CN114735743A - CeO with polyhedral morphology2Granules and process for their preparation - Google Patents
CeO with polyhedral morphology2Granules and process for their preparation Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 47
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000012695 Ce precursor Substances 0.000 claims abstract description 5
- 239000006210 lotion Substances 0.000 claims abstract description 4
- 239000002105 nanoparticle Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 25
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 235000011164 potassium chloride Nutrition 0.000 claims description 9
- 239000001103 potassium chloride Substances 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- 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 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 17
- 238000001878 scanning electron micrograph Methods 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 238000004321 preservation Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000001354 calcination Methods 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
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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
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- 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
- C01F17/10—Preparation or treatment, e.g. separation or purification
-
- 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
-
- 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
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses CeO with polyhedral morphology2A method of preparing a particle comprising the steps of: grinding and mixing a cerium precursor and a molten salt system according to a molar ratio of 1 (5-30) to obtain a mixture; step two, drying the mixture prepared in the step one, then placing the mixture into a tubular atmosphere furnace, introducing reducing atmosphere for roasting, wherein the roasting temperature system is that the temperature is increased to 700-900 ℃ at the speed of 5 ℃/min, preserving heat for 2h at the temperature, then reducing the temperature to 700 ℃ at the speed of 2 ℃/min, preserving heat for 2h, finally reducing the temperature to 500 ℃ at the speed of 2 ℃/min, then naturally cooling, and finally obtaining a precipitate which is CeO (CeO) from a product lotion after reaction2A nanoparticle; CeO prepared by the invention2The particles are in the shape of polyhedron, and polyhedron, octahedron and truncated octahedron CeO can be realized by controlling the atmosphere and temperature conditions2The preparation method of the invention selects the cheap raw materialsThe method has the advantages of simple price and process, short production period and suitability for large-scale production and preparation.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to CeO with polyhedral morphology2Granules and a process for their preparation.
Background
Cerium oxide, as a lanthanide rare earth oxide, has been widely studied and applied due to its unique crystal structure and electronic properties. A large number of researchers control the morphology, particle size and surface defect concentration of cerium oxide to remove CeO2The catalyst is applied to the aspects of degradation of dye, CO oxidation and the like. In addition, since CeO2The particles have appropriate mechanical properties and chemical activity, are widely used as rare earth polishing materials, and obviously improve SiO-pair ratio2Polishing efficiency and quality of the substrate material. Polishing powders of various specifications containing cerium oxide as a main component have been used in large quantities for polishing plate glasses and lenses. Furthermore, CMP slurries formulated based on nano/submicron cerium oxide abrasive particles are important semiconductor materials. Thus, research and development of CeO2The preparation process of the particles has great value in application prospect and economic benefit.
Many researchers are working on CeO2The patent CN111099650A discloses a method for preparing spherical CeO with the size of about 100-800nm by a molten salt method2The method of the nano powder, but the particles prepared by the method are all spherical in shape and have obvious agglomeration phenomenon. Research shows that the shape and size characteristics of CeO2The performance of the particles is greatly influenced, and the cerium oxide particles with the polyhedral morphology can obviously enhance CeO due to the exposure of specific crystal faces2The chemical activity of the particles and the morphology of the polyhedra in CMP applications can significantly improve material removal rates due to the specific contact behavior. Patent CN104176759A discloses a molten salt method for preparing cubic CeO2The method of nanoparticles, which requires accurately controlled process parameters, is difficult to prepare on a large scale. Therefore, the method develops the polyhedron CeO with cheap selected raw materials and simple process2Controllable preparation process of particles with high weightPractical significance and economic benefit.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide CeO with polyhedral morphology2Particle, preparation method thereof and prepared CeO2The particles have the characteristic of polyhedral morphology, and the raw materials are cheap and the preparation process is simple.
In order to achieve the purpose, the invention adopts the following technical scheme:
CeO with polyhedral morphology2A method of preparing a particle comprising the steps of:
grinding and mixing a cerium precursor and a molten salt system according to a molar ratio of 1 (5-30) to obtain a mixture;
the cerium precursor is any one of cerium nitrate hexahydrate, cerium carbonate, ammonium cerium nitrate or cerium sulfate;
the molten salt system is a binary molten salt prepared by taking any two of potassium chloride, sodium chloride, lithium chloride, sodium nitrate and potassium nitrate as raw materials according to the molar ratio of 1 (1-2);
step two, drying the mixture prepared in the step one, then placing the mixture into a tubular atmosphere furnace, introducing reducing atmosphere for roasting, wherein the roasting temperature system is that the temperature is increased to 700-900 ℃ at the speed of 5 ℃/min, preserving heat for 2h at the temperature, then reducing the temperature to 700 ℃ at the speed of 2 ℃/min, preserving heat for 2h, finally reducing the temperature to 500 ℃ at the speed of 2 ℃/min, then naturally cooling, and finally obtaining a precipitate which is CeO (CeO) from a product lotion after reaction2And (3) nanoparticles.
