CN111960465A - Spherical ZrO2Method for preparing powder - Google Patents

Spherical ZrO2Method for preparing powder Download PDF

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CN111960465A
CN111960465A CN202010812957.1A CN202010812957A CN111960465A CN 111960465 A CN111960465 A CN 111960465A CN 202010812957 A CN202010812957 A CN 202010812957A CN 111960465 A CN111960465 A CN 111960465A
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powder
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于洋
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Xiamen Xiaruibo Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00Compounds of zirconium
    • C01G25/02Oxides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/41Particle morphology extending in three dimensions octahedron-like
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/50Agglomerated particles
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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Abstract

The invention discloses a spherical ZrO2A method of preparing a powder comprising the steps of: (1) ZrO with grain size of 10 nm-50 mu m2Uniformly mixing the base powder and the binder to obtain a mixture; (2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, and the ZrO2The particle size of the large particle cluster is 5-1000 mu m; (3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, and separating ZrO with different particle size ranges from the sintered large particle clusters through vibration screening2Powder; (4) screened ZrO2The powder is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder. The invention provides spherical ZrO2The particle manufacturing method can provide ZrO with ideal sphericity for the ceramic additive manufacturing technology2The raw material of the particles can greatly expand the ceramic additive manufacturing technologyThe application range of the technology accelerates the development speed of ceramic additive manufacturing.

