CN108083316A - A kind of preparation method of nano rareearth oxidate powder body - Google Patents
A kind of preparation method of nano rareearth oxidate powder body Download PDFInfo
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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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- 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
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- 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
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to a kind of preparation method of oxide nano rare earth, the preparation method includes the following steps：1) rare-earth salts and precipitating reagent with betaine type amphoteric surfactant are mixed respectively, obtains solution A and B；2) solution A, B are mixed to get rare-earth precipitation；3) rare-earth precipitation for obtaining step 2) is calcined, and oxide nano rare earth is prepared.Betaine type amphoteric surfactant is added in the preparation method, the addition of the betaine type amphoteric surfactant, solution surface tension can effectively be reduced, improve the agglomeration of nano particle, the surfactant of various concentration can form the micelle of different structure and in aqueous solution as template, so as to control the pattern of nano-powder material and size, the oxide nano rare earth of pattern uniform, controllable is obtained.
Description
Technical field
The invention belongs to nano rare earth powder technology fields, and in particular to a kind of preparation side of nano rareearth oxidate powder body
Method.
Background technology
Nano material is since it is with significantly different and individual material peculiar property, in electricity, optics, biology and medicine
Etc. have been widely used.Rare earth element brings light, electricity, magnetic etc. due to its unique 4f electronic structure for it
Excellent performance, it is considered to be new light sources, new magnetic source, new energy, the treasure-house of new material, while be also to rebuild traditional industry, promoted
" vitamin " of traditional product.Rare earth oxide is the important raw and processed materials for preparing non-metal kind rare earth new material, nano rare earth oxygen
Compound combines the double grading of rare earth and nanometer, is capable of the performance of significant increase material.
Preparing the method for oxide nano rare earth mainly has solid-phase synthesis, hydrothermal synthesis method, sol-gal process, spraying heat
Solution, microemulsion method and precipitation method etc..The product granularity and dispersiveness of the wherein described solid-phase synthesis production are extremely difficult to
It is required that although the nanometer that high quality can be prepared using hydro-thermal method, sol-gal process, spray pyrolysis, microemulsion method etc. is produced
Product, but since the problems such as of high cost, efficiency is low, the cycle is long is difficult to mass produce (bibliography：Hong Guangyan " nano rare earth materials
The preparation and assembling of material " China rare earth journal, 2006, the page number).So far, the precipitation method are still to prepare nano oxide powder
Optimal selection, the precipitation method can point-device control material chemical composition, while cost of material is low, the requirement for equipment
Relatively low, simple for process, easy to operate, product surface activity obtained is high, and purity is high.But the precipitation method due to precipitation when forming core compared with
More, particle is tiny, easily reunites under the action of Coulomb force, Van der Waals force and various chemical bonds, pattern is difficult to control, and makes product
Nano-meter characteristic is lost, therefore solves the agglomeration traits when precipitation method prepare nano material and pattern control to become current research weight
Point.
At present, preparing nano-powder using surfactant-modified precipitation has had some patent reports.Patent
CN101683999A obtains cerium oxide of the granularity in 300-450nm using surfactant polyethylene or enuatrol, but not
See morphology analysis picture；Patent CN103449496A is using cetyl trimethylammonium bromide as surfactant, using urea
Make precipitating reagent, 5-6 nanometers of ceria oxide powder is prepared for hydrothermal deposition method, but from its electron microscopic picture, there are still reunions
Phenomenon.For patent CN201410193490.1 using ethylenediamine as template, urea is raw material, and hexagonal nanosheet has been made in hydro-thermal method
Shape cerium oxide, but hydro-thermal method is produced in batches due to being difficult to, and can not promote industrial production；Patent CN103539195A uses sulfate
Or disulfate, as electrostatic stabilization agent, ethyl orthosilicate makees surfactant, it is relatively narrow to be prepared for particle diameter distribution with the precipitation method
Nano yttrium oxide powder, but have no morphology analysis picture.Patent CN1150130C is dilute in the carbonic acid of generation using ammonium bicarbonate as precipitating reagent
Surfactant sodium dodecyl base sodium sulfonate, oleic acid, polyvinyl alcohol are added in native precursor, solid foam is thermally formed, after calcining
Obtain D50Oxide nano rare earth less than 400nm, but still there are agglomerations.It can thus be seen that addition surface-active
Agent is to solve the effective ways of particle agglomeration in precipitation process, and reason is mainly that appropriate surfactant can be in particle surface
One layer of molecular film is formed, so as to hinder contacting with each other between particle and reduce surface tension, reduces capillary attraction
Power, and space steric effect can be generated.More than patent is previously mentioned method in same system, can only prepare the nanometer of single shape
Powder, it is impossible to the nano particle of different-shape is obtained by changing condition, and granule-morphology is inhomogenous.
