CN109371304B - Molybdenum-based composite material reinforced by in-situ generated molybdenum carbide and preparation method thereof - Google Patents
Molybdenum-based composite material reinforced by in-situ generated molybdenum carbide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an in-situ generated molybdenum carbide reinforced molybdenum-based composite material, which comprises 5-15% of molybdenum carbide, no more than 0.1% of impurities and the balance of molybdenum according to mass fraction, wherein the sum of the mass fractions of the components is 100%. The invention also discloses a preparation method of the molybdenum-based composite material reinforced by in-situ generated molybdenum carbide, which comprises the steps of carrying out ball milling mixing on molybdenum powder and graphene powder to obtain mixed powder, and carrying out high-energy ball milling treatment on the mixed powder; and (3) performing hot-pressing sintering on the mixed powder subjected to the ball milling treatment, and removing the surface layer. The molybdenum carbide reinforced molybdenum-based composite material generated in situ has uniform and compact structure, fine crystal grains and higher hardness and strength; the preparation method of the molybdenum-based composite material reinforced by in-situ generated molybdenum carbide has the advantages of low equipment requirement, simple and feasible preparation process, low cost and easy realization of industrial production.
Description
Technical Field
The invention belongs to the technical field of powder metallurgy, relates to an in-situ generated molybdenum carbide reinforced molybdenum-based composite material, and further relates to a preparation method of the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
Background
Molybdenum is a precious rare refractory metal material, and has the properties of high melting point, elastic modulus and wear resistance, good electric and heat conduction performance, low thermal expansion coefficient, good acid and alkali resistance, liquid metal corrosion resistance and the like, so that molybdenum has wide application prospects in various departments such as aerospace, power electronics, mechanical manufacturing, ferrous metallurgy, energy and chemical engineering, medical instruments, military industry and the like, and is one of indispensable high-temperature-resistant materials. With the rapid development of science and technology, molybdenum metal materials have difficulty meeting higher performance requirements due to insufficient strength. Therefore, how to prepare a high-strength novel molybdenum-based material becomes a necessary development trend, and the general means is mainly divided into two aspects of component design and process optimization.
At present, the research field of molybdenum alloy mainly comprises solid solution strengthening molybdenum alloy, ASK doped molybdenum alloy, carbide doped molybdenum alloy and oxide doped molybdenum alloyMolybdenum alloys, multi-component molybdenum alloys, and the like. They show excellent performance in different application fields, but have a plurality of problems, such as insignificant strengthening and toughening effect, high cost, complex process and the like. Therefore, research and development of new molybdenum-based materials are necessary and urgent. Mo2C has been used in the field of cermet as a reinforcing material due to its high melting point and hardness, good thermal and mechanical stability, excellent corrosion resistance, but Mo has not been researched and developed yet2The public report of C reinforced molybdenum matrix composite material.
Disclosure of Invention
The invention aims to provide an in-situ generated molybdenum carbide reinforced molybdenum-based composite material which is uniform and compact in structure and high in hardness and strength.
The first technical scheme adopted by the invention is that the molybdenum-carbide-reinforced molybdenum-based composite material generated in situ comprises, by mass, 5% -15% of molybdenum carbide, no more than 0.1% of impurities and the balance of molybdenum, wherein the sum of the mass fractions of the components is 100%.
The first technical scheme of the invention is also characterized in that:
the molybdenum carbide is uniformly distributed in the molybdenum matrix, the size of the molybdenum carbide crystal grain is 1-3 μm, and the size of the molybdenum crystal grain is 2-5 μm.
The other technical scheme adopted by the invention is as follows:
a preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, performing ball milling and mixing on molybdenum powder and graphene powder to obtain mixed powder;
step 2, carrying out high-energy ball milling treatment on the mixed powder;
and 3, carrying out hot-pressing sintering on the mixed powder subjected to ball milling treatment, and removing the surface layer to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
The other technical scheme of the invention is also characterized in that:
the mass fraction of the graphene powder in the mixed powder obtained in the step 1 is 0.3-0.9%.
