US20170342304A1 - Polishing composition - Google Patents

Polishing composition Download PDF

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US20170342304A1
US20170342304A1 US15/544,425 US201615544425A US2017342304A1 US 20170342304 A1 US20170342304 A1 US 20170342304A1 US 201615544425 A US201615544425 A US 201615544425A US 2017342304 A1 US2017342304 A1 US 2017342304A1
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Prior art keywords
sulfonic acid
colloidal silica
polishing composition
less
acid
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Inventor
Keiji Ashitaka
Shogo Tsubota
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Fujimi Inc
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Fujimi Inc
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Publication of US20170342304A1 publication Critical patent/US20170342304A1/en
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    • 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
    • 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
    • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
    • 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
    • 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
    • C09K3/1436—Composite particles, e.g. coated particles
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • H01L21/3105—After-treatment
    • H01L21/31051—Planarisation of the insulating layers
    • H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step

Definitions

  • the present invention relates to a polishing composition.
  • CMP chemical mechanical polishing
  • the silicon nitride film usually has unevenness, when polishing such a material, not only the convex portions but also the concave portions are scraped together, and the unevenness are hardly sufficiently eliminated.
  • the semiconductor wafer is constituted of dissimilar materials including polycrystalline silicon forming a circuit, silicon oxide being an insulating material, and silicon nitride for protecting a silicon dioxide surface that is not part of the trench or the via from the damages during etching. Therefore, a phenomenon such as dishing, in which a material that is relatively soft and easily reacts with a polishing agent, such as polycrystalline silicon, and silicon oxide is scraped excessively as compared with the silicon nitride or the like surrounding the material, is generated, and unevenness is left.
  • a polishing agent such as polycrystalline silicon
  • JP 2012-040671 A for the purpose of providing a polishing composition capable of polishing at a high speed an object to be polished that is poor in chemical reactivity, such as silicon nitride, a technique in which colloidal silica which is immobilized with an organic acid (sulfonic acid-modified aqueous anionic silica sol) is allowed to be contained in the composition as abrasive grains, and the pH is adjusted to 6 or less has been disclosed.
  • silica sol such as colloidal silica is unstable because silica particles aggregate with each other under an acidic condition.
  • sulfonic acid-modified aqueous anionic sol having a zeta potential of ⁇ 15 mV or less at an acidic of pH 2 or more has been disclosed.
  • JP 2010-269985 A as a method for producing the anionic sol described above, a technique in which a silane coupling agent having a functional group chemically convertible to a sulfonic acid group (for example, a mercapto group) is added to colloidal silica, and then the functional group is converted to a sulfonic acid group has been disclosed.
  • a silane coupling agent having a functional group chemically convertible to a sulfonic acid group for example, a mercapto group
  • silica sol containing water and methanol as a dispersing medium is heated and concentrated under alkaline and normal pressure conditions, and then into the silica sol, a mercapto group-containing silane coupling agent (3-mercaptopropyl trimethoxysilane) is added, and the resultant mixture is refluxed at a boiling point and heat aged.
  • a mercapto group-containing silane coupling agent (3-mercaptopropyl trimethoxysilane)
  • JP 2013-41992 A there is a disclosure about the production of similar sulfonic acid-modified aqueous anionic silica sol, referring to the above-described JP 2010-269985 A, and J. Ind. Eng. Chem., Vol. 12, No. 6 (2006) 911-917.
  • silica sol containing water as a dispersing medium is added, the resultant mixture is stirred at room temperature for one hour, and then into the mixture hydrogen peroxide water is added, and the resultant mixture is left to stand at room temperature for 48 hours, as a result, sulfonic acid-modified aqueous anionic silica sol is obtained.
  • an object of the present invention is to provide a technique in which the stability of the SiN polishing rate with time can be improved in a case where the polishing composition is used as a polishing composition for polishing an object to be polished that contains SiN, in a polishing composition containing sulfonic acid-modified aqueous anionic sol.
  • the present inventors carried out intensive studies. As a result, it was found that in the method for producing sulfonic acid-modified aqueous anionic silica sol, which is described in JP 2010-269985 A, by adding a silane coupling agent into silica sol after the reduction of the amount of the fine silica particles contained in the silica sol before the addition of a silane coupling agent, performing a reaction in the similar manner, and subsequently, performing an oxidation step, sulfonic acid-modified aqueous anionic silica sol that can solve the above-described problem is obtained. Based on the above findings, the present inventors thus have completed the present invention.
  • a polishing composition having a pH of 6 or less contains sulfonic acid-modified colloidal silica obtained by immobilizing sulfonic acid on surfaces of silica particles, and water.
  • the sulfonic acid-modified colloidal silica is characterized by being derived from the sulfonic acid-modified aqueous anionic silica sol produced by a production method including a first reaction step of obtaining a reactant by heating raw colloidal silica having a number distribution ratio of 10% or less of microparticles having a particle diameter of 40% or less relative to a volume average particle diameter based on Heywood diameter (equivalent circle diameter) as determined by image analysis using a scanning electron microscope in the presence of a silane coupling agent having a functional group chemically convertible to a sulfonic acid group, and a second reaction step of converting the functional group to a sulfonic acid group by treating the reactant.
  • a technique in which the stability of the SiN polishing rate with time can be improved in a case where the polishing composition is used as a polishing composition for polishing an object to be polished that contains SiN can be provided.
  • FIG. 1 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Example 1, observed with a scanning electron microscope (SEM) (magnification: 100000 times).
  • FIG. 2 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Example 1, observed with a transmission electron microscope (TEM) (magnification: 400000 times).
