WO2011071168A1 - Ｃｍｐ研磨液、基板の研磨方法及び電子部品 - Google Patents

Ｃｍｐ研磨液、基板の研磨方法及び電子部品 Download PDF

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Publication number
WO2011071168A1
WO2011071168A1 PCT/JP2010/072291 JP2010072291W WO2011071168A1 WO 2011071168 A1 WO2011071168 A1 WO 2011071168A1 JP 2010072291 W JP2010072291 W JP 2010072291W WO 2011071168 A1 WO2011071168 A1 WO 2011071168A1
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WIPO (PCT)
Prior art keywords
polishing
liquid
film
substrate
cerium
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PCT/JP2010/072291
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English (en)
French (fr)
Japanese (ja)
Inventor
隆 篠田
和宏 榎本
利明 阿久津
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日立化成工業株式会社
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Application filed by 日立化成工業株式会社 filed Critical 日立化成工業株式会社
Priority to KR1020117030563A priority Critical patent/KR101277029B1/ko
Priority to KR1020127028711A priority patent/KR20120135921A/ko
Priority to US13/265,926 priority patent/US20120299158A1/en
Priority to CN201080028913.4A priority patent/CN102473621B/zh
Publication of WO2011071168A1 publication Critical patent/WO2011071168A1/ja
Priority to US13/670,356 priority patent/US20130059439A1/en

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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
    • H01L21/04—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
    • C09K3/1472—Non-aqueous liquid suspensions
    • 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
    • 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 substrate polishing method, and an electronic component.
  • This CMP technique can reduce the burden of the exposure technique by almost completely planarizing the layer to be exposed in the manufacturing process of the semiconductor device, and can stabilize the yield at a high level. Therefore, the CMP technique is an essential technique when performing, for example, planarization of an interlayer insulating film, a BPSG film, shallow trench isolation, and the like.
  • the CMP polishing liquid that is generally used is a CMP polishing liquid whose main object is polishing a silicon oxide film, and a silicon oxide film or a polysilicon film is polished five times or more faster than a silicon nitride film. There is usually a characteristic.
  • Patent Document 1 there is a technique that increases the polishing rate of the silicon nitride film by adding phosphoric acid in an amount of 1.0% by mass or more, thereby enabling practical use of the polishing process of the silicon nitride film.
  • Patent Document 1 enables practical use of such a polishing process in which a silicon oxide film and a silicon nitride film are polished at a practical polishing rate and a polysilicon film is used as a stopper film. It is not a thing.
  • the technique disclosed in Patent Document 1 cannot be applied to a polishing process in which two types of films, a silicon oxide film and a silicon nitride film, are selectively polished with respect to a polysilicon film.
  • the present invention can improve the polishing rate of the silicon oxide film and the silicon nitride film relative to the polishing rate of the polysilicon film, and polish the silicon oxide film and the silicon nitride film by using the polysilicon film as a stopper film.
  • the present invention provides a CMP polishing liquid that can be applied to a process, a method for polishing a substrate using the CMP polishing liquid, and an electronic component that includes the substrate polished by the polishing method.
  • the present invention is a CMP polishing liquid used by mixing a first liquid and a second liquid, and the first liquid contains cerium-based abrasive grains, a dispersant, and water.
  • the second liquid contains a polyacrylic acid compound, a surfactant, a pH adjuster, at least one phosphoric acid compound of phosphoric acid or a phosphoric acid derivative, and water, and the pH of the second liquid is
  • the first liquid and the second liquid are mixed so that the phosphoric acid compound content is 0.01 to 1.0% by mass based on the total mass of the CMP polishing liquid.
  • a CMP polishing liquid is provided.
  • Such a CMP polishing liquid of the present invention can improve the polishing rate of the silicon oxide film and the silicon nitride film with respect to the polishing rate of the polysilicon film, and the silicon oxide film using the polysilicon film as a stopper film,
  • the present invention can be applied to a polishing process for polishing a silicon nitride film.
  • the second liquid can contain a basic compound having a pKa of 8 or more as a pH adjuster.
  • the second liquid preferably contains a nonionic surfactant as a surfactant.
  • the polishing rate of the silicon oxide film and the silicon nitride film can be further improved with respect to the polishing rate of the polysilicon film.
  • the pH of the first liquid is preferably 7.0 or higher.
  • the first liquid preferably contains cerium oxide particles as cerium-based abrasive grains. More preferably, the first liquid contains cerium oxide particles as cerium-based abrasive grains, and the average particle diameter of the cerium-based abrasive grains is 0.01 to 2.0 ⁇ m.
  • the first liquid contains a polyacrylic acid type dispersant as a dispersant.
  • the polishing rate of the silicon oxide film and the silicon nitride film can be further improved with respect to the polishing rate of the polysilicon film.
  • the present invention also includes a cerium-based abrasive, a dispersant, a polyacrylic acid compound, a surfactant, a pH adjuster, at least one phosphoric acid compound of phosphoric acid or a phosphoric acid derivative, and water.
  • a CMP polishing liquid is provided, wherein the content of the phosphoric acid compound is 0.01 to 1.0% by mass based on the total mass of the CMP polishing liquid.
