EP1546437A2 - Films minces en materiaux oxydiques a constante dielectrique elevee - Google Patents
Films minces en materiaux oxydiques a constante dielectrique eleveeInfo
- Publication number
- EP1546437A2 EP1546437A2 EP03757799A EP03757799A EP1546437A2 EP 1546437 A2 EP1546437 A2 EP 1546437A2 EP 03757799 A EP03757799 A EP 03757799A EP 03757799 A EP03757799 A EP 03757799A EP 1546437 A2 EP1546437 A2 EP 1546437A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- substrate
- glycol mono
- suspension
- coating
- ether
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000000463 material Substances 0.000 title description 6
- 239000010409 thin film Substances 0.000 title description 2
- 239000000725 suspension Substances 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011248 coating agent Substances 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 14
- 239000010419 fine particle Substances 0.000 claims abstract 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 23
- -1 glycol ethers Chemical class 0.000 claims description 9
- 239000000375 suspending agent Substances 0.000 claims description 4
- 150000001298 alcohols Chemical class 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 19
- 239000010936 titanium Substances 0.000 description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical group CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 239000000203 mixture Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- YJTIFIMHZHDNQZ-UHFFFAOYSA-N 2-[2-(2-methylpropoxy)ethoxy]ethanol Chemical compound CC(C)COCCOCCO YJTIFIMHZHDNQZ-UHFFFAOYSA-N 0.000 description 4
- HCGFUIQPSOCUHI-UHFFFAOYSA-N 2-propan-2-yloxyethanol Chemical compound CC(C)OCCO HCGFUIQPSOCUHI-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 4
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 4
- 229940046892 lead acetate Drugs 0.000 description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 4
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 3
- HHAPGMVKBLELOE-UHFFFAOYSA-N 2-(2-methylpropoxy)ethanol Chemical compound CC(C)COCCO HHAPGMVKBLELOE-UHFFFAOYSA-N 0.000 description 3
- HRWADRITRNUCIY-UHFFFAOYSA-N 2-(2-propan-2-yloxyethoxy)ethanol Chemical compound CC(C)OCCOCCO HRWADRITRNUCIY-UHFFFAOYSA-N 0.000 description 3
- DJCYDDALXPHSHR-UHFFFAOYSA-N 2-(2-propoxyethoxy)ethanol Chemical compound CCCOCCOCCO DJCYDDALXPHSHR-UHFFFAOYSA-N 0.000 description 3
- YEYKMVJDLWJFOA-UHFFFAOYSA-N 2-propoxyethanol Chemical compound CCCOCCO YEYKMVJDLWJFOA-UHFFFAOYSA-N 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- BDLXTDLGTWNUFM-UHFFFAOYSA-N 2-[(2-methylpropan-2-yl)oxy]ethanol Chemical compound CC(C)(C)OCCO BDLXTDLGTWNUFM-UHFFFAOYSA-N 0.000 description 2
- GICQWELXXKHZIN-UHFFFAOYSA-N 2-[2-[(2-methylpropan-2-yl)oxy]ethoxy]ethanol Chemical compound CC(C)(C)OCCOCCO GICQWELXXKHZIN-UHFFFAOYSA-N 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- KQNKJJBFUFKYFX-UHFFFAOYSA-N acetic acid;trihydrate Chemical compound O.O.O.CC(O)=O KQNKJJBFUFKYFX-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 2
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 229960004592 isopropanol Drugs 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 230000015654 memory Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- WYIXXSYDQFHKFE-UHFFFAOYSA-L strontium;dihydroxide;hydrate Chemical compound O.[OH-].[OH-].[Sr+2] WYIXXSYDQFHKFE-UHFFFAOYSA-L 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- KKQVUWHSUOGDEI-UHFFFAOYSA-N 2-(2-butan-2-yloxyethoxy)ethanol Chemical compound CCC(C)OCCOCCO KKQVUWHSUOGDEI-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- QUVMSYUGOKEMPX-UHFFFAOYSA-N 2-methylpropan-1-olate;titanium(4+) Chemical compound [Ti+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] QUVMSYUGOKEMPX-UHFFFAOYSA-N 0.000 description 1
- YMJMHACKPJBWMC-UHFFFAOYSA-N 2-methylpropan-1-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-].CC(C)C[O-] YMJMHACKPJBWMC-UHFFFAOYSA-N 0.000 description 1
