WO2017150114A1 - 研磨用組成物 - Google Patents

研磨用組成物 Download PDF

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Publication number
WO2017150114A1
WO2017150114A1 PCT/JP2017/004582 JP2017004582W WO2017150114A1 WO 2017150114 A1 WO2017150114 A1 WO 2017150114A1 JP 2017004582 W JP2017004582 W JP 2017004582W WO 2017150114 A1 WO2017150114 A1 WO 2017150114A1
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WO
WIPO (PCT)
Prior art keywords
polishing composition
polishing
water
mass
abrasive grains
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PCT/JP2017/004582
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English (en)
French (fr)
Japanese (ja)
Inventor
孝一 福井
雄大 湯浅
優二 川浦
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信越半導体株式会社
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Application filed by 信越半導体株式会社 filed Critical 信越半導体株式会社
Priority to KR1020187017929A priority Critical patent/KR20180118603A/ko
Publication of WO2017150114A1 publication Critical patent/WO2017150114A1/ja

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Classifications

    • 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
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/04—Aqueous dispersions
    • 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
    • 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
    • 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 suitable for polishing a silicon wafer for manufacturing a semiconductor substrate. More specifically, the present invention relates to a polishing composition suitable for final polishing of a bare silicon wafer for manufacturing a semiconductor substrate.
  • Bare silicon wafers for manufacturing semiconductor substrates are required to have a low number of particles remaining on the surface and a haze value, but the design rules of semiconductor substrates tend to become finer, so these surface quality requirements Has become even more severe.
  • Patent Document 1 a proposal to use a hydrolyzate as hydroxyethyl cellulose contained in the polishing composition (Patent Document 1), or to reduce microparticles on the silicon wafer surface, low
  • Patent Document 2 The use of hydroxyethyl cellulose having a molecular weight has been proposed (Patent Document 2).
  • Patent Document 3 As a polishing liquid composition capable of obtaining a silicon wafer having a small number of particles and a haze value, a polishing composition containing silica particles, a water-soluble alkali compound, an alkyl polyglycoside, and a cationized polyvinyl alcohol has been proposed. (Patent Document 3).
  • the present invention is intended to solve the above-described problems, and is a polishing composition that is excellent in wafer protection ability (alkali etching resistance) and can be expected to reduce the haze value while maintaining a low particle level.
  • Particles are foreign materials such as abrasives, polishing pad scraps and silicon chips adhering to the wafer surface, and haze is when a light beam is applied to fine irregularities that are difficult to measure with a surface roughness meter on the wafer surface. Observed cloudiness. A smaller haze value means higher surface smoothness.
  • a factor that causes the polishing composition to deteriorate the quality of the surface of the silicon wafer is roughness of the surface of the silicon wafer due to the etching ability of the composition itself.
  • the present invention provides a polishing composition that enables a good haze value reduction as a result of excellent silicon wafer protection ability (alkali etching resistance).
  • the surface of the silicon wafer immediately after polishing has an appropriate hydrophilicity.
  • This invention provides the polishing composition which can give moderate hydrophilicity to the silicon wafer surface immediately after grinding
  • the present invention (A) abrasive grains, (B) a water-soluble alkali compound, (C) at least one organic compound selected from hydroxyethyl cellulose (D) alkyl glucoside and alkanolamide having a weight average molecular weight of 500,000 or less, And (E) water, A polishing composition comprising
  • polishing composition in which the abrasive grains are colloidal silica is a preferred embodiment of the present invention.
  • the above-described polishing composition in which the colloidal silica has an average primary particle diameter determined by a nitrogen adsorption method (BET method) of 5 to 100 nm is a preferred embodiment of the present invention.
  • polishing composition in which the colloidal silica is vertical colloidal silica obtained by reacting an alkoxysilane condensate with water in the presence of ammonia or an ammonium salt catalyst, is a preferred embodiment of the present invention.
  • Abrasive grains are 0.05 to 1.0% by mass
  • (C) hydroxyethyl cellulose is 0.005% based on the entire composition.
  • the polishing composition described above in which the amount of the organic compound component is 0.0001 to 0.02% by mass is in a preferred embodiment of the present invention.
  • polishing composition used for polishing a silicon wafer is a preferred embodiment of the present invention.
  • the present invention also provides a method for polishing a silicon wafer, comprising a step of polishing a silicon wafer using the polishing composition described above.
  • a polishing composition that is excellent in wafer protection ability (alkali etching resistance) and as a result can be expected to have a good haze reduction.
