CN113798487B - Fe-based spherical shielding alloy powder and preparation method thereof - Google Patents

Fe-based spherical shielding alloy powder and preparation method thereof Download PDF

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CN113798487B
CN113798487B CN202110995961.0A CN202110995961A CN113798487B CN 113798487 B CN113798487 B CN 113798487B CN 202110995961 A CN202110995961 A CN 202110995961A CN 113798487 B CN113798487 B CN 113798487B
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alloy powder
powder
alloy
shielding
ball milling
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CN113798487A (en
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刘颖
李军
孙伦高
陈康为
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Sichuan University
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Sichuan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/22—Ferrous alloys, e.g. steel alloys containing chromium with molybdenum or tungsten
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
    • G21F1/085—Heavy metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/0848—Melting process before atomisation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors

Abstract

The invention relates to the field of nuclear radiation shielding materials, and particularly discloses Fe-based spherical shielding alloy powder and a preparation method thereof. The iron-based alloy powder comprises the following components in percentage by weight: 13.6-28.9% of W, 0.8-1.7% of B, 0-15.0% of Cr and the balance of Fe. The alloy powder is prepared by weighing the raw materials according to the components and the component proportion, smelting and atomizing under the protection of argon to obtain alloy powder, and then carrying out heat treatment and ball milling dispersion on the alloy powder to finally obtain the alloy powder with high sphericity and high fluidity, uniform boride phase distribution and good comprehensive shielding property. The Fe-based shielding alloy powder can be widely applied to the field of filling of special-shaped structures of nuclear radiation shielding and the field of repairing of Fe-based shielding body materials.

Description

Fe-based spherical shielding alloy powder and preparation method thereof
Technical Field
The invention relates to the field of nuclear radiation shielding materials, in particular to Fe-based spherical shielding alloy powder and a preparation method thereof.
Background
The nuclear energy is a clean energy with stable structure and high density energy, and is beneficial to supplement of human energy supply. In nuclear energy systems, the reactor is the core. In nuclear reactors, various radiation rays generated by nuclear fission (or fusion), such as neutrons of different energy levels, gamma rays, secondary gamma rays, other charged particles, and high-energy rays, can directly damage the human body, and can indirectly damage the human body by contaminating the air, soil, water sources, food, and the like. After a certain dose of rays enter a human body, ionization is generated on tissues of the human body, so that cells are deformed, the tissues are damaged, and diseases such as organ dysfunction, metabolism disorder and the like of the human body are caused. Meanwhile, the structure material and the machine equipment can generate heat and activate, and the service life of the structure material and the machine equipment is shortened. Therefore, the radiation generated by the nuclear reactor must be effectively shielded.
The large shielding structural member in the existing nuclear reactor is difficult to be integrally formed, and a large amount of special-shaped areas are inevitably generated by widely adopted welding processing means, become weak areas of radiation shielding and threaten the safety of personnel and equipment. At present, the heterogeneous region is densely filled with powder with good fluidity, high sphericity and excellent comprehensive shielding performance, so that the defect of the shielding performance of a main body is overcome, and the shielding performance of a shielding body is improved. In addition, some large-scale Fe-based shielding body materials are locally worn or corroded in the using process, so that the shielding performance of the shielding body is reduced, so that the defects of the shielding body are filled and repaired by Fe-based alloy powder with excellent shielding performance, and the maintenance and repair cost of a shielding system is greatly reduced.
At present, boron-containing stainless steel powder prepared by a gas atomization method is most widely applied in the fields and has the advantages of high sphericity, good fluidity, good thermal neutron shielding performance, corrosion resistance and the like. It also has some disadvantages: in the boron-containing stainless steel powder, the relative atomic mass of elements such as Fe, Ni, Cr, etc. is small, and the shielding effect on gamma rays is limited. Meanwhile, B element is segregated on the matrix grain boundary, and the microscopic uniformity of the alloy element needs to be optimized. W, B element-rich Fe-based shielding alloy is used as a novel nuclear radiation shielding material, wherein W, B element exists in the form of stable ternary boride FeWB phase. B element in the material has a high thermal neutron absorption cross section and can effectively shield thermal neutrons, and W element belongs to heavy element and can effectively shield gamma rays; at present, the prepared Fe-W-B alloy powder avoids element segregation to a certain extent and is beneficial to improving the comprehensive shielding performance of the alloy powder. However, the powder had to be further improved in terms of sphericity (only 82.7%), flowability (19.14s/50g) and oxygen content (0.7934 wt%).
