CN113215444A - Nano-particle reinforced TC4 metal powder material and preparation method thereof - Google Patents
Nano-particle reinforced TC4 metal powder material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano-particle reinforced TC4 metal powder and a preparation method thereof, belonging to the field of metal powder material preparation. The preparation method provided by the invention adopts a fused salt-ultrasonic dispersion combination step to prepare a product, and effectively introduces nano-sized solid ceramic particles into the TC4 metal material, the metal powder material prepared by the method has the characteristics of high hardness, high strength, high wear resistance and the like, the raw material guarantee is provided for expanding the application of the TC 4-based composite material in the industrial field, and the ceramic particles have high utilization rate of the nano-particles; meanwhile, the nanometer titanium carbide particle reinforced TC4 powder material can also expand the application of the titanium-based composite material in the fields of additive manufacturing, hot isostatic pressing and powder metallurgy. The preparation method of the material has the advantages of simple operation steps, high repeatability, safety and environmental protection, and can realize industrialized small-scale production.
Description
Technical Field
The invention relates to the field of metal powder material preparation, in particular to a nano-particle reinforced TC4 metal powder material and a preparation method thereof.
Background
The titanium alloy has excellent performances of low density, high specific strength, high temperature resistance, corrosion resistance, no magnetism and the like, and related products are widely applied to the fields of aviation, aerospace, navigation, medical appliances, thermal power generation and the like. The TC4 titanium alloy material is used as an alpha + beta type titanium alloy, and the comprehensive mechanical property is more excellent. However, with the change of external environment, the conventional TC4 titanium alloy is difficult to meet increasingly severe service conditions in order to approach the service limit. Therefore, improving the mechanical properties or improving the mechanical properties under high temperature conditions is a new direction for the future research of the TC 4-based composite material. At present, the main forming modes of titanium alloy products include powder metallurgy, hot isostatic pressing and additive manufacturing technologies, and the main raw material of the titanium alloy products is titanium alloy powder. Therefore, the preparation of the titanium alloy material with excellent performance is a prerequisite for preparing the titanium alloy material with high performance.
The ceramic particle reinforced metal-based composite material is a metal-based composite material formed by adding reinforcing phase ceramic particles which are dispersed and distributed in a metal matrix. The reinforcing phase is mainly selected from ceramic particles with high strength, high hardness and high melting point. Because the content of the reinforcing phase is relatively low, the distribution is relatively uniform, and the particles are fine, the composite material basically keeps the original physical properties of the matrix metal. In addition, the reinforced phase ceramic particles are dispersed in the metal matrix, and the pinning effect of the particles can effectively block dislocation movement in the metal matrix, so that the mechanical property of the material can be greatly improved. Conventional reinforcement phase materials are predominantly micron or sub-micron sized particles. Studies have shown that the strengthening effect of the same mass or volume fraction of nanoparticles in the matrix is more pronounced than that of conventional micron or submicron sized particles.
The titanium carbide ceramic has excellent performances of high temperature resistance, high strength, high hardness, high heat conductivity, low density, corrosion resistance and the like, and products of the titanium carbide ceramic are widely applied to the industrial fields of petroleum, chemical industry, microelectronics, automobiles, aerospace, aviation, paper making, laser, mining industry, atomic energy and the like. The nanometer titanium carbide ceramic particles inherit the advantages of titanium carbide ceramic, and if the nanometer titanium carbide ceramic particles are introduced into TC4 powder to prepare the nanometer titanium carbide ceramic reinforced TC4 powder, the mechanical property of the TC4 powder can be improved, and the nanometer titanium carbide ceramic reinforced TC4 powder has positive significance for expanding the application of titanium alloy-based composite materials in the industrial field.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a preparation method of a nano-particle reinforced TC4 metal powder material, which introduces high-strength nano-ceramic material particles titanium carbide into TC4 powder by a molten salt-ultrasonic dispersion method, so that the purposes of enhancing mechanical properties such as hardness and strength of products are achieved, and the high utilization rate of nano-particles can be guaranteed. The method has simple and controllable operation steps, high large-scale production efficiency and guaranteed product quality among batches.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of preparing a nanoparticle reinforced TC4 metal powder, comprising the steps of:
(1) mixing TC4 metal powder, nano titanium carbide and inorganic salt uniformly, performing ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide is 1: 0.07-0.35, and the mass ratio of the sum of the TC4 metal powder and the nano titanium carbide to the inorganic salt is as follows: m (TC4 metal powder + nano titanium carbide): m (inorganic salt) is 3-15: 85-97;
(2) vacuum heating the precursor powder A in the step (1), carrying out ultrasonic dispersion treatment on the obtained melt after the powder is melted, cooling, and crushing the obtained massive solid to powder particles with the particle size less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2；
(3) Dissolving and stirring the precursor powder B obtained in the step (2) in deionized water, then precipitating the dissolved suspension, pouring out the upper suspension to leave black granular substances at the bottom layer, and repeating the step three times to obtain a bottom layer mixed solution C;
(4) and (4) carrying out suction filtration and drying on the bottom layer mixed solution C obtained in the step (3), and sequentially crushing and sieving the obtained black powder to obtain the nano-particle enhanced TC4 metal powder.