  • Such a CMP polishing liquid of the present invention can improve the polishing rate of the silicon oxide film and the silicon nitride film with respect to the polishing rate of the polysilicon film, and the silicon oxide film using the polysilicon film as a stopper film,
  • the present invention can be applied to a polishing process for polishing a silicon nitride film.
  • the CMP polishing liquid of the present invention can contain a basic compound having a pKa of 8 or more as a pH adjuster.
  • the CMP polishing liquid of the present invention preferably contains a nonionic surfactant as a surfactant.
  • the polishing rate of the silicon oxide film and the silicon nitride film can be further improved with respect to the polishing rate of the polysilicon film.
  • the CMP polishing liquid of the present invention preferably contains cerium oxide particles as cerium-based abrasive grains.
  • the CMP polishing liquid of the present invention preferably contains cerium oxide particles as cerium-based abrasive grains, and the average particle diameter of the cerium-based abrasive grains is preferably 0.01 to 2.0 ⁇ m.
  • the CMP polishing liquid of the present invention preferably contains a polyacrylic acid dispersant as a dispersant.
  • the polishing rate of the silicon oxide film and the silicon nitride film can be further improved with respect to the polishing rate of the polysilicon film.
  • the CMP polishing liquid is applied between the film to be polished and the polishing cloth in a state where the film to be polished on the substrate having the film to be polished on at least one surface is pressed against the polishing cloth of the polishing surface plate.
  • a substrate polishing method comprising a polishing step of polishing a film to be polished by relatively moving a substrate and a polishing surface plate while supplying.
  • the present invention provides a first liquid containing cerium-based abrasive grains, a dispersant and water, and at least one phosphoric acid compound of a polyacrylic acid compound, a surfactant, a pH adjuster, phosphoric acid or a phosphoric acid derivative.
  • a second liquid containing water and having a pH of 6.5 or higher, and the phosphoric acid compound content is 0.01 to 1.0 mass% based on the total mass of the CMP polishing liquid. Polishing of the substrate, comprising: a polishing liquid preparation step for obtaining a CMP polishing liquid; and a polishing step for polishing the polishing target film of the substrate having the polishing target film formed on at least one surface using the CMP polishing liquid.
  • a method comprising: a polishing liquid preparation step for obtaining a CMP polishing liquid; and a polishing step for polishing the polishing target film of the substrate having the polishing target film formed on at least one surface using the CMP polishing liquid.
  • the substrate polishing method of the present invention can improve the polishing rate of the silicon oxide film and the silicon nitride film with respect to the polishing rate of the polysilicon film.
  • the silicon oxide film and the silicon nitride are formed using the polysilicon film as a stopper film.
  • the present invention can be applied to a polishing process for polishing a film.
  • the pH of the first liquid is preferably 7.0 or more.
  • the one surface of the substrate may have a step.
  • a polysilicon film is formed between the substrate and the film to be polished, and in the polishing step, the film to be polished may be polished using the polysilicon film as a stopper film.
  • at least one of a silicon oxide film and a silicon nitride film may be formed on the substrate as a film to be polished.
  • the present invention provides an electronic component comprising a substrate polished by the substrate polishing method.
  • Such an electronic component according to the present invention has an excellent substrate corresponding to fine processing by providing a substrate capable of improving the polishing rate of the silicon oxide film and the silicon nitride film with respect to the polishing rate of the polysilicon film. Have good quality.
  • the CMP polishing liquid and the substrate polishing method using the CMP polishing liquid of the present invention can polish the silicon oxide film and the silicon nitride film at a sufficiently practical speed while suppressing the polishing speed of the polysilicon film. It can be applied to a polishing process in which a silicon oxide film and a silicon nitride film are polished using a polysilicon film as a stopper film. Further, an electronic component including a substrate polished by the polishing method of the present invention has excellent quality corresponding to processing miniaturization.
  • the CMP polishing liquid of this embodiment contains cerium-based abrasive grains, a dispersant, a polyacrylic acid compound, a surfactant, a pH adjuster, phosphoric acid or at least one phosphoric acid derivative, and water. .
  • the CMP polishing liquid of this embodiment can be obtained by mixing a slurry (first liquid) and an additive liquid (second liquid).
  • the slurry contains cerium-based abrasive grains, a dispersant, and water.
  • cerium-based abrasive particles are preferably dispersed in water with a dispersant.
  • Cerium-based abrasive grains are defined as abrasive grains containing cerium as a constituent element.
  • the CMP polishing liquid of this embodiment is cerium oxide, cerium hydroxide, ammonium cerium nitrate, cerium acetate, cerium sulfate hydrate, cerium bromate, cerium bromide, cerium chloride, cerium oxalate, cerium nitrate.
  • the method for producing the cerium oxide particles is not particularly limited, and for example, an oxidation method using baking or hydrogen peroxide can be used.
  • the cerium oxide particles can be obtained, for example, by oxidizing a cerium compound such as carbonate, nitrate, sulfate, or oxalate.
  • the firing temperature is preferably 350 to 900 ° C.
  • the cerium-based abrasive preferably contains a polycrystalline cerium-based abrasive having a grain boundary. Since such polycrystalline cerium-based abrasive grains become fine during polishing and active surfaces appear one after another, a high polishing rate for a silicon oxide film can be maintained at a high level.
