CN115369299A - High-specific-gravity energy-containing two-phase high-entropy alloy and preparation method thereof - Google Patents
High-specific-gravity energy-containing two-phase high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a chairA specific gravity energy-containing two-phase high-entropy alloy and a preparation method thereof, belonging to the technical field of high-entropy alloys. The high-entropy alloy is a solid solution matrix phase formed by a hard solid solution phase of an A-type element and a B, C element, and the density of the high-entropy alloy is more than or equal to 9.5g/cm 3 The energy-containing two-phase high-entropy alloy obtains the two-phase high-entropy alloy with high density, high strength, good energy release characteristic and good plasticity by optimizing the composition of the alloy and regulating and controlling the microstructure; in addition, the high-entropy alloy is prepared by adopting a laser instantaneous liquid phase sintering technology, the preparation process is simple, the period is short, the limitation on the geometric dimension is small, the cost is low, and the prepared high-entropy alloy has excellent performances such as large density adjustable range, high strength, good energy release characteristics and good plasticity, and has huge application prospects in the aspect of preparing high-specific-gravity energy-containing high-entropy alloys.
Description
Technical Field
The invention relates to a high-specific-gravity energy-containing two-phase high-entropy alloy and a preparation method thereof, belonging to the technical field of high-entropy alloys.
Background
The high-specific-gravity energy-containing high-entropy alloy is one of refractory high-entropy alloys, mainly comprises W, mo and other high-density elements, three or more of Ta, hf, nb, ti, zr, V and Cr, and a small amount of other elements, and is also called a medium-entropy alloy when the number of alloy elements is less than four. The alloy system has high melting point and density and good energy release characteristics, and the characteristics enable the alloy system to have wide application prospects in high-temperature structures, weaponry and nuclear industries.
In the alloy system, the contents of W, mo Ta and Hf determine the specific gravity of the alloy, and elements such as Ta, hf, nb, ti, zr and V endow the alloy with energy release characteristics in the failure process. In the actual use process, elements such as Ta, hf and the like are beneficial to the performance, but the addition amount is usually less due to higher cost; the economical alloy elements such as W, mo have the problem of high ductile-brittle transition temperature, and the plasticity and toughness of the alloy are rapidly reduced after the alloy elements are added, so that the advantages of large specific gravity and good high-temperature performance are difficult to exert.
In addition, the alloy containing high-melting-point components has higher smelting difficulty, and large undissolved raw materials are easy to remain due to unreasonable smelting process; if a sintering process is used, a long incubation at very high temperatures is required in order to achieve the highest possible densification, which in turn leads to a coarse structure. The prior art still has more difficulties in preparing high-specific gravity energy-containing high/medium entropy alloy parts, and seriously hinders the practical application of the high-specific gravity energy-containing high/medium entropy alloy parts.
Disclosure of Invention
Aiming at the problems of the high-specific-gravity energy-containing high-entropy alloy at present, the invention provides the high-specific-gravity energy-containing two-phase high-entropy alloy and the preparation method thereof, and the two-phase high-entropy alloy with high density, high strength, good energy release characteristic and good plasticity is obtained by optimizing the composition of the alloy and regulating and controlling the microstructure; in addition, the biphase high-entropy alloy is prepared by adopting a laser instantaneous liquid phase sintering technology, and by utilizing the characteristics of high heating temperature, short heat preservation time, rapid solidification and the like, the alloy components can be selectively melted, the reaction among the alloy components is reduced, the growth of crystal grains is limited, and the deterioration of alloy performance caused by residual large undissolved raw materials or excessive reaction among the alloy components is avoided.
The purpose of the invention is realized by the following technical scheme.
A high-specific-gravity energy-containing biphase high-entropy alloy is composed of a hard solid solution phase of A-type elements and a solid solution matrix phase formed by B, C elements, and has a density of 9.5g/cm or more 3 The energetic biphase high-entropy alloy has a chemical formula of A according to atomic percentage x B y C z Wherein, the A element contains one or two of W and Mo, x is more than or equal to 55 and less than or equal to 80, the B element contains three of Ti, zr and Nb, ti is more than or equal to 5 and less than or equal to 25,5 and less than or equal to 25,5 and less than or equal to Nb 25 and less than or equal to 15 and less than or equal to 35, the C element contains at least one of Al, V, ta, hf, co, mn, ni, cr, fe and B, z is more than or equal to 5 and less than or equal to 30, x + y + z =100.