The content of the invention
To solve the above-mentioned problems, it is an object of the invention to provide a kind of preparation method of oxide nano rare earth,
It can solve using during study of nanometer rare earth oxides prepared by precipitation methods, the reunion of nano particle and pattern control problem pass through
The concentration of surfactant in reaction system is adjusted, it is made to form the micella that structure is different, concentration is different in aqueous solution, is realized
Prepare under same system the oxide nano rare earth of different-shape.
The present invention seeks to what is be achieved through the following technical solutions：
A kind of preparation method of oxide nano rare earth, which is characterized in that the preparation method includes the following steps：
1) rare-earth salts and precipitating reagent with betaine type amphoteric surfactant are mixed respectively, obtains solution A and solution B；
2) solution A that step 1) is prepared with solution B is mixed, obtains rare-earth precipitation；
3) rare-earth precipitation for obtaining step 2) is calcined, and obtains oxide nano rare earth.
According to the present invention, the betaine type amphoteric surfactant refers to the amphoteric surfactant with betaine structure,
Preferably, shown in the chemical structural formula of the betaine type amphoteric surfactant such as formula (I)：
Wherein, R is optionally from C1-16Alkyl ,-C1-16Alkyl-NH2CO-C1-16Alkyl ,-C1-16Alkyl-NH2-C1-16Alkyl ,-
C1-16Alkyl-SO2-C1-16Alkyl.
Preferably, R is optionally from C6-16Alkyl ,-C1-6Alkyl-NH2CO-C6-16Alkyl ,-C1-6Alkyl-NH2-C6-16Alkyl ,-
C1-6Alkyl-SO2-C6-16Alkyl.
The betaine type amphoteric surfactant is, for example, Cocoamidopropyl betaine.
According to the present invention, in step 1), the rare-earth salts is single rare earth salting liquid.Wherein, the rare-earth salt solution
Inorganic acid salt solution selected from rare earth elements such as lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttriums.
Preferably, the rare-earth salts be rare earth element inorganic acid salt, preferably be selected from soluble rare earth nitrades, chlorate,
One or more of sulfate.
Preferably, the rare-earth salt solution concentration is 0.01~5mol/L, further preferably 0.05~2.0mol/L, more
Preferably 0.05~1.0mol/L.
According to the present invention, in step 1), in solution A or solution B, the concentration of the surfactant is surface-active
The critical micelle concentration (CMC) of agent is to 30 times of critical micelle concentrations.The concentration of the surfactant is preferably the surface-active
The critical micelle concentration of agent, 10 times of critical micelle concentrations or 20 times of critical micelle concentrations.
According to the present invention, in step 1), the precipitating reagent is selected from ammonium carbonate, ammonium hydrogen carbonate, oxalic acid, tartaric acid, lemon
One or more in sour ammonium, sodium hydroxide are preferably ammonium hydrogen carbonate.
According to the present invention, in step 1), the precipitant solution concentration is 0.05~1.0mol/L, preferably 0.1~
0.75mol/L, further preferably 0.1~0.5mol/L.
According to the present invention, in step 2), solution A is preferably added drop-wise in solution B by the mixing.
Wherein, the drop rate is 1~10mL/min, is preferably 1~5mL/min.
According to the present invention, in step 2), the molar feed ratio of the rare-earth salts and precipitating reagent is 1:1~10, preferably
For 1:2~8, further preferably 1:3.5~6.
According to the present invention, in step 2), the reaction still further comprises stirring, ageing, obtains rare-earth precipitation.
Wherein, the mixing speed is 400~1000rpm/min.The digestion time for 1~for 24 hours, be preferably 2~
12h。
According to the present invention, in step 3), the calcining heat is 500~1200 DEG C, is preferably 600~1100 DEG C, into
Preferably 700~1000 DEG C of one step；The calcination time is 0.5~8h, is preferably 1~6h, further preferably 1~4h.
According to the present invention, in step 3), also needed through pre-treatment before the calcining, the pre-treatment is included step 2) institute
Obtained rare-earth precipitation separation, purifies, dry.
Wherein, it is described separation, purification be specially：By rare-earth precipitation object using first centrifuge filter afterwards by the way of purify, to institute
It obtains sediment to be first washed with deionized 2~5 times, then washs 2~6 times with ethyl alcohol and obtain rare-earth precipitation object filter cake.
