CN111054914A - TC4 titanium alloy powder for selective electron beam melting forming and preparation method and application thereof - Google Patents
TC4 titanium alloy powder for selective electron beam melting forming and preparation method and application thereof Download PDFInfo
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- B22F2009/0824—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 with a specific atomising fluid
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- 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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- 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
- B22F2009/0836—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 with electric or magnetic field or induction
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- 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
- B22F2009/0888—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 casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
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Abstract
The invention discloses TC4 titanium alloy powder for selective melting forming of an electron beam and a preparation method and application thereof, belonging to the technical field of additive manufacturing. The invention aims to provide TC4 titanium alloy powder which is suitable for selective electron beam melting forming and has good fluidity, sphericity and granularity, so as to meet the application requirements of the selective electron beam melting forming aerospace precise structural parts in the aerospace field. The invention adopts a vacuum induction melting gas atomization process, alloy solution is crushed under the impact of inert gas, titanium alloy powder is obtained by cooling and solidifying, and then the obtained spherical TC4 titanium alloy powder is screened by adopting a cyclone separation technology. The TC4 titanium alloy powder prepared by the method has the advantages of wide particle size range, high fine powder yield, good sphericity and the like. The powder has good powder spreading effect in the electron beam forming cabin, uniform printing performance and excellent surface quality.
Description
Technical Field
The invention relates to TC4 titanium alloy powder for selective melting forming of an electron beam and a preparation method and application thereof, belonging to the technical field of additive manufacturing.
Background
With the continuous development of the domestic metal additive manufacturing technology, various titanium alloy parts produced by the additive manufacturing technology have already completed the engineering verification in aerospace model products, so that the application advantage of the metal additive manufacturing technology is more obvious. As a raw material for metal additive manufacturing, TC4 titanium alloy powder used for selective electron beam melting forming is consumable powder with great preparation difficulty due to the chemical properties of high melting point, high activity and the like. And the flowability, the component uniformity, the particle size uniformity, the sphericity and the like of the powder have a remarkable influence on the melting forming quality of the electron beam selected area. Therefore, the TC4 titanium alloy powder which is suitable for selective electron beam melting forming and has good fluidity, sphericity and granularity is provided, and the application requirement of the aerospace field on selective electron beam melting forming of aerospace precise structural parts is very necessary.
Disclosure of Invention
The invention aims to provide an optimized preparation method of TC4 titanium alloy powder for electron beam selective melting forming, which is used for preparing TC 4-based alloy powder with uniform components, good fluidity, uniform particle size, good sphericity and low impurity content in batches, and meets the application requirements of the field of aerospace on electron beam selective melting forming of aerospace precise structural members.
The technical scheme of the invention is as follows:
TC4 titanium alloy powder for selective electron beam melting forming is spherical particle with particle diameter of 15-500 μm, fluidity of 30s/50g or less, and apparent density of 2.25g/cm3The following.
A method for preparing TC4 titanium alloy powder for electron beam selective melting forming comprises the following steps:
step one, atomizing to prepare powder: after cleaning the TC4 titanium alloy ingot, carrying out induction melting and atomization powder making treatment on the TC4 titanium alloy ingot by using atomization powder making equipment to obtain TC4 titanium alloy powder with the particle size of 53-106 microns;
step two, screening treatment: adopting a cyclone separation technology to sieve TC4 titanium alloy powder with the grain diameter of 15-500 mu m to obtain TC4 titanium alloy powder for selective melting forming of electron beams with the grain diameter range of 53-106 mu m. The invention selects the titanium alloy powder with the grain size range of 53-106 mu m to be used for electron beam selective melting and forming in an electron beam selective area, wherein the grain size range of the titanium alloy powder can be obtained by a cyclone separation technology, and the grain size ranges of the titanium alloy powder are 15-52 mu m, 53-106 mu m, 107-250 mu m, 251-500 mu m and the like.
Further limiting, the chemical components of the TC4 titanium alloy ingot are as follows by mass percent: al: 5.50% -6.75%, V: 3.50% -4.50%, Fe: less than or equal to 0.3 percent, C: less than or equal to 0.3 percent, H: less than or equal to 0.12 percent, O: less than or equal to 0.18 percent, N: less than or equal to 0.04 percent and the balance of Ti.
Further limiting, the specific operation process of cleaning the TC4 titanium alloy ingot in the step one is as follows: washing the TC4 titanium alloy ingot with deionized water after acid washing with acid washing solution, and wiping with absolute ethyl alcohol; wherein the pickling solution is prepared from HF and HNO3And distilled water, wherein HF, HNO3And H2The mass ratio of O is 2:5: 93.
Further limiting, induction melting is carried out by using a split water-cooled copper crucible in the atomization powder preparation process of the step one, and the induction melting process comprises the following steps: after the 100KW is kept warm for 1-2 min, the temperature is kept for 2-3 min after the temperature rises to 200KW, then the temperature is kept for 1-2 min after the temperature rises to 250KW, then the temperature is kept for 2-3 min after the temperature rises to 300KW, and finally the temperature is kept for 2-3 min after the temperature rises to 370 KW.
