WO2020021730A1 - スラリ、研磨液の製造方法、及び、研磨方法 - Google Patents
スラリ、研磨液の製造方法、及び、研磨方法 Download PDFInfo
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- WO2020021730A1 WO2020021730A1 PCT/JP2018/035441 JP2018035441W WO2020021730A1 WO 2020021730 A1 WO2020021730 A1 WO 2020021730A1 JP 2018035441 W JP2018035441 W JP 2018035441W WO 2020021730 A1 WO2020021730 A1 WO 2020021730A1
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- 230000002265 prevention Effects 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 235000019423 pullulan Nutrition 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- 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
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
- H01L22/26—Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Definitions
- the conventional cerium oxide-based polishing liquid has a problem that the removal rate (capture efficiency) of coarse particles in filtration is low.
- a method of reducing the pore size of the filter can be considered.
- the removal rate of coarse particles decreases due to clogging, or the polishing rate decreases because the particle size distribution changes before and after filtration due to the particles adhering to the filter medium.
- a polishing method includes a step of polishing a surface to be polished using the polishing liquid obtained by the above-described method for producing a polishing liquid. According to such a polishing method, polishing scratches generated during polishing can be reduced.
- the present invention it is possible to provide a slurry capable of obtaining an excellent removal rate of coarse particles in filtration. Further, according to the present invention, it is possible to provide a method for producing a polishing liquid using the slurry. Further, according to the present invention, it is possible to provide a polishing method using a polishing liquid obtained by the method for producing a polishing liquid. ADVANTAGE OF THE INVENTION According to this invention, the application to the grinding
- a numerical range indicated by using “to” indicates a range including numerical values described before and after “to” as a minimum value and a maximum value, respectively.
- the upper limit or the lower limit of a numerical range in one step can be arbitrarily combined with the upper limit or the lower limit of a numerical range in another step.
- the upper limit or the lower limit of the numerical range may be replaced with the value shown in the embodiment.
- “A or B” may include one of A and B, and may include both.
- the materials exemplified in the present specification can be used alone or in combination of two or more, unless otherwise specified.
- polishing liquid (polishing liquid, abrasive) is defined as a composition that comes into contact with a surface to be polished during polishing.
- polishing liquid itself does not limit the components contained in the polishing liquid at all.
- Specific surface area represents the total surface area of the sample per unit mass. When measured by the BET method, it is called “BET specific surface area”.
- the sample may contain particles having different specific surface areas. In this case, information on the specific surface area (true value) of each particle cannot be obtained, but an effective value obtained by averaging the contribution to the surface area of all particles can be obtained.
- the BET specific surface area can be measured using a gas adsorption method, for example, using a specific surface area / pore diameter analyzer (trade name: QUADRASORB EVO) manufactured by Quantachrome under the following conditions. As the BET specific surface area of the abrasive grains, an average value of two measurements can be used.
- an excellent removal rate of coarse particles can be obtained.
- polishing scratches generated during polishing can be reduced.
- the removal rate of the coarse particles is large, the number of the coarse particles tends to be easily reduced, and the polishing scratches can be effectively reduced.
- the reason why such an excellent removal rate of coarse particles can be obtained includes, for example, the following reasons. However, the reason is not limited to the following.
- the composite particles in the present embodiment can maintain a dispersed state even when an interaction occurs. This is presumed to be because repulsive interaction occurs between the second particles. That is, other second particles (such as particles that are not in contact with the first particles) are unlikely to approach the second particles that have come into contact with the first particles. Therefore, since new adsorption of the second particles is suppressed, it is estimated that coarse aggregates are not formed. Since the repulsive interaction between the second particles is sufficiently large with respect to the attractive interaction between the first particles and the second particles, the composite particles in the present embodiment are in a dispersed state. It is estimated that can be maintained.
- the above-mentioned repulsive interaction is not particularly limited, and examples thereof include an electrostatic repulsion, an osmotic pressure, a three-dimensional repulsion by a surface adsorption layer, and the like.
