WO2011058816A1 - Cmp研磨液、並びに、これを用いた研磨方法及び半導体基板の製造方法 - Google Patents
Cmp研磨液、並びに、これを用いた研磨方法及び半導体基板の製造方法 Download PDFInfo
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- WO2011058816A1 WO2011058816A1 PCT/JP2010/065863 JP2010065863W WO2011058816A1 WO 2011058816 A1 WO2011058816 A1 WO 2011058816A1 JP 2010065863 W JP2010065863 W JP 2010065863W WO 2011058816 A1 WO2011058816 A1 WO 2011058816A1
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- Prior art keywords
- polishing
- polishing liquid
- cmp polishing
- cerium oxide
- mass
- Prior art date
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- 238000005498 polishing Methods 0.000 title claims abstract description 352
- 239000007788 liquid Substances 0.000 title claims abstract description 180
- 238000000034 method Methods 0.000 title claims description 52
- 239000000758 substrate Substances 0.000 title claims description 50
- 239000004065 semiconductor Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 18
- 239000002245 particle Substances 0.000 claims abstract description 88
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 83
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 31
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- 150000003839 salts Chemical class 0.000 claims abstract description 17
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- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 42
- 150000001875 compounds Chemical class 0.000 claims description 29
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- 238000002156 mixing Methods 0.000 claims description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- LXOFYPKXCSULTL-UHFFFAOYSA-N 2,4,7,9-tetramethyldec-5-yne-4,7-diol Chemical compound CC(C)CC(C)(O)C#CC(C)(O)CC(C)C LXOFYPKXCSULTL-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 239000000654 additive Substances 0.000 description 53
- 230000000996 additive effect Effects 0.000 description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 30
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
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- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 4
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
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- 150000003863 ammonium salts Chemical class 0.000 description 3
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- 238000005268 plasma chemical vapour deposition Methods 0.000 description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 101100107923 Vitis labrusca AMAT gene Proteins 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001345 alkine derivatives Chemical class 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
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- 238000002955 isolation Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- 229920000058 polyacrylate Polymers 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
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- 230000001681 protective effect Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- JTACNIAVBSQMCU-UHFFFAOYSA-N 2,4-dimethylhex-5-yn-3-ol Chemical compound CC(C)C(O)C(C)C#C JTACNIAVBSQMCU-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- NUYADIDKTLPDGG-UHFFFAOYSA-N 3,6-dimethyloct-4-yne-3,6-diol Chemical compound CCC(C)(O)C#CC(C)(O)CC NUYADIDKTLPDGG-UHFFFAOYSA-N 0.000 description 1
- PQUCIEFHOVEZAU-UHFFFAOYSA-N Diammonium sulfite Chemical compound [NH4+].[NH4+].[O-]S([O-])=O PQUCIEFHOVEZAU-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001785 cerium compounds Chemical class 0.000 description 1
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
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- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- ILLHQJIJCRNRCJ-UHFFFAOYSA-N dec-1-yne Chemical compound CCCCCCCCC#C ILLHQJIJCRNRCJ-UHFFFAOYSA-N 0.000 description 1
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- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000005677 ethinylene group Chemical group [*:2]C#C[*:1] 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
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- 125000000466 oxiranyl group Chemical group 0.000 description 1
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- 239000011496 polyurethane foam Substances 0.000 description 1
- BHZRJJOHZFYXTO-UHFFFAOYSA-L potassium sulfite Chemical compound [K+].[K+].[O-]S([O-])=O BHZRJJOHZFYXTO-UHFFFAOYSA-L 0.000 description 1
- 235000019252 potassium sulphite Nutrition 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
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- 239000010980 sapphire Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
Definitions
- the present invention relates to a CMP polishing liquid, a polishing method using the same, and a method for manufacturing a semiconductor substrate.
- the present invention is used in a flattening process of a substrate surface in an electronic component manufacturing technology such as a semiconductor element, for example, a flattening process of an interlayer insulating film, a forming process of STI (Shallow Trench Isolation), etc.
- the present invention relates to a CMP polishing liquid, a polishing method using the same, and a method for manufacturing a semiconductor substrate.
- a CMP (chemical mechanical polishing) technique is an example of a technique that satisfies such a demand for strict miniaturization.
- the CMP technique can flatten the surface of a layer to be exposed in the manufacturing process of an electronic component such as a semiconductor device, reduce the technical burden in the exposure process, and stabilize the yield. Therefore, the CMP technique is an essential technique when, for example, planarizing an interlayer insulating film, forming an STI, or the like.
- a silica-based CMP polishing liquid containing fumed silica has been studied.
- the silica-based CMP polishing liquid is produced by growing particles by a method such as thermally decomposing silica particles into tetrachlorosilicic acid and adjusting the pH.
- such a CMP polishing liquid has a technical problem that the polishing rate of the inorganic insulating film as the film to be polished is lowered.
- a CMP polishing liquid containing cerium oxide particles is used as a CMP polishing liquid for glass surfaces such as photomasks and lenses. Since cerium oxide particles have a lower hardness than silica particles and alumina particles, even if used for polishing, the surface to be polished is less likely to be damaged. Accordingly, the cerium oxide particles are useful for finish mirror polishing. Further, the CMP polishing liquid containing cerium oxide particles has an advantage that the polishing rate is superior to the CMP polishing liquid containing silica particles. In recent years, a CMP polishing liquid for semiconductors using high-purity cerium oxide particles is known (see, for example, Patent Document 1).
- cerium oxide particles have a higher density than silica particles, they tend to settle, and the polishing rate may decrease. Therefore, from the viewpoint of improving the polishing rate, a CMP polishing liquid in which dispersibility of cerium oxide particles is improved by using an appropriate dispersant is known (see, for example, Patent Document 2).
- the mounting density of integrated circuits tends to be further increased.
- the CMP polishing liquid containing cerium oxide particles has the advantage that there are fewer polishing flaws than the CMP polishing liquid containing silica particles as described above, the conventional level of polishing flaw reduction is not sufficient. The demand for reducing polishing flaws is becoming more severe.
- a technique for reducing polishing scratches as a technique for reducing polishing scratches, a technique for removing impurities in cerium oxide particles, a technique for reducing the particle diameter of cerium oxide particles, and a method for removing large particles.
- Methods are being studied.
- problems such as a decrease in flatness of the surface to be polished and a polishing rate occur, and it may be difficult to suppress the generation of polishing flaws and other characteristics.
- a decrease in the polishing rate causes a decrease in throughput, it is desired to suppress the decrease in the polishing rate and suppress the generation of polishing flaws.