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides Fe-based shielding alloy powder with high sphericity, high fluidity and excellent comprehensive shielding performance and a preparation method thereof. On the premise of ensuring excellent comprehensive shielding performance, the Fe-based alloy powder provided by the invention greatly improves the sphericity and the fluidity of the Fe-based alloy powder, and solves the problems mentioned in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the Fe-based spherical shielding alloy powder comprises the following components in percentage by weight: 13.6-28.9% of W, 0.8-1.7% of B, 0-15.0% of Cr and the balance of Fe.
Preferably, the Fe-based alloy powder comprises the following components in percentage by weight: 13.6-18.7% of W, 0.8-1.4% of B, 5-13.0% of Cr and the balance of Fe.
The iron-based shielding powder has high sphericity, good fluidity, uniform dispersion of the second phase in the powder and good comprehensive shielding performance.
A preparation method of Fe-based spherical shielding alloy powder comprises the following steps: under the condition of argon protection, the alloy raw materials are smelted and atomized to obtain atomized alloy powder, and then the atomized alloy powder is subjected to heat treatment and ball milling dispersion to obtain Fe-based spherical shielding alloy powder.
Preferably, the preparation method specifically comprises the following steps:
s1, alloy smelting: proportioning according to the component ratio, firstly smelting raw materials of industrial pure iron, ferrochromium and ferrotungsten to obtain alloy liquid, and then adding ferroboron into the alloy liquid for refining treatment;
s2, atomizing to prepare powder: pouring the refined alloy liquid into a tundish after the refined alloy liquid reaches the atomization temperature, adjusting the atomization pressure, carrying out atomization powder preparation, and collecting the cooled alloy powder to obtain atomized alloy powder;
s3, heat treatment: carrying out heat treatment on the atomized alloy powder by adopting a vacuum tube furnace;
s4, ball milling and dispersing: and carrying out ball milling and dispersion on the heat-treated powder by adopting a planetary ball mill.
Preferably, the smelting temperature in the step S1 is 1600-1700 ℃, and the refining time is 1-4 min; adding ferroboron into the alloy liquid, wherein the atomic ratio of boron to tungsten is 1: 1.
Preferably, the atomization temperature in the step S2 is 1650-1750 ℃, the atomization medium is argon, and the atomization pressure is 3.5-5.5 MPa;
preferably, the heat treatment temperature in the step S3 is 900-1200 ℃, and the heat treatment time is 0.5-3 h.
Preferably, the heat treatment temperature in the step S3 is 1000-1100 ℃, and the heat treatment time is 1-2 h.
Preferably, in the ball milling process of the heat-treated powder in the step S4, non-magnetic stainless steel balls with the specification of phi 3-8 mm are selected, mixed according to a ball-to-material ratio of 1:1, and ball milling is performed under the protection of argon atmosphere, wherein the ball milling rotation speed is 50-300 r/min, and the ball milling time is 0.5-3 h.
The invention has the beneficial effects that:
a. the powder has the following advantages: the powder is prepared by a gas atomization method, the oxygen partial pressure in the atomization furnace is strictly controlled, the oxidation of W and B elements is avoided, and the comprehensive shielding performance of the powder is ensured. The addition of the Cr element can also improve the balance electrode potential of the alloy powder, effectively improve the corrosion resistance of the powder and ensure that the alloy powder can be suitable for more complex service environments.
b. The surface appearance advantage of the powder is as follows: due to the addition of the Cr element, the melting point, the heat conductivity coefficient, the specific heat capacity and other parameters of the metal melt during atomization can be reduced, the solidification rate of the melt is slowed down, and the solidification time of the melt is prolonged. Therefore, the alloy droplets can be sufficiently spheroidized before they are completely solidified, forming metal powder of high sphericity. The powder bonded in the heat treatment process is dispersed by ball milling, the average sphericity of the obtained alloy powder can reach more than 87%, and the fluidity is superior to 17.0s/50 g.
c. Powder microstructure advantages: by atomization and subsequent heat treatment, a dispersed boride phase is obtained. By regulating Cr element, FeWB, (Fe, Cr) WB, (Fe, Cr) W can be obtained from the alloy2B2The three different compositions and structures of the boronated phase and combinations thereof. The boride phase is uniformly dispersed in the powder, the size can reach submicron or even nanometer size, and the alloy elements can reach high uniformity. Therefore, the Fe-based shielding alloy powder can have excellent comprehensive shielding performance of thermal neutrons and gamma rays.
d. The application advantages are as follows: the Fe-based shielding alloy powder can be applied to the filling field of nuclear radiation shielding special-shaped structures and the repairing field of Fe-based shielding body materials due to excellent fluidity, sphericity and comprehensive shielding performance.
