WO2012026437A1 - シリコンウェハ加工液およびシリコンウェハ加工方法 - Google Patents
シリコンウェハ加工液およびシリコンウェハ加工方法 Download PDFInfo
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- WO2012026437A1 WO2012026437A1 PCT/JP2011/068899 JP2011068899W WO2012026437A1 WO 2012026437 A1 WO2012026437 A1 WO 2012026437A1 JP 2011068899 W JP2011068899 W JP 2011068899W WO 2012026437 A1 WO2012026437 A1 WO 2012026437A1
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- WIPO (PCT)
- Prior art keywords
- silicon wafer
- wafer processing
- processing liquid
- nitrogen
- water
- Prior art date
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 74
- 239000010703 silicon Substances 0.000 title claims abstract description 74
- 238000003672 processing method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000006061 abrasive grain Substances 0.000 claims abstract description 21
- 239000003607 modifier Substances 0.000 claims abstract description 14
- 150000002391 heterocyclic compounds Chemical class 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 54
- 235000012431 wafers Nutrition 0.000 claims description 52
- -1 nitrogen-containing compound Chemical class 0.000 claims description 33
- 239000012530 fluid Substances 0.000 claims description 26
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 7
- 239000012964 benzotriazole Substances 0.000 claims description 7
- HJBLUNHMOKFZQX-UHFFFAOYSA-N 3-hydroxy-1,2,3-benzotriazin-4-one Chemical compound C1=CC=C2C(=O)N(O)N=NC2=C1 HJBLUNHMOKFZQX-UHFFFAOYSA-N 0.000 claims description 5
- HYZJCKYKOHLVJF-UHFFFAOYSA-N 1H-benzimidazole Chemical compound C1=CC=C2NC=NC2=C1 HYZJCKYKOHLVJF-UHFFFAOYSA-N 0.000 claims description 3
- BAXOFTOLAUCFNW-UHFFFAOYSA-N 1H-indazole Chemical compound C1=CC=C2C=NNC2=C1 BAXOFTOLAUCFNW-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 150000001875 compounds Chemical class 0.000 abstract description 8
- 238000005299 abrasion Methods 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 13
- 238000003754 machining Methods 0.000 description 12
- 238000005520 cutting process Methods 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 150000002334 glycols Chemical class 0.000 description 3
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 3
- 239000003755 preservative agent Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- 229920003169 water-soluble polymer Polymers 0.000 description 3
- XQIOBBHIEUGFCI-UHFFFAOYSA-N 3,4-dihydropyrido[1,2-a]pyrimidin-2-one Chemical compound C1=CC=CC2=NC(=O)CCN21 XQIOBBHIEUGFCI-UHFFFAOYSA-N 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- PGRHXDWITVMQBC-UHFFFAOYSA-N dehydroacetic acid Chemical compound CC(=O)C1C(=O)OC(C)=CC1=O PGRHXDWITVMQBC-UHFFFAOYSA-N 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000006078 metal deactivator Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000004584 polyacrylic acid Substances 0.000 description 2
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 2
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- HHPDFYDITNAMAM-UHFFFAOYSA-N 2-[cyclohexyl(2-hydroxyethyl)amino]ethanol Chemical compound OCCN(CCO)C1CCCCC1 HHPDFYDITNAMAM-UHFFFAOYSA-N 0.000 description 1
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 description 1
- WONYMNWUJVKVII-UHFFFAOYSA-N 3,5-diiodothyropropionic acid Chemical compound IC1=CC(CCC(=O)O)=CC(I)=C1OC1=CC=C(O)C=C1 WONYMNWUJVKVII-UHFFFAOYSA-N 0.000 description 1
- XZOYHFBNQHPJRQ-UHFFFAOYSA-N 7-methyloctanoic acid Chemical compound CC(C)CCCCCC(O)=O XZOYHFBNQHPJRQ-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 239000004287 Dehydroacetic acid Substances 0.000 description 1
- 229920006309 Invista Polymers 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 150000007514 bases Chemical class 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 229960004365 benzoic acid Drugs 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 235000019258 dehydroacetic acid Nutrition 0.000 description 1
- 229940061632 dehydroacetic acid Drugs 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- MTNDZQHUAFNZQY-UHFFFAOYSA-N imidazoline Chemical compound C1CN=CN1 MTNDZQHUAFNZQY-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 229940083082 pyrimidine derivative acting on arteriolar smooth muscle Drugs 0.000 description 1
- 150000003230 pyrimidines Chemical class 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
Classifications
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23D—PLANING; SLOTTING; SHEARING; BROACHING; SAWING; FILING; SCRAPING; LIKE OPERATIONS FOR WORKING METAL BY REMOVING MATERIAL, NOT OTHERWISE PROVIDED FOR
- B23D61/00—Tools for sawing machines or sawing devices; Clamping devices for these tools
