WO2016143323A1 - Composition pour meulage et procédé pour le meulage d'un substrat en silicium - Google Patents

Composition pour meulage et procédé pour le meulage d'un substrat en silicium Download PDF

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Publication number
WO2016143323A1
WO2016143323A1 PCT/JP2016/001226 JP2016001226W WO2016143323A1 WO 2016143323 A1 WO2016143323 A1 WO 2016143323A1 JP 2016001226 W JP2016001226 W JP 2016001226W WO 2016143323 A1 WO2016143323 A1 WO 2016143323A1
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Prior art keywords
general formula
group
polishing
polishing composition
bond
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PCT/JP2016/001226
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English (en)
Japanese (ja)
Inventor
雄彦 村瀬
彩 西村
修平 ▲高▼橋
誠 田畑
森　嘉男
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Fujimi Inc
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Fujimi Inc
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Priority to JP2017504864A priority Critical patent/JPWO2016143323A1/ja
Publication of WO2016143323A1 publication Critical patent/WO2016143323A1/fr
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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
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • 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
    • H10P52/00—Grinding, lapping or polishing of wafers, substrates or parts of devices

Definitions

  • the present invention relates to a polishing composition and a method for polishing a silicon substrate.
  • An object of the present invention is to provide a polishing composition and a method for polishing a silicon substrate that can solve the above-mentioned problems of the prior art and can realize both good surface quality and high polishing rate. .
  • X 1 in the general formula (1) represents a hydrogen atom, an amino group, or a bond to the C 1 atom in the general formula (1).
  • the general formula (1 The H 1 atom in) does not exist.
  • X 2 in the general formula (1) hydrogen atom, an amino group, showed binding aminoalkyl group, or the C 1 atom, typically a C 1 atom if X 2 represents a bond to C 1 atom
  • the bond with the N 1 atom in formula (1) is a double bond, and there is no H 2 atom in general formula (1).
  • l in the general formula (1) is an integer of 1 to 6
  • m is an integer of 1 to 4
  • n is an integer of 0 to 4.
  • a in the general formula (2) represents nitrogen or phosphorus.
  • R 1 , R 2 , R 3 and R 4 in the general formula (2) are each independently an alkyl group having 1 to 4 carbon atoms, a hydroxyalkyl group having 1 to 4 carbon atoms, or a substituent. The aryl group which may be made is shown. Further, X ⁇ in the general formula (2) represents an anion.
  • R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 in the general formula (3) are each independently a hydrogen atom or an alkyl group having 4 or less carbon atoms.
  • p, q, and r in General formula (3) are 1 or more and 4 or less integers.
  • Y and Z in the general formula (4) each independently have a functional group having at least one of carbon, nitrogen, oxygen, sulfur, phosphorus, and hydrogen, and having a double bond or a triple bond.
  • R 11 and R 12 in the general formula (4) are each independently a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a hydroxyalkyl group having 1 to 4 carbon atoms, or substituted. A good aryl group is indicated.
  • s in the general formula (4) is an integer of 0 or more and 2 or less.
  • the cyclic portion in the general formula (5) is a carbon six-membered ring, and the carbon-carbon bond is a single bond or a double bond.
  • Q in General formula (5) shows an anionic functional group.
  • X 3 , X 4 , X 5 , X 6 and X 7 in the general formula (5) are each independently hydrogen, a carboxy group or a salt thereof, a sulfonic acid group or a salt thereof, a phosphonic acid group or a salt thereof.
  • a method for polishing a silicon substrate comprising polishing a silicon substrate using the polishing composition according to the above aspect.
  • the polishing composition of this embodiment contains abrasive grains, a basic compound, and at least one of a multiple bond-containing compound and an anionic group-containing compound.
  • This basic compound includes a cyclic compound represented by the following general formula (1).
  • the basic compound is represented by an alkali metal hydroxide, an alkali metal hydrogen carbonate, an alkali metal carbonate, a cyclic compound represented by the following general formula (1), or the following general formula (2).
  • the multiple bond-containing compound is represented by the following general formula (4), and the anionic group-containing compound is represented by the following general formula (5).
  • X 1 in the general formula (1) represents a hydrogen atom, an amino group, or a bond to the C 1 atom in the general formula (1).
  • the general formula (1 The H 1 atom in) does not exist.
  • X 2 in the general formula (1) hydrogen atom, an amino group, showed binding aminoalkyl group, or the C 1 atom, typically a C 1 atom if X 2 represents a bond to C 1 atom
  • the bond with the N 1 atom in formula (1) is a double bond, and there is no H 2 atom in general formula (1).
  • l in the general formula (1) is an integer of 1 to 6
  • m is an integer of 1 to 4
  • n is an integer of 0 to 4.
  • X 1 and X 2 in general formula (1) may be the same or different.
  • a in the general formula (2) represents nitrogen or phosphorus.
  • R 1 , R 2 , R 3 and R 4 in the general formula (2) are each independently an alkyl group having 1 to 4 carbon atoms, a hydroxyalkyl group having 1 to 4 carbon atoms, or a substituent.
  • the aryl group which may be made (the aryl group which may have a substituent) is shown.