Drawings
FIG. 1 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 1 of the present invention;
FIG. 2 is a surface topography of the Fe-based alloy powder prepared in example 1 of the present invention;
FIG. 3 is a sectional view of Fe-based alloy powder according to example 1 of the present invention;
FIG. 4 is a surface topography of Fe-based alloy powder prepared in example 2 of the present invention;
FIG. 5 is a sectional view of the Fe-based alloy powder produced in example 2 of the present invention;
FIG. 6 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 3 of the present invention;
FIG. 7 is a surface topography of Fe-based alloy powder produced in example 3 of the present invention;
FIG. 8 is a sectional view of Fe-based alloy powder according to example 3 of the present invention;
FIG. 9 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 4 of the present invention;
FIG. 10 is a surface topography of Fe-based alloy powder prepared in example 4 of the present invention;
FIG. 11 is a sectional view of Fe-based alloy powder according to example 4 of the present invention;
FIG. 12 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 6 of the present invention;
FIG. 13 is a surface topography map of Fe-based alloy powder produced in example 6 of the present invention;
FIG. 14 is a sectional view of Fe-based alloy powder according to example 6 of the present invention;
FIG. 15 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 7 of the present invention;
FIG. 16 is a surface topography of Fe-based alloy powder produced in example 7 of the present invention;
FIG. 17 is a sectional view of the Fe-based alloy powder produced in example 7 of the present invention;
FIG. 18 is a surface morphology diagram of Fe-based alloy powder prepared in comparative example 1 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 to 17, a novel Fe-based spherical shielding alloy powder having high sphericity, high fluidity and excellent comprehensive shielding performance, the Fe-based alloy powder comprising the following components in percentage by weight: 13.6-28.9% of W, 0.8-1.7% of B, 0-15.0% of Cr and the balance of Fe.
The Fe-based alloy provided by the invention comprises 13.6-28.9 wt% of W. According to the invention, W is added into the Fe-based alloy, and the content of W is controlled within the range, so that a stable boride phase can be obtained, and gamma rays can be effectively shielded, thereby improving the shielding performance of the alloy powder.
The Fe-based alloy provided by the invention comprises 0.8-1.7 wt% of B. According to the invention, the B is added into the Fe-based alloy, and the content of the B is controlled within the range, so that a stable boride phase can be obtained, and thermal neutrons can be effectively shielded, thereby improving the shielding performance of the alloy.
The Fe-based alloy provided by the invention comprises 0-15.0% of Cr in percentage by weight. According to the invention, Cr is added into the Fe-based alloy powder, and the content of Cr is controlled within the range, so that the sphericity, the fluidity, the uniformity of microstructure and the corrosion resistance of the alloy powder are improved.
The Fe-based alloy provided by the invention comprises the balance of Fe.
The invention provides a preparation method of Fe-based shielding alloy powder with high sphericity, high fluidity and excellent comprehensive shielding performance, which comprises the following steps:
under the protection of argon, the alloy raw materials are subjected to smelting and atomizing processes in atomizing equipment, and the sieved atomized powder is subjected to vacuum heat treatment and ball milling to obtain Fe-based alloy shielding powder. The smelting temperature is 1600-1700 ℃; the atomization pressure of the alloy is 3.5-5.5 MPa; the heat treatment temperature of the alloy powder is 900-1200 ℃, and the heat treatment time is 0.5-3 h. The ball milling speed is 50-300 r/min, and the ball milling time is 0.5-3 h. The chemical components of the alloy powder are consistent with the components of the Fe-based shielding alloy powder in the technical scheme.
