CN111484339A - Preparation method of zirconia powder for ceramics - Google Patents

Preparation method of zirconia powder for ceramics Download PDF

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CN111484339A
CN111484339A CN202010308568.5A CN202010308568A CN111484339A CN 111484339 A CN111484339 A CN 111484339A CN 202010308568 A CN202010308568 A CN 202010308568A CN 111484339 A CN111484339 A CN 111484339A
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蒋央芳
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Abstract

The invention discloses a preparation method of zirconia powder for ceramics. Carrying out thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, and then cooling to a temperature of less than or equal to 100 ℃ and discharging; adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined material, heating, stirring and dissolving, then adding into a grinder, grinding to a particle size of 200-400nm, and then carrying out spray drying to obtain a spray-dried material; calcining the spray-dried material in a rotary kiln, and then cooling to a material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material; and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 2-10 mu m. The powder with a coating structure is formed and used for firing zirconia ceramics, the thermal conductivity of the ceramics is low, the mechanical strength and the thermal expansion coefficient are high, and the powder prepared by the method has small primary particles, high crystallinity, good sphericity, good dispersibility and convenient processing.

Description

Preparation method of zirconia powder for ceramics
Technical Field
The invention relates to a preparation method of zirconia powder for ceramics, belonging to the technical field of new energy lithium battery materials.
Background
The zirconia has the characteristics of strong thermal shock resistance, high temperature resistance, good chemical stability, outstanding material composite property and the like. Mixing stabilized zirconia with other materials (Al)2O3、SiO2) The composite material can greatly improve the performance parameters of the material, and improve the fracture toughness, the bending strength and the like. Therefore, the method is applied not only to the fields of structural ceramics and functional ceramics but also to the improvement of the surface characteristics (thermal conductivity, thermal shock resistance, high-temperature oxidation resistance, etc.) of metallic materials.
The usual zirconia stabilizers are rare earth or alkaline earth oxides and have only an ionic radius Zr4+Oxides whose radii differ by no more than 40% can act as stabilizers for zirconia. Wherein the more common is yttrium oxide and oxygenCalcium oxide, magnesium oxide and calcium oxide. The performance of the stabilized zirconia is not the same but the performance of the stabilized zirconia is substantially the same when stabilized by the stabilizers, and the performance of the stabilized zirconia obtained by adding the same stabilizer in different amounts is also greatly different. In application, a reasonable and proper amount of stabilizer is often selected and added according to the actual use requirement. The stable zirconia doped with yttria has good comprehensive performance and is the most applied solid electrolyte at present; the stabilized zirconia doped with calcium oxide has better performance than other stabilizers, is relatively cheap, and is easy to decalcify and destabilize; the electrical conductivity of the cerium oxide doped stabilized zirconia is best, but its mechanical properties are relatively poor; the stable zirconia doped with magnesia has common conductivity and low price, but has poor long-term service performance and is generally used as an easily-consumed product.
The mechanism of stabilization is not fully understood at present and is generally explained as: y is3+、Mg2+、Ce4+、Ca2+The cation of the stabilizing agent has certain stability in the zirconia, can replace Zr4+ in the zirconia to form a replacement solid solution, and hinder the transformation from the tetragonal crystal form (t) to the monoclinic crystal form (m), so that the temperature of t → m phase transition of the zirconia ceramic is reduced, and the t-ZrO2 is metastable to room temperature. Zirconia ceramics with different phase compositions can be obtained by adding different amounts of stabilizer if part of the t-ZrO2 is metastable to room temperature. Obtaining partial zirconia, PSZ for short; if t-ZrO2 is all metastable to room temperature, obtaining a polycrystal containing only tetragonal zirconia, named TZP for short; if the c-ZrO2 is metastable to the room temperature, the c-ZrO2 single-phase material, namely the fully stabilized zirconia, is obtained, and is called FSZ for short.
The atomic fraction of the stabilizer yttria is typically between 2% and 3%. The sintering temperature of the yttria-stabilized zirconia is about 1780-1800 ℃, the material has good sintering performance and high density. Has excellent normal temperature mechanical property, and also shows good wear resistance and corrosion resistance. However, the yttrium-stabilized zirconia has a significant disadvantage that t → m isothermal phase transformation occurs inside the material surface when the yttrium-stabilized zirconia is used in a low temperature region of 100-400 ℃ for a long time, resulting in a sharp decrease in mechanical properties, i.e., low temperature property aging. This aging phenomenon of low temperature performance severely restricts the application, so the way of studying the aging mechanism and preventing low temperature aging is becoming the hot spot of zirconia material research in recent years.