A preparation method of a high-specific-gravity energy-containing two-phase high-entropy alloy specifically comprises the following steps:
loading raw material powder into a powder storage tank of coaxial powder feeding laser additive manufacturing equipment, opening a laser heat source, synchronously starting to convey the raw material powder, scanning by laser according to a preset program path, obtaining a block blank body of the high-specific-gravity energy-containing biphase high-entropy alloy in a required shape on a substrate after printing is finished, and then performing post-treatment to improve the density and reduce the porosity of the block blank body to obtain the high-specific-gravity energy-containing biphase high-entropy alloy;
the raw material powder is a mixture of simple substance powder corresponding to A, B, C type elements, or a mixture of simple substance powder of A type elements and alloy powder consisting of B, C type elements; the post-treatment is heat treatment, or hot isostatic pressing treatment and heat treatment.
Further, the particle size of the raw material powder is 5 to 150 μm.
Further, the process parameters in the printing process are as follows: the diameter of a laser spot is 0.5-6 mm, the scanning speed is 5-30 mm/s, the laser power is 500-3000W, the powder feeding rate is 0.5-5 r/min, and the single-layer deposition thickness is 1-4 mm.
Furthermore, the temperature and the time of the heat treatment are 700-1200 ℃ and 2-8 h respectively, and the pressure, the temperature and the time of the hot isostatic pressing are 100-180 MPa, 1000-1500 ℃ and 2-10 h respectively.
Has the advantages that:
(1) In the high-entropy alloy, the high-density and high-strength characteristics are endowed by the high-content A element, the B, C element forms a solid solution matrix phase with good plasticity and toughness and provides an energy release characteristic, and meanwhile, the hard solid solution phase formed by the A element and the solid solution matrix phase are uniformly distributed and have fine tissues, so that the high-entropy alloy has excellent mechanical properties of good strength and plasticity matching.
(2) The invention adopts coaxial powder feeding laser additive manufacturing equipment to prepare high-specific gravity energy-containing biphase high-entropy alloy, mainly utilizes a laser instantaneous liquid phase sintering technology to realize high and controllable heating temperature, can be selectively melted according to the melting point of each element, has short sintering time and can be rapidly solidified, can ensure that the B, C elements in a molten pool are not melted or slightly melted while the A elements are melted in the laser printing process, reduces the alloy performance deterioration caused by the melting of the A elements into the B, C elements or mutual reaction, and can also limit the excessive growth of crystal grains, thereby obtaining the biphase high-entropy alloy consisting of a granular phase of the A elements and a matrix phase formed by melting the B, C elements.
(3) The method has the advantages of simple preparation process, short period, small limitation on the geometric dimension and low cost, and the prepared biphase high-entropy alloy has the excellent performances of large density adjustable range, high strength, good energy release characteristic, good plasticity and the like, and has huge application prospect in the preparation of high-specific-gravity energy-containing high-entropy alloy.
Drawings
FIG. 1 shows W prepared in example 5 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 X-ray diffraction (XRD) pattern of (a).
FIG. 2 shows W prepared in example 5 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 Scanning Electron Microscope (SEM) images of (a).
FIG. 3 shows W prepared in example 5 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 Quasi-static stretch profile of (a).
FIG. 4 shows W prepared in example 5 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 Dynamic compressive true stress-strain curve.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the processes are conventional unless otherwise specified, and the starting materials are commercially available from a public source without further specification.
In the following examples:
1) Reagent and apparatus
The metal purities of W, mo, ti, zr, V, nb, al, hf, ta, cr, mn, fe, co and Ni are all more than 99.9wt.%, the bulk metal simple substance is purchased from Zhongnuo New materials (Beijing) science and technology limited, and the powder metal simple substance is purchased from star dust science and technology limited; the purity of the argon gas is more than or equal to 99.999 vol%, and the argon gas is purchased from the pleex gas; the main device information is detailed in table 1.
