CN114671679A - Zirconium pyrophosphate complex phase ceramic material and preparation method thereof - Google Patents
Zirconium pyrophosphate complex phase ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a zirconium pyrophosphate complex phase ceramic material and a preparation method thereof. The technical scheme is as follows: firstly, mixing ammonium dihydrogen phosphate, zirconia and rare earth oxide, performing ball milling by taking ethanol as a ball milling medium, and drying; preserving heat at 600-900 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder; mixing 35-54 wt% of magnesium oxide, 12-25 wt% of molybdenum oxide and 22-41 wt% of vanadium oxide, mixing with the zirconium pyrophosphate complex phase powder, ball-milling, and drying to obtain zirconium pyrophosphate complex phase ceramic powder; carrying out mechanical pressing forming and cold isostatic pressing forming on the zirconium pyrophosphate multiphase ceramic powder to obtain a zirconium pyrophosphate multiphase ceramic blank; and heating the zirconium pyrophosphate complex phase ceramic blank to 1000-1300 ℃, and preserving heat to prepare the zirconium pyrophosphate complex phase ceramic material. The product prepared by the invention has the advantages of low dielectric constant, small dielectric loss, high density, excellent thermal expansion performance, and obviously improved bending strength and thermal insulation performance.
Description
Technical Field
The invention belongs to the technical field of zirconium pyrophosphate ceramic materials. In particular to a zirconium pyrophosphate complex phase ceramic material and a preparation method thereof.
Background
Zirconium pyrophosphate ceramics have recently received much attention from researchers because of their advantages such as low thermal expansion coefficient, high temperature resistance, good dielectric properties, good corrosion resistance, and low thermal conductivity. Zirconium pyrophosphate ceramic is used as a novel ceramic material with excellent performance and wide prospect, and can be widely applied to the field of materials such as solid electrolyte, heat insulation materials, wave-transmitting materials, low-expansion materials and the like.
The heat generated by the friction of supersonic aircraft surfaces affects the service and life of the components inside the aircraft. In order to protect parts inside the aircraft, higher requirements are placed on the heat insulation performance of the wave-transparent material, and therefore, the supersonic aircraft adopting the wave-transparent material needs to have good heat insulation performance and wave-transparent matching performance. In the existing technical research of wave-transparent materials, phosphate ceramics have the advantages of high temperature resistance, low thermal conductivity and the like compared with other inorganic non-metallic ceramics, but the research of the phosphate ceramics for the wave-transparent materials is less than that of the other inorganic non-metallic ceramics.
The conventional preparation method of zirconium pyrophosphate powder commonly comprises a coprecipitation method, a hydrothermal method and a solid phase method, wherein the zirconium pyrophosphate powder prepared by the coprecipitation method and the hydrothermal method has small crystal grains, but has the defects of complex process, high production cost and low yield, and is difficult to realize large-scale production; the solid phase method has strong practical significance because the process is simple, the preparation period is short, and the synthesis purity is high. The single-phase pyrophosphate ceramic material is difficult to meet the requirement of practical application.
At present, the existing technology for preparing zirconium pyrophosphate ceramic material, such as the technology of the 'preparation method of zirconium phosphate ceramic material' (CN1844042A) patent, discloses a preparation method of zirconium pyrophosphate ceramic material, wherein zirconium oxide and phosphoric acid with the concentration of 85% are selected as raw materials, zirconium pyrophosphate ceramic is prepared by a solid phase method, but phosphoric acid is volatile in the heating process, is easy to generate harm to human bodies and environment, meanwhile, the sintering temperature is as high as 1500 ℃, the sintering temperature is not favorable for energy conservation and emission reduction, the flexural strength is only 132MPa at most, the application to scenes with higher flexural strength requirements is difficult, the dielectric constant is 7.5-8.5, and the dielectric loss is 4.0-7.5 multiplied by 10-3The dielectric constant and the dielectric loss are both high, and the lowest density is only 95.8%; as another example of the 'zirconium phosphate ceramic material and preparation method thereof' (ZL201911257987.4) patent technology, zirconium pyrophosphate ceramic material is prepared by using zirconium oxide and ammonium dihydrogen phosphate through a solid phase method, because the main crystal phase of the ceramic material is zirconium pyrophosphate, a small amount of low-melting-point phase exists at the same time, the maximum flexural strength is only 194.6MPa (lower than 200MPa), the sintering temperature is as high as 1400 ℃, energy conservation and emission reduction are not easy, the dielectric constant is 4.3-7.8, and the dielectric loss is 2.5-7.4 × 10-3The dielectric constant and the dielectric loss are still high, the normal-temperature heat conductivity coefficient is 0.27-0.58W/(m.K), the heat insulation performance is poor, and the density is still low even if the density is 96.2% at the lowest.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide the zirconium pyrophosphate complex phase ceramic material which has simple process, short production period, low sintering temperature and environmental protection and can obviously improve the bending strength and the heat preservation and insulation performance on the basis of low dielectric constant, small dielectric loss, excellent thermal expansion performance and high density.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the molar ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 1.8-2.8: 0.8: 0.05-0.2 to obtain a mixture I; then, ball-milling and drying the mixture I by taking ethanol as a ball-milling medium; and then preserving heat for 1-6 hours at the temperature of 600-900 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 35-54 wt% of magnesium oxide, 12-25 wt% of molybdenum oxide and 22-41 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 1-5, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing machine-pressing molding on the zirconium pyrophosphate complex phase ceramic powder under the condition of 20-50 MPa, and performing cold isostatic pressing molding under the condition of 200-500 MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1000-1300 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 1-5 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
The purity of the ammonium dihydrogen phosphate is more than 99.0 percent; the particle size is less than 100 μm.
