CN116240437B - High-density tungsten alloy with high adiabatic shear sensitivity and high plasticity and preparation method thereof - Google Patents
High-density tungsten alloy with high adiabatic shear sensitivity and high plasticity and preparation method thereof Download PDFInfo
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- 229910001080 W alloy Inorganic materials 0.000 title claims abstract description 132
- 230000035945 sensitivity Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000006104 solid solution Substances 0.000 claims abstract description 25
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 3
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 68
- 239000000843 powder Substances 0.000 claims description 57
- 239000011812 mixed powder Substances 0.000 claims description 56
- 238000005245 sintering Methods 0.000 claims description 39
- 239000000956 alloy Substances 0.000 claims description 37
- 229910045601 alloy Inorganic materials 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 34
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- 238000000137 annealing Methods 0.000 claims description 9
- 229910052721 tungsten Inorganic materials 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 40
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- 238000002844 melting Methods 0.000 description 14
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 8
- 238000011049 filling Methods 0.000 description 8
- 238000007789 sealing Methods 0.000 description 8
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- 229910052802 copper Inorganic materials 0.000 description 7
- 239000010949 copper Substances 0.000 description 7
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- 238000009689 gas atomisation Methods 0.000 description 7
- 238000000227 grinding Methods 0.000 description 7
- 230000001681 protective effect Effects 0.000 description 7
- 238000010008 shearing Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 229910020639 Co-Al Inorganic materials 0.000 description 4
- 229910020675 Co—Al Inorganic materials 0.000 description 4
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- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
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- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1035—Liquid phase sintering
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- C22C1/00—Making non-ferrous alloys
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
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Abstract
The invention relates to a high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity and a preparation method thereof, belonging to the technical field of high-density tungsten alloys. The tungsten alloy consists of W element, co element, al element, M element and N element according to a certain proportion, wherein the M element is at least one of Ni, fe, V, cr, ta and Nb, the N element is at least one of Y, V, mo, mn, hf and Ti, the microstructure structure of the tungsten alloy comprises W phase, gamma solid solution phase and L1 2 phase, the density is 17.5-18.4 g/cm 3, the quasi-static compression strength is above 1900MPa, the quasi-static compression elongation is above 20%, and the tungsten alloy shows adiabatic shear failure after dynamic compression, so that the tungsten alloy has high density, ultrahigh strength, high plasticity and excellent adiabatic shear sensitivity. The preparation process of the tungsten alloy is simple, is easy to operate, meets the requirement of large-scale production, and has good application prospect in the field of weapon industry.
Description
Technical Field
The invention relates to a high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity and a preparation method thereof, belonging to the technical field of high-density tungsten alloys.
Background
The high-density tungsten alloy generally refers to an alloy mainly comprising a tungsten phase of a BCC structure and a gamma solid solution phase of an FCC structure, and having a density of 16.5-19.0 g/cm 3, and the densities of the high-density tungsten alloys with different composition are different. The high-density tungsten alloy has great effect in weapon industry, especially in the aspect of armor piercing bullet core bar material because of its excellent characteristics of high density, high strength, no pollution to environment and the like.
However, the conventional tungsten alloy represented by the W-Ni-Fe alloy at present is easy to form a mushroom-shaped passivation warhead in the kinetic energy penetration process, so that energy loss is caused, and the penetration capacity of the tungsten alloy is limited. In order to improve the adiabatic shear sensitivity of the high-specific gravity tungsten alloy, means such as large deformation grain refinement are generally adopted, but the process is relatively complex and the lifting space is limited. For example, chinese patent CN115007645A (a method for improving the adiabatic shearing sensitivity of pure tungsten metal by crystal texture design, publication No. 2022-09-06) changes the initial crystal orientation of tungsten metal by large deformation, and improves the adiabatic shearing sensitivity of pure tungsten metal, but the method has high requirement on the plasticity of materials and has higher production difficulty.
The "self-sharpening" effect is a means commonly used at present to enhance the penetration ability of high specific gravity tungsten alloys. For example, chinese patent CN111283212A (a self-sharpening tungsten alloy material with a stripping structure, a preparation method and application thereof, publication No. 2020-06-16) discloses rolling bending and deforming a plate-type tungsten-nickel-iron alloy to obtain a deformed tungsten-nickel-iron alloy, and prepares the self-sharpening tungsten alloy material with the stripping structure, but does not obtain the self-sharpening effect from the material per se, and increases the processing cost to a certain extent.
