JP2004312004A - 低誘電体材料及びその作製方法 - Google Patents
低誘電体材料及びその作製方法 Download PDFInfo
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- JP2004312004A JP2004312004A JP2004106326A JP2004106326A JP2004312004A JP 2004312004 A JP2004312004 A JP 2004312004A JP 2004106326 A JP2004106326 A JP 2004106326A JP 2004106326 A JP2004106326 A JP 2004106326A JP 2004312004 A JP2004312004 A JP 2004312004A
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- Prior art keywords
- dielectric
- mixture
- dielectric constant
- film
- silicon
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- 239000000463 material Substances 0.000 title claims abstract description 94
- 238000004519 manufacturing process Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 156
- 239000000203 mixture Substances 0.000 claims abstract description 103
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 76
- 125000000962 organic group Chemical group 0.000 claims abstract description 57
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 49
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000003361 porogen Substances 0.000 claims abstract description 45
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 41
- 239000003989 dielectric material Substances 0.000 claims abstract description 39
- 230000005865 ionizing radiation Effects 0.000 claims abstract description 27
- 229910052799 carbon Chemical group 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 86
- 238000010894 electron beam technology Methods 0.000 claims description 49
- 239000012528 membrane Substances 0.000 claims description 36
- 239000000758 substrate Substances 0.000 claims description 33
- 150000001875 compounds Chemical class 0.000 claims description 29
- 239000011148 porous material Substances 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 25
- 239000010410 layer Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 16
- 239000010703 silicon Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 12
- 125000000217 alkyl group Chemical group 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 230000001133 acceleration Effects 0.000 claims description 10
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
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- 239000000126 substance Substances 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 7
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- 230000000996 additive effect Effects 0.000 claims description 6
- 239000011203 carbon fibre reinforced carbon Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229910002808 Si–O–Si Inorganic materials 0.000 claims description 5
- 239000011229 interlayer Substances 0.000 claims description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 5
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 3
- 150000004756 silanes Chemical class 0.000 claims description 3
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- 239000010408 film Substances 0.000 description 107
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- 230000008569 process Effects 0.000 description 27
- 238000001723 curing Methods 0.000 description 22
