WO2012039428A1 - 研磨液組成物の製造方法 - Google Patents
研磨液組成物の製造方法 Download PDFInfo
- Publication number
- WO2012039428A1 WO2012039428A1 PCT/JP2011/071501 JP2011071501W WO2012039428A1 WO 2012039428 A1 WO2012039428 A1 WO 2012039428A1 JP 2011071501 W JP2011071501 W JP 2011071501W WO 2012039428 A1 WO2012039428 A1 WO 2012039428A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- filter
- polishing
- less
- particles
- filter aid
- Prior art date
Links
Images
Classifications
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B5/00—Recording by magnetisation or demagnetisation of a record carrier; Reproducing by magnetic means; Record carriers therefor
- G11B5/84—Processes or apparatus specially adapted for manufacturing record carriers
- G11B5/8404—Processes or apparatus specially adapted for manufacturing record carriers manufacturing base layers
-
- 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
- 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
Definitions
- the present invention relates to a method for producing a polishing liquid composition and a polishing liquid composition produced by the production method.
- Recent memory hard disk drives are required to have a high capacity and a small diameter, and in order to increase the recording density, the flying height of the magnetic head is reduced to reduce the unit recording area. Accordingly, the surface quality required after polishing in the manufacturing process of the magnetic disk substrate is becoming stricter year by year. That is, it is necessary to reduce the surface roughness, micro waviness, roll-off and protrusions according to the low flying height of the head, and the allowable number of scratches per substrate surface is small according to the decrease in the unit recording area, Its size and depth are getting smaller and smaller.
- a filter using diatomaceous earth as a filter aid is used as a filter for a polishing composition used for circulating polishing of a glass substrate (Patent Document 3), or a silica fine particle dispersion used as a coating liquid for an ink jet recording sheet. (Patent Document 4).
- JP 2006-075975 JP 2006-136996 A Japanese Unexamined Patent Publication No. 2007-098485 JP 2007-099586
- silica particles used in the polishing liquid composition need to reduce coarse particles, and are often prepared by the filtration system shown in the schematic diagram of FIG. That is, silica slurry 6 obtained by subjecting general-purpose colloidal silica to centrifugal separation or the like is circulated and filtered with depth filter 3 (tank 1 ⁇ pipe P1 ⁇ depth filter 3 ⁇ pipe P5 ⁇ tank 1), and then with pleated filter 5 Silica particles for the polishing composition are prepared from a filtration system including filtration (depth filter 3 ⁇ pipe P6 ⁇ pleated filter 5 ⁇ pipe 4).
- the present invention provides a polishing liquid composition that can economically manufacture a polishing liquid composition that has a small surface roughness of an object to be polished and that can effectively reduce particles that are important in densification.
- a method and a polishing liquid composition produced by the production method are provided.
- the present invention is a method for producing a polishing liquid composition
- a method for producing a polishing liquid composition comprising a step of subjecting a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm to a filter containing a filter aid.
- the filter aid relates to a method for producing a polishing liquid composition (hereinafter also referred to as “the production method of the present invention”) having an average pore diameter of 0.1 to 3.5 ⁇ m by mercury porosimetry.
- the present invention further includes a step of subjecting a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm to a filter containing a filter aid, the filter aid being
- the present invention relates to a polishing liquid composition (hereinafter also referred to as “the polishing liquid composition of the present invention”) that can be manufactured by a manufacturing method of a polishing liquid composition having an average pore diameter of 0.1 to 3.5 ⁇ m by mercury porosimetry.
- coarse particles and starch in the silica dispersion can be effectively removed by the step of filtration with the filter containing the filter aid, and the silica dispersion of the filtration is included.
- the polishing composition can effectively reduce scratches and particles during polishing.
- polishing composition produced by the production method of the present invention when used, for example, in a polishing step of a precision component substrate for high density or high integration, fine scratches and particles can be effectively reduced, In addition, it is possible to economically manufacture precision component substrates such as high-quality memory hard disk substrates and semiconductor element substrates having excellent surface properties.
- FIG. 1 is a schematic view for explaining an embodiment of the production method of the present invention.
- FIG. 2 is a schematic view illustrating an example of a conventional method for producing a polishing liquid composition.
- the method for producing a polishing liquid composition of the present invention comprises treating a silica dispersion containing colloidal silica having an average primary particle diameter of 1 to 100 nm with a filter containing a filter aid (hereinafter referred to as “filter aid containing filter”).
- filter aid containing filter a filter aid
- the average pore diameter of the filter aid by the mercury intrusion method is 0.1 to 3.5 ⁇ m.
- the present inventors have found that starch in the polishing composition is a cause of particles.
- the reason why the polishing composition that can reduce particles on the substrate surface after polishing is economically produced by the production method of the present invention is not clear, but the inside of the filter aid layer (cake layer) of the filter containing the filter aid In the sub-micron pores existing between the particles formed by the filter aid of several tens of ⁇ m, the sub-micron gaps of secondary aggregates, and the filter aid particles themselves, the starch causing the particles is efficiently removed. Estimated to be.
- the term “coarse particles” refers to coarse colloidal silica particles having a particle diameter of 0.5 ⁇ m or more, and the number of coarse particles in the polishing composition is determined by the 0.45 ⁇ m filter described in Examples below.
- the amount of liquid can be quantitatively evaluated as coarse particles in the polishing composition.
- the colloidal silica particles in the polishing liquid composition include not only primary particles but also aggregated particles obtained by aggregating primary particles.
- starch is a silica aggregate of 50 to 500 nm, and the amount of starch can be indirectly evaluated by ⁇ CV or polishing evaluation described later.
- “scratch” is a physical property that is important for high density or high integration, particularly in a memory hard disk substrate or a semiconductor device substrate, having a depth of 1 nm or more, less than 100 nm, and a width of 5 nm or more. These are fine scratches on the substrate surface of less than 500 nm and a length of 100 ⁇ m or more. This scratch can be detected by an optical entire surface defect inspection machine (OSA6100: manufactured by KLA-Tencor) described in the examples described later, and can be quantitatively evaluated as the number of scratches. Further, the depth and width can be measured using an atomic force microscope (AFM).
- OSA6100 manufactured by KLA-Tencor
- particles are protrusions on a substrate, and can be quantitatively evaluated as the number of particles by measurement with an optical entire surface defect inspection machine (OSA6100: manufactured by KLA-Tencor) described in the examples described later.
- OSA6100 optical entire surface defect inspection machine
- Analyzing particle parts with a scanning electron microscope (SEM) enables identification of protrusions (silica, alumina, titania, Fe compounds (stainless steel), organic substances, nickel compounds (NiP polishing scrap, nickel hydroxide, etc.)) It is.
- SEM scanning electron microscope
- the length and width of the protrusion can be measured using an atomic force microscope (AFM).
- Examples of the filter aid used in the production method of the present invention include insoluble mineral substances such as silicon dioxide, kaolin, acid clay, diatomaceous earth, perlite, bentonite, and talc. From the viewpoint of scratch and particle reduction, among the filter aids, silicon dioxide, diatomaceous earth, and pearlite are preferable, diatomaceous earth and pearlite are more preferable, and diatomaceous earth is more preferable.
- the filter aid is preferably pretreated with an acid from the viewpoint of reducing scratches and particles and improving the productivity of the polishing composition.
- the pretreatment with an acid is a treatment in which a filter aid is immersed in an aqueous acid solution such as an inorganic acid or an organic acid for a certain time.
- an aqueous acid solution such as an inorganic acid or an organic acid for a certain time.
- hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, phosphonic acid, oxalic acid, citric acid In view of scratches and particle reduction, treatment with hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid and phosphonic acid is more preferred, and treatment with hydrochloric acid, sulfuric acid and phosphonic acid is more preferred.
- the filter aid has an average pore diameter of 0.1 to 3.5 ⁇ m, preferably 0.1 to 3 ⁇ m by a mercury intrusion method, from the viewpoint of scratch and particle reduction and from the viewpoint of improving the productivity of the polishing composition.
- the “average pore diameter by mercury intrusion method” is the average value of the volume-based pore diameters of the filter aid particles, and can be measured by the method described in the examples.
- the cumulative pore volume of 0.5 ⁇ m or less by the mercury intrusion method of the filter aid is preferably 2.5 mL / g or more, more preferably 2.7 mL / g or more, more preferably from the viewpoint of scratching and particle reduction. 3.0 mL / g or more, even more preferably 4.0 mL / g or more, and even more preferably 4.5 mL / g or more. Further, from the viewpoint of improving the productivity of the polishing composition, it is preferably 1000 mL / g or less, more preferably 100 mL / g or less, still more preferably 50 mL / g or less, even more preferably 20 mL / g or less, and even more preferably.
- the cumulative pore volume of 0.5 ⁇ m or less of the filter aid is preferably 2.5 mL / g or more, more preferably 2 from the viewpoint of scratch and particle reduction and the improvement of the productivity of the polishing composition.
- the cumulative pore volume of 0.5 ⁇ m or less by the mercury intrusion method of the filter aid means the pore volume of 0.5 ⁇ m or less in the volume-based pore distribution of the filter aid particles by the mercury intrusion method. It is the sum and can be measured by the method described in the examples.
- the BET specific surface area of the filter aid is preferably 4.0 m 2 / g or more, more preferably 10.0 m 2 / g or more, still more preferably 15.0 m 2 / g or more, from the viewpoint of scratch and particle reduction. Even more preferably, it is 18.0 m 2 / g or more.
- the specific surface area is preferably 1000.0m 2 / g or less, more preferably 100.0 m 2 / g or less, more preferably 50.0 m 2 / g or less Even more preferably, it is 30.0 m 2 / g or less, and still more preferably 25.0 m 2 / g or less.
- the specific surface area is preferably 4.0 ⁇ 1000.0m 2 / g, more preferably 10.0 ⁇ 100.0m 2 / g, more preferably 15.0 ⁇ 50.0m 2 / g, more preferably Is 15.0 to 30.0 m 2 / g, still more preferably 18.0 to 30.0 m 2 / g, still more preferably 18.0 to 25.0 m 2 / g.
- the filter aid BET specific surface area can be determined by the method described in the examples.
- the integrated pore volume of 0.15 ⁇ m or less by the nitrogen adsorption method of the filter aid is preferably 0.3 mL / g or more, more preferably 0.4 mL / g or more, and further preferably from the viewpoint of scratch and particle reduction. It is 0.6 mL / g or more.
- the integrated pore volume is preferably 100.0 mL / g or less, more preferably 50.0 mL / g or less, still more preferably 10.0 mL / g or less, from the viewpoint of improving the productivity of the polishing composition.
- the cumulative pore volume is preferably 0.3 to 100.0 mL / g, more preferably 0.4 to 50.0 mL / g, still more preferably 0.6 to 10.0 mL / g, and even more preferably.
- the cumulative pore volume of 0.15 ⁇ m or less by the nitrogen adsorption method of the filter aid is the sum of the pore volumes of 0.15 ⁇ m or less in the volume-based pore distribution of the filter aid by the nitrogen adsorption method. Specifically, it can be determined by the method described in the examples.
- the water permeability of the filter aid when water is filtered with respect to the filter aid at 0.015 MPa is scratch and particle. From the viewpoint of reduction, it is preferably 9.9 ⁇ 10 ⁇ 14 m 2 or less, more preferably 5.0 ⁇ 10 ⁇ 14 m 2 or less, and further preferably 3.0 ⁇ 10 ⁇ 14 m 2 or less. is there. From the viewpoint of improving the productivity of the polishing composition, the transmittance is preferably 2.0 ⁇ 10 ⁇ 15 m 2 or more, more preferably 5.0 ⁇ 10 ⁇ 15 m 2 or more, Preferably, it is 9.9 ⁇ 10 ⁇ 15 m 2 or more.
- the transmittance is preferably 2.0 ⁇ 10 ⁇ 15 to 9.9 ⁇ 10 ⁇ 14 m 2 , more preferably 5.0 ⁇ 10 ⁇ 15 to 5.0 ⁇ 10 ⁇ 14 m 2 . More preferably 9.9 ⁇ 10 ⁇ 15 to 3.0 ⁇ 10 ⁇ 14 m 2 .
- the transmittance of the filter aid can be specifically determined by the method described in Examples.
- the laser average particle diameter of the filter aid is preferably 1 to 30 ⁇ m, more preferably 1 to 20 ⁇ m, still more preferably 1 to 18 ⁇ m, still more preferably 1 to 16 ⁇ m, and still more preferably, from the viewpoint of scratching and particle reduction. Is 2 to 16 ⁇ m, even more preferably 5 to 16 ⁇ m, and even more preferably 7 to 16 ⁇ m.
- the “laser average particle size” of the filter aid is the average particle size of the filter aid particles measured by a laser particle size distribution measuring device, and can be measured by the method described in the examples.
- the filter aid-containing filter used in the production method of the present invention is not particularly limited as long as it contains the filter aid on the filter surface and / or inside the filter.
- the filter aperture is preferably 1/10 or less of the average particle size of the filter aid, more preferably 1/20 or less, and even more preferably 1/30 or less.
- a body feed may be further combined with the precoat.
- the filter opening is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, still more preferably 3 ⁇ m or less, even more preferably 2 ⁇ m or less, and particularly preferably 1 ⁇ m or less from the viewpoint of preventing leakage of the filter aid.
- pre-coating is a method for forming a cake filtration filter, which is to form a thin layer of a filter aid having a thickness of about several millimeters on a filter material (filter medium) described later.
