CN101356248A - Cerium-based abrasive material - Google Patents
Cerium-based abrasive material Download PDFInfo
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- CN101356248A CN101356248A CNA2007800011752A CN200780001175A CN101356248A CN 101356248 A CN101356248 A CN 101356248A CN A2007800011752 A CNA2007800011752 A CN A2007800011752A CN 200780001175 A CN200780001175 A CN 200780001175A CN 101356248 A CN101356248 A CN 101356248A
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- abrasive material
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 81
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000003082 abrasive agent Substances 0.000 title claims abstract description 46
- 239000002245 particle Substances 0.000 claims abstract description 39
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 23
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 10
- 229910017488 Cu K Inorganic materials 0.000 claims abstract description 9
- 229910017541 Cu-K Inorganic materials 0.000 claims abstract description 9
- 238000007561 laser diffraction method Methods 0.000 claims abstract description 7
- 238000000790 scattering method Methods 0.000 claims abstract description 7
- 230000001186 cumulative effect Effects 0.000 claims abstract description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 3
- 239000002002 slurry Substances 0.000 claims description 19
- 238000005498 polishing Methods 0.000 abstract 2
- 238000000227 grinding Methods 0.000 description 69
- 239000000126 substance Substances 0.000 description 61
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 51
- 239000002994 raw material Substances 0.000 description 44
- 239000002253 acid Substances 0.000 description 31
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 27
- 229910002091 carbon monoxide Inorganic materials 0.000 description 27
- 238000000034 method Methods 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- 239000000203 mixture Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- 238000007598 dipping method Methods 0.000 description 10
- 238000001035 drying Methods 0.000 description 9
- 239000011521 glass Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000001914 filtration Methods 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 6
- 239000011737 fluorine Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000002612 dispersion medium Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002609 medium Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000004438 BET method Methods 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 229910052772 Samarium Inorganic materials 0.000 description 2
- 230000005260 alpha ray Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- HDXXSUQVQKJEBI-UHFFFAOYSA-N carbonic acid;cerium Chemical compound [Ce].OC(O)=O HDXXSUQVQKJEBI-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010333 wet classification Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 150000000703 Cerium Chemical class 0.000 description 1
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000004520 agglutination Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010332 dry classification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- SBNFWQZLDJGRLK-UHFFFAOYSA-N phenothrin Chemical compound CC1(C)C(C=C(C)C)C1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 SBNFWQZLDJGRLK-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- -1 rare-earth compounds Chemical class 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C19/00—Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Mechanical Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
A cerium-based abrasive material which inhibits polishing scratches from generating and attains a significantly improved polishing rate. The cerium-based abrasive material has a cerium oxide content of 95 mass% or higher based on the total rare-earth oxides (TREO), and is characterized in that the particle diameter (D50) corresponding to the cumulative volume of 50% from the small-particle-diameter side in examination by the laser diffraction/scattering method is 1.3-4.0 [mu]m. When analyzed by X-ray diffractometry with a Cu-K(alph1) line, the cerium-based abrasive material preferably is one in which the maximum peak for cerium oxide has a half band width of 0.1-0.5 DEG in terms of 2theta.
Description
Technical field
The present invention relates to contain the cerium based abrasive material and the cerium based abrasive material slurry of high-purity cerium oxide.
Background technology
Cerium based abrasive material (being designated hereinafter simply as abrasive substance) was widely used with material as the grinding of glass material in the past.Particularly in recent years because the quick growth in electric/electronic device fields such as hard disk and liquid-crystal display (LCD), photomask, so increase as their its demand of abrasive substance of glass substrate etc.
Here, in fields such as above-mentioned electric/electronic device,, require higher grinding precision for glass grinding faces such as substrates along with the development of miniaturization and densification.Therefore, in these fields, adopted the high high purity cerium based abrasive material of cerium content in recent years.This high purity cerium based abrasive material is the material that the content of the element beyond the cerium is decreased, and is the abrasive substance that content is less, recirculation is good that has the fluorine etc. of environmental problem.
For example, in patent documentation 1 or patent documentation 2 etc., disclosed above-mentioned highly purified cerium based abrasive material.In addition, as the high purity cerium based abrasive material that structurally has feature, in patent documentation 3, disclosed the polymorph semi-conductor abrasive substance that cerium oxide particles is made of crystallite with crystal boundary.Because this abrasive substance generates the new surface that does not contact with medium and substrate is ground when grinding, therefore be the material that can reduce the generation of grinding damage.In addition, disclose the crystalline technical scheme that decides the cerium particle with the angle of diffraction of X-ray diffraction in the patent documentation 4, disclosed the high purity cerium based abrasive material that the oversize particle that causes grinding damage is few, have the agglutination particle of appropriateness in the patent documentation 5.