  • a polishing composition capable of imparting appropriate hydrophilicity to the silicon wafer surface immediately after polishing is provided, so that dry adhesion such as abrasive grains and polishing waste generated during polishing is prevented, and these As a result, it is possible to provide a polishing composition that can be expected to realize good surface quality.
  • the present invention provides a polishing composition that is excellent in wafer protection ability (alkali etching resistance) and can impart appropriate wettability to a polished wafer.
  • Patent Documents 1 to 8 Alkanolamide and alkyl glucoside are both compounds known as nonionic surfactants.
  • the polishing composition using the specific components (A) to (E) of the present invention has a high wafer protection ability because of its low etching property to a silicon wafer, and in addition, achieves a good polishing rate.
  • the wafer surface after polishing has an excellent effect of having good hydrophilicity.
  • the present invention (A) abrasive grains, (B) a water-soluble alkali compound, (C) Provided is a polishing composition comprising at least one organic compound selected from hydroxyethylcellulose (D) alkyl glucoside and alkanolamide having a weight average molecular weight of 500,000 or less and (E) water.
  • the abrasive grains contained in the polishing composition of the present invention are not particularly limited as long as they are abrasive grains usually used for polishing, and include inorganic particles, organic particles, organic-inorganic composite particles, and the like. Among these, inorganic particles are preferable. Examples of inorganic particles that can be used as abrasive grains include particles containing silicon dioxide, aluminum oxide, cerium oxide, zirconium oxide, titanium oxide, silicon nitride, manganese dioxide, silicon carbide, zinc oxide, diamond, and magnesium oxide. .
  • the inorganic particles of the abrasive material include silicon dioxide such as colloidal silica, fumed silica, and surface-modified silica; ⁇ -alumina, ⁇ -alumina, ⁇ -alumina, ⁇ -alumina, ⁇ -alumina, Aluminum oxide such as regular alumina, fumed alumina, colloidal alumina; cerium oxide with trivalent or tetravalent oxidation number, hexagonal, equiaxed or face-centered cubic cerium oxide, and other oxidations Cerium; monoclinic, tetragonal, or amorphous zirconium oxide, fumed zirconium, other zirconium oxides; titanium monoxide, titanium dioxide, titanium dioxide, fumed titania, etc.
  • Titanium oxide Titanium oxide; ⁇ -silicon nitride, ⁇ -silicon nitride, amorphous silicon nitride, other silicon nitrides; ⁇ -manganese dioxide, ⁇ Manganese dioxide, ⁇ - manganese dioxide, ⁇ - manganese dioxide, ⁇ - manganese dioxide, ⁇ - manganese dioxide, and other manganese dioxide, and the like.
  • These abrasive grains may be used alone or in admixture of two or more.
  • silicon dioxide is preferable, and colloidal silica is more preferable.
  • As an abrasive grain it is preferable that it is a slurry form from a viewpoint of operativity.
  • the average primary particle diameter determined by the nitrogen adsorption method (BET method) of silica particles is 5 to 100 nm, preferably 10 to 40 nm, particularly preferably. 10 to 25 nm.
  • the secondary particle size distribution of the silica particles can be measured by a dynamic light scattering method, and the cumulative 50% particle size D50 of the distribution (volume display) is called the average secondary particle size.
  • the average secondary particle size of the silica particles is desirably 10 to 90 nm, preferably 20 to 80 nm, more preferably 25 to 70 nm, and further preferably 25 to 40 nm.
  • the variation coefficient CV of the secondary particle diameter of the silica particles is 0.10 to 0.50, preferably 0.20 to 0.40.
  • Particularly preferred silica particles have an average secondary particle diameter D50 of 25 to 40 nm and a coefficient of variation CV of 0.20 to 0.40.
  • the shape (outer shape) of the abrasive grains may be spherical or non-spherical.
  • specific examples of non-spherical abrasive grains include a peanut shape (that is, a peanut shell shape), a bowl shape, a confetti shape, and a rugby ball shape.
  • abrasive grains in which most of the abrasive grains have a peanut shape or a bowl shape can be preferably employed. Of these, a bowl-shaped abrasive is preferred.
  • the method for synthesizing the abrasive grains is not limited.
  • Examples of the method for synthesizing silica particles include a hydrothermal synthesis method from water glass, a sol-gel method from alkoxysilane or a condensate thereof, and a gas phase synthesis method from silicon chloride.