TABLE 1
2) Testing and characterization
(1) Phase analysis: the XRD sample size is 5mm multiplied by 10mm, the sharp edge is firstly polished to be smooth by 120# abrasive paper, and then the sharp edge is sequentially ground by 240# to 2000# abrasive paper; the X-ray source is a K alpha ray of a Cu target, the wavelength is lambda =0.1542nm, the working voltage is 40kV, the working current is 40mA, the step length is 0.02 degrees, the scanning speed is 5 degrees/min, the measurement angle is 20 degrees to 100 degrees, and the measurement error angle is less than 0.01 degrees.
(2) And (3) testing the density: the density of the high-entropy alloy is tested by using a DT-100 type precision balance, the execution standard is GB5363-2005, and the size of the sample is consistent with that of an XRD sample.
(3) And (3) morphology characterization: the sample size is 5mm multiplied by 5mm, after being embedded on a hot embedding machine, the sample is sequentially ground by sand paper from 240# to 7000# and is polished by silicon dioxide suspension with the granularity of 0.05 mu m; the microstructure is characterized by adopting a Japanese Riviz Regulus8230 type cold field emission scanning electron microscope, and secondary electron imaging is carried out at the working voltage of 15kV.
(4) Quasi-static tensile test: the test sample is made into an I-shaped part sample according to the specification of GB/T228.1-2010 and is carried out on a CMT4305 microcomputer electronic universal testing machine, and the stretching rate is 10 -3 /s。
(5) Dynamic compression and energy release test: according to the GJB-5365-2005 standard, the sample size is phi 4 multiplied by 4mm, and the axial room temperature dynamic compression mechanical property of the alloy is tested by adopting a Separated Hopkinson Pressure Bar (SHPB), and the strain rate is 10 to 10 3 S; and gradually increasing the strain rate until the alloy generates fire when loaded, wherein the strain rate at the moment is regarded as the energy release threshold of the alloy, and the lower the threshold is, the better the energy release effect of the alloy is.
Example 1
High-specific-gravity energy-containing two-phase high-entropy alloy Mo with dimensions of 30mm multiplied by 20mm multiplied by 10mm (length multiplied by width multiplied by thickness) prepared on the basis of laser instantaneous liquid phase sintering technology 55 Ti 10 Zr 15 Nb 10 Al 10 The method comprises the following specific steps:
(1) Under the protection of argon, according to the following ratio of 10:15:10: mixing the surface-treated Ti, zr, nb and Al metal simple substances according to the atomic ratio of 10, alloying and smelting, after the mixed metal simple substances are completely melted into alloy liquid, preparing powder by a gas atomization method, and screening to obtain TiZrNbAl alloy powder with the particle size of 45-150 mu m;
(2) The method comprises the following steps of (1) mixing the subsphaeroidal Mo elementary powder with the grain diameter of 5-25 mu m and the TiZrNbAl alloy powder prepared in the step (1) according to a ratio of 55: mixing the powder in the mixer for 240min according to the atomic ratio of 45, then drying in vacuum, and then loading into a powder storage tank of a powder feeder;
(3) Inputting corresponding data in control software for 3D printing based on the macroscopic size of the prepared high-specific-gravity energy-containing biphase high-entropy alloy, completing CAD three-dimensional modeling, and subsequently generating a program path for automatic laser forming;
(4) Placing the TC4 titanium alloy substrate into a gas protection chamber, fastening, and filling argon into the gas protection chamber to ensure that the oxygen content in the gas protection chamber is lower than 150ppm;
(5) Introducing a laser heat source, synchronously starting a powder feeder to convey mixed powder to a laser heating area of 3D printing equipment, continuously lifting a laser heat source processing head in a forming process (at the moment, a substrate is not moved), scanning laser along a section cutting track of a CAD model of a part, depositing the synchronously conveyed mixed powder on the substrate, stacking layer by layer until printing is finished, and obtaining a block blank of high-specific-gravity energy-containing biphase high-entropy alloy with a required shape on the substrate;
the 3D printing process parameters are as follows: the diameter of a laser spot is 1mm, the scanning speed of the laser spot is 8mm/s, the laser power is 800W, the powder feeding rate is 0.8r/min, and the single-layer deposition thickness is 1.1mm;
(6) Carrying out hot isostatic pressing treatment on the block-shaped green body obtained in the step (5), namely treating for 2 hours under the conditions that the pressure is 110MPa and the temperature is 1100 ℃, and obtaining the density of 11.83g/cm 3 The high specific gravity energetic biphase high entropy alloy has a chemical formula of Mo 55 Ti 10 Zr 20 Nb 10 Al 5 。
According to the morphology characterization result, in the SEM image, the light-color particles are a hard solid solution phase of Mo, the dark-color part is a solid solution matrix phase composed of Ti, zr, nb and Al, and the hard solid solution phase and the solid solution matrix phase are uniformly distributed, have fine structures and have clear two-phase interfaces.