Description

Spherical ZrO2Method for preparing powder
Technical Field
The invention relates to the field of non-metallic material forming and processing, in particular to spherical ZrO2A method for preparing powder.
Background
Ceramic materials are widely used in various fields due to their excellent mechanical properties, chemical stability, high temperature properties, etc. However, the inherent properties of high strength and high hardness have made it difficult to form ceramic parts. The difficulty can be effectively overcome by introducing an Additive Manufacturing (AM) technology into ceramic forming, and a brand-new possibility is provided for a complex ceramic material forming process.
The mainstream ceramic additive manufacturing technology at present is mainly divided into four types, namely a rapid prototyping technology based on a laser technology, a digital rapid prototyping technology based on adhesive bonding, a rapid prototyping technology based on an extrusion technology, and a rapid prototyping technology based on digital light processing (curing). The four additive manufacturing technologies, especially the first two, have higher requirements on the sphericity of the used ceramic particle raw material, but the prior traditional technology for preparing ceramic particles cannot achieve the situation that the sphericity is very ideal, and the prior art for preparing ZrO2The sphericity of the particles is very low, and the fluidity is poor, so that the powder laying is not uniform; while the internal density of the part after AM molding is not uniform, ZrO2The surface is rough, and the size precision is low, thereby restricting the application and the development of the ceramic AM.
Disclosure of Invention
In view of the above problems, the present invention provides a spherical ZrO2The powder manufacturing method can provide ZrO with ideal sphericity for ceramic additive manufacturing technology2Powder raw material.
In order to achieve the purpose, the invention adopts the following technical scheme:
spherical ZrO2A method of preparing a powder comprising the steps of:
(1) ZrO with grain size of 10 nm-50 mu m2Uniformly mixing the base powder and the binder to obtain a mixture;
(2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, and the ZrO2The particle size of the large particle cluster is 5-1000 mu m;
(3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, and separating ZrO with different particle size ranges from the sintered large particle clusters through vibration screening2Powder;
(4) screened ZrO2The powder is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder.
Adopt above-mentioned technical scheme's beneficial effect: ZrO within the above particle diameter range which is used in the present invention2The surface energy of the base powder particle is large, the sintering is easy, and the ZrO2The raw material base powder is low in price and easy to obtain;
the invention firstly uses ZrO2Carrying out atomization granulation on the base powder and the binder together, wherein ZrO is subjected to the atomization granulation process2The base powder particles form a liquid bridge through the adhesive, the base powder particles are agglomerated together to form a large particle, the particles soaked by the adhesive collide with the surrounding particles and are adhered together, and the particles are connected together through a solid bridge to form the large particle; the method has the advantages of high growth speed, large specific surface area, good solubility, various particle sizes, irregular shape and poor mechanical property.
Therefore, the invention regularly spheroidizes the agglomerated large particles through sintering and plasma spheroidization, so that the agglomerated large particles have high sphericity.
Furthermore, after the particles with irregular shapes are sprayed into the plasma arc by the carrier gas through the charging gun, the particles are rapidly heated and melted under the action of four heat transfer mechanisms of radiation, convection, conduction and chemistry. The molten particles form liquid drops with high sphericity under the action of surface tension, and the liquid drops are rapidly solidified under extremely high temperature gradient, and the aggregates are shrunk into spherical particles with better sphericity, and meanwhile, the sintering defect in a single sphere is eliminated.
Preferably, the binder is a polyethylene glycol aqueous solution, and the mass concentration of the polyethylene glycol aqueous solution is 1-3%.
Preferably, in the step (1), the mass of the binder accounts for 0.05-5% of the mass of the mixture, and the ZrO 22The volume of the base powder accounts for 50-95% of the volume of the mixture.
Preferably, the mass of the binder in the step (1) is 0.5-1% of the mass of the mixture, and the ZrO 22The volume of the base powder accounts for 90-95% of the volume of the mixture.
Adopt above-mentioned technical scheme's beneficial effect: content of binder to finally prepared spherical ZrO2The particle size, shape and strength of the powder have a great influence. The content of the binder is too low, the base powder particles cannot be agglomerated into large particles, and the small particlesThe bonding strength among the particles is not high, and the particles are easy to scatter when subsequent processes are carried out; the binder content is too high, the cost is higher, the degreasing difficulty required to be removed before sintering is increased, the binder residue is increased, and the product performance is also adversely affected. Therefore, the invention obtains the optimal binder dosage through research and ensures the performance of the product.
Preferably, in the atomization granulation process in the step (2), the inlet temperature of an atomization granulator is 270 ℃, the outlet temperature is 90-100 ℃, the diameter of an atomization disc is 100mm, and the rotation speed of the atomization disc is 2000 rad/min.
Adopt above-mentioned technical scheme's beneficial effect: the powder (the particle size is less than 20um) suitable for manufacturing 3D printing is obtained, and the yield is high and reaches 40%.
