CN111036931A - Tungsten-cobalt alloy powder and preparation method thereof - Google Patents
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Abstract
The invention discloses a preparation method of tungsten-cobalt alloy powder, which adopts doping and plasma reduction methods to prepare small-size tungsten-cobalt alloy powder. Different elements and oxides thereof can be uniformly dispersed in the crystal grains and in the crystal boundary by doping, so that the size of the crystal grains is reduced, the compactness is improved, and the hardness of the material can be enhanced; and sintering the powder precursor by a two-step discharge plasma sintering method. Because the plasma has the characteristics of high temperature, large volume of the plasma torch, high energy density, high heat transfer and cooling speed and the like, the powder can quickly absorb heat and melt when passing through the plasma, and then can be condensed into a spherical shape under the action of surface tension, and can be solidified into the metal alloy powder with high sphericity, good fluidity and high purity in a very short time.
Description
Technical Field
The invention relates to the field of powder materials, in particular to small-size spherical tungsten-cobalt alloy powder and a preparation method thereof.
Background
In recent years, metal 3D printing technology gradually receives wide attention and application due to infinite design space, and the quality requirement for 3D printing metal powder is higher and higher. Compared with other foil materials and block materials, the small-sized metal spherical powder has the advantages of easiness in preparation, high material utilization rate, wide category and the like, and is widely applied to the field of metal 3D printing.
The tungsten-cobalt alloy is an alloy formed by adding cobalt and other elements into tungsten serving as a main body. Tungsten is metal with the highest melting point, has the characteristics of good heat conduction, electric conductivity, creep resistance, high temperature resistance, large specific gravity and the like, is used for manufacturing hard alloy and alloy additives, and is widely applied to the fields of electronics, aerospace, weapons and the like for manufacturing heating elements, contacts, heat shields, rocket nozzles, armor piercing cores and the like. At present, many research and development units at home and abroad research and develop small-size spherical metal powder materials and processes, wherein the research and development units mainly comprise Optomec in the United states, EOS in Germany, and Pulin, Sai-platinute and the like in China. At present, the widely adopted technologies for preparing small-size metal powder at home and abroad are a water/gas atomization method, a plasma atomization method, an electrolysis method, an atomization granulation method, a high-energy ball milling method, a rotary electrode method and the like. The water/gas atomization method is a technique of directly crushing liquid metal or alloy into fine liquid droplets under the action of external force and rapidly condensing the fine liquid droplets to prepare powder. Plasma atomization refers to a technology of injecting solid particles into inert gas plasma, completely evaporating the solid particles under the action of high temperature of the plasma, existing in a steam form, and then rapidly cooling the solid particles by using a gas quenching cooling technology to rapidly condense, nucleate and grow saturated steam to form ultrafine powder. The electrolytic powder preparation is to deposit and separate metal powder on a cathode by electrolyzing molten salt or aqueous solution of the salt. The atomization granulation method is a method in which a raw material is dispersed into mist droplets by an atomizer, and the mist droplets are directly contacted with hot air or other gas to obtain a powder. The high-energy ball milling method is a technology that raw material powder is placed in a high-energy ball mill to run for a long time, powder particles are impacted by grinding balls, namely, rotary mechanical energy is transferred to the powder, meanwhile, the powder bears the action of various forces of impact, shearing, friction and compression under the repeated impact of a ball milling medium to generate serious deformation, and the powder is subjected to repeated extrusion, cold welding and crushing processes to become ultra-fine particles in dispersion distribution, so that the formation of nano particles is realized in a solid state. The rotating electrode method is a powder-making method in which a consumable electrode made of metal or alloy is heated by an electric arc and melted into liquid, the liquid is thrown out and crushed into fine liquid droplets by the centrifugal force of the high-speed rotation of the electrode, and then the fine liquid droplets are condensed into powder.
