CN105565359A - Preparation method of superfine cerium oxide polishing powder adjustable in average grain diameter - Google Patents
Preparation method of superfine cerium oxide polishing powder adjustable in average grain diameter Download PDFInfo
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- CN105565359A CN105565359A CN201510966080.0A CN201510966080A CN105565359A CN 105565359 A CN105565359 A CN 105565359A CN 201510966080 A CN201510966080 A CN 201510966080A CN 105565359 A CN105565359 A CN 105565359A
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- cerium oxide
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- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
Disclosed is a preparation method of superfine cerium oxide polishing powder adjustable in average grain diameter. The micro-nano cerium oxide polishing powder is prepared by adopting a hydrothermal-calcining method. The preparation method includes: hydrothermally synthesizing cerium oxide Ce(IV) as a precursor; calcining and after-treating the precursor to obtain the polishing powder. Size and shape of the cerium oxide precursor are controlled by adjusting a hydrothermal reaction parameter (system pH value) so as to realize control on shape and granularity of the polishing powder. The cerium oxide polishing powder prepared is sphere-like, median grain diameter d 50 is adjustable between 100 nm-1.5 um, and granularity distribution R is greater than 0 and less than 0.8. The powder prepared by the method has good polishing effect on K9 glass.
Description
Technical field
The invention belongs to technical field of rare earth material preparation, relate to the precise polished preparation method with micro-nano cerium rouge.
Background technology
Chemically machinery polished (CMP) is one of the most effective planarization in high-accuracy optics and super large-scale integration manufacturing technology, the development of CMP technology cause to the polish abrasive with controlled physical property and chemical constitution in the urgent need to.Compared to SiO
2and Al
2o
3, CeO
2abrasive material have polishing speed high, to, the advantage such as glazed surface roughness low little by throwing surface damage, be widely used in that glass is precise polished, the polishing of super large-scale integration medium layer and monocrystalline silicon piece and semiconductor substrate materials polishing etc.
The parameter such as pattern, granularity, size-grade distribution of polishing powder directly affects by the surface property throwing workpiece.Modern precision optics and super large-scale integration need polishing workpiece surface finish to reach nano level rigors, there is larger challenge and limitation in tradition polish abrasive, and use submicron order and nano level polish abrasive to be inevitable development trend in polishing selectivity, surface accuracy, Stability of Slurry.
Chinese invention patent CN1699282A is with solubility cerium salt for raw material, and urea is precipitation agent, has prepared the spherical submicron cerium rouge of median size at about 300nm through precipitation from homogeneous solution and calcining.Chinese invention patent CN1821314A contacts containing cerium ion with alkaline matter with the solution of tensio-active agent, hierarchy of control pH value, generate throw out I, throw out I oxalic acid transforms, control reaction end pH value, be precipitated thing II, throw out II calcines and obtains fine cerium oxide polishing powder at 600 ~ 1000 DEG C, the method preparation process more complicated, the product cut size obtained is distributed between 10nm ~ 3 μm.Chinese invention patent CN101284983A with solubility cerium salt for raw material, the mixture of one or more in ammoniacal liquor, bicarbonate of ammonia, volatile salt is that presoma prepared by precipitation agent, by regulating the ionic strength of mother liquor of precipitation of ammonium, increase the surface electrical behavior of granular precursor, then sieve through high temperature ageing, filtration, drying, calcining, ball milling and obtain high, the ultra-fine cerium rouge of good dispersity, nodularization degree, the preparation process also more complicated of the method, obtained Granularity Distribution is between 20nm ~ 2 μm.
At present, the preparation of micro-nano cerium rouge adopts precipitation-calcination method mostly, and namely precipitator method synthesis Ce (III) throw out is as presoma, then calcines Ce (III) throw out and obtains CeO
2polishing powder, prepared Granularity Distribution is wider, still has difficulties in pattern and size controlling.
Summary of the invention
The present invention is directed to prior art deficiency, the preparation method of the micro-nano cerium rouge that a kind of pattern is even, narrow particle size distribution, median size are adjustable is provided, first Hydrothermal Synthesis cerium oxide Ce (IV) is as presoma, then presoma to be calcined and aftertreatment obtains polishing powder product, by regulating the form of Hydrothermal Synthesis state modulator presoma and size thus the control realized finished product cerium rouge form and granularity.The cerium rouge pattern utilizing the present invention to prepare for class spherical, median d50 is adjustable between 100nm ~ 1.5 μm, 0< size-grade distribution R<0.8.