  • TEM transmission electron microscope
  • FIG. 3 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Comparative Example 1, observed with a scanning electron microscope (SEM) (magnification: 100000 times).
  • FIG. 4 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Comparative Example 1, observed with a transmission electron microscope (TEM) (magnification: 400000 times).
  • TEM transmission electron microscope
  • FIG. 5 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Comparative Example 2, observed with a scanning electron microscope (SEM) (magnification: 100000 times).
  • FIG. 6 is a photograph of sulfonic acid-modified aqueous anionic silica sol obtained in Comparative Example 2, observed with a transmission electron microscope (TEM) (magnification: 400000 times).
  • TEM transmission electron microscope
  • An embodiment of the present invention is a polishing composition having a pH of 6 or less, containing sulfonic acid-modified colloidal silica obtained by immobilizing sulfonic acid on surfaces of silica particles, and water, wherein the sulfonic acid-modified colloidal silica is derived from sulfonic acid-modified aqueous anionic silica sol produced by a production method including a first reaction step of obtaining a reactant by heating raw colloidal silica having a number distribution ratio of 10% or less of microparticles having a particle diameter of 40% or less relative to a volume average particle diameter based on Heywood diameter (equivalent circle diameter) as determined by image analysis using a scanning electron microscope in the presence of a silane coupling agent having a functional group chemically convertible to a sulfonic acid group, and a second reaction step of converting the functional group to a sulfonic acid group by treating the reactant.
  • the polishing composition according to the present embodiment is prepared by mixing in water the sulfonic acid-modified colloidal silica (abrasive grains) obtained by immobilizing sulfonic acid on surfaces of silica particles, and by adjusting the pH.
  • the polishing composition is preferably used mainly for an application of polishing silicon nitride, and more specifically, the polishing composition is more preferably used mainly for an application of polishing the surface containing silicon nitride in an object to be polished such as a semiconductor wiring substrate.
  • the sulfonic acid-modified colloidal silica (abrasive grains) contained in the composition is derived from a sulfonic acid-modified aqueous anionic silica sol produced by a specific production method.
  • the production method for producing the sulfonic acid-modified colloidal silica to be contained in the polishing composition according to the present embodiment will be described in detail.
  • the raw colloidal silica is heated in the presence of a silane coupling agent having a functional group chemically convertible to a sulfonic acid group.
  • a reactant in which a silane coupling agent having a functional group chemically convertible to a sulfonic acid group is bonded to surfaces of silica particles.
  • the raw colloidal silica used in the first reaction step is not particularly limited as long as having a silanol group on the surface. However, it is preferred not to contain diffusible metal impurities and corrosive ions such as chlorine in a semiconductor, therefore, in consideration of this point, it is preferred that a hydrolyzable silicon compound (for example, an alkoxysilane or a derivative thereof) is used as a starting material, and the colloidal silica obtained by hydrolysis and condensation is used as the raw colloidal silica.
  • the silicon compound may be used singly alone, or may also be used in combination of two or more kinds thereof.
  • the silicon compound is preferably an alkoxysilane represented by the following general formula (1) or a derivative thereof.
  • R is an alkyl group, preferably a lower alkyl group having 1 to 8 carbon atoms, and more preferably a lower alkyl group having 1 to 4 carbon atoms.
  • examples of the R include a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, a pentyl group, and a hexyl group, and tetramethoxysilane in which R is a methyl group, tetraethoxysilane in which R is an ethyl group, and tetraisopropoxysilane in which R is an isopropyl group are preferred.
  • the derivative of the alkoxysilane a low condensate obtained by partially hydrolyzing the alkoxysilane is mentioned.
  • the silicon compound is hydrolyzed and condensed in a reaction solvent, and becomes colloidal silica.
  • a reaction solvent water or an organic solvent containing water can be used.
  • the organic solvent include a hydrophilic organic solvent including alcohols such as methanol, ethanol, isopropanol, n-butanol, t-butano, pentanol, ethylene glycol, propylene glycol, and 1,4-butanediol; ketones such as acetone and methyl ethyl ketone; and the like.
  • organic solvents it is preferred to use particularly alcohols such as methanol, ethanol, and isopropanol, and from the viewpoint of the post-processing of the reaction solvent, and the like, it is more preferred to use alcohols having the same alkyl group as the alkyl group (R) of the starting material silicon compound (for example, methanol to tetramethoxysilane).
  • alcohols having the same alkyl group as the alkyl group (R) of the starting material silicon compound (for example, methanol to tetramethoxysilane).
  • These organic solvents may be used singly alone, or may also be used in combination of two or more kinds thereof.
  • the use amount of the organic solvent is not particularly limited, but is preferably around 5 to 50 mol per 1 mol of the silicon compound.
  • the amount of the water to be added into the organic solvent is not particularly limited, as long as the amount required for the hydrolysis of the silicon compound is present, and around 2 to 15 mol per 1 mol of the silicon compound is preferred.
  • the amount of the water to be mixed in the organic solvent largely affects the particle diameter of the colloidal silica to be formed. By increasing the addition amount of water, the particle diameter of the colloidal silica can be increased. Further, by decreasing the addition amount of water, the particle diameter of the colloidal silica can be reduced. Accordingly, by changing the mixing ratio of the water and the organic solvent, the particle diameter of the colloidal silica to be produced can be arbitrarily adjusted.
  • the reaction solvent is adjusted to preferably pH 8 to 11, and more preferably to pH 8.5 to 10.5, and the colloidal silica can be rapidly formed.
  • the basic catalyst organic amine and ammonia are preferred from the viewpoint of preventing the contamination of impurities, in particular, ethylenediamine, diethylenetriamine, triethylenetetramine, ammonia, urea, ethanol amine, tetramethylammonium hydroxide, and the like can be preferably mentioned.