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- 238000012545 processing Methods 0.000 description 13
- 229920005989 resin Polymers 0.000 description 13
- 239000011347 resin Substances 0.000 description 13
- 229910052760 oxygen Inorganic materials 0.000 description 12
- 239000000523 sample Substances 0.000 description 12
- -1 vapor Substances 0.000 description 11
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 10
- 125000004429 atom Chemical group 0.000 description 10
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
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- 125000003118 aryl group Chemical group 0.000 description 7
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- 150000001412 amines Chemical class 0.000 description 6
- 229920001577 copolymer Polymers 0.000 description 6
- 238000004132 cross linking Methods 0.000 description 6
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- 150000002500 ions Chemical class 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000001590 oxidative effect Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 239000002002 slurry Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229910008051 Si-OH Inorganic materials 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- 229910006358 Si—OH Inorganic materials 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 150000004820 halides Chemical group 0.000 description 5
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- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 description 4
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- 229920000736 dendritic polymer Polymers 0.000 description 4
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 4
- 230000006870 function Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-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
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- TVJPBVNWVPUZBM-UHFFFAOYSA-N [diacetyloxy(methyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(OC(C)=O)OC(C)=O TVJPBVNWVPUZBM-UHFFFAOYSA-N 0.000 description 3
- PWDHJVSLINAQFE-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methyl-dimethoxy-phenylsilane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C[Si](OC)(OC)C1=CC=CC=C1 PWDHJVSLINAQFE-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
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- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
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- FKJVYOFPTRGCSP-UHFFFAOYSA-N 2-[3-aminopropyl(2-hydroxyethyl)amino]ethanol Chemical compound NCCCN(CCO)CCO FKJVYOFPTRGCSP-UHFFFAOYSA-N 0.000 description 2
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- OPHLEQJKSDAYRR-UHFFFAOYSA-N [diethoxy(methyl)silyl]oxy-diethoxy-methylsilane Chemical compound CCO[Si](C)(OCC)O[Si](C)(OCC)OCC OPHLEQJKSDAYRR-UHFFFAOYSA-N 0.000 description 2
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- TZPAJACAFHXKJA-UHFFFAOYSA-N methoxy-[[methoxy(dimethyl)silyl]methyl]-dimethylsilane Chemical compound CO[Si](C)(C)C[Si](C)(C)OC TZPAJACAFHXKJA-UHFFFAOYSA-N 0.000 description 2