  • X ⁇ in the general formula (2) represents an anion.
  • R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 in the general formula (3) are each independently a hydrogen atom or an alkyl group having 4 or less carbon atoms.
  • p, q, and r in General formula (3) are 1 or more and 4 or less integers.
  • Y and Z in the general formula (4) each independently have a functional group having at least one of carbon, nitrogen, oxygen, sulfur, phosphorus, and hydrogen, and having a double bond or a triple bond.
  • R 11 and R 12 in the general formula (4) are each independently a hydrogen atom, an alkyl group having 1 to 4 carbon atoms, a hydroxyalkyl group having 1 to 4 carbon atoms, or substituted. A good aryl group is indicated.
  • s in the general formula (4) is an integer of 0 or more and 2 or less.
  • Y and Z may be the same functional group or different functional groups.
  • the cyclic portion in the general formula (5) is a carbon six-membered ring, and the carbon-carbon bond is a single bond or a double bond.
  • Q in General formula (5) shows an anionic functional group.
  • X 3 , X 4 , X 5 , X 6 and X 7 in the general formula (5) are each independently hydrogen, a carboxy group or a salt thereof, a sulfonic acid group or a salt thereof, a phosphonic acid group or a salt thereof.
  • the polishing composition is substantially free of an oxidizing agent.
  • an oxidizing agent is contained in the polishing composition, the polishing composition is supplied to the object to be polished, whereby the surface of the object to be polished is oxidized to form an oxide film, thereby increasing the polishing rate. It can be a downward trend.
  • polishing composition does not contain an oxidizing agent substantially, such inconvenience can be avoided.
  • Such a polishing composition of this embodiment can be suitably used particularly for polishing a single silicon substrate.
  • polishing composition of the present embodiment will be described in detail.
  • the various operations and physical property measurements described below were performed under conditions of room temperature (20 ° C. to 25 ° C.) and relative humidity of 40% to 50% unless otherwise specified.
  • the kind of abrasive grain contained in the polishing composition of the present embodiment is not particularly limited, and any of inorganic particles, organic particles, and organic-inorganic composite particles can be used.
  • the inorganic particles include particles made of metal oxides such as silica, alumina, ceria, titania and chromium oxide, and particles made of ceramics such as silicon nitride, silicon carbide and boron nitride.
  • Specific examples of the organic particles include polymethyl methacrylate (PMMA) particles.
  • PMMA polymethyl methacrylate
  • These abrasive grains may be used alone or in combination of two or more. Among these abrasive grains, silica such as colloidal silica, fumed silica and sol-gel silica is preferable, and colloidal silica is more preferable.
  • the average primary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment may be 20 nm or more, preferably 30 nm or more, and more preferably 40 nm or more. When the average primary particle diameter of the abrasive grains is within the above range, the polishing rate of the object to be polished by the polishing composition is improved. On the other hand, the average primary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment may be 150 nm or less, preferably 100 nm or less, and more preferably 70 nm or less. If the average primary particle diameter of the abrasive grains is within the above range, it is easy to obtain a surface to be polished having a good surface roughness by polishing.
  • the average primary particle diameter of an abrasive grain can be calculated from the specific surface area measured, for example by the nitrogen adsorption method (BET method).
  • the specific surface area of the abrasive grains can be measured using, for example, “FlowSorbII 2300” manufactured by Micromeritex Corporation.
  • the content of abrasive grains in the polishing composition of the present embodiment may be 0.1% by mass or more, preferably 0.5% by mass or more, and more preferably 1% by mass or more. If content of an abrasive grain exists in said range, the grinding
  • the shape (outer shape) of the abrasive grains may be spherical or non-spherical.
  • a non-spherical shape is preferred.
  • 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.
  • the abrasive grains may have a structure in which two or more primary particles are associated.
  • the average value (average aspect ratio) of the major axis / minor axis ratio of the primary particles of the abrasive grains is not particularly limited, but is in principle 1.0 or more, preferably 1.1 or more, more preferably 1.2. That's it. Higher polishing rates can be achieved by increasing the average aspect ratio of the abrasive grains.
  • the average aspect ratio of the abrasive is preferably 4.0 or less, more preferably 3.0 or less, and further preferably 2.5 or less, from the viewpoint of reducing scratches and the like.
  • the shape (outer shape) and average aspect ratio of the abrasive grains can be grasped by, for example, observation with an electron microscope.
  • a predetermined number (for example, 200) of abrasive particles capable of recognizing the shape of independent particles using a scanning electron microscope (SEM) is used.
  • SEM scanning electron microscope
  • the value obtained by dividing the length of the long side (major axis value) by the length of the short side (minor axis value) is the major axis / minor axis ratio (aspect ratio).
  • the average aspect ratio can be obtained by arithmetically averaging the aspect ratios of the predetermined number of abrasive grains.
  • the basic compound chemically polishes the surface of an object to be polished such as a silicon substrate and chemically polishes it (chemical etching). Thereby, it becomes easy to improve the polishing rate when polishing the object to be polished.