- the present invention has been made to solve the above-described problem, and a CMP polishing liquid capable of suppressing a decrease in polishing rate and suppressing generation of polishing flaws, a polishing method using the same, and a semiconductor substrate It aims at providing the manufacturing method of.
- the inventors of the present invention have intensively studied.
- the CMP polishing liquid containing cerium oxide particles contains a trace amount of an organic compound having an acetylene bond. It has been found that the reduction of the polishing rate can be suppressed and the generation of polishing flaws can be suppressed.
- the first aspect of the CMP polishing liquid according to the present invention includes cerium oxide particles, an organic compound having an acetylene bond, and water, and the content of the organic compound having an acetylene bond is such that the total mass of the CMP polishing liquid is It is 0.00001 mass% (0.1 ppm) or more and 0.01 mass% (100 ppm) or less on the basis.
- the CMP polishing liquid contains a very small amount of an organic compound having an acetylene bond as described above, thereby suppressing a decrease in polishing speed and suppressing generation of polishing flaws. Can do. Further, in the first aspect of the CMP polishing liquid, the flatness improving effect (the effect of preferentially polishing the convex portion) is promoted in polishing of the surface to be polished with less unevenness and polishing for roughing the surface to be polished. You can also.
- Patent Document 4 discloses that the flatness of the polished surface after polishing is improved by adding an organic compound having an acetylene bond.
- the present inventors presume that, based on the difference in the content of the organic compound having an acetylene bond, the present invention and the technique of Patent Document 4 are essentially different in the action that occurs during polishing.
- the content of the organic compound having an acetylene bond is high, whereas in the first aspect of the CMP polishing liquid according to the present invention, the content of the organic compound having an acetylene bond is high. Trace amount (ppm order). Therefore, in the CMP polishing liquid of Patent Document 4, there is a limit to highly satisfying both the effect of improving the polishing rate by the organic compound having an acetylene bond and the effect of reducing polishing scratches, whereas the CMP according to the present invention is limited. In the first aspect of the polishing liquid, both the effect of improving the polishing rate and the effect of reducing polishing flaws can be achieved at a high level.
- the first aspect of the CMP polishing liquid can be obtained by mixing a first liquid containing cerium oxide particles and water and a second liquid containing an organic compound having an acetylene bond and water.
- the present inventors can also polish by adding a trace amount of an organic compound having an acetylene bond to a CMP polishing liquid containing cerium oxide particles and a predetermined anionic polymer compound or a salt thereof. It has been found that the decrease in speed can be suppressed and the generation of polishing flaws can be suppressed.
- a composition containing cerium oxide particles, an organic compound having an acetylene bond, and a vinyl compound having an anionic substituent as monomer components is polymerized.
- the content of the organic compound containing an anionic polymer compound or a salt thereof obtained and water and having an acetylene bond is 0.000001 mass% (0.01 ppm) or more and 0.05 mass based on the total mass of the CMP polishing liquid. % (500 ppm).
- the CMP polishing liquid contains a trace amount of the organic compound having an acetylene bond as described above, and also contains a predetermined anionic polymer compound or a salt thereof. It is possible to suppress a decrease in the polishing rate and suppress the generation of polishing flaws. Further, in the second aspect of the CMP polishing liquid, it is possible to polish a surface to be polished with many irregularities with good flatness.
- the second aspect of the CMP polishing liquid includes a third liquid containing cerium oxide particles and water, and a fourth liquid containing an organic compound having an acetylene bond, an anionic polymer compound or a salt thereof, and water. It can also be obtained by mixing.
- the vinyl compound having an anionic substituent is preferably at least one selected from acrylic acid and methacrylic acid. In this case, it is possible to suppress the decrease in the polishing rate and further suppress the generation of polishing flaws.
- the content of the anionic polymer compound or a salt thereof is preferably larger than the content of the organic compound having an acetylene bond. In this case, it is possible to suppress the decrease in the polishing rate and further suppress the generation of polishing flaws.
- the content of the anionic polymer compound or a salt thereof is preferably 0.01 to 2.00% by mass based on the total mass of the CMP polishing liquid. In this case, it is possible to suppress the decrease in the polishing rate and further suppress the generation of polishing flaws.
- the organic compound having an acetylene bond is preferably acetylene glycols.
- the acetylene glycol is more preferably a compound represented by the following general formula (1), more preferably 2,4,7,9-tetramethyl-5-decyne-4,7-diol.
- R 1 to R 4 each independently represents a hydrogen atom or a substituted or unsubstituted alkyl group having 1 to 5 carbon atoms
- R 5 and R 6 each independently represents 1 to 5 carbon atoms.
- 5 represents a substituted or unsubstituted alkylene group
- m and n each independently represents 0 or a positive number.
- the polishing method according to the present invention includes a step of polishing a film to be polished formed on a substrate using the CMP polishing liquid.
- the polishing method according to the present invention since the CMP polishing liquid is used, it is possible to suppress a decrease in the polishing rate and to suppress generation of polishing flaws.
- a method for manufacturing a semiconductor substrate according to the present invention includes a step of polishing an inorganic insulating film formed on a semiconductor substrate using the CMP polishing liquid.
- a CMP polishing liquid capable of suppressing a decrease in polishing rate and suppressing generation of polishing flaws, a polishing method using the same, and a method for manufacturing a semiconductor substrate.
- the CMP polishing liquid according to the first embodiment includes cerium oxide particles, an organic compound having an acetylene bond (hereinafter referred to as “acetylene compound”), and water.
- the CMP polishing liquid according to the second embodiment includes an anionic polymer compound obtained by polymerizing a composition containing cerium oxide particles, an acetylene compound, and a vinyl compound having an anionic substituent as a monomer component, or a composition thereof. Contains salt and water.
- each component contained in the CMP polishing liquid will be described.
- cerium oxide particles may be any particles as long as they have a particle shape.
- the production method of the cerium oxide particles is not limited, but conventionally known cerium oxide particles can be widely used in general.
- Examples of the method for producing cerium oxide particles include a firing method, an oxidation method using hydrogen peroxide, and the like.
- a firing method it is preferable to obtain a fired powder by firing the cerium compound at 350 to 900 ° C. for 1 hour or longer in the firing step.
- the firing temperature is more preferably 500 to 900 ° C, and still more preferably 600 to 900 ° C.
- the upper limit of the firing time can be about 3 hours.
- the half-value width of the diffraction peak due to the (111) plane of the cerium oxide crystal is preferably 0.20 to 0.50 °, and preferably 0.20 to 0.40. ° is more preferred.
- cerium oxide particles having an appropriate degree of crystallization and an appropriate crystallite size (minimum crystal unit) can be obtained.
- the half width of the diffraction peak can be appropriately adjusted depending on the firing temperature and firing time in the firing step.