- GRWPYGBKJYICOO-UHFFFAOYSA-N 2-methylpropan-2-olate;titanium(4+) Chemical compound [Ti+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] GRWPYGBKJYICOO-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VNSWULZVUKFJHK-UHFFFAOYSA-N [Sr].[Bi] Chemical compound [Sr].[Bi] VNSWULZVUKFJHK-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 229940049676 bismuth hydroxide Drugs 0.000 description 1
- TZSXPYWRDWEXHG-UHFFFAOYSA-K bismuth;trihydroxide Chemical compound [OH-].[OH-].[OH-].[Bi+3] TZSXPYWRDWEXHG-UHFFFAOYSA-K 0.000 description 1
- BSDOQSMQCZQLDV-UHFFFAOYSA-N butan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] BSDOQSMQCZQLDV-UHFFFAOYSA-N 0.000 description 1
- HWCXFDGMZPRMRX-UHFFFAOYSA-N butan-2-olate;titanium(4+) Chemical compound CCC(C)O[Ti](OC(C)CC)(OC(C)CC)OC(C)CC HWCXFDGMZPRMRX-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical class O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- ITNVWQNWHXEMNS-UHFFFAOYSA-N methanolate;titanium(4+) Chemical compound [Ti+4].[O-]C.[O-]C.[O-]C.[O-]C ITNVWQNWHXEMNS-UHFFFAOYSA-N 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- WEMICRSBTLTNGT-UHFFFAOYSA-N pentan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCC[O-].CCCCC[O-].CCCCC[O-].CCCCC[O-] WEMICRSBTLTNGT-UHFFFAOYSA-N 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- HSXKFDGTKKAEHL-UHFFFAOYSA-N tantalum(v) ethoxide Chemical compound [Ta+5].CC[O-].CC[O-].CC[O-].CC[O-].CC[O-] HSXKFDGTKKAEHL-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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
- H01L21/02172—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
- H01L21/02197—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 the material having a perovskite structure, e.g. BaTiO3
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/10—Coating starting from inorganic powder by application of heat or pressure and heat with intermediate formation of a liquid phase in the layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
- C01G35/006—Compounds containing, besides tantalum, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/468—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
- C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/47—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on strontium titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/475—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on bismuth titanates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
- C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
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Definitions
- the present invention relates to a method for coating a substrate by coating a finely divided, stable suspension of crystalline oxide particles on the substrate, which may need to be tempered, evaporating the suspension medium and sintering at elevated temperature.
- Oxidic materials with a high dielectric constant such as barium titanate, strontium titanate, mixed titanates made of barium and strontium, lead zircon titanates or strontium bismuth tantalate are used as dielectrics or ferroelectrics for memory chips in microelectronics.
- These materials act as a dielectric on a substrate if they are applied as a film in layer thicknesses of approximately 100 nm in crystalline form. To produce a film, a temperature treatment at 300 to 1000 ° C must be carried out.
- the object of the present invention was therefore to remedy the disadvantages mentioned above.
- a new and improved method for coating a substrate which is characterized in that a finely divided suspension of crystalline oxide particles is applied to a substrate by coating, the suspension medium is evaporated and the coating is sintered on the substrate.
- the method according to the invention can be carried out as follows:
- the oxide suspensions can be sprayed onto a substrate by means of a suitable device, such as spray nozzles, which is optionally heated to such a high temperature that the suspension medium evaporates. Evaporation can also be carried out in a separate step by subsequent heating.