Disclosure of Invention
Aiming at the problem that the existing high-specific gravity tungsten alloy is difficult to achieve the organic combination of high density, high strength and high heat insulation shearing performance, the invention provides the high-density tungsten alloy with high heat insulation shearing sensitivity and high strength and the preparation method thereof, the components of the high-specific gravity tungsten alloy are selected and the content of each component is optimized, so that the L1 2 phase with certain stability and certain content is separated out from the gamma solid solution phase, the tungsten alloy is ensured to have high density, ultrahigh strength, high plasticity and excellent heat insulation shearing sensitivity, the preparation process of the tungsten alloy is simple, the operation is easy, the requirement of large-scale production is met, and the tungsten alloy has good application prospect in the weapon industry field.
The aim of the invention is achieved by the following technical scheme.
A high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity is composed of W element, co element, al element, M element and N element according to the mass percentage of a:b:c:d:e, wherein M element is at least one of Ni, fe, V, cr, ta and Nb, N element is at least one of Y, V, mo, mn, hf and Ti, a is more than or equal to 90% and less than or equal to 95%, b is more than or equal to 1% and less than or equal to 8%, c is more than or equal to 0.5% and less than or equal to 4.5%, d is more than or equal to 0 and less than or equal to 3%, e is more than or equal to 0 and less than or equal to 3%, d+e is less than b, and a+b+c+d+e=100%. The microstructure of the tungsten alloy comprises a W phase, a gamma solid solution phase and an L1 2 phase, the density is 17.5-18.4 g/cm 3, the quasi-static compression strength is above 1900MPa, the quasi-static compression elongation is above 20%, and the microstructure shows adiabatic shear failure after dynamic compression.
Preferably, the M element is at least one of Ni, fe, and Ta, and the N element is one or both of Hf and Ti.
Preferably, 90% or less a or less than 95%,3% or less b or less than 7%,0.5% or less c or less than 3%, 0% or less d or less than 2.5%, 0% or less e or less than 2.5%, and d+e < b, a+b+c+d+e=100%.
The preparation method of the high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity comprises the following steps:
(1) Uniformly mixing the elemental powder corresponding to each element, or uniformly mixing the W elemental powder and CoAlMN alloy powder to obtain mixed powder;
(2) Carrying out liquid phase sintering on the mixed powder to obtain a sintered body;
(3) And (3) annealing or hot isostatic pressing the sintered body to obtain the tungsten alloy.
In the step (1), after weighing the raw material powder, uniformly mixing for 4-24 hours at the rotating speed of 30-600 r/min under the protection of inert gas, and then placing the mixture in a vacuum drying oven at the temperature of 100-180 ℃ for vacuum drying for 2-8 hours to obtain mixed powder.
In the step (2), a sintered body may be prepared by a conventional liquid phase sintering process or a laser transient liquid phase sintering process. The traditional liquid phase sintering process uses a box-type high-temperature sintering furnace, firstly heats to 700-1000 ℃ at a temperature rising rate of 5-20 ℃ per minute and keeps the temperature for 60-120 min, then heats to 1300-1700 ℃ at a temperature rising rate of 2-20 ℃ per minute and keeps the temperature for 0-120 h, and finally obtains a sintered body after cooling. The laser transient liquid phase sintering process takes laser as a heat source, only melts a matrix in a micro molten pool, and simultaneously keeps most of tungsten particles in the molten pool from melting, so that ultra-short-time liquid phase sintering is realized.
In the step (3), the annealing temperature of the annealing treatment is 500-1100 ℃ and the annealing time is 2-24 hours, and the temperature of the hot isostatic pressing treatment is 800-1500 ℃, the pressure is 80-230 MPa and the time is 2-24 hours.
The beneficial effects are that:
(1) According to the tungsten alloy disclosed by the invention, the W element is introduced into the matrix, and through element proportion regulation and control, the W element is combined with other elements in the matrix phase to generate Co 3 (Al, W) which is an L1 2 type precipitated phase, so that the high density and high strength of the tungsten alloy are ensured on the premise of avoiding alloy embrittlement.
