WO2022009990A1 - Polishing composition and polishing method - Google Patents
Polishing composition and polishing method Download PDFInfo
- Publication number
- WO2022009990A1 WO2022009990A1 PCT/JP2021/026014 JP2021026014W WO2022009990A1 WO 2022009990 A1 WO2022009990 A1 WO 2022009990A1 JP 2021026014 W JP2021026014 W JP 2021026014W WO 2022009990 A1 WO2022009990 A1 WO 2022009990A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polishing
- acid
- polished
- polishing composition
- abrasive grains
- Prior art date
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- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical class C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 1
- 235000004279 alanine Nutrition 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000003429 antifungal agent Substances 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- UREZNYTWGJKWBI-UHFFFAOYSA-M benzethonium chloride Chemical compound [Cl-].C1=CC(C(C)(C)CC(C)(C)C)=CC=C1OCCOCC[N+](C)(C)CC1=CC=CC=C1 UREZNYTWGJKWBI-UHFFFAOYSA-M 0.000 description 1
- 229960001950 benzethonium chloride Drugs 0.000 description 1
- 150000001565 benzotriazoles Chemical class 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical class [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000011222 crystalline ceramic Substances 0.000 description 1
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- XQRLCLUYWUNEEH-UHFFFAOYSA-N diphosphonic acid Chemical compound OP(=O)OP(O)=O XQRLCLUYWUNEEH-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- DUYCTCQXNHFCSJ-UHFFFAOYSA-N dtpmp Chemical compound OP(=O)(O)CN(CP(O)(O)=O)CCN(CP(O)(=O)O)CCN(CP(O)(O)=O)CP(O)(O)=O DUYCTCQXNHFCSJ-UHFFFAOYSA-N 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- GTTBQSNGUYHPNK-UHFFFAOYSA-N hydroxymethylphosphonic acid Chemical compound OCP(O)(O)=O GTTBQSNGUYHPNK-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- RMIODHQZRUFFFF-UHFFFAOYSA-N methoxyacetic acid Chemical compound COCC(O)=O RMIODHQZRUFFFF-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002918 oxazolines Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 150000003222 pyridines Chemical class 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- DVUVKWLUHXXIHK-UHFFFAOYSA-N tetraazanium;tetrahydroxide Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[OH-].[OH-].[OH-].[OH-] DVUVKWLUHXXIHK-UHFFFAOYSA-N 0.000 description 1
- USFPINLPPFWTJW-UHFFFAOYSA-N tetraphenylphosphonium Chemical class C1=CC=CC=C1[P+](C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 USFPINLPPFWTJW-UHFFFAOYSA-N 0.000 description 1
- 150000003536 tetrazoles Chemical class 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Definitions
- the present invention relates to a polishing composition and a polishing method.
- the substrate for electronic parts is often formed of single crystal ceramics (for example, single crystal sapphire), but when the substrate for electronic parts is formed of polycrystalline ceramics, the shape is larger than that of single crystal ceramics. In some cases, advantageous properties such as high degree of freedom, low manufacturing cost, and excellent optical characteristics can be obtained.
- An object of the present invention is to provide a polishing composition and a polishing method capable of smoothly polishing the surface of polycrystalline ceramics.
- the polishing composition according to one aspect of the present invention is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water, and has an average secondary order of abrasive grains.
- the gist is that the particle size is 5 nm or more and 40 nm or less.
- the polishing method according to another aspect of the present invention is intended to polish an object to be polished containing polycrystalline ceramics by using the polishing composition according to the above one aspect.
- the polishing composition of the present embodiment is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water.
- the average secondary particle diameter of the abrasive grains is 5 nm or more and 40 nm or less.
- the polishing method of the present embodiment is a method of polishing an object to be polished containing polycrystalline ceramics by using the polishing composition of the present embodiment.
- polishing the object to be polished containing the polycrystalline ceramics using the polishing composition of the present embodiment it is possible to smoothly polish the surface of the polycrystalline ceramics having uneven steps at the grain boundary portions. Is. Therefore, for example, even when a substrate for electronic components is formed of polycrystalline ceramics, the surface can be smoothed, and the degree of freedom in shape is high, the manufacturing cost is low, and the optical characteristics are excellent as compared with single crystal ceramics. Etc. and other superior properties can be obtained.
- polishing composition and the polishing method of the present embodiment will be described in detail.
- 1. About the object to be polished
- the polishing composition and the polishing method of the present embodiment can be used for polishing an object to be polished containing polycrystalline ceramics. Since polycrystalline ceramics have uneven steps at the grain boundaries, it is difficult to obtain a sufficiently smooth surface by polishing. However, polishing using the polishing composition and polishing method of the present embodiment is sufficient. It is possible to obtain a smooth surface.
- the types of polycrystalline ceramics are not particularly limited, but are, for example, metal-containing oxides, metal-containing nitrides, metal-containing carbides, metal-containing boroides, and metal-containing fluorides. Among these, oxides containing a metal, nitrides containing a metal, and carbides containing a metal are preferable.
- metal-containing oxides metal-containing nitrides, and metal-containing carbides
- silicon-containing oxides silicon-containing nitrides, silicon-containing carbides, aluminum-containing oxides, and aluminum.
- a nitride containing the above, and an oxide containing ittrium are preferable.
- These polycrystalline ceramics are used as substrates for electronic components such as communication devices, power semiconductors, communication high frequency devices, and pressure sensors.
- the substrate is particularly required to have a smooth surface.
- the oxides containing silicon the nitrides containing silicon, the carbides containing silicon, the oxides containing aluminum, the nitrides containing aluminum, and the oxides containing yttrium, the oxidation containing aluminum in particular.
- At least one of the material and the nitride containing aluminum is preferable.
- silicon oxide such as quartz as an oxide containing silicon
- silicon nitride SiN
- silicon carbide SiO 2
- examples of the aluminum-containing oxide include alumina (Al 2 O 3 ) such as translucent alumina and spinel ( Mg Al 2 O 4 )
- examples of the aluminum-containing nitride include aluminum nitride (Al N).
- examples of the oxide containing yttrium include ytria (Y 2 O 3 ) and YAG (Y 3 Al 5 O 12 ).
- the object to be polished may be any one containing polycrystalline ceramics, and may be entirely formed of polycrystalline ceramics or a part thereof may be formed of polycrystalline ceramics. Further, the type of the polycrystalline ceramics contained in the object to be polished may be one kind or a plurality of kinds. Specific examples of the object to be polished include a sintered body of a powder of polycrystalline ceramics.
- abrasive grains contained in the polishing composition of the present embodiment is not particularly limited, but for example, abrasive grains containing silica (SiO 2 ) or diamond can be used.
- the type of silica is not particularly limited, and examples thereof include colloidal silica, fumed silica, sol-gel method silica, and precipitation method silica. These silicas may be used alone or in combination of two or more.
- colloidal silica is preferable from the viewpoint of more efficiently smoothing the surface of polycrystalline ceramics.
- the average secondary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment needs to be 5 nm or more and 40 nm or less in order to sufficiently smooth the surface of the polycrystalline ceramics, but is 7 nm. It is preferably 35 nm or less.
- the surface of the single crystal ceramics can be easily sufficiently smoothed, so that the average secondary particle size is larger than the specific particle size (average secondary particles).
- Abrasive particles with a diameter larger than 40 nm) were used, but when polishing polycrystalline ceramics with crystal grain boundaries, the average secondary particle size is smaller than the specific particle size (average secondary particle size). It is important to use abrasive particles (abrasive particles of 5 nm or more and 40 nm or less).
- abrasive grains with an average secondary grain size larger than the specific grain size are used, the convex and concave portions of the grain boundaries are processed at the same time, so it is not possible to fill the grain boundary steps and a sufficiently smooth surface can be obtained.
- abrasive grains with an average secondary particle size smaller than the specific grain size are used, the abrasive grains do not come into contact with the concave portions of the grain boundary steps and only the convex portions are processed, so that the grain boundary steps are eliminated and the grain boundaries are sufficiently smooth.
- the surface can be obtained.
- the average secondary particle size of the abrasive grains can be measured using, for example, a laser diffraction / scattering type particle size distribution measuring device (for example, "LA-950" manufactured by HORIBA, Ltd.).
- the content of the abrasive grains in the polishing composition of the present embodiment is not particularly limited, but is preferably 1% by mass or more and 30% by mass or less, and is preferably 3% by mass or more and 25% by mass or less. It is more preferable to do so.
- a polishing composition having an abrasive grain content within the above range the surface of the polycrystalline ceramic can be polished more smoothly.
- the polishing composition of the present embodiment is a slurry containing the above-mentioned abrasive grains and water.
- Water functions as a dispersion medium or solvent that disperses abrasive grains and disperses or dissolves other components.
- a mixture of water and an organic solvent may be used as a dispersion medium or a solvent.
- the water used is preferably water containing as little impurities as possible from the viewpoint of suppressing the inhibition of the action of the above other components. Specifically, pure water, ultrapure water, or distilled water from which foreign substances have been removed through a filter after removing impurity ions with an ion exchange resin is preferable.
- the pH of the polishing composition of the present embodiment is not particularly limited, but is preferably 1.5 or more and 9.0 or less, and more preferably 2.0 or more and 8.5 or less. By using a polishing composition having a pH within the above range, the surface of the polycrystalline ceramic can be polished more smoothly.
- the pH of the polishing composition of the present embodiment may be adjusted by an additive pH adjuster. As the pH adjuster, one type may be used alone, or two or more types may be mixed or used.
- the polishing composition of the present embodiment may optionally contain an additive (for example, a pH adjuster) which is the above-mentioned other component.
- a pH adjuster known acids, bases, or salts thereof can be used.
- Specific examples of acids that can be used as a pH adjuster include inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, boric acid, carbonic acid, hypophobic acid, phobic acid, and phosphoric acid, and formic acid, acetic acid, and propion.
- 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, pimelli acid, maleic acid, phthalic acid, malic acid, tartrate acid, citric acid, Examples thereof include organic acids such as lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetratetracarboxylic acid, methoxyacetic acid, methoxyphenylacetic acid, and phenoxy
- an inorganic acid sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid and the like are preferable from the viewpoint of improving the polishing speed, and when an organic acid is used as the pH adjuster, glycolic acid, succinic acid, maleic acid and the like are preferable.
- an organic acid glycolic acid, succinic acid, maleic acid and the like are preferable.
- Citric acid, tartrate acid, malic acid, gluconic acid, itaconic acid and the like are preferable.
- Bases that can be used as a pH adjuster include amines such as aliphatic amines and aromatic amines, organic bases such as tetraammonium hydroxide, hydroxides of alkali metals such as potassium hydroxide, and hydroxylation of alkaline earth metals. Things, ammonia and the like can be mentioned. Among these bases, potassium hydroxide and ammonia are preferable because of their availability.
- a salt such as an ammonium salt or an alkali metal salt of the acid may be used as a pH adjuster in place of the acid or in combination with the acid.
- a pH buffering action can be expected, and in the case of a salt of a strong acid and a strong base, a buffering action of pH can be expected.
