WO2016103575A1 - 研磨用組成物、研磨方法、及びセラミック製部品の製造方法 - Google Patents
研磨用組成物、研磨方法、及びセラミック製部品の製造方法 Download PDFInfo
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- WO2016103575A1 WO2016103575A1 PCT/JP2015/005880 JP2015005880W WO2016103575A1 WO 2016103575 A1 WO2016103575 A1 WO 2016103575A1 JP 2015005880 W JP2015005880 W JP 2015005880W WO 2016103575 A1 WO2016103575 A1 WO 2016103575A1
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- acid
- polishing composition
- abrasive grains
- ceramic
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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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
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Definitions
- the present invention relates to a polishing composition, a polishing method, and a method for manufacturing a ceramic part.
- a technique is known in which the surface of a ceramic part is polished by using a polishing composition containing abrasive grains made of diamond to perform mirror finishing or smoothing (see, for example, Patent Documents 1 and 2).
- a polishing composition containing abrasive grains made of diamond is expensive and has a problem in that scratches tend to occur and it is difficult to obtain a high-quality mirror surface.
- the present invention solves the problems of the prior art as described above, and is a polishing composition, a polishing method, and a ceramic part that are inexpensive and can perform high-quality mirror finish on ceramics. It is an object to provide a manufacturing method.
- a polishing composition according to one embodiment of the present invention is a polishing composition for polishing ceramic, contains abrasive grains, and has a pH of 6.0 or more and 9.0 or less. This is the gist.
- Another aspect of the polishing method according to the present invention is to polish an object to be polished using the polishing composition according to the above aspect.
- the gist of a method for manufacturing a ceramic part according to still another aspect of the present invention includes polishing the ceramic part by the polishing method according to the other aspect.
- the polishing composition, the polishing method, and the method for producing a ceramic part of the present invention are inexpensive and can provide a high-quality mirror finish to ceramic.
- the polishing composition of this embodiment is a polishing composition for polishing ceramics, contains abrasive grains, and has a pH of 6.0 or more and 9.0 or less. And this abrasive grain may contain a silica. Further, the difference in zeta potential between the ceramic and the abrasive may be 20 mV to 60 mV.
- Such a polishing composition of the present embodiment is suitably used for polishing ceramics, and since scratches do not easily occur, high-gloss and high-quality mirror finish can be performed on ceramics. Further, the polishing composition of the present embodiment is inexpensive because it does not contain abrasive grains made of diamond. Furthermore, the polishing composition of this embodiment can polish a ceramic that is harder and harder to polish than materials such as metals and resins at a sufficiently high polishing rate.
- a ceramic part having a high texture for example, high-quality feeling
- a mirror-finished surface can be produced.
- materials such as metals and resins have a limit in improving the surface texture, ceramics can give a higher texture to the mirror finish, so that products with higher customer satisfaction can be produced.
- Ceramics with excellent strength, durability, light weight, and design as a material ornaments (for example, accessories, watches), electronic devices (for example, mobile phone terminals, personal computers), cameras, sports / healthcare products, dental supplies (For example, dentures), parts of various articles such as automobile interior members can be manufactured.
- the demand for surface design is particularly strong for decorative products, electronic devices, automobile interior parts, etc.
- high-grade products are strongly demanded for surface design that emphasizes texture (for example, luxury).
- the polishing composition of the present embodiment is suitable for the production of ceramic parts of various articles.
- the mirror finish by polishing can give a better mirror finish, and no paint or coating is required.
- the mirror surface by polishing has higher durability than the mirror surface by painting, coating, plating, etc., the mirror surface lasts for a long period of time. From these points, the mirror finish by polishing is superior to the mirror finish by painting, coating, plating, or the like.
- the texture refers to a material feeling peculiar to ceramic inclusions, and can be expressed as, for example, a feeling of weight or presence.
- ceramic can produce a color tone different from that of metal or resin.
- the texture of ceramics unlike metallic and plastic materials, for example, includes depth, warmth, and unique luster, which can be used by those who see the beauty and luxury of ceramics, for example. Can be given to those who touch.
- Ceramic with a mirror-finished surface has a glossy texture, so it has a glossy texture that is different from metals and resins, and the glossy surface has, for example, ceramics as a craft or art object Although it is different from, it may be inferior or have a better aesthetics and luxury.
- a ceramic part having a highly smooth surface is excellent in touch feeling and can be excellent in strength such as impact resistance.
- Ceramics to be polished The type of ceramic that can be applied to polishing with the polishing composition of the present embodiment is not particularly limited, and Mg, Ca, Sr, Ba, Sc, Y, La, Ti, Zr , Hf, V, Nb, Ta, Cr, Mo, W, Mn, Fe, Co, Ni, Cu, Ag, Au, Zn, Al, Ga, In, Sn, Pb, Bi, Ce, Pr, Nd, Er Ceramics mainly composed of oxides of metal elements such as Lu and Lu. These ceramics may be used individually by 1 type, and 2 or more types may be mixed and used for them.
- ceramics mainly composed of oxides of Mg, Y, Ti, Zr, Cr, Mn, Fe, Zn, Al, and Er are suitable as ceramics to be polished with the polishing composition of the present embodiment.
- Zirconia and alumina are more preferred.
