WO2015052988A1 - Agent de polissage, ensemble d'agent de polissage et procédé pour base de polissage - Google Patents

Agent de polissage, ensemble d'agent de polissage et procédé pour base de polissage Download PDF

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Publication number
WO2015052988A1
WO2015052988A1 PCT/JP2014/071232 JP2014071232W WO2015052988A1 WO 2015052988 A1 WO2015052988 A1 WO 2015052988A1 JP 2014071232 W JP2014071232 W JP 2014071232W WO 2015052988 A1 WO2015052988 A1 WO 2015052988A1
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WIPO (PCT)
Prior art keywords
polishing
abrasive
mass
insulating material
cmp
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PCT/JP2014/071232
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English (en)
Japanese (ja)
Inventor
友洋 岩野
知里 吉川
利明 阿久津
久貴 南
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日立化成株式会社
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Publication of WO2015052988A1 publication Critical patent/WO2015052988A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • 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
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • C09D5/4476—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications comprising polymerisation in situ
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/44—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications
    • C09D5/448—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes for electrophoretic applications characterised by the additives used
    • 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
    • C09K3/1454—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
    • H01L21/31—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
    • 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
    • H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
    • H01L21/71—Manufacture of specific parts of devices defined in group H01L21/70
    • H01L21/76—Making of isolation regions between components
    • H01L21/762—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers
    • H01L21/76224—Dielectric regions, e.g. EPIC dielectric isolation, LOCOS; Trench refilling techniques, SOI technology, use of channel stoppers using trench refilling with dielectric materials

Definitions

  • the present invention relates to an abrasive, an abrasive set, and a method for polishing a substrate.
  • the present invention relates to a polishing agent, a polishing agent set, and a substrate polishing method used in a substrate surface flattening step, which is a semiconductor element manufacturing technique. More particularly, the present invention relates to a polishing agent, a polishing agent set, and a substrate polishing method used in a flattening process of a shallow trench isolation (STI) insulating material, a premetal insulating material, an interlayer insulating material, and the like.
  • STI shallow trench isolation
  • CMP Chemical Mechanical Polishing
  • silica-based abrasive containing silica (silicon oxide) particles such as fumed silica and colloidal silica as abrasive grains.
  • silica silica
  • colloidal silica as abrasive grains.
  • Silica-based abrasives are characterized by high versatility, and a wide variety of materials can be polished regardless of insulating materials and conductive materials by appropriately selecting the abrasive content, pH, additives, and the like.
  • abrasives containing cerium compound particles as abrasive grains mainly for insulating materials such as silicon oxide there is an increasing demand for abrasives containing cerium compound particles as abrasive grains mainly for insulating materials such as silicon oxide.
  • a cerium oxide-based abrasive containing cerium oxide (ceria) particles as abrasive grains can polish silicon oxide at high speed even with a lower abrasive grain content than a silica-based abrasive (see, for example, Patent Documents 1 and 2 below).
  • a stopper (a polishing stop layer including a stopper material) disposed on the convex portion of the substrate having the concavo-convex pattern, and the substrate and the stopper so as to fill the concave portion of the concavo-convex pattern.
  • a laminated body having an insulating material (e.g., silicon oxide) disposed on the substrate is polished. In such polishing, the polishing of the insulating material is stopped by a stopper. That is, the polishing of the insulating material is stopped when the stopper is exposed.
  • Patent Document 8 listed below uses an abrasive containing hydroxide particles of a tetravalent metal element and at least one of a cationic polymer and a polysaccharide, using silicon nitride as a stopper material. Polishing the insulating material is disclosed.
  • an insulating material is polished using polysilicon as a stopper material by using an abrasive containing hydroxide particles of a tetravalent metal element and polyvinyl alcohol having a saponification degree of 95 mol% or less. Is disclosed.
  • JP-A-10-106994 Japanese Patent Application Laid-Open No. 08-022970 International Publication No. 2002/067309 International Publication No. 2012/070541 International Publication No. 2012/070542 JP 2006-249129 A International Publication No. 2012/070544 International Publication No. 2009/131133 International Publication No. 2010/143579
  • the present invention is intended to solve these problems, and an object thereof is to provide an abrasive, an abrasive set, and a substrate polishing method that can improve the polishing selectivity of an insulating material with respect to a stopper material. .
  • the present inventor uses a combination of abrasive grains containing a hydroxide of a tetravalent metal element, an ⁇ -glucose polymer having a specific weight average molecular weight, and a cationic polymer to insulate the stopper material. It has been found that the polishing selectivity of the material is further increased as compared with the prior art.
  • the abrasive according to the present invention contains water, abrasive grains containing a hydroxide of a tetravalent metal element, an ⁇ -glucose polymer, and a cationic polymer, and the weight of the ⁇ -glucose polymer
  • the average molecular weight is 20.0 ⁇ 10 3 or less.
  • weight average molecular weight is defined as the weight average molecular weight determined by gel permeation chromatography (GPC) analysis.
  • the polishing agent according to the present invention can improve the polishing selectivity of the insulating material with respect to the stopper material.
  • silicon nitride has been used for many years, but in recent years, processes using polysilicon have been increasing. In this case, it is necessary to suppress the polishing rate of polysilicon from the viewpoint of increasing the polishing selectivity of the insulating material with respect to polysilicon.
  • conventional abrasives do not have sufficient polishing selectivity for insulating materials relative to both silicon nitride and polysilicon, and there is room for improvement.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved regardless of whether silicon nitride or polysilicon is used as the stopper material.
  • the polishing agent according to the present invention in the CMP technology for flattening the shallow trench isolation insulating material, the premetal insulating material, the interlayer insulating material, etc., the insulating material can be reduced with low polishing scratches while highly flattening the insulating material. It can also be polished.
  • dishing may occur in the CMP process or the like for forming STI conventionally.
  • Dishing is a phenomenon in which an insulating material embedded in a recess is excessively removed, and a part of the surface to be polished is recessed like a dish. Therefore, in order to improve flatness, it is necessary to suppress the progress of dishing.
  • the present inventor uses a combination of an abrasive containing a hydroxide of a tetravalent metal element, a specific ⁇ -glucose polymer, a cationic polymer, and an amino group-containing sulfonic acid compound as a stopper. It has been found that the polishing selectivity of the insulating material with respect to the material is further enhanced as compared with the conventional material and the progress of dishing can be suppressed.
  • the abrasive according to the present invention may further include an amino group-containing sulfonic acid compound, and the degree of polymerization of ⁇ -glucose in the ⁇ -glucose polymer may be 3 or more.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved and the progress of dishing can be suppressed.
  • the surface to be polished can be flattened by suppressing the progress of dishing while maintaining the polishing selectivity of the insulating material with respect to the stopper material.
  • the ⁇ -glucose polymer preferably has at least one selected from the group consisting of a structural unit represented by the following formula (IA) and a structural unit represented by the following formula (IB). .
  • the polishing selectivity of the insulating material with respect to the stopper material can be further enhanced.
  • the tetravalent metal element hydroxide preferably contains a cerium hydroxide.
  • the pH of the abrasive according to the present invention is preferably 3.0 or more and 7.0 or less.
  • the insulating material can be polished at a suitable polishing rate, and the polishing selectivity of the insulating material to the stopper material can be further increased.
  • One embodiment of the present invention relates to the use of the abrasive for polishing a surface to be polished containing silicon oxide. That is, one embodiment of the abrasive according to the present invention is preferably used for polishing a surface to be polished containing silicon oxide.
  • the constituents of the abrasive are stored separately in a first liquid and a second liquid, the first liquid contains abrasive grains and water, and the second liquid is ⁇ .
  • - contains glucose polymer, cationic polymer and water.
  • the second liquid may contain an amino group-containing sulfonic acid compound.
  • the method for polishing a substrate according to the present invention may comprise a step of polishing the surface to be polished of the substrate using the abrasive. According to such a method for polishing a substrate, the same effects as those of the abrasive according to the present invention can be obtained.
  • the substrate polishing method according to the present invention includes a step of polishing a surface to be polished of the substrate using an abrasive obtained by mixing the first liquid and the second liquid in the abrasive set. May be. According to such a method for polishing a substrate, the same effects as those of the abrasive according to the present invention can be obtained.
  • a polishing agent capable of improving the polishing selectivity of the insulating material with respect to the stopper material.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved in the polishing of the insulating material using the stopper.
  • the polishing selectivity of the insulating material with respect to the stopper material can be improved and the progress of dishing can be suppressed.
  • the polishing selectivity of the insulating material with respect to the stopper material is improved. Can be made.
  • the polishing selectivity of the insulating material with respect to the stopper material is increased. It is possible to improve and suppress the progress of dishing.
  • an abrasive or an abrasive set for polishing an insulating material using a stopper.
  • process is not limited to an independent process, and is included in the term if the intended action of the process is achieved even when it cannot be clearly distinguished from other processes. It is.
  • a numerical range indicated by using “to” indicates a range including the numerical values described before and after “to” as the minimum value and the maximum value, respectively.
  • this embodiment includes the first embodiment and the second embodiment.
  • polishing agent which concerns on this embodiment is a composition which touches a to-be-polished surface at the time of grinding
  • the abrasive according to the first embodiment contains at least water, abrasive grains containing a hydroxide of a tetravalent metal element, an ⁇ -glucose polymer, and a cationic polymer.
  • the abrasive according to the second embodiment includes water, abrasive grains containing a hydroxide of a tetravalent metal element, an ⁇ -glucose polymer having a degree of polymerization of ⁇ -glucose of 3 or more, a cationic polymer, And at least an amino group-containing sulfonic acid compound.
  • abrasive grains containing a hydroxide of a tetravalent metal element an ⁇ -glucose polymer having a degree of polymerization of ⁇ -glucose of 3 or more
  • a cationic polymer a cationic polymer
  • the essential components and components that can be optionally added are described below.
  • polishing agent which concerns on this embodiment contains the abrasive grain containing the hydroxide of a tetravalent metal element.
  • the “tetravalent metal element hydroxide” is a compound containing a tetravalent metal (M 4+ ) and at least one hydroxide ion (OH ⁇ ).
  • the hydroxide of the tetravalent metal element may contain an anion other than the hydroxide ion (for example, nitrate ion NO 3 ⁇ , sulfate ion SO 4 2 ⁇ ).
  • a hydroxide of a tetravalent metal element may contain an anion (for example, nitrate ion NO 3 ⁇ , sulfate ion SO 4 2 ⁇ ) bonded to the tetravalent metal element.
  • an anion for example, nitrate ion NO 3 ⁇ , sulfate ion SO 4 2 ⁇
  • the abrasive grains containing a hydroxide of the tetravalent metal element are more reactive with an insulating material (for example, silicon oxide) than conventional abrasive grains made of silica or ceria, and the insulating material can be removed at a high polishing rate. Can be polished.
