CN110438384B - Iron-nickel-based ultrafine-grained hard alloy and preparation method thereof - Google Patents
Iron-nickel-based ultrafine-grained hard alloy and preparation method thereof Download PDFInfo
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Abstract
The invention provides an iron-nickel-based ultrafine-grained hard alloy and a preparation method thereof, belonging to the technical field of metal materials. The invention adds Al and M in the iron-nickel matrixo, microalloying is carried out, so that the iron-nickel-based hard alloy has the effect of strengthening the iron-nickel binding phase by solid solution and can improve the strength of the iron-nickel-based hard alloy; meanwhile, the dissolution and precipitation of WC in the iron-nickel matrix can be inhibited, so that the growth of WC crystal grains is inhibited; in addition, after the iron-nickel matrix is microalloyed by using Al and Mo, FeAl, NiAl and Ni can be used as a binding phase of the hard alloy during sintering and aging treatment3Al、Fe3Al and other long-range ordered phases are precipitated in the iron-nickel matrix in a desolvation manner to form a nano-scale strengthening phase which is dispersed and compatible with the iron-nickel matrix, so that the toughness of the iron-nickel-based hard alloy is improved.
Description
Technical Field
The invention relates to the technical field of metal materials, in particular to an iron-nickel-based ultrafine grained hard alloy and a preparation method thereof.
Background
The hard alloy consists of hard carbide and soft binding metal, the carbide provides load bearing capacity and wear resistance for the hard alloy, and the binding metal endows the hard alloy with impact-resistant toughness through the capacity of plastic deformation at room temperature. The hard alloy combines the advantages of high-hardness refractory metal carbide and bonding metal with better ductility, has a series of excellent performances of high strength and hardness, good wear resistance, good red hardness, small thermal expansion coefficient, high elastic modulus, good chemical stability and the like, and is widely applied to the fields of cutting tools, mine tools, wear-resistant parts and the like.
The common hard phases in cemented carbide are mainly WC, TiC, TaC, NbC, VC and the like, the WC is taken as the main component, and metal Co has good wettability and cohesiveness to the hard phases such as WC and the like, so that Co is usually selected as the binder phase in cemented carbide. However, Co is expensive, and Co dust, especially ultra-fine or nano-sized Co dust, has adverse effects on the environment and human health.
In recent years, a new cemented carbide using an iron-nickel alloy or an intermetallic compound instead of cobalt as a binder phase has attracted much attention from researchers at home and abroad. However, the iron-nickel cobalt-substituted hard alloy in the prior art has the problem of poor mechanical properties such as hardness, bending strength and the like; and FeAl, NiAl and Ni are adopted3Al、Fe3The performance of the hard alloy taking Fe-Ni alloyed by intermetallic compounds such as Al as a binding phase is improved compared with that of the common Fe-Ni cobalt-substituted hard alloy, but is still lower than that of the traditional WC-Co hard alloy.
Disclosure of Invention
The invention aims to provide an iron-nickel-based ultrafine grained hard alloy and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an iron-nickel-based ultrafine-grained hard alloy which comprises the following preparation raw materials in parts by weight:
75-90 parts of WC powder;
0.3-1 part of VC powder;
3-15 parts of Fe powder;
3-20 parts of Ni powder;
0.5-2 parts of Al powder;
0.3-1.5 parts of Mo powder.
Preferably, the purity of the WC powder is more than or equal to 99.9%, and the granularity is 0.1-0.5 μm;
the purity of the VC powder, the purity of the Fe powder, the purity of the Ni powder, the purity of the Al powder and the purity of the Mo powder are respectively more than or equal to 99.5%, and the particle size of the VC powder, the purity of the Fe powder, the purity of the Ni powder, the purity of the Al powder and the purity of the Mo powder are respectively 1-.
The invention provides a preparation method of the iron-nickel-based ultrafine grained hard alloy in the technical scheme, which comprises the following steps:
mixing the preparation raw materials of the iron-nickel-based ultrafine grained hard alloy, and then sequentially carrying out ball milling, press forming, sintering and aging treatment to obtain the iron-nickel-based ultrafine grained hard alloy.