The purity of the zirconia is more than 99.9%; the particle size is less than 2 μm.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide; the purity of the rare earth oxide is more than 99.9%, and the particle size is less than 0.5 μm.
The purity of the magnesium oxide is more than 99.9%; the particle size is less than 0.5 μm.
The purity of the molybdenum oxide is more than 99.9%; the particle size is less than 0.5 μm.
The purity of the vanadium oxide is more than 99.9 percent; the particle size is less than 0.5 μm.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the zirconium pyrophosphate multiphase ceramic material is prepared by mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide, ball-milling by taking ethanol as a ball-milling medium, drying, performing heat treatment and crushing to obtain zirconium pyrophosphate multiphase powder, then mixing with a mixture prepared by mixing magnesium oxide, molybdenum oxide and vanadium oxide, performing ball-milling, drying, mechanical pressing and cold isostatic pressing, and heating to 1000-1300 ℃. The method has the advantages of simple process and short production period, obviously reduces the sintering temperature and has obvious energy-saving and emission-reducing effects compared with zirconium pyrophosphate ceramics without rare earth oxide.
2. According to the invention, rare earth phosphate can be generated in the sintering process by adding rare earth oxide, and the in-situ synthesized rare earth phosphate can effectively combine zirconium pyrophosphate particles; therefore, the rare earth phosphate can play a role of a binding agent, achieve the effect of complex phase reinforcement, inhibit the growth of crystal grains, and improve the flexural strength and the density of the zirconium pyrophosphate complex phase ceramic material. Meanwhile, the rare earth element is dissolved in the phosphate structure in a solid way, so that the heat conductivity of the zirconium pyrophosphate complex phase ceramic material is reduced, and the heat insulation performance is improved.
3. According to the invention, magnesium oxide, molybdenum oxide and vanadium oxide are used as sintering aids, and the low-melting-point phase formed by reaction with zirconium pyrophosphate promotes the sintering of the zirconium pyrophosphate ceramic material, so that the flexural strength and the density of the zirconium pyrophosphate complex phase ceramic material can be remarkably improved.
The zirconium pyrophosphate complex phase ceramic material prepared by the invention is analyzed by X-ray diffraction, the main crystal phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate. Through detection: the density is 97.2-99.8%; the bulk density is 2.82-3.14 g/cm3(ii) a The normal-temperature flexural strength is 215.4-327.6 MPa; a coefficient of thermal expansion of 0.7 to 1.6 x 10-6V. (0-600 ℃); the dielectric constant at normal temperature is 3.3-5.7 (the frequency is 10 GHz); the dielectric loss at room temperature is 7.4-9.8 x 10-4(frequency 10 GHz); the coefficient of thermal conductivity at room temperature is 0.15-0.42W/(mK).
Therefore, the invention has the characteristics of simple process, short production period and environmental protection, and the prepared zirconium pyrophosphate complex phase ceramic material has obviously improved bending strength and heat preservation and insulation performance on the basis of low dielectric constant, small dielectric loss, excellent thermal expansion performance and high density.
Drawings
FIG. 1 is an XRD pattern of a zirconium pyrophosphate complex phase ceramic material prepared by the present invention;
FIG. 2 is an SEM image of the zirconium pyrophosphate composite ceramic material shown in FIG. 1 after polishing treatment.
