CN114657431A - Energetic tungsten alloy material and preparation method thereof - Google Patents
Energetic tungsten alloy material and preparation method thereof Download PDFInfo
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- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
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- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F3/1035—Liquid phase sintering
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- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
- B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
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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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
The invention provides an energetic tungsten alloy material and a preparation method thereof, wherein the energetic tungsten alloy material comprises the following components in percentage by mass: 80-95% of tungsten and 5-20% of other elements; wherein, the other elements are one or more of rhenium, molybdenum, niobium, hafnium, cobalt, manganese, zirconium, ytterbium and cerium. The energy-containing tungsten alloy material is obtained by optimally designing the alloy components, can be applied to the traditional small-caliber composite armor-piercing bullet core material, and has ideal effects of energy content, frangibility and secondary damage in the striking process; according to the invention, through hot isostatic pressing treatment and deformation strengthening treatment, the prepared energetic tungsten alloy material has energetic characteristics and simultaneously has high-strength and high-toughness armor piercing capability.
Description
Technical Field
The invention belongs to the technical field of refractory metals, and particularly relates to an energetic tungsten alloy material and a preparation method thereof.
Background
Tungsten alloys are widely used in military and civil industries due to their excellent properties of high strength, high hardness, high ductility, good processability, etc. Especially in the field of national defense industry, the armor-piercing core material is often applied to various antitanks and air-bound missile systems. With the continuous development and progress of science and technology and the continuous upgrading of military industrial equipment, the modern war has raised higher requirements on the killing power or damage efficiency of the warhead. Therefore, the material demand is gradually converted from single kinetic energy demand to functional demand, and the material is required to have the function of hitting targets in the fighting process and simultaneously have multilayer damage effects of damaging target personnel, electronic components, explosives and the like.
The traditional armor piercing bullet and armor breaking bullet mostly adopt conventional tungsten alloy as armor piercing main body materials, although the traditional armor piercing bullet and armor breaking bullet have better penetrating and penetrating capabilities, the armor piercing aftereffect is small, and the explosive damage effect is difficult to form. In recent years, in order to increase the after-effect and multi-layer damage effect of the material armor piercing, researchers have developed a new approach in the direction of material research with the after-effect of damage. At present, the heat value is often taken as one of important indexes for evaluating energetic materials, the heat value can represent the capability of the materials for releasing heat under the conditions of high temperature and high pressure, and theoretically, the higher the heat value is, the better the after-effect and explosive damage effect of the armor piercing bullet made of tungsten alloy are. The heat value of pure tungsten is about 4606J/g, and the heat value is improved to a limited extent by the addition elements (mainly Ni and Fe elements) in the traditional high specific gravity tungsten alloy.
Therefore, the patent develops research around optimization of components and processes to improve the energy-release heat value of the material as an entry point, invents the energy-containing tungsten alloy material, and can enhance the after-effect of nail penetration while meeting the nail penetration capability. The requirement of the novel battle component on the material is further met, and reference is provided for the subsequent research and development of the material.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an energy-containing tungsten alloy material and a preparation method thereof. The energy-containing tungsten alloy material is obtained by optimally designing the alloy components, can be applied to the traditional small-caliber composite armor-piercing bullet core material, and has ideal effects of energy content, frangibility and secondary damage in the striking process; according to the invention, through hot isostatic pressing treatment and deformation strengthening treatment, the prepared energetic tungsten alloy material has energetic characteristics and simultaneously has high-strength and high-toughness armor piercing capability.
In order to achieve the above object, a first aspect of the present invention provides an energetic tungsten alloy material, which adopts the following technical scheme:
an energetic tungsten alloy material comprises the following components in percentage by mass: 80-95% (such as 82%, 85%, 87%, 90%, 92%, 94%) of tungsten (W) and 5-20% (such as 6%, 8%, 10%, 13%, 15%, 18%) of other elements;
wherein the other elements are one or more of rhenium (Re), molybdenum (Mo), niobium (Nb), hafnium (Hf), cobalt (Co), manganese (Mn), zirconium (Zr), ytterbium (Yb) and cerium (Ce).
In the energy-containing tungsten alloy material, as a preferred embodiment, the energy-containing tungsten alloy material further includes one or two of nickel (Ni) and iron (Fe) among the other elements.