The outstanding advantages of magnesia-stabilized zirconia over yttria-stabilized zirconia are excellent mechanical properties and creep resistance at relatively high temperatures, but research and development of magnesia-stabilized zirconia is limited by two disadvantages: firstly, the solid solution temperature of magnesium oxide in the cubic region of zirconia is very high, so that stable zirconia with stable magnesium is not easy to be completely sintered; and secondly, when the temperature of the zirconia is higher than 1000 ℃, the magnesia is easy to generate crystal phase separation and a large amount of tetragonal phase instability, so that the performance of the material is degraded, and the application of the magnesia in a high-temperature area is severely restricted. Therefore, the future research of stabilizing zirconia by magnesia mainly aims to reduce the sintering temperature and realize low-temperature sintering; meanwhile, the high-temperature mechanical property of the material is improved, and the application range is expanded.
The stabilizing agent such as calcium oxide, magnesium oxide, yttrium oxide, cerium oxide, etc. is added to form a cubic crystal structure zirconium dioxide solid solution which is stable from room temperature to 2000 ℃, the yttrium oxide stabilized zirconium oxide product has good chemical stability, is not eroded with molten steel, has large high-temperature structural strength, small thermal conductivity [ 2.2W/(m.K) ], high thermal expansion coefficient (9.4 × 10-6/° C at 25-1500 ℃), is generally prepared by using yttrium stabilized zirconium oxide as a raw material and finely grinding or preparing hollow balls together with the stabilizing agent, and roasting at 1780 ℃ to prepare the yttrium oxide stabilized zirconium oxide serving as a refractory material, which is applied to electronic ceramic sintered support pads, and refractory materials for melting glass and metallurgical metals, and the application in the high-tech field is increasingly expanded.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing zirconia powder for ceramics, wherein a powder body with a coating structure is formed, the coating layer is yttria and calcium oxide stabilizer, the inner core is zirconia, the powder body with the structure is used for firing zirconia ceramics, compared with zirconia/yttria/calcium oxide prepared by coprecipitation or mechanically mixed zirconia/yttria/calcium oxide, the thermal conductivity of the ceramics is low, and the mechanical strength and the thermal expansion coefficient are high.
The invention solves the technical problems by the following technical means:
the invention relates to a preparation method of zirconia powder for ceramics, which comprises the following steps:
(1) performing thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is at least one of nitrogen atmosphere, argon atmosphere, carbon monoxide atmosphere, methane atmosphere and hydrogen atmosphere, the temperature is raised to 280 ℃ through 1-2h in the temperature raising process, then the temperature is kept for 1-2h at the temperature, the temperature is raised to 1500 ℃ through 1000 ℃ at the temperature raising speed of 250 ℃/h in 200 ℃ plus materials, the temperature is kept for 3-6h at the temperature, and then the material is discharged after the temperature is reduced to be less than or equal to 100 ℃;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined material, heating, stirring and dissolving, then adding into a grinder, grinding to a particle size of 200-400nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray drying material in a rotary kiln at the calcining temperature of 500-700 ℃ for 5-10h, and then cooling to the material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 2-10 mu m.
The mol ratio of the n-butyl alcohol zirconium to the yttrium nitrate to the calcium nitrate to the dispersing agent to the water is 0.7-0.8:0.04-0.05:0.01-0.02: 0.05-0.1: 15-20.
And (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
And (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.1-0.2 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 25-30cm, the rotating speed is 15000-20000r/min, the air inlet temperature is 200-300 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a cyclone dust collector and a cloth bag dust collector are combined for spray drying, and the cyclone material and the dust collecting material are mixed together.
And (3) the material accounts for 5-10% of the volume of the rotary kiln, air is introduced into the rotary kiln in the calcining process, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 2-4 r/min.
In the step (4), a fluidized bed type airflow pulverizer is adopted for pulverization, the adopted air source pressure is 5-8 atmospheric pressures, the diameter of a nozzle is 8-15mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 15-20cm, the rotating speed of the grading wheel is 400-one-material at 600r/min, the thickness of blades of the grading wheel is 1-2cm, the length of the blades is 10-15cm, the width of the blades is 3-6cm, and the gap between the blades is 1-3 cm.
And (4) screening and packaging the material subjected to airflow crushing in the step (4), wherein a 200-mesh 300-mesh ultrasonic vibration screen is adopted for screening.