(2) The L1 2 phase is introduced into the tungsten alloy, and the tungsten alloy has high adiabatic shear sensitivity and has the capability of shearing self-sharpening by utilizing the characteristic of pyrolysis of the L1 2 phase.
(3) The tungsten alloy can regulate and control the content of intermetallic compounds in the alloy by regulating the types and the content of M, N elements, thereby better regulating and controlling the properties of the alloy such as mechanical property, density, adiabatic shear sensitivity and the like. When M, N elements are not added, the precipitated phases in the tungsten alloy are fewer, the strength is lower, and when M, N elements are excessively added, the variety and the content of intermetallic compounds in the tungsten alloy are changed, so that the plasticity and the adiabatic shear sensitivity of the tungsten alloy are not facilitated.
(4) In the preparation process of the tungsten alloy, the traditional liquid phase sintering and the laser transient liquid phase sintering are adopted, so that the coordination between W particle size control and W-W connectivity control can be effectively realized, various performance indexes of the tungsten alloy are ensured, the content and the form of a precipitated phase can be effectively regulated and controlled through subsequent heat treatment, and the performance of the alloy is ensured.
(5) The tungsten alloy provided by the invention has the advantages of high density, ultrahigh strength, high plasticity, excellent adiabatic shear sensitivity, simple preparation process, high production efficiency, easiness in industrial production and good application prospect in the field of weapon industry.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by conventional liquid phase sintering techniques of example 1.
FIG. 2 is a Scanning Electron Microscope (SEM) image of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared according to conventional liquid phase sintering techniques of example 1.
Fig. 3 is a partial magnified scanning electron microscope image of the L1 2 phase in fig. 2.
FIG. 4 is a quasi-static compressive stress-strain curve of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by conventional liquid phase sintering techniques of example 1.
FIG. 5 is an X-ray diffraction pattern of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by laser transient liquid phase sintering technique of example 4.
FIG. 6 is a scanning electron microscope image of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by laser transient liquid phase sintering technique of example 4.
Fig. 7 is a partial magnified scanning electron microscope image of the L1 2 phase in fig. 6.
FIG. 8 is a quasi-static compressive stress-strain curve of the 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by laser transient liquid phase sintering technique of example 4.
FIG. 9 is a dynamic compressive true stress-strain curve of a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy prepared by laser transient liquid phase sintering technique of example 4.
Detailed Description
The present invention will be further described with reference to the following detailed description, wherein the processes are conventional, and wherein the starting materials are commercially available from the open market, unless otherwise specified.
Performance testing and structural characterization:
(1) Measuring density, namely measuring the density of the tungsten alloy by adopting a DT-100 precise balance according to the standard GB-5365-2005, wherein the size of a sample is phi 4mm multiplied by 4mm;
(2) The phase analysis is carried out by adopting a D8 advanced X-ray diffractometer of Bruker AXS company, the working voltage and the current are respectively 40kV and 40mA, the X-ray source is CuK alpha (lambda= 0.1542 nm) rays, the scanning speed is 0.2sec/step, the scanning step length is 0.02 DEG/step, and the scanning range is 20 DEG-100 DEG;
(3) Performing appearance observation, namely performing microscopic appearance characterization by adopting a REGULUS 8230 cold field emission scanning electron microscope of Japanese Hitachi, and performing back scattering electron imaging, wherein the working voltage is 10-25 kV;
(4) Dynamic compression test, namely testing the room-temperature axial dynamic compression mechanical property of the tungsten alloy by adopting a split Hopkins compression bar (SHPB) according to a standard GJB-5365-2005, wherein the size of a sample is phi 4 multiplied by 4mm, and the strain rate is 10 3s-1;
(5) And (3) testing the room-temperature axial quasi-static compression mechanical property of the tungsten alloy by using INSTRON5582 equipment according to standard GB/T7314-2017, wherein the size of a sample is phi 4 multiplied by 6mm, and the strain rate is 10 -3s-1.