FIG. 3 is an EDS energy spectrum within the black box region shown in FIG. 2;
FIG. 4 is an SEM image of the fracture morphology of the zirconium pyrophosphate complex phase ceramic material shown in FIG. 1;
fig. 5 is a back-scattered SEM image of fig. 4.
Detailed Description
The invention is further described with reference to the following figures and detailed description, without limiting the scope of the invention.
A zirconium pyrophosphate complex phase ceramic material and a preparation method thereof are disclosed: the preparation method shown in the specific embodiment comprises the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the molar ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 1.8-2.8: 0.8: 0.05-0.2 to obtain a mixture I; then, taking ethanol as a ball milling medium, carrying out ball milling on the mixture I, and drying; and then preserving heat for 1-6 hours at the temperature of 600-900 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 35-54 wt% of magnesium oxide, 12-25 wt% of molybdenum oxide and 22-41 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 1-5, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing machine-pressing molding on the zirconium pyrophosphate complex phase ceramic powder under the condition of 20-50 MPa, and performing cold isostatic pressing molding under the condition of 200-500 MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1000-1300 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 1-5 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide.
In this embodiment:
the purity of the ammonium dihydrogen phosphate is more than 99.0 percent; the grain diameter is less than 100 mu m;
the purity of the zirconia is more than 99.9%; the grain diameter is less than 2 mu m;
the purity of the rare earth oxide is more than 99.9%, and the particle size is less than 0.5 mu m;
the purity of the magnesium oxide is more than 99.9%; the grain diameter is less than 0.5 mu m;
the purity of the molybdenum oxide is more than 99.9%; the grain diameter is less than 0.5 mu m;
the purity of the vanadium oxide is more than 99.9%; the particle size is less than 0.5 μm.
The details in the embodiments are not repeated.
Example 1
Zirconium pyrophosphate complex phase ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the molar ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 1.8: 0.8: 0.05 to obtain a mixture I; then, taking ethanol as a ball milling medium, carrying out ball milling on the mixture I, and drying; then preserving the heat for 1 hour at the temperature of 600 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 35 wt% of magnesium oxide, 25 wt% of molybdenum oxide and 40 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 1, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing mechanical pressing on the zirconium pyrophosphate complex phase ceramic powder under the condition of 20MPa, and performing cold isostatic pressing under the condition of 200MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1000 ℃ under the conditions of air atmosphere and normal pressure, and preserving heat for 1 hour to prepare the zirconium pyrophosphate complex phase ceramic material.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide;
the zirconium pyrophosphate complex phase ceramic material prepared by the embodiment is analyzed by X-ray diffraction, the main crystal phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate. And (3) detection: the density is 97.2%; the bulk density is 2.82g/cm3(ii) a The normal temperature rupture strength is 215.4 MPa; coefficient of thermal expansion of 0.7X 10-6V. (0-600 ℃); the dielectric constant at normal temperature is 3.3 (the frequency is 10 GHz); dielectric loss at room temperature of 7.4X 10-4(frequency 10 GHz); the thermal conductivity at normal temperature is 0.15W/(mK).
Example 2
Zirconium pyrophosphate complex phase ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the mol ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 2.2: 0.8: 0.1 to obtain a mixture I; then, ball-milling and drying the mixture I by taking ethanol as a ball-milling medium; then preserving the heat for 3 hours at the temperature of 700 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 54 wt% of magnesium oxide, 12 wt% of molybdenum oxide and 34 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 3, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing mechanical pressing on the zirconium pyrophosphate complex phase ceramic powder under the condition of 30MPa, and performing cold isostatic pressing under the condition of 400MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1100 ℃ under the conditions of air atmosphere and normal pressure, and preserving heat for 3 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide;
the zirconium pyrophosphate complex phase ceramic material prepared by the embodiment is analyzed by X-ray diffraction, the main crystal phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate. Through detection: the density is 97.6%; the bulk density is 2.98g/cm3(ii) a The normal temperature rupture strength is 280.6 MPa; coefficient of thermal expansion of 1.0X 10-6V. (0-600 ℃); the dielectric constant at normal temperature is 4.2 (the frequency is 10 GHz); dielectric loss at room temperature of 7.9X 10-4(frequency 10 GHz); the thermal conductivity at room temperature is 0.24W/(mK).
