CN108083316B - Preparation method of nano rare earth oxide powder - Google Patents
Preparation method of nano rare earth oxide powder Download PDFInfo
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- CN108083316B CN108083316B CN201611055990.4A CN201611055990A CN108083316B CN 108083316 B CN108083316 B CN 108083316B CN 201611055990 A CN201611055990 A CN 201611055990A CN 108083316 B CN108083316 B CN 108083316B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a preparation method of a nanometer rare earth oxide, which comprises the following steps: 1) respectively mixing rare earth salt and a precipitator with a betaine surfactant to obtain solutions A and B; 2) mixing the solution A, B to obtain rare earth precipitate; 3) calcining the rare earth precipitate obtained in the step 2) to prepare the nano rare earth oxide. The betaine surfactant is added in the preparation method, the surface tension of the solution can be effectively reduced, the agglomeration phenomenon of nano particles is improved, the surfactants with different concentrations can form micelles with different structures in the aqueous solution and become templates, so that the morphology and the size of the nano powder material are controlled, and the nano rare earth oxide with uniform and controllable morphology is obtained.
Description
Technical Field
The invention belongs to the technical field of nano rare earth powder, and particularly relates to a preparation method of nano rare earth oxide powder.
Background
The nanometer material has different unique properties from individual material, and thus has wide application in electricity, optics, biology, medicine and other fields. Due to the unique 4f electronic structure, the rare earth element brings excellent performances in the aspects of light, electricity, magnetism and the like, is considered as a new light source, a new magnetic source, a new energy source, a new treasure house of materials, and is also a vitamin for transforming the traditional industry and improving the traditional products. The rare earth oxide is an important raw material for preparing a novel nonmetal rare earth material, and the nanometer rare earth oxide combines the dual characteristics of rare earth and nanometer, so that the performance of the material can be greatly improved.
The method for preparing the nanometer rare earth oxide mainly comprises a solid phase synthesis method, a hydrothermal synthesis method, a sol-gel method, a spray pyrolysis method, a micro-emulsion method, a precipitation method and the like. The granularity and the dispersibility of the product produced by the solid-phase synthesis method are difficult to meet the requirements, and although the high-quality nano product can be prepared by a hydrothermal method, a sol-gel method, a spray pyrolysis method, a microemulsion method and the like, the large-scale production is difficult due to the problems of high cost, low efficiency, long period and the like (reference: Hongguangyi 'preparation and assembly of nano rare earth materials' China rare earth academy 2006, page number). So far, the precipitation method is still the optimal choice for preparing the nano oxide powder, the precipitation method can very accurately control the chemical composition of the material, simultaneously, the cost of raw materials is low, the requirement on equipment is lower, the process is simple, the operation is convenient, and the prepared product has high surface activity and high purity. However, the precipitation method has many nuclei and fine particles during precipitation, and is easy to agglomerate under the action of coulomb force, van der waals force and various chemical bonds, the morphology is difficult to control, and the product loses the nanometer characteristic, so that the solution of the agglomeration problem and the morphology control during the preparation of the nanometer material by the precipitation method become the key research point at present.
At present, some patents report that the surfactant is used for modifying and precipitating to prepare the nano powder. In patent CN101683999A, surfactant polyethylene glycol or sodium oleate is used to obtain cerium oxide with particle size of 300-450nm, but no figure for morphological analysis is available; in patent CN103449496A, cetyl trimethyl ammonium bromide is used as surfactant, urea is used as precipitant, and hydrothermal precipitation is used to prepare cerium oxide powder of 5-6 nm, but the agglomeration phenomenon still exists in the electron microscope picture. In the patent CN201410193490.1, ethylene diamine is used as a template agent, urea is used as a raw material, and a hydrothermal method is used for preparing hexagonal nano flaky cerium oxide, but the hydrothermal method is difficult to produce in batches and cannot be popularized in industrial production; patent CN103539195A adopts sulfate or bisulfate as electrostatic stabilizer, ethyl orthosilicate as surfactant, and nanometer yttrium oxide powder with narrow particle size distribution is prepared by precipitation method, but no figure analysis picture is seen. CN1150130C patent uses ammonium bicarbonate as precipitant, and adds surfactant in generated rare earth carbonate precursorSodium dodecyl sulfate, oleic acid and polyvinyl alcohol, heating to form solid foam, and calcining to obtain D50The nano rare earth oxide with the particle size less than 400nm still has agglomeration phenomenon. Therefore, the addition of the surfactant is an effective method for solving the problem of particle agglomeration in the precipitation process, and the reason is mainly that the proper surfactant can form a molecular film on the surfaces of the particles, so that the mutual contact among the particles is prevented, the surface tension is reduced, the capillary adsorption force is reduced, and the steric hindrance effect can be generated. The method mentioned in the above patent can only prepare nanopowder with a single morphology in the same system, cannot obtain nanoparticles with different morphologies by changing conditions, and has non-uniform particle morphology.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a method for preparing a nano rare earth oxide, which can solve the problems of aggregation and morphology control of nanoparticles in a process of preparing a nano rare earth oxide by a precipitation method, and can form micelles with different structures and different concentrations in an aqueous solution by adjusting the concentration of a surfactant in a reaction system, thereby realizing preparation of nano rare earth oxides with different morphologies in the same system.
