CN111331141A - Preparation method of TA32 titanium alloy powder for 3D printing - Google Patents
Preparation method of TA32 titanium alloy powder for 3D printing Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C14/00—Alloys based on titanium
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/088—Fluid nozzles, e.g. angle, distance
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0896—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid particle transport, separation: process and apparatus
Abstract
The invention discloses a preparation method of TA32 titanium alloy powder for 3D printing, and belongs to the technical field of 3D printing. The method is to prepare a TA32 titanium alloy ingot; carrying out acid pickling on the surface of a TA32 titanium alloy ingot by using an acid pickling solution, removing a surface reaction layer, wiping the surface reaction layer after cleaning, putting the surface reaction layer into a water-cooling split copper crucible, then placing the surface reaction layer into a smelting chamber of inert gas atomization powder production equipment, and carrying out induction smelting on the inert gas atomization powder production equipment by starting a heating program of the inert gas atomization powder production equipment after cabin environment control is carried out on the inert gas atomization powder production equipment: promoting the cooling of atomized liquid drops by adopting annular auxiliary gas, and reversely spraying argon gas at the bottom of the atomization chamber; and under the protection of inert gas, screening the prepared spherical titanium alloy powder by adopting a cyclone separation technology. According to the invention, the qualified metal powder meeting the requirements of the 3D printing process is prepared by using the gas atomization technology, and powerful guarantee is provided for stable production of aerospace high-temperature resistant structural parts.
Description
Technical Field
The invention relates to a preparation method of TA32 titanium alloy powder for 3D printing, and belongs to the technical field of 3D printing.
Background
The heat resistant titanium alloy has solid solution strengthened near α and α + β titanium alloys, near α type heat resistant titanium alloys operating at 550 ℃ and containing high α stable elements, almost 7 equivalent of aluminum and a small amount of β stable elements, the alloys have more α phases and a small amount of β phases in a balanced state, so that the alloys not only have higher creep resistance, fatigue resistance and fracture toughness but also have sufficient plasticity and instantaneous strength at high temperature, and the near α type alloys have excellent comprehensive properties, thereby becoming a main system of the heat resistant alloys.
The 3D printing technology is a novel digital processing technology, powder is melted by high-energy heat sources such as laser and electric arc, and layer-by-layer printing is carried out according to three-dimensional discrete data of a part to finally obtain the part. The 3D printing has high quality requirements on raw material powder, and needs that the properties such as chemical composition, fluidity, particle morphology and the like meet certain requirements, and it is difficult to efficiently produce titanium alloy powder meeting the requirements by general titanium alloy powder preparation technology, for example: a rotary electrode method, a hydrogenation and dehydrogenation powder preparation method, a plasma spheroidization method and the like.
Disclosure of Invention
Aiming at the harsh requirements of 3D printing on the properties of titanium alloy powder such as chemical composition, fluidity, particle morphology and the like, the problem that the titanium alloy powder meeting the conditions is difficult to efficiently produce by the common titanium alloy powder preparation technology is solved. The invention provides a preparation method of TA32 titanium alloy powder for 3D printing, and the TA32 base alloy powder with uniform components, good fluidity, uniform particle size, good sphericity and low impurity content can be prepared in batches by the method, so that the application requirements of the 3D printing technology in the aerospace field are met. The technical scheme is as follows:
the invention aims to provide a preparation method of TA32 titanium alloy powder for 3D printing, which comprises the following steps:
the method comprises the following steps: preparing 15 kg-30 kg of TA32 titanium alloy ingot by vacuum induction melting according to the following mass percentage of 5.0-6.5% of Al, 2.5-4% of Zr, 0.2-1.0% of Nb, 0.3-2.0% of Mo, 3.0-4.5% of Sn, 0.2-0.8% of Ta, 0.1-0.6% of Si and the balance of Ti and inevitable impurities;
step two: pickling the surface of a TA32 titanium alloy ingot by using a pickling solution to remove a surface reaction layer, cleaning and drying the surface reaction layer, putting the cleaned surface reaction layer into a water-cooled split copper crucible, and then putting the water-cooled split copper crucible into a smelting chamber of inert gas atomization powder production equipment;
step three: performing cabin environment control on inert gas atomization powder-making production equipment, firstly pumping the vacuum degree of a smelting chamber to be below 0.1Pa, then filling inert gas into the smelting chamber, stopping filling gas when the gas pressure reaches 91-93 KPa, standing for observation, filling inert gas into an atomization cabin when the leakage rate of the smelting chamber is observed to be less than 150Pa, stopping filling gas when the gas pressure reaches 91-93 KPa, and standing for observation;
step four: and after the leakage rate of the atomizing chamber is less than 150Pa and the pressure of the gas storage tank is more than or equal to 6.5Mpa, starting a heating program of inert gas atomization powder production equipment to perform induction melting on the TA32 titanium alloy ingot in a water-cooling split copper crucible, wherein the induction melting program is as follows: 100KW, 1-2 min; 200KW, 2-3 min; 250KW, 2-3 min; 300KW, 2-3 min; 390KW, 1-2 min; 400KW, 1-2 min;
step five: when the temperature of the molten titanium is raised to be above 1750 ℃, starting a high-pressure inert gas nozzle, promoting atomized liquid drops to be cooled by adopting annular auxiliary gas, and reversely spraying argon gas at the bottom of an atomization cabin;
step six: and under the protection of inert gas, screening the prepared spherical titanium alloy powder by adopting a cyclone separation technology.
Preferably, in the step one, the TA32 titanium alloy ingot with the weight of 15 kg-30 kg is prepared by vacuum induction melting, the prepared raw materials are placed in a copper crucible, then the copper crucible is placed in induction melting equipment, the power of the equipment is increased at the speed of 50KW/min, when the power reaches 390 KW-400 KW, the power is maintained until the temperature of titanium liquid in the copper crucible reaches 1750-1800 ℃, melting is carried out for 5 min-10 min, and then the titanium liquid flows into a mold through a flow guide nozzle for cooling, solidifying and forming, so that the TA32 titanium alloy ingot with the weight of 15 kg-30 kg is obtained.
Preferably, the acid wash solution of step two consists of HF, HNO3, and water, wherein: the mass concentration of HF is 3-5%, HNO3The mass concentration of (A) is 5-15%. More preferably, the mass concentration of HF is 4%, HNO3The mass concentration of (2) is 7%.
Preferably, the pressure of the high-pressure inert gas in the fifth step is 3.5MPa to 5.0 MPa; fifthly, the diameter of a flow guide pipe of the nozzle is 4-6 mm; fifthly, the back-spraying pressure of the back-spraying argon is 0.1 MPa-0.5 MPa.
Preferably, the cyclone separation technology in the sixth step is that the airflow classification pressure is 0.1-0.8 MPa, the induced air frequency is 10-15 Hz, and the classification frequency is 1-3 times. More preferably, the cyclone separation technology in the sixth step is that the airflow classification pressure is 0.5MPa, the induced air frequency is 13Hz, and the classification times are 2 times.
Preferably, the classification particle size range of the screening treatment in the step six is selected from any one or a combination of several ranges in the following ranges: 20 to 63 mu m, 63 to 106 mu m, 106 to 250 mu m and 250 to 500 mu m.
The invention also provides TA32 high-temperature-resistant alloy powder for 3D printing, which is prepared by any one of the preparation methods.
The invention also provides application of the TA32 high-temperature-resistant alloy powder for 3D printing prepared by any one of the preparation methods in 3D printing structural parts.