- B23D61/18—Sawing tools of special type, e.g. wire saw strands, saw blades or saw wire equipped with diamonds or other abrasive particles in selected individual positions
- B23D61/185—Saw wires; Saw cables; Twisted saw strips
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- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
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- 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
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- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/016—Diazonium salts or compounds
- G03F7/021—Macromolecular diazonium compounds; Macromolecular additives, e.g. binders
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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
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
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- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—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
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- 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
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M2215/221—Six-membered rings containing nitrogen and carbon only
- C10M2215/222—Triazines
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
- C10M2215/224—Imidazoles
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
Definitions
- the present invention relates to a silicon wafer processing liquid and a silicon wafer processing method.
- processing such as cutting of a silicon ingot or polishing of the silicon wafer is performed.
- the cutting of the silicon ingot is performed while pouring a working fluid over the wire.
- a free abrasive grain method in which the silicon ingot is cut in a state where abrasive grains are dispersed in the working fluid, and a fixing in which the silicon ingot is cut in a state where the abrasive grains are fixed in advance on the surface of the wire.
- abrasive system There is an abrasive system.
- Examples of the working fluid used in the free abrasive grain method include water-soluble working fluid containing a friction coefficient reducing agent, a rust preventive power auxiliary agent, and the like. Unsaturated fatty acids are used as the friction coefficient reducing agent contained in the working fluid, and benzotriazole is used as the rust-preventing power auxiliary agent (see Patent Document 1).
- Examples of the processing liquid used in the fixed abrasive method include water-soluble processing liquids containing glycols, carboxylic acids, alkanolamines, and the like (see Patent Document 2).
- an object of the present invention is to provide a silicon wafer processing liquid and a silicon wafer processing method capable of suppressing abrasive wear and hydrogen generation.
- the present invention provides the following silicon wafer processing liquid and silicon wafer processing method.
- a silicon wafer processing liquid comprising a friction modifier containing a nitrogen-containing compound, wherein the nitrogen-containing compound has a mass ratio to water (the nitrogen-containing compound / the water) of 1/99.
- a silicon wafer processing liquid characterized by sometimes having a pH of 2 or more and 8 or less.
- the heterocyclic compound is benzotriazole, 3,4-dihydro-3-hydroxy-4-oxo-1,2,3-benzotriazine, indazole, benzimidazole, And a silicon wafer processing liquid characterized by being at least one of the derivatives thereof.
- the silicon wafer processing liquid of the present invention described above wherein the silicon wafer processing liquid has a pH of 3 or more and 9 or less.
- the silicon wafer processing liquid of the present invention described above wherein the content of the nitrogen-containing compound is 0.05% by mass or more and 10% by mass or less based on the total amount of the processing liquid.
- a silicon wafer processing liquid according to the present invention which is used for processing a silicon wafer with a wire to which abrasive grains are fixed.
- a silicon wafer processing liquid and a silicon wafer processing method capable of suppressing abrasion of abrasive grains and generation of hydrogen.
- the silicon wafer processing liquid of the present invention (hereinafter sometimes abbreviated as “processing liquid”) is used when processing a silicon wafer with a wire.
- processing liquid is formed by blending a friction modifier.
- the friction modifier contains a nitrogen-containing compound, and the nitrogen-containing compound has a pH of 2 or more and 8 or less when the mass ratio with water (nitrogen-containing compound / water) is 1/99. If the pH is less than 2, the wire, wire saw, silicon, etc. may be corroded.