The method comprises the steps of firstly, thermally decomposing organic zirconium salt in an inert atmosphere, decomposing organic carbon chains into carbon dioxide, carbon monoxide, water vapor, hydrogen and the like through thermal decomposition, leaving residual carbon ash, combining with zirconium simultaneously to obtain a carbon/zirconium carbide compound, then adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the compound, dissolving the yttrium nitrate, the calcium nitrate and the dispersing agent in the water, uniformly suspending the slurry in the dispersing agent, grinding the slurry to 200-400nm after dissolving, then carrying out spray drying, carrying out centrifugal spray drying, generating fog drops taking solid particles as cores and externally having solution, carrying out spray drying, evaporating moisture, coating crystallized calcium acetate and yttrium acetate on the surfaces of the solid particles, and carrying out high-temperature oxidation calcination to oxidize the carbon/zirconium carbide compound into zirconium dioxide, the acetate is thermally decomposed into oxide, so that a coating layer with a structure of yttrium oxide and calcium oxide stabilizer and an internal core with zirconium dioxide is formed.
The invention has the beneficial effects that: the powder with a coating structure is formed, the coating layer is yttria and calcium oxide stabilizer, the inner core is zirconia, the powder with the structure is used for firing zirconia ceramics, compared with zirconia/yttria/calcium oxide prepared by coprecipitation or mechanically mixed zirconia/yttria/calcium oxide, the ceramics has low thermal conductivity, high mechanical strength and high thermal expansion coefficient, and the powder prepared by the invention has small primary particles, high crystallinity, good sphericity, good dispersibility and convenient processing; no sewage is generated.
Drawings
FIG. 1 is an SEM of the product of example 1 of the present invention at 1000 Xmagnification.
FIG. 2 is an SEM of the product of example 1 of the present invention at 5000 magnification.
Detailed Description
The invention will be described in detail below with reference to the following figures and specific examples: the preparation method of the zirconia powder for ceramics of this embodiment includes the following steps:
(1) performing thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is at least one of nitrogen atmosphere, argon atmosphere, carbon monoxide atmosphere, methane atmosphere and hydrogen atmosphere, the temperature is raised to 280 ℃ through 1-2h in the temperature raising process, then the temperature is kept for 1-2h at the temperature, the temperature is raised to 1500 ℃ through 1000 ℃ at the temperature raising speed of 250 ℃/h in 200 ℃ plus materials, the temperature is kept for 3-6h at the temperature, and then the material is discharged after the temperature is reduced to be less than or equal to 100 ℃;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined material, heating, stirring and dissolving, then adding into a grinder, grinding to a particle size of 200-400nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray drying material in a rotary kiln at the calcining temperature of 500-700 ℃ for 5-10h, and then cooling to the material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 2-10 mu m.
The mol ratio of the n-butyl alcohol zirconium to the yttrium nitrate to the calcium nitrate to the dispersing agent to the water is 0.7-0.8:0.04-0.05:0.01-0.02: 0.05-0.1: 15-20.
And (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
And (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.1-0.2 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 25-30cm, the rotating speed is 15000-20000r/min, the air inlet temperature is 200-300 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a cyclone dust collector and a cloth bag dust collector are combined for spray drying, and the cyclone material and the dust collecting material are mixed together.
And (3) the material accounts for 5-10% of the volume of the rotary kiln, air is introduced into the rotary kiln in the calcining process, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 2-4 r/min.
In the step (4), a fluidized bed type airflow pulverizer is adopted for pulverization, the adopted air source pressure is 5-8 atmospheric pressures, the diameter of a nozzle is 8-15mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 15-20cm, the rotating speed of the grading wheel is 400-one-material at 600r/min, the thickness of blades of the grading wheel is 1-2cm, the length of the blades is 10-15cm, the width of the blades is 3-6cm, and the gap between the blades is 1-3 cm.
And (4) screening and packaging the material subjected to airflow crushing in the step (4), wherein a 200-mesh 300-mesh ultrasonic vibration screen is adopted for screening.
Example 1
A preparation method of zirconia powder for ceramics comprises the following steps:
(1) carrying out thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is a nitrogen atmosphere, the temperature is raised to 245 ℃ after 2 hours, then the temperature is kept for 2 hours, then the temperature is raised to 1200 ℃ at the temperature raising speed of 200 ℃/h, the temperature is kept for 5 hours at the temperature, and then the temperature is lowered to be less than or equal to 100 ℃ before discharging;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined discharge material, heating, stirring and dissolving, then adding into a grinder, grinding to reach the particle size of 235nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray-dried material in a rotary kiln at 700 ℃ for 8h, and then cooling to a material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 6.3 mu m.
The molar ratio of the n-butyl zirconium, the yttrium nitrate, the calcium nitrate, the dispersing agent and the water is 0.7:0.04:0.01: 0.05: 15.
and (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
And (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.1 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 30cm, the rotating speed is 20000r/min, the air inlet temperature is 200 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a mode of combining a cyclone dust collector and a cloth bag dust collector is adopted for spray drying, and the cyclone material and the dust collecting material are mixed together.
