WO2017204035A1 - 研磨液、研磨液の製造方法、研磨液原液、及び化学的機械的研磨方法 - Google Patents

研磨液、研磨液の製造方法、研磨液原液、及び化学的機械的研磨方法 Download PDF

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Publication number
WO2017204035A1
WO2017204035A1 PCT/JP2017/018353 JP2017018353W WO2017204035A1 WO 2017204035 A1 WO2017204035 A1 WO 2017204035A1 JP 2017018353 W JP2017018353 W JP 2017018353W WO 2017204035 A1 WO2017204035 A1 WO 2017204035A1
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Prior art keywords
polishing liquid
polishing
mass
group
oxidizing agent
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PCT/JP2017/018353
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English (en)
French (fr)
Japanese (ja)
Inventor
上村　哲也
Original Assignee
富士フイルム株式会社
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Application filed by 富士フイルム株式会社 filed Critical 富士フイルム株式会社
Priority to KR1020187033226A priority Critical patent/KR20180132893A/ko
Priority to KR1020227032177A priority patent/KR102609113B1/ko
Priority to JP2018519205A priority patent/JP6876687B2/ja
Priority to KR1020217024029A priority patent/KR20210097826A/ko
Publication of WO2017204035A1 publication Critical patent/WO2017204035A1/ja

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09G—POLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00—Polishing compositions
    • C09G1/02—Polishing compositions containing abrasives or grinding agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • 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
    • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to a polishing liquid, a manufacturing method of the polishing liquid, a polishing liquid stock solution, and a chemical mechanical polishing method.
  • CMP chemical mechanical polishing
  • a polishing liquid used in CMP for example, Patent Document 1 describes “a polishing liquid in which a reaction layer having a thickness of 100 nm or more is formed on a surface to be polished that has been in contact with the polishing liquid for 24 hours”. Has been.
  • the present inventor examined the polishing liquid described in Patent Document 1 and found that when colloidal silica was blended, there was a problem that dishing was likely to occur on the surface to be polished of the object to be polished.
  • an object of the present invention is to provide a polishing liquid that can obtain an excellent polishing rate and is less likely to cause dishing on a surface to be polished when applied to CMP.
  • Another object of the present invention is to provide a polishing liquid production method, a polishing liquid stock solution, and a chemical mechanical polishing method.
  • the present inventors have solved the above-mentioned problems with a polishing liquid that contains a predetermined component and can form a reaction layer having a predetermined thickness when brought into contact with a copper substrate.
  • the present invention has been completed. That is, it has been found that the above-described problem can be achieved by the following configuration.
  • a polishing liquid for chemical mechanical polishing containing colloidal silica, an amino acid, two or more azole compounds, and an oxidizing agent, wherein the polishing liquid and a copper substrate are brought into contact with each other for 24 hours.
  • the content of the oxidizing agent is 0.3 to 2.0% by mass with respect to the total mass of the polishing liquid.
  • the organic solvent is further contained, and the content of the organic solvent is 0.01 to 2.0% with respect to the total mass of the polishing liquid, according to any one of [1] to [7] Polishing liquid.
  • a polishing solution stock solution containing colloidal silica, an amino acid, and two or more azole compounds is mixed with an oxidizing agent or an oxidizing agent and water, and any one of [1] to [11]
  • Oxidizing agent or oxidizing agent and water are mixed with the polishing liquid stock so that the dilution step has an oxidizing agent content of 0.3 to 2.0% by mass with respect to the total mass of the polishing liquid.
  • the manufacturing method of polishing liquid as described in [12] which is a process to perform.
  • a chemical mechanical polishing method comprising a step of relatively moving a body and a polishing pad to polish a surface to be polished to obtain a polished body to be polished.
  • the chemical mechanical polishing method according to [15], wherein the object to be polished contains at least one metal layer selected from the group consisting of copper and a copper alloy.
  • an excellent polishing rate when applied to CMP, an excellent polishing rate can be obtained, and dishing is less likely to occur on the surface to be polished (hereinafter also referred to as “having the effect of the present invention”). Can be provided.
  • a numerical range expressed using “to” means a range including numerical values described before and after “to” as a lower limit value and an upper limit value.