- the amount of the pH adjuster added is not particularly limited, and the pH may be appropriately adjusted so that the polishing composition has a desired pH.
- the polishing composition of the present embodiment may further contain an additive other than the pH adjuster, if necessary, but from the viewpoint of polishing the surface of the polycrystalline ceramic more smoothly, the pH adjuster. It is preferable that it does not contain any additives other than.
- the polishing composition may contain additives such as a complexing agent, an etching agent, and an oxidizing agent, which have an effect of further increasing the polishing rate.
- the polishing composition may contain a water-soluble polymer (a copolymer, a salt thereof, or a derivative thereof) that acts on the surface of the object to be polished or the surface of the abrasive grains.
- the polishing composition may contain additives such as a dispersant that improves the dispersibility of the abrasive grains and a dispersion aid that facilitates the redispersion of the aggregates of the abrasive grains. Further, the polishing composition may contain known additives such as preservatives, fungicides and rust inhibitors.
- additives are known in many patent documents and the like as those that can be usually added in a polishing composition, and the type and amount of the additives are not particularly limited. However, when these additives are added, the amount added is preferably less than 1% by mass, and more preferably less than 0.5% by mass, respectively, with respect to the entire polishing composition. These additives may be used alone or in combination of two or more.
- complexing agents include inorganic acids, organic acids, amino acids, nitrile compounds, chelating agents and the like.
- the inorganic acid include sulfuric acid, nitric acid, boric acid, carbonic acid and the like.
- organic acids 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, malein Examples thereof include acid, phthalic acid, malic acid, tartrate acid, citric acid, lactic acid and the like.
- Organic sulfuric acids such as methanesulfonic acid, ethanesulfonic acid, and isethionic acid can also be used.
- Salts such as alkali metal salts of inorganic or organic acids may be used in place of or in combination with the inorganic or organic acids.
- complexing agents glycine, alanine, malic acid, tartaric acid, citric acid, glycolic acid, isethionic acid, or salts thereof are preferable.
- chelating agents include carboxylic acid-based chelating agents such as gluconic acid, amine-based chelating agents such as ethylenediamine, diethylenetriamine, and trimethyltetraamine, ethylenediaminetetraacetic acid, nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, and triethylenetetramine.
- carboxylic acid-based chelating agents such as gluconic acid
- amine-based chelating agents such as ethylenediamine, diethylenetriamine, and trimethyltetraamine
- ethylenediaminetetraacetic acid nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, and triethylenetetramine.
- polyaminopolycarboxylic acid-based chelating agents such as hexaacetic acid and diethylenetriaminepentaacetic acid.
- etching agents include inorganic acids such as nitrate, sulfuric acid, hydrochloric acid, phosphoric acid and hydrofluoric acid, organic acids such as acetic acid, citric acid, tartaric acid and methanesulfonic acid, potassium hydroxide, sodium hydroxide and ammonia.
- examples thereof include inorganic alkalis such as amines and organic alkalis such as quaternary ammonium hydroxide.
- the oxidizing agent include hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchlorate, persulfate, nitric acid, potassium permanganate and the like.
- water-soluble polymers may be copolymers, salts thereof, derivatives
- examples of water-soluble polymers include polycarboxylic acids such as polyacrylates, polyphosphonic acids, polysulfonic acids such as polystyrene sulfonic acid, chitansan gum, sodium alginate and the like.
- examples thereof include the polysaccharides of the above, and cellulose derivatives such as hydroxyethyl cellulose and carboxymethyl cellulose.
- polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, sorbitan monooleate, an oxyalkylene polymer having a single type or a plurality of types of oxyalkylene units, and the like can also be mentioned as examples of the water-soluble polymer.
- Examples of the dispersion aid include pyrophosphate, condensed phosphate such as hexamethaphosphate, and the like.
- Examples of preservatives include sodium hypochlorite and the like.
- Examples of antifungal agents include oxazolines such as oxazolidine-2,5-dione.
- Examples of the anticorrosive agent include surfactants, alcohols, polymers, resins, amines, pyridines, tetraphenylphosphonium salts, benzotriazoles, triazoles, tetrazole, benzoic acid and the like.
- the surfactant examples include a nonionic surfactant, an anionic surfactant, a cationic surfactant, and an amphoteric surfactant.
- examples of the nonionic surfactant include ether type, ether ester type, ester type and nitrogen-containing type, and examples of the anionic surfactant include carboxylate, sulfonate, sulfate ester and phosphoric acid ester salt. Can be mentioned.
- Examples of the cationic surfactant include an aliphatic amine salt, an aliphatic quaternary ammonium salt, a benzalkonium chloride salt, a benzethonium chloride, a pyridinium salt and an imidazolinium salt, and examples of the amphoteric surfactant include carboxy. Examples thereof include betaine type, aminocarboxylate, imidazolinium betaine, lecithin, and alkylamine oxide.
- the manufacturing method of the polishing composition of this embodiment is not particularly limited, and it is manufactured by stirring and mixing abrasive grains and various additives in water, if desired. be able to.
- the temperature at which each component is mixed is not particularly limited, but is preferably 10 ° C. or higher and 40 ° C. or lower, and may be heated in order to improve the dissolution rate. Further, the mixing time is not particularly limited.
- the polishing composition of the present embodiment may be a one-dosage form, or may be a two-dosage form or a multi-dosage form in which a part or all of the components of the polishing composition are mixed at an arbitrary ratio. good. Further, the polishing composition of the present embodiment may be prepared by diluting the undiluted solution of the polishing composition with water, for example, 10 times or more.
- the order of mixing and diluting the two raw material compositions which are the raw materials of the polishing composition is arbitrary. For example, one raw material composition may be diluted with water and then mixed with the other raw material composition, both raw material compositions may be mixed and diluted with water at the same time, or both. The raw material composition of the above may be mixed and then diluted with water.
- polishing device and polishing method The polishing composition of the present embodiment can be used, for example, in a polishing device and polishing conditions generally used for polishing an object to be polished made of single crystal ceramics or polycrystalline ceramics.
- a polishing device a general single-sided polishing device or double-sided polishing device can be used.
- a holder called a carrier is used to hold the object to be polished, and while supplying the polishing composition, a surface plate to which a polishing pad is attached is attached to one side of the object to be polished.
- One side of the object to be polished is polished by pressing it against the surface and rotating the surface plate.
- a carrier When polishing using a double-sided polishing device, a carrier is used to hold the object to be polished, and while supplying the polishing composition, a platen to which a polishing pad is attached is pressed against both sides of the object to be polished for polishing. Both sides of the object to be polished are polished by rotating the pad and the object to be polished in opposite directions. Regardless of which polishing device is used, the object to be polished is due to the physical action of friction between the polishing pad and the composition for polishing and the object to be polished, and the chemical action that the composition for polishing brings to the object to be polished. Is polished.
- the type of polishing pad is not particularly limited, and those having various physical properties such as material, thickness, and hardness can be used.
- Examples of the material of the polishing pad include polyurethane, epoxy resin, non-woven fabric, suede and the like.
- the polished surface to be polished in contact with the object to be polished preferably has a C hardness of 94 or more.
- the C hardness is the hardness immediately after the pressed surface is in close contact with the test method specified in Annex 2 “Spring hardness test type C test method” of JIS K7312: 1996.
- the pressure surface of the tester when the pressure surface of the tester is brought into close contact with the surface of the test piece, the distance at which the push needle protruding from the hole in the center of the pressure surface by the spring pressure is pushed back by the test piece.
- the structure shown on the scale as the hardness is used.
- the measuring surface of the test piece shall be at least larger than the pressurized surface of the testing machine. Further, it is preferable that the surface of the polishing pad has grooves such as a grid pattern. If the surface of the polishing pad has grooves, the smoothness of the surface to be polished of the object to be polished is improved.
- the surface roughness Ra of the polishing pad is preferably 0.75 ⁇ m or less, and more preferably 0.1 ⁇ m or less. When the surface roughness of the polishing pad is in this range, the variation in the thickness (TTV) of the object to be polished in the polishing batch is reduced.
- the method for reducing the surface roughness Ra of the polishing pad is not particularly limited, but a method of dressing between batches using a dresser containing abrasive grains such as diamond is preferable.
- the average particle size of the abrasive grains such as diamond contained in the dresser is preferably 10 ⁇ m or less, more preferably 5 ⁇ m or less, and most preferably 2 ⁇ m or less. When the average particle size of the dresser's abrasive grains is in this range, the variation in the thickness (TTV) of the object to be polished in the polishing batch is reduced.
- the supply amount of the polishing composition is not particularly limited, but 20 mL or more per minute is preferable, and 100 mL or more is more preferable. When the supply amount of the polishing composition is within this range, the smoothness of the surface to be polished of the object to be polished is improved.
- Example ⁇ Examples and comparative examples are shown below, and the present invention will be described in more detail.
- Abrasive grains made of colloidal silica and water were mixed to disperse the abrasive grains in water to produce polishing compositions of Examples 1 to 10 and Comparative Examples 1 to 7.
- the average secondary particle diameter of the abrasive grains used in each Example and Comparative Example and the content of the abrasive grains in the polishing composition are as shown in Table 1.
- the average secondary particle size of colloidal silica was measured using a laser diffraction / scattering type particle size distribution measuring device LA-950 manufactured by HORIBA, Ltd.
- the object to be polished is a plate-shaped member formed of a sintered body of a powder of translucent alumina, aluminum nitride, or silicon nitride, which is a polycrystalline ceramic.
- the polishing pad was dressed with a dresser containing diamond having a particle size of # 270 (53 ⁇ m), and the surface roughness Ra of the polishing pad was set to 1.1 ⁇ m. Then, the surface roughness Ra of the surface to be polished and the step (unevenness step of the crystal grain boundary portion) of the surface to be polished were measured, and the polishing speed was calculated.
- polishing conditions are as follows. Polishing device: Single-sided polishing device EJ-380IN manufactured by Engis (surface plate diameter 380 mm) Polishing pad: Epoxy resin polishing pad Polishing load: 29.4 kPa (300 gf / cm 2 ) Surface plate rotation speed: 110min -1 Polishing speed (linear speed): 84 m / min Polishing time: 30 minutes Supply speed of polishing composition: 20 mL / min
- the surface roughness Ra of the surface to be polished of the object to be polished after polishing was measured under the condition of a viewing angle of 143 ⁇ 107 ⁇ m using a measuring device NewView5032 manufactured by Zygo.
- the step on the surface to be polished of the object to be polished after polishing was measured as follows. That is, the step on the surface to be polished of the object to be polished after polishing was evaluated by the value of PV using a measuring device NewView5032 manufactured by Zygo.
- the PV value is a value indicating the maximum height and the maximum depth in the measurement range, but since the viewing angle (viewing angle 143 ⁇ 107 ⁇ m) this time is not affected by the swell, the maximum height is the remaining part of the crystal (the remaining part of the crystal (viewing angle 143 ⁇ 107 ⁇ m).
- the convex portion) and the maximum depth are the deciduous portions (concave portions) of the crystal, and the grain boundary step correlates with the PV value.