Preferably, the sintering temperature in the step (3) is controlled to be 1000-1400 ℃, and the sintering time is 30-200 min.
Adopt above-mentioned technical scheme's beneficial effect: ZrO (ZrO)2Sintering the large particle clusters to prepare spherical powder, and preparing ZrO with different particle sizes and densities by controlling the particle size and porosity of atomization granulation2Spherical powder, ZrO during sintering2The internal porosity in the large particle clusters is densified, ZrO2The large particle clusters are subjected to preliminary spheroidization, incomplete sintering is performed at the sintering temperature and time, and the sintering can be further sintered in the subsequent plasma spheroidization and 3D printing processes to complete sintering, so that the condition that the appearance and the performance of the large particle clusters are influenced by overburning in the 3D printing process after complete sintering is avoided.
Preferably, the plasma spheroidizing process in the step (4) specifically comprises the following steps: sieving the ZrO2Spraying carrier gas for powder into a plasma torch through a powder feeder, wherein the powder feeding speed is 0.5-2 Kg/min, and the plasma spheroidization adopts a high-frequency plasma power supply: the power is 80-120KW, and the frequency is 3.0 MHz.
Adopt above-mentioned technical scheme's beneficial effect: ZrO (ZrO)2The powder absorbs a large amount of heat in high-temperature plasma, and the surface is rapidly melted; and enters the reactor at an extremely high speed and is rapidly cooled in an inert atmosphereAnd cooling and solidifying the mixture into spherical powder under the action of surface tension.
The last defects in the sintered sphere can be removed by means of rapid melting and cooling, and meanwhile, the sphericity of the sintered sphere is better, and the surface of the sintered sphere is smoother.
Preferably, the spherical ZrO2The particle size of the powder is 3-800 mu m; and the spherical ZrO2The powder is separated by a vibration screening system to obtain spherical ZrO with particle size of 3-20 μm, 20-50 μm, 50-100 μm and above 100 μm2And (3) powder.
Adopt above-mentioned technical scheme's beneficial effect: the invention can obtain spherical ZrO with different particle size ranges2Powder, can meet the requirements of different technologies, and expands the spherical ZrO2The application range of the powder.
Further, spherical ZrO prepared by the above preparation method2The powder can be used in the following fields:
1. spherical ZrO with particle size not less than 3 and not more than 20 mu m2The powder is suitable for a binder spray forming (3D Printing, 3DP) process;
2. using spherical ZrO with particle size less than or equal to 50 μm in a range of 20%2Mixing the powder with a binder for 3D printing in an extrusion molding mode;
3. spherical ZrO with a particle size of not less than 3 and not more than 20 mu m is used2Mixing the powder with a binder for 3D printing by laser exposure;
4. spherical ZrO of 100 μm or more2The powder can be used as a grinding aid for polishing or grinding processes.
Compared with the prior art, the spherical ZrO provided by the invention2The particle manufacturing method can provide ZrO with ideal sphericity for the ceramic additive manufacturing technology2The particle raw material can greatly expand the application range of the ceramic additive manufacturing technology and accelerate the development speed of the ceramic additive manufacturing.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a schematic view of a spherical ZrO of the present invention2Schematic diagram of the preparation method of the powder;
FIG. 2 is a view showing ZrO of the present invention2A schematic of the formation of the powder particles;
FIG. 3 is a schematic view of atomized and granulated ZrO produced in example 1 of the present invention2Large particle cluster electron microscope photographs;
FIG. 4 is a schematic view of sintered ZrO produced in example 1 of the present invention2Electron micrograph of the powder;
FIG. 5 is a schematic view showing plasma-spheroidized spherical ZrO prepared in example 1 of the present invention2Electron micrograph of the powder;
FIG. 6 is a schematic view of spherical ZrO produced in example 1 of the present invention2A powder particle size distribution diagram;
among them, fig. 2 includes: 1-schematic representation of granules after atomization and granulation; 2-schematic representation of the particles after sintering (internal defects); 3-schematic of the particles after plasma spheronization (internal defect elimination).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Spherical ZrO2A method of preparing a powder comprising the steps of:
(1) the technical grade ZrO of which the grain diameter is between 10 and 50 mu m (the average grain size is 100nm)2Mixing 2kg of base powder and 5L of 2.5% polyethylene glycol aqueous solution to obtain slurry to obtain a mixture;
(2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, wherein the inlet temperature of an atomizing granulator is 270 ℃, the outlet temperature is 90 ℃, the diameter of an atomizing disc is 100mm, and the rotating speed of the atomizing disc is 2000 rad/min; and the ZrO2The particle size of the large particle cluster is 5-1000 mu m;
(3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, controlling the sintering temperature at 1350 ℃ and the sintering time at 150min, and separating ZrO in different particle size ranges from the sintered large particle clusters through vibration screening2Powder;
(4) sieving the ZrO2The powder is sprayed into the plasma torch by carrier gas through a powder feeder, the powder feeding speed is 1.5Kg/min, and the plasma spheroidizing process adopts a high-frequency plasma power supply: 100KW power and 3.0MHz frequency, and is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder.
Spherical ZrO prepared in this example2The particle size of the powder is between 3 and 800 mu m; separating spherical ZrO with particle size of 3-20 μm, 20-50 μm, 50-100 μm, and above 100 μm by vibration sieving system2And (3) powder.