In the present invention, when the alloy raw materials include W, B, Cr and Fe, the preparation method of the alloy powder includes the steps of:
(1) proportioning according to the component ratio, firstly smelting raw materials of industrial pure iron, ferrochromium and ferrotungsten to obtain alloy liquid, and then adding ferroboron into the alloy liquid for refining treatment;
(2) and pouring the refined alloy liquid into a tundish after the refined alloy liquid reaches the atomization temperature, adjusting the atomization pressure, and carrying out atomization to prepare powder. Collecting the cooled alloy powder to obtain atomized alloy powder;
(3) carrying out heat treatment on the atomized alloy powder by adopting a vacuum tube furnace;
(4) and carrying out ball milling and dispersion on the heat-treated powder by adopting a planetary ball mill.
In the present invention, the starting materials are all commercially available products unless otherwise specified. In the embodiment of the invention, the purity of the pure metal of the industrial pure iron Fe is more than or equal to 99.9 percent in percentage by mass. The ferrotungsten, ferroboron and ferrochrome are binary intermediate alloys corresponding to W, B, Cr. In the ferrotungsten binary alloy, by mass percent, tungsten is 77.81%, and the balance is Fe; in the ferroboron binary alloy, by mass percent, boron is 20.05%, and the balance is Fe. In the ferrochrome binary alloy, by mass percent, the chromium is 59.12 percent, and the balance is Fe;
in the invention, the raw materials corresponding to Fe, W and Cr are preferably smelted under the protection of argon, and then the raw material corresponding to B is added for refining treatment, so that the B with low content can be fully mixed with other raw materials, and the volatilization of the B can be avoided.
After obtaining the alloy liquid, mixing the alloy liquid with the raw materials of the corresponding components of B, wherein the atomic ratio of boron (B) to tungsten (W) is 1:1, and then refining for 1-4 min.
In the invention, after the temperature of the melt reaches 1670-1730 ℃, the refined alloy liquid is poured into a tundish for atomization and pulverization to obtain atomized alloy powder, wherein the atomization pressure is 3.5-5.5 MPa.
In the invention, the vacuum heat treatment temperature is 900-1200 ℃, and preferably 1000-1100 ℃.
In the invention, the vacuum heat treatment time is 0.5-3 h, preferably 1-2 h.
In the invention, the cooling modes of the heat treatment are furnace cooling.
The ball milling speed is 50-300 r/min, and the ball milling time is 0.5-3 h.
In the invention, the Fe-based alloy powder is obtained by smelting alloy raw materials under the protection of argon gas, and then atomizing, thermally treating and ball-milling and dispersing; the smelting temperature is 1600-1700 ℃, then argon gas atomization is carried out to prepare powder, and precipitated phases in the microstructure of the obtained alloy powder are distributed in a net shape. Therefore, the temperature of the mixed powder is raised to 900-1200 DEG CThen, the temperature is maintained for 0.5 to 3 hours, and the heat treatment is preferably carried out for 1 to 2 hours. By promoting the diffusion of W, B elements, the reticular precipitated phase in the Fe-based alloy powder provided by the invention is crushed into dispersed particles and finally converted into stable boride phases FeWB, (Fe, Cr) WB and (Fe, Cr) W2B2The purposes of improving the shape, element uniformity and phase structure stability of the powder micro-area are achieved. And finally, performing ball milling dispersion treatment to re-disperse the slightly bonded powder generated by heat treatment so as to improve the flowability of the powder.
Example 1
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 67.2% Fe, 13% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1650 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form alloy liquid, adding ferroboron into the secondary charging hopper, and refining for 3 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1700 ℃, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and packaging in vacuum.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder had D50 of 75.31 μm, fluidity of 15.36s/50g, sphericity of 92.3% and oxygen content of 0.0375 wt%.
FIG. 1 is an X-ray diffraction chart of Fe-based alloy powder obtained in example 1 of the present invention. The abscissa 2 theta is the diffraction angle, i.e. the angle between the incident X-ray and the diffraction line, and the ordinate is the diffraction intensity (dimensionless), in an X-ray diffraction diagram, each phase has its pairThe corresponding characteristic peaks, i.e. phase differences, will show diffraction peaks at different angles. FIG. 2 is a surface topography of the Fe-based alloy powder prepared in example 1 of the present invention. FIG. 3 is a sectional view of the Fe-based alloy powder obtained in example 1 of the present invention. FIG. 1 is a view showing that the Fe-based alloy powder provided in example 1 of the present invention has a matrix of α - (Fe, Cr) and a precipitated phase of (Fe, Cr) W2B2Structural phase. FIG. 2 shows that the Fe-based alloy powder provided in example 1 of the present invention has less satellite powder and higher sphericity. FIG. 3 is a diagram illustrating (Fe, Cr) W in Fe-based alloy powder provided in example 1 of the present invention2B2The particle phase is fine and is in dispersion distribution, higher microstructure uniformity is shown, and higher comprehensive shielding performance is favorably obtained.