- the pH is preferably 3 or more and 7 or less, and more preferably 4 or more and 6 or less.
- nitrogen compounds having a specific pH include heterocyclic compounds, and specific examples include benzotriazole, 3,4-dihydro-3-hydroxy-4-oxo-1,2,3-benzoate. And triazine, indazole, benzimidazole, and derivatives thereof. Of these, benzotriazole and 3,4-dihydro-3-hydroxy-4-oxo-1,2,3-benzotriazine are preferred.
- the nitrogen-containing compound of the present invention improves the lubricity of the wire, suppresses the wear of the abrasive grains fixed to the wire, and prevents the abrasive grains from falling off the wire. Therefore, it is possible to prevent the wire from being disconnected and improve the processing efficiency and cutting accuracy, so that the yield can be improved. Moreover, such nitrogen-containing compounds can suppress the generation of hydrogen due to the reaction between the silicon ingot chips and water. As a result, it is possible to prevent the machining liquid from overflowing from the machining liquid tank.
- the processing liquid of the present invention preferably has a pH of 3 or more and 9 or less, more preferably 5 or more and 7 or less. Since the pH is in the range from moderately acidic to weakly alkaline, generation of hydrogen can be further suppressed. Furthermore, corrosion of wires and silicon can be prevented.
- the content of the nitrogen-containing compound of the present invention is preferably 0.05% by mass or more and 10% by mass or less, more preferably 0.1% by mass or more and 5% by mass or less, based on the total amount of the working fluid.
- content is 0.05% by mass or more, abrasion of abrasive grains and generation of hydrogen can be further suppressed, and corrosion of wires, silicon, and the like can be prevented.
- content is 10 mass% or less, cost can be held down.
- the working fluid of the present invention contains water, and the water is not particularly limited and may be tap water or purified water.
- the water content is preferably 50% by mass or more and 99.95% by mass or less, and more preferably 60% by mass or more and 95% by mass or less. By setting it as 50 mass% or more, compared with ethylene glycol etc. which are conventionally used as a main component, an environmental load can be made small. Moreover, since water is the main component, flammability can be lowered.
- the silicon wafer processing method of the present invention is, for example, a fixed abrasive method, and abrasive particles are fixed to the wire in advance.
- a silicon ingot is introduced into a processing chamber of a wire saw in which wires are stretched. Then, the silicon ingot is cut while pouring the working fluid of the present invention over the wire. Since the working fluid of the present invention contains a nitrogen-containing compound having a specific pH, the abrasive grains can be prevented from being worn. Although silicon ingot chips are generated, the nitrogen-containing compound of the present invention can suppress the reaction between the chips and water.
- the working fluid of the present invention is a friction modifier, an antifoaming agent, a metal deactivator, a bactericidal agent (preservative), a viscosity modifier, a pH adjuster, and a thickener as long as they do not contradict the purpose of the present invention.
- a known additive such as a dispersant may be included.
- the friction modifier is used to suppress abrasive wear.
- various surfactants and water-soluble polymers can be used as the friction modifier.
- the surfactant include nonionic surfactants such as glycols.
- the water-soluble polymer include carboxylic acid polymer compounds such as polyacrylic acid and alkylene glycol polymer compounds such as polyethylene glycol.
- the antifoaming agent is used to prevent the processing liquid from overflowing from the processing liquid tank provided in the processing chamber.
- the antifoaming agent include silicone oil, fluorosilicone oil, and fluoroalkyl ether.
- the metal deactivator include imidazoline, pyrimidine derivatives, thiadiazole, benzotriazole and the like.
- a disinfectant (preservative) is used to prevent the wire or the like from corroding.
- bactericides (preservatives) include paraoxybenzoates (parabens), benzoic acid, salicylic acid, sorbic acid, dehydroacetic acid, p-toluenesulfonic acid and their salts, phenoxyethanol, and the like.
- the pH adjuster is used to adjust the pH of the processing liquid of the present invention to a range of 3 or more and 9 or less.
- a pH regulator is classified into an acidic regulator and a basic regulator.
- the acid modifier include acidic compounds such as polyacrylic acid and isononanoic acid.
- the basic adjuster include basic compounds such as N-methyldiethanolamine and cyclohexyldiethanolamine.
