WO2016132676A1 - シリコンウェーハ研磨用組成物および研磨方法 - Google Patents
シリコンウェーハ研磨用組成物および研磨方法 Download PDFInfo
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- WO2016132676A1 WO2016132676A1 PCT/JP2016/000322 JP2016000322W WO2016132676A1 WO 2016132676 A1 WO2016132676 A1 WO 2016132676A1 JP 2016000322 W JP2016000322 W JP 2016000322W WO 2016132676 A1 WO2016132676 A1 WO 2016132676A1
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- Prior art keywords
- polishing
- polishing composition
- silicon wafer
- acid
- water
- Prior art date
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- 238000005498 polishing Methods 0.000 title claims abstract description 171
- 239000000203 mixture Substances 0.000 title claims abstract description 119
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- 238000004821 distillation Methods 0.000 description 1
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- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
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- GTTBQSNGUYHPNK-UHFFFAOYSA-N hydroxymethylphosphonic acid Chemical compound OCP(O)(O)=O GTTBQSNGUYHPNK-UHFFFAOYSA-N 0.000 description 1
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- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- LQPLDXQVILYOOL-UHFFFAOYSA-I pentasodium;2-[bis[2-[bis(carboxylatomethyl)amino]ethyl]amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC(=O)[O-])CCN(CC([O-])=O)CC([O-])=O LQPLDXQVILYOOL-UHFFFAOYSA-I 0.000 description 1
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- 229960005141 piperazine Drugs 0.000 description 1
- 229960003506 piperazine hexahydrate Drugs 0.000 description 1
- AVRVZRUEXIEGMP-UHFFFAOYSA-N piperazine;hexahydrate Chemical compound O.O.O.O.O.O.C1CNCCN1 AVRVZRUEXIEGMP-UHFFFAOYSA-N 0.000 description 1
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- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
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- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 229940086066 potassium hydrogencarbonate Drugs 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- ARIWANIATODDMH-UHFFFAOYSA-N rac-1-monolauroylglycerol Chemical compound CCCCCCCCCCCC(=O)OCC(O)CO ARIWANIATODDMH-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- 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
-
- 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
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
- H01L21/02024—Mirror polishing
-
- 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
Definitions
- the present invention relates to a polishing composition for a silicon wafer, and more particularly to a polishing composition and a polishing method used when finish polishing a silicon wafer.
- a polishing composition containing silica particles and a water-soluble polymer is suitably used for polishing a silicon wafer.
- a protective film derived from a water-soluble polymer is formed on the polished silicon wafer surface. Since this protective film imparts hydrophilicity to the substrate surface after polishing, handling of the substrate after polishing becomes easy.
- the water-soluble polymer used in the polishing composition has a molecular weight of several hundred thousand or more, it may form an aggregate with silica particles.
- the aggregate composed of the silica particles and the water-soluble polymer may cause a substrate surface defect called “Light Point Defect (LPD)”.
- LPD Light Point Defect
- Patent Document 2 proposes that a surfactant or the like is added to the polishing composition to improve the dispersibility of the abrasive grains.
- Patent Document 3 provides a polishing composition having high dispersibility of abrasive grains while imparting high hydrophilicity to the substrate surface after polishing by including an aggregation inhibitor in the polishing composition. It has been proposed to do.
- finish polishing of a silicon wafer it is also important to suppress contamination of not only LPD caused by aggregates but also metals and metal compounds, particularly nickel (Ni) and copper (Cu).
- Patent Document 1 JP 2005-518668 A Patent Document 2: JP 2001-15461 A Patent Document 3: International Publication 2013/061771 Pamphlet
- An object of the present invention is to polish a silicon wafer while polishing LPD while suppressing contamination of metals, particularly nickel and copper.
- a polishing composition containing abrasive grains, a water-soluble polymer, a basic compound, a chelating agent and water, the particle size determined by a dynamic light scattering method.
- the particle size corresponding to 10% of the volume accumulation from the small particle size side is D10
- the particle size corresponding to 50% of the volume accumulation from the smaller particle size is D50
- the particle size corresponding to 90% of the volume accumulation from the smaller particle size is D90
- a composition for polishing a silicon wafer having a coarse particle frequency parameter A defined by (1) of less than 1.7 is provided.
- A (D90-D50) / (D50-D10) (Formula 1)
- the weight ratio of the abrasive grains, the water-soluble polymer, the basic compound and the chelating agent in the polishing composition is 50 to 95: 1 to It may be 20: 1 to 30: 1 to 10.
- the water-soluble polymer may have a weight average molecular weight of 10,000 to 1,000,000 in the polishing composition.
- the final polishing composition for a silicon wafer is the above polishing composition, wherein the chelating agent is ethylenediaminetetrakis (methylenephosphonic acid) (EDTPO), triethylenetetraminehexaacetic acid (TTHA), diethyl One or more selected from triaminepentaacetic acid (DTPA) may be included.
- the abrasive grains may contain colloidal silica produced by a sol-gel method.
- Another embodiment of the present invention provides a polishing method for performing final polishing in the polishing of a silicon wafer using the polishing composition described above.
- FIG. 1 shows a polishing composition feeder used in the polishing method of the embodiment of the present invention.
- the polishing composition of this embodiment is prepared by mixing abrasive grains, a water-soluble polymer, a basic compound, a chelating agent, and water.
- the abrasive grains serve to physically polish the substrate surface.
- Carbide particles such as nitride particles, silicon carbide particles and boron carbide particles; diamond particles, carbonates such as calcium carbonate and barium carbonate, and the like.
- silica is preferred.
- Specific examples of the silica include silica particles selected from colloidal silica, fumed silica, and sol-gel silica.
- silica particles it is preferable to use silica particles selected from colloidal silica and fumed silica, particularly colloidal silica, from the viewpoint of reducing scratches generated on the polished surface of the silicon wafer substrate.
- one kind may be used alone, or two or more kinds may be used in combination.
- a part of the water-soluble polymer is adsorbed on the abrasive grains, or aggregates of abrasive grains mediated by the water-soluble polymer are formed.
- the average particle size of the particles present in the polishing composition tends to be larger than the polishing composition not containing the water-soluble polymer. is there.
- particles present in the polishing composition are mediated by abrasive raw materials, water-soluble polymer adsorbents of abrasive grains that do not form aggregates, or water-soluble polymers. It is used as a term including agglomerates of abrasive grains.