  • the crystallite diameter of the cerium-based abrasive is preferably 1 to 400 nm.
  • the crystallite diameter can be measured by a TEM photograph image or an SEM image.
  • a cerium oxide slurry (hereinafter also simply referred to as “slurry”) used for polishing a silicon oxide film formed by TEOS-CVD or the like, the crystallite diameter of the cerium oxide particles is larger and the crystal distortion is smaller. The better the crystallinity, the faster the polishing is possible.
  • the crystallite size is the size of a single crystal of a cerium-based abrasive grain, and in the case of a polycrystal having a crystal grain boundary, it means the size of a single particle constituting the polycrystal. .
  • the cerium-based abrasive is agglomerated, it is preferably mechanically pulverized.
  • 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, those described in “Chemical Engineering Papers”, Vol. 6, No. 5, (1980), pages 527 to 532 can be used.
  • Such a cerium-based abrasive is dispersed in water as a dispersion medium to obtain a slurry.
  • a dispersion method for example, a homogenizer, an ultrasonic disperser, a wet ball mill, or the like can be used in addition to a dispersion treatment using a normal stirrer, using a dispersant described later.
  • a sedimentation classification method is used by forcibly sedimenting the slurry after centrifugation with a small centrifuge and taking out only the supernatant liquid.
  • a high-pressure homogenizer that collides cerium-based abrasive grains in the dispersion medium with each other at high pressure may be used as a method for forming fine particles.
  • the average particle size of the cerium-based abrasive grains in the slurry is preferably 0.01 to 2.0 ⁇ m, more preferably 0.08 to 0.5 ⁇ m, and still more preferably 0.08 to 0.4 ⁇ m. Further, it is preferable that the CMP polishing liquid of this embodiment contains cerium oxide particles, and the average particle diameter of the cerium-based abrasive grains is 0.01 to 2.0 ⁇ m. When the average particle size is 0.01 ⁇ m or more, the polishing rate of the silicon oxide film and the silicon nitride film can be further improved. When the average particle size is 2.0 ⁇ m or less, it is possible to suppress the polishing film from being scratched.
  • the average particle diameter of cerium-based abrasive grains refers to the median diameter of volume distribution measured with a laser diffraction particle size distribution meter. Specifically, such an average particle size can be obtained by using LA-920 (trade name) manufactured by Horiba, Ltd. First, a sample containing cerium-based abrasives (which may be a slurry or a CMP polishing liquid) is diluted or concentrated so that the measurement transmittance (H) with respect to a He—Ne laser is 60 to 70%, and then a measurement sample. Get. Then, the measurement sample is put into LA-920 and measured, and the obtained arithmetic average diameter (mean size) is obtained.
  • LA-920 trade name
  • the content of the cerium-based abrasive is preferably 0.2 to 3.0 mass%, more preferably 0.3 to 2.0 mass%, and more preferably 0.5 to 1.5 mass% based on the total mass of the CMP polishing liquid. % Is more preferable.
  • the content of the cerium-based abrasive is 3.0% by mass or less, the effect of adjusting the polishing rate by the additive liquid is further improved. Further, when the content of the cerium-based abrasive is 0.2% by mass or more, the polishing rate of the silicon oxide film is further improved, and a desired polishing rate can be easily obtained.
  • the dispersant used in the CMP polishing liquid of this embodiment is not limited as long as it is a compound that can be dissolved in water and can disperse the cerium-based abrasive grains.
  • a compound having a solubility in water of 0.1 to 99.9% by mass is generally preferable.
  • a water-soluble anionic dispersant, a water-soluble nonionic dispersant, Examples thereof include a cationic dispersant and a water-soluble amphoteric dispersant, and a polycarboxylic acid type polymer dispersant described later is preferable.
  • water-soluble anionic dispersant examples include lauryl sulfate triethanolamine, ammonium lauryl sulfate, polyoxyethylene alkyl ether sulfate triethanolamine, and polycarboxylic acid type polymer dispersants.
  • polycarboxylic acid type polymer dispersant examples include polymers of carboxylic acid monomers having an unsaturated double bond such as acrylic acid, methacrylic acid, maleic acid, fumaric acid, and itaconic acid, and unsaturated dicarboxylic acids. Examples thereof include a copolymer of a carboxylic acid monomer having a heavy bond and another monomer having an unsaturated double bond, and an ammonium salt or an amine salt thereof.
  • the polycarboxylic acid type polymer dispersant is preferably a polyacrylic acid type dispersant, and more preferably a polymer dispersant having an ammonium acrylate salt as a constituent unit as a copolymerization component.
  • the polymer dispersing agent having an acrylic acid ammonium salt as a structural unit as the copolymer component described above for example, a polyacrylic acid ammonium salt, an ammonium salt of a copolymer of alkyl acrylate and acrylic acid, or the like is preferably used. it can. Further, it may be used as two or more kinds of dispersants including at least one kind of polymer dispersant having an acrylic acid ammonium salt as a structural unit as a copolymer component and at least one kind selected from other dispersants. it can.
  • the weight average molecular weight of the polycarboxylic acid type polymer dispersant is preferably 100,000 or less.
  • a weight average molecular weight can be measured using GPC on the following conditions, for example.
