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WO2013035545A1 - Grains abrasifs, leur procédé de fabrication, bouillie de polissage et procédé de fabrication de produits verriers - Google Patents

Grains abrasifs, leur procédé de fabrication, bouillie de polissage et procédé de fabrication de produits verriers Download PDF

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Publication number
WO2013035545A1
WO2013035545A1 PCT/JP2012/071349 JP2012071349W WO2013035545A1 WO 2013035545 A1 WO2013035545 A1 WO 2013035545A1 JP 2012071349 W JP2012071349 W JP 2012071349W WO 2013035545 A1 WO2013035545 A1 WO 2013035545A1
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Prior art keywords
cerium
acid
phase particles
coated
mass
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Ceased
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PCT/JP2012/071349
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English (en)
Japanese (ja)
Inventor
酒井　智弘
有衣子 吉田
浩之 朝長
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AGC Inc
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Asahi Glass Co Ltd
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Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Publication of WO2013035545A1 publication Critical patent/WO2013035545A1/fr
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    • 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
    • C09K3/1436—Composite particles, e.g. coated particles

Definitions

  • the present invention relates to abrasive grains, a method for producing the same, a polishing slurry, and a method for producing a glass product.
  • polishing process in the manufacture of glass products such as magnetic disks, liquid crystal glass, semiconductor substrates or photomasks for hard disk drives, improvement of the polishing rate by various means has been studied in order to improve productivity.
  • Patent Document 1 discloses that the polishing rate can be improved by adding an additive to a polishing slurry containing ceria crystal microparticles or ceria-zirconia solid solution crystal particles, and good glass substrate surface properties can be obtained. It is shown.
  • Patent Document 2 shows that by containing cerium oxide particles produced using cerium carbonate having a primary particle diameter of 3 to 60 ⁇ m as a raw material, an abrasive capable of high-speed polishing without scratches can be obtained. Has been.
  • Patent Document 3 discloses that a polishing target composition is polished using a composite oxide containing cerium and zirconium in a polishing liquid composition, so that generation of scratches on the polishing target substrate can be suppressed and high speed can be achieved. It has been shown that smooth polishing is possible.
  • cerium oxide is mainly used in the polishing process in the manufacture of glass products such as magnetic disks for hard disk drives, glass for liquid crystals, semiconductor substrates or photomasks because of the high polishing rate.
  • cerium is difficult to supply stably because the area where it can be mined is limited, and in recent years the price has risen.
  • an object of the present invention is to provide abrasive grains and polishing slurry that can polish an object to be polished at a high polishing rate with a small amount of cerium oxide used.
  • the inventors of the present invention can polish an object to be polished at a high polishing rate with a small amount of cerium oxide used by using abrasive grains having mother phase particles coated with cerium oxide for polishing the object to be polished.
  • the present invention has been completed by finding out what can be done.
  • the present invention is as follows. 1. Polishing abrasive grains in which matrix phase particles are coated with cerium oxide. 2.
  • the mother phase particles are sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid, formic acid, glycolic acid, acetic acid, ascorbic acid, hydrogen peroxide, ammonia, sodium hydroxide, potassium hydroxide, carbonic acid.
  • the abrasive grain according to item 1 which is soluble in at least one aqueous solution selected from sodium and potassium carbonate. 3.
  • a polishing slurry comprising the polishing abrasive grain according to any one of 1 to 6 above. 8).
  • a method for producing abrasive grains in which matrix particles are coated with cerium oxide comprising the following steps (1) to (3) in sequence.
  • (1) A step of obtaining a cerium source aqueous solution by dissolving a cerium compound in water (2)
  • step (2) the cerium source aqueous solution is sprayed on the mother phase particles to obtain mother phase particles coated with the cerium source aqueous solution.
  • step (3) the cerium source aqueous solution is sprayed on the mother phase particles to obtain mother phase particles coated with the cerium source aqueous solution.
  • the cerium compound is at least one selected from the group consisting of cerium acetate, cerium nitrate, cerium hydroxide, and cerium sulfate.
  • 11. 8 A method for producing a glass product, comprising a step of polishing glass using the abrasive grains according to any one of items 1 to 6 or the polishing slurry according to item 7.