- a method of dispersing filter aid particles in water and scraping the filter aid with a filter medium to form a filter aid layer can be mentioned.
- Body feed is a method in which a certain amount of filter aid is added to a stock solution that is subjected to cake filtration during filtration, and the purpose is to improve the filterability of the stock solution. This is effective for a stock solution that has a fine particle size and quickly maximizes the cake resistance (cannot be filtered).
- the content of the filter aid in the filter aid containing filter (g / cm 2), from the viewpoint of the scratch and particle reduction is preferably 0.001 g / cm 2 or more, more preferably 0.005 g / cm 2 or more, further Preferably it is 0.01 g / cm 2 or more, even more preferably 0.02 g / cm 2 or more, even more preferably 0.04 g / cm 2 or more, and even more preferably 0.1 g / cm 2 or more. Further, from the viewpoint of improving the filtration rate, it is preferably 1 g / cm 2 or less, more preferably 0.8 g / cm 2 or less, still more preferably 0.6 g / cm 2 or less, and even more preferably 0.4 g / cm 2.
- the content (g / cm 2 ) of the filter aid is preferably 0.001 to 1 g / cm 2 , more preferably 0.005 to 0.8 g / cm 2 , and still more preferably 0.01 to 0.00. 6 g / cm 2 , even more preferably 0.02 to 0.4 g / cm 2 , even more preferably 0.04 to 0.3 g / cm 2 , even more preferably 0.04 to 0.2 g / cm 2 , Even more preferably, it is 0.1 to 0.2 g / cm 2 .
- the filter material of the filter aid-containing filter examples include filter paper, polyethylene, polypropylene, polyethersulfone, cellulose acetate, nylon, polycarbonate, Teflon (registered trademark) and other plastics, ceramics, and metal meshes.
- plastics such as filter paper, polyethylene, polypropylene, polyethersulfone, cellulose acetate, nylon, polycarbonate, and Teflon (registered trademark) are preferable.
- Filter paper, polyethylene, polypropylene, polyethersulfone, cellulose acetate, Nylon is more preferable, and filter paper, polyethylene, and polypropylene are more preferable.
- the shape of the filter aid-containing filter is not particularly limited, but from the viewpoint of ease of handling, scratching and particle reduction, a sheet type, a cylindrical type, a disk type, and a folding type are preferable, and a sheet type, a disk type, and a folding type are more preferable. A disk type and a folding type are more preferable.
- the conditions for filtration using the filter aid-containing filter are not particularly limited, but from the viewpoint of achieving both improved filtration accuracy and improved productivity, the differential pressure during filtration is preferably 0.01 to 10 MPa, and 0.05 to 1 MPa. Is more preferable, and 0.05 to 0.5 MPa is more preferable.
- the number of stages of the filter aid-containing filter is preferably from 1 to 5 stages, more preferably from 1 to 3 stages, and further preferably from 1 to 2 stages, from the viewpoint of improving both filtration accuracy and productivity.
- Filtration rate in terms of both productivity and the filtration accuracy is preferably 0.1 ⁇ 30L / (min ⁇ m 2), 0.5 ⁇ 25L / ( min ⁇ m 2), more preferably, 1 to 20 L / (min ⁇ m 2 ) is more preferable.
- the silica dispersion it is preferable to filter the silica dispersion to be treated with a depth filter, and then filter with a filter aid-containing filter, and further filter with a filter aid-containing filter, and then pleats. It is more preferable to filter with a mold filter. By removing particularly large coarse particles with a depth type filter, it is presumed that the excellent performance of the filter aid-containing filter is more remarkably exhibited, and it is possible to efficiently remove coarse particles and starch.
- the present invention provides, in other embodiments, step 1) a step of filtering a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm with a depth filter, and step 2 )
- step 1) a step of filtering a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm with a depth filter
- step 2 A method for producing a polishing liquid composition comprising a step of filtering the silica dispersion obtained in step 1 with a filter containing a filter aid having an average pore size of 0.1 to 3.5 ⁇ m by mercury porosimetry. (Hereinafter, also referred to as “production method (2) of the present invention”).
- the amount of coarse particles having a particle diameter of 0.5 ⁇ m or more in the silica dispersion obtained by filtration with a depth filter in Step 1 extends the life of the filter aid-containing filter used in Step 2 and increases productivity. From the viewpoint of improving, 11.0 ⁇ 10 4 pieces / mL or less is preferable, more preferably 10.0 ⁇ 10 4 pieces / mL or less, still more preferably 7.0 ⁇ 10 4 pieces / mL or less, and even more preferably.
- the present invention in still another aspect, comprises a step 1) silica dispersion to be treated containing colloidal silica having an average primary particle size of 1 to 100 nm, and a coarse particle amount of 11.0 ⁇ 10 4 particles / a filter containing a filter aid having a mean pore size of 0.1 to 3.5 ⁇ m by a mercury intrusion method, wherein the silica dispersion obtained in Step 2) and Step 1 is filtered.
- the manufacturing method (3) of this invention of the polishing liquid composition including the process of filtering-processing by.
- the amount of coarse particles in the silica dispersion obtained by the filtration treatment in Step 1 is 11.0 ⁇ 10 4 particles / mL is preferably 10.0 ⁇ 10 4 pieces / mL or less, more preferably 7.0 ⁇ 10 4 pieces / mL or less, still more preferably 6.0 ⁇ 10 4 pieces / mL or less, and even more preferably 5.0 ⁇ 10 4 pieces / mL or less, even more preferably 4.0 ⁇ 10 4 pieces / mL or less, and even more preferably 3.0 ⁇ 10 4 pieces / mL or less.
- the type of filtration in Step 1 is not limited, but is preferably a filtration treatment using a depth filter from the viewpoint of improving the removal efficiency of coarse particles and reducing the cost.
- FIG. 1 is a non-limiting embodiment of the production methods (2) and (3) of the present invention, and includes an embodiment including the steps shown in the schematic diagram of FIG.
- FIG. 1 is a schematic view of a process for preparing silica particles used in the polishing liquid composition.
- a depth type filter 3, a filter aid-containing filter 4, and a pleat type filter 5 are arranged in this order in the pipes P1 to P4. Are connected in series.
- the silica dispersion 2 to be treated put into the tank 1 is filtered in one pass through a filtration system composed of a depth filter 3, a filter aid-containing filter 4, and a pleat filter 5, and is used for the polishing composition.
- Silica particles Silica particles.
- the silica dispersion obtained in Step 2 of the production methods (2) and (3) of the present invention is further used as Step 3. It is preferable to have the process of filtering with a pleated filter.
- general-purpose colloidal silica refers to colloidal silica generally distributed in the market.
- “general-purpose colloidal silica” has a coarse particle amount of, for example, 20.0 ⁇ 10 4 particles / mL or more, 30.0 ⁇ 10 4 particles / mL or more, or 34.0 ⁇ 10 4 particles.
- Colloidal silica that is / mL or more. Examples of the upper limit of the amount of coarse particles include 200.0 ⁇ 10 4 particles / mL or less, 100.0 ⁇ 10 4 particles / mL or less, and 70.0 ⁇ 10 4 particles / mL or less.
- the amount of coarse particles of the general-purpose colloidal silica used in the present invention is preferably 20.0 ⁇ 10 4 to 200.0 ⁇ 10 4 particles / mL, and 20.0 ⁇ 10 4 to 100.0 ⁇ 10 4 particles / mL. Is more preferably 30.0 ⁇ 10 4 to 100.0 ⁇ 10 4 / mL, even more preferably 34.0 ⁇ 10 4 to 100.0 ⁇ 10 4 / mL, and 34.0 ⁇ 10 even more preferably 4 ⁇ 70.0 ⁇ 10 4 cells / mL.
- the depth type filter used in the production method of the present invention include a bag type (Sumitomo 3M Co., Ltd.) and a cartridge type filter (Advantech Toyo Co., Nippon Pole Co., CUNO Co., Daiwabo Co., Ltd.). Can be mentioned.
- the depth type filter has a feature that the pore structure of the filter medium is rough on the inlet side, finer on the outlet side, and finer continuously or stepwise from the inlet side to the outlet side. That is, among coarse particles, large particles are collected in the vicinity of the inlet side, and small particles are collected in the vicinity of the outlet side, so that effective filtration is possible.
- the shape of the depth filter may be a bag-like bag type or a hollow cylindrical cartridge type.
- a filter medium having the above-described characteristics that is simply formed into a pleat shape has a function of a depth filter, and is therefore classified as a depth filter.
- the depth type filter may be used in a single stage, or may be used in combination in multiple stages (for example, in a series arrangement). From the viewpoint of improving productivity, it is preferable to make filters of different diameters in multiple stages in a large order. . Moreover, you may use combining a bag type and a cartridge type.
- the coarse particles to be removed are appropriately selected according to the number of coarse particles in the silica dispersion to be treated, by appropriately selecting the pore size of the filter and the structure of the filter medium, and further appropriately selecting the processing order of the filter. Particle size control (filtration accuracy) and economy can be improved. That is, when a filter having a large pore structure is used upstream (upstream) of a fine filter, there is an effect that the lifetime of the filter can be extended as a whole manufacturing process.
- a filter medium is generally formed into a pleated shape (pleated shape) into a hollow cylindrical cartridge type (Advantech Toyo Co., Ltd., Nippon Pole Co., CUNO). Company, Daiwabo Co., Ltd.).
- pleated filters are said to have a thin filter material and are mainly collected on the filter surface, and generally have high filtration accuracy. It is a feature.
- the pleated filter may be used in one stage, or may be used in combination in multiple stages (for example, in a series arrangement).
- multi-stage filtration appropriately selects the filter pore size and the structure of the filter medium, and appropriately selects the processing order of the filter, so that the productivity of the polishing liquid composition in the present invention is improved.
- the filter used later can stabilize the quality in polishing liquid composition more by making the filter of the same hole diameter into a multistage.
- the pore size of the depth type filter and the pleated type filter is generally expressed as a filtration accuracy capable of removing 99%.
- a pore size of 1.0 ⁇ m indicates a filter capable of removing 99% of particles having a diameter of 1.0 ⁇ m.
- the pore diameter preferably exceeds 0.0 ⁇ m in order to exhibit the function of the filter.
- the pore size of the depth filter is preferably 5.0 ⁇ m or less, more preferably 3.0 ⁇ m or less, still more preferably 2.0 ⁇ m or less, and even more preferably 1.0 ⁇ m or less, from the viewpoint of reducing the coarse particle removal load. More preferably, it is 0.5 ⁇ m or less.
- the depth filter is multistage (for example, in series)
- the final filter has a pore size of submicron or less
- the coarse particle removal load in the filtration process using the filter aid-containing filter is further increased. It can be reduced and productivity can be improved.
- the pore size of the pleated filter is preferably 1.0 ⁇ m or less, more preferably 0.8 ⁇ m or less, further preferably 0.6 ⁇ m or less, and further preferably 0.5 ⁇ m or less from the viewpoint of reducing coarse particles.
- the filtration method in the present invention may be a recirculation method that repeatedly filters or a one-pass method.
- a batch method that repeats the one-pass method may be used.
- the circulation method preferably uses a pump in the circulation type, and uses a pump in the one-pass system.
- a pressure filtration with a small fluctuation range of the filter inlet pressure by introducing air pressure or the like into the tank. Can be used.
- a general dispersion step or particle removal step may be provided in addition to using the depth type filter or the pleated type filter.
- a dispersion process using a high-pressure dispersion apparatus such as a high-speed dispersion apparatus or a high-pressure homogenizer, or a coarse particle sedimentation process using a centrifugal separator or the like can be used.
- a high-pressure dispersion apparatus such as a high-speed dispersion apparatus or a high-pressure homogenizer, or a coarse particle sedimentation process using a centrifugal separator or the like
- each may be processed independently or may be processed in combination of two or more, and there is no limitation on the processing order of the combination. Further, the processing conditions and the number of processing times can be appropriately selected and used.
- the “silica dispersion to be treated” refers to a silica slurry (silica dispersion) before being subjected to a filtration treatment with a filter aid-containing filter.
- the “silica dispersion to be treated” may refer to a silica dispersion introduced into the first filter (first-stage filter) of the filtration system.
- the silica dispersion to be treated includes one containing colloidal silica and water, for example, one comprising colloidal silica and water, one containing other components, or a slurry of general-purpose colloidal silica. Is mentioned.
- the silica dispersion to be treated includes those prepared by mixing other components that can be blended in the polishing composition described below.
- the state of the silica dispersion to be treated is preferably a state in which colloidal silica is dispersed.
- a polishing liquid composition can be produced by subjecting a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm to filtration with a filter aid-containing filter. Specifically, the treated silica dispersion prepared by mixing colloidal silica, water, and other components is subjected to the filtration, or the treated silica dispersion containing colloidal silica and water is filtered. Then, the polishing composition can be produced by mixing other components with the obtained filtrate (filtered silica slurry).
- the colloidal silica used in the present invention can be obtained, for example, by a production method produced from a silicic acid aqueous solution.
- those obtained by surface modification or surface modification of these abrasive particles with functional groups, those obtained by compounding with surfactants or other abrasives, and the like can also be used.
- the average particle diameter of the primary particles of colloidal silica is 1 to 100 nm from the viewpoint of reducing scratches and particles and from the viewpoint of reducing the surface roughness (centerline average roughness: Ra, Peak to Valley value: Rmax). 1 to 80 nm is preferable. From the viewpoint of simultaneously improving the polishing rate, the thickness is more preferably 3 to 80 nm, further preferably 4 to 50 nm, further preferably 5 to 40 nm, and further preferably 5 to 30 nm.