- other than metal oxide ceramics aluminum titanate, aluminum nitride, silicon nitride, silicon carbide, etc. can be applied to polishing with the polishing composition of the present embodiment.
- the ceramic in the present invention does not include single crystals such as sapphire and silicon carbide.
- abrasive grain contained in the polishing composition of this embodiment is not specifically limited,
- the abrasive grain containing a silica can be used.
- the type of silica is not particularly limited, and examples thereof include colloidal silica, fumed silica, and sol-gel silica. These silicas may be used alone or in combination of two or more. Among these, fumed silica and colloidal silica are preferable from the viewpoint that the surface of the ceramic can be more efficiently smoothed.
- Colloidal silica can be produced by the following known methods. For example, a method by hydrolysis of alkoxysilane described in pages 154 to 156 of “Science of Sol-Gel Method” by Sakuo Sakuo (published by Agne Jofu Co., Ltd.); described in JP-A-11-60232 A method in which methyl silicate or a mixture of methyl silicate and methanol is dropped into water, methanol, and a mixed solvent composed of ammonia or ammonia and an ammonium salt to react methyl silicate with water; As described in JP-A-2007-52032, a method of hydrolyzing an alkyl silicate koji with an acid catalyst and then adding an alkali catalyst and heating to advance polymerization of silicic acid to grow particles; And a method of using a specific type of hydrolysis catalyst in a specific amount at the time of hydrolysis of alkoxysilane. In addition, a method for producing sodium silicate by ion exchange is also mentioned.
- fumed silica As a method for producing fumed silica, there is a method using a gas phase reaction in which silicon tetrachloride is vaporized and burned in an oxyhydrogen flame. Further, fumed silica can be made into an aqueous dispersion by a known method. Examples of methods for making an aqueous dispersion include, for example, JP-A-2004-43298, JP-A-2003-176123, and JP-A-2002. And the method described in Japanese Patent No. 309239.
- the average primary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment may be 5 nm or more, preferably 10 nm or more, and more preferably 15 nm or more. When the average primary particle diameter of the abrasive grains is within the above range, the polishing rate of the ceramic is improved. On the other hand, the average primary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment may be 400 nm or less, preferably 300 nm or less, more preferably 200 nm or less, and even more preferably 100 nm or less. . If the average primary particle diameter of the abrasive grains is within the above range, it is easy to obtain a surface with low defects and low surface roughness by polishing.
- abrasive grains having a large particle diameter remain on the surface of the ceramic after polishing
- abrasive grains having a small particle diameter for example, an average primary particle diameter of 200 ⁇ m or less
- the average primary particle diameter of an abrasive grain can be calculated from the specific surface area measured, for example by the nitrogen adsorption method (BET method). More specifically, it can be determined by the method described in Examples described later.
- the content of abrasive grains in the polishing composition may be 1% by mass or more, and preferably 2% by mass or more. If the content of the abrasive grains is within the above range, the polishing rate of the ceramic with the polishing composition is improved. On the other hand, the content of abrasive grains in the polishing composition may be 50% by mass or less, preferably 45% by mass or less. If content of an abrasive grain is in said range, the manufacturing cost of polishing composition will reduce. Further, the amount of abrasive grains remaining on the surface of the ceramic after polishing is reduced, and the cleanliness of the ceramic surface is improved.
- the difference between the zeta potential of the ceramic that is the object to be polished and the zeta potential of the abrasive grains contained in the polishing composition of the present embodiment is in the range of 20 mV to 60 mV, preferably 40 mV to 55 mV. It is. When the difference between the two zeta potentials is within the above range, the polishing rate of the ceramic by the polishing composition becomes higher.
- the value of the zeta potential of ceramic and abrasive grains can be measured by, for example, electrophoretic light scattering or electroacoustic spectroscopy.
- the measuring apparatus include “ELS-Z” manufactured by Otsuka Electronics Co., Ltd. and “DT-1200” manufactured by Dispersion Technology Inc.
- the measurement of the zeta potential of the ceramic can be replaced by the measurement of the zeta potential of the fine particles comprising the main constituent components of the ceramic.
- the pH of the polishing composition of this embodiment is 6.0 or more and 9.0 or less, Preferably it is 7.0 or more and 8.5 or less.
- the polishing rate becomes higher.
- the reason why the polishing rate increases when the pH is in the above range is presumed to be related to the zeta potential of the ceramic that is the object to be polished.
- the pH of the polishing composition can be adjusted, for example, by adding a pH adjuster described later.
- a pH adjuster an etching agent, an oxidizing agent, a water-soluble polymer (a copolymer may be used as necessary).
- various additives such as anticorrosives, chelating agents, dispersion aids, preservatives, and antifungal agents may be added.
- the pH value of the polishing composition of the present embodiment can be adjusted by adding a pH adjuster.
- the pH adjuster used as necessary to adjust the pH value of the polishing composition to a desired value may be either acid or alkali, and may be a salt thereof.
- the addition amount of the pH adjuster is not particularly limited, and may be appropriately adjusted so that the polishing composition has a desired pH.
- the acid as the pH adjusting agent include inorganic acids, organic acids such as carboxylic acids and organic sulfuric acids.