- the polishing composition of the present embodiment has a particle size distribution in the particle size distribution of the particles present in the polishing composition of the present embodiment based on the volume-based particle size of the particles measured by a particle size distribution measuring apparatus using a dynamic light scattering method.
- the particle size corresponding to 10% of the volume accumulation from the smaller particle size is D10
- the particle size corresponding to 50% of the volume accumulation from the smaller particle size is D50
- the volume accumulation from the smaller particle size is D50.
- the value of the coarse particle frequency parameter A defined by the following (formula 1) is less than 1.7.
- A (D90-D50) / (D50-D10) (Formula 1)
- the value of the coarse particle frequency parameter A indicates the dispersion stability of the abrasive grains in the polishing composition.
- the value of the coarse particle frequency parameter A is less than 1.7, preferably less than 1.5, and more preferably less than 1.4. As the value of the coarse particle frequency parameter A decreases, the dispersion stability of the polishing composition improves and defects are reduced.
- the value of the coarse particle frequency parameter A is in principle 1.0 or more, preferably 1.1 or more. By increasing the value of the coarse particle frequency parameter A, the polishing rate of the silicon wafer is improved.
- the average particle size of the particles present in the polishing composition of the present embodiment is preferably 10 nm or more, more preferably 20 nm or more. By increasing the average particle size of the particles present in the polishing composition, the polishing rate of the silicon wafer is improved. Moreover, it is preferable that the average particle diameter of the particle
- the value of the average particle diameter of the particles is a volume average particle diameter measured by a particle size distribution measuring apparatus using a dynamic light scattering method, and is measured using, for example, model “UPA-UT151” manufactured by Nikkiso Co., Ltd. Can do.
- the average primary particle diameter of the abrasive grains is preferably 5 nm or more, more preferably 10 nm or more.
- the polishing rate of the silicon wafer is improved.
- the average temporary particle diameter of an abrasive grain is 100 nm or less, More preferably, it is 50 nm or less.
- the storage stability of the polishing composition is improved by reducing the average temporary particle size of the abrasive grains.
- the value of the average primary particle diameter of the abrasive grains can be calculated based on the specific surface area of the abrasive grains measured by the BET method.
- the specific surface area of the abrasive grains is, for example, a model “FlowSorbII 2300” manufactured by Micromeritex Corporation. Can be measured.
- the shape (outer shape) of the abrasive grains may be spherical or non-spherical.
- the non-spherical shape include, for example, a so-called saddle shape having a constriction at the center, a shape having a plurality of protrusions on the surface, and a rugby ball shape.
- abrasive grains in which most of the abrasive grains have a peanut shape can be preferably employed.
- the abrasive grains may have a structure in which two or more primary particles are associated.
- the average value of the major axis / minor axis ratio (average aspect ratio) of the primary particles of the abrasive grains is 1.0 or more in principle, preferably 1.1 or more, more preferably 1. 2 or more. Higher polishing rates can be achieved by increasing the average aspect ratio of the abrasive grains.
- the average aspect ratio of the abrasive is preferably 4.0 or less, more preferably 3.0 or less, and further preferably 2.5 or less, from the viewpoint of reducing scratches and the like.
- the shape (outer shape) and average aspect ratio of the abrasive grains can be grasped by, for example, observation with an electron microscope.
- a predetermined number for example, 200
- SEM scanning electron microscope
- the value obtained by dividing the length of the long side (major axis value) by the length of the short side (minor axis value) is the major axis / minor axis ratio (aspect ratio).
- An average aspect ratio can be obtained by arithmetically averaging the aspect ratios of the predetermined number of particles.
- the content of abrasive grains in the polishing composition is preferably 0.01% by weight or more, more preferably 0.03% by weight or more, and still more preferably 0.05% by weight or more.
- the content of abrasive grains in the polishing composition is preferably 5% by weight or less, more preferably 1% by weight or less, and still more preferably 0.5% by weight or less.
- the dispersion stability of the polishing composition is improved, and the abrasive residue after polishing is reduced, so that LPD is reduced.
- polishing composition contains the water-soluble polymer of the solid raw material thrown into water in the solid or solid state as water-soluble polymer at the time of preparation of polishing composition.
- the solid material means a material in a solid or solid state visually in an environment of a material before being dissolved in water at a temperature of 23 ° C., a relative humidity of 50%, and 1 atmosphere.
- water-soluble polymers are synthesized from monomers in water or a mixed solvent of water and an aqueous organic solvent such as alcohol, ketone, etc., but in the form of an aqueous liquid in its solution state, Or the thing of the aqueous solution form which distilled off the volatile solvent is also included.
- water-soluble polymer as a solid raw material “water-soluble polymer in water-based form”, and “water-soluble polymer in aqueous solution form” are simply referred to as “water-soluble polymer”.
- water-soluble polymer those having at least one functional group selected from a cationic group, an anionic group and a nonionic group in the molecule, specifically, a hydroxyl group, a carboxyl group, an acyloxy group, a sulfo group, Any of those containing an amide group, an amidino group, an imino group, an imide group, a quaternary nitrogen structure, a heterocyclic structure containing the functional group unit, a vinyl structure, a polyoxyalkylene structure, or the like can be used.
- cellulose derivatives include cellulose derivatives, polyvinyl alcohol, poly (meth) acrylic acid, poly (meth) acrylamide alkyl sulfonic acid, polyisoprene sulfonic acid, polyvinyl sulfonic acid, polyallyl sulfonic acid, polyisoamylene sulfonic acid, polystyrene sulfone.
- Acid salt poly (meth) acrylamide, polyalkylaminoalkyl (meth) acrylamide, polyvinylpyrrolidone, copolymer containing polyvinylpyrrolidone as part of its structure, polyvinylcaprolactam, copolymer containing polyvinylcaprolactam as part of its structure, Polyalkoxyalkyl (meth) acrylamide, polyhydroxyalkyl (meth) acrylamide, poly (meth) acryloylmorpholine, polyamidine, polyethyleneimine, hydrophilic polyimide, various poly Imine derivatives such as mino acid, poly (N-acylalkyleneimine), polyvinyl alcohol derivatives in which part of the hydroxyl group of polyvinyl alcohol is substituted with a quaternary nitrogen structure, polyoxyethylene, a polymer having a polyoxyalkylene structure, Examples thereof include polymers having a plurality of types of structures such as diblock type, triblock type, random type, and alternating type
- the water-soluble polymers cellulose derivatives, polyvinyl alcohol, polyvinyl pyrrolidone, polyacryloylmorpholine, from the viewpoints of improving wettability on the polished surface of a silicon wafer substrate, suppressing adhesion of particles, and reducing surface roughness, etc.