However, metal powder prepared by the water/gas atomization method and the high-energy ball milling method is easy to have more satellite balls, so that the nodularity and the sphericity are relatively low, the apparent density and the apparent density are low, and the metal powder is easy to carry gas to generate hollow balls; the powder prepared by the electrolytic method is dendritic in morphology, and the powder particles have large internal stress, poor flowability and high cost; the powder prepared by the atomization granulation method is generally loose and porous, and has low density and loose density; the powder prepared by the rotary electrode method has larger size of more than 100 μm generally and high cost.
Therefore, those skilled in the art have made an effort to develop a method for preparing a tungsten-cobalt alloy powder having high purity, high sphericity, high fluidity, low hollow sphere fraction in fine powder, and high yield of fine powder.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is how to prepare high-purity, high-sphericity, high-fluidity tungsten-cobalt alloy powder with low hollow sphere rate of fine powder and high fine powder yield.
In order to achieve the purpose, the invention provides a preparation method of tungsten-cobalt alloy powder, which comprises the following steps:
1) mixing 90-97 wt% of cobalt tungstate solid particles and 1-8 wt% of Y2O3、Al2O3The mixture is evenly mixed and stirred,
2) adding polyvinyl pyrrolidone (PVP, K17) with the mass ratio of 1% -2% during the mixing process to obtain precursor powder, washing the precursor powder with water and anhydrous ethanol for 4-5 times, fully drying at 70-85 deg.C for 12h,
3) transferring the dried precursor powder into a hopper of a plasma sintering furnace, feeding by taking argon and/or helium as powder carrier gas,
4) controlling the flow of reducing atmosphere to be 10-20L/min, heating the plasma sintering furnace to 600-fold-material 800 ℃, preserving heat for 2-10min at the heating rate of 5-10 ℃/min, adjusting the pressure of the vacuum hot press to be 40-50MPa, continuously heating to 1200-fold-material 1500 ℃, preserving heat for 1-15min at the heating rate of 80-100 ℃/min,
5) cooling to room temperature to obtain the product.
Further, the particle size of the cobalt tungstate solid particles in the step 1) is 10-50 μm.
Further, Y in step 1)2O3、Al2O3Has a particle diameter of 3-8 μm.
Further, the polyvinyl pyrrolidone in step 2) may be replaced by polyvinyl alcohol.
Further, in the step 3), argon and/or helium gas is used as a powder carrier gas, the feeding speed of the argon and/or helium gas is 30-50L/min, and the pressure is 90-110 kPa.
Further, the reducing atmosphere in the step 4) is hydrogen or argon-hydrogen mixed gas.
Further, the cooling rate in the step 5) is 10-25 ℃/min.
The invention also provides the tungsten-cobalt alloy powder, wherein the average grain size of the tungsten-cobalt alloy powder is not more than 700nm, and the Vickers hardness is not less than 600 hv.
Furthermore, the flowability of the tungsten-cobalt alloy powder is less than 18s/50g, the loose packing density is 5.6-5.8g/cm3, and the oxygen content is not more than 0.8%.
Further, the sphericity ratio of the tungsten-cobalt alloy powder is not less than 92%.
Technical effects
According to the method for preparing the spherical metal powder by the plasma reduction, the prepared tungsten-cobalt alloy powder is good in sphericity and high in fluidity;
the invention mixes polyvinyl pyrrolidone and doped Y into precursor2O3、Al2O3The compound prepared tungsten-cobalt alloy powder has high spheroidization rate, uniform and fine size and high strength.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a scanning electron microscope of tungsten-cobalt alloy powder particles in a preferred embodiment of the invention;
FIG. 2 is a statistical plot of the particle sizes of the W-Co alloy powder in a preferred embodiment of the present invention;
FIG. 3 is a particle size distribution diagram of a W-Co alloy powder according to a preferred embodiment of the present invention;
FIG. 4 is a particle size distribution diagram of the tungsten-cobalt alloy powder in comparative example 1.