- the specific surface area of the coarse particles in the slurry is not necessarily large, but other particles having a larger specific surface area (hereinafter, referred to as “particle A”; for example, second particles) are the surface of the coarse particles.
- particle A for example, second particles
- a phenomenon may occur in which the coarse particles behave as particles having a specific surface area equal to or larger than the specific surface area originally possessed. That is, it is considered that the large particles A having a large specific surface area are adsorbed to the coarse particles, so that the adhesion of the coarse particles to the filter medium is increased, so that the coarse particles are easily removed by filtration.
- the polishing rate of the insulating material is improved as described above include, for example, the following reasons. However, the reason is not limited to the following.
- the BET specific surface area of the solid phase obtained when the slurry is centrifuged at a centrifugal acceleration of 1.1 ⁇ 10 4 G for 30 minutes is excellent. From the viewpoint of obtaining a removal rate of coarse particles, it is 24 m 2 / g or more.
- the BET specific surface area of the solid phase the dried BET specific surface area of the solid phase obtained by centrifuging the slurry can be used.
- the lower limit of the BET specific surface area of the solid phase is preferably 25 m 2 / g or more, more preferably 28 m 2 / g or more, still more preferably 30 m 2 / g or more, from the viewpoint of easily obtaining an excellent removal rate of coarse particles. It is particularly preferably at least 35 m 2 / g, particularly preferably at least 40 m 2 / g.
- the upper limit of the BET specific surface area of the solid phase is preferably 200 m 2 / g or less from the viewpoint that particles are less likely to adhere to each other and aggregation of particles is easily suppressed.
- Materials constituting the filter include polypropylene, nylon, glass, polyester, polyether sulfone, polytetrafluoroethylene, polycarbonate, polyvinylidene fluoride, and cellulose derivatives. These materials may be processed into a membrane or a fiber.
- the filtration may be performed in one stage, or a multi-stage process combining a plurality of filters may be performed.
- the slurry may be passed once through a single filter, and the same filter may be subjected to circulation processing a plurality of times.
- the abrasive grains in the present embodiment contain composite particles including the first particles and the second particles in contact with the first particles.
- the lower limit of the particle size of the second particles is preferably 1 nm or more, more preferably 2 nm or more, and still more preferably 3 nm or more, from the viewpoint of further improving the polishing rate of the insulating material.
- the upper limit of the particle size of the second particles is preferably 50 nm or less, more preferably 30 nm or less, and 25 nm from the viewpoint that the dispersibility of the abrasive grains is improved and that the surface to be polished is easily suppressed from being damaged.
- the thickness is particularly preferably 20 nm or less, particularly preferably 15 nm or less, and very preferably 10 nm or less. From the above viewpoint, the particle size of the second particles is more preferably 1 to 50 nm.
- the average particle size (average secondary particle size) of the second particles may be in the above range.
- the first particles contain a cerium oxide (eg, ceria), and the second particles contain a cerium compound.
- the cerium compound of the second particles include cerium hydroxide and cerium oxide.
- the cerium compound of the second particles a compound different from cerium oxide can be used.
- the cerium compound preferably contains cerium hydroxide. Abrasive grains containing cerium hydroxide have a higher reactivity (chemical action) with an insulating material (eg, silicon oxide) due to the action of a hydroxyl group than particles made of silica, cerium oxide, and the like. Polishing can be performed at a higher polishing rate.
- Cerium hydroxide is, for example, a compound containing tetravalent cerium (Ce 4+ ) and at least one hydroxide ion (OH ⁇ ).
- Cerium hydroxide may include anions other than hydroxide ions (eg, nitrate ions NO 3 ⁇ and sulfate ions SO 4 2 ⁇ ).
- cerium hydroxide may include anions (eg, nitrate NO 3 ⁇ and sulfate SO 4 2 ⁇ ) bound to tetravalent cerium.
- Cerium hydroxide can be produced by reacting a cerium salt with an alkali source (base).