Example 1
The specific steps for preparing the 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co, al, ta and Ti with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Ta to Ti=40:5:3:2, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder preparation furnace according to the sequence of the melting point of the mixed raw materials from low to high, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, taking argon as an atomization medium after the alloy is completely melted into alloy liquid, atomizing the alloy liquid under the conditions of heating power of 160kW and atomization air pressure of 4MPa, and obtaining Co-Al-Ta-Ti pre-alloy powder with particle size of 38-150 mu m through vacuum sieving equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 95:5 from spherical W powder with the particle size of 15-25 mu m to Co-Al-Ta-Ti prealloy powder prepared in the step (1), putting the mixed powder into a cleaned and blow-dried V-shaped powder mixer, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying oven for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 150MPa, maintaining pressure for 25min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 900 ℃ according to the heating rate of 20 ℃ per min, preserving heat for 120min, heating to 1600 ℃ according to the heating rate of 10 ℃ per min, preserving heat for 12h, and cooling to obtain a sintered body;
(4) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at 900 ℃ and 120MPa to obtain the tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2 Ti.
The density of the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy is 17.6g/cm 3.
The prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy was subjected to phase analysis, and as can be seen from the XRD spectrum of FIG. 1, the tungsten alloy consisted mainly of W phase and gamma solid solution phase, and contained a small amount of L1 2 phase and Co 7W6 phase.
Microscopic morphology observation of the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy shows that the light-colored W phase is uniformly distributed in the dark-colored gamma solid solution phase to form a large number of two-phase interfaces, and the nano-sized L1 2 phase is also present in the gamma solid solution phase (as shown in FIG. 3). The addition of Ta and Ti can well improve the content of the L1 2 phase, so that more L1 2 phases participate in improving the adiabatic shear sensitivity, the adiabatic shear sensitivity of the tungsten alloy is improved, meanwhile, the addition of Ta and Ti also plays a good solid solution strengthening role, and the mechanical property of the tungsten alloy is improved. In addition, high levels of W lead to Co 7W6 phases in the tungsten alloy, which can further enhance the adiabatic shear sensitivity, but at the expense of the plasticity of the tungsten alloy to some extent.
The prepared tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2Ti is subjected to a quasi-static compression experiment, and the test result of FIG. 4 shows that the compressive strength of the tungsten alloy is 2200MPa, and the fracture deformation amount is 34%.
Dynamic compression experiments were performed on the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy that exhibited adiabatic shear failure.
Example 2
The specific steps for preparing the 90W-8Co-1.5Al-0.3Ta-0.2Ti tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Mixing W, co, al, ta with purity not less than 99.99% and Ti simple substance powder according to the mass ratio of 90:8:1.5:0.3:0.2, weighing 1000+/-0.01 g of mixed powder, pouring into a V-shaped powder mixer which is cleaned and dried, mixing for 24 hours at the speed of 300r/min, and then vacuum drying for 4 hours in a 130 ℃ vacuum drying box to obtain uniformly mixed and dried mixed powder, wherein the particle size of the W simple substance powder is not more than 15 mu m, and the particle size of other metal simple substance powder is not more than 38 mu m;
(2) Placing the mixed powder obtained in the step (1) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 170MPa, maintaining pressure for 75min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 900 ℃ according to the heating rate of 20 ℃ per min, preserving heat for 120min, heating to 1600 ℃ according to the heating rate of 10 ℃ per min, preserving heat for 24h, and cooling to obtain a sintered body;
(3) The sintered body was hot isostatic pressed for 10h at 1000 ℃ and 120MPa, 90W-8Co-1.5Al-0.3Ta-0.2Ti tungsten alloy.
The density of the prepared 90W-8Co-1.5Al-0.3Ta-0.2Ti tungsten alloy is 17.1g/cm 3.
Microscopic morphology observation is carried out on the prepared 90W-8Co-1.5Al-0.3Ta-0.2Ti tungsten alloy, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, and a micron-sized L1 2 phase is precipitated in the gamma solid solution phase.
Dynamic compression experiments were performed on the prepared 90W-8Co-1.5Al-0.3Ta-0.2Ti tungsten alloy that exhibited adiabatic shear failure.
