CN112355315B - Preparation method of spherical iron-based vanadium titanium carbide metal ceramic powder - Google Patents
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Abstract
The invention belongs to the technical field of alloy powder preparation, and particularly relates to a preparation method of spherical iron-based vanadium-titanium carbide metal ceramic powder. The technical scheme adopted by the invention for solving the technical problems is to provide a preparation method of spherical iron-based vanadium titanium carbide metal ceramic powder. The method comprises the following steps: a. adding TiO into the mixture 2 、V 2 O 5 Mixing with graphite uniformly, and pressing into a pressing block; b. putting the briquettes into a reactor, vacuumizing the reactor, introducing inert gas, heating, and carrying out carbothermic reduction reaction to obtain titanium vanadium carbide solid solution powder; c. mixing the titanium vanadium carbide solid solution powder and an iron ingot, placing the mixture into a smelting container, smelting the mixture to molten mixed liquid, and carrying out gas atomization to prepare powder, thus obtaining the spherical iron-based vanadium titanium carbide metal ceramic powder. The product prepared by the method has small pollution risk, can reduce the oxygen content in the product, has the oxygen content of 0.019-0.033 percent, and is suitable for large-scale production of high-quality spherical iron-based vanadium-titanium carbide powder.
Description
Technical Field
The invention belongs to the technical field of alloy powder preparation, and particularly relates to a preparation method of spherical iron-based vanadium-titanium carbide metal ceramic powder.
Background
The iron-based vanadium titanium carbide metal spherical ceramic powder has excellent properties of high strength, high hardness, high wear resistance and the like at high temperature, and can be used for injection molding of aerospace, electronics, automobiles and advanced weapons in the fields of aviation, aerospace and military industry. The components of the iron-based vanadium-titanium carbide metal ceramic powder prepared by the existing gas atomization method have large deviation from the designed components and are refractory, so that the iron-based vanadium-titanium carbide part has uneven alloy components, unstable structure and difficult forming.
At present, the production method of spherical iron-based vanadium titanium carbide powder is mainly an inert gas atomization method, and the inert gas atomization method is to use iron ingots and TiO 2 、V 2 O 5 The method comprises the steps of introducing inert gas into molten powder for atomizing and cooling, and finally solidifying the powder to form powder, wherein the three raw materials are directly mixed and smelted by the existing inert gas atomizing method, the smelting temperature is high, the controllability of the components of the final powder is poor due to the complex reaction of a Ti-V-Fe system, the deoxidation of the components is insufficient during the high-temperature reaction, the oxygen content of spherical powder is high, and the quality of a product formed by 3D printing is influenced, for example, the air holes in a printed part are increased, so that the application of the iron-based vanadium titanium carbide spherical powder in the field of additive manufacturing is greatly limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of spherical iron-based vanadium titanium carbide metal ceramic powder, so that the prepared product powder has controllable components and low oxygen content.
The technical scheme adopted by the invention for solving the technical problems is to provide a preparation method of spherical iron-based vanadium titanium carbide metal ceramic powder. The method comprises the following steps:
a. adding TiO into the mixture 2 、V 2 O 5 Mixing with graphite uniformly, and pressing into a pressing block;
b. putting the briquettes into a reactor, vacuumizing the reactor, introducing inert gas, heating, and carrying out carbothermic reduction reaction to obtain titanium vanadium carbide solid solution powder;
c. mixing the titanium vanadium carbide solid solution powder and an iron ingot, placing the mixture into a smelting container, smelting the mixture to molten mixed liquid, and carrying out gas atomization to prepare powder, thus obtaining the spherical iron-based vanadium titanium carbide metal ceramic powder.
Wherein, in the step a, in the preparation method of the spherical iron-based vanadium titanium carbide cermet powder, tiO is added 2 、V 2 O 5 And graphite are all in powder form.
Further, in step a，TiO 2 、V 2 O 5 Mixing with graphite in the mass ratio of 2-3:1-3:1-2.