And (3) the material accounts for 5% of the volume of the rotary kiln, air is introduced into the rotary kiln in the calcining process, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 2 r/min.
And (3) in the step (4), a fluidized bed type jet mill is adopted for crushing, the pressure of an adopted air source is 8 atmospheric pressures, the diameter of a nozzle is 8mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 15cm, the rotating speed of the grading wheel is 500r/min, the thickness of blades of the grading wheel is 1cm, the length of the blades of the grading wheel is 10cm, the width of the blades of the grading wheel is 3cm, and the gap between the blades of the grading wheel is 1 cm.
And (4) screening and packaging the material crushed by the airflow in the step (4), wherein a 200-mesh ultrasonic vibration screen is adopted for screening.
As shown in figures 1 and 2, the obtained product particles are spherical, have good sphericity and good dispersibility, have a primary particle size of 10-50nm and a secondary particle size of 1.5-3 mu m, and are convenient for feeding, mixing and molding in the processing process.
Example 2
A preparation method of zirconia powder for ceramics comprises the following steps:
(1) carrying out thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is methane atmosphere, the temperature is increased to 280 ℃ after 2h, then the temperature is kept for 2h, then the temperature is increased to 1500 ℃ at the temperature increasing speed of 250 ℃/h, the temperature is kept for 6h at the temperature, and then the temperature is reduced to be less than or equal to 100 ℃ and then the material is discharged;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined discharge material, heating, stirring and dissolving, then adding into a grinder, grinding to reach the particle size of 400nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray-dried material in a rotary kiln at 500 ℃ for 10h, and then cooling to a material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 8.3 mu m.
The molar ratio of the n-butyl alcohol zirconium to the yttrium nitrate to the calcium nitrate to the dispersing agent to the water is 0.8:0.05:0.02: 0.1: 20.
and (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
And (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.2 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 30cm, the rotating speed is 20000r/min, the air inlet temperature is 300 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a mode of combining a cyclone dust collector and a cloth bag dust collector is adopted for spray drying, and the cyclone material and the dust collecting material are mixed together.
And (3) filling air into the rotary kiln in the calcining process, wherein the material accounts for 10% of the volume of the rotary kiln, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 4 r/min.
And (3) in the step (4), a fluidized bed type jet mill is adopted for crushing, the pressure of an adopted air source is 8 atmospheric pressures, the diameter of a nozzle is 15mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 20cm, the rotating speed of the grading wheel is 600r/min, the thickness of blades of the grading wheel is 2cm, the length of the blades of the grading wheel is 15cm, the width of the blades of the grading wheel is 3cm, and gaps among the blades of the grading wheel are 3 cm.
And (4) screening and packaging the material crushed by the airflow in the step (4), wherein a 250-mesh ultrasonic vibration screen is adopted for screening.
Example 3
A preparation method of zirconia powder for ceramics comprises the following steps:
(1) carrying out thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is argon atmosphere, the temperature is raised to 200 ℃ after 2h, then the temperature is kept for 2h, then the temperature is raised to 1000 ℃ at the temperature raising speed of 200 ℃/h, the temperature is kept for 6h at the temperature, and then the temperature is lowered to be less than or equal to 100 ℃ before discharging;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined discharge material, heating, stirring and dissolving, then adding into a grinder, grinding to a particle size of 300nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray-dried material in a rotary kiln at the calcining temperature of 600 ℃ for 10h, and then cooling to the material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 4.4 mu m.
The molar ratio of the n-butyl zirconium, the yttrium nitrate, the calcium nitrate, the dispersing agent and the water is 0.75:0.045:0.01: 0.05: 20.
and (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
And (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.1 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 30cm, the rotating speed is 15000r/min, the air inlet temperature is 200 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a mode of combining a cyclone dust collector and a cloth bag dust collector is adopted for spray drying, and the cyclone material and the dust collecting material are mixed together.
And (3) the material accounts for 5% of the volume of the rotary kiln, air is introduced into the rotary kiln in the calcining process, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 2 r/min.
And (3) in the step (4), a fluidized bed type jet mill is adopted for crushing, the adopted air source pressure is 5 atmospheric pressures, the diameter of a nozzle is 8mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 15cm, the rotating speed of the grading wheel is 400r/min, the thickness of blades of the grading wheel is 1cm, the length of the blades of the grading wheel is 15cm, the width of the blades of the grading wheel is 6cm, and the gap between the blades of the grading wheel is 3 cm.