Example 3
The specific steps for preparing the 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Mixing W, co, al, ta with Ti simple substance powder with purity not less than 99.99% according to the mass ratio of 95:4:0.5:0.3:0.2, weighing 1000+/-0.01 g of mixed powder, pouring into a V-shaped powder mixer which is cleaned and dried, mixing for 24 hours at the speed of 300r/min, and then vacuum drying for 4 hours in a 130 ℃ vacuum drying box to obtain uniformly mixed and dried mixed powder, wherein the particle size of the W simple substance powder is not more than 15 mu m, and the particle size of other metal simple substance powder is not more than 38 mu m;
(2) Placing the mixed powder obtained in the step (1) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 200MPa, maintaining pressure for 75min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 900 ℃ according to the heating rate of 20 ℃ per min, preserving heat for 120min, heating to 1600 ℃ according to the heating rate of 10 ℃ per min, preserving heat for 24h, and cooling to obtain a sintered body;
(3) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at the temperature of 1000 ℃ and the pressure of 120MPa to obtain the tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2 Ti.
The density of the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy is 17.7g/cm 3.
Microscopic morphology observation is carried out on the prepared tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2Ti, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, and a micron-sized L1 2 phase is precipitated in the gamma solid solution phase.
Dynamic compression experiments were performed on the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy that exhibited adiabatic shear failure.
Example 4
The specific steps for preparing the 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy by the laser transient liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co, al, ta and Ti with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Ta to Ti=40:5:3:2, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder preparation furnace according to the sequence of the melting point of the mixed raw materials from low to high, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, taking argon as an atomization medium after the alloy is completely melted into alloy liquid, atomizing the alloy liquid under the conditions of heating power of 160kW and atomization air pressure of 4MPa, and obtaining Co-Al-Ta-Ti pre-alloy powder with particle size of 38-150 mu m through vacuum sieving equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 95:5 from spherical W powder with the particle size of 15-25 mu m to Co-Al-Ta-Ti prealloy powder prepared in the step (1), putting the mixed powder into a cleaned and blow-dried V-shaped powder mixer, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying oven for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Filling the mixed powder obtained in the step (2) into a powder tank of a laser transient liquid phase sintering device, setting laser power to 1800W, scanning speed to 900mm/min, powder feeding speed to 28g/min, scanning interval to 2.0mm and lifting to 0.35mm, and preparing a sintered body by taking laser as a heat source;
(4) The sintered body was annealed at 700℃for 10 hours to obtain a 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy.
The density of the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy is 17.4g/cm 3.
The prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy was subjected to phase analysis, and as can be seen from the XRD spectrum of FIG. 5, the tungsten alloy consisted mainly of W phase and gamma solid solution phase, while also containing a small amount of L1 2 phase.
Microscopic morphology observation was performed on the prepared 95W-4Co-0.5Al-0.3Ta-0.2Ti tungsten alloy, and as can be seen from the SEM image of FIG. 6, the light-colored W phase is uniformly distributed in the dark-colored gamma solid solution phase to form a large number of two-phase interfaces, and the L1 2 phase with the size of 100 nanometers exists in the gamma solid solution of the tungsten alloy (as shown in FIG. 7).
The prepared tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2Ti is subjected to a quasi-static compression experiment, and the test result of FIG. 8 shows that the compressive strength of the tungsten alloy is 2400MPa, and the fracture deformation amount is 25%.
The dynamic compression experiment is carried out on the prepared tungsten alloy of 95W-4Co-0.5Al-0.3Ta-0.2Ti, and the test result of FIG. 9 shows that the dynamic compression strength of the tungsten alloy is 2750MPa, and the fracture strain is 20%. After dynamic compression testing, adiabatic shear failure was exhibited.
Example 5
The specific steps for preparing the 93W-3.5Co-3Hf-0.5Al tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co, hf and Al with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Hf to Al=35 to 30 to 5, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder preparation furnace according to the sequence from low melting point to high melting point, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, completely melting the alloy into alloy liquid, atomizing the alloy liquid with argon as an atomizing medium under the heating power of 150kW and the atomizing air pressure of 4MPa, and obtaining Co-Hf-Al prealloy powder with particle size not more than 38 mu m through vacuum screening equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 93:7 from spherical W powder with the particle size of not more than 15 mu m to Co-Hf-Al prealloy powder prepared in the step (1), putting the mixed powder into a V-shaped powder mixer which is cleaned and dried, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying box for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 150MPa, maintaining pressure for 75min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 850 ℃ according to the heating rate of 20 ℃ per min, preserving heat for 120min, heating to 1500 ℃ according to the heating rate of 10 ℃ per min, preserving heat for 16h, and cooling to obtain a sintered body;
(4) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at 900 ℃ and 120MPa to obtain the 93W-3.5Co-3Hf-0.5Al tungsten alloy.