The nanometer particle reinforced TC4 metal powder is prepared by adopting a fused salt-ultrasonic dispersion combined method, the fused TC4 liquid metal, titanium carbide ceramic particles and the fused salt are mutually insoluble, the fused salt is used as a dispersion carrier, the nanometer-sized solid ceramic particles are effectively introduced into a TC4 metal material, and the reinforced material particles are uniformly dispersed in the liquid metal by ultrasonic dispersion; meanwhile, the nanometer titanium carbide particle reinforced TC4 powder material can also expand the application of the titanium-based composite material in the fields of additive manufacturing, hot isostatic pressing and powder metallurgy. The preparation method of the material has the advantages of simple operation steps, high repeatability, safety and environmental protection, and can realize industrialized small-scale production.
Preferably, in the step (1), the mass ratio of the TC4 metal powder to the nano titanium carbide is 1: 0.2-0.35, and the mass ratio of the sum of the TC4 metal powder and the nano titanium carbide to the inorganic salt is: m (TC4 metal powder + nano titanium carbide): m (inorganic salt) is 5-10: 95-90.
After repeated experiments by the inventor, the titanium carbide is added in an excessive amount, so that nanoparticles can be agglomerated on the surface of liquid metal, and the ultrasonic dispersion efficiency is reduced; if the amount is too small, the desired performance-enhancing effect cannot be achieved. Under the proportion, the dispersion uniformity of the titanium carbide ceramic particles in the melt after ultrasonic dispersion is higher, and the mechanical property of the obtained product is enhanced to a greater extent.
In addition, the inorganic salt as a carrier for the TC4 titanium alloy and reinforcing particles in molten salt-dispersion inevitably causes problems in material uniformity and production efficiency if the ratio is not proper.
Preferably, the average grain diameter of the nano titanium carbide is 40-60 nm.
The titanium carbide ceramic particles with specific sizes can effectively inhibit dislocation motion of materials after being dispersed in a metal matrix, so that the mechanical property of the product is improved; if the size is not proper, the reinforcing effect is not good, and the uniformity of the precursor of the product during melting and ultrasonic dispersion is affected. When the particle size of the modified ceramic particles is too small, the particles are too fine, and the particles are easy to agglomerate in the mixing and smelting process, so that a good dispersion enhancing effect cannot be achieved; if the particle size of the particles is too large, although the agglomeration defect can be improved to a certain extent, the performance improvement effect is not good, the waste of the added particles is caused, and the cost is obviously improved.
Preferably, the average particle size of the TC4 metal powder is 15-74 μm, and the average particle size of the inorganic salt is 500-650 μm;
more preferably, in the step (1), the ball milling medium adopted when the TC4 metal powder, the nano titanium carbide and the inorganic salt are subjected to ball milling treatment is titanium carbide grinding balls, and the mass ratio of the titanium carbide grinding balls to ball materials of the TC4 metal powder, the nano titanium carbide and the inorganic salt is 3-5: 1; the ball milling treatment time is 12-24 h, and the rotating speed is 250-300 r/min.