- a polymer having a polyoxyalkylene structure is suitable.
- Specific examples of the cellulose derivative include hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose, methyl cellulose, ethyl cellulose, ethyl hydroxyethyl cellulose, carboxymethyl cellulose and the like.
- hydroxyethyl cellulose is particularly preferable because it has a high ability to impart wettability to the polished surface of a silicon wafer substrate and has good detergency.
- a water-soluble polymer may be used individually by 1 type, and may be used in combination of 2 or more type.
- the weight average molecular weight of the water-soluble polymer in the polishing composition is preferably 10,000 or more in terms of polyethylene oxide.
- the increase in the weight average molecular weight of the water-soluble polymer tends to increase the wettability of the polished surface of the silicon wafer substrate.
- the weight average molecular weight of the water-soluble polymer in the polishing composition is preferably 2,000,000 or less, more preferably 1,000,000 or less, still more preferably 500,000 or less, Preferably it is 300,000 or less.
- a decrease in the weight average molecular weight of the water-soluble polymer tends to maintain the stability of the polishing composition. Further, the haze level of the polished surface of the silicon wafer substrate tends to be reduced.
- the content of the water-soluble polymer in the polishing composition is preferably 0.0001% by weight or more, more preferably 0.001% by weight or more, and further preferably 0.005% by weight or more.
- the content of the water-soluble polymer in the polishing composition is preferably 0.5% by weight or less, more preferably 0.1% by weight or less, and still more preferably 0.05% by weight or less.
- the polishing composition contains a basic compound.
- the basic compound chemically polishes the polishing surface of the silicon wafer substrate by applying a chemical action (chemical etching). Thereby, it becomes easy to improve the polishing rate at the time of polishing the silicon wafer substrate.
- Specific examples of the basic compound include inorganic basic compounds, alkali metal or alkaline earth metal hydroxides or salts, quaternary ammonium hydroxide or salts thereof, ammonia, amines, and the like.
- Specific examples of the alkali metal include potassium and sodium.
- Specific examples of the salt include carbonate, hydrogen carbonate, sulfate, acetate, and the like.
- the quaternary ammonium include tetramethylammonium, tetraethylammonium, tetrabutylammonium and the like.
- the alkali metal hydroxide or salt include potassium hydroxide, potassium carbonate, potassium hydrogen carbonate, potassium sulfate, potassium acetate, potassium chloride and the like.
- Specific examples of the quaternary ammonium hydroxide or a salt thereof include tetramethylammonium hydroxide, tetraethylammonium hydroxide, and tetrabutylammonium hydroxide.
- amines include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N- ( ⁇ -aminoethyl) ethanolamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, anhydrous piperazine , Piperazine hexahydrate, 1- (2-aminoethyl) piperazine, N-methylpiperazine, guanidine, azoles such as imidazole and triazole, and the like. These basic compounds may be used individually by 1 type, and may be used in combination of 2 or more type.
- the basic compounds at least one selected from ammonia, ammonium salts, alkali metal hydroxides, alkali metal salts, and quaternary ammonium hydroxides is preferable.
- At least one selected from ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, and tetraethylammonium hydroxide is more preferable, and more preferably at least one of ammonia and tetramethylammonium hydroxide. Yes, most preferably ammonia.
- the content of the basic compound in the polishing composition is preferably 0.0001% by weight or more, more preferably 0.001% by weight or more, and further preferably 0.005% by weight or more.
- the content of the basic compound in the polishing composition is preferably 0.5% by weight or less, more preferably 0.1% by weight or less, still more preferably 0.05% by weight or less, Preferably it is 0.01 weight% or less. Due to the decrease in the content of the basic compound in the polishing composition, the smoothness of the substrate surface after polishing tends to be improved.
- the polishing composition contains a chelating agent.
- the chelating agent suppresses metal contamination of the silicon wafer substrate by capturing metal impurity components in the polishing system to form a complex.
- a chelating agent is contained in the polishing composition, the dispersion stability of the particles of the composition is lowered.
- a chelating agent is generally not included.
- the inventors pay attention to the particle size distribution of the particles present in the polishing composition, and even when a chelating agent is used, when the value of the coarse particle frequency parameter A satisfies less than 1.7, the particles of the composition It has been found that since the dispersion stability is not impaired, defects can be reduced and contamination of metals such as nickel and copper on the silicon wafer substrate can be suppressed.
- chelating agents include aminocarboxylic acid chelating agents and organic phosphonic acid chelating agents.
- Specific examples of the aminocarboxylic acid-based chelating agent include, for example, ethylenediaminetetraacetic acid, ethylenediaminetetraacetic acid sodium, nitrilotriacetic acid, nitrilotriacetic acid sodium, nitrilotriacetic acid ammonium, hydroxyethylethylenediaminetriacetic acid, hydroxyethylethylenediaminetriacetic acid sodium salt, Examples include diethylenetriaminepentaacetic acid, sodium diethylenetriaminepentaacetate, triethylenetetraminehexaacetic acid and sodium triethylenetetraminehexaacetate.
- organic phosphonic acid chelating agent examples include, for example, 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetrakis (methylenephosphonic acid), diethylenetriaminepenta (Methylenephosphonic acid), ethane-1,1-diphosphonic acid, ethane-1,1,2-triphosphonic acid, ethane-1-hydroxy-1,1-diphosphonic acid, ethane-1-hydroxy-1,1,2 -Triphosphonic acid, ethane-1,2-dicarboxy-1,2-diphosphonic acid, methanehydroxyphosphonic acid, 2-phosphonobutane-1,2-dicarboxylic acid, 1-phosphonobutane-2,3,4-tricarboxylic acid and ⁇ -Methylphosphonosuccinic acid.
- 2-aminoethylphosphonic acid 1-hydroxyethylidene-1,1-diphospho
- ethylenediaminetetraacetic acid, diethyltriaminepentaacetic acid, triethylenetetraminehexaacetic acid, ethylenediaminetetrakis (methylenephosphonic acid), and diethylenetriaminepenta (methylenephosphonic acid) are preferably used, and ethylenediaminetetrakis (methylenephosphonic acid) is used. Most preferably, it is used.