Through quasi-static tensile test, mo 55 Ti 10 Zr 15 Nb 10 Al 10 Has a yield strength of 620MPa, tensile strength of 910MPa, and elongation of 4.2%. Through dynamic compression and energy release tests, mo shows that 55 Ti 10 Zr 15 Nb 10 Al 10 The dynamic compression strength of the material is 1600MPa, the fracture strain is 49 percent, and the material generates fire light under dynamic loading, and the energy release threshold value of the material is 3800s -1 。
Example 2
High specific gravity energy-containing two-phase high-entropy alloy W with the size of 30mm multiplied by 20mm multiplied by 10mm (length multiplied by width multiplied by thickness) prepared based on laser instantaneous liquid phase sintering technology 60 Ti 10 Zr 10 Nb 15 V 5 The method comprises the following specific steps:
(1) Under the protection of argon, according to the following ratio of 10:10:15:5, mixing the surface-treated Ti, zr, nb and V metal simple substances, alloying and smelting, after the mixed metal simple substances are completely melted into alloy liquid, performing powder preparation by a rotary electrode method, and screening to obtain TiZrNbV alloy powder with the particle size of 45-150 mu m;
(2) The method comprises the following steps of mixing the subsphaeroidal W elementary powder with the grain diameter of 5-25 mu m and the TiZrNbV alloy powder prepared in the step (1) according to a ratio of 60: mixing 40 atomic ratio in a mixer for 360min, vacuum drying, and then loading into a powder storage tank of a powder feeder;
(3) Inputting corresponding data in control software for 3D printing based on the macroscopic size of the prepared high-specific-gravity energy-containing two-phase high-entropy alloy to complete CAD three-dimensional modeling and subsequently generate a program path for automatic laser forming;
(4) Placing the TC4 titanium alloy substrate into a gas protection chamber, fastening, and filling argon into the gas protection chamber to ensure that the oxygen content in the gas protection chamber is lower than 150ppm;
(5) Introducing a laser heat source, synchronously starting a powder feeder to convey mixed powder to a laser heating area of 3D printing equipment, continuously lifting a forming process through a laser heat source processing head, scanning laser along a section slicing track of a CAD model of a part, depositing the synchronously conveyed mixed powder on a substrate, stacking layer by layer until printing is finished, and obtaining a block blank of high-specific-gravity energy-containing two-phase high-entropy alloy in a required shape on the substrate;
the 3D printing process parameters are as follows: the diameter of a laser spot is 6mm, the scanning speed of the laser spot is 15mm/s, the laser power is 1600W, the powder feeding rate is 2.5r/min, and the thickness of single-layer deposition is 2.4mm;
(6) Carrying out heat treatment on the block-shaped blank obtained in the step (5), namely carrying out water cooling after the block-shaped blank is treated at 800 ℃ for 8 hours to obtain the block-shaped blank with the density of 12.73g/cm 3 The high specific gravity energy-containing two-phase high-entropy alloy has a chemical formula of W 60 Ti 10 Zr 10 Nb 15 V 5 。
According to the morphology characterization result, in the SEM image, the light-color particles are a hard solid solution phase of W, the dark-color part is a solid solution matrix phase composed of Ti, zr, nb and V, and the hard solid solution phase and the solid solution matrix phase are uniformly distributed, have fine structures and are clear in two-phase interface.