- silicon nitride the correlation between the PV value and the grain boundary step is low, and the grain boundary step cannot be accurately measured by this method, so the evaluation has not been performed.
- the polishing speed was calculated from the difference, the polishing time, and the area of the surface to be polished by measuring the mass of the object to be polished before and after polishing. These results are shown in Table 1 (the step of silicon nitride is shown as "ND").
- Comparative Examples 2 to 7 since the average secondary particle diameter of the abrasive grains exceeds 40 nm, the step of the surface to be polished of the object to be polished after polishing is large, and the object to be polished made of polycrystalline ceramics. The surface of the ceramic could not be polished smoothly. Since it is difficult to stably produce abrasive grains having an average secondary particle diameter of less than 5 nm, Comparative Example 1 could not be compared and examined.
- a dresser containing diamond having a grain size of # 270 (53 ⁇ m) was used as a dresser between polishing batches, and a dresser containing diamond having a grain size of 1 ⁇ m was used for dressing.
- the surface roughness Ra of the polishing pad was set to 0.05 ⁇ m and the polishing was performed in the same manner, the polishing was performed in the same manner as when the surface roughness Ra of the polishing pad was 1.1 ⁇ m and the dresser containing diamond having a grain size of # 270 (53 ⁇ m) was used.
- the variation in the thickness of the object to be polished (TTV) in the polishing batch was reduced to 60 to 80%.
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Abstract
The present invention provides a polishing composition which is capable of polishing the surface of a polycrystalline ceramic smooth. This polishing composition contains abrasive grains and water; and the average secondary particle diameter of the abrasive grains is from 5 nm to 40 nm. This polishing composition is used for polishing of a polishing object that contains a polycrystalline ceramic.
Description
本発明は研磨用組成物及び研磨方法に関する。
The present invention relates to a polishing composition and a polishing method.
近年、通信システムの発達に伴って様々な電子部品にセラミックスが使用されるようになっている。一般的に、電子部品用の基板は単結晶セラミックス(例えば単結晶サファイア)で形成されることが多いが、多結晶セラミックスで電子部品用の基板を形成すると、単結晶セラミックスに比べて、形状の自由度が高い、製造コストが低い、光学特性が優れる等の優位な性質が得られる場合がある。
In recent years, with the development of communication systems, ceramics have come to be used for various electronic components. Generally, the substrate for electronic parts is often formed of single crystal ceramics (for example, single crystal sapphire), but when the substrate for electronic parts is formed of polycrystalline ceramics, the shape is larger than that of single crystal ceramics. In some cases, advantageous properties such as high degree of freedom, low manufacturing cost, and excellent optical characteristics can be obtained.
多結晶セラミックスで電子部品用の基板を形成する際には、平滑な表面が求められる場合がある。しかしながら、多結晶セラミックスは、結晶粒界部分の凹凸段差を有するため、従来の研磨用組成物(例えば特許文献1を参照)を用いて研磨しても、十分に平滑な表面を得ることができない場合があった。
本発明は、多結晶セラミックスの表面を平滑に研磨することが可能な研磨用組成物及び研磨方法を提供することを課題とする。 When forming a substrate for electronic components from polycrystalline ceramics, a smooth surface may be required. However, since polycrystalline ceramics have uneven steps at the grain boundary portions, even if they are polished using a conventional polishing composition (see, for example, Patent Document 1), a sufficiently smooth surface cannot be obtained. There was a case.
An object of the present invention is to provide a polishing composition and a polishing method capable of smoothly polishing the surface of polycrystalline ceramics.
本発明は、多結晶セラミックスの表面を平滑に研磨することが可能な研磨用組成物及び研磨方法を提供することを課題とする。 When forming a substrate for electronic components from polycrystalline ceramics, a smooth surface may be required. However, since polycrystalline ceramics have uneven steps at the grain boundary portions, even if they are polished using a conventional polishing composition (see, for example, Patent Document 1), a sufficiently smooth surface cannot be obtained. There was a case.
An object of the present invention is to provide a polishing composition and a polishing method capable of smoothly polishing the surface of polycrystalline ceramics.
本発明の一態様に係る研磨用組成物は、多結晶セラミックスを含有する研磨対象物の研磨に使用される研磨用組成物であって、砥粒及び水を含有し、砥粒の平均2次粒子径が5nm以上40nm以下であることを要旨とする。
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、多結晶セラミックスを含有する研磨対象物を研磨することを要旨とする。 The polishing composition according to one aspect of the present invention is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water, and has an average secondary order of abrasive grains. The gist is that the particle size is 5 nm or more and 40 nm or less.
Further, the polishing method according to another aspect of the present invention is intended to polish an object to be polished containing polycrystalline ceramics by using the polishing composition according to the above one aspect.
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、多結晶セラミックスを含有する研磨対象物を研磨することを要旨とする。 The polishing composition according to one aspect of the present invention is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water, and has an average secondary order of abrasive grains. The gist is that the particle size is 5 nm or more and 40 nm or less.
Further, the polishing method according to another aspect of the present invention is intended to polish an object to be polished containing polycrystalline ceramics by using the polishing composition according to the above one aspect.
本発明によれば、多結晶セラミックスの表面を平滑に研磨することが可能である。
According to the present invention, it is possible to polish the surface of polycrystalline ceramics smoothly.
本発明の一実施形態について詳細に説明する。なお、以下の実施形態は本発明の一例を示したものであって、本発明は本実施形態に限定されるものではない。また、以下の実施形態には種々の変更又は改良を加えることが可能であり、その様な変更又は改良を加えた形態も本発明に含まれ得る。
An embodiment of the present invention will be described in detail. The following embodiments show an example of the present invention, and the present invention is not limited to the present embodiment. In addition, various changes or improvements can be added to the following embodiments, and the modified or improved embodiments may be included in the present invention.
本実施形態の研磨用組成物は、多結晶セラミックスを含有する研磨対象物の研磨に使用される研磨用組成物であって、砥粒及び水を含有する。本実施形態の研磨用組成物においては、砥粒の平均2次粒子径は5nm以上40nm以下である。
本実施形態の研磨方法は、上記本実施形態の研磨用組成物を用いて、多結晶セラミックスを含有する研磨対象物を研磨する方法である。 The polishing composition of the present embodiment is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water. In the polishing composition of the present embodiment, the average secondary particle diameter of the abrasive grains is 5 nm or more and 40 nm or less.
The polishing method of the present embodiment is a method of polishing an object to be polished containing polycrystalline ceramics by using the polishing composition of the present embodiment.
本実施形態の研磨方法は、上記本実施形態の研磨用組成物を用いて、多結晶セラミックスを含有する研磨対象物を研磨する方法である。 The polishing composition of the present embodiment is a polishing composition used for polishing an object to be polished containing polycrystalline ceramics, and contains abrasive grains and water. In the polishing composition of the present embodiment, the average secondary particle diameter of the abrasive grains is 5 nm or more and 40 nm or less.
The polishing method of the present embodiment is a method of polishing an object to be polished containing polycrystalline ceramics by using the polishing composition of the present embodiment.
多結晶セラミックスを含有する研磨対象物の研磨を上記本実施形態の研磨用組成物を用いて行えば、結晶粒界部分の凹凸段差を有する多結晶セラミックスの表面を、平滑に研磨することが可能である。
よって、例えば電子部品用の基板を多結晶セラミックスで形成する場合でも、表面を平滑にすることができ、単結晶セラミックスに比べて、形状の自由度が高い、製造コストが低い、光学特性が優れる等の優位な性質が得られる。 By polishing the object to be polished containing the polycrystalline ceramics using the polishing composition of the present embodiment, it is possible to smoothly polish the surface of the polycrystalline ceramics having uneven steps at the grain boundary portions. Is.
Therefore, for example, even when a substrate for electronic components is formed of polycrystalline ceramics, the surface can be smoothed, and the degree of freedom in shape is high, the manufacturing cost is low, and the optical characteristics are excellent as compared with single crystal ceramics. Etc. and other superior properties can be obtained.
よって、例えば電子部品用の基板を多結晶セラミックスで形成する場合でも、表面を平滑にすることができ、単結晶セラミックスに比べて、形状の自由度が高い、製造コストが低い、光学特性が優れる等の優位な性質が得られる。 By polishing the object to be polished containing the polycrystalline ceramics using the polishing composition of the present embodiment, it is possible to smoothly polish the surface of the polycrystalline ceramics having uneven steps at the grain boundary portions. Is.
Therefore, for example, even when a substrate for electronic components is formed of polycrystalline ceramics, the surface can be smoothed, and the degree of freedom in shape is high, the manufacturing cost is low, and the optical characteristics are excellent as compared with single crystal ceramics. Etc. and other superior properties can be obtained.
以下に、本実施形態の研磨用組成物及び研磨方法について詳細に説明する。
1.研磨対象物について
本実施形態の研磨用組成物及び研磨方法は、多結晶セラミックスを含有する研磨対象物の研磨に用いることができる。多結晶セラミックスは、結晶粒界部分の凹凸段差を有するため、研磨によって十分に平滑な表面を得られにくいが、本実施形態の研磨用組成物及び研磨方法を用いて研磨を行えば、十分に平滑な表面を得ることが可能である。 Hereinafter, the polishing composition and the polishing method of the present embodiment will be described in detail.
1. 1. About the object to be polished The polishing composition and the polishing method of the present embodiment can be used for polishing an object to be polished containing polycrystalline ceramics. Since polycrystalline ceramics have uneven steps at the grain boundaries, it is difficult to obtain a sufficiently smooth surface by polishing. However, polishing using the polishing composition and polishing method of the present embodiment is sufficient. It is possible to obtain a smooth surface.
1.研磨対象物について
本実施形態の研磨用組成物及び研磨方法は、多結晶セラミックスを含有する研磨対象物の研磨に用いることができる。多結晶セラミックスは、結晶粒界部分の凹凸段差を有するため、研磨によって十分に平滑な表面を得られにくいが、本実施形態の研磨用組成物及び研磨方法を用いて研磨を行えば、十分に平滑な表面を得ることが可能である。 Hereinafter, the polishing composition and the polishing method of the present embodiment will be described in detail.
1. 1. About the object to be polished The polishing composition and the polishing method of the present embodiment can be used for polishing an object to be polished containing polycrystalline ceramics. Since polycrystalline ceramics have uneven steps at the grain boundaries, it is difficult to obtain a sufficiently smooth surface by polishing. However, polishing using the polishing composition and polishing method of the present embodiment is sufficient. It is possible to obtain a smooth surface.
多結晶セラミックスの種類は特に限定されるものではないが、例えば、金属を含有する酸化物、金属を含有する窒化物、金属を含有する炭化物、金属を含有するホウ化物、金属を含有するフッ化物が挙げられ、これらの中でも金属を含有する酸化物、金属を含有する窒化物、金属を含有する炭化物が好ましい。
The types of polycrystalline ceramics are not particularly limited, but are, for example, metal-containing oxides, metal-containing nitrides, metal-containing carbides, metal-containing boroides, and metal-containing fluorides. Among these, oxides containing a metal, nitrides containing a metal, and carbides containing a metal are preferable.