  • silica particles produced by a sol-gel method from an alkoxysilane or a condensate thereof are preferred.
  • vertical silica particles prepared by a method including a step of reacting an alkoxysilane condensate with water (sol-gel reaction step) (sometimes referred to as new vertical silica particles in distinction from other vertical silica particles) (Japanese Patent No.
  • the average condensation degree of the condensate is preferably 2 to 10, and more preferably 2 to 8.
  • the soot type includes a new soot type.
  • water-soluble alkali compounds include nitrogen-containing basic compounds, alkali metal and alkaline earth metal hydroxides from the viewpoint of preventing agglomeration of abrasive grains and providing an appropriate polishing rate by a chemical polishing action.
  • examples thereof include carbonates and bicarbonates.
  • the nitrogen-containing basic compound include ammonia (ammonium hydroxide), ammonium carbonate, ammonium hydrogen carbonate, organic amines, piperazines, quaternary ammonium hydroxides and the like.
  • alkali metal and alkaline earth metal hydroxides, carbonates, and bicarbonates include potassium hydroxide, sodium hydroxide, potassium carbonate, potassium bicarbonate, sodium carbonate, and sodium bicarbonate. Can be mentioned. These basic compounds may be used alone or in combination of two or more.
  • water-soluble alkali compounds from the viewpoint of not containing alkali metal ions, ammonia, organic amines, and quaternary ammonium hydroxides such as tetramethylammonium hydroxide are preferable. From the viewpoint of improving the surface accuracy of the polished surface, ammonia is particularly preferable.
  • the weight average molecular weight (Mw) of the hydroxyethyl cellulose of the present invention (hereinafter sometimes abbreviated as HEC) is 500,000 or less, preferably 200,000 or less, more preferably 10,000 or more and less than 200,000.
  • HEC has a weight average molecular weight of 500,000 or less, preferably 200,000 or less, more preferably less than 200,000.
  • the weight average molecular weight of HEC is desirably 10,000 or more. When the amount falls within the above range, good cleaning properties are exhibited while imparting sufficient hydrophilicity to the wafer, and a particle reduction effect is expected.
  • alkanolamide is a compound in which an alkanolamine and a fatty acid are amide-bonded, and the fatty acid has an alkyl chain length of 6 to 22, more preferably 6 to 18, and even more preferably 8 to 14 linear or branched chain. It is desirable to have Examples of fatty acids include caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid and the like. Examples of alkanolamines include diethanolamine, isopropanolamine, monoethanolamine, 2-aminoethyl-ethanolamine and the like.
  • alkanolamides include caprylic acid diethanolamide, pelargonic acid diethanolamide, capric acid diethanolamide, lauric acid diethanolamide, myristic acid diethanolamide, palmitic acid diethanolamide, stearic acid diethanolamide, oleic acid diethanolamide diethanolamide, Examples thereof include lauric acid monoethanolamide. A mixture thereof may be used.
  • alkyl glucoside is a compound in which glucose (saccharide) and a higher alcohol are glucoside-bonded, and the alkyl chain length is 6 to 22, more preferably 6 to 18, and still more preferably 8 to 14 carbon atoms. Those having a chain are desirable. Moreover, what has condensed saccharides in which saccharides may condense may be called alkylpolyglucoside, However, The alkylglucoside of this invention is used by the meaning containing alkylpolyglucoside.
  • alkyl glucoside having a sugar condensation degree of 1.0 to 10.0, more preferably 1.0 to 5.0, and still more preferably 1.0 to 3.0 in the alkyl glucoside.
  • Specific examples of the alkyl glucoside include octyl glucoside, decyl glucoside, lauryl glucoside and the like. A mixture thereof may be used.
  • water examples of water used in the present invention include ion exchange water (deionized water), pure water, ultrapure water, and distilled water.
  • ion exchange water deionized water
  • pure water pure water
  • ultrapure water ultrapure water
  • distilled water distilled water.
  • the purity of water can be increased by operations such as removal of impurity ions with an ion exchange resin, removal of foreign matters with a filter, and distillation.
  • the polishing composition of the present invention may contain other components as long as the object of the present invention is not impaired.
  • Such other components can be used for water-soluble polymers other than HEC, chelating agents, organic acids, organic acid salts, inorganic acids, inorganic acid salts, preservatives, fungicides, and other polishing compositions.
  • Known additives can be mentioned.