In the energy-containing tungsten alloy material, tungsten is an alloy matrix phase, and the mass percent of tungsten in the tungsten alloy material is 80% -95%, so that the properties of the material, such as armor piercing, striking inertia and the like, are the most important, if the mass percent of tungsten exceeds 95%, the properties of the prepared energy-containing tungsten alloy material are unstable, and if the mass percent of tungsten is lower than 80%, the density of the prepared energy-containing tungsten alloy material cannot meet the requirements; among other elements, the elements Re, Mo, Nb, Zr and Hf are refractory metal elements together with tungsten, so that the yield strength of the tungsten alloy material can be improved, and the heat value can be improved; ni, Fe, Co and Mn are the most common binder phase components in the existing high-specific gravity tungsten alloy, and the basic properties of the tungsten alloy such as strength, toughness and the like are ensured by adding the elements; in the invention, Yb and Ce are lanthanide metals and are added as trace elements, so that the energetic characteristics of the tungsten alloy material can be improved.
The invention provides a preparation method of an energetic tungsten alloy material, which comprises the following steps:
weighing tungsten powder and other element powder according to the component proportion of the energetic tungsten alloy material, and performing high-energy ball milling treatment to obtain tungsten alloy powder; then, the screening treatment, the press forming treatment, the liquid phase sintering treatment, the vacuum heat treatment and the low-temperature continuous rolling treatment are sequentially carried out.
In the above production method, as a preferred embodiment, hot isostatic pressing treatment is performed after the liquid-phase sintering treatment and before vacuum heat treatment; preferably, the hot isostatic pressing treatment pressure is 100-150 MPa (such as 105MPa, 110MPa, 120MPa, 125MPa, 130MPa and 140MPa), the temperature is 1300-1500 ℃ (such as 1350 ℃, 1400 ℃, 1420 ℃, 1450 ℃, 1460 ℃, 1470 ℃, 1480 ℃ and 1495 ℃), and the heat and pressure holding time is 0.5-3 h (such as 1h, 1.5h, 2h and 2.5 h); preferably, the pressurized medium of the hot isostatic pressing treatment is an inert gas; more preferably, the pressurizing medium for hot isostatic pressing is nitrogen or argon.
The principle and the advantages of the preparation method of the energetic tungsten alloy material are as follows: and activating the mixed powder in a high-energy ball milling mode to enhance the sintering activation energy of the material. Sintering in a hydrogen environment to obtain a rapidly densified sintering blank, and then reprocessing the sintering blank by using a hot isostatic pressing process to further consolidate the sintering effect. The preparation process is beneficial to material sintering densification, ensures that the alloy obtains special performance and simultaneously better improves the performance in subsequent processing treatment. In order to further improve the mechanical property of the material, the material is subjected to deformation strengthening treatment by adopting a low-temperature continuous rolling mode, and has good dynamic stretching and armor piercing properties while considering the energy-containing explosion characteristics.
The principle of hot isostatic pressing treatment after liquid phase sintering treatment and before vacuum heat treatment in the invention is as follows: the sintering effect is enhanced, and the densification degree of the material is further improved. If the material is densified as desired (relative density of 95% or more) by the liquid phase sintering process, the hot isostatic pressing process can be omitted.
In the above production method, as a preferred embodiment, the tungsten powder is industrial tungsten powder having a fisher's particle size of 2.0 to 4.0 μm (e.g., 2.1 μm, 2.2 μm, 2.4 μm, 2.5 μm, 2.6 μm, 2.8 μm, 3.0 μm, 3.2 μm, 3.4 μm, 3.5 μm, 3.6 μm, 3.7 μm, 3.8 μm, 3.9 μm), and among the other element powders, the nickel powder is electrolytic nickel powder or carbonyl nickel powder, the iron powder is electrolytic iron powder or carbonyl iron powder, the molybdenum, rhenium, niobium, cobalt powder, and manganese powder are industrial powders, the hafnium, zirconium hydride powder is hafnium hydride powder, zirconium hydride powder, and the ytterbium, cerium hydride powder is laboratory grade powder, and the purity is 99.9%.