The invention also has the following technical characteristics:
preferably, the drying in the second step is drying for 3-5 hours at 50-80 ℃.
Preferably, the reducing atmosphere in the second step is any one of introduced argon, nitrogen, argon-hydrogen mixed gas or hydrogen, and the flow rate of the introduced gas is 30-120 ml/min.
Further, the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 5%.
Preferably, the lotion in the second step is washed 3-5 times by deionized water.
The invention also provides CeO with polyhedral morphology prepared by the method2Particles of the CeO2The particles are polyhedral, the particle size is uniformly distributed within the range of 100-700 nm, and the dispersibility is good.
Compared with the prior art, the invention has the following technical effects:
CeO prepared by the invention2The particles are in the shape of polyhedron, and polyhedron, octahedron and anoectoid CeO can be realized by controlling the atmosphere and temperature conditions2The controllable preparation of the particles can be realized by setting stepped cooling, the particle size of the prepared particles is uniform, the particle size of the prepared particles is 100-700 nm, and the obtained CeO with the polyhedral morphology2The particles have good application prospects in the fields of catalysis, polishing materials and the like;
the preparation method has the advantages of cheap raw materials, simple process and short production period, and is suitable for large-scale production and preparation.
Drawings
FIG. 1 shows CeO prepared in examples 1 to 52XRD pattern of the powder, wherein (a) - (d) are CeO prepared under the condition of introducing argon-hydrogen mixed gas2XRD pattern of powder, (e) CeO prepared under hydrogen condition2XRD spectrum of the powder;
FIG. 2 shows polyhedral CeO obtained by calcining at 700 ℃ for 4 hours in example 1 in an argon-hydrogen mixed gas atmosphere2SEM image of nanometer powder;
FIG. 3 shows polyhedral CeO obtained by calcining at 750 deg.C for 2h in the presence of mixed argon-hydrogen gas, cooling to 700 deg.C, and maintaining for 2h in example 22SEM image of nanometer powder;
FIG. 4 shows octahedral CeO obtained by calcining in example 3 at 800 deg.C for 2h in a mixed gas of argon and hydrogen, cooling to 700 deg.C, and keeping the temperature for 2h2SEM image of nanometer powder;
FIG. 5 shows the octahedral CeO removed by calcining at 900 deg.C for 2h in the presence of mixed argon-hydrogen gas, cooling to 700 deg.C, and keeping the temperature for 2h in example 42SEM image of nanometer powder;
FIG. 6 shows octahedral CeO obtained by calcining in example 5 at 800 deg.C for 2h in hydrogen gas atmosphere, cooling to 700 deg.C, and holding for 2h2SEM image of nanopowder.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
2.1711g (5mmol) of cerous nitrate hexahydrate, 1.8638g (25mmol) of potassium chloride and 1.4610g (25mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying for 5h at 50 ℃, then placing the crucible and the obtained mixture into a tubular atmosphere furnace filled with argon-hydrogen mixed gas for roasting, wherein the gas flow rate is 60ml/min, raising the temperature to 700 ℃ at the temperature rise rate of 5 ℃/min, roasting, keeping the temperature for 4h, and then reducing the temperature to 500 ℃ at the temperature drop rate of 2 ℃/min for natural cooling; washing the reaction product with deionized water to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And the powder, wherein the volume percentage of hydrogen in the argon-hydrogen mixed gas is 5%.
The SEM image is shown in FIG. 2, and the particles are polyhedral CeO particles of 100nm in size and are uniformly dispersed2And (3) granules.
Example 2
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
2.1711g (5mmol) of cerous nitrate hexahydrate, 1.8638g (25mmol) of potassium chloride and 1.4610g (25mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying at 80 deg.C for 3 hr, placing together with the crucible in a tubular atmosphere furnace filled with argon-hydrogen mixed gas, roasting at gas flow rate of 60ml/min, heating to 800 deg.C at a heating rate of 5 deg.C/min, maintaining for 2 hr, roasting at 2 deg.C/mReducing the in temperature to 700 ℃, preserving the temperature for 2h, then reducing the temperature to 500 ℃ at the cooling rate of 2 ℃/min, and naturally cooling; washing the reaction product with deionized water to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And powder, wherein the volume percentage of hydrogen in the argon-hydrogen mixed gas is 5%.
The SEM image is shown in FIG. 3, and the particles are octahedral CeO with a uniform dispersion size of 200-250 nm2And (3) particles.