  • water-soluble polymers other than HEC examples include polyethylene glycol (polyethylene oxide), polypropylene glycol, a random copolymer of ethylene oxide and propylene oxide, a block copolymer of ethylene oxide and propylene oxide, a polyoxyalkylene alkyl ether, Polyoxyalkylene sorbitan fatty acid esters can be mentioned, and polyethylene glycol and polypropylene glycol are particularly preferable. One or more of these may be used, or two or more of the same and different molecular weights may be used in combination. Their average molecular weight is preferably 300 to 30,000.
  • the content thereof is 0.00001 to 0.1% by mass, preferably 0.0001 to 0.01% by mass, based on the entire composition. Is desirable.
  • the polyethylene glycol is 0.0001 to 0.1% by mass, preferably 0.0001 to 0.01% by mass
  • the polypropylene glycol is 0.00001% to the entire composition. Is 0.01% by mass, preferably 0.00001-0.005% by mass.
  • the average molecular weight of polyethylene glycol is preferably 1000 to 30000, and more preferably 3000 to 10,000.
  • the average molecular weight of polypropylene glycol is preferably 300 to 5000, more preferably 300 to 2000.
  • the average molecular weight of polyethylene glycol and polypropylene glycol can be determined from the hydroxyl value.
  • the ratio of (B) the water-soluble alkali compound is 0.002 to 0.5% by mass, preferably 0.01 to 0.2% by mass, based on 1% by mass of (A) abrasive grains.
  • (C) hydroxyethyl cellulose is 0.002 to 0.5% by mass, preferably 0.01 to 0.2% by mass, based on 1% by mass of (A) abrasive grains, and (D) an organic compound It is desirable that the component is 0.0002 to 0.2% by mass, preferably 0.001 to 0.1% by mass, based on 1% by mass of (A) abrasive grains.
  • each component of the polishing composition of the present invention when used for polishing is 0.01 to 2.0% by mass, preferably 0, of (A) abrasive grains with respect to the entire polishing composition. 0.05-1.0% by mass, (B) 0.0001-0.1% by mass of the water-soluble alkali compound, preferably 0.001-0.05% by mass, and (C) hydroxyethyl cellulose, 0.001 to 0.1% by mass, preferably 0.005 to 0.05% by mass, and (D) the organic compound component is 0.00001 to 0.05% by mass, preferably 0.0001 to 0.00%. It is desirable that it is 02 mass%.
  • the method for producing the polishing composition of the present invention is not particularly limited, and was selected from (A) abrasive grains, (B) water-soluble alkali compounds, (C) hydroxyethyl cellulose, (D) alkyl glucosides and alkanolamides. It can be prepared by mixing at least one organic compound and (E) water and optional components as necessary.
  • preparing a polishing composition concentrate by mixing a slurry of abrasive grains, a hydroxyethyl cellulose solution previously dissolved in water, water and at least one organic compound selected from alkyl glucoside and alkanolamide.
  • a polishing composition concentrate is obtained, and diluted with water at a predetermined dilution ratio immediately before polishing a silicon wafer, to obtain a desired polishing composition.
  • each component at the stage of the polishing composition concentrate is, for example, (A) 1-30% by mass of abrasive grains, preferably 2-20% by mass with respect to the entire polishing composition concentrate.
  • (B) water-soluble alkali compound is 0.01 to 2.0% by mass, preferably 0.1 to 1.0% by mass
  • (C) hydroxyethyl cellulose is 0.02 to 2.0% by mass.
  • % By weight, preferably 0.1 to 1.0% by weight
  • the organic compound component is 0.001 to 1.0% by weight, preferably 0.005 to 0.5% by weight. Good.
  • the polishing composition of the present invention can be used as an abrasive for various objects to be polished. In particular, it can be suitably used for a silicon wafer polishing step in the process of manufacturing a semiconductor substrate. Furthermore, the polishing composition of the present invention is a polishing composition suitable for final polishing of a bare silicon wafer for producing a semiconductor substrate.
  • the average secondary particle diameter of abrasive grains is indicated by the cumulative 50% particle diameter D50 of the particle size distribution (volume display) measured by the dynamic light scattering method. It was. Further, SD was defined as 1/2 of the difference between the cumulative 84% particle diameter and the cumulative 16% particle diameter.
  • the particle size distribution measurement by the dynamic light scattering method is made by Microtrac manufactured by Nikkiso Co., Ltd. Model UPA-UT151 was used. The measurement sample was prepared by diluting a slurry containing colloidal silica with ion-exchanged water so that the silica concentration was 0.1%.