Further limiting, the vacuum degree of a smelting chamber for induction smelting is less than 10Pa, the charging pressure of the smelting chamber is 90KPa to 93KPa, the leakage rate of the smelting chamber is less than 150Pa/h, the vacuum degree of an atomization chamber is less than 10Pa, the charging pressure of the atomization chamber is 90KPa to 93KPa, the leakage rate of the atomization chamber is less than 150Pa/h, and the pressure of a gas storage tank is more than 6.5 MPa.
Further limiting, in the atomization powder preparation process of the first step, an inert gas nozzle is opened at the titanium liquid temperature of 1750-1800 ℃, and the gas injection pressure is 4.5-5.5 MPa.
And further limiting, in the atomization powder preparation process in the step one, annular auxiliary gas is adopted to promote the cooling of atomized liquid drops, and back-spray argon is carried out at the bottom of the atomization chamber, wherein the pressure of the back-spray gas is 0.4 MPa.
Further limiting, the airflow classification pressure of the cyclone separation in the screening process of the second step is 0.5MPa, and the induced air frequency is 13 Hz.
The TC4 titanium alloy powder prepared by the method is subjected to selective electron beam melting forming printing method, and the technological parameters of selective electron beam melting forming of the method are as follows: the off-focus current was 25mA, the scan line spacing was 0.20mm, and the scan velocity index was 18.
The invention has the following beneficial effects: the TC4 titanium alloy powder with the particle size of 53-106 mu m is prepared by the method, is applied to selective melting forming of electron beams, and has the yield of 20-40%. The TC4 titanium alloy powder prepared by the method has the advantages of wide particle size range, high fine powder yield and good sphericity. The powder spreading effect in the electron beam forming cabin is good, the printing performance is uniform, the surface quality is good, and the like. In addition, the printing component obtained by melting and forming the TC4 titanium alloy powder prepared by the invention through electron beam selective melting has the advantages of excellent mechanical property, high strength and the like.
Drawings
FIG. 1 is a topographical view and a partial enlarged view of a TC4 titanium alloy powder;
FIG. 2 is an enlarged view of a portion of FIG. 1;
fig. 3 is a schematic view of a test member obtained using TC4 titanium alloy powder using electron beam 3D printing.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
Embodiment mode 1:
preparation of TC4 titanium alloy powder for electron beam selective melting forming
Step one, pulverizing: first, an ingot of TC4 titanium alloy was pickled with a pickling solution, and then washed with deionized water and wiped with absolute ethanol. Wherein the pickling solution is prepared from HF and HNO3And distilled water, wherein HF, HNO3And H2The mass ratio of O is 2:5: 93; the TC4 titanium alloy ingot comprises the following chemical components in percentage by mass: al: 5.50% -6.75%, V: 3.50% -4.50%, Fe: less than or equal to 0.3 percent, C: less than or equal to 0.3 percent, H: less than or equal to 0.12 percent, O: less than or equal to 0.18 percent, N: less than or equal to 0.04 percent and the balance of Ti. Then, a split water-cooled copper crucible is used for carrying out induction melting on the TC4 titanium alloy ingot, the vacuum degree of a melting chamber for the induction melting is 4 +/-0.2 Pa, the charging pressure of the melting chamber is 92 +/-0.2 KPa, the leakage rate of the melting chamber is 120 +/-0.2 Pa/h, the vacuum degree of an atomization chamber is 4 +/-0.2 Pa, the charging pressure of the atomization chamber is 92 +/-0.2 KPa, the leakage rate of the atomization chamber is 120 +/-0.2 Pa/h, the pressure of a gas storage tank is 8.5 +/-0.2 MPa, and the induction melting process is shown in the following table.
Loaded power | 100KW | 200KW | 250KW | 300KW | 370KW |
Time of heat preservation | 12min | 2min | 2min | 3min | 3min |
When the actual temperature of the titanium liquid reaches 1780 +/-10 ℃, a high-pressure inert gas nozzle is opened, and the gas injection pressure is 5.0 +/-0.2 MPa. And annular auxiliary gas is adopted to promote the cooling of atomized liquid drops, and back-spraying argon is carried out at the bottom of the atomization chamber, wherein the pressure of the back-spraying air pressure is 0.4 MPa. Obtaining TC4 titanium alloy powder with the grain diameter of 15-500 mu m. The argon gas is reversely sprayed at the bottom of the atomization cabin, so that not only can powder adhesion and agglomeration be avoided, but also the alloy liquid drops can be cooled while the liquid drop spraying speed is reduced, and therefore the powder adhesion and agglomeration are avoided, and the number of satellite balls is reduced.
Step two, screening treatment: adopting a cyclone separation technology to sieve TC4 titanium alloy powder with the particle size of 15-500 mu m, wherein the airflow classification pressure is 0.5MPa, the induced air frequency is 13Hz, the classification frequency is 3 times, obtaining TC4 titanium alloy powder for electron beam selective melting forming with the particle size range of 53-106 mu m, the yield is 38.8%, the powder fluidity is 25s/50g, and the apparent density is 2.3g/cm3。
Embodiment mode 2:
electron beam selective melt forming printing test Using the titanium alloy powder prepared in accordance with embodiment 1
TC4 titanium alloy powder with the grain diameter of 15-500 mu m is used for carrying out electron beam selective melting forming, a component with the printing size of 20 x 50mm is printed, and the process parameters of the printing process are as follows: the off-focus current was 25mA, the scan line pitch was 0.20mm, and the scan speed was 18.