Concrete synthesis step of the present invention is as follows:
1) Hydrothermal Synthesis cerium oxide precursor body: six water cerous nitrates and polyvinylpyrrolidone are dissolved in distilled water and form homogeneous mixture solotion, wherein Ce
3+concentration is 0.005 ~ 0.5mol/L, six water cerous nitrates and polyvinylpyrrolidone mass ratio are 1:0.25 ~ 1, stir lower acid or alkali regulator solution pH value to 2 ~ 8, then this solution is transferred in reactor, at 150 ~ 220 DEG C of temperature, react 4 ~ 24h, react complete, centrifugation, washing, gained solid product is cerium oxide precursor body; Polyvinylpyrrolidone molecular-weight average used is 10000 ~ 1300000; The acid used of regulator solution pH value is any one in nitric acid, hydrochloric acid, sulfuric acid, and alkali used is any one in sodium hydroxide, potassium hydroxide; By controlling Hydrothermal Synthesis system pH, the class spherical alumina cerium precursor that particle diameter is adjustable can be obtained.
2) presoma calcining and aftertreatment: presoma is fully dry at 45 ~ 65 DEG C of temperature, then at 600 ~ 1200 DEG C of calcining 0.5 ~ 6h, gained powder wet ball grinding 0.5 ~ 4h, then centrifugation, cryodrying obtain cerium rouge.
Get obtained cerium rouge and be made into solid content 0.5 ~ 5wt% polishing fluid, polishing fluid pH=~ 7, use UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) to carry out polishing to K9 glass; Calculating material removes speed (MRR) as follows,
MRR(nm/min)=(m
0-m)/(ρts)
Wherein m
0for the quality (g) of workpiece material before polishing, m is the quality (g) of workpiece material after polishing, and ρ is the density of K9 material, the contact area (cm of t to be polishing time (min), s be workpiece material and polishing pad
2).
Size-grade distribution of the present invention is defined as:
R=(d90-d10)/2d50
Wherein, d90 is the particle diameter that the diameter of 90% particle is less than d90; D50 is the particle diameter that the diameter of 50% particle is less than d50; D10 is the particle diameter that the diameter of 10% particle is less than d10.
Advantage of the present invention is: adopt hydrothermal-sintering process to prepare micro-nano cerium rouge, by regulating form and the size of hydro-thermal reaction parameter (system pH) controlled oxidization cerium precursor, thus realizes the control to finished product polishing powder form and granularity; Prepared cerium rouge is that class is spherical, and narrow particle size distribution, median size is adjustable, effective to K9 glass polishing.
Accompanying drawing explanation
Figure 1 – Fig. 4 is the SEM photo of Hydrothermal Synthesis cerium oxide precursor body under condition of different pH;
Fig. 5 is the presoma of embodiment 1 synthesis and the XRD spectra of this presoma calcining gained polishing powder;
Fig. 6 is the SEM photo of finished product cerium rouge prepared by embodiment 1.
Embodiment
Embodiment 1
Take 32.6gCe (NO
3)
3˙ 6H
2o and 16.8g polyvinylpyrrolidone (molecular-weight average 30000) is dissolved in 500ml water, drips 0.1mol/L sodium hydroxide solution to system pH=6.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 180 DEG C of reaction 18h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 65 DEG C of thermostat containers fully dry, then put into calcining furnace in 950 DEG C of calcinings 4h, the powder wet ball grinding 3h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=199nm, size-grade distribution R=0.286.Get a certain amount of powder and be made into 1wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=181.15nm/min.
Embodiment 2
Take 8.0gCe (NO
3)
3˙ 6H
2o and 8.0g polyvinylpyrrolidone (molecular-weight average 10000) is dissolved in 600ml water, drips 0.1mol/L ammoniacal liquor to system pH=4.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 220 DEG C of reaction 12h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 50 DEG C of thermostat containers fully dry, then put into calcining furnace in 600 DEG C of calcinings 3h, the powder wet ball grinding 1h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=683nm, size-grade distribution R=0.731.Get a certain amount of powder and be made into 0.5wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=131.61nm/min.