- the pulverization method for example, dry pulverization using a jet mill or the like, or wet pulverization using a planetary bead mill or the like is preferable.
- the jet mill for example, a method described in “Chemical Engineering Journal”, Vol. 6, No. 5, (1980), pages 527 to 532 can be used.
- the cerium oxide particles used as the abrasive grains preferably include polycrystalline cerium oxide particles having crystal grain boundaries.
- the pulverization step it is preferable to pulverize the fired powder so that polycrystalline cerium oxide particles composed of a plurality of crystallites and having crystal grain boundaries are formed. Polycrystalline cerium oxide particles with grain boundaries become fine during polishing, and at the same time, new surfaces (active surfaces) that do not touch the medium appear before each other, so that a high polishing rate for silicon oxide films is achieved at a high level. Can be maintained.
- Such cerium oxide particles are described, for example, in a republished patent WO99 / 31195 pamphlet.
- the average particle size of the cerium oxide particles is not particularly limited, but generally, the smaller the average particle size, the lower the polishing rate, and the larger the average particle size, the more likely to cause polishing flaws. From the viewpoint of further improving the polishing rate, the average particle size is preferably 0.05 ⁇ m or more, and more preferably 0.07 ⁇ m or more. From the viewpoint of further suppressing the generation of polishing flaws, the average particle size is preferably 1.00 ⁇ m or less, and more preferably 0.40 ⁇ m or less.
- the average particle diameter of the cerium oxide particles refers to an average value of volume distribution measured by a laser diffraction / scattering particle size distribution meter with a liquid containing cerium oxide particles as a measurement target.
- the measurement object is the final CMP polishing liquid when the CMP polishing liquid is stored as one liquid, and the slurry containing cerium oxide particles before mixing when the two polishing liquids are stored.
- the average particle size of the cerium oxide particles is obtained by diluting the CMP polishing liquid or slurry to be measured to a concentration suitable for measurement, and supplying this measurement sample to a laser diffraction / scattering particle size distribution analyzer. Can be measured. More specifically, the average particle diameter of the cerium oxide particles can be measured as follows using LA-920 (light source: He—Ne laser and W laser) manufactured by HORIBA, Ltd. First, a measurement polishing sample or a slurry is diluted to a concentration suitable for measurement so that a measurement transmittance (H) with respect to a He—Ne laser is 60 to 70% to obtain a measurement sample. Then, this measurement sample is put into LA-920, and the average particle diameter is obtained as the arithmetic average diameter (mean size) obtained at that time.
- LA-920 light source: He—Ne laser and W laser
- the content of the cerium oxide particles in the CMP polishing liquid is not particularly limited, but the lower limit of the content of the cerium oxide particles is 0.00 on the basis of the total mass of the CMP polishing liquid from the viewpoint of obtaining a better polishing rate. 10 mass% or more is preferable, 0.20 mass% or more is more preferable, and 0.30 mass% or more is still more preferable.
- the upper limit of the content of the cerium oxide particles is preferably 20% by mass or less, more preferably 10% by mass or less, more preferably 5% by mass or less based on the total mass of the CMP polishing liquid from the viewpoint of improving the dispersibility of the particles and further reducing polishing scratches. A mass% or less is more preferable.
- acetylene compound examples include at least one selected from alkynes, acetylene alcohols, and acetylene glycols.
- alkynes examples include 1-decyne and 5-decyne.
- acetylene alcohols examples include 3,5-dimethyl-1-hexyn-3-ol, 2,4-dimethyl-5-hexyn-3-ol, and the like.
- acetylene glycols include compounds represented by the following general formula (1). These acetylene compounds can be used alone or in combination of two or more.
- R 1 to R 4 each independently represents a hydrogen atom or a substituted or unsubstituted alkyl group having 1 to 5 carbon atoms
- R 5 and R 6 each independently represents 1 to 5 carbon atoms
- 5 represents a substituted or unsubstituted alkylene group
- m and n each independently represents 0 or a positive number.
- acetylene glycols are preferable, and a compound represented by the above general formula (1) is more preferable in that an effect of reducing polishing scratches is easily obtained.
- m and n are 0. More preferred are compounds such as 2,4,7,9-tetramethyl-5-decyne-4,7-diol and 3,6-dimethyl-4-octyne-3,6-diol, which are readily available.
- 2,4,7,9-tetramethyl-5-decyne-4,7-diol is very preferable in that it has an excellent polishing scratch reduction effect.
- the lower limit of the content of the first additive is 0.00001% by mass (0.1 ppm) or more based on the total mass of the CMP polishing liquid, and the polishing scratch reduction effect is further improved. From the viewpoint of being efficiently obtained, 0.00002 mass% (0.2 ppm) or more is preferable, 0.00003 mass% (0.3 ppm) or more is more preferable, and 0.00005 mass% (0.5 ppm) or more is more preferable. preferable.
- the upper limit of the content of the first additive is 0.01% by mass (100 ppm) or less based on the total mass of the CMP polishing liquid, and 0.008% by mass from the viewpoint of more efficiently obtaining a polishing scratch reduction effect.
- the content of the first additive when the content of the first additive is 0.00001 mass% or more, it is compared with the case where the first additive is not added at all (content: 0 mass%). As a result, the number of polishing scratches rapidly decreases. In the CMP polishing liquid according to the first embodiment, when the content of the first additive is 0.01% by mass or less, an effect of reducing polishing scratches is easily obtained. Further, the content of the first additive is preferably 0.00001 to 10 parts by mass with respect to 100 parts by mass of the cerium oxide particles.
- the lower limit of the content of the first additive is 0.000001% by mass (0.01 ppm) or more based on the total mass of the CMP polishing liquid, and the polishing scratch reduction effect is further improved.
- 0.000003 mass% (0.03 ppm) or more is preferable, 0.000005 mass% (0.05 ppm) or more is more preferable, and 0.00001 mass% (0.1 ppm) or more is further more preferable.
- 0.00005 mass% (0.5 ppm) or more is particularly preferable.
- the upper limit of the content of the first additive is less than 0.05% by mass (500 ppm) on the basis of the total mass of the CMP polishing liquid, and 0.03% by mass from the viewpoint of more efficiently obtaining a polishing scratch reduction effect. (300 ppm) or less is preferred, 0.02 mass% (200 ppm) or less is more preferred, and 0.01 mass% (100 ppm) or less is even more preferred.
- the content of the first additive is 0.000001% by mass or more, it is compared with the case where the first additive is not added at all (content: 0% by mass). As a result, the number of polishing scratches rapidly decreases.
- the content of the first additive when the content of the first additive is less than 0.05% by mass, an effect of reducing polishing scratches is easily obtained. Further, the content of the first additive is preferably 0.00001 to 50 parts by mass with respect to 100 parts by mass of the cerium oxide particles.