Preferably, the ball milling is carried out in the presence of a forming agent, the forming agent comprises paraffin or polyethylene glycol, and the mass ratio of the forming agent to the raw materials for preparing the iron-nickel-based ultrafine grained cemented carbide is (1.8-2.2): 100, respectively;
the ball milling medium adopted by the ball milling comprises ethanol or isopropanol, and the liquid-solid ratio of the ball milling is 50-100 mL/kg.
Preferably, the ball milling is performed in a protective atmosphere; the ball-material ratio of the ball mill is (4-10): 1, the ball milling time is 48-72 h.
Preferably, drying is further performed after the ball milling, and the drying mode comprises spray drying or vacuum drying; the drying temperature is 60-300 ℃.
Preferably, the compression molding manner comprises cold isostatic pressing, unidirectional pressing or bidirectional pressing; the pressure intensity of the pressing forming is 150-350 MPa.
Preferably, the sintering is carried out in a protective atmosphere, the sintering pressure is 5-10 MPa, the sintering temperature is 1300-1500 ℃, and the heat preservation time is 30-90 min.
Preferably, the sintering process further comprises degreasing treatment, wherein the degreasing treatment is carried out in a hydrogen atmosphere, the degreasing treatment temperature is 30-450 ℃, and the heat preservation time is 4-10 hours.
Preferably, the temperature of the aging treatment is 900-1300 ℃, and the heat preservation time is 1-3 h.
The invention provides an iron-nickel-based ultrafine-grained hard alloy which comprises the following preparation raw materials in parts by weight: 75-90 parts of WC powder; 0.3-1 part of VC powder; 3-15 parts of Fe powder; 3-20 parts of Ni powder; 0.5-2 parts of Al powder; 0.3-1.5 parts of Mo powder. According to the invention, Al and Mo are added into the iron-nickel matrix for microalloying, so that the iron-nickel matrix has the effect of strengthening the iron-nickel binding phase by solid solution, and the strength of the iron-nickel matrix hard alloy can be improved; meanwhile, the dissolution and precipitation of WC in the iron-nickel matrix can be inhibited, so that the growth of WC crystal grains is inhibited; in addition, after the iron-nickel matrix is microalloyed by using Al and Mo, FeAl, NiAl and Ni can be used as a binding phase of the hard alloy during sintering and aging treatment3Al、Fe3Al has a long rangeThe order phase is desolventized and separated out in the iron-nickel matrix to form a nano-scale strengthening phase which is dispersed and coherent with the iron-nickel matrix, thereby improving the obdurability of the iron-nickel-based hard alloy, solving the problem of lower iron-nickel bonding phase strength in the traditional iron-nickel-based hard alloy, and simultaneously avoiding directly adding FeAl, NiAl and Ni3Al、Fe3The problem of coarse and uneven distribution of strengthening phase particles caused by strengthening the iron-nickel matrix by the strengthening phase particles such as Al. The results of the examples show that the grain size of WC in the iron-nickel-based ultrafine grain hard alloy provided by the invention is 0.30-0.40 μm, the hardness is 90.5-92 HRA, and the bending strength is 4051-4260 MPa.
Drawings
FIG. 1 is a scanning electron microscope image of the microstructure of the Fe-Ni based ultrafine grained cemented carbide prepared in example 1 at a low magnification (magnification of 1500 times);
fig. 2 is a high-magnification (3 ten thousand-fold magnification) scanning electron microscope image of the microstructure of the iron-nickel-based ultrafine grained cemented carbide prepared in example 1.
Detailed Description
The invention provides an iron-nickel-based ultrafine-grained hard alloy which comprises the following preparation raw materials in parts by weight:
75-90 parts of WC powder;
0.3-1 part of VC powder;
3-15 parts of Fe powder;
3-20 parts of Ni powder;
0.5-2 parts of Al powder;
0.3-1.5 parts of Mo powder.