- the average particle diameter of the primary particles of colloidal silica is a value measured by the method described in Examples.
- the content of colloidal silica in the silica dispersion to be treated is preferably 1 to 50% by weight, more preferably 10 to 45% by weight, and still more preferably from the viewpoint of reducing scratches and particles and improving productivity. Is 20 to 40% by weight, still more preferably 30 to 40% by weight.
- the content of coarse particles in the silica dispersion to be treated is usually 1 ⁇ 10 4 to 200 ⁇ 10 4 particles / mL, and from the viewpoint of reducing scratches and particles, 100 ⁇ 10 4 particles / mL.
- the following is preferable, 70 ⁇ 10 4 pieces / mL or less is more preferable, 50 ⁇ 10 4 pieces / mL or less is further preferable, and 40 ⁇ 10 4 pieces / mL or less is even more preferable.
- it is preferably 1 ⁇ 10 4 to 100 ⁇ 10 4 pieces / mL, more preferably 1 ⁇ 10 4 to 70 ⁇ 10 4 pieces / mL, and more preferably 1 ⁇ 10 4 to 50 ⁇ 10 4 pieces / mL, and even more preferably 1 ⁇ 10 4 to 40 ⁇ 10 4 pieces / mL.
- the silica dispersion to be treated may be a slurry of general-purpose colloidal silica or the amount of coarse particles is 20.
- the silica slurry may be 0 ⁇ 10 4 pieces / mL or more, 30.0 ⁇ 10 4 pieces / mL or more, or 34.0 ⁇ 10 4 pieces / mL or more. Therefore, from the viewpoint of reducing scratches and particles and improving productivity, it is preferably 20.0 ⁇ 10 4 to 200 ⁇ 10 4 particles / mL, more preferably 30.0 ⁇ 10 4 to 100 ⁇ . 10 4 pieces / mL, more preferably 34.0 ⁇ 10 4 to 70 ⁇ 10 4 pieces / mL.
- the content of coarse particles in the silica dispersion to be treated is a value measured by the method described in Examples.
- the 0.45 ⁇ m filter flow rate of the silica dispersion to be treated is usually 1 to 10 mL, preferably 2 to 10 mL, more preferably from the viewpoint of reducing scratches and particles and improving productivity. Is 3 to 10 mL, more preferably 4 to 10 mL, and even more preferably 5 to 10 mL.
- the 0.45 ⁇ m filter flow rate of the silica dispersion to be treated is a value measured by the method described in the examples.
- the ⁇ CV value of the silica dispersion to be treated is usually 1 to 20%, and preferably 1 to 15%, more preferably 1 to 13 from the viewpoint of reducing scratches and particles and improving productivity. %, More preferably 1 to 12%, still more preferably 1 to 11%.
- the ⁇ CV value of the silica dispersion to be treated is obtained by dividing the standard deviation obtained by measurement based on the scattering intensity distribution at a detection angle of 30 degrees (forward scattering) by the dynamic light scattering method by the average particle diameter.
- the coefficient of variation (CV30) multiplied by 100 and the coefficient of variation obtained by dividing the standard deviation by the average particle size and multiplying by 100, obtained by measurement based on the scattering intensity distribution at a detection angle of 90 degrees (side scatter). It is the difference ( ⁇ CV CV30 ⁇ CV90) from the value (CV90), and can be specifically measured by the method described in the examples.
- the ⁇ CV value of the polishing liquid composition is It is considered that scratches and particles after polishing can be reduced by adjusting to a predetermined range (reference: JP 2011-13078).
- the content of colloidal silica in the polishing composition when polishing the object to be polished is preferably 0.5% by weight or more, more preferably 1% by weight or more, and still more preferably 2 from the viewpoint of improving the polishing rate.
- the content of the colloidal silica may be either the content at the time of polishing composition production or the content at the time of use. Usually, it is produced as a concentrated liquid and diluted when used. There are many.
- water used in the polishing liquid composition examples include ion exchange water, distilled water, and ultrapure water.
- the content of water in the polishing composition corresponds to the balance obtained by removing the abrasive and other components from 100% by weight, preferably 60 to 99% by weight, more preferably 80 to 97% by weight.
- the pH of the silica dispersion to be treated is preferably 9 to 11, more preferably 9.2 to 10.8, and still more preferably 9.4 to from the viewpoint of suppressing the generation of coarse particles and improving the stability of colloidal silica. 10.6, even more preferably 9.5 to 10.5.
- the pH of the polishing composition produced in the present invention is not particularly limited, but when the polishing composition is used for polishing, the pH is preferably 0.1 to 7. In alkaline, scratches tend to occur more easily than acidic. The generation mechanism is not clear, but in an alkaline atmosphere in which abrasive particles repel each other due to surface charges, aggregates of abrasive primary particles or coarse abrasive primary particles contained in the polishing composition are dense in the polishing part.
- the pH is preferably determined according to the type of the object to be polished and the required characteristics.
- the pH is preferably 6 or less, more preferably 5 from the viewpoint of improving the polishing rate.
- it is further preferably 4 or less, still more preferably 3 or less, and still more preferably 2 or less.
- it is preferably 0.5 or more, more preferably 1.0 or more, and still more preferably 1.4 or more.
- the pH is 0.5 to 6 in consideration of the above viewpoint. More preferably, it is 1.0 to 5, still more preferably 1.4 to 4, still more preferably 1.4 to 3, and still more preferably 1.4 to 2.
- the pH of the polishing composition can be adjusted as appropriate with the following acid, salt, or alkali, for example. Specifically, nitric acid, sulfuric acid, nitrous acid, persulfuric acid, hydrochloric acid, perchloric acid, phosphoric acid, phosphonic acid, phosphinic acid, pyrophosphoric acid, tripolyphosphoric acid, amidosulfuric acid and other inorganic acids or salts thereof, 2-amino Ethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetra (methylenephosphonic acid), diethylenetriaminepenta (methylenephosphonic acid), ethane-1,1-diphosphonic acid, ethane- 1,1,2-triphosphonic acid, ethane-1-hydroxy-1,1-diphosphonic acid, ethane-1-hydroxy-1,1,2-triphosphonic acid, ethane-1,2-dicarboxy-1,2-
- nitric acid, sulfuric acid, hydrochloric acid, perchloric acid or salts thereof are more preferable.
- organic phosphonic acids or salts thereof 1-hydroxyethylidene-1,1-diphosphone is preferred. More preferred are acids, aminotri (methylenephosphonic acid), ethylenediaminetetra (methylenephosphonic acid), diethylenetriaminepenta (methylenephosphonic acid) or salts thereof. You may use these individually or in mixture of 2 or more types.
- the acid salt is not particularly limited, and specific examples include salts with metals, ammonia, and alkylamines.
- Specific examples of the metal include metals belonging to 1A, 1B, 2A, 2B, 3A, 3B, 4A, 6A, 7A, or Group 8 of the periodic table (long period type). From the viewpoint of reducing scratches, ammonia or a metal belonging to Group 1A is preferable.
- the polishing composition for polishing the object to be polished preferably contains a heterocyclic aromatic compound from the viewpoint of scratching the substrate after polishing and reducing particles.
- the heterocyclic aromatic compound is preferably 1H-benzotriazole from the viewpoint of scratching the substrate after polishing and particle reduction.
- the content of the heterocyclic aromatic compound in the polishing liquid composition is 0.01 to 10% by weight with respect to the total weight of the polishing liquid composition from the viewpoint of reducing scratches and particles on the substrate after polishing.
- 0.02 to 5 wt% is more preferable, 0.05 to 2 wt% is further preferable, 0.06 to 1 wt% is even more preferable, 0.07 to 0.5 wt% is still more preferable, Even more preferred is 0.08-0.3 wt%.
- the heterocyclic aromatic compound in the polishing composition may be one kind or two or more kinds.
- a polishing liquid composition for polishing an object to be polished is a water-soluble polymer having an anionic group (AFM-Rmax) from the viewpoint of reducing scratches, particles and maximum surface roughness of the substrate after polishing (AFM-Rmax).
- a polishing liquid composition for polishing an object to be polished is a water-soluble polymer having an anionic group (AFM-Rmax) from the viewpoint of reducing scratches, particles and maximum surface roughness of the substrate after polishing (AFM-Rmax).
- a polishing liquid composition for polishing an object to be polished is a water-soluble polymer having an anionic group (AFM-Rmax) from the viewpoint of reducing scratches, particles and maximum surface roughness of the substrate after polishing (AFM-Rmax).
- a polishing liquid composition for polishing an object to be polished is a water-soluble polymer having an anionic group (AFM-Rmax) from the viewpoint of reducing scratches, particles and maximum surface roughness of the substrate after polishing (AFM-Rmax).
- anionic group of the anionic water-soluble polymer examples include a carboxylic acid group, a sulfonic acid group, a sulfuric acid ester group, a phosphoric acid ester group, and a phosphonic acid group.
- the maximum value of scratches, particles, and surface roughness From the viewpoint of reducing (AFM-Rmax), those having a carboxylic acid group and / or a sulfonic acid group are more preferable, and those having a sulfonic acid group are more preferable.
- These anionic groups may take the form of neutralized salts.
- water-soluble polymers having a carboxylic acid group and / or a sulfonic acid group examples include (meth) acrylic acid / sulfonic acid copolymers, and (meth) acrylic acid / 2- (meth) acrylamido-2-methylpropanesulfonic acid.
- a copolymer is preferred.
- the weight average molecular weight of the anionic water-soluble polymer is preferably 500 or more and 100,000 or less, more preferably 500 or more and 50,000 or less, further preferably 500 or more and 20,000 or less, from the viewpoint of scratch and particle reduction and productivity maintenance. Even more preferably, it is 1000 or more and 10,000 or less, still more preferably 1000 or more and 8000 or less, still more preferably 1000 or more and 5000 or less, still more preferably 1000 or more and 4000 or less, and still more preferably 1000 or more and 3000 or less. Specifically, the weight average molecular weight is measured by the measurement method described in Examples.
- the content of the anionic water-soluble polymer in the polishing composition is preferably 0.001 to 1% by weight or more, more preferably 0.005 to more preferably from the viewpoint of achieving both scratch and particle reduction and productivity. It is 0.5% by weight, more preferably 0.08 to 0.2% by weight, still more preferably 0.01 to 0.1% by weight, and still more preferably 0.01 to 0.075% by weight.
- the polishing liquid composition for polishing the object to be polished preferably contains an aliphatic amine compound or an alicyclic amine compound from the viewpoint of scratching the substrate surface after polishing and reducing particles.
- the aliphatic amine compound is preferably N-aminoethylethanolamine from the viewpoint of scratching the substrate surface after polishing and reducing particles.
- the alicyclic amine compound is preferably N- (2-aminoethyl) piperazine and hydroxyethylpiperazine from the viewpoint of scratching the substrate surface after polishing and reducing particles.
- the content of the aliphatic amine compound or alicyclic amine compound in the polishing liquid composition is 0.001 to the weight of the entire polishing liquid composition from the viewpoint of reducing scratches and particles on the substrate surface after polishing. It is preferably 10% by weight, more preferably 0.005 to 5% by weight, even more preferably 0.008 to 2% by weight, still more preferably 0.01 to 1% by weight, and 0.01 to 0.5%. % By weight is even more preferred, and 0.01 to 0.1% by weight is even more preferred.
- the aliphatic amine compound or alicyclic amine compound in polishing liquid composition may be one type, and may be two or more types.
- the polishing composition preferably contains an oxidizing agent from the viewpoint of improving the polishing rate.
- an oxidizing agent that can be used in the polishing liquid composition of the present invention, from the viewpoint of improving the polishing rate, peroxide, permanganic acid or a salt thereof, chromic acid or a salt thereof, peroxo acid or a salt thereof, oxygen acid or an acid thereof Examples thereof include salts, metal salts, nitric acids, sulfuric acids and the like.
- Examples of the peroxide include hydrogen peroxide, sodium peroxide, barium peroxide and the like.
- Examples of permanganic acid or a salt thereof include potassium permanganate, and examples of chromic acid or a salt thereof include chromic acid metal salt and metal dichromate.
- a peroxo acid or a salt thereof includes peroxo acid. Examples include disulfuric acid, ammonium peroxodisulfate, metal peroxodisulfate, peroxophosphoric acid, peroxosulfuric acid, sodium peroxoborate, performic acid, peracetic acid, perbenzoic acid, perphthalic acid, etc.
- Hypochlorous acid, hypobromite, hypoiodous acid, chloric acid, bromic acid, iodic acid, sodium hypochlorite, calcium hypochlorite and the like, and metal salts include iron chloride (III ), Iron (III) sulfate, iron (III) nitrate, iron (III) citrate, and iron (III) ammonium sulfate.
- the oxidizing agent include hydrogen peroxide, iron (III) nitrate, peracetic acid, ammonium peroxodisulfate, iron (III) sulfate, and iron (III) ammonium sulfate.
- hydrogen peroxide is mentioned from the viewpoint that metal ions do not adhere to the surface and are generally used and inexpensive.
- These oxidizing agents may be used alone or in admixture of two or more.