Patent documentation 1: the special public clear 63-27389 communique of Japanese Patent
Patent documentation 2: the Japanese Patent spy opens the 2001-89748 communique
Patent documentation 3: No. 3727241 specification sheets of Japanese Patent
Patent documentation 4: the Japanese Patent spy opens the 2000-26840 communique
Patent documentation 5: the Japanese Patent spy opens the 2004-175964 communique
The announcement of invention
As mentioned above, the high purity cerium based abrasive material is grinding precision height, the good material of recirculation.But, about its grinding precision, grind the performance that damage takes place though have abundant inhibition, the requirement that improves its grinding rate is also arranged sometimes.For example, now grinding rate is not enough because of the difference of purposes is omited for the abrasive substance of patent documentation 1 or patent documentation 2, and the calcining when therefore imagination is at high temperature implemented manufacturing improves grinding rate.But the present inventor thinks, if these abrasive substances are carried out sintering, then produces oversize particle in a large number, is prone to grind damage.In addition, the abrasive substance of patent documentation 3 or patent documentation 4 is the low-down material of grinding rate when the grinding of carrying out glass substrate etc., if wish to improve grinding rate, then grinds damage with above-mentioned can the generation equally.In addition, patent documentation 5 has disclosed the abrasive substance that grinding rate also is improved when suppressing to grind the generation that damages, but when grinding rate was had extra high the requirement, grinding rate was also slightly existing not enough.
Therefore, the purpose of this invention is to provide and suppress to grind the cerium based abrasive material that the balance of having improved the grinding precision of grinding rate when damage takes place further turns for the better.
In order to address the above problem, the present inventor has carried out conscientiously studying to improve grinding rate to the high purity cerium based abrasive material of various particle diameters.Found that the particle diameter of cerium based abrasive material is in specialized range the time, can obtain grinding rate faster when damage takes place suppressing to grind, thereby expect the present invention.
Promptly, the present invention relates to cerium based abrasive material, it is characterized in that it is the cerium based abrasive material of cerium oxide content more than 95 quality % with respect to whole rare-earth oxides (TREO), the particle diameter (D of the cumulative volume 50% that begins from the small particle size side that utilizes that the laser diffraction and scattering method records
50) value is 1.3～4.0 μ m.
The particle size distribution measuring method (with reference to JIS R 1629-1997 " the particle size distribution measuring method of utilizing laser diffraction and scattering method of fine ceramics raw material ") of the particle diameter of abrasive substance of the present invention by utilizing the laser diffraction and scattering method surveyed the particle diameter (D of the periodic cumulative volume 50% that begins from the small particle size side
50) value is 1.3～4.0 μ m.If less than 1.3 μ m, then grinding rate descends, if surpass 4.0 μ m, the tendency of the generation increase of the damage of grinding is arranged then.This D
50Value is preferably 1.4～3.5 μ m, more preferably 1.5～3.0 μ m.
Among the present invention, cerium oxide (CeO
2) content CeO
2/ TREO is more than the 95 quality %, is preferably more than the 99 quality %, more preferably more than the 99.6 quality %, is preferably more than the 99.9 quality %.When being lower than 95 quality %, grinding rate descends.In addition, though no problem aspect quality, because the raw material high price, so CeO
2/ TREO is preferably below the 99.999 quality %.
Here, cerium based abrasive material of the present invention is the specific surface area that records of benchmark 0.8～8m more fortunately with " (3.5) one point methods of 6.2 flow methods " of JIS R 1626-1996 (utilizing the measuring method of specific surface area of the gas adsorption BET method of fine ceramics powder)
2In the scope of/g, 1～7m more preferably
2/ g is well 1.5～6m again
2/ g.If be lower than 0.8m
2/ g, the generation that then grinds damage is big, if surpass 8m
2/ g, then grinding rate descends.
Cerium based abrasive material of the present invention is the bigger material of particle diameter, if but to surpass the content of oversize particle of particle size range of the application's regulation too much, and then easily produce and grind damage, the variable serious tendency of small percent ripple of abrasive surface is arranged.Therefore, the content of oversize particle in abrasive substance more than the particle diameter 10 μ m is more fortunately below the 1000 quality ppm, better below 500 quality ppm, more fortunately below the 300 quality ppm.
Cerium based abrasive material of the present invention passes through based on Cu-K α
1The half-width of the maximum peak of the cerium oxide that the X-ray diffraction analysis of ray is measured is preferably 0.1～0.5 ° in 2 θ, more preferably 0.15～0.45 °, is 0.2～0.4 ° well again.If 0.1 ° of 2 θ less than, the generation that then grinds damage is big, if surpass 0.5 °, and the tendency that then has grinding rate to descend.Here, 2 θs of the maximum peak of cerium oxide at the peak of (111) face are about 28.6 ° and locate to occur.In addition, based on Cu-K α
1The X-ray diffraction of ray is except shining Cu-K α to sample
1Beyond the situation of ray, also comprise to sample irradiation Cu-K alpha-ray, gained diffraction X ray being divided into α based on Cu-K
1The ray of ray and based on Cu-K α
2The ray of ray, to based on Cu-K α
1The situation that the diffraction X ray of ray is resolved.