  • a polishing liquid according to an embodiment of the present invention is a polishing liquid for chemical mechanical polishing containing colloidal silica, an amino acid, two or more azole compounds, and an oxidizing agent, and the polishing liquid
  • colloidal silica colloidal silica
  • amino acid amino acid
  • two or more azole compounds two or more azole compounds
  • an oxidizing agent an oxidizing agent
  • the reaction layer is obtained by immersing a copper substrate having a 10 mm ⁇ 10 mm surface to be polished in 10 mL of polishing liquid and bringing the copper substrate and the polishing liquid into contact at 25 ° C. for 24 hours.
  • a reaction layer formed on the surface to be polished is intended.
  • substrate for example, silicon substrate
  • the reaction layer has a thickness of 1 nm or more, preferably 2 nm or more.
  • the thickness of the reaction layer is 20 nm or less, preferably 15 nm or less, and more preferably 10 nm or less. If the thickness of the reaction layer is less than 1 nm, it is difficult to obtain a sufficient polishing rate. On the other hand, if the thickness of the reaction layer exceeds 20 nm, dishing is likely to occur on the surface of the polished surface.
  • the polishing liquid contains colloidal silica in order to improve the polishing rate. Colloidal silica comes into contact with the reaction layer during CMP and scrapes off the reaction layer.
  • the reaction layer contains a copper atom.
  • the reaction layer may further contain oxygen atoms and the like, and it is preferable that the surface of the reaction layer contains a complex of components in the polishing liquid.
  • the thickness of the reaction layer is determined by bringing the polishing liquid and the copper substrate into contact with each other for 24 hours, and then using a scanning electron microscope (SEM) to obtain a cross section of the copper substrate after the contact. The thickness obtained by observation by the described method is intended.
  • the pH of the polishing liquid is not particularly limited, but is usually 1.0 to 14.0. Of these, 5.0 to 8.0 is more preferable, and 6.0 to 7.5 is even more preferable.
  • the pH is in the range of 5.0 to 8.0, the occurrence of dishing is further suppressed when the polishing liquid is applied to CMP.
  • the pH is 5.0 or more, a polishing liquid having better colloidal silica dispersion stability can be obtained. Since the isoelectric point of the zeta potential on the surface of colloidal silica is around pH 4.0, if the pH of the polishing liquid is adjusted within the above range larger than the isoelectric point, a polishing liquid having better dispersion stability can be obtained. can get.
  • the pH is 8.0 or less, it is easy to adjust the thickness of the reaction layer under a predetermined condition to a desired range.
  • the polishing liquid contains colloidal silica as an essential component. Colloidal silica has the effect of scraping off the reaction layer formed in the object to be polished.
  • the polishing liquid contains colloidal silica, and the thickness of the reaction layer formed under predetermined conditions is estimated to be 1 to 20 nm, which is presumed to be one of the reasons for the effects of the present invention.
  • the average primary particle diameter of the colloidal silica is not particularly limited, but is preferably 1 to 100 nm in that the polishing liquid has more excellent dispersion stability.
  • the average primary particle size can be confirmed by a manufacturer's catalog or the like.
  • Examples of commercially available colloidal silica include PL-1, PL-3, PL-7, and PL-10H (all are trade names, manufactured by Fuso Chemical Industry Co., Ltd.).
  • the content of colloidal silica is not particularly limited, and the lower limit is preferably 0.01% by mass or more, more preferably 0.05% by mass or more, and 0.05% by mass with respect to the total mass of the polishing liquid. It is more preferable to exceed.
  • the upper limit is preferably 10% by mass or less, more preferably 5% by mass or less, still more preferably 0.2% by mass or less, and 0.2% by mass in that dishing hardly occurs when the polishing liquid is applied to CMP. Less than% is particularly preferred.
  • colloidal silica may be used individually by 1 type, or may use 2 or more types together. When using 2 or more types of colloidal silica together, it is preferable that total content is in the said range.
  • the polishing liquid contains an amino acid.
  • the amino acid is a compound different from the oxidizing agent, and has an action of promoting oxidation of the metal, adjusting the pH of the polishing liquid, and a buffering agent.
  • amino acids include glycine, ⁇ -alanine, ⁇ -alanine, N-methylglycine, L-2-aminobutyric acid, L-norvaline, L-valine, L-leucine or derivatives thereof, L-proline, L-ornithine , L-lysine, taurine, L-serine, L-threonine, L-allothreonine, L-homoserine, L-tyrosine, L-thyroxine, 4-hydroxy-L-proline, L-cystine, L-methionine, L- Ethionine, L-cystine or a derivative thereof, L-cystine acid, L-aspartic acid, L-glutamic acid, 4-aminobutyric acid, L-asparagine, L-glutamine, azaserine, L-arginine, L-can
  • glycine, ⁇ -alanine, ⁇ -alanine, L-aspartic acid, or N-methylglycine is preferable as the amino acid in that the polishing liquid has the superior effect of the present invention.