- the cerium hydroxide is preferably produced by mixing a cerium salt and an alkaline liquid (for example, an alkaline aqueous solution).
- an alkaline liquid for example, an alkaline aqueous solution.
- Cerium hydroxide can be obtained by mixing a cerium salt solution (for example, a cerium salt aqueous solution) and an alkali solution.
- the cerium salt include Ce (NO 3 ) 4 , Ce (SO 4 ) 2 , Ce (NH 4 ) 2 (NO 3 ) 6 , Ce (NH 4 ) 4 (SO 4 ) 4 and the like.
- Water-soluble polymer is defined as a polymer that is soluble in 0.1 g or more in 100 g of water.
- the polymer corresponding to the polyoxyalkylene compound is not included in the “water-soluble polymer”.
- the water-soluble polymer is not particularly limited, and includes acrylic polymers such as polyacrylamide and polydimethylacrylamide; polysaccharides such as carboxymethylcellulose, agar, curdlan, dextrin, cyclodextrin, and pullulan; polyvinyl alcohol, polyvinylpyrrolidone, and polysaccharide.
- Vinyl-based polymers such as acrolein; glycerin-based polymers such as polyglycerin and polyglycerin derivatives; and polyethylene glycol.
- 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; and GeSbTe. Phase change materials; inorganic conductive materials such as ITO; and polymer resin materials such as polyimide, polybenzoxazole, acrylic, epoxy, and phenol.
- This embodiment is applicable not only to the manufacture of semiconductor elements, but also to image display devices such as TFTs and organic ELs; optical components such as photomasks, lenses, prisms, optical fibers, and single-crystal scintillators; A light-emitting element such as a solid-state laser or a blue laser LED; and a light-emitting element such as a magnetic disk or a magnetic head.
- image display devices such as TFTs and organic ELs
- optical components such as photomasks, lenses, prisms, optical fibers, and single-crystal scintillators
- a light-emitting element such as a solid-state laser or a blue laser LED
- a light-emitting element such as a magnetic disk or a magnetic head.
- cerium oxide slurry A was put into a centrifuge (trade name: himac CR7) manufactured by Hitachi Koki Co., Ltd., centrifugation was performed at a centrifugal acceleration of 1.1 ⁇ 10 4 G for 30 minutes. After the supernatant was removed and the solid phase was dried under vacuum, the solid phase was pulverized using a mortar to obtain finely divided powder. This powder was placed in a vacuum measurement cell (capacity: 1.5 cm 3 ), and then the amount of nitrogen gas adsorbed at 77.35 K using a specific surface area / pore diameter analyzer (trade name: QUADRASORB evo) manufactured by Quantachrome. Was measured to obtain a BET specific surface area (m 2 / g). The BET specific surface area was 22.9 m 2 / g.
- the obtained precipitate (precipitate containing cerium hydroxide) was centrifuged (4000 min -1 , 5 minutes), and then the liquid phase was removed by decantation to perform solid-liquid separation. After mixing 10 g of the particles obtained by the solid-liquid separation and 990 g of water, the particles are dispersed in water using an ultrasonic cleaner, and the particles containing cerium hydroxide (second particles; hereinafter, referred to as “second particles”). A cerium hydroxide slurry containing “cerium hydroxide particles” (particle content: 1.0% by mass) was prepared.
- Example 1 While stirring at a rotation speed of 300 rpm using two stirring blades, 150 g of the cerium hydroxide slurry and 150 g of ion-exchanged water were mixed to obtain a mixed solution. Subsequently, 200 g of the cerium oxide slurry A was mixed with the mixed solution while stirring the mixed solution, and the mixture was irradiated with ultrasonic waves using an ultrasonic cleaning machine (device name: US-105) manufactured by SND Corporation. While stirring.