- the content of the oxidizing agent in the polishing liquid composition is preferably 0.01% by weight or more, more preferably 0.05% by weight or more, and further preferably 0.1% by weight or more from the viewpoint of improving the polishing rate. From the viewpoint of reducing the surface roughness of the substrate, it is preferably 4% by weight or less, more preferably 2% by weight or less, and still more preferably 1% by weight or less. Therefore, in order to improve the polishing rate while maintaining the surface quality, the content is preferably 0.01 to 4% by weight, more preferably 0.05 to 2% by weight, and still more preferably 0.1 to 1%. % By weight.
- polishing liquid composition can be blended in the polishing liquid composition as necessary.
- a thickener a dispersant, a rust inhibitor, a basic substance, a surfactant, and the like can be given.
- the amount of the polishing composition liquid obtained by the production method of the present invention is preferably 25 mL or more, more preferably 30 mL or more, and 50 mL or more. More preferably, 70 mL or more is even more preferable, and 100 mL or more is even more preferable.
- the amount of filter liquid passing through the polishing composition is a value measured by the method described in Examples.
- the content of coarse particles in the polishing composition obtained by the production method of the present invention is preferably 0.5 ⁇ 10 4 to 10 ⁇ 10 4 from the viewpoints of scratch and particle reduction and productivity.
- content of the coarse particle in polishing liquid composition is measured by the method as described in an Example.
- the ⁇ CV value of the polishing composition obtained by the production method of the present invention is preferably 0.1 to 10%, more preferably 0.1 from the viewpoint of reducing scratches and particles and improving productivity. -5.0%, more preferably 0.1-4.0%, even more preferably 0.1-3.0%, still more preferably 0.1-2.5%.
- the polishing liquid composition obtained by the production method of the present invention is supplied, for example, between a non-woven organic polymer polishing cloth or the like (polishing pad) and the substrate to be polished, that is, the polishing liquid composition is polished.
- the substrate is supplied to a substrate polishing surface sandwiched between polishing pads with a pad attached thereto, and is used in the polishing step while contacting the substrate by moving the polishing plate and / or the substrate under a predetermined pressure. By this polishing, generation of scratches and particles can be remarkably suppressed.
- the polishing liquid composition is particularly suitable for the production of precision component substrates.
- it is suitable for polishing precision component substrates such as substrates of magnetic recording media such as magnetic disks and magneto-optical disks, optical disks, photomask substrates, optical lenses, optical mirrors, optical prisms, and semiconductor substrates.
- the manufacturing method of the present invention is used in a polishing process of a silicon wafer (bare wafer), a formation process of a buried element isolation film, a planarization process of an interlayer insulating film, a formation process of a buried metal wiring, a formation process of a buried capacitor, etc.
- the polishing liquid composition obtained in (1) can be used.
- the polishing composition obtained by the production method of the present invention is particularly effective in the polishing process, but can be similarly applied to other polishing processes such as a lapping process.
- Suitable materials for the polishing object using the polishing composition obtained by the production method of the present invention include, for example, metals or semi-metals such as silicon, aluminum, nickel, tungsten, copper, tantalum, titanium, or the like.
- metals or semi-metals such as silicon, aluminum, nickel, tungsten, copper, tantalum, titanium, or the like.
- glassy substances such as alloys, glass, glassy carbon, and amorphous carbon, ceramic materials such as alumina, silicon dioxide, silicon nitride, tantalum nitride, and titanium carbide, and resins such as polyimide resins.
- a Ni—P plated aluminum alloy substrate or a glass substrate such as crystallized glass or tempered glass is more suitable
- a Ni—P plated aluminum alloy substrate is more suitable.
- the polishing liquid composition of the present invention has a shape having a flat portion such as a disk shape, a plate shape, a slab shape, a prism shape, or a shape having a curved surface portion such as a lens. Things are used. Among them, it is excellent for polishing a disk-shaped workpiece.
- the surface roughness which is a measure of surface smoothness, is not limited in its evaluation method, but for example, it is evaluated as a roughness that can be measured at a short wavelength of 10 ⁇ m or less in an atomic force microscope (AFM), and the center line average It can be expressed as roughness Ra (AFM-Ra).
- the polishing composition of the present invention is suitable for a polishing process for a magnetic disk substrate, and further for a polishing process for reducing the surface roughness (AFM-Ra) of the substrate after polishing to 2.0 mm or less.
- the polishing composition obtained by the production method of the present invention after the second process, which significantly reduces scratches and particles, and is excellent. From the viewpoint of obtaining surface smoothness, it is more preferably used in the finish polishing step.
- the finish polishing process refers to at least one final polishing process when there are a plurality of polishing processes.
- polishing machines may be used, and when different polishing machines are used, a substrate is provided for each process. It is preferable to wash.
- the polishing machine is not particularly limited.
- the substrate produced in this manner has significantly reduced scratches and particles and is excellent in surface smoothness. That is, the surface roughness after polishing (AFM-Ra) is, for example, 1 mm or less, preferably 0.9 mm or less, more preferably 0.8 mm or less.
- the surface property of the substrate before being subjected to the polishing step using the polishing composition after the filtration treatment using the filter aid-containing filter in the present invention is not particularly limited.
- the AFM-Ra is 10 mm or less.
- a substrate having surface properties is suitable.
- the abrasive used in the production of such a substrate may be the same as that used in the polishing composition of the present invention.
- the polishing step is preferably performed after the second step among the plurality of polishing steps, and particularly preferably performed in the finish polishing step.
- the substrate produced as described above has excellent surface smoothness and a surface roughness (AFM-Ra) of, for example, 1.0 mm or less, preferably 0.9 mm or less, more preferably 0.8 mm or less. can get.
- AFM-Ra surface roughness
- the manufactured substrate has very few scratches. Therefore, when the substrate is, for example, a memory hard disk substrate, a recording density of 750 GB / Disk (3.5 inches), further 1 TB / Disk (3.5 inches) can be supported.
- Example 1 to 9 Comparative Examples 1 to 8
- the silica dispersion to be treated was filtered using a diatomaceous earth filter, and polishing compositions were produced by the production methods of Examples 1 to 9 and Comparative Examples 1 to 8.
- the substrate was polished using the polishing composition, and the substrate surface after polishing was evaluated.
- the silica dispersion to be treated, the diatomaceous earth filter, the filtration method, and the measurement methods for various parameters are as follows.
- colloidal silica slurry B JGC Catalysts & Chemicals, Inc.
- ⁇ Measuring method of average particle diameter of primary particles of colloidal silica> First, 1.5 g of the colloidal silica slurry A to C is collected in a 200 mL beaker, and 100 mL of ion exchange water is added and mixed with a stirrer. Next, the pH of the sample solution is adjusted to 3.0 with a 0.1 mol / L hydrochloric acid standard solution using a potentiometric titrator. Add 30.0 g of sodium chloride and dissolve with a stirrer, add ion-exchanged water up to the 150 mL mark of the beaker and mix with a stirrer. Immerse in a constant temperature water bath (20 ⁇ 2 ° C.) for about 30 minutes.
- the measurement sample was a colloidal silica slurry before (or after) filtration with a filter containing a filter aid, sulfuric acid (special grade made by Wako Pure Chemical Industries), HEDP (1-hydroxyethylidene-1,1-diphosphonic acid, Thermos Japan) and hydrogen peroxide (Asahi Denka Co., Ltd., concentration: 35% by weight) were added to an aqueous solution diluted with ion-exchanged water, mixed, and then filtered through a 1.20 ⁇ m filter (Minisart 17593, Sartorius). Prepared.
- colloidal silica, sulfuric acid, HEDP, and hydrogen peroxide were 5 wt%, 0.4 wt%, 0.1 wt%, and 0.4 wt%, respectively.
- 20 mL of the obtained measurement sample was put into a dedicated 21 ⁇ cylindrical cell and set in a dynamic light scattering apparatus DLS-6500 manufactured by Otsuka Electronics.
- DLS-6500 manufactured by Otsuka Electronics.
- the CV value (CV90) of colloidal silica at a detection angle of 90 degrees was calculated as a value obtained by dividing the standard deviation in the scattering intensity distribution measured according to the above measurement method by the particle size and multiplying by 100. Similar to the CV90 measurement method, the CV value (CV30) of colloidal silica at a detection angle of 30 degrees was measured, and the value obtained by subtracting CV90 from CV30 was determined as the ⁇ CV value of the silica particles.
- ⁇ Measurement method of coarse particle amount The colloidal silica slurry before (or after) filtering the measurement sample with a filter containing a filter aid was injected into the following measuring device with a 6 mL syringe, and the amount of coarse particles was measured.
- ⁇ Measurement method of filter flow rate> A colloidal silica slurry before (or after) filtering the measurement sample with a filter containing a filter aid is filtered with a predetermined filter (hydrophilic PTFE 0.45 ⁇ m filter, model: 25HP045AN, manufactured by Advantech) at an air pressure of 0.25 MPa. The solution was passed through the filter under a constant pressure, and the amount of solution passed until the filter was closed was determined.
- a predetermined filter hydrophilic PTFE 0.45 ⁇ m filter, model: 25HP045AN, manufactured by Advantech
- Measurement condition Measurement cell: Micromeritics 5cc-Powder (08-0444) Measurement method: Pressure control method (pressure table mode) Low Pressure equilibrium time 5secs High pressure equilibrium time 5secs Parameters relating to Hg: contact angle: 130 °, surface tension: 485 dynes / cm Stem Volume Used: Adjust the sample volume to about 50% below 100%
- ⁇ Measurement method of BET specific surface area of filter aid About 1 g of each filter aid precisely weighed was set in ASAP2020 (manufactured by Shimadzu Corporation, specific surface area / pore distribution measuring device), the BET specific surface area was measured by a multipoint method, and the BET constant C was positive. Values were derived within a range. The sample was pretreated by raising the temperature at 10 ° C./min and holding at 100 ° C. for 2 hours. In addition, deaeration was performed up to 500 ⁇ m Hg at 60 ° C. Deaeration was performed.
- ⁇ Method for measuring laser average particle size of filter aid The value obtained as a volume-based median diameter obtained by measuring each filter aid with a laser diffraction / scattering particle size distribution analyzer (trade name LA-920, manufactured by Horiba Seisakusho) was defined as the laser average particle diameter.
- ⁇ Measurement method of integrated pore volume of 0.15 ⁇ m or less> The accumulated pore volume of 0.15 ⁇ m or less of the filter aid was measured by a nitrogen adsorption method. Specifically, about 1 g of each filter aid precisely weighed is set in ASAP2020 (manufactured by Shimadzu Corporation, specific surface area / pore distribution measuring device), and is obtained from the nitrogen adsorption isotherm by the Halsey equation of the BJH method. The total pore volume of 0.15 ⁇ m or less was defined as the cumulative pore volume of 0.15 ⁇ m or less. The sample was pretreated by raising the temperature at 10 ° C./min and holding at 100 ° C. for 2 hours. In addition, deaeration was performed up to 500 ⁇ m Hg at 60 ° C.
- the filter aid is No. manufactured by Advantech. The plate was sandwiched between 5A filter papers and placed in a 90 mm ⁇ flat plate type SUS housing (INLET90-TL manufactured by Sumitomo 3M Co., Ltd., effective filtration area 55.4 cm 2 ) and filtered.
- the transmittance k was calculated by introducing the following values ( ⁇ ⁇ L indicates a different value for each sample).
- ⁇ Preparation of filter aid containing filter> (Filter aid)
- the following a to k were used as filter aids.
- c Radiolite DX-P5 (Laser average particle size 14.5 ⁇ m, diatomaceous earth, Showa Chemical Industry Co., Ltd.)
- Radiolite No. 200 (Laser average particle size 13.9 ⁇ m, diatomaceous earth, Showa Chemical Industries, Ltd.)
- the filter aid dispersion aqueous solution is filtered at a pressure of 0.1 MPa or less to form a uniform cake layer of the filter aid on the filter paper, and then washed with 1-2 L of ion exchange water. A filter containing diatomaceous earth was obtained.
- the colloidal silica slurry A to C is filtered for 1 L at a pressure of 0.1 MPa while the diatomaceous earth-containing filter remains wet with washing water without being dried, and the filtered colloidal for use in a polishing liquid composition Silica was obtained.
- ⁇ Measurement method of filter flow rate The filtered colloidal silica obtained by the above filtration is passed through the filter under a constant pressure of 0.25 MPa with a predetermined filter (hydrophilic PTFE 0.45 ⁇ m filter, model: 25HP045AN, manufactured by Advantech). The amount of liquid passing until the blockage was determined.
- polishing liquid compositions (Examples 1 to 4). And Comparative Examples 1 to 4>
- 0.1% by weight of benzotriazole Na salt 0.1% by weight of benzotriazole Na salt, 0.03% by weight of N-aminoethylethanolamine, acrylic acid / acrylamido-2-methylpropanesulfonic acid copolymer sodium salt (molar ratio 90 / 10, weight average molecular weight 2000, manufactured by Toagosei Co., Ltd.) 0.02% by weight, sulfuric acid 0.4% by weight, 1-hydroxyethylidene-1,1-diphosphonic acid 0.05% by weight, hydrogen peroxide 0 4% by weight of the mixed aqueous solution was stirred, and the filtered colloidal silica filtered through the diatomaceous earth-containing filter was added to 5% by weight to prepare polishing liquid compositions (Examples 1 to 4). And Comparative Examples 1 to 4).
- the pH of each polishing composition was 1.4 to 1.5.
- polishing composition was prepared by adding silica at 5% by weight (Examples 5 to 9 and Comparative Examples 5 to 8). Note that the pH of each polishing composition was 1.3 to 1.5.
