WO2013161701A1 - Procédé de fabrication d'une composition de polissage - Google Patents

Procédé de fabrication d'une composition de polissage Download PDF

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Publication number
WO2013161701A1
WO2013161701A1 PCT/JP2013/061621 JP2013061621W WO2013161701A1 WO 2013161701 A1 WO2013161701 A1 WO 2013161701A1 JP 2013061621 W JP2013061621 W JP 2013061621W WO 2013161701 A1 WO2013161701 A1 WO 2013161701A1
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Prior art keywords
polishing composition
polishing
water
silica particles
acid
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PCT/JP2013/061621
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English (en)
Japanese (ja)
Inventor
正利 戸松
修平 ▲高▼橋
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Fujimi Inc
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Fujimi Inc
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Priority to JP2014512521A priority Critical patent/JP6069308B2/ja
Publication of WO2013161701A1 publication Critical patent/WO2013161701A1/fr
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
    • H10P90/00—Preparation of wafers not covered by a single main group of this subclass, e.g. wafer reinforcement
    • H10P90/12—Preparing bulk and homogeneous wafers
    • H10P90/129—Preparing bulk and homogeneous wafers by polishing
    • 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

Definitions

  • the present invention relates to a method for producing a polishing composition that suppresses aggregation during the preparation of the polishing composition.
  • a polishing composition used for polishing a silicon substrate or a semiconductor wafer having a film such as a metal film and an oxide film on its surface contains silica particles as abrasive grains and a basic compound as an etching agent. It has been known.
  • Patent Document 1 an etching solution is prepared by adding hydroxyethyl cellulose as a water-soluble polymer to an aqueous solution containing a basic compound, and then silica diluted with pure water is added to the etching solution. It is disclosed that a polishing composition is prepared.
  • the method for producing a polishing composition disclosed in Patent Document 1 has a problem that aggregation (gelation) occurs during the preparation of the polishing composition.
  • the occurrence of this aggregation is considered to be caused by a decrease in the stability of components in the polishing composition. Suppressing the aggregation of the polishing composition is extremely important from the viewpoint of improving the stability of the polishing composition.
  • An object of the present invention is to provide a method for producing a polishing composition that can suppress aggregation during the preparation of the polishing composition.
  • the method for producing a polishing composition of the present invention comprises a step of preparing a mixture by mixing silica particles as abrasive grains, a basic compound, and water, And a step of adding an aqueous solution containing a functional polymer.
  • the aqueous solution is preferably basic.
  • the polishing composition is preferably used for polishing a silicon substrate.
  • the polishing composition is preferably used for final polishing of a silicon substrate.
  • aggregation of the polishing composition can be suppressed during preparation of the polishing composition.
  • the method for producing a polishing composition of the present embodiment includes a step of preparing a mixture by mixing silica particles as abrasive grains, a basic compound, and water, and adding an aqueous solution containing a water-soluble polymer to the mixture.
  • the polishing composition thus obtained is preferably used for polishing the surface of a silicon substrate.
  • the silicon substrate polishing step includes, for example, a preliminary polishing step (primary polishing and secondary polishing) for flattening the surface of a disk-shaped silicon substrate sliced from a silicon single crystal ingot, and a surface of the silicon substrate after the preliminary polishing step And a final polishing step of removing the fine irregularities present in the surface to make a mirror surface.
  • the polishing composition is particularly preferably used in the final polishing step.
  • a silicon substrate whose surface has been polished with a polishing composition can be suitably used for the production of a semiconductor substrate.
  • Silica particles function to mechanically polish the surface to be polished.
  • silica particles include colloidal silica, fumed silica, and sol-gel silica.
  • colloidal silica is preferable.
  • colloidal silica or fumed silica is used, particularly when colloidal silica is used, scratches generated on the polished surface of the silicon substrate are reduced.