  • the polishing composition of the present embodiment includes an alkali metal hydroxide, an alkali metal hydrogen carbonate, an alkali metal carbonate, a cyclic compound represented by the above general formula (1), and the above general formula (2). At least 1 sort (s) of the ionic compound represented and cyclic diamine compound represented by said General formula (3) contains. These basic compounds may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the type of alkali metal hydroxide is not particularly limited, and examples thereof include sodium hydroxide and potassium hydroxide.
  • the kind of alkali metal hydrogencarbonate is not specifically limited, For example, sodium hydrogencarbonate and potassium hydrogencarbonate are mention
  • the kind of alkali metal carbonate is not specifically limited, For example, sodium carbonate and potassium carbonate are mention
  • the kind of cyclic compound represented by the above general formula (1) is not particularly limited, and examples thereof include the following cyclic amine compounds.
  • X 1 and X 2 in the general formula (1) are hydrogen atoms
  • l in the general formula (1) is an integer of 1 to 6
  • m is an integer of 1 to 4.
  • n is an integer of 0 or more and 4 or less
  • m is preferably an integer of 2 or more and 4 or less
  • n is preferably an integer of 1 or more and 4 or less.
  • Specific examples of the cyclic amine compound in which X 1 and X 2 in the general formula (1) are hydrogen atoms include N-methylpiperazine, N-ethylpiperazine, N-butylpiperazine and the like.
  • l in the general formula (1) is an integer of 1 or more and 6 or less, and m is 1 or more. It is an integer of 4 or less, n is an integer of 0 or more and 4 or less, l is preferably an integer of 2 or more and 6 or less, m is preferably an integer of 2 or more and 4 or less, and n is 1 or more It is preferably an integer of 4 or less.
  • the cyclic amine compound in which X 1 in the general formula (1) is an amino group and X 2 is a hydrogen atom include aminoalkylpiperazine, and specific examples thereof include N-aminomethylpiperazine. N- (2-aminoethyl) piperazine and N- (3-aminopropyl) piperazine. Of these, N- (2-aminoethyl) piperazine is preferred.
  • examples of the cyclic amine compound in which X 1 in the general formula (1) is an amino group and X 2 is an aminoalkyl group include bisaminoalkylpiperazine, and specific examples thereof include 1,4 -Bis (2-aminoethyl) piperazine, 1,4-bis (3-aminopropyl) piperazine.
  • l in the general formula (1) is an integer of 1 to 6, and m is 1 to 4 N is an integer of 0 or more and 4 or less, l is preferably an integer of 3 or more and 6 or less, m is preferably 2 or 3, and n is an integer of 0 or more and 2 or less
  • Examples of the cyclic amine compound in which X 1 and X 2 in the general formula (1) represent a bond to the C 1 atom include 1,8-diazabicyclo [5.4.0] undec-7-ene, 1,5-diazabicyclo [4.3.0] -5-nonene.
  • the kind of ionic compound represented by the above general formula (2) is not particularly limited, and various ammonium salts and phosphonium salts are exemplified.
  • the kind of the anion (X ⁇ ) in the general formula (2) is not particularly limited, and may be an organic anion or an inorganic anion.
  • halide ions eg, F ⁇ , Cl ⁇ , Br ⁇ , I ⁇
  • hydroxide ions OH ⁇
  • tetrahydroborate ions BH 4 ⁇
  • nitrate ions nitrite ions
  • chlorate ions Chlorite ion, hypochlorite ion, perchlorite ion (ClO 4 ⁇ )
  • sulfate ion hydrogen sulfate ion, sulfite ion, thiosulfate ion, carbonate ion, phosphate ion, dihydrogen phosphate ion, Hydrogen phosphate ion, sulfamate ion, carboxylate ion (for example, formate ion, acetate ion, propionate ion, benzoate ion, glycinate ion, butyrate ion, citrate ion, tart
  • Preferred anions include OH ⁇ , F ⁇ , Cl ⁇ , Br ⁇ , I ⁇ , ClO 4 ⁇ , BH 4 ⁇ and the like.
  • hydroxide ions OH ⁇
  • hydroxide ions are more preferable.
  • R 1 , R 2 , R 3 , and R 4 in the general formula (2) are each independently an alkyl group having 1 to 4 carbon atoms, a hydroxyalkyl group having 1 to 4 carbon atoms, or a substituted group. All of R 1 , R 2 , R 3 , and R 4 may be the same as each other, part of them may be the same and the rest may be different, or all of them may be different from each other It may be.
  • Examples of the alkyl group having 1 to 4 carbon atoms include a methyl group, an ethyl group, a propyl group, and a butyl group. These alkyl groups may be linear, branched or cyclic.
  • Examples of the hydroxyalkyl group having 1 to 4 carbon atoms include a hydroxymethyl group, a hydroxyethyl group, a hydroxypropyl group, and a hydroxybutyl group. These hydroxyalkyl groups may be linear, branched or cyclic.
  • aryl group in addition to an aryl group having no substituent (for example, a phenyl group), one or more hydrogen atoms are substituted (for example, an alkyl group having 1 to 4 carbon atoms, a carbon number And aryl groups substituted with 1 to 4 hydroxyalkyl groups, hydroxy groups, halogen groups and the like.