  • Sample 10 ⁇ L Standard polystyrene: Standard polystyrene manufactured by Tosoh Corporation (molecular weight: 190000, 17900, 9100, 2980, 578, 474, 370, 266)
  • Detector manufactured by Hitachi, Ltd., RI-monitor, product name “L-3000” Integrator: Hitachi, Ltd., GPC integrator, product name “D-2200”
  • Pump Hitachi, Ltd., trade name “L-6000”
  • Degassing device Showa Denko Co., Ltd., trade name "Shodex DEGAS” Column: manufactured by Hitachi Chemical Co., Ltd., trade names “GL-R440”, “GL-R430”, “GL-R420” are used in this order and are used
  • Eluent Tetrahydrofuran
  • water-soluble nonionic dispersant examples include polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether, polyoxyethylene higher alcohol ether, polyoxyethylene octylphenyl.
  • Ether polyoxyethylene nonylphenyl ether, polyoxyalkylene alkyl ether, polyoxyethylene derivative, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan tristearate Rate, polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan trioleate, tetraoleate Polyoxyethylene sorbate, polyethylene glycol monolaurate, polyethylene glycol monostearate, polyethylene glycol distearate, polyethylene glycol monooleate, polyoxyethylene alkylamine, polyoxyethylene hydrogenated castor oil, 2-hydroxyethyl methacrylate, And alkyl alkanolamides.
  • water-soluble cationic dispersant examples include polyvinyl pyrrolidone, coconut amine acetate, stearyl amine acetate and the like.
  • water-soluble amphoteric dispersant examples include lauryl betaine, stearyl betaine, lauryl dimethylamine oxide, 2-alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine and the like.
  • the various dispersants described above can be used alone or in combination of two or more.
  • the CMP polishing liquid obtained by mixing the slurry and the additive liquid can use the same material as the polyacrylic acid compound and surfactant described later as the dispersant.
  • the CMP polishing liquid obtained by mixing the slurry and the additive liquid contains a substance derived from the slurry and a substance derived from the additive liquid.
  • the content of the dispersant in the slurry is 1.0 to 5.0% by mass on the basis of the total mass of the abrasive grains in the slurry in that the abrasive grains can be sufficiently dispersed and aggregation and sedimentation can be suppressed during storage. Is preferable, and 1.0 to 4.0% by mass is more preferable.
  • the content of impurity ions (alkali metals such as sodium ions and potassium ions, halogen atoms and sulfur atoms) in the total dispersant, It is preferable to keep the mass ratio to 10 ppm or less based on the entire CMP polishing liquid.
  • the pH of the slurry is preferably 7.0 or more, more preferably 7.0 to 12.0, and even more preferably 7.0 to 11.0.
  • the pH is 7.0 or more, aggregation of particles can be suppressed.
  • the pH is 12.0 or less, good flatness can be obtained.
  • the water used as a medium for diluting the slurry, additive liquid or concentrated liquid is not particularly limited, but deionized water and ultrapure water are preferable.
  • the content of water is not particularly limited, and may be the remainder of the content of other components.
  • the additive liquid contains a polyacrylic acid compound, a surfactant, a pH adjusting agent, at least one phosphoric acid compound of phosphoric acid or a phosphoric acid derivative, and water.
  • the additive solution contains a polyacrylic acid compound as one component of the additive solution component.
  • the polyacrylic acid compound include polyacrylic acid formed from a polymer of acrylic acid alone and a copolymer of acrylic acid and a water-soluble alkyl acrylate.
  • the polyacrylic acid compound include polyacrylic acid, a copolymer of acrylic acid and methyl acrylate, a copolymer of acrylic acid and methacrylic acid, and a copolymer of acrylic acid and ethyl acrylate. Among them, it is preferable to use polyacrylic acid. These can be used alone or in combination of two or more.
  • the weight average molecular weight of the polyacrylic acid compound is preferably 500000 or less, and more preferably 50000 or less. When the weight average molecular weight is 500,000 or less, for example, when polyacrylic acid is used, the polyacrylic acid is easily adsorbed uniformly on the film to be polished.
  • the weight average molecular weight can be measured using GPC under the same conditions as for the polycarboxylic acid type polymer dispersant.
  • the content of the polyacrylic acid compound is preferably 0.05 to 2.0% by mass, more preferably 0.08 to 1.8% by mass, based on the total mass of the CMP polishing liquid, and 0.10 to 1.5%. More preferred is mass%.
  • the polishing rate of the silicon oxide film can be further improved. Flatness can be improved as content of a polyacrylic acid compound is 0.05 mass% or more.
  • the additive liquid contains a surfactant as one component of the additive liquid component.
  • the surfactant include an anionic surfactant, a nonionic surfactant, a cationic surfactant, and a zwitterionic surfactant. These can be used alone or in combination of two or more. Among the above surfactants, nonionic surfactants are particularly preferable.
  • nonionic surfactant examples include polyoxypropylene, polyoxyethylene alkyl ether, polyoxyethylene alkyl ether, polyoxyethylene alkyl allyl ether, polyoxyethylene polyoxypropylene ether derivatives, and polyoxypropylene glyceryl ether.