In addition, contain fluorine in the cerium based abrasive material sometimes, if but fluorine content height then has the tendency that is increased by the surface roughness of abrasive surface.Therefore, the fluorine content in the abrasive substance is more fortunately below the 0.5 quality %, better below 0.2 quality %, more fortunately below the 0.1 quality %.
TREO content in the abrasive substance is more fortunately more than the 97 quality %, better more than 98 quality %.When being less than 97 quality %, owing to contain impurity such as metallic element oxide compound beyond the more rare earth element and silicon oxide, so it is multiple or because of underroasting remaining carbanion and moisture in abrasive substance, grinding rate can descend sometimes to grind damage.
In addition, in enforcement of the present invention, preferably adopt the cerium based abrasive material slurry that contains above-mentioned cerium based abrasive material.Cerium based abrasive material slurry (being designated hereinafter simply as the abrasive substance slurry) contains dispersion medium such as above-mentioned cerium based abrasive material and water at least, also can contain additives such as dispersion agent.Here, as dispersion medium, preferably water, the solubleness in water be more than 5% organic solvent or in the scope of this organic solvent of dissolving with the mixture of water.As organic solvent, preferably use alcohols, polyalcohols, ketone, tetrahydrofuran (THF), N, dinethylformamide, methyl-sulphoxide etc.
Slurry concentration during grinding is preferably 1～700g/L in TREO, and more preferably 10～500g/L is well 30～400g/L again.On the other hand, implement to make under slurry state, when transportation, keeping etc., slurry concentration can be identical when grinding, if but concentration is too low, then need site of storage mostly, and transportation cost also can improve.Therefore, slurry concentration is preferably 100～1000g/L in TREO, and more preferably 150～850g/L is well 200～700g/L again.Before grinding, use after can diluting slurry as required.
Shown below for obtaining the preferable production process of cerium based abrasive material of the present invention.Basic manufacturing process is, employing through carrying out roasting after the operations such as pulverizing, filtration, drying, is pulverized based on cerous carbonate, according to circumstances implement the raw material that vapour cure or dipping heat treated etc. obtain with pre-burning again, classification can obtain the abrasive substance as object.
[raw material]
When making cerium based abrasive material of the present invention, モ ノ オ キ シ charcoal acid セ リ ウ system) or basic carbonate cerium (Japanese: at least one side water acidifying charcoal acid セ リ ウ system) preferably adopt the mixture of cerous carbonate, cerous carbonate and cerium oxide or cerous carbonate is carried out pre-burning and any a kind of raw material in the raw material that obtains, also contain carbon monoxide acid cerium (Japanese: in this raw material with the degree that is not converted into oxide compound fully.If the use above-mentioned raw materials, even the high purity cerium based abrasive material, sintering also can moderately be implemented equably when roasting, makes the poor cerium based abrasive material of oversize particle.
In addition, the raw material (also can contain the basic carbonate cerium) that contains cerous carbonate and carbon monoxide acid cerium better is that scorching hot decrement (with the quality behind 105 ℃ of thorough drying objects is benchmark, is shown in the rate of mass reduction of 1000 ℃ of heating after 2 hours) is the material of 25～40 quality %.If less than 25 quality %, then the generation of carbon monoxide acid cerium is too much, if surpass 40 quality %, then the generation of the cerium of carbon monoxide acid on the contrary has very few tendency.In addition, when this raw material was carried out pre-burning, scorching hot decrement was advisable with 5～20 quality %.If in the raw material of having implemented pre-burning, add water etc. after the pre-burning, then can not carry out 105 ℃ drying.Here, rare-earth compounds is difficult to reach constant under 650 (± 50) of the benchmark of the scorching hot temperature of conduct shown in the JIS K 0067-1992 " decrement of chemical preparations and residual component test method " ℃, so must carry out repeatedly scorching hot repeatedly.Therefore, even the present invention carries out scorching hot processing for only implementing under 1 scorching hot temperature of 1000 ℃ that also can fully reach constant in scorching hot temperature.Implement under the situation of this scorching hot condition, also change hardly, can reach the benchmark of the constant shown in the above-mentioned JIS even further carry out scorching hot quality.
[manufacture method of raw material]
Shown below is the preferable production process of the raw material of above-mentioned cerium based abrasive material.At first, be preferably, the rare earth class concentrate that contains cerium is decomposed by having used the known methods such as solvent extraction of organic solvent, refining, obtain CeO
2/ TREO is the above cerium refined liquid of 95 quality %.Mix carbonic acid class precipitation agents such as this cerium refined liquid and bicarbonate of ammonia, can obtain cerous carbonate.In the present invention, can directly cerous carbonate be used as raw material, still, utilizing only is that the abrasive substance that raw material obtains has carried out under the situation of grinding with the cerous carbonate, exists to produce and grinds the tendency that damage waits the nonferromagnetic substance deterioration.Therefore, preferably by following method etc., make and contain carbon monoxide acid cerium or basic carbonate cerium in the cerous carbonate.In addition, the CeO that utilizes aforesaid method to make
2/ TREO is that the above cerous carbonate of 95 quality % can be from acquisitions such as China.