And (4) screening and packaging the material crushed by the airflow in the step (4), wherein a 300-mesh ultrasonic vibration screen is adopted for screening.
Finally, the results of the tests of the products obtained in examples 1, 2 and 3 of the present invention are as follows:
Figure BDA0002456729190000061
Figure BDA0002456729190000071
the powders of 1/2 and 3 of the invention are prepared into zirconia ceramics, then zirconia, yttria and calcia are mixed and sintered into zirconia ceramics, the content of Zr/Y/Ca in the zirconia ceramics is 69.5%, 2.1% and 0.5%, the sintering process is the same, finally the zirconia ceramics are sintered into the zirconia ceramics, the performance of the zirconia ceramics is detected, the result is as follows:
Figure BDA0002456729190000072
finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.

Claims (7)

1. The preparation method of the zirconia powder for ceramics is characterized by comprising the following steps:
(1) performing thermal decomposition on zirconium n-butyl alcohol to obtain thermal decomposition powder, wherein the thermal decomposition adopts a certain atmosphere, the atmosphere is at least one of nitrogen atmosphere, argon atmosphere, carbon monoxide atmosphere, methane atmosphere and hydrogen atmosphere, the temperature is raised to 280 ℃ through 1-2h in the temperature raising process, then the temperature is kept for 1-2h at the temperature, the temperature is raised to 1500 ℃ through 1000 ℃ at the temperature raising speed of 250 ℃/h in 200 ℃ plus materials, the temperature is kept for 3-6h at the temperature, and then the material is discharged after the temperature is reduced to be less than or equal to 100 ℃;
(2) adding yttrium nitrate, calcium nitrate, a dispersing agent and water into the calcined material, heating, stirring and dissolving, then adding into a grinder, grinding to a particle size of 200-400nm, and then carrying out spray drying to obtain a spray-dried material;
(3) calcining the spray drying material in a rotary kiln at the calcining temperature of 500-700 ℃ for 5-10h, and then cooling to the material temperature of less than or equal to 120 ℃ to obtain a secondary calcined material;
(4) and (3) carrying out air flow crushing on the secondary calcined material, and crushing to obtain zirconia powder for ceramics, wherein the grain size of the zirconia powder is 2-10 mu m.
2. The method according to claim 1, wherein the method comprises the steps of: the mol ratio of the n-butyl alcohol zirconium to the yttrium nitrate to the calcium nitrate to the dispersing agent to the water is 0.7-0.8:0.04-0.05:0.01-0.02: 0.05-0.1: 15-20.
3. The method according to claim 1, wherein the method comprises the steps of: and (2) calcining in the step (1) in a roller furnace, and discharging waste gas generated in the temperature rise process by using a draught fan.
4. The method according to claim 1, wherein the method comprises the steps of: and (3) when the grinding machine in the step (2) is used for grinding, a zirconia ball with the diameter of 0.1-0.2 mu m is adopted, a centrifugal spray dryer is adopted for spray drying, the diameter of a centrifugal wheel is 25-30cm, the rotating speed is 15000-20000r/min, the air inlet temperature is 200-300 ℃, the discharging temperature is controlled to be less than or equal to 100 ℃, a cyclone dust collector and a cloth bag dust collector are combined for spray drying, and the cyclone material and the dust collecting material are mixed together.
5. The method according to claim 1, wherein the method comprises the steps of: and (3) the material accounts for 5-10% of the volume of the rotary kiln, air is introduced into the rotary kiln in the calcining process, the volume fraction of oxygen in the rotary kiln is maintained to be more than or equal to 19%, and the rotating speed of the rotary kiln is 2-4 r/min.
6. The method according to claim 1, wherein the method comprises the steps of: in the step (4), a fluidized bed type airflow pulverizer is adopted for pulverization, the adopted air source pressure is 5-8 atmospheric pressures, the diameter of a nozzle is 8-15mm, a grading wheel is arranged at the same time, the diameter of the grading wheel is 15-20cm, the rotating speed of the grading wheel is 400-one-material at 600r/min, the thickness of blades of the grading wheel is 1-2cm, the length of the blades is 10-15cm, the width of the blades is 3-6cm, and the gap between the blades is 1-3 cm.
7. The method according to claim 1, wherein the method comprises the steps of: and (4) screening and packaging the material subjected to airflow crushing in the step (4), wherein a 200-mesh 300-mesh ultrasonic vibration screen is adopted for screening.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116239134A (en) * 2022-12-07 2023-06-09 雅安百图高新材料股份有限公司 Treatment method of aluminum oxide calcined powder for heat conduction field

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