CN116082022B - Preparation method of ceramic powder and ceramic powder - Google Patents
Preparation method of ceramic powder and ceramic powder Download PDFInfo
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Abstract
The invention belongs to the field of conductive ceramics, and particularly relates to a preparation method of ceramic powder and the ceramic powder, wherein the method comprises the following steps: dispersing manganous oxide powder and cobaltosic oxide powder in a solvent through ball milling treatment to obtain first slurry, and separating and treating the first slurry to obtain suspension and precipitate, wherein the manganous oxide and the cobaltosic oxide in the suspension are mixed in a nanoscale, and the mass ratio of the manganous oxide powder to the cobaltosic oxide powder is 0.8:1-1:0.8; spray drying the suspension to obtain agglomerated powder; and sintering the agglomerated powder to obtain the ceramic powder, wherein the sintering temperature is 1120-1200 ℃ and the sintering time is 10 min-1 h. The ceramic powder provided by the invention has two crystal grains of cubic phase and tetragonal phase, and the two crystal grains form a biphase eutectic fine crystal structure, so that rich phase interfaces and rich electron conduction channels can be provided, and the ceramic powder has higher conductivity.
Description
Technical Field
The invention belongs to the field of conductive ceramics, and particularly relates to a preparation method of ceramic powder and the ceramic powder.
Background
The conductive ceramic has the characteristics of oxidation resistance, corrosion resistance, radiation resistance, high temperature resistance and the like, and is widely applied to the electronic fields of a sensor Gao Wenyuan device, a fixed resistor, a solid oxide fuel cell, a ferrite material and the like. The conductive ceramic material is generally prepared by doping modification to increase the concentration of electrons, holes or oxygen ions in the crystal lattice of the material to enhance the conductivity of the material, such as rare earth doped (LaBa) CoO 3 Ceramic, cuO doped NiO-NiFe 2 O 4 Composite ceramic, alN-SiC-MoSi 2 Etc. To ensure the long-term performance stability of the conductive ceramicsThe ceramic preparation process needs to adopt a high-temperature sintering process, and most ceramic materials can be changed into good electronic conductors at a higher temperature, however, at a high temperature, grains in the ceramic are easy to aggregate and grow up, the defect concentration is reduced, and the conductivity of the conductive ceramic is greatly influenced.
Disclosure of Invention
The invention aims to overcome the defects of the ceramic powder in the prior art, such as aggregation growth of internal grains, low defect concentration and low conductivity, and provides a preparation method of the ceramic powder and the ceramic powder.
In order to achieve the above object, in a first aspect, the present invention provides a method for producing ceramic powder, the method comprising:
dispersing manganous oxide powder and cobaltosic oxide powder in a solvent through ball milling treatment to obtain first slurry, and separating and treating the first slurry to obtain suspension and precipitate, wherein the manganous oxide and the cobaltosic oxide in the suspension are mixed in a nanoscale, and the mass ratio of the manganous oxide powder to the cobaltosic oxide powder is 0.8:1-1:0.8;
spray drying the suspension to obtain agglomerated powder; and sintering the agglomerated powder to obtain the ceramic powder, wherein the sintering temperature is 1120-1200 ℃ and the sintering time is 10 min-1 h.
In some preferred embodiments, the average particle size of the manganous oxide powder and the tricobalt oxide powder is 0.1-10 μm.
In some preferred embodiments, the mixed powder of manganous oxide and tricobalt tetraoxide in the first slurry has a content of 60 to 75wt%, a content of the solvent has a content of 20 to 35wt%, and a content of the binder has a content of 5 to 10wt%.
In some preferred embodiments, the ball milling treatment uses a ball mill with a ball mill diameter of 2.5-3.5 mm with a ratio of 20-30wt% and a ball mill with a ball mill diameter of 4.5-5.5mm with a ratio of 70-80wt%, and the ball milling treatment has a rotation speed of 500-2000r/min for 20-50h.
In some preferred embodiments, the separation treatment comprises filtering the first slurry to obtain a second slurry, and precipitating the second slurry to obtain the suspension and the precipitate.
More preferably, the filtration treatment comprises filtration treatment with a screen having a pore diameter of 4 to 6 μm, and the time of the precipitation treatment is not less than 10 hours.
In some preferred embodiments, the particle size of the particles in the suspension is less than 50nm.
In some preferred embodiments, the precipitate is returned to a ball milling apparatus for the ball milling process.