  • examples of other abrasive grains that can be used in combination with the abrasive grains containing a hydroxide of a tetravalent metal element include silica particles, alumina particles, and ceria particles.
  • composite particles of tetravalent metal element hydroxide particles and silica particles can be used as abrasive grains containing a tetravalent metal element hydroxide.
  • the lower limit of the content of the tetravalent metal element hydroxide in the abrasive is preferably 80% by mass or more, more preferably 90% by mass or more, and still more preferably 95% by mass or more based on the total mass of the abrasive grains. 98 mass% or more is especially preferable, and 99 mass% or more is very preferable.
  • the abrasive grains are composed of hydroxide particles of the tetravalent metal element from the viewpoint of easy preparation of an abrasive and further excellent polishing properties (substantially 100% by mass of the abrasive grains is the tetravalent metal). Elemental hydroxide particles).
  • Tetravalent metal element hydroxides are rare earth element hydroxides and zirconium hydroxides from the viewpoint of suppressing the generation of polishing scratches on the surface to be polished while further improving the polishing selectivity of the insulating material with respect to the stopper material. It is preferable to include at least one selected from the group consisting of
  • the tetravalent metal element is preferably a rare earth element from the viewpoint of further improving the polishing rate of the insulating material.
  • Examples of rare earth elements that can be tetravalent include lanthanoids such as cerium, praseodymium, and terbium, and cerium is more preferable from the viewpoint of easy availability and excellent polishing rate.
  • a rare earth element hydroxide and a zirconium hydroxide may be used in combination, and two or more rare earth elements may be selected and used.
  • a method for producing abrasive grains containing a hydroxide of a tetravalent metal element a technique of mixing a salt containing a tetravalent metal element and an alkali solution can be used. This method is described in, for example, “Science of rare earths” [edited by Adiya Ginya, Kagaku Dojin, 1999], pages 304-305.
  • a method for producing abrasive grains containing a hydroxide of a tetravalent metal element that is most suitable for the abrasive according to this embodiment is described in Patent Document 7. The descriptions of these documents are incorporated herein by reference.
  • M is preferably chemically active cerium (Ce).
  • Basic compounds in the alkaline solution include organic bases such as imidazole, tetramethylammonium hydroxide (TMAH), guanidine, triethylamine, pyridine, piperidine, pyrrolidine, chitosan; ammonia, potassium hydroxide, sodium hydroxide, calcium hydroxide.
  • organic bases such as imidazole, tetramethylammonium hydroxide (TMAH), guanidine, triethylamine, pyridine, piperidine, pyrrolidine, chitosan; ammonia, potassium hydroxide, sodium hydroxide, calcium hydroxide.
  • Inorganic bases such as Among these, from the viewpoint of further improving the polishing rate of the insulating material, at least one selected from the group consisting of ammonia and imidazole is preferable, and imidazole is more preferable.
  • Abrasive grains containing a hydroxide of a tetravalent metal element synthesized by the above method can be washed to remove metal impurities.
  • a method for cleaning the abrasive grains a method of repeating solid-liquid separation several times by centrifugation or the like can be used.
  • the abrasive grains can be washed in steps such as centrifugation, dialysis, ultrafiltration, and ion removal using an ion exchange resin.
  • abrasive grains obtained above are aggregated, it is preferable to disperse them in water by an appropriate method.
  • a method for dispersing abrasive grains in water which is the main dispersion medium, mechanical dispersion treatment using a homogenizer, an ultrasonic disperser, a wet ball mill, or the like can be used in addition to the dispersion treatment using a normal stirrer.
  • the dispersion method and the particle size control method for example, the method described in Chapter 3 “Latest Development Trends and Selection Criteria of Various Dispersers” in “Dispersion Technology Complete Collection” [Information Organization, July 2005] Can be used.
  • the water content of the tetravalent metal element can also be reduced by reducing the electrical conductivity (for example, 500 mS / m or less) of the dispersion containing abrasive grains containing a hydroxide of the tetravalent metal element by performing the above-described cleaning treatment.
  • the dispersibility of the abrasive grains containing the oxide can be increased. Therefore, the cleaning process may be applied as a dispersion process, and the cleaning process and the dispersion process may be used in combination.
  • the lower limit of the average grain size of the abrasive grains is preferably 1 nm or more, more preferably 2 nm or more, and further preferably 3 nm or more from the viewpoint of obtaining a more suitable polishing rate for the insulating material.
  • the upper limit of the average grain size of the abrasive grains is preferably 300 nm or less, more preferably 250 nm or less, and even more preferably 200 nm or less, from the viewpoint of further suppressing scratches on the surface to be polished. From the above viewpoint, the average grain size of the abrasive grains is more preferably 1 nm or more and 300 nm or less.
  • the “average particle diameter” of the abrasive grains means the average secondary particle diameter of the abrasive grains.
  • the average particle diameter of the abrasive grains can be measured, for example, by a photon correlation method for a slurry or a slurry in a polishing agent set described later.
  • the average particle size of the abrasive grains can be measured by, for example, device name: Zetasizer 3000HS manufactured by Malvern Instruments, device name: N5 manufactured by Beckman Coulter, and the like.
  • the measuring method using N5 can be performed as follows.
  • an aqueous dispersion in which the content of abrasive grains is adjusted to 0.2% by mass is prepared, and this aqueous dispersion is about 4 mL (L is “liter” in a 1 cm square cell. ) Put the cell in the device.
  • the value obtained by setting the refractive index of the dispersion medium to 1.33, the viscosity to 0.887 mPa ⁇ s, and measuring at 25 ° C. can be adopted as the average particle diameter of the abrasive grains.
  • the lower limit of the content of the abrasive grains is preferably 0.01% by mass or more and more preferably 0.02% by mass or more based on the total mass of the abrasive from the viewpoint of obtaining a more suitable polishing rate for the insulating material.
  • the upper limit of the content of the abrasive is preferably 20% by mass or less, more preferably 15% by mass or less, and further preferably 10% by mass or less, based on the total mass of the abrasive, from the viewpoint of increasing the storage stability of the abrasive.
  • 5 mass% or less is particularly preferable, 1 mass% or less is very preferable, and 0.5 mass% or less is very preferable.
  • the content of the abrasive grains is more preferably 0.01% by mass or more and 20% by mass or less based on the total mass of the abrasive.
  • polishing agent which concerns on this embodiment contains an additive.
  • the “additive” refers to a polishing agent other than water and abrasive grains in order to adjust polishing characteristics such as polishing rate and polishing selectivity; abrasive characteristics such as abrasive dispersibility and storage stability. Refers to the substance contained.
  • the abrasive according to this embodiment contains an ⁇ -glucose polymer as the first additive.
  • ⁇ -glucose polymer is defined as a polymer (for example, sugar) having a degree of polymerization of ⁇ -glucose of 2 or more unless otherwise specified.
  • a polymer (for example, sugar) having a degree of polymerization of ⁇ -glucose of 3 or more is used.
  • the first additive has an effect of suppressing an excessive increase in the polishing rate of the stopper material (for example, silicon nitride and polysilicon). Regarding the reason why this effect is obtained, it is presumed that the first additive covers the stopper, thereby suppressing the progress of polishing by the abrasive grains and suppressing the polishing rate from becoming excessively high.
  • Examples of ⁇ -glucose polymer include amylose; amylopectin; dextran; dextrin; maltodextrin; cyclodextrins such as ⁇ -cyclodextrin, ⁇ -cyclodextrin, ⁇ -cyclodextrin; maltose, isomaltose, maltotriose, stachyose, etc.
  • Examples include oligosaccharides.
  • the ⁇ -glucose polymer used in the second embodiment includes amylose; amylopectin; dextran; dextrin; maltodextrin; cyclodextrins such as ⁇ -cyclodextrin, ⁇ -cyclodextrin, and ⁇ -cyclodextrin; maltotriose, stachyose And oligosaccharides.
  • the DE value of the ⁇ -glucose polymer (for example, the value according to the “LANE-EYNON method”) is preferably 13 to 50 from the viewpoint of further enhancing the polishing selectivity of the insulating material with respect to the stopper material.
  • dextrin having an aldehyde group at the end of the decomposition product obtained by decomposition of starch referred to as “general dextrin” for distinction from other dextrins
  • general dextrin for distinction from other dextrins
  • difficult to be partially decomposed in the process of starch decomposition Examples include indigestible dextrin collected by purifying the product; reduced dextrin in which the aldehyde end is reduced by hydrogenation and changed to a hydroxyl group. Any of these compounds can be used as the dextrin.
  • the ⁇ -glucose polymer used in the second embodiment includes “NSD” series manufactured by Sanei Saccharification Co., Ltd .; “Sandek” series manufactured by Sanwa Starch Co., Ltd .; “H-PDX” manufactured by Matsutani Chemical Co. “Max 1000”, “TK-16”, “Fiber Sol 2”, “Fiber Sol 2H” and the like.
  • the structural unit represented by the following formula (IA) and the following formula It is preferable to have at least one selected from the group consisting of structural units represented by IB), more preferably at least one selected from the group consisting of dextrin and maltose (dextrin is more preferable in the second embodiment) ).
  • the arrangement thereof is not limited and may be regular or random.
  • the ⁇ -glucose polymer is preferably at least one selected from the group consisting of dextrin and maltose from the viewpoint of excellent versatility (dextrin is more preferred in the second embodiment).
  • the ⁇ -glucose polymer preferably has at least one structural unit represented by the following formulas (II) to (VII), and more preferably has a structural unit represented by the formula (III).
  • the polishing selectivity of the insulating material with respect to the stopper material can be further enhanced.
  • the lower limit of the degree of polymerization of ⁇ -glucose is 2 or more, preferably 3 or more, and more preferably 5 or more from the viewpoint of further improving the polishing selectivity of the insulating material with respect to the stopper material.
  • the upper limit of the degree of polymerization of ⁇ -glucose is preferably 120 or less, more preferably 90 or less, and even more preferably 60 or less, from the viewpoint that a good polishing rate of the insulating material can be easily obtained.
  • the lower limit of the polymerization degree of ⁇ -glucose is 3 or more, preferably 5 or more, more preferably 7 or more from the viewpoint of further enhancing the polishing selectivity of the insulating material with respect to the stopper material and suppressing the progress of dishing. More preferred is 10 or more.
  • the upper limit of the degree of polymerization of ⁇ -glucose is preferably 120 or less, more preferably 90 or less, and even more preferably 60 or less, from the viewpoint that a good polishing rate of the insulating material can be easily obtained.
  • the “degree of polymerization of ⁇ -glucose” is defined as the number of structural units derived from ⁇ -glucose in one molecule.
  • the formula (IA) and the formula (I— B) is the total number of structural units represented by the formulas (II) to (VII) in one molecule.
  • the ⁇ -glucose polymer can be used alone or in combination of two or more for the purpose of adjusting polishing characteristics such as polishing selectivity.