  • / or methylglycine is more preferred.
  • an amino acid may be used individually by 1 type, or may use 2 or more types together.
  • polishing liquid contains a 2 or more types of amino acid at the point from which the polishing liquid which has the effect of this invention more excellent is obtained.
  • the two or more amino acids are not particularly limited, and the above amino acids can be used in combination.
  • the combination of glycine and alanine, alanine and N-methylglycine, or glycine and N-methylglycine is preferable as the two or more amino acids in that a polishing liquid having a better effect of the present invention can be obtained.
  • the polishing liquid contains an amino acid having high reactivity with the copper substrate, it is estimated that the reaction layer can be formed efficiently. Therefore, compared with a polishing liquid that does not contain amino acids (for example, a polishing liquid that contains only other organic acids), the polishing liquid can obtain an excellent polishing rate even if the reaction layer is thin. Presumed to be.
  • the amino acid content is not particularly limited and is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, still more preferably 1.0% by mass or more, based on the total mass of the polishing liquid. % By mass or less is preferable, 25% by mass or less is more preferable, 20% by mass or less is further preferable, and 10% by mass or less is particularly preferable.
  • % By mass or less is preferable, 25% by mass or less is more preferable, 20% by mass or less is further preferable, and 10% by mass or less is particularly preferable.
  • the content of the amino acid is 0.1% by mass or more, a better polishing rate can be obtained when the polishing liquid is applied to CMP. If the amino acid content is 50% by mass or less, dishing is less likely to occur on the surface to be polished when the polishing liquid is applied to CMP.
  • an amino acid may be used individually by 1 type, or may use 2 or more types together.
  • the total content is preferably within the above range.
  • the polishing liquid contains two or more azole compounds.
  • An azole compound has the effect
  • the azole compound means a compound containing a hetero five-membered ring containing one or more nitrogen atoms, and the number of nitrogen atoms is preferably 1 to 4.
  • the azole compound may contain atoms other than nitrogen atoms as heteroatoms.
  • guide_body intends the compound which has the substituent which the said heterocyclic 5-membered ring can contain.
  • the azole compound examples include pyrrole skeleton, imidazole skeleton, pyrazole skeleton, isothiazole skeleton, isoxazole skeleton, triazole skeleton, tetrazole skeleton, imidazole skeleton, thiazole skeleton, oxazole skeleton, isoxazole skeleton, thiadiazole skeleton, and oxadiazole. Examples thereof include compounds having a skeleton and a tetrazole skeleton.
  • the azole compound may be an azole compound containing a polycyclic structure containing a condensed ring in the skeleton.
  • Examples of the azole compound containing a polycyclic structure include compounds containing an indole skeleton, a purine skeleton, an indazole skeleton, a benzimidazole skeleton, a carbazole skeleton, a benzoxazole skeleton, a benzothiazole skeleton, a benzothiadiazole skeleton, and a naphthimidazole skeleton. Is mentioned.
  • the substituent that the azole compound may contain is not particularly limited, and examples thereof include a halogen atom (a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom), an alkyl group (a linear, branched, or cyclic alkyl group, A polycyclic alkyl group such as an alkyl group or an active methine group may be included), an alkenyl group, an alkynyl group, an aryl group, a heterocyclic group (regarding the position of substitution), an acyl group, an alkoxycarbonyl group , Aryloxycarbonyl group, heterocyclic oxycarbonyl group, carbamoyl group (Examples of the carbamoyl group having a substituent include N-hydroxycarbamoyl group, N-acylcarbamoyl group, N-sulfonylcarbamoyl group, N-carbamoylcarbamoyl
  • a halogen atom (a fluorine atom, a chlorine atom, a bromine atom, or an iodine atom
  • an alkyl group (a linear, branched or cyclic alkyl group, even a polycyclic alkyl group such as a bicycloalkyl group, An active methine group may be included), an alkenyl group, an alkynyl group, an aryl group, or a heterocyclic group (regarding the position of substitution).
  • active methine group means a methine group substituted with two electron-attracting groups.
  • the “electron withdrawing group” is, for example, an acyl group, an alkoxycarbonyl group, an aryloxycarbonyl group, a carbamoyl group, an alkylsulfonyl group, an arylsulfonyl group, a sulfamoyl group, a trifluoromethyl group, a cyano group, a nitro group, or A carbonimidoyl group is intended.