In the step 1, when the molybdenum powder and the graphene powder are subjected to ball milling and mixing, introducing Ar gas atmosphere with the pressure of 0.3-0.6 MPa; the ball milling and mixing time is 6-12 h.
In the step 1, ball milling and mixing are carried out in a planetary ball mill, the ball milling tank and the milling balls are made of agate materials, the ball-material ratio is 1: 1-3: 1, and the rotating speed is 300-450 r/min.
When the high-energy ball milling treatment is carried out in the step 2, introducing Ar gas atmosphere with the pressure of 0.3-0.6 MPa; the time of the high-energy ball milling treatment is 15-30 h.
Performing high-energy ball milling in a planetary high-energy ball mill in the step 2, wherein the high-energy ball milling is performed for 50-60 min, then stopping for 5-15 min, and repeating the high-energy ball milling and stopping for 10-30 times; when the high-energy ball mill is used for high-energy ball milling, the ball milling tank and the milling balls are made of tungsten carbide, the ball-material ratio is 12:1 to 8:1, and the rotating speed of the planetary high-energy ball mill is 200-.
In step 3, the mixed powder after the high-energy ball milling treatment is firstly screened by a Taylor sieve of 200 meshes to 300 meshes and then is put into a graphite mold, and then the graphite mold is put into a graphite mold with the vacuum degree of 7 multiplied by 10-3Pa×10-2And (2) in a Pa vacuum hot-pressing sintering furnace, gradually heating to 1600-1700 ℃, axially pressurizing to 40-50 MPa, carrying out hot-pressing sintering for 2-3 h, unloading after heat preservation and pressure maintaining, cooling to room temperature along with the furnace to obtain a sintered body, and removing the surface layer of the sintered body by 0.3-0.5mm to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
The temperature is raised by a two-step method, the temperature is raised to 1100-1200 ℃ at the speed of 10-20 ℃/min, the temperature is kept for 0.5-1.5 h, and then the temperature is raised to 1600-1700 ℃ at the speed of 10-20 ℃/min.
The invention has the advantages that
(1) The molybdenum-carbide-reinforced molybdenum-based composite material generated in situ has uniform and compact structure and fine crystal grains;
(2) the molybdenum-based composite material strengthened by in-situ generated molybdenum carbide has higher hardness and strength.
(3) The preparation method for in-situ generation of the molybdenum carbide reinforced molybdenum-based composite material has the advantages of low equipment requirement, simple and feasible preparation process, low cost and easy realization of industrial production.
Drawings
FIG. 1 is a scanning electron microscope photomicrograph of a microstructure of an in situ formed molybdenum carbide reinforced molybdenum-based composite of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
An in-situ generated molybdenum carbide reinforced molybdenum-based composite material comprises, by mass, 5% -15% of molybdenum carbide, no more than 0.1% of impurities, and the balance of molybdenum, wherein the sum of the mass fractions of the components is 100%; wherein the molybdenum carbide is uniformly distributed in the molybdenum matrix, the size of the molybdenum carbide crystal grain is 1-3 μm, and the size of the molybdenum crystal grain is 2-5 μm.
As shown in figure 1, the molybdenum carbide reinforced molybdenum-based composite material generated in situ has uniform and compact structure and fine crystal grains.
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.3MP-0.6MPa, and performing ball milling and mixing for 6h-12h to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.3% -0.9%; when ball milling and mixing are carried out, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 1: 1-3: 1, 4-8 grinding balls with the diameter of 20mm, 20-30 grinding balls with the diameter of 10mm and 30-50 grinding balls with the diameter of 6mm are used as the grinding balls, and the rotating speed of the ball mill is 300-450 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.3-0.6MPa, and performing high-energy ball milling treatment for 15-30 h; when the high-energy ball milling is carried out, the high-energy ball milling is carried out for 50min to 60min, then the machine is stopped for 5min to 15min, and the high-energy ball milling is repeated for 10 to 30 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 12:1 to 8:1, the used grinding balls are 3-6 grinding balls with the diameter of 20mm, 30-50 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 200-300 r/min.