  • an optionally substituted aryl group include a phenyl group, a benzyl group, a naphthyl group, and a naphthylmethyl group.
  • a butyl group is a concept including various structural isomers thereof (n-butyl group, isobutyl group, sec-butyl group, and tert-butyl group). The same applies to other functional groups.
  • Examples of the ionic compound represented by the general formula (2) include tetraalkylammonium salts and tetraalkylphosphonium salts in which R 1 , R 2 , R 3 , and R 4 are all alkyl groups. Specific examples thereof include tetramethylammonium salt, tetraethylammonium salt, tetrapropylammonium salt, tetrabutylammonium salt, tetramethylphosphonium salt, tetraethylphosphonium salt, tetrapropylphosphonium salt, and tetrabutylphosphonium salt.
  • tetraalkylammonium salts in which R 1 , R 2 , R 3 , and R 4 are all linear alkyl groups are preferred.
  • tetrabutylammonium salts such as tetrabutylammonium hydroxide are preferred.
  • ionic compound represented by the general formula (2) examples include tetrahydroxyalkylammonium salts in which R 1 , R 2 , R 3 , and R 4 are all hydroxyalkyl groups (for example, hydroxylated). ) And tetrahydroxyalkylphosphonium salts (for example, hydroxides). Specific examples thereof include tetrahydroxyethylammonium salt, tetrahydroxypropylammonium salt, tetrahydroxybutylammonium salt, tetrahydroxyethylphosphonium salt, tetra Examples thereof include hydroxypropyl phosphonium salt and tetrahydroxybutyl phosphonium salt.
  • tetraaryl ammonium salts for example, hydroxides
  • R 1 , R 2 , R 3 , and R 4 are all aryl groups.
  • tetraarylphosphonium salts for example, hydroxide
  • specific examples thereof include tetraphenylammonium salt, tetrabenzylammonium salt, tetraphenylphosphonium salt, and tetrabenzylphosphonium salt.
  • R 1 , R 2 , R 3 , and R 4 are a hydroxyalkyl group, and the rest is an alkyl group. Things can be given. Specific examples thereof include hydroxymethyltrimethylammonium salt, hydroxyethyltrimethylammonium salt, hydroxypropyltrimethylammonium salt, hydroxybutyltrimethylammonium salt, dihydroxyethyldimethylammonium salt, hydroxymethyltrimethylphosphonium salt, hydroxyethyltrimethylphosphonium salt, hydroxy Examples thereof include propyltrimethylphosphonium salt, hydroxybutyltrimethylphosphonium salt, and dihydroxyethyldimethylphosphonium salt.
  • R 1 , R 2 , R 3 , and R 4 are an alkyl group and the rest is an aryl group Can be given.
  • Specific examples thereof include trimethylphenylammonium salt, triethylphenylammonium salt, benzyltrimethylammonium salt, methyltriphenylammonium salt, tribenzylmethylammonium salt, trimethylphenylphosphonium salt, triethylphenylphosphonium salt, benzyltrimethylphosphonium salt, methyl Examples thereof include triphenylphosphonium salt and tribenzylmethylphosphonium salt.
  • R 1 , R 2 , R 3 , and R 4 are a hydroxyalkyl group, and the rest is an aryl group. Things can be raised. Specific examples thereof include hydroxymethyltriphenylammonium salt, tribenzylhydroxymethylammonium salt, hydroxymethyltriphenylphosphonium salt, and tribenzylhydroxymethylphosphonium salt.
  • R ⁇ 5 >, R ⁇ 6 >, R ⁇ 7 >, R ⁇ 8> , R ⁇ 9 >, and R ⁇ 10 > are hydrogen atoms. The thing which is.
  • one of R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 has 4 or less carbon atoms (preferably A structure of 1 to 3 (typically 1 or 2) alkyl group and the other 5 are hydrogen atoms, two of R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 are A structure in which an alkyl group having 4 or less carbon atoms and the other four are hydrogen atoms, three of R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 are alkyl groups having 4 or less carbon atoms And the other three are hydrogen atoms, four of R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 are alkyl groups having 4 or less carbon atoms, and the other two are hydrogen atoms And five of the structures R 5 , R 6 , R 7 , R 8 , R 9 , and R 10 has 4 or less carbon atoms (preferably A structure of 1 to 3
  • cyclic diamine compound represented by the general formula (3) examples include 2-methyl-1,4-diazabicyclo [2.2.2] octane, 2-ethyl-1,4-diazabicyclo [2. 2.2] octane, 2-propyl-1,4-diazabicyclo [2.2.2] octane, 2-butyl-1,4-diazabicyclo [2.2.2] octane, 2,5-dimethyl-1, 4-diazabicyclo [2.2.2] octane, 2,5-diethyl-1,4-diazabicyclo [2.2.2] octane, 2,5-dipropyl-1,4-diazabicyclo [2.2.2] Examples include octane, 2,5-dibutyl-1,4-diazabicyclo [2.2.2] octane, and 2-methyl-5-ethyl-1,4-diazabicyclo [2.2.2]
  • amines can contain ammonia, amines and the like.