  • Two electron-withdrawing groups may be bonded to each other to form a cyclic structure.
  • the term “salt” is intended to include cations such as alkali metals, alkaline earth metals, and heavy metals; organic cations such as ammonium ions and phosphonium ions.
  • azole compound examples include 5-methylbenzotriazole, 5-aminobenzotriazole, benzotriazole, 5,6-dimethylbenzoatriazole, 3-amino-1,2,4-triazole, 1,2, Examples include 4-triazole, 3,5-dimethylpyrazole, pyrazole, and imidazole.
  • a benzotriazole compound compound containing a benzotriazole skeleton
  • a compound different from the benzotriazole compound benzotriazole
  • a polishing liquid having a better effect of the present invention can be obtained.
  • a compound not containing a skeleton A compound containing a benzotriazole skeleton strongly coordinates to copper oxidized by an oxidizing agent and easily forms a reaction layer.
  • the compound which does not contain a benzotriazole skeleton is coordinated relatively weakly to oxidized copper and is likely to form a reaction layer.
  • a reaction layer formed when a polishing liquid containing a benzotriazole compound and a compound different from benzotriazole is applied to CMP is formed of a layer formed of the benzotriazole compound and a compound different from benzotriazole. It is estimated that the layer to be contained. It is presumed that the layer formed of the benzotriazole compound that coordinates strongly with oxidized copper is dense and has a function of further suppressing the occurrence of dishing. On the other hand, a layer formed of a compound different from the benzotriazole compound weakly coordinated by oxidized copper is more easily removed, and as a result, it is presumed that a better polishing rate is easily obtained. Therefore, when the polishing liquid containing the two or more azole compounds is applied to CMP, a higher polishing rate can be obtained, and dishing is less likely to occur on the polished surface.
  • the compound that does not contain the benzotriazole skeleton is not particularly limited, but includes a 1,2,4-triazole compound, a pyrazole compound, and an imidazole compound in that a polishing liquid having a better effect of the present invention can be obtained. It is preferably at least one selected from the group.
  • the content of each of the two or more azole compounds is not particularly limited, but is 0.0001 to each of the total mass of the polishing liquid in that a polishing liquid having a better effect of the present invention can be obtained. 2 mass% is preferable, 0.0005 to 2 mass% is more preferable, and 0.001 to 2 mass% is still more preferable.
  • the mass ratio of the contents of the other azole compounds to the azole compound having the smallest content in the polishing liquid is 1. It is preferably greater than 0 (hereinafter referred to as “over 1.0”), more preferably over 10, more preferably over 150, preferably 1000 or less, and more preferably 500 or less.
  • the azole compound having the smallest content in the polishing liquid is intended to have the least content of two or more azole compounds, and a plurality of azole compounds among the two or more azole compounds are included in this. May be applicable.
  • an azole compound may use 3 or more types together. When using 3 or more types of azole compounds together, it is preferable that content of each azole compound is in the said range, respectively.
  • the polishing liquid contains an oxidizing agent.
  • the oxidizing agent has a function of oxidizing a metal to be polished existing on the surface to be polished of the object to be polished. It does not restrict
  • the oxidizing agent include hydrogen peroxide, peroxide, nitric acid, nitrate, iodate, periodate, hypochlorite, chlorite, chlorate, perchlorate, and persulfate. Examples thereof include salts, dichromates, permanganates, ozone water, silver (II) salts, and iron (III) salts. Of these, hydrogen peroxide is preferable.
  • an oxidizing agent may be used individually by 1 type, or may use 2 or more types together. When using 2 or more types of oxidizing agents together, it is preferable that total content is in the said range.
  • the polishing liquid may contain components other than the above as optional components. Below, an arbitrary component is demonstrated.
  • the polishing liquid may further contain abrasive grains other than colloidal silica.
  • the abrasive grains are not particularly limited, and abrasive grains other than known colloidal silica can be used.
  • abrasive grains include inorganic abrasive grains such as silica (precipitated silica other than colloidal silica, or fumed silica), alumina, zirconia, ceria, titania, germania, and silicon carbide; polystyrene, polyacryl, polyvinyl chloride, and the like Organic abrasive grains.
  • the polishing liquid may further contain an organic acid other than amino acids.
  • Organic acids other than amino acids are compounds different from oxidizing agents.
  • As the organic acid a water-soluble organic acid is preferable.
  • the organic acid is not particularly limited, and a known organic acid can be used.