- the second additive forms a protective film by adsorbing to the surface to be polished when polishing the surface to be polished having unevenness, and suppresses the progress of polishing in the recessed portion where the polishing pad does not contact, Is a compound suitable for preferentially polishing.
- the second additive is an anionic polymer compound or a salt thereof obtained by polymerizing a composition containing a vinyl compound having an anionic substituent as a monomer component. is there.
- the second additive adsorbs on the surface to be polished to form a protective film, the generation of polishing scratches tends to be somewhat suppressed, but the effect is not sufficient when used alone.
- a remarkable polishing flaw reduction effect can be obtained by using the first additive and the second additive in combination.
- Examples of the anionic substituent of the vinyl compound having an anionic substituent include a carboxyl group, a hydroxyl group, an amino group, an oxirane ring, and an acid anhydride.
- Examples of the vinyl compound having an anionic substituent include acrylic acid, methacrylic acid, and methyl acrylate. These vinyl compounds can be used alone or in combination of two or more.
- As the anionic polymer compound or a salt thereof a polymer obtained by polymerizing a composition containing at least one selected from acrylic acid and methacrylic acid as a monomer component or a salt thereof is preferable.
- Examples of the salt of the anionic polymer compound include ammonium salt, potassium salt, sodium salt and the like, and among them, ammonium salt is preferable.
- the weight average molecular weight of the second additive is preferably 100 to 150,000, and more preferably 1000 to 20000.
- the weight average molecular weight of the second additive is a value measured by GPC and converted to standard polystyrene, and specifically includes the following conditions.
- the lower limit of the content of the second additive is preferably 0.01% by mass or more, more preferably 0.05% by mass or more based on the total mass of the CMP polishing liquid, from the viewpoint of further improving the planarization characteristics. 08 mass% or more is still more preferable, and 0.10 mass% or more is especially preferable.
- the upper limit of the content of the second additive is preferably 2.00% by mass or less, more preferably 1.00% by mass or less, from the viewpoint of further improving the polishing rate and suppressing the occurrence of aggregation of abrasive grains. 0.50 mass% or less is still more preferable. Further, the content of the second additive is preferably larger than the content of the first additive.
- the content of the second additive is 10 to 1000 with respect to 100 parts by mass of the cerium oxide particles from the viewpoint of improving dispersibility of the abrasive grains in the CMP polishing liquid, preventing sedimentation, and maintaining excellent flatness. Mass parts are preferred, and 20 to 200 parts by mass are more preferred.
- the water that is the medium of the CMP polishing liquid is not particularly limited, but deionized water, ion exchange water, ultrapure water, and the like are preferable.
- the content of water in the CMP polishing liquid may be the remainder of the content of the above-described components, and is not particularly limited as long as it is contained in the CMP polishing liquid.
- the CMP polishing liquid may further contain a solvent other than water, for example, a polar solvent such as ethanol, acetic acid, and acetone, if necessary.
- a dispersant may be added to the CMP polishing liquid in order to disperse the cerium oxide particles in water.
- the dispersant known dispersants such as a water-soluble nonionic dispersant, a water-soluble cationic dispersant, and a water-soluble amphoteric dispersant can be used.
- a dispersing agent both the same compound as the anionic polymer compound which is a 2nd additive, and a different compound can be used.
- an anionic polymer compound is used as the dispersant, the content of the anionic polymer compound in the entire CMP polishing liquid is set within the range of the content of the second additive, and other components are added. Before mixing, it is preferable to mix a small amount of anionic polymer compound with cerium oxide particles in advance so as not to affect other components.
- the content of the dispersing agent is preferably from 0.1 to 5.0 parts by weight, more preferably from 0.1 to 2.0 parts by weight, based on 100 parts by weight of the cerium oxide particles used as abrasive grains.
- the content of the dispersant is 0.1 parts by mass or more, the stability of the abrasive grains can be improved, and when the content is 5.0 parts by mass or less, aggregation of the abrasive grains can be suppressed. It is.
- the weight average molecular weight of the dispersing agent is preferably from 100 to 150,000, more preferably from 1,000 to 20,000.
- the weight average molecular weight of the dispersant is a value measured by GPC and converted to standard polystyrene.
- the CMP polishing liquid may contain, in addition to the above components, materials generally used for the CMP polishing liquid such as a pH adjuster and a colorant as long as the effects of the CMP polishing liquid are not impaired.
- materials generally used for the CMP polishing liquid such as a pH adjuster and a colorant as long as the effects of the CMP polishing liquid are not impaired.
- the pH adjuster include acid components such as nitric acid, sulfuric acid and acetic acid, and alkali components such as ammonia, potassium hydroxide and tetramethylammonium hydroxide.
- the pH of the CMP polishing liquid is preferably in the range of 3 to 10 from the viewpoint of improving the storage stability of the CMP polishing liquid and further suppressing the generation of polishing flaws.
- the pH of the CMP polishing liquid can be adjusted by the pH adjusting agent.
- the pH of the CMP polishing liquid can be measured with a pH meter (for example, model number “PHL-40” manufactured by Electrochemical Instruments Co., Ltd.). More specifically, the pH is determined using a standard buffer (phthalate pH buffer solution pH: 4.01 (25 ° C.), neutral phosphate pH buffer solution pH: 6.86 (25 ° C.)). After calibrating two points, the value after the electrode is put into the polishing liquid and stabilized after 2 minutes or more can be measured as the pH value.
- a pH meter for example, model number “PHL-40” manufactured by Electrochemical Instruments Co., Ltd.
- the viscosity of the CMP polishing liquid is not particularly limited, but 0.5 to 5 mPa ⁇ s is preferable from the viewpoint of improving the storage stability of the CMP polishing liquid.
- the viscosity of the CMP polishing liquid can be measured by, for example, an Ubbelohde viscometer.
- the viscosity of the slurry containing cerium oxide is preferably 0.5 to 5 mPa ⁇ s from the viewpoint of obtaining excellent storage stability.
- the CMP polishing liquid may be stored as a one-part type containing all necessary raw materials, or the components contained in the two-part liquid may be stored in a two-part type to obtain a CMP polishing liquid by mixing both liquids during use. Good.
- the CMP polishing liquid according to the first embodiment includes, for example, a slurry containing cerium oxide particles and water (first liquid, hereinafter referred to as “cerium oxide slurry”), and an additive liquid containing first additive and water (first 2 liquids) and 2 liquids.
- the CMP polishing liquid according to the second embodiment includes, for example, a slurry containing cerium oxide particles and water (third liquid, hereinafter referred to as “cerium oxide slurry”), a first additive, a second additive, and water. It is divided into two liquids including an additive liquid (fourth liquid).