- UQNPZTRHCNSLML-UHFFFAOYSA-N methoxy-[[methoxy(diphenyl)silyl]methyl]-diphenylsilane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(OC)C[Si](OC)(C=1C=CC=CC=1)C1=CC=CC=C1 UQNPZTRHCNSLML-UHFFFAOYSA-N 0.000 description 2
- XKINWJBZPLWKCW-UHFFFAOYSA-N methoxy-[methoxy(dimethyl)silyl]oxy-dimethylsilane Chemical compound CO[Si](C)(C)O[Si](C)(C)OC XKINWJBZPLWKCW-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
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- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1262—Process of deposition of the inorganic material involving particles, e.g. carbon nanotubes [CNT], flakes
- C23C18/127—Preformed particles
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
- C23C18/143—Radiation by light, e.g. photolysis or pyrolysis
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
- C23C18/145—Radiation by charged particles, e.g. electron beams or ion irradiation
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- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/46—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes silicones
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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
- H01L21/02126—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
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- 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
- H01L21/02203—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 porous
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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
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Abstract
【解決手段】 少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有し、該有機基内の少なくとも1つの水素原子が電離放射線源への露光によって除去可能である少なくとも1つのシリカ源;並びに[少なくとも1つのポロゲン質量]/[少なくとも1つのポロゲン質量及び少なくとも1つのシリカ源によって与えられたSiO2質量]の比が0.4以上である少なくとも1つのポロゲンを含んで成る、多孔質の低k誘電体材料を形成するための混合物を提供する。
【選択図】 なし
Description
XP=空隙率の値
k=誘電率の測定値
Dayらの2次元円孔モデル:
qc=0.9069=パーコレーション閾値、円が重なりかつ弾性率がゼロになる空隙率
ql=1/3=初期勾配
m=1.5=臨界指数
α=−0.251=正確な臨界振幅を得るためのパラメータ
θ=−1.83=自由フィッティングパラメータ
円筒に対して垂直な3次元拡張:
q=空隙率
E0=壁体弾性率
ペンチルが好ましい。上記化合物は、単独で又はそれらのうち2つ以上の混合物として使用できる。
Rg=(0.046/d)Va 1.75 式(5)
式(5)において、Rgは材料の電子範囲(μm)又はGrun範囲、dは膜密度(g/cm3)、Vaは加速電圧又は電子エネルギー(keV)である。所与の膜厚について、より低い密度を有する多孔質膜は、膜を硬化するのにより低い電子ビームエネルギーを必要とし、それによって電子ビームが下地の半導体デバイスに損傷を与える可能性を低下させる。例えば、2.2g/cm3の密度を有する10,000Å厚さの非多孔質膜は、硬化のために9.1keVの加速電圧を必要とする場合があるが、2.2g/cm3の壁密度及び0.65の空隙率を有する組成的に同一の10,000Å厚さの多孔質膜は、硬化のために5.0keVの加速電圧を必要とする場合がある。同様に、2.2g/cm3の密度を有する5,000Å厚さの非多孔質膜は、硬化のために6.1keVの加速電圧を必要とする場合があるが、2.2g/cm3の壁密度及び0.65の空隙率を有する組成的に同一の5,000Å厚さの多孔質膜は、硬化のために3.4keVの加速電圧を必要とする場合がある。
CS=CSi(CT−Cb)/[CSi−(CT−Cb)] 式(6)
各膜の誘電率は式(7)により算出し、式中、dは膜厚、Aは水銀電極面積、ε0は真空中の誘電率である。
以下の例で用いた試薬は、反応混合物への添加に先立ち、ドイツのFinnigan of Bremenにより製造されているFinnigan Element 1、高分解能Inductively Coupled Plasma/Mass Spectrometer(ICP/MS)を用いてICP/MSによって分析した。試薬中の金属不純物のレベルが50ppbを越える場合には試薬を精製した。その組成に応じて、試薬は、減圧下で又は金属イオンがカラム中に保持され、水素イオンがその代わりに放出されるイオン交換カラムのもとで、蒸留などの標準的な手順によって精製した。表Aは、本明細書に記載される精製プロセスを受けるとき又はその後での、さまざまな異なる試薬についての元素分析を与える。