The invention also provides a method for 3D printing a structural part by using the TA32 titanium alloy powder for 3D printing prepared by the preparation method, wherein the method selects the particle size range of 20-63 mu m, the fluidity of 20-30 s/50g and the bulk density of 2.0g/cm3～2.4g/cm3The TA32 titanium alloy powder for 3D printing is used for 3D laser printing according to the structure of a pre-printed structural part under the conditions that the laser power is 200W-350W, the scanning speed is 900 mm/s-1100 mm/s, the scanning distance is 0.1 mm-0.15 mm and the powder layer thickness is 0.025-0.035 mm.
The invention has the beneficial effects that:
according to the invention, the TiAl-based heat-resistant titanium alloy is used as a base material, and the qualified metal powder meeting the requirements of the 3D printing process is prepared by using an atomization technology, so that a powerful guarantee is provided for stable production of aerospace high-temperature resistant structural parts.
Aiming at the problems that the 3D printing technology is adopted in the invention, the development period of parts can be greatly shortened, the production cost is reduced, and the problems of long processing period and high production cost of precise structural members of heat-resistant parts in aerospace can be solved.
The invention aims at the alloy element components designed for the titanium alloy for 3D laser printing, and can effectively improve the melting rate and the component uniformity of the titanium alloy ingot.
The titanium alloy powder prepared by the invention can be obtained with the particle size range of 20-63 mu m by a cyclone separation technology, can be respectively used for laser 3D printing, and meets the application of 3D printing technology with different high-energy beam as heat sources.
The TA32 titanium alloy powder obtained by the invention has wide particle size range, high fine powder yield and good sphericity. The powder spreading effect in the laser forming cabin is good, the printing performance is uniform, and the surface quality is excellent.
The titanium alloy powder printing piece prepared by the invention has the advantages of excellent mechanical property, high strength and good high temperature resistance.
The invention can efficiently and fully smelt the titanium alloy ingot by adopting the water-cooling split copper crucible induction smelting technology, and avoids the volatilization of low-melting-point elements and the introduction of impurity elements caused by overlong time. And the induction melting of the TA32 titanium alloy ingot is carried out by adopting water-cooling split copper, the powder preparation efficiency can be improved by more than 20%, the fine powder yield is improved to more than 30%, and the spherical powder accounts for more than 90%. Further solves the problems of low production efficiency, poor sphericity and low fine powder yield of the titanium alloy powder.
Drawings
FIG. 1 is a drawing of a TA32 titanium alloy powder for 3D printing prepared by the invention.
Fig. 2 is a diagram of a laser 3D printed structural member object prepared by the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the present invention is not limited to these examples.
Example 1:
the invention provides TA32 titanium alloy powder for 3D printing and a preparation method thereof, wherein the preparation method comprises the following steps:
the method comprises the following steps: proportioning Al 5.0%, Zr 2.5%, Nb 0.2%, Mo 0.3%, Sn3.0%, Ta 0.2%, Si 0.1%, and the balance Ti and inevitable impurities, putting the proportioned raw materials into a copper crucible, then putting the copper crucible into induction melting equipment, increasing the power of the equipment at the rate of 50KW/min, maintaining the power until the temperature of titanium liquid in the copper crucible reaches 1750-1800 ℃ when 390 KW-400 KW is reached, melting for 5-10 min, and then flowing into a die through a flow guide nozzle for cooling, solidifying and forming, thereby obtaining a TA32 titanium alloy ingot with the weight of 15-30 kg;