  • Ether type surfactants such as polyethylene glycol, methoxypolyethylene glycol, oxyethylene adducts of acetylenic diol, ester type surfactants such as sorbitan fatty acid ester and glycerol borate fatty acid ester, amino ethers such as polyoxyethylene alkylamine Type surfactant, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerol borate fatty acid ester, polyoxyethylene Ether ester type surfactants such as alkyl esters, fatty acid alkanolamides, alkanolamide type surfactants such as polyoxyethylene fatty acid alkanolamides, oxyethylene adducts of acetylenic diols, polyvinylpyrrolidone, polyacrylamide, polydimethylacrylamide, etc. Can be mentioned.
  • the content of the surfactant is preferably 0.01 to 1.0% by mass, more preferably 0.02 to 0.7% by mass, and 0.03 to 0.5% by mass based on the total mass of the CMP polishing liquid. % Is more preferable.
  • the surfactant content is 1.0% by mass or less, the polishing rate of the silicon oxide film is further improved.
  • the surfactant content is 0.01% by mass or more, an increase in the polishing rate of the polysilicon film can be further suppressed.
  • the pH of the additive solution needs to be 6.5 or more, preferably 6.7 to 12.0, and more preferably 6.8 to 11.0.
  • the pH is 6.5 or more, it is possible to suppress aggregation of particles contained in the slurry when the additive solution and the slurry are mixed.
  • the pH is 12.0 or less, good flatness can be obtained when the additive solution and the slurry are mixed.
  • the pH of the additive solution can be measured with a pH meter using a general glass electrode.
  • trade name: Model (F-51) manufactured by HORIBA, Ltd. can be used for measuring pH.
  • the pH of the additive solution is as follows: phthalate pH standard solution (pH: 4.01), neutral phosphate pH standard solution (pH: 6.86), and borate pH standard solution (pH: 9.18).
  • the pH meter is calibrated at three points, the electrode of the pH meter is placed in the additive solution, and the value after 2 minutes has elapsed and stabilized is measured.
  • the liquid temperature of the standard buffer solution and the additive solution can be both 25 ° C., for example.
  • the pH of the slurry can be measured by the same method.
  • the CMP polishing liquid of this embodiment contains a pH adjuster as one component of the additive liquid component.
  • the pH adjuster include water-soluble basic compounds and water-soluble acid compounds.
  • the basic compound include basic compounds having a pKa of 8 or more.
  • pKa means the acid dissociation constant of the first dissociable acidic group, and is the negative common logarithm of the equilibrium constant Ka of the group.
  • water-soluble organic amines, aqueous ammonia and the like are preferably used.
  • pH of an additive liquid can also be adjusted with other containing components, such as the said polyacrylic acid compound.
  • water-soluble organic amines examples include ethylamine, diethylamine, triethylamine, diphenylguanidine, piperidine, butylamine, dibutylamine, isopropylamine, tetramethylammonium oxide, tetramethylammonium chloride, tetramethylammonium bromide, and tetramethylammonium fluoride.
  • Tetrabutylammonium hydroxide Tetrabutylammonium chloride, tetrabutylammonium bromide, tetrabutylammonium fluoride, tetramethylammonium nitrate, tetramethylammonium acetate, tetramethylammonium propionate, tetramethylammonium maleate, tetramethyl Examples thereof include ammonium sulfate.
  • the content of the pH adjuster is preferably 0.01 to 10.0% by mass, more preferably 0.05 to 5.0% by mass based on the total mass of the CMP polishing liquid, More preferably, the content is 1 to 3.0% by mass.
  • the content of the pH adjuster is restricted by the pH to be adjusted, it is determined by the content of other components (strong acid, polyacrylic acid compound, etc.) and there is no particular limitation.
  • the additive liquid contains at least one phosphoric acid compound of phosphoric acid or a phosphoric acid derivative as one component of the additive liquid component.
  • the “phosphoric acid compound” includes phosphoric acid and phosphoric acid derivatives.
  • the phosphoric acid derivative include a polymer of phosphoric acid such as dimer and trimer (for example, pyrophosphoric acid, pyrophosphorous acid, and trimetaphosphoric acid), and a compound containing a phosphoric acid group (for example, sodium hydrogen phosphate, Sodium phosphate, ammonium phosphate, potassium phosphate, calcium phosphate, sodium pyrophosphate, polyphosphoric acid, sodium polyphosphate, metaphosphoric acid, sodium metaphosphate, ammonium phosphate, etc.).
  • dimer and trimer for example, pyrophosphoric acid, pyrophosphorous acid, and trimetaphosphoric acid
  • a compound containing a phosphoric acid group for example, sodium hydrogen phosphate, Sodium phosphate, ammoni
  • the content of the phosphoric acid compound is 0.01 to 1.0% by mass based on the total mass of the CMP polishing liquid, preferably 0.02 to 0.7% by mass, and 0.03 to 0.5% by mass. More preferred.
  • the polishing rate of the silicon nitride film can be further improved.
  • the content of the phosphoric acid compound is 0.01% by mass or more, the polishing rate of the silicon nitride film can be further improved.
  • the CMP polishing liquid of this embodiment is preferably stored as, for example, a two-part polishing liquid divided into a slurry in which cerium-based abrasive grains are dispersed in water with a dispersant and an additive liquid.