In a second aspect, the present invention provides a ceramic powder produced by the production method of the first aspect.
In some preferred embodiments, the ceramic powder has a grain size of less than 100nm, and a cubic phase (Mn, co) in the ceramic powder 3 O 4 The phase content of (C) is 45% -55%, and tetragonal phase (Mn, co) 3 O 4 The phase content of the ceramic powder is 45% -55%, and the strength of the ceramic powder is more than 500Mpa.
According to the invention, the manganese oxide powder and the cobalt oxide powder with the mass ratio of 0.8:1-1:0.8 are mixed by ball milling, so that a first slurry obtained by crushing and uniformly mixing the manganese oxide powder and the cobalt oxide powder can be obtained, a suspension obtained by uniformly mixing the manganese oxide powder and the cobalt oxide powder at a nanometer scale can be obtained by separating and treating the first slurry, an agglomerated powder can be obtained by preparing the suspension into the agglomerated powder by spray drying, and the agglomerated powder obtained by uniformly mixing the manganese oxide powder and the cobalt oxide powder at the nanometer scale can be obtained, and cobalt element can rapidly enter an original manganese oxide phase to form a cubic phase (Mn, co) in the sintering treatment process of the agglomerated powder at a specific temperature 3 O 4 Manganese element can quickly enter the original cobaltosic oxide phase to form tetragonal phase (Mn, co) 3 O 4 Forming a cubic phase (Mn, co) 3 O 4 And tetragonal phase (Mn, co) 3 O 4 Nano-scale fine grain structure of biphasic eutectic crystals. Cubic phase (Mn, co) 3 O 4 And four (IV)Square phase (Mn, co) 3 O 4 The crystal is just thermodynamic equilibrium at high temperature, exists in a two-phase eutectic form, is not easy to grow even at high temperature based on the eutectic principle, and can keep the grain size below 100nm. The ceramic powder prepared by the method of the invention has cubic phase (Mn, co) 3 O 4 And tetragonal phase (Mn, co) 3 O 4 The nano-scale diphase eutectic structure is formed, the grain size is smaller than 100nm, rich phase interfaces can be provided, rich electron conduction channels are provided, and finally the conductivity of the ceramic powder can be improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of the microscopic morphology of the ceramic powder of example 1;
FIG. 2 is a scanning electron microscope image of the internal nano-eutectic structure of the ceramic powder of example 1.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the prior art, in order to ensure the long-term performance stability of ceramics, high-temperature sintering treatment is generally required, in order to ensure that ceramic powder has stronger conductivity, the concentration of electrons, holes or oxygen ions in a material lattice is generally improved through doping modification, however, in the high-temperature sintering process, grains in the ceramics are easy to aggregate and grow up, the concentration of electrons, holes and oxygen ions in the lattice is reduced, the common grain size of the conventional ceramic material is larger, and the conductivity and the long-term performance stability cannot be simultaneously achieved.
In this regard, in a first aspect, the present invention provides a method of preparing a ceramic powder, the method comprising:
dispersing manganous oxide powder and cobaltosic oxide powder in a solvent through ball milling treatment to obtain first slurry, and separating and treating the first slurry to obtain suspension and precipitate, wherein the manganous oxide and the cobaltosic oxide in the suspension are mixed in a nanoscale, and the mass ratio of the manganous oxide powder to the cobaltosic oxide powder is 0.8:1-1:0.8;
spray drying the suspension to obtain agglomerated powder; and sintering the agglomerated powder to obtain the ceramic powder, wherein the sintering temperature is 1120-1200 ℃ and the sintering time is 10 min-1 h.
The nano-scale mixing of the manganous oxide and the cobaltosic oxide in the suspension in the invention means that the nano-scale and fully and uniformly mixing of the manganous oxide powder and the cobaltosic oxide powder in the suspension obtained after ball milling and separation treatment.
In order to improve the conductivity of the ceramic powder, the present invention proposes to form phase interfaces in the ceramic powder and to form rich phase interfaces in the ceramic powder, the present invention proposes to form a nano-sized two-phase eutectic structure in the ceramic powder.