As shown by the test, the density of the prepared 93W-3.5Co-3Hf-0.5Al tungsten alloy is 17.5g/cm 3.
Microscopic morphology observation is carried out on the prepared 93W-3.5Co-3Hf-0.5Al tungsten alloy, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, wherein a small amount of L1 2 phase is precipitated in the gamma solid solution. The addition of Hf effectively increases the L1 2 phase through alloying, and meanwhile, the addition of Hf obviously improves the adiabatic shear sensitivity of the tungsten alloy.
Dynamic compression experiments were performed on the prepared 93W-3.5Co-3Hf-0.5Al tungsten alloy, which exhibited adiabatic shear failure.
Example 6
The specific steps for preparing the 93W-3.5Co-3Fe-0.5Al tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co, fe and Al with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Fe to Al=35:30:5, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder preparation furnace according to the sequence from low melting point to high melting point, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, completely melting the alloy into alloy liquid, atomizing the alloy liquid with argon as an atomizing medium under the heating power of 150kW and the atomizing air pressure of 4MPa, and obtaining Co-Fe-Al prealloy powder with particle size not more than 38 mu m through vacuum sieving equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 93:7 from spherical W powder with the particle size of not more than 15 mu m to Co-Fe-Al prealloy powder prepared in the step (1), putting the mixed powder into a V-shaped powder mixer which is cleaned and dried, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying box for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 100MPa, maintaining pressure for 120min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 850 ℃ at a heating rate of 30 ℃ per min, preserving heat for 120min, heating to 1500 ℃ at a heating rate of 10 ℃ per min, preserving heat for 16h, and cooling to obtain a sintered body;
(4) The sintered body was hot isostatic pressed for 10 hours at 900 ℃ and 120MPa to obtain 93W-3.5Co-3Fe-0.5Al tungsten alloy.
As a result of the test, the density of the prepared 93W-3.5Co-3Fe-0.5Al tungsten alloy was 17.5g/cm 3.
Microscopic morphology observation is carried out on the prepared 93W-3.5Co-3Fe-0.5Al tungsten alloy, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, and a small amount of L1 2 phase is washed out from the gamma solid solution.
Dynamic compression experiments were performed on the prepared 93W-3.5Co-3Fe-0.5Al tungsten alloy, which exhibited adiabatic shear failure.
Example 7
The specific steps for preparing the 90W-8Co-2Al tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co and Al with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Al=8:2, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder making furnace according to the sequence from low melting point to high melting point, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, taking argon as an atomization medium after the alloy is completely melted into alloy liquid, pulverizing the alloy liquid under the conditions that the heating power is 150kW and the atomization pressure is 4MPa, and obtaining Co-Al prealloy powder with particle size not more than 38 mu m through vacuum screening equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 90:10 from spherical W powder with the particle size of not more than 15 mu m to Co-Al prealloy powder prepared in the step (1), putting the mixed powder into a V-shaped powder mixer which is cleaned and dried, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying box for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 100MPa, maintaining pressure for 120min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 850 ℃ at a heating rate of 30 ℃ per min, preserving heat for 120min, heating to 1500 ℃ at a heating rate of 10 ℃ per min, preserving heat for 16h, and cooling to obtain a sintered body;
(4) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at 900 ℃ and 120MPa to obtain the 90W-8Co-2Al tungsten alloy.
The density of the prepared 90W-8Co-2Al tungsten alloy is 17.7g/cm 3.
Microscopic morphology observation is carried out on the prepared 90W-8Co-2Al tungsten alloy, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, wherein a small amount of L1 2 phase is precipitated in the gamma solid solution phase.
Dynamic compression experiments were performed on the prepared 90W-8Co-2Al tungsten alloy, and it was found that the tungsten alloy exhibited adiabatic shear failure.