The purpose of the invention is realized by the following technical scheme:
the preparation method of the nanometer rare earth oxide is characterized by comprising the following steps:
1) mixing rare earth salt and a precipitator with a betaine surfactant respectively to obtain a solution A and a solution B;
2) mixing the solution A prepared in the step 1) with the solution B to obtain rare earth precipitate;
3) calcining the rare earth precipitate obtained in the step 2) to obtain the nano rare earth oxide.
According to the present invention, the betaine type surfactant refers to an amphoteric surfactant having a betaine structure, and preferably, the chemical structural formula of the betaine type surfactant is represented by formula (i):
wherein R is selected from C1-16Alkyl, -C1-16alkyl-NH2CO-C1-16Alkyl, -C1-16alkyl-NH2-C1-16Alkyl, -C1-16alkyl-SO2-C1-16An alkyl group.
Preferably, R is optionally selected from C6-16Alkyl, -C1-6alkyl-NH2CO-C6-16Alkyl, -C1-6alkyl-NH2-C6-16Alkyl, -C1-6alkyl-SO2-C6-16An alkyl group.
The betaine type surfactant is, for example, cocamidopropyl betaine.
According to the invention, in step 1), the rare earth salt is a single rare earth salt solution. The rare earth salt solution is selected from inorganic acid salt solutions of rare earth elements such as lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium and the like.
Preferably, the rare earth salt is an inorganic acid salt of a rare earth element, and is preferably one or more of soluble rare earth nitrate, chloride and sulfate.
Preferably, the concentration of the rare earth salt solution is 0.01-5 mol/L, more preferably 0.05-2.0 mol/L, and still more preferably 0.05-1.0 mol/L.
According to the invention, in step 1), the concentration of the surfactant in solution a or solution B is between the Critical Micelle Concentration (CMC) of the surfactant and 30 times the critical micelle concentration. The concentration of the surfactant is preferably the critical micelle concentration, 10 times the critical micelle concentration, or 20 times the critical micelle concentration of the surfactant.
According to the invention, in step 1), the precipitant is selected from one or more of ammonium carbonate, ammonium bicarbonate, oxalic acid, tartaric acid, ammonium citrate, sodium hydroxide, preferably ammonium bicarbonate.
According to the invention, in the step 1), the concentration of the precipitant solution is 0.05-1.0 mol/L, preferably 0.1-0.75 mol/L, and more preferably 0.1-0.5 mol/L.
According to the invention, in step 2), the mixing, preferably the dropwise addition of solution a to solution B, is carried out.
Wherein the dropping rate is 1-10 mL/min, preferably 1-5 mL/min.
According to the invention, in the step 2), the molar feeding ratio of the rare earth salt to the precipitant is 1: 1-10, preferably 1: 2-8, and more preferably 1: 3.5-6.
According to the invention, in the step 2), the reaction further comprises stirring and aging to obtain rare earth precipitate.
Wherein the stirring speed is 400-1000 rpm/min. The aging time is 1-24 h, preferably 2-12 h.
According to the invention, in the step 3), the calcination temperature is 500-1200 ℃, preferably 600-1100 ℃, and further preferably 700-1000 ℃; the calcination time is 0.5-8 h, preferably 1-6 h, and more preferably 1-4 h.
According to the invention, in the step 3), a pretreatment is required before the calcination, and the pretreatment comprises the steps of separating, purifying and drying the rare earth precipitate obtained in the step 2).
Wherein, the separation and purification specifically comprises the following steps: and purifying the rare earth precipitate by adopting a mode of firstly centrifuging and then filtering, washing the obtained precipitate for 2-5 times by using deionized water, and then washing for 2-6 times by using ethanol to obtain a rare earth precipitate filter cake.