- an ultrasonic cleaning machine device name: US-105
- Cerium oxide particles (cerium oxide particles B different from cerium oxide particles A), a trade name of Wako Pure Chemical Industries, Ltd .: polyacrylic acid 5000 (weight average molecular weight: 5000), and ion-exchanged water Cerium oxide slurry B (content of cerium oxide particles: 5.0% by mass) was prepared by mixing. The blending amount of polyacrylic acid was adjusted to 1% by mass based on the total amount of the cerium oxide particles. Similarly to the cerium oxide slurry A, the average particle size and zeta potential of the cerium oxide particles in the cerium oxide slurry B were measured to be 145 nm and -55 mV.
- Example 3 A composite particle containing cerium oxide particles and cerium hydroxide particles in contact with the cerium oxide particles by performing the same procedure as in Example 1 except that the amount of the cerium hydroxide slurry used was changed. (A content of cerium oxide particles: 2.0% by mass, a content of cerium hydroxide particles: 0.13% by mass) was prepared.
- Example 4 A composite particle containing cerium oxide particles and cerium hydroxide particles in contact with the cerium oxide particles by performing the same procedure as in Example 1 except that the amount of the cerium hydroxide slurry used was changed. (A content of cerium oxide particles: 2.0% by mass, a content of cerium hydroxide particles: 0.07% by mass) was prepared.
- Comparative Example 4 By mixing colloidal ceria particles having a primary particle diameter of 50 nm (cerium oxide particles D different from cerium oxide particles A, B and C) and ion-exchanged water, a test slurry containing cerium oxide particles ( The content of cerium oxide particles: 2.0% by mass (solid content)) was prepared.
- ⁇ Average particle size of abrasive particles> The appropriate amount of each of the test slurries described above was charged into Microtrac MT3300EXII (trade name, manufactured by Microtrac Bell Inc.), and the average particle size of the abrasive grains was measured. The indicated average particle size value was obtained as the average particle size of the abrasive grains (average secondary particle size). Table 1 shows the measurement results.
- ⁇ BET specific surface area of solid phase> (Preparation of particle powder)
- the content of the abrasive grains (the total amount of the abrasive grains) was 2.0% by mass by adjusting the content of the abrasive grains in the test slurry with ion-exchanged water as needed.
- 100 g of the measurement sample was put into a centrifuge (trade name: himac CR7) manufactured by Hitachi Koki Co., Ltd., and then centrifuged at a centrifugal acceleration of 1.1 ⁇ 10 4 G for 30 minutes. After removing the supernatant, the solid phase was vacuum dried. Then, the solid phase was pulverized using a mortar to obtain finely divided powder (particle powder).
- the removal rate of coarse particles was 50% or less. Yes, it was confirmed that the content of coarse particles in ion-exchanged water was small. As a result, it was confirmed that the LPC was not overestimated than the true value due to the mixing of the coarse particles in the ion-exchanged water used for preparing the measurement sample for the removal rate and the foreign matter attached to the container.
- ⁇ CMP evaluation> By adding ion-exchanged water to the filtrate obtained by performing the same filtration as above, a CMP polishing liquid having a content of abrasive grains (total amount of abrasive grains) of 0.1% by mass was obtained.
- the substrate to be polished was polished under the following polishing conditions using the CMP polishing liquid.
- Substrate to be Polished As a blanket wafer on which no pattern was formed, a substrate to be polished having a silicon oxide film having a thickness of 2 ⁇ m formed on a silicon substrate by a plasma CVD method was used.