  • the silicon compound that is a starting material is added to an organic solvent, and the resultant mixture is stirred at a temperature condition of 0 to 100° C., and preferably 0 to 50° C.
  • a temperature condition of 0 to 100° C., and preferably 0 to 50° C. By hydrolyzing and condensing the silicon compound while stirring the silicon compound in an organic solvent containing water, colloidal silica having a spherical shape and a uniform particle diameter can be obtained.
  • a silane coupling agent having a functional group chemically convertible to a sulfonic acid group is added, in the similar manner as in the technique described in JP 2010-269985 A.
  • a silane coupling agent having a functional group chemically convertible to a sulfonic acid group is added, in the similar manner as in the technique described in JP 2010-269985 A.
  • the raw colloidal silica used in the first reaction step of the production method according to the present embodiment is characterized in the point that a number distribution ratio of microparticles having a particle diameter of 40% or less relative to a volume average particle diameter (hereinafter, also simply referred to as “microparticles”) based on Heywood diameter (equivalent circle diameter) as determined by image analysis using a scanning electron microscope is 10% or less.
  • the number distribution ratio is preferably 5% or less, more preferably 2% or less, furthermore preferably 1% or less, still more preferably 0.5% or less, particularly preferably 0.3% or less, and most preferably 0.2% or less.
  • the lower limit value of the number distribution ratio is not particularly limited, but is, for example, 0.001% or more.
  • the method for measuring the number distribution ratio is performed in accordance with the description in Examples described later.
  • the expression “whether or not the residual organic solvent concentration in the colloidal silica is less than 1° by mass” is synonymous with the expression “whether or not the organic solvent is detected in the colloidal silica” in the method for measuring the organic solvent concentration (methanol concentration in Examples) using the gas chromatography that is described in Examples described later. That is, the above-described expression “so that the residual organic solvent concentration in the colloidal silica becomes less than 1% by mass” can also be paraphrased as the expression “so that the organic solvent in the colloidal silica measured by the measurement method using the gas chromatography that is described in the Examples, becomes lower than the detection limit”.
  • the amount of the microparticles contained in the raw colloidal silica can be decreased.
  • the organic solvent concentration in the colloidal silica obtained by the above-described Stober method usually exceeds 1% by mass. Accordingly, in an embodiment of the production method according to the present invention, a step in which an organic solvent is removed so that the residual organic solvent concentration in colloidal silica becomes 1% by mass or less after the colloidal silica is obtained by a Stober method is further included.
  • the technique for removing the organic solvent coexisting with the colloidal silica a method in which a dispersion (silica sol) of colloidal silica is heated and the organic solvent is distilled off can be mentioned. At this time, by replacing the organic solvent to be removed with water, the liquid amount of the colloidal silica dispersion can be maintained.
  • the pH of the colloidal silica dispersion at the time of distilling off the organic solvent is preferably pH 7 or more.
  • the technique for setting the number distribution ratio of the microparticles contained in the raw colloidal silica to 10% or less a method for removing the organic solvent coexisting with the colloidal silica has been explained in detail as an example, but by a technique different from this, the number distribution ratio of the microparticles contained in the raw colloidal silica may be set to 10% or less.
  • a technique of using oligomers as a starting material a technique of optimizing the composition at the time of synthesis, a technique of performing a high temperature and pressure treatment after synthesis, a technique of performing centrifugation after synthesis, and the like can be mentioned, and a technique other than these techniques may also be used of course.
  • various treatment steps may be applied to the raw colloidal silica obtained in the above.
  • a step of lowering the viscosity of the raw colloidal silica can be mentioned.
  • a step of adding an alkaline solution (aqueous solution of various bases, such as ammonia water) or an organic solvent to the raw colloidal silica can be mentioned.
  • the amount of the alkaline solution or organic solvent to be added at this time is not particularly limited, and may be appropriately set in consideration of the viscosity of the raw colloidal silica to be obtained after the addition.
  • the raw colloidal silica having a small content of microparticles is heated in the presence of a silane coupling agent having a functional group chemically convertible to a sulfonic acid group.
  • a reactant can be obtained.
  • the reason why the silane coupling agent having a functional group different from a sulfonic acid group is reacted with the raw colloidal silica, and then the functional group is converted to a sulfonic acid group (the second reaction step described later) is because in general, it is difficult to stably obtain a silane coupling agent in a form of being replaced with sulfonic acid groups.
  • silane coupling agent having a functional group chemically convertible to a sulfonic acid group for example, 1) a silane coupling agent having a sulfonic acid ester group convertible to a sulfonic acid group by hydrolysis, and 2) a silane coupling agent having a mercapto group and/or a sulfide group convertible to a sulfonic acid group by oxidation can be mentioned.
  • a silane coupling agent having a sulfonic acid ester group convertible to a sulfonic acid group by hydrolysis for example, 1) a silane coupling agent having a mercapto group and/or a sulfide group convertible to a sulfonic acid group by hydrolysis, and 2) a silane coupling agent having a mercapto group and/or a sulfide group convertible to a sulfonic acid group by oxidation can be mentioned.
  • the sulfonic acid modification on the colloidal silica surface is
  • silane coupling agent having a mercapto group examples include 3-mercaptopropyl trimethoxysilane, 2-mercaptopropyl triethoxysilane, 2-mercaptoethyl trimethoxysilane, and 2-mercaptoethyl triethoxysilane.
  • the coupling agent having a sulfide group for example, bis(3-triethoxysilylpropyl)disulfide, or the like can be mentioned.
  • silane coupling agent is hydrolyzed in advance with an acid, and then the condensation reaction to the raw colloidal silica may also be performed.