step two: pickling the surface of a TA32 titanium alloy ingot by using a pickling solution to remove a surface reaction layer and prevent pollution of other elements, cleaning the surface of the TA32 titanium alloy ingot by using deionized water, putting the cleaned surface of the TA32 titanium alloy ingot into a water-cooling split copper crucible, and putting the water-cooling split copper crucible into a smelting chamber of inert gas atomization powder production equipment; wherein: the acid washing solution is prepared from HF and HNO3And water, wherein the mass ratio of HF: HNO3：H2O＝3:5:92；
Step three: performing cabin environment control on inert gas atomization powder-making production equipment, firstly pumping the vacuum degree of a smelting chamber to 0.1Pa, then filling inert gas into the smelting chamber, stopping filling gas when the gas pressure reaches 91KPa, standing and observing, filling inert gas into an atomization cabin when the leakage rate of the smelting chamber is observed to be less than 150Pa, stopping filling gas when the gas pressure reaches 91KPa, and standing and observing;
step four: and after the leakage rate of the atomizing chamber is less than 150Pa and the pressure of the gas storage tank is more than or equal to 6.5Mpa, starting a heating program of inert gas atomization powder production equipment to perform induction melting on the TA32 titanium alloy ingot in a water-cooling split copper crucible, wherein the induction melting program is as follows: 100KW for 1 min; 200KW, 2 min; 250KW, 2 min; 300KW, 2 min; 390KW, 1 min; 400KW for 1 min;
step five: when the temperature of the molten titanium is increased to above 1750 ℃, a high-pressure inert gas nozzle is opened, the annular auxiliary gas is adopted to promote the cooling of atomized liquid drops, the reverse-spraying argon is implemented at the bottom of the atomization cabin to avoid the agglomeration of powder adhesion, the liquid drop injection speed is reduced, and the alloy liquid drops are cooled, so that the agglomeration of the powder adhesion is avoided, and the number of satellite balls is reduced, wherein: the pressure of the high-pressure inert gas is 3.5MPa, the diameter of a flow guide pipe of the nozzle is phi 5mm, and the back-spray pressure of the back-spray argon is 0.3 MPa;
step six: under the protection of inert gas, the prepared spherical titanium alloy powder is screened by adopting a cyclone separation technology, the air flow classification pressure range is 0.5MPa, the induced air frequency is 13Hz, the classification frequency is 2 times, and the classification particle size range is as follows: 20 to 63 μm.
The embodiment also provides a method for 3D printing a structural part by using the TA32 titanium alloy powder for 3D printing prepared by the preparation method, wherein the method comprises the steps of selecting the titanium alloy powder with the particle size range of 20-63 mu m, the fluidity of 30s/50g and the apparent density of 2.1g/cm3The TA32 titanium alloy powder for 3D printing is subjected to 3D laser printing according to the structure of a pre-printed structural member under the conditions that the laser power is 300W, the scanning speed is 900mm/s, the scanning interval is 0.12mm and the powder layer thickness is 0.03 mm. Through detection, the mechanical property of the formed test piece is as follows: the yield strength is 850MPa, the tensile strength is 923MPa, and the elongation is 12%.
Example 2:
the invention provides TA32 titanium alloy powder for 3D printing and a preparation method thereof, wherein the preparation method comprises the following steps:
the method comprises the following steps: the method comprises the following steps of proportioning Al 6.5%, Zr 4%, Nb 1.0%, Mo 2.0%, Sn 4.5%, Ta 0.8%, Si 0.6%, and the balance Ti and inevitable impurities, putting the proportioned raw materials into a copper crucible, putting the copper crucible into induction melting equipment, increasing the power of the equipment at the rate of 50KW/min, maintaining the power until the temperature of titanium liquid in the copper crucible reaches 1750-1800 ℃ when 390 KW-400 KW is reached, melting for 5-10 min, and then flowing into a die through a diversion nozzle to cool, solidify and form, thereby obtaining a TA32 titanium alloy ingot with the weight of 15-30 kg;