- a thickener is used in order to improve the viscosity of the processing liquid of this invention and to improve the adhesiveness to a wire. Thereby, abrasion of an abrasive grain can be suppressed.
- the thickener include carboxylic acid polymer compounds and alkylene glycol polymer compounds similar to the friction modifier.
- the dispersant is used to suppress the accumulation of chips on the wire saw.
- examples of the dispersant include various surfactants similar to the friction modifier, water-soluble polymers, and the like.
- the content of these additives may be appropriately set according to the purpose, but the total amount of these additives is usually about 0.01% by mass or more and about 30% by mass based on the total amount of the processing liquid.
- the processing liquid of this invention showed the structure used when cut
- the manufacturing method of the processing liquid of this invention is not specifically limited. From the viewpoint of ease of transportation and sale, for example, a processing liquid in a concentrated state with a small water content may be prepared, and the concentration may be adjusted by adding water before use. And although the process liquid of this invention demonstrated the structure which has water as a main component, it is good also considering glycols as a main component.
- Example 1 A working fluid having the composition shown in Table 1 was prepared, and various tests were performed and evaluated. The components contained in the machining fluid and various test items are shown below. Table 1 also shows the evaluation results and the pH of the processing liquid.
- machining fluid ⁇ Components of machining fluid> (1) Water: Tap water (2) Propylene glycol (3) Nitrogen-containing compound: Benzotriazole (Chitech BT manufactured by Dipro Kasei Co., Ltd.) (4) Nitrogen-containing compound: 3,4-dihydro-3-hydroxy-4-oxo-1,2,3-benzotriazine (5) Nitrogen-containing compound: imidazole (6) Nitrogen-containing compound: 3,4-dihydro- 2H-pyrido (1,2-a) pyrimidin-2-one (7) Nitrogen-containing compound: N-methyldiethanolamine (Aminoalcohol MDA manufactured by Nippon Emulsifier Co., Ltd.) (8) Dodecanedioic acid (registered trademark Corfree M1 manufactured by Invista Japan Co., Ltd.)