In order to form a nano-scale diphase eutectic structure, the invention provides a method for mixing and sintering manganic oxide and cobaltosic oxide in nano scale, wherein cobalt element can quickly enter an original manganic oxide phase in the sintering process to form a cubic phase (Mn, co) 3 O 4 Manganese element can quickly enter the original cobaltosic oxide phase to form tetragonal phase (Mn, co) 3 O 4 Forming a cubic phase (Mn, co) 3 O 4 And tetragonal phase (Mn, co) 3 O 4 Nano-scale fine grain structure of biphasic eutectic crystals. Cubic phase (Mn, co) 3 O 4 And tetragonal phase (Mn, co) 3 O 4 Just heat at high temperatureThe crystal is in a two-phase eutectic form, and based on the eutectic principle, two-phase crystal grains are not easy to grow even at high temperature, and the grain size of a two-phase eutectic structure is smaller than 100nm.
In order to mix the manganous oxide and the cobaltosic oxide in the nanometer scale before sintering treatment, the invention provides ball milling and mixing the manganous oxide powder and the cobaltosic oxide powder to obtain first slurry which is obtained by crushing and uniformly mixing the manganous oxide powder and the cobaltosic oxide powder, separating and treating the first slurry to obtain suspension which is uniformly mixed in the nanometer scale, preparing the suspension into agglomerated powder by spray drying, mixing the manganous oxide and the cobaltosic oxide in the agglomerated powder in the nanometer scale, and sintering the agglomerated powder.
The invention provides a method for preparing agglomeration powder by uniformly mixing manganic oxide and cobaltosic oxide in nano scale, and sintering the agglomeration powder.
According to the invention, the manganese oxide and the cobalt oxide are sintered after being mixed in a nano scale, the diffusion path of the cobalt element and the manganese element is short, and the surface tunnel reaction of the particle surface in the nano scale can be exerted, namely, the elements can be rapidly diffused on the nano surface, and the cobalt element and the manganese element can be rapidly diffused to form a biphase eutectic structure in the sintering process.
If the mass ratio of the manganic oxide powder to the cobaltosic oxide powder is lower than 0.8:1 or higher than 1:0.8, a complete eutectic structure cannot be formed in the sintering process, and if the mass ratio is too low or too high, cubic phases (Mn, co) cannot be formed simultaneously in the sintering process 3 O 4 And tetragonal phase (Mn, co) 3 O 4 。
If the sintering temperature is too high, more than 1200 ℃, the powder is easy to agglomerate in the sintering process, ceramic powder cannot be obtained, if the sintering temperature is too low, less than 1120 ℃, cobalt element and manganese element cannot be fully diffused in the sintering process, and cubic phases (Mn, co) are affected 3 O 4 And tetragonal phase (Mn,Co) 3 O 4 The invention can promote the mutual diffusion of cobalt element and manganese element to form a phase interface, improve conductivity, and can sinter and fuse the inside of powder particles to improve the density, strength and fluidity of the powder.
In the invention, the particle size of the manganic oxide raw material powder and the cobaltosic oxide raw material powder can be selected in a wider range, and only a suspension of the manganic oxide and the cobaltosic oxide mixed in a nanometer scale can be obtained after ball milling treatment and separation treatment. In some preferred embodiments, the average particle size of the manganic oxide raw material powder and the cobaltosic oxide raw material powder is 0.1-10 μm, and under the preferred scheme, the ball milling treatment and the separation treatment are more beneficial to obtain a mixed suspension of the manganic oxide and the cobaltosic oxide in nanometer scale, so that the mutual diffusion of cobalt element and manganese element in the sintering process is promoted, and a biphasic eutectic fine crystal structure is formed.
In the invention, the composition of the first slurry has wider optional range, the manganic oxide raw material powder and the cobaltosic oxide raw material powder can be crushed and uniformly mixed only through ball milling treatment, and the mixed suspension of the manganic oxide and the cobaltosic oxide in nanometer scale can be obtained after separation treatment, and meanwhile, the agglomerated powder can be prepared only through later spray drying. In some preferred embodiments, the mixed powder of manganous oxide and tricobalt tetraoxide in the first slurry has a content of 60 to 75wt%, a content of the solvent has a content of 20 to 35wt%, and a content of the binder has a content of 5 to 10wt%. Under the preferred scheme, the method is more beneficial to obtaining the mixed suspension of the manganic oxide and the cobaltosic oxide in the nanometer scale after separation treatment. The content of the binder in the first slurry is controlled to be 5-10wt%, so that the agglomeration powder is prepared by spray drying in the later period.