The mechanical properties of the obtained members having dimensions of 20X 50mm were tested, and the yield strength was 1032MPa, the tensile strength was 936MPa and the elongation was 15.1%.
Claims (10)
1. The TC4 titanium alloy powder for selective electron beam melting forming is characterized in that the TC4 titanium alloy powder is spherical particles, the particle size is 53-106 mu m, the fluidity is below 30s/50g, and the apparent density is 2.25g/cm3The following.
2. The method for preparing the TC4 titanium alloy powder for selective electron beam melting forming according to claim 1, comprising the steps of:
step one, pulverizing: after cleaning the TC4 titanium alloy ingot, carrying out induction melting and powder making treatment on the TC4 titanium alloy ingot by using atomization powder making equipment to obtain TC4 titanium alloy powder with the particle size of 15-500 microns;
step two, screening treatment: adopting a cyclone separation technology to sieve TC4 titanium alloy powder with the grain diameter of 15-500 mu m, and selecting the titanium alloy powder with the grain diameter of 53-106 mu m to obtain the TC4 titanium alloy powder for selective electron beam melting forming.
3. The method for preparing the TC4 titanium alloy powder for selective melting forming of the electron beam as claimed in claim 2, wherein the TC4 titanium alloy ingot comprises the following chemical components by mass percent: al: 5.50% -6.75%, V: 3.50% -4.50%, Fe: less than or equal to 0.3 percent, C: less than or equal to 0.3 percent, H: less than or equal to 0.12 percent, O: less than or equal to 0.18 percent, N: less than or equal to 0.04 percent and the balance of Ti.
4. The method for preparing the TC4 titanium alloy powder for selective melting forming of the electron beam as claimed in claim 2, wherein the specific operation process of cleaning the TC4 titanium alloy ingot in the first step is as follows: washing the TC4 titanium alloy ingot with deionized water after acid washing with acid washing solution, and wiping with absolute ethyl alcohol; wherein the pickling solution is prepared from HF and HNO3And distilled water, wherein HF, HNO3And H2The mass ratio of O is 2:5: 93.
5. The method for preparing the TC4 titanium alloy powder for selective electron beam melting and forming as claimed in claim 2, wherein the induction melting in the first step is performed by using a split water-cooled copper crucible, and the induction melting process comprises: after the 100KW is kept warm for 1-2 min, the temperature is kept for 2-3 min after the temperature rises to 200KW, then the temperature is kept for 1-2 min after the temperature rises to 250KW, then the temperature is kept for 2-3 min after the temperature rises to 300KW, and finally the temperature is kept for 2-3 min after the temperature rises to 370 KW.
6. The method of claim 2 or 5, wherein the vacuum degree of the melting chamber in the induction melting is 10Pa or less, the charging pressure of the melting chamber is 90KPa to 93KPa, the leakage rate of the melting chamber is 150Pa/h or less, the vacuum degree of the atomizing chamber is 10Pa or less, the charging pressure of the atomizing chamber is 90KPa to 93KPa, the leakage rate of the atomizing chamber is 150Pa/h or less, and the pressure of the gas storage tank is 6.5MPa or more.
7. The method for preparing the TC4 titanium alloy powder for selective melting forming of electron beams as claimed in claim 2, wherein the inert gas nozzle is opened with a gas injection pressure of 4.5 MPa-5.5 MPa at a titanium solution temperature of 1750-1800 ℃ during the powder preparation treatment in the first step.
8. The method for preparing the TC4 titanium alloy powder for selective electron beam melting forming as claimed in claim 2, wherein the first atomization pulverization step uses ring-shaped auxiliary gas to promote cooling of atomized liquid droplets, and back-injection of argon gas is performed at the bottom of the atomization chamber, and the back-injection pressure is 0.4 MPa.
9. The method for preparing the TC4 titanium alloy powder for selective electron beam melting and forming as claimed in claim 2, wherein the classifying pressure of the cyclone gas flow in the sieving process in the second step is 0.5MPa, and the induced air frequency is 13 Hz.
10. The method for printing by selective electron beam melting forming using the TC4 titanium alloy powder of claim 1, wherein the process parameters of the selective electron beam melting forming of the method are: the off-focus current was 25mA, the scan line spacing was 0.20mm, and the scan velocity index was 18.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113308615A (en) * | 2021-05-26 | 2021-08-27 | 西北工业大学 | High-tensile-strength TC4 alloy and preparation method thereof |
CN114717446A (en) * | 2022-05-25 | 2022-07-08 | 湖南英捷高科技有限责任公司 | High-strength powder metallurgy titanium alloy and preparation method thereof |
CN114717446B (en) * | 2022-05-25 | 2024-05-03 | 湖南英捷高科技有限责任公司 | High-strength powder metallurgy titanium alloy and preparation method thereof |
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