- Cutting conditions Wire saw: CS810 (single wire saw) manufactured by DWT Wire usage: 30m (repeated by reciprocating operation) Wire traveling speed: Average value 340 m / min Wire deflection setting: 5 ° 3. Test conditions Test time: 3 days Amount of processing fluid to stand still: 100 g Measuring cylinder capacity: 200ml
- Comparative Examples 1 to 5 do not contain a nitrogen-containing compound having a predetermined pH, which is essential in the present invention, as a friction modifier, and therefore cannot suppress both an increase in the friction coefficient and the amount of hydrogen generated. Moreover, in the comparative example 4, since propylene glycol is the main component, the environmental load is large and resource saving is poor.
- the silicon wafer processing liquid and the silicon wafer processing method of the present invention are suitably used for cutting a silicon ingot with a wire to which abrasive grains are fixed.
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Abstract
Description
遊離砥粒方式に用いられる加工液としては、例えば、摩擦係数低下剤および防錆力補助剤などが含まれる水溶性の加工液がある。この加工液に含まれる摩擦係数低下剤としては、不飽和脂肪酸が用いられ、防錆力補助剤としては、ベンゾトリアゾールが用いられる(特許文献1参照)。
固定砥粒方式に用いられる加工液としては、例えば、グリコール類、カルボン酸、アルカノールアミンなどが含まれる水溶性の加工液がある(特許文献2参照)。
そこで、特許文献2のような固定砥粒方式によれば、あらかじめワイヤーに砥粒を固定するため、ワイヤーを細くすることができ、切粉を少なくできる。しかし、このような固定砥粒方式でも、ワイヤーを使用するに従って砥粒が摩耗したり、脱落する。その結果、ワイヤーが断線したり加工能率や切断精度が低下するため、歩留まりが低下するという問題がある。また、切粉と水が反応して水素が発生し、加工液タンクから加工液がオーバーフローするなどの問題もある。
(2)前述の本発明のシリコンウェハ加工液において、前記含窒素化合物は、複素環化合物であることを特徴とするシリコンウェハ加工液。
(3)前述の本発明のシリコンウェハ加工液において、前記複素環化合物がベンゾトリアゾール、3,4-ジヒドロ-3-ヒドロキシ-4-オキソ-1,2,3-ベンゾトリアジン、インダゾール、ベンズイミダゾール、およびそれらの誘導体のうちの少なくともいずれかであることを特徴とするシリコンウェハ加工液。
(4)前述の本発明のシリコンウェハ加工液において、当該シリコンウェハ加工液は、pHが3以上9以下であることを特徴とするシリコンウェハ加工液。
(5)前述の本発明のシリコンウェハ加工液において、前記含窒素化合物の含有量は、加工液全量基準で0.05質量%以上10質量%以下であることを特徴とするシリコンウェハ加工液。
(6)前述の本発明のシリコンウェハ加工液において、当該シリコンウェハ加工液は、加工液全量基準で50質量%以上99.95質量%以下の水を含むことを特徴とするシリコンウェハ加工液。
(7)前述の本発明のシリコンウェハ加工液において、砥粒が固定されたワイヤーによるシリコンウェハの加工に用いられることを特徴とするシリコンウェハ加工液。
(8)含窒素化合物を含む摩擦調整剤を配合してなるシリコンウェハ加工液を用いて、砥粒が固定されたワイヤーによりシリコンウェハを加工するシリコンウェハ加工方法であって、前記含窒素化合物は、水との質量比(前記含窒素化合物/前記水)を1/99としたときにpHが2以上8以下であることを特徴とするシリコンウェハ加工方法。
本発明の加工液は、摩擦調整剤を配合してなるものである。摩擦調整剤は、含窒素化合物を含み、この含窒素化合物は、水との質量比(含窒素化合物/水)を1/99としたときにpHが2以上8以下である。
pHが2未満の場合、ワイヤー、ワイヤーソー、シリコンなどを腐食させるおそれがある。一方、pHが8を越える場合、シリコンインゴットを切断する際の摩擦係数が増加し、摩擦が大きくなる。それ故、pHは、3以上7以下であることが好ましく、さらに好ましくは、4以上6以下である。