  • the raw colloidal silica substantially does not contain the organic solvent, and the dispersing medium of the raw colloidal silica is substantially composed of water.
  • an organic solvent hydrophilic solvent
  • the above-described organic solvents such as methanol, ethanol, and isopropanol can be mentioned.
  • the sulfonic acid-modified aqueous anionic silica sol from which the sulfonic acid-modified colloidal silica contained in the polishing composition according to the present invention is derived is anionic silica sol in which the surfaces of silica particles have been modified with a sulfonic acid group
  • the technique is the same as that described in JP 2010-269985 A.
  • the addition amount of the silane coupling agent used in the first reaction step is not particularly limited, but is, based on 100% by mass of the silica particles contained in the raw colloidal silica, preferably 0.5 to 10% by mass, more preferably 1 to 5% by mass, and furthermore preferably 1 to 3% by mass.
  • the addition amount of the silane coupling agent is 0.5% by mass or more, the surfaces of the silica particles can be sufficiently anionized, and an excellent performance can be exerted in a case of being used as a polishing agent (abrasive grains in a polishing composition).
  • the addition amount of the silane coupling agent is 10% by mass or less, gelation with time of the reactant (surface-modified silica sol) to be obtained can be prevented.
  • the amount of the organic solvent (hydrophilic solvent) used for dissolving the silane coupling agent is, based on 100% by mass of the silane coupling agent, preferably around 500 to 10000% by mass, and more preferably 1000 to 5000% by mass.
  • the temperature at which the silane coupling agent is added is not limited, but is preferably in the range of room temperature (around 20° C.) to the boiling point of the reaction solvent.
  • the reaction time is not also limited, but is preferably 10 minutes to 10 hours, and more preferably 30 minutes to 2 hours. However, from the viewpoint of terminating the hydrolysis of the coupling agent, it is preferred that the first reaction step is performed under a condition that a temperature condition of 90° C. or more is continued for 30 minutes or more.
  • the pH at the time of addition is also not limited, but is preferably 7 or more to 11 or less.
  • the reactant in which a silane coupling agent having a functional group chemically convertible to a sulfonic acid group is bonded to surfaces of silica particles, which has been obtained in the above-described first reaction step, is treated.
  • the “functional group chemically convertible to a sulfonic acid group” possessed by the silane coupling agent is converted to a sulfonic acid group.
  • the specific form of the above-described “treatment” for converting the “functional group chemically convertible to a sulfonic acid group” possessed by the silane coupling agent to a sulfonic acid group is not particularly limited, and can be appropriately selected depending on the structure of the silane coupling agent to be used.
  • the first reaction step in a case where the above-described 1) a silane coupling agent having a sulfonic acid ester group convertible to a sulfonic acid group by hydrolysis is used, by subjecting the reactant to a hydrolysis treatment, the functional group (sulfonic acid ester group) possessed by the silane coupling agent can be hydrolyzed. As a result, the sulfonic acid ester group is converted to a sulfonic acid group.
  • the first reaction step in a case where the above-described 2) a silane coupling agent having a mercapto group and/or a sulfide group convertible to a sulfonic acid group by oxidation is used, by subjecting the reactant to an oxidation treatment, the functional group (mercapto group and/or sulfide group) possessed by the silane coupling agent can be oxidized. As a result, the mercapto group or the sulfide group is converted to a sulfonic acid group.
  • the reactant may be reacted with an oxidizing agent.
  • the oxidizing agent include nitric acid, hydrogen peroxide, oxygen, ozone, organic peracid (percarboxylic acid), bromine, hypochlorite, potassium permanganate, and chromic acid.
  • hydrogen peroxide and organic peracid peracetic acid, and perbenzoic acids are preferred in the point of being relatively easy to handle and being favorable in the oxidation yield. Further, in consideration of the substances by-produced in the reaction, it is most preferred to use hydrogen peroxide.
  • the addition amount of the oxidizing agent is preferably 3 to 5 mol times the amount of the silane coupling agent.
  • the addition amount of the oxidizing agent is preferably 3 to 5 mol times the amount of the silane coupling agent.
  • the specific numerical value of the residual oxidizing agent concentration in the aqueous anionic silica sol to be obtained is not particularly limited, but is preferably 1000 ppm by mass or less, more preferably 700 ppm by mass or less, and particularly preferably 500 ppm by mass or less.
  • a residual oxidizing agent concentration in the obtained aqueous anionic silica sol exceeds 1000 ppm by mass, in storing and transporting the anionic silica sol itself, or the polishing composition in which the silica sol have been added as abrasive grains, in a state of being enclosed in a sealed container, there may be a case where an oxidizing agent such as hydrogen peroxide is decomposed, gas such as oxygen is generated, and the internal pressure of the container increases.
  • an oxidizing agent such as hydrogen peroxide
  • gas such as oxygen
  • colloidal silica and the silane coupling agent each of them has a structure that is stable in the oxidation reaction except for the functional groups to be oxidized (converted) to sulfonic acid groups, therefore, by-products are not present.
  • the dispersing medium mainly containing a reaction solvent may be replaced with water as needed.
  • this water replacement may be performed after the addition of the silane coupling agent and before the addition of the oxidizing agent.
  • the method for replacing the solvent other than water with water is not particularly limited, and for example, a method in which water is added dropwise by a fixed amount while heating the silica sol can be mentioned. Further, a method in which the silica sol is separated from the solvent other than water by precipitation and separation, centrifugation, or the like, and then redispersed in water can also be mentioned.
  • the sulfonic acid-modified aqueous anionic silica sol obtained by the production method according to the present invention a sulfonic acid group is immobilized on the surfaces of silica particles in the sol.