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
The method adopts doping and plasma reduction methods to prepare the small-size tungsten-cobalt alloy powder. Different elements and oxides thereof can be uniformly dispersed in the crystal grains and at the crystal boundary by doping, so that the crystal grain size is reduced, the compactness is improved, and the hardness of the material can be enhanced. And sintering the powder precursor by a two-step discharge plasma sintering method, namely heating to 800 ℃ at a heating rate of 5-10 ℃/min under the condition of controlling hydrogen flow (10-20L/min), preserving heat for 2-10min, reducing the composite powder, heating to 1500 ℃ at 80-100 ℃/min, preserving heat for 1-15min, increasing the pressure of a vacuum hot press to 40-50MPa before the final sintering temperature is started, and cooling to room temperature after sintering is finished to obtain a tungsten-cobalt alloy sample, wherein the plasma power is 30-100 kW. Because the plasma has the characteristics of high temperature, large volume of the plasma torch, high energy density, high heat transfer and cooling speed and the like, the powder can quickly absorb heat and melt when passing through the plasma, and then can be condensed into a spherical shape under the action of surface tension, and can be solidified into the metal alloy powder with high sphericity, good fluidity and high purity in a very short time.
Example 1
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) 97 percent of cobalt tungstate (CoWO) with the size of 15-25 mu m4) The particle size of the solid particles accounting for 2 percent of the mass is 5-8 mu mY2O3Mixing uniformly;
2) adding polyvinyl pyrrolidone (PVP, K17) with the mass percent of 1% in the mixing process, then washing for 5 times by using water and absolute ethyl alcohol, and fully drying for 12 hours at the temperature of 80 ℃;
3) transferring the dried precursor powder into a hopper, feeding by taking argon as powder carrier gas, wherein the air inlet speed is 30L/min;
4) adjusting the hydrogen flow to 12L/min, heating the plasma sintering furnace to 600 ℃, preserving the heat for 5min, and reducing the composite powder at the heating rate of 5 ℃/min; then adjusting the pressure of the vacuum hot press to 40MPa, heating to 1400 ℃, and keeping the temperature for 10min, wherein the heating rate is 85 ℃/min;
5) and cooling the alloy powder to room temperature at a cooling speed of 15 ℃/min, and collecting a sample to obtain the product.
When the obtained alloy powder is detected, the average grain size of the powder is 520nm, the Vickers hardness is 697.4hv, the oxygen content is 0.5%, the fluidity is 16s/50g, the powder sphericity is good, the nodularity is high (not less than 94%), a scanning electron micrograph is shown in figure 1, a statistical graph of the particle size of the alloy powder is shown in figure 2, and a distribution graph of the particle size of the alloy powder is shown in figure 3.
Example 2
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) 97 percent of cobalt tungstate (CoWO) with the grain diameter of 30-45 mu m4) The particle diameter of 1% of the particles by mass is 5-8 mu mY2O3Mixing uniformly;
2) adding polyvinyl pyrrolidone (PVP, K17) with the mass percent of 1% in the mixing process, then washing for 5 times by using water and absolute ethyl alcohol, and fully drying for 12 hours at the temperature of 80 ℃;
3) transferring the dried precursor powder into a hopper, and feeding with argon as powder carrier gas at an air inlet speed of 35L/min;
4) controlling the hydrogen flow to be 14L/min, heating the plasma sintering furnace to 600 ℃, keeping the temperature for 8min, wherein the heating rate is 8 ℃/min, increasing the pressure of a vacuum hot press to 40MPa, heating to 1200 ℃, keeping the temperature for 12min, and the heating rate is 90 ℃/min;
5) and cooling the alloy powder to room temperature at a cooling speed of 15 ℃/min, and collecting a sample to obtain the spherical tungsten-cobalt alloy powder.
The obtained alloy powder is detected, the average grain size of the powder is 630nm, the Vickers hardness is 632.6hv, the oxygen content is 0.6%, the fluidity is 18s/50g, the powder sphericity is good, and the spheroidization rate is high (more than or equal to 93%).