According to the invention, Al and Mo are added into the iron-nickel matrix for microalloying, so that the iron-nickel matrix has the effect of strengthening the iron-nickel binding phase by solid solution, and the strength of the iron-nickel matrix hard alloy can be improved; meanwhile, the dissolution and precipitation of WC in the iron-nickel matrix can be inhibited, so that the growth of WC crystal grains is inhibited; in addition, after the Fe-Ni matrix is microalloyed by Al and Mo, the Fe-Ni matrix is used as a binding phase of the hard alloy, and when sintering and aging treatment are carried out, long-range ordered B2 phase Al (Al, Fe) can be desolventized and separated out in the Fe-Ni binding phase matrix, and the separated phase is coherent with the Fe-Ni binding phase matrix, so that the second-phase particle dispersion strengthening effect is obtained, meanwhile, the toughness of the Fe-Ni-based hard alloy is improved, and the problem of the traditional Fe-Ni-based hard alloy is solvedThe problem of low strength of iron-nickel binding phase in the nickel-based hard alloy is solved, and simultaneously, the direct addition of FeAl, NiAl and Ni is avoided3Al、Fe3The problem of coarse and uneven distribution of strengthening phase particles caused by strengthening the iron-nickel matrix by the strengthening phase particles such as Al.
According to the mass portion, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 75-90 parts of WC powder, preferably 82-90 parts, and further preferably 85-88 parts. In the invention, the purity of the WC powder is preferably equal to or more than 99.9%, and the granularity is preferably 0.1-0.5 μm.
Based on the mass parts of the WC powder, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 0.3-1 part of VC powder, preferably 0.3-0.8 part, and further preferably 0.3-0.6 part. In the invention, the purity of the VC powder is preferably more than or equal to 99.5%, and the granularity is preferably 1-3 μm.
Based on the mass parts of the WC powder, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 3-15 parts of Fe powder, preferably 4-10 parts of Fe powder, and further preferably 4-6.5 parts of Fe powder. In the invention, the purity of the Fe powder is preferably more than or equal to 99.5%, and the granularity is preferably 1-3 μm.
Based on the mass parts of the WC powder, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 3-20 parts of Ni powder, preferably 6-15 parts of Ni powder, and further preferably 6-12 parts of Ni powder. In the invention, the purity of the Ni powder is preferably equal to or more than 99.5%, and the granularity is preferably 1-3 μm.
Based on the mass parts of the WC powder, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 0.5-2 parts of Al powder, and preferably 0.5-1 part of Al powder. In the invention, the purity of the Al powder is preferably more than or equal to 99.5%, and the granularity is preferably 1-3 μm.
Based on the mass parts of the WC powder, the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy comprise 0.3-1.5 parts of Mo powder, preferably 0.5-1 part. In the invention, the purity of the Mo powder is preferably more than or equal to 99.5%, and the granularity is preferably 1-3 μm.
The invention provides a preparation method of the iron-nickel-based ultrafine grained hard alloy in the technical scheme, which comprises the following steps:
mixing the preparation raw materials of the iron-nickel-based ultrafine grained hard alloy, and then sequentially carrying out ball milling, press forming, sintering and aging treatment to obtain the iron-nickel-based ultrafine grained hard alloy.
The invention mixes the preparation raw materials of the iron-nickel-based ultrafine grain hard alloy and then carries out ball milling. In the invention, the ball milling is preferably carried out in the presence of a forming agent, the forming agent preferably comprises paraffin or polyethylene glycol, and the mass ratio of the forming agent to the raw materials for preparing the iron-nickel-based ultrafine grained cemented carbide is preferably (1.8-2.2): 100, respectively; more preferably 2: 100. the forming agent is utilized to improve the compression forming performance of the material, and the generation of defects such as cracks, layering and the like in the subsequent compression forming process is reduced.
In the invention, the ball milling medium adopted by the ball milling preferably comprises ethanol or isopropanol, and the liquid-solid ratio of the ball milling is preferably 50-100 mL/kg, more preferably 70-100 mL/kg. In the present invention, the ball milling is preferably carried out in a protective atmosphere; the protective gas for providing the protective atmosphere in the present invention is not particularly limited, and specifically, argon gas is used. In the invention, the ball-to-material ratio of the ball mill is preferably (4-10): 1, more preferably (6-8): 1; the ball milling time is preferably 48 to 72 hours, and more preferably 60 to 72 hours. The invention preferably performs ball milling under the conditions, can fully mix all materials, and simultaneously avoids material oxidation.
According to the invention, the ball-milling slurry obtained after ball milling is preferably dried to obtain the mixed powder. In the present invention, the drying means preferably includes spray drying or vacuum drying, more preferably spray drying; the drying temperature is preferably 60-300 ℃, more preferably 150-300 ℃, and further preferably 200-280 ℃. According to the invention, the drying mode is preferably adopted, so that the mixed powder with good fluidity can be obtained, the press forming performance of the material is favorably improved, and the subsequent press forming is ensured to be carried out smoothly.