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Mechanical Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Disintegrating Or Milling (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
Abstract
Description
本明細書において、「~」を用いて示された数値範囲は、「~」の前後に記載される数値をそれぞれ最小値及び最大値として含む範囲を示す。本明細書に段階的に記載されている数値範囲において、ある段階の数値範囲の上限値又は下限値は、他の段階の数値範囲の上限値又は下限値と任意に組み合わせることができる。本明細書に記載されている数値範囲において、その数値範囲の上限値又は下限値は、実施例に示されている値に置き換えてもよい。「A又はB」とは、A及びBのどちらか一方を含んでいればよく、両方とも含んでいてもよい。本明細書に例示する材料は、特に断らない限り、1種を単独で又は2種以上を組み合わせて用いることができる。本明細書において、組成物中の各成分の含有量は、組成物中に各成分に該当する物質が複数存在する場合、特に断らない限り、組成物中に存在する当該複数の物質の合計量を意味する。「工程」との語は、独立した工程だけではなく、他の工程と明確に区別できない場合であってもその工程の所期の作用が達成されれば、本用語に含まれる。
使用機器:日立L-6000型[株式会社日立製作所製]
カラム:ゲルパックGL-R420+ゲルパックGL-R430+ゲルパックGL-R440[日立化成株式会社製 商品名、計3本]
溶離液:テトラヒドロフラン
測定温度:40℃
流量:1.75mL/min
検出器:L-3300RI[株式会社日立製作所製]
前処理:真空脱気(100℃、2時間)
測定方式:定容法
吸着ガス:窒素ガス
測定温度:77.35K
測定セルサイズ:1.5cm3
測定項目:P/P0の値を0~0.3の範囲で変化させて数点を測定
解析項目:BET多点法による比表面積
測定回数:試料を変えて2回測定
本実施形態に係るスラリは、必須成分として砥粒と液状媒体とを含有する。砥粒は、第1の粒子と、当該第1の粒子に接触した第2の粒子と、を含む複合粒子を含有する。第1の粒子はセリウム酸化物を含有し、第2の粒子はセリウム化合物を含有する。砥粒の含有量が2.0質量%である場合において、本実施形態に係るスラリを遠心加速度1.1×104Gで30分間遠心分離したときに得られる固相のBET比表面積は、24m2/g以上である。
(a)比表面積が大きい粒子がスラリ中に存在する。
(b)比表面積が大きい粒子の二次粒径が大きい。
本実施形態における砥粒は、上述のとおり、第1の粒子と、当該第1の粒子に接触した第2の粒子と、を含む複合粒子を含有する。
吸光度 =-LOG10(光透過率[%]/100)
液状媒体としては、特に制限はないが、脱イオン水、超純水等の水が好ましい。液状媒体の含有量は、他の構成成分の含有量を除いたスラリ又は研磨液の残部でよく、特に限定されない。
本実施形態に係るスラリ又は研磨液は、任意の添加剤を更に含有していてもよい。任意の添加剤としては、カルボキシル基を有する材料(ポリオキシアルキレン化合物又は水溶性高分子に該当する化合物を除く)、ポリオキシアルキレン化合物、水溶性高分子、酸化剤(例えば過酸化水素)、分散剤(例えばリン酸系無機塩)等が挙げられる。添加剤のそれぞれは、一種を単独で又は二種以上を組み合わせて使用することができる。
本実施形態に係るスラリ又は研磨液のpHの下限は、絶縁材料の研磨速度が更に向上する観点から、2.0以上が好ましく、2.5以上がより好ましく、2.8以上が更に好ましく、3.0以上が特に好ましく、3.2以上が極めて好ましく、3.5以上が非常に好ましく、4.0以上がより一層好ましく、4.2以上が更に好ましく、4.3以上が特に好ましい。pHの上限は、スラリ又は研磨液の保存安定性が更に向上する観点から、7.0以下が好ましく、6.5以下がより好ましく、6.0以下が更に好ましく、5.0以下が特に好ましく、4.8以下が極めて好ましく、4.7以下が非常に好ましく、4.6以下がより一層好ましく、4.5以下が更に好ましく、4.4以下が特に好ましい。前記観点から、pHは、2.0~7.0であることがより好ましい。pHは、液温25℃におけるpHと定義する。