Example 3
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) mixing 92% by mass of 30-45 μm size cobalt tungstate (CoWO)4) Solid particles and 7% by mass of Al having a particle size of 6 μm2O3Mixing uniformly;
2) adding polyvinyl pyrrolidone (PVP, K17) with the mass percent of 1% in the mixing process, then washing for 5 times by using water and absolute ethyl alcohol, and fully drying for 12 hours at the temperature of 80 ℃;
3) transferring the dried precursor powder into a hopper, feeding by taking argon as powder carrier gas, wherein the air inlet speed is 45L/min;
4) controlling the hydrogen flow at 18L/min, heating the plasma sintering furnace to 700 ℃, keeping the temperature for 8min, wherein the heating rate is 10 ℃/min, increasing the pressure of a vacuum hot press to 50MPa, heating to 1300 ℃, keeping the temperature for 12min, and the heating rate is 80 ℃/min;
5) and cooling the alloy powder to room temperature at a cooling speed of 20 ℃/min, and collecting a sample to obtain the spherical tungsten-cobalt alloy powder.
The obtained tungsten-cobalt alloy is detected, the average grain size of the tungsten-cobalt alloy powder is 660nm, the Vickers hardness is 612.9hv, the oxygen content is 0.6%, the fluidity is 17s/50g, the powder sphericity is good, and the nodularity is high (more than or equal to 93%).
Comparative example 1
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) weighing and proportioning the precursor powder according to the proportion in the embodiment 1, and uniformly mixing;
2) pouring the precursor material into a high-energy ball mill for wet milling for 2 h;
3) after the ball milling is finished, drying the prepared powder at 80 ℃ for 12 h;
4) adding the powder into a single-column hydraulic press, pressurizing to 11.4MPa, and performing press forming;
5) putting the powder after the press forming into an annealing furnace, and keeping the temperature of 900 ℃ for 3h under the hydrogen atmosphere at the hydrogen flow rate of 5L/min;
6) and performing ball milling on the annealed powder for 1h again to obtain the tungsten-cobalt alloy powder.
When the obtained tungsten-cobalt alloy is detected, the average particle size of the powder is 1.01 mu m, the Vickers hardness is 406.5hv, the oxygen content is 1.4%, the fluidity is 27s/50g, the sphericity of the powder is poor, the spheroidization rate is low (not less than 84%), and the particle size distribution diagram of the alloy powder is shown in figure 4.
Comparative example 2
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) weighing and proportioning the precursor powder according to the proportion in the embodiment 2, and uniformly mixing;
2) pouring the precursor material into a high-energy ball mill for wet milling for 2 h;
3) after the ball milling is finished, drying the prepared powder at 80 ℃ for 12 h;
4) adding the powder into a single-column hydraulic press, pressurizing by 10.3MPa, and performing press forming;
5) putting the powder after the press forming into an annealing furnace, and keeping the temperature of 900 ℃ for 3h under the hydrogen atmosphere at the hydrogen flow rate of 5L/min;
6) and performing ball milling on the annealed powder for 1h again to obtain the tungsten-cobalt alloy powder.
The obtained tungsten-cobalt alloy is detected, the average particle size of the powder is 1.11 mu m, the Vickers hardness is 416.7hv, the oxygen content is 1.3%, the fluidity is 26s/50g, the sphericity of the powder is poor, and the spheroidization rate is low (more than or equal to 86%).
Comparative example 3
A manufacturing method of spherical tungsten-cobalt alloy powder comprises the following steps:
1) weighing and proportioning the precursor powder according to the proportion in the embodiment 3, and uniformly mixing;
2) pouring the precursor material into a high-energy ball mill for wet milling for 2 h;
3) after the ball milling is finished, drying the prepared powder at 80 ℃ for 12 h;
4) adding the powder into a single-column hydraulic press, pressurizing by 10MPa, and performing press forming;
5) and putting the powder after the pressing forming into an annealing furnace, and keeping the temperature of 900 ℃ for 3h under the hydrogen atmosphere at the hydrogen flow rate of 5L/min.
6) And performing ball milling on the annealed powder for 1h again to obtain the tungsten-cobalt alloy powder.