- a chelating agent may be used individually by 1 type, and may be used in combination of 2 or more type.
- the content of the chelating agent in the polishing composition is preferably 0.0001% by weight or more, more preferably 0.001% by weight or more, and most preferably 0.002% by weight or more.
- the content of the chelating agent in the polishing composition is preferably 1% by weight or less, more preferably 0.5% by weight or less, and most preferably 0.1% by weight or less.
- the weight ratio of the abrasive grains, the water-soluble polymer, the basic compound and the chelating agent may be 50 to 95: 1 to 20: 1 to 30: 1 to 10.
- Water becomes a dispersion medium or solvent for other components.
- the total content of transition metal ions is preferably 100 ppb or less.
- the purity of water can be increased by operations such as removal of impurity ions using an ion exchange resin, removal of particles by a filter, and distillation. Specifically, it is preferable to use ion exchange water, pure water, ultrapure water, distilled water or the like.
- the pH of the polishing composition is preferably 8.0 or more, more preferably 8.5 or more, and still more preferably 9.0 or more. By increasing the pH of the polishing composition, a high polishing rate tends to be obtained when the silicon wafer substrate is polished. It is preferable that pH of polishing composition is 11.0 or less, More preferably, it is 10.8 or less, More preferably, it is 10.5 or less. A decrease in the pH of the polishing composition tends to reduce the roughness of the silicon wafer substrate.
- the polishing composition may further contain a surfactant.
- a surfactant By adding the surfactant, it is possible to suppress the roughness of the substrate surface due to the chemical etching action of the basic compound, and the surface smoothness is improved.
- the surfactant include an anionic or nonionic surfactant.
- nonionic surfactants are preferably used. Since the nonionic surfactant has low foaming property, it is easy to handle at the time of preparation and use of the polishing composition. In addition, for example, pH adjustment is easier than when an ionic surfactant is used.
- nonionic surfactants include oxyalkylene homopolymers, multiple types of oxyalkylene copolymers, and polyoxyalkylene adducts.
- Specific examples of the oxyalkylene homopolymer include polyoxyethylene, polyethylene glycol, polyoxypropylene and polyoxybutylene.
- Specific examples of the plural types of oxyalkylene copolymers include polyoxyethylene polyoxypropylene glycol and polyoxyethylene polyoxybutylene glycol.
- polyoxyalkylene adducts include polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene alkylamine, polyoxyethylene fatty acid ester, polyoxyethylene glyceryl ether fatty acid ester, polyoxyethylene sorbitan fatty acid ester Etc.
- polyoxyethylene polyoxypropylene copolymer polyoxyethylene glycol, polyoxyethylene propyl ether, polyoxyethylene butyl ether, polyoxyethylene pentyl ether, polyoxyethylene hexyl ether, polyoxyethylene octyl ether, Polyoxyethylene-2-ethylhexyl ether, polyoxyethylene nonyl ether, polyoxyethylene decyl ether, polyoxyethylene isodecyl ether, polyoxyethylene tridecyl ether, polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene Stearyl ether, polyoxyethylene isostearyl ether, polyoxyethylene oleyl ether, polyoxyethylene Phenyl ether, polyoxyethylene octyl phenyl ether, polyoxyethylene nonyl phenyl ether, polyoxyethylene dodecyl phenyl ether, polyoxyethylene styrenated phenyl ether, polyoxyethylene lauryl
- the ratio of oxyethylene units in the oxyalkylene homopolymer or the plurality of types of oxyalkylene copolymers is preferably 85% by mass or more, and more preferably 90% by mass or more. The increase in the ratio of oxyethylene units in the polymer tends to suppress the adhesion of particles to the polished surface of the polished silicon wafer substrate.
- the molecular weight of the surfactant is typically less than 10,000, and is preferably 9500 or less from the viewpoints of filterability of the polishing composition and cleanability of the object to be polished.
- the molecular weight of the surfactant is typically 200 or more, preferably 250 or more, more preferably 300 or more, and further preferably 500 or more from the viewpoint of the haze reduction effect and the like.
- the molecular weight of the surfactant may be a weight average molecular weight (Mw) determined by GPC (aqueous, polyethylene glycol equivalent) or a molecular weight calculated from a chemical formula.
- the more preferable range of the molecular weight of the surfactant may vary depending on the type of the surfactant.
- the Mw is preferably 1000 or more, more preferably 2000 or more, and even more preferably 5000 or more.
- the HLB (hydrophile-lipophile balance) value of the nonionic surfactant is preferably 8 or more, more preferably 10 or more, and further preferably 12 or more. Due to the increase in the HLB value of the nonionic surfactant, the adhesion of particles to the polished surface of the polished silicon wafer substrate tends to be suppressed.
- a surfactant may be used individually by 1 type, and may be used in combination of 2 or more type.
- the content of the surfactant in the polishing composition is preferably 0.0001% by mass or more, and more preferably 0.001% by mass or more. By increasing the surfactant content, the haze of the semiconductor substrate surface after polishing tends to be further reduced.
- the content of the surfactant in the polishing composition is preferably 0.05% by mass or less, more preferably 0.02% by mass or less. Due to the decrease in the surfactant content, the adhesion of particles to the polished surface of the polished silicon wafer substrate tends to be suppressed.
- the polishing composition further contains known additives generally contained in the polishing composition as necessary, for example, organic acids, organic acid salts, inorganic acids, inorganic acid salts, preservatives, antifungal agents and the like. May be.
- organic acids organic acid salts
- inorganic acids inorganic acid salts
- preservatives antifungal agents and the like. May be.
- the hydrophilicity of the polished surface of the polished silicon wafer substrate is improved by the interaction with the water-soluble polymer. be able to.
- organic acids include fatty acids such as formic acid, acetic acid and propionic acid, aromatic carboxylic acids such as benzoic acid and phthalic acid, citric acid, oxalic acid, tartaric acid, malic acid, maleic acid, fumaric acid, succinic acid, Organic sulfonic acid, organic phosphonic acid, etc. are mentioned.
- organic acid salt include alkali metal salts such as sodium salts and potassium salts of organic acids described in the specific examples of organic acids, or ammonium salts.
- the inorganic acid include sulfuric acid, nitric acid, hydrochloric acid, carbonic acid and the like.
- Specific examples of the inorganic acid salt include alkali metal salts such as sodium salts and potassium salts of inorganic acids described in the specific examples of inorganic acids, or ammonium salts.