  • These silica particles may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the average primary particle diameter of the silica particles is preferably 5 nm or more, more preferably 10 nm or more, and further preferably 20 nm or more. As the average primary particle diameter of the silica particles increases, the polishing rate of the silicon substrate improves.
  • the average primary particle diameter of the silica particles is preferably 100 nm or less, more preferably 70 nm or less, and even more preferably 50 nm or less. As the average primary particle diameter of the silica particles decreases, the dispersion stability of the polishing composition improves.
  • the value of the average primary particle diameter of the silica particles is calculated from, for example, the specific surface area measured by the BET method.
  • the specific surface area of the silica particles can be measured using, for example, “Flow SorbII 2300” manufactured by Micromeritex.
  • the average secondary particle diameter of the silica particles is preferably 10 nm or more, more preferably 20 nm or more, and further preferably 30 nm or more. As the average secondary particle diameter of the silica particles increases, a higher polishing rate is obtained when polishing.
  • the average secondary particle diameter of the silica particles is preferably 200 nm or less, more preferably 150 nm or less, and still more preferably 100 nm or less. As the average secondary particle diameter of the silica particles decreases, the dispersion stability of the polishing composition improves.
  • the average secondary particle diameter of the silica particles can be measured, for example, by a dynamic light scattering method using FPAR-1000 manufactured by Otsuka Electronics Co., Ltd.
  • the average value of the major axis / minor axis ratio of the silica particles is preferably 1.0 or more, more preferably 1.05 or more, and still more preferably 1.1 or more. As the average value of the major axis / minor axis ratio increases, a higher polishing rate is obtained.
  • the average value of the major axis / minor axis ratio of the silica particles is preferably 3.0 or less, more preferably 2.0 or less, and still more preferably 1.5 or less. As the average value of the major axis / minor axis ratio decreases, scratches generated on the polished surface decrease.
  • the major axis / minor axis ratio is a value relating to the shape of the silica particles, and can be determined using, for example, an electron microscope image of the silica particles. Specifically, in a scanning electron microscope image of a predetermined number (for example, 200) of silica particles, a minimum circumscribed rectangle is drawn for each particle. Next, for each minimum circumscribed rectangle, by calculating a value obtained by dividing the length of the long side (major axis value) by the length of the short side (minor axis value), and calculating the average value thereof The average value of the major axis / minor axis ratio can be determined.
  • the true specific gravity of the silica particles is preferably 1.5 or more, more preferably 1.6 or more, and even more preferably 1.7 or more. As the true specific gravity of the silica particles increases, a higher polishing rate is obtained.
  • the true specific gravity of the silica particles is preferably 2.2 or less. The true specific gravity is calculated from the mass of the dried silica particles and the total mass after the silica particles are immersed in ethanol with a known volume.
  • the content of silica particles in the mixture obtained by mixing silica particles, a basic compound, and water is preferably 1% by mass or more, more preferably 3% by mass or more, and further preferably 5% by mass or more. As the content of silica particles in the mixture increases, it becomes easier to increase the content of silica particles in the polishing composition.
  • the content of silica particles in the mixture is preferably 50% by mass or less, more preferably 40% by mass or less, and still more preferably 30% by mass or less. As the content of silica particles in the mixture decreases, aggregation during the preparation of the polishing composition is suppressed.
  • the content of silica particles in the finally obtained polishing composition is preferably 0.1% by mass or more, more preferably 0.2% by mass or more, and further preferably 0.3% by mass or more. is there. As the content of silica particles increases, surface processing performance such as polishing rate for the surface to be polished improves.
  • the content of silica particles in the polishing composition is preferably 10% by mass or less, more preferably 8% by mass or less, and further preferably 6% by mass or less. As the content of silica particles decreases, the dispersion stability of the polishing composition improves, and the silica particles remaining on the polished surface decrease.
  • the basic compound serves to chemically polish the surface to be polished, and improves the polishing rate.
  • the basic compound serves to improve the dispersion stability of the polishing composition.
  • Specific examples of basic compounds include alkali 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.