  • the slurry and additive are not mixed and stored as a two-component polishing liquid, the cerium-based abrasive grains can be prevented from agglomerating, and the effect of suppressing polishing flaws and the fluctuation of the polishing rate can be suppressed.
  • the slurry and the additive solution may be mixed in advance or may be mixed immediately before use.
  • B method of mixing the slurry and additive liquid immediately before polishing C method of supplying the slurry and additive separately on the polishing surface plate and mixing both liquids on the polishing surface plate, and adding the slurry and the material in advance
  • the D method etc. which supply what mixed the liquid with supply piping can be used. By arbitrarily changing the blend of these two liquids, it is possible to adjust the planarization characteristics and the polishing rate.
  • the mixing ratio of the slurry and the additive liquid is preferably about 1:10 to 10: 1 (slurry: additive liquid) in mass ratio.
  • the slurry or additive solution may be preliminarily concentrated in a reduced amount of water, and may be diluted with deionized water during mixing as necessary.
  • the substrate polishing method of this embodiment is a method for polishing the above-described CMP polishing liquid in a state where the polishing target film of a substrate having a polishing target film formed on at least one surface is pressed against a polishing cloth of a polishing surface plate.
  • a polishing step of polishing the film to be polished by relatively moving the substrate and the polishing surface plate while supplying the film between the film and the polishing cloth is provided.
  • the substrate polishing method of the present embodiment includes a polishing liquid preparation step of mixing the slurry and the additive liquid to obtain the CMP polishing liquid described above, and at least one surface using the obtained CMP polishing liquid.
  • the substrate polishing method of the present embodiment is particularly suitable for a polishing step of polishing the one surface of the substrate to flatten the step when the one surface on which the film to be polished of the substrate is formed has a step. is there.
  • the film to be polished when a polysilicon film is formed between the substrate and the film to be polished, the film to be polished can be polished using the polysilicon film as a stopper film in the polishing step.
  • the film to be polished after forming a stopper film along the separation groove on the substrate on which the separation groove is formed, forming the film to be polished on the stopper film, the film to be polished can be removed until the stopper film is exposed. .
  • a substrate 100 shown in FIG. 1A has shallow trench isolation (STI) formed by embedding an insulator 2 such as silicon dioxide in a groove formed in silicon 1.
  • An insulating film (High-k insulating film) 3 having high conductivity is laminated on the silicon 1.
  • a dummy gate 4 made of a polysilicon film is formed at a predetermined position on the insulating film 3, and a side wall 5 made of a silicon nitride film is formed on the side of the dummy gate 4.
  • a stress liner 6 of a silicon nitride film is laminated so as to cover the surface, and finally a silicon oxide film 7 is laminated.
  • the silicon oxide film 7 and a part of the silicon nitride stress liner 6 on such a substrate are polished by using the CMP polishing liquid according to the present embodiment until the polysilicon dummy gate 4 is exposed.
  • a substrate 200 having a structure as shown in FIG. 1B can be obtained.
  • the polysilicon film as the dummy gate 4 functions as a stopper film for suppressing excessive polishing.
  • polishing method will be further described by taking as an example a semiconductor substrate on which at least one of a silicon oxide film and a silicon nitride film is formed as a film to be polished.
  • a polishing apparatus used in the polishing method of the present embodiment for example, a holder for holding a substrate having a film to be polished and a motor or the like capable of attaching a polishing cloth (pad) and capable of changing the number of rotations are attached.
  • a general polishing apparatus or the like having a certain polishing surface plate can be used.
  • polishing apparatus examples include a polishing apparatus manufactured by Ebara Manufacturing Co., Ltd., model number: EPO-111, polishing apparatus manufactured by AMAT (Applied Materials), trade name: Mira3400, Reflection polishing machine, and the like.
  • polishing cloth For example, a general nonwoven fabric, a polyurethane foam, a porous fluororesin, etc. can be used. Moreover, it is preferable that the polishing cloth is subjected to groove processing so that a polishing liquid is accumulated.
  • the polishing conditions are not particularly limited, but from the viewpoint of suppressing the semiconductor substrate from popping out, the rotation speed of the polishing platen is preferably a low rotation of 200 rpm or less.
  • the pressure applied to the semiconductor substrate (processing load) is preferably 100 kPa or less from the viewpoint of suppressing the generation of scratches after polishing.
  • polishing it is preferable to continuously supply the polishing liquid to the surface of the polishing cloth with a pump or the like. Although there is no restriction
  • the supply method of the polishing liquid is the A method in which the two liquids are fed through separate pipes, these pipes are joined, mixed immediately before the supply pipe outlet, and supplied onto the polishing platen.
  • B method for mixing the liquid just before polishing C method for supplying the two liquids separately onto the polishing platen, and D method for supplying a mixture of slurry and additive liquid in advance through a supply pipe .
  • the semiconductor substrate after polishing is preferably washed in running water and then dried after removing water droplets adhering to the semiconductor substrate using a spin dryer or the like.
  • polishing the inorganic insulating layer, which is a film to be polished, with the above polishing liquid surface irregularities can be eliminated and a smooth surface can be obtained over the entire surface of the semiconductor substrate.