金属を含有する酸化物、金属を含有する窒化物、金属を含有する炭化物の中でも、シリコンを含有する酸化物、シリコンを含有する窒化物、シリコンを含有する炭化物、アルミニウムを含有する酸化物、アルミニウムを含有する窒化物、イットリウムを含有する酸化物が好ましい。これらの多結晶セラミックスは、通信用デバイス、パワー半導体、通信用高周波デバイス、圧力センサー等の電子部品の基板として用いられる。上記基板は特に平滑な表面が求められる。
Among metal-containing oxides, metal-containing nitrides, and metal-containing carbides, silicon-containing oxides, silicon-containing nitrides, silicon-containing carbides, aluminum-containing oxides, and aluminum. A nitride containing the above, and an oxide containing ittrium are preferable. These polycrystalline ceramics are used as substrates for electronic components such as communication devices, power semiconductors, communication high frequency devices, and pressure sensors. The substrate is particularly required to have a smooth surface.
シリコンを含有する酸化物、シリコンを含有する窒化物、シリコンを含有する炭化物、アルミニウムを含有する酸化物、アルミニウムを含有する窒化物、イットリウムを含有する酸化物の中でも、特に、アルミニウムを含有する酸化物及びアルミニウムを含有する窒化物の少なくとも一方が好ましい。
Among the oxides containing silicon, the nitrides containing silicon, the carbides containing silicon, the oxides containing aluminum, the nitrides containing aluminum, and the oxides containing yttrium, the oxidation containing aluminum in particular. At least one of the material and the nitride containing aluminum is preferable.
具体例としては、シリコンを含有する酸化物として石英等の酸化ケイ素(SiO2)が挙げられ、シリコンを含有する窒化物として窒化ケイ素(SiN)が挙げられ、シリコンを含有する炭化物として炭化ケイ素(SiC)が挙げられる。また、アルミニウムを含有する酸化物として透光性アルミナ等のアルミナ(Al2O3)、スピネル(MgAl2O4)が挙げられ、アルミニウムを含有する窒化物として窒化アルミニウム(AlN)が挙げられ、イットリウムを含有する酸化物としてイットリア(Y2O3)、YAG(Y3Al5O12)が挙げられる。
Specific examples include silicon oxide (SiO 2 ) such as quartz as an oxide containing silicon, silicon nitride (SiN) as a nitride containing silicon, and silicon carbide (SiO 2) as a carbide containing silicon. SiC). Further, examples of the aluminum-containing oxide include alumina (Al 2 O 3 ) such as translucent alumina and spinel ( Mg Al 2 O 4 ), and examples of the aluminum-containing nitride include aluminum nitride (Al N). Examples of the oxide containing yttrium include ytria (Y 2 O 3 ) and YAG (Y 3 Al 5 O 12 ).
なお、研磨対象物は、多結晶セラミックスを含有するものであればよく、その全部が多結晶セラミックスで形成されていてもよいし、その一部分が多結晶セラミックスで形成されていてもよい。また、研磨対象物が含有する多結晶セラミックスの種類は、1種類であってもよいし、複数種であってもよい。研磨対象物の具体例としては、多結晶セラミックスの粉末の焼結体が挙げられる。
The object to be polished may be any one containing polycrystalline ceramics, and may be entirely formed of polycrystalline ceramics or a part thereof may be formed of polycrystalline ceramics. Further, the type of the polycrystalline ceramics contained in the object to be polished may be one kind or a plurality of kinds. Specific examples of the object to be polished include a sintered body of a powder of polycrystalline ceramics.
2.砥粒について
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(SiO2)やダイヤモンド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、沈降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、これらの砥粒の中でも、多結晶セラミックスの表面をより効率的に平滑化できるという観点から、コロイダルシリカが好ましい。 2. 2. Abrasive grains The type of abrasive grains contained in the polishing composition of the present embodiment is not particularly limited, but for example, abrasive grains containing silica (SiO 2 ) or diamond can be used. The type of silica is not particularly limited, and examples thereof include colloidal silica, fumed silica, sol-gel method silica, and precipitation method silica. These silicas may be used alone or in combination of two or more. Among these abrasive grains, colloidal silica is preferable from the viewpoint of more efficiently smoothing the surface of polycrystalline ceramics.
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(SiO2)やダイヤモンド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、沈降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、これらの砥粒の中でも、多結晶セラミックスの表面をより効率的に平滑化できるという観点から、コロイダルシリカが好ましい。 2. 2. Abrasive grains The type of abrasive grains contained in the polishing composition of the present embodiment is not particularly limited, but for example, abrasive grains containing silica (SiO 2 ) or diamond can be used. The type of silica is not particularly limited, and examples thereof include colloidal silica, fumed silica, sol-gel method silica, and precipitation method silica. These silicas may be used alone or in combination of two or more. Among these abrasive grains, colloidal silica is preferable from the viewpoint of more efficiently smoothing the surface of polycrystalline ceramics.
本実施形態の研磨用組成物に含有される砥粒の平均2次粒子径は、多結晶セラミックスの表面を十分に平滑に研磨するためには、5nm以上40nm以下とする必要があるが、7nm以上35nm以下とすることが好ましい。
従来、単結晶セラミックスを研磨する際には、容易に単結晶セラミックスの表面を十分に平滑に研磨することができるため、平均2次粒子径が特定粒径よりも大きい砥粒(平均2次粒子径が40nmよりも大きい砥粒)を用いていたが、結晶粒界を有する多結晶セラミックスを研磨する際には平均2次粒子径が特定粒径よりも小さい砥粒(平均2次粒子径が5nm以上40nm以下である砥粒)を用いることが重要である。 The average secondary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment needs to be 5 nm or more and 40 nm or less in order to sufficiently smooth the surface of the polycrystalline ceramics, but is 7 nm. It is preferably 35 nm or less.
Conventionally, when polishing single crystal ceramics, the surface of the single crystal ceramics can be easily sufficiently smoothed, so that the average secondary particle size is larger than the specific particle size (average secondary particles). Abrasive particles with a diameter larger than 40 nm) were used, but when polishing polycrystalline ceramics with crystal grain boundaries, the average secondary particle size is smaller than the specific particle size (average secondary particle size). It is important to use abrasive particles (abrasive particles of 5 nm or more and 40 nm or less).
従来、単結晶セラミックスを研磨する際には、容易に単結晶セラミックスの表面を十分に平滑に研磨することができるため、平均2次粒子径が特定粒径よりも大きい砥粒(平均2次粒子径が40nmよりも大きい砥粒)を用いていたが、結晶粒界を有する多結晶セラミックスを研磨する際には平均2次粒子径が特定粒径よりも小さい砥粒(平均2次粒子径が5nm以上40nm以下である砥粒)を用いることが重要である。 The average secondary particle diameter of the abrasive grains contained in the polishing composition of the present embodiment needs to be 5 nm or more and 40 nm or less in order to sufficiently smooth the surface of the polycrystalline ceramics, but is 7 nm. It is preferably 35 nm or less.
Conventionally, when polishing single crystal ceramics, the surface of the single crystal ceramics can be easily sufficiently smoothed, so that the average secondary particle size is larger than the specific particle size (average secondary particles). Abrasive particles with a diameter larger than 40 nm) were used, but when polishing polycrystalline ceramics with crystal grain boundaries, the average secondary particle size is smaller than the specific particle size (average secondary particle size). It is important to use abrasive particles (abrasive particles of 5 nm or more and 40 nm or less).
平均2次粒子径が特定粒径よりも大きい砥粒を用いると、結晶粒界の凸部と凹部を同時に加工するため、粒界段差を埋めることができず十分に平滑な表面を得ることができないが、平均2次粒子径が特定粒径よりも小さい砥粒を用いると、粒界段差の凹部に砥粒が接触せず凸部のみ加工が進むため、粒界段差がなくなり十分に平滑な表面を得ることができる。
なお、砥粒の平均2次粒子径は、例えば、レーザー回折/散乱式粒子径分布測定装置(例えば、株式会社堀場製作所製の“LA-950”)を用いて測定することができる。 If abrasive grains with an average secondary grain size larger than the specific grain size are used, the convex and concave portions of the grain boundaries are processed at the same time, so it is not possible to fill the grain boundary steps and a sufficiently smooth surface can be obtained. However, if abrasive grains with an average secondary particle size smaller than the specific grain size are used, the abrasive grains do not come into contact with the concave portions of the grain boundary steps and only the convex portions are processed, so that the grain boundary steps are eliminated and the grain boundaries are sufficiently smooth. The surface can be obtained.
The average secondary particle size of the abrasive grains can be measured using, for example, a laser diffraction / scattering type particle size distribution measuring device (for example, "LA-950" manufactured by HORIBA, Ltd.).
なお、砥粒の平均2次粒子径は、例えば、レーザー回折/散乱式粒子径分布測定装置(例えば、株式会社堀場製作所製の“LA-950”)を用いて測定することができる。 If abrasive grains with an average secondary grain size larger than the specific grain size are used, the convex and concave portions of the grain boundaries are processed at the same time, so it is not possible to fill the grain boundary steps and a sufficiently smooth surface can be obtained. However, if abrasive grains with an average secondary particle size smaller than the specific grain size are used, the abrasive grains do not come into contact with the concave portions of the grain boundary steps and only the convex portions are processed, so that the grain boundary steps are eliminated and the grain boundaries are sufficiently smooth. The surface can be obtained.
The average secondary particle size of the abrasive grains can be measured using, for example, a laser diffraction / scattering type particle size distribution measuring device (for example, "LA-950" manufactured by HORIBA, Ltd.).
また、本実施形態の研磨用組成物中の砥粒の含有量は特に限定されるものではないが、1質量%以上30質量%以下とすることが好ましく、3質量%以上25質量%以下とすることがより好ましい。砥粒の含有量が上記範囲内にある研磨用組成物を使用することによって、多結晶セラミックスの表面をより平滑に研磨することができる。
The content of the abrasive grains in the polishing composition of the present embodiment is not particularly limited, but is preferably 1% by mass or more and 30% by mass or less, and is preferably 3% by mass or more and 25% by mass or less. It is more preferable to do so. By using a polishing composition having an abrasive grain content within the above range, the surface of the polycrystalline ceramic can be polished more smoothly.
3.研磨用組成物について
本実施形態の研磨用組成物は、上記砥粒及び水を含有するスラリーである。水は、砥粒を分散させ且つ他の成分を分散又は溶解する分散媒又は溶媒として機能する。なお、水と有機溶剤の混合物を分散媒又は溶媒として用いてもよい。使用する水は、上記他の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、又は蒸留水が好ましい。 3. 3. About the polishing composition The polishing composition of the present embodiment is a slurry containing the above-mentioned abrasive grains and water. Water functions as a dispersion medium or solvent that disperses abrasive grains and disperses or dissolves other components. A mixture of water and an organic solvent may be used as a dispersion medium or a solvent. The water used is preferably water containing as little impurities as possible from the viewpoint of suppressing the inhibition of the action of the above other components. Specifically, pure water, ultrapure water, or distilled water from which foreign substances have been removed through a filter after removing impurity ions with an ion exchange resin is preferable.