The invention carries out compression molding on the mixed powder to obtain a powder compact. In the present invention, the compression molding preferably includes cold isostatic pressing, unidirectional pressing, or bidirectional pressing; the pressure intensity of the compression molding is preferably 150-350 MPa, more preferably 200-300 MPa, and further preferably 250-300 MPa. The mixed powder is preferably placed in a die for compression molding, and after the compression molding is finished, the die is removed to obtain the powder pressed compact. The invention preferably carries out compression molding under the conditions, can reduce the generation of defects such as cracks, delamination and the like in the compression molding process, and ensures that the obtained powder compact has higher strength and higher density.
And after obtaining a powder compact, sintering the powder compact to obtain a hard alloy sintered body. In the present invention, the sintering process preferably further comprises a degreasing process, wherein the degreasing process is preferably performed in a hydrogen atmosphere; the degreasing temperature is preferably 30-450 ℃, more preferably 60-350 ℃, and further preferably 250-350 ℃; the heat preservation time is preferably 4-10 h, more preferably 5-9 h, and further preferably 6-8 h. In the present invention, the sintering is preferably carried out in a protective atmosphere; the protective gas for providing the protective atmosphere in the invention is not particularly limited, such as argon; the sintering pressure is preferably 5-10 MPa, more preferably 6-9 MPa, and further preferably 7-9 MPa, and is specifically provided by protective gas; the sintering temperature is preferably 1300-1500 ℃, more preferably 1350-1450 ℃, further preferably 1390-1430 ℃, and further preferably 1410-1430 ℃; the heat preservation time is preferably 30-90 min, more preferably 50-80 min, and further preferably 60-70 min. In the present invention, the degreasing treatment and sintering are preferably performed in a degreasing-sintering integrated furnace. The present invention can obtain a cemented carbide sintered body having high density and a uniform and fine structure by preferably sintering under the above conditions.
After the hard alloy sintered body is obtained, the hard alloy sintered body is subjected to aging treatment to obtain the iron-nickel-based ultrafine grained hard alloy. In the invention, the temperature of the aging treatment is preferably 900-1300 ℃, more preferably 1000-1200 ℃, and further preferably 1100-1200 ℃; the heat preservation time is preferably 1-3 h, and more preferably 1-2 h. In the present invention, the aging treatment is preferably performed in a vacuum heat treatment furnace. The invention preferably carries out aging treatment under the conditions, and can disperse and precipitate the nano-scale strengthening phase in the iron-nickel binding phase matrix of the hard alloy, thereby improving the obdurability of the hard alloy.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) The raw materials comprise the following components in parts by weight: 85 parts of WC powder, 0.5 part of VC powder, 4.5 parts of Fe powder, 9 parts of Ni powder, 0.5 part of Al powder and 0.5 part of Mo powder, wherein the purity of the WC powder is more than or equal to 99.9 percent, and the granularity of the WC powder is 0.1-0.5 mu m; the purity of VC powder, Fe powder, Ni powder, Al powder and Mo powder is more than or equal to 99.5%, and the granularity is 1-3 mu m;
(2) adding the prepared preparation raw materials into a ball milling barrel, adding paraffin (the addition amount is 2 percent of the total mass of the preparation raw materials) as a forming agent, adding a phi 6.0 hard alloy ball, wherein the ball-to-material ratio is 6: 1, adding ball milling medium alcohol into a ball milling barrel according to a liquid-solid ratio of 50mL/kg, and carrying out ball milling for 48 hours under the protection of argon to obtain ball milling slurry;
(3) spray drying the ball-milling slurry at 220 ℃ to obtain mixed powder;
(4) putting the mixed powder into a die, performing compression molding in a cold isostatic pressing mode under the condition that the pressure is 150MPa, and demolding to obtain a powder compact;
(5) placing the powder pressed compact into a degreasing-sintering integrated furnace, carrying out degreasing treatment for 5h under the conditions of hydrogen atmosphere and 60 ℃, and then sintering for 70min under the conditions of argon atmosphere, argon pressure of 6MPa and 1410 ℃; cooling along with the furnace after sintering is finished to obtain a hard alloy sintered body;
(6) and placing the hard alloy sintered body in a vacuum heat treatment furnace, carrying out aging treatment for 2h at 1000 ℃, and cooling along with the furnace after the aging treatment is finished to obtain the iron-nickel-based ultrafine grained hard alloy.