  • Specific examples of the quaternary ammonium include tetramethylammonium, tetraethylammonium, tetrabutylammonium and the like.
  • Specific examples of the alkali metal hydroxide or salt include potassium hydroxide, potassium carbonate, potassium hydrogen carbonate, potassium sulfate, potassium acetate, potassium chloride and the like.
  • 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 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 compound is at least one selected from ammonia, ammonium salt, alkali metal hydroxide, alkali metal salt, and quaternary ammonium hydroxide. More preferably, the basic compound is ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, tetraethylammonium hydroxide, ammonium bicarbonate, ammonium carbonate, potassium bicarbonate, potassium carbonate, sodium bicarbonate, and carbonate. It is at least one selected from sodium.
  • the basic compound is at least one selected from ammonia, potassium hydroxide, sodium hydroxide, tetramethylammonium hydroxide, and tetraethylammonium hydroxide, more preferably at least ammonia and tetramethylammonium hydroxide. On the other hand, most preferably ammonia.
  • the content of the basic compound in the mixture obtained by mixing the silica particles, the basic compound, and water is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, and further preferably 0.1% by mass. That's it. As the content of the basic compound in the mixture increases, aggregation during the preparation of the polishing composition is suppressed.
  • the content of the basic compound in the mixture is preferably 10% by mass or less, more preferably 5% by mass or less, and still more preferably 3% by mass or less. As the content of the basic compound in the mixture decreases, it becomes easier to reduce the content of the basic compound in the polishing composition.
  • the content of the basic compound in the polishing composition finally obtained is preferably 0.001% by mass or more, more preferably 0.002% by mass or more, and further preferably 0.003% by mass or more. It is. As the content of the basic compound in the polishing composition increases, the chemical polishing action on the surface to be polished increases, and the dispersion stability of the polishing composition improves.
  • the content of the basic compound in the polishing composition is preferably 1.0% by mass or less, more preferably 0.5% by mass or less, and still more preferably 0.2% by mass or less. As the content of the basic compound in the polishing composition decreases, the smoothness of the polished surface improves.
  • Water is a dispersion medium for silica particles and a solvent for other components. It is preferable that water does not inhibit the function of other components. Examples of such water include water having a total content of transition metal ions of 100 ppb or less.
  • the purity of water can be increased, for example, by removing impurity ions using an ion exchange resin, removing foreign matter using a filter, or distillation. Specifically, for example, ion exchange water, pure water, ultrapure water, distilled water or the like is preferably used.
  • the pH of a mixture obtained by mixing silica particles, a basic compound, and water is preferably 8 or more, more preferably 9 or more. As pH increases, aggregation is suppressed when an aqueous solution containing a water-soluble polymer is added to the mixture. Thereby, the dispersion stability of the polishing composition finally obtained improves.
  • the pH of the mixture is preferably 12 or less, more preferably 10.5 or less. As the pH decreases, silica dissolution is suppressed.
  • the pH of the mixture can be adjusted by the blending amount of the basic compound.
  • Water-soluble polymer works to improve the wettability of the surface to be polished.
  • the 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 can be used.
  • a functional group include a hydroxyl group, a carboxyl group, an acyloxy group, a sulfo group, a quaternary nitrogen structure, a heterocyclic structure, a vinyl structure, and a polyoxyalkylene structure.
  • water-soluble polymer examples include cellulose derivatives, imine derivatives such as poly (N-acylalkyleneimine), polyvinyl alcohol, polyvinyl pyrrolidone, copolymers containing polyvinyl pyrrolidone as part of the structure, polyvinyl caprolactam, and polyvinyl caprolactam.
  • a water-soluble polymer may be used individually by 1 type, and may be used in combination of 2 or more type.
  • a cellulose derivative, polyvinyl pyrrolidone, or a polymer having a polyoxyalkylene structure is preferable from the viewpoint of imparting good hydrophilicity to the polished substrate surface.