本実施形態に係る研磨方法(基体の研磨方法等)の第1態様は、前記研磨液の製造方法により得られた研磨液を用いて被研磨面を研磨する工程を備えている。本実施形態に係る研磨方法(基体の研磨方法等)の第2態様は、前記スラリ(ろ過前のスラリ)を研磨液として用いて被研磨面(基体の被研磨面等)を研磨する研磨工程を備えている。本実施形態によれば、絶縁材料の高い研磨速度を達成することができる。本実施形態に係るスラリは、例えば、研磨液(CMP研磨液)として用いることができる。研磨工程における研磨液は、前記研磨液セットにおける第1の液と第2の液とを混合して得られる研磨液であってもよい。被研磨面は、例えば、酸化珪素を含む。
セリウム酸化物を含む粒子(第1の粒子。以下、「セリウム酸化物粒子」という。セリウム酸化物粒子A)と、和光純薬工業株式会社製の商品名:リン酸二水素アンモニウム(分子量:97.99)とを混合して、セリウム酸化物粒子を5.0質量%(固形分含量)含有するセリウム酸化物スラリA(pH:7)を調製した。リン酸二水素アンモニウムの配合量は、セリウム酸化物粒子の全量を基準として1質量%に調整した。
(セリウム水酸化物の合成)
480gのCe(NH4)2(NO3)650質量%水溶液(日本化学産業株式会社製、商品名:CAN50液)を7450gの純水と混合して溶液を得た。次いで、この溶液を撹拌しながら、750gのイミダゾール水溶液(10質量%水溶液、1.47mol/L)を5mL/minの混合速度で滴下して、セリウム水酸化物を含む沈殿物を得た。セリウム水酸化物の合成は、温度20℃、撹拌速度500min-1で行った。撹拌は、羽根部全長5cmの3枚羽根ピッチパドルを用いて行った。
ベックマン・コールター株式会社製、商品名:N5を用いてセリウム水酸化物スラリにおけるセリウム水酸化物粒子の平均粒径(平均二次粒径)を測定したところ、10nmであった。測定法は次のとおりである。まず、1.0質量%のセリウム水酸化物粒子を含む測定サンプル(セリウム水酸化物スラリ。水分散液)を1cm角のセルに約1mL入れた後、N5内にセルを設置した。N5のソフトの測定サンプル情報の屈折率を1.333、粘度を0.887mPa・sに設定し、25℃において測定を行い、Unimodal Size Meanとして表示される値を読み取った。
ベックマン・コールター株式会社製の商品名:DelsaNano C内に適量のセリウム水酸化物スラリを投入し、25℃において測定を2回行った。表示されたゼータ電位の平均値をゼータ電位として得た。セリウム水酸化物スラリにおけるセリウム水酸化物粒子のゼータ電位は+50mVであった。
セリウム水酸化物スラリを適量採取し、真空乾燥してセリウム水酸化物粒子を単離した後に純水で充分に洗浄して試料を得た。得られた試料について、FT-IR ATR法による測定を行ったところ、水酸化物イオン(OH-)に基づくピークの他に、硝酸イオン(NO3 -)に基づくピークが観測された。また、同試料について、窒素に対するXPS(N-XPS)測定を行ったところ、NH4 +に基づくピークは観測されず、硝酸イオンに基づくピークが観測された。これらの結果より、セリウム水酸化物粒子は、セリウム元素に結合した硝酸イオンを有する粒子を少なくとも一部含有することが確認された。また、セリウム元素に結合した水酸化物イオンを有する粒子がセリウム水酸化物粒子の少なくとも一部に含有されることから、セリウム水酸化物粒子がセリウム水酸化物を含有することが確認された。これらの結果より、セリウムの水酸化物が、セリウム元素に結合した水酸化物イオンを含むことが確認された。
(実施例1)