  • an object to be polished can be polished at a high polishing rate without using a large amount of cerium oxide.
  • FIG. 1 shows the X-ray profile of manganese oxide.
  • the abrasive grains of the present invention are abrasive grains in which matrix phase particles are coated with cerium oxide, and include matrix phase particles and cerium oxide covering the matrix phase particles.
  • mother phase particles examples include manganese oxide (Mn 3 O 4 , Mn 2 O 3 , MnO 2 ), zinc oxide (ZnO), iron oxide (Fe 3 O 4 , Fe 2 O 3 ), copper oxide (Cu 2 ). O, CuO), aluminum oxide (Al 2 O 3 ), silica (SiO 2 ), chromium oxide (Cr 2 O 3 , CrO 2 ) and zirconium oxide (ZrO 2 ). These mother phase particles can be those commercially available.
  • the cerium oxide coated on the mother phase particles has a drawback that it has poor adhesion after polishing because it has high adhesion to the object to be polished and cannot be easily dissolved. Therefore, from the viewpoint of improving the cleanability after polishing, among these, sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid, formic acid, glycolic acid, acetic acid, ascorbic acid, hydrogen peroxide It is preferable to use particles that are soluble in at least one aqueous solution selected from ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate as mother phase particles.
  • mother phase particles that are soluble in at least one selected aqueous solution include manganese oxide (Mn 3 O 4 , Mn 2 O 3 , MnO 2 ), zinc oxide (ZnO), and iron oxide (Fe 3 O 4). , Fe 2 O 3 ) and copper oxide (Cu 2 O, CuO).
  • manganese oxide (Mn 3 O 4 , Mn 2 O 3 , MnO 2 ) can be dissolved by hydrochloric acid, sulfuric acid, nitric acid, ascorbic acid, hydrogen peroxide, or the like.
  • Zinc oxide (ZnO) can be dissolved by hydrochloric acid, nitric acid, sulfuric acid or the like.
  • Iron oxide Fe 3 O 4 , Fe 2 O 3
  • hydrochloric acid nitric acid, sulfuric acid or the like.
  • Copper oxide (Cu 2 O, CuO) can be dissolved by hydrochloric acid, nitric acid, sulfuric acid or the like.
  • matrix particles may be used alone or in combination of two or more.
  • manganese oxide or zinc oxide is more preferable.
  • Manganese oxide or zinc oxide is highly soluble in acids, alkalis, oxidizing agents, or reducing agents, so using manganese oxide or zinc oxide for the matrix phase particles will not affect the workpiece.
  • a high cleaning effect can be obtained with a cleaning liquid containing an acid, an alkali, an oxidizing agent, or a reducing agent.
  • soluble means sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid, formic acid, glycolic acid, acetic acid, ascorbic acid, peroxidation at room temperature for 1 hour.
  • 0.1 to 1% by mass of mother phase particles were dissolved in an aqueous solution containing 0.01 to 2 mol% of one selected from hydrogen, ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate. Sometimes the amount of elution is 90% by mass or more.
  • the solubility of the matrix phase particles can be tested according to the dissolution test described later in the Examples.
  • sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid formic acid, glycolic acid, acetic acid, hydrogen peroxide, ascorbic acid, hydrogen peroxide, ammonia, sodium hydroxide, water
  • sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid are used in a cleaning process after polishing using at least one aqueous solution selected from potassium oxide, sodium carbonate and potassium carbonate.
  • the object to be polished is cleaned with a cleaning liquid containing at least one selected from acids, formic acid, glycolic acid, acetic acid, hydrogen peroxide, ascorbic acid, hydrogen peroxide, ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
  • a cleaning liquid containing at least one selected from acids, formic acid, glycolic acid, acetic acid, hydrogen peroxide, ascorbic acid, hydrogen peroxide, ammonia, sodium hydroxide, potassium hydroxide, sodium carbonate and potassium carbonate.
  • the coating amount of the mother phase particles with cerium oxide is preferably 0.1 to 25% by mass, more preferably 0.1 to 20% by mass, further preferably 1 to 10% by mass, in terms of cerium oxide, and 1 to 5% by mass. % Is particularly preferred.