  • 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 preferable because it has a high ability to impart wettability to a polished surface and has good cleaning and removing properties.
  • the weight average molecular weight of the water-soluble polymer is preferably 1,000 or more in terms of polyethylene oxide, more preferably 10,000 or more, still more preferably 100,000 or more, and still more preferably 200,000 or more. . As the weight average molecular weight of the water-soluble polymer increases, the hydrophilicity of the polished surface increases.
  • the weight average molecular weight of the water-soluble polymer is preferably 2,000,000 or less, more preferably 1,500,000 or less, still more preferably 1,000,000 or less, and most preferably 500,000 or less. is there. As the weight average molecular weight of the water-soluble polymer decreases, the dispersion stability of the polishing composition improves.
  • the content of the water-soluble polymer in the aqueous solution is preferably 0.02% by mass or more, more preferably 0.05% by mass or more, and further preferably 0.1% by mass or more. As the content of the water-soluble polymer in the aqueous solution increases, it becomes easier to increase the content of the water-soluble polymer in the polishing composition.
  • the content of the water-soluble polymer in the aqueous solution is preferably 10% by mass or less, more preferably 5% by mass or less, and still more preferably 3% by mass or less. As the content of the water-soluble polymer in the aqueous solution decreases, aggregation during the preparation of the polishing composition is suppressed.
  • the content of the water-soluble polymer in the polishing composition finally obtained is preferably 0.002% by mass or more, more preferably 0.004% by mass or more, and further preferably 0.006% by mass. That's it. As the content of the water-soluble polymer in the polishing composition increases, the wettability of the polished surface increases.
  • the content of the water-soluble polymer in the polishing composition is preferably 0.5% by mass or less, more preferably 0.2% by mass or less, and still more preferably 0.1% by mass or less. As the content of the water-soluble polymer in the polishing composition decreases, the dispersion stability of the polishing composition improves.
  • the aqueous solution is preferably adjusted to a range from approximately neutral to basic, more preferably basic (for example, pH 8 to 12).
  • the pH of the aqueous solution is preferably 8 or more, more preferably 9 or more.
  • As the pH of the aqueous solution increases aggregation of the silica particles when the aqueous solution is added to a mixture containing silica particles, a basic compound, and water is suppressed. Thereby, the dispersion stability of the polishing composition finally obtained improves.
  • the pH of the aqueous solution is preferably 12 or less, more preferably 10.5 or less. As the pH of the aqueous solution decreases, silica dissolution is suppressed.
  • the addition rate of the aqueous solution to the mixture is preferably 0.1 mL / min or more, more preferably 1 mL / min or more, and further preferably 5 mL / min or more with respect to 1 L of the mixture. As the addition rate increases, the production efficiency of the polishing composition improves.
  • the addition rate of the aqueous solution to the mixture is preferably 500 mL / min or less, more preferably 100 mL / min or less, and further preferably 50 mL / min or less with respect to 1 L of the mixture. As the addition rate decreases, silica agglomeration is suppressed.
  • the aqueous solution is preferably filtered before being added to the mixture.
  • filtration By filtration, foreign matters or aggregates contained in the aqueous solution are reduced. Filtration may be natural filtration performed under normal pressure, suction filtration, pressure filtration, or centrifugal filtration.
  • the filter used for filtration is preferably selected on the basis of the opening.
  • the aperture of the filter is preferably 0.05 ⁇ m or more, more preferably 0.1 ⁇ m or more, and further preferably 0.2 ⁇ m or more. As the aperture of the filter increases, the production efficiency of the polishing composition improves.
  • the opening of the filter is preferably 100 ⁇ m or less, more preferably 70 ⁇ m or less, and even more preferably 50 ⁇ m or less. As the aperture of the filter is reduced, the removal efficiency of foreign matters or aggregates contained in the aqueous solution is improved. Thereby, the dispersion stability of the polishing composition is further improved.