Example 3
A zirconium pyrophosphate complex phase ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the mol ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 2.8: 0.8: 0.2 to obtain a mixture I; then, ball-milling and drying the mixture I by taking ethanol as a ball-milling medium; then preserving the heat for 5 hours at the temperature of 800 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 39 wt% of magnesium oxide, 20 wt% of molybdenum oxide and 41 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 5, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing mechanical pressing on the zirconium pyrophosphate complex phase ceramic powder under the condition of 50MPa, and performing cold isostatic pressing under the condition of 500MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1200 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 5 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide;
the zirconium pyrophosphate complex phase ceramic material prepared by the embodiment is analyzed by X-ray diffraction, the main crystal phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate. Through detection: the density is 99.8%; the bulk density is 3.14g/cm3(ii) a The normal-temperature rupture strength is 327.6 MPa; coefficient of thermal expansion of 1.6X 10-6V. (0-600 ℃); the dielectric constant at normal temperature is 5.7 (the frequency is 10 GHz); dielectric loss at room temperature of 9.8X 10-4(frequency 10 GHz); the thermal conductivity at room temperature is 0.42W/(mK).
Example 4
A zirconium pyrophosphate complex phase ceramic material and a preparation method thereof. The preparation method of the embodiment comprises the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the mol ratio of 2.4: 0.8: 0.15 to obtain a mixture I; then, taking ethanol as a ball milling medium, carrying out ball milling on the mixture I, and drying; and then preserving the heat for 1-6 hours at 900 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder.
Step two, mixing 53 wt% of magnesium oxide, 25 wt% of molybdenum oxide and 22 wt% of vanadium oxide to obtain a mixture II; and mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 3, ball-milling and drying to obtain the zirconium pyrophosphate complex phase ceramic powder.
And thirdly, performing mechanical pressing on the zirconium pyrophosphate complex phase ceramic powder under the condition of 40MPa, and performing cold isostatic pressing under the condition of 400MPa to obtain a zirconium pyrophosphate complex phase ceramic blank.
And step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1300 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 3 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
The rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide;
the zirconium pyrophosphate complex phase ceramic material prepared by the embodiment is analyzed by X-ray diffraction, the main crystal phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate. Through detection: the density is 98.5%; the bulk density is 3.03g/cm3(ii) a The normal-temperature rupture strength is 297.3 MPa; coefficient of thermal expansion of 1.4X 10-6V. (0-600 ℃); the dielectric constant at normal temperature is 5.2 (the frequency is 10 GHz); dielectric loss at room temperature of 9.2X 10-4(frequency 10 GHz); the thermal conductivity at room temperature is 0.35W/(mK).
Compared with the prior art, the specific implementation mode has the following positive effects:
1. in the specific embodiment, ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide are mixed, ethanol is used as a ball milling medium for ball milling, drying is carried out, heat treatment and crushing are carried out to obtain zirconium pyrophosphate complex phase powder, then the zirconium pyrophosphate complex phase powder is mixed with a mixture of magnesium oxide, molybdenum oxide and vanadium oxide, ball milling, drying, mechanical pressing and cold isostatic pressing are carried out, heating is carried out to 1000-1300 ℃, and the zirconium pyrophosphate complex phase ceramic material is prepared. The specific implementation mode has the advantages of simple process and short production period, and compared with zirconium pyrophosphate ceramics without rare earth oxide, the specific implementation mode reduces the sintering temperature and achieves the effects of energy conservation and emission reduction.
2. The zirconium pyrophosphate complex phase ceramic material prepared by adding rare earth oxide in the specific embodiment is shown in the attached drawing: FIG. 1 is an XRD pattern of the zirconium pyrophosphate complex phase ceramic material prepared in example 3, FIG. 2 is an SEM pattern of the zirconium pyrophosphate complex phase ceramic material prepared in example 3 after polishing treatment, and FIG. 3 is aFIG. 2 is an EDS spectrum in a black frame region, FIG. 4 is a SEM image of a fracture morphology of the zirconium pyrophosphate complex phase ceramic material prepared in example 3, and FIG. 5 is a back-scattering SEM image of FIG. 4; as can be seen from FIG. 1, the primary crystal phase in the phase is zirconium pyrophosphate, and the secondary crystal phase is rare earth phosphate; from FIG. 2 and FIG. 3 in conjunction with FIG. 1, it can be seen that the white area in FIG. 2 is CePO4Particles; from FIGS. 4 and 5, it can be seen that CePO4The particles are distributed around the zirconium pyrophosphate particles and are tightly combined, and the rare earth phosphate can play a better role in combining in the zirconium pyrophosphate phase. Rare earth phosphate can be generated in the sintering process of the rare earth oxide, and the in-situ synthesized rare earth phosphate can be effectively combined with zirconium pyrophosphate particles, so that the in-situ rare earth phosphate can play a role of a binding agent, the effect of complex phase reinforcement is achieved, the growth of crystal grains is inhibited, and the flexural strength and the density of the material are improved. Meanwhile, rare earth elements are dissolved in a phosphate structure in a solid mode, the heat conductivity of the material is reduced, the heat insulation performance is improved, and compared with zirconium pyrophosphate ceramics only added with a sintering aid, the sintering temperature is reduced, and the effects of energy conservation and emission reduction are achieved.