Through quasi-static tensile test, W 60 Ti 10 Zr 10 Nb 15 V 5 The yield strength of (2) was 660MPa, the tensile strength was 930MPa, and the elongation was 3.9%. Through dynamic compression and energy release tests, W is known 60 Ti 10 Zr 10 Nb 15 V 5 The dynamic compression strength of the material is 1900MPa, the breaking strain is 46 percent, intense fire light is generated under dynamic loading, and the energy release threshold value is 4060s -1 。
Example 3
High-specific-gravity energy-containing two-phase high-entropy alloy Mo with dimensions of 30mm multiplied by 20mm multiplied by 10mm (length multiplied by width multiplied by thickness) prepared on the basis of laser instantaneous liquid phase sintering technology 60 Ti 10 Zr 10 Nb 10 Hf 10 The method comprises the following specific steps:
(1) The method comprises the following steps of mixing the metal simple substances of nearly spherical Mo, ti, zr, nb and Hf with the particle size of 5-25 mu m according to a ratio of 60:10:10:10: mixing the powder with the atomic ratio of 10 in a mixer for 400min, then drying in vacuum, and then loading into a powder storage tank of a powder feeder;
(2) Inputting corresponding data in control software for 3D printing based on the macroscopic size of the prepared high-specific-gravity energy-containing two-phase high-entropy alloy to complete CAD three-dimensional modeling and subsequently generate a program path for automatic laser forming;
(3) Placing the TC4 titanium alloy substrate into a gas protection chamber, fastening, and filling argon into the gas protection chamber to ensure that the oxygen content in the gas protection chamber is lower than 150ppm;
(4) Introducing a laser heat source, synchronously starting a powder feeder to convey mixed powder to a laser heating area of 3D printing equipment, continuously lifting a forming process through a laser heat source processing head, scanning laser along a section slicing track of a CAD model of a part, depositing the synchronously conveyed mixed powder on a substrate, stacking layer by layer until printing is finished, and obtaining a block blank of high-specific-gravity energy-containing two-phase high-entropy alloy in a required shape on the substrate;
the 3D printing process parameters are as follows: the diameter of a laser spot is 4mm, the scanning speed of the laser spot is 6mm/s, the laser power is 2800W, the powder feeding rate is 3r/min, and the single-layer deposition thickness is 1.8mm;
(5) Carrying out hot isostatic pressing treatment on the block-shaped green body obtained in the step (4), namely treating for 4 hours under the conditions that the pressure is 120MPa and the temperature is 1200 ℃, and obtaining the density of 9.52g/cm 3 The high specific gravity energetic biphase high entropy alloy has a chemical formula of Mo 60 Ti 10 Zr 10 Nb 10 Hf 10 。
According to the morphology characterization result, in the SEM image, the light-color particles are a hard solid solution phase of Mo, the dark-color part is a solid solution matrix phase composed of Ti, zr, nb and Hf, and the hard solid solution phase and the solid solution matrix phase are uniformly distributed, have fine structures and have clear two-phase interfaces.
Through quasi-static tensile test, mo 60 Ti 10 Zr 10 Nb 10 Hf 10 The yield strength of (D) was 790MPa, the tensile strength was 970MPa, and the elongation was 4.2%. Through dynamic compression and energy release tests, mo is proved 60 Ti 10 Zr 10 Nb 10 Hf 10 The dynamic compression strength of the material is 1980MPa, the breaking strain is 40 percent, obvious flame is generated under dynamic loading, and the energy release threshold value is 4800s -1 。
Example 4
High-specific-gravity energy-containing two-phase high-entropy alloy Mo with dimensions of 30mm multiplied by 20mm multiplied by 10mm (length multiplied by width multiplied by thickness) prepared on the basis of laser instantaneous liquid phase sintering technology 70 Ti 10 Zr 5 Nb 5 Ta 10 The method comprises the following specific steps:
(1) Under the protection of argon, according to the following ratio of 10:5:5: mixing the surface-treated Ti, zr, nb and Ta metal simple substances according to the atomic ratio of 10, alloying and smelting, after the mixed metal simple substances are completely melted into alloy liquid, preparing powder by a plasma spheroidization method, and screening to obtain TiZrNbTa alloy powder with the particle size of 45-150 mu m;
(2) The preparation method comprises the following steps of (1) mixing approximately spherical Mo elementary powder with the grain diameter of 5-25 mu m and TiZrNbTa alloy powder prepared in the step (1) according to the weight ratio of 70: mixing powder in a mixer for 360min at an atomic ratio of 30, vacuum drying, and then putting into a powder storage tank of a powder feeder;
(3) Inputting corresponding data in control software for 3D printing based on the macroscopic size of the prepared high-specific-gravity energy-containing two-phase high-entropy alloy to complete CAD three-dimensional modeling and subsequently generate a program path for automatic laser forming;
(4) Placing and fastening a TC4 titanium alloy substrate in a gas protection chamber, and filling argon into the gas protection chamber to ensure that the oxygen content in the gas protection chamber is lower than 150ppm;