  • the sulfonic acid-modified aqueous anionic silica sol is in a state in which an organic material having a sulfonic acid group at the terminal is bonded to the surfaces of silica particles in the sol. Accordingly, even in a case of using an acidic dispersing medium, aggregation and gelation of the silica sol are suppressed, and the dispersion can be stably performed for a long time.
  • the polishing composition pH 6 or less
  • the high stability can be exerted over a long period of time.
  • the polishing composition according to another embodiment provided by the present invention is as follows: a polishing composition having a pH of 6 or less, and used for an application of polishing silicon nitride, containing sulfonic acid-modified colloidal silica obtained by immobilizing sulfonic acid on surfaces of silica particles, wherein the sulfonic acid-modified colloidal silica is derived from sulfonic acid-modified aqueous anionic silica sol in which when a SiN wafer is subjected to an immersion treatment under a pH 2 condition and then washed with pure water, the number of the particles having a particle diameter of less than 40% of a volume average particle diameter adhering to a surface of the SiN wafer is 50% or less
  • the proportion is preferably 30% or less, more preferably 10% or less, and furthermore preferably 5% or less.
  • the lower limit value of this proportion is not particularly limited, but is, for example, 0.1% or more.
  • the measurement method of this proportion is as follows (described as “condition 8” also in a section of Examples).
  • the sulfonic acid-modified aqueous anionic silica sol obtained by the production method according to the present invention is preferred also in the point that the content of metal impurities is reduced.
  • the metal impurities include an alkali metal such as sodium, and potassium; an alkaline earth metal such as calcium, and magnesium; and a heavy metal or light metal such as aluminum, iron, titanium, nickel, chromium, copper, zinc, lead, silver, manganese, and cobalt.
  • the total content of the metal impurities is 1 ppm by mass or less. The total content is preferably 0.5 ppm by mass or less.
  • the method for measuring the total content of the metal impurities is performed in accordance with the description in Examples described later.
  • the sulfonic acid-modified aqueous anionic silica sol is preferred because of containing no corrosive halogen element such as chlorine, and bromine.
  • the particle diameter of the silica particles contained in the sulfonic acid-modified aqueous anionic silica sol according to the present invention is not particularly limited, and is for example, 1000 nm or less, preferably 5 to 500 nm, and more preferably 10 to 300 nm.
  • the particle diameter of the silica particles means the volume average particle diameter based on Heywood diameter (equivalent circle diameter) as measured by the technique described in Examples described later.
  • the sulfonic acid-modified aqueous anionic silica sol according to the present invention is excellent in the long-term dispersion stability in a wide pH range.
  • the stability of the silica sol can be evaluated by measuring the zeta potential of the silica sol.
  • the zeta potential is a potential difference generated at the interface between solid and liquid, which are in contact with each other, when the solid and the liquid are moved relatively to each other.
  • the absolute value of the zeta potential increases, the repulsion between the particles becomes stronger and the stability of the particles becomes higher, and as the absolute value of the zeta potential approaches zero, the particles tend to aggregate more easily.
  • the sulfonic acid-modified aqueous anionic silica sol according to the present invention has high stability in the acidic region. Since a coupling agent having an anionic group is used as a modifier, the zeta potential when the dispersing medium is acidic of pH 2 or more is negative potential ( ⁇ 15 mV or less), and even if the dispersing medium is acidic, the dispersion stability is high. As described above, since the absolute value of the zeta potential is large, the dispersion stability is high, and along with this, the kinematic viscosity of the silica sol is also small. Therefore, even if the sulfonic acid-modified aqueous anionic silica sol is contained in the polishing composition (pH 6 or less) according to the present embodiment, the high stability can be exerted over a long period of time.
  • the sulfonic acid-modified aqueous anionic silica sol according to the present invention can be stably dispersed for a long time in a wide pH range when being contained as abrasive grains in the polishing composition according to the present invention.
  • the sulfonic acid-modified aqueous anionic silica sol according to the present invention in which the proportion of the microparticles adhering to a SiN wafer is kept low, is used particularly as a polishing agent for CMP polishing of a semiconductor wafer (SiN wafer), the fluctuation with time of the polishing rate can be minimized (excellent in the stability with time), therefore, the sulfonic acid-modified aqueous anionic silica sol is extremely suitably used for the applications, and can sufficiently cope also with the high performance requirements accompanying the miniaturization.
  • the polishing composition of the present invention contains water as a dispersing medium or a solvent for dispersing or dissolving each component. From the viewpoint of suppressing the blocking of the action of other components, water containing impurities as little as possible is preferred, and specifically, pure water or ultrapure water in which impurity ions have been removed by an ion exchange resin and then foreign matters have been removed through a filter, or distilled water is preferred.
  • water the water contained in the above-described sulfonic acid-modified aqueous anionic silica sol can be used as it is.
  • the pH value of the polishing composition of the present invention is 6 or less.
  • the pH value exceeds 6 the positive charge on a surface of an object to be polished such as silicon nitride becomes small, therefore, it becomes difficult to polish an object to be polished at a high speed using the abrasive grains (sulfonic acid-modified colloidal silica) according to the present invention, of which the surfaces are negatively charged.
  • the pH value of the polishing composition is preferably 5 or less, more preferably 4 or less, and particularly preferably 3 or less.
  • the pH value of the polishing composition is preferably 1 or more, and more preferably 1.5 or more.
  • the polishing composition of the present invention may contain a pH adjusting agent.
  • a pH adjusting agent the following acid, base, or a chelating agent can be used.