The cerous carbonate that contains the either party of carbon monoxide acid cerium or basic carbonate cerium or both sides can be in the manufacturing process of above-mentioned cerous carbonate, method of temperature when adjusting the precipitation by the cerium refined liquid, cerous carbonate is carried out dipping methods of heating treatment under vapour cure or the gentle condition, perhaps the method for mixed carbonic acid cerium and carbon monoxide acid cerium or basic carbonate cerium and obtaining.Below, describe making the method that contains carbon monoxide acid cerium or basic carbonate cerium in the cerous carbonate.
The first, can be by containing carbon monoxide acid cerium or basic carbonate cerium in the cerium refined liquid, adding precipitation agent under the temperature more than 50 ℃ and mix.Usually, generate carbon monoxide acid cerium in this case, if but the consumption of carbonic acid class precipitation agent is more than 1.5 times of theoretical amount, then easily generate the basic carbonate cerium.
The second, by cerous carbonate is carried out vapour cure, also can make and contain carbon monoxide acid cerium etc. in the cerous carbonate.Here used steam can adopt by general steam and produce with the steam more than 100 ℃ that boiler produced, and the steam consumption is the preferred 0.05～0.5kg of the TREO of every 1kg.In addition, by vapour cure, easily generate carbon monoxide acid cerium.
In addition, in the aqueous solution that cerous carbonate be impregnated in water or alkalescence, implement the dipping heat treated of 40～70 ℃ heating, also can contain carbon monoxide acid cerium etc., implement pre-burning and can obtain raw material.Implemented under the situation of the dipping heat treated in water, easily generated carbon monoxide acid cerium, the dipping heat treated in alkaline aqueous solution easily generates the basic carbonate cerium.In addition, the dipping heat treated under 40～70 ℃ a low temperature only part changes carbon monoxide acid cerium or basic carbonate cerium into, if implement to handle being higher than under 70 ℃ the temperature, the tendency that almost changes carbon monoxide acid cerium all into is arranged then.
In addition, also can in cerous carbonate, mix carbon monoxide acid cerium or basic carbonate cerium.At this moment, with the TREO mass conversion, for preferred 20: 1～1: 5 of the ratio of mixture of the carbon monoxide of cerous carbonate acid cerium or basic carbonate cerium.Being used for this blended carbon monoxide acid cerium can be by impregnated in cerous carbonate in water, obtains 60～100 ℃ of processing of heating, the basic carbonate cerium can by in the cerium refined liquid excessively mixed carbonic acid class precipitation agent make carbonate generate, heat in 60～100 ℃ and obtain.At this moment, if do not mix to realize the state of abundant homogeneous, then therefore the sintering heterogeneity that easily becomes when carrying out roasting must be noted that.
The cerous carbonate that contains carbon monoxide acid cerium or basic carbonate cerium by acquisitions such as aforesaid methods can directly use as raw material of the present invention, but also can carry out using as raw material after the pre-burning.Preferred 200～600 ℃ of the calcined temperature of this moment, the scorching hot decrement after the pre-burning preferably reaches 5～20 quality %.At this moment, be preferably the carbon monoxide hydrochlorate in the raw material that utilizes after X-ray diffraction is confirmed pre-burning or the peak of hydroxide carbonate.
In addition, also can mix above-mentioned cerous carbonate and the cerium oxide that contains carbon monoxide acid cerium etc., the gained mixture is used as raw material.With the TREO mass conversion, containing the cerous carbonate of carbon monoxide acid cerium etc. and the ratio of mixture of cerium oxide is 1: 4, and perhaps comparable this ratio of mixture of the ratio of cerium oxide is low.The cerium oxide that uses this moment is preferably at 550～750 ℃ of cerium oxide of cerous carbonate being calcined for a long time and obtaining.
[raw material pulverizing]
Preferably the raw material that obtains by aforesaid method being pulverized makes particle diameter (D50) value of the cumulative volume 50% that begins from the small particle size side that utilizes that the laser diffraction and scattering method records reach 0.5～4.0 μ m.Pulverize the preferred wet type medium grinding machine that uses, the gravel size decision diameter of crushing medium is 0.2～5mm.During case of wet attrition, preferably filter before the roasting, dry and broken.