Step 3, screening the mixed powder subjected to the high-energy ball milling treatment by a Taylor sieve of 200 meshes to 300 meshes, then placing the mixed powder into a graphite mold with the inner diameter of 30mm to 60mm, and then placing the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 7 multiplied by 10-3Pa×10-2In a Pa vacuum hot-pressing sintering furnace, heating to 1100-1200 ℃ at the speed of 10-20 ℃/min, preserving heat for 0.5-1.5 h, then heating to 1600-1700 ℃ at the speed of 10-20 ℃/min, axially applying the pressure of 40-50 MPa for hot-pressing sintering for 2-3 h, preserving heat and pressure, unloading, cooling to room temperature along with the furnace, taking out a mold, processing the sintered body obtained after demolding, and removing the surface layer by 0.3-0.5mm to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
In the preparation method of the molybdenum-based composite material reinforced by in-situ generated molybdenum carbide, provided by the invention, graphene powder is added into molybdenum, and 2Mo + C-Mo occurs in the sintering process2C reaction, Mo2The C is uniformly distributed in the molybdenum matrix as a reinforcing phase, not only plays a role in refining molybdenum grains in the sintering process of the composite material, but also obviously improves the hardness and the strength of the composite material. Compared with a pure molybdenum material, the strength of the material at room temperature is improved by more than 70%, and the hardness is improved by more than 50%.
The high-energy ball milling treatment is carried out, so that powder particles can be effectively refined, and the graphene powder and the molybdenum powder are further uniformly mixed to form mixed powder in which the graphene powder is uniformly distributed in the molybdenum powder, thereby being beneficial to reducing the grain size of the sintered composite material, remarkably improving the surface energy of the mixed powder and promoting the subsequent in-situ reaction; the preparation method comprises the steps of carrying out hot-pressing sintering on the mixed powder subjected to high-energy ball milling in a vacuum environment, wherein in the sintering process, Mo generated by the reaction of graphene and molybdenum2C is uniformly distributed in the molybdenum matrix and well combined with molybdenum crystal grains, and simultaneously, the hot-pressing sintering method which is a reinforced sintering method can be adopted to quickly finish densificationTo remove and avoid Mo2Coarsening of C and molybdenum grains.
Example 1
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.3MPa, and carrying out ball milling and mixing for 6 hours to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.3%; when ball milling and mixing are carried out, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 1:1, 4 grinding balls with the diameter of 20mm, 20 grinding balls with the diameter of 10mm and 30 grinding balls with the diameter of 6mm are used as the grinding balls, and the rotating speed of the ball mill is 300 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.3MPa, and performing high-energy ball milling treatment for 15 hours; when high-energy ball milling is carried out, high-energy ball milling is carried out for 50min, then the machine is stopped for 5min, and the high-energy ball milling is repeated and stopped for 10 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 8:1, the used grinding balls are 3 grinding balls with the diameter of 20mm and 30 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 200 r/min.
Step 3, screening the mixed powder subjected to the high-energy ball milling treatment by a 200-mesh Taylor sieve, then placing the mixed powder into a graphite mold with the inner diameter of 30mm, and then placing the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 7 multiplied by 10-3And (2) in a Pa vacuum hot-pressing sintering furnace, heating to 1100 ℃ at the speed of 10 ℃/min, preserving heat for 0.5h, then heating to 1600 ℃ at the speed of 10 ℃/min, axially pressing at 40MPa for hot-pressing sintering for 2h, preserving heat and pressure, unloading, cooling to room temperature along with the furnace, taking out a mold, processing the sintered body obtained after demolding, and removing the surface layer by 0.3mm to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
Example 2
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.6MPa, and carrying out ball milling and mixing for 12 hours to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.9%; during ball milling and mixing, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 3: 1, 8 grinding balls with the diameter of 20mm, 30 grinding balls with the diameter of 10mm and 50 grinding balls with the diameter of 6mm are used as the grinding balls, and the rotating speed of the ball mill is 450 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.6MPa, and performing high-energy ball milling treatment for 30 hours; when high-energy ball milling is carried out, high-energy ball milling is carried out for 60min, then the machine is stopped for 15min, and the high-energy ball milling is repeated and stopped for 30 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 8:1, the used grinding balls are 6 grinding balls with the diameter of 20mm and 50 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 300 r/min.