4つの異なる反応混合物を、表1に与えられる試薬及び量を用いて調製した。これら反応混合物のそれぞれは、TAZMOモデルの#SW12132HM装置を用いて、150Åの熱酸化物(R<0.02Ωcm)を有する200mmのSiウェハ上にスピンオン堆積法によって堆積させた。3ml体積の反応混合物を200回転/分(rpm)の速度で回転するウェハ上に投与し、次いで、1800rpmで回転させて4つの膜を得た。堆積の後、熱板上で90℃、140℃及び400℃の温度でそれぞれ60秒、60秒及び180秒間、周囲雰囲気においてこれらの膜を熱硬化した。各膜の厚さ、屈折率、誘電率、及び硬度を表2に与える。
Claims (59)
- 約2.2以下の誘電率を有する多孔質のシリカに基づいた材料を形成するための混合物であって、
少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有し、該有機基内の少なくとも1つの水素原子が電離放射線源への露光によって除去可能である少なくとも1つのシリカ源;並びに
[少なくとも1つのポロゲン質量]/[少なくとも1つのポロゲン質量及び少なくとも1つのシリカ源によって与えられたSiO2質量]の比が0.4以上である少なくとも1つのポロゲン
を含んで成る、約2.2以下の誘電率を有する多孔質のシリカに基づいた材料を形成するための混合物。 - 約500ppm以下の金属不純物含有量を有する、請求項1に記載の混合物。
- イオン添加剤をさらに含んで成る、請求項2に記載の混合物。
- 溶媒をさらに含んで成る、請求項1に記載の混合物。
- 水をさらに含んで成る、請求項1に記載の混合物。
- 前記有機基が、1〜6の炭素原子を有するアルキル基を含んで成る、請求項1に記載の混合物。
- 前記有機基がメチル基を含んで成る、請求項6に記載の混合物。
- 前記メチル基/ケイ素のモル比が0.2以上である、請求項7に記載の混合物。
- 前記メチル基/ケイ素のモル比が0.6以上である、請求項8に記載の混合物。
- 前記有機基がネオペンチル基を含んで成る、請求項6に記載の混合物。
- 前記少なくとも1つのシリカ源が、以下の式、即ち、
i. RaSi(OR1)4−a(式中、R及びR1は独立して同じであるか若しくは異なることができ、Rは水素原子又は一価の有機基を表し、R1は一価の有機基を表し、aは1〜3の整数である);
ii. R3 b(R4O)3−bSi−(R7)−Si(OR5)3−cR6 c(式中、R3及びR6は独立して同じであるか若しくは異なることができ、それぞれ水素原子若しくは一価の有機基を表し、R4及びR5は独立して同じであるか若しくは異なることができ、それぞれ一価の有機基を表し、b及びcは独立して同じであるか若しくは異なることができ、それぞれ0〜3の数であり、R7は酸素原子、フェニレン基若しくは−(CH2)n−で表される基を表し、式中nは1〜6の整数である);又はそれらの組み合せ
によって表される化合物の群より選択された1つ又は複数のシラン化合物の加水分解及び縮合生成物である、請求項1に記載の混合物。 - 前記混合物が、以下の式、即ち、
i. Si(OR2)4(式中、R2は一価の有機基を表す);
ii. RaSi(OR1)4−a(式中、Rは水素原子を表し、R1は一価の有機基を表し、aは1〜3の整数である);
iii. R3 b(R4O)3−bSi−O−Si(OR5)3−cR6 c(式中、R3及びR6は水素原子を表し、R4及びR5は独立して同じであるか若しくは異なることができ、それぞれ一価の有機基を表し、b及びcは独立して同じであるか若しくは異なることができ、それぞれ0〜3の数である);又はそれらの組み合せ
によって表される化合物の群より選択された1つ又は複数のシラン化合物の加水分解及び縮合生成物をさらに含んで成る、請求項11に記載の混合物。 - 前記混合物が触媒をさらに含んで成る、請求項11に記載の混合物。
- 前記触媒がハライドを含有しない酸触媒を含んで成る、請求項13に記載の混合物。
- 請求項1に記載の混合物から生成された、シリカに基づいた材料。
- 前記材料の回折パターンが10Åを超えるd間隔で回折ピークを示さない、請求項15に記載の材料。
- 前記材料の回折パターンが10Åを超えるd間隔で回折ピークを示す、請求項15に記載の材料。
- 前記材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約16GPa以上である、請求項15に記載の材料。
- 前記材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約22GPa以上である、請求項18に記載の材料。
- 前記材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約34GPa以上である、請求項19に記載の材料。
- 前記誘電率が2.1以下である、請求項15に記載の材料。
- 2.2以下の誘電率を有する誘電体膜を形成するための方法であって、
少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有する少なくとも1つのシリカ源、並びに少なくとも1つのポロゲンを含んで成る混合物を提供すること;
基材上に該混合物を堆積させて被覆された基材を形成すること;
該ポロゲンの少なくとも一部を除去して多孔質膜を形成するのに十分な時間及び少なくとも1つの温度で以って、1つ又は複数のエネルギー源を用いて該被覆された基材を硬化する硬化工程;並びに
該多孔質膜内の該水素原子の少なくとも一部を除去して該誘電体膜を提供するのに十分な電離放射線源に該多孔質膜をさらす露光工程
を含んで成る、2.2以下の誘電率を有する誘電体膜を形成するための方法。 - 前記硬化工程のエネルギー源が、熱源、α粒子、β粒子、γ線、X線、高エネルギー電子、電子ビーム、紫外光、可視光、赤外光、マイクロ波、高周波波長、プラズマ又はそれらの2種以上から成る群より選択された少なくとも1つである、請求項22に記載の方法。
- 前記露光工程の電離放射線源が、α粒子、β粒子、γ線、X線、高エネルギー電子、電子ビーム又はそれらの2種以上から成る群より選択された少なくとも1つである、請求項22に記載の方法。
- 前記電離放射線源が電子ビームである、請求項24に記載の方法。
- 前記電子ビームの加速電圧が17kV以下である、請求項25に記載の方法。
- 前記電子ビームの加速電圧が10kV以下である、請求項26に記載の方法。
- 前記硬化工程が450℃以下の温度で実施される、請求項22に記載の方法。
- 前記硬化工程が400℃以下の温度で実施される、請求項28に記載の方法。
- 前記硬化工程が約30分以下の時間実施される、請求項22に記載の方法。
- 前記硬化工程が約15分以下の時間実施される、請求項30に記載の方法。
- 前記硬化工程が約6分以下の時間実施される、請求項31に記載の方法。
- 前記硬化工程の少なくとも一部が、前記露光工程の少なくとも一部の間に実施される、請求項22に記載の方法。
- 前記露光工程中の前記基材の温度が100〜450℃である、請求項22に記載の方法。
- 請求項22に記載の方法によって形成された誘電体膜。
- 前記誘電体膜が、ケイ素−炭素結合、炭素−炭素結合、ケイ素−酸素結合、及びケイ素−水素結合から成る群より選択された1つ又は複数の結合タイプを有する、請求項35に記載の誘電体膜。