- organic acid salts and inorganic acid salts ammonium salts are preferable from the viewpoint of suppressing metal contamination of the silicon wafer substrate.
- An organic acid and its salt, and an inorganic acid and its salt may be used individually by 1 type, and may be used in combination of 2 or more type.
- FIG. 1 is a perspective view showing a single-side polishing apparatus according to an embodiment of the present invention.
- the polishing apparatus 11 includes a disk-shaped rotating surface plate 12 having a polishing pad 14 attached to the upper surface.
- the rotating surface plate 12 is provided so as to be integrally rotatable with respect to the first shaft 13 that rotates in the direction of the arrow 13a in FIG.
- At least one wafer holder 15 is provided above the rotating platen 12.
- the wafer holder 15 is provided so as to be integrally rotatable with respect to the second shaft 16 that rotates in the direction of the arrow 16a in FIG.
- a wafer holding plate 19 having wafer holding holes 18 is detachably attached to the bottom surface of the wafer holder 15 via a ceramic plate 17 and a urethane sheet (not shown).
- the polishing apparatus 11 further includes a polishing composition supply machine 21 and a rinse composition supply machine (not shown).
- the polishing composition supply machine 21 discharges the polishing composition through the nozzle 21a, and the rinsing composition supply machine discharges the rinsing composition through a nozzle (not shown).
- Either one of the polishing composition supply machine 21 and the rinsing composition supply machine is disposed above the rotating platen 12.
- One feeder disposed above the rotating surface plate 12 and the other feeder not disposed above the rotating surface plate 12 can be replaced with each other.
- a polishing composition supply machine 21 is disposed above the rotating platen 12 as shown in FIG.
- the silicon wafer to be polished is sucked into the wafer holding hole 18 and held by the wafer holder 15.
- the rotation of the wafer holder 15 and the rotating surface plate 12 is started, and the polishing composition is discharged from the polishing composition supply machine 21 to supply the polishing composition onto the polishing pad 14.
- the wafer holder 15 is moved toward the rotating surface plate 12 in order to press the silicon wafer against the polishing pad 14. Thereby, the surface of the silicon wafer in contact with the polishing pad 14 is polished.
- the polished silicon wafer can be rinsed.
- a rinsing composition supply machine is disposed above the rotating platen 12 instead of the polishing composition supply machine 21.
- the rinsing composition is discharged from the rinsing composition supply machine and the rinsing composition is supplied onto the polishing pad 14. As a result, the surface of the silicon wafer in contact with the polishing pad 14 is rinsed.
- the polishing of the silicon wafer surface is preferably performed in a plurality of stages.
- the silicon wafer surface may be polished in three stages: a first stage of rough polishing, a second stage of precision polishing, and a third stage of final polishing.
- the polishing composition of the present invention is used in finish polishing when polishing in a plurality of stages.
- abrasive grains colloidal silica having a volume average particle diameter of 46 nm measured using a model “UPA-UT151” manufactured by Nikkiso Co., Ltd. was used.
- two cleaning tanks equipped with an ultrasonic oscillator having a frequency of 950 kHz are prepared, and the cleaning liquid is accommodated in each of the first and second cleaning tanks and held at 60 ° C., and the surface-treated silicon wafer Was immersed in the first cleaning tank for 6 minutes, then passed through an ultrapure water and ultrasonic rinsing tank, and then immersed in the second cleaning tank for 6 minutes, each with the ultrasonic oscillator being operated.
- the total number of defects measured by a wafer inspection apparatus (MAGICS M5350, manufactured by Lasertec Corporation) was evaluated. The results are shown in Table 1.
- the number of PIDs is less than 150, S, 150 to less than 250, A, 250 to less than 300, B, 300 to less than 350, C, The case of 350 or more was expressed as D.
- the particle diameter of the composition indicates a value measured by a dynamic light scattering method using UPA-UT151 manufactured by Nikkiso Co., Ltd. All aggregates of abrasive grains mediated by water-soluble polymer adsorbents or water-soluble polymers are included.
- the parameter A represented by (Equation 1) was less than 1.7, and in Examples 1 to 13 containing a chelating agent, the number of PIDs was less than 350. In Comparative Examples 1, 3, and 4 where A was 1.7 or more, the PID number was 350 or more, and in Comparative Example 2 containing no chelating agent, the PID was less than 350. In Comparative Example 5 containing no chelating agent, the PID number was less than 150. However, as described later, the amount of metal contamination of Cu and Ni was large.
- the polishing composition containing abrasive grains, water-soluble polymer, chelating agent, and basic compound of the same type and content as used in the PID defect evaluation test shown in Table 1 is further added to 0.005 wt.
- a polishing composition forcibly contaminated with Ni and Cu in an amount of 150% a silicon wafer having a diameter of 150 mm is polished under the following conditions, followed by cleaning to evaluate metal contamination. Went.
- the load was set to 31.5 kPa using a single-wafer grinder, model “SPM-15” manufactured by Fujikoshi Machinery Co., Ltd. as the grinder.
- Polishing was performed for 900 seconds with a platen rotation speed of 30 rpm, a wafer holder rotation speed of 120 rpm, a composition supply speed of 8.0 liters / minute (using a flow-through), and a polishing composition temperature of 23 ° C.
- DIW deionized water
- one cleaning tank equipped with an ultrasonic oscillator with a frequency of 950 kHz is prepared, the cleaning liquid is accommodated in this cleaning tank and held at 80 ° C., and the surface-treated silicon wafer is stored in the cleaning tank for 6 minutes. It was immersed in a state where the sonic oscillator was activated, and then washed with ultrapure water and ultrasonic waves.
- Cu amount is, 1 ⁇ 10 9 atoms / the case of cm 2 S, 1 ⁇ 10 9 atoms / cm 2 or more 3 ⁇ 10 9 atoms / cm 2 less than the case A, 3 ⁇ 10 9 atoms / cm 2 or more 10 ⁇ 10 9 a case where less than atoms / cm 2 of B, less than 10 ⁇ 10 9 atoms / cm 2 or more 15 ⁇ 10 9 atoms / cm 2 C, 15
- the case of ⁇ 10 9 atoms / cm 2 or more was expressed as D.