2枚羽根の撹拌羽根を用いて300rpmの回転数で撹拌しながら、前記セリウム水酸化物スラリ150gと、イオン交換水150gとを混合して混合液を得た。続いて、前記混合液を撹拌しながら前記セリウム酸化物スラリA200gを前記混合液に混合した後、株式会社エスエヌディ製の超音波洗浄機(装置名:US-105)を用いて超音波を照射しながら撹拌した。これにより、セリウム酸化物粒子と、当該セリウム酸化物粒子に接触したセリウム水酸化物粒子と、を含む複合粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%、セリウム水酸化物粒子の含有量:0.3質量%)を調製した。
セリウム酸化物粒子(セリウム酸化物粒子Aとは異なるセリウム酸化物粒子B)と、和光純薬工業株式会社製の商品名:ポリアクリル酸5000(重量平均分子量:5000)と、イオン交換水とを混合することにより、セリウム酸化物スラリB(セリウム酸化物粒子の含有量:5.0質量%)を調製した。ポリアクリル酸の配合量は、セリウム酸化物粒子の全量を基準として1質量%に調整した。セリウム酸化物スラリAと同様に、セリウム酸化物スラリBにおけるセリウム酸化物粒子の平均粒径及びゼータ電位を測定したところ、145nm及び-55mVであった。
前記セリウム水酸化物スラリの使用量を変更したことを除き実施例1と同様に行うことにより、セリウム酸化物粒子と、当該セリウム酸化物粒子に接触したセリウム水酸化物粒子と、を含む複合粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%、セリウム水酸化物粒子の含有量:0.13質量%)を調製した。
前記セリウム水酸化物スラリの使用量を変更したことを除き実施例1と同様に行うことにより、セリウム酸化物粒子と、当該セリウム酸化物粒子に接触したセリウム水酸化物粒子と、を含む複合粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%、セリウム水酸化物粒子の含有量:0.07質量%)を調製した。
前記セリウム酸化物スラリAとイオン交換水とを混合することにより、セリウム酸化物粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%)を調製した。
前記セリウム酸化物スラリBとイオン交換水とを混合することにより、セリウム酸化物粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%)を調製した。
セリウム酸化物粒子(セリウム酸化物粒子A及びBとは異なるセリウム酸化物粒子C)と、酢酸(和光純薬工業株式会社製)と、イオン交換水とを混合することにより、セリウム酸化物粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%)を調製した。酢酸の配合量は、セリウム酸化物粒子の全量を基準として1.0質量%であった。
一次粒径50nmのコロイダルセリア粒子(セリウム酸化物粒子A、B及びCとは異なるセリウム酸化物粒子D)と、イオン交換水とを混合することにより、セリウム酸化物粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%(固形分含量))を調製した。
前記セリウム水酸化物スラリの使用量を変更したことを除き実施例1と同様に行うことにより、セリウム酸化物粒子と、当該セリウム酸化物粒子に接触したセリウム水酸化物粒子と、を含む複合粒子を含有する試験用スラリ(セリウム酸化物粒子の含有量:2.0質量%、セリウム水酸化物粒子の含有量:0.01質量%)を調製した。
マイクロトラック・ベル株式会社製の商品名:マイクロトラックMT3300EXII内に上述の各試験用スラリを適量投入し、砥粒の平均粒径の測定を行った。表示された平均粒径値を砥粒の平均粒径(平均二次粒径)として得た。測定結果を表1に示す。
(粒子粉末の作製)
必要に応じてイオン交換水で試験用スラリの砥粒の含有量を調整することにより、砥粒の含有量(砥粒の総量)が2.0質量%である測定試料を得た。次に、測定試料100gを日立工機株式会社製の遠心分離機(商品名:himac CR7)に入れた後、遠心加速度1.1×104Gで30分間遠心分離を行った。上澄み液を除去した後、固相を真空乾燥した。そして、乳鉢を用いて固相を粉砕して、細粒化した粉末(粒子粉末)を得た。