  • organic acid examples include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n- Heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, malein
  • the polishing liquid preferably contains an organic solvent. It does not restrict
  • methyl ethyl ketone, tetrahydrofuran, dioxane, N-methylpyrrolidone, methanol, ethanol, ethylene glycol and the like are preferable.
  • the content of the organic solvent is not particularly limited, but is preferably 0.001 to 5.0% by mass, and more preferably 0.01 to 2.0% by mass with respect to the total mass of the polishing liquid.
  • the organic solvent may be used individually by 1 type, or may use 2 or more types together.
  • the total content is preferably within the above range.
  • the polishing liquid may contain a surfactant and / or a hydrophilic polymer.
  • Surfactants and hydrophilic polymers (hereinafter also referred to as “hydrophilic polymers”) have a function of reducing the contact angle of the polishing liquid to the surface to be polished, and the polishing liquid tends to wet and spread on the surface to be polished.
  • the surfactant is not particularly limited, and a known surfactant selected from the group consisting of an anionic surfactant, a cationic surfactant, an amphoteric surfactant, a nonionic surfactant, and the like may be used. it can.
  • anionic surfactant examples include carboxylic acid salts, sulfonic acid salts such as alkylbenzene sulfonic acids, sulfuric acid ester salts, and phosphoric acid ester salts.
  • cationic surfactant examples include aliphatic amine salts, aliphatic quaternary ammonium salts, benzalkonium chloride salts, benzethonium chloride, pyridinium salts, and imidazolinium salts.
  • amphoteric surfactants include carboxybetaine type, aminocarboxylate, imidazolinium betaine, lecithin, and alkylamine oxide.
  • nonionic surfactant examples include ether type, ether ester type, ester type, nitrogen-containing type, glycol type, and fluorine type surfactant.
  • hydrophilic polymers include polyglycols such as polyethylene glycol, alkyl ethers of polyglycols, polysaccharides such as polyvinyl alcohol, polyvinyl pyrrolidone, and alginic acid, carboxylic acid-containing polymers such as polymethacrylic acid, and polyacrylic acid, Examples include polyacrylamide, polymethacrylamide, and polyethyleneimine. Specific examples of such a hydrophilic polymer include water-soluble polymers described in JP2009-88243A, paragraphs 0042 to 0044, and JP2007-194261A, paragraph 0026.
  • the water-soluble polymer is preferably a water-soluble polymer selected from polyacrylamide, polymethacrylamide, polyethyleneimine, and polyvinylpyrrolidone.
  • polyacrylamide or polymethacrylamide those having a hydroxyalkyl group on a nitrogen atom (for example, N- (2-hydroxyethyl) acrylamide polymer) or those having a substituent having a polyalkyleneoxy chain are preferred, and the weight average The molecular weight is more preferably 2000 to 50000.
  • the polyethyleneimine those having a polyalkyleneoxy chain on the nitrogen atom are preferred, and those having a repeating unit represented by the following general formula are more preferred.
  • n a number of 2 to 200 (in the case of a mixture, the average number thereof).
  • Polyethyleneimine preferably has an HLB (Hydrophile-Lipophile Balance) value of 16 to 19.
  • the content of the surfactant or the hydrophilic polymer is not particularly limited, but is preferably 0.00001 to 2.0% by mass, more preferably 0.0001 to 1.0% by mass with respect to the total mass of the polishing liquid. 0.0001 to 0.5% by mass is more preferable, and 0.0001 to 0.1% by mass is particularly preferable.
  • the content of the surfactant or the hydrophilic polymer is in the range of 0.0001 to 1.0% by mass, a polishing liquid having a more excellent effect of the present invention can be obtained.
  • surfactant or a hydrophilic polymer may be used individually by 1 type, or may use 2 or more types together. Further, a surfactant and a hydrophilic polymer may be used in combination. When two or more kinds of surfactants, or two or more kinds of hydrophilic polymers, or a surfactant and a hydrophilic polymer are used in combination, the total content is preferably within the above range.
  • the polishing liquid may further contain a pH adjusting agent and / or a pH buffering agent so as to have a predetermined pH.
  • the pH adjusting agent and / or pH buffering agent include acid agents and / or alkali agents.