The ball milling treatment is carried out by adopting the grinding balls made of the same materials as the reinforcing materials, and the size and ball milling parameters of the ball milling raw materials are limited, so that the ball milling efficiency can be effectively improved.
Preferably, the inorganic salt comprises at least one of calcium chloride and barium chloride.
The two inorganic salts have similar properties, can be mixed at any proportion and can be effectively used as molten salt and a dispersion carrier.
Preferably, the temperature of the vacuum heating in the step (2) is 1675-1695 ℃, and the time is 5-10 min.
Preferably, the time of the ultrasonic dispersion treatment in the step (2) is 2-3 min, and the power is 800-1000W.
The ultrasonic dispersion treatment is carried out on a molten salt particle mixture, so that specific time and power are required to ensure that the ceramic titanium carbide particles in the melt can be effectively and uniformly dispersed into the powder material.
More preferably, in the ultrasonic dispersion treatment in the step (2), the ceramic ultrasonic probe is inserted into the melt for ultrasonic dispersion, and when the ceramic ultrasonic probe is inserted into the melt, the tip of the probe is positioned two thirds below the liquid level of the melt.
Preferably, the mass ratio of the deionized water to the precursor powder B in the step (3) is more than 5: 1;
preferably, the time for the suspension liquid in the step (3) to precipitate is 1-2 min.
Preferably, the drying temperature in the step (4) is 100-150 ℃.
Another object of the present invention is to provide a nanoparticle reinforced TC4 metal powder material prepared by the method for preparing the nanoparticle reinforced TC4 metal powder material.
Compared with the existing titanium alloy material, the nano-particle reinforced TC4 metal powder material prepared by the invention has higher high temperature resistance, wear resistance and mechanical strength.
The invention has the beneficial effects that the invention provides the nano-particle reinforced TC4 metal powder and the preparation method thereof. The preparation method adopts the fused salt-ultrasonic dispersion combination step to prepare the product, utilizes the characteristic that the fused TC4 liquid metal, titanium carbide ceramic particles and the fused salt are not mutually soluble, effectively introduces the nano-sized solid ceramic particles into the TC4 metal material by using the fused salt as a dispersion carrier, and utilizes the ultrasonic dispersion to uniformly disperse the reinforcing material particles in the liquid metal, because the titanium carbide has the advantages of high strength, high hardness, high temperature resistance, small thermal expansion coefficient and the like, the metal powder material prepared by the method has the characteristics of high hardness, high strength, high wear resistance and the like, the raw material guarantee is provided for expanding the application of the TC 4-based composite material in the industrial field, and the ceramic particles have higher utilization rate of the nano-particles; meanwhile, the nanometer titanium carbide particle reinforced TC4 powder material can also expand the application of the titanium-based composite material in the fields of additive manufacturing, hot isostatic pressing and powder metallurgy. The preparation method of the material has the advantages of simple operation steps, high repeatability, safety and environmental protection, and can realize industrialized small-scale production.
Drawings
Fig. 1 is an SEM image of nanoparticle reinforced TC4 metal powder material prepared according to the present invention.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for implementing the invention are common reagents and instruments unless otherwise specified.
Example 1
An embodiment of the method for preparing nanoparticle reinforced TC4 metal powder according to the present invention comprises the steps of:
(1) placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 8:2: 90; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
(2) heating the precursor powder A obtained in the step (1) in vacuum for 10min, inserting the obtained melt into a ceramic ultrasonic probe after the powder is melted, enabling the tip of the probe to be located at two thirds of the position below the liquid level of the melt, carrying out ultrasonic dispersion treatment for 3min at the power of 800W, pouring into a ceramic boat for cooling, and crushing the obtained blocky solid into powder particles with the particle size of less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2(ii) a The heating temperature is 1695 ℃;
(3) dissolving and stirring the precursor powder B obtained in the step (2) in deionized water, then precipitating the dissolved suspension for 2min, pouring out the upper suspension to leave black granular substances at the bottom layer, and repeating the step three times to obtain a bottom layer mixed solution C; the mass ratio of the deionized water to the precursor powder B is more than 5: 1;
(4) and (4) carrying out suction filtration and drying at 120 ℃ on the bottom layer mixed solution C obtained in the step (3), and then sequentially crushing and sieving the obtained black powder to obtain the nano-particle enhanced TC4 metal powder.