Fig. 1 is a scanning electron microscope image of microstructure low-power (1500 times magnification) of the iron-nickel-based ultrafine grained cemented carbide prepared in this example, and fig. 2 is a scanning electron microscope image of microstructure high-power (3 ten thousand times magnification) of the iron-nickel-based ultrafine grained cemented carbide prepared in this example, and it can be seen from fig. 1 and fig. 2 that the iron-nickel-based ultrafine grained cemented carbide prepared in this example has uniform and fine structure, iron-nickel binder phase is uniformly distributed around WC, WC grains are uniform and fine, and no abnormal growth occurs. The grain size of WC in the iron-nickel-based ultrafine grain hard alloy prepared in the embodiment is 0.35 μm, the hardness is 91.5HRA, and the bending strength is 4200MPa (the bending strength test adopts the national standard GB 3851-.
Example 2
(1) The raw materials comprise the following components in parts by weight: 82 parts of WC powder, 0.7 part of VC powder, 6.5 parts of Fe powder, 9 parts of Ni powder, 1.3 parts of Al powder and 0.5 part of Mo powder, wherein the purity of the WC powder is more than or equal to 99.9 percent, and the granularity of the WC powder is 0.1-0.5 mu m; the purity of VC powder, Fe powder, Ni powder, Al powder and Mo powder is more than or equal to 99.5%, and the granularity is 1-3 mu m;
(2) adding the prepared preparation raw materials into a ball milling barrel, adding polyethylene glycol (the addition amount is 2% of the total mass of the preparation raw materials) as a forming agent, adding phi 6.0 hard alloy balls, wherein the ball-to-material ratio is 7: adding ball-milling medium isopropanol into a ball-milling barrel according to a liquid-solid ratio of 80mL/kg, and carrying out ball milling for 60 hours under the protection of argon to obtain ball-milling slurry;
(3) spray drying the ball-milling slurry at the drying temperature of 230 ℃ to obtain mixed powder;
(4) filling the mixed powder into a die, performing compression molding in a one-way compression mode under the condition that the pressure is 250MPa, and demolding to obtain a powder compact;
(5) placing the powder compact in a degreasing-sintering integrated furnace, degreasing for 8h under the conditions of hydrogen atmosphere and 200 ℃, and then sintering for 70min under the conditions of argon atmosphere, argon pressure of 7MPa and 1390 ℃; cooling along with the furnace after sintering is finished to obtain a hard alloy sintered body;
(6) and placing the hard alloy sintered body in a vacuum heat treatment furnace, carrying out aging treatment for 3h at 1100 ℃, and cooling along with the furnace after the aging treatment is finished to obtain the iron-nickel-based ultrafine grained hard alloy.
The scanning electron microscope image of the microstructure of the iron-nickel-based ultrafine grained cemented carbide prepared in this example is substantially the same as that in fig. 1 and 2. The grain size of WC in the iron-nickel-based ultrafine grain hard alloy prepared in the embodiment is 0.40 μm, the hardness is 90.5HRA, and the bending strength is 4051MPa (the bending strength test adopts the national standard GB 3851-.
Example 3
(1) The raw materials comprise the following components in parts by weight: 88 parts of WC powder, 0.4 part of VC powder, 4 parts of Fe powder, 6 parts of Ni powder, 0.6 part of Al powder and 1 part of Mo powder, wherein the purity of the WC powder is more than or equal to 99.9 percent, and the granularity of the WC powder is 0.1-0.5 mu m; the purity of VC powder, Fe powder, Ni powder, Al powder and Mo powder is more than or equal to 99.5%, and the granularity is 1-3 mu m;
(2) adding the prepared preparation raw materials into a ball milling barrel, adding paraffin (the addition amount is 2 percent of the total mass of the preparation raw materials) as a forming agent, adding a phi 6.0 hard alloy ball, wherein the ball-to-material ratio is 8: 1, adding ball milling medium alcohol into a ball milling barrel according to a liquid-solid ratio of 100mL/kg, and carrying out ball milling for 72 hours under the protection of argon to obtain ball milling slurry;
(3) spray drying the ball-milling slurry at the drying temperature of 225 ℃ to obtain mixed powder;
(4) filling the mixed powder into a die, performing compression molding in a two-way compression mode under the condition that the pressure is 300MPa, and demolding to obtain a powder compact;
(5) placing the powder pressed compact in a degreasing-sintering integrated furnace, carrying out degreasing treatment for 6h under the conditions of hydrogen atmosphere and 350 ℃, and then sintering for 70min under the conditions of argon atmosphere, argon pressure of 9MPa and 1430 ℃; cooling along with the furnace after sintering is finished to obtain a hard alloy sintered body;
(6) and placing the hard alloy sintered body in a vacuum heat treatment furnace, carrying out aging treatment for 1h at 1200 ℃, and cooling along with the furnace after the aging treatment is finished to obtain the iron-nickel-based ultrafine grained hard alloy.