step two: pickling the surface of a titanium alloy ingot by using a pickling solution to remove a surface reaction layer and prevent pollution of other elements, cleaning the titanium alloy ingot by using absolute ethyl alcohol after cleaning by using deionized water, putting the titanium alloy ingot into a water-cooling split copper crucible, and then putting the water-cooling split copper crucible into a smelting chamber of inert gas atomization powder production equipment; wherein: the acid washing solution is prepared from HF and HNO3And water, wherein the mass ratio of HF: HNO3：H2O＝1:3:40；
Step three: performing cabin environment control on inert gas atomization powder-making production equipment, firstly pumping the vacuum degree of a smelting chamber to 0.1Pa, then filling inert gas into the smelting chamber, stopping filling gas when the gas pressure reaches 93KPa, standing and observing, filling inert gas into an atomization cabin when the leakage rate of the smelting chamber is observed to be less than 150Pa, stopping filling gas when the gas pressure reaches 91KPa, and standing and observing;
step four: and after the leakage rate of the atomizing chamber is less than 150Pa and the pressure of the gas storage tank is more than or equal to 6.5Mpa, starting a heating program of inert gas atomization powder production equipment to perform induction melting on the TA32 titanium alloy ingot in a water-cooling split copper crucible, wherein the induction melting program is as follows: 100KW, 2 min; 200KW for 3 min; 250KW, 3 min; 300KW for 3 min; 390KW, 2 min; 400KW for 2 min;
step five: when the temperature of the molten titanium is increased to above 1750 ℃, a high-pressure inert gas nozzle is opened, the annular auxiliary gas is adopted to promote the cooling of atomized liquid drops, the reverse-spraying argon is implemented at the bottom of the atomization cabin to avoid the agglomeration of powder adhesion, the liquid drop injection speed is reduced, and the alloy liquid drops are cooled, so that the agglomeration of the powder adhesion is avoided, and the number of satellite balls is reduced, wherein: the pressure of the high-pressure inert gas is 4.0MPa, the diameter of a flow guide pipe of the nozzle is phi 5mm, and the back-spray pressure of the back-spray argon is 0.5 MPa;
step six: under the protection of inert gas, the prepared spherical titanium alloy powder is screened by adopting a cyclone separation technology, the air flow classification pressure range is 0.5MPa, the induced air frequency is 13HZ, the classification frequency is 2 times, and the classification particle size range is as follows: 20 to 63 μm.
The embodiment also provides a method for 3D printing a structural part by using the TA32 titanium alloy powder for 3D printing prepared by the preparation method, wherein the method comprises the steps of selecting the titanium alloy powder with the particle size range of 20-63 mu m, the fluidity of 22s/50g and the apparent density of 2.2g/cm3The TA32 titanium alloy powder for 3D printing is subjected to 3D laser printing according to the structure of a pre-printed structural member under the conditions that the laser power is 280W, the scanning speed is 900mm/s, the scanning interval is 0.12mm and the powder layer thickness is 0.03 mm. Through detection, the mechanical property of the formed test piece is as follows: the yield strength is 821MPa, the tensile strength is 850MPa, and the elongation is 10 percent.
Example 3:
the invention provides TA32 titanium alloy powder for 3D printing and a preparation method thereof, wherein the preparation method comprises the following steps:
the method comprises the following steps: the method comprises the following steps of proportioning Al 5.5%, Zr 3%, Nb 0.5%, Mo 0.6%, Sn 3.5%, Ta 0.5%, Si 0.4%, and the balance Ti and inevitable impurities, putting the proportioned raw materials into a copper crucible, putting the copper crucible into induction melting equipment, increasing the power of the equipment at the rate of 50KW/min, maintaining the power until the temperature of titanium liquid in the copper crucible reaches 1750-1800 ℃ when 390 KW-400 KW is reached, melting for 5-10 min, and then flowing into a die through a diversion nozzle to cool, solidify and form, thereby obtaining a TA32 titanium alloy ingot with the weight of 15-30 kg;