- the weight average molecular weight of the anionic water-soluble polymer (acrylic acid / acrylamido-2-methylpropanesulfonic acid copolymer sodium salt) was measured by gel permeation chromatography (GPC) method under the following measurement conditions.
- the substrate to be polished was polished using the polishing composition produced by the production methods of Examples 1 to 9 and Comparative Examples 1 to 8 prepared as described above, and washed with pure water to obtain a substrate for evaluation. .
- the number of scratches and the number of particles of this evaluation substrate were evaluated.
- the evaluation results are shown in Table 1 below.
- a method for preparing the polishing liquid composition, a method for measuring each parameter, a polishing condition (polishing method), a cleaning condition, and an evaluation method are as follows.
- a Ni—P plated aluminum alloy substrate having an outer diameter of 95 mm ⁇ and an inner diameter of 25 mm ⁇ having a thickness of 1.27 mm and roughly polished with a polishing solution containing an alumina abrasive in advance and having an AFM-Ra of 5 to 15 mm.
- Polishing tester Speed Fam Co., double-sided 9B polishing machine
- Polishing pad Fujibow Co., urethane finishing polishing pad
- Upper plate rotation speed 32.5 r / min
- Polishing liquid composition supply amount 100 mL / Minute / Main polishing time: 4 minutes / Main polishing load: 7.8 kPa ⁇ Number of loaded substrates: 10
- Measurement equipment Candela OSA6100 manufactured by KLA-Tencor ⁇ Evaluation: Randomly select 4 out of the substrates put into the polishing tester, and divide the total number of particles (pieces) on both sides of each of the 4 substrates by 8 The number of particles was calculated.
- Example 10 and Comparative Examples 9 to 10 The silica dispersion to be treated was filtered with a filtration system combining a depth filter, a diatomaceous earth-containing filter, and a pleated filter to produce a polishing composition (Example 10).
- a polishing liquid composition was produced by filtering two types of silica dispersions using a filtration system that combines a circulation filtration of a depth filter and a pleated filter (Comparative Examples 9 and 10).
- the substrate was polished using each polishing composition, and the substrate surface after polishing was evaluated. Unless otherwise specified, the measurement methods for various parameters described in Table 2 below were the same as those in Example 1.
- the manufacturing method of the polishing liquid composition of Example 10 As a filtration system for obtaining the filtered colloidal silica used in the polishing liquid composition of Example 10, one depth filter is provided in the first stage, and one diatomaceous earth-containing filter (cake filter) is provided in the second stage. A filtration system in which one pleated filter was provided at the stage and these filters were arranged in three stages in this order was employed. As a schematic diagram of this filtration system, reference can be made to FIG. The filtered colloidal silica was obtained by carrying out 1-pass filtration of the colloidal silica slurry D which is a to-be-processed silica dispersion liquid with the said filtration system.
- a polishing composition was prepared in the same manner as in Example 1.
- the time required for processing 50 L of colloidal silica slurry D through the filtration system with a small diaphragm pump was 0.9 hours (average flow rate was 0.95 L / min, average filtration rate was 17.5). 9L / (min ⁇ m2)) (Table 2 below).
- the filters used are as follows.
- the manufacturing method of the polishing liquid composition of the comparative example 9> As the first-stage filtration system for obtaining the filtered colloidal silica used in the polishing liquid composition of Comparative Example 9, a circulation filtration system in which two depth filters were arranged was adopted. And the filtration system which has arrange
- the colloidal silica after filtration was obtained by carrying out 1-pass filtration with the said 2nd stage filtration system.
- a polishing composition was prepared in the same manner as in Example 1.
- the time required to circulate 50 L of colloidal silica slurry D through the first-stage filtration system with a small diaphragm pump and to perform filtration equivalent to 8 passes was 3.3 hours (average flow rate was 2 0.0 L / min).
- the time required for filtering the second stage filtration system in one pass was 0.4 hours. Therefore, the time required for the first and second stages of filtration was 3.7 hours in total (Table 2 below).
- the depth type and pleat type filters used are the same as those in Example 10.
- a polishing composition was prepared in the same manner as in Comparative Example 9, except that colloidal silica slurry E was used instead of colloidal silica slurry D, which is the silica dispersion to be treated.
- the time required to circulate 50 L of colloidal silica slurry E through the first-stage filtration system with a small diaphragm pump and to perform filtration equivalent to 8 passes was 3.3 hours (average flow rate was 2 0.0 L / min).
- the time required for filtering the second stage filtration system in one pass was 0.4 hours. Therefore, the time required for the first and second stages of filtration was 3.7 hours in total (Table 2 below).
- the substrate to be polished was polished using the polishing composition produced by the production method of Example 10 and Comparative Examples 9 to 10, and the number of scratches and the number of particles of the polished substrate were evaluated.
- the evaluation results are shown in Table 2 below.
- the substrate to be polished, the polishing conditions (polishing method) and the evaluation method are the same as in Example 1.
- Comparative Example 10 includes filtering a silica slurry (slurry E) obtained by subjecting a general-purpose colloidal silica slurry (slurry D) to an additional treatment (for example, a centrifugal separation treatment) with a circulation filter system of a depth type filter. It is a manufacturing method of the conventional polishing liquid composition. On the other hand, Example 10 is the manufacturing method of the polishing liquid composition which employ
- the manufacturing method of Example 10 can use the general-purpose colloidal silica slurry (slurry E) as it is without performing an additional treatment (for example, a centrifugal separation treatment), so that costs and time can be reduced, and productivity can be reduced. Will improve.
- Examples 11 to 13 and Comparative Example 11 A polishing composition was produced in the same manner as in Example 10 except that a depth type filter having a different history of filtration throughput was used as the depth type filter of Example 10 (Examples 11 to 13). Moreover, the polishing liquid composition was manufactured with the manufacturing method similar to Example 10 except not using a depth type filter (comparative example 11). The substrate was polished using each polishing composition, and the substrate surface after polishing was evaluated. Unless otherwise specified, the measurement methods for various parameters described in Table 3 below were the same as in Example 1.
- a polishing composition was prepared in the same manner as in Example 1.
- the depth type filter, diatomaceous earth-containing filter, and pleated type filter used are the same as in Example 10.
- a depth type filter having a history of filtration amount in the order of Examples 11, 12, and 13 was used.
- the depth filter has a reduced ability to remove coarse particles as its usage history (filtration history) increases. That is, the coarse particles contained in the silica dispersion after the first-stage depth filter filtration increase in the order of Examples 11, 12, and 13 (Table 3 below).
- the amount that can be processed before the second stage diatomite filter is blocked is measured, and the results are shown in Table 3 below.
- the substrate to be polished was polished using the polishing composition produced by the production methods of Examples 11 to 13 and Comparative Example 11 as described above, and the number of scratches and particles of the polished substrate were evaluated. The evaluation results are shown in Table 3 below.
- the substrate to be polished, the polishing conditions (polishing method) and the evaluation method are the same as in Example 1.
- the polishing composition produced by the production method of the present invention can be used, for example, in a polishing process of a precision component substrate for high density or high integration.
- the present invention relates to: ⁇ 1> A method for producing a polishing composition comprising a step of subjecting a silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm to a filter containing a filter aid, The method for producing a polishing composition, wherein the filter aid has an average pore size of 0.1 to 3.5 ⁇ m by a mercury intrusion method; ⁇ 2> The method for producing a polishing composition according to ⁇ 1>, wherein the filter aid is diatomaceous earth; ⁇ 3> The method for producing a polishing liquid composition according to ⁇ 1> or ⁇ 2>, wherein an accumulated pore volume of 0.5 ⁇ m or less by a mercury intrusion method of the filter aid is 2.5 mL / g or more; ⁇ 4> The filter aid has a BET specific surface area of 4.0 m 2 / g or more, and an integrated pore volume of 0.15 ⁇ m or less by a nitrogen ad
- Step 2 A step of filtering the silica dispersion obtained in Step 1 with a filter containing a filter aid having an average pore size of 0.1 to 3.5 ⁇ m by mercury porosimetry.
- the coarse particle amount is preferably 10.0 ⁇ 10 4 particles / mL or less, more preferably 7.0 ⁇ 10 4 particles / mL or less, and further preferably.
- the amount of coarse particles having a particle diameter of 0.5 ⁇ m or more in the treated silica dispersion liquid is 20.0 ⁇ 10 4 particles / mL or more, according to any one of ⁇ 1> to ⁇ 13>.
- a method for producing a polishing composition ⁇ 15>
- the amount of coarse particles having a particle diameter of 0.5 ⁇ m or more in the silica dispersion to be treated is 200.0 ⁇ 10 4 particles / mL or less, according to any one of ⁇ 1> to ⁇ 14>.
- a method for producing a polishing composition ⁇ 16> The method for producing a polishing liquid composition according to any one of ⁇ 1> to ⁇ 15>, wherein the content of colloidal silica in the silica dispersion to be treated is 1 to 50% by weight; ⁇ 17> The above ⁇ 1> to ⁇ 16>, wherein the content of coarse particles having a particle size of 0.5 ⁇ m or more in the obtained polishing liquid composition is 0.5 to 10 ⁇ 10 4 particles / mL
- Production method ⁇ 19> The method for producing a polishing liquid composition according to any one of ⁇ 1> to ⁇ 18>, wherein a differential pressure during filtration in the filtration treatment using the filter containing the filter aid is 0.01 to 10 MPa. ; ⁇ 20> The polishing composition according to any one of ⁇ 1> to ⁇ 19>, wherein a filtration rate in a filtration treatment using the filter containing the filter aid is 0.1 to 30 L / (min ⁇ m 2 ). Manufacturing method; ⁇ 21> The average pore diameter of the filter aid by mercury porosimetry is preferably 0.1 to 3.0 ⁇ m, more preferably 0.1 to 2.7 ⁇ m, still more preferably 1.0 to 2.7 ⁇ m, and even more.
- the manufacturing method of the polishing liquid composition in any one of ⁇ 1> to ⁇ 20>; ⁇ 22>
- the cumulative pore volume of 0.5 ⁇ m or less by a mercury intrusion method of the filter aid is preferably 2.5 to 1000 mL / g, more preferably 2.7 to 100 mL / g, and still more preferably 3.0 to 50 mL / g, even more preferably 4.0 to 20 mL / g, even more preferably 4.5 to 10 mL / g, and even more preferably 4.5 to 6 mL / g.
- the method for producing a polishing composition according to any one of ⁇ 1> to ⁇ 21>, which is 2.5 mL / g or more; ⁇ 23> BET specific surface area of the filter aid is preferably 4.0 ⁇ 1000.0m 2 / g, more preferably 10.0 ⁇ 100.0m 2 / g, more preferably 15.0 ⁇ 50.0 m 2 / G, more preferably 15.0 to 30.0 m 2 / g, even more preferably 18.0 to 30.0 m 2 / g, still more preferably 18.0 to 25.0 m 2 / g, 1> to ⁇ 22> a method for producing the polishing composition according to any one of the above; ⁇ 24> An integrated pore volume of 0.15 ⁇ m or less by nitrogen adsorption method is preferably 0.3 to 100.0 mL / g, more preferably 0.4 to 50.0 mL / g, and still more preferably 0.6 to 10.0 mL / g, even more preferably 0.6-5.0
- step 1 the silica dispersion to be treated containing colloidal silica having an average primary particle diameter of 1 to 100 nm is used in a coarse particle amount of 0.5 ⁇ m or more, preferably 10.0 ⁇ 10.
- the amount of coarse particles having a particle diameter of 0.5 ⁇ m or more in the silica dispersion to be treated is preferably 20.0 ⁇ 10 4 to 200.0 ⁇ 10 4 particles / mL, more preferably 20.0 ⁇ 10.
- the content of coarse particles having a particle size of 0.5 ⁇ m or more in the obtained polishing composition is preferably 0.5 ⁇ 10 4 to 5 ⁇ 10 4 particles / mL, more preferably 0.5 ⁇ 10.
- polishing composition according to any one of ⁇ 1> to ⁇ 27>, which is 4 to 4 ⁇ 10 4 pieces / mL, more preferably 0.5 ⁇ 10 4 to 3 ⁇ 10 4 pieces / mL.
- Method; ⁇ 29> A polishing composition produced by the production method according to any one of ⁇ 1> to ⁇ 28>; ⁇ 30> The description ⁇ 29>, further comprising an acid, an oxidizing agent, a water-soluble polymer having an anionic group, a heterocyclic aromatic compound, and an aliphatic amine compound or an alicyclic amine compound.
- a polishing liquid composition of ⁇ 31> A polishing composition is produced by the production method according to any one of ⁇ 1> to ⁇ 28>, and the polishing composition is supplied to a surface to be polished of a substrate to be polished, and the polishing is performed.