Step 3, screening the mixed powder after the high-energy ball milling treatment by a 300-mesh Taylor sieve, then putting the mixed powder into a graphite mold with the inner diameter of 60mm, and then putting the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 1 multiplied by 10-2And (2) in a Pa vacuum hot-pressing sintering furnace, heating to 1200 ℃ at the speed of 20 ℃/min, preserving heat for 1.5h, then heating to 1700 ℃ at the speed of 20 ℃/min, axially pressing at 50MPa for hot-pressing sintering for 3h, preserving heat and pressure, unloading, cooling to room temperature along with the furnace, taking out a mold, processing the sintered body obtained after demolding, and removing the surface layer by 0.5mm to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
Example 3
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.5MPa, and carrying out ball milling and mixing for 9 hours to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.6%; during ball milling and mixing, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 2.1, the used grinding balls comprise 6 grinding balls with the diameter of 20mm, 25 grinding balls with the diameter of 10mm and 40 grinding balls with the diameter of 6mm, and the rotating speed of the ball mill is 350 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.5MPa, and performing high-energy ball milling treatment for 22 h; when the high-energy ball milling is carried out, the high-energy ball milling is carried out for 55min, then the machine is stopped for 10min, and the high-energy ball milling is repeated and the machine is stopped for 20 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 10:1, the used grinding balls are 4 grinding balls with the diameter of 20mm and 40 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 250 r/min.
Step 3, screening the mixed powder subjected to the high-energy ball milling treatment by a 250-mesh Taylor sieve, then placing the mixed powder into a graphite mold with the inner diameter of 45mm, and then placing the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 9 multiplied by 10-3And (2) in a Pa vacuum hot-pressing sintering furnace, heating to 1150 ℃ at the speed of 15 ℃/min, preserving heat for 1.0h, then heating to 1650 ℃ at the speed of 15 ℃/min, axially pressing at 45MPa for hot-pressing sintering for 2.5h, preserving heat and pressure, unloading, cooling to room temperature along with the furnace, taking out a mold, processing the demolded sintered body to remove 0.4mm of the surface layer, and thus obtaining the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
Example 4
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.4MPa, and carrying out ball milling and mixing for 7 hours to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.5%; during ball milling and mixing, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 1:1, the used grinding balls comprise 5 grinding balls with the diameter of 20mm, 22 grinding balls with the diameter of 10mm and 35 grinding balls with the diameter of 6mm, and the rotating speed of the ball mill is 350 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.4MPa, and performing high-energy ball milling treatment for 20 hours; when the high-energy ball milling is carried out, the high-energy ball milling is carried out for 52min, then the machine is stopped for 8min, and the high-energy ball milling is repeated and stopped for 15 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 9:1, the used grinding balls are 4 grinding balls with the diameter of 20mm and 35 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 220 r/min.
Step 3, screening the mixed powder subjected to the high-energy ball milling treatment by a 220-mesh Taylor sieve, then placing the mixed powder into a graphite mold with the inner diameter of 35mm, and then placing the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 7 multiplied by 10-3And (2) in a Pa vacuum hot-pressing sintering furnace, heating to 1120 ℃ at the speed of 12 ℃/min, preserving heat for 0.6h, heating to 1630 ℃ at the speed of 13 ℃/min, axially pressing at 42MPa for hot-pressing sintering for 2.2h, preserving heat and pressure, unloading, cooling to room temperature along with the furnace, taking out a mold, processing the demolded sintered body to remove 0.35mm of the surface layer, and thus obtaining the in-situ generated molybdenum carbide reinforced molybdenum-based composite material.