このような特定のpHを有する窒素化合物としては、例えば、複素環化合物であり、具体的には、ベンゾトリアゾール、3,4-ジヒドロ-3-ヒドロキシ-4-オキソ-1,2,3-ベンゾトリアジン、インダゾール、ベンズイミダゾール、およびそれらの誘導体などが挙げられる。これらの中で、ベンゾトリアゾールおよび3,4-ジヒドロ-3-ヒドロキシ-4-オキソ-1,2,3-ベンゾトリアジンが好ましい。
本発明のシリコンウェハ加工方法は、例えば、固定砥粒方式であり、ワイヤーにはあらかじめ砥粒が固定されている。
本発明のシリコンウェハ加工方法を実施する際には、ワイヤーを張り巡らしたワイヤーソーの加工室内にシリコンインゴットを導入する。
そしてワイヤーに本発明の加工液を掛け流しながら、シリコンインゴットを切断する。
本発明の加工液は、特定のpHを有する含窒素化合物を含むため、砥粒が摩耗することを防止できる。また、シリコンインゴットの切粉が発生するが、本発明の含窒素化合物により、切粉と水が反応することを抑制できる。
摩擦調整剤は、砥粒の摩耗を抑制するために用いられる。摩擦調整剤としては、各種界面活性剤、水溶性高分子を用いることができる。界面活性剤としては、グリコール類などの非イオン界面活性剤が挙げられる。水溶性高分子としては、ポリアクリル酸などのカルボン酸系高分子化合物、ポリエチレングリコールなどのアルキレングリコール系高分子化合物が挙げられる。
消泡剤は、加工室内に設けられた加工液タンクから加工液がオーバーフローしてしまうことを防止するために用いられる。消泡剤としては、例えば、シリコーン油、フロオロシリコーン油、フルオロアルキルエーテルなどが挙げられる。
金属不活性化剤としては、イミダゾリン、ピリミジン誘導体、チアジアゾール、ベンゾトリアゾールなどが挙げられる。
殺菌剤(防腐剤)は、ワイヤーなどが腐食することを防止するために用いられる。殺菌剤(防腐剤)としては、パラオキシ安息香酸エステル類(パラベン類)、安息香酸、サリチル酸、ソルビン酸、デヒドロ酢酸、p-トルエンスルホン酸およびそれらの塩類、フェノキシエタノールなどが挙げられる。
pH調整剤は、本発明の加工液のpHを3以上9以下の範囲に調整するために用いられる。pH調整剤は、酸性調整剤と塩基性調整剤に区別される。酸性調整剤としては、ポリアクリル酸、イソノナン酸などの酸性化合物が挙げられる。塩基性調整剤としては、N-メチルジエタノールアミン、シクロヘキシルジエタノールアミンなどの塩基性化合物が挙げられる。
増粘剤は、本発明の加工液の粘度を向上させて、ワイヤーへの付着性を向上させるために用いられる。これにより、砥粒の摩耗を抑制することができる。増粘剤としては、摩擦調整剤と同様のカルボン酸系高分子化合物、アルキレングリコール系高分子化合物などが挙げられる。
分散剤は、切粉のワイヤーソーへの堆積を抑制するために用いられる。分散剤としては、上記摩擦調整剤と同様の各種界面活性剤、水溶性高分子などが挙げられる。
これらの添加剤の含有量は、目的に応じて適宜設定すればよいが、これらの添加剤の合計量は加工液全量を基準にして、通常0.01質量%以上30質量%程度である。
また、本発明の加工液の製造方法は、特に限定されない。運搬、販売の容易さの観点から、例えば、水の含有量が少ない濃縮状態にある加工液を調製し、使用前に水を加えて濃度を調整するようにしても良い。
そして、本発明の加工液は、水を主成分とする構成を説明したが、グリコール類を主成分としても良い。
表1に示す組成の加工液を調製して、各種試験を実施し評価した。以下に加工液の含まれる成分と各種試験項目を示す。表1には評価結果および加工液のpHも併せて示す。
(1)水:水道水
(2)プロピレングリコール
(3)含窒素化合物:ベンゾトリアゾール(ジプロ化成(株)製 シーテックBT)
(4)含窒素化合物:3,4-ジヒドロ-3-ヒドロキシ-4-オキソ-1,2,3-ベンゾトリアジン
(5)含窒素化合物:イミダゾール
(6)含窒素化合物:3,4-ジヒドロ-2H-ピリド(1,2-a)ピリミジン-2-オン
(7)含窒素化合物:N-メチルジエタノールアミン(日本乳化剤(株)製 アミノアルコールMDA)
(8)ドデカン二酸(インビスタジャパン(株)製 登録商標Corfree M1)
(1)往復動摩擦試験
1.評価方法
下記試験条件に基づき、摩擦係数を測定することにより評価した。
2.試験条件
試験機:(株)オリエンテック製F-2100
球:3/16インチSUJ2
試験板:多結晶シリコン
摺動速度:20mm/s
摺動距離:2cm
荷重:200g
1.評価方法
Niメッキダイヤモンドワイヤー(素線径0.12mm、粒度12μm以上25μm以下)に加工液1600gを掛け流しながら、下記切断条件により、多結晶シリコン(□156mm)を切断した。加工液は循環使用し、切断を4回実施した。これにより、活性なシリコンの切粉を含む加工液を作製した。切粉を含む加工液100gを静置し、発生するガスを水上置換法によりメスシリンダーに回収し、下記試験条件により定量した。なお、比較例1,2については、摩擦係数が大きいため、試験していない。
2.切断条件
ワイヤーソー:DWT社製CS810(シングルワイヤーソー)
ワイヤー使用量:30m(往復動作により繰返して使用)
ワイヤー走行速度:平均値340m/min
ワイヤー撓み設定:5°
3.試験条件
試験時間:3日間
静置する加工液量:100g
メスシリンダー容量:200ml
1.評価方法
下記評価基準に基づき、加工液に含まれる水の含有量により加工液を評価した。
2.評価基準
水の含有量80%以上:A