  • the pH adjusting agent and the pH buffering agent are compounds different from the above amino acids. Although it does not restrict
  • the alkali agent is not particularly limited, but ammonia; ammonium hydroxide and organic ammonium hydroxide; alkanolamines such as diethanolamine, triethanolamine, and triisopropanolamine; sodium hydroxide, potassium hydroxide, and lithium hydroxide Alkali metal hydroxides; carbonates such as sodium carbonate; phosphates such as trisodium phosphate; borate and tetraborate; hydroxybenzoate;
  • the content of the pH adjusting agent and / or the pH buffering agent is not particularly limited as long as it is an amount necessary to maintain the pH within a desired range, and is usually 0.0001 to the total amount of the polishing liquid. 0.1 mass% is preferable.
  • the polishing liquid preferably contains water.
  • the water contained in the polishing liquid is not particularly limited, but ion exchange water, pure water, or the like can be used.
  • the water content is not particularly limited, but is preferably 90 to 99% by mass based on the total mass of the polishing liquid.
  • the polishing liquid may contain a chelating agent (that is, a hard water softening agent) as necessary in order to reduce adverse effects such as mixed polyvalent metal ions.
  • a chelating agent for example, a general-purpose hard water softening agent which is a precipitation inhibitor of calcium and / or magnesium or an analogous compound thereof can be used, and two or more of them may be used in combination as necessary.
  • the content of the chelating agent may be an amount sufficient to sequester metal ions such as mixed polyvalent metal ions, and is preferably 0.001 to 2.0% by mass in the total mass of the polishing liquid, for example. .
  • the polishing liquid can be produced by a known method. For example, it can manufacture by mixing each said component. The order and / or timing in particular of mixing each said component are not restrict
  • the polishing liquid is preferably produced by the following method.
  • the manufacturing method of the polishing liquid according to one embodiment of the present invention includes an oxidizing agent or an oxidizing agent and water with respect to a polishing liquid stock solution containing colloidal silica, an amino acid, and two or more azole compounds.
  • a method for producing a polishing liquid, comprising a step of mixing to obtain the above polishing liquid (hereinafter also referred to as a “dilution step”).
  • the content of the oxidizing agent relative to the total mass of the polishing liquid Easy to control to a desired range. This is because some oxidizing agents decompose over time and the content in the polishing liquid changes.
  • the dilution step is a step of obtaining a polishing liquid by mixing an oxidizing agent or an oxidizing agent and water with a polishing liquid stock solution containing predetermined components.
  • the aspect of the polishing liquid is as described above. Moreover, it does not restrict
  • the polishing liquid stock solution used in the dilution step is a polishing liquid stock solution containing colloidal silica, an amino acid, and two or more azole compounds, and further mixed with an oxidizing agent or an oxidizing agent and water.
  • a polishing liquid stock solution used for producing a polishing liquid As the polishing liquid stock solution, it is only necessary to obtain the polishing liquid by mixing an oxidizing agent or an oxidizing agent and water.
  • an organic solvent, a surfactant, a hydrophilic polymer, and a pH adjustment as desired.
  • An agent, a pH buffering agent, water, a chelating agent and the like may be contained.
  • the polishing liquid stock solution may contain all of the water in the total amount of water in the total mass of the polishing liquid obtained through the dilution step, or may contain some water. .
  • the polishing liquid stock solution contains components other than the oxidizing agent, the polishing liquid can be manufactured more easily. Moreover, it becomes easy to control the content of the oxidizing agent in the polishing liquid within a desired range by mixing the oxidizing agent at the time of use to produce the polishing liquid.
  • the method for producing the polishing liquid stock solution is not particularly limited, and can be produced by a known method. For example, it can manufacture by mixing each said component.
  • the order of mixing the above components is not particularly limited, and colloidal silica may be dispersed in advance in water and / or an organic solvent whose pH has been adjusted, and predetermined components may be sequentially mixed.
  • a concentrated liquid of a polishing liquid containing a predetermined component is prepared, and at least one selected from the group consisting of an oxidant and water is added to the polishing liquid.
  • examples thereof include a method for producing a polishing liquid having characteristics.
  • the concentrated liquid of the polishing liquid for example, among the components of the polishing liquid containing colloidal silica, an amino acid, two or more azole compounds, an oxidizing agent, and water, components other than water are previously included. What mixed is mentioned.
  • a chemical mechanical polishing method comprising a step of relatively moving a polishing target and a polishing pad to polish a surface to be polished to obtain a polished target (hereinafter also referred to as “polishing step”).
  • polishing step comprising a step of relatively moving a polishing target and a polishing pad to polish a surface to be polished to obtain a polished target
  • CMP method also referred to as “CMP method”.