[roasting]
Preferred 800～1200 ℃ of the temperature of the roasting of carrying out after the pulverizing, more preferably 850～1120 ℃.During less than 800 ℃, grinding rate descends, if surpass 1200 ℃, a large amount of tendencies that occur of the damage of grinding is arranged then.Preferred 0.2～72 hour of roasting time, more preferably 0.5～48 hour.During less than 0.2 hour, the grinding rate of gained abrasive substance has the tendency of decline, even surpass 72 hours, the characteristic of gained abrasive substance does not almost change yet.
[crushing and classification]
Preferably implementing dry type after the roasting pulverizes and dry classification.In addition, carry out case of wet attrition or wet classification and also can obtain the cerium based abrasive material slurry.The mixing of dispersion medium such as abrasive substance powder and water also can be obtained the abrasive substance slurry.
The best mode that carries out an invention
Below, preferred implementation of the present invention is described.
Embodiment 1: in the present embodiment, the rerum natura that makes the cerium based abrasive material under the situation that maturing temperature taken place to change after the raw material pulverizing and abrasive substance performance etc. are described.
As raw material, adopt CeO
2/ TREO be 99.9 quality % above in homemade cerous carbonate, the ratio that reaches 0.2kg with the vapor volume with respect to the TREO of 1kg is implemented vapour cure.Then, add pure water, reach the condition slurryization of 200g/L, adopt wet type medium grinding machine, carry out case of wet attrition with the zirconium white of diameter 4mm with TREO.At this moment, the D of the raw material after the pulverizing
50Value is 1.5 μ m.
Then, utilize pressure filter to filter,, implement again to carry out 12 hours roasting after the fragmentation in 120 ℃ of dryings 48 hours.Each sample that changes between 700～1280 ℃ for maturing temperature at this moment carries out the dry type pulverizing again, and classification obtains the cerium based abrasive material as object.The composition transitivity of gained abrasive substance (content of the oversize particle that 10 μ m are above, the specific surface area, the particle diameter (D that utilize the BET method to measure
50), the half-width of utilizing X-ray diffraction to measure) the following enforcement of mensuration.
[TREO, composition]
The analysis of TREO concentration is at first abrasive substance to be dissolved in acid to add the precipitation that the oxalic acid after-filtration generates, and calcines, and obtains the TREO oxide compound.Then, this TREO sample is carried out quality determination, obtain CeO as benchmark
2, La
2O
3, Pr
6O
11, Nd
2O
3, Sm
2O
3Content (CeO
2/ TREO, La
2O
3/ TREO, Pr
6O
11/ TREO, Nd
2O
3/ TREO, Sm
2O
3/ TREO).Here, the TREO sample is dissolved in the acid back and obtains La by the ICP-AES method
2O
3/ TREO, Pr
6O
11/ TREO, Nd
2O
3/ TREO, Sm
2O
3/ TREO.Then, for CeO
2Directly do not measure, but the value of trying to achieve more than adopting, by 100-{ (La
2O
3/ TREO)+(Pr
6O
11/ TREO)+(Nb
2O
3/ TREO)+(Sm
2O
3/ TREO) formula calculate.
In addition, the quantivative approach of fluorine composition is to make sample alkali molten, and the water hot extraction measures by the fluoride ion electrode method.In addition, for Fe, Ca, Ba, make sample be dissolved in the acid back and measure by the ICP-AES method.The result of this analysis is that all below 0.05 quality %, all below 0.01 quality %, all below 0.01 quality %, Ba content is all below 0.01 quality % for Ca content for Fe content for the F content of the abrasive substance of embodiment 1 gained.
[oversize particle (more than the 10 μ m) content]
The oversize particle Determination on content is that the cerium based abrasive material that 200g makes is got in weighing, makes it be scattered in 0.1% sodium hexametaphosphate solution, stirs 2 minutes, makes slurry.Miniature sieve with aperture 10 μ m filters this slurry, reclaims the residue on the sieve.Make the residue of recovery be scattered in 0.1% sodium hexametaphosphate solution once more and slurryization.At this moment, finish dispersion by the ultrasonic stirring of implementing 1 minute.Then, the miniature sieve with aperture 10 μ m filters slurry.Implement the slurryization again and the filtration of 2 above-mentioned recovery residues.Make weighing after the coarse particle thorough drying of recovery, calculate its content.
[specific surface area, particle diameter]
Method with the BET method measurement the specific area of the aforementioned JIS of utilization regulation is that benchmark is implemented, and carrier gas is adopted helium and as the mixed gas of the nitrogen of adsorbed gas.Median size (D
50: the particle diameter of the mass accumulation 50 quality % that begin from the small particle size side) (Horiba Ltd's system: LA-920) size-grade distribution of measuring each abrasive substance raw material and each cerium based abrasive material is tried to achieve by adopting laser diffraction and scattering method particle size distribution analyzer.