The obtained tungsten-cobalt alloy is detected, the average particle size of the powder is 1.03 mu m, the Vickers hardness is 408.6hv, the oxygen content is 1.4%, the fluidity is 26s/50g, the powder sphericity is poor, and the nodularity is low (more than or equal to 83%).
The results of the performance tests of examples 1-3 and comparative examples 1-3 are listed below:
| sample numbering | Fluidity (s/50g) | Bulk Density (g/cm)3) | Oxygen content% | Hardness (hv) |
| Example 1 | 16 | 5.6 | 0.5 | 697.4 |
| Example 2 | 18 | 5.7 | 0.6 | 632.6 |
| Example 3 | 17 | 5.8 | 0.6 | 612.9 |
| Comparative example 1 | 27 | 7.6 | 1.4 | 406.5 |
| Comparative example 2 | 26 | 7.9 | 1.3 | 416.7 |
| Comparison ofExample 3 | 26 | 7.7 | 1.4 | 408.6 |
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made according to the purpose of the invention, and all changes, modifications, substitutions, combinations or simplifications made according to the technical solutions of the present invention shall be equivalent substitution ways, so long as the invention is consistent with the purpose of the present invention, and all the changes belong to the protection scope of the present invention.
Claims (10)
1. The preparation method of the tungsten-cobalt alloy powder is characterized by comprising the following steps of:
1) mixing 90-97 wt% of cobalt tungstate solid particles and 1-8 wt% of Y2O3、Al2O3The mixture is evenly mixed and stirred,
2) adding polyvinyl pyrrolidone (PVP, K17) with the mass ratio of 1-2% during the mixing process to obtain precursor powder, washing the precursor powder with water and absolute ethyl alcohol for 4-5 times, fully drying at 70-85 deg.C for 12h,
3) transferring the dried precursor powder into a hopper of a plasma sintering furnace, feeding by taking argon and/or helium as powder carrier gas,
4) controlling the flow of reducing atmosphere to be 10-20L/min, heating the plasma sintering furnace to 600-fold-material 800 ℃, preserving heat for 2-10min at the heating rate of 5-10 ℃/min, adjusting the pressure of the vacuum hot press to be 40-50MPa, continuously heating to 1200-fold-material 1500 ℃, preserving heat for 1-15min at the heating rate of 80-100 ℃/min,
5) and cooling to room temperature to obtain the tungsten-cobalt alloy powder.
2. The method for preparing a tungsten-cobalt alloy powder as claimed in claim 1, wherein the particle size of the solid particles of cobalt tungstate in step 1) is 10 to 50 μm.
3. The method of preparing a tungsten-cobalt alloy powder according to claim 2, wherein Y in step 1)2O3、Al2O3Has a particle diameter of 3-8 μm.
4. The method of preparing a tungsten-cobalt alloy powder according to claim 1, wherein the polyvinyl alcohol pyrrolidone in step 2) is replaced with polyvinyl alcohol.
5. The method of preparing a tungsten-cobalt alloy powder according to claim 1, wherein argon and/or helium is fed as a powder carrier gas in step 3), the feeding speed of the argon and/or helium is 30 to 50L/min, and the pressure is 90 to 110 kPa.
6. The method of preparing a tungsten-cobalt alloy powder according to claim 1, wherein the reducing atmosphere in the step 4) is hydrogen or a mixture of argon and hydrogen.
7. The method of preparing a tungsten-cobalt alloy powder according to claim 1, wherein the cooling rate in step 5) is 10 to 25 ℃/min.
8. A tungsten-cobalt alloy powder, characterized in that the average grain size of the tungsten-cobalt alloy powder is not more than 700nm, and the Vickers hardness is not less than 600 hv.
9. The W-Co alloy powder of claim 8, wherein the W-Co alloy powder has a flowability of less than 18s/50g and a bulk density of 5.6-5.8g/cm3The oxygen content is not more than 0.8%.
10. The tungsten-cobalt alloy powder of claim 8, wherein the sphericity ratio of the tungsten-cobalt alloy powder is not less than 92%.
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