Further, in the step a, the density of the briquette is 3.00-4.00 g/cm 3 。
Further, the briquette is a rectangular block of 25mm × 8mm × 7.5 mm.
The preparation method of the spherical iron-based vanadium titanium carbide metal ceramic powder is characterized by comprising the following steps: in the step b, the temperature of the carbothermic reduction reaction is 1300-1500 ℃; the time is 120-240 min.
Further, in step b, the inert gas is argon.
Further, in step b, the temperature raising process is performed in stages: heating from room temperature to 300-350 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 300-350 ℃ to 500-700 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 500-700 ℃ to 1000-1200 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 1000-1200 deg.c to 1300-1500 deg.c at 10-30 deg.c/min.
In the preparation method of the spherical iron-based vanadium titanium carbide metal ceramic powder, in the step c, the addition amount of the titanium vanadium carbide solid solution powder is 5-25% of the mass of the iron ingot.
Further, in the step c, the superheat degree of the molten mixed liquid is controlled to be 50 to 150 ℃.
Further, in step c, the gas atomization medium is argon; the pressure is 5-15 MPa.
The invention has the beneficial effects that:
according to the method, the titanium vanadium carbide solid solution powder generated by carbothermic reduction reaction and the iron ingot are smelted and then gas is atomized into the spherical iron-based vanadium titanium carbide powder, so that the components of a Ti-V-Fe system after reaction are greatly stabilized, the oxygen content is reduced, the prepared iron-based vanadium titanium carbide has a regular shape and good sphericity and size uniformity, and the volume fraction of the prepared spherical iron-based vanadium titanium carbide powder with the particle size of less than 200 mu m is 45-60%. The method has good controllability on the components of the product, is particularly suitable for melting vanadium titanium carbide with high melting point, and can realize controllability on the adding amount of the vanadium titanium carbide in the preparation process of the iron-based vanadium titanium carbide metal alloy, thereby controlling the hardness of the alloy. The product prepared by the method has small pollution risk, can reduce the oxygen content in the product, has the oxygen content of 0.019-0.033 percent, and is suitable for large-scale production of high-quality spherical iron-based vanadium-titanium carbide powder.
Drawings
FIG. 1 is an SEM picture of the iron-based vanadium titanium carbide powder prepared in example 1.
FIG. 2 is an SEM picture of the iron-based vanadium titanium carbide powder prepared in example 2.
FIG. 3 is an SEM picture of the iron-based vanadium titanium carbide powder prepared in example 3.
Detailed Description
Specifically, the invention provides a preparation method of spherical iron-based vanadium titanium carbide metal ceramic powder. The method comprises the following steps:
a. mixing powdered TiO 2 、V 2 O 5 Uniformly mixing the graphite and the graphite according to the mass ratio of 2-3:1-3:1-2, and pressing the mixture into a rectangular block;
b. putting the pressed rectangular block into a crucible, putting the crucible in the middle of a hearth of a tubular furnace, vacuumizing, introducing argon as protective gas, heating from room temperature to 300-350 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 300-350 ℃ to 500-700 ℃ at a speed of 10-30 ℃/min, and preserving the heat for 30-120 min; heating from 500-700 ℃ to 1000-1200 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 1000-1200 ℃ to 1300-1500 ℃ at a speed of 10-30 ℃/min, and preserving heat for 120-240 min to carry out carbothermic reduction reaction to prepare titanium vanadium carbide solid solution powder;
c. mixing titanium vanadium carbide solid solution powder with an iron ingot according to 5-25% of the mass of the iron ingot, placing the mixture and the iron ingot in a melting crucible, melting the mixture to a mixed liquid with a superheat degree of 50-150 ℃, and carrying out gas atomization powder preparation by adopting gas atomization powder preparation equipment, wherein the gas atomization medium is argon; the pressure is 5-15 MPa, and the spherical iron-based vanadium titanium carbide metal ceramic powder is obtained.