For ZrO prepared in each stage2Scanning the powder by electron microscope, FIG. 3 ZrO after granulation by atomization2Large particle cluster electron microscope photographs; FIG. 4 is a schematic representation of sintered ZrO2Electron micrograph of the powder; FIG. 5 is a schematic view of a spherical ZrO after plasma spheroidization2Electron micrograph of the powder.
As can be seen in fig. 3: atomized and granulated ZrO2The large particle cluster has rough surface, more internal defects and poor sphericity.
As can be seen in fig. 4: sintered ZrO2The powder surface roughness is reduced, the internal defects are reduced, and the sphericity is improved.
As can be seen from fig. 5: spherical ZrO after plasma spheroidization2The powder has smooth surface, uniform internal structure and excellent sphericity.
Spheroidized spherical Zr by using laser diameter gaugeO2The powder was tested and the results are shown in fig. 6, from which it can be seen that: spherical ZrO prepared in example 12The proportion of particles with the powder size of less than 20um is up to 40 percent.
Example 2
Spherical ZrO2A method of preparing a powder comprising the steps of:
(1) the technical grade ZrO of which the grain diameter is between 10 and 50 mu m (the average grain size is 100nm)2Mixing 2kg of base powder and 5L of 2.5% polyethylene glycol aqueous solution to obtain slurry to obtain a mixture;
(2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, the inlet temperature of the atomizing granulator is 270 ℃, the outlet temperature is 90 ℃, the diameter of the atomizing disk is 100mm, and the rotating speed of the atomizing disk is 2000 rad/min. And the ZrO2The particle size of the large particle cluster is 5-1000 mu m;
(3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, controlling the sintering temperature at 1350 ℃ and the sintering time at 200min, and separating ZrO in different particle size ranges from the sintered large particle clusters through vibration screening2Powder;
(4) sieving the ZrO2The powder is sprayed into the plasma torch by carrier gas through a powder feeder, the powder feeding speed is 1.5Kg/min, and the plasma spheroidizing process adopts a high-frequency plasma power supply: 100KW power and 3.0MHz frequency, and is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder.
Spherical ZrO prepared in this example2The particle size of the powder is between 3 and 800 mu m; separating spherical ZrO with particle size of 3-20 μm, 20-50 μm, 50-100 μm, and above 100 μm by vibration sieving system2And (3) powder.
Example 3
Spherical ZrO2A method of preparing a powder comprising the steps of:
(1) the technical grade ZrO with the grain diameter of 10nm to 50 mu m (average grain size of 120nm)2Mixing 2kg of base powder and 5L of 2.5% polyethylene glycol aqueous solution to obtain slurry to obtain a mixture;
(2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, the inlet temperature of the atomizing granulator is 270 ℃, the outlet temperature is 100 ℃, the diameter of the atomizing disk is 100mm, and the rotating speed of the atomizing disk is 2000 rad/min. And the ZrO2The particle size of the large particle cluster is 5-1000 mu m;
(3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, controlling the sintering temperature at 1400 ℃, the sintering time at 200min, and separating ZrO in different particle size ranges from the sintered large particle clusters through vibration screening2Powder;
(4) sieving the ZrO2The powder is sprayed into the plasma torch by carrier gas through a powder feeder, the powder feeding speed is 1.5Kg/min, and the plasma spheroidizing process adopts a high-frequency plasma power supply: 100KW power and 3.0MHz frequency, and is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder.
Spherical ZrO prepared in this example2The particle size of the powder is between 3 and 800 mu m; separating spherical ZrO with particle size of 3-20 μm, 20-50 μm, 50-100 μm, and above 100 μm by vibration sieving system2And (3) powder.
Example 4
Spherical ZrO2The 3DP printing method of the powder comprises the following process steps:
1) spheroidized ZrO prepared in example 1 without defects in the inside25000 g of powder, spheroidized ZrO2The particle size of the powder is 5-20 μm;
2) 20 g of a curing agent was taken and mixed with the above ZrO2Stirring the powder uniformly;
3) putting the mixed powder into an oven, and drying at the drying temperature of 75 ℃;
4) putting the dried powder into a material box of special ceramic 3DP printing equipment;
5) putting the bonding resin into a main ink barrel of special ceramic 3DP printing equipment, introducing a formed slice file, and setting the thickness of a printing layer to be 0.03 mm;
6) printing, wherein powder is scraped to a forming cylinder by a powder spreading trolley, bonding resin is selectively sprayed on a powder layer in the forming cylinder by a spray head according to a slice file, so that curing components in the powder are subjected to curing reaction with the powder layer, the powder layer is rapidly dried and bonded, and then the processes of powder spreading and jet printing are circulated until the model printing is finished;
7) taking out the formed model, cleaning, embedding the model into glass beads, then putting the model into an oven, heating the model to 120 ℃, carrying out secondary curing, and slowly cooling the model to room temperature;
8) degreasing at 155 ℃ for 2 hours, and then sintering at 1405 ℃ for 4 hours.
Compared with other powder raw materials, the powder using the invention has very good spherical outer surface, so that the problem of uneven powder laying caused by powder fluidity can not occur in the powder laying process, and the problem of sintering deformation caused by uneven powder density in a solidified printing body can be avoided.
Meanwhile, the invention discloses spherical ZrO2The preparation method of the powder has the advantages that the spherical powder with a larger proportion (40%) of particles with the particle size range of 5-20 mu m suitable for 3-D printing can be produced, and the preparation method has better economic value.
The present invention has been described in detail, and the principle and embodiments of the present invention are explained herein by using specific examples, which are only used to help understand the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.