[half-width]
The half-width of abrasive substance adopts x-ray analysis equipment (Japanese MAC science Co., Ltd. system: MXP18), measure in the tube current of the tube voltage of Cu target, 40kV, 150mA, the sweep velocity of measurement range, 0.02deg sampling width, 4deg/ minute with 5～80 ° of 2 θ.The diffraction X ray of gained is divided into the α based on CuK
1The ray of ray and based on CuK α
2The ray of ray is for based on CuK α
1The diffraction X ray of ray, the half-width of the maximum peak of mensuration cerium oxide.In addition, pulverize the mensuration of after filtering the raw material before dry being utilized X-ray diffraction, except not separating the diffraction X ray that obtains by the CuK alpha-ray, by measuring with above-mentioned same method.
For the evaluation of nonferromagnetic substance, adopt the abrasive substance slurry that in the gained cerium based abrasive material, adds pure water, TREO is adjusted into 100g/L.As the evaluation of nonferromagnetic substance, implement grinding rate, grind the evaluation that damages.About by the condition of surface of abrasive surface, measure average surface rugosity Ra, small percent ripple.Below, the particular content of each measuring method is described.
Shredder adopts rub tester (the smart machine in platform east Co., Ltd. system: the HSP-2I type).This rub tester is the machine that with grinding pad grinding object face is ground when grinding the object face to supply with the abrasive substance of paste-like.Dispersion medium only adopts water, and the wear particle concentration of abrasive substance slurry is 100g/L.In this grinding test, the abrasive substance of paste-like is supplied with 5L/ minute ratio, recycles abrasive substance.Grinding object is the smooth plate glass of 65mm φ.Grinding pad uses urethane system pad.Grinding pad is 9.8kPa (100g/cm to the pressure of abrasive surface
2), the speed of rotation of rub tester is set at 100 minutes
-1(rpm), implement 30 minutes milled processed.
[grinding rate, grinding damage]
Measure the glass weight before and after grinding, estimate the grinding value based on the decrement of the glass weight that causes because of grinding.This grinding value as benchmark (100), is calculated relative evaluation value for other embodiment with comparative example 1.Then,, observe the glass surface after grinding,, be divided into full marks with 100 and adopt the modes that subtract the branch evaluation to estimate the grinding damage the number fractionation of macrolesion and microlesion by with the reflection method of 300,000 halogen lamps of reining in as the light source use.During this grind to be estimated, " ◎ " represent more than 98 minutes, 95 fens above less thaies of " zero " expression 98 minutes, and 90 fens above less thaies of " △ " expression 95 minutes, " * " represents less than 90 minutes.
[grinding precision]
With pure water washing by grind the glass that gets by abrasive surface, after making its drying under the dustless state, carry out the evaluation of grinding precision.In the measurement range of 10 * 10 μ m, the glass after measure grinding with atomic force microscope (AFM) by the surface roughness of abrasive surface, calculate its mean value Ra.In addition, small percent ripple adopts three-dimensional surface structure elucidation microscope (wise Europe (Zygo) corporate system NewView200), with the mensuration wavelength of 0.2～1.4mm, measures with white light scanning abrasive surface.The measurement result of embodiment 1 is shown in following table 1.
Table 1
*: in all comparative examples of table 1 and the abrasive substance of embodiment, be CeO with respect to the content of each compound of TREO
2Be more than the 99.9 quality %, La
2O
3, Pr
6O
11, Nd
2O
3All be below the 0.02 quality %, Sm
2O
3Be below the 0.01 quality %.
As known from Table 1, D
50Value is that the embodiment 1～10 of 1.3～4.0 μ m compares with comparative example, grinds damage and is difficult for producing, and grinding rate is also very fast.In addition, the surface roughness Ra of these abrasive substances and small percent ripple are little, show after the grinding by the smoothness of abrasive surface.In addition, among the embodiment 1～10, if D
50Value reaches better 1.4～3.5 μ m, and the abrasive substance of then all embodiment can further suppress to grind the generation of damage, if reach further better 1.5～3.0 μ m, then grinding rate is faster when suppressing to grind damage.In addition, among the embodiment 1～10, confirm that half-width 2 θ are that 0.1～0.5 ° the grinding rate of abrasive substance is faster, grind the more difficult generation of damage.Confirm to be more preferably half-width 2 θ and be 0.15～0.45 ° abrasive substance, further be more preferably 0.2～0.4 ° abrasive substance.
In addition, if consider grinding rate and grind the balance of damage, confirm that then oversize particle content is preferably below the 1000 quality ppm, more preferably below the 500 quality ppm, further more preferably below the 300 quality ppm, the preferable range of specific surface area is 0.8～8m
2/ g, more preferably 1～7m
2/ g, further 1.5～6m more preferably
2/ g.In addition, the maturing temperature of the abrasive substance that the above-mentioned nonferromagnetic substance of affirmation acquisition is good is preferred 800～1200 ℃.
Embodiment 2: following for homemade cerous carbonate in using in the raw material, the situation of having used the different cerous carbonate of the cerium oxide content among the TREO is described.