  • the pH of the polishing composition finally obtained is preferably 8 or more, more preferably 8.5 or more, and still more preferably 9 or more.
  • the pH of the polishing composition is preferably 12.5 or less, more preferably 12 or less, and still more preferably 11.5 or less.
  • the smoothness of the polished surface improves.
  • the polishing composition may contain, for example, a surfactant, an organic acid, an organic acid salt, an inorganic acid, an inorganic acid salt, a chelating agent and the like within a range not impairing the effects of the present invention.
  • Surfactant functions to suppress roughening of the polished surface. Thereby, it becomes easy to reduce the haze level of the polished surface.
  • the polishing composition contains a basic compound
  • the polished surface is easily roughened by chemical etching with the basic compound. For this reason, the combined use of a basic compound and a surfactant is effective.
  • the surfactant examples include an ionic or nonionic surfactant having a weight average molecular weight of less than 1,000.
  • the surfactants nonionic surfactants are preferable. Since the nonionic surfactant has low foaming property, it is easy to handle at the time of preparation and use of the polishing composition. Moreover, when a nonionic surfactant is used, pH adjustment of polishing composition becomes easy.
  • nonionic surfactant examples include oxyalkylene polymers such as polyethylene glycol and polypropylene glycol, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene alkylamine, polyoxyethylene fatty acid ester, polyoxyethylene Examples include polyoxyalkylene adducts such as ethylene glyceryl ether fatty acid esters and polyoxyethylene sorbitan fatty acid esters.
  • 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 organic acid and its salt, and the inorganic acid and its salt serve to improve the hydrophilicity of the polished surface.
  • 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 salt and potassium salt of these organic acids, and ammonium salt.
  • inorganic acids 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 salt and potassium salt of these inorganic acids, and ammonium salt.
  • ammonium salts are preferable from the viewpoint of suppressing metal contamination of abrasive products.
  • Organic acids and salts thereof and inorganic acids and salts thereof may be used alone or in combination of two or more.
  • the chelating agent functions to suppress metal contamination of the abrasive product by capturing metal impurities and forming a complex.
  • Specific examples of the chelating agent include aminocarboxylic acid chelating agents and organic phosphonic acid chelating agents.
  • Specific examples of the aminocarboxylic acid chelating agent include ethylenediaminetetraacetic acid, sodium ethylenediaminetetraacetate, nitrilotriacetic acid, sodium nitrilotriacetate, ammonium nitrilotriacetate, hydroxyethylethylenediaminetriacetic acid, sodium hydroxyethylethylenediaminetriacetate, diethylenetriamine Examples include acetic acid, sodium diethylenetriaminepentaacetate, triethylenetetraminehexaacetic acid, and sodium triethylenetetraminehexaacetate.
  • organic phosphonic acid-based chelating agents include 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetrakis (methylenephosphonic acid), diethylenetriaminepenta (methylene Phosphonic acid), triethylenetetraamine hexa (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, ⁇ -methylphosphonosucci Etc.
  • chelating agents may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the chelating agent is an organic phosphonic acid chelating agent, more preferably ethylenediaminetetrakis (methylenephosphonic acid).
  • the method for producing the polishing composition of the present embodiment comprises a step of preparing a mixture by mixing silica particles, a basic compound, and water, and an aqueous solution containing a water-soluble polymer in the mixture.
  • the process of adding When the stability of the silica particles in the mixture is low (for example, the mixture is almost neutral), when the aqueous solution is added to the mixture, the aggregation of silica particles is caused by the action of the water-soluble polymer in the aqueous solution. appear.
  • high-purity silica particles with few impurities are used in a polishing composition used for final polishing of a silicon substrate.
  • the pH of a solution in which such high-purity silica particles are dispersed in ultrapure water is almost neutral.
  • the pH of the silica particle dispersion is adjusted to basic so as to increase the stability of the silica particles. Aggregation can be suppressed.