Embodiment 3
Take 86.8gCe (NO
3)
3˙ 6H
2o and 30.7g polyvinylpyrrolidone (molecular-weight average 58000) is dissolved in 500ml water, drips 0.1mol/L hydrochloric acid soln to system pH=2.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 160 DEG C of reaction 14h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 60 DEG C of thermostat containers fully dry, then put into calcining furnace in 1000 DEG C of calcinings 2h, the powder wet ball grinding 2h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=1.476 μm, size-grade distribution R=0.467.Get a certain amount of powder and be made into 3wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=145.82nm/min.
Embodiment 4
Take 46.2gCe (NO
3)
3˙ 6H
2o and 12.8g polyvinylpyrrolidone (molecular-weight average 1300000) is dissolved in 600ml water, drips 0.1mol/L potassium hydroxide solution to system pH=7.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 190 DEG C of reaction 7h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 45 DEG C of thermostat containers fully dry, then put into calcining furnace in 850 DEG C of calcinings 5h, the powder wet ball grinding 3h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=182nm, size-grade distribution R=0.786.Get a certain amount of powder and be made into 2wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=163.87nm/min.
Embodiment 5
Take 32.6gCe (NO
3)
3˙ 6H
2o and 16.8g polyvinylpyrrolidone (molecular-weight average 40000) is dissolved in 500ml water, drips 0.1mol/L sodium hydroxide solution to system pH=5.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 180 DEG C of reaction 24h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 65 DEG C of thermostat containers fully dry, then put into calcining furnace in 1050 DEG C of calcinings 4h, the powder wet ball grinding 4h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=327nm, size-grade distribution R=0.320.Get a certain amount of powder and be made into 5wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=168.53nm/min.
Embodiment 6
Take 12.6gCe (NO
3)
3˙ 6H
2o and 7.0g polyvinylpyrrolidone (molecular-weight average 360000) is dissolved in 500ml water, drips 0.1mol/L salpeter solution to system pH=3.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 200 DEG C of reaction 8h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 55 DEG C of thermostat containers fully dry, then put into calcining furnace in 1200 DEG C of calcinings 1h, the powder wet ball grinding 1h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=781nm, size-grade distribution R=0.641.Get a certain amount of powder and be made into 1wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=155.81nm/min.
Embodiment 7
Take 58.6gCe (NO
3)
3˙ 6H
2o and 41.4g polyvinylpyrrolidone (molecular-weight average 24000) is dissolved in 500ml water, drips 0.2mol/L sodium hydroxide solution to system pH=8.0 under stirring in above-mentioned solution, is then transferred in 1L reactor by this solution, at 170 DEG C of reaction 10h.React complete, carry out centrifugation to solid product, washing, obtains cerium oxide precursor body.Presoma is put into 50 DEG C of thermostat containers fully dry, then put into calcining furnace in 900 DEG C of calcinings 4h, the powder wet ball grinding 2h obtained, then centrifugation, cryodrying, obtain cerium rouge, this polishing powder median d50=108nm, size-grade distribution R=0.509.Get a certain amount of powder and be made into 0.7wt% polishing slurries (pH=~ 7), UNIPOL-802 type precise grinding polisher (Shenyang section is brilliant) is used to carry out polishing to K9 glass, rotating speed 130r/min, pressure 0.104MPa, 25 DEG C of polishing 1h, material removal rate MRR=146.51nm/min.
Claims (3)
1. a preparation method for the fine cerium oxide polishing powder that median size is adjustable, is characterized in that:
1) Hydrothermal Synthesis cerium oxide precursor body: six water cerous nitrates and polyvinylpyrrolidone are dissolved in distilled water and form homogeneous mixture solotion, wherein Ce
3+concentration is 0.005 ~ 0.5mol/L, six water cerous nitrates and polyvinylpyrrolidone mass ratio are 1:0.25 ~ 1, stir lower acid or alkali regulator solution pH value to 2 ~ 8, then this solution is transferred in reactor, at 150 ~ 220 DEG C of temperature, react 4 ~ 24h, react complete, centrifugation, washing, gained solid product is cerium oxide precursor body; Polyvinylpyrrolidone molecular-weight average used is 10000 ~ 1300000;
2) presoma calcining and aftertreatment: presoma is fully dry at 45 ~ 65 DEG C of temperature, then at 600 ~ 1200 DEG C of calcining 0.5 ~ 6h, gained powder wet ball grinding 0.5 ~ 4h, then centrifugation, cryodrying obtain cerium rouge.