  • amines include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N- ( ⁇ -aminoethyl) ethanolamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, anhydrous piperazine , Piperazine hexahydrate, guanidine, azoles such as imidazole and triazole, and the like.
  • These basic compounds may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the content of the basic compound in the polishing composition of the present embodiment may be 0.001% by mass or more, preferably 0.01% by mass or more, and more preferably 0.05% by mass or more. If content of a basic compound exists in said range, the grinding
  • the polishing composition of this embodiment contains at least one of the multiple bond-containing compound represented by the general formula (4) and the anionic group-containing compound represented by the general formula (5). To do. This makes it easy to improve the polishing rate while maintaining good surface roughness of the surface to be polished of the object to be polished.
  • the acid dissociation constant pKa of the multiple bond-containing compound and the anionic group-containing compound is preferably 2 or more and 7 or less. If the acid dissociation constant pKa is within this numerical range, the nucleophilicity with respect to the object to be polished works more efficiently, so that the above effect becomes better. When the multiple bond-containing compound and the anionic group-containing compound dissociate in multiple stages, it is sufficient that at least one acid dissociation constant pKa is within the above numerical range.
  • the type of the multiple bond-containing compound contained in the polishing composition of the present embodiment is not particularly limited as long as it is a compound represented by the general formula (4).
  • Z is preferably a functional group having a carbon-carbon double bond, a carbon-oxygen double bond, a nitrogen-oxygen double bond, a sulfur-oxygen double bond, or a phosphorus-oxygen double bond.
  • a functional group having a group, carboxy group, carbonyl group, acyl group, ester group, nitro group, sulfo group, phosphono group, or amino group is more preferable.
  • Y and Z are preferably a phenyl group, a carboxy group, a carbonyl group, and an acyl group, and more preferably a carboxy group and a carbonyl group.
  • Y or Z in the general formula (4) is also preferably a functional group having a carbon-nitrogen triple bond, for example, a functional group having a cyano group.
  • the multiple bond-containing compound represented by the general formula (4) can have a functional group such as an amino group.
  • the multiple bond-containing compound represented by the general formula (4) include dicarboxylic acids such as malonic acid, oxalic acid, malic acid, methacrylic acid, and cyanoacetic acid. Among these, malon Acid is more preferred. Since dicarboxylic acid has two carboxy groups, it has a high nucleophilicity with respect to a polishing object such as a silicon substrate.
  • dicarboxylic acid has two carboxy groups, it has a high nucleophilicity with respect to a polishing object such as a silicon substrate.
  • One of these multiple bond-containing compounds represented by the general formula (4) may be used alone, or two or more thereof may be used in combination.
  • the kind of anionic group containing compound which the polishing composition of this embodiment contains will not be specifically limited if it is a cyclic compound represented by General formula (5).
  • the cyclic moiety in the general formula (5) is a carbon six-membered ring, and the carbon-carbon bond is a single bond or a double bond, the cyclic moiety in the general formula (5) may be, for example, a cyclohexane ring.
  • a benzene ring may be used, but a benzene ring is preferable.
  • Q in the general formula (5) is preferably a carboxy group or a salt thereof, a sulfonic acid group or a salt thereof, a phosphonic acid group or a salt thereof, or a hydroxy group or a salt thereof, and more preferably a carboxy group. .
  • anionic group-containing compound represented by the general formula (5) examples include benzoic acid (the cyclic portion in the general formula (5) is a benzene ring, Q is a carboxy group, and X 3 , X 4 , X 5 , X 6 , and X 7 are all hydrogen), benzenedicarboxylic acid (the cyclic part in the general formula (5) is a benzene ring, Q is a carboxy group, X 3 , A compound in which any one of X 4 , X 5 , X 6 , and X 7 is a carboxy group and the remainder is all hydrogen, trimellitic acid (the cyclic portion in the general formula (5) is a benzene ring, A compound in which Q, X 3 , and X 5 are carboxy groups, and X 4 , X 6 , and X 7 are hydrogen), hydroxybenzoic acid (the cyclic moiety in the general formula (5) is a benzene ring,
  • the total content of the multiple bond-containing compound and the anionic group-containing compound in the polishing composition of the present embodiment may be 0.005% by mass or more, preferably 0.05% by mass or more, more preferably It is 0.1 mass% or more.
  • the polishing rate of the object to be polished by the polishing composition is improved.
  • the total content of the multiple bond-containing compound and the anionic group-containing compound in the polishing composition may be 5% by mass or less, preferably 2% by mass or less, more preferably 0.6% by mass or less. It is.
  • the production cost of the polishing composition is reduced.
  • the pH of the polishing composition of the present embodiment is not particularly limited, but may be 9.0 or more and 11.5 or less, and more preferably 10.0 or more and 10.8 or less. When the pH is within the above range, the polishing rate becomes higher.
  • a water-soluble polymer (a copolymer may be used, or a salt or derivative thereof), a surfactant, a chelate may be used as necessary.
  • Various additives such as agents and fungicides may be added. However, it is preferable that the oxidizing agent is not substantially contained.