- a homogeneous spray cone can be achieved by coupling the spray nozzle (s) to an ultrasonic oscillator or by superimposing an ultrasonic oscillation during metering or by metering the suspension onto a suitably shaped ultrasonic oscillator.
- the spraying of the optionally moderately tempered (temperature from room temperature to below the boiling point of the suspension medium) suspension can be achieved in a two-component nozzle by means of an auxiliary gas (such as nitrogen or argon) and / or by supporting the spraying process, for example, by superimposed ultrasonic vibrations.
- an auxiliary gas such as nitrogen or argon
- Coating can be carried out by spraying or by a spin-on process, in which a certain amount of flowable suspension is metered in at any point, for example in the center, of a rotating substrate and the suspension is distributed uniformly over the substrate due to the centrifugal force.
- the system can be heated to the crystallization temperature adequate for the oxide and the desired coherent film can be produced by sintering together the nano-particles.
- the sintering temperatures for nanoparticles are generally well below the sintering temperature for particles on the micrometer scale.
- the sintering temperature for nanoparticles is approx. 750 ° C in contrast to micrometer particles (grain sizes of 2 to 5 ⁇ m) at approx. 1350 ° C.
- the oxide particles In the suspensions of finely divided, crystalline oxide particles, water or organic suspension media are generally used, which give the oxide particles an average particle size of 0.5 to 9.9 nm, preferably 0.6 to 9 nm, particularly preferably 1 to 8 nm contain.
- Wafers made of high-purity silicon, which are already structured, are generally suitable as substrates, the structuring taking place according to the known “damascene” process.
- the actual substrate layers are electrically conductive layers that are created in the Damascene process.
- Suitable organic suspending agents are generally polar organic suspending agents, especially aliphatic alcohols, ether alcohols or their mixtures with a boiling point below approximately 300 ° C. under normal pressure. These can be used in anhydrous form or, preferably, in commercially available aqueous form.
- Suitable alcohols are C ⁇ ⁇ to Cs-alkanols, preferably C ⁇ ⁇ to C -alkanols such as methanol, ethanol, n-propanol, iso-propanol, n-butanol, iso-butanol, sec-butanol or tert.
- -Butanol particularly preferably C ⁇ ⁇ to C -alkanol such as methanol, ethanol, n-propanol or iso-propanol, especially methanol or ethanol.
- Suitable ether alcohols are all known glycol ethers, for example ethylene glycol mono-methyl ether, ethylene glycol mono-ethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mino-n-butyl ether, ethylene glycol ono -iso-butyl ether, ethylene glycol mono-sec.
- -butyl ether diethylene glycol tert-butyl ether, preferably ethylene glycol mono-ethyl ether, ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mono-n-butyl ether, ethylene glycol mono -iso-butyl ether, ethylene glycol mono-sec. -butyl ether, ethylene glycol tert.
- -butyl ether diethylene glycol mono-ethyl ether, diethylene glycol mono-n-propyl ether, diethylene glycol mono-isopropyl ether, diethylene glycol mono-n-butyl ether, diethylene glycol mono-iso-butyl ether, diethylene glycol mono-sec. butyl ether and diethylene glycol tert-butyl ether, particularly preferably ethylene glycol mono-n-propyl ether, ethylene glycol mono-iso-propyl ether, ethylene glycol mono-n-butyl ether, ethylene glycol mono-iso-butyl ether, ethylene glycol mono-sec. -butyl ether, ethylene glycol tert.
- butyl ether diethylene glycol mono-n-propyl ether, diethylene glycol mono-iso-propyl ether, diethylene glycol mono-n-butyl ether, Diethylene glycol mono-iso-butyl ether, diethylene glycol mono-sec. - Butyl ether and diethylene glycol ter. -butyl ether, especially ethylene glycol mono-iso-propyl ether, ethylene glycol mono-iso-butyl ether, ethylene glycol tert-butyl ether, diethylene glycol 5-mono-iso-propyl ether, diethylene glycol mono-iso-butyl ether and diethylene glycol tert. -butyl ether.