- specific examples of the inorganic acid include hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, boric acid, carbonic acid, hypophosphorous acid, phosphorous acid, phosphoric acid and the like.
- carboxylic acid examples include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid, n-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycolic acid, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid , Maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetrahydrofurancarboxylic acid, methoxy
- organic sulfuric acid examples include methanesulfonic acid, ethanesulfonic acid, isethionic acid and the like. These acids may be used individually by 1 type, and may be used in combination of 2 or more type. Among these, sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, etc. are preferable from the viewpoint of improving the polishing rate among inorganic acids, and glycolic acid, succinic acid, maleic acid, citric acid, tartaric acid, malic acid, gluconic acid, itacone are preferable as organic acids. An acid or the like is preferable.
- the base as the pH adjuster include amines such as aliphatic amines and aromatic amines, organic bases such as quaternary ammonium hydroxide compounds, hydroxides of alkali metals such as potassium hydroxide, alkalis Examples include earth metal hydroxides and ammonia. Among these, potassium hydroxide and ammonia are preferable from the viewpoint of availability. These bases may be used individually by 1 type, and may be used in combination of 2 or more type.
- alkali metal examples include potassium and sodium.
- alkaline earth metal include calcium and strontium.
- specific examples of the salt include carbonate, hydrogen carbonate, sulfate, acetate, and the like.
- specific examples of quaternary ammonium include tetramethylammonium, tetraethylammonium, tetrabutylammonium and the like.
- the quaternary ammonium hydroxide compound includes quaternary ammonium hydroxide or a salt thereof, and specific examples thereof include tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrabutylammonium hydroxide and the like.
- amines include methylamine, dimethylamine, trimethylamine, ethylamine, diethylamine, triethylamine, ethylenediamine, monoethanolamine, N- ( ⁇ -aminoethyl) ethanolamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine
- examples include anhydrous piperazine, piperazine hexahydrate, 1- (2-aminoethyl) piperazine, N-methylpiperazine, guanidine and the like.
- a salt such as an ammonium salt of an acid or an alkali metal salt may be used as a pH adjuster.
- a salt of a weak acid and a strong base a salt of a strong acid and a weak base, or a salt of a weak acid and a weak base is used, a buffering action of pH can be expected.
- a salt it is possible to adjust not only the pH but also the conductivity by adding a small amount.
- An etching agent may be added to the polishing composition of the present embodiment in order to promote dissolution of the ceramic.
- the etching agent include inorganic acids such as nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid and hydrofluoric acid, organic acids such as acetic acid, citric acid, tartaric acid and methanesulfonic acid, inorganic alkalis such as potassium hydroxide and sodium hydroxide, Organic alkali such as ammonia, amine, quaternary ammonium hydroxide and the like can be mentioned.
- These etching agents may be used individually by 1 type, and may be used in combination of 2 or more type.
- Oxidizing Agent may be added to the polishing composition of this embodiment in order to oxidize the surface of the ceramic.
- the oxidizing agent include hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchlorate, persulfate, nitric acid and the like.
- Specific examples of the persulfate include sodium persulfate, potassium persulfate, and ammonium persulfate. These oxidizing agents may be used individually by 1 type, and may be used in combination of 2 or more type.
- the polishing composition of the present embodiment may be a water-soluble polymer (copolymer, acting on the surface of the ceramic or the abrasive grains, or a salt or derivative thereof). .) May be added.
- water-soluble polymers, water-soluble copolymers, and salts or derivatives thereof include polycarboxylic acids such as polyacrylates, polysulfonic acids such as polyphosphonic acid and polystyrene sulfonic acid, chitansan gum, and sodium alginate.
- Examples thereof include saccharides, cellulose derivatives such as hydroxyethyl cellulose and carboxymethyl cellulose, polyethylene glycol, polyvinyl alcohol, polyvinyl pyrrolidone, sorbitan monooleate, and oxyalkylene polymers having a single kind or plural kinds of oxyalkylene units. These may be used individually by 1 type and may be used in combination of 2 or more type.
- An anticorrosive agent may be added to the polishing composition of the present embodiment in order to suppress corrosion of the ceramic surface.
- Specific examples of the anticorrosive include amines, pyridines, tetraphenylphosphonium salts, benzotriazoles, triazoles, tetrazoles, benzoic acid and the like.
- One of these anticorrosive agents may be used alone, or two or more thereof may be used in combination.
- a chelating agent may be added to the polishing composition of this embodiment.
- Specific examples of chelating agents include carboxylic acid chelating agents such as gluconic acid, amine chelating agents such as ethylenediamine, diethylenetriamine, and trimethyltetraamine, ethylenediaminetetraacetic acid, nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetramine hexa Polyaminopolycarboxylic acid chelating agents such as acetic acid and diethylenetriaminepentaacetic acid, 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetrakis (methylenephosphonic acid), diethylenetriamine Penta (methylenephosphonic acid), ethane-1,1-diphosphonic acid, ethane-1,1,2-triphosphonic acid, methane
- a dispersion aid may be added in order to facilitate the redispersion of the aggregate of abrasive grains.
- Specific examples of the dispersion aid include condensed phosphates such as pyrophosphate and hexametaphosphate. These dispersing aids may be used alone or in combination of two or more.