Example 2
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 65.2% Fe, 15% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1680 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form alloy liquid, adding the ferroboron into the secondary charging hopper, and refining for 3 min; and after the temperature of the alloy liquid reaches 1730 ℃, pouring the alloy liquid into a tundish, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder had D50 of 87.37 μm, fluidity of 15.74s/50g, sphericity of 91.7% and oxygen content of 0.0318 wt%.
FIG. 4 shows Fe-based alloy powder obtained in example 2 of the present inventionAnd (4) a final surface topography. FIG. 5 is a sectional view of Fe-based alloy powder according to example 2 of the present invention. FIG. 4 shows that the Fe-based alloy powder provided in example 2 of the present invention has less satellite powder and higher sphericity. FIG. 5 is a diagram illustrating (Fe, Cr) W in Fe-based alloy powder provided in example 2 of the present invention2B2The particle phase is fine and is in dispersion distribution, higher microstructure uniformity is shown, and higher comprehensive shielding performance is favorably obtained.
Example 3
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 69.2% Fe, 10% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1630 ℃ until the industrial pure iron, ferrotungsten and ferrochrome are completely melted to form an alloy liquid, adding ferroboron into the secondary charging hopper, and refining for 3 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1680 ℃, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder has D50 of 84.64 μm, fluidity of 15.88s/50g, sphericity of 90.1% and oxygen content of 0.0472 wt%.
FIG. 6 is an X-ray diffraction chart of Fe-based alloy powder obtained in example 3 of the present invention. The abscissa 2 theta is a diffraction angle, namely an included angle between an incident X-ray and a diffraction line, the ordinate is diffraction intensity (dimensionless), and each phase in an X-ray diffraction pattern has a corresponding characteristic peak, namely, the phases are different and the diffraction peaks appear at different angles. Figure 7 is the bookThe surface topography of the Fe-based alloy powder prepared in the invention example 3 is shown. FIG. 8 is a sectional view of Fe-based alloy powder according to example 3 of the present invention. FIG. 6 is a graph showing that the Fe-based alloy powder provided in example 3 of the present invention has a matrix of α - (Fe, Cr) and a precipitated phase of (Fe, Cr) W2B2And (Fe, Cr) WB structure phases, both stable boride phases. FIG. 7 shows that the Fe-based alloy powder provided in example 3 of the present invention has less satellite powder and higher sphericity. Fig. 8 illustrates that boride particle phases in the Fe-based alloy powder provided in embodiment 3 of the present invention are fine and dispersed, and exhibit high microstructure uniformity, which is advantageous for obtaining high comprehensive shielding performance.
Example 4
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 72.2% Fe, 8% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1620 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form alloy liquid, adding the ferroboron into the secondary charging hopper, and refining for 2 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1670 ℃, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 0.5h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are as follows: the alloy powder had D50 of 87.37 μm, fluidity of 16.04s/50g, sphericity of 89.51% and oxygen content of 0.0518 wt%.
FIG. 9 is an X-ray diffraction chart of the Fe-based alloy powder obtained in example 4 of the present invention. The abscissa 2 theta is a diffraction angle, namely an included angle between an incident X-ray and a diffraction line, the ordinate is diffraction intensity (dimensionless), and each phase in an X-ray diffraction pattern has a corresponding characteristic peak, namely, the phases are different and the diffraction peaks appear at different angles. FIG. 10 is a surface topography of the Fe-based alloy powder prepared in example 4 of the present invention. FIG. 11 is a sectional view of Fe-based alloy powder according to example 4 of the present invention. FIG. 10 shows that the Fe-based alloy powder provided in example 4 of the present invention has a matrix of α - (Fe, Cr) and a precipitated phase of a stable ternary boride phase (Fe, Cr) WB. FIG. 10 shows that the Fe-based alloy powder provided in example 4 of the present invention has less satellite powder and higher sphericity. Fig. 11 illustrates that boride particle phases in the Fe-based alloy powder provided in example 4 of the present invention are fine and dispersed, and exhibit high microstructure uniformity, which is advantageous for obtaining high comprehensive shielding performance.