- the parameter A represented by (Formula 1) is less than 1.7, and in Examples 1 to 13 containing a chelating agent, the amount of Cu is less than 10 ⁇ 10 9 atoms / cm 2 , Whereas the amount of Ni was less than 10 ⁇ 10 9 atoms / cm 2 , the amount of Cu was less than 10 ⁇ 10 9 atoms / cm 2 in Comparative Examples 1, 3 and 4 where the parameter A was 1.7 or more, Although the amount of Ni was less than 10 ⁇ 10 9 atoms / cm 2 , in Comparative Example 2 not including a chelating agent, the amount of Cu was 15 ⁇ 10 9 atoms / cm 2 or more, and the amount of Ni was 10 ⁇ 10 9 atoms. / cm 2 or more, and the Comparative example 5, Cu amount is 10 ⁇ 10 9 atoms / cm 2 or more, Ni amount was 10 ⁇ 10 9 atoms / cm 2 or more.
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Abstract
Description
また、シリコンウェーハの仕上げ研磨においては、凝集体に起因するLPDだけでなく、金属や金属化合物、特に、ニッケル(Ni)、銅(Cu)の汚染を抑制することも重要である。
特許文献2 : 特開2001-15461号公報
特許文献3 : 国際公開2013/061771号パンフレット
A=(D90-D50)/(D50-D10) (式1)
本発明の他の実施態様のシリコンウェーハの仕上げ研磨用組成物は、上記研磨用組成物において、水溶性高分子が、重量平均分子量が10,000~1,000,000であってもよい。
本発明の他の実施態様のシリコンウェーハの仕上げ研磨用組成物は、上記研磨用組成物において、前記砥粒はゾルゲル法により製造されるコロイダルシリカを含んでもよい。
本発明の他の実施態様は、上記の研磨用組成物を使用して、シリコンウェーハの研磨における仕上げ研磨を行う研磨方法を提供する。
本実施形態の研磨用組成物は、砥粒、水溶性高分子、塩基性化合物、キレート剤及び水を混合することにより調製される。
(砥粒)
砥粒は、基板表面を物理的に研磨する働きをする。シリカ粒子、アルミナ粒子、酸化セリウム粒子、酸化クロム粒子、二酸化チタン粒子、酸化ジルコニウム粒子、酸化マグネシウム粒子、二酸化マンガン粒子、酸化亜鉛粒子、ベンガラ粒子等の酸化物粒子、窒化ケイ素粒子、窒化ホウ素粒子等の窒化物粒子、炭化ケイ素粒子、炭化ホウ素粒子等の炭化物粒子;ダイヤモンド粒子、炭酸カルシウムや炭酸バリウム等の炭酸塩等が挙げられる。
A=(D90-D50)/(D50-D10) (式1)
粗大粒子頻度パラメータAの値は、原理的に1.0以上であり、好ましくは1.1以上ある。粗大粒子頻度パラメータAの値の増大によって、シリコンウェーハの研磨速度が向上する。
研磨用組成物中の砥粒の含有量は5重量%以下であることが好ましく、より好ましくは1重量%以下であり、更に好ましくは0.5重量%以下である。砥粒の含有量が上記の範囲内にある場合、研磨用組成物の分散安定性が向上し、また、研磨後の砥粒残渣が減少するため、LPDが低減する。
水溶性高分子は、研磨時やリンス処理時等のシリコンウェーハ基板の表面処理時において、シリコンウェーハ基板の研磨面の濡れ性を高める。研磨用組成物は、水溶性高分子として、研磨用組成物の調製時に固体又は固形の状態で水に投入される固体原料の水溶性高分子を含有する。固体原料とは、水に溶解する前の原料の状態において、温度23℃、相対湿度50%、及び1気圧の環境下にて目視で固体又は固形の状態のものを意味する。又、水溶性高分子は水、又は水とアルコール、ケトン等の水系有機溶剤との混合溶剤中において単量体から合成されるものもあるが、その溶液状態のままの水系液形態のもの、あるいは、揮発性溶剤を留去した水溶液形態のものも含む。なお、以下では「固体原料の水溶性高分子」や「水系形態の水溶性高分子」、「水溶液形態の水溶性高分子」を単純に「水溶性高分子」と記載する。
研磨用組成物中の水溶性高分子の重量平均分子量は、好ましくは2,000,000以下であり、より好ましくは1,000,000以下であり、更に好ましくは500,000以下であり、最も好ましくは300,000以下である。水溶性高分子の重量平均分子量の減少によって、研磨用組成物の安定性がより保たれる傾向となる。また、更にシリコンウェーハ基板の研磨面のヘイズレベルが低減する傾向となる。
研磨用組成物中の水溶性高分子の含有量は、好ましくは0.5重量%以下であり、より好ましくは0.1重量%以下であり、更に好ましくは0.05重量%以下である。研磨用組成物中における水溶性高分子の含有量の減少によって、研磨用組成物の安定性がより保たれる傾向となる。
研磨用組成物は、塩基性化合物を含有する。塩基性化合物は、シリコンウェーハ基板の研磨面に対して、化学的な作用を与えて化学的に研磨する(ケミカルエッチング)。これにより、シリコンウェーハ基板を研磨する際の研磨速度を向上させることが容易となる。
塩基性化合物の具体例としては、無機の塩基性化合物、アルカリ金属またはアルカリ土類金属の水酸化物又は塩、水酸化第四級アンモニウム又はその塩、アンモニア、アミン等が挙げられる。アルカリ金属の具体例としては、カリウム、ナトリウム等が挙げられる。塩の具体例としては、炭酸塩、炭酸水素塩、硫酸塩、酢酸塩等が挙げられる。第四級アンモニウムの具体例としては、テトラメチルアンモニウム、テトラエチルアンモニウム、テトラブチルアンモニウム等が挙げられる。アルカリ金属の水酸化物又は塩の具体例としては、水酸化カリウム、炭酸カリウム、炭酸水素カリウム、硫酸カリウム、酢酸カリウム、塩化カリウム等が挙げられる。水酸化第四級アンモニウム又はその塩の具体例としては、水酸化テトラメチルアンモニウム、水酸化テトラエチルアンモニウム、水酸化テトラブチルアンモニウム等が挙げられる。アミンの具体例としては、メチルアミン、ジメチルアミン、トリメチルアミン、エチルアミン、ジエチルアミン、トリエチルアミン、エチレンジアミン、モノエタノールアミン、N-(β-アミノエチル)エタノールアミン、ヘキサメチレンジアミン、ジエチレントリアミン、トリエチレンテトラミン、無水ピペラジン、ピペラジン六水和物、1-(2-アミノエチル)ピペラジン、N-メチルピペラジン、グアニジン、イミダゾールやトリアゾール等のアゾール類等が挙げられる。これらの塩基性化合物は、一種を単独で用いてもよいし、二種以上を組み合わせて用いてもよい。
