CN117361601A - Method for preparing nano yttrium oxide powder by solid phase grinding - Google Patents
Method for preparing nano yttrium oxide powder by solid phase grinding Download PDFInfo
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- CN117361601A CN117361601A CN202311412031.3A CN202311412031A CN117361601A CN 117361601 A CN117361601 A CN 117361601A CN 202311412031 A CN202311412031 A CN 202311412031A CN 117361601 A CN117361601 A CN 117361601A
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- 239000000843 powder Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 42
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000227 grinding Methods 0.000 title claims abstract description 15
- 239000007790 solid phase Substances 0.000 title claims abstract description 14
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 27
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 150000003746 yttrium Chemical class 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 238000002844 melting Methods 0.000 claims abstract description 9
- 239000011858 nanopowder Substances 0.000 claims abstract description 6
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 14
- -1 polyoxypropylene Polymers 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 8
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical group C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 6
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 229920001983 poloxamer Polymers 0.000 claims description 6
- 229960000502 poloxamer Drugs 0.000 claims description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims description 6
- JRKVGRAQLBXGQB-UHFFFAOYSA-K yttrium(3+);triacetate;hydrate Chemical compound O.[Y+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JRKVGRAQLBXGQB-UHFFFAOYSA-K 0.000 claims description 6
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 3
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 5
- 238000004438 BET method Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000002296 dynamic light scattering Methods 0.000 description 4
- 238000005118 spray pyrolysis Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01F17/218—Yttrium oxides or hydroxides
-
- 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
-
- 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
- C01P2004/01—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
- C01P2004/30—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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing nano yttrium oxide powder by solid-phase grinding, which comprises the steps of dispersing low-melting yttrium salt by using a molten dispersing agent, uniformly dispersing yttrium element on a dispersing agent matrix by vacuum heating decomposition, obtaining non-agglomerated yttrium precursor powder with high dispersity, and finally obtaining the nano yttrium oxide powder by a calcination process. The particle size of the yttrium oxide nano-powder prepared by the invention is 50-650 nm, and the specific surface area is 10-200 m 2 And/g, can be applied to the fields of electronic ceramic materials, fluorescent materials, other functional ceramics and the like.
Description
Technical field:
the invention relates to a method for preparing nanometer yttrium oxide powder by solid phase grinding.
The background technology is as follows:
yttrium oxide is an important rare earth oxide, and can be applied to the fields of optical glass, electronic ceramic materials, fluorescent materials and the like, and can also be used for manufacturing film capacitors, special refractory materials, magnetic bubble materials of high-pressure mercury lamps, lasers, storage elements and the like.
The preparation method of yttrium oxide is more, mainly comprises a precipitation method, a hydrothermal method, a sol-gel method, a spray pyrolysis method and the like. (1) The precipitation method is one of the most common methods in industry, and is generally to dissolve inorganic salts of yttrium element in water, then add a precipitant to precipitate yttrium ions out of the solution, collect and wash the precipitate, and then calcine to obtain yttrium oxide powder. The precipitation method has the advantages of simple process, low cost and the like, but the prepared yttrium oxide powder has the defects of large secondary particle size, poor particle size dispersibility, serious agglomeration, poor sintering activity and the like. (2) The hydrothermal method for preparing yttrium oxide is divided into a hydrothermal hydrolysis method and a hydrothermal precipitation method, and the hydrothermal precipitation method generally used in industrial production adopts high-temperature and high-pressure resistant reaction kettle equipment, and is characterized in that an aqueous solution containing an yttrium source and a precipitant is heated and pressurized, and after a long reaction time of precipitation, dissolution and recrystallization, a reaction precipitate is obtained, and then the reaction precipitate is washed and dried to obtain the nano yttrium oxide powder. The powder material prepared by the hydrothermal precipitation method has the advantages of good crystal form, high purity, small secondary particle size, small agglomeration degree, good sintering activity, high equipment requirement by the hydrothermal precipitation method, difficult control of technological parameters, long production period and the like. (3) Sol-gel process is also a common process for preparing yttrium oxide, which is generally to add complexing agent into aqueous solution containing yttrium element, form sol solution under certain condition, gel yttrium precursor gel after long-time gelation, and then calcine to obtain yttrium oxide powder. The method has the advantages of good crystal form, small secondary particle size, narrow particle size distribution, high activity, long period of sol in the gel process, high shrinkage rate caused by easy agglomeration during drying, complex operation and the like of the prepared powder. (4) The spray pyrolysis method is to spray a metal salt solution containing yttrium ions into a high-temperature air atmosphere at a high speed in the form of mist droplets, at this time, evaporation of a solvent and thermal decomposition of yttrium salt are immediately caused, and then a solid phase is separated out due to supersaturation, so that yttrium oxide nano-powder is directly obtained. The spray pyrolysis method for preparing the nano powder has the advantages of simple preparation, convenient operation and good controllability, but industrialization is still difficult to realize due to the fact that the thermal decomposition temperature of yttrium salt is high, equipment is corrosive, and the requirement on spray pyrolysis equipment is high.