Wherein the drying specifically comprises: and (3) drying the rare earth precipitate filter cake in a vacuum drying oven at 60-100 ℃ for 1-4 h in vacuum.
According to the invention, when the concentration of the surfactant is controlled to be equal to the CMC value, the prepared nano rare earth oxide is well dispersed spherical particles; when the concentration of the surfactant is controlled to be equal to 10 times of CMC, the prepared nano rare earth oxide is a leaf-shaped nano sheet with uniform appearance; when the concentration of the surfactant is controlled to be equal to or more than 20 times of CMC, the prepared nano rare earth oxide is in a quasi-spherical shape with good dispersion.
According to the present invention, when the surfactant concentration is controlled to be equal to its CMC value, the average particle size of the prepared well-dispersed spherical particles is, for example, 50 to 100 nm; when the concentration of the surfactant is controlled to be equal to 10 times of CMC, the prepared leaf-shaped nano-sheet has the leaf length of 8 microns, the leaf width of 4 microns and the thickness of 50 nanometers; when the surfactant concentration is controlled to be equal to or greater than 20 times CMC, the prepared quasi-spherical shape has an average particle size of, for example, 100 nm.
In the invention, in the same system, by changing the concentration of the surfactant, the surfactant can form micelles with different structures and different concentrations in an aqueous solution, so that the surface tension is obviously reduced, the micelle plays a role of a template, and the morphology of the nano particles is controlled by the micelle molecules with different structures, thereby obtaining nano products with different morphologies. Compared with the traditional precipitation method, only products with single appearance can be obtained in the same system, and the preparation method has important research significance.
The invention has the beneficial effects that:
the invention provides a preparation method of a nanometer rare earth oxide, wherein a betaine type surfactant is added in the preparation method, the addition of the betaine type surfactant can effectively reduce the surface tension of a solution and improve the agglomeration phenomenon of nanometer particles, and the surfactants with different concentrations can form micelles with different structures in an aqueous solution and become templates, so that the morphology and the size of a nanometer powder material are controlled, and the nanometer rare earth oxide with uniform and controllable morphology is obtained. The preparation method has the advantages of simple process, high controllability, short operation period, high production efficiency and low production cost, and can realize industrial production.
Drawings
FIG. 1 is a scanning electron micrograph of the nano-neodymium oxide prepared in example 1 (surfactant concentration equals CMC concentration).
FIG. 2 is a scanning electron micrograph of the nano-neodymium oxide prepared in example 2 (surfactant concentration equal to 10 times CMC concentration).
FIG. 3 is a scanning electron micrograph of the nano-neodymium oxide prepared in example 3 (surfactant concentration equal to 20 times CMC concentration).
Fig. 4 is a scanning electron micrograph of the nano yttrium oxide prepared in example 4 (surfactant concentration equals CMC concentration).
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the description of the present invention, and such equivalents also fall within the scope of the invention.
In the invention, an S-4800 Field Emission Scanning Electron Microscope (FESEM) is adopted to observe sample particles and appearance.
In the present invention, the Critical Micelle Concentration (CMC) of a surfactant was measured using a Sigma701 advanced extended surface tensiometer, KSV, finland.
In order to make the technical features and aspects of the present invention clearer, preferred embodiments of the present invention are described below, and the preferred embodiments described herein are only for illustrating and explaining the present invention and are not intended to limit the present invention.
In the embodiment of the invention, the rare earth raw material is commercially available high-purity neodymium chloride with the purity of 99.999%.
In the present embodiment, the betaine surfactant used is cocamidopropyl betaine having the formula (II):
the cocamidopropyl betaine is a zwitterionic liquid, and the CMC value is measured to be 0.001 mol/L.
Example 1
1) To 100ml of a 0.5mol/L neodymium chloride solution, 0.034g of cocamidopropyl betaine was added to prepare a solution A, and to 350ml of a 0.5mol/L ammonium bicarbonate solution, 0.120g of cocamidopropyl betaine was added to prepare a solution B. The concentration of cocamidopropyl betaine in the solution was made 0.001 mol/L.
2) Dropwise adding the solution A prepared in the step 1) into the solution B at the speed of 1mL/min to obtain a rare earth precipitate. Stirring the reaction system at the speed of 600rpm in the dripping process, continuing stirring for 1 hour after the dripping is finished, then aging for 4 hours, filtering, washing for 2-5 times by using deionized water, and then washing for 2-6 times by using ethanol to obtain a precipitate filter cake. Putting the precipitate filter cake into a vacuum drying oven, and vacuum-drying at 80 ℃ for 4 hours.