In the preparation method, as a preferred embodiment, in the high-energy ball milling treatment, the ball milling time is 2-8 h (e.g., 3h, 4h, 5h, 6h, 7h), the rotation speed is 100-500 r/min (e.g., 120r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min), the ball-to-material ratio is 2: 1-4: 1.
in the above preparation method, as a preferred embodiment, in the sieving treatment, the mesh number of the sieve is 80 to 140 meshes (for example, 90 meshes, 100 meshes, 110 meshes, 120 meshes, 130 meshes), and after the sieving treatment, the undersize powder is taken out for subsequent treatment.
In the above production method, as a preferred embodiment, the press forming process is cold isostatic pressing, the forming pressure is 150 to 250MPa (e.g., 160MPa, 170MPa, 180MPa, 185MPa, 190MPa, 200MPa, 210MPa, 220MPa, 230MPa, 240MPa), and the pressure holding time is 30 to 120min (e.g., 40min, 45min, 50min, 60min, 70min, 80min, 90min, 100min, 105min, 110min, 115 min).
In the above preparation method, as a preferred embodiment, in the liquid phase sintering treatment, the sintering temperature is 1500 to 2300 ℃ (such as 1520 ℃, 1540 ℃, 1560 ℃, 1570 ℃, 1580 ℃, 1605 ℃, 1650 ℃, 1685 ℃, 1700 ℃, 1720 ℃, 1740 ℃, 1745 ℃, 1800 ℃, 1900 ℃, 2000 ℃, 2100 ℃ and 2200 ℃), and the sintering time is 0.5 to 4 hours (such as 1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours and 3.5 hours); preferably, the liquid phase sintering is performed in a sintering furnace, and the sintering atmosphere is vacuum condition, hydrogen or argon.
In the preparation method of the energy-containing tungsten alloy material, if the sintering temperature of the liquid phase sintering treatment is lower than 1500 ℃, the density of the prepared energy-containing tungsten alloy material cannot meet the requirement, and the mechanical property of the material is influenced; if the sintering temperature of the liquid phase sintering process is higher than 2300 ℃, the loss of other elements in the raw material except for the high melting point is caused. The density of the energetic tungsten alloy material prepared by the invention is required to be more than 16g/cm3The tensile strength is more than 600MPa, and the energy-containing tungsten alloy material which meets the use requirement of density and mechanical index can be prepared according to the specific practical application scene.
In the above production method, as a preferable embodiment, in the vacuum heat treatment, the degree of vacuum is less than 10- 1Pa (e.g. 5X 10)-2Pa、1×10-2Pa、8×10-3Pa、5×10-3Pa), the temperature of the vacuum heat treatment is 900-1200 ℃ (such as 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃), and the time of the vacuum heat treatment is 1-8 h (such as 1.5h, 2 h)h、2.5h、3h、4.5h、5h、6h、7h、7.5h)。
In the above production method, as a preferred embodiment, in the low-temperature continuous rolling treatment, a one-fire low-temperature continuous rolling method is used for deformation treatment, wherein the cogging temperature (i.e., the heating temperature before cogging) is 150 to 300 ℃ (for example, 160 ℃, 170 ℃, 180 ℃, 200 ℃, 220 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃, 280 ℃, 290 ℃, 295 ℃) and the holding time is 5 to 30 min; preferably, in the low-temperature continuous rolling treatment, the deformation amount is not more than 10%.
The continuous rolling pass in the invention is determined according to different components, and the selection of the cogging temperature is increased along with the increase of the content of refractory metals in the alloy billet. Note that, in this step, the total deformation amount of the material does not exceed 10%. The deformation in the invention refers to the deformation of the cross section area of the bar, namely the deformation (sectional area before rolling-sectional area after rolling)/sectional area before rolling, if the total deformation of the material is too large, the heat energy of the material can be released in advance; the heat preservation time in the invention is to preserve heat for 5-30 min at 150-300 ℃ before cogging. The reason why the deformation treatment is carried out in a one-fire low-temperature continuous rolling mode is that the heating temperature of the energy-containing components in the energy-containing tungsten alloy material cannot be too high, and if the temperature is too high, the heat energy of the material can be released in advance; the invention does not carry out heat treatment after low-temperature continuous rolling treatment, and the heat treatment can cause the toughness of the deformed material to rebound.
