフェニルスルホンとヘプテンジアミンとジアミノベンゾフェノンとジアミノオクタンとジアミノノナンとジアミノシクロヘキシルメタンとメチルシクロヘキシルアミンとよりなる群から選択される1以上の材料を含む請求項1記載の成膜方法。 - 前記改質された絶縁膜の表面に更にバリア膜を形成する請求項1記載の成膜方法。
- 成膜装置であって、
被処理体を収容する処理容器と、
前記処理容器内で前記被処理体を保持する保持手段と、
前記処理容器内を真空引きする真空排気系と、
前記処理容器内へ酸無水物よりなる第1の原料ガスを供給する第1のガス供給手段と、
前記処理容器内へジアミンよりなる第2の原料ガスを供給する第2のガス供給手段と、
前記被処理体を加熱する加熱手段と、
装置全体を制御する装置制御部と、を備え、
該装置制御部は、前記第1のガス供給手段に前記第1の原料ガスを供給させるとともに、前記第2のガス供給手段に前記第2の原料ガスを供給させ、前記被処理体の表面に高分子薄膜よりなる絶縁膜を形成させ、次いで、前記第1のガス供給手段から前記第1の原料ガスを継続的に供給させるとともに、前記第2のガス供給手段から前記第2の原料ガスの供給を停止させる制御を行う成膜装置。 - 前記装置制御部は、前記処理容器内のプロセス温度が20~450℃の範囲内となるように前記加熱手段を制御する請求項6に記載の成膜装置。
- 前記装置制御部は、前記処理容器内のプロセス圧力が0.1~1.0Torrの範囲内となるように前記真空排気系を制御する請求項6に記載の成膜装置。
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Also Published As
Publication number | Publication date |
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JP2014170764A (ja) | 2014-09-18 |
JP6020239B2 (ja) | 2016-11-02 |
US20150087158A1 (en) | 2015-03-26 |
KR101607802B1 (ko) | 2016-03-30 |
US9349584B2 (en) | 2016-05-24 |
TW201405657A (zh) | 2014-02-01 |
KR20150009961A (ko) | 2015-01-27 |
TWI540641B (zh) | 2016-07-01 |
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