  • the coating amount is 0.1% by mass or more, an effect of improving the polishing rate can be obtained.
  • the coating amount is 25% by mass or less, the amount of cerium used can be reduced. be able to.
  • the specific surface area of abrasive grains of the matrix phase particles were coated with the cerium oxide is preferably 0.1 ⁇ 20m 2 / g, more preferably 0.5 ⁇ 15m 2 / g, 1 ⁇ 10m 2 / g is more preferred.
  • the specific surface area of the abrasive grains is 0.1 m 2 / g or more, polishing scratches due to coarse grains can be suppressed, and when it is 20 m 2 / g or less, a sufficient polishing rate can be obtained.
  • the specific surface area of the abrasive grains is measured by the method described later in the examples.
  • the abrasive grains of the present invention can be produced by a production method that sequentially includes the following steps (1) to (3).
  • steps (1) to (3) (1) Step of dissolving cerium compound in water to obtain cerium source aqueous solution (2) Covering mother phase particles with cerium source aqueous solution obtained in step (1), and coating mother phase particles coated with cerium source aqueous solution Step of obtaining (3) Step of firing mother phase particles coated with cerium source aqueous solution obtained in step (2) to obtain mother phase particles coated with cerium oxide
  • each step will be described.
  • cerium acetate, cerium nitrate, cerium hydroxide, or cerium sulfate is preferable in terms of availability and solubility in water.
  • cerium compounds may be used individually by 1 type, and may be used in combination of 2 or more type.
  • the concentration of the cerium compound in the cerium source aqueous solution can be adjusted as appropriate in consideration of the amount of cerium oxide to be coated on the mother phase particles and the amount of the cerium source aqueous solution coated on the mother phase particles in step (2) described later. Good. It is preferable to set the concentration of the cerium compound in the cerium source aqueous solution to be equal to or lower than the solubility of the cerium compound because the cerium source aqueous solution can be uniformly coated on the mother phase particles in the step (2) described later.
  • the concentration of the cerium compound in the cerium source aqueous solution should be 5 to 60% by mass. It is preferably 10 to 60% by mass.
  • the concentration of the cerium compound in the cerium source aqueous solution is preferably 1 to 40% by mass. More preferably, the content is 1 to 20% by mass.
  • the concentration of the cerium compound in the cerium source aqueous solution is preferably 1 to 60% by mass. More preferably, the content is 1 to 40% by mass.
  • Step (2) is the cerium obtained in step (1)
  • the mother phase particles are coated with the source aqueous solution, and the cerium compound is precipitated on the surface of the mother phase particles using water as a medium.
  • Examples of the method of coating the mother phase particles with the cerium source aqueous solution include spraying, dipping or coating. Among these, spraying does not require a drying step and is preferable from an industrial viewpoint.
  • Specific methods include, for example, a method in which matrix particles are placed in a plastic bag and a cerium source aqueous solution is sprayed with a spray.
  • the cerium source aqueous solution may be sprayed while being thermally dried with a rotary kiln and stirring the mother phase particles with a rotary machine, which is industrially advantageous.
  • the spray amount of the aqueous cerium source solution on the mother phase particles is preferably 0.1 to 40% by mass, more preferably 5 to 30% by mass, and 10 to 25% by mass with respect to the mother phase particles. More preferably.
  • the aqueous solution reaches the entire matrix phase particles, and uniform coating is possible.
  • the amount of 40% by mass or less is preferable because it does not become paste or liquid and can be taken as it is to the firing step, so that the drying step can be omitted.
  • the spraying conditions are usually preferably 0 to 200 ° C.
  • the mother phase particles are immersed in the cerium source aqueous solution to coat the mother phase particles with the cerium source aqueous solution.
  • the amount of the mother phase particles immersed in the cerium source aqueous solution is usually preferably 1 to 60% by mass and more preferably 10 to 50% by mass with respect to the aqueous solution.
  • the amount of matrix particles immersed in the aqueous cerium source solution By setting the amount of matrix particles immersed in the aqueous cerium source solution to 1% by mass or more, the amount of water to be evaporated can be reduced, and by setting it to 60% by mass or less, the cerium compound can be uniformly coated. .