The invention comprises the following steps:
the invention aims to provide a method for preparing nano yttrium oxide powder by solid phase grinding.
The invention is realized by the following technical scheme:
a method for preparing nano yttrium oxide powder by solid phase grinding comprises the following steps:
(1) The yttrium salt with low melting point and the dispersant with low melting point are mixed according to the mass ratio of 2-4: 1, mixing in a clean mortar, and grinding and dispersing at 50-70 ℃ to obtain a colloidal mixture of yttrium salt and a dispersing agent which are uniformly mixed; the low-melting-point yttrium salt is selected from one of yttrium nitrate hexahydrate and yttrium acetate hydrate, and the low-melting-point dispersing agent is poloxamer F127 or polyoxypropylene polyoxyethylene copolymer P123;
(2) Rapidly transferring the colloidal mixture obtained in the step (1) into a vacuum drying oven, heating to the decomposition temperature of yttrium salt of 180-240 ℃ in vacuum with the vacuum degree of 0.1-10 Pa, preferably 200-240 ℃, and preserving the temperature for 1-2 h to decompose the colloidal mixture to obtain yttrium precursor powder;
(3) And carrying out heat treatment on yttrium precursor powder at 600-900 ℃ in an air atmosphere to obtain yttrium oxide nano-powder.
Preferably, the mass ratio of yttrium salt to dispersant in the step (1) is 2.5:1.
preferably, the specific steps of the step (3) are as follows: transferring yttrium precursor powder into a muffle furnace, heating to 400 ℃ at a speed of 5 ℃/min under an air atmosphere, preserving heat for 1-2 hours, heating to 600-900 ℃ at a speed of 1-5 ℃/min, and preserving heat for 1-3 hours.
More preferably, the specific step of step (3) is: transferring yttrium precursor powder into a muffle furnace, heating to 400 ℃ at a speed of 5 ℃/min under the air atmosphere, preserving heat for 1-2 hours, heating to 650-850 ℃ at a speed of 5 ℃/min, and preserving heat for 2-3 hours.
The solid-phase grinding method adopted by the invention is to grind yttrium salt with low melting point and dispersant with low melting point under solid phase, so that the yttrium salt is uniformly dispersed in the dispersant in a molten state, then the dispersant mixed with the yttrium salt is heated in vacuum, and finally the nanometer yttrium oxide powder is obtained after calcination treatment. The key point of the method is the melt dispersion of yttrium salt with low melting point. The yttrium metal ions are melted and dispersed in a specific dispersing agent method by a grinding method, so that the particle shape and size of yttrium oxide can be controlled more easily, and the method is simple to operate, easy to obtain raw materials and beneficial to industrial production.
The beneficial effects of the invention are as follows:
1. the invention uses the molten dispersing agent to disperse the yttrium salt with low melting point, then uniformly disperses yttrium element on the dispersing agent matrix through vacuum heating decomposition, can obtain the yttrium precursor powder with high dispersity and no agglomeration, and finally obtains the nanometer yttrium oxide powder through the calcination process.