本実施形態の研磨用組成物は、上記砥粒及び水を含有するスラリーである。水は、砥粒を分散させ且つ他の成分を分散又は溶解する分散媒又は溶媒として機能する。なお、水と有機溶剤の混合物を分散媒又は溶媒として用いてもよい。使用する水は、上記他の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、又は蒸留水が好ましい。 3. 3. About the polishing composition The polishing composition of the present embodiment is a slurry containing the above-mentioned abrasive grains and water. Water functions as a dispersion medium or solvent that disperses abrasive grains and disperses or dissolves other components. A mixture of water and an organic solvent may be used as a dispersion medium or a solvent. The water used is preferably water containing as little impurities as possible from the viewpoint of suppressing the inhibition of the action of the above other components. Specifically, pure water, ultrapure water, or distilled water from which foreign substances have been removed through a filter after removing impurity ions with an ion exchange resin is preferable.
本実施形態の研磨用組成物のpHは特に限定されるものではないが、1.5以上9.0以下とすることが好ましく、2.0以上8.5以下とすることがより好ましい。pHが上記範囲内にある研磨用組成物を使用することによって、多結晶セラミックスの表面をより平滑に研磨することができる。本実施形態の研磨用組成物のpHの調整は、添加剤であるpH調整剤によって行ってもよい。pH調整剤は、1種を単独で用いてもよいし、2種以上を混合しても用いてもよい。
The pH of the polishing composition of the present embodiment is not particularly limited, but is preferably 1.5 or more and 9.0 or less, and more preferably 2.0 or more and 8.5 or less. By using a polishing composition having a pH within the above range, the surface of the polycrystalline ceramic can be polished more smoothly. The pH of the polishing composition of the present embodiment may be adjusted by an additive pH adjuster. As the pH adjuster, one type may be used alone, or two or more types may be mixed or used.
本実施形態の研磨用組成物は、砥粒及び水の他、上記他の成分である添加剤(例えばpH調整剤)を所望により含有していてもよい。
pH調整剤としては、公知の酸、塩基、又はそれらの塩を使用することができる。pH調整剤として使用できる酸の具体例としては、塩酸、硫酸、硝酸、フッ酸、ホウ酸、炭酸、次亜リン酸、亜リン酸、及びリン酸等の無機酸や、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2-メチル酪酸、n-ヘキサン酸、3,3-ジメチル酪酸、2-エチル酪酸、4-メチルペンタン酸、n-ヘプタン酸、2-メチルヘキサン酸、n-オクタン酸、2-エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、リンゴ酸、酒石酸、クエン酸、乳酸、ジグリコール酸、2-フランカルボン酸、2,5-フランジカルボン酸、3-フランカルボン酸、2-テトラヒドロフランカルボン酸、メトキシ酢酸、メトキシフェニル酢酸、及びフェノキシ酢酸等の有機酸が挙げられる。 In addition to the abrasive grains and water, the polishing composition of the present embodiment may optionally contain an additive (for example, a pH adjuster) which is the above-mentioned other component.
As the pH adjuster, known acids, bases, or salts thereof can be used. Specific examples of acids that can be used as a pH adjuster include inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, boric acid, carbonic acid, hypophobic acid, phobic acid, and phosphoric acid, and formic acid, acetic acid, and propion. 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, pimelli acid, maleic acid, phthalic acid, malic acid, tartrate acid, citric acid, Examples thereof include organic acids such as lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetratetracarboxylic acid, methoxyacetic acid, methoxyphenylacetic acid, and phenoxyacetic acid.
pH調整剤としては、公知の酸、塩基、又はそれらの塩を使用することができる。pH調整剤として使用できる酸の具体例としては、塩酸、硫酸、硝酸、フッ酸、ホウ酸、炭酸、次亜リン酸、亜リン酸、及びリン酸等の無機酸や、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2-メチル酪酸、n-ヘキサン酸、3,3-ジメチル酪酸、2-エチル酪酸、4-メチルペンタン酸、n-ヘプタン酸、2-メチルヘキサン酸、n-オクタン酸、2-エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、リンゴ酸、酒石酸、クエン酸、乳酸、ジグリコール酸、2-フランカルボン酸、2,5-フランジカルボン酸、3-フランカルボン酸、2-テトラヒドロフランカルボン酸、メトキシ酢酸、メトキシフェニル酢酸、及びフェノキシ酢酸等の有機酸が挙げられる。 In addition to the abrasive grains and water, the polishing composition of the present embodiment may optionally contain an additive (for example, a pH adjuster) which is the above-mentioned other component.
As the pH adjuster, known acids, bases, or salts thereof can be used. Specific examples of acids that can be used as a pH adjuster include inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, hydrofluoric acid, boric acid, carbonic acid, hypophobic acid, phobic acid, and phosphoric acid, and formic acid, acetic acid, and propion. 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, pimelli acid, maleic acid, phthalic acid, malic acid, tartrate acid, citric acid, Examples thereof include organic acids such as lactic acid, diglycolic acid, 2-furancarboxylic acid, 2,5-furandicarboxylic acid, 3-furancarboxylic acid, 2-tetratetracarboxylic acid, methoxyacetic acid, methoxyphenylacetic acid, and phenoxyacetic acid.
pH調整剤として無機酸を使用する場合は、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、pH調整剤として有機酸を使用する場合は、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、及びイタコン酸等が好ましい。
When an inorganic acid is used as the pH adjuster, sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid and the like are preferable from the viewpoint of improving the polishing speed, and when an organic acid is used as the pH adjuster, glycolic acid, succinic acid, maleic acid and the like are preferable. , Citric acid, tartrate acid, malic acid, gluconic acid, itaconic acid and the like are preferable.
pH調整剤として使用できる塩基としては、脂肪族アミン、芳香族アミン等のアミン、水酸化第四アンモニウム等の有機塩基、水酸化カリウム等のアルカリ金属の水酸化物、アルカリ土類金属の水酸化物、及びアンモニア等が挙げられる。これらの塩基の中でも、入手容易性から水酸化カリウム、アンモニアが好ましい。
Bases that can be used as a pH adjuster include amines such as aliphatic amines and aromatic amines, organic bases such as tetraammonium hydroxide, hydroxides of alkali metals such as potassium hydroxide, and hydroxylation of alkaline earth metals. Things, ammonia and the like can be mentioned. Among these bases, potassium hydroxide and ammonia are preferable because of their availability.
また、前記の酸の代わりに、又は前記の酸と組み合わせて、前記酸のアンモニウム塩やアルカリ金属塩等の塩をpH調整剤として用いてもよい。特に、弱酸と強塩基の塩、強酸と弱塩基の塩、又は弱酸と弱塩基の塩の場合には、pHの緩衝作用を期待することができ、さらに強酸と強塩基の塩の場合には、少量で、pHだけでなく電導度の調整が可能である。
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。 Further, a salt such as an ammonium salt or an alkali metal salt of the acid may be used as a pH adjuster in place of the acid or in combination with the acid. In particular, in the case of 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, a pH buffering action can be expected, and in the case of a salt of a strong acid and a strong base, a buffering action of pH can be expected. With a small amount, it is possible to adjust not only the pH but also the conductivity.
The amount of the pH adjuster added is not particularly limited, and the pH may be appropriately adjusted so that the polishing composition has a desired pH.
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。 Further, a salt such as an ammonium salt or an alkali metal salt of the acid may be used as a pH adjuster in place of the acid or in combination with the acid. In particular, in the case of 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, a pH buffering action can be expected, and in the case of a salt of a strong acid and a strong base, a buffering action of pH can be expected. With a small amount, it is possible to adjust not only the pH but also the conductivity.
The amount of the pH adjuster added is not particularly limited, and the pH may be appropriately adjusted so that the polishing composition has a desired pH.
本実施形態の研磨用組成物は、必要に応じて、pH調整剤以外の添加剤をさらに含有してもよいが、多結晶セラミックスの表面をより平滑に研磨するという観点からは、pH調整剤以外の添加剤を含有しないことが好ましい。例えば、研磨用組成物は、錯化剤、エッチング剤、酸化剤等の研磨速度をさらに高める作用を有する添加剤を含有してもよい。また、研磨用組成物は、研磨対象物の表面や砥粒の表面に作用する水溶性重合体(共重合体やその塩、誘導体でもよい)を含有してもよい。さらに、研磨用組成物は、砥粒の分散性を向上させる分散剤や砥粒の凝集体の再分散を容易にする分散助剤のような添加剤を含有してもよい。さらに、研磨用組成物は、防腐剤、防黴剤、防錆剤のような公知の添加剤を含有してもよい。
The polishing composition of the present embodiment may further contain an additive other than the pH adjuster, if necessary, but from the viewpoint of polishing the surface of the polycrystalline ceramic more smoothly, the pH adjuster. It is preferable that it does not contain any additives other than. For example, the polishing composition may contain additives such as a complexing agent, an etching agent, and an oxidizing agent, which have an effect of further increasing the polishing rate. Further, the polishing composition may contain a water-soluble polymer (a copolymer, a salt thereof, or a derivative thereof) that acts on the surface of the object to be polished or the surface of the abrasive grains. Further, the polishing composition may contain additives such as a dispersant that improves the dispersibility of the abrasive grains and a dispersion aid that facilitates the redispersion of the aggregates of the abrasive grains. Further, the polishing composition may contain known additives such as preservatives, fungicides and rust inhibitors.
これらの各種添加剤は、研磨用組成物において通常添加できるものとして、多くの特許文献等において公知であり、添加剤の種類及び添加量は特に限定されるものではない。ただし、これらの添加剤を添加する場合の添加量は、研磨用組成物全体に対して、それぞれ1質量%未満であることが好ましく、それぞれ0.5質量%未満であることがより好ましい。これらの添加剤は、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。
These various additives are known in many patent documents and the like as those that can be usually added in a polishing composition, and the type and amount of the additives are not particularly limited. However, when these additives are added, the amount added is preferably less than 1% by mass, and more preferably less than 0.5% by mass, respectively, with respect to the entire polishing composition. These additives may be used alone or in combination of two or more.