- 材料の回折パターンが10Åを超えるd間隔で回折ピークを示さない、請求項35に記載の膜。
- 材料の回折パターンが10Åを超えるd間隔で回折ピークを示す、請求項35に記載の膜。
- 材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約16GPa以上である、請求項35に記載の膜。
- 前記材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約22GPa以上である、請求項39に記載の膜。
- 前記材料の誘電率に部分的に由来する標準化壁体弾性率(E0’)が約34GPa以上である、請求項40に記載の膜。
- 誘電率が2.1以下である、請求項35に記載の膜。
- 前記誘電体膜が、集積回路内の絶縁層、層間誘電層、金属間誘電層、キャッピング層、化学機械平坦化層、バリヤー層、又は付着層である、請求項35に記載の誘電体膜。
- 少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有する少なくとも1つのシリカ源を含んで成る多孔質材料を、多孔質膜内の該水素原子の少なくとも一部を除去して誘電体材料を提供するのに十分な電離放射線源にさらすことを含んで成る、誘電体膜を形成するための方法であって、該誘電体材料が、ケイ素−炭素結合、炭素−炭素結合、ケイ素−酸素結合、及びケイ素−水素結合から成る群より選択された1つ又は複数の結合タイプを有する、誘電体材料を形成するための方法。
- 前記多孔質材料が0.4を超える空隙率を有する、請求項44に記載の方法。
- 前記多孔質材料が0.5を超える空隙率を有する、請求項45に記載の方法。
- 前記多孔質材料が0.6を超える空隙率を有する、請求項46に記載の方法。
- 前記電離放射線源が電子ビームである、請求項44に記載の方法。
- 前記電子ビームの加速電圧が17kV以下である、請求項48に記載の方法。
- 前記誘電体材料の誘電率に部分的に由来する該誘電体材料の標準化壁体弾性率(E0’)が約16GPa以上である、請求項44に記載の方法。
- 前記誘電体材料の誘電率に部分的に由来する該誘電体材料の標準化壁体弾性率(E0’)が約22GPa以上である、請求項50に記載の方法。
- 前記誘電体材料の誘電率に部分的に由来する該誘電体材料の標準化壁体弾性率(E0’)が約32GPa以上である、請求項51に記載の方法。
- 前記誘電体材料の誘電率に部分的に由来する該誘電体材料の標準化壁体弾性率(E0’)が約37GPa以上である、請求項52に記載の方法。
- 前記誘電体材料が炭素−炭素結合を有する、請求項44に記載の方法。
- 2.1〜3.7の誘電率と、材料の誘電率に部分的に由来する約32GPa以上の標準化壁体弾性率(E0’)とを有する、多孔質のシリカに基づいた材料を形成するための混合物であって、
少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有し、該有機基内の少なくとも1つの水素原子が電離放射線源への露光によって除去可能である少なくとも1つのシリカ源;並びに
[少なくとも1つのポロゲン質量]/[少なくとも1つのポロゲン質量及び少なくとも1つのシリカ源によって与えられたSiO2質量]の比が0.15以上である少なくとも1つのポロゲン
を含んで成る、多孔質のシリカに基づいた材料を形成するための混合物。 - 前記材料の標準化壁体弾性率が約37GPa以上である、請求項55に記載の混合物。
- 前記材料の誘電率が2.4よりも大きい、請求項55に記載の混合物。
- 2.2〜3.7の誘電率を有する誘電体膜を形成するための方法であって、
少なくとも1つのケイ素原子と、該ケイ素原子に結合した炭素及び水素原子を含んで成る有機基とを有する少なくとも1つのシリカ源、並びに少なくとも1つのポロゲンを含んで成る混合物を提供すること;
基材上に該混合物を堆積させて被覆された基材を形成すること;
該ポロゲンの少なくとも一部を除去して多孔質膜を形成するのに十分な時間及び少なくとも1つの温度で以って、1つ又は複数のエネルギー源を用いて該被覆された基材を硬化すること;並びに
該多孔質膜内の該水素原子の少なくとも一部を除去して該誘電体膜を提供するのに十分な電離放射線源に該多孔質膜をさらすこと
を含んで成る、2.2〜3.7の誘電率を有する誘電体膜を形成するための方法。 - 前記誘電体材料の誘電率に部分的に由来する該誘電体材料の標準化壁体弾性率(E0’)が約32GPa以上である、請求項58に記載の方法。
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JP2013518982A (ja) * | 2010-02-09 | 2013-05-23 | ソガンデハッキョー・サンハックヒョップリョックダン | 高温オゾン処理を含むナノ細孔の超低誘電薄膜の製造方法及びこれによって製造されたナノ細孔の超低誘電薄膜 |
US9679761B2 (en) | 2010-02-09 | 2017-06-13 | Industry-University Cooperation Foundation | Method for preparing a nanoporous ultra-low dielectric thin film including a high-temperature ozone treatment and a nanoporous ultra-low dielectric thin film prepared by the same method |
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Publication number | Publication date |
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EP1832351A2 (en) | 2007-09-12 |
ATE413930T1 (de) | 2008-11-15 |
JP4028512B2 (ja) | 2007-12-26 |
EP1832351B1 (en) | 2008-11-12 |
EP1837086A3 (en) | 2007-12-05 |
SG113504A1 (en) | 2005-08-29 |
TW200640785A (en) | 2006-12-01 |
TW200420493A (en) | 2004-10-16 |
US20050260420A1 (en) | 2005-11-24 |
EP1832351A3 (en) | 2007-12-05 |
TWI299321B (en) | 2008-08-01 |
EP1464410A1 (en) | 2004-10-06 |
DE602004017794D1 (de) | 2008-12-24 |
EP1837086A2 (en) | 2007-09-26 |
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