  • the object to be polished to which the CMP method according to the above embodiment can be applied is not particularly limited, but the object to be polished (metal layer) containing at least one metal layer selected from the group consisting of copper and copper alloys. (Attached substrate) is preferable. Although it does not restrict
  • the electrode may be a through silicon via.
  • the object to be polished used in the CMP method according to the above embodiment can be manufactured by, for example, the following method.
  • an interlayer insulating film such as silicon dioxide is laminated on a silicon substrate.
  • a concave portion (substrate exposed portion) having a predetermined pattern is formed on the surface of the interlayer insulating film by a known means such as resist layer formation or etching to form an interlayer insulating film composed of convex portions and concave portions.
  • tantalum or the like is deposited by vapor deposition, CVD (chemical vapor deposition), or the like as a barrier layer covering the interlayer insulating film along the surface irregularities.
  • a metal layer a conductive material layer that covers the barrier layer so as to fill the recess, and has a laminated structure.
  • a polished body is obtained.
  • the thicknesses of the interlayer insulating film, the barrier layer, and the metal layer are preferably about 0.01 to 2.0 ⁇ m, 1 to 100 nm, and 0.01 to 2.5 ⁇ m, respectively.
  • the material constituting the barrier layer is not particularly limited, and a known low-resistance metal material can be used. For example, TiN, TiW, Ta, TaN, W, or WN is preferable as the low-resistance metal material, and Ta or TaN is more preferable.
  • the polishing apparatus capable of performing the CMP method is not particularly limited, and a known chemical mechanical polishing apparatus (hereinafter also referred to as “CMP apparatus”) can be used.
  • CMP apparatus for example, a holder that holds an object to be polished (for example, a semiconductor substrate) having a surface to be polished and a polishing pad to which a polishing pad is attached (a motor that can change the number of revolutions is attached).
  • a general CMP apparatus provided with a board can be used.
  • Reflexion manufactured by Applied Materials
  • polishing is preferably performed at a polishing pressure, that is, a pressure generated on the contact surface between the surface to be polished and the polishing pad of 3000 to 25000 Pa, and more preferably 6500 to 14000 Pa. .
  • the polishing is preferably performed at a rotation speed of the polishing platen of 50 to 200 rpm (revolution per minute), more preferably 60 to 150 rpm.
  • the holder may be further rotated and / or swayed, the polishing platen may be rotated on a planetary surface, or the belt-shaped polishing pad may be long. It may be moved linearly in one direction of the scale direction.
  • the holder may be in a fixed, rotating, or swinging state.
  • polishing liquid supply method In the CMP method according to the above embodiment, the polishing liquid is continuously supplied to the polishing pad on the polishing surface plate by a pump or the like while the surface to be polished is polished. Although there is no restriction
  • the aspect of the polishing liquid is as described above.
  • the CMP method according to the above embodiment may further include the following steps before the polishing step.
  • the process of mixing an oxidizing agent or an oxidizing agent, and water is mentioned with respect to the polishing liquid stock solution containing colloidal silica, an amino acid, and 2 or more types of azole compounds, for example.
  • the step is selected from the group consisting of an oxidizing agent and water with respect to a polishing liquid concentrate containing, for example, colloidal silica, an amino acid, two or more azole compounds, and an oxidizing agent.
  • a step of mixing at least one of the above.
  • the content of the oxidizing agent in the polishing liquid can be easily controlled in a desired range by mixing the oxidizing agent and the like immediately before use to produce the polishing liquid.
  • the aspects of the polishing liquid, the polishing liquid stock solution, and the concentrated liquid are as described above.
  • Example 1 Each component shown below was mixed to prepare a chemical mechanical polishing liquid.
  • Colloidal silica (average primary particle size: 35 nm, product name “PL3”, manufactured by Fuso Chemical Industries) 0.1 mass% ⁇ Glycine (corresponds to amino acid) 1.5% by mass ⁇ 5-methylbenzotriazole (corresponds to azole compound containing benzotriazole skeleton) 0.001% by mass ⁇
  • Ethylene glycol corresponds to organic solvent, partly used as a solvent to dissolve 5-methylbenzotriazole) 0.05% by mass ⁇ 3-amino-1,2,4-triazole (corresponds to a compound not containing a benzotriazole skeleton and a compound containing a 1,2,4-triazole skeleton) 0.2% by mass ⁇
  • Hydrogen peroxide (corresponds to oxidizing agent) 1.0% by mass ⁇ Water (pure water) remaining
  • the pH of the polishing liquid in Table 1 was adjusted to a predetermined value using sulfuric acid and / or tetramethylammonium hydroxide as necessary.