In the invention, the ball milling treatment condition has wider optional range, so that the manganic oxide raw material powder and the cobaltosic oxide raw material powder can be crushed and uniformly mixed through the ball milling treatment, and the suspension of the manganic oxide and the cobaltosic oxide mixed in nano scale can be obtained after the separation treatment. In some preferred embodiments, the ball milling treatment uses a ball mill with a ball mill diameter of 2.5-3.5 mm with a ratio of 20-30wt% and a ball mill with a ball mill diameter of 4.5-5.5mm with a ratio of 70-80wt%, and the ball milling treatment has a rotation speed of 500-2000r/min for 20-50h. Under the preferred scheme, the method is more beneficial to obtaining the suspension of the mixture of the manganic oxide and the cobaltosic oxide in the nanometer scale after separation treatment, promotes the mutual diffusion of cobalt element and manganese element in the sintering process, forms a biphase eutectic fine crystal structure, and improves the conductivity, the strength and the compactness of the conductive powder.
In the present invention, the range of choice for the solvent is wide as long as the mixed powder raw material can be sufficiently dispersed and removed in the spray drying process, and the solvent is optionally water, ethanol or the like.
In the present invention, the optional range of the binder is wide as long as the mixed powder can be formed into agglomerated powder by spray drying, and the binder is optionally polyvinyl alcohol or the like.
In the present invention, the method of separation treatment may include filtration, precipitation, and the like. In some preferred embodiments, the separation treatment comprises filtering the first slurry to obtain a second slurry, and precipitating the second slurry to obtain the suspension and the precipitate. The large-particle manganic oxide and cobaltosic oxide powder in the first slurry can be filtered through filtration treatment to obtain a filtrate containing fine particles distributed in a certain size fraction, and the filtrate containing the fine particles can be subjected to precipitation treatment to obtain a suspension of the mixture of the manganic oxide and the cobaltosic oxide in a nano scale.
In the invention, the filtering method and the time of the precipitation treatment can be selected within a wider range, and the suspension of the manganese tetraoxide and the cobalt tetraoxide mixed in the nanometer scale can be obtained after the filtering and the precipitation treatment. In some preferred embodiments, the filtration treatment comprises filtration treatment with a screen having a pore size of 4-6 μm, and the precipitation treatment is performed for a period of not less than 10 hours. Under the preferred scheme, the mixed suspension of the manganic oxide and the cobaltosic oxide in the nanometer scale can be efficiently obtained, and the mutual diffusion of cobalt element and manganese element in the sintering process is promoted to form a biphase eutectic fine crystal structure.
In the present invention, the range of options for particle size of the particles in the suspension is broad. In some preferred embodiments, the particle size of the particles in the suspension is less than 50nm. Under the preferred scheme, the diffusion paths of cobalt element and manganese element are short, the surface tunnel reaction of nano-scale particles is easily exerted, and eutectic structures are easily obtained.
In the invention, the precipitate obtained by the separation treatment can be recycled. In some preferred embodiments, the precipitate is returned to a ball milling apparatus for the ball milling process. The particle size of the precipitate obtained by separation treatment is thicker, if the precipitate is directly granulated and sintered, the diffusion path of cobalt element and manganese element among large particles is too large, the nano surface tunnel effect cannot be exerted, the cobalt element and manganese element cannot be rapidly and fully diffused, the phase of the original powder still remains in the prepared ceramic powder, the grain size is large, a complete biphasic eutectic fine crystal structure cannot be formed, the strength of the ceramic powder is further influenced, and the conductivity of the ceramic powder is influenced due to the fact that the complete biphasic eutectic fine crystal structure cannot be formed, the phase interface is less, the electron conduction channels are less, but the ceramic powder can be reused as a return material for crushing and mixing treatment, and the suspension of the manganese tetraoxide and the cobalt tetraoxide mixed in the nanometer scale is prepared.
In the present invention, the operating conditions for the spray drying and the particle size of the agglomerated powder are selected within a wide range. In some preferred embodiments, the agglomerated powder has an average particle size of 20 to 50 μm. In some preferred embodiments, the spray drying inlet temperature is 200-350 ℃, the spray drying outlet temperature is 120-180 ℃, the rotating speed of the atomizing disk is 30-40Hz, and the feeding flow rate is 70-150g/min.
In a second aspect, the present invention provides a ceramic powder produced by the production method of the first aspect.