In the invention, tiO is used 2 And V 2 O 5 Is composed of the raw materials are mixed and stirred to prepare the raw material,the preparation cost is reduced. The titanium vanadium carbide solid solution powder generated by the carbothermic reduction reaction and the iron ingot are smelted and then subjected to gas atomization to form spherical iron-based vanadium titanium carbide powder, so that the components of a Ti-V-Fe system after reaction are greatly stabilized, and the prepared iron-based vanadium titanium carbide has a regular shape, good sphericity and size uniformity.
In the step c, titanium vanadium carbide solid solution powder and an iron ingot are mixed and placed in a melting crucible, the mixture is melted to be molten mixed liquid, the superheat degree of the molten mixed liquid is controlled to be 50-150 ℃, the superheat degree is overhigh, the granularity is too fine, and the oxygen content is high; if the degree of superheat is too low, satellite balls can appear. The invention controls the superheat degree of the molten mixed liquid at 50-150 ℃ to ensure that the prepared iron-based vanadium titanium carbide has moderate granularity and low oxygen content, and few powder in the product appears as satellite balls.
The spherical iron-based vanadium titanium carbide prepared by the method has good sphericity and size uniformity, and the volume fraction of the product with the particle size of less than 200 mu m is 45-60%. The oxygen content in the product can be reduced by controlling the particle size range of the product, and the oxygen content in the product is 0.019% -0.033%.
The present invention will be further illustrated by the following specific examples.
Example 1
Mixing powdered TiO 2 、V 2 O 5 And graphite are uniformly mixed according to the mass ratio of 2;
putting the pressed rectangular block into a crucible, putting the crucible in the middle of a hearth of a tubular furnace, vacuumizing, introducing argon as protective gas, heating from room temperature to 350 ℃ at a speed of 20 ℃/min, and keeping the temperature for 30min; heating from 350 deg.C to 700 deg.C at 20 deg.C/min, and maintaining for 60min; heating from 700 deg.C to 1100 deg.C at 20 deg.C/min, and maintaining for 60min; raising the temperature from 1000 ℃ to 1400 ℃ at a rate of 20 ℃/min, and preserving the temperature for 120min to carry out carbothermic reduction reaction to prepare the titanium vanadium carbide solid solution powder.
Mixing titanium vanadium carbide solid solution powder with an iron ingot according to 5% of the mass of the iron ingot, placing the mixture and the iron ingot in a melting crucible, melting the mixture until the superheat degree is 50 ℃ molten mixed liquid, and carrying out gas atomization powder preparation by adopting gas atomization powder preparation equipment, wherein the gas atomization medium is argon; the pressure is 5MPa, and the spherical iron-based vanadium titanium carbide metal ceramic powder is obtained.
The preparation method of the spherical iron-based vanadium titanium carbide cermet powder prepared in the embodiment 1 is mainly spherical and approximately spherical, and has a very small amount of satellite balls; the grain diameter is 80-200 mu m, D 50 Is 107 μm; the oxygen content of the spherical iron-based vanadium titanium carbide powder is 0.019%.
Example 2
Mixing powdered TiO 2 、V 2 O 5 And graphite are uniformly mixed according to the mass ratio of 2;
putting the pressed rectangular block into a crucible, putting the crucible in the middle of a hearth of a tubular furnace, vacuumizing, introducing argon as protective gas, heating from room temperature to 350 ℃ at a speed of 20 ℃/min, and keeping the temperature for 30min; heating from 350 deg.C to 700 deg.C at 20 deg.C/min, and maintaining for 60min; heating from 700 deg.C to 1100 deg.C at 20 deg.C/min, and maintaining for 60min; raising the temperature from 1000 ℃ to 1400 ℃ at a rate of 20 ℃/min, preserving the temperature for 120min, and carrying out carbothermic reduction reaction to prepare the titanium vanadium carbide solid solution powder.
Mixing titanium vanadium carbide solid solution powder with an iron ingot according to 10% of the mass of the iron ingot, placing the mixture and the iron ingot in a melting crucible, melting the mixture to a mixed liquid with a superheat degree of 100 ℃, and carrying out gas atomization powder preparation by adopting gas atomization powder preparation equipment, wherein the gas atomization medium is argon; the pressure is 5MPa, and the spherical iron-based vanadium titanium carbide metal ceramic powder is obtained.