The preparation method of the energy-containing tungsten alloy material also comprises machining treatment, namely shaping, removing a sheath and the like of the blank before and after the hot isostatic pressing treatment, and machining and sampling the material after the low-temperature continuous rolling treatment, which can be realized by conventional operation.
Compared with the prior art, the invention has the following positive effects:
(1) in order to meet the actual use requirements of energy content, burning explosion and the like of the damaged part at present, various other elements are introduced, and the material components are purposefully redesigned;
(2) in order to match with new components, a process route is customized, and the preparation process is adjusted and improved. The material has special properties such as energy content, combustion and explosion and the like, and has stable comprehensive mechanical properties.
Drawings
FIG. 1 is a flow chart of a preparation process of the energetic tungsten alloy material of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.
The starting materials described in the examples below are all commercially available from the open literature.
The specific embodiment of the invention provides an energetic tungsten alloy material, and the adopted preparation method is shown in figure 1, and specifically comprises the following steps:
(1) preparing tungsten alloy powder: selecting raw materials meeting the requirements, putting the raw materials into a high-energy ball mill for high-energy ball milling treatment, wherein the ball milling time is 2-8 h, the rotating speed is 100-500 r/min, and the ball-material ratio is 2: 1-4: 1, obtaining tungsten alloy powder, then sieving the tungsten alloy powder, wherein the mesh number of a sieve is 80-140 meshes, and taking undersize products;
(2) and (3) compression molding treatment: carrying out cold isostatic pressing on the undersize obtained in the step (1), wherein the forming pressure is 150-250 MPa, and the pressure maintaining time is 30-120 min, so as to obtain a tungsten alloy bar blank;
(3) liquid-phase sintering treatment: placing the tungsten alloy bar pressed blank obtained in the step (2) in a sintering furnace, performing liquid phase sintering under the conditions of hydrogen atmosphere, argon atmosphere or vacuum, wherein the sintering temperature is 1500-2300 ℃, and the sintering time is 0.5-4 h, so as to obtain a tungsten alloy sintered blank, and detecting the relative density of the tungsten alloy sintered blank, wherein hot isostatic pressing treatment is not required if the relative density is more than 95%;
(4) hot isostatic pressing treatment: machining the tungsten alloy sintered blank obtained in the step (3), then loading the tungsten alloy sintered blank into a sheath, and performing hot isostatic pressing treatment under inert gas, wherein the hot isostatic pressing treatment pressure is 100-150 MPa, the temperature is 1300-1500 ℃, and the heat and pressure preservation time is 0.5-3 h;
(5) vacuum heat treatment: removing the sheath, taking out the blank in the step (4), and placing the blank in a vacuum furnace for heat treatment, wherein the vacuum degree is lower than 10-1Pa, the temperature of vacuum heat treatment is 900-1200 ℃, and the time of vacuum heat treatment is 1-8 h;
(6) low-temperature continuous rolling treatment: and (3) carrying out deformation treatment on the blank in the step (5) by adopting a one-fire low-temperature continuous rolling mode, wherein the cogging temperature is 150-300 ℃, the heat preservation time is 5-30 min, and the deformation amount in the low-temperature continuous rolling treatment is not more than 10%.
Embodiment 1 a method of preparing an energetic tungsten alloy material, comprising:
(1) preparation of 90W4Mo4Re2Zr tungsten alloy powder: tungsten powder with the Fisher particle size of 3.5 mu m, purchased rhenium powder, molybdenum powder and zirconium hydride powder (wherein corresponding figures are the mass percentage content of each component in 90W4Mo4Re2Zr tungsten alloy) are respectively weighed and put into a high-energy ball mill for high-energy ball milling treatment, the ball milling time is 4h, the rotating speed is 200r/min, and the ball-to-material ratio is 3: 1, obtaining tungsten alloy powder, then, sieving the tungsten alloy powder, wherein the mesh number of the sieve is 120 meshes, and taking undersize products.
(2) And (3) compression molding treatment: and (2) placing the undersize obtained in the step (1) into a dipping sleeve die for cold isostatic pressing, wherein the forming pressure is 180MPa, and the pressure maintaining time is 30min, so that a tungsten alloy bar blank is obtained.