  • the polishing composition When polishing the surface of the silicon substrate using the polishing composition, the polishing composition is supplied to the surface of the silicon substrate and the polishing pad is pressed against the surface to rotate the silicon substrate and the polishing pad. At this time, physical action by friction between the polishing pad and the silicon substrate surface, physical action by friction between silica particles in the polishing composition and the silicon substrate, and basic compound in the polishing composition The surface of the silicon substrate is polished by the chemical action caused by.
  • an aqueous solution containing a water-soluble polymer is added after preparing a mixture of silica particles, a basic compound, and water. Thereby, aggregation of the silica particle at the time of preparation of polishing composition can be suppressed, and the dispersion stability of polishing composition can be improved.
  • the aqueous solution is preferably basic. In this case, aggregation during the preparation of the polishing composition can be further suppressed.
  • the polishing composition is preferably used for polishing a silicon substrate. In this case, it becomes easy to obtain a high-quality silicon substrate.
  • the polishing composition is preferably used for final polishing of a silicon substrate. In this case, even when high-purity silica particles with few metal impurities are used as the abrasive grains, aggregation during the preparation of the polishing composition can be suppressed.
  • any one of a mixture of silica particles, a basic compound and water, or an aqueous solution containing a water-soluble polymer may be prepared first.
  • -Polishing composition may contain well-known additives, such as antiseptic
  • antiseptic and antifungal agent include, for example, isothiazoline compounds, paraoxybenzoates, phenoxyethanol and the like.
  • the polishing composition may be in a concentrated state at the time of manufacture and sale. That is, the polishing composition may be manufactured and sold in the form of a stock solution of the polishing composition.
  • the polishing composition may be prepared by diluting a stock solution of the polishing composition with water.
  • the dilution rate is preferably 2 times or more, more preferably 5 times or more, and further preferably 10 times or more.
  • the dilution ratio is preferably 100 times or less, more preferably 50 times or less, and further preferably 40 times or less.
  • the stability of the stock solution of the polishing composition improves.
  • Each component contained in the polishing composition may be filtered with a filter immediately before the polishing composition is produced. Moreover, polishing composition may be filtered with a filter immediately before use. By performing the filtration treatment, coarse foreign matters in the polishing composition are removed, and the quality is improved.
  • the material and structure of the filter used for the filtration process are not particularly limited.
  • the filter material include cellulose, nylon, polysulfone, polyethersulfone, polypropylene, polytetrafluoroethylene (PTFE), polycarbonate, and glass.
  • the filter structure include a depth filter, a pleated filter, and a membrane filter.
  • the type of polishing pad used in the polishing method using the polishing composition is not particularly limited.
  • any of non-woven fabric type, suede type, those containing abrasive grains, and those not containing abrasive grains may be used.
  • the polishing composition once used for polishing may be collected and used again for polishing the substrate.
  • a method of reusing the polishing composition for example, there is a method in which the used polishing composition discharged from the polishing apparatus is once collected in a tank and then recycled from the tank to the polishing apparatus. Can be mentioned.
  • the amount of the polishing composition discharged as a waste liquid can be reduced, and the amount of the polishing composition used can be reduced. This is useful in that the environmental load can be reduced and the cost for polishing the substrate can be suppressed.
  • each component such as a water-soluble polymer in the polishing composition is consumed and lost by polishing. For this reason, it is preferable to supplement the polishing composition with a reduced amount of each component such as a water-soluble polymer.
  • the components to be replenished may be added individually to the polishing composition, or may be added to the polishing composition in a state where two or more components are mixed.
  • the method for preparing the water-soluble polymer follows the method for producing the polishing composition of the above embodiment.
  • the polishing composition may be applied to an object to be polished other than a silicon substrate.
  • the polishing object other than the silicon substrate include metals such as stainless steel, silicon oxide substrates, plastic substrates, glass substrates, and quartz substrates.
  • the component contained in polishing composition may be suitably changed according to a grinding
  • the shape of the abrasive grains may be spherical or non-spherical.