  • the upper limit of the weight average molecular weight of the first additive is 20.0 ⁇ 10 3 from the viewpoint of obtaining a good polishing rate of the insulating material (for example, silicon oxide) and improving the polishing selectivity of the insulating material with respect to the stopper material. It is as follows.
  • the upper limit of the weight average molecular weight of the first additive is 20.0 ⁇ from the viewpoint of obtaining a better polishing rate of the insulating material (for example, silicon oxide) and further improving the polishing selectivity of the insulating material with respect to the stopper material.
  • the weight average molecular weight of the first additive in the first embodiment is preferably less than 10 3, more preferably 18.0 ⁇ 10 3 or less, more preferably 15.0 ⁇ 10 3 or less, particularly preferably 12.0 ⁇ 10 3 or less, very preferably 10.0 ⁇ 10 3 or less.
  • the lower limit of the weight average molecular weight of the first additive in the first embodiment is preferably 250 or more, more preferably 350 or more, still more preferably 500 or more, from the viewpoint of further improving polishing selectivity and flatness. 0 ⁇ 10 3 or more is particularly preferable, and 1.5 ⁇ 10 3 or more is extremely preferable. From the above viewpoint, the weight average molecular weight of the first additive in the first embodiment is more preferably 250 or more and 20.0 ⁇ 10 3 or less.
  • the lower limit of the weight average molecular weight of the first additive in the second embodiment is preferably 350 or more, more preferably 500 or more, still more preferably 800 or more. 0 ⁇ 10 3 or more is particularly preferable, and 1.5 ⁇ 10 3 or more is extremely preferable. From the above viewpoint, the weight average molecular weight of the first additive in the second embodiment is more preferably 350 or more and 20.0 ⁇ 10 3 or less.
  • a weight average molecular weight can be measured on condition of the following by the gel permeation chromatography method (GPC) using the calibration curve of a standard polystyrene, for example.
  • the lower limit of the content of the first additive is preferably 0.01% by mass or more, more preferably 0.1% by mass or more, based on the total mass of the abrasive, from the viewpoint of further improving polishing selectivity and flatness. Preferably, 0.3% by mass or more is more preferable, and 0.5% by mass or more is particularly preferable.
  • the upper limit of the content of the first additive is preferably 5.0% by mass or less, more preferably 3.0% by mass or less, based on the total mass of the abrasive, from the viewpoint of obtaining an appropriate polishing rate of the insulating material. 2.0 mass% or less is still more preferable.
  • the content of the first additive is more preferably 0.01% by mass or more and 5.0% by mass or less based on the total mass of the abrasive.
  • the sum total of content of each compound satisfy
  • polishing agent which concerns on this embodiment contains a cationic polymer as a 2nd additive other than said 1st additive.
  • the “cationic polymer” is a polymer having a cationic group or a group that can be ionized into a cationic group in a main chain or a side chain.
  • the cationic polymer has an effect of suppressing an excessive increase in the polishing rate of the stopper material (for example, silicon nitride and polysilicon) when used in combination with the first additive. Also, there is an effect of increasing the polishing rate of the insulating material (for example, silicon oxide) without deteriorating the flatness.
  • the polishing rate of the stopper material can be suppressed, and the first additive excessively covers the insulating material to reduce the polishing rate of the insulating material. It is considered that the polishing rate of the insulating material can be improved by suppressing this.
  • the cationic polymer interacts with the first additive so that the first additive appropriately coats the insulating material, thereby improving the polishing rate of the convex portion of the insulating material and insulating. In order to suppress the polishing rate of the concave portions of the material, it is considered that high flatness can be maintained.
  • the cationic polymer is at least one selected from the group consisting of an allylamine polymer, a diallylamine polymer, a vinylamine polymer, and an ethyleneimine polymer from the viewpoint of obtaining further excellent polishing selectivity of the insulating material with respect to the stopper material.
  • These polymers can be obtained by polymerizing at least one monomer component selected from the group consisting of allylamine, diallylamine, vinylamine, ethyleneimine, and derivatives thereof.
  • the polymer may have a structural unit derived from a monomer component other than allylamine, diallylamine, vinylamine, ethyleneimine and derivatives thereof, acrylamide, dimethylacrylamide, diethylacrylamide, hydroxyethylacrylamide, acrylic acid, It may have a structural unit derived from methyl acrylate, methacrylic acid, maleic acid, sulfur dioxide or the like.
  • Cationic polymers include allylamine, diallylamine, vinylamine, ethyleneimine homopolymer (polyallylamine, polydiallylamine, polyvinylamine, polyethyleneimine); homopolymers of derivatives of these monomer components; allylamine, diallylamine, Examples thereof include a copolymer having a structural unit derived from vinylamine, ethyleneimine or a derivative thereof. In the copolymer, the arrangement of structural units is arbitrary.
  • the cationic polymer may form a salt.
  • salts include organic acid salts such as acetic acid; halogen acid salts such as hydrochloride and bromate; inorganic acid salts such as phosphate, sulfate, nitrate, and carbonate.
  • the allylamine polymer is a polymer having a structure obtained by polymerizing allylamine or a derivative thereof, and examples thereof include a polymer having a structural unit represented by the following formula (VIII) or (IX).
  • the allylamine derivative include alkoxycarbonylated allylamine, methylcarbonylated allylamine, aminocarbonylated allylamine, ureated allylamine and the like.
  • each R independently represents a hydrogen atom or a monovalent organic group
  • X ⁇ represents an anion.
  • the diallylamine polymer is a polymer having a structure obtained by polymerizing diallylamine or a derivative thereof, and examples thereof include a polymer having a structural unit represented by the following formula (X) or (XI).
  • diallylamine derivatives include methyl diallylamine, diallyldimethylammonium salt, diallylmethylethylammonium salt, acylated diallylamine, aminocarbonylated diallylamine, alkoxycarbonylated diallylamine, aminothiocarbonylated diallylamine, hydroxyalkylated diallylamine, and the like.
  • ammonium salts include ammonium chloride. [In the formula, each R independently represents a hydrogen atom or a monovalent organic group, and X ⁇ represents an anion. ]
  • the vinylamine polymer is a polymer having a structure obtained by polymerizing vinylamine or a derivative thereof, and examples thereof include a polymer having a structural unit represented by the following formula (XII).
  • Examples of the vinylamine derivative include alkylated vinylamine, amidated vinylamine, ethylene oxideated vinylamine, propylene oxided vinylamine, alkoxylated vinylamine, carboxymethylated vinylamine, acylated vinylamine, and ureaated vinylamine.
  • R shows a hydrogen atom or a monovalent organic group each independently.
  • the ethyleneimine polymer is a polymer having a structure obtained by polymerizing ethyleneimine or a derivative thereof, and examples thereof include a polymer having a structural unit represented by the following formula (XIII).
  • Examples of the ethyleneimine derivative include aminoethylated acrylic polymer, alkylated ethyleneimine, ureaated ethyleneimine, propylene oxideated ethyleneimine and the like. [Wherein, R represents a hydrogen atom or a monovalent organic group. ]
  • Examples of the monovalent organic group represented by R in formulas (VIII) to (XIII) include an alkyl group such as a methyl group, an ethyl group, and a propyl group; and an amino group such as a primary amino group, a secondary amino group, and a tertiary amino group An amide group and the like.
  • X ⁇ in formula (IX) and formula (XI) is an organic acid ion such as acetate ion; halide ion such as chloride ion or bromide ion; inorganic such as phosphate ion, sulfate ion, nitrate ion or carbonate ion An acid ion etc. are mentioned.
  • cationic polymers examples include acrylic polymers such as cation-modified polyacrylamide and cation-modified polydimethylacrylamide; copolymers of dialkylenetriamines such as diethylenetriamine and other monomers (dicyandiamide / diethylenetriamine copolymer, etc.) Dicyandiamide / dialkylenetriamine copolymer, etc.); polysaccharides such as chitosan, chitosan derivatives, cation-modified cellulose, cation-modified dextran; obtained by polymerizing monomers derived from structural units constituting these compounds A copolymer or the like may be used.
  • acrylic polymers such as cation-modified polyacrylamide and cation-modified polydimethylacrylamide
  • copolymers of dialkylenetriamines such as diethylenetriamine and other monomers (dicyandiamide / diethylenetriamine copolymer, etc.) Dicyandiamide / dialkylenetriamine copolymer, etc
  • cationic polymers from the viewpoint of further improving the polishing selectivity of the insulating material (for example, silicon oxide) with respect to the stopper material (for example, silicon nitride and polysilicon), and from the viewpoint of further improving the polishing rate of the insulating material, Preferred are at least one selected from the group consisting of homopolymers of allylamine, homopolymers of allylamine derivatives, polymers having structural units derived from diallyldimethylammonium salts, and dicyandiamide / diethylenetriamine copolymers. More preferred is at least one selected from the group consisting of diallyldimethylammonium chloride.
  • Cationic polymers can be used alone or in combination of two or more for the purpose of adjusting polishing properties such as polishing selectivity and flatness.
  • the lower limit of the weight average molecular weight of the cationic polymer is preferably 100 or more, more preferably 300 or more from the viewpoint of further improving the polishing selectivity of the insulating material (for example, silicon oxide) with respect to the stopper material (for example, silicon nitride and polysilicon). 500 or more is more preferable.
  • the upper limit of the weight average molecular weight of the cationic polymer is preferably 1000 ⁇ 10 3 or less from the viewpoint of further improving the polishing selectivity of the insulating material (eg, silicon oxide) with respect to the stopper material (eg, silicon nitride and polysilicon), and 800 ⁇ 10 3 or less is more preferable, and 500 ⁇ 10 3 or less is more preferable.
  • the weight average molecular weight of the cationic polymer is more preferably 100 or more and 1000 ⁇ 10 3 or less.
  • the weight average molecular weight of the cationic polymer can be measured by the same method as the weight average molecular weight of the first additive.
  • the lower limit of the content of the cationic polymer is preferably 0.0001% by mass or more, more preferably 0.0002% by mass or more, based on the total mass of the abrasive, from the viewpoint of further improving polishing selectivity and flatness. 0.0005% by mass or more is more preferable, and 0.001% by mass or more is particularly preferable.
  • the upper limit of the content of the cationic polymer is preferably 1% by mass or less, more preferably 0.5% by mass or less, more preferably 0.1% by mass, based on the total mass of the abrasive, from the viewpoint of further excellent polishing selectivity.
  • the content of the cationic polymer is more preferably 0.0001% by mass or more and 1% by mass or less based on the total mass of the abrasive.
  • the polishing selectivity of the insulating material with respect to the stopper material for example, silicon nitride and polysilicon
  • the flatness the content of the cationic polymer can be improved. It is preferable to adjust appropriately according to the type or filming conditions.