研磨用組成物中の塩基性化合物の含有量は、好ましくは0.5重量%以下であり、より好ましくは0.1重量%以下であり、更に好ましくは0.05重量%以下であり、最も好ましくは0.01重量%以下である。研磨用組成物中における塩基性化合物の含有量の減少によって、研磨後の基板表面の平滑性が向上する傾向となる。
研磨用組成物は、キレート剤を含有する。キレート剤は、研磨系中の金属不純物成分を捕捉して錯体を形成することによってシリコンウェーハ基板の金属汚染を抑制する。
一般に研磨用組成物にキレート剤が含まれると、組成物の粒子の分散安定性が低下する。特に水溶性高分子を含有する場合、組成物の粒子の分散安定性が大きく損なわれるため、一般的にはキレート剤は含まれない。本発明者らは、研磨用組成物中に存在する粒子の粒度分布に着目し、キレート剤を使用しても、粗大粒子頻度パラメータAの値が1.7未満を満たすときには、組成物の粒子の分散安定性が損なわれないため、欠陥を低減することができるとともに、シリコンウェーハ基板のニッケル、銅等の金属の汚染を抑制することができることを見出した。
研磨用組成物中のキレート剤の含有量は、好ましくは1重量%以下、より好ましくは0.5重量%以下、最も好ましくは0.1重量%以下である。キレート剤の含有量の低減によって、研磨用組成物の安定性がより保たれる傾向となる。
上記研磨用組成物において、砥粒、水溶性高分子、塩基性化合物およびキレート剤の重量比が、50~95:1~20:1~30:1~10であるといよい。各成分比をこの範囲にすることによって、研磨組成物の分散安定性が向上し、かつ洗浄後のシリコンウェーハの清浄性が向上する。
水は他の成分の分散媒又は溶媒となる。水は研磨用組成物に含有される他の成分の働きが阻害されることを極力回避するため、例えば遷移金属イオンの合計含有量が100ppb以下とされることが好ましい。例えば、イオン交換樹脂を用いる不純物イオンの除去、フィルターによる粒子の除去、蒸留等の操作によって水の純度を高めることができる。具体的にはイオン交換水、純水、超純水、蒸留水等を用いることが好ましい。
研磨用組成物のpHは8.0以上であることが好ましく、より好ましくは8.5以上であり、更に好ましくは9.0以上である。研磨用組成物のpHの増大によって、シリコンウェーハ基板を研磨する際に高い研磨速度が得られる傾向となる。研磨用組成物のpHは11.0以下であることが好ましく、より好ましくは10.8以下であり、更に好ましくは10.5以下である。研磨用組成物のpHの減少によって、シリコンウェーハ基板の粗さを低減できる傾向となる。
研磨用組成物は、更に界面活性剤を含有してもよい。界面活性剤を添加することで、塩基性化合物のケミカルエッチング作用に起因する基板表面の荒れを抑制することができ、表面の平滑性が向上する。
界面活性剤としては、アニオン性又はノニオン性の界面活性剤が挙げられる。界面活性剤の中でも、ノニオン性界面活性剤が好適に用いられる。ノニオン性界面活性剤は、起泡性が低いため、研磨用組成物の調製時や使用時の取り扱いが容易となる。また、例えばイオン性の界面活性剤を用いた場合よりも、pH調整が容易となる。
また、オキシアルキレンの単独重合体又は複数の種類のオキシアルキレンの共重合体におけるオキシエチレン単位の比率は、85質量%以上であることが好ましく、より好ましくは90質量%以上である。重合体中のオキシエチレン単位の比率の増大によって、研磨後のシリコンウェーハ基板の研磨面に対するパーティクルの付着が抑制される傾向がある。
また、ノニオン性界面活性剤のHLB(hydrophile-lipophile Balance)値は、8以上であることが好ましく、より好ましくは10以上、さらに好ましくは12以上である。ノニオン性界面活性剤のHLB値の増大によって、研磨後のシリコンウェーハ基板の研磨面に対するパーティクルの付着が抑制される傾向がある。
研磨用組成物は、必要に応じて研磨用組成物に一般に含有されている公知の添加剤、例えば有機酸、有機酸塩、無機酸、無機酸塩、防腐剤、防カビ剤等を更に含有してもよい。例えば、有機酸、有機酸塩、無機酸及び無機酸塩のいずれかを添加した場合には、水溶性高分子との相互作用により、研磨後のシリコンウェーハ基板の研磨面の親水性を向上させることができる。
有機酸塩及び無機酸塩の中でも、シリコンウェーハ基板の金属汚染を抑制するという点から、アンモニウム塩が好ましい。
有機酸及びその塩、並びに無機酸及びその塩は、一種を単独で用いてもよく、二種以上を組み合わせて用いてもよい。
次に、研磨装置について説明する。図1は、本発明の一実施形態による片面研磨装置を示す斜視図である。
研磨装置11は、上面に研磨パッド14が貼り付けられた円板状の回転定盤12を備えている。回転定盤12は、図1の矢印13a方向に回転する第1シャフト13に対して一体回転可能に設けられている。回転定盤12の上方には少なくとも一つのウェーハホルダ15が設けられている。ウェーハホルダ15は、図1の矢印16a方向に回転する第2シャフト16に対して一体回転可能に設けられている。ウェーハホルダ15の底面には、セラミックプレート17及び図示しないウレタンシートを介して、ウェーハ保持孔18を有するウェーハ保持プレート19が取り外し可能に取り付けられている。研磨装置11は、研磨用組成物供給機21及び図示しないリンス用組成物供給機をさらに備えている。研磨用組成物供給機21は、ノズル21aを通じて研磨用組成物を吐出し、リンス用組成物供給機は図示しないノズルを通じてリンス用組成物を吐出する。研磨用組成物供給機21及びリンス用組成物供給機のいずれか一方が回転定盤12の上方に配置される。回転定盤12の上方に配置された一方の供給機と回転定盤12の上方に配置されない他方の供給機とは互いに取り替え可能である。
(PID欠陥評価試験)