The spherical iron-based vanadium titanium carbide metal ceramic powder prepared in the embodiment 2 is mostly spherical and approximately spherical, and few powder has satellite balls; the particle diameter is 50-150 mu m, D 50 85 μm; the oxygen content of the spherical iron-based vanadium titanium carbide powder was 0.033%.
Example 3
Mixing powdered TiO 2 、V 2 O 5 And graphite are uniformly mixed according to the mass ratio of 2;
putting the pressed rectangular block into a crucible, putting the crucible in the middle of a hearth of a tubular furnace, vacuumizing, introducing argon as protective gas, heating from room temperature to 350 ℃ at a speed of 20 ℃/min, and keeping the temperature for 30min; heating from 350 deg.C to 700 deg.C at 20 deg.C/min, and maintaining for 60min; heating from 700 deg.C to 1100 deg.C at 20 deg.C/min, and maintaining for 60min; raising the temperature from 1000 ℃ to 1400 ℃ at a rate of 20 ℃/min, preserving the temperature for 120min, and carrying out carbothermic reduction reaction to prepare the titanium vanadium carbide solid solution powder.
Mixing titanium vanadium carbide solid solution powder with an iron ingot according to 20% of the mass of the iron ingot, placing the mixture in a melting crucible, melting the mixture until the superheat degree is 50 ℃ molten mixed liquid, and carrying out gas atomization powder preparation by adopting gas atomization powder preparation equipment, wherein the gas atomization medium is argon; the pressure is 5MPa, and the spherical iron-based vanadium titanium carbide metal ceramic powder is obtained.
The spherical iron-based vanadium titanium carbide metal ceramic powder prepared in the embodiment 3 is mostly spherical and approximately spherical, and few satellite balls are available; the grain diameter is 70-200 mu m, and the D50 is 96 mu m; the oxygen content of the spherical iron-based vanadium titanium carbide powder was 0.023%.
Claims (3)
1. The preparation method of the spherical iron-based vanadium titanium carbide metal ceramic powder is characterized by comprising the following steps of: the method comprises the following steps:
a. adding TiO into the mixture 2 、V 2 O 5 Mixing with graphite uniformly, pressing into a press block, wherein the TiO is 2 、V 2 O 5 Mixing the graphite with the graphite according to the mass ratio of 2-3:1-3:1-2;
b. putting the pressing block into a reactor, vacuumizing the reactor, introducing inert gas, heating, and carrying out carbothermic reduction reaction at 1300-1500 ℃ for 120-240 min to obtain titanium vanadium carbide solid solution powder; the temperature rise process is carried out in a segmented mode: heating from room temperature to 300-350 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 300-350 ℃ to 500-700 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 500-700 ℃ to 1000-1200 ℃ at a speed of 10-30 ℃/min, and keeping the temperature for 30-120 min; heating from 1000-1200 ℃ to 1300-1500 ℃ at a speed of 10-30 ℃/min;
c. mixing titanium vanadium carbide solid solution powder and an iron ingot, placing the mixture into a smelting container, smelting the mixture to molten mixed liquid, and carrying out gas atomization to prepare powder to obtain spherical iron-based vanadium titanium carbide metal ceramic powder, wherein the addition amount of the titanium vanadium carbide solid solution powder is 5-25% of the mass of the iron ingot, and the superheat degree of the molten mixed liquid is controlled to be 50-150 ℃.
2. The method for preparing a spherical iron-based vanadium titanium carbide cermet powder according to claim 1, characterized in that: in the step a, the density of the briquetting is 3.00-4.00 g/cm 3 。
3. The method for preparing a spherical iron-based vanadium titanium carbide cermet powder according to any one of claims 1 or 2, characterized in that: in the step c, the gas atomization medium is argon; the pressure is 5-15 MPa.
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