- a method of manufacturing a magnetic disk substrate comprising bringing a polishing pad into contact with a target surface and moving the polishing pad and / or the substrate to be polished to polish the polishing target surface.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
Description
珪藻土フィルターを用いて被処理シリカ分散液をろ過し、実施例1~9及び比較例1~8の製造方法で研磨液組成物を製造した。該研磨液組成物を使用して基板の研磨を行い、研磨後の基板表面を評価した。被処理シリカ分散液及び珪藻土フィルター並びにろ過方法及び各種パラメータの測定方法は以下のとおり。
被処理シリカ分散液として、コロイダルシリカスラリーA(日揮触媒化成社製、一次粒子の平均粒径24nm、シリカ粒子濃度40重量%品、pH=10.0)、コロイダルシリカスラリーB(日揮触媒化成社製、一次粒子の平均粒径50nm、シリカ粒子濃度40重量%品、pH=9.7)、及びコロイダルシリカスラリーC(日揮触媒化成社製、一次粒子の平均粒径24nm、シリカ粒子濃度40重量%品、pH=10.0)を用いた。
まず、前記コロイダルシリカスラリーA~Cを固形分で1.5g分を200mLビーカーに採取し、イオン交換水100mLを加えてスターラーで混合する。次に、電位差滴定装置を用いて、0.1mol/Lの塩酸標準溶液で試料溶液のpHを3.0に調整する。塩化ナトリウム30.0gを加えスターラーで溶解して、ビーカーの150mLの標線までイオン交換水を加えスターラーで混合する。恒温水槽(20±2℃)に約30分間浸漬する。電位差滴定装置を用いて、0.1mol/Lの水酸化ナトリウム標準溶液で滴定をおこない、pHが4.0から9.0に変化したときの水酸化ナトリウム標準溶液の消費量(A)を読み取る。同時に空試験をおこない、空試験の滴定に要した水酸化ナトリウム標準溶液の消費量(B)を読み取る。そして、下記計算式により平均粒子径(nm)を算出する。
平均粒子径(nm)= 3100÷26.5×(A-B)÷試料採取量(g)
測定試料は、ろ過助剤を含むフィルターでろ過処理する前(又は後)のコロイダルシリカスラリーを、硫酸(和光純薬工業社製 特級)、HEDP(1-ヒドロキシエチリデン-1,1-ジホスホン酸、サーモスジャパン製)、過酸化水素水(旭電化製 濃度:35重量%)をイオン交換水で希釈した水溶液に添加し、これらを混合した後に1.20μmフィルター(ザルトリウス社製 Minisart 17593)でろ過して調製した。コロイダルシリカ、硫酸、HEDP、過酸化水素の含有量は、それぞれ、5重量%、0.4重量%、0.1重量%、0.4重量%とした。得られた測定試料20mLを専用の21φ円筒セルに入れて、大塚電子社製動的光散乱装置DLS-6500にセットした。同装置に添付された説明書に従い、200回積算した際の検出角90度におけるCumulant法によって得られる散乱強度分布の面積が全体の50%となる粒径を求めた。また、検出角90度におけるコロイダルシリカのCV値(CV90)を、上記測定法に従って測定した散乱強度分布における標準偏差を前記粒径で除して100をかけた値として算出した。前記CV90の測定法と同様に、検出角30度におけるコロイダルシリカのCV値(CV30)を測定し、CV30からCV90を引いた値を求め、シリカ粒子のΔCV値とした。
(DLS-6500の測定条件)
検出角:90°
Sampling time : 4(μm)
Correlation Channel : 256(ch)
Correlation Method : TI
Sampling temperature: 26.0(℃)
検出角:30°
Sampling time : 10(μm)
Correlation Channel : 1024(ch)
Correlation Method : TI
Sampling temperature: 26.0(℃)
測定試料を、ろ過助剤を含むフィルターでろ過処理する前(又は後)のコロイダルシリカスラリーを6mLのシリンジで下記測定機器に注入し、粗大粒子量を測定した。
・測定機器:PSS社製「アキュサイザー780APS」
・インジェクション・ループ・ボリューム(Injection Loop Volume):1mL
・フローレート(Flow Rate):60mL/分
・データ・コレクション・タイム(Data Collection Time):60 sec
・チャンネル数(Number Channels):128
測定試料を、ろ過助剤を含むフィルターでろ過処理する前(又は後)のコロイダルシリカスラリーを所定のフィルター(アドバンテック社製 親水性PTFE0.45μmフィルター、型式:25HP045AN)で、エアー圧力0.25MPaの一定圧力の下でフィルターに通液させ、フィルターが閉塞するまでの通液量を求めた。
各ろ過助剤を4桁天秤で約0.1~0.3g精秤し、水銀をヘキサンでよく洗浄した5cc粉末用測定セルにステム内やスリ部にサンプルを付着させないように入れ、AutoPoreIV-9500(島津製作所社製 水銀圧入法 細孔分布測定装置)にセルをセットした。次に、パソコンでアプリケーション(AutoPoreIV-9500 ver1.07)を立上げ、Sample Information(先に測定したろ過助剤の重量)、Analysis Condition(Standardを選択)、Penetrometer Property(セル重量)、Report condition(Standardを選択)に必要事項をInputし、測定を行った。低圧部、高圧部の順に測定を行い、自動的にMedian Pore Diameter (Volume)(μm)と各Pore Size Diameter(μm)に対するLog Differential Pore Volume(mL/g)の結果を得た。
測定セル:Micromeritics社製 5cc-Powder(08-0444)
測定方式:圧力制御方式(圧力テーブルモード)
Low Pressure equilibrium time 5secs
High pressure equilibrium time 5secs
Hgに関するパラメータ:接触角:130°、表面張力:485dynes/cm
Stem Volume Used:100%以下で約50%にサンプル量を調整
Median Pore Diameter (Volume)をろ過助剤の平均細孔径(μm)とした。
0.55μm以下のLog Differential Pore Volume(mL/g)の値を積算して0.5μm以下の積算細孔容積とした。
精秤した約1gの各ろ過助剤をASAP2020(株式会社島津製作所社製、比表面積・細孔分布測定装置)にセットし、多点法でBET比表面積を測定し、BET定数Cが正になる範囲で値を導出した。なお、試料の前処理は、10℃/分で昇温させ100℃で2時間保持させて行った。また、60℃の時点で500μmHgまで脱気を行なった。脱気を行なった。
各ろ過助剤をレーザー回折/散乱式粒度分布計(商品名LA-920、堀場製作所製)で測定して得られた体積基準のメジアン径として得られた値をレーザー平均粒径とした。
ろ過助剤の0.15μm以下の積算細孔容積は、窒素吸着法により測定した。具体的には、精秤した約1gの各ろ過助剤をASAP2020(株式会社島津製作所社製、比表面積・細孔分布測定装置)にセットし、窒素吸着等温線からBJH法のHalsey式により求めた0.15μm以下の細孔容積の総和を、0.15μm以下の積算細孔容積とした。なお、試料の前処理は、10℃/分で昇温させ100℃で2時間保持させて行った。また、60℃の時点で500μmHgまで脱気を行なった。
アドバンテック社製 親水性PTFE0.20μmフィルター(25HP020AN)でろ過した超純水を0.015MPaの条件下で、ろ過助剤を用いてろ過測定を行なった。このときの超純水のろ過時間から、ろ過助剤の透過率を下記数式(1)より算出した。
k=1/A * dV/dθ* uL/P ・・・(1)
A:透過層断面積〔m2〕
V:透過量〔m2〕
θ:透過時間〔s〕
k:透過率〔m2〕
P:透過層の圧力損失〔Pa〕
u:透過流体の粘度〔Pa・s〕
L:透過層厚さ〔m〕
なお、ろ過を行なう際、ろ過助剤はアドバンテック社製No.5A濾紙により上下で挟み90mmφの平板型SUS製ハウジング(住友3M社製INLET90-TL、有効ろ過面積55.4cm2)にセットし、ろ過を行なった。
今回の実験系では、以下の値を導入して透過率kを算出した(θ・Lはサンプルごとで異なる値を示す)。
A:0.0055〔m2〕
V:0.0005〔m2〕
θ:変数
P:15000〔Pa〕
u:0.001〔Pa・s〕
L:変数
(ろ過助剤)
ろ過助剤には、以下a~kを用いた。
a:CelpureP65(レーザー平均粒径12.7μm、珪藻土、SIGMA-ALDRICH社製)
b:ラジオライト No.100(レーザー平均粒径15.7μm、珪藻土、昭和化学工業社製)
c:ラジオライト DX-P5(レーザー平均粒径14.5μm、珪藻土、昭和化学工業社製)
d:ラジオライト No.200(レーザー平均粒径13.9μm、珪藻土、昭和化学工業社製)
e:ラジオライト No.500(レーザー平均粒径28.4μm、珪藻土、昭和化学工業社製)
f:ラジオライト No.600(レーザー平均粒径21.9μm、珪藻土、昭和化学工業社製)
g:ラジオライト New Ace(レーザー平均粒径31.6μm、珪藻土、昭和化学工業社製)
h:Celite500 fine(レーザー平均粒径15.0μm、珪藻土、SIGMA-ALDRICH社製)
i:Celpure300(レーザー平均粒径12.6μm、珪藻土、SIGMA-ALDRICH社製)
j:NA-500(レーザー平均粒径13.5μm、珪藻土、ADVANTEC社製)
k:ラジオライト Dx-W50(レーザー平均粒径25.2μm、珪藻土、昭和化学工業社製)
上記a~kの各ろ過助剤50gに17.5%塩酸水溶液200mLに加え、撹拌・混合する。撹拌を止めて48時間ほど静置した後、上澄みを除去する。イオン交換水を加えてスターラーで5分間撹拌し、上澄みが透明になるまで静置した後、上澄み液を除去し、ろ過助剤を洗浄した。この操作を上澄みが中性(pH=5~8)になるまで繰り返した。最後にろ紙上にろ過して自然乾燥させ、酸処理したろ過助剤を得た。
前記酸処理したろ過助剤10gに100mLのイオン交換水を加え、撹拌・混合しろ過助剤分散水溶液を得た。次に、90mmφの平板型SUS製ハウジング(住友3M社製INLET90-TL、有効ろ過面積55.4cm2)にろ紙(No.5A:アドバンテック社製、目開きと相関する保留粒子径は7μm、セルロース製)をセットし、0.1MPa以下の圧力でろ過助剤分散水溶液をろ過して濾紙上にろ過助剤の均一なケーク層を形成させた後、1~2Lのイオン交換水で洗浄し、珪藻土含有フィルターを得た。
前記珪藻土含有フィルターを乾燥させずに洗浄水で濡れたままの状態で、0.1MPaの圧力で前記コロイダルシリカスラリーA~Cを1L分ろ過し、研磨液組成物に使用するためのろ過済みコロイダルシリカを得た。
上記ろ過により得られたろ過済みコロイダルシリカを所定のフィルター(アドバンテック社製 親水性PTFE0.45μmフィルター、型式:25HP045AN、)で、エアー圧力0.25MPaの一定圧力の下でフィルターに通液させ、フィルターが閉塞するまでの通液量を求めた。
イオン交換水に、ベンゾトリアゾールNa塩を0.1重量%、N-アミノエチルエタノールアミンを0.03重量%、アクリル酸/アクリルアミド-2-メチルプロパンスルホン酸共重合体ナトリウム塩(モル比90/10、重量平均分子量2000、東亞合成社製)を0.02重量%、硫酸を0.4重量%、1-ヒドロキシエチリデン-1,1-ジホスホン酸を0.05重量%、過酸化水素を0.4重量%添加、混合した水溶液の撹拌下に、前記珪藻土含有フィルターでろ過したろ過済みコロイダルシリカを5重量%になるように添加して、研磨液組成物を調製した(実施例1~4及び比較例1~4)。なおいずれの研磨液組成物もpHは1.4~1.5であった。
イオン交換水に、アクリル酸/アクリルアミド-2-メチルプロパンスルホン酸共重合体ナトリウム塩(モル比90/10、重量平均分子量2000、東亞合成社製)を0.02重量%、硫酸を0.4重量%、1-ヒドロキシエチリデン-1,1-ジホスホン酸を0.05重量%、過酸化水素を0.4重量%添加、混合した水溶液の撹拌下に、前記珪藻土含有フィルターでろ過したろ過済みコロイダルシリカを5重量%になるように添加して、研磨液組成物を調製した(実施例5~9及び比較例5~8)。なおいずれの研磨液組成物もpHは1.3~1.5であった。
アニオン性水溶性高分子(アクリル酸/アクリルアミド-2-メチルプロパンスルホン酸共重合体ナトリウム塩)の重量平均分子量は、下記測定条件におけるゲルパーミエーションクロマトグラフィー(GPC)法により測定した。
(GPC条件)
カラム:TSKgel G4000PWXL+TSKgel G2500PWXL(東ソー製)
ガードカラム:TSKguardcolumn PWXL(東ソー製)
溶離液:0.2Mリン酸バッファー/CH3CN=9/1(体積比)
温度:40℃
流速:1.0mL/分
試料サイズ:5mg/mL
検出器:RI
換算標準:ポリアクリル酸Na(分子量(Mp):11.5万、2.8万、4100、1250(創和科学及びAmerican Polymer Standards Corp.製))
・研磨試験機:スピードファム社製、両面9B研磨機
・研磨パッド:フジボウ社製、ウレタン製仕上げ研磨用パッド
・上定盤回転数:32.5r/分
・研磨液組成物供給量:100mL/分
・本研磨時間:4分
・本研磨荷重:7.8kPa
・ 投入した基板の枚数:10枚
研磨した基板をヒカリ社製Sub基板洗浄機で、以下の工程で洗浄した。
(1)US(超音波)浸漬洗浄 (950kHz)
(2)スクラブ洗浄 スポンジブラシ3段
(3)USシャワー洗浄 (950kHz)
(4)スピンリンス
(5)スピンドライ
・測定機器:KLA-Tencor社製 Candela OSA6100
・評価:研磨試験機に投入した基板の中、無作為に4枚を選択し、各々の基板を10000rpmにてレーザーを照射してスクラッチを測定した。その4枚の基板の各々両面にあるスクラッチ数(本)の合計を8で除して、基板面当たりのスクラッチ数を算出した。
・測定機器:KLA-Tencor社製 Candela OSA6100
・評価:研磨試験機に投入した基板の中、無作為に4枚を選択し、その4枚の基板の各々両面にあるパーティクル数(個)の合計を8で除して、基板面当たりのパーティクル数を算出した。