- the solids content of the suspensions can be varied within wide limits, is generally 1 to 35% by weight, preferably 10 5 to 25% by weight, and can be adjusted in the synthesis of the suspensions or subsequently by dilution or concentration.
- the nanocrystalline oxide suspensions can be produced as follows:
- Titanium alcoholates can be introduced in an alkanol, a glycol ether or mixtures thereof and at a temperature of 50 to 150 ° C, preferably 60 to 120 ° C, particularly preferably 20 70 to 110 ° C, in particular at the reflux temperature and a pressure of 0.1 up to 3 bar, preferably 0.5 to 2 bar, particularly preferably at atmospheric pressure (normal pressure) with barium or strontium hydroxide hydrate.
- the concentration of the alcoholic titanium alcoholate solution can be varied within wide limits.
- the concentration is preferably 50 to 800 g / liter, particularly preferably 100 to 600 g / liter, very particularly preferably 200 to 400 g / liter.
- hydroxide hydrates are suitable as barium or strontium hydroxide hydrates, e.g. Barium or strontiu - hydroxide octahydra.
- Suitable titanium alcoholates are, for example, titanium tetra-methanolate, titanium tetraethanolate, titanium tetra-n-propanolate, titanium tetra-iso-propanolate, titanium tetra-n-butanolate, titanium tetra-iso-butanolate, titanium tetra-sec-butanolate, titanium tetra-tert. -butanolate, titanium tetra-n-pentanolate and titanium tetra-
- iso-pentanolate preferably titanium tetraethanolate, titanium tetra-n-propanolate, titanium butanolate, titanium tetra-sec. -butanolate and titanium tetra-tert-butanolate, particularly preferably titanium tetra-n-propanolate, titanium tetra-iso-propanolate, titanium tetra-n-butanolate and titrantetra-iso-butanolate or mixtures thereof.
- the commercially available alkoxides preferably zirconium tetraisobutylate and / or zirconium tetra-n-butoxide, are used as zirconium alkoxides.
- lead acetate trihydrate is generally used as the lead component, or a mixture of the basic lead acetate [Pb (OAc) 2 »Pb (OH) 2 ].
- the proportion of the water of reaction can be predetermined by the mixing ratio of lead acetate trihydrate and basic lead acetate, the acetate residues being split off as acetic acid and this, together with the alcohol present as a component in the suspension medium, providing further water with ester formation.
- the addition of small amounts of additional acetic acid to form water of reaction may be advantageous.
- the commercially available tantalum pentaethoxide Ta (OC 2 H 5 ) 5 is generally used as the alkoxide, preferably Sr (OH) 8H 2 0 as the Sr component, optionally in a mixture with anhydrous Sr (0H) , and as bismuth component Bi (OCOCH 3 ) 3 or bismuth hydroxide Bi (0H) 3 .
- Bi 4 _ x La x Ti 3 0 ⁇ is generally produced using anhydrous lithium hydroxide as the Li component and titanium alcoholates as listed above as the titanium component.
- An advantageous embodiment consists in that no additional water other than the water from the components and the suspending agent is introduced into the reaction in the oxide suspensions.
- doping elements such as Mg, Ca, Zn, Zr, V, Nb, Ta, Bi, Cr, Mo, W, Mn, Fe, Co, Ni, Pb, Ce, or mixtures thereof, preferably Mg, Ca, Cr, Fe , Co, Ni, Pb or mixtures thereof, for example in the form of their hydroxides, oxides, carbonates, carboxylates or nitrates.
- the mixed oxides produced according to the invention generally have an average particle diameter of less than 10 nm, preferably 5 to 9.9 nm, particularly preferably 0.6 to 9 nm, in particular 1 to 8 nm.