  • the immersion conditions are preferably 0.1 to 24 hours at 0 to 90 ° C.
  • the cerium compound can be deposited on the surface of the mother phase particles by coating the mother phase particles with the cerium source aqueous solution by immersion and then drying.
  • the drying conditions are usually 80 to 200 ° C. and preferably 2 to 24 hours.
  • the coating amount of the cerium compound on the mother phase particles after dipping the mother phase particles in the aqueous cerium source solution and drying is preferably 1 to 50% by mass with respect to the mother phase particles. It is more preferably 5 to 50% by mass, and further preferably 5 to 30% by mass.
  • the coating amount is 1% by mass or more, the cerium compound is distributed over the entire matrix phase, and uniform coating can be achieved. When it is 50% by mass or less, cerium oxide does not precipitate alone.
  • the cerium source aqueous solution is applied to the mother phase particles with a rolling granulator or the like, and the mother phase particles are coated with the cerium source aqueous solution.
  • the coating amount of the aqueous cerium source solution on the mother phase particles is preferably 1 to 100% by mass, more preferably 5 to 80% by mass, and more preferably 10 to 60% by mass with respect to the mother phase particles. Is more preferable.
  • the coating amount is 1% by mass or more and 100% by mass or less, the aqueous solution reaches the entire matrix phase particles, and uniform coating can be achieved.
  • the application conditions are usually preferably 0 to 90 ° C.
  • Step (3) Step of firing mother phase particles coated with cerium source aqueous solution obtained in step (2) to obtain mother phase particles coated with cerium oxide Step (3) is obtained in step (2).
  • the mother phase particles coated with the aqueous cerium source solution are fired to oxidize the cerium compound, thereby obtaining mother phase particles coated with cerium oxide.
  • the firing temperature is preferably 300 to 1000 ° C, more preferably 400 to 1000 ° C, and still more preferably 400 to 800 ° C.
  • the cerium compound can be decomposed to deposit cerium oxide, and by setting it to 1000 ° C. or lower, the generation of coarse grains due to grain growth is suppressed, and the polishing abrasive with few scratches. Grains can be made.
  • the firing atmosphere is preferably in the air from the viewpoint of cost.
  • the firing time is usually preferably 2 to 72 hours.
  • the coarse particles may be removed by classifying the fired product.
  • classification method include known methods such as a sieve or a classifier.
  • the abrasive grains in the present invention can be produced by the above steps (1) to (3), but other steps may be performed as long as they do not affect each step. Examples of other steps include the above-described drying or classification step.
  • the abrasive grains in the present invention may be produced by a method that does not have one or more of the steps (1) to (3).
  • the abrasive grains of the present invention can be dispersed in a dispersion medium such as water to form a polishing slurry.
  • the abrasive grain concentration in the polishing slurry is preferably from 0.1 to 40% by mass, more preferably from 1 to 30% by mass, and even more preferably from 1 to 20% by mass.
  • the abrasive grain concentration is 0.1% by mass or more, a sufficient polishing rate can be obtained, and when it is 40% by mass or less, polishing can be performed efficiently.
  • Examples of the dispersion medium include water and alcohol.
  • Examples of the alcohol include methanol, ethanol, 2-propanol and ethylene glycol.
  • a dispersant may be added to the slurry.
  • the dispersant known ones can be used. Examples thereof include sodium citrate, sodium polyacrylate, ammonium polyacrylate, polyacrylic acid-maleic acid copolymer, pyridinecarboxylic acid and carboxymethylcellulose. Preferably mentioned.
  • the polishing slurry may be dispersed.
  • a known method can be used for the dispersion treatment, and examples thereof include a homogenizer, an ultrasonic homogenizer, a ball mill, a bead mill, and a wet jet mill.
  • the pH of the polishing slurry is preferably 2 to 12, more preferably 5 to 12, and still more preferably 5 to 11.
  • polishing can be performed without dissolving abrasive grains, and when the pH is 12 or less, polishing can be performed without affecting the object to be polished.