錯化剤の例としては、無機酸、有機酸、アミノ酸、ニトリル化合物、及びキレート剤等が挙げられる。無機酸の具体例としては、硫酸、硝酸、ホウ酸、炭酸等が挙げられる。有機酸の具体例としては、ギ酸、酢酸、プロピオン酸、酪酸、吉草酸、2-メチル酪酸、n-ヘキサン酸、3,3-ジメチル酪酸、2-エチル酪酸、4-メチルペンタン酸、n-ヘプタン酸、2-メチルヘキサン酸、n-オクタン酸、2-エチルヘキサン酸、安息香酸、グリコール酸、サリチル酸、グリセリン酸、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、マレイン酸、フタル酸、リンゴ酸、酒石酸、クエン酸、乳酸等が挙げられる。メタンスルホン酸、エタンスルホン酸、及びイセチオン酸等の有機硫酸も使用可能である。無機酸又は有機酸の代わりにあるいは無機酸又は有機酸と組み合わせて、無機酸又は有機酸のアルカリ金属塩等の塩を用いてもよい。これらの錯化剤の中でもグリシン、アラニン、リンゴ酸、酒石酸、クエン酸、グリコール酸、イセチオン酸、又はそれらの塩が好ましい。
Examples of complexing agents include inorganic acids, organic acids, amino acids, nitrile compounds, chelating agents and the like. Specific examples of the inorganic acid include sulfuric acid, nitric acid, boric acid, carbonic acid and the like. Specific examples of organic acids 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, malein Examples thereof include acid, phthalic acid, malic acid, tartrate acid, citric acid, lactic acid and the like. Organic sulfuric acids such as methanesulfonic acid, ethanesulfonic acid, and isethionic acid can also be used. Salts such as alkali metal salts of inorganic or organic acids may be used in place of or in combination with the inorganic or organic acids. Among these complexing agents, glycine, alanine, malic acid, tartaric acid, citric acid, glycolic acid, isethionic acid, or salts thereof are preferable.
キレート剤の例としては、グルコン酸等のカルボン酸系キレート剤や、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や、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があげられる。また、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や、フェノール誘導体や、1,3-ジケトン等も、キレート剤の例として挙げることができる。
Examples of chelating agents include carboxylic acid-based chelating agents such as gluconic acid, amine-based chelating agents such as ethylenediamine, diethylenetriamine, and trimethyltetraamine, ethylenediaminetetraacetic acid, nitrilotriacetic acid, hydroxyethylethylenediaminetriacetic acid, and triethylenetetramine. Examples thereof include polyaminopolycarboxylic acid-based chelating agents such as hexaacetic acid and diethylenetriaminepentaacetic acid. In addition, 2-aminoethylphosphonic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, aminotri (methylenephosphonic acid), ethylenediaminetetrakis (methylenephosphonic acid), diethylenetriaminepenta (methylenephosphonic acid), ethane-1,1- Organic phosphonic acid-based chelating agents such as diphosphonic acid, ethane-1,1,2-triphosphonic acid, methanehydroxyphosphonic acid, 1-phosphonobutane-2,3,4-tricarboxylic acid, phenol derivatives, 1,3-diketone Etc. can also be mentioned as an example of a chelating agent.
エッチング剤の例としては、硝酸、硫酸、塩酸、リン酸、フッ酸等の無機酸や、酢酸、クエン酸、酒石酸、メタンスルホン酸等の有機酸や、水酸化カリウム、水酸化ナトリウム、アンモニア等の無機アルカリや、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挙げられる。
酸化剤の例としては、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、過マンガン酸カリウム等が挙げられる。 Examples of etching agents include inorganic acids such as nitrate, sulfuric acid, hydrochloric acid, phosphoric acid and hydrofluoric acid, organic acids such as acetic acid, citric acid, tartaric acid and methanesulfonic acid, potassium hydroxide, sodium hydroxide and ammonia. Examples thereof include inorganic alkalis such as amines and organic alkalis such as quaternary ammonium hydroxide.
Examples of the oxidizing agent include hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchlorate, persulfate, nitric acid, potassium permanganate and the like.
酸化剤の例としては、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、過マンガン酸カリウム等が挙げられる。 Examples of etching agents include inorganic acids such as nitrate, sulfuric acid, hydrochloric acid, phosphoric acid and hydrofluoric acid, organic acids such as acetic acid, citric acid, tartaric acid and methanesulfonic acid, potassium hydroxide, sodium hydroxide and ammonia. Examples thereof include inorganic alkalis such as amines and organic alkalis such as quaternary ammonium hydroxide.
Examples of the oxidizing agent include hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchlorate, persulfate, nitric acid, potassium permanganate and the like.
水溶性重合体(共重合体やその塩、誘導体でもよい)の例としては、ポリアクリル酸塩等のポリカルボン酸や、ポリホスホン酸や、ポリスチレンスルホン酸等のポリスルホン酸や、キタンサンガム、アルギン酸ナトリウム等の多糖類や、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が挙げられる。また、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も、水溶性重合体の例として挙げることができる。
Examples of water-soluble polymers (may be copolymers, salts thereof, derivatives) include polycarboxylic acids such as polyacrylates, polyphosphonic acids, polysulfonic acids such as polystyrene sulfonic acid, chitansan gum, sodium alginate and the like. Examples thereof include the polysaccharides of the above, and cellulose derivatives such as hydroxyethyl cellulose and carboxymethyl cellulose. Further, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, sorbitan monooleate, an oxyalkylene polymer having a single type or a plurality of types of oxyalkylene units, and the like can also be mentioned as examples of the water-soluble polymer.
分散助剤の例としては、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挙げられる。防腐剤の例としては、次亜塩素酸ナトリウム等が挙げられる。防黴剤の例としては、オキサゾリジン-2,5-ジオン等のオキサゾリン等が挙げられる。
防食剤の例としては、界面活性剤、アルコール類、高分子、樹脂、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、安息香酸等が挙げられる。 Examples of the dispersion aid include pyrophosphate, condensed phosphate such as hexamethaphosphate, and the like. Examples of preservatives include sodium hypochlorite and the like. Examples of antifungal agents include oxazolines such as oxazolidine-2,5-dione.
Examples of the anticorrosive agent include surfactants, alcohols, polymers, resins, amines, pyridines, tetraphenylphosphonium salts, benzotriazoles, triazoles, tetrazole, benzoic acid and the like.
防食剤の例としては、界面活性剤、アルコール類、高分子、樹脂、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、安息香酸等が挙げられる。 Examples of the dispersion aid include pyrophosphate, condensed phosphate such as hexamethaphosphate, and the like. Examples of preservatives include sodium hypochlorite and the like. Examples of antifungal agents include oxazolines such as oxazolidine-2,5-dione.
Examples of the anticorrosive agent include surfactants, alcohols, polymers, resins, amines, pyridines, tetraphenylphosphonium salts, benzotriazoles, triazoles, tetrazole, benzoic acid and the like.
界面活性剤としては、ノニオン性界面活性剤、アニオン性界面活性剤、カチオン性界面活性剤、両性界面活性剤が挙げられる。ノニオン性界面活性剤としては、エーテル型、エーテルエステル型、エステル型、含窒素型が挙げられ、アニオン性界面活性剤としては、カルボン酸塩、スルホン酸塩、硫酸エステル塩、リン酸エステル塩が挙げられる。また、カチオン性界面活性剤としては、脂肪族アミン塩、脂肪族四級アンモニウム塩、塩化ベンザルコニウム塩、塩化ベンゼトニウム、ピリジニウム塩、イミダゾリニウム塩が挙げられ、両性界面活性剤としては、カルボキシベタイン型、アミノカルボン酸塩、イミダゾリニウムベタイン、レシチン、アルキルアミンオキサイドが挙げられる。
Examples of the surfactant include a nonionic surfactant, an anionic surfactant, a cationic surfactant, and an amphoteric surfactant. Examples of the nonionic surfactant include ether type, ether ester type, ester type and nitrogen-containing type, and examples of the anionic surfactant include carboxylate, sulfonate, sulfate ester and phosphoric acid ester salt. Can be mentioned. Examples of the cationic surfactant include an aliphatic amine salt, an aliphatic quaternary ammonium salt, a benzalkonium chloride salt, a benzethonium chloride, a pyridinium salt and an imidazolinium salt, and examples of the amphoteric surfactant include carboxy. Examples thereof include betaine type, aminocarboxylate, imidazolinium betaine, lecithin, and alkylamine oxide.
4.研磨用組成物の製造方法について
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、水中で撹拌、混合することによって製造することができる。各成分を混合する際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。 4. About the manufacturing method of the polishing composition The manufacturing method of the polishing composition of this embodiment is not particularly limited, and it is manufactured by stirring and mixing abrasive grains and various additives in water, if desired. be able to. The temperature at which each component is mixed is not particularly limited, but is preferably 10 ° C. or higher and 40 ° C. or lower, and may be heated in order to improve the dissolution rate. Further, the mixing time is not particularly limited.
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、水中で撹拌、混合することによって製造することができる。各成分を混合する際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。 4. About the manufacturing method of the polishing composition The manufacturing method of the polishing composition of this embodiment is not particularly limited, and it is manufactured by stirring and mixing abrasive grains and various additives in water, if desired. be able to. The temperature at which each component is mixed is not particularly limited, but is preferably 10 ° C. or higher and 40 ° C. or lower, and may be heated in order to improve the dissolution rate. Further, the mixing time is not particularly limited.
本実施形態の研磨用組成物は、一剤型であってもよいし、研磨用組成物の成分の一部又は全部を任意の比率で混合した二剤型以上の多剤型であってもよい。また、本実施形態の研磨用組成物は、研磨用組成物の原液を水で例えば10倍以上に希釈することにより調製されてもよい。研磨用組成物が二剤型である場合には、研磨用組成物の原料となる二つの原料組成物の混合と希釈の順序は任意である。例えば、一方の原料組成物を水で希釈した後、他方の原料組成物と混合してもよいし、両方の原料組成物の混合と水での希釈を同時に行ってもよいし、あるいは、両方の原料組成物を混合した後に水で希釈してもよい。
The polishing composition of the present embodiment may be a one-dosage form, or may be a two-dosage form or a multi-dosage form in which a part or all of the components of the polishing composition are mixed at an arbitrary ratio. good. Further, the polishing composition of the present embodiment may be prepared by diluting the undiluted solution of the polishing composition with water, for example, 10 times or more. When the polishing composition is a two-dosage form, the order of mixing and diluting the two raw material compositions which are the raw materials of the polishing composition is arbitrary. For example, one raw material composition may be diluted with water and then mixed with the other raw material composition, both raw material compositions may be mixed and diluted with water at the same time, or both. The raw material composition of the above may be mixed and then diluted with water.
5.研磨装置及び研磨方法について
本実施形態の研磨用組成物は、例えば、単結晶セラミックスや多結晶セラミックスからなる研磨対象物の研磨で一般的に用いられる研磨装置及び研磨条件で使用することができる。研磨装置としては、一般的な片面研磨装置や両面研磨装置が使用可能である。
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研磨対象物を保持し、研磨用組成物を供給しながら、研磨パッドが貼付された定盤を研磨対象物の片面に押しつけ、定盤を回転させることにより研磨対象物の片面を研磨する。 5. Polishing device and polishing method The polishing composition of the present embodiment can be used, for example, in a polishing device and polishing conditions generally used for polishing an object to be polished made of single crystal ceramics or polycrystalline ceramics. As the polishing device, a general single-sided polishing device or double-sided polishing device can be used.
When polishing using a single-sided polishing device, a holder called a carrier is used to hold the object to be polished, and while supplying the polishing composition, a surface plate to which a polishing pad is attached is attached to one side of the object to be polished. One side of the object to be polished is polished by pressing it against the surface and rotating the surface plate.