3) Calcining the rare earth precipitate prepared in the step 2) to obtain the nano neodymium oxide powder. And putting the precipitate into a muffle furnace for calcining at 1000 ℃ for 3 hours.
As shown in figure 1, the prepared nanometer neodymium oxide is spherical and has an average particle size of 50 nanometers.
Example 2
1) To 100ml of a 0.5mol/L neodymium chloride solution, 0.34g of cocamidopropyl betaine was added to prepare a solution A, and to 350ml of a 0.5mol/L ammonium bicarbonate solution, 1.2g of cocamidopropyl betaine was added to prepare a solution B. The concentration of cocamidopropyl betaine in the solution was made 0.01 mol/L.
2) Dropwise adding the solution A prepared in the step 1) into the solution B at the speed of 1.5mL/min to obtain a rare earth precipitate. Stirring the reaction system at the speed of 700rpm in the dripping process, continuing stirring for 1 hour after the dripping is finished, then aging for 4 hours, filtering, washing for 2-5 times by using deionized water, and then washing for 2-6 times by using ethanol to obtain a precipitate filter cake. Putting the precipitate filter cake into a vacuum drying oven, and vacuum-drying for 4 hours at 100 ℃.
3) Calcining the rare earth precipitate prepared in the step 2) to obtain the nano neodymium oxide powder. And putting the precipitate into a muffle furnace for calcining at 1000 ℃ for 3 hours.
As shown in FIG. 2, the prepared nanometer neodymium oxide is leaf-shaped, the leaf length is 8 microns, the leaf width is 4 microns, and the thickness is 50 nanometers.
Example 3
1) To 100ml of a 0.5mol/L neodymium chloride solution, 0.68g of cocamidopropyl betaine was added to prepare a solution A, and to 350ml of a 0.5mol/L ammonium bicarbonate solution, 2.4g of cocamidopropyl betaine was added to prepare a solution B. The concentration of cocamidopropyl betaine in the solution was made 0.02 mol/L.
2) Dropwise adding the solution A prepared in the step 1) into the solution B at the speed of 1mL/min to obtain a rare earth precipitate. Stirring the reaction system at the speed of 800rpm in the dripping process, continuing stirring for 2 hours after the dripping is finished, then aging for 3 hours, filtering, washing for 2-5 times by using deionized water, and then washing for 2-6 times by using ethanol to obtain a precipitate filter cake. And putting the precipitate filter cake into a vacuum drying oven, and performing vacuum drying for 5 hours at 90 ℃.
3) Calcining the rare earth precipitate prepared in the step 2) to obtain the nano neodymium oxide powder. And putting the precipitate into a muffle furnace for calcining at 1000 ℃ for 3 hours.
As shown in FIG. 3, the prepared nano neodymium oxide is in a quasi-spherical shape, and the average particle size is 100 nm.
Example 4
1) To 100ml of 0.5mol/L yttrium chloride solution was added 0.034g of cocamidopropyl betaine to prepare solution A, and to 350ml of 0.5mol/L ammonium bicarbonate solution was added 0.120g of cocamidopropyl betaine to prepare solution B. The concentration of cocamidopropyl betaine in the solution was made 0.001 mol/L.
2) Dropwise adding the solution A prepared in the step 1) into the solution B at the speed of 1mL/min to obtain a rare earth precipitate. Stirring the reaction system at the speed of 500rpm in the dripping process, continuing stirring for 1 hour after the dripping is finished, then aging for 4 hours, filtering, washing for 2-5 times by using deionized water, and then washing for 2-6 times by using ethanol to obtain a precipitate filter cake. Putting the precipitate filter cake into a vacuum drying oven, and vacuum-drying at 80 ℃ for 4 hours.
3) Calcining the rare earth precipitate prepared in the step 2) to obtain the nano yttrium oxide powder. And putting the precipitate into a muffle furnace for calcining at 900 ℃ for 3 hours.