(3) Liquid phase sintering treatment: and (3) placing the tungsten alloy bar blank obtained in the step (2) in a sintering furnace, sintering in a hydrogen atmosphere at 1650 ℃ for 2h to obtain a tungsten alloy sintered blank, and detecting that the relative density of the tungsten alloy sintered blank is 98.7% (without hot isostatic pressing treatment).
(4) Vacuum heat treatment: carrying out vacuum heat treatment on the tungsten alloy sintered blank obtained in the step (3), wherein the heat treatment temperature is 1050 ℃, the heat preservation time is 1h, and the vacuum degree is 5 multiplied by 10-2Pa, and obtaining the tungsten alloy bar billet after heat treatment.
(5) Low-temperature continuous rolling treatment: heating the tungsten alloy bar blank subjected to heat treatment obtained in the step (4) in an oven at the heating temperature of 220 ℃ for 20min, and then carrying out 2-pass continuous rolling to obtain the bar blank
Is reduced to
The deformation is about 9 percent, and the tungsten alloy bar after continuous rolling is obtained.
Respectively sampling the tungsten alloy bar blank obtained after the vacuum heat treatment and the tungsten alloy bar obtained after the low-temperature continuous rolling treatment, and then carrying out a room-temperature tensile property test (GB/T228.1-2010), wherein the test results are shown in Table 1; the energy release heat value of the prepared tungsten alloy rod finished product is tested by an oxygen elasticity calorimeter (refer to GB/213-2003 heat value detection national standard 'petroleum fuel/coal calorific value determination method', and the test method of the following embodiment is the same), and the energy release heat value of the energy-containing tungsten alloy material obtained in the embodiment 1 is 6352J/g.
Table 1 shows the performance data of the tungsten alloy rods obtained in example 1, namely, the tungsten alloy rods obtained in the vacuum heat treatment and the tungsten alloy rods obtained in the low-temperature continuous rolling treatment
Embodiment 2 an energetic tungsten alloy material, its preparation method includes:
(1) preparation of 81W6Mo5Nb8Hf tungsten alloy powder: tungsten powder with Fisher particle size of 3.2 mu m, industrial molybdenum powder, niobium powder and hafnium hydride powder (wherein corresponding figures refer to the mass percentage of the components in 81W6Mo5Nb8Hf tungsten alloy) are respectively weighed and put into a high-energy ball mill for high-energy ball milling treatment, the ball milling time is 6h, the rotating speed is 220r/min, the ball-to-material ratio is 2:1, tungsten alloy powder is obtained, then, sieving treatment is carried out, the mesh number of a sieve is 110 meshes, and undersize materials are taken.
(2) And (3) compression molding treatment: and (2) placing the undersize obtained in the step (1) into a dipping sleeve die for cold isostatic pressing, wherein the forming pressure is 200MPa, and the pressure maintaining time is 50min, so that a tungsten alloy bar blank is obtained.
(3) Liquid phase sintering treatment: and (3) placing the tungsten alloy bar blank obtained in the step (2) in a sintering furnace, sintering at 1760 ℃ in a hydrogen atmosphere for 3 hours to obtain a tungsten alloy sintered blank, and detecting that the relative density of the tungsten alloy sintered blank is 93.7%.
(4) Hot isostatic pressing treatment: and (4) performing hot isostatic pressing treatment on the tungsten alloy sintered blank obtained in the step (3), wherein the pressure is 130MPa, the hot pressing temperature is 1450 ℃, the heat preservation and pressure maintaining time is 2.5h, and the pressurizing medium is argon, so as to obtain a tungsten alloy bar subjected to hot isostatic pressing. The relative density of the tungsten alloy bar after hot isostatic pressing reaches 96.4 percent through detection.
(5) Vacuum heat treatment: carrying out vacuum heat treatment on the tungsten alloy bar material subjected to the hot isostatic pressing obtained in the step (4), wherein the heat treatment temperature is 1200 ℃, the heat preservation time is 1h, and the vacuum degree is 1 multiplied by 10-2Pa, and obtaining the tungsten alloy bar billet after heat treatment.
(6) Low-temperature continuous rolling treatment: heating the tungsten alloy bar blank subjected to heat treatment obtained in the step (5) in an oven at 250 ℃ for 30min, and then carrying out continuous rolling for 3 times to obtain the bar blank
Is reduced to
The deformation is about 8.4 percent, and the tungsten alloy bar after continuous rolling is obtained.