本実施形態の研磨用組成物は、例えば、単結晶セラミックスや多結晶セラミックスからなる研磨対象物の研磨で一般的に用いられる研磨装置及び研磨条件で使用することができる。研磨装置としては、一般的な片面研磨装置や両面研磨装置が使用可能である。
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研磨対象物を保持し、研磨用組成物を供給しながら、研磨パッドが貼付された定盤を研磨対象物の片面に押しつけ、定盤を回転させることにより研磨対象物の片面を研磨する。 5. Polishing device and polishing method The polishing composition of the present embodiment can be used, for example, in a polishing device and polishing conditions generally used for polishing an object to be polished made of single crystal ceramics or polycrystalline ceramics. As the polishing device, a general single-sided polishing device or double-sided polishing device can be used.
When polishing using a single-sided polishing device, a holder called a carrier is used to hold the object to be polished, and while supplying the polishing composition, a surface plate to which a polishing pad is attached is attached to one side of the object to be polished. One side of the object to be polished is polished by pressing it against the surface and rotating the surface plate.
両面研磨装置を用いて研磨する場合には、キャリアを用いて研磨対象物を保持し、研磨用組成物を供給しながら、研磨パッドが貼付された定盤を研磨対象物の両面に押しつけ、研磨パッドと研磨対象物を相反する方向に回転させることにより研磨対象物の両面を研磨する。
いずれの研磨装置を用いた場合でも、研磨パッド及び研磨用組成物と研磨対象物との間の摩擦による物理的作用と、研磨用組成物が研磨対象物にもたらす化学的作用によって、研磨対象物は研磨される。 When polishing using a double-sided polishing device, a carrier is used to hold the object to be polished, and while supplying the polishing composition, a platen to which a polishing pad is attached is pressed against both sides of the object to be polished for polishing. Both sides of the object to be polished are polished by rotating the pad and the object to be polished in opposite directions.
Regardless of which polishing device is used, the object to be polished is due to the physical action of friction between the polishing pad and the composition for polishing and the object to be polished, and the chemical action that the composition for polishing brings to the object to be polished. Is polished.
いずれの研磨装置を用いた場合でも、研磨パッド及び研磨用組成物と研磨対象物との間の摩擦による物理的作用と、研磨用組成物が研磨対象物にもたらす化学的作用によって、研磨対象物は研磨される。 When polishing using a double-sided polishing device, a carrier is used to hold the object to be polished, and while supplying the polishing composition, a platen to which a polishing pad is attached is pressed against both sides of the object to be polished for polishing. Both sides of the object to be polished are polished by rotating the pad and the object to be polished in opposite directions.
Regardless of which polishing device is used, the object to be polished is due to the physical action of friction between the polishing pad and the composition for polishing and the object to be polished, and the chemical action that the composition for polishing brings to the object to be polished. Is polished.
研磨パッドの種類は特に限定されるものではなく、材質、厚さ、硬度等の物性が種々異なるものを用いることができる。研磨パッドの材質としては、例えば、ポリウレタン、エポキシ樹脂、不織布、スウェード等が挙げられる。
研磨パッドの表面のうち、研磨対象物に接触して研磨を行う研磨面は、C硬度が94以上であることが好ましい。C硬度とは、JIS K7312:1996の付属書2「スプリング硬さ試験タイプC試験方法」で規定された試験方法による、加圧面が密着した直後の硬さである。この試験方法では、スプリング硬さ試験機として、試験片の表面に試験機の加圧面を密着させたとき、加圧面の中心の孔からばね圧力で突き出ている押針が試験片によって押し戻される距離を、硬さとして目盛に示す構造のものを用いる。試験片の測定面は、少なくとも試験機の加圧面以上の大きさのものとする。
また、研磨パッドの表面には格子状などの溝が入っていることが好ましい。研磨パッドの表面に溝が入っていると、研磨対象物の被研磨面の平滑性が向上する。 The type of polishing pad is not particularly limited, and those having various physical properties such as material, thickness, and hardness can be used. Examples of the material of the polishing pad include polyurethane, epoxy resin, non-woven fabric, suede and the like.
Of the surface of the polishing pad, the polished surface to be polished in contact with the object to be polished preferably has a C hardness of 94 or more. The C hardness is the hardness immediately after the pressed surface is in close contact with the test method specified in Annex 2 “Spring hardness test type C test method” of JIS K7312: 1996. In this test method, as a spring hardness tester, when the pressure surface of the tester is brought into close contact with the surface of the test piece, the distance at which the push needle protruding from the hole in the center of the pressure surface by the spring pressure is pushed back by the test piece. , The structure shown on the scale as the hardness is used. The measuring surface of the test piece shall be at least larger than the pressurized surface of the testing machine.
Further, it is preferable that the surface of the polishing pad has grooves such as a grid pattern. If the surface of the polishing pad has grooves, the smoothness of the surface to be polished of the object to be polished is improved.
研磨パッドの表面のうち、研磨対象物に接触して研磨を行う研磨面は、C硬度が94以上であることが好ましい。C硬度とは、JIS K7312:1996の付属書2「スプリング硬さ試験タイプC試験方法」で規定された試験方法による、加圧面が密着した直後の硬さである。この試験方法では、スプリング硬さ試験機として、試験片の表面に試験機の加圧面を密着させたとき、加圧面の中心の孔からばね圧力で突き出ている押針が試験片によって押し戻される距離を、硬さとして目盛に示す構造のものを用いる。試験片の測定面は、少なくとも試験機の加圧面以上の大きさのものとする。
また、研磨パッドの表面には格子状などの溝が入っていることが好ましい。研磨パッドの表面に溝が入っていると、研磨対象物の被研磨面の平滑性が向上する。 The type of polishing pad is not particularly limited, and those having various physical properties such as material, thickness, and hardness can be used. Examples of the material of the polishing pad include polyurethane, epoxy resin, non-woven fabric, suede and the like.
Of the surface of the polishing pad, the polished surface to be polished in contact with the object to be polished preferably has a C hardness of 94 or more. The C hardness is the hardness immediately after the pressed surface is in close contact with the test method specified in Annex 2 “Spring hardness test type C test method” of JIS K7312: 1996. In this test method, as a spring hardness tester, when the pressure surface of the tester is brought into close contact with the surface of the test piece, the distance at which the push needle protruding from the hole in the center of the pressure surface by the spring pressure is pushed back by the test piece. , The structure shown on the scale as the hardness is used. The measuring surface of the test piece shall be at least larger than the pressurized surface of the testing machine.
Further, it is preferable that the surface of the polishing pad has grooves such as a grid pattern. If the surface of the polishing pad has grooves, the smoothness of the surface to be polished of the object to be polished is improved.
研磨パッドは、表面粗さRaが0.75μm以下であると好ましく、0.1μm以下であるとより好ましい。研磨パッドの表面粗さがこの範囲であると、研磨バッチ内の研磨対象物の厚さのバラつき(TTV)が低減する。
The surface roughness Ra of the polishing pad is preferably 0.75 μm or less, and more preferably 0.1 μm or less. When the surface roughness of the polishing pad is in this range, the variation in the thickness (TTV) of the object to be polished in the polishing batch is reduced.
研磨パッドの表面粗さRaを低減する方法は特に限定されないが、ダイヤモンドなどの砥粒を含有したドレッサーを用いてバッチ間にドレスをかける方法が好ましい。ドレッサーに含有されるダイヤモンドなどの砥粒の平均粒径は10μm以下であると好ましく、5μm以下であるとさらに好ましく、2μm以下であると最も好ましい。ドレッサーの砥粒の平均粒径がこの範囲であると、研磨バッチ内の研磨対象物の厚さのバラつき(TTV)が低減する。
The method for reducing the surface roughness Ra of the polishing pad is not particularly limited, but a method of dressing between batches using a dresser containing abrasive grains such as diamond is preferable. The average particle size of the abrasive grains such as diamond contained in the dresser is preferably 10 μm or less, more preferably 5 μm or less, and most preferably 2 μm or less. When the average particle size of the dresser's abrasive grains is in this range, the variation in the thickness (TTV) of the object to be polished in the polishing batch is reduced.
研磨用組成物の供給量は特に限定されないが、1分あたり20mL以上が好ましく、100mL以上であるとより好ましい。研磨用組成物の供給量がこの範囲であると、研磨対象物の被研磨面の平滑性が向上する。
The supply amount of the polishing composition is not particularly limited, but 20 mL or more per minute is preferable, and 100 mL or more is more preferable. When the supply amount of the polishing composition is within this range, the smoothness of the surface to be polished of the object to be polished is improved.
〔実施例〕
以下に実施例及び比較例を示し、本発明をさらに具体的に説明する。
コロイダルシリカからなる砥粒と水とを混合して、砥粒を水に分散させ、実施例1~10及び比較例1~7の研磨用組成物を製造した。各実施例及び比較例において使用した砥粒の平均2次粒子径と、研磨用組成物中の砥粒の含有量は、表1に示すとおりである。なお、コロイダルシリカの平均2次粒子径は、株式会社堀場製作所製のレーザー回折/散乱式粒子径分布測定装置LA-950を使用して測定した。 〔Example〕
Examples and comparative examples are shown below, and the present invention will be described in more detail.
Abrasive grains made of colloidal silica and water were mixed to disperse the abrasive grains in water to produce polishing compositions of Examples 1 to 10 and Comparative Examples 1 to 7. The average secondary particle diameter of the abrasive grains used in each Example and Comparative Example and the content of the abrasive grains in the polishing composition are as shown in Table 1. The average secondary particle size of colloidal silica was measured using a laser diffraction / scattering type particle size distribution measuring device LA-950 manufactured by HORIBA, Ltd.
以下に実施例及び比較例を示し、本発明をさらに具体的に説明する。
コロイダルシリカからなる砥粒と水とを混合して、砥粒を水に分散させ、実施例1~10及び比較例1~7の研磨用組成物を製造した。各実施例及び比較例において使用した砥粒の平均2次粒子径と、研磨用組成物中の砥粒の含有量は、表1に示すとおりである。なお、コロイダルシリカの平均2次粒子径は、株式会社堀場製作所製のレーザー回折/散乱式粒子径分布測定装置LA-950を使用して測定した。 〔Example〕
Examples and comparative examples are shown below, and the present invention will be described in more detail.
Abrasive grains made of colloidal silica and water were mixed to disperse the abrasive grains in water to produce polishing compositions of Examples 1 to 10 and Comparative Examples 1 to 7. The average secondary particle diameter of the abrasive grains used in each Example and Comparative Example and the content of the abrasive grains in the polishing composition are as shown in Table 1. The average secondary particle size of colloidal silica was measured using a laser diffraction / scattering type particle size distribution measuring device LA-950 manufactured by HORIBA, Ltd.