The obtained product is observed under a scanning electron microscope, and the result is shown in figure 1, the titanium carbide particles are uniformly dispersed in the powder material, and no obvious agglomeration phenomenon exists.
Example 2
The difference between this embodiment and embodiment 1 is only that step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 7.5:2.5: 90; the average grain diameter of the nano titanium carbide is 40 nm; the average particle size of the TC4 metal powder is 53 mu m, and the average particle size of the inorganic salt is 550 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
example 3
The difference between this embodiment and embodiment 1 is only that step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 7.5:2.5: 90; the average grain diameter of the nano titanium carbide is 60 nm; the average particle size of the TC4 metal powder is 74 mu m, and the average particle size of the inorganic salt is 650 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
example 4
The difference between this embodiment and embodiment 1 is only that step (1) is:
placing TC4 metal powder, nano titanium carbide, calcium chloride and barium chloride into a mixing bottle in a glove box protected by argon gas, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride to the barium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (calcium chloride): m (barium chloride) ═ 7.5:2.5:10: 80; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the calcium chloride is 500 mu m; the average particle size of barium chloride is 650 μm; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
example 5
The difference between this embodiment and embodiment 1 is only that step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) 3.75:1.25: 95; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
example 6
The difference between this embodiment and embodiment 1 is only that step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 2.3:0.7: 97; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
example 7
The difference between this embodiment and embodiment 1 is only that the steps (1) and (2) are:
(1) placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 10:0.7: 89.3; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
(2) heating the precursor powder A in the step (1) in vacuum for 10min, inserting the obtained melt into a ceramic ultrasonic probe after the powder is melted, carrying out ultrasonic dispersion treatment for 2min at 1000W power, pouring into a ceramic boat for cooling, and crushing the obtained blocky solid to powder particles with the particle size less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2(ii) a What is needed isThe heating temperature is 1675 ℃;
example 8
The difference between this embodiment and embodiment 1 is only that the steps are:
(1) placing TC4 metal powder, nano titanium carbide, barium chloride and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride to the barium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (calcium chloride): m (barium chloride) ═ 10:2:80: 8; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the calcium chloride is 500 mu m; the average particle size of barium chloride is 600 μm; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
(2) heating the precursor powder A in the step (1) in vacuum for 10min, inserting the obtained melt into a ceramic ultrasonic probe after the powder is melted, carrying out ultrasonic dispersion treatment for 3min at the power of 800W, pouring into a ceramic boat for cooling, and crushing the obtained blocky solid to powder particles with the particle size less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2(ii) a The heating temperature is 1695 ℃;
(3) dissolving and stirring the precursor powder B obtained in the step (2) in deionized water, then precipitating the dissolved suspension for 3min, pouring out the upper suspension to leave black granular substances at the bottom layer, and repeating the step three times to obtain a bottom layer mixed solution C; the mass ratio of the deionized water to the precursor powder B is more than 5: 1;
(4) and (4) carrying out suction filtration and drying at 150 ℃ on the bottom layer mixed solution C obtained in the step (3), and then sequentially crushing and sieving the obtained black powder to obtain the nano-particle enhanced TC4 metal powder.