- a dispersing agent is contained in a cerium oxide slurry as needed.
- the cerium oxide slurry can be stored in a concentrated state and diluted with a diluent such as water for polishing.
- the CMP polishing liquid according to the first embodiment is a total of three liquids, that is, a cerium oxide slurry, an additive liquid, and a diluting liquid.
- the one-component CMP polishing liquid can also be stored in a concentrated state and diluted for use in polishing, and this form is also collectively referred to as one-component.
- the planarization characteristics and the polishing rate can be adjusted by arbitrarily changing the composition of these two liquids.
- the additive solution is sent through a pipe separate from the cerium oxide slurry pipe, and the slurry pipe and the additive pipe are merged just before the outlet of the supply pipe to mix the two liquids and CMP polishing.
- a method of supplying a CMP polishing liquid onto the polishing surface plate or a method of mixing the cerium oxide slurry and the additive liquid immediately before polishing is taken.
- the polishing method according to this embodiment includes a step of polishing a film to be polished formed on a substrate using the CMP polishing liquid.
- the method for manufacturing a semiconductor substrate according to this embodiment includes a step of polishing a film to be polished formed on the semiconductor substrate using the CMP polishing liquid.
- the film to be polished is, for example, an inorganic insulating film such as a silicon oxide film.
- a polishing method using a CMP polishing liquid and a method for manufacturing a semiconductor substrate include a first step (roughing step) for polishing a film to be polished formed on a semiconductor substrate at a high speed, and a relatively low amount of the remaining film to be polished. And a second step (finishing step) for polishing so that the surface to be polished is finally flattened at a speed.
- FIG. 1 is a schematic cross-sectional view showing a process in which an STI structure is formed on a semiconductor substrate by polishing a film to be polished.
- FIG. 1A is a schematic cross-sectional view showing a substrate before polishing.
- FIG. 1B is a schematic cross-sectional view showing the substrate after the first step.
- FIG. 1C is a schematic cross-sectional view showing the substrate after the second step.
- the process of forming the STI structure in order to eliminate the step D of the silicon oxide film (inorganic insulating film) 3 formed on the silicon substrate (semiconductor substrate) 1, it is unnecessary to protrude partially. These parts are removed preferentially by CMP. In order to stop the polishing appropriately when the surface is flattened, it is preferable to previously form a stopper film 2 having a low polishing rate under the silicon oxide film 3. A silicon nitride film is generally used as the stopper film, but a polysilicon film or the like is also used. By going through the first and second steps, the step D of the silicon oxide film 3 is eliminated, and an element isolation structure having a buried portion 5 is formed.
- the silicon substrate 1 is disposed on the polishing pad so that the surface to be polished of the silicon oxide film 3 and the polishing pad are in contact with each other, and the surface to be polished of the silicon oxide film 3 is formed by the polishing pad. Grind. More specifically, while the polishing surface of the silicon oxide film 3 is pressed against the polishing pad of the polishing surface plate, the polishing liquid is supplied between the polishing surface and the polishing pad while the substrate and the polishing pad are relative to each other. The silicon oxide film 3 is polished by moving it.
- the CMP polishing liquid can be suitably used for both the first step and the second step.
- polishing apparatus used for polishing
- an apparatus including a holder for holding a substrate, a polishing surface plate to which a polishing pad is attached, and means for supplying a polishing liquid onto the polishing pad
- the polishing apparatus include a polishing apparatus (model number: EPO-111) manufactured by Ebara Manufacturing Co., Ltd., an AMAT polishing apparatus (trade name: Mira3400, Reflexion polishing machine), and the like.
- the polishing pad is exemplified as the polishing member, the polishing member is not limited to this.
- a polishing pad For example, a general nonwoven fabric, a polyurethane foam, a porous fluororesin, etc. can be used.
- the polishing pad is preferably subjected to groove processing so that the polishing liquid is accumulated.
- the polishing pad is preferably such that the surface tension of the CMP polishing liquid is smaller than the critical surface tension of the polishing pad surface. By using these polishing pads, the CMP polishing liquid can be uniformly dispersed on the polishing pad.
- the polishing conditions are not particularly limited, but from the viewpoint of preventing the substrate from popping out, the rotation speed of the polishing platen is preferably 200 min ⁇ 1 or less. Further, the pressure (working load) applied to the substrate is preferably 100 kPa or less from the viewpoint of further suppressing an increase in scratches on the polished surface.
- the processing load is more preferably 5 to 50 kPa in order to satisfy the uniformity of the polishing rate within the surface to be polished and the flatness of the pattern.
- the supply amount of the polishing liquid is not limited, but it is preferable that the surface of the polishing pad is always covered with the polishing liquid. Specifically, it is preferable to supply 0.005 to 0.40 ml / min of polishing liquid per 1 cm 2 of area of the polishing pad.
- the substrate is thoroughly washed in running water, and further, water droplets adhering to the substrate are removed using a spin dryer or the like and then dried.
- a spin dryer or the like By such treatment, unevenness on the substrate surface can be eliminated, and a smooth surface can be obtained over the entire surface of the substrate.
- a substrate having a desired number of layers can be manufactured by repeating the formation of the film and the step of polishing the film a predetermined number of times.
- the substrate thus obtained can be used as various electronic components.
- semiconductor elements include semiconductor elements, optical glasses such as photomasks, lenses, and prisms, inorganic conductive films such as ITO, optical integrated circuits / optical switching elements / optical waveguides composed of glass and crystalline materials, end faces of optical fibers, Examples thereof include optical single crystals such as scintillators, solid laser single crystals, sapphire substrates for blue laser LEDs, semiconductor single crystals such as SiC, GaP, and GaAs, glass substrates for magnetic disks, and magnetic heads.
- optical single crystals such as scintillators, solid laser single crystals, sapphire substrates for blue laser LEDs, semiconductor single crystals such as SiC, GaP, and GaAs, glass substrates for magnetic disks, and magnetic heads.
- Cerium oxide particles were prepared by a firing method. That is, about 6 kg of cerium carbonate was put in an alumina container and calcined in the air at 800 ° C. for 2 hours to obtain about 3 kg of yellowish white calcined powder. When the phase of this calcined powder was identified by an X-ray diffraction method using CuK ⁇ rays as a radiation source, it was confirmed that the powder was cerium oxide. Further, the half width of the diffraction peak of the (111) plane of the cerium oxide crystal determined from the powder X-ray diffraction pattern was 0.31 °.