  • Example 2 to 42 Each component shown in Table 1 was mixed by the same method as in Example 1 to obtain each polishing liquid.
  • each abbreviation in Table 1 shows the following compounds.
  • PL3 Cold silica, product name “PL3”, manufactured by Fuso Chemical Industries, average primary particle size: 35 nm
  • PL2 Cold silica, product name “PL2”, manufactured by Fuso Chemical Industries, average primary particle size: 25 nm
  • Gly corresponds to glycine and amino acid
  • Ala corresponds to alanine and amino acid
  • Asp corresponds to aspartic acid and amino acid
  • NMG N-methylglycine, corresponding to amino acids
  • 5-MBTA corresponds to 5-methylbenzotriazole, azole compound containing benzotriazole skeleton
  • -BTA corresponds to benzotriazole, azole compound containing benzotriazole skeleton
  • 5,6-DMBTA corresponds to
  • a silicon substrate on which copper having a thickness of 1500 nm is deposited is cut into a square of about 10 mm and left in a polyethylene cup having an internal volume of about 100 ml containing 10 ml of the above polishing liquid at room temperature (about 25 ° C.) for 24 hours. And soaked. After immersion, the sample taken out from the polishing liquid was washed with water and further air-dried using nitrogen to obtain a sample having a reaction layer formed on the copper surface.
  • Polishing was performed while supplying the polishing liquid to the polishing pad under the following conditions, and the polishing rate and dishing were evaluated.
  • Polishing device Reflexion (manufactured by Applied Materials) ⁇
  • Substance to be polished wafer: (1) For polishing speed calculation; 300 mm diameter blanket wafer with a 1.5 ⁇ m thick Cu film formed on a silicon substrate (2)
  • 300 mm diameter copper wiring wafer (pattern wafer) (Mask pattern 754CMP (ATDF))
  • the average value obtained by dividing by the value was used as the polishing rate and evaluated according to the following criteria.
  • polishing rate C or more is a practical range.
  • D The polishing rate is less than 200 nm / min.
  • Dishing is more than 30 nm and 35 nm or less.
  • F Dishing is more than 35 nm and 40 nm or less.
  • G Dishing is more than 40 nm and 45 nm or less.
  • H Dishing is over 45 nm.
  • a polishing liquid for chemical mechanical polishing containing colloidal silica, an amino acid, two or more azole compounds, and an oxidizing agent, which was in contact with the polishing liquid for 24 hours.
  • the polishing liquids of Examples 1 to 42 in which a reaction layer having a thickness of 1 to 20 nm was formed on the copper substrate had the desired effects.
  • the polishing liquids of Comparative Examples 1 to 4 did not achieve the desired effects.
  • the polishing liquids of Examples 1, 3, and 4 in which the content of the oxidizing agent is 0.3 to 2.0% by mass with respect to the total mass of the polishing liquid are the polishing liquids of Examples 2 and 5. In comparison, it was found that the present invention has a better effect of the present invention.
  • the polishing liquid of Example 1 in which two or more azole compounds contain a benzotriazole compound and an azole compound different from the benzotriazole compound includes Example 33 and two or more benzotriazole compounds. Compared with 34 polishing liquid, it had the effect of this invention more excellent. Further, the polishing liquids of Examples 1, 7 and 8 in which the mass ratio (B) / (A) of the content of the azole compound (A) and the azole compound (B) is greater than 1.0 and 1000 or less. Compared with the polishing liquids of Examples 6 and 9, it was found that dishing is less likely to occur on the polished surface when applied to CMP.
  • polishing liquids of Examples 1, 11, and 12 in which the pH of the polishing liquid is in the range of 5.0 to 8.0 are more excellent than the polishing liquids of Examples 10 and 13. Had the effect of.
  • the polishing liquids of Examples 1 and 15 in which the amino acid content is 1.0 to 20% by mass with respect to the total mass of the polishing liquid are compared with the polishing liquids of Example 14 and Example 16. There was no lowest evaluation rank evaluation rank (polishing rate “C”) within the practical range, and the effects of the present invention were more excellent.
  • polishing liquid of Example 1 or Example 19 in which the amino acid was glycine or methylglycine had a more excellent effect of the present invention than the polishing liquids of Examples 17 and 18.
  • the polishing liquid of Example 32 containing two or more amino acids had a better effect of the present invention than the polishing liquid of Example 1.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • ing And Chemical Polishing (AREA)
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