Example 5
A preparation method of in-situ generated molybdenum carbide reinforced molybdenum-based composite material specifically comprises the following steps:
step 1, putting molybdenum powder and graphene powder into a planetary ball mill (QM-3SP2), introducing Ar gas atmosphere with the pressure of 0.5MPa, and carrying out ball milling and mixing for 11 hours to obtain mixed powder, wherein the mass fraction of the graphene powder in the mixed powder is 0.8%; during ball milling and mixing, the ball milling tank and the grinding balls are made of agate materials, the ball material ratio is 3: 1, the used grinding balls comprise 7 grinding balls with the diameter of 20mm, 28 grinding balls with the diameter of 10mm and 45 grinding balls with the diameter of 6mm, and the rotating speed of the ball mill is 420 r/min;
step 2, putting the mixed powder into a planetary high-energy ball mill (Retsch-PM400 type), introducing Ar gas atmosphere with the pressure of 0.5MPa, and performing high-energy ball milling treatment for 25 hours; when high-energy ball milling is carried out, the high-energy ball milling is carried out for 58min, then the machine is stopped for 13min, and the high-energy ball milling is repeated and stopped for 28 times;
during high-energy ball milling, the ball milling tank and the grinding balls are made of tungsten carbide, the ball material ratio is 11:1, the used grinding balls are 5 grinding balls with the diameter of 20mm and 45 grinding balls with the diameter of 10mm, and the rotating speed of the planetary high-energy ball mill is 280 r/min.
Step 3, screening the mixed powder after the high-energy ball milling treatment by a 280-mesh Taylor sieve, then putting the mixed powder into a graphite mold with the inner diameter of 50mm, and then putting the graphite mold filled with the mixed powder into a graphite mold with the vacuum degree of 9 multiplied by 10-3In a vacuum hot-pressing sintering furnace of Paa, the temperature is raised to 1180 ℃ at the speed of 18 ℃/min, the temperature is kept for 1.2h, then the temperature is raised to 1680 ℃ at the speed of 18 ℃/min, the axial pressure is applied to 48MPa for hot-pressing sintering for 2.8h, the unloading is carried out after the temperature and pressure are kept, then the mold is taken out after the furnace is cooled to the room temperature, the surface layer of the sintered body obtained after demolding is processed and removed by 0.45mm, and the molybdenum carbide reinforced molybdenum-based composite material generated in situ is obtained.
Microstructure observation is carried out on the in-situ generated molybdenum carbide reinforced molybdenum-based composite materials obtained in the embodiments 1 and 5, hardness test is carried out by adopting an HV1000 type micro Vickers hardness measuring instrument, and room temperature compression test is carried out according to the national standard GB/T4740-1999, so that the micro Vickers hardness and room temperature compression yield strength of the in-situ generated molybdenum carbide reinforced molybdenum-based composite materials obtained in the embodiments 1 and 5 are respectively obtained, as shown in the table 1, the in-situ generated molybdenum carbide reinforced molybdenum-based composite materials obtained in the invention have higher hardness and strength.