  • a water-soluble polymer (which may be a copolymer, or a salt or derivative thereof) that acts on the surface of the object to be polished or the surface of the abrasive grains is added. Also good.
  • water-soluble polymers, water-soluble copolymers, and salts or derivatives thereof include polycarboxylic acids such as polyacrylates and polysulfonic acids such as polyphosphonic acids and polystyrene sulfonic acids.
  • Other specific examples include polysaccharides such as chitansan gum and sodium alginate, and cellulose derivatives such as hydroxyethylcellulose and carboxymethylcellulose.
  • water-soluble polymers having a pyrrolidone unit for example, polyvinylpyrrolidone, polyvinylpyrrolidone polyacrylic acid copolymer, polyvinylpyrrolidone vinyl acetate copolymer), polyethylene glycol, polyvinyl alcohol, sorbitan monooleate And oxyalkylene polymers having a single kind or plural kinds of oxyalkylene units.
  • water-soluble polymers having pyrrolidone units are preferable, and polyvinyl pyrrolidone is more preferable.
  • These water-soluble polymers may be used alone or in combination of two or more.
  • a surfactant may be added to the polishing composition of the present embodiment.
  • the surfactant include an anionic or nonionic surfactant.
  • nonionic surfactants are preferably used.
  • nonionic surfactants include oxyalkylene homopolymers, multiple types of oxyalkylene copolymers, and polyoxyalkylene adducts.
  • nonionic surfactants it is preferable to use a plurality of types of oxyalkylene copolymers or polyoxyalkylene adducts.
  • chelating agent A chelating agent may be added to the polishing composition of the present embodiment.
  • the chelating agent suppresses metal contamination of the silicon substrate by capturing metal impurity components in the polishing system to form a complex.
  • Specific examples of chelating agents include carboxylic acid chelating agents such as gluconic acid, amine chelating agents such as ethylenediamine, diethylenetriamine, and trimethyltetraamine, ethylenediaminetetraacetic acid, nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetramine hexa Polyaminopolycarboxylic acid chelating agents such as acetic acid and diethylenetriaminepentaacetic acid, 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetrakis (methylenephosphonic acid), diethylenetriamine Penta
  • organic phosphonic acid chelating agents particularly ethylenediaminetetrakis (methylenephosphonic acid).
  • chelating agents may be used individually by 1 type, and may be used in combination of 2 or more type.
  • An antifungal agent may be added to the polishing composition of the present embodiment.
  • Specific examples of the antifungal agent include oxazolines such as oxazolidine-2,5-dione.
  • the polishing composition disclosed here contains substantially no oxidizing agent.
  • an oxidizing agent is contained in the polishing composition, the polishing composition is supplied to a polishing object (for example, a silicon wafer) so that the surface of the polishing object is oxidized to produce an oxide film, This is because the required polishing time becomes long.
  • the oxidizing agent include hydrogen peroxide (H 2 O 2 ), sodium persulfate, ammonium persulfate, potassium permanganate, sodium dichloroisocyanurate, and the like.
  • that polishing composition does not contain an oxidizing agent substantially means not containing an oxidizing agent at least intentionally.
  • a trace amount for example, the molar concentration of the oxidant in the polishing composition is 0.0005 mol / L or less, preferably 0.0001 mol or less, more preferably 0.00001 mol /
  • Water serves as a dispersion medium or solvent for dispersing or dissolving other components (abrasive grains, basic compound, multiple bond-containing compound, anionic group-containing compound, additive, etc.) of the polishing composition.
  • water having a total content of transition metal ions of 100 ppb or less, for example.
  • the purity of water can be increased by operations such as removal of impurity ions using an ion exchange resin, removal of particles by a filter, and distillation.
  • ion exchange water pure water, ultrapure water, distilled water or the like.
  • the method for producing the polishing composition of the present embodiment is not particularly limited, and includes abrasive grains, a basic compound, at least one of a multiple bond-containing compound and an anionic group-containing compound, and various types as desired.
  • the additive can be produced by stirring and mixing in a liquid medium such as water.
  • the temperature at the time of mixing is not specifically limited, 10 to 40 degreeC is preferable and you may heat in order to improve a dissolution rate. Further, the mixing time is not particularly limited.
  • Polishing of an object to be polished using the polishing composition of the present embodiment can be performed by a polishing apparatus and polishing conditions used for normal polishing.
  • a polishing apparatus and polishing conditions used for normal polishing For example, a single-side polishing apparatus or a double-side polishing apparatus can be used.
  • a polishing target is a silicon substrate and polishing is performed using a single-side polishing apparatus
  • the silicon substrate is held using a holder called a carrier, and a surface plate with a polishing cloth is attached to one side of the silicon substrate.
  • One surface of the silicon substrate is polished by rotating the surface plate while pressing and supplying the polishing composition.
  • the silicon substrate is held using a holder called a carrier, and a surface plate to which a polishing cloth is attached is applied from both sides of the silicon substrate to both sides of the silicon substrate. Both sides of the silicon substrate are polished by rotating the surface plates on both sides while pressing each other and supplying the polishing composition.