Example 5
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 75.2% Fe, 5% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing to the vacuum degree of 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1615 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form alloy liquid, adding the ferroboron into the secondary charging hopper, and refining for 2 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1665 ℃, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, fluidity, sphericity, oxygen content. The test results are as follows: the alloy powder had D50 of 88.62 μm, fluidity of 16.18s/50g, sphericity of 89.12% and oxygen content of 0.0524 wt%.
Example 6
An Fe-based shielding alloy powder: 77.2% Fe, 3% Cr, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1610 ℃ until the industrial pure iron, ferrotungsten and ferrochrome are completely melted to form alloy liquid, adding ferroboron into the secondary charging hopper, and refining for 2 min; atomizing the alloy melt at 1660 ℃ by adopting argon atomization pressure of 5MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was thermally treated at 1050 ℃ for 1h in a vacuum tube furnace. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 3 hours at the ball milling rotating speed of 300 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder has D50 of 101.36 μm, fluidity of 16.29s/50g, sphericity of 88.92% and oxygen content of 0.0530 wt%.
FIG. 12 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 6 of the present invention. The abscissa 2 theta is a diffraction angle, namely an included angle between an incident X-ray and a diffraction line, the ordinate is diffraction intensity (dimensionless), and each phase in an X-ray diffraction pattern has a corresponding characteristic peak, namely, the phases are different and the diffraction peaks appear at different angles. FIG. 13 is a surface topography of the Fe-based alloy powder prepared in example 6 of the present invention. FIG. 14 is a sectional view of the Fe-based alloy powder produced in example 6 of the present invention. FIG. 12 shows that the Fe-based alloy powder provided in example 6 of the present invention has a matrix of α - (Fe, Cr) and a precipitated phase of a stable ternary boride phase (Fe, Cr) WB. FIG. 13 shows that example 6 of the present invention provides less satellite powder and higher sphericity of Fe-based alloy powder. Fig. 14 illustrates that boride particle phases in the Fe-based alloy powder provided in example 6 of the present invention are fine and dispersed, and exhibit high microstructure uniformity, which is advantageous for obtaining high comprehensive shielding performance.
Example 7
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 80.2% Fe, 18.7% W, 1.1% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochromium into a magnesia crucible according to a component proportion, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon gas to 0.1MPa (micro positive pressure), smelting at 1620 ℃ until the industrial pure iron, the ferrotungsten and the ferrochromium are completely melted to form an alloy liquid, adding ferroboron in the secondary charging hopper, and refining for 3 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1670 ℃, atomizing the alloy melt by adopting argon atomization pressure of 4MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1000 ℃ for 1 hour. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 250 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder has D50 of 96.88 mu m, fluidity of 16.48s/50g, sphericity of 87.17% and oxygen content of 0.0622 wt%.
FIG. 15 is an X-ray diffraction chart of an Fe-based alloy powder obtained in example 7 of the present invention. The abscissa 2 theta is a diffraction angle, namely an included angle between an incident X-ray and a diffraction line, the ordinate is diffraction intensity (dimensionless), and each phase in an X-ray diffraction pattern has a corresponding characteristic peak, namely, the phases are different and the diffraction peaks appear at different angles. FIG. 16 is a surface topography of the Fe-based alloy powder prepared in example 7 of the present invention. FIG. 17 is a sectional view of the Fe-based alloy powder produced in example 7 of the present invention. FIG. 15 is a graph showing that the Fe-based alloy powder provided in example 7 of the present invention has α -Fe as the matrix and FeWB as the stable ternary boride phase as the precipitated phase. FIG. 16 shows that example 7 of the present invention provides less satellite powder and higher sphericity of Fe-based alloy powder. Fig. 17 illustrates that boride particles in the Fe-based alloy powder provided in example 7 of the present invention are fine and dispersed, and exhibit high microstructure uniformity, which is beneficial to obtaining high comprehensive shielding performance.