(5) Introducing a laser heat source, synchronously starting a powder feeder to convey mixed powder to a laser heating area of 3D printing equipment, continuously lifting a forming process through a laser heat source processing head, scanning laser along a section slicing track of a CAD model of a part, depositing the synchronously conveyed mixed powder on a substrate, stacking layer by layer until printing is finished, and obtaining a block blank of high-specific-gravity energy-containing biphase high-entropy alloy with a required shape on the substrate;
the 3D printing process comprises the following parameters: the diameter of a laser spot is 3mm, the scanning speed of the laser spot is 30mm/s, the laser power is 2000W, the powder feeding rate is 2r/min, and the single-layer deposition thickness is 2.2mm;
(6) Carrying out hot isostatic pressing treatment on the block-shaped blank obtained in the step (5) and then carrying out heat treatment, wherein the pressure, the temperature and the time of the hot isostatic pressing treatment are respectively 170MPa, 1400 ℃ and 8h, and the temperature, the time and the cooling mode of the heat treatment are respectively 1100 ℃, 5h and air cooling, so that the density is 9.61g/cm 3 The high specific gravity energetic biphase high entropy alloy has a chemical formula of Mo 70 Ti 10 Zr 5 Nb 5 Ta 10 。
According to the appearance characterization result, in the SEM picture, the light-color particles are a hard solid solution phase of Mo, the dark-color part is a solid solution matrix phase consisting of Ti, zr, nb and Ta, and the hard solid solution phase and the solid solution matrix phase are uniformly distributed, have fine tissues and have clear two-phase interfaces.
Through quasi-static tensile test, mo 70 Ti 10 Zr 5 Nb 5 Ta 10 The yield strength of (A) was 850MPa, the tensile strength was 990MPa, and the elongation was 3.5%. Through dynamic compression and energy release tests, mo is proved 70 Ti 10 Zr 5 Nb 5 Ta 10 The dynamic compression strength of the material is 2060MPa, the breaking strain is 33 percent, the material generates fire light under the dynamic loading, and the energy release threshold value is 5200s -1 。
Example 5
High specific gravity energy-containing two-phase high-entropy alloy W with the size of 30mm multiplied by 20mm multiplied by 10mm (length multiplied by width multiplied by thickness) prepared based on laser instantaneous liquid phase sintering technology 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 The method comprises the following specific steps:
(1) Under the protection of argon, according to the following ratio of 10:5:5:5:5, mixing the surface-treated Ti, zr, V, nb and Al metal simple substances and carrying out alloying smelting, after the mixed metal simple substances are completely melted into alloy liquid, carrying out powder preparation by a gas atomization method and carrying out screening to obtain TiZrVNbAl alloy powder with the particle size of 45-150 mu m;
(2) The method comprises the following steps of mixing approximately spherical W elementary substance powder with the grain diameter of 5-25 mu m and TiZrVNbAl alloy powder prepared in the step (1) according to the weight ratio of 70: mixing powder in a mixer for 360min at an atomic ratio of 30, vacuum drying, and then putting into a powder storage tank of a powder feeder;
(3) Inputting corresponding data in control software for 3D printing based on the macroscopic size of the prepared high-specific-gravity energy-containing two-phase high-entropy alloy to complete CAD three-dimensional modeling and subsequently generate a program path for automatic laser forming;
(4) Placing and fastening a TC4 titanium alloy substrate in a gas protection chamber, and filling argon into the gas protection chamber to ensure that the oxygen content in the gas protection chamber is lower than 150ppm;
(5) Introducing a laser heat source, synchronously starting a powder feeder to convey mixed powder to a laser heating area of 3D printing equipment, continuously lifting a forming process through a laser heat source processing head, scanning laser along a section slicing track of a CAD model of a part, depositing the synchronously conveyed mixed powder on a substrate, stacking layer by layer until printing is finished, and obtaining a block blank of high-specific-gravity energy-containing two-phase high-entropy alloy in a required shape on the substrate;
the 3D printing process parameters are as follows: the diameter of a laser spot is 6mm, the scanning speed of the laser spot is 25mm/s, the laser power is 2500W, the powder feeding speed is 4.5r/min, and the single-layer deposition thickness is 3.8mm;
(6) Carrying out hot isostatic pressing treatment on the block-shaped green body obtained in the step (5), namely treating for 4 hours under the conditions of 140MPa of pressure and 1300 ℃ of temperature to obtain the block-shaped green body with the density of 14.72g/cm 3 The high specific gravity energetic biphase high entropy alloy has a chemical formula abbreviated as W 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 。
To W 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 By performing phase analysis, it can be seen from fig. 1 that the high-entropy alloy consists of a hard solid solution phase and a solid solution matrix phase, both BCC, without the remaining impurity phases.