  • the silicon substrate is polished by the physical action caused by friction (friction between the polishing cloth and the polishing composition and the silicon substrate) and the chemical action that the polishing composition brings to the silicon substrate. Is done.
  • polishing cloth various materials such as polyurethane, non-woven fabric, and suede can be used. In addition to the difference in materials, materials having various physical properties such as hardness and thickness can be used. Furthermore, both those containing abrasive grains and those not containing abrasive grains can be used. Further, those having a hole-like structure in which a liquid polishing composition is accumulated, and those having a groove processing to serve as a flow path for the liquid polishing composition can be used.
  • the polishing load (pressure applied to the object to be polished) among the polishing conditions is not particularly limited, but may be 5 kPa or more and 50 kPa or less, preferably 8 kPa or more and 40 kPa or less, more preferably 10 kPa or more and 30 kPa or less.
  • the polishing load is within this range, a sufficient polishing rate is exhibited, and it is possible to suppress the polishing object from being damaged by the load or the occurrence of defects such as scratches on the surface of the polishing object. .
  • the relative speed (linear speed) between the polishing cloth used for polishing and the polishing target such as a silicon substrate is not particularly limited, but may be 10 m / min or more and 300 m / min or less, preferably 30 m. / Min to 200 m / min. If the relative speed between the polishing cloth and the object to be polished is within this range, a sufficient polishing speed can be obtained. Further, the polishing cloth can be prevented from being damaged by the friction of the object to be polished, and the friction is sufficiently transmitted to the object to be polished, so that the so-called state of slipping of the object to be polished can be suppressed and the object can be sufficiently polished.
  • the supply amount of the polishing composition among the polishing conditions varies depending on the type of the polishing object, the type of the polishing apparatus, and the polishing conditions, but the polishing composition is uneven between the polishing object and the polishing cloth. It is sufficient that the amount is sufficient to be supplied to the entire surface.
  • the polishing composition may not be supplied to the entire polishing object, or the polishing composition may dry and solidify to cause defects on the surface of the polishing object.
  • the supply amount of the polishing composition is large, it is not economical, and there is a possibility that friction is hindered by an excessive polishing composition (particularly a liquid medium such as water) and the polishing is hindered.
  • polishing such as mirror surface finishing. If there are processing damage or scratches on the surface of the object to be polished, it will be uneconomical because it takes a lot of time to mirror these scratches in one polishing process. There is a possibility that the smoothness of the surface of the glass may be impaired.
  • the polishing time required in the final polishing step can be shortened, and an excellent mirror surface can be obtained efficiently.
  • the preliminary polishing composition used in the preliminary polishing step it is preferable to use a composition having a higher polishing power than the final polishing composition used in the final polishing step.
  • the polishing composition of the present embodiment can be used in both the preliminary polishing step and the final polishing step, but is more suitable as a preliminary polishing composition.
  • the polishing composition of the present embodiment can be recovered after being used for polishing the polishing object and reused for polishing the polishing object.
  • the method of reusing the polishing composition there is a method in which the polishing composition discharged from the polishing apparatus is collected in a tank and is circulated again into the polishing apparatus to be used for polishing. If the polishing composition is circulated, the amount of the polishing composition discharged as a waste liquid can be reduced, so that the environmental load can be reduced. Moreover, since the quantity of the polishing composition to be used can be reduced, the manufacturing cost required for grinding
  • one of the abrasive grains, basic compounds, multiple bond-containing compounds, anionic group-containing compounds, additives, etc. consumed and lost due to use in polishing. It is good to reuse after adding a part or all as a composition regulator.
  • a composition regulator what mixed abrasive grain, a basic compound, a multiple bond containing compound, an anionic group containing compound, an additive, etc. by arbitrary mixing ratios can be used.
  • the polishing composition is adjusted to a composition suitable for reuse and suitable polishing can be performed. Concentrations of abrasive grains, basic compounds, multiple bond-containing compounds, anionic group-containing compounds, and other additives contained in the composition modifier are arbitrary and are not particularly limited, depending on the tank size and polishing conditions May be adjusted accordingly.
  • the polishing composition of the present embodiment may be a one-component type or a multi-component type such as a two-component type in which some or all of the components of the polishing composition are mixed at an arbitrary ratio. May be.
  • polishing may be performed using the composition of the polishing composition of this embodiment prepared as it is, but a concentrated liquid (for example, 10 times or more) of the polishing composition is used. You may grind
  • Example ⁇ Examples will be shown below, and the present invention will be described more specifically with reference to Table 1.
  • Abrasive grains made of colloidal silica, a basic compound, a multiple bond-containing compound or an anionic group-containing compound, and water as a liquid medium are mixed so as to have the contents shown in Table 1,
  • the polishing compositions of Examples 1 to 28 and Comparative Examples 1 to 7 were prepared by dispersing the grains in water and further mixing potassium hydroxide to adjust the pH to 10.5.