  • the volume-based median diameter (D 50 ) of the polishing slurry is preferably from 0.1 to 20 ⁇ m, more preferably from 0.5 to 20 ⁇ m, still more preferably from 0.5 to 10 ⁇ m.
  • the median diameter of the polishing slurry is measured by the method described later in the examples.
  • the median diameter of the polishing slurry is 0.1 ⁇ m or more, a sufficient polishing rate can be obtained, and when it is 20 ⁇ m or less, polishing scratches can be suppressed.
  • the manufacturing method of the glass product of this invention includes the grinding
  • the polishing method in the present invention is not particularly limited.
  • the glass and the polishing cloth are brought into contact with each other, and the polishing cloth and the glass are relatively moved while supplying the polishing abrasive grains or the polishing slurry. It is preferable to grind to the shape.
  • An example of the polishing cloth is a urethane polishing pad.
  • the cleaning process should be appropriately selected depending on the glass product. For example, in manufacturing a glass substrate for a magnetic disk, the following cleaning process is exemplified.
  • the method for producing a glass product of the present invention includes sulfuric acid, hydrochloric acid, nitric acid, sulfamic acid, phosphoric acid, oxalic acid, tartaric acid, citric acid, formic acid, glycolic acid, acetic acid, ascorbic acid, hydrogen peroxide, ammonia, sodium hydroxide, Including a step of cleaning the abrasive grains or polishing slurry adhering to the glass using a cleaning liquid containing at least one selected from potassium hydroxide, sodium carbonate and potassium carbonate (hereinafter also referred to as a cleaning liquid used in the present invention). Is preferred.
  • the total content of at least one selected from potassium is preferably 0.001 to 2 mol%, and more preferably 0.01 to 1 mol%.
  • the cleaning liquid used in the present invention preferably contains a cleaning auxiliary.
  • the cleaning aid include a surfactant for lowering the surface tension, and an acid having a buffering effect for stably maintaining pH.
  • surfactant examples include nonionic surfactants such as acetylene diol and anionic surfactants such as sodium polyacrylate.
  • examples of the acid having a buffering effect for stably maintaining pH include an acid having a pKa of 2 to 5 and having one or more carboxylic acids.
  • citric acid can be cited as an acid that can be expected to have a buffering effect, but many other organic acids can be used.
  • the cleaning liquid used in the present invention preferably contains water as a solvent.
  • water examples include deionized water, ultrapure water, charged ion water, hydrogen water, and ozone water. Since water has a function of controlling the fluidity of the cleaning liquid used in the present invention, its content can be appropriately set according to the target cleaning characteristics such as the cleaning speed, but usually 55 to 98 mass. % Is preferable.
  • the cleaning step it is preferable to perform cleaning by bringing the cleaning liquid into direct contact with glass.
  • the method of bringing the cleaning liquid into direct contact with the glass include, for example, dip cleaning in which the cleaning liquid is filled in a cleaning tank, and glass is placed in the cleaning tank, a method of spraying the cleaning liquid onto the glass from a nozzle, and scrub cleaning using a sponge made of polyvinyl alcohol Etc.
  • the cleaning liquid used in the present invention can be applied to any of the above methods, but dip cleaning using ultrasonic cleaning is preferred because more efficient cleaning can be performed.
  • the time for bringing the cleaning liquid into contact with the glass is preferably 30 seconds or more. By setting it to 30 seconds or more, a sufficient cleaning effect can be obtained.
  • the temperature of the washing solution may be room temperature, and may be used after being heated to about 40 to 80 ° C., but is preferably 80 ° C. or less.
  • the temperature of the cleaning liquid By setting the temperature of the cleaning liquid to 80 ° C. or lower, it is possible to prevent the acid, alkali, oxidizing agent or reducing agent contained in the cleaning liquid from causing thermal decomposition. Further, because of the configuration of the apparatus, when the cleaning liquid reaches a temperature close to 100 ° C., it becomes difficult to control pH by evaporation of water, and therefore, the temperature is preferably 80 ° C. or lower.
  • the glass product is a glass substrate for magnetic disks, a glass substrate for high-quality liquid crystal display, etc., the glass main surface of the present invention after the cleaning step, It is preferable to include a final polishing step of polishing using a slurry containing colloidal silica abrasive grains.