  • Polishing test 1 A polishing test was performed using a polishing composition prepared by diluting a polishing composition concentrate with ion-exchanged water at a predetermined dilution rate. Polishing test 1 was performed with the following apparatus and conditions. Polishing machine: LGP-15S-I manufactured by Micro Engineering Co., Ltd.
  • Wafer 4-inch silicon wafer (P-type, resistivity 1 to 10 ⁇ ⁇ cm, crystal plane (100)) Surface pressure: 0.12 kgf / cm 2 Wafer rotation speed: 50 rpm Pad: SURFIN SSWI manufactured by Fujimi Pad rotation speed: 50 rpm Polishing slurry supply rate: 100 mL / min Polishing time: 10 minutes The polishing amount was determined from the change in weight of the wafer before and after polishing. The surface wettability (%) is the area of the wafer surface covered with water / the total area of the wafer surface (%). (1) Immediately after polishing (before removing the wafer from the polishing machine) and (2) Polishing After removing from the machine and applying ion exchange water to the surface, it was visually confirmed at the two timings.
  • Polishing test 2 was performed with the following apparatus and conditions.
  • Polishing machine PNX-332B manufactured by Okamoto Machine Tool Works
  • Wafer 12-inch silicon wafer (P-type, resistivity 1 to 100 ⁇ ⁇ cm, crystal plane (100))
  • Surface pressure 0.12 kgf / cm 2
  • Wafer rotation speed 30 rpm
  • Pad urethane foam pad
  • Rotation speed 30 rpm
  • Polishing slurry supply rate 100 mL / min
  • Polishing time Predetermined time (denoted as x1), twice the predetermined time (denoted as x2)
  • Particle and haze measurement Surfscan SP3 from KLA-Tencor
  • colloidal silica slurry having a silica concentration of 17.0 wt% and an NH 3 concentration of 1560 ppm.
  • Preparation Example 3 ⁇ Preparation of polishing composition (polishing slurry)> The colloidal silica slurry prepared in Preparation Example 1 and the HEC solution prepared in Preparation Example 2, NH 3 water, ion-exchanged water, and surfactants shown in Table 1 below, and as required. A predetermined amount of the PEG / PPG mixed solution was mixed to prepare a polishing composition concentrate. The polishing composition concentrate was diluted with ion-exchanged water at a predetermined dilution rate immediately before polishing to prepare a polishing composition.
  • Example 1 According to the preparation method of Preparation Example 3, using AA-A as a surfactant, 5.00 parts by weight of a 1% surfactant solution, 52.9 parts by weight of colloidal silica slurry, 17.6 parts by weight of HEC solution, A polishing composition concentrate was prepared by mixing 2.21 parts by weight of 3 % NH 3 water and 22.2 parts by weight of water. The concentrations of surfactant, abrasive grains, NH 3 and HEC contained in the resulting polishing composition concentrate are shown in Table 2. Subsequently, the obtained polishing composition concentrate was diluted with ion-exchanged water at a dilution rate shown in Table 2 to prepare a polishing composition.
  • an etching test, a polishing test 1 and a wettability test were performed.
  • the results are shown in Table 2.
  • the etching test the smaller the etching amount, the better.
  • the average etching amount (mg / day) was determined to be good when it was less than 0.10 mg, and poor when 0.10 mg or more.
  • the polishing test 1 the higher the polishing amount, the better. In this condition, it was determined that the polishing amount of 0.5 mg or more was good and less than 0.5 mg was bad.
  • the wettability test immediately after polishing and the wettability test after water rinse closer to 100% is preferable, and both are determined to be 90% or more as good and less than 90% as poor.
  • Example 2 In Example 1, the mixing ratio of each component was changed to 2.50 parts by weight of a 1% surfactant solution, 54.1 parts by weight of colloidal silica slurry, 21.5 parts by weight of HEC solution, 4% NH 3 water 2.
  • a polishing composition concentrate and a polishing composition were prepared in the same manner except for changing to 88 parts by weight and 19.0 parts by weight of water.
  • an etching test, a polishing test 1 and a wettability test were performed. The results are shown in Table 2.
  • Examples 3 and 4 A polishing composition concentrate and a polishing composition concentrate were prepared in the same manner as in Examples 1 and 2, except that each surfactant was replaced with AG-A. Using the obtained polishing composition concentrate and the polishing composition, an etching test, a polishing test 1 and a wettability test were performed. The results are shown in Table 2.