Cubic phase (Mn, co) in the ceramic powder of the invention 3 O 4 And tetragonal phase (Mn, co) 3 O 4 Constituting nanoscaleThe grains are very small, so that a rich phase interface can be provided, a rich electron conduction channel is provided, and the conductivity of the ceramic powder is improved. The ceramic powder is very suitable for thermal spraying, glue injection molding, casting and other processes.
In some preferred embodiments, the ceramic powder has a grain size of less than 100nm, and a cubic phase (Mn, co) in the ceramic powder 3 O 4 The phase content of (C) is 45% -55%, and tetragonal phase (Mn, co) 3 O 4 The phase content of the ceramic powder is 45% -55%, and the strength of the ceramic powder is more than 500Mpa.
The invention will be further described in detail with reference to specific examples.
Example 1
A preparation method of ceramic powder comprises the following steps:
step one: adding 400g of manganous oxide powder, 500g of cobaltosic oxide powder, 500g of deionized water and 80g of polyvinyl alcohol binder into a ball milling device, and performing ball milling for 20 hours at the speed of 500 r/min, wherein the average particle size of the manganous oxide powder is 0.1 mu m, the average particle size of the cobaltosic oxide powder is 0.1 mu m, the 3mm diameter ball accounts for 25 wt percent of grinding balls used in ball milling, the 5mm diameter ball accounts for 75wt percent of grinding balls, and obtaining first slurry after ball milling treatment;
filtering the first slurry by using a 5 mu m screen to obtain second slurry containing fine particles, and naturally precipitating the second slurry for 10 hours to obtain an upper suspension and a lower precipitate;
granulating the upper suspension serving as a spray drying raw material in a spray drying device to obtain agglomerated powder, wherein in the spray drying process, the inlet temperature is 200-350 ℃, the outlet temperature is 120-180 ℃, the rotating speed of an atomizing disk is 30-40Hz, and the feeding flow rate is 150g/min;
and fourthly, sintering the agglomerated powder in a muffle furnace, wherein the sintering temperature is 1120 ℃, the sintering time is 1h, and the ceramic powder is obtained after the sintering.
Example 2
Reference example 1 was made, except that in step one, the addition amount of the manganese tetraoxide powder was 500g, the addition amount of the cobalt tetraoxide powder was 400g, the addition amount of deionized water was 500g, and the addition amount of the polyvinyl alcohol binder was 80g.
Example 3
Reference example 1 was made, except that in step one, the average particle diameter of the manganous oxide powder was 10 μm and the average particle diameter of the tricobalt tetraoxide powder was 10 μm.
Example 4
The process was carried out with reference to example 1, except that the lower precipitate of step two was returned to the ball milling apparatus for ball milling treatment.
Example 5
Reference example 1 was made, except that in step four, the sintering treatment was performed at 1200 ℃ for 10min.
Comparative example 1
Reference example 1 was carried out, except that in step one, 1000g (Mn, co) was added to the ball mill 3 O 4 Powder (tetragonal phase), 500g deionized water and 80g polyvinyl alcohol binder.
Comparative example 2
Reference example 1 was made, except that only the lower precipitate obtained in step two was subjected to sintering treatment in a muffle furnace.
Comparative example 3
The procedure was carried out in accordance with example 1, except that the sintering treatment in step four was not carried out, and the upper suspension in step two was spray-dried to directly obtain ceramic powder.
Comparative example 4
Reference example 1 was made, except that the sintering treatment temperature was 1250℃and the sintering treatment time was 10min.
Comparative example 5
Reference example 1 was made, except that the sintering treatment temperature was 1100℃and the sintering treatment time was 50 hours.
Test case
The ceramic powder of example 1 was examined for its microscopic morphology and internal nano-eutectic structure, and the results are shown in fig. 1 and 2.
The phase composition and phase content of the ceramic powders of examples 1 to 5 and comparative examples 1 to 5 were measured by X-ray diffraction analysis (GB/T5225-1985), and the measurement results are shown in Table 1.
The grain sizes of the ceramic powders of examples 1 to 5 and comparative examples 1 to 5 were examined, and the specific examination method of the grain sizes was electron microscopic image analysis (JY/T010-1996), and the examination results are shown in Table 1.
The strength of the ceramic powders of examples 1 to 5 and comparative examples 1 to 5 was measured, and the specific measurement method of the strength was powder particle compression strength analysis (JIS R1639-5:2007), and the test results are shown in Table 1.