Wherein, the drying is specially：The rare-earth precipitation object filter cake is done in 60~100 DEG C of vacuum in vacuum drying chamber
Dry 1~4h.
According to the present invention, when control surface surfactant concentration is equal to its CMC value, prepared oxide nano rare earth is
Well dispersed spheric granules；When control surface surfactant concentration is equal to 10 times of CMC, prepared oxide nano rare earth is shape
The homogeneous leaf shape nanometer sheet of looks；When control surface surfactant concentration is equal to or more than 20 times of CMC, prepared nano rare earth oxygen
Compound is well dispersed torispherical.
According to the present invention, when control surface surfactant concentration is equal to its CMC value, prepared well dispersed spherical
The particle mean size of grain is, for example, 50-100 nanometers；When control surface surfactant concentration is equal to 10 times of CMC, prepared leaf shape
Nanometer sheet is, for example, 8 microns of leaf length, 4 microns of leaf width, 50 nanometers of thickness；When control surface surfactant concentration is equal to or more than 20
During times CMC, the particle mean size of prepared torispherical is, for example, 100 nanometers.
In the present invention, in same system, by changing the concentration of surfactant, surfactant can be made water-soluble
The micella that structure is different, concentration is different is formed in liquid, surface tension is not only significantly reduced, also acts as the effect of template, is led to
The micella molecule of different structure is crossed to control the pattern of nano-particle, so as to obtain the different nanometer product of pattern.Compared to
Traditional precipitation method, can only obtain the product of single shape in same system, and preparation method of the present invention has important
Research significance.
Beneficial effects of the present invention：
The present invention provides a kind of preparation method of oxide nano rare earth, betaine type table is added in the preparation method
Face activating agent, the addition of betaine type amphoteric surfactant can effectively reduce solution surface tension, and the reunion for improving nano particle shows
As the surfactant of various concentration can form the micelle of different structure and as template in aqueous solution, be received so as to control
The pattern and size of rice powder body material, obtain the oxide nano rare earth of pattern uniform, controllable.The preparation method technique letter
Single, highly controllable, the operation cycle is short, production efficiency is high, and production cost is low, it can be achieved that industrialized production.
Description of the drawings
Fig. 1 is that (it is dense that surfactant concentration is equal to CMC to Nanometer-sized Neodymium Oxide scanning electron microscope (SEM) photograph prepared in embodiment 1
Degree).
Fig. 2 is that (surfactant concentration is equal to 10 times of CMC to Nanometer-sized Neodymium Oxide scanning electron microscope (SEM) photograph prepared in embodiment 2
Concentration).
Fig. 3 is that (surfactant concentration is equal to 20 times of CMC to Nanometer-sized Neodymium Oxide scanning electron microscope (SEM) photograph prepared in embodiment 3
Concentration).
Fig. 4 is that (it is dense that surfactant concentration is equal to CMC to nano yttrium oxide scanning electron microscope (SEM) photograph prepared in embodiment 4
Degree).
Specific embodiment
With reference to specific embodiment, the present invention is further explained.It is to be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.Furthermore, it is to be understood that after recorded content of the invention has been read, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within limited range of the present invention.
In the present invention, sample particle and morphology observation are carried out using S-4800 field emission scanning electron microscopes (FESEM).
In the present invention, facing for surfactant is measured using Finland's KSV companies Sigma701 level expansions surface tension instrument
Boundary's micellar concentration (CMC).
In order to make the technical characterstic of the present invention and scheme clearer, preferable examples of the present invention will be described below,
Preferred embodiment described herein is merely to illustrate and explain the present invention, and is not intended to limit the present invention.
In present example, rare earths material used is commercially available 99.999% high-purity neodymium chloride.
In present example, the betaine type amphoteric surfactant used is Cocoamidopropyl betaine, and structural formula is such as
Shown in formula (II)：
The Cocoamidopropyl betaine is a kind of amphoteric ion liquid, measures its CMC value as 0.001mol/L.
Embodiment 1
1) 0.034g Cocoamidopropyl betaines are added into the neodymium chloride solution of 100mL0.5mol/L, preparation obtains
Solution A, 0.120g Cocoamidopropyl betaines are added in into the ammonium bicarbonate soln of 350ml0.5mol/L, and preparation obtains molten
Liquid B.It is 0.001mol/L to make the concentration of Cocoamidopropyl betaine in the solution.