- Preservative An antiseptic may be added to the polishing composition of this embodiment.
- Specific examples of the preservative include sodium hypochlorite and the like.
- a preservative may be used individually by 1 type, and may be used in combination of 2 or more type.
- 5-9 Antifungal Agent An antifungal agent may be added to the polishing composition of this embodiment.
- Specific examples of the antifungal agent include oxazolines such as oxazolidine-2,5-dione.
- the polishing composition of this embodiment may contain abrasive grains and a liquid medium such as water or an organic solvent. At this time, various additives may be added as desired.
- the liquid medium functions as a dispersion medium or solvent for dispersing or dissolving each component (abrasive grains, additives, etc.) of the polishing composition.
- the liquid medium include water and organic solvents.
- One kind can be used alone, or two or more kinds can be mixed and used, but it is preferable to contain water. However, it is preferable to use water containing as little impurities as possible from the viewpoint of suppressing the inhibition of the action of each component. Specifically, pure water, ultrapure water, or distilled water from which foreign substances are removed through a filter after removing impurity ions with an ion exchange resin is preferable.
- the manufacturing method of the polishing composition of this embodiment is not specifically limited, Abrasive grains and various additives as required are stirred and mixed in a liquid medium such as water. Can be manufactured. For example, it can manufacture by stirring and mixing the abrasive grain which consists of silica, and various additives, such as a pH adjuster, in water.
- a liquid medium such as water.
- it can manufacture by stirring and mixing the abrasive grain which consists of silica, and various additives, such as a pH adjuster, in water.
- the temperature at the time of mixing is not specifically limited, 10 to 40 degreeC is preferable and you may heat in order to improve a dissolution rate. Further, the mixing time is not particularly limited.
- Polishing Method and Ceramic Part Manufacturing Method Ceramic polishing using the polishing composition of the present embodiment can be performed by a polishing apparatus and polishing conditions used for normal polishing.
- a single-side polishing apparatus or a double-side polishing apparatus can be used.
- the substrate is held using a holder called a carrier, and a surface plate on which a polishing cloth is attached One side of the substrate is polished by rotating the platen while pressing the substrate against one side of the substrate while supplying the polishing composition.
- the substrate is held using a holder called a carrier, and a surface plate to which a polishing cloth is attached is applied to both sides of the substrate from both sides of the substrate. Both surfaces of the substrate are polished by rotating the surface plates on both sides while pressing and supplying the polishing composition.
- the substrate is polished by the physical action caused by friction (friction between the polishing cloth and the polishing composition and the ceramic) and the chemical action that the polishing composition provides to the ceramic.
- a conventional polishing method for polishing a ceramic part using a polishing composition containing abrasive grains made of diamond, from copper, cast iron, tin, tin alloy, or a mixture of these metals and resin baked In the polishing method for polishing ceramic parts using the polishing composition of the present embodiment, polishing is performed using a platen to which a polishing cloth is attached. Therefore, an excellent mirror surface can be obtained more easily than the conventional polishing method described above.
- polishing cloth various materials such as polyurethane, non-woven fabric, and suede can be used. In addition to the difference in materials, materials having various physical properties such as hardness and thickness can be used. Furthermore, any of those containing abrasive grains and those not containing abrasive grains can be used, but those containing no abrasive grains are preferably used. Furthermore, although there is no particular limitation on the polishing load (pressure load to polishing object) of the polishing conditions, 4.9 kPa (50 gf / cm 2) or more 98 kPa (1000 gf / cm 2) it may be less, preferably 7.
- the polishing rate (linear velocity) of the polishing conditions is not particularly limited, but may be 10 m / min or more and 300 m / min or less, and preferably 30 m / min or more and 200 m / min or less. If the polishing rate (linear velocity) is within this range, a sufficient polishing rate can be obtained. Further, the polishing cloth can be prevented from being damaged by the friction of the object to be polished, and the friction is sufficiently transmitted to the object to be polished, so that the so-called state of slipping of the object to be polished can be suppressed and sufficient polishing can be performed.
- the supply amount of the polishing composition among the polishing conditions varies depending on the type of the polishing object, the type of the polishing apparatus, and the polishing conditions, but the polishing composition is uneven between the polishing object and the polishing cloth. It is sufficient that the amount is sufficient to be supplied to the entire surface.
- the polishing composition may not be supplied to the entire polishing object, or the polishing composition may dry and solidify to cause defects on the surface of the polishing object.
- the supply amount of the polishing composition is large, it is not economical, and there is a possibility that friction is hindered by an excessive polishing composition (particularly a liquid medium such as water) and the polishing is hindered.
- the polishing time required in the main polishing step using the polishing composition of the present embodiment can be shortened, and an excellent mirror surface can be obtained. Can be obtained efficiently.
- the pre-polishing composition used in the pre-polishing step it is preferable to use a pre-polishing composition having a higher polishing power than the polishing composition of the present embodiment. Specifically, it is preferable to use abrasive grains having higher hardness and a larger average secondary particle diameter than the abrasive grains used in the polishing composition of the present embodiment.