  • a semiconductor substrate having a desired number of layers can be manufactured.
  • Examples of a method for manufacturing a silicon oxide film and a silicon nitride film that are films to be polished include a low-pressure CVD method, a plasma CVD method, and the like.
  • a silicon oxide film is formed by a low pressure CVD method, monosilane: SiH 4 can be used as the Si source, and oxygen: O 2 can be used as the oxygen source.
  • the silicon oxide film can be obtained by performing this SiH 4 —O 2 oxidation reaction at a low temperature of 400 ° C. or lower.
  • the silicon oxide film may be heat-treated at a temperature of 1000 ° C. or lower after the film is formed by the CVD method.
  • the silicon oxide film may be doped with an element such as phosphorus or boron.
  • an element such as phosphorus or boron.
  • P doping silicon
  • P phosphorus
  • the plasma CVD method has an advantage that a chemical reaction that requires a high temperature can be performed at a low temperature under normal thermal equilibrium.
  • As reaction gases SiH 4 -N 2 O gas using SiH 4 as Si source and N 2 O as oxygen source, and TEOS-O 2 gas (TEOS) using tetraethoxysilane (TEOS) as Si source are used.
  • TEOS-O 2 gas TEOS-O 2 gas
  • TEOS tetraethoxysilane
  • a silicon nitride film is formed by a low pressure CVD method
  • dichlorosilane: SiH 2 Cl 2 can be used as the Si source
  • ammonia: NH 3 can be used as the nitrogen source.
  • the silicon nitride film can be obtained by performing a SiH 2 Cl 2 —NH 3 based oxidation reaction at a high temperature of 900 ° C.
  • Examples of the reactive gas in the plasma CVD method include SiH 4 —NH 3 gas using SiH 4 as a Si source and NH 3 as a nitrogen source.
  • the substrate temperature is preferably 300 to 400 ° C.
  • the substrate used in this embodiment includes individual semiconductors such as diodes, transistors, compound semiconductors, thermistors, varistors, thyristors, DRAMs (dynamic random access memories), SRAMs (static random access memories), EPROM (Eraseable Programmable Read Only Memory), Mask ROM (Mask Read Only Memory), EEPROM (Electrically Erasable Programmable Read Only Memory), Flash Memory and other Memory Elements, Microprocessor, Theoretical circuit elements such as DSP and ASIC, integrated circuit elements such as compound semiconductors represented by MMIC (monolithic microwave integrated circuit), hybrid integrated circuits (hybrid IC), Photodiode, and a substrate having a photoelectric conversion element such as a charge coupled device.
  • individual semiconductors such as diodes, transistors, compound semiconductors, thermistors, varistors, thyristors, DRAMs (dynamic random access memories), SRAMs (static random access memories), EPROM (Eraseable Programmable Read Only Memory), Mask ROM (Mask
  • the CMP polishing liquid of the present embodiment is not only a silicon nitride film and a silicon oxide film formed on a semiconductor substrate, but also an inorganic insulating film such as a silicon oxide film, glass, and silicon nitride formed on a wiring board having a predetermined wiring.
  • a film mainly containing polysilicon, Al, Cu, Ti, TiN, W, Ta, TaN or the like can be polished.
  • the electronic component of this embodiment uses a substrate polished by the above-described polishing method.
  • Electronic components include not only semiconductor elements but also optical glasses such as photomasks, lenses, and prisms, inorganic conductive films such as ITO, optical integrated circuits, optical switching elements, optical waveguides, and optical fibers composed of glass and crystalline materials. It includes end faces, optical single crystals such as scintillators, solid state laser single crystals, blue laser LED sapphire substrates, semiconductor single crystals such as SiC, GaP, and GaAs, glass substrates for magnetic disks, magnetic heads, and the like.
  • Cerium carbonate hydrate 40 kg was put in an alumina container and calcined in air at 830 ° C. for 2 hours to obtain 20 kg of yellowish white powder. When this powder was phase-identified by X-ray diffraction, it was confirmed to be cerium oxide. Further, as a result of measuring the particle size of the fired powder with a laser diffraction particle size distribution meter, 95% or more of the particle size of the fired powder was distributed between 1 and 100 ⁇ m.
  • Cerium oxide powder 10.0 kg and deionized water: 116.65 kg are mixed, and a commercially available ammonium polyacrylate aqueous solution (weight average molecular weight: 8000, 40% by mass): 228 g is added as a dispersant, and cerium oxide dispersion is added.
  • a commercially available ammonium polyacrylate aqueous solution weight average molecular weight: 8000, 40% by mass
  • cerium oxide dispersion is added.
  • ultrasonic irradiation was performed in the pipe for feeding the liquid while feeding it to another container.
  • the ultrasonic frequency was 400 kHz, and the cerium oxide dispersion was fed over 30 minutes.
  • cerium oxide dispersion (cerium oxide slurry) was measured and found to be 4.0% by mass.
  • the pH of this slurry was measured and found to be 9.0.
  • the average particle diameter of cerium oxide particles in the slurry was measured with a refractive index of 1.93 and a transmittance of 68%. As a result, it was 0.11 ⁇ m.
  • Impurity ions Na, K, Fe, Al, Zr, Cu, Si, Ti
  • the mass ratio was 1 ppm or less.