2. The particle size of the yttrium oxide nano-powder prepared by the invention is 50-650 nm, and the specific surface area is 10-200 m 2 And/g, can be applied to the fields of electronic ceramic materials, fluorescent materials, other functional ceramics and the like.
Description of the drawings:
FIG. 1 is a scanning electron micrograph of yttria prepared in example 1 of the invention.
The specific embodiment is as follows:
the following is a further illustration of the invention and is not a limitation of the invention.
Example 1: method for preparing nano yttrium oxide by solid phase grinding
The method comprises the following steps:
(1) At room temperature and normal pressure, 19.15g of yttrium nitrate hexahydrate and 7.66g of poloxamer F127 are weighed and mixed in an agate mortar, heated in a ventilated drying oven at 60 ℃ for 20min, taken out and quickly ground until yttrium nitrate hexahydrate particles and poloxamer F127 powder are uniformly mixed into a white viscous colloidal mixture.
(2) Rapidly transferring the colloidal mixture into a vacuum drying oven, keeping the vacuum degree in the vacuum drying oven at 1Pa, keeping the temperature at 200 ℃ and preserving the temperature for 1h to obtain light yellow yttrium precursor powder.
(3) Heating the light yellow yttrium precursor powder to 400 ℃ at the speed of 5 ℃/min under the air atmosphere, preserving heat for 1 hour, heating to 750 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, cooling to room temperature along with a furnace, and taking out to obtain the nano yttrium oxide powder.
Performance detection is carried out on the yttrium oxide powder prepared in the embodiment, and the particle size measured by a laser dynamic light scattering method is D 50 Specific surface area of powder calculated by BET method of 142.21 m=0.127 μm 2 And/g, the scanning electron microscope (figure 1) shows that the scanning electron microscope is spherical, and the diameter is 521.74nm.
Example 2: method for preparing nano yttrium oxide by solid phase grinding
The method comprises the following steps:
(1) At room temperature and normal pressure, 12.77g of yttrium nitrate hexahydrate and 4.26g of polyoxypropylene polyoxyethylene copolymer P123 are weighed and mixed in an agate mortar, heated in a ventilated drying oven at 60 ℃ for 20min, taken out and quickly ground until yttrium nitrate hexahydrate particles and polyoxypropylene polyoxyethylene copolymer P123 powder are evenly mixed into a white viscous colloidal mixture.
(2) Rapidly transferring the colloidal mixture into a vacuum drying oven, keeping the vacuum degree in the vacuum drying oven at 1Pa, keeping the temperature at 200 ℃ and preserving the temperature for 1h to obtain light yellow yttrium precursor powder.
(3) Heating the light yellow yttrium precursor powder to 400 ℃ at the speed of 5 ℃/min under the air atmosphere, preserving heat for 1 hour, heating to 700 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, cooling to room temperature along with a furnace, and taking out to obtain the nano yttrium oxide powder.
Performance detection is carried out on the yttrium oxide powder prepared in the embodiment, and the particle size measured by a laser dynamic light scattering method is D 50 Specific surface area of powder calculated by BET method was 45.94 m=0.167 μm 2 And/g, the scanning electron microscope shows that the scanning electron microscope is in a sphere-like shape, and the diameter is about 640nm.
Example 3: method for preparing nano yttrium oxide by solid phase grinding
The method comprises the following steps:
(1) 13.3g of yttrium acetate hydrate and 5.32g of poloxamer F127 are weighed and mixed in an agate mortar at room temperature and normal pressure, heated in a ventilated drying oven at 60 ℃ for 20min, taken out and quickly ground until yttrium acetate hydrate particles and poloxamer F127 powder are uniformly mixed into a white viscous colloidal mixture.
(2) Rapidly transferring the colloidal mixture into a vacuum drying oven, keeping the vacuum degree in the vacuum drying oven at 1Pa, and keeping the temperature at 240 ℃ for 1h to obtain yellowish yttrium precursor powder.
(3) Heating the light yellow yttrium precursor powder to 400 ℃ at the speed of 5 ℃/min under the air atmosphere, preserving heat for 1 hour, heating to 650 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with a furnace, and taking out to obtain the nano yttrium oxide powder.