Example 3
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
2.1711g (5mmol) of cerous nitrate hexahydrate, 1.8638g (25mmol) of potassium chloride and 1.4610g (25mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and performing magnetic stirring and uniform mixing; pouring the obtained mixture into a crucible, drying for 4h at 60 ℃, then placing the crucible and the obtained mixture into a tubular atmosphere furnace filled with argon-hydrogen mixed gas for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 850 ℃ at the heating rate of 5 ℃/min, roasting and heat preservation are carried out for 2h, the temperature is reduced to 700 ℃ at the temperature of 2 ℃/min, heat preservation is carried out for 2h, and then the temperature is reduced to 500 ℃ at the cooling rate of 2 ℃/min, and naturally cooling is carried out; washing the reaction product with deionized water to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And powder, wherein the volume percentage of hydrogen in the argon-hydrogen mixed gas is 5%.
The SEM image is shown in FIG. 4, and the particles are uniformly dispersed truncated octahedral CeO with the size of 300-350 nm2And (3) granules.
Example 4
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
2.1711g (5mmol) of cerous nitrate hexahydrate, 1.8638g (25mmol) of potassium chloride and 1.4610g (25mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; the obtained mixture was poured into a crucible, dried at 55 ℃ for 5 hours, and then calcined together with the crucible in a tube-type atmosphere furnace filled with argon-hydrogen mixed gas at a gas flow rate of 60mlMin, heating to 900 ℃ at the heating rate of 5 ℃/min, roasting, keeping the temperature for 2h, cooling to 700 ℃ at the temperature of 2 ℃/min, keeping the temperature for 2h, then cooling to 500 ℃ at the cooling rate of 2 ℃/min, and naturally cooling; washing the reaction product with deionized water to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And powder, wherein the volume percentage of hydrogen in the argon-hydrogen mixed gas is 5%.
The SEM image is shown in FIG. 5, and the particles are uniformly dispersed truncated octahedral CeO with the size of 600-700 nm2And (3) granules.
Example 5
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
2.1711g (5mmol) of cerous nitrate hexahydrate, 1.8638g (25mmol) of potassium chloride and 1.4610g (25mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and performing magnetic stirring and uniform mixing; pouring the obtained mixture into a crucible, drying for 3.5h at 70 ℃, then placing the crucible and the obtained mixture into a tubular atmosphere furnace filled with hydrogen for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 800 ℃ at the temperature rising rate of 5 ℃/min, roasting and heat preservation are carried out for 2h, the temperature is reduced to 700 ℃ at the temperature rising rate of 2 ℃/min, heat preservation is carried out for 2h, and then the temperature is reduced to 500 ℃ at the temperature lowering rate of 2 ℃/min, and naturally cooling is carried out; washing with deionized water for 3 times after reaction to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And (3) powder.
The SEM image is shown in FIG. 6, and the particles are octahedral CeO with a uniform dispersion size of 200-250 nm2And (3) granules.
Example 6
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
1.3808g (3mmol) of hydrated cerium carbonate, 1.8198g (18mmol) of potassium nitrate and 0.6709g (9mmol) of potassium chloride are weighed and appropriately ground to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; the obtained mixture is poured into a crucible, dried for 4 hours at 65 ℃, then placed in a tubular atmosphere furnace which is filled with argon together with the crucible for roasting, the gas flow rate is 120ml/min,heating to 800 ℃ at a heating rate of 5 ℃/min, roasting, keeping the temperature for 2h, cooling to 700 ℃ at a temperature of 2 ℃/min, keeping the temperature for 2h, cooling to 500 ℃ at a cooling rate of 2 ℃/min, and naturally cooling; washing the reaction product with deionized water to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And (3) powder.
Example 7
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
1.645g (3mmol) of ammonium ceric nitrate, 3.8246g (45mmol) of sodium nitrate and 2.6298g (45mmol) of sodium chloride were weighed and ground appropriately to fine powder; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying for 3h at 60 ℃, then placing the crucible and the mixture into a nitrogen-filled tubular atmosphere furnace for roasting, wherein the gas flow rate is 30ml/min, the temperature is increased to 800 ℃ at the temperature rise rate of 5 ℃/min, the roasting and heat preservation are carried out for 2h, the temperature is reduced to 700 ℃ at the temperature rise rate of 2 ℃/min, the heat preservation is carried out for 2h, and then the temperature is reduced to 500 ℃ at the temperature reduction rate of 2 ℃/min, and the mixture is naturally cooled; washing with deionized water for 4 times after reaction to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And (3) powder.