それぞれ表1に示される種類と含有量の砥粒、水溶性高分子(ヒドロキシエチルセルロース:HEC、ポリビニルピロリドン:PVP、ポリアクリロイルモルホリン:PACMO)、キレート剤、塩基性化合物を含む研磨用組成物を使用して、直径300mmのシリコンウェーハを以下の条件により、研磨、これに続いて洗浄を行い、PID(欠陥)の評価を行った。なお、砥粒として、日機装株式会社製の型式「UPA-UT151」を用いて測定された体積平均粒子径が46nmのコロイダルシリカを用いた。
研磨後のシリコンウェーハを、NH4OH(29%):H2O2(31%):脱イオン水(DIW)=1:3:30(体積比)の洗浄液を用いて洗浄した(SC-1洗浄)。その際、周波数950kHzの超音波発振器を取り付けた洗浄槽を2つ用意し、それら第1および第2の洗浄槽の各々に上記洗浄液を収容して60℃に保持し、表面処理後のシリコンウェーハを第1の洗浄槽に6分、その後超純水と超音波によるリンス槽を経て、第2の洗浄槽に6分、それぞれ上記超音波発振器を作動させた状態で浸漬した。
なお、表1において、PID数が150個未満の場合をS、150個以上250個未満の場合をA、250個以上300個未満の場合をB、300個以上350個未満の場合をC、350個以上の場合をDと表記した。また、表1において組成物粒子径は日機装株式会社製のUPA-UT151を用いた動的光散乱法で測定した値を示しており、砥粒原料、凝集体を形成していない砥粒の水溶性高分子吸着体あるいは水溶性高分子によって媒介された砥粒の凝集体を全て含んでいる。
表1に示されるように、(式1)で表されるパラメータAが1.7未満であり、キレート剤を含む実施例1~13ではPID数が350個未満であったのに対し、パラメータAが1.7以上の比較例1、3および4ではPID数が350個以上となり、キレート剤を含まない比較例2ではPIDは350個未満であった。また、キレート剤を含まない比較例5はPID数は150未満であったが、後に述べるように、CuおよびNiの金属汚染量が多かった。
次に、表1に示されるPID欠陥評価試験で使用したと同じ種類と含有量の砥粒、水溶性高分子、キレート剤、塩基性化合物を含む研磨用組成物にさらに、それぞれ0.005重量%のNiとCuを添加させて、強制的に汚染させた研磨用組成物を使用して、直径150mmのシリコンウェーハを以下の条件により、研磨、これに続いて洗浄を行い、金属汚染の評価を行った。
研磨機として不二越機械工業株式会社製の枚葉研磨機、型式「SPM-15」を使用して、荷重を31.5kPaに設定した。定盤回転数を30rpm、ウェーハホルダ回転数を120rpm、組成物の供給速度を8.0リットル/分(掛け流し使用)、研磨組成物の温度を23℃とし、900秒間研磨を行った。
研磨後のシリコンウェーハを、HCl(36%):H2O2(31%):脱イオン水(DIW)=1:1:6(体積比)の洗浄液を用いて洗浄した(SC-2洗浄)。その際、周波数950kHzの超音波発振器を取り付けた洗浄槽を1つ用意し、この洗浄槽に上記洗浄液を収容して80℃に保持し、表面処理後のシリコンウェーハを洗浄槽に6分上記超音波発振器を作動させた状態で浸漬し、その後超純水と超音波により洗浄した。
上記の条件により研磨、洗浄を行った後、シリコンウェーハを200℃で48時間熱処理を行い、シリコンウェーハ内部の金属不純物をシリコンウェーハ表面にまで移動させた。シリコンウェーハ表面の自然酸化膜をフッ酸蒸気により気相分解して、これをフッ酸と過酸化水素水とを含有する液滴で回収し、回収液中の金属不純物を誘導結合プラズマ質量分析(ICP-MS)によって定量分析した。結果を表1に示した。
また、表1において、Ni量が、1×109原子数/cm2未満の場合をA、1×109原子数/cm2以上3×109原子数/cm2未満の場合をB、3×109原子数/cm2以上10×109原子数/cm2未満の場合をC、10×109原子数/cm2以上の場合をDと表記した。
Claims (6)
- 砥粒、水溶性高分子、塩基性化合物、キレート剤及び水を含有する研磨用組成物であって、
前記研磨用組成物中に存在する粒子の粒度分布において、粒径が小さい側からの体積累積が10%に相当する粒径をD10とし、粒径が小さい側からの体積累積が50%に相当する粒径をD50とし、粒径が小さい側からの体積累積が90%に相当する粒径をD90とするときに、下記(式1)で定義される粗大粒子頻度パラメータAの値が1.7未満であり、
シリコンウェーハ研磨における仕上げ研磨に使用されることを特徴とする研磨用組成物。
A=(D90-D50)/(D50-D10) (式1) - 前記砥粒、前記水溶性高分子、前記塩基性化合物および前記キレート剤の重量比は、50~95:1~20:1~30:1~10であることを特徴とする請求項1に記載の研磨用組成物。
- 前記水溶性高分子は、重量平均分子量が10,000~1,000,000であることを特徴とする請求項1または2に記載の研磨用組成物。
- 前記キレート剤は、 エチレンジアミンテトラキス(メチレンホスホン酸)(EDTPO)、トリエチレンテトラミン六酢酸(TTHA)、ジエチルトリアミン五酢酸(DTPA)から選ばれる1または2以上を含むことを特徴とする請求項1~3のいずれか一項に記載の研磨用組成物。
- 前記砥粒はゾルゲル法により製造されるコロイダルシリカを含むことを特徴とする請求項1~4のいずれか一項に記載の研磨用組成物。
- 請求項1~5のいずれか一項に記載の研磨用組成物を使用して、シリコンウェーハの研磨における仕上げ研磨を行うことを特徴とするシリコンウェーハの研磨方法。
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EP3261114A1 (en) | 2017-12-27 |
KR102515826B1 (ko) | 2023-03-30 |
TWI683895B (zh) | 2020-02-01 |
EP3261114A4 (en) | 2018-02-14 |
EP3261114B1 (en) | 2021-01-13 |
KR20170118690A (ko) | 2017-10-25 |
JPWO2016132676A1 (ja) | 2017-11-24 |
JP6572299B2 (ja) | 2019-09-04 |
TW201702347A (zh) | 2017-01-16 |
US20180066161A1 (en) | 2018-03-08 |
US10273383B2 (en) | 2019-04-30 |
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