- the kind of abrasive grains contained in the preliminary polishing composition is not particularly limited, and examples thereof include boron carbide, silicon carbide, aluminum oxide (alumina), zirconia, zircon, ceria, titania and the like. These may be used individually by 1 type and may be used in combination of 2 or more type. Among these abrasive grains, boron carbide and silicon carbide are particularly preferable as the abrasive grains contained in the preliminary polishing composition. Boron carbide and silicon carbide may contain an impurity element such as iron or carbon.
- the average secondary particle diameter of the abrasive grains contained in the preliminary polishing composition may be 0.1 ⁇ m or more, preferably 0.3 ⁇ m or more. Moreover, the average secondary particle diameter of the abrasive grains contained in the preliminary polishing composition may be 20 ⁇ m or less, and preferably 5 ⁇ m or less. As the average secondary particle size of the abrasive grains contained in the preliminary polishing composition decreases, it is easy to obtain a surface with low defects and low surface roughness. In addition, the average secondary particle diameter of the abrasive grains contained in the preliminary polishing composition can be measured by, for example, an electric resistance method. An example of an apparatus using this electrical resistance method is Multisizer III manufactured by Beckman Coulter.
- the content of abrasive grains in the preliminary polishing composition may be 0.5% by mass or more, and preferably 1% by mass or more. As the abrasive content increases, the polishing rate of the ceramic with the pre-polishing composition is improved. On the other hand, the content of abrasive grains in the preliminary polishing composition may be 40% by mass or less, and preferably 30% by mass or less. As the abrasive content decreases, the production cost of the preliminary polishing composition decreases.
- the preferred pH of the preliminary polishing composition is the same as the polishing composition of the present embodiment, the type of ceramic that is the object to be polished, the type of abrasive grains, the average secondary particle diameter of the abrasive grains, It depends on the manufacturing history of the abrasive grains.
- the pH of the preliminary polishing composition is adjusted with an acid, a base, or a salt thereof, similarly to the pH of the polishing composition of the present embodiment.
- the pre-polishing composition may contain various additives as desired, for example, a re-dispersing agent, like the polishing composition of the present embodiment.
- redispersant examples include fine particles having an average secondary particle diameter of 0.2 ⁇ m or less, a water-soluble polymer, a water-soluble copolymer, or a salt thereof optionally added to the polishing composition of the present embodiment. Can be given.
- the kind of fine particles having an average secondary particle diameter of 0.2 ⁇ m or less is not particularly limited, but for example, alumina, zirconia, zircon, ceria, titania, silica, chromium oxide, iron oxide, silicon nitride, titanium nitride, Examples thereof include titanium boride, tungsten boride, and manganese oxide. These fine particles may be used alone or in combination of two or more. Moreover, you may use the microparticles
- alumina for example, ⁇ -alumina, intermediate alumina, fumed alumina, alumina sol or a mixture thereof
- hydrated alumina for example, boehmite
- Aluminum hydroxide and silica for example, colloidal silica, fumed silica, sol-gel silica
- the average secondary particle diameter of the fine particles is preferably 0.005 ⁇ m or more, more preferably 0.01 ⁇ m or more, from the viewpoint of availability.
- the average secondary particle diameter of the fine particles is preferably 0.5 ⁇ m or less, more preferably 0.2 ⁇ m or less, and further preferably 0.1 ⁇ m or less. If the average secondary particle diameter of the fine particles is within the above range, not only the cost is reduced, but also the settling of the abrasive grains hardly occurs, and the redispersibility of the abrasive grains of the preliminary polishing composition is further increased.
- the average secondary particle diameter of the fine particles can be measured by, for example, a dynamic light scattering method.
- An example of a measuring apparatus using the dynamic light scattering method is UPA-UT151 manufactured by Nikkiso Co., Ltd.
- the polishing composition of the present embodiment can be recovered after being used for polishing the polishing object and reused for polishing the polishing object.
- the method of reusing the polishing composition there is a method in which the polishing composition discharged from the polishing apparatus is collected in a tank and is circulated again into the polishing apparatus to be used for polishing. If the polishing composition is circulated, the amount of the polishing composition discharged as a waste liquid can be reduced, so that the environmental load can be reduced. Moreover, since the quantity of the polishing composition to be used can be reduced, the manufacturing cost required for grinding
- the abrasive grains, additives, etc. consumed and lost due to use in polishing are added as a composition modifier and reused. Good.
- a composition regulator what mixed abrasive grain, an additive, etc. by arbitrary mixing ratios can be used.
- the polishing composition is adjusted to a composition suitable for reuse and suitable polishing can be performed.
- concentrations of the abrasive grains and other additives contained in the composition regulator are arbitrary and are not particularly limited, and may be appropriately adjusted according to the size of the tank and the polishing conditions.
- the polishing composition of the present embodiment may be a one-component type or a multi-component type such as a two-component type in which some or all of the components of the polishing composition are mixed at an arbitrary ratio. May be. Further, in polishing the polishing object, polishing may be performed using the stock solution of the polishing composition of the present embodiment as it is, but the polishing composition is diluted 10 times or more with a diluent such as water. Polishing may be performed using a diluted product.
- Example ⁇ Examples will be shown below, and the present invention will be described more specifically with reference to Table 1.
- Abrasive grains made of silica, water as a liquid medium, and a pH adjuster as an additive are mixed, and the abrasive grains are dispersed in water.
- a composition was prepared.