  • Examples of the acid include carboxylic acid such as formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, capric acid, lauric acid, myristic acid, palmitic acid, margaric acid, stearic acid, oleic acid, linoleic acid, linolenic acid, arachidonic acid, docosahexaenoic acid, eicosapentaenoic acid, lactic acid, malic acid, citric acid, benzoic acid, phthalic acid, isophthalic acid, terephthalic acid, salicylic acid, gallic acid, mellitic acid, cinnamic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, fumaric acid, maleic acid, aconitic acid, amino acid, and nitro carboxylic acid; and
  • examples of the acid also include inorganic acid such as carbonic acid, hydrochloric acid, nitric acid, phosphoric acid, hypophosphorous acid, phosphorous acid, phosphonic acid, sulfuric acid, boric acid, hydrofluoric acid, orthophosphoric acid, pyrophosphoric acid, polyphosphoric acid, metaphosphoric acid, and hexametaphosphoric acid.
  • inorganic acid such as carbonic acid, hydrochloric acid, nitric acid, phosphoric acid, hypophosphorous acid, phosphorous acid, phosphonic acid, sulfuric acid, boric acid, hydrofluoric acid, orthophosphoric acid, pyrophosphoric acid, polyphosphoric acid, metaphosphoric acid, and hexametaphosphoric acid.
  • the base examples include an amine such as an aliphatic amine, and an aromatic amine, an organic base such as quaternary ammonium hydroxide, a hydroxide of an alkali metal, such as potassium hydroxide, a hydroxide of an alkaline earth metal, and ammonia.
  • potassium hydroxide or ammonia is preferred from the viewpoint of easy availability.
  • a salt such as an ammonium salt or an alkali metal salt of the acid may be used as a pH adjusting agent.
  • a weak acid and a strong base, a strong acid and a weak base, or a weak acid and a weak base are used in combination, the buffering action of pH can be expected, and further, when a strong acid and a strong base are used in combination, not only the pH but also the electric conductivity can be adjusted with a small amount.
  • Examples of the chelating agent include polyamine, polyphosphonic acid, polyamino carboxylic acid, and polyamino phosphonic acid.
  • pH adjusting agents can also be used alone or by mixing two or more kinds thereof.
  • an inorganic acid and a carboxylic acid are preferred.
  • the addition amount of the pH adjusting agent is not particularly limited, and may be appropriately selected so that the pH is within the above pH range.
  • the polishing composition of the present invention contains water. From the viewpoint of preventing other components of the polishing composition from being influenced by the impurities, it is preferred to use water with purity as high as possible. Specifically, pure water or ultrapure water in which impurity ions have been removed by an ion exchange resin and then foreign matters have been removed through a filter, or distilled water is preferred. Further, as a dispersing medium or a solvent, for the purpose of controlling the dispersibility and the like of other components of the polishing composition, an organic solvent and the like may further be contained.
  • the polishing composition of the present invention may further contain as needed other components such as a complexing agent, a metal anticorrosive, an antiseptic agent, an antifungal agent, an oxidizing agent, a reducing agent, a surfactant, and a water-soluble polymer.
  • a complexing agent such as a metal anticorrosive, an antiseptic agent, an antifungal agent, an oxidizing agent, a reducing agent, a surfactant, and a water-soluble polymer.
  • the oxidizing agent capable of being added into the polishing composition has an action of oxidizing the surface of an object to be polished, and improves the polishing rate for the object to be polished with the polishing composition.
  • Examples of the usable oxidizing agent include hydrogen peroxide, sodium peroxide, barium peroxide, an organic oxidizing agent, ozone water, a silver (II) salt, an iron (III) salt, permanganic acid, chromic acid, bichromic acid, peroxodisulfuric acid, peroxophosphoric acid, peroxosulfuric acid, peroxoboric acid, performic acid, peracetic acid, perbenzoic acid, perphthalic acid, hypochlorous acid, hypobromous acid, hypoiodous acid, chloric acid, chlorous acid, perchloric acid, bromic acid, iodic acid, periodic acid, persulfuric acid, and dichloroisocyanuric acid; and salts thereof.
  • These oxidizing agents may be used alone or by mixing two or more kinds thereof. Among them, hydrogen peroxide, ammonium persulfate, periodic acid, hypochlorous acid, and sodium dichloroisocyanurate are preferred.
  • the content of the oxidizing agent in the polishing composition is preferably 0.1 g/L or more, more preferably 1 g/L or more, and furthermore preferably 3 g/L or more. As the content of the oxidizing agent increases, the polishing rate for an object to be polished with the polishing composition is more improved.
  • the content of the oxidizing agent in the polishing composition is preferably 200 g/L or less, more preferably 100 g/L or less, and furthermore preferably 40 g/L or less.
  • the content of the oxidizing agent decreases, the material cost of the polishing composition can be reduced, and further the load of the treatment of the polishing composition after use in polishing, that is, the load of the waste liquid treatment can also be reduced.
  • the risk of excessive oxidation on the surface of an object to be polished by an oxidizing agent can also be reduced.
  • antiseptic agent and the antifungal agent examples include an isothiazoline-based antiseptic agent such as 2-methyl-4-isothiazolin-3-one, and 5-chloro-2-methyl-4-isothiazolin-3-one; paraoxybenzoic acid esters and phenoxyethanol.
  • isothiazoline-based antiseptic agent such as 2-methyl-4-isothiazolin-3-one, and 5-chloro-2-methyl-4-isothiazolin-3-one
  • paraoxybenzoic acid esters paraoxybenzoic acid esters and phenoxyethanol.
  • antiseptic agent and antifungal agent may also be used alone or by mixing two or more kinds thereof.
  • a water-soluble polymer for the purpose of improving the hydrophilicity on the surface of an object to be polished, or improving the dispersion stability of abrasive grains, a water-soluble polymer may be added.