TABLE 1
As can be seen from fig. 1 and 2, with the embodiment of the present invention, it is possible to form spherical ceramic powder having a two-phase eutectic structure, the grain size of which is nano-scale. As can be seen from Table 1 and FIGS. 1 and 2, with the embodiment of the present invention, the crystal grain size < 100nm can be formed with cubic phases (Mn, co) at the same time, compared with the comparative example 3 O 4 And tetragonal phase (Mn, co) 3 O 4 The strength of the ceramic powder is higher and reaches more than 500MPa. Further, it can be seen from example 1 and comparative example 1 that only tetragonal phase (Mn, co) was used 3 O 4 The powder is used as a raw material, the formed ceramic powder has one phase, no phase interface and large grain size, and a rapid channel can not be provided for electronic conduction; as can be seen from example 1 and comparative example 2, if the lower layer precipitation sintering with a larger particle size is adopted, the original powder phase remains in the ceramic powder, the grain size is larger, the biphasic eutectic fine crystal structure cannot be obtained, and the strength of the ceramic powder is limited; as can be seen from example 1 and comparative example 3, if the sintering treatment is not performed, the agglomerated powder of the trimanganese tetraoxide and tricobalt tetraoxide mixed at the nano scale does not exhibit a biphasic eutectic structure, the strength of the powder is low, and according to example 1, comparative examples 4 and 5, it is possible toIt can be seen that if the sintering temperature is too high, more than 1200 ℃, the powder is easy to agglomerate in the sintering process, ceramic powder cannot be obtained, and if the sintering temperature is too low, less than 1120 ℃, cobalt element and manganese element cannot be fully diffused, and cubic phases (Mn, co) are affected 3 O 4 And tetragonal phase (Mn, co) 3 O 4 Is formed of a biphasic eutectic structure.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. A method of preparing ceramic powder, the method comprising:
dispersing manganous oxide powder and cobaltosic oxide powder in a solvent through ball milling treatment to obtain first slurry, and separating and treating the first slurry to obtain suspension and precipitate, wherein the manganous oxide and the cobaltosic oxide in the suspension are mixed in a nanoscale, and the mass ratio of the manganous oxide powder to the cobaltosic oxide powder is 0.8:1-1:0.8; the particle size of the particles in the suspension is less than 50nm;
spray drying the suspension to obtain agglomerated powder; sintering the agglomerated powder to obtain the ceramic powder, wherein the sintering temperature is 1120-1200 ℃ and the sintering time is 10 min-1 h;
the ceramic powder has a cubic phase (Mn, co) 3 O 4 And tetragonal phase (Mn, co) 3 O 4 The grain size of the dual-phase eutectic structure is less than 100nm.
2. The method according to claim 1, wherein the average particle size of the manganic oxide powder and the tricobalt tetraoxide powder is 0.1 to 10 μm.
3. The preparation method according to claim 1, wherein the content of the mixed powder of the manganic oxide and the tricobalt tetraoxide in the first slurry is 60-75wt%, the content of the solvent is 20-35wt%, and the content of the binder is 5-10wt%.
4. The preparation method according to claim 1, wherein the ball milling treatment is performed at a rotation speed of 500-2000r/min for 20-50h, wherein the ball milling treatment is performed at a rotation speed of 2.5-3.5 mm, wherein the ball milling treatment is performed at a rotation speed of 20-30 wt% and the ball milling treatment is performed at a rotation speed of 4.5-5.5 mm.
5. The method of claim 1, wherein the separating comprises filtering the first slurry to obtain a second slurry, and precipitating the second slurry to obtain the suspension and the precipitate.
6. The method according to claim 5, wherein the filtration treatment comprises filtration treatment with a screen having a pore size of 4 to 6 μm, and the time of the precipitation treatment is not less than 10 hours.
7. The method according to claim 1, wherein the ball milling is performed by returning the precipitate to a ball milling apparatus.
8. Ceramic powder, characterized in that it is produced by the production method according to any one of claims 1 to 7.
9. The ceramic powder of claim 8, wherein the ceramic powder has a grain size of less than 100nm, and wherein the ceramic powder has a cubic phase (Mn, co) 3 O 4 The phase content of (C) is 45% -55%, and tetragonal phase (Mn, co) 3 O 4 The phase content of the ceramic powder is 45% -55%, and the strength of the ceramic powder is more than 500Mpa.
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