Comparative example 1
The comparative example differs from example 1 only in that the step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 9:6: 85; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the ball material mass ratio of the titanium carbide grinding balls to TC4 metal powder, nano titanium carbide and inorganic salt is 3: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
comparative example 2
The comparative example differs from example 1 only in that the step (1) is:
placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) 9.99:0.01: 90; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
comparative example 3
The comparative example differs from example 1 only in that the procedure is:
(1) placing TC4 metal powder, nano titanium carbide and calcium chloride into a mixing bottle in an argon-protected glove box, adding titanium carbide grinding balls, sealing, placing on a mixer for ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide to the calcium chloride is as follows: m (TC4 metal powder): m (nano titanium carbide): m (inorganic salt) ═ 8:2: 90; the average grain diameter of the nano titanium carbide is 50 nm; the average particle size of the TC4 metal powder is 15 mu m, and the average particle size of the inorganic salt is 500 mu m; the mass ratio of the titanium carbide grinding balls to the ball materials of TC4 metal powder, nano titanium carbide and inorganic salt is 4: 1; the ball milling treatment time is 24 hours, and the rotating speed is 300 r/min;
(2) heating the precursor powder A in the step (1) in vacuum for 10min, conventionally stirring for 3min after the powder is melted, pouring the mixture into a ceramic boat for cooling, and crushing the obtained blocky solid to powder particles with the particle size less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2(ii) a The heating temperature is 1695 ℃;
(3) dissolving and stirring the precursor powder B obtained in the step (2) in deionized water, then precipitating the dissolved suspension for 2min, pouring out the upper suspension to leave black granular substances at the bottom layer, and repeating the step three times to obtain a bottom layer mixed solution C; the mass ratio of the deionized water to the precursor powder B is more than 5: 1;
(4) and (4) carrying out suction filtration and drying at 120 ℃ on the bottom layer mixed solution C obtained in the step (3), and then sequentially crushing and sieving the obtained black powder to obtain the TC4 metal powder.
Effect example 1
In order to verify the reinforcing effect of the nanoparticle reinforced TC4 metal powder material of the present invention, hardness tests were performed on the powder materials prepared in examples 2, 6 and 8 and comparative examples 1 to 3 and pure TC4 powder at room temperature (25 ℃), 100 ℃, 200 ℃, 300 ℃ and 400 ℃ respectively, and the results are shown in table 1; meanwhile, the nanoparticle utilization ratio of each product was sampled at multiple points and the range values were counted, and the results are shown in table 2 (the nanoparticle utilization ratio is defined as the ratio of the mass fraction of nanoparticles per unit mass of the composite metal powder to the mass of nanoparticles (nano titanium carbide) added to the theoretical raw material to the TC4 powder).
TABLE 1
| Product(s) | HV/25℃ | HV/100℃ | HV/200℃ | HV/300℃ | HV/400℃ |
| TC4 | 306 | 280 | 271.2 | 256 | 238 |
| Example 2 | 591.7 | 570.5 | 563.6 | 551.4 | 535.1 |
| Example 6 | 586.3 | 567.9 | 560.2 | 548.8 | 533.4 |
| Example 8 | 563.4 | 541.9 | 534.5 | 524.2 | 510.7 |
| Comparative example 1 | 583.1 | 561.8 | 552.7 | 540.5 | 527.0 |
| Comparative example 2 | 331.2 | 309.0 | 300.8 | 287.7 | 271.4 |
| Comparative example 3 | 478.6 | 455.7 | 447.2 | 434.6 | 419.2 |
TABLE 2
| Product(s) | Nanoparticle utilization (%) |
| Example 2 | 65～71 |
| Example 6 | 67～73 |
| Example 8 | 69～76 |
| Comparative example 1 | 52～57 |
| Comparative example 2 | 78～83 |
| Comparative example 3 | 55～62 |
From the results, compared with pure TC4 powder, the nano titanium carbide particle reinforced spherical TC4 powder obtained by the molten salt-ultrasonic dispersion method has higher room temperature and high temperature mechanical properties, and the modified ceramic particles in each product have higher utilization rate of the nano particles. The product obtained in the comparative example 1 has the performance improvement equivalent to that of the example, but the particle utilization rate is lower, while the product obtained in the comparative example 2 has the ceramic particle utilization rate higher than that of pure TC4 powder, so that the addition ratio of the TC4 metal powder, the nano titanium carbide and the inorganic salt in the precursor powder is optimized at the same time to give consideration to both the raw material use efficiency and the mechanical property of the product; the product obtained in the comparative example 3 has unsatisfactory mechanical properties and nanoparticle utilization rate due to the use of a non-optimal preparation process.
For those skilled in the art, it is possible to make other various compositions based on the above-described technical solutions and concepts, that is, the generating phase is based on the TC4 material reinforced by nano titanium carbide particles (TiC)np/TC4) of the particle size of the raw materials, the proportions of the raw materials, the dispersing process, the ultrasonic power, the drying process, and all such modifications and variants are intended to be within the scope of the claims.