To W 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 The morphology characterization is carried out, and as can be seen from fig. 2, the light-colored particles are a hard solid solution phase of W, the dark-colored part is a solid solution matrix phase composed of Ti, zr, nb, V and Al, the hard solid solution phase and the solid solution matrix phase are uniformly distributed, the structure is fine, and the two-phase interface is clear.
Through quasi-static tensile test, W 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 The yield strength of (A) was 990MPa, the tensile strength was 1230MPa, and the elongation was 3.7%, as shown in FIG. 3. Through dynamic compression and energy release tests, W is known 70 Ti 10 Zr 5 Nb 5 V 5 Al 5 The dynamic compression strength of the steel is 1980MPa, the breaking strain is 43 percent, and the steel generates violent flame under the dynamic loading, and the energy release threshold value of the steel is 4100 -1 As shown in fig. 4.
In summary, the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A high specific gravity energetic biphase high entropy alloy is characterized in that: the density of the hard solid solution phase of the A-type element and the solid solution matrix phase formed by the B, C element is more than or equal to 9.5g/cm 3 The energetic biphase high-entropy alloy has a chemical formula of A according to atomic percentage x B y C z Wherein, the A element contains one or two of W and Mo, x is more than or equal to 55 and less than or equal to 80, the B element contains three of Ti, zr and Nb, ti is more than or equal to 5 and less than or equal to 25,5 and less than or equal to 25,5 and less than or equal to Nb 25 and less than or equal to 15 and less than or equal to 35, the C element contains at least one of Al, V, ta, hf, co, mn, ni, cr, fe and B, z is more than or equal to 5 and less than or equal to 30, x + y + z =100.
2. A method for preparing the high specific gravity energetic dual-phase high entropy alloy as claimed in claim 1, characterized in that: the method specifically comprises the following steps of,
loading raw material powder into a powder storage tank of coaxial powder feeding laser additive manufacturing equipment, opening a laser heat source, synchronously starting to convey the raw material powder, scanning by laser according to a preset program path, obtaining a block blank body of the high-specific-gravity energy-containing biphase high-entropy alloy in a required shape on a substrate after printing is finished, and then performing post-treatment to improve the density and reduce the porosity of the block blank body to obtain the high-specific-gravity energy-containing biphase high-entropy alloy;
the raw material powder is a mixture of simple substance powder corresponding to A, B, C type elements, or a mixture of simple substance powder of A type elements and alloy powder consisting of B, C type elements; the post-treatment is heat treatment, or hot isostatic pressing treatment and heat treatment.
3. The preparation method of the high specific gravity energetic dual-phase high entropy alloy according to claim 2, characterized in that: the particle size of the raw material powder is between 5 and 150 mu m.
4. The preparation method of the high specific gravity energetic dual-phase high entropy alloy according to claim 2, characterized in that: the process parameters in the printing process are as follows: the diameter of a laser spot is 0.5-6 mm, the scanning speed is 5-30 mm/s, the laser power is 500-3000W, the powder feeding rate is 0.5-5 r/min, and the single-layer deposition thickness is 1-4 mm.
5. The method for preparing the high specific gravity energetic dual-phase high entropy alloy according to any one of claims 2 to 4, characterized in that: the temperature and time of the heat treatment are 700-1200 ℃ and 2-8 h respectively, and the pressure, temperature and time of the hot isostatic pressing are 100-180 MPa, 1000-1500 ℃ and 2-10 h respectively.
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