TABLE 1 micro Vickers hardness and Room temperature compressive yield Strength Table
Claims (4)
1. The preparation method of the in-situ generated molybdenum carbide reinforced molybdenum-based composite material is characterized in that the in-situ generated molybdenum carbide reinforced molybdenum-based composite material comprises the following components in parts by mass: 5-15% of molybdenum carbide, impurities not more than 0.1% and the balance of molybdenum, wherein the sum of the mass fractions of the components is 100%; the molybdenum carbide is uniformly distributed in the molybdenum matrix, the size of molybdenum carbide crystal grains is 1-3 mu m, and the size of the molybdenum crystal grains is 2-5 mu m;
the method specifically comprises the following steps:
step 1, performing ball milling and mixing on molybdenum powder and graphene powder to obtain mixed powder;
the mass fraction of graphene powder in the mixed powder obtained in the step 1 is 0.6-0.9%;
step 2, carrying out high-energy ball milling treatment on the mixed powder;
performing high-energy ball milling in a planetary high-energy ball mill in the step 2, wherein the high-energy ball milling is performed for 50-60 min, then stopping for 5-15 min, and repeating the high-energy ball milling and stopping for 10-30 times; when high-energy ball milling is carried out, the ball milling tank and the milling balls are made of tungsten carbide, the ball-material ratio is 8:1 to 12:1, and the rotating speed of the planetary high-energy ball mill is 200-;
step 3, performing hot-pressing sintering on the mixed powder subjected to ball milling treatment, and removing the surface layer to obtain an in-situ generated molybdenum carbide reinforced molybdenum-based composite material;
in the step 3, the mixed powder after the high-energy ball milling treatment is firstly screened by a Taylor sieve of 200 meshes to 300 meshes and then is put into a graphite mold, and then the graphite mold is put into a vacuum degree of 7 multiplied by 10-3Pa-1×10-2In a Pa vacuum hot-pressing sintering furnace, gradually heating to 1600-1700 ℃, axially pressurizing to 40-50 MPa for hot-pressing sintering for 2-3 h, unloading after heat preservation and pressure maintaining, cooling to room temperature along with the furnace to obtain a sintered body, and removing the surface layer of the sintered body by 0.3-0.5mm to obtain the in-situ generated molybdenum carbide reinforced molybdenum-based composite material;
the temperature rise adopts a two-step method, the temperature rise is firstly carried out to 1100-1200 ℃ at the speed of 10-20 ℃/min, the temperature is kept for 0.5-1.5 h, and then the temperature rise is carried out to 1600-1700 ℃ at the speed of 10-20 ℃/min.
2. The method for preparing the molybdenum-carbide-reinforced molybdenum-based composite material through in-situ generation according to claim 1, wherein in the step 1, when the molybdenum powder and the graphene powder are subjected to ball milling and mixing, an Ar gas atmosphere with a pressure of 0.3MP-0.6MPa is introduced; the ball milling and mixing time is 6-12 h.
3. The method as claimed in claim 1, wherein the step 1 is carried out by ball milling in a planetary ball mill, the ball milling pot and the milling balls are made of agate, the ball-to-material ratio is 1 ׃ 1-3 ׃ 1, and the rotation speed is 300-450 r/min.
4. The method for preparing the molybdenum-carbide-reinforced molybdenum-based composite material by in-situ generation according to claim 1, wherein when the high-energy ball milling treatment is performed in the step 2, an Ar gas atmosphere with the pressure of 0.3-0.6MPa is introduced; the time of the high-energy ball milling treatment is 15-30 h.
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| JPH01156449A (en) * | 1987-12-11 | 1989-06-20 | Tokyo Tungsten Co Ltd | Molybdenum sintered compact and its production |
| CN103386487A (en) * | 2013-08-16 | 2013-11-13 | 苏州艾默特材料技术有限公司 | Preparation method for carbide-enhanced molybdenum alloy |
| CN108034875A (en) * | 2017-11-21 | 2018-05-15 | 西安理工大学 | A kind of Mo-Si-B alloys of rare earth doped oxide and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01156449A (en) * | 1987-12-11 | 1989-06-20 | Tokyo Tungsten Co Ltd | Molybdenum sintered compact and its production |
| CN103386487A (en) * | 2013-08-16 | 2013-11-13 | 苏州艾默特材料技术有限公司 | Preparation method for carbide-enhanced molybdenum alloy |
| CN108034875A (en) * | 2017-11-21 | 2018-05-15 | 西安理工大学 | A kind of Mo-Si-B alloys of rare earth doped oxide and preparation method thereof |
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