  • the abrasive according to this embodiment includes the first additive and the second additive for the purpose of adjusting polishing characteristics such as polishing speed; abrasive characteristics such as abrasive dispersibility and storage stability.
  • a third additive may be further contained.
  • the amino group-containing sulfonic acid compound described later is not included in the third additive referred to here.
  • Examples of the third additive include carboxylic acid and amino acid. These may be used alone or in combination of two or more. By using these compounds, the balance between abrasive dispersibility and polishing characteristics is improved. In addition, although an amino acid has a carboxyl group, the compound corresponding to an amino acid is excluded as carboxylic acid.
  • Carboxylic acid has the effect of stabilizing the pH and further improving the polishing rate of the insulating material.
  • the carboxylic acid include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, and lactic acid.
  • Amino acids have the effect of improving the dispersibility of abrasive grains containing a hydroxide of a tetravalent metal element and further improving the polishing rate of the insulating material.
  • amino acids arginine, lysine, aspartic acid, glutamic acid, asparagine, glutamine, histidine, proline, tyrosine, tryptophan, serine, threonine, glycine, ⁇ -alanine, ⁇ -alanine, methionine, cysteine, phenylalanine, leucine, valine, isoleucine Etc.
  • the content of the third additive is based on the total mass of the abrasive from the viewpoint of obtaining the additive effect of the third additive while suppressing sedimentation of the abrasive grains. 0.001 mass% or more and 10 mass% or less are preferable. In addition, when using a some compound as a 3rd additive, it is preferable that the sum total of content of each compound satisfy
  • the polishing agent according to the second embodiment contains an amino group-containing sulfonic acid compound as another additive different from the first additive and the second additive.
  • the abrasive according to the first embodiment may contain an amino group-containing sulfonic acid compound as another additive different from the first additive and the second additive.
  • the “amino group-containing sulfonic acid compound” means at least one selected from the group consisting of a sulfonic acid group (sulfo group, —SO 3 H) and a sulfonic acid group (—SO 3 M: M is a metal atom), an amino group (—NH 2 ) in one molecule.
  • Examples of the metal atom M of the sulfonate group include alkali metals such as Na and K, and alkaline earth metals such as Mg and Ca.
  • the amino group-containing sulfonic acid in combination with the first additive and the second additive, polishing of the insulating material after exposure to the stopper (for example, the insulating material embedded in the recess) is suppressed, and the dishing progresses. Therefore, high flatness can be obtained.
  • Amino group-containing sulfonic acid compounds may be used alone or in combination of two or more for the purpose of adjusting polishing properties such as polishing selectivity and flatness.
  • the mechanism by which the amino group-containing sulfonic acid compound suppresses the progress of dishing is presumed as follows.
  • the sulfonyl group (—S ( ⁇ O) 2 —) is considered to form a protective layer on the surface of the insulating material by forming a hydrogen bond with a hydroxyl group (—OH) on the surface of the insulating material (eg, silicon oxide). .
  • a hydroxyl group eg, silicon oxide
  • the amino group also has hydrogen bonding ability, but it is considered that a highly polar sulfonyl group acts preferentially.
  • the reason why the amino group-containing sulfonic acid compound selectively protects only the concave portion is that the adsorption force to the material to be polished is weak and the amino group-containing sulfonic acid compound is detached at the convex portion where a higher load is applied. Is considered to progress.
  • the amino group-containing sulfonic acid compound preferably has a small number of sulfonic acid groups and sulfonic acid groups and amino groups present in one molecule.
  • the total of sulfonic acid groups and sulfonic acid groups present in one molecule is preferably 5 or less, more preferably 3 or less, still more preferably 2 or less, and particularly preferably 1.
  • the amino group present in one molecule is preferably 5 or less, more preferably 3 or less, still more preferably 2 or less, and particularly preferably 1.
  • the upper limit of the molecular weight of the amino group-containing sulfonic acid compound is preferably 1000 or less, more preferably 800 or less, and even more preferably 500 or less.
  • the lower limit of the molecular weight of the amino group-containing sulfonic acid compound is, for example, 97 or more.
  • the amino group-containing sulfonic acid compound is preferably a compound having one amino group and one sulfonic acid group or one sulfonic acid group in one molecule, specifically, sulfamic acid (also known as amidosulfuric acid); Aminomethanesulfonic acid, aminoethanesulfonic acid (1-aminoethanesulfonic acid, 2-aminoethanesulfonic acid (also known as taurine), etc.), aminoalkylsulfonic acid such as aminopropanesulfonic acid; aminobenzenesulfonic acid (alternic acid (also known as alternative acid) 2-aminobenzenesulfonic acid), metanilic acid (also known as 3-aminobenzenesulfonic acid), sulfanilic acid (also known as 4-aminobenzenesulfonic acid)), aminonaphthalenesulfonic acid and the like; salts thereof; Etc.
  • sulfamic acid also known as
  • amino group-containing sulfonic acid compound aminoalkyl sulfonic acid and fragrance are used from the viewpoint of further improving the flatness by further suppressing the polishing of the insulating material after exposure to the stopper (for example, the insulating material embedded in the recess).
  • group aminosulfonic acids At least one selected from the group consisting of group aminosulfonic acids is preferred, at least one selected from the group consisting of aminoethanesulfonic acid, alternic acid, metanilic acid and sulfanilic acid is more preferred, from aminoethanesulfonic acid and sulfanilic acid More preferably, at least one selected from the group consisting of
  • the lower limit of the content of the amino group-containing sulfonic acid compound is preferably 0.0005% by mass or more, more preferably 0.001% by mass or more, based on the total mass of the abrasive. 0.002% by mass or more is more preferable, and 0.005% by mass or more is particularly preferable.
  • the upper limit of the content of the amino group-containing sulfonic acid compound is preferably 0.2% by mass or less, more preferably 0.1% by mass or less, based on the total mass of the abrasive, from the viewpoint of further improving the polishing rate of the insulating material.
  • the content of the amino group-containing sulfonic acid compound is more preferably 0.0005% by mass or more and 0.2% by mass or less based on the total mass of the abrasive.
  • the content of the amino group-containing sulfonic acid compound is determined from the viewpoint of further improving the polishing rate of the insulating material, the polishing selectivity of the insulating material with respect to the stopper material, and the flatness (kind or filming conditions). It is preferable to adjust appropriately according to.
  • the polishing agent according to this embodiment has flatness, in-plane uniformity, polishing selectivity of silicon oxide with respect to silicon nitride (silicon oxide polishing rate / silicon nitride polishing rate), and polishing selectivity of silicon oxide with respect to polysilicon (
  • a water-soluble polymer may be contained for the purpose of adjusting polishing characteristics such as (silicon oxide polishing rate / polysilicon polishing rate).
  • the “water-soluble polymer” is defined as a polymer that dissolves 0.1 g or more in 100 g of water at 25 ° C. The first additive and the second additive are not included in the “water-soluble polymer”.
  • the water-soluble polymer is not particularly limited, and is a polysaccharide such as alginic acid, pectinic acid, carboxymethylcellulose, agar, curdlan, guar gum, or the like; a vinyl polymer such as polyvinyl alcohol, polyvinyl pyrrolidone, or polyacrolein; Examples thereof include glycerin polymers such as glycerin derivatives.
  • the water-soluble polymers can be used alone or in combination of two or more.
  • the lower limit of the content of the water-soluble polymer is 0 on the basis of the total mass of the abrasive from the viewpoint of obtaining the effect of adding the water-soluble polymer while suppressing sedimentation of the abrasive grains.
  • 0.0001 mass% or more is preferable, 0.001 mass% or more is more preferable, and 0.01 mass% or more is still more preferable.
  • the upper limit of the content of the water-soluble polymer is preferably 5% by mass or less, preferably 1% by mass based on the total mass of the abrasive, from the viewpoint of obtaining the effect of adding the water-soluble polymer while suppressing sedimentation of the abrasive grains.
  • the content of the water-soluble polymer is more preferably 0.0001% by mass or more and 5% by mass or less based on the total mass of the abrasive.
  • the sum total of content of each compound satisfy
  • the lower limit of the pH of the abrasive according to the first embodiment is preferably 3.0 or more, more preferably 3.5 or more, still more preferably 3.8 or more, from the viewpoint of further improving the polishing rate of the insulating material. 0.0 or more is particularly preferable.
  • the upper limit of the pH is preferably 7.0 or less, more preferably 6.5 or less, and even more preferably 6.0 or less from the viewpoint of further improving the polishing rate of the insulating material. From the above viewpoint, the pH of the abrasive is more preferably 3.0 or more and 7.0 or less.
  • the pH is defined as the pH at a liquid temperature of 25 ° C.
  • the lower limit of the pH of the abrasive according to the second embodiment is preferably 3.0 or more, more preferably 3.5 or more, still more preferably 4.0 or more, from the viewpoint of further improving the polishing rate of the insulating material. .5 or more is particularly preferable.
  • the upper limit of the pH is preferably 7.0 or less, more preferably 6.5 or less, still more preferably 6.0 or less, and particularly preferably 5.5 or less from the viewpoint of further improving the polishing rate of the insulating material. From the above viewpoint, the pH of the abrasive is more preferably 3.0 or more and 7.0 or less.
  • the pH is defined as the pH at a liquid temperature of 25 ° C.
  • the pH of the polishing agent can be adjusted with an acid component such as an inorganic acid or an organic acid; an alkali component such as ammonia, sodium hydroxide, potassium hydroxide, tetramethylammonium hydroxide (TMAH), imidazole, or 2-methylimidazole.
  • a buffer may be added to stabilize the pH. Examples of such a buffer include acetate buffer and phthalate buffer.
  • the pH of the abrasive according to this embodiment can be measured with a pH meter (for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.). Specifically, for example, after calibrating two pH meters using a phthalate pH buffer solution (pH 4.01) and a neutral phosphate pH buffer solution (pH 6.86) as standard buffers, The value is measured after the electrode is placed in an abrasive and stabilized after 2 minutes or more. At this time, the liquid temperature of the standard buffer and the abrasive is both 25 ° C.
  • a pH meter for example, model number PHL-40 manufactured by Electrochemical Instrument Co., Ltd.
  • the abrasive according to this embodiment may be stored as a one-component abrasive containing at least abrasive grains, a first additive, a second additive, and water.
  • an additive liquid (second liquid) are mixed into a slurry and an additive liquid so that the composition of the abrasive is divided into a slurry and an additive liquid so as to become the abrasive.
  • the slurry includes at least abrasive grains and water, for example.
  • the additive liquid includes, for example, at least a first additive, a second additive, and water.
  • the first additive, the second additive, the third additive, the amino group-containing sulfonic acid compound, the water-soluble polymer, and the buffer solution are preferably included in the additive solution among the slurry and the additive solution.
  • the constituents of the abrasive are stored separately in a slurry (first liquid) and an additive liquid (second liquid), and the slurry contains abrasive grains and water, and the additive liquid May be an embodiment containing the first additive, the second additive, the amino group-containing sulfonic acid compound and water.
