CN111826566A - Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof - Google Patents
Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof Download PDFInfo
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- CN111826566A CN111826566A CN201911263343.6A CN201911263343A CN111826566A CN 111826566 A CN111826566 A CN 111826566A CN 201911263343 A CN201911263343 A CN 201911263343A CN 111826566 A CN111826566 A CN 111826566A
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- 239000000843 powder Substances 0.000 title claims abstract description 97
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 95
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 239000000956 alloy Substances 0.000 title claims abstract description 86
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 86
- 239000010937 tungsten Substances 0.000 title claims abstract description 86
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 85
- 229910052726 zirconium Inorganic materials 0.000 title claims abstract description 84
- 239000006104 solid solution Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 72
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000004886 process control Methods 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000010935 stainless steel Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 230000000694 effects Effects 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 7
- 238000002485 combustion reaction Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000012300 argon atmosphere Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003657 tungsten Chemical class 0.000 description 2
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- B22F1/0003—
-
- 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
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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
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
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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
- 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
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- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Abstract
The invention discloses a tungsten/zirconium supersaturated solid solution alloy powder and a preparation method thereof, wherein the alloy powder consists of tungsten and zirconium; the mass fraction of zirconium in the alloy powder is 5-40%; the preparation method comprises the steps of firstly weighing tungsten and zirconium raw materials according to the mass ratio, then adding grinding balls and process control agents according to a certain ratio of the total mass of the tungsten and zirconium raw materials, and then carrying out ball milling in an inert atmosphere to obtain tungsten/zirconium supersaturated solid solution alloy powder. The activity of tungsten is changed due to the solid solution of zirconium, so that the alloy powder provided by the invention can be combusted in the air, and the tungsten can also be combusted to release energy; the preparation method provided by the invention has the advantages of simple process, low cost, short preparation period and wide application range, and can realize that zirconium is completely and fixedly dissolved in tungsten particles at normal temperature to form supersaturated solid solution alloy powder.
Description
Technical Field
The invention relates to the technical field of alloy material preparation, in particular to tungsten/zirconium supersaturated solid solution alloy powder and a preparation method thereof.
Background
Tungsten-based alloys have high density, strength, hardness and toughness and are attractive in the field of defense industry because they can be used as armor piercing projectile cores for kinetic energy penetration weapons.
In recent years, tungsten (W) has been frequently added to energetic materials to increase the density of the material, but tungsten is generally considered to be an inert component in energetic materials because of its high thermal inertia and low adiabatic flame problems making it difficult to ignite or self-sustaining combustion.
Disclosure of Invention
The invention provides tungsten/zirconium supersaturated solid solution alloy powder and a preparation method thereof, which are used for overcoming the defects that tungsten is difficult to ignite or self-sustaining burn when used in energetic materials in the prior art, zirconium is completely and fixedly dissolved in tungsten particles to form supersaturated solid solution alloy powder, and the activity of the powder is changed due to the solid solution of the zirconium, so that the supersaturated solid solution alloy powder can realize the combustion in the air, and the tungsten can also burn and release energy.
In order to achieve the above object, the present invention proposes a supersaturated solid solution alloy powder of tungsten/zirconium (W/Zr), the alloy powder being composed of tungsten and zirconium; the mass fraction of zirconium in the alloy powder is 5-40%; the alloy powder is high-energy-density powder and is easy to burn and release energy.
In order to achieve the above object, the present invention further provides a method for preparing a supersaturated tungsten/zirconium solid solution alloy powder, comprising the following steps:
s1: according to the mass ratio (60-95): (5-40) weighing tungsten and zirconium as raw materials, uniformly mixing, and putting into a ball milling tank;
s2: adding grinding balls according to the ratio (5:1) - (20:1) of the mass of the grinding balls to the total mass of the raw material tungsten and the raw material zirconium, adding a process control agent according to 3-5% of the total mass of the raw material tungsten and the raw material zirconium, and sealing a ball milling tank;
s3: and ball-milling for 10-30 h at the rotating speed of 200-250 r/min in an inert atmosphere to obtain the tungsten/zirconium supersaturated solid solution alloy powder.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides tungsten/zirconium supersaturated solid solution alloy powder which consists of tungsten and zirconium; the mass fraction of zirconium in the alloy powder is 5-40%; according to the invention, a certain amount of zirconium is added into tungsten, and the zirconium is completely and fixedly dissolved in tungsten particles to form supersaturated solid solution alloy powder; introducing high-activity element zirconium into tungsten, so that the activity of the tungsten is changed, and the tungsten/zirconium supersaturated solid solution alloy powder can be combusted in the air; therefore, the tungsten and the zirconium in the alloy powder can be combusted, and the alloy powder has high energy density.