Example 8
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 72.6% Fe, 13% Cr, 13.6% W, 0.8% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1620 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form alloy liquid, adding the ferroboron into the secondary charging hopper, and refining for 2 min; and pouring the alloy liquid into a tundish after the temperature of the alloy liquid reaches 1670 ℃, atomizing the alloy melt by adopting argon atomization pressure of 3.5MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 900 ℃ for 0.5 h. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 1h at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder had D50 of 94.65 μm, fluidity of 16.27s/50g, sphericity of 90.35% and oxygen content of 0.0632 wt%.
Example 9
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 61.8% Fe, 13% Cr, 23.8% W, 1.4% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing to the vacuum degree of 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1675 ℃ until the industrial pure iron, the ferrotungsten and the ferrochrome are completely melted to form an alloy liquid, adding the ferroboron into the secondary charging hopper, and refining for 3 min; and after the temperature of the alloy liquid reaches 1725 ℃, pouring the alloy liquid into a tundish, atomizing the alloy melt by adopting argon atomization pressure of 5MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1100 ℃ for 2 hours. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 2 hours at the ball milling rotating speed of 200 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, fluidity, sphericity, oxygen content. The test results are: the alloy powder had D50 of 99.43 μm, fluidity of 15.94s/50g, sphericity of 88.56% and oxygen content of 0.0467 wt%.
Example 10
A Fe-based shielding alloy powder with high sphericity, high fluidity and good comprehensive shielding performance: 56.4% Fe, 13% Cr, 28.9% W, 1.7% B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1700 ℃ until the industrial pure iron, ferrotungsten and ferrochrome are completely melted to form alloy liquid, adding ferroboron into the secondary charging hopper, and refining for 4 min; and atomizing the alloy melt to prepare powder by adopting argon atomization pressure of 5.5MPa at 1750 ℃, and collecting the powder. Subsequently, the collected powder was heat-treated in a vacuum tube furnace at 1200 ℃ for 3 hours. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 3 hours at the ball milling rotating speed of 300 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder had D50 of 103.32 μm, fluidity of 16.13s/50g, sphericity of 87.6% and oxygen content of 0.0539 wt%.
Comparative example 1
An Fe-based shielding alloy powder: 80.2% Fe, 18.7% W, 1.1B. The preparation method of the alloy comprises the following steps: adding raw materials of industrial pure iron, ferrotungsten and ferrochrome into a magnesia crucible according to a component ratio, adding ferroboron into a secondary charging hopper, charging tightly, vacuumizing until the vacuum degree is 4Pa, charging argon to 0.1MPa (micro positive pressure), smelting at 1700 ℃ until the industrial pure iron, ferrotungsten and ferrochrome are completely melted to form alloy liquid, adding ferroboron into the secondary charging hopper, and refining for 4 min; atomizing the alloy melt at 1750 ℃ by adopting the water pressure of 5MPa to prepare powder, and collecting the powder. Subsequently, the collected powder was thermally treated at 1050 ℃ for 1h in a vacuum tube furnace. Subsequently, the atomized powder and the stainless steel balls are placed into a planetary ball milling tank according to the ball-to-material ratio of 1:1, and ball milling is carried out for 3 hours at the ball milling rotating speed of 300 r/min. And finally, taking out the alloy powder subjected to ball milling, and carrying out vacuum packaging.
The performance of the Fe-based shielding alloy powder is tested, and the test contents are as follows: laser particle size, flowability, sphericity, oxygen content. The test results are: the alloy powder had D50 of 110.53 μm, fluidity of 19.14s/50g, sphericity of 78.47% and oxygen content of 0.7934 wt%.
FIG. 18 is a surface morphology chart of the Fe-based alloy powder prepared in comparative example 1 of the present invention. FIG. 18 shows that the Fe-based alloy powder provided in comparative example 1 of the present invention has a low sphericity of the whole powder, and there are a large amount of shaped powder and satellite powder, so that the sphericity of the powder is low. The Fe-based spherical shielding alloy powder prepared by the method has the following advantages:
a. the powder has the following advantages: by adopting the gas atomization method for preparing powder, the oxygen partial pressure in the atomization furnace is strictly controlled, the oxidation of W and B elements is avoided, and the comprehensive shielding performance of the powder is ensured. The addition of the Cr element can also improve the balance electrode potential of the alloy powder, effectively improve the corrosion resistance of the powder and ensure that the alloy powder can be suitable for more complex service environments.