Claims (10)

1. Spherical ZrO2The preparation method of the powder is characterized by comprising the following steps:
(1) ZrO with grain size of 10 nm-50 mu m2Uniformly mixing the base powder and the binder to obtain a mixture;
(2) preparing the mixture into ZrO through an atomization granulation process2Large particle clusters, and the ZrO2The particle size of the large particle cluster is 5-1000 mu m;
(3) subjecting the ZrO to2Placing the large particle clusters in a sintering furnace for degreasing and sintering, and separating ZrO with different particle size ranges from the sintered large particle clusters through vibration screening2Powder;
(4) screened ZrO2The powder is prepared into spherical ZrO with no defect inside by a plasma spheroidizing process2And (3) powder.
2. A spherical ZrO according to claim 12The preparation method of the powder is characterized in that the binder in the step (1) is a polyethylene glycol aqueous solution, and the mass concentration of the polyethylene glycol aqueous solution is 1-3%.
3. Spherical ZrO according to claim 1 or 22The preparation method of the powder is characterized in that in the step (1), the mass of the binder accounts for 0.05-5% of the mass of the mixture, and the ZrO 22The volume of the base powder accounts for 50-95% of the volume of the mixture.
4. A spherical ZrO according to claim 32The preparation method of the powder is characterized in that in the step (1), the mass of the binder accounts for 0.5-1% of the mass of the mixture, and the ZrO 22The volume of the base powder accounts for 90-95% of the volume of the mixture.
5. A spherical ZrO according to claim 12The preparation method of the powder is characterized in that the inlet temperature of an atomizing granulator in the atomizing granulation process in the step (2) is 270 ℃, the outlet temperature is 90-100 ℃, the diameter of an atomizing disc is 100mm, and the rotating speed of the atomizing disc is 2000 rad/min.
6. A spherical ZrO according to claim 12The preparation method of the powder is characterized in that in the step (3), the sintering temperature is controlled to be 1000-1400 ℃, and the sintering time is 30-200 min.
7. According to claim 1The spherical ZrO2The preparation method of the powder is characterized in that the plasma spheroidizing process in the step (4) comprises the following specific steps: sieving the ZrO2Spraying carrier gas for powder into a plasma torch through a powder feeder, wherein the powder feeding speed is 0.5-2 Kg/min, and the plasma spheroidization adopts a high-frequency plasma power supply: the power is 80-120KW, and the frequency is 3.0 MHz.
8. A spherical ZrO according to claim 12A method for producing a powder, characterized in that the spherical ZrO of step (4)2The particle size of the powder is 3-800 mu m; and the spherical ZrO2The powder is separated by a vibration screening system to obtain spherical ZrO with particle size of 3-20 μm, 20-50 μm, 50-100 μm and above 100 μm2And (3) powder.
9. A spherical ZrO according to any one of claims 1 to 82Method for preparing powder and spherical ZrO prepared by method2And (3) powder.
10. A spherical ZrO according to claim 92Use of a powder in the field of 3D printing and milling processes.
CN202010812957.1A 2020-08-13 2020-08-13 Spherical ZrO2Method for preparing powder Pending CN111960465A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114605149A (en) * 2020-12-03 2022-06-10 中国科学院福建物质结构研究所 Preparation method and application of zirconia microspheres

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1637080A (en) * 2004-12-09 2005-07-13 武汉理工大学 Prepn of nanometer aggregated zirconia powder for hot spraying
CN105801092A (en) * 2016-03-04 2016-07-27 广东工业大学 Raw materials of transparent ceramic as well as preparation method and application
CN106927833A (en) * 2017-03-13 2017-07-07 南京云启金锐新材料有限公司 High purity high dense zirconium oxide boron nitride composite ceramics insulating part and preparation method thereof
CN106938931A (en) * 2017-03-13 2017-07-11 南京云启金锐新材料有限公司 High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof
WO2020132881A1 (en) * 2018-12-24 2020-07-02 北京科技大学 Metal sintering densification and grain dimension control method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1637080A (en) * 2004-12-09 2005-07-13 武汉理工大学 Prepn of nanometer aggregated zirconia powder for hot spraying
CN105801092A (en) * 2016-03-04 2016-07-27 广东工业大学 Raw materials of transparent ceramic as well as preparation method and application
CN106927833A (en) * 2017-03-13 2017-07-07 南京云启金锐新材料有限公司 High purity high dense zirconium oxide boron nitride composite ceramics insulating part and preparation method thereof
CN106938931A (en) * 2017-03-13 2017-07-11 南京云启金锐新材料有限公司 High purity high dense yttrium stable zirconium oxide ceramics and preparation method thereof
WO2020132881A1 (en) * 2018-12-24 2020-07-02 北京科技大学 Metal sintering densification and grain dimension control method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114605149A (en) * 2020-12-03 2022-06-10 中国科学院福建物质结构研究所 Preparation method and application of zirconia microspheres

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