  • Example 5 A polishing composition concentrate and a polishing composition concentrate were prepared in the same manner except that the surfactant was replaced with AG-B in Example 1. Using the obtained polishing composition concentrate and the polishing composition, an etching test, a polishing test 1 and a wettability test were performed. The results are shown in Table 2.
  • Example 3 A polishing composition concentrate and a polishing composition concentrate were prepared in the same manner as in Example 1 except that the surfactant was replaced with PEG, and an etching test, a polishing test 1 and a wettability test were performed. The results are shown in Table 2.
  • Example 6 In Example 1, the amount of the surfactant solution was changed to 1.00 parts by weight, and the surfactant was POEAE-B (Comparative Example 6), POEAE-C (Comparative Example 7) or POEAPE-A (Comparative Example 8).
  • the polishing composition concentrate and the polishing composition concentrate were prepared in the same manner except that the polishing test 1 and the wettability test were performed. The results are shown in Table 2. The etching test was omitted.
  • polishing composition concentrate or polishing composition (Examples 1 to 5) to which alkanolamide or alkyl glucoside was added, all tests were satisfactory.
  • the etching test, the polishing test 1 or the wettability test was inferior.
  • Example 6 According to the preparation method of Preparation Example 3, using AA-A as a surfactant, 4.50 parts by weight of a 1% surfactant solution, 54.1 parts by weight colloidal silica slurry, 21.5 parts by weight of HEC solution, A polishing composition concentrate was prepared by mixing 2.88 parts by weight of 3 % NH 3 water, 4.50 parts by weight of a PEG / PPG mixed solution and 12.5 parts by weight of water. The concentrations of the surfactant, abrasive grains, NH 3 , HEC and other components contained in the obtained polishing composition concentrate are shown in Table 3.
  • the PEG / PPG mixed solution used in this example is an aqueous solution containing 8000 ppm of PEG-6000S manufactured by Sanyo Chemical Industries, Ltd. and 2000 ppm of Newpol PP1000 manufactured by the same company.
  • the obtained polishing composition concentrate was diluted with ion-exchanged water at a dilution rate shown in Table 3 to prepare a polishing composition.
  • Polishing test 2 was performed using the obtained polishing composition concentrate and polishing composition. The results are shown in Table 3.
  • the haze is shown as a relative value with the value of Comparative Example 9 below as 100. If it was less than 95, it was judged as good ( ⁇ ), 95 or more but less than 105 was acceptable ( ⁇ ), and 105 or more was judged as bad (x). The particles (26 nm or more) are shown as relative values with the value of Comparative Example 9 below as 100. If it was less than 90, it was judged as good ( ⁇ ), 90 or more but less than 200 was acceptable ( ⁇ ), and 200 or more was judged as bad (x).
  • Example 7 A polishing composition concentrate and a polishing composition were prepared in the same manner as in Example 6 except that the surfactant was replaced with AG-A (Example 7) or AG-B (Example 8). 2 was performed. The results are shown in Table 3.
  • Example 6 (Comparative Example 9) In Example 6, a polishing composition concentrate and a polishing composition were similarly prepared except that the use of a surfactant was omitted, and polishing test 2 was performed. The results are shown in Table 3.
  • the polishing composition provided by the present invention is excellent in wafer protection ability (alkali etching resistance), and as a result, a good haze value reduction can be expected.
  • a polishing composition capable of imparting appropriate hydrophilicity to the silicon wafer surface immediately after polishing is provided, so that it is easy to wash away and remove the abrasive grains and fine silicon debris generated during polishing. It becomes.
  • a polishing composition that can be expected to realize good surface quality is provided.
  • the polishing composition provided by the present invention is a polishing composition that is excellent in wafer protection ability (alkali etching resistance) and can impart appropriate wettability to a polished wafer.
  • the polishing composition provided by the present invention is used as a polishing agent for various objects to be polished, and can be suitably used particularly for a silicon wafer polishing step in the process of manufacturing a semiconductor substrate. Furthermore, the polishing composition of the present invention is a polishing composition suitable for final polishing of a bare silicon wafer for producing a semiconductor substrate.

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  • Organic Chemistry (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
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  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
PCT/JP2017/004582 2016-03-04 2017-02-08 研磨用組成物 WO2017150114A1 (ja)

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CN114829521A (zh) * 2019-12-13 2022-07-29 Cmc材料株式会社 化学机械抛光组合物及使用其的化学机械抛光方法

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