Example 8
CeO with polyhedral morphology2The preparation method of the particles comprises the following specific process steps:
4.3422g (10mmol) of cerous nitrate hexahydrate, 2.2366g (30mmol) of potassium chloride and 1.1688g (20mmol) of sodium chloride are weighed respectively and ground properly to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying for 4h at 55 ℃, then placing the crucible and the obtained mixture into a tubular atmosphere furnace filled with argon-hydrogen mixed gas for roasting, wherein the gas flow rate is 60ml/min, raising the temperature to 800 ℃ at the temperature rise rate of 5 ℃/min, keeping the temperature for 2h, reducing the temperature to 700 ℃ at the temperature rise rate of 2 ℃/min, keeping the temperature for 2h, and then reducing the temperature to 500 ℃ at the temperature fall rate of 2 ℃/min for natural cooling; washing with deionized water for 5 times after reaction to obtain white precipitate which is CeO2Granulating, and drying to obtain CeO2And powder, wherein the volume percentage of hydrogen in the argon-hydrogen mixed gas is 5%.
The above specific embodiments are only examples selected for clearly illustrating the effects achieved by the present invention, and are not to be considered as all embodiments of the present invention, and it is obvious to those skilled in the art that other variations may be made on the basis of the above description of the embodiments, and the embodiments are not exhaustive, and any numerical changes that are introduced under the principle of the present invention still fall within the scope of the claims.
Claims (6)
1. CeO with polyhedral morphology2A method for preparing particles, comprising the steps of:
grinding and mixing a cerium precursor and a molten salt system according to a molar ratio of 1 (5-30) to obtain a mixture;
the cerium precursor is any one of cerium nitrate hexahydrate, cerium carbonate, ammonium cerium nitrate or cerium sulfate;
the molten salt system is a binary molten salt prepared by taking any two of potassium chloride, sodium chloride, lithium chloride, sodium nitrate and potassium nitrate as raw materials according to the molar ratio of 1 (1-2);
step two, drying the mixture prepared in the step one, placing the mixture into a tubular atmosphere furnace, introducing reducing atmosphere for roasting, heating to 700-900 ℃ at the temperature of 5 ℃/min according to a roasting temperature schedule, preserving heat for 2h at the temperature, cooling to 700 ℃ at the cooling rate of 2 ℃/min according to a cooling rate of 2 ℃/min, preserving heat for 2h, cooling to 500 ℃ at the cooling rate of 2 ℃/min, naturally cooling, and obtaining precipitates, namely CeO, of the product lotion obtained after the reaction2And (3) nanoparticles.
2. CeO with polyhedral morphology according to claim 12The preparation method of the particles is characterized in that the drying in the step two is drying for 3-5 hours at 50-80 ℃.
3. CeO with polyhedral morphology according to claim 12The preparation method of the particles is characterized in that the reducing atmosphere in the step two is argon, nitrogen and argon-hydrogen mixed gas orThe flow rate of the introduced gas in any one of the hydrogen gases is 30-120 ml/min.
4. CeO with polyhedral morphology according to claim 32The preparation method of the particles is characterized in that the volume percentage of the hydrogen in the argon-hydrogen mixed gas is 5 percent.
5. CeO with polyhedral morphology according to claim 12The preparation method of the particles is characterized in that the detergent in the step two is washed for 3-5 times by deionized water.
6. CeO with polyhedral morphology prepared by the method of any one of claims 1 to 52Particles, characterized in that the CeO2The particles are polyhedral, the particle size is uniformly distributed within the range of 100-700 nm, and the dispersibility is good.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080132403A1 (en) * | 2004-07-29 | 2008-06-05 | Jun-Seok Nho | Cerium Oxide Power and Process for Producing the Same |
| WO2016106765A1 (en) * | 2014-12-29 | 2016-07-07 | 尹先升 | Method for preparing cerium oxide crystals and cmp polishing application thereof |
| CN111099650A (en) * | 2020-01-21 | 2020-05-05 | 江苏理工学院 | CeO2Molten salt method for synthesizing nano spherical particles |
| CN114032034A (en) * | 2021-12-06 | 2022-02-11 | 陕西科技大学 | CeO for chemical mechanical polishing2Method for producing abrasive particles and use thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080132403A1 (en) * | 2004-07-29 | 2008-06-05 | Jun-Seok Nho | Cerium Oxide Power and Process for Producing the Same |
| WO2016106765A1 (en) * | 2014-12-29 | 2016-07-07 | 尹先升 | Method for preparing cerium oxide crystals and cmp polishing application thereof |
| CN111099650A (en) * | 2020-01-21 | 2020-05-05 | 江苏理工学院 | CeO2Molten salt method for synthesizing nano spherical particles |
| CN114032034A (en) * | 2021-12-06 | 2022-02-11 | 陕西科技大学 | CeO for chemical mechanical polishing2Method for producing abrasive particles and use thereof |
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