  • the constituents of the abrasive may be stored as an abrasive set divided into three or more liquids.
  • abrasive set slurry and additive liquid are mixed immediately before or during polishing to prepare an abrasive.
  • the one-component abrasive is stored as an abrasive stock solution with a reduced water content, and may be diluted with water immediately before or during polishing.
  • the two-component abrasive set is stored as a slurry storage solution and an additive storage solution with a reduced water content, and may be diluted with water immediately before or during polishing.
  • a method of supplying the abrasive onto the polishing surface plate a method of feeding and supplying the abrasive directly; a storage solution for abrasive and water are sent through separate pipes, A method in which these are combined, mixed and supplied; a method in which an abrasive stock solution and water are mixed and supplied in advance can be used.
  • the polishing rate can be adjusted by arbitrarily changing the combination of these two components.
  • methods for supplying the abrasive onto the polishing surface plate include the following methods. For example, the slurry and the additive liquid are sent through separate pipes, and these pipes are combined, mixed and supplied; the slurry storage liquid, the additive liquid storage liquid and water are sent through separate pipes, A method in which these are combined and mixed and supplied; a method in which slurry and additive solution are mixed and supplied in advance; and a method in which slurry storage solution, additive solution storage solution and water are mixed in advance and supplied it can.
  • polishing agent set on a polishing surface plate, respectively can also be used.
  • the surface to be polished is polished using an abrasive obtained by mixing the slurry and the additive liquid on the polishing platen.
  • the substrate polishing method according to the present embodiment may include a polishing step of polishing the surface to be polished of the substrate using the one-part polishing agent, and the slurry and additive liquid in the polishing agent set are mixed. You may provide the grinding
  • the substrate polishing method according to the present embodiment may be a substrate polishing method having an insulating material and a stopper material.
  • the one-part abrasive or the slurry and additive liquid in the abrasive set A polishing step of selectively polishing the insulating material with respect to the stopper material may be provided using an abrasive obtained by mixing the above.
  • the base body may have, for example, a member containing an insulating material and a member (stopper) containing a stopper material.
  • the stopper material is preferably at least one selected from the group consisting of polysilicon and silicon nitride.
  • the stopper material is more preferably polysilicon.
  • silicon nitride is more preferable as the stopper material.
  • the abrasive is supplied between the material to be polished and the polishing pad in a state where the material to be polished of the substrate having the material to be polished is pressed against the polishing pad (polishing cloth) of the polishing surface plate.
  • the material to be polished is polished by relatively moving the substrate and the polishing surface plate.
  • at least a part of the material to be polished is removed by polishing.
  • Examples of the substrate to be polished include a substrate.
  • a material to be polished is formed on a substrate for manufacturing a semiconductor element (for example, a semiconductor substrate on which an STI pattern, a gate pattern, a wiring pattern, etc. are formed).
  • a substrate is mentioned.
  • materials to be polished include insulating materials such as silicon oxide; stopper materials such as polysilicon and silicon nitride.
  • the material to be polished may be a single material or a plurality of materials. When a plurality of materials are exposed on the surface to be polished, they can be regarded as materials to be polished.
  • the material to be polished may be in the form of a film (film to be polished), and may be a silicon oxide film, a polysilicon film, a silicon nitride film, or the like.
  • the material to be polished (such as an insulating material such as silicon oxide) formed on such a substrate is polished with the above-mentioned abrasive and the excess portions are removed to eliminate the unevenness of the surface of the material to be polished, A smooth surface is obtained over the entire surface of the abrasive material.
  • the abrasive according to this embodiment is preferably used for polishing a surface to be polished containing silicon oxide.
  • the insulating material in can be polished.
  • the stopper material constituting the stopper is a material whose polishing rate is lower than that of the insulating material, and polysilicon, silicon nitride and the like are preferable.
  • polishing method for a semiconductor substrate on which an insulating material is formed.
  • a polishing apparatus a general polishing apparatus having a holder capable of holding a substrate such as a semiconductor substrate having a surface to be polished and a polishing surface plate to which a polishing pad can be attached.
  • a motor or the like whose rotation speed can be changed is attached to each of the holder and the polishing surface plate.
  • the polishing apparatus include an APPLIED MATERIALS polishing apparatus (trade name: Mira-3400, Reflexion LK) and a polishing apparatus manufactured by Ebara Corporation (trade name: F REX-300).
  • polishing pad general nonwoven fabric, foam, non-foam, etc.
  • material of the polishing pad include polyurethane, acrylic, polyester, acrylic-ester copolymer, polytetrafluoroethylene, polypropylene, polyethylene, poly-4-methylpentene, cellulose, cellulose ester, polyamide (for example, nylon (trade name) and Aramid), polyimide, polyimide amide, polysiloxane copolymer, oxirane compound, phenol resin, polystyrene, polycarbonate, epoxy resin and the like can be used.
  • foamed polyurethane and non-foamed polyurethane are particularly preferable from the viewpoint of obtaining a further excellent polishing rate and flatness.
  • the polishing pad may be grooved so that the abrasive is collected.
  • the rotation speed of the polishing platen is preferably 200 min ⁇ 1 (rpm) or less so that the semiconductor substrate does not pop out, and the polishing pressure (processing load) applied to the semiconductor substrate causes polishing scratches. From the viewpoint of sufficiently suppressing this, 100 kPa or less is preferable.
  • the surface of a polishing pad is always covered with the abrasive
  • the semiconductor substrate after polishing is preferably washed well under running water to remove particles adhering to the substrate.
  • dilute hydrofluoric acid or ammonia water may be used in addition to pure water, and a brush may be used to improve cleaning efficiency.
  • a brush may be used to improve cleaning efficiency.
  • the abrasive, the abrasive set and the polishing method according to this embodiment can be suitably used for forming STI.
  • the lower limit of the polishing selection ratio of the insulating material (eg, silicon oxide) to the stopper material (eg, silicon nitride and polysilicon) is preferably 50 or more, more preferably 120 or more, still more preferably 180 or more, and particularly preferably 200 or more.
  • polishing agent which concerns on one Embodiment, 210 or more are very preferable.
  • the polishing selection ratio is less than 50, the polishing rate of the insulating material with respect to the polishing rate of the stopper material is small, and it is difficult to stop polishing at a predetermined position when forming the STI.
  • the polishing selection ratio is 50 or more, the polishing can be easily stopped, which is more suitable for the formation of STI.
  • the abrasive, the abrasive set and the polishing method according to this embodiment can also be used for polishing a premetal insulating material.
  • a premetal insulating material in addition to silicon oxide, for example, phosphorus-silicate glass or boron-phosphorus-silicate glass is used, and further, silicon oxyfluoride, fluorinated amorphous carbon, and the like can be used.
  • the abrasive, the abrasive set and the polishing method according to this embodiment can be applied to materials other than insulating materials such as silicon oxide.
  • materials include high dielectric constant materials such as Hf-based, Ti-based, and Ta-based oxides; semiconductor materials such as silicon, amorphous silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, and organic semiconductors; GeSbTe Inorganic conductive materials such as ITO; polymer resins such as polyimides, polybenzoxazoles, acrylics, epoxies, and phenols.
  • the polishing agent, the polishing agent set, and the polishing method according to the present embodiment are not only film-like objects to be polished, but also various types composed of glass, silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, sapphire, plastic, and the like. It can also be applied to substrates.
  • the polishing agent, the polishing agent set, and the polishing method according to the present embodiment are not only for manufacturing semiconductor elements, but also for image display devices such as TFTs and organic ELs; optical parts such as photomasks, lenses, prisms, optical fibers, and single crystal scintillators Optical elements such as optical switching elements and optical waveguides; light emitting elements such as solid lasers and blue laser LEDs; and magnetic storage devices such as magnetic disks and magnetic heads.
  • the container containing the metal salt aqueous solution was placed in a water tank filled with water.
  • the water temperature of the water tank was adjusted to 40 [° C.] using an external circulation device COOLNICS circulator (manufactured by Tokyo Rika Kikai Co., Ltd. (EYELA), product name cooling thermopump CTP101).
  • COOLNICS circulator manufactured by Tokyo Rika Kikai Co., Ltd. (EYELA), product name cooling thermopump CTP101
  • the alkali solution was mixed in the container at a mixing speed of 8.5 ⁇ 10 ⁇ 6 [m 3 / min].
  • a slurry precursor 1 containing abrasive grains containing tetravalent cerium hydroxide was obtained.
  • the pH of the slurry precursor 1 was 2.2.
  • the aqueous metal salt solution was stirred using a three-blade pitch paddle with a total length of 5 cm.
  • the obtained slurry precursor 1 was ultrafiltered while being circulated, and the ion content was removed until the conductivity was 50 mS / m or less. 2 was obtained.
  • the ultrafiltration was performed using a liquid level sensor while adding water so that the water level of the tank containing the slurry precursor 1 was kept constant.
  • the nonvolatile content of the slurry precursor 2 was calculated.
  • a cerium hydroxide slurry stock solution was collected and diluted with water so that the abrasive grain content was 0.2% by mass to obtain a measurement sample (aqueous dispersion).
  • a measurement sample aqueous dispersion
  • About 4 mL of the measurement sample was placed in a 1 cm square cell, and the cell was installed in a device name: N5 manufactured by Beckman Coulter.
  • the dispersion medium was set to have a refractive index of 1.33 and a viscosity of 0.887 mPa ⁇ s, measured at 25 ° C., and the displayed average particle size value was defined as the average secondary particle size of the abrasive grains. The result was 21 nm.
  • Example A1 100 g of an additive stock solution containing 10% by weight of maltose [manufactured by Sanwa Starch Co., Ltd., Sanmalto-S], 0.08% by weight of 2-methylimidazole, 0.06% by weight of acetic acid and 89.86% by weight of water Then, 50 g of a cerium hydroxide slurry storage solution, 820 g of water, and 30 g of an aqueous solution containing 0.1% by mass of polydiallyldimethylammonium chloride [Senka Co., Ltd., Unisense FPA1000L] as a cationic polymer are mixed.
  • an abrasive for CMP 1000 g having the composition shown in Table 1 was prepared.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of maltose, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • the weight average molecular weight of the said maltose was measured on condition of the following, it was 259 (theoretical value from a chemical structure is 342).
  • Example A2 Maltose as a dextrin [Sandek # 300, manufactured by Sanwa Starch Co., Ltd. DE value (Dextrose Equivalent value): 31 to 36 (value according to “LANE-EYNON method”, the same shall apply hereinafter), moisture: 4% by mass or less.
  • a polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A1 except that all were changed to the manufacturer's nominal values.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • the dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Example A3 Maltose as a dextrin [Sandek # 180, manufactured by Sanwa Starch Co., Ltd. DE value: 22 to 25, moisture: 5% by mass or less.