Performance detection is carried out on the yttrium oxide powder prepared in the embodiment, and the particle size measured by a laser dynamic light scattering method is D 50 Specific surface area of powder calculated by BET method of 64.08 m=0.104 μm 2 And/g, the scanning electron microscope shows that the particle is spherical, and the diameter is 358.57nm.
Example 4: method for preparing nano yttrium oxide by solid phase grinding
The method comprises the following steps:
(1) 26.6g of yttrium acetate hydrate and 6.65g of polyoxypropylene polyoxyethylene copolymer P123 are weighed and mixed in an agate mortar at room temperature and normal pressure, heated in a ventilated drying oven at 60 ℃ for 40min, taken out and quickly ground until yttrium acetate hydrate particles and polyoxypropylene polyoxyethylene copolymer P123 powder are uniformly mixed into a white viscous colloidal mixture.
(2) Rapidly transferring the colloidal mixture into a vacuum drying oven, keeping the vacuum degree in the vacuum drying oven at 1Pa, and keeping the temperature at 240 ℃ for 1h to obtain yellowish yttrium precursor powder.
(3) Heating the light yellow yttrium precursor powder to 400 ℃ at the speed of 5 ℃/min under the air atmosphere, preserving heat for 1 hour, heating to 850 ℃ at the speed of 5 ℃/min, preserving heat for 3 hours, and cooling to room temperature along with a furnace, and taking out to obtain the nano yttrium oxide powder.
Performance detection is carried out on the yttrium oxide powder prepared in the embodiment, and the particle size measured by a laser dynamic light scattering method is D 50 Specific surface area of powder calculated by BET method of 21.08m 2 And/g, scanning electron microscope shows that the lens is sphere-like, and the diameter is about 600nm.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (5)
1. The method for preparing the nano yttrium oxide powder by solid phase grinding is characterized by comprising the following steps:
(1) The yttrium salt with low melting point and the dispersant with low melting point are mixed according to the mass ratio of 2-4: 1, mixing in a clean mortar, and grinding and dispersing at 50-70 ℃ to obtain a colloidal mixture of yttrium salt and a dispersing agent which are uniformly mixed; the low-melting-point yttrium salt is selected from one of yttrium nitrate hexahydrate and yttrium acetate hydrate, and the low-melting-point dispersing agent is poloxamer F127 or polyoxypropylene polyoxyethylene copolymer P123;
(2) Rapidly transferring the colloidal mixture obtained in the step (1) into a vacuum drying oven, heating to the decomposition temperature of yttrium salt of 180-240 ℃ in vacuum with the vacuum degree of 0.1-10 Pa, and preserving the heat for 1-2 h, wherein the colloidal mixture is decomposed to obtain yttrium precursor powder;
(3) And carrying out heat treatment on yttrium precursor powder at 600-900 ℃ in an air atmosphere to obtain yttrium oxide nano-powder.
2. The method of claim 1, wherein the mass ratio of yttrium salt to dispersant of step (1) is 2.5:1.
3. the method according to claim 1, wherein the temperature of step (2) is 200 to 240 ℃.
4. The method according to claim 1, wherein the step (3) comprises the specific steps of: transferring yttrium precursor powder into a muffle furnace, heating to 400 ℃ at a speed of 5 ℃/min under an air atmosphere, preserving heat for 1-2 hours, heating to 600-900 ℃ at a speed of 1-5 ℃/min, and preserving heat for 1-3 hours.
5. The method according to claim 4, wherein the step (3) comprises the specific steps of: transferring yttrium precursor powder into a muffle furnace, heating to 400 ℃ at a speed of 5 ℃/min under the air atmosphere, preserving heat for 1-2 hours, heating to 650-850 ℃ at a speed of 5 ℃/min, and preserving heat for 2-3 hours.
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| CN202311412031.3A CN117361601A (en) | 2023-10-27 | 2023-10-27 | Method for preparing nano yttrium oxide powder by solid phase grinding |
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| CN202311412031.3A CN117361601A (en) | 2023-10-27 | 2023-10-27 | Method for preparing nano yttrium oxide powder by solid phase grinding |
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