  • Specific examples of the non-spherical shape include a so-called bowl-shaped shape having an ellipsoid shape having a constriction at the center, a spherical shape having a plurality of protrusions on the surface, and a rugby ball shape.
  • Example 1 70 g of 29% aqueous ammonia as a basic compound was added to 5000 g of pH 7.0 colloidal silica dispersion (concentration: 20% by mass) to prepare a colloidal silica dispersion of pH 10.3. Next, 2000 g of a 2% by weight aqueous solution of hydroxyethyl cellulose having a pH of 7.0 (weight average molecular weight 250,000) as a cellulose derivative was added to the colloidal silica dispersion. Finally, 3000 g of ultrapure water was added to prepare the polishing composition of Example 1.
  • the polishing composition thus obtained the presence or absence of gelation was evaluated visually. As a result, it was found that the polishing composition of Example 1 was a uniform solution without gelation.
  • the presence or absence of gelation was also evaluated by the content of particles having a predetermined particle diameter or more in the polishing composition. Specifically, the number of particles having a size of 0.1 ⁇ m or more (hereinafter referred to as LPC) contained in the polishing composition was measured using “Accuriser FX” manufactured by PSS (Particle Sizing Systems). . As a result, the LPC was 53000 / mL.
  • Example 2 60 g of 29% ammonia water was added to 5000 g of pH 7.0 colloidal silica dispersion (concentration 20 mass%) to prepare a colloidal silica dispersion of pH 10.2.
  • 10 g of 29% ammonia water was added to 2000 g of a 2% by mass aqueous solution of hydroxyethyl cellulose (weight average molecular weight 250,000) at pH 7.0 to prepare a pH 10.0 aqueous solution of hydroxyethyl cellulose.
  • 2010 g of the hydroxyethyl cellulose aqueous solution was added to 5060 g of the colloidal silica dispersion.
  • 3000 g of ultrapure water was added to prepare the polishing composition of Example 2.
  • the polishing composition thus obtained the presence or absence of gelation was evaluated visually.
  • the polishing composition of Example 2 was a uniform solution without gelation.
  • LPC was measured in the same manner as in Example 1.
  • the LPC was 44000 / mL, which was a better result than that of Example 1.
  • Comparative Example 1 70 g of 29% ammonia water was added to 2000 g of a 2 mass% aqueous solution of hydroxyethyl cellulose (weight average molecular weight 250,000) to prepare a hydroxyethyl cellulose aqueous solution having a pH of 10.6. Next, 2070 g of the hydroxyethyl cellulose aqueous solution was added to 5000 g of colloidal silica dispersion (concentration: 20% by mass) having a pH of 7.0. Finally, 3000 g of ultrapure water was added to prepare the polishing composition of Comparative Example 1.
  • the presence or absence of gelation was evaluated visually. As a result, mild gelation was observed when the hydroxyethyl cellulose aqueous solution and the colloidal silica dispersion were mixed.
  • Comparative Example 2 To 5000 g of colloidal silica dispersion having a pH of 7.0 (concentration of 20% by mass), 2000 g of a 2% by mass aqueous solution of hydroxyethyl cellulose having a pH of 7.0 (weight average molecular weight of 250,000) was added. Next, 70 g of 29% ammonia water was added, and finally 3000 g of ultrapure water was added to prepare a polishing composition of Comparative Example 2.
  • the aggregation of the polishing composition can be suppressed by a procedure of mixing silica particles, a basic compound, and water and then adding an aqueous solution containing a water-soluble polymer.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

La présente invention a trait à un procédé de fabrication d'une composition de polissage, lequel procédé est caractérisé en ce qu'il comprend : une étape consistant à mélanger des particules de silice en tant que grains abrasifs, un composé basique et de l'eau, et à préparer un mélange ; et une étape consistant à ajouter une solution aqueuse contenant un polymère hydrosoluble au mélange. La solution aqueuse mentionnée ci-dessus est de préférence basique. La composition de polissage est de préférence utilisée pour polir des substrats de silicium. La composition de polissage est de préférence utilisée pour procéder au polissage final de substrats de silicium.