- potassium hydroxide was used as the pH adjuster, and for the other polishing compositions (pH 2.0 to 9.7), nitric acid was used as the pH adjuster. .
- the average primary particle diameter of silica used as abrasive grains is 45 nm.
- the content of abrasive grains in the entire polishing composition is 23% by mass.
- the average primary particle diameter of the abrasive grains is calculated from the specific surface area of the abrasive grains measured by the BET method using “Flow SorbII 2300” manufactured by Micromeritex and the density of the abrasive grains.
- Polishing device Single-side polishing device (surface plate diameter: 380 mm)
- Polishing cloth Polyurethane polishing cloth Polishing load: 17.6 kPa (180 gf / cm 2 )
- Table 2 shows the zeta potentials of silica, zirconia, and alumina. As can be seen from Table 2, the zeta potential varies with pH. From the zeta potential shown in Table 2, the difference between the zeta potential of the polishing object (zirconia) at each pH and the zeta potential of the abrasive grains (silica) contained in the polishing composition was calculated. The calculated zeta potential difference is shown in Table 1.
- the polishing rates of Examples 1 to 3 were higher than the polishing rates of Comparative Examples 1 to 5.
- the surface of the rectangular plate member made of white zirconia ceramic was a high-quality mirror surface with few scratches.
- the difference in zeta potential from zirconia is at the same level (for example, when the pH is 7), even when alumina is used as the abrasive grains, the same result as in this example using silica as the abrasive grains is obtained. was gotten.
Abstract
Description
また、本発明の他の態様に係る研磨方法は、上記一態様に係る研磨用組成物を用いて研磨対象物を研磨することを要旨とする。
さらに、本発明のさらに他の態様に係るセラミック製部品の製造方法は、上記他の態様に係る研磨方法でセラミック製部品を研磨することを含むことを要旨とする。
1.研磨対象物であるセラミックについて
本実施形態の研磨用組成物による研磨に適用可能なセラミックの種類は特に限定されるものではなく、Mg,Ca,Sr,Ba,Sc,Y,La,Ti,Zr,Hf,V,Nb,Ta,Cr,Mo,W,Mn,Fe,Co,Ni,Cu,Ag,Au,Zn,Al,Ga,In,Sn,Pb,Bi,Ce,Pr,Nd,Er,Lu等の金属元素の酸化物を主成分とするセラミックがあげられる。これらのセラミックは、1種を単独で用いてもよいし、2種以上を混合して用いてもよい。
さらに、金属酸化物系のセラミック以外では、チタン酸アルミニウム、窒化アルミニウム、窒化ケイ素、炭化ケイ素等は、本実施形態の研磨用組成物による研磨に適用可能である。
なお、本発明におけるセラミックには、サファイア、炭化ケイ素等の単結晶は含まれない。
本実施形態の研磨用組成物に含有される砥粒の種類は特に限定されるものではないが、例えば、シリカを含有する砥粒を使用することができる。シリカの種類は特に限定されるものではないが、例えば、コロイダルシリカ、フュームドシリカ、ゾルゲル法シリカ等があげられる。これらのシリカは、1種を単独で用いてもよいし、2種以上を併用してもよい。また、これらの中でも、セラミックの表面をより効率的に平滑化できるという観点から、フュームドシリカ、コロイダルシリカが好ましい。
なお、砥粒の平均一次粒子径は、例えば窒素吸着法(BET法)により測定した比表面積から算出することができる。さらに具体的には、後述する実施例に記載の方法によって求めることができる。
研磨対象物であるセラミックのゼータ電位と本実施形態の研磨用組成物に含有される砥粒のゼータ電位との差は、20mV以上60mV以下の範囲内とし、好ましくは40mV以上55mV以下である。両者のゼータ電位の差が上記範囲内であれば、研磨用組成物によるセラミックの研磨速度がより高くなる。