  • a polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A1 except that all were changed to the manufacturer's nominal values.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride. When the weight average molecular weight of the dextrin was measured in the same manner as in Example A1, it was 5.4 ⁇ 10 3 .
  • the dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Example A4 Maltose as a dextrin [Sandek # 100, manufactured by Sanwa Starch Co., Ltd. DE value: 13 to 16, water content: 5% by mass or less.
  • a polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A1 except that all were changed to the manufacturer's nominal values.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride. When the weight average molecular weight of the dextrin was measured in the same manner as in Example A1, it was 18.4 ⁇ 10 3 .
  • the dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Example A5 Maltose as dextrin [manufactured by Sanei Saccharification Co., Ltd., NSD # 700 (powder type). A polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A1, except that the DE value was changed to 17 to 21 (manufacturer nominal value).
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride. When the weight average molecular weight of the dextrin was measured in the same manner as in Example A1, it was 7.9 ⁇ 10 3 .
  • the dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Example A6 A polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A5 except that polydiallyldimethylammonium chloride was changed to a dicyandiamide / diethylenetriamine copolymer [Senka Co., Ltd., Unisense KHP10L].
  • the abrasive for CMP contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of a dicyandiamide / diethylenetriamine copolymer.
  • Example A7 When preparing 100 g of the stock solution for additive solution, the amount of acetic acid added was changed to 0.1% by mass, and the amount of water increased by acetic acid was reduced. A polishing slurry for CMP having the following composition was prepared.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • Example A8 Maltose reduced dextrin [Matsuya Chemical Co., Ltd., H-PDX. The water content is 5% by mass or less. ]
  • a polishing slurry for CMP having the composition shown in Table 1 was prepared in the same manner as in Example A1 except that the above was changed.
  • the abrasive for CMP contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride. When the weight average molecular weight of the reduced dextrin was measured by the same method as in Example A1, it was 2.0 ⁇ 10 3 .
  • the reduced dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Glucose [Wako Pure Chemical Industries, Ltd., Wako first grade D (+)-glucose. Molecular weight: 130] 100 g of additive solution containing 10% by mass, 0.08% by mass of 2-methylimidazole, 0.06% by mass of acetic acid and 89.86% by mass of water, and a storage solution for cerium hydroxide slurry By mixing 50 g and 850 g of water, an abrasive for CMP (1000 g) having the composition described in Table 2 was prepared. The CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 1.0% by mass of glucose.
  • Glucose [Wako Pure Chemical Industries, Ltd., Wako first grade D (+)-glucose. Molecular weight: 130] 100 g of additive solution containing 10% by mass, 0.08% by mass of 2-methylimidazole, 0.06% by mass of acetic acid and 89.86% by mass of water, and a storage solution for cerium hydroxide slurry 50 g, 820 g of water, and 30 g of an aqueous solution containing 0.1% by mass of polydiallyldimethylammonium chloride [manufactured by Senka Co., Ltd., Unisense FPA1000L] as a cationic polymer, are described in Table 2.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of glucose, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • Comparative Example A3 A polishing slurry for CMP having the composition described in Table 2 was prepared in the same manner as in Comparative Example A1, except that glucose was changed to dextrin (Sandex # 300, manufactured by Sanwa Starch Co., Ltd.).
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 1.0% by mass of dextrin.
  • Comparative Example A4 A polishing slurry for CMP having the composition shown in Table 2 was prepared in the same manner as in Comparative Example A1, except that glucose was changed to dextrin [Sandek # 180, manufactured by Sanwa Starch Co., Ltd.].
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 1.0% by mass of dextrin.
  • a polishing slurry for CMP having the composition shown in Table 2 was prepared in the same manner as in Comparative Example A1 except that glucose was changed to dextrin [manufactured by Sanei Saccharification Co., Ltd., NSD # 700].
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 1.0% by mass of dextrin.
  • Glucose dextrin [Sandex # 30, manufactured by Sanwa Starch Co., Ltd. DE value: 3 to 7, moisture: 5% by mass or less.
  • a CMP polishing slurry having the composition shown in Table 2 was prepared in the same manner as in Comparative Example A2 except that all were changed to the manufacturer's nominal values.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • the weight average molecular weight of the dextrin was measured by the same method as in Example A1, and found to be 147 ⁇ 10 3 .
  • Glucose was dextrin [NSD # 300, manufactured by Sanei Saccharification Co., Ltd.
  • a polishing slurry for CMP having the composition shown in Table 2 was prepared in the same manner as in Comparative Example A2, except that the DE value was changed to 10 to 12 (manufacturer nominal value).
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride. In addition, it was 20.4 * 10 ⁇ 3 > when the weight average molecular weight of the said dextrin was measured by the method similar to Example A1.
  • PH Measurement temperature: 25 ⁇ 5 ° C
  • Measuring device manufactured by Electrochemical Instrument Co., Ltd., model number PHL-40 Measurement method: After calibrating two points using a standard buffer (phthalate pH buffer, pH: 4.01 (25 ° C.); neutral phosphate pH buffer, pH 6.86 (25 ° C.)), The electrode was placed in a CMP abrasive and the pH after the passage of 2 minutes or more and stabilized was measured with the measuring device. The results are shown in Tables 1 and 2.
  • a measurement sample (aqueous dispersion). About 4 mL of the measurement sample was placed in a 1 cm square cell, and the cell was installed in a device name: N5 manufactured by Beckman Coulter. The dispersion medium was set to have a refractive index of 1.33 and a viscosity of 0.887 mPa ⁇ s, measured at 25 ° C., and the displayed average particle size value was defined as the average particle size (average secondary particle size). As a result, the average particle diameter was in the range of 14 to 16 nm in both Examples and Comparative Examples.
  • the substrate to be polished was polished under the following polishing conditions using each of the CMP polishing agents.
  • polishing device Mirra-3400 (manufactured by APPLIED MATERIALS) ⁇ CMP abrasive flow rate: 200 mL / min
  • Substrate to be polished a blanket wafer on which a pattern is not formed, a substrate in which a silicon oxide film having a thickness of 1 ⁇ m (1000 nm) is formed on a silicon substrate by a plasma CVD method, and polysilicon having a thickness of 0.2 ⁇ m (200 nm)
  • a substrate in which a film was formed on a silicon substrate by a CVD method and a substrate in which a silicon nitride film having a thickness of 0.2 ⁇ m (200 nm) was formed on a silicon substrate by a CVD method were used.
  • polishing pad foamed polyurethane resin having closed cells (Rohm and Haas Japan, model number IC1010), Shore D hardness: 60
  • Polishing pressure 20 kPa (3.0 psi) ⁇ Number of rotations of substrate and polishing surface plate:
  • Substrate / polishing surface plate 93/87 min ⁇ 1 (rpm) ⁇
  • Polishing time 1 min -Cleaning and drying of wafer: After CMP treatment, cleaning with a PVA brush (polyvinyl alcohol brush) was performed, followed by drying with a spin dryer.
  • PVA brush polyvinyl alcohol brush
  • Polishing rate of each film to be polished (silicon oxide film, silicon nitride film and polysilicon film) polished and cleaned under the above conditions (silicon oxide film polishing rate: SiO 2 RR, silicon nitride film polishing rate: SiNRR, polysilicon
  • the film polishing rate: p-SiRR) was determined from the following formula. Further, polishing selection ratios SiO 2 RR / SiNRR and SiO 2 RR / p-SiRR were determined.
  • Tables 1 and 2 show the measurement results obtained in Examples A1 to A8 and Comparative Examples A1 to A7.
  • Example A1 SiO 2 RR is 478 nm / min, SiNRR is 1.4 nm / min, p-SiRR is 1.0 nm / min, polishing selectivity SiO 2 RR / SiNRR is 341, and polishing selectivity SiO 2 RR / p -SiRR was 478, and the polishing selectivity ratio of the insulating material to the silicon nitride film and the polysilicon film was higher than those of Comparative Examples A1 to A7.
  • Example A2 the SiO 2 RR was 438 nm / min, the SiNRR was 0.5 nm / min, the polishing selection ratio SiO 2 RR / SiNRR was 876, and the polishing selection ratio was higher than those of Comparative Examples A1 to A7.
  • Example A3 SiO 2 RR was 355 nm / min, SiNRR was 0.6 nm / min, p-SiRR was 0.8 nm / min, polishing selectivity SiO 2 RR / SiNRR was 592, and polishing selectivity SiO 2 RR / p -SiRR was 444, and the polishing selectivity ratio of the insulating material to the silicon nitride film and the polysilicon film was higher than those of Comparative Examples A1 to A7.
  • Example A4 SiO 2 RR was 316 nm / min, SiNRR was 1.8 nm / min, p-SiRR was 0.5 nm / min, polishing selectivity SiO 2 RR / SiNRR was 176, polishing selectivity SiO 2 RR / p -SiRR was 632, and the polishing selectivity ratio of the insulating material to the silicon nitride film and the polysilicon film was higher than those of Comparative Examples A1 to A7.
  • Example A5 SiO 2 RR was 356 nm / min, SiNRR was 0.6 nm / min, p-SiRR was 0.4 nm / min, polishing selectivity SiO 2 RR / SiNRR was 593, and polishing selectivity SiO 2 RR / p -SiRR was 890, and the polishing selectivity ratio of the insulating material to the silicon nitride film and the polysilicon film was higher than those of Comparative Examples A1 to A7.
  • Example A6 SiO 2 RR was 316 nm / min, SiNRR was 1.2 nm / min, polishing selectivity SiO 2 RR / SiNRR was 263, and the polishing selectivity was higher than those of Comparative Examples A1 to A7.
  • Example A7 SiO 2 RR was 203 nm / min, SiNRR was 0.8 nm / min, polishing selectivity SiO 2 RR / SiNRR was 254, and the polishing selectivity was higher than those of Comparative Examples A1 to A7.
  • Example A8 SiO 2 RR was 383 nm / min, SiNRR was 0.5 nm / min, polishing selectivity SiO 2 RR / SiNRR was 766, and the polishing selectivity was higher than those of Comparative Examples A1 to A7.
  • the SiO 2 RR was 11 nm / min
  • the SiNRR was 77 nm / min
  • the polishing selection ratio SiO 2 RR / SiNRR was 0.1.
  • SiO 2 RR was 429 nm / min
  • SiNRR was 45 nm / min
  • p-SiRR was 2.1 nm / min
  • polishing selectivity SiO 2 RR / SiNRR was 10
  • polishing selectivity SiO 2 RR / p-SiRR. was 204.
  • SiO 2 RR was 128 nm / min
  • SiNRR was 33 nm / min
  • polishing selectivity SiO 2 RR / SiNRR was 3.9.
  • the SiO 2 RR was 159 nm / min
  • the SiNRR was 17 nm / min
  • the polishing selectivity ratio SiO 2 RR / SiNRR was 9.4.