PCT/JP2013/061621 2012-04-26 2013-04-19 Procédé de fabrication d'une composition de polissage Ceased WO2013161701A1 (fr)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015159259A (ja) * 2014-02-25 2015-09-03 株式会社フジミインコーポレーテッド 半導体基板を連続的に製造する方法
KR20160135752A (ko) * 2014-03-17 2016-11-28 니혼 캐보트 마이크로일렉트로닉스 가부시키가이샤 슬러리 조성물 및 기판 연마 방법
JP2019182987A (ja) * 2018-04-09 2019-10-24 花王株式会社 合成石英ガラス基板用研磨液組成物
WO2022049845A1 (fr) * 2020-09-04 2022-03-10 信越半導体株式会社 Composition de polissage, procédé destiné à usiner une plaquette, et plaquette de silicium

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7477964B2 (ja) * 2019-12-13 2024-05-02 インテグリス・インコーポレーテッド 化学機械研磨組成物及びそれを用いた化学機械研磨方法
CN115197645B (zh) * 2021-04-02 2024-02-20 Sk恩普士有限公司 半导体工艺用抛光组合物以及半导体器件的制造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005029563A1 (fr) * 2003-09-24 2005-03-31 Nippon Chemical Industrial Co.,Ltd. Composition de polissage pour plaquette en silicium et procede de polissage
JP2006128518A (ja) * 2004-10-29 2006-05-18 Fujimi Inc 研磨用組成物
JP2006202932A (ja) * 2005-01-20 2006-08-03 Nippon Chem Ind Co Ltd 研磨用組成物、その製造方法及び該研磨用組成物を用いる研磨方法
JP2012079964A (ja) * 2010-10-04 2012-04-19 Nissan Chem Ind Ltd 半導体ウェーハ用研磨液組成物

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005029563A1 (fr) * 2003-09-24 2005-03-31 Nippon Chemical Industrial Co.,Ltd. Composition de polissage pour plaquette en silicium et procede de polissage
JP2006128518A (ja) * 2004-10-29 2006-05-18 Fujimi Inc 研磨用組成物
JP2006202932A (ja) * 2005-01-20 2006-08-03 Nippon Chem Ind Co Ltd 研磨用組成物、その製造方法及び該研磨用組成物を用いる研磨方法
JP2012079964A (ja) * 2010-10-04 2012-04-19 Nissan Chem Ind Ltd 半導体ウェーハ用研磨液組成物

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2015159259A (ja) * 2014-02-25 2015-09-03 株式会社フジミインコーポレーテッド 半導体基板を連続的に製造する方法
KR20160135752A (ko) * 2014-03-17 2016-11-28 니혼 캐보트 마이크로일렉트로닉스 가부시키가이샤 슬러리 조성물 및 기판 연마 방법
KR102411832B1 (ko) 2014-03-17 2022-06-22 씨엠씨 마테리알즈 가부시키가이샤 슬러리 조성물 및 기판 연마 방법
JP2019182987A (ja) * 2018-04-09 2019-10-24 花王株式会社 合成石英ガラス基板用研磨液組成物
JP7008564B2 (ja) 2018-04-09 2022-01-25 花王株式会社 合成石英ガラス基板用研磨液組成物
WO2022049845A1 (fr) * 2020-09-04 2022-03-10 信越半導体株式会社 Composition de polissage, procédé destiné à usiner une plaquette, et plaquette de silicium
JP2022043424A (ja) * 2020-09-04 2022-03-16 信越半導体株式会社 研磨用組成物、ウェーハの加工方法、及びシリコンウェーハ
JP7380492B2 (ja) 2020-09-04 2023-11-15 信越半導体株式会社 研磨用組成物及びウェーハの加工方法

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TW201402734A (zh) 2014-01-16

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