- 3 kg of the cerium oxide powder obtained as described above was dry-ground using a jet mill so that polycrystalline cerium oxide particles composed of a plurality of crystallites and having grain boundaries remain. Either or both of the grinding time and the grinding pressure were adjusted to obtain cerium oxide particles having average particle diameters of 0.18 ⁇ m and 0.20 ⁇ m, respectively.
- the average particle size of the cerium oxide particles was measured using LA-920 (light source: He—Ne laser and W laser) manufactured by Horiba.
- CMP polishing liquid (Preparation of CMP polishing liquid) As shown in Tables 1 and 2, cerium oxide particles having an average particle size of 0.18 ⁇ m or 0.20 ⁇ m were dispersed in water using a dispersant to obtain a dispersion.
- the compounding quantity of the dispersing agent was made into the small quantity of the grade which does not affect the compounding quantity of the 1st, 2nd additive.
- each CMP polishing liquid was measured using a pH meter (manufactured by Electrochemical Instruments, model number “PHL-40”). After calibrating two points using a standard buffer solution (phthalate pH buffer solution pH: 4.01 (25 ° C), neutral phosphate pH buffer solution pH: 6.86 (25 ° C)), the electrode was subjected to CMP. The value after putting it in polishing liquid and stabilizing for 2 minutes or more was made into pH.
- a silicon oxide (SiO 2 ) film having a thickness of 1000 nm was formed on a ⁇ 200 mm silicon (Si) substrate by a plasma-CVD method to obtain a bare wafer having a flat silicon oxide film as a film to be polished.
- a pattern wafer (trade name: SEMATECH864, manufactured by ADVANTECH) having an uneven silicon oxide film as a film to be polished was prepared.
- a silicon nitride film is formed as a stopper film on a part of a ⁇ 200 mm silicon substrate, and a recess is formed by etching the silicon substrate without the silicon nitride film by 350 nm, and then by plasma-CVD. It is obtained by forming a 600 nm silicon oxide film on the stopper film and in the recess.
- the silicon oxide films of the bare wafer and the pattern wafer were polished using the CMP polishing liquid. Further, using the polished wafer, the number of polishing flaws, the polishing rate, and the remaining step after polishing were measured under the following conditions. The polishing of the substrates and the respective measurements in Examples 1 to 6 and Comparative Examples 1 to 5 were performed on the same day.
- Each wafer was polished as follows using a polishing apparatus (polishing apparatus manufactured by Ebara Corporation: model number EPO111).
- a polishing apparatus manufactured by Ebara Corporation: model number EPO111.
- the bare wafer or the pattern wafer was set in a holder to which a suction pad for attaching a substrate was attached.
- a polishing pad made of a porous urethane resin (groove shape: perforate type, manufactured by Rohm and Haas, model number IC1000) was attached to a polishing surface plate of ⁇ 600 mm of the polishing apparatus.
- the holder was installed so that the film to be polished was opposed to the polishing pad.
- the processing load was set to 34.3 kPa.
- the polishing surface plate and the bare wafer or the pattern wafer were each rotated at 50 min ⁇ 1 for 1 minute, and the film to be polished was polished with the polishing pad.
- the polished wafer was thoroughly washed with pure water and then dried.
- A Ammonium polyacrylate having a weight average molecular weight of 10,000 obtained by copolymerizing acrylic acid and methyl acrylate (product name A6114, manufactured by Toagosei Co., Ltd.).
- B D: Polyacrylic acid potassium salt having a weight average molecular weight of 4000 obtained by polymerizing an acrylic acid monomer using potassium sulfite as an initiator.
- C A polyacrylic acid ammonium salt having a weight average molecular weight of 4000 obtained by polymerizing an acrylic acid monomer using 2,2′-azobisisobutyronitrile as an initiator.
- E Ammonium polyacrylate having a weight average molecular weight of 4000 obtained by polymerizing an acrylic acid monomer using ammonium sulfite as an initiator.
- Example 9 to 14 and Comparative Examples 6 to 9 In Examples 9 to 14 and Comparative Examples 6 to 9, the average particle diameter of cerium oxide was fixed to 0.18 ⁇ m, and the influence of the concentration of the first additive on the polishing characteristics was observed. At the same time, in order to confirm the influence of the concentration of the cerium oxide particles on the polishing characteristics, the cerium oxide concentration was fixed at 0.50% by mass in Examples 13 and 14, and the cerium oxide in Examples 9 to 12 and Comparative Examples 6 to 9 The concentration was fixed at 1.00% by mass. In addition, the 2nd additive which mainly functions as a planarizing agent was not added.
- Each component is contained in each compounding amount shown in Table 3 in the same manner as in Examples 1 to 8, except that an aqueous solution of the first additive shown in Table 3 was added to the dispersion to obtain a CMP polishing liquid.
- a CMP polishing liquid was prepared, and the number of polishing flaws and the polishing rate after polishing the bare wafer were measured.
- Each measurement in Examples 9 to 14 and Comparative Examples 6 to 9 was performed on the same day.
- Table 3 shows the measurement results.
- the measurement results of Examples 9 to 12 and Comparative Examples 6 to 9 are shown in FIG.
- FIG. 2 is a diagram showing the relationship between the concentration of the first additive, the polishing rate, and the number of polishing flaws. In FIG. 2, the left axis shows the polishing rate, and the right axis shows the number of polishing flaws.
- Example 15 to 19 and Comparative Examples 10 to 12 In Examples 15 to 19 and Comparative Examples 10 to 12, the influence of the concentration of the first additive on the polishing characteristics was observed.
- CMP polishing liquids containing each component were prepared in the respective compounding amounts shown in Table 4. Using each CMP polishing liquid, the number of polishing flaws and the polishing rate were measured for the bare wafer, and the level difference remaining after polishing was measured for the pattern wafer. The measurements in Examples 15 to 19 and Comparative Examples 10 to 12 were performed on the same day. Table 4 shows the measurement results.
- Example 20 a CMP polishing liquid (single liquid type) having the same blending amount as in Example 1 was prepared again.
- Example 21 a cerium oxide slurry containing cerium oxide particles, a dispersing agent and water, and an additive liquid containing a first additive and a second additive are supplied by separate pipes, and the pipes are connected immediately before dropping. The resulting mixture was mixed so that a CMP polishing liquid having the same blending amount as in Example 1 was finally obtained.
- Example 22 the same cerium oxide slurry and additive liquid as in Example 21 are supplied through separate pipes and mixed on the polishing pad, finally resulting in a CMP polishing liquid having the same blending amount as in Example 1. I did it.
- SYMBOLS 1 Silicon substrate (semiconductor substrate), 2 ... Stopper film, 3 ... Silicon oxide film (inorganic insulating film), 5 ... Embedded part, D ... Elevation difference (step) of film thickness of silicon oxide film.