Respectively sampling the tungsten alloy bar billet subjected to the vacuum heat treatment and the tungsten alloy bar subjected to the low-temperature continuous rolling treatment, and then performing a room-temperature tensile property test (GB/T228.1-2010), wherein the test results are shown in Table 2: the energetic tungsten alloy material obtained in example 2 was measured to have a calorific value of 8526J/g.
Table 2 shows the performance data of the tungsten alloy rods obtained by the vacuum heat treatment and the low-temperature continuous rolling treatment in example 2
Embodiment 3 an energetic tungsten alloy material, the preparation method of which comprises:
(1) preparation of 93W3Re2Ni1Fe1Yb tungsten alloy powder: tungsten powder with the Fisher particle size of 2.8 mu m, industrial rhenium powder, nickel carbonyl powder, electrolytic iron powder and laboratory grade ytterbium powder are respectively weighed, the purity is 99.9% (wherein corresponding figures are the mass percentage content of each component in 93W3Re2Ni1Fe1Yb tungsten alloy), the tungsten powder, the industrial rhenium powder, the nickel carbonyl powder, the electrolytic iron powder and the laboratory grade ytterbium powder are put into a high-energy ball mill for high-energy ball milling treatment, the ball milling time is 3h, the rotating speed is 150r/min, and the ball-to-material ratio is 4: 1, obtaining tungsten alloy powder, then, sieving the tungsten alloy powder, wherein the mesh number of the sieve is 90 meshes, and taking undersize products.
(2) And (3) compression molding treatment: and (2) placing the undersize obtained in the step (1) into a dipping sleeve die for cold isostatic pressing, wherein the forming pressure is 240MPa, and the pressure maintaining time is 50min, so that a tungsten alloy bar blank is obtained.
(3) Liquid-phase sintering treatment: and (3) placing the tungsten alloy bar blank obtained in the step (2) in a sintering furnace, sintering at 1550 ℃ in a hydrogen atmosphere for 1h to obtain a tungsten alloy sintered blank, and detecting that the relative density of the tungsten alloy sintered blank is 93.5%.
(4) Hot isostatic pressing treatment: and (4) carrying out hot isostatic pressing treatment on the tungsten alloy sintered blank obtained in the step (3), wherein the pressure is 140MPa, the hot pressing temperature is 1300 ℃, the heat preservation and pressure maintaining time is 2h, and the pressurizing medium is nitrogen, so that a hot isostatic pressed tungsten alloy bar is obtained. The relative density of the tungsten alloy bar after hot isostatic pressing reaches 95.7 percent through detection.
(5) Vacuum heat treatment: carrying out vacuum heat treatment on the tungsten alloy bar material subjected to the hot isostatic pressing obtained in the step (4), wherein the heat treatment temperature is 950 ℃, the heat preservation time is 1h, and the vacuum degree is 5 multiplied by 10-3Pa, and obtaining the tungsten alloy bar billet after heat treatment.
(6) And (3) low-temperature continuous rolling treatment: heating the tungsten alloy bar blank subjected to heat treatment obtained in the step (5) in an oven at the heating temperature of 160 ℃ for 20min, and then carrying out 2-pass continuous rolling to obtain the bar blank
Is reduced to
The deformation is about 7.4 percent, and the tungsten alloy bar after continuous rolling is obtained.
Respectively sampling the tungsten alloy bar billet subjected to the vacuum heat treatment and the tungsten alloy bar obtained by the low-temperature continuous rolling treatment, and then performing a room-temperature tensile property test (GB/T228.1-2010), wherein the test results are shown in Table 3: the energetic heat value of the energetic tungsten alloy material obtained in example 3 was measured to be 4963J/g.
Table 3 shows the performance data of the tungsten alloy rods obtained by the vacuum heat treatment of the tungsten alloy rods obtained by the heat treatment and the low-temperature continuous rolling treatment
Embodiment 4 a method of making an energetic tungsten alloy material, comprising:
(1) preparation of 88W6Re3Nb3Zr tungsten alloy powder: tungsten powder, industrial rhenium powder, niobium powder and zirconium hydride powder (wherein corresponding figures are the mass percentage content of each component in 88W6Re3Nb3Zr tungsten alloy) with the Fisher particle size of 3.8 mu m are respectively weighed and put into a high-energy ball mill for high-energy ball milling treatment, the ball milling time is 2h, the rotating speed is 350r/min, and the ball-to-material ratio is 3: 1, obtaining tungsten alloy powder, then, sieving the tungsten alloy powder, wherein the mesh number of the sieve is 130 meshes, and taking undersize products.