2. The preparation method of the tungsten/zirconium supersaturated solid solution alloy powder comprises the following steps of firstly weighing tungsten and zirconium raw materials according to a mass ratio, wherein the tungsten and the zirconium in a proper mass ratio can realize the combustion of tungsten and can ensure that the prepared alloy powder can keep the original excellent performance of the tungsten; then adding grinding balls and process control agents according to a certain proportion of the total mass of the tungsten and zirconium raw materials, wherein a proper amount of grinding balls ensure that the tungsten and zirconium raw materials are fully ball-milled to realize that zirconium is completely dissolved in tungsten particles at normal temperature, the ball-milling efficiency is improved, and in addition, a proper amount of process control agents promote that zirconium is dissolved in tungsten particles in a solid manner, and meanwhile, the damage to the original excellent performance of tungsten is avoided; then ball milling is carried out in an inert atmosphere to obtain tungsten/zirconium supersaturated solid solution alloy powder, ball milling is carried out in the inert atmosphere to avoid oxidation of the surface of zirconium to form an oxide film to influence the activity of the zirconium, and the ball milling rotation speed and time are controlled to promote the ball milling efficiency and ensure the quality of the formed alloy powder; finally, alloy powder meeting the requirements is obtained. The high-activity element zirconium is introduced into the tungsten, so that the activity of the tungsten is changed, the tungsten/zirconium supersaturated solid solution alloy powder can be combusted in the air, and the combustion energy release of the tungsten is also realized. However, at normal temperature, the solid solubility of zirconium in tungsten is very low, the melting points of two metals are very high, particularly tungsten, the melting point reaches 3400 ℃ (the melting point of zirconium is 1852 ℃), and the tungsten/zirconium supersaturated solid solution alloy prepared by the existing method has great difficulty and even if the realization cost is very high. The preparation method provided by the invention has the advantages of simple process, low cost, short preparation period and wide application range, and can realize that zirconium is completely and fixedly dissolved in tungsten particles at normal temperature to form supersaturated solid solution alloy powder.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
FIG. 1 is an SEM photograph of a tungsten/zirconium supersaturated solid solution alloy powder prepared in example 1;
FIG. 2 is an XRD pattern of the tungsten/zirconium supersaturated solid solution alloy powder prepared in example 1;
FIG. 3 is an SEM photograph of the tungsten/zirconium supersaturated solid solution alloy powder prepared in example 2;
FIG. 4 is an XRD pattern of the tungsten/zirconium supersaturated solid solution alloy powder prepared in example 2;
FIG. 5 is an SEM photograph of the tungsten/zirconium supersaturated solid solution alloy powder prepared in example 3;
fig. 6 is an XRD pattern of the tungsten/zirconium supersaturated solid solution alloy powder prepared in example 3.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
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.
In addition, the technical solutions in the embodiments of the present invention may be combined with each other, but it must be based on the realization of those skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination of technical solutions should not be considered to exist, and is not within the protection scope of the present invention.
The drugs/reagents used are all commercially available without specific mention.
The invention provides tungsten/zirconium supersaturated solid solution alloy powder, which consists of tungsten and zirconium; the mass fraction of zirconium in the alloy powder is 5-40%. The alloy powder is high-energy-density powder and is easy to burn and release energy.
The activity of the alloy powder is changed due to the solid solution of zirconium, so that the supersaturated solid solution alloy powder can be combusted in the air, and tungsten can also be combusted to release energy.
Preferably, the average grain diameter of the alloy powder is 1-4 μm; the elements of the alloy powder are uniformly distributed; the thermal stability of the alloy powder can reach more than 1350 ℃.
The invention also provides a preparation method of the tungsten/zirconium supersaturated solid solution alloy powder, which comprises the following steps:
s1: according to the mass ratio (60-95): (5-40) weighing tungsten and zirconium as raw materials, uniformly mixing, and putting into a ball milling tank;
preferably, the purity of the raw material tungsten is more than 99.0%, and the particle size is 1-4 μm; the purity of the raw material zirconium is more than 99.0%, and the particle size is 35-40 mu m. The purity of the raw materials is controlled to ensure that the final product contains less impurities and has excellent performance; the grain diameter of the raw materials is controlled to shorten the preparation period, and simultaneously, the zirconium can be completely and fixedly dissolved in the tungsten particles at normal temperature to form supersaturated solid solution alloy powder.