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Abstract
Description
酸化セリウム粒子は、粒子状を有するものであればどのようなものでもよい。酸化セリウム粒子は、その製造方法を限定するものではないが、従来公知の酸化セリウム粒子を広く一般的に使用することができる。
アセチレン化合物としては、例えば、アルキン類、アセチレンアルコール類及びアセチレングリコール類から選ばれる少なくとも一種が挙げられる。アルキン類としては、1-デシン、5-デシン等が挙げられる。アセチレンアルコール類としては、3,5-ジメチル-1-ヘキシン-3-オール、2,4-ジメチル-5-ヘキシン-3-オール等が挙げられる。アセチレングリコール類としては、下記一般式(1)で表される化合物等が挙げられる。これらのアセチレン化合物は、単独で又は二種類以上を組み合わせて使用することができる。
第2の添加剤は、凹凸を有する被研磨面を研磨する際に、被研磨面に吸着して保護膜を形成し、研磨パッドが接触しない凹部において研磨が進行することを抑制し、凸部を優先的に研磨することに好適な化合物である。第2実施形態に係るCMP研磨液において、第2の添加剤は、アニオン性置換基を有するビニル化合物を単量体成分として含む組成物を重合させて得られるアニオン性高分子化合物又はその塩である。なお、第2の添加剤が被研磨面に吸着して保護膜を形成することにより、研磨傷の発生が多少抑えられる傾向があるが、単独での使用では、その効果は充分ではない。第2の実施形態に係るCMP研磨液では、第1の添加剤と第2の添加剤とを併用することにより、顕著な研磨傷低減効果が得られる。
(条件)
試料:10μL
標準ポリスチレン:東ソー株式会社製標準ポリスチレン(重量平均分子量:190000、17900、9100、2980、578、474、370、266)
検出器:株式会社日立製作所社製、RI-モニター、商品名「L-3000」
インテグレーター:株式会社日立製作所社製、GPCインテグレーター、商品名「D-2200」
ポンプ:株式会社日立製作所社製、商品名「L-6000」
デガス装置:昭和電工株式会社製、商品名「Shodex DEGAS」
カラム:日立化成工業株式会社製、商品名「GL-R440」、「GL-R430」、「GL-R420」をこの順番で連結して使用
溶離液:テトラヒドロフラン(THF)
測定温度:23℃
流速:1.75mL/分
測定時間:45分
CMP研磨液の媒体である水としては、特に制限されないが、脱イオン水、イオン交換水、超純水等が好ましい。CMP研磨液における水の含有量は、上記含有成分の含有量の残部でよく、CMP研磨液中に含有されていれば特に限定されない。なお、CMP研磨液は、必要に応じて水以外の溶媒、例えばエタノール、酢酸、アセトン等の極性溶媒等を更に含有してもよい。
CMP研磨液には、酸化セリウム粒子を水に分散させるために分散剤を添加することができる。分散剤としては、水溶性ノニオン性分散剤、水溶性カチオン性分散剤、水溶性両性分散剤等の公知の分散剤を使用することができる。また、分散剤としては、第2の添加剤であるアニオン性高分子化合物と同じ化合物及び異なる化合物のいずれも使用することができる。分散剤としてアニオン性高分子化合物を用いる場合には、CMP研磨液全体におけるアニオン性高分子化合物の含有量を上記第2の添加剤の含有量の範囲内とすることや、他の含有成分を混合する前に、他の含有成分に影響を与えない程度に少量のアニオン性高分子化合物を酸化セリウム粒子と予め混合することが好ましい。
CMP研磨液のpHは、CMP研磨液の保存安定性を向上させ研磨傷の発生を更に抑制する観点から、3~10の範囲が好ましい。CMP研磨液のpHは、上記pH調整剤により調整可能である。
本実施形態に係る研磨方法は、上記CMP研磨液を用いて、基体に形成された被研磨膜を研磨する工程を備える。本実施形態に係る半導体基板の製造方法は、上記CMP研磨液を用いて半導体基板に形成された被研磨膜を研磨する工程を備える。被研磨膜は、例えば、酸化ケイ素膜等の無機絶縁膜である。
(酸化セリウム粒子の作製)
酸化セリウム粒子を焼成法により作製した。すなわち、炭酸セリウム約6kgをアルミナ製容器に入れ、800℃で2時間空気中で焼成することにより黄白色の焼成粉末を約3kg得た。線源をCuKα線とするX線回折法でこの焼成粉末の相同定を行ったところ酸化セリウムであることを確認した。また、粉末X線回折パターンから求められる酸化セリウム結晶の(111)面による回折ピークの半値幅は0.31°であった。
表1,2に示すように、平均粒径が0.18μm又は0.20μmの酸化セリウム粒子を分散剤を使用して水に分散させ、分散液を得た。得られた分散液に表1,2に示す第2の添加剤の水溶液を添加し、更に第1の添加剤を加えて、表1,2に示す配合量で各成分を含有するCMP研磨液を得た。なお、分散剤の配合量は、第1,第2の添加剤の配合量に影響を与えない程度の少量とした。
φ200mmのシリコン(Si)基板上に、プラズマ-CVD法で厚さ1000nmの酸化ケイ素(SiO2)膜を成膜して、被研磨膜として平坦な酸化ケイ素膜を有するベアウエハを得た。
研磨終了後のベアウエハについて、AMAT製Complusを用いて、検出異物サイズを0.2μmに設定して異物を検出した。検出される異物には、傷以外の付着物が含まれるため、SEMで各異物を観察し、凹みを研磨傷と判断し、研磨傷数をカウントした。なお、測定には、死角面積3000mm2のφ200mmベアウエハを使用した。研磨傷数の測定結果を表1,2に示す。
SCREEN製のRE-3000を用いてベアウエハにおける酸化ケイ素膜の研磨前後の膜厚を測定し、1分当たりの研磨速度を算出した。研磨速度の測定結果を表1,2に示す。
パターンウエハ研磨後、Line/Spece=500/500μm、100/100μmの部分で、研磨後に残った段差(研磨後残段差)を測定した。結果を表1,2に示す。なお、表1,2では、Line/Spece=500/500μmの部分の段差を「段差500/500」として示し、Line/Spece=100/100μmの部分の段差を「段差100/100」として示した。
A:アクリル酸とアクリル酸メチルとを共重合して得られた重量平均分子量10000のポリアクリル酸アンモニウム塩(東亞合成(株)製、製品名A6114)。
B、D:亜硫酸カリウムを開始剤にアクリル酸モノマーを重合して得られた重量平均分子量4000のポリアクリル酸カリウム塩。
C:2,2’-アゾビスイソブチロニトルを開始剤にアクリル酸モノマーを重合して得られた重量平均分子量4000のポリアクリル酸アンモニウム塩。
E:亜硫酸アンモニウムを開始剤にアクリル酸モノマーを重合して得られた重量平均分子量4000のポリアクリル酸アンモニウム塩。
(条件)
試料:10μL
標準ポリスチレン:東ソー株式会社製標準ポリスチレン(重量平均分子量:190000、17900、9100、2980、578、474、370、266)
検出器:株式会社日立製作所社製、RI-モニター、商品名「L-3000」
インテグレーター:株式会社日立製作所社製、GPCインテグレーター、商品名「D-2200」
ポンプ:株式会社日立製作所社製、商品名「L-6000」