  • glass products manufactured by the manufacturing method of the present invention include magnetic disk substrates for hard disk drives, glass substrates such as semiconductor substrates, photomask substrates, and display substrates, lenses, blue filter glasses for CCDs, and cover glasses. Can be mentioned.
  • a magnetic disk can be manufactured by forming a magnetic recording layer on the main surface of a glass substrate for a magnetic disk manufactured by the manufacturing method of the present invention.
  • the obtained oxide was manganese oxide (Mn 2 O 3 ).
  • the X-ray profile of the obtained manganese oxide was measured by TTR-III (manufactured by Rigaku Corporation). The result is shown in FIG.
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured with MT3300EXII (manufactured by Nikkiso Co., Ltd.), and the pH is shown in Table 1.
  • Example 2 30 g of manganese oxide obtained in Example 1 was put in a plastic bag, and 6.9 g of an aqueous solution of 16.9% by mass of cerium acetate monohydrate (manufactured by Kanto Chemical Co., Inc.) was sprayed by spraying. The spray amount was 23% by mass with respect to manganese oxide, and 2% by mass in terms of cerium oxide.
  • the obtained oxide was Mn 2 O 3 coated with CeO 2 .
  • the X-ray profile of the obtained manganese oxide coated with cerium oxide was analyzed in the same manner as in Example 1. The result is shown in FIG. As shown in FIG. 1, a peak attributed to CeO 2 was observed at 28.4 ° in addition to Mn 2 O 3 , confirming that cerium oxide was precipitated.
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 3 20 g of zinc oxide (manufactured by Kokusei Kagaku Co., Ltd., reagent), 378 g of distilled water and 2 g of a dispersant (Lion Co., Ltd., Polyty A-550), which were baked at 700 ° C. for 8 hours in the atmosphere, were mixed, and a homogenizer was added for 15 minutes. A polishing slurry was obtained. The abrasive grain concentration in the polishing slurry was 5% by mass, and the dispersant concentration was 0.5% by mass.
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 4 30 g of zinc oxide similar to Example 3 was sprayed with 5.4 g of an aqueous solution of 5.4% by mass of cerium acetate monohydrate (manufactured by Kanto Chemical Co., Ltd., reagent) by spraying.
  • the spray amount is 18% by mass with respect to zinc oxide, and is 0.5% by mass in terms of cerium oxide.
  • it baked at 700 degreeC for 8 hours in air
  • the resulting oxide was ZnO which CeO 2 is coated.
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 5 It put into the type
  • the amount of the cerium acetate monohydrate aqueous solution was 200% by mass with respect to manganese oxide, and was 10% by mass in terms of cerium oxide. Then, it baked at 700 degreeC for 8 hours in air
  • the obtained oxide was Mn 2 O 3 coated with CeO 2 .
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 6 It put into the type
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 7 A flask made of 50 g of zinc oxide (manufactured by High Purity Chemical Co., reagent) and 100 g of an aqueous solution of 9.7% by mass of cerium acetate monohydrate (manufactured by Kanto Chemical Co., Ltd.) baked at 700 ° C. for 8 hours in the atmosphere. The flask was dried while rotating the flask with an evaporator. The amount of cerium acetate monohydrate aqueous solution is 200% by mass with respect to zinc oxide, and 10% by mass in terms of cerium oxide. Then, it baked at 700 degreeC for 8 hours in air
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • Example 8 A type flask comprising 50 g of zinc oxide (manufactured by High Purity Chemical Co., reagent) and 150 g of an aqueous solution of 13.0% by mass of cerium acetate monohydrate (manufactured by Kanto Chemical Co., Ltd.) baked in the atmosphere at 700 ° C. for 8 hours.
  • the flask was dried while rotating the flask with an evaporator.
  • the amount of the cerium acetate monohydrate aqueous solution is 300% by mass with respect to zinc oxide, and is 20% by mass in terms of cerium oxide. Thereafter, it was baked at 700 ° C. for 8 hours in the atmosphere.
  • the obtained oxide was ZnO coated with CeO2.
  • the volume-based median diameter (D 50 ) of the obtained polishing slurry was measured in the same manner as in Example 1, and the pH is shown in Table 1.