2. the preparation method of the fine cerium oxide polishing powder that a kind of median size according to claim 1 is adjustable, is characterized in that: the acid used of described regulator solution pH value is any one in nitric acid, hydrochloric acid, sulfuric acid.
3. the preparation method of the fine cerium oxide polishing powder that a kind of median size according to claim 1 is adjustable, is characterized in that: described regulator solution pH value alkali used is any one in sodium hydroxide, potassium hydroxide.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
CN108117842A (en) * | 2016-11-30 | 2018-06-05 | 上海新昇半导体科技有限公司 | A kind of chemical mechanical polishing liquid and preparation method thereof |
CN108637925A (en) * | 2018-04-24 | 2018-10-12 | 安徽禾臣新材料有限公司 | A kind of precision optics polishing damping cloth and preparation method thereof |
CN108807943A (en) * | 2018-07-19 | 2018-11-13 | 齐鲁工业大学 | A kind of hollow-core construction CeO2@C core-shell structure copolymer nanocomposites and the preparation method and application thereof |
CN111117566A (en) * | 2018-10-31 | 2020-05-08 | 信越化学工业株式会社 | Polishing particle for polishing synthetic quartz glass substrate, method for producing same, and method for polishing synthetic quartz glass substrate |
CN113247941A (en) * | 2021-06-16 | 2021-08-13 | 四川大学 | Method for synthesizing uniform spherical nano cerium oxide material at low temperature |
CN115058199A (en) * | 2022-08-18 | 2022-09-16 | 广东粤港澳大湾区黄埔材料研究院 | High-dispersion ball-like nano cerium oxide polishing solution and application thereof |
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Cited By (13)
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CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
CN106044829B8 (en) * | 2016-05-25 | 2018-11-27 | 赣州湛海工贸有限公司 | A kind of preparation method of white pure zirconia cerium |
CN106044829B (en) * | 2016-05-25 | 2018-03-23 | 南昌大学 | A kind of preparation method of white pure zirconia cerium |
CN108117842A (en) * | 2016-11-30 | 2018-06-05 | 上海新昇半导体科技有限公司 | A kind of chemical mechanical polishing liquid and preparation method thereof |
CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
CN108637925A (en) * | 2018-04-24 | 2018-10-12 | 安徽禾臣新材料有限公司 | A kind of precision optics polishing damping cloth and preparation method thereof |
CN108637925B (en) * | 2018-04-24 | 2020-08-04 | 安徽禾臣新材料有限公司 | Damping cloth for polishing precision optical device and preparation method thereof |
CN108807943A (en) * | 2018-07-19 | 2018-11-13 | 齐鲁工业大学 | A kind of hollow-core construction CeO2@C core-shell structure copolymer nanocomposites and the preparation method and application thereof |
CN108807943B (en) * | 2018-07-19 | 2020-12-25 | 齐鲁工业大学 | CeO with hollow structure2@ C core-shell nano composite material and preparation method and application thereof |
CN111117566A (en) * | 2018-10-31 | 2020-05-08 | 信越化学工业株式会社 | Polishing particle for polishing synthetic quartz glass substrate, method for producing same, and method for polishing synthetic quartz glass substrate |
CN113247941A (en) * | 2021-06-16 | 2021-08-13 | 四川大学 | Method for synthesizing uniform spherical nano cerium oxide material at low temperature |
CN115058199A (en) * | 2022-08-18 | 2022-09-16 | 广东粤港澳大湾区黄埔材料研究院 | High-dispersion ball-like nano cerium oxide polishing solution and application thereof |
CN115058199B (en) * | 2022-08-18 | 2022-11-15 | 广东粤港澳大湾区黄埔材料研究院 | High-dispersion ball-like nano cerium oxide polishing solution and application thereof |
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