デプス型フィルターと珪藻土含有フィルターとプリーツ型フィルターとを組み合わせたろ過システムで被処理シリカ分散液をろ過して研磨液組成物を製造した(実施例10)。また、デプス型フィルターの循環ろ過とプリーツ型フィルターとを組み合わせたろ過システムで2種類の被処理シリカ分散液をろ過して研磨液組成物を製造した(比較例9及び10)。各研磨液組成物を使用して基板の研磨を行い、研磨後の基板表面を評価した。特に記載のない場合は、下記表2に記載の各種パラメータの測定方法は、実施例1と同様とした。
被処理シリカ分散液として、汎用コロイダルシリカスラリーD(日揮触媒化成社製、一次粒子の平均粒径24nm、粗大粒子量47.9×104個/mL、シリカ粒子濃度40重量%品、pH=9.9)、及び、コロイダルシリカスラリーDを遠心処理して粗大粒子量を低減したコロイダルシリカスラリーE(一次粒子の平均粒径24nm、粗大粒子量6.9×104個/mL、シリカ粒子濃度40重量%品、pH=9.9)を使用した。
実施例10の研磨液組成物に使用するろ過済みコロイダルシリカを得るためのろ過システムとして、1段目にデプス型フィルターを1本、2段目に珪藻土含有フィルター(ケークフィルター)を1本、3段目にプリーツ型フィルターを1本備え、これらのフィルターがこの順で3段直列に配置されたろ過システムを採用した。このろ過システムの概略図として図1を参照できる。被処理シリカ分散液であるコロイダルシリカスラリーDを前記ろ過システムで1パスろ過することにより、ろ過済みコロイダルシリカを得た。得られたろ過済みコロイダルシリカを用い、実施例1と同様にして、研磨液組成物を作製した。50LのコロイダルシリカスラリーDを小型ダイアフラムポンプで前記ろ過システムに通液させて処理するのに要した時間は、0.9時間(平均通液量は0.95L/分、平均ろ過速度は17.9L/(分・m2))であった(下記表2)。なお、使用したフィルターは下記のとおりである。
デプス型フィルター:長さ250mmの日本ポール社製「プロファイルII-003」(孔径0.3um)、ポリプロピレン製
ケークフィルター:アドバンテック東洋社製多用途ディスクフォルダーKS-293-UH(有効ろ過面積:530cm2)にろ紙(No.5A:アドバンテック東洋社製、セルロース製)をセットし、前記珪藻土ろ過助剤a(酸処理なし)(100g)の水分散液をプレコートし均一なケーク層を形成させた後、10Lのイオン交換水でろ過助剤の洗浄を行って作製したフィルター。
プリーツ型フィルター:長さ250mmのアドバンテック東洋社製「TCS-045」(孔径0.45um)、ポリエーテルスルホン製
比較例9の研磨液組成物に使用するろ過済みコロイダルシリカを得るための1段目のろ過システムとして、デプス型フィルターを2本配置した循環ろ過システムを採用した。そして、2段目のろ過システムとしてプリーツ型フィルターを1本配置したろ過システムを採用した。このろ過システムの概略図として図2を参照できる。被処理シリカ分散液であるコロイダルシリカスラリーDを前記1段目のろ過システムで循環通液ろ過を行い、見掛け上8パス相当のろ過を行った。その後、前記2段目のろ過システムで1パスろ過することにより、ろ過済みコロイダルシリカを得た。得られたろ過済みコロイダルシリカを用い、実施例1と同様にして、研磨液組成物を作製した。50LのコロイダルシリカスラリーDを小型ダイアフラムポンプで前記1段目のろ過システムに循環通液させ見掛け上8パス相当のろ過をするのに要した時間は、3.3時間(平均通液量は2.0L/分)であった。また、前記2段目のろ過システムを1パスでろ過するのに要した時間は0.4時間であった。したがって、1段目及び2段目のろ過で要した時間はトータル3.7時間であった(下記表2)。なお、使用したデプス型及びプリーツ型フィルターは実施例10と同じである。
被処理シリカ分散液であるコロイダルシリカスラリーDに換えてコロイダルシリカスラリーEを使用したほかは、比較例9と同様にして研磨液組成物を作製した。50LのコロイダルシリカスラリーEを小型ダイアフラムポンプで前記1段目のろ過システムに循環通液させ見掛け上8パス相当のろ過をするのに要した時間は、3.3時間(平均通液量は2.0L/分)であった。また、前記2段目のろ過システムを1パスでろ過するのに要した時間は0.4時間であった。したがって、1段目及び2段目のろ過で要した時間はトータル3.7時間であった(下記表2)。
実施例10のデプス型フィルターとしてろ過処理量の履歴が異なるデプス型フィルターを用いたこと以外は実施例10と同様な製造方法で、研磨液組成物を製造した(実施例11~13)。また、デプス型フィルターを使用しないこと以外は実施例10と同様な製造方法で、研磨液組成物を製造した(比較例11)。各研磨液組成物を使用して基板の研磨を行い、研磨後の基板表面を評価した。特に記載のない場合は、下記表3に記載の各種パラメータの測定方法は、実施例1と同様とした。
被処理シリカ分散液として、汎用コロイダルシリカスラリーF(日揮触媒化成社製、一次粒子の平均粒径24nm、粗大粒子量55.3万個/mL、シリカ粒子濃度40重量%品、pH=9.9)を使用した。
実施例11~13の研磨液組成物に使用するろ過済みコロイダルシリカを得るためのろ過システムとして、1段目にデプス型フィルターを1本、2段目に珪藻土含有フィルター(ケークフィルター)を1本、3段目にプリーツ型フィルターを1本備え、これらのフィルターがこの順で3段直列に配置されたろ過システムを採用した。このろ過システムの概略図として図1を参照できる。被処理シリカ分散液であるコロイダルシリカスラリーFを前記ろ過システムで1パスろ過することにより、ろ過済みコロイダルシリカを得た。得られたろ過済みコロイダルシリカを用い、実施例1と同様にして、研磨液組成物を作製した。使用したデプス型フィルター、珪藻土含有フィルター、及びプリーツ型フィルターは、実施例10と同様である。但し、デプス型フィルターは、実施例11、12、13の順で、ろ過処理量の履歴が多いものを使用した。デプス型フィルターは使用履歴(ろ過処理量履歴)が多くなるにつれ、粗大粒子の除去能力が低下していく。すなわち、1段目のデプス型フィルターろ過後のシリカ分散液中に含まれる粗大粒子は、実施例11、12、13の順で増加する(下記表3)。これらのデプス型フィルターを使用した場合に、2段目の珪藻土フィルターが閉塞するまでに処理できる量を測定し、その結果を下記表3に示す。
比較例11の研磨液組成物に使用するろ過済みコロイダルシリカを得るためのろ過システムとして、1段目に珪藻土含有フィルター(ケークフィルター)を1本、2段目にプリーツ型フィルターを1本備え、これらのフィルターがこの順で2段直列に配置されたろ過システムを採用した。すなわち、被処理シリカ分散液であるコロイダルシリカスラリーFを、デプス型フィルターでろ過することなく、1段目のケークフィルターに導入して1パスろ過することにより、ろ過済みコロイダルシリカを得た。得られたろ過済みコロイダルシリカを用い、実施例1と同様にして、研磨液組成物を作製した。使用した珪藻土含有フィルター、及びプリーツ型フィルターは、実施例10と同様である。1段目のケークフィルターが閉塞するまでに処理できる量を測定し、その結果を下記表3に示す。
<1>一次粒子の平均粒子径が1~100nmのコロイダルシリカを含有する被処理シリカ分散液を、ろ過助剤を含むフィルターでろ過処理する工程を有する研磨液組成物の製造方法であって、前記ろ過助剤は水銀圧入法による平均細孔径が0.1~3.5μmである、研磨液組成物の製造方法;
<2>ろ過助剤が珪藻土である、前記<1>記載の研磨液組成物の製造方法;
<3>ろ過助剤の水銀圧入法による0.5μm以下の積算細孔容積が2.5mL/g以上である、前記<1>又は<2>に記載の研磨液組成物の製造方法;
<4>前記ろ過助剤は、BET比表面積が4.0m2/g以上であり、且つ窒素吸着法による0.15μm以下の積算細孔容積が0.3mL/g以上である、前記<1>から<3>のいずれかに記載の研磨液組成物の製造方法;
<5>前記ろ過助剤に対して0.015MPaの条件で水をろ過させたときの前記ろ過助剤の水の透過率が、5.0×10-14m2以下である、前記<1>から<4>の研磨液組成物の製造方法;
<6>下記工程1及び2を有する、前記<1>から<5>のいずれかに記載の研磨液組成物の製造方法;
工程1)一次粒子の平均粒子径が1~100nmのコロイダルシリカを含有する被処理シリカ分散液を、粒子径が0.5μm以上の粗大粒子量が11.0×104個/mL以下になるようにろ過処理する工程。
工程2)工程1で得られたシリカ分散液を、水銀圧入法による平均細孔径が0.1~3.5μmであるろ過助剤を含むフィルターでろ過処理する工程。
<7>前記工程1において、前記被処理シリカ分散液を、前記粗大粒子量が好ましくは10.0×104個/mL以下、より好ましくは7.0×104個/mL以下、さらに好ましくは6.0×104個/mL以下、さらにより好ましくは5.0×104個/mL以下、さらにより好ましくは4.0×104個/mL以下、さらにより好ましくは3.0×104個/mL以下になるようにろ過処理する、前記<6>記載の研磨液組成物の製造方法;
<8>前記工程1におけるろ過処理が、デプス型フィルターを用いたろ過処理である、前記<6>又は<7>に記載の研磨液組成物の製造方法;
<9>前記デプス型フィルターの孔径が、5.0μm以下である、前記<8>記載の研磨液組成物の製造方法;
<10>前記工程1におけるろ過処理が、前記デプス型フィルターを用いた多段のろ過処理である、前記<8>又は<9>に記載の研磨液組成物の製造方法;
<11>さらに下記工程3を有する、前記<6>から<10>のいずれかに記載の研磨液組成物の製造方法;
工程3)前記工程2で得られたシリカ分散液を、プリーツ型フィルターでろ過処理する工程。
<12>前記プリーツ型フィルターの孔径が、1.0μm以下である、前記<11>記載の研磨液組成物の製造方法;
<13>前記工程1及び前記工程2におけるろ過処理を1パスで行う、前記<6>から<12>のいずれかに記載の研磨液組成物の製造方法;
<14>前記被処理シリカ分散液における粒子径が0.5μm以上の粗大粒子量が、20.0×104個/mL以上である、前記<1>から<13>のいずれかに記載の研磨液組成物の製造方法;
<15>前記被処理シリカ分散液における粒子径が0.5μm以上の粗大粒子量が、200.0×104個/mL以下である、前記<1>から<14>のいずれかに記載の研磨液組成物の製造方法;
<16>前記被処理シリカ分散液におけるコロイダルシリカの含有量が、1~50重量%である、前記<1>から<15>のいずれかに記載の研磨液組成物の製造方法;
<17>得られる研磨液組成物における粒子径が0.5μm以上の粗大粒子の含有量が、0.5~10×104個/mLである、前記<1>から<16>のいずれかに記載の研磨液組成物の製造方法;
<18>前記ろ過助剤を含むフィルターにおける前記ろ過助剤の含有量が、0.001~1g/cm2である、前記<1>から<17>のいずれかに記載の研磨液組成物の製造方法;
<19>前記ろ過助剤を含むフィルターによるろ過処理におけるろ過時の差圧が、0.01~10MPaである、前記<1>から<18>のいずれかに記載の研磨液組成物の製造方法;
<20>前記ろ過助剤を含むフィルターによるろ過処理におけるろ過速度が、0.1~30L/(分・m2)である、前記<1>から<19>のいずれかに記載の研磨液組成物の製造方法;
<21>ろ過助剤の水銀圧入法による平均細孔径が、好ましくは0.1~3.0μm、より好ましくは0.1~2.7μm、さらに好ましくは1.0~2.7μm、さらにより好ましくは2.0~2.7μm、さらにより好ましくは2.1~2.7μm、さらにより好ましくは2.2~2.6μm、さらにより好ましくは2.2~2.4μmである、前記<1>から<20>のいずれかに記載の研磨液組成物の製造方法;
<22>ろ過助剤の水銀圧入法による0.5μm以下の積算細孔容積が、好ましくは2.5~1000mL/g、より好ましくは2.7~100mL/g、さらに好ましくは3.0~50mL/g、さらにより好ましくは4.0~20mL/g、さらにより好ましくは4.5~10mL/g、さらにより好ましくは4.5~6mL/gである。2.5mL/g以上である、前記<1>から<21>のいずれかに記載の研磨液組成物の製造方法;
<23>ろ過助剤のBET比表面積が、好ましくは4.0~1000.0m2/g、より好ましくは10.0~100.0m2/g、さらに好ましくは15.0~50.0m2/g、さらに好ましくは15.0~30.0m2/g、さらにより好ましくは18.0~30.0m2/g、さらに好ましくは18.0~25.0m2/gである、前記<1>から<22>のいずれかに記載の研磨液組成物の製造方法;
<24>窒素吸着法による0.15μm以下の積算細孔容積が、好ましくは0.3~100.0mL/g、より好ましくは0.4~50.0mL/g、さらに好ましくは0.6~10.0mL/g、さらにより好ましくは0.6~5.0mL/g、さらにより好ましくは0.6~2.0mL/g、さらにより好ましくは0.6~1.0mL/g、さらにより好ましくは0.6~0.7mL/gである、前記<1>から<23>のいずれかに記載の研磨液組成物の製造方法;
<25>前記ろ過助剤に対して0.015MPaの条件で水をろ過させたときの前記ろ過助剤の水の透過率が、好ましくは2.0×10-15~9.9×10-14m2、より好ましくは5.0×10-15~5.0×10-14m2であり、さらに好ましくは9.9×10-15~3.0×10-14m2である、前記<1>から<24>のいずれかに記載の研磨液組成物の製造方法;
<26>工程1が、一次粒子の平均粒子径が1~100nmのコロイダルシリカを含有する被処理シリカ分散液を、粒子径が0.5μm以上の粗大粒子量が、好ましくは10.0×104個/mL以下、より好ましくは7.0×104個/mL以下、さらに好ましくは6.0×104個/mL以下、さらにより好ましくは5.0×104個/mL以下、さらにより好ましくは4.0×104個/mL以下、さらにより好ましくは3.0×104個/mL以下になるようにろ過処理する工程である、前記<1>から<25>のいずれかに記載の研磨液組成物の製造方法;
<27>前記被処理シリカ分散液における粒子径が0.5μm以上の粗大粒子量が、好ましくは20.0×104~200.0×104個/mL、より好ましくは20.0×104~100.0×104個/mL、さらに好ましくは30.0×104~100.0×104個/mL、さらにより好ましくは34.0×104~100.0×104個/mL、さらにより好ましくは34.0×104~70.0×104個/mLである、前記<1>から<26>のいずれかに記載の研磨液組成物の製造方法;
<28>得られる研磨液組成物における粒子径が0.5μm以上の粗大粒子の含有量が、好ましくは0.5×104~5×104個/mL、より好ましくは0.5×104~4×104個/mL、さらに好ましくは0.5×104~3×104個/mLである、前記<1>から<27>のいずれかに記載の研磨液組成物の製造方法;