In addition, the invention is also applicable to other titanium alloy powders, such as TC11 and TA15 metal powders, and all of the modifications of these raw material powders should fall within the scope of the claims of the present invention.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method of preparing a nanoparticle reinforced TC4 metal powder, comprising the steps of:
(1) mixing TC4 metal powder, nano titanium carbide and inorganic salt uniformly, performing ball milling treatment, and sieving to obtain precursor powder A; the mass ratio of the TC4 metal powder to the nano titanium carbide is 1: 0.07-0.35, and the mass ratio of the sum of the TC4 metal powder and the nano titanium carbide to the inorganic salt is as follows: m (TC4 metal powder + nano titanium carbide): m (inorganic salt) is 3-15: 85-97;
(2) vacuum heating the precursor powder A in the step (1), carrying out ultrasonic dispersion treatment on the obtained melt after the powder is melted, cooling, and crushing the obtained massive solid to powder particles with the particle size less than 5mm to obtain precursor powder B; the vacuum degree during vacuum heating is less than or equal to 6 multiplied by 10-2；
(3) Dissolving and stirring the precursor powder B obtained in the step (2) in deionized water, then precipitating the dissolved suspension, pouring out the upper suspension to leave black granular substances at the bottom layer, and repeating the step three times to obtain a bottom layer mixed solution C;
(4) and (4) carrying out suction filtration and drying on the bottom layer mixed solution C obtained in the step (3), and sequentially crushing and sieving the obtained black powder to obtain the nano-particle enhanced TC4 metal powder.
2. The method for preparing the metal powder of TC4 reinforced by nanoparticles as claimed in claim 1, wherein the mass ratio of the TC4 metal powder to the nano-titanium carbide in step (1) is 1: 0.2-0.35, and the mass ratio of the sum of the TC4 metal powder and the nano-titanium carbide to the inorganic salt is: m (TC4 metal powder + nano titanium carbide): m (inorganic salt) is 5-10: 95-90.
3. The method of preparing the nanoparticle reinforced TC4 metal powder of claim 1, wherein the nano titanium carbide has an average particle size of 40 to 60 nm.
4. The method of preparing the nanoparticle reinforced TC4 metal powder of claim 1, wherein the TC4 metal powder has an average particle size of 15 to 74 μm and the inorganic salt has an average particle size of 500 to 650 μm.
5. The method for preparing the metal powder of TC4 reinforced by nanoparticles as claimed in claim 1, wherein the ball milling media used in the ball milling process of the metal powder of TC4, the nano titanium carbide and the inorganic salt in step (1) are titanium carbide grinding balls, and the ball material mass ratio of the titanium carbide grinding balls to the three raw materials of the metal powder of TC4, the nano titanium carbide and the inorganic salt is m (titanium carbide grinding balls): m (TC4 metal powder, nano titanium carbide and inorganic salt) is 3-5: 1; the ball milling treatment time is 12-24 h, and the rotating speed is 250-300 r/min.
6. The method for preparing the nanoparticle reinforced TC4 metal powder according to claim 1, wherein the vacuum heating in the step (2) is carried out at 1675-1695 ℃ for 5-10 min.
7. The method for preparing the nano-particle reinforced TC4 metal powder according to claim 1, wherein the ultrasonic dispersion treatment in the step (2) is carried out for 2-3 min at a power of 800-1000W.
8. The method of preparing the TC4 metal powder reinforced with nanoparticles as claimed in claim 7, wherein the ultrasonic dispersion treatment in the step (2) is carried out by inserting a ceramic ultrasonic probe into the melt and the tip of the ceramic ultrasonic probe is located two thirds below the surface of the melt.
9. The method of preparing the nanoparticle reinforced TC4 metal powder of claim 1, wherein the suspension of step (3) is precipitated for 1-2 min; and (4) drying at the temperature of 100-150 ℃.
10. The nanoparticle reinforced TC4 metal powder material prepared by the method for preparing the nanoparticle reinforced TC4 metal powder material as claimed in any one of claims 1 to 9.
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