上記粉末を真空測定用セル(容量:1.5cm3)に入れた後、Quantachrome社製の比表面積・細孔径分析装置(商品名:QUADRASORB evo)を用いて77.35Kにおける窒素ガスの吸着量を測定することによりBET比表面積(m2/g)を得た。2回の測定の平均値を砥粒のBET比表面積として得た。測定結果を表1に示す。
(スラリのろ過)
必要に応じてイオン交換水で試験用スラリの砥粒の含有量を調整することにより、砥粒の含有量(砥粒の総量)2.0質量%の測定試料200gを作製した。株式会社ロキテクノ製の47mmφディスクフィルタ(商品名:SCP-005、ろ材:ポリプロピレン、公称孔径:0.5μm)を設置した円筒形状の簡易ろ過装置に上記測定試料を入れた後に0.2MPaで圧送することにより、上記フィルタを通過した測定試料(ろ液)を回収した。循環処理を行わず、単一のフィルタに対してスラリを一回通液することによりろ過を行った。
100mL容器に測定試料(ろ過前後のそれぞれの測定試料)10gとイオン交換水90gとを加えることにより測定試料を10倍希釈した後にミックスローターに容器を設置した。測定装置における粗大粒子数の上限の測定限界を下回る範囲に調整する観点から、前記のとおり測定試料を希釈した。次に、回転数100rpmで10分間攪拌した。続いて、上記容器をリオン株式会社製の光遮断式液中パーティカルセンサ(装置名:KS-71)に静かに設置した後、ろ過前後のそれぞれにおける3μm以上の大きさ(粒径)の粗大粒子の数(LPC:Large Particle Counts。5回の測定の平均値)を下記の測定条件で測定した。測定試料のろ過前後の粗大粒子数に基づき粗大粒子の除去率(粗大粒子の除去率[%]=(1-(ろ過後のLPC[個/mL])/(ろ過前のLPC[個/mL]))×100)を算出した。測定結果を表1に示す。
測定液量:10mL/回
流量:60mL/min
測定回数:5回
上記と同様のろ過を行って得られたろ液にイオン交換水を加えることにより、砥粒の含有量(砥粒の総量)0.1質量%のCMP研磨液を得た。このCMP研磨液を用いて下記研磨条件で被研磨基板を研磨した。
[CMP研磨条件]
研磨装置:MIRRA(APPLIED MATERIALS社製)
研磨液の流量:200mL/min
被研磨基板:パターンが形成されていないブランケットウエハとして、プラズマCVD法で形成された厚さ2μmの酸化珪素膜をシリコン基板上に有する被研磨基板を用いた。
研磨パッド:独立気泡を有する発泡ポリウレタン樹脂(ダウ・ケミカル日本株式会社製、型番IC1010)
研磨圧力:13kPa(2.0psi)
被研磨基板及び研磨定盤の回転数:被研磨基板/研磨定盤=93/87rpm
研磨時間:1min
ウエハの洗浄:CMP処理後、超音波を印加しながら水で洗浄し、さらに、スピンドライヤで乾燥させた。
研磨速度(RR)=(研磨前後での酸化珪素膜の膜厚差[nm])/(研磨時間:1[min])
Claims (7)
- 砥粒と、液状媒体と、を含有するスラリであって、
前記砥粒が、第1の粒子と、当該第1の粒子に接触した第2の粒子と、を含み、
前記第1の粒子がセリウム酸化物を含有し、
前記第2の粒子がセリウム化合物を含有し、
前記砥粒の含有量が2.0質量%である場合において遠心加速度1.1×104Gで30分間前記スラリを遠心分離したときに得られる固相のBET比表面積が24m2/g以上である、スラリ。 - 前記セリウム化合物がセリウム水酸化物を含む、請求項1に記載のスラリ。
- 前記砥粒の平均粒径が16~1050nmである、請求項1又は2に記載のスラリ。
- 前記砥粒の含有量が0.01~10質量%である、請求項1~3のいずれか一項に記載のスラリ。
- 請求項1~4のいずれか一項に記載のスラリをろ過する工程を備える、研磨液の製造方法。
- 請求項5に記載の研磨液の製造方法により得られた研磨液を用いて被研磨面を研磨する工程を備える、研磨方法。
- 前記被研磨面が酸化珪素を含む、請求項6に記載の研磨方法。
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