水の含有量70%以上80%未満:B
水の含有量60%以上70%未満:C
水の含有量60%未満:D
表1における実施例1から3までの結果より、本発明の加工液は、所定の含窒素化合物を含むため摩擦係数を低減できる。それ故、砥粒の摩耗を抑制し、砥粒の脱落を防止できることがわかる。また、本発明の加工液は、水素の発生量を低減でき、加工液タンクから加工液がオーバーフローすることも防止できることがわかる。さらに、本発明の加工液は、水を主成分としているため、環境負荷が小さく、省資源性に優れる。
一方、比較例1から5まででは、本発明で必須とされる所定のpHを有する含窒素化合物を摩擦調整剤として含まないため、摩擦係数と水素の発生量の増大を両方抑制できない。また、比較例4では、プロピレングリコールを主成分としているため、環境負荷が大きく、省資源性に乏しい。
Claims (8)
- 含窒素化合物を含む摩擦調整剤を配合してなるシリコンウェハ加工液であって、
前記含窒素化合物は、水との質量比(前記含窒素化合物/前記水)を1/99としたときにpHが2以上8以下である
ことを特徴とするシリコンウェハ加工液。 - 請求項1に記載のシリコンウェハ加工液において、
前記含窒素化合物は、複素環化合物である
ことを特徴とするシリコンウェハ加工液。 - 請求項2に記載のシリコンウェハ加工液において、
前記複素環化合物は、ベンゾトリアゾール、3,4-ジヒドロ-3-ヒドロキシ-4-オキソ-1,2,3-ベンゾトリアジン、インダゾール、ベンズイミダゾール、およびそれらの誘導体のうちの少なくともいずれかである
ことを特徴とするシリコンウェハ加工液。 - 請求項1から請求項3までのいずれか1項に記載のシリコンウェハ加工液において、
当該シリコンウェハ加工液は、pHが3以上9以下である
ことを特徴とするシリコンウェハ加工液。 - 請求項1から請求項4までのいずれか1項に記載のシリコンウェハ加工液において、
前記含窒素化合物の含有量は、加工液全量基準で0.05質量%以上10質量%以下である
ことを特徴とするシリコンウェハ加工液。 - 請求項1から請求項5までのいずれか1項に記載のシリコンウェハ加工液において、
当該シリコンウェハ加工液は、加工液全量基準で50質量%以上99.95質量%以下の水を含む
ことを特徴とするシリコンウェハ加工液。 - 請求項1から請求項6までのいずれか1項に記載のシリコンウェハ加工液において、
砥粒が固定されたワイヤーによるシリコンウェハの加工に用いられる
ことを特徴とするシリコンウェハ加工液。 - 含窒素化合物を含む摩擦調整剤を配合してなるシリコンウェハ加工液を用いて、砥粒が固定されたワイヤーによりシリコンウェハを加工するシリコンウェハ加工方法であって、
前記含窒素化合物は、水との質量比(前記含窒素化合物/前記水)を1/99としたときにpHが2以上8以下である
ことを特徴とするシリコンウェハ加工方法。
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EP11819900.9A EP2610896A4 (en) | 2010-08-24 | 2011-08-23 | SILICON WAFER PROCESSING SOLUTION AND SILICON WAFER PROCESSING METHOD |
US13/816,938 US20130143405A1 (en) | 2010-08-24 | 2011-08-23 | Silicon wafer processing solution and silicon wafer processing method |
KR1020137004357A KR101809778B1 (ko) | 2010-08-24 | 2011-08-23 | 실리콘 웨이퍼 가공액 및 실리콘 웨이퍼 가공 방법 |
CN201180040687.6A CN103053010B (zh) | 2010-08-24 | 2011-08-23 | 硅晶片加工液及硅晶片加工方法 |
SG2013009261A SG187749A1 (en) | 2010-08-24 | 2011-08-23 | Silicon wafer processing solution and silicon wafer processing method |
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CN103053010A (zh) | 2013-04-17 |
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EP2610896A4 (en) | 2016-03-30 |
TWI550077B (zh) | 2016-09-21 |
US20130143405A1 (en) | 2013-06-06 |
US9441179B2 (en) | 2016-09-13 |
KR101809778B1 (ko) | 2017-12-15 |
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TW201217505A (en) | 2012-05-01 |
JP5588786B2 (ja) | 2014-09-10 |
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