  • SiO 2 RR was 3.9 nm / min
  • SiNRR was 1.4 nm / min
  • polishing selectivity SiO 2 RR / SiNRR was 2.8.
  • the SiO 2 RR was 2.1 nm / min
  • the SiNRR was 0.8 nm / min
  • the polishing selectivity ratio SiO 2 RR / SiNRR was 2.6.
  • the abrasive for CMP includes 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, and 0.02% of sulfanilic acid. Contains by mass%. It was 2.0 * 10 ⁇ 3 > when the weight average molecular weight of the said reduced dextrin was measured on condition of the following.
  • the reduced dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB).
  • Example B2 Example B1 except that the content of sulfanilic acid was changed to 0.03% by mass, the content of 2-methylimidazole was changed to 0.02% by mass, and the content of acetic acid was changed to 0.005% by mass
  • an abrasive for CMP having the composition shown in Table 3 was prepared.
  • the abrasive for CMP includes 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, and 0.03% of sulfanilic acid. Contains by mass%.
  • Example B3 Reduced dextrin is resistant to digestion [Miyagen Co., Ltd., Fiber Sol 2H. Moisture: 5% by mass or less. Manufacturer's nominal value], sulfanilic acid content changed to 0.01 mass%, 2-methylimidazole content changed to 0.012 mass%, and acetic acid content changed to 0.005 mass%
  • a polishing slurry for CMP having the composition shown in Table 3 was prepared in the same manner as in Example B1 except that the above was changed.
  • the CMP polishing slurry was 0.05% by weight of abrasive grains containing cerium hydroxide, 1.0% by weight of indigestible dextrin, 0.003% by weight of polydiallyldimethylammonium chloride, and 0.02% of sulfanilic acid. Contains 01% by mass.
  • the indigestible dextrin has at least one selected from the group consisting of a structural unit represented by the formula (IA) and a structural unit represented by the formula (IB). In addition, it was 2.5 * 10 ⁇ 3 > when the weight average molecular weight of the said indigestible dextrin was measured by the method similar to Example B1.
  • Example B4 CMP of the composition described in Table 3 was carried out in the same manner as in Example B3 except that the content of sulfanilic acid was changed to 0.02% by mass and the content of 2-methylimidazole was changed to 0.018% by mass.
  • a polishing slurry was prepared.
  • the CMP polishing slurry was 0.05% by weight of abrasive grains containing cerium hydroxide, 1.0% by weight of indigestible dextrin, 0.003% by weight of polydiallyldimethylammonium chloride, and 0.02% of sulfanilic acid. Contains 02% by mass.
  • Example B5 Example B3 except that 0.01% by mass of sulfanilic acid was changed to 0.02% by mass of 2-aminoethanesulfonic acid (taurine) and the content of 2-methylimidazole was changed to 0.08% by mass.
  • an abrasive for CMP having the composition shown in Table 3 was prepared.
  • the abrasive for CMP includes 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of indigestible dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, 2-aminoethanesulfone. Contains 0.02% by weight of acid.
  • Example B6 The abrasive content was changed to 0.02 mass%, the sulfanilic acid content was changed to 0.06 mass%, the 2-methylimidazole content was changed to 0.033 mass%, and the acetic acid content was changed.
  • a polishing slurry for CMP having the composition shown in Table 3 was prepared in the same manner as in Example B1, except that the amount was changed to 0.005% by mass.
  • the abrasive for CMP is 0.02% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, and 0.06% of sulfanilic acid. Contains by mass%.
  • the abrasive for CMP contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of D (+)-glucose, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • Example B7 For CMP having the composition shown in Table 4 in the same manner as in Example B1, except that sulfanilic acid was changed to 2-acrylamido-2-methylpropanesulfonic acid and the acetic acid content was changed to 0.005% by mass.
  • An abrasive was prepared.
  • the CMP abrasive is 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, 2-acrylamido-2- It contains 0.02% by mass of methylpropanesulfonic acid.
  • Example B8 Example B1 except that the content of 2-methylimidazole was changed to 0.08% by mass, the content of acetic acid was changed to 0.005% by mass, and an abrasive for CMP was prepared without using sulfanilic acid. Similarly, an abrasive for CMP having the composition shown in Table 4 was prepared. The abrasive for CMP contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • Example B2 A polishing slurry for CMP having the composition shown in Table 4 was prepared in the same manner as in Example B8 except that the reduced dextrin was changed to polyoxyethylene styrenated phenyl ether [Daiichi Kogyo Seiyaku Co., Ltd., Neugen EA207D]. did.
  • the abrasive for CMP contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of polyoxyethylene styrenated phenyl ether, and 0.003% by mass of polydiallyldimethylammonium chloride.
  • Example B3 Without using a cationic polymer, the sulfanilic acid content was changed to 0.01% by mass, the acetic acid content was changed to 0.005% by mass, and the 2-methylimidazole content was 0.013% by mass.
  • a polishing slurry for CMP having the composition shown in Table 4 was prepared in the same manner as in Example B1, except that the percentage was changed to%.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, and 0.01% by mass of sulfanilic acid.
  • Example B4 A polishing slurry for CMP having the composition shown in Table 5 was prepared in the same manner as in Example B1, except that the content of acetic acid was changed to 0.005% by mass without using reduced dextrin and cationic polymer. did.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 0.02% by mass of sulfanilic acid.
  • Example B5 A CMP abrasive having the composition shown in Table 5 was prepared in the same manner as in Example B8 except that the abrasive for CMP was prepared without using reduced dextrin.
  • the CMP abrasive contains 0.05% by mass of abrasive grains containing cerium hydroxide and 0.003% by mass of polydiallyldimethylammonium chloride.
  • the abrasive for CMP includes 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of polyoxyethylene styrenated phenyl ether, 0.003% by mass of polydiallyldimethylammonium chloride, sulfanilic acid Is contained in an amount of 0.02% by mass.
  • Example B9 CMP of the composition described in Table 5 was performed in the same manner as in Example B8 except that 0.02% by mass of p-toluenesulfonic acid was added and the content of 2-methylimidazole was changed to 0.017% by mass.
  • a polishing slurry was prepared.
  • the CMP polishing slurry comprises 0.05% by weight abrasive grains containing cerium hydroxide, 1.0% by weight reduced dextrin, 0.003% by weight polydiallyldimethylammonium chloride, and p-toluenesulfonic acid. Contains 0.02% by mass.
  • Example B10 The same procedure as in Example B9 except that p-toluenesulfonic acid was changed to glycine (the content was not changed and was 0.02% by mass), and the content of 2-methylimidazole was changed to 0.008% by mass.
  • an abrasive for CMP having the composition shown in Table 5 was prepared.
  • the CMP abrasive is 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of reduced dextrin, 0.003% by mass of polydiallyldimethylammonium chloride, and 0.02% by mass of glycine. %contains.
  • Example B11 Table 5 shows the same as in Example B2, except that the reduced dextrin was changed to maltose [Sanmalto-S, manufactured by Sanwa Starch Co., Ltd.] (content is 1.0% by mass without change).
  • An abrasive for CMP having the composition described above was prepared.
  • the abrasive for CMP includes 0.05% by mass of abrasive grains containing cerium hydroxide, 1.0% by mass of maltose, 0.003% by mass of polydiallyldimethylammonium chloride, and 0.03% by mass of sulfanilic acid. contains.
  • the theoretical value of the molecular weight of maltose is 342.30, it was 259 when the weight average molecular weight of the said maltose was measured by the method similar to Example B1.
  • PH Measurement temperature: 25 ⁇ 5 ° C
  • Measuring device manufactured by Electrochemical Instrument Co., Ltd., model number PHL-40 Measurement method: After calibrating two points using a standard buffer (phthalate pH buffer, pH: 4.01 (25 ° C.); neutral phosphate pH buffer, pH 6.86 (25 ° C.)), The electrode was placed in a CMP abrasive and the pH after the passage of 2 minutes or more and stabilized was measured with the measuring device. The results are shown in Tables 3-5.
  • a measurement sample (aqueous dispersion). About 4 mL of the measurement sample was placed in a 1 cm square cell, and the cell was installed in a device name: N5 manufactured by Beckman Coulter. The dispersion medium was set to have a refractive index of 1.33 and a viscosity of 0.887 mPa ⁇ s, measured at 25 ° C., and the displayed average particle size value was defined as the average particle size (average secondary particle size). As a result, in both the examples and the comparative examples, the average particle size was in the range of 10 to 30 nm.
  • Example B6 Reflexion LK (manufactured by APPLIED MATERIALS) was used, and in other examples and comparative examples, FREX-300 (manufactured by Ebara Corporation) was used.
  • ⁇ CMP abrasive flow rate 200 mL / min
  • Substrate to be polished a blanket wafer on which a pattern is not formed, a substrate in which a silicon oxide film having a thickness of 1 ⁇ m (1000 nm) is formed on a silicon substrate by a plasma CVD method, and a silicon nitride having a thickness of 0.2 ⁇ m (200 nm) A substrate in which a film was formed on a silicon substrate by a CVD method was used.
  • the polishing rate (silicon oxide film polishing rate: SiO 2 RR, silicon nitride film polishing rate: SiNRR) of each film to be polished (silicon oxide film, silicon nitride film) polished and cleaned under the above conditions was obtained from the following formula. . Further, the polishing selection ratio SiO 2 RR / SiNRR was determined. In addition, the film thickness difference of each to-be-polished film
  • formula film thickness apparatus (Filmetrics company make, brand name: F80). (Polishing rate: RR) (Thickness difference of each film to be polished before and after polishing (nm)) / (Polishing time (min))
  • Polishing apparatus The same polishing apparatus as that used for polishing the blanket wafer was used.
  • Pattern wafer As a pattern wafer on which a simulated pattern was formed, a 764 wafer (trade name, diameter: 300 mm) manufactured by SEMATECH was used.
  • a silicon nitride film is stacked on a silicon substrate as a stopper, a trench is formed in an exposure process, and a silicon oxide film is formed as an insulating film on the silicon substrate and the silicon nitride film so as to fill the silicon nitride film and the trench. It was a wafer obtained by laminating (SiO 2 film).
  • the silicon oxide film was formed by the HDP (High Density Plasma) method.
  • the pattern wafer has a line (convex portion) & space (concave portion) width of 1000 ⁇ m pitch, 200 ⁇ m pitch, 100 ⁇ m pitch, and a convex pattern density of 50%.
  • the line and space is a simulated pattern in which an active portion masked with a silicon nitride film that is a convex portion and a trench portion in which a groove that is a concave portion is formed are alternately arranged.
  • the line and space has a pitch of 100 ⁇ m means that the total width of the line portion and the space portion is 100 ⁇ m.