  • the water-soluble polymer include a cellulose derivative such as hydroxymethyl cellulose, hydroxyethyl cellulose (HEC), hydroxypropyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose, methyl cellulose, ethyl cellulose, ethyl hydroxyethyl cellulose, and carboxymethyl cellulose; an imine derivative such as poly(N-acylalkyleneimine); polyvinyl alcohol; modified (cationic modified or nonionic modified) polyvinyl alcohol; polyvinyl pyrrolidone; polyvinyl caprolactam; and polyoxyalkylene such as polyoxyethylene; and copolymers containing these constituent units.
  • These water-soluble polymer may be used alone, or may also be used by
  • the polishing composition according to the present invention is used for an application of polishing silicon nitride. That is, it is preferred that the object to be polished contains essentially silicon nitride.
  • an object to be polished may have a layer containing silicon nitride, and a layer containing a material different from silicon nitride. Examples of the material different from silicon nitride include polycrystalline silicon, monocrystalline silicon, tetraethyl orthosilicate (TEOS), and silicon oxide. These material may also be used alone or in combination of two or more kinds thereof.
  • the layer containing a material different from silicon nitride, which is an object to be polished may also have a single layer structure, or a multilayer structure of two or more kinds thereof. In a case of a multilayer structure, each layer may contain the same materials, or different materials.
  • the polishing composition according to the present invention can polish silicon nitride at a high speed, but for polycrystalline silicon, the polishing composition may be the one that does not polish the polycrystalline silicon at a high speed. Such a performance is sometimes required in a case of using a polishing composition for an application of polishing the surface of the object to be polished containing not only silicon nitride but also polycrystalline silicon.
  • the ratio of the polishing rate of silicon nitride to the polishing rate of polycrystalline silicon is preferably 2 or more, more preferably 4 or more, furthermore preferably 6 or more, and particularly preferably 8 or more.
  • the polishing composition according to the present invention is suitably used for polishing silicon nitride. Therefore, according to further another embodiment of the present invention, a polishing method including a step of polishing silicon nitride using the polishing composition according to the present invention is provided. Further, according to further another embodiment of the present invention, a method for producing a substrate including a step of polishing silicon nitride by the polishing method is also provided.
  • the apparatus and conditions used for ordinary metal polishing can be used.
  • a general polishing device there are a one-side polishing device and a double side polishing device.
  • a substrate is held by using a holder called a carrier, and while supplying a polishing composition from the above, one side of an object to be polished is polished by rotating a surface plate on which a polishing pad is attached to the surface opposite to the substrate while pressing the surface plate.
  • the object to be polished is polished by the physical action due to the friction between the polishing pad and the polishing composition, and the object to be polished, and by the chemical action on the object to be polished from the polishing composition.
  • the polishing pad a porous body such as nonwoven fabric, polyurethane, and swede can be used without any particular limitation. It is preferred that a polishing pad is processed so as to accumulate a polishing liquid.
  • polishing conditions in the polishing method according to the present invention a polishing load, a rotation speed of a surface plate, a rotation speed of a carrier, a flow rate of a polishing composition, and a polishing time can be mentioned.
  • polishing conditions are not particularly limited, but for example, the polishing load is, per unit area of the substrate, preferably 0.1 psi or more to 10 psi or less, more preferably 0.5 psi or more to 8.0 psi or less, and furthermore preferably 1.0 psi or more to 6.0 psi or less.
  • the polishing rate increases.
  • the rotation speed of a surface plate and the rotation speed of a carrier are preferably 10 to 500 rpm.
  • the supply amount of the polishing composition may be a supply amount that covers the entire substrate of an object to be polished, and may be adjusted according to the conditions such as the size of the substrate.
  • the polishing composition according to the present invention may be a one-pack type, or may also be a multi-pack type including a two-pack type. Further, the polishing composition according to the present invention may be prepared by, for example, diluting the stock solution of the polishing composition with a diluent such as water by 10 times or more.
  • Gas chromatography GC-14B (manufactured by Shimadzu Corporation) Measurement: 4 ⁇ T, of a sample is taken out using a 10 ⁇ L syringe and injected to the present apparatus. The methanol concentration is calculated from the amount of moisture and the amount of methanol, which are obtained in the measurement.
  • the silica sol obtained in the above was observed with a scanning electron microscope (SEM) (the following condition 2) ( FIG. 1 ), and when the particle size distribution was analyzed by using image analysis software (the following condition 3) based on the SEM photograph, the number distribution ratio of the microparticles having a diameter of 40% or less of the volume average particle diameter by SEM image analysis was less than 1%.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • Apparatus Scanning electron microscope 54700 (manufactured by Hitachi High-Technologies Corporation) Procedures: The one obtained by dispersing silica sol in an organic solvent and subjecting the resultant mixture to dry-solidifying on a sample table is placed in the main body, and irradiated with an electron beam at 12 kV by the present apparatus, and then ten viewing fields are observed at a magnification of 100000 times.
  • Apparatus Image analysis software MacView Ver. 4 (manufactured by Mountech Co., Ltd.) Procedures: Using the taken SEM photograph, 500 particles are counted by the present apparatus. After that, the volume average particle diameter based on Heywood diameter (equivalent circle diameter) was calculated, and the particle size distribution in terms of the proportion of the number of particles is calculated.
  • Apparatus Transmission electron microscope HD-2700 (manufactured by Hitachi High-Technologies Corporation) Procedures: Silica sol is dispersed in an organic solvent, the resultant mixture is added dropwise on a surface of dedicated Cu mesh and dry-solidified, the dry-solidified one is irradiated with an electron beam at 200 kV by the present apparatus, and then ten viewing fields are observed at a magnification of 400000 times.