Comparative example 1
The specific steps for preparing the 90W-5Co-5Al tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co and Al with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Al=5 to 5, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder making furnace according to the sequence from low melting point to high melting point, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, taking argon as an atomization medium after the alloy is completely melted into alloy liquid, pulverizing the alloy liquid under the conditions that the heating power is 150kW and the atomization pressure is 4MPa, and obtaining Co-Al prealloy powder with particle size not more than 38 mu m through vacuum screening equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 90:10 from spherical W powder with the particle size of not more than 15 mu m to Co-Al prealloy powder prepared in the step (1), putting the mixed powder into a V-shaped powder mixer which is cleaned and dried, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying box for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 100MPa, maintaining pressure for 120min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 850 ℃ at a heating rate of 30 ℃ per min, preserving heat for 120min, heating to 1500 ℃ at a heating rate of 10 ℃ per min, preserving heat for 16h, and cooling to obtain a sintered body;
(4) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at 900 ℃ and 120MPa to obtain the 90W-5Co-5Al tungsten alloy.
The density of the prepared 90W-5Co-5Al tungsten alloy is 17.7g/cm 3 through testing.
Microscopic morphology observation is carried out on the prepared 90W-5Co-5Al tungsten alloy, and the tungsten alloy is mainly composed of a W phase and a gamma solid solution phase, and a large amount of L1 2 phases are precipitated in the gamma solid solution phase.
Dynamic compression experiments are carried out on the prepared 90W-5Co-5Al tungsten alloy, and the tungsten alloy is found to be in an upsetting form and has no adiabatic shearing fracture.
Comparative example 2
The specific steps for preparing the 90W-4Co-0.5Al-3.5Ta-2Ti tungsten alloy by the traditional liquid phase sintering process are as follows:
(1) Grinding, cleaning and drying pure metal blocks of Co, al, ta and Ti with purity not less than 99.7%, weighing mixed raw materials with total mass of 2000+/-0.01 g according to the mass ratio of Co to Ta to Ti=40 to 5 to 35 to 20, sequentially placing the weighed mixed raw materials into a water-cooled copper crucible of a vacuum gas atomization powder preparation furnace according to the sequence of the melting point of the mixed raw materials from low to high, vacuumizing until the vacuum degree in the furnace reaches 3×10 -3 Pa, filling high-purity argon as protective gas, alloying and smelting, taking argon as an atomization medium after the alloy is completely melted into alloy liquid, atomizing the alloy liquid under the conditions of heating power of 160kW and atomization air pressure of 4MPa, and obtaining Co-Al-Ta-Ti pre-alloy powder with particle size of 38-150 mu m through vacuum sieving equipment;
(2) Weighing mixed powder with the total mass of 1000+/-0.01 g according to the mass ratio of 9:1 by using spherical W powder with the particle size of 15-25 mu m and the Co-Al-Ta-Ti pre-alloy powder prepared in the step (1), putting the mixed powder into a cleaned and dried V-shaped powder mixer, mixing the mixed powder for 24 hours at the speed of 300r/min, and then placing the mixed powder into a 130 ℃ vacuum drying oven for vacuum drying for 4 hours to obtain uniformly mixed and dried mixed powder;
(3) Placing the mixed powder obtained in the step (2) into a cold isostatic pressing die with phi of 20mm multiplied by 180mm, sealing, placing into a cold isostatic pressing machine, pressurizing to 150MPa, maintaining pressure for 25min, taking out, cleaning and demolding to obtain a pressed compact, placing the pressed compact into a crucible filled with alumina particles, placing into a box-type high-temperature sintering furnace, heating to 900 ℃ according to the heating rate of 20 ℃ per min, preserving heat for 120min, heating to 1600 ℃ according to the heating rate of 10 ℃ per min, preserving heat for 12h, and cooling to obtain a sintered body;
(4) And carrying out hot isostatic pressing treatment on the sintered body for 10 hours at 900 ℃ and 120MPa to obtain the 90W-4Co-0.5Al-3.5Ta-2Ti tungsten alloy.
The density of the prepared 90W-4Co-0.5Al-3.5Ta-2Ti tungsten alloy is 17.2g/cm 3.