  • the abrasive grains obtained by using manganese oxide or zinc oxide as mother phase particles and coating the mother phase particles with cerium oxide have higher solubility in the cleaning liquid than cerium oxide. Indicated.
  • Polishing Test A polishing test was performed using the polishing slurries of Examples 1 to 8 obtained in (1).
  • Example 1 polishing slurry of Example 2 Example 2 polishing slurry of Example 4, Comparative Example 1 of Example 1 polishing slurry, Comparative Example 2 of Example 3 polishing slurry, Example 3 of Example 5 polishing slurry, Example 4 used the polishing slurry of Example 6,
  • Example 5 used the polishing slurry of Example 7, and Example 6 used the polishing slurry of Example 8.
  • polishing pressure was 12 kPa
  • platen rotation speed was 40 rpm.
  • a 12B single-side polishing machine (manufactured by Speed Fam) was used as the polishing machine, and FX8H-101U (manufactured by Fujibow) was used as the polishing pad.
  • the polishing slurry was circulated at 100 ml / min and polished for 20 minutes.
  • the polishing rate ( ⁇ m / min) was calculated from the weight difference before and after polishing. The results are shown in Table 3.
  • the coating amount of the mother phase particles with cerium oxide is preferably 0.1 to 25% by mass in terms of cerium oxide.
  • the abrasive grains and polishing slurry of the present invention are used in the manufacture of glass products such as magnetic disk substrates for hard disk drives, glass substrates such as semiconductor substrates, photomask substrates and display substrates, lenses, and blue filter glasses and cover glasses for CCD It can be used for the polishing process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Surface Treatment Of Glass (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Grinding Of Cylindrical And Plane Surfaces (AREA)

Abstract

La présente invention a pour but de proposer des grains abrasifs et une bouillie de polissage, les deux rendant possible de polir un objet devant être poli à un taux de polissage élevé même lorsque la quantité d'oxyde de cérium utilisée est réduite. La présente invention concerne des grains abrasifs obtenus par enrobage des particules de base par de l'oxyde de cérium.
PCT/JP2012/071349 2011-09-09 2012-08-23 Grains abrasifs, leur procédé de fabrication, bouillie de polissage et procédé de fabrication de produits verriers Ceased WO2013035545A1 (fr)

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JPWO2014034746A1 (ja) * 2012-08-28 2016-08-08 Hoya株式会社 磁気ディスク用ガラス基板の製造方法
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CN104673101A (zh) * 2015-02-12 2015-06-03 柳州豪祥特科技有限公司 一种稀土抛光粉的制备工艺
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JPWO2014034746A1 (ja) * 2012-08-28 2016-08-08 Hoya株式会社 磁気ディスク用ガラス基板の製造方法
WO2015049942A1 (fr) * 2013-10-03 2015-04-09 三井金属鉱業株式会社 Substance abrasive, procédé pour sa production et boue abrasive la contenant
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WO2015098945A1 (fr) * 2013-12-24 2015-07-02 堺化学工業株式会社 Particules d'oxyde de zinc recouvertes d'oxyde de cérium, procédé pour leur préparation, agent protecteur contre le rayonnement ultraviolet et produit cosmétique
JPWO2015098945A1 (ja) * 2013-12-24 2017-03-23 堺化学工業株式会社 酸化セリウム被覆酸化亜鉛粒子、その製造方法、紫外線遮蔽剤及び化粧料
JP2015155139A (ja) * 2014-01-20 2015-08-27 信越化学工業株式会社 合成石英ガラス基板の製造方法
US10696563B2 (en) 2014-02-07 2020-06-30 Sakai Chemical Industry Co., Ltd. Hexagonal plate-shaped zinc oxide particles, method for production of the same, and cosmetic, filler, resin composition, infrared reflective material, and coating composition containing the same
WO2016158328A1 (fr) * 2015-04-01 2016-10-06 三井金属鉱業株式会社 Abrasif et suspension épaisse contenant ce dernier
JPWO2016158328A1 (ja) * 2015-04-01 2017-09-14 三井金属鉱業株式会社 研摩材および研摩スラリー

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