The different raw material of cerium oxide content in using TREO, adopt with the same method of embodiment 1 and implement.In addition, maturing temperature all is 950 ℃.The results are shown in table 2.F content in the abrasive substance that embodiment 2 obtains all is below the 0.05 quality %, and Fe content all is below the 0.01 quality %, and Ca content all is below the 0.01 quality %, and Ba content all is below the 0.01 quality %.
Table 2
Can find out from table 2, use CeO
2/ TREO is the CeO of the abrasive substance that makes of the following raw material of 95 quality %
2/ TREO also reaches below the 95 quality %.The comparative example 5 of cerium oxide below 95 quality % and the D of comparative example 6
50Value is below 1.3 μ m, and half-width is above 0.5 °.Consequently, the specific surface area of gained abrasive substance surpasses 8m
2/ g about nonferromagnetic substance, compares with embodiment, and grinding rate slows down, and the grinding damage is more.
Embodiment 3: present embodiment is adjusted maturing temperature and is made particle diameter D adopting the different raw material of cerium oxide content among the TREO
50Value enters the situation that makes abrasive substance in the scope of the present invention and describes.
Same with embodiment 2, adopt CeO
2The raw material that/TREO is different, the temperature when adjusting roasting makes D
50Value reaches the identical value of embodiment 4 (1.58 μ m) with embodiment 1.Other method adopts the method same with embodiment 1.In addition, the F content of the abrasive substance that embodiment 3 obtains all is below the 0.05 quality %, and Fe content all is below the 0.01 quality %, and Ca content all is below the 0.01 quality %, and Ba content all is below the 0.01 quality %.
Table 3
Shown in the comparative example 7 and comparative example 8 of table 3, adopt CeO
2When/TREO was the following raw material of 95 quality %, even particle diameter within the scope of the invention promptly about 1.6 μ m, oversize particle content was also more, and aspect nonferromagnetic substance, the generation that grinds damage is many, the grinding rate deficiency.In addition, show that maturing temperature at this moment must reach the high temperature more than 1000 ℃.Therefore, by embodiment 2 and present embodiment as can be known, prerequisite of the present invention is CeO
2/ TREO is the above high purity cerium based abrasive materials of 95 quality %.
Embodiment 4: present embodiment describes the situation that raw material has carried out vapour cure or dipping heat treated.Except the manufacture method of raw material, adopt the method same with embodiment 1.Maturing temperature all is 950 ℃.
Embodiment 17 carries out the vapour cure of cerous carbonate according to the method same with embodiment 1, generate carbon monoxide acid cerium after, in 500 ℃ of pre-burnings of carrying out 5 hours, be that the product of 9 quality % is as raw material with scorching hot decrement.18 of embodiment mix the ammoniacal liquor of cerous carbonate with 0.5 mol, form the slurry that TREO is 200g/L, in 50 ℃ of dipping heat treated after-filtration that carry out 3 hours, the washing, with products therefrom as raw material.
Comparative example 9 is not carry out vapour cure, will only implement the cerous carbonate of case of wet attrition as raw material.Comparative example 10 is at 500 ℃ the cerous carbonate of equally only having implemented case of wet attrition with comparative example 9 to be carried out 5 hours pre-burning, is that the product of 9 quality % is as raw material with scorching hot decrement.Comparative example 11 is mixed carbonic acid cerium and pure water, and forming TREO is the slurry of 200g/L, in 90 ℃ of dipping heat treated after-filtration that carry out 10 hours, with products therefrom as raw material.Comparative example 12 is that the cerous carbonate that uses with embodiment 12 is as raw material, only utilizing injector-type mill to implement dry type pulverizes, in 750 ℃ of roastings, calcining matter is carried out wet classification, obtain abrasive substance (this manufacturing process implements according to the embodiment 2 of above-mentioned patent documentation 2).In addition, comparative example 13 is raw material with the cerous carbonate that embodiment 12 uses, after case of wet attrition, filtration, drying, put after keeping 4 hours in 1000 ℃ with electric furnace and to be chilled to room temperature, repeat with hammer mill pulverizing, classification 6 times, obtain the few abrasive substance of oversize particle (this manufacturing process implements according to the comparative example 2 of above-mentioned patent documentation 5).
Table 4
* 1: make and pulverize the raw material that filters before the after drying in the scorching hot decrement of the product of 105 ℃ of dryings after 12 hours
* 2:C is cerous carbonate (ICDD card No.38-0377Ce
2(CO
3)
38H
2O), M is carbon monoxide acid cerium (No.44-0617Ce
2(CO
3)
2OH
2O), H is basic carbonate cerium (No.32-0189CeCO
3OH), O is cerium oxide (No.34-0394 or 43-1002CeO
2)
The content with respect to TREO of each compound in the whole comparative example in the table 4 and the abrasive substance of embodiment gained is CeO
2Be more than the 99.9 quality %, La
2O
3, Pr
6O
11, Nd
2O
3All be below the 0.02 quality %, Sm
2O
3Be below the 0.01 quality %.