The phase analysis is carried out on the prepared 90W-4Co-0.5Al-3.5Ta-2Ti tungsten alloy, the tungsten alloy mainly comprises a W phase and a gamma solid solution phase, a large amount of Co 3 W phase appears in an alloy matrix, and no L1 2 phase is separated out.
Because the tungsten alloy has poor strength and plasticity, the quasi-static mechanical property test and the dynamic mechanical property test cannot be completed.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity is characterized by comprising W element, co element, al element, M element and N element according to the mass percentage of a, b, c, d, e, wherein M element is at least one of Ni, fe, V, cr, ta and Nb, N element is at least one of Y, V, mo, mn, hf and Ti, a is not less than 90% and not more than 95%, b is not less than 1% and not more than 8%, c is not less than 0.5% and not more than 4.5%, d is not less than 0 and not more than 3%, e is not more than 0 and not more than 3%, d+e is less than 2, a+b+c+d+e=100%, and the microstructure of the tungsten alloy comprises W phase, gamma solid solution phase and L1 2 phase;
The preparation method of the high-density tungsten alloy specifically comprises the following steps:
(1) Uniformly mixing the elemental powder corresponding to each element, or uniformly mixing the W elemental powder and CoAlMN alloy powder to obtain mixed powder;
(2) Carrying out liquid phase sintering on the mixed powder to obtain a sintered body;
(3) And (3) annealing or hot isostatic pressing the sintered body to obtain the tungsten alloy.
2. The high-density tungsten alloy with high thermal insulation and shear sensitivity and high plasticity according to claim 1, wherein M is at least one of Ni, fe and Ta, and N is one or both of Hf and Ti.
3. A high density tungsten alloy having high adiabatic shear sensitivity and high plasticity as claimed in claim 1 or 2, wherein a is 90% or less than 95%, b is 3% or less than 7%, c is 0.5% or less than 3%, d is 0 or less than 2.5%, e is 0 or less than 2.5%, and d+e < b, a+b+c+d+e=100%.
4. A method for producing a high-density tungsten alloy having high adiabatic shear sensitivity and high plasticity as claimed in any one of claims 1 to 3, comprising the steps of:
(1) Uniformly mixing the elemental powder corresponding to each element, or uniformly mixing the W elemental powder and CoAlMN alloy powder to obtain mixed powder;
(2) Carrying out liquid phase sintering on the mixed powder to obtain a sintered body;
(3) And (3) annealing or hot isostatic pressing the sintered body to obtain the tungsten alloy.
5. The method for preparing the high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity, which is characterized in that in the step (1), after weighing all raw material powder, uniformly mixing for 4-24 hours at the rotating speed of 30-600 r/min under the protection of inert gas, and then placing the mixture in a vacuum drying oven at the temperature of 100-180 ℃ for vacuum drying for 2-8 hours to obtain mixed powder.
6. The method for preparing the high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity according to claim 4, wherein in the step (2), a traditional liquid phase sintering process is adopted to prepare a sintered body, the specific process conditions are that a box-type high-temperature sintering furnace is selected, the temperature is firstly increased to 700-1000 ℃ at a temperature increasing rate of 5-20 ℃ per minute and is kept for 60-120 min, then the temperature is increased to 1300-1700 ℃ at a temperature increasing rate of 2-20 ℃ per minute and is kept for 0-120 h, and the sintered body is obtained after cooling.
7. The method for preparing the high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity according to claim 4, wherein in the step (2), a laser transient liquid phase sintering process is adopted to prepare a sintered body, and the specific process conditions are that the laser power is 800-2000W, the scanning speed is 300-1500 mm/min, the powder feeding speed is 15-45 g/min, the scanning interval is 1.0-3.0 mm, and the elevation is 0.1-0.5 mm.
8. The method of claim 4, wherein in the step (3), the annealing temperature of the annealing treatment is 500-1100 ℃ and the annealing time is 2-24 h.
9. The method for preparing a high-density tungsten alloy with high adiabatic shear sensitivity and high plasticity according to claim 4, wherein in the step (3), the temperature of the hot isostatic pressing treatment is 800-1500 ℃, the pressure is 80-230 MPa, and the time is 2-24 hours.
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