2) solution A prepared by step 1) is added drop-wise to the speed of 1mL/min in solution B, obtains rare-earth precipitation object.Drop
System is stirred to react with the speed of 600rpm during adding, after completion of dropwise addition, continue stirring 1 it is small when, when rear ageing 4 is small, filtering,
It is first washed with deionized 2-5 times, then washs 2-6 times with ethyl alcohol and obtain sediment filter cake.Above-mentioned sediment filter cake is put into very
In empty drying box, when 80 DEG C of vacuum drying 4 are small.
3) the rare-earth precipitation object that step 2) is prepared is calcined, you can obtains Nanometer-sized Neodymium Oxide powder.Sediment is put into horse
It is not calcined in stove, calcining heat is 1000 DEG C, when the time is 3 small.
As shown in Figure 1, the Nanometer-sized Neodymium Oxide being prepared is spherical shape, particle mean size is 50 nanometers.
Embodiment 2
1) 0.34g Cocoamidopropyl betaines are added into the neodymium chloride solution of 100mL0.5mol/L, preparation obtains molten
Liquid A, 1.2g Cocoamidopropyl betaines are added in into the ammonium bicarbonate soln of 350ml0.5mol/L, and preparation obtains solution B.
It is 0.01mol/L to make the concentration of Cocoamidopropyl betaine in the solution.
2) solution A prepared by step 1) is added drop-wise to the speed of 1.5mL/min in solution B, obtains rare-earth precipitation object.
System is stirred to react with the speed of 700rpm during dropwise addition, after completion of dropwise addition, continue stirring 1 it is small when, when rear ageing 4 is small, mistake
Filter, is first washed with deionized 2-5 times, then washs 2-6 times with ethyl alcohol and obtain sediment filter cake.Above-mentioned sediment filter cake is put into
In vacuum drying chamber, when 100 DEG C of vacuum drying 4 are small.
3) the rare-earth precipitation object that step 2) is prepared is calcined, you can obtains Nanometer-sized Neodymium Oxide powder.Sediment is put into horse
It is not calcined in stove, calcining heat is 1000 DEG C, when the time is 3 small.
As shown in Fig. 2, the Nanometer-sized Neodymium Oxide being prepared is leaf shape, leaf grows 8 microns, and 4 microns of leaf width, thickness 50 is received
Rice.
Embodiment 3
1) 0.68g Cocoamidopropyl betaines are added into the neodymium chloride solution of 100mL0.5mol/L, preparation obtains molten
Liquid A, 2.4g Cocoamidopropyl betaines are added in into the ammonium bicarbonate soln of 350ml0.5mol/L, and preparation obtains solution B.
It is 0.02mol/L to make the concentration of Cocoamidopropyl betaine in the solution.
2) solution A prepared by step 1) is added drop-wise to the speed of 1mL/min in solution B, obtains rare-earth precipitation object.Drop
System is stirred to react with the speed of 800rpm during adding, after completion of dropwise addition, continue stirring 2 it is small when, when rear ageing 3 is small, filtering,
It is first washed with deionized 2-5 times, then washs 2-6 times with ethyl alcohol and obtain sediment filter cake.Above-mentioned sediment filter cake is put into very
In empty drying box, when 90 DEG C of vacuum drying 5 are small.
3) the rare-earth precipitation object that step 2) is prepared is calcined, you can obtains Nanometer-sized Neodymium Oxide powder.Sediment is put into horse
It is not calcined in stove, calcining heat is 1000 DEG C, when the time is 3 small.
As shown in figure 3, the Nanometer-sized Neodymium Oxide being prepared is torispherical, particle mean size 100nm.
Embodiment 4
1) 0.034g Cocoamidopropyl betaines are added into the yttrium chloride solution of 100mL0.5mol/L, preparation obtains
Solution A, 0.120g Cocoamidopropyl betaines are added in into the ammonium bicarbonate soln of 350ml0.5mol/L, and preparation obtains molten
Liquid B.It is 0.001mol/L to make the concentration of Cocoamidopropyl betaine in the solution.
2) solution A prepared by step 1) is added drop-wise to the speed of 1mL/min in solution B, obtains rare-earth precipitation object.Drop
System is stirred to react with the speed of 500rpm during adding, after completion of dropwise addition, continue stirring 1 it is small when, when rear ageing 4 is small, filtering,
It is first washed with deionized 2-5 times, then washs 2-6 times with ethyl alcohol and obtain sediment filter cake.Above-mentioned sediment filter cake is put into very
In empty drying box, when 80 DEG C of vacuum drying 4 are small.
3) the rare-earth precipitation object that step 2) is prepared is calcined, you can obtains nano yttrium oxide powder.Sediment is put into horse
It is not calcined in stove, calcining heat is 900 DEG C, when the time is 3 small.