デガス装置:昭和電工株式会社製、商品名「Shodex DEGAS」
カラム:日立化成工業株式会社製、商品名「GL-R440」、「GL-R430」、「GL-R420」をこの順番で連結して使用
溶離液:テトラヒドロフラン(THF)
測定温度:23℃
流速:1.75mL/分
測定時間:45分
実施例9~14及び比較例6~9では、酸化セリウムの平均粒径を0.18μmに固定して、研磨特性に対する第1の添加剤の濃度の影響を観察した。同時に、研磨特性に対する酸化セリウム粒子の濃度の影響を確認するため、実施例13及び14では酸化セリウム濃度を0.50質量%に固定し、実施例9~12、比較例6~9では酸化セリウム濃度を1.00質量%に固定した。なお、主に平坦化剤として機能する第2の添加剤は添加しなかった。
実施例15~19、比較例10~12では、研磨特性に対する第1の添加剤の濃度による影響を観察した。実施例1~8と同様にして、表4に示す各配合量で各成分を含有するCMP研磨液を作製した。各CMP研磨液を用いて、ベアウエハについて研磨傷数及び研磨速度を測定し、パターンウエハについて研磨後に残った段差を測定した。なお、実施例15~19、比較例10~12における各測定は、同日に行った。各測定結果を表4に示す。
実施例20~22では、CMP研磨液の供給方法が研磨特性に与える影響を観察した。
Claims (12)
- 酸化セリウム粒子と、アセチレン結合を有する有機化合物と、水とを含み、
前記アセチレン結合を有する有機化合物の含有量が、CMP研磨液全質量基準で0.00001質量%以上0.01質量%以下である、CMP研磨液。 - 前記酸化セリウム粒子及び前記水を含む第1の液と、前記アセチレン結合を有する有機化合物及び前記水を含む第2の液とを混合して得られる、請求項1に記載のCMP研磨液。
- 酸化セリウム粒子と、アセチレン結合を有する有機化合物と、アニオン性置換基を有するビニル化合物を単量体成分として含む組成物を重合させて得られるアニオン性高分子化合物又はその塩と、水とを含み、
前記アセチレン結合を有する有機化合物の含有量が、CMP研磨液全質量基準で0.000001質量%以上0.05質量%未満である、CMP研磨液。 - 前記酸化セリウム粒子及び前記水を含む第3の液と、前記アセチレン結合を有する有機化合物、前記アニオン性高分子化合物又はその塩並びに前記水を含む第4の液とを混合して得られる、請求項3に記載のCMP研磨液。
- 前記アニオン性置換基を有するビニル化合物が、アクリル酸及びメタクリル酸から選ばれる少なくとも一種である、請求項3又は4に記載のCMP研磨液。
- 前記アニオン性高分子化合物又はその塩の含有量が、前記アセチレン結合を有する有機化合物の含有量より多い、請求項3~5のいずれか一項に記載のCMP研磨液。
- 前記アニオン性高分子化合物又はその塩の含有量が、CMP研磨液全質量基準で0.01~2.00質量%である、請求項3~6のいずれか一項に記載のCMP研磨液。
- 前記アセチレン結合を有する有機化合物が、アセチレングリコール類である、請求項1~7のいずれか一項に記載のCMP研磨液。
- 前記アセチレングリコール類が、2,4,7,9-テトラメチル-5-デシン-4,7-ジオールである、請求項8又は9に記載のCMP研磨液。
- 請求項1~10のいずれか一項に記載のCMP研磨液を用いて、基体に形成された被研磨膜を研磨する工程を備える、研磨方法。
- 請求項1~10のいずれか一項に記載のCMP研磨液を用いて半導体基板に形成された無機絶縁膜を研磨する工程を備える、半導体基板の製造方法。
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EP10829776.3A EP2500928A4 (en) | 2009-11-12 | 2010-09-14 | CHEMICAL MECHANICAL POLISHING LIQUID AND METHOD FOR MANUFACTURING SEMICONDUCTOR SUBSTRATE, AND POLISHING METHOD USING THE POLISHING LIQUID |
JP2011540440A JP5516594B2 (ja) | 2009-11-12 | 2010-09-14 | Cmp研磨液、並びに、これを用いた研磨方法及び半導体基板の製造方法 |
US13/504,738 US20120214307A1 (en) | 2009-11-12 | 2010-09-14 | Chemical-mechanical polishing liquid, and semiconductor substrate manufacturing method and polishing method using said polishing liquid |
KR1020127012168A KR101357328B1 (ko) | 2009-11-12 | 2010-09-14 | Cmp 연마액, 및 이것을 이용한 연마 방법 및 반도체 기판의 제조 방법 |
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KR102476738B1 (ko) * | 2014-05-30 | 2022-12-13 | 쇼와덴코머티리얼즈가부시끼가이샤 | Cmp용 연마액, cmp용 연마액 세트 및 연마 방법 |
SG11201610744YA (en) * | 2014-07-31 | 2017-02-27 | Hoya Corp | Method for manufacturing magnetic-disk glass substrate and method for manufacturing magnetic disk |
KR20210118469A (ko) * | 2016-12-30 | 2021-09-30 | 후지필름 일렉트로닉 머티리얼스 유.에스.에이., 아이엔씨. | 폴리싱 조성물 |
CN110998800B (zh) * | 2017-08-14 | 2023-09-22 | 株式会社力森诺科 | 研磨液、研磨液套剂及研磨方法 |
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JP5516594B2 (ja) | 2014-06-11 |
KR101357328B1 (ko) | 2014-02-03 |
CN102686360A (zh) | 2012-09-19 |
EP2500928A4 (en) | 2014-06-25 |
KR20120073327A (ko) | 2012-07-04 |
EP2500928A1 (en) | 2012-09-19 |
US20120214307A1 (en) | 2012-08-23 |
TW201127944A (en) | 2011-08-16 |
JPWO2011058816A1 (ja) | 2013-03-28 |
TWI488952B (zh) | 2015-06-21 |
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