As shown in FIG. 4, the prepared nano yttrium oxide is spherical and has an average particle size of 100 nm.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (14)
1. The preparation method of the nanometer rare earth oxide is characterized by comprising the following steps:
1) mixing rare earth salt and a precipitator with a betaine surfactant respectively to obtain a solution A and a solution B;
2) mixing the solution A prepared in the step 1) with the solution B to obtain rare earth precipitate;
3) calcining the rare earth precipitate obtained in the step 2) to obtain a nano rare earth oxide;
in the step 1), in the solution A or the solution B, the concentration of the surfactant is 30 times of the critical micelle concentration of the surfactant;
wherein, when the concentration of the surfactant is controlled to be equal to the CMC value, the prepared nano rare earth oxide is spherical particles; when the concentration of the surfactant is controlled to be equal to 10 times of CMC, the prepared nano rare earth oxide is a leaf-shaped nano sheet; when the concentration of the surfactant is controlled to be equal to or more than 20 times of CMC, the prepared nano rare earth oxide is quasi-spherical.
2. The method according to claim 1, wherein the betaine type surfactant is represented by formula (I):
wherein R is selected from C1-16Alkyl, -C1-16alkyl-NH2CO-C1-16Alkyl, -C1-16alkyl-NH2-C1-16Alkyl, -C1-16alkyl-SO2-C1-16An alkyl group.
3. The method of claim 2, wherein R is optionally selected from C6-16Alkyl, -C1-6alkyl-NH2CO-C6-16Alkyl, -C1-6alkyl-NH2-C6-16Alkyl, -C1-6alkyl-SO2-C6-16An alkyl group.
4. The method according to claim 1, wherein in step 1), the rare earth salt solution is a single rare earth salt solution; wherein the rare earth salt solution is selected from inorganic acid salt solutions of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium.
5. The preparation method according to claim 1, wherein the inorganic acid salt of rare earth element is one or more selected from rare earth nitrate, chloride and sulfate.
6. The method according to claim 1, wherein the rare earth salt solution has a concentration of 0.01 to 5mol/L in step 1).
7. The method according to claim 1, wherein in step 1), the precipitant is selected from one or more of ammonium carbonate, ammonium bicarbonate, oxalic acid, tartaric acid, ammonium citrate, and sodium hydroxide.
8. The method according to claim 1, wherein in the step 1), the concentration of the precipitant solution is 0.05 to 1.0 mol/L.
9. The production method according to any one of claims 1 to 8, wherein in step 2), the mixing is performed by dropping the solution A into the solution B; the dropping rate is 1-10 mL/min.
10. The preparation method of claim 9, wherein in the step 2), the molar charge ratio of the rare earth salt to the precipitant is 1: 1-10.
11. The method according to any one of claims 1 to 8, wherein in step 3), the calcination temperature is 500 to 1200 ℃; the calcination time is 0.5-8 h.
12. The preparation method according to claim 11, wherein in the step 3), the calcination temperature is 600 to 1100 ℃; the calcination time is 1-6 h.
13. The method according to claim 12, wherein in the step 3), the calcination temperature is 700 to 1000 ℃; the calcination time is 1-4 h.
14. The preparation method according to claim 1, when the surfactant concentration is controlled to be equal to its CMC value, the average particle size of the prepared spherical particles is 50 to 100 nm; when the concentration of the surfactant is controlled to be equal to 10 times of CMC, the prepared leaf-shaped nanosheet is 8 microns in leaf length, 4 microns in leaf width and 50 nanometers in thickness; when the surfactant concentration was controlled to be equal to or greater than 20 times CMC, the prepared quasi-spherical shape had an average particle size of 100 nm.
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| CN110510654B (en) * | 2019-09-27 | 2022-06-14 | 中国恩菲工程技术有限公司 | Method for preparing micron-sized scandium carbonate |
| CN111017978A (en) * | 2019-12-27 | 2020-04-17 | 江西鑫泰功能材料科技有限公司 | Preparation method of nano holmium oxide for dielectric ceramic capacitor |
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| CN1704339A (en) * | 2004-06-03 | 2005-12-07 | 中南大学 | Process for preparing high purity active nano ceria |
| CN101834291A (en) * | 2010-04-09 | 2010-09-15 | 中南大学 | Preparation method of submicron level LiniO.5MnO.5O2 cathode material |
| CN105251421A (en) * | 2015-11-19 | 2016-01-20 | 天津城建大学 | Low-temperature preparation method for micron cerium oxide micro-ball |
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| CN1704339A (en) * | 2004-06-03 | 2005-12-07 | 中南大学 | Process for preparing high purity active nano ceria |
| CN101834291A (en) * | 2010-04-09 | 2010-09-15 | 中南大学 | Preparation method of submicron level LiniO.5MnO.5O2 cathode material |
| CN105251421A (en) * | 2015-11-19 | 2016-01-20 | 天津城建大学 | Low-temperature preparation method for micron cerium oxide micro-ball |
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