本実施形態の研磨用組成物のpHは、6.0以上9.0以下であり、好ましくは7.0以上8.5以下である。pHが上記範囲内であれば、研磨速度がより高くなる。pHが上記範囲内であると研磨速度が高くなる理由は、研磨対象物であるセラミックのゼータ電位が関係していると推察される。研磨用組成物のpHは、例えば後述するpH調整剤を添加することにより調整することができる。
本実施形態の研磨用組成物には、その性能を向上させるために、必要に応じてpH調整剤、エッチング剤、酸化剤、水溶性重合体(共重合体でもよい。また、これらの塩、誘導体でもよい)、防食剤、キレート剤、分散助剤、防腐剤、防黴剤等の各種添加剤を添加してもよい。
本実施形態の研磨用組成物のpHの値は、pH調整剤の添加により調整することができる。研磨用組成物のpHの調整により、セラミックの研磨速度や砥粒の分散性等を制御することができる。研磨用組成物のpHの値を所望の値に調整するために必要に応じて使用されるpH調整剤は、酸及びアルカリのいずれであってもよく、また、それらの塩であってもよい。pH調整剤の添加量は、特に限定されるものではなく、研磨用組成物が所望のpHとなるように適宜調整すればよい。
これらの中では、無機酸では硫酸、硝酸、塩酸、リン酸等が研磨速度向上の観点から好ましく、有機酸ではグリコール酸、コハク酸、マレイン酸、クエン酸、酒石酸、リンゴ酸、グルコン酸、イタコン酸等が好ましい。
水酸化第四級アンモニウム化合物としては、水酸化第四級アンモニウム又はその塩を含み、具体例としては、水酸化テトラメチルアンモニウム、水酸化テトラエチルアンモニウム、水酸化テトラブチルアンモニウム等があげられる。
本実施形態の研磨用組成物には、セラミックの溶解を促進するためにエッチング剤を添加してもよい。エッチング剤の例としては、硝酸、硫酸、塩酸、リン酸、フッ酸等の無機酸、酢酸、クエン酸、酒石酸、メタンスルホン酸等の有機酸、水酸化カリウム、水酸化ナトリウム等の無機アルカリ、アンモニア、アミン、第四級アンモニウム水酸化物等の有機アルカリ等があげられる。これらのエッチング剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、セラミックの表面を酸化させるために酸化剤を添加してもよい。酸化剤の具体例としては、過酸化水素、過酢酸、過炭酸塩、過酸化尿素、過塩素酸塩、過硫酸塩、硝酸等があげられる。過硫酸塩の具体例としては、過硫酸ナトリウム、過硫酸カリウム、過硫酸アンモニウム等があげられる。これら酸化剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、セラミックの表面や砥粒の表面に作用する水溶性重合体(共重合体でもよい。また、これらの塩、誘導体でもよい。)を添加してもよい。水溶性重合体、水溶性共重合体、これらの塩又は誘導体の具体例としては、ポリアクリル酸塩等のポリカルボン酸、ポリホスホン酸、ポリスチレンスルホン酸等のポリスルホン酸、キタンサンガム、アルギン酸ナトリウム等の多糖類、ヒドロキシエチルセルロース、カルボキシメチルセルロース等のセルロース誘導体、ポリエチレングリコール、ポリビニルアルコール、ポリビニルピロリドン、ソルビタンモノオレエート、単一種又は複数種のオキシアルキレン単位を有するオキシアルキレン系重合体等があげられる。これらは、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、セラミックの表面の腐食を抑制するために防食剤を添加してもよい。防食剤の具体例としては、アミン類、ピリジン類、テトラフェニルホスホニウム塩、ベンゾトリアゾール類、トリアゾール類、テトラゾール類、安息香酸等があげられる。これらの防食剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、キレート剤を添加してもよい。キレート剤の具体例としては、グルコン酸等のカルボン酸系キレート剤、エチレンジアミン、ジエチレントリアミン、トリメチルテトラアミン等のアミン系キレート剤、エチレンジアミン四酢酸、ニトリロ三酢酸、ヒドロキシエチルエチレンジアミン三酢酸、トリエチレンテトラミン六酢酸、ジエチレントリアミン五酢酸等のポリアミノポリカルボン酸系キレート剤、2-アミノエチルホスホン酸、1-ヒドロキシエチリデン-1,1-ジホスホン酸、アミノトリ(メチレンホスホン酸)、エチレンジアミンテトラキス(メチレンホスホン酸)、ジエチレントリアミンペンタ(メチレンホスホン酸)、エタン-1,1-ジホスホン酸、エタン-1,1,2-トリホスホン酸、メタンヒドロキシホスホン酸、1-ホスホノブタン-2,3,4-トリカルボン酸等の有機ホスホン酸系キレート剤、フェノール誘導体、1,3-ジケトン等があげられる。これらのキレート剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、砥粒の凝集体の再分散を容易にするために分散助剤を添加してもよい。分散助剤の具体例としては、ピロリン酸塩やヘキサメタリン酸塩等の縮合リン酸塩等があげられる。これらの分散助剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態の研磨用組成物には、防腐剤を添加してもよい。防腐剤の具体例としては、次亜塩素酸ナトリウム等があげられる。防腐剤は、1種を単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
5-9 防黴剤について
本実施形態の研磨用組成物には、防黴剤を添加してもよい。防黴剤の具体例としては、オキサゾリジン-2,5-ジオン等のオキサゾリン等があげられる。
本実施形態の研磨用組成物は、砥粒と、水、有機溶剤等の液状媒体と、を含有してもよい。このとき、所望により各種添加剤を添加してもよい。
液状媒体は、研磨用組成物の各成分(砥粒、添加剤等)を分散又は溶解するための分散媒又は溶媒として機能する。液状媒体としては水、有機溶剤があげられ、1種を単独で用いることができるし、2種以上を混合して用いることができるが、水を含有することが好ましい。ただし、各成分の作用を阻害することを抑制するという観点から、不純物をできる限り含有しない水を用いることが好ましい。具体的には、イオン交換樹脂にて不純物イオンを除去した後にフィルタを通して異物を除去した純水や超純水、あるいは蒸留水が好ましい。