  • the line and space is 100 ⁇ m pitch and the convex pattern density is 50%” means a pattern in which convex widths: 50 ⁇ m and concave widths: 50 ⁇ m are alternately arranged.
  • the thickness of the silicon oxide film was 600 nm on both the silicon substrate and the silicon nitride film. Specifically, the thickness of the silicon nitride film on the silicon substrate is 150 nm, the thickness of the convex portion of the silicon oxide film is 600 nm, the thickness of the concave portion of the silicon oxide film is 600 nm, and the silicon oxide film The recess depth was 500 nm (trench depth 350 nm + silicon nitride film thickness 150 nm).
  • the remaining step is 100 nm or less by polishing the wafer using a known CMP abrasive having self-stopping properties (the polishing rate decreases when the remaining step of the simulated pattern decreases).
  • the wafer in a state was used. Specifically, using an abrasive in which HS-8005-D4 manufactured by Hitachi Chemical Co., Ltd., HS-7303GP manufactured by Hitachi Chemical Co., Ltd., and water are mixed at a ratio of 2: 1.2: 6.8, A wafer in which the film thickness of the convex silicon oxide film in a 1000 ⁇ m pitch 50% density pattern was polished to 130 nm was used.
  • the amount of residual step (dishing) is obtained from the following equation: Asked.
  • the film thickness of the film to be polished before and after polishing was determined using an optical interference film thickness apparatus (manufactured by Nanometrics, trade name: Nanospec AFT-5100).
  • Remaining step (dishing) (350 nm + silicon nitride film thickness (nm)) ⁇ (recessed silicon oxide film remaining film thickness (nm))
  • Tables 3 to 5 show the measurement results obtained in Examples B1 to B11 and Comparative Examples B1 to B6.
  • B1 H-PDX (reduced dextrin)
  • B2 Fibersol 2H (digestible dextrin)
  • B3 D (+)-glucose
  • B4 Neugen EA207D (polyoxyethylene styrenated phenyl ether)
  • B5 San Marto-S (Maltos)
  • P1 polydiallyldimethylammonium chloride
  • S1 2-acrylamido-2-methylpropanesulfonic acid
  • Example B1 the SiO 2 RR is 478 nm / min, the SiNRR is 0.9 nm / min, the polishing selectivity ratio SiO 2 RR / SiNRR is 531, SiNRR is smaller than the comparative example, and the polishing selectivity ratio is the comparative example. It showed a higher value.
  • the remaining steps when the silicon nitride film was exposed were 11 nm, 4 nm, and 1 nm (1000 ⁇ m pitch, 200 ⁇ m pitch, and 100 ⁇ m pitch), respectively.
  • Comparative Example B1 since the ⁇ -glucose polymer was not used, it was confirmed that the polishing selectivity was low. Moreover, in comparative example B1, since the amino group containing sulfonic acid compound was not used, it was confirmed that the progress of dishing is not suppressed. In Examples B7 to B10, since the amino group-containing sulfonic acid compound was not used, the progress of dishing was not suppressed, but it was confirmed that the polishing selectivity was higher than that of the comparative example. In Comparative Examples B2 and B5, it was confirmed that the polishing selectivity was low because no ⁇ -glucose polymer was used. In Comparative Example B3, since no cationic polymer was used, it was confirmed that the polishing selection ratio was low.
  • Comparative Example B4 it was confirmed that the polishing selectivity was low because ⁇ -glucose polymer and cationic polymer were not used. In Comparative Example B6, it was confirmed that the polishing selectivity was low because no ⁇ -glucose polymer was used. In Example B11, since ⁇ -glucose polymer having a degree of polymerization of ⁇ -glucose of 3 or more was not used, it was confirmed that although the progress of dishing was not suppressed, the polishing selectivity was higher than that of the comparative example. It was done.
  • Pattern wafer evaluation 2 A pattern wafer similar to the pattern wafer evaluation 1 was prepared except that a polysilicon film was formed instead of the silicon nitride film.
  • polishing was performed using the polishing agent described in Examples B1 to B6 under the same conditions as in the pattern wafer evaluation 1, the remaining step was small before and after overpolishing, and the progress of dishing was suppressed. It was confirmed that it was obtained. From this, it was confirmed that even when the stopper material is polysilicon, the polishing selectivity of the insulating material with respect to the stopper material can be improved and the progress of dishing can be suppressed.
  • a polishing agent capable of improving the polishing selectivity of the insulating material with respect to the stopper material in polishing of the insulating material using the stopper.
  • the polishing selectivity of the insulating material with respect to the stopper material is improved.
  • a polishing agent, a polishing agent set and a polishing method that can be provided.
  • a polishing agent capable of improving the polishing selectivity of the insulating material with respect to the stopper material and suppressing the progress of dishing in polishing of the insulating material using the stopper.
  • polishing selection of the insulating material with respect to the stopper material it is possible to provide a polishing agent, a polishing agent set and a polishing method capable of improving the performance and suppressing the progress of dishing.
  • a process using polysilicon in addition to silicon nitride is also increasing.
  • insulation against the stopper material is achieved.
  • the polishing selectivity of the material can be improved and the progress of dishing can be suppressed.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (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)

Abstract

Agent de polissage contenant de l'eau, des grains abrasifs contenant un hydroxyde d'un élément métallique tétravalent, un produit de polymérisation d'α-glucose et un polymère cationique, le produit de polymérisation d'α-glucose présentant une masse moléculaire moyenne en poids de 20,0 × 103 ou moins.
PCT/JP2014/071232 2013-10-10 2014-08-11 Agent de polissage, ensemble d'agent de polissage et procédé pour base de polissage WO2015052988A1 (fr)

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JP2013-213008 2013-10-10
JP2013213008 2013-10-10
JP2014097065 2014-05-08
JP2014-097065 2014-05-08
JP2014-097066 2014-05-08
JP2014097066 2014-05-08

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WO2017057156A1 (fr) * 2015-09-30 2017-04-06 株式会社フジミインコーポレーテッド Procede de polissage
JP2018059054A (ja) * 2016-09-29 2018-04-12 花王株式会社 研磨液組成物
WO2018179787A1 (fr) * 2017-03-27 2018-10-04 日立化成株式会社 Liquide de polissage, ensemble de liquide de polissage, et procédé de polissage
KR20190055112A (ko) 2016-09-29 2019-05-22 카오카부시키가이샤 연마액 조성물
WO2019182063A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Boue, ensemble de boues et procédé de polissage
WO2019182057A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Suspension é paisse, ensemble suspension épaisse et procédé de polissage
WO2019181015A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Liquide de polissage, ensemble liquide de polissage et procédé de polissage
US11492526B2 (en) 2018-07-26 2022-11-08 Showa Denko Materials Co., Ltd. Slurry, method for producing polishing liquid, and polishing method
US11566150B2 (en) 2017-03-27 2023-01-31 Showa Denko Materials Co., Ltd. Slurry and polishing method

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WO2012123839A1 (fr) * 2011-03-11 2012-09-20 Basf Se Procédé pour la formation de trous d'interconnexion à travers la tranche de base
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Cited By (28)

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Publication number Priority date Publication date Assignee Title
WO2017057156A1 (fr) * 2015-09-30 2017-04-06 株式会社フジミインコーポレーテッド Procede de polissage
JPWO2017057156A1 (ja) * 2015-09-30 2018-07-19 株式会社フジミインコーポレーテッド 研磨方法
US10478939B2 (en) 2015-09-30 2019-11-19 Fujimi Incorporated Polishing method
JP2018059054A (ja) * 2016-09-29 2018-04-12 花王株式会社 研磨液組成物
KR20190052026A (ko) 2016-09-29 2019-05-15 카오카부시키가이샤 연마액 조성물
KR20190055112A (ko) 2016-09-29 2019-05-22 카오카부시키가이샤 연마액 조성물
US11814548B2 (en) 2017-03-27 2023-11-14 Resonac Corporation Polishing liquid, polishing liquid set, and polishing method
US11773291B2 (en) 2017-03-27 2023-10-03 Resonac Corporation Polishing liquid, polishing liquid set, and polishing method
US11566150B2 (en) 2017-03-27 2023-01-31 Showa Denko Materials Co., Ltd. Slurry and polishing method
KR102278256B1 (ko) * 2017-03-27 2021-07-15 쇼와덴코머티리얼즈가부시끼가이샤 연마액, 연마액 세트 및 연마 방법
KR20190122224A (ko) * 2017-03-27 2019-10-29 히타치가세이가부시끼가이샤 연마액, 연마액 세트 및 연마 방법
WO2018179787A1 (fr) * 2017-03-27 2018-10-04 日立化成株式会社 Liquide de polissage, ensemble de liquide de polissage, et procédé de polissage
JPWO2018179787A1 (ja) * 2017-03-27 2019-12-19 日立化成株式会社 研磨液、研磨液セット及び研磨方法
JPWO2019182063A1 (ja) * 2018-03-22 2021-02-25 昭和電工マテリアルズ株式会社 研磨液、研磨液セット及び研磨方法
US11572490B2 (en) 2018-03-22 2023-02-07 Showa Denko Materials Co., Ltd. Polishing liquid, polishing liquid set, and polishing method
WO2019181015A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Liquide de polissage, ensemble liquide de polissage et procédé de polissage
JP7067614B2 (ja) 2018-03-22 2022-05-16 昭和電工マテリアルズ株式会社 研磨液、研磨液セット及び研磨方法
US11352523B2 (en) 2018-03-22 2022-06-07 Showa Denko Materials Co., Ltd. Polishing liquid, polishing liquid set and polishing method
WO2019182063A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Boue, ensemble de boues et procédé de polissage
WO2019181014A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Liquide de polissage, ensemble liquide de polissage et procédé de polissage
US11767448B2 (en) 2018-03-22 2023-09-26 Resonac Corporation Polishing liquid, polishing liquid set, and polishing method
KR102520409B1 (ko) * 2018-03-22 2023-04-11 가부시끼가이샤 레조낙 연마액, 연마액 세트 및 연마 방법
WO2019182057A1 (fr) * 2018-03-22 2019-09-26 日立化成株式会社 Suspension é paisse, ensemble suspension épaisse et procédé de polissage
KR20200128741A (ko) * 2018-03-22 2020-11-16 쇼와덴코머티리얼즈가부시끼가이샤 연마액, 연마액 세트 및 연마 방법
US11518920B2 (en) 2018-07-26 2022-12-06 Showa Denko Materials Co., Ltd. Slurry, and polishing method
US11505731B2 (en) 2018-07-26 2022-11-22 Showa Denko Materials Co., Ltd. Slurry and polishing method
US11499078B2 (en) 2018-07-26 2022-11-15 Showa Denko Materials Co., Ltd. Slurry, polishing solution production method, and polishing method
US11492526B2 (en) 2018-07-26 2022-11-08 Showa Denko Materials Co., Ltd. Slurry, method for producing polishing liquid, and polishing method

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