As shown in figure 4, the nano yttrium oxide being prepared is spherical shape, particle mean size 100nm.
More than, embodiments of the present invention are illustrated.But the present invention is not limited to the above embodiments.It is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in the guarantor of the present invention
Within the scope of shield.
Claims (9)
1. a kind of preparation method of oxide nano rare earth, which is characterized in that the preparation method includes the following steps：
1) rare-earth salts and precipitating reagent with beet alkali surface activator are mixed respectively, obtains solution A and solution B；
2) solution A that step 1) is prepared with solution B is mixed, obtains rare-earth precipitation；
3) rare-earth precipitation for obtaining step 2) is calcined, and obtains oxide nano rare earth.
2. preparation method according to claim 1, which is characterized in that the betaine type amphoteric surfactant such as formula (I) institute
Show：
Wherein, R is optionally from C1-16Alkyl ,-C1-16Alkyl-NH2CO-C1-16Alkyl ,-C1-16Alkyl-NH2-C1-16Alkyl ,-C1-16Alkane
Base-SO2-C1-16Alkyl；Preferably, R is optionally from C6-16Alkyl ,-C1-6Alkyl-NH2CO-C6-16Alkyl ,-C1-6Alkyl-NH2-
C6-16Alkyl ,-C1-6Alkyl-SO2-C6-16Alkyl.
3. preparation method according to claim 1 or 2, which is characterized in that in step 1), the rare-earth salt solution is single
One rare-earth salt solution；Wherein, the rare-earth salt solution preferably be selected from lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium,
The inorganic acid salt solution of the rare earth elements such as lutetium, yttrium.
4. according to the preparation method described in any one of claim 1-3 claim, which is characterized in that the rare earth element
Inorganic acid salt is selected from one or more of rare earth nitrades, chlorate, sulfate.
5. according to the preparation method described in any one of claim 1-4 claim, which is characterized in that in step 1), institute
Rare-earth salt solution concentration is stated as 0.01~5mol/L, further preferably 0.05~2.0mol/L, more preferably 0.05~
1.0mol/L。
6. according to the preparation method described in any one of claim 1-5 claim, which is characterized in that in step 1), molten
In liquid A or solution B, the concentration of surfactant for surfactant critical micelle concentration to 30 times of critical micelle concentrations；Institute
The concentration for stating surfactant is preferably the critical micelle concentration of the surfactant (CMC), 10 times of critical micelle concentrations (CMC)
Or 20 times of critical micelle concentrations (CMC).
7. according to the preparation method any one of claim 1-6, which is characterized in that in step 1), the precipitating reagent
One or more in ammonium carbonate, ammonium hydrogen carbonate, oxalic acid, tartaric acid, ammonium citrate, sodium hydroxide are preferably bicarbonate
Ammonium.
Preferably, in step 1), the precipitant solution concentration is 0.05~1.0mol/L, is preferably 0.1~0.75mol/
L, further preferably 0.1~0.5mol/L.
8. according to the preparation method described in any one of claim 1-7 claim, which is characterized in that in step 2), institute
Mixing is stated, for solution A is added drop-wise in solution B；The drop rate is 1~10mL/min, is preferably 1~5mL/min.
Preferably, in step 2), the molar feed ratio of the rare-earth salts and precipitating reagent is 1:1~10, it is preferably 1:2~8.
9. according to the preparation method described in any one of claim 1-8 claim, which is characterized in that in step 3), institute
Calcining heat is stated as 500~1200 DEG C, is preferably 600~1100 DEG C, further preferably 700~1000 DEG C；During the calcining
Between for 0.5~8h, preferably 1~6h, further preferably 1~4h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108752190A (en) * | 2018-06-27 | 2018-11-06 | 湖南稀土金属材料研究院 | The preparation method of double oxalate of rare earth ammonium and the preparation method of rare earth oxide |
| CN110510654A (en) * | 2019-09-27 | 2019-11-29 | 中国恩菲工程技术有限公司 | The method for preparing micron order 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 |
| CN111634935A (en) * | 2020-04-24 | 2020-09-08 | 广西科学院 | Microwave preparation method of nano rare earth oxide |
| CN114890451A (en) * | 2022-06-30 | 2022-08-12 | 北京印刷学院 | Preparation method of light nano yttrium oxide |
| CN114931661A (en) * | 2022-03-28 | 2022-08-23 | 上海威高医疗技术发展有限公司 | Amino acid/rare earth nanocrystalline/TPU (thermoplastic polyurethane) antibacterial wound dressing and preparation method thereof |
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