(2) And (3) compression molding treatment: and (2) placing the undersize obtained in the step (1) into a dipping sleeve die for cold isostatic pressing, wherein the forming pressure is 185MPa, and the pressure maintaining time is 30min, so that a tungsten alloy bar blank is obtained.
(3) Liquid-phase sintering treatment: and (3) placing the tungsten alloy bar-stock pressed blank obtained in the step (2) in a sintering furnace, sintering in a hydrogen atmosphere at the sintering temperature of 2100 ℃ for 2h to obtain a tungsten alloy sintered blank, and detecting that the relative density of the tungsten alloy sintered blank is 96.7% (without hot isostatic pressing treatment).
(4) Vacuum heat treatment: carrying out vacuum heat treatment on the tungsten alloy sintered blank obtained in the step (3), wherein the heat treatment temperature is 1100 ℃, the heat preservation time is 2h, and the vacuum degree is 10-1Pa, and obtaining the tungsten alloy bar billet after heat treatment.
(5) Low-temperature continuous rolling treatment: heating the tungsten alloy bar blank subjected to heat treatment obtained in the step (4) in an oven at the heating temperature of 270 ℃ for 30min, then carrying out 2-pass continuous rolling,
is reduced to
The deformation amount is about 9.57%, and the tungsten alloy rod after continuous rolling is obtained.
Sampling is respectively carried out on the tungsten alloy bar billet subjected to the vacuum heat treatment and the tungsten alloy bar obtained by the low-temperature continuous rolling treatment, and then a room temperature tensile property test (GB/T228.1-2010) is carried out, wherein the test results are shown in Table 4: the energetic tungsten alloy material obtained in example 4 was measured to have a calorific value of 5896J/g.
Table 4 shows the performance data of the tungsten alloy rods obtained by the vacuum heat treatment and the low-temperature continuous rolling treatment in example 4
Embodiment 5 an energetic tungsten alloy material, its preparation method includes:
(1) preparation of 86W8Nb6Zr tungsten alloy powder: tungsten powder with the Fisher particle size of 3.4 mu m, industrial niobium powder and zirconium hydride powder (wherein corresponding figures are the mass percentage of the components in 86W8Nb6Zr tungsten alloy) are respectively weighed and put into a high-energy ball mill for high-energy ball milling treatment, the ball milling time is 3h, the rotating speed is 200r/min, and the ball-to-material ratio is 3: 1, obtaining tungsten alloy powder, then, sieving the tungsten alloy powder with a sieve with 110 meshes, and taking undersize products.
(2) And (3) compression molding treatment: and (2) placing the undersize obtained in the step (1) into a dipping sleeve die for cold isostatic pressing, wherein the forming pressure is 190MPa, and the pressure maintaining time is 50min, so that a tungsten alloy bar blank is obtained.
(3) Liquid phase sintering treatment: and (3) placing the tungsten alloy bar blank obtained in the step (2) in a sintering furnace, sintering in a hydrogen atmosphere at the sintering temperature of 2200 ℃ for 3h to obtain a tungsten alloy sintered blank, and detecting that the relative density of the tungsten alloy sintered blank is 96.6% (without hot isostatic pressing treatment).
(4) Vacuum heat treatment: carrying out vacuum heat treatment on the tungsten alloy sintered blank obtained in the step (3), wherein the heat treatment temperature is 1050 ℃, the heat preservation time is 2h, and the vacuum degree is 10-2Pa, and obtaining the tungsten alloy bar billet after heat treatment.
(5) Low-temperature continuous rolling treatment: heating the tungsten alloy bar blank subjected to heat treatment obtained in the step (4) in an oven at 290 ℃ for 30min, then carrying out 2-pass continuous rolling,
is reduced to
The deformation amount is about 9.7 percent, and the tungsten alloy rod after continuous rolling is obtained.