- DRAMs Dynamic Random Access Memories
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Abstract
La présente invention concerne un procédé pour revêtir un substrat, selon lequel une suspension de fines particules d'oxyde cristallines est appliquée sur un substrat, l'agent de suspension est vaporisé et le revêtement est fritté sur le substrat.
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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DE10244285 | 2002-09-23 | ||
DE10244285A DE10244285A1 (de) | 2002-09-23 | 2002-09-23 | Dünne Filme oxidischer Materialien mit hoher Dielektrizitätskonstante |
DE10260091A DE10260091A1 (de) | 2002-12-19 | 2002-12-19 | Dünne Filme oxidischer Materialien mit hoher Dielektrizitätskonstante |
DE10260091 | 2002-12-19 | ||
PCT/EP2003/009945 WO2004028999A2 (fr) | 2002-09-23 | 2003-09-08 | Films minces en materiaux oxydiques a constante dielectrique elevee |
Publications (1)
Publication Number | Publication Date |
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EP1546437A2 true EP1546437A2 (fr) | 2005-06-29 |
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP03757799A Withdrawn EP1546437A2 (fr) | 2002-09-23 | 2003-09-08 | Films minces en materiaux oxydiques a constante dielectrique elevee |
Country Status (8)
Country | Link |
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US (1) | US20050220993A1 (fr) |
EP (1) | EP1546437A2 (fr) |
JP (1) | JP4183681B2 (fr) |
KR (1) | KR20050057540A (fr) |
CN (1) | CN100471996C (fr) |
AU (1) | AU2003273836A1 (fr) |
TW (1) | TWI291903B (fr) |
WO (1) | WO2004028999A2 (fr) |
Families Citing this family (4)
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US6737364B2 (en) * | 2002-10-07 | 2004-05-18 | International Business Machines Corporation | Method for fabricating crystalline-dielectric thin films and devices formed using same |
EP2282198A1 (fr) * | 2004-11-24 | 2011-02-09 | Sensirion Holding AG | Procédé for appliquer une couche sur un substrat |
FI122009B (fi) * | 2007-06-08 | 2011-07-15 | Teknologian Tutkimuskeskus Vtt | Nanopartikkeleihin perustuvat rakenteet ja menetelmä niiden valmistamiseksi |
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2003
- 2003-09-08 AU AU2003273836A patent/AU2003273836A1/en not_active Abandoned
- 2003-09-08 WO PCT/EP2003/009945 patent/WO2004028999A2/fr active Application Filing
- 2003-09-08 KR KR1020057004899A patent/KR20050057540A/ko not_active Application Discontinuation
- 2003-09-08 EP EP03757799A patent/EP1546437A2/fr not_active Withdrawn
- 2003-09-08 CN CNB038226170A patent/CN100471996C/zh not_active Expired - Fee Related
- 2003-09-08 JP JP2004538872A patent/JP4183681B2/ja not_active Expired - Fee Related
- 2003-09-08 US US10/527,548 patent/US20050220993A1/en not_active Abandoned
- 2003-09-09 TW TW092124896A patent/TWI291903B/zh active
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Title |
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See references of WO2004028999A2 * |
Also Published As
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US20050220993A1 (en) | 2005-10-06 |
AU2003273836A8 (en) | 2004-04-19 |
TWI291903B (en) | 2008-01-01 |
JP2006500777A (ja) | 2006-01-05 |
CN100471996C (zh) | 2009-03-25 |
AU2003273836A1 (en) | 2004-04-19 |
WO2004028999A2 (fr) | 2004-04-08 |
TW200406263A (en) | 2004-05-01 |
WO2004028999B1 (fr) | 2004-06-17 |
WO2004028999A3 (fr) | 2004-05-13 |
KR20050057540A (ko) | 2005-06-16 |
JP4183681B2 (ja) | 2008-11-19 |
CN1685082A (zh) | 2005-10-19 |
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