<29>前記<1>から<28>のいずれかに記載の製造方法により製造される研磨液組成物;
<30>さらに、酸と、酸化剤と、アニオン性基を有する水溶性高分子と、複素環芳香族化合物と、脂肪族アミン化合物又は脂環式アミン化合物とを含有する、前記<29>記載の研磨液組成物;
<31>前記<1>から<28>のいずれかに記載の製造方法により研磨液組成物を製造すること、及び、前記研磨液組成物を被研磨基板の研磨対象面に供給し、前記研磨対象面に研磨パッドを接触させ、前記研磨パッド及び/又は前記被研磨基板を動かして、前記研磨対象面を研磨することを含む、磁気ディスク基板の製造方法。
Claims (23)
- 一次粒子の平均粒子径が1~100nmのコロイダルシリカを含有する被処理シリカ分散液を、ろ過助剤を含むフィルターでろ過処理する工程を有する研磨液組成物の製造方法であって、前記ろ過助剤は水銀圧入法による平均細孔径が0.1~3.5μmである、研磨液組成物の製造方法。
- ろ過助剤が珪藻土である、請求項1記載の研磨液組成物の製造方法。
- ろ過助剤の水銀圧入法による0.5μm以下の積算細孔容積が2.5mL/g以上である、請求項1又は2記載の研磨液組成物の製造方法。
- 前記ろ過助剤は、BET比表面積が4.0m2/g以上であり、且つ窒素吸着法による0.15μm以下の積算細孔容積が0.3mL/g以上である、請求項1から3のいずれかに記載の研磨液組成物の製造方法。
- 前記ろ過助剤に対して0.015MPaの条件で水をろ過させたときの前記ろ過助剤の水の透過率が、5.0×10-14m2以下である、請求項1から4のいずれかに記載の研磨液組成物の製造方法。
- 下記工程1及び2を有する、請求項1から5のいずれかに記載の研磨液組成物の製造方法。
工程1)一次粒子の平均粒子径が1~100nmのコロイダルシリカを含有する被処理シリカ分散液を、粒子径が0.5μm以上の粗大粒子量が11.0×104個/mL以下になるようにろ過処理する工程。
工程2)工程1で得られたシリカ分散液を、水銀圧入法による平均細孔径が0.1~3.5μmであるろ過助剤を含むフィルターでろ過処理する工程。 - 前記工程1において、前記被処理シリカ分散液を、前記粗大粒子量が7.0×104個/mL以下になるようにろ過処理する、請求項6記載の研磨液組成物の製造方法。
- 前記工程1におけるろ過処理が、デプス型フィルターを用いたろ過処理である、請求項6又は7に記載の研磨液組成物の製造方法。
- 前記デプス型フィルターの孔径が、5.0μm以下である、請求項8記載の研磨液組成物の製造方法。
- 前記工程1におけるろ過処理が、前記デプス型フィルターを用いた多段のろ過処理である、請求項8又は9に記載の研磨液組成物の製造方法。
- さらに下記工程3を有する、請求項6から10のいずれかに記載の研磨液組成物の製造方法。
工程3)前記工程2で得られたシリカ分散液を、プリーツ型フィルターでろ過処理する工程。 - 前記プリーツ型フィルターの孔径が、1.0μm以下である、請求項11記載の研磨液組成物の製造方法。
- 前記工程1及び前記工程2におけるろ過処理を1パスで行う、請求項6から12のいずれかに記載の研磨液組成物の製造方法。
- 前記被処理シリカ分散液における粒子径が0.5μm以上の粗大粒子量が、20.0×104個/mL以上である、請求項1から13のいずれかに記載の研磨液組成物の製造方法。
- 前記被処理シリカ分散液における粒子径が0.5μm以上の粗大粒子量が、200.0×104個/mL以下である、請求項1から14のいずれかに記載の研磨液組成物の製造方法。
- 前記被処理シリカ分散液におけるコロイダルシリカの含有量が、1~50重量%である、請求項1から15のいずれかに記載の研磨液組成物の製造方法。
- 得られる研磨液組成物における粒子径が0.5μm以上の粗大粒子の含有量が、0.5×104~10×104個/mLである、請求項1から16のいずれかに記載の研磨液組成物の製造方法。
- 前記ろ過助剤を含むフィルターにおける前記ろ過助剤の含有量が、0.001~1g/cm2である、請求項1から17のいずれかに記載の研磨液組成物の製造方法。
- 前記ろ過助剤を含むフィルターによるろ過処理におけるろ過時の差圧が、0.01~10MPaである、請求項1から18のいずれかに記載の研磨液組成物の製造方法。
- 前記ろ過助剤を含むフィルターによるろ過処理におけるろ過速度が、0.1~30L/(分・m2)である、請求項1から19のいずれかに記載の研磨液組成物の製造方法。
- 請求項1から20いずれか記載の製造方法により製造される研磨液組成物。
- さらに、酸と、酸化剤と、アニオン性基を有する水溶性高分子と、複素環芳香族化合物と、脂肪族アミン化合物又は脂環式アミン化合物と、を含有する請求項21に記載の研磨液組成物。
- 請求項1から20いずれか記載の製造方法により研磨液組成物を製造すること、及び、
前記研磨液組成物を被研磨基板の研磨対象面に供給し、前記研磨対象面に研磨パッドを接触させ、前記研磨パッド及び/又は前記被研磨基板を動かして、前記研磨対象面を研磨することを含む、磁気ディスク基板の製造方法。
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US13/824,235 US20130183889A1 (en) | 2010-09-24 | 2011-09-21 | Process for producing polishing liquid composition |
CN201180045169.3A CN103119122B (zh) | 2010-09-24 | 2011-09-21 | 研磨液组合物的制造方法 |
Applications Claiming Priority (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2010-214083 | 2010-09-24 | ||
JP2010214083 | 2010-09-24 | ||
JP2011-002537 | 2011-01-07 | ||
JP2011002537A JP5698989B2 (ja) | 2011-01-07 | 2011-01-07 | 研磨液組成物の製造方法 |
JP2011-202262 | 2011-09-15 | ||
JP2011202262A JP5833390B2 (ja) | 2010-09-24 | 2011-09-15 | 研磨液組成物の製造方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2012039428A1 true WO2012039428A1 (ja) | 2012-03-29 |
Family
ID=45873912
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2011/071501 WO2012039428A1 (ja) | 2010-09-24 | 2011-09-21 | 研磨液組成物の製造方法 |
Country Status (1)
Country | Link |
---|---|
WO (1) | WO2012039428A1 (ja) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20140248823A1 (en) * | 2013-03-04 | 2014-09-04 | Cabot Microelectronics Corporation | Composition and method for polishing glass |
US9080080B2 (en) | 2010-12-24 | 2015-07-14 | Kao Corporation | Method for producing polishing liquid composition |
JP2017117847A (ja) * | 2015-12-21 | 2017-06-29 | 花王株式会社 | シリカ分散液の製造方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11165006A (ja) * | 1997-10-03 | 1999-06-22 | Kyushu Electric Power Co Inc | 発電所ヒータードレン水の処理方法 |
JP2003190780A (ja) * | 2001-12-25 | 2003-07-08 | Asahi Kasei Corp | 濾過助剤 |
JP2003190781A (ja) * | 2001-12-27 | 2003-07-08 | Mitsubishi Chemicals Corp | 濾過助剤用シリカゲル |
JP2006136996A (ja) * | 2004-10-12 | 2006-06-01 | Kao Corp | 研磨液組成物の製造方法 |
JP2007099586A (ja) * | 2005-10-07 | 2007-04-19 | Oji Paper Co Ltd | シリカ微粒子分散液の製造方法、シリカ微粒子分散液、及びインクジェット記録シート |
-
2011
- 2011-09-21 WO PCT/JP2011/071501 patent/WO2012039428A1/ja active Application Filing
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH11165006A (ja) * | 1997-10-03 | 1999-06-22 | Kyushu Electric Power Co Inc | 発電所ヒータードレン水の処理方法 |
JP2003190780A (ja) * | 2001-12-25 | 2003-07-08 | Asahi Kasei Corp | 濾過助剤 |
JP2003190781A (ja) * | 2001-12-27 | 2003-07-08 | Mitsubishi Chemicals Corp | 濾過助剤用シリカゲル |
JP2006136996A (ja) * | 2004-10-12 | 2006-06-01 | Kao Corp | 研磨液組成物の製造方法 |
JP2007099586A (ja) * | 2005-10-07 | 2007-04-19 | Oji Paper Co Ltd | シリカ微粒子分散液の製造方法、シリカ微粒子分散液、及びインクジェット記録シート |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9080080B2 (en) | 2010-12-24 | 2015-07-14 | Kao Corporation | Method for producing polishing liquid composition |
US20140248823A1 (en) * | 2013-03-04 | 2014-09-04 | Cabot Microelectronics Corporation | Composition and method for polishing glass |
US9358659B2 (en) * | 2013-03-04 | 2016-06-07 | Cabot Microelectronics Corporation | Composition and method for polishing glass |
JP2017117847A (ja) * | 2015-12-21 | 2017-06-29 | 花王株式会社 | シリカ分散液の製造方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5833390B2 (ja) | 研磨液組成物の製造方法 | |
US20130183889A1 (en) | Process for producing polishing liquid composition | |
JP5698989B2 (ja) | 研磨液組成物の製造方法 | |
JP5844135B2 (ja) | 研磨液組成物の製造方法 | |
JP2006136996A (ja) | 研磨液組成物の製造方法 | |
US20100190413A1 (en) | Polishing composition | |
JP6304841B2 (ja) | 研磨液組成物の製造方法 | |
JP4836441B2 (ja) | 研磨液組成物 | |
JP6033077B2 (ja) | 研磨液組成物の製造方法 | |
WO2012039428A1 (ja) | 研磨液組成物の製造方法 | |
JP2015127987A (ja) | 研磨液組成物の製造方法 | |
JP2007320031A (ja) | 研磨液組成物 | |
JP4214093B2 (ja) | 研磨液組成物 | |
JP5377117B2 (ja) | 粒子分散液中の非球状粒子を検出する方法 | |
JP5473587B2 (ja) | 磁気ディスク基板用研磨液組成物 | |
JP2003211351A (ja) | 微小突起の低減方法 | |
JP4648367B2 (ja) | 研磨液組成物 | |
JP6680652B2 (ja) | 砥粒分散液、およびこれを含む研磨用組成物キット、ならびにこれらを用いた研磨用組成物の製造方法、研磨用組成物、研磨方法および磁気ディスク用基板の製造方法 | |
JP6081317B2 (ja) | 磁気ディスク基板の製造方法 | |
JP6425965B2 (ja) | 研磨液組成物の製造方法 | |
JP4640981B2 (ja) | 基板の製造方法 | |
JP6251567B2 (ja) | 研磨液組成物の製造方法 | |
JP4214107B2 (ja) | 研磨液組成物 | |
JP6418915B2 (ja) | 研磨液組成物の製造方法 | |
JP2017065797A (ja) | 容器入りシリカ分散液の製造方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201180045169.3 Country of ref document: CN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 11826873 Country of ref document: EP Kind code of ref document: A1 |
|
WWE | Wipo information: entry into national phase |
Ref document number: 13824235 Country of ref document: US |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 11826873 Country of ref document: EP Kind code of ref document: A1 |