  • the additive solution was prepared by the following steps. Ultrapure water: 900 g is weighed into a 1000 mL container a. A 40 mass% polyacrylic acid aqueous solution (weight average molecular weight: 3000): 10.0 g is put in a container a. Surfactant: Polyethoxylate of 2,4,7,9-tetramethyl-5-decyne-4,7-diol: 15.0 g is placed in a container a. Phosphoric acid: 85 mass% phosphoric acid aqueous solution is put into the container a so that it may become 8.5g.
  • the amount of addition is adjusted so that the pH of the additive solution is 7.0, and ammonia water (25% by mass aqueous solution) is placed in the container a.
  • An appropriate amount of ultrapure water was added so that the total amount was 1000 g to prepare an additive solution.
  • Example 2 to 11> In the same manner as in Example 1, an additive solution was prepared by blending as shown in Table 1.
  • a blanket wafer without a pattern is formed as a silicon oxide film having a film thickness of 1000 nm on a Si substrate and a film having a film thickness of 200 nm on a Si substrate.
  • a silicon nitride film and a polysilicon film formed with a thickness of 100 nm on a Si substrate were used.
  • the pattern wafer includes a silicon substrate 8 having a trench on the surface, a silicon nitride film 9 stacked on the silicon substrate 8 so as to avoid the trench, and a silicon substrate 8 and And a silicon oxide (SiO 2 ) film (insulating film) 10 laminated on the silicon nitride film 9.
  • the silicon oxide film 10 is formed by HDP (High Density Plasma) method, and the film thickness is 600 nm on both the silicon substrate 8 and the silicon nitride film 9.
  • the film thickness of the silicon nitride film 9 is 150 nm
  • the film thickness of the convex part of the silicon oxide film 10 is 600 nm
  • the film thickness of the concave part of the silicon oxide film 10 is 600 nm
  • the silicon oxide film 10 The recess depth is 500 nm (trench depth 350 nm + silicon nitride film thickness 150 nm).
  • the wafer was polished using a known CMP polishing liquid capable of sufficiently selectively polishing the silicon oxide film with respect to the silicon nitride film, and the silicon nitride film was exposed ( Pattern wafer A).
  • a wafer having a structure similar to that of the pattern wafer A and having a polysilicon film thickness of 150 nm was used instead of the silicon nitride film (pattern wafer B).
  • a line (convex portion) & space (concave portion) width of 200 ⁇ m pitch and a convex pattern density of 50% were used.
  • the line & space is a simulated pattern in which an active portion masked with Si 3 N 4 that is a convex portion and a trench portion that is formed with a groove that is a concave portion are alternately arranged.
  • the line and space has a pitch of 100 ⁇ m means that the total width of the line portion and the space portion is 100 ⁇ m.
  • the convex pattern density is 10%
  • the convex pattern density of 90% A width: 90 ⁇ m and a recess width: 10 ⁇ m mean a pattern in which the rows are arranged alternately.
  • test wafer was set in a holder to which a suction pad for mounting a substrate was attached in a polishing apparatus (Applied Materials, trade name: MIRRA 3400). Further, a polishing pad made of porous urethane resin (Rodel, model number: IC-1010) was attached to a polishing plate for 200 mm wafer.
  • a polishing pad made of porous urethane resin Rodel, model number: IC-1010
  • a holder with the insulating film face down was placed on the polishing pad, and the membrane pressure was set to 31 kPa.
  • cerium oxide slurry was simultaneously dropped onto the polishing platen at a rate of 160 mL / min, and the additive solutions of Examples 1 to 11 and Comparative Examples 1 to 7 were simultaneously dropped at a rate of 40 mL / min.
  • the wafer were operated at 123 rpm and 113 rpm, respectively, and the blanket wafer of silicon oxide film (P-TEOS film), silicon nitride film, and polysilicon film was polished for 1 minute.
  • the pattern wafers A and B were polished for 100 seconds. The polished wafer was thoroughly washed with pure water and then dried.
  • an optical interference type film thickness apparatus manufactured by Dainippon Screen Mfg. Co., Ltd., trade name: RE-3000. The residual film thickness at the point was measured, and the polishing rate per minute was calculated from the amount of film thickness reduction before polishing.
  • the pattern wafer the remaining film thickness of the silicon nitride film on the pattern wafer A and the recesses on the pattern wafer B using an optical interference film thickness device (Dainippon Screen Mfg.
  • the polishing rate ratio is that the silicon oxide film / polysilicon film is 64 to 110, the silicon nitride film / polysilicon film is 18 or more, and polysilicon. It can be seen that the polishing rate of the film is suppressed to 40 ⁇ / min or less, and the polishing rate of the silicon oxide film and the silicon nitride film is improved while suppressing the polishing rate of the polysilicon film.
  • Examples 1 to 11 are compared with Comparative Examples 1 to 7, it is clear that Examples 1 to 11 are particularly improved in the polishing rate of the silicon nitride film. Further, from the evaluation results on the pattern wafer A, it is clear that in Examples 1 to 11, the silicon nitride film was sufficiently polished. Further, from the evaluation results on the pattern wafer B, it can be seen that all of Examples 1 to 11 have a small flatness value and good flatness.

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