Respectively sampling the tungsten alloy bar blank after the heat treatment obtained after the vacuum heat treatment and the tungsten alloy bar obtained after the low-temperature continuous rolling treatment, and then carrying out a room-temperature tensile property test (GB/T228.1-2010), wherein the test results are shown in Table 5; the energetic tungsten alloy material obtained in example 5 was measured to have a calorific value of 6568J/g.
Table 5 shows the performance data of the tungsten alloy bar billet after the vacuum heat treatment and the tungsten alloy bar obtained by the low-temperature continuous rolling treatment in example 5
The above description is only exemplary of the invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the invention is intended to be covered by the appended claims.
Claims (10)
1. The energetic tungsten alloy material is characterized by comprising the following components in percentage by mass: 80-95% of tungsten and 5-20% of other elements; wherein the other elements are one or more of rhenium, molybdenum, niobium, hafnium, cobalt, manganese, zirconium, ytterbium and cerium.
2. The energetic tungsten alloy material of claim 1, wherein the other elements further comprise one or both of nickel and iron.
3. The preparation method of the energy-containing tungsten alloy material is characterized by comprising the following steps of: respectively weighing tungsten powder and other element powder according to the component proportion of the energetic tungsten alloy material as claimed in claim 1 or 2, and performing high-energy ball milling treatment to obtain tungsten alloy powder; then, the screening treatment, the press forming treatment, the liquid phase sintering treatment, the vacuum heat treatment and the low-temperature continuous rolling treatment are sequentially carried out.
4. The method of producing the energetic tungsten alloy material according to claim 3, characterized in that a hot isostatic pressing treatment is performed after the liquid phase sintering treatment and before the vacuum heat treatment; preferably, the pressure of the hot isostatic pressing treatment is 100-150 MPa, the temperature is 1300-1500 ℃, and the heat preservation and pressure maintaining time is 0.5-3 h; preferably, the pressurized medium of the hot isostatic pressing treatment is an inert gas; more preferably, the pressurizing medium for hot isostatic pressing is nitrogen or argon.
5. The method according to claim 3 or 4, wherein the tungsten powder is industrial tungsten powder and has a Fisher size of 2.0 to 4.0 μm, the nickel powder is electrolytic nickel powder or carbonyl nickel powder, the iron powder is electrolytic iron powder or carbonyl iron powder, the molybdenum, rhenium, niobium, cobalt powder and manganese powder are industrial powder, the hafnium and zirconium are hafnium hydride powder and zirconium hydride powder, and the ytterbium and cerium powder are laboratory grade powder, and the purity is 99.9%.
6. The preparation method of the energy-containing tungsten alloy material according to any one of claims 3 to 5, wherein in the high-energy ball milling treatment, the ball milling time is 2-8 h, the rotating speed is 100-500 r/min, and the ball-to-material ratio is 2: 1-4: 1;
preferably, in the sieving treatment, the mesh number of the sieve is 80-140 meshes, and after the sieving treatment, the sieved powder is taken for subsequent treatment.
7. The method for producing the energetic tungsten alloy material according to any one of claims 3 to 6, characterized in that the press forming treatment is cold isostatic pressing, the forming pressure is 150 to 250MPa, and the dwell time is 30 to 120 min.
8. The method for preparing the energetic tungsten alloy material according to any one of claims 3 to 7, wherein in the liquid phase sintering treatment, the sintering temperature is 1500 to 2300 ℃, and the sintering time is 0.5 to 4 hours; preferably, the liquid phase sintering is performed in a sintering furnace, and the sintering atmosphere is vacuum condition, hydrogen or argon.
9. The method of producing the energetic tungsten alloy material according to any one of claims 3 to 8, characterized in that in the vacuum heat treatment, the degree of vacuum is less than 10-1Pa, the temperature of the vacuum heat treatment is 900-1200 ℃, and the time of the vacuum heat treatment is 1-8 h.
10. The preparation method of the energy-containing tungsten alloy material according to any one of claims 3 to 9, characterized in that in the low-temperature continuous rolling treatment, a one-fire low-temperature continuous rolling mode is adopted for deformation treatment, wherein the cogging temperature is 150-300 ℃, and the holding time is 5-30 min; preferably, in the low-temperature continuous rolling treatment, the deformation amount is not more than 10%.
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