  • the water-soluble polymer polyvinyl pyrrolidone (Pitzkol K-50 manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) as an additive has a content as shown in Table 1. Added to. In Table 1, polyvinyl pyrrolidone is indicated as “PVP”. Moreover, the multiple bond containing compound and the anionic group containing compound are not added to the polishing composition of Comparative Example 2. Further, in the polishing compositions of Comparative Examples 3 to 6, the multiple bond-containing compound and the anionic group-containing compound are not added, and the “other components” shown in Table 1 have the contents shown in Table 1. Was added as follows. Furthermore, the basic compound and potassium hydroxide for pH adjustment are not added to the polishing composition of Comparative Example 7.
  • AEP means N- (2-aminoethyl) piperazine
  • BAPP means 1,4-bis (3-aminopropyl) piperazine
  • TMAH means tetramethylammonium hydroxide
  • TBAH means tetrabutylammonium hydroxide
  • DABCO means 1,4-diazabicyclo [2.2.2] octane.
  • the average primary particle diameters of the colloidal silica used as the abrasive grains are as shown in Table 1. This average primary particle diameter is calculated from the specific surface area of the abrasive grains measured by the BET method and the density of the abrasive grains.
  • a silicon wafer was polished under the following polishing conditions.
  • the conductivity type of this silicon wafer is P-type, the crystal orientation is ⁇ 100>, and the resistivity is not less than 0.1 ⁇ ⁇ cm and less than 100 ⁇ ⁇ cm.
  • the silicon wafer is cut out in a rectangular plate shape, and the dimensions are 60 mm in length and 60 mm in width.
  • Polishing device Single-side polishing device manufactured by Nippon Engis Co., Ltd. Model “EJ-380IN” Polishing pad (polishing cloth): “MH S-15A” manufactured by Nitta Haas Co., Ltd. Polishing load: 26.7 kPa Surface plate rotation speed: 50 min -1 Head rotation speed: 40 min -1 Polishing time: 10 min Supply rate of polishing composition: 100 mL / min (circulation use) Polishing composition temperature: 25 ° C.
  • the surface roughness Ra of the surface to be polished after polishing was measured.
  • the results are shown in Table 1.
  • the surface roughness Ra was measured using a non-contact surface shape measuring instrument (trade name “NewView 5032” manufactured by Zygo) under the conditions of a magnification of 10 times and a measurement area of 700 ⁇ m ⁇ 500 ⁇ m.
  • the polishing compositions of Examples 1 to 28 had a high polishing rate and excellent surface roughness of the surface to be polished.
  • the polishing composition of Comparative Example 1 since the basic compound is not a compound represented by the general formula (1), the surface roughness of the polished surface was poor although the polishing rate of the silicon wafer was high. . Moreover, since the polishing composition of Comparative Example 2 does not contain a multiple bond-containing compound and an anionic group-containing compound, although the surface roughness of the polished surface is excellent, the polishing rate of the silicon wafer is insufficient. there were. Further, in the polishing compositions of Comparative Examples 3 to 6, since the multiple bond-containing compound is not a compound represented by the general formula (4), the surface roughness of the surface to be polished is excellent, but the polishing rate of the silicon wafer Was insufficient. Furthermore, since the polishing composition of Comparative Example 7 did not contain a basic compound, the polishing rate of the silicon wafer was insufficient and the surface roughness of the surface to be polished was poor.

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

Abstract

L'invention concerne une composition pour meulage, qui permet d'obtenir à la fois une excellente qualité de surface et une vitesse de meulage élevée, et un procédé pour le meulage d'un substrat en silicium. La composition pour meulage contient des grains abrasifs, un composé basique et un composé contenant une liaison multiple et/ou un composé contenant un groupe anionique. Le composé basique contient au moins un composé choisi parmi un hydroxyde de métal alcalin, un bicarbonate de métal alcalin, un carbonate de métal alcalin, un composé cyclique, un composé ionique et un composé de diamine cyclique.
PCT/JP2016/001226 2015-03-11 2016-03-07 Composition pour meulage et procédé pour le meulage d'un substrat en silicium Ceased WO2016143323A1 (fr)

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JP7015663B2 (ja) 2017-09-21 2022-02-03 株式会社フジミインコーポレーテッド 研磨用組成物及びその製造方法並びに研磨方法
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CN113388328A (zh) * 2020-03-13 2021-09-14 福吉米株式会社 研磨用组合物、研磨用组合物的制造方法、研磨方法及半导体基板的制造方法
WO2022074831A1 (fr) * 2020-10-09 2022-04-14 花王株式会社 Composition de solution de polissage pour substrat de silicium
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JPWO2022074831A1 (fr) * 2020-10-09 2022-04-14
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JP7599502B2 (ja) 2020-10-09 2024-12-13 花王株式会社 シリコン基板用研磨液組成物
KR102756908B1 (ko) 2020-10-09 2025-01-21 카오카부시키가이샤 실리콘 기판용 연마액 조성물
WO2022074835A1 (fr) * 2020-10-09 2022-04-14 花王株式会社 Procédé de polissage de substrat de silicium
JP2022169478A (ja) * 2021-04-27 2022-11-09 ローム アンド ハース エレクトロニック マテリアルズ シーエムピー ホウルディングス インコーポレイテッド 研磨組成物及び向上した欠陥低減を有する基材を研磨する方法

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