As shown in the Examples, when adopting the raw material of the dipping heat treated of having carried out vapour cure or alkaline aqueous solution, the result of the X-ray diffraction of gained abrasive substance demonstration contains carbon monoxide acid cerium or basic carbonate cerium.The abrasive substance of these embodiment shows damage, the fast nonferromagnetic substance of grinding rate does not take place to grind.Corresponding to this, the abrasive substance that comparative example 9, comparative example 12 and comparative example 13 obtain only is a cerous carbonate, and the material of comparative example 10 only contains cerium oxide, and nonferromagnetic substance is not good.About the nonferromagnetic substance of comparative example 11, because this material is only formed by carbon monoxide acid cerium, though therefore the grinding damage is not obvious, grinding rate is not enough.
The possibility of utilizing on the industry
As mentioned above, the invention provides suppress grinding and improved having of grinding rate when damage takes place The cerium based abrasive material of the nonferromagnetic substance that balance is good. In addition, cerium based abrasive material of the present invention is to cause grinding The fluorine that wearing and tearing are hindered and the poor material of oversize grain.
Claims (3)
1. cerium based abrasive material, it is characterized in that, it is that cerium oxide content with respect to whole rare-earth oxides (TREO) is the above cerium based abrasive materials of 95 quality %, the particle diameter (D of the cumulative volume 50% that begins from the small particle size side that utilizes that the laser diffraction and scattering method records
50) value is 1.3～4.0 μ m.
2. cerium based abrasive material as claimed in claim 1 is characterized in that, by based on Cu-K α
1The half-width of the maximum peak of the cerium oxide that the X-ray diffraction analysis of ray is measured is counted 0.1～0.5 ° with 2 θ.
3. the cerium based abrasive material slurry is characterized in that, contains the described cerium based abrasive material of claim 1 or claim 2.
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| JP2006054749A JP2007231158A (en) | 2006-03-01 | 2006-03-01 | Cerium-based abrasive |
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| CN103509472A (en) * | 2013-10-25 | 2014-01-15 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
| CN107603490A (en) * | 2017-09-27 | 2018-01-19 | 甘肃稀土新材料股份有限公司 | A kind of cerium based relief polishing powder containing samarium and its preparation technology |
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| JP5588114B2 (en) * | 2009-03-25 | 2014-09-10 | 三井金属鉱業株式会社 | Manufacturing method and processing method of cerium-based abrasive |
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| JP2001089748A (en) * | 1999-07-16 | 2001-04-03 | Seimi Chem Co Ltd | Abrasive |
| JP2001167430A (en) * | 1999-12-08 | 2001-06-22 | Asahi Techno Glass Corp | Substrate for magnetic disk and its manufacturing method |
| JP2004175694A (en) * | 2002-11-26 | 2004-06-24 | Mitsubishi Chemicals Corp | Method for producing gallic acid glycoside |
| JP2004175964A (en) * | 2002-11-28 | 2004-06-24 | Mitsui Mining & Smelting Co Ltd | Manufacturing process of high purity cerium oxide abrasive, and high purity cerium oxide abrasive obtained by the process |
| TWI313707B (en) * | 2003-04-17 | 2009-08-21 | Mitsui Mining & Smelting Co | Cerium-based abrasive |
| CN101104791B (en) * | 2003-06-30 | 2010-06-16 | 三井金属鉱业株式会社 | Cerium based polishing material and raw materials therefor |
| TWI332981B (en) * | 2003-07-17 | 2010-11-11 | Showa Denko Kk | Method for producing cerium oxide abrasives and cerium oxide abrasives obtained by the method |
| JP4282434B2 (en) * | 2003-10-21 | 2009-06-24 | 三井金属鉱業株式会社 | Cerium oxide, cerium oxide for abrasives and method for producing them |
| WO2005042661A1 (en) * | 2003-10-31 | 2005-05-12 | Mitsui Mining & Smelting Co., Ltd. | Cerium polishing agent and method for producing cerium polishing agent |
| JP4395049B2 (en) * | 2004-10-29 | 2010-01-06 | 三井金属鉱業株式会社 | Cerium-based abrasive and method for producing cerium-based abrasive |
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| CN103509472A (en) * | 2013-10-25 | 2014-01-15 | 上海华明高纳稀土新材料有限公司 | Cerium-based mixed rare earth polishing powder and preparation method thereof |
| CN107603490A (en) * | 2017-09-27 | 2018-01-19 | 甘肃稀土新材料股份有限公司 | A kind of cerium based relief polishing powder containing samarium and its preparation technology |
| CN107603490B (en) * | 2017-09-27 | 2020-06-26 | 甘肃稀土新材料股份有限公司 | Samarium-cerium-based polishing powder and preparation process thereof |
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