3. According to the specific embodiment, magnesium oxide, molybdenum oxide and vanadium oxide are used as sintering aids, and the sintering of the zirconium pyrophosphate ceramic material is promoted by forming a low-melting-point phase through reaction with zirconium pyrophosphate, so that the flexural strength and the compactness of the zirconium pyrophosphate complex-phase ceramic material can be remarkably improved.
Therefore, the specific implementation mode has the characteristics of simple process, short production period and environmental friendliness, and the prepared zirconium pyrophosphate complex phase ceramic material has obviously improved bending strength and heat insulation performance on the basis of low dielectric constant, small dielectric loss, excellent thermal expansion performance and high density.
Claims (8)
1. A preparation method of zirconium pyrophosphate complex phase ceramic material is characterized by comprising the following steps:
step one, mixing ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide according to the molar ratio of ammonium dihydrogen phosphate, zirconium oxide and rare earth oxide of 1.8-2.8: 0.8: 0.05-0.2 to obtain a mixture I; then, taking ethanol as a ball milling medium, carrying out ball milling on the mixture I, and drying; then preserving heat for 1-6 hours at the temperature of 600-900 ℃, and crushing to obtain zirconium pyrophosphate complex phase powder;
step two, mixing 35-54 wt% of magnesium oxide, 12-25 wt% of molybdenum oxide and 22-41 wt% of vanadium oxide to obtain a mixture II; mixing the zirconium pyrophosphate complex phase ceramic powder and the mixture II according to the mass ratio of 100: 1-5, ball-milling and drying to obtain zirconium pyrophosphate complex phase ceramic powder;
thirdly, mechanically pressing the zirconium pyrophosphate complex phase ceramic powder under the condition of 20-50 MPa, and then carrying out cold isostatic pressing under the condition of 200-500 MPa to obtain a zirconium pyrophosphate complex phase ceramic blank;
and step four, heating the zirconium pyrophosphate complex phase ceramic blank to 1000-1300 ℃ under the conditions of air atmosphere and normal pressure, and preserving the heat for 1-5 hours to prepare the zirconium pyrophosphate complex phase ceramic material.
2. The method for preparing zirconium pyrophosphate complex phase ceramic material according to claim 1, characterized in that the purity of said ammonium dihydrogen phosphate is more than 99.0%; the particle size is less than 100 μm.
3. The method for preparing zirconium pyrophosphate complex phase ceramic material according to claim 1, characterized in that the purity of said zirconium oxide is more than 99.9%; the particle size is less than 2 μm.
4. The method for preparing zirconium pyrophosphate multiphase ceramic material according to claim 1, wherein the rare earth oxide is one of cerium oxide, neodymium oxide, europium oxide and samarium oxide; the purity of the rare earth oxide is more than 99.9%, and the particle size is less than 0.5 μm.
5. The method for preparing zirconium pyrophosphate complex phase ceramic material according to claim 1, characterized in that the purity of said magnesium oxide is more than 99.9%; the particle size is less than 0.5 μm.
6. The method for preparing zirconium pyrophosphate complex phase ceramic material according to claim 1, characterized in that the purity of said molybdenum oxide is more than 99.9%; the particle size is less than 0.5 μm.
7. The method for preparing zirconium pyrophosphate complex phase ceramic material according to claim 1, characterized in that the purity of said vanadium oxide is more than 99.9%; the particle size is less than 0.5 μm.
8. The zirconium pyrophosphate complex phase ceramic material is characterized in that the zirconium pyrophosphate complex phase ceramic material is prepared by the preparation method of the zirconium pyrophosphate complex phase ceramic material according to any one of claims 1 to 7.
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