  • the amount of the impurities of 13 metal elements in the anionic silica sol thus obtained was measured with the metal impurity concentration measurement (the following condition 5) by an inductively coupled plasma (ICP) emission spectrometer, and in addition, the amount of the supernatant Si in the obtained anionic silica sol was measured with the supernatant Si concentration measurement (the following condition 6) by an inductively coupled plasma (ICP) emission spectrometer.
  • ICP inductively coupled plasma
  • the supernatant Si concentration is a value obtained by measuring the supernatant, which has been obtained by centrifuging the anionic silica sol, by an inductively coupled plasma (ICP) emission spectrometer, and the fact that this value varies with time means that aggregation of microparticles and incorporation of microparticles to large particles are generated, and the physical properties are changed.
  • ICP inductively coupled plasma
  • ICPS-8100 manufactured by Shimadzu Corporation
  • Procedures 10 ml of a sample is collected, into the collected sample, 3 ml of nitric acid and 10 ml of hydrofluoric acid are added, and the resultant mixture is evaporated and dry-solidified. After the dry-solidifying, 0.5 ml of nitric acid and around 20 ml of ultrapure water are added, and the resultant mixture is heated until steam is generated. The whole amount is recovered, adjusted to 50 g with ultrapure water, and measurements are performed by using each of the above apparatuses.
  • Centrifugal device High-performance high-speed refrigerated centrifuge, Avanti HP-30I (manufactured by Beckman Coulter, Inc.)
  • ICP measuring apparatus ICP-AES SPS3510 (manufactured by Hitachi High-Tech Science Corporation) Procedures: Silica sol is placed in a dedicated resin tube, and centrifugation is performed at 26000 rpm for 2 hours. Subsequently, a calibration curve is drawn with Si standard samples of 0, 25, 50, and 75 ppm by ICP-AES, 1 g of the supernatant after the centrifugation is collected, and diluted with ultrapure water by 20 times, and then measurement is performed by the present apparatus.
  • Apparatus 300 mm CMP one-side polishing device (manufactured by Ebara Corporation) Polishing pad: polyurethane foam Polishing wafer: 300 mm SiN bare wafer Rotation speed: 60 rpm
  • the polishing rate is calculated by dividing each wafer thickness difference obtained by measuring before and after the polishing by using an optical interference-type film thickness measuring device by the polishing time.
  • Comparative Example 1 Corresponding to Example 1 of JP 2010-269985 A
  • TMOS tetramethoxysilane
  • the silica sol obtained in the above was heated and concentrated to 3500 mL under normal pressure.
  • the methanol concentration of the mixture was measured in the similar manner as in the above, 71% by mass was obtained.
  • the silica sol obtained in the above was observed with a scanning electron microscope (SEM) in the similar manner as in the above ( FIG. 3 ), and when the particle size distribution was analyzed by using image analysis software based on the SEM photograph, the number distribution ratio of the microparticles having a diameter of 40% or less of the volume average particle diameter by SEM image analysis was 47.6%.
  • TEM transmission electron microscope
  • the amount of the impurities of 13 metal elements was measured with the metal impurity concentration measurement by an inductively coupled plasma (ICP) emission spectrometer, and in addition, the amount of the supernatant Si in the obtained anionic silica sol was measured with the supernatant Si concentration measurement by an inductively coupled plasma (ICP) emission spectrometer.
  • ICP inductively coupled plasma
  • the amount of supernatant Si in the anionic silica sol thus obtained was measured with the metal impurity concentration measurement by an ICP emission spectrometer in the similar manner as in the above, and further, in the similar manner as in the above, a test of the SiN polishing rate was performed with a 300 mm CMP one-side polishing device (manufactured by Ebara Corporation).
  • the amount of the supernatant Si (depending on the amount of microparticles) contained in the obtained silica sol was also reduced, and further, the amount of supernatant Si did not change also with time.
  • the ratio of the SiN polishing rate of the polishing composition of Example 1 also does not change with time, and the polishing composition is excellent extremely in the stability with time.
  • the silica sol contained in the polishing composition produced by the production methods of Comparative Examples 1 and 2 had unevenness on the surfaces of the silica particles, and the amount of the microparticles adhered to the SiN wafer was also large.
  • the amount of the supernatant Si contained in the obtained silica sol was also large, and further, the amount of supernatant Si changed with time.
  • the ratio of the SiN polishing rate of the polishing composition of Comparative Examples 1 to 2 also fluctuates largely with time, and the polishing composition is inferior in the stability with time.
  • Example 2 Ni 0.1 0.1 0.2 Cu ⁇ 0.05 ⁇ 0.05 ⁇ 0.05 Zn ⁇ 5 ⁇ 5 ⁇ 5 Ag ⁇ 3 ⁇ 3 ⁇ 3 Al ⁇ 5 ⁇ 5 ⁇ 5 Ca 2.1 1.9 1.7 Cr ⁇ 5 ⁇ 5 ⁇ 5 Fe ⁇ 10 ⁇ 10 ⁇ 10 K ⁇ 55 ⁇ 55 ⁇ 55 Mg ⁇ 3 ⁇ 3 ⁇ 3 Na 12.6 13.2 12.4 Pb ⁇ 14 ⁇ 14 ⁇ 14 Ti ⁇ 5 ⁇ 5 ⁇ 5 ⁇ 5

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JPWO2016117559A1 (ja) 2017-10-26
CN107207945A (zh) 2017-09-26
US20190144728A1 (en) 2019-05-16
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US10570322B2 (en) 2020-02-25
TWI763621B (zh) 2022-05-11

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