step two: acid pickling of titanium alloy ingot surface with acid pickling solutionRemoving a surface reaction layer to prevent pollution of other elements, cleaning the surface reaction layer by using absolute ethyl alcohol after deionized water is cleaned, putting the cleaned surface reaction layer into a water-cooling split copper crucible, and then putting the water-cooling split copper crucible into a smelting chamber of inert gas atomization powder production equipment; wherein the acid washing solution is prepared from HF and HNO3And water, wherein the mass ratio of HF: HNO3：H2O＝3:5:92；
Step three: performing cabin environment control on inert gas atomization powder-making production equipment, firstly pumping the vacuum degree of a smelting chamber to 0.1Pa, then filling inert gas into the smelting chamber, stopping filling gas when the gas pressure reaches 93KPa, standing and observing, filling inert gas into an atomization cabin when the leakage rate of the smelting chamber is observed to be less than 150Pa, stopping filling gas when the gas pressure reaches 92KPa, and standing and observing;
step four: and after the leakage rate of the atomizing chamber is less than 150Pa and the pressure of the gas storage tank is more than or equal to 6.5Mpa, starting a heating program of inert gas atomization powder production equipment to perform induction melting on the TA32 titanium alloy ingot in a water-cooling split copper crucible, wherein the induction melting program is as follows: 100KW for 1 min; 200KW for 3 min; 250KW, 3 min; 300KW, 2 min; 390KW, 1 min; 400KW for 1 min;
step five: when the temperature of the molten titanium is increased to above 1750 ℃, a high-pressure inert gas nozzle is opened, the annular auxiliary gas is adopted to promote the cooling of atomized liquid drops, the reverse-spraying argon is implemented at the bottom of the atomization cabin to avoid the agglomeration of powder adhesion, the liquid drop injection speed is reduced, and the alloy liquid drops are cooled, so that the agglomeration of the powder adhesion is avoided, and the number of satellite balls is reduced, wherein: the pressure of the high-pressure inert gas is 5.0MPa, the diameter of a flow guide pipe of the nozzle is phi 5mm, and the back-spray pressure of the back-spray argon is 0.4 MPa;
step six: under the protection of inert gas, the prepared spherical titanium alloy powder is screened by adopting a cyclone separation technology, the air flow classification pressure range is 0.5MPa, the induced air frequency is 13HZ, the classification frequency is 2 times, and the classification particle size range is as follows: 20 to 63 μm.
The embodiment also provides a method for 3D printing the structural part by using the TA32 titanium alloy powder for 3D printing prepared by the preparation method, wherein the method is to select the particle size range from 20 micrometers to 63 micrometers25s/50g of fluidity and 2.1g/cm of apparent density3The TA32 titanium alloy powder for 3D printing is subjected to 3D laser printing according to the structure of a pre-printed structural part under the conditions of laser power of 280W, scanning speed of 1000mm/s, scanning interval of 0.12mm and powder layer thickness of 0.03 mm. Through detection, the mechanical property of the formed test piece is as follows: the yield strength is 895MPa, the tensile strength is 923MPa, and the elongation is 9%.
The TA32 titanium alloy powder real object for 3D printing prepared by the invention is shown in fig. 1, and the laser 3D printing structural part real object is shown in fig. 2.
The following experiments illustrate the effects that can be achieved by the present invention:
the TA32 titanium alloy powder for 3D printing prepared in examples 1 to 3 and the printed material thereof were subjected to the fine powder yield, flowability, bulk density, and mechanical property tests, and the test results are shown in table 1.