次に、実施例1~10及び比較例1~7の研磨用組成物を使用して、研磨対象物の研磨を行った。研磨対象物は、多結晶セラミックスである透光性アルミナ、窒化アルミニウム、又は窒化ケイ素の粉末の焼結体で形成された板状部材である。なお、研磨前には、研磨パッドを粒度#270(53μm)のダイヤモンドを含有したドレッサーを用いてドレスをし、研磨パッドの表面粗さRaを1.1μmとした。そして、研磨した研磨対象物の被研磨面の表面粗さRa及び被研磨面の段差(結晶粒界部分の凹凸段差)を測定するとともに、研磨速度を算出した。
Next, the polishing target was polished using the polishing compositions of Examples 1 to 10 and Comparative Examples 1 to 7. The object to be polished is a plate-shaped member formed of a sintered body of a powder of translucent alumina, aluminum nitride, or silicon nitride, which is a polycrystalline ceramic. Before polishing, the polishing pad was dressed with a dresser containing diamond having a particle size of # 270 (53 μm), and the surface roughness Ra of the polishing pad was set to 1.1 μm. Then, the surface roughness Ra of the surface to be polished and the step (unevenness step of the crystal grain boundary portion) of the surface to be polished were measured, and the polishing speed was calculated.
研磨条件は以下の通りである。
研磨装置:Engis社製片面研磨装置EJ-380IN(定盤径380mm)
研磨パッド:エポキシ樹脂製研磨パッド
研磨荷重:29.4kPa(300gf/cm2)
定盤の回転速度:110min-1
研磨速度(線速度):84m/分
研磨時間:30分
研磨用組成物の供給速度:20mL/分 The polishing conditions are as follows.
Polishing device: Single-sided polishing device EJ-380IN manufactured by Engis (surface plate diameter 380 mm)
Polishing pad: Epoxy resin polishing pad Polishing load: 29.4 kPa (300 gf / cm 2 )
Surface plate rotation speed: 110min -1
Polishing speed (linear speed): 84 m / min Polishing time: 30 minutes Supply speed of polishing composition: 20 mL / min
研磨装置:Engis社製片面研磨装置EJ-380IN(定盤径380mm)
研磨パッド:エポキシ樹脂製研磨パッド
研磨荷重:29.4kPa(300gf/cm2)
定盤の回転速度:110min-1
研磨速度(線速度):84m/分
研磨時間:30分
研磨用組成物の供給速度:20mL/分 The polishing conditions are as follows.
Polishing device: Single-sided polishing device EJ-380IN manufactured by Engis (surface plate diameter 380 mm)
Polishing pad: Epoxy resin polishing pad Polishing load: 29.4 kPa (300 gf / cm 2 )
Surface plate rotation speed: 110min -1
Polishing speed (linear speed): 84 m / min Polishing time: 30 minutes Supply speed of polishing composition: 20 mL / min
研磨後の研磨対象物の被研磨面の表面粗さRaは、Zygo社製の測定装置NewView5032を使用して視野角143×107μmの条件で測定した。研磨後の研磨対象物の被研磨面の段差は、以下のようにして測定した。すなわち、研磨後の研磨対象物の被研磨面の段差は、Zygo社製の測定装置NewView5032を使用してPVの値で評価した。PV値は、測定範囲における最大高さと最大深さを示す値であるが、今回の視野角(視野角143×107μm)ではうねりの影響を受けていないため、最大高さは結晶の残存部分(凸部)、最大深さは結晶の脱粒部分(凹部)となり、粒界段差がPV値と相関する。ただし、窒化ケイ素においては、PV値と粒界段差の相関性が低く、この方法では粒界段差を正確に測定することができないため、評価をしていない。研磨速度は、研磨前後の研磨対象物の質量を測定し、その差と研磨時間と被研磨面の面積から算出した。これらの結果を表1に示す(窒化ケイ素の段差は「N.D」と示した)。
The surface roughness Ra of the surface to be polished of the object to be polished after polishing was measured under the condition of a viewing angle of 143 × 107 μm using a measuring device NewView5032 manufactured by Zygo. The step on the surface to be polished of the object to be polished after polishing was measured as follows. That is, the step on the surface to be polished of the object to be polished after polishing was evaluated by the value of PV using a measuring device NewView5032 manufactured by Zygo. The PV value is a value indicating the maximum height and the maximum depth in the measurement range, but since the viewing angle (viewing angle 143 × 107 μm) this time is not affected by the swell, the maximum height is the remaining part of the crystal (the remaining part of the crystal (viewing angle 143 × 107 μm). The convex portion) and the maximum depth are the deciduous portions (concave portions) of the crystal, and the grain boundary step correlates with the PV value. However, in silicon nitride, the correlation between the PV value and the grain boundary step is low, and the grain boundary step cannot be accurately measured by this method, so the evaluation has not been performed. The polishing speed was calculated from the difference, the polishing time, and the area of the surface to be polished by measuring the mass of the object to be polished before and after polishing. These results are shown in Table 1 (the step of silicon nitride is shown as "ND").
表1に示す結果から分かるように、実施例1~10は、砥粒の平均2次粒子径が5nm以上40nm以下であるため、研磨後の研磨対象物の被研磨面の段差が小さく、多結晶セラミックス製の研磨対象物の表面を平滑に研磨することができた。また、研磨後の研磨対象物の被研磨面の表面粗さRaも小さく、研磨速度も十分に高かった。
As can be seen from the results shown in Table 1, in Examples 1 to 10, since the average secondary particle diameter of the abrasive grains is 5 nm or more and 40 nm or less, the step on the surface to be polished of the object to be polished after polishing is small and many. The surface of the object to be polished made of crystalline ceramics could be polished smoothly. In addition, the surface roughness Ra of the surface to be polished of the object to be polished after polishing was small, and the polishing speed was sufficiently high.
これに対して、比較例2~7は、砥粒の平均2次粒子径が40nm超過であるため、研磨後の研磨対象物の被研磨面の段差が大きく、多結晶セラミックス製の研磨対象物の表面を平滑に研磨することができなかった。なお、平均2次粒子径が5nm未満である砥粒は安定した製造が困難であるため、比較例1は比較検討することができなかった。
On the other hand, in Comparative Examples 2 to 7, since the average secondary particle diameter of the abrasive grains exceeds 40 nm, the step of the surface to be polished of the object to be polished after polishing is large, and the object to be polished made of polycrystalline ceramics. The surface of the ceramic could not be polished smoothly. Since it is difficult to stably produce abrasive grains having an average secondary particle diameter of less than 5 nm, Comparative Example 1 could not be compared and examined.
これに加えて、各実施例において、研磨バッチ間のドレッサーとして粒度#270(53μm)のダイヤモンドを含有したドレッサーを用いていたものを、粒度1μmのダイヤモンドを含有したドレッサーを用いてドレスをし、研磨パッドの表面粗さRaを0.05μmとして同様に研磨したところ、研磨パッドの表面粗さRaが1.1μm、かつ粒度#270(53μm)のダイヤモンドを含有したドレッサーによるときに比べて、研磨対象物の表面粗さRa、段差は維持した上で、研磨バッチ内の研磨対象物の厚さのバラつき(TTV)が60~80%に低減した。
In addition to this, in each example, a dresser containing diamond having a grain size of # 270 (53 μm) was used as a dresser between polishing batches, and a dresser containing diamond having a grain size of 1 μm was used for dressing. When the surface roughness Ra of the polishing pad was set to 0.05 μm and the polishing was performed in the same manner, the polishing was performed in the same manner as when the surface roughness Ra of the polishing pad was 1.1 μm and the dresser containing diamond having a grain size of # 270 (53 μm) was used. While maintaining the surface roughness Ra and the step of the object, the variation in the thickness of the object to be polished (TTV) in the polishing batch was reduced to 60 to 80%.
Claims (8)
- 多結晶セラミックスを含有する研磨対象物の研磨に使用される研磨用組成物であって、砥粒及び水を含有し、前記砥粒の平均2次粒子径が5nm以上40nm以下である研磨用組成物。 A polishing composition used for polishing an object to be polished containing polycrystalline ceramics, which contains abrasive grains and water and has an average secondary particle diameter of 5 nm or more and 40 nm or less. thing.
- 前記多結晶セラミックスは、アルミニウムを含有する酸化物及びアルミニウムを含有する窒化物の少なくとも一方である請求項1に記載の研磨用組成物。 The polishing composition according to claim 1, wherein the polycrystalline ceramic is at least one of an aluminum-containing oxide and an aluminum-containing nitride.
- 前記研磨対象物は前記多結晶セラミックスの粉末の焼結体である請求項1又は請求項2に記載の研磨用組成物。 The polishing composition according to claim 1 or 2, wherein the object to be polished is a sintered body of the powder of the polycrystalline ceramics.
- 前記砥粒がコロイダルシリカである請求項1~3のいずれか一項に記載の研磨用組成物。 The polishing composition according to any one of claims 1 to 3, wherein the abrasive grains are colloidal silica.
- 前記砥粒の含有量が1質量%以上30質量%以下である請求項1~4のいずれか一項に記載の研磨用組成物。 The polishing composition according to any one of claims 1 to 4, wherein the content of the abrasive grains is 1% by mass or more and 30% by mass or less.
- 請求項1~5のいずれか一項に記載の研磨用組成物を用いて、多結晶セラミックスを含有する研磨対象物を研磨する研磨方法。 A polishing method for polishing an object to be polished containing polycrystalline ceramics using the polishing composition according to any one of claims 1 to 5.
- 研磨前の研磨パッドの表面粗さRaを0.75μm以下とする、請求項6に記載の研磨方法。 The polishing method according to claim 6, wherein the surface roughness Ra of the polishing pad before polishing is 0.75 μm or less.
- 研磨前の研磨パッドを平均粒径が10μm以下の砥粒を含有したドレッサーを用いてドレスする、請求項6又は請求項7に記載の研磨方法。 The polishing method according to claim 6 or 7, wherein the polishing pad before polishing is dressed using a dresser containing abrasive grains having an average particle size of 10 μm or less.
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JPS60155359A (en) * | 1984-01-20 | 1985-08-15 | Sumitomo Special Metals Co Ltd | Holeless polishing method of ceramic material |
JPH09131662A (en) * | 1995-11-10 | 1997-05-20 | Fuji Elelctrochem Co Ltd | Ceramics polishing method |
JP2003117806A (en) * | 2001-10-10 | 2003-04-23 | Kobe Steel Ltd | Mirror-polishing method for polycrystalline ceramics |
JP2020029472A (en) * | 2018-08-20 | 2020-02-27 | 株式会社ダイセル | Slurry composition for polishing polycrystalline YAG |
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Publication number | Priority date | Publication date | Assignee | Title |
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JPS60155359A (en) * | 1984-01-20 | 1985-08-15 | Sumitomo Special Metals Co Ltd | Holeless polishing method of ceramic material |
JPH09131662A (en) * | 1995-11-10 | 1997-05-20 | Fuji Elelctrochem Co Ltd | Ceramics polishing method |
JP2003117806A (en) * | 2001-10-10 | 2003-04-23 | Kobe Steel Ltd | Mirror-polishing method for polycrystalline ceramics |
JP2020029472A (en) * | 2018-08-20 | 2020-02-27 | 株式会社ダイセル | Slurry composition for polishing polycrystalline YAG |
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JP2024541256A (en) * | 2021-10-27 | 2024-11-08 | インテグリス・インコーポレーテッド | Polishing of polycrystalline materials |
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