本実施形態の研磨用組成物の製造方法は特に限定されるものではなく、砥粒と、所望により各種添加剤とを、水等の液状媒体中で攪拌、混合することによって製造することができる。例えば、シリカからなる砥粒と、pH調整剤等の各種添加剤とを、水中で攪拌、混合することによって製造することができる。混合時の温度は特に限定されるものではないが、10℃以上40℃以下が好ましく、溶解速度を向上させるために加熱してもよい。また、混合時間も特に限定されない。
本実施形態の研磨用組成物を用いたセラミックの研磨は、通常の研磨に用いられる研磨装置や研磨条件により行うことができる。例えば片面研磨装置や両面研磨装置を使用することができる。
例えば、研磨対象物であるセラミック製部品をセラミック製の基板とし、片面研磨装置を用いて研磨する場合には、キャリアと呼ばれる保持具を用いて基板を保持し、研磨布が貼付された定盤を基板の片面に押しつけて研磨用組成物を供給しながら定盤を回転させることにより、基板の片面を研磨する。
また、両面研磨装置を用いてセラミック製の基板を研磨する場合には、キャリアと呼ばれる保持具を用いて基板を保持し、研磨布が貼付された定盤を基板の両側から基板の両面にそれぞれ押しつけて、研磨用組成物を供給しながら両側の定盤を回転させることにより、基板の両面を研磨する。
ダイヤモンドからなる砥粒を含有する研磨用組成物を用いてセラミック製部品を研磨する従来の研磨方法においては、銅、鋳鉄、スズ、スズ合金、又はこれら金属と樹脂を混合し焼き固めたものからなる定盤を使用して研磨を行うが、本実施形態の研磨用組成物を用いてセラミック製部品を研磨する研磨方法においては、研磨布が貼付された定盤を使用して研磨を行うことができるので、上記の従来の研磨方法に比べて優れた鏡面がより得られやすい。
さらに、研磨条件のうち研磨荷重(研磨対象物に負荷する圧力)については特に限定されないが、4.9kPa(50gf/cm2)以上98kPa(1000gf/cm2)以下としてもよく、好ましくは7.8kPa(80gf/cm2)以上78kPa(800gf/cm2)以下であり、より好ましくは9.8kPa(100gf/cm2)以上59kPa(600gf/cm2)以下である。研磨荷重がこの範囲内であれば、十分な研磨速度が発揮され、荷重により研磨対象物が破損したり、研磨対象物の表面に傷等の欠陥が発生したりすることを抑制することができる。
さらに、予備研磨用組成物は、本実施形態の研磨用組成物と同様に、所望により各種添加剤を含有してもよく、例えば再分散剤を含有してもよい。再分散剤としては、平均二次粒子径が0.2μm以下である微粒子や、本実施形態の研磨用組成物に所望により添加される水溶性重合体、水溶性共重合体、又はこれらの塩があげられる。
これらの中でも、入手が容易で低コストであることから、金属酸化物が好ましく、アルミナ(例えばα-アルミナ、中間アルミナ、フュームドアルミナ、アルミナゾルやこれらの混合物)、水和アルミナ(例えばベーマイト)、水酸化アルミニウム、シリカ(例えばコロイダルシリカ、ヒュームドシリカ、ゾルゲル法シリカ)がより好ましい。
以下に実施例を示し、表1を参照しながら本発明をさらに具体的に説明する。
シリカからなる砥粒と、液状媒体である水と、添加剤であるpH調整剤と、を混合して、砥粒を水に分散させ、実施例1~3及び比較例1~5の研磨用組成物を製造した。比較例5の研磨用組成物(pH12.0)についてはpH調整剤として水酸化カリウムを用い、その他の研磨用組成物(pH2.0~9.7)についてはpH調整剤として硝酸を用いた。
なお、砥粒の平均一次粒子径は、マイクロメリテックス社製の“Flow SorbII 2300”を用いてBET法により測定された砥粒の比表面積と、砥粒の密度から算出したものである。
研磨装置:片面研磨装置(定盤の直径:380mm)
研磨布:ポリウレタン製研磨布
研磨荷重:17.6kPa(180gf/cm2)
定盤の回転速度:90min-1
研磨速度(線速度):71.5m/分
研磨時間:15分
研磨用組成物の供給速度:26mL/分
なお、ジルコニアとのゼータ電位の差が同レベルである場合には(例えばpHが7の場合)、砥粒としてアルミナを用いた場合でも、砥粒としてシリカを用いた本実施例と同様の結果が得られた。
Claims (5)
- セラミックを研磨する研磨用組成物であって、砥粒を含有し、pHが6.0以上9.0以下である研磨用組成物。
- 前記砥粒がシリカを含む請求項1に記載の研磨用組成物。
- 前記セラミックと前記砥粒のゼータ電位の差が20mV以上60mV以下である請求項1又は請求項2に記載の研磨用組成物。
- 請求項1~3のいずれか一項に記載の研磨用組成物を用いて研磨対象物を研磨する研磨方法。
- 請求項4に記載の研磨方法でセラミック製部品を研磨することを含むセラミック製部品の製造方法。
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Also Published As
Publication number | Publication date |
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CN107109196B (zh) | 2019-01-04 |
JP2016124047A (ja) | 2016-07-11 |
KR20170099842A (ko) | 2017-09-01 |
TW201636405A (zh) | 2016-10-16 |
EP3239262A4 (en) | 2018-01-10 |
JP6756460B2 (ja) | 2020-09-16 |
US20170355881A1 (en) | 2017-12-14 |
US10626297B2 (en) | 2020-04-21 |
EP3239262A1 (en) | 2017-11-01 |
CN107109196A (zh) | 2017-08-29 |
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