Table 1 test results of TA32 titanium alloy powder for 3D printing prepared in examples 1 to 3 and its printed material
As can be seen from Table 1: the yield of the titanium alloy fine powder prepared by the technology is high and is over 30 percent; the flowability is good, the requirement of the existing 3D printing equipment on the flowability of the powder is met, and the bulk density reflects the stacking state of the powder well; the prepared titanium alloy powder printing forming part has high mechanical property test strength and good plasticity, and can meet the requirements of actual processing and application.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A preparation method of TA32 titanium alloy powder for 3D printing is characterized by comprising the following steps:
the method comprises the following steps: preparing 15 kg-30 kg of TA32 titanium alloy ingot by vacuum induction melting according to the following mass percentage of Al 5.0-6.5%, Zr 2.5-4%, Nb 0.2-1.0%, Mo0.3-2.0%, Sn 3.0-4.5%, Ta 0.2-0.8%, Si 0.1-0.6%, and the balance of Ti and inevitable impurities;
step two: pickling the surface of a TA32 titanium alloy ingot by using a pickling solution to remove a surface reaction layer, cleaning and drying the surface reaction layer, putting the cleaned surface reaction layer into a water-cooled split copper crucible, and then putting the water-cooled split copper crucible into a smelting chamber of inert gas atomization powder production equipment;
step three: performing cabin environment control on inert gas atomization powder-making production equipment, firstly pumping the vacuum degree of a smelting chamber to be below 0.1Pa, then filling inert gas into the smelting chamber, stopping filling gas when the gas pressure reaches 91-93 KPa, standing for observation, filling inert gas into an atomization cabin when the leakage rate of the smelting chamber is observed to be less than 150Pa, stopping filling gas when the gas pressure reaches 91-93 KPa, and standing for observation;
step four: and after the leakage rate of the atomizing chamber is less than 150Pa and the pressure of the gas storage tank is more than or equal to 6.5Mpa, starting a heating program of inert gas atomization powder production equipment to perform induction melting on the TA32 titanium alloy ingot in a water-cooling split copper crucible, wherein the induction melting program is as follows: 100KW, 1-2 min; 200KW, 2-3 min; 250KW, 2-3 min; 300KW, 2-3 min; 390KW, 1-2 min; 400KW, 1-2 min;
step five: when the temperature of the molten titanium is raised to be above 1750 ℃, starting a high-pressure inert gas nozzle, promoting atomized liquid drops to be cooled by adopting annular auxiliary gas, and reversely spraying argon gas at the bottom of an atomization cabin;
step six: and under the protection of inert gas, screening the prepared spherical titanium alloy powder by adopting a cyclone separation technology.
2. The method according to claim 1, wherein the acid cleaning solution of step two is selected from the group consisting of HF, HNO3And water, wherein: the mass concentration of HF is 3-5%, HNO3The mass concentration of (A) is 5-15%.
3. The method according to claim 1, wherein the pressure of the high-pressure inert gas in the fifth step is 3.5 to 5.0 MPa; fifthly, the diameter of a flow guide pipe of the nozzle is 4-6 mm; fifthly, the back-spraying pressure of the back-spraying argon is 0.1 MPa-0.5 MPa.
4. The preparation method according to claim 1, wherein the cyclone separation technology of the sixth step is that the air flow classification pressure is 0.1MPa to 0.8MPa, the induced air frequency is 10Hz to 15Hz, and the classification frequency is 1 to 3 times.
5. The preparation method according to claim 1, wherein the classification particle size range of the screening treatment in the step six is selected from any one or a combination of several ranges in the following ranges: 20 to 63 mu m, 63 to 106 mu m, 106 to 250 mu m and 250 to 500 mu m.
6. TA32 high-temperature-resistant alloy powder for 3D printing prepared by the preparation method of any one of claims 1 to 5.
7. The TA32 high-temperature-resistant alloy powder for 3D printing of claim 6, wherein the alloy powder is used for 3D printing of structural parts.
8. A method for 3D printing a structural member by using TA32 titanium alloy powder for 3D printing prepared by the preparation method according to claim 1, wherein the selected particle size range is 20 μm to 63 μm, the fluidity is (20 to 30) s/50g, and the bulk density is 2.0g/cm3～2.4g/cm3The TA32 titanium alloy powder for 3D printing is used for 3D laser printing according to the structure of a pre-printed structural part under the conditions that the laser power is 200W-350W, the scanning speed is 900 mm/s-1100 mm/s, the scanning distance is 0.1 mm-0.15 mm and the powder layer thickness is 0.025-0.035 mm.
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