b. The surface appearance advantage of the powder is as follows: due to the addition of the Cr element, the melting point, the heat conductivity coefficient, the specific heat capacity and other parameters of the metal melt during atomization can be reduced, the solidification rate of the melt is slowed down, and the solidification time of the melt is prolonged. Therefore, the alloy droplets can be sufficiently spheroidized before they are completely solidified, forming metal powder of high sphericity. The powder bonded in the heat treatment process is dispersed by ball milling, the average sphericity of the obtained alloy powder can reach more than 87%, and the fluidity is superior to 17.0s/50 g.
c. Powder microstructure advantage: powder microstructure advantage: by atomization and subsequent heat treatment, a dispersion of boride phases is obtained. By regulating Cr element, FeWB, (Fe, Cr) WB, (Fe, Cr) W can be obtained from the alloy2B2The three different compositions and structures of the boronated phase and combinations thereof. The boride phase is uniformly dispersed in the powder, the size can reach submicron or even nanometer size, and the alloy elements can reach high uniformity. Therefore, the Fe-based shielding alloy powder can have excellent comprehensive shielding performance of thermal neutrons and gamma rays.
d. The application advantages are as follows: the Fe-based shielding alloy powder can be applied to the filling field of nuclear radiation shielding special-shaped structures and the repairing field of Fe-based shielding body materials due to excellent fluidity, sphericity and comprehensive shielding performance.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.

Claims (6)

1. The Fe-based spherical shielding alloy powder is characterized by comprising the following components in percentage by weight: 13.6-28.9% of W, 0.8-1.7% of B, 0-15.0% of Cr and the balance of Fe; the average sphericity of the alloy powder can reach more than 87%, and the fluidity of the alloy powder is superior to 17.0s/50 g; the alloy powder contains FeWB, (Fe, Cr) WB, (Fe, Cr) W2B2Three boronated phases of different composition and structure and combinations thereof.
2. The Fe-based spherical shielding alloy powder according to claim 1, wherein the Fe-based spherical shielding alloy powder comprises the following components in percentage by weight: 13.6-18.7% of W, 0.8-1.4% of B, 5-13.0% of Cr and the balance of Fe.
3. The method for producing an Fe-based spherical shielding alloy powder according to claim 1 or 2, wherein: the method comprises the following steps: under the condition of argon protection, smelting and atomizing alloy raw materials to obtain atomized alloy powder, and then carrying out heat treatment and ball milling dispersion on the atomized alloy powder to obtain Fe-based spherical shielding alloy powder; the preparation method comprises the following specific steps:
s1, alloy smelting: proportioning according to the component proportion, firstly smelting raw materials of industrial pure iron, ferrochromium and ferrotungsten to obtain alloy liquid, and then adding ferroboron into the alloy liquid for refining treatment;
s2, atomizing to prepare powder: pouring the refined alloy liquid into a tundish after the refined alloy liquid reaches the atomization temperature, adjusting the atomization pressure, carrying out atomization powder making, and collecting the cooled alloy powder to obtain atomized alloy powder, wherein the atomization temperature is 1650-1750 ℃, the atomization medium adopts argon, and the atomization pressure is 3.5-5.5 Mpa;
s3, heat treatment: carrying out heat treatment on the atomized alloy powder by using a vacuum tube furnace, wherein the heat treatment temperature is 900-1200 ℃, and the heat treatment time is 0.5-3 h;
s4, ball milling and dispersing: and carrying out ball milling and dispersion on the heat-treated powder by adopting a planetary ball mill.
4. The production method according to claim 3, characterized in that: the smelting temperature in the step S1 is 1600-1700 ℃, and the refining time is 1-4 min; adding ferroboron into the alloy liquid, wherein the atomic ratio of boron to tungsten is 1: 1.
5. The production method according to claim 3, characterized in that: the heat treatment temperature in the step S3 is 1000-1100 ℃, and the heat treatment time is 1-2 h.
6. The production method according to claim 3, characterized in that: and S4, selecting nonmagnetic stainless steel balls with the specification of phi 3-8 mm, mixing the balls according to a ball-material ratio of 1:1, and carrying out ball milling under the protection of argon atmosphere, wherein the ball milling rotation speed is 50-300 r/min, and the ball milling time is 0.5-3 h.
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