The scanning electron microscope images of the iron-nickel-based ultrafine grained cemented carbide prepared in this example are substantially the same as those in fig. 1 and 2. The grain size of WC in the iron-nickel-based ultrafine grain hard alloy prepared in the embodiment is 0.30 μm, the hardness is 92.0HRA, and the bending strength is 4260MPa (the bending strength test adopts the national standard GB 3851-1983, B sample standard).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The iron-nickel-based ultrafine-grained hard alloy is characterized by being prepared from the following preparation raw materials in parts by weight:
82-90 parts of WC powder;
0.3-1 part of VC powder;
4-15 parts of Fe powder;
6-20 parts of Ni powder;
0.5-2 parts of Al powder;
0.3-1.5 parts of Mo powder;
the preparation method of the iron-nickel-based ultrafine grained hard alloy comprises the following steps:
mixing the preparation raw materials of the iron-nickel-based ultrafine grained hard alloy, and then sequentially carrying out ball milling, press forming, sintering and aging treatment to obtain the iron-nickel-based ultrafine grained hard alloy.
2. The iron-nickel-based ultrafine grained cemented carbide according to claim 1, wherein the purity of the WC powder is not less than 99.9%, and the grain size is 0.1 to 0.5 μm;
the purity of the VC powder, the purity of the Fe powder, the purity of the Ni powder, the purity of the Al powder and the purity of the Mo powder are respectively more than or equal to 99.5%, and the particle size of the VC powder, the purity of the Fe powder, the purity of the Ni powder, the purity of the Al powder and the purity of the Mo powder are respectively 1-.
3. The method for preparing the Fe-Ni based ultrafine grained cemented carbide according to claim 1 or 2, comprising the steps of:
mixing the preparation raw materials of the iron-nickel-based ultrafine grained hard alloy, and then sequentially carrying out ball milling, press forming, sintering and aging treatment to obtain the iron-nickel-based ultrafine grained hard alloy.
4. The preparation method according to claim 3, wherein the ball milling is carried out in the presence of a forming agent, the forming agent comprises paraffin or polyethylene glycol, and the mass ratio of the forming agent to the raw materials for preparing the iron-nickel-based ultrafine grained hard alloy is (1.8-2.2): 100, respectively;
the ball milling medium adopted by the ball milling comprises ethanol or isopropanol, and the liquid-solid ratio of the ball milling is 50-100 mL/kg.
5. The method of claim 4, wherein the ball milling is performed in a protective atmosphere; the ball-material ratio of the ball mill is (4-10): 1, the ball milling time is 48-72 h.
6. The preparation method according to claim 4 or 5, characterized in that the ball milling is followed by drying, wherein the drying comprises spray drying or vacuum drying; the drying temperature is 60-300 ℃.
7. The method according to claim 3, wherein the compression molding means includes cold isostatic pressing, unidirectional pressing, or bidirectional pressing; the pressure intensity of the pressing forming is 150-350 MPa.
8. The preparation method according to claim 3, wherein the sintering is carried out in a protective atmosphere, the sintering pressure is 5-10 MPa, the temperature is 1300-1500 ℃, and the holding time is 30-90 min.
9. The preparation method according to claim 3 or 8, characterized by further comprising degreasing treatment before sintering, wherein the degreasing treatment is carried out in a hydrogen atmosphere, the degreasing treatment is carried out at 30-450 ℃ and the heat preservation time is 4-10 h.
10. The preparation method according to claim 3, wherein the temperature of the aging treatment is 900-1300 ℃, and the holding time is 1-3 h.
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