S2: adding grinding balls according to the ratio (5:1) - (20:1) of the mass of the grinding balls to the total mass of the raw material tungsten and the raw material zirconium, adding a process control agent according to 3-5% of the total mass of the raw material tungsten and the raw material zirconium, and sealing a ball milling tank;
preferably, the grinding balls are at least one of cemented carbide balls and stainless steel balls. The grinding balls are made of metal materials with high strength, so that the raw materials can be sufficiently ball-milled, and the raw materials cannot be polluted due to damage in the ball-milling process due to low strength.
Preferably, the grinding balls comprise grinding balls with different particle sizes, and the mass ratio of the grinding balls with different particle sizes is different, so that the ball milling efficiency is improved.
Preferably, the process control agent is an organic solvent. The process control agent is added to ensure uniform product fineness, low energy consumption of the product per unit weight, and avoidance of dust flying, and simultaneously, noise is reduced. And the organic solvent is easy to volatilize and is convenient to remove.
Preferably, the organic solvent is at least one of absolute ethyl alcohol, n-hexane, methanol and acetone. The selected organic solvent is common organic solvent, is easy to obtain, has low price, is preferably absolute ethyl alcohol and n-hexane, and has low toxicity.
S3: ball-milling for 10-30 h at a rotating speed of 200-250 r/min in an inert atmosphere to obtain tungsten/zirconium supersaturated solid solution alloy powder;
preferably, the ball milling adopts a batch ball milling mode, and specifically comprises the following steps:
ball milling is carried out for 5min, the suspension is carried out for 5min, and then the ball milling is carried out for 5min in the reverse direction. The intermittent ball milling mode is adopted to avoid the influence on the alloying process due to the overhigh heat generated by the continuous ball milling.
Preferably, the process control agent is added every 5h of the ball mill in the same amount as in S2. Because heat is generated during the ball milling process to make the process control agent continuously volatilize, the process control agent needs to be added in stages to ensure the ball milling quality.
Example 1
The embodiment provides a preparation method of tungsten/zirconium supersaturated solid solution alloy powder, which specifically comprises the following steps:
weighing 1.5Kg of Zr powder and 8.5Kg of 8.5KgW powder in an argon atmosphere protective glove box, uniformly mixing, and putting into a stainless steel ball milling tank; adding stainless steel balls according to 10 times of the total mass of the tungsten powder and the zirconium powder, wherein the mass ratio of the stainless steel balls with the diameters of 5mm, 8mm and 10mm is 5:3: 2; adding absolute ethyl alcohol according to 3 percent of the total mass of the tungsten powder and the zirconium powder, and sealing the ball milling tank. The ball milling equipment adopts a planetary ball mill, the ball milling mode adopts intermittent ball milling, namely, the ball milling is suspended for 5min and reversed for 5min every time the ball milling is carried out for 5min, the circulation is carried out, and the ball milling is carried out for 5h at the rotating speed of 220r/min under the argon atmosphere; adding absolute ethyl alcohol according to 3% of the total mass of the tungsten powder and the zirconium powder, sealing, and continuing to perform ball milling for 5 hours at the rotating speed of 220 r/min; anhydrous ethanol was added once every 5h of ball milling, which was performed for a total of 20h in this example. After the ball milling is finished, standing and cooling to room temperature, and taking out alloy powder in an argon atmosphere protective glove box, wherein the average particle size of the powder is 1-4 microns.
The SEM (scanning electron microscope) photograph and XRD (X-ray diffraction) pattern of the alloy powder prepared in this example are shown in fig. 1 and 2. As can be seen from FIG. 1, the alloy powder particles are irregularly flat, and are finely dispersed, and the average particle diameter is 1 to 3 μm. As can be seen from FIG. 2, the diffraction peak of Zr has completely disappeared after 20h ball milling, only the diffraction peak of W is remained, which shows that Zr is gradually dissolved into W crystal lattice during ball milling, and finally W (Zr) single phase exceeding saturated solid solution is formed. The diffraction peaks of W are gradually broadened due to the reduction of the grain size and the introduction of micro strain during the ball milling process (micro strain causes micro stress inside the grains or between several grains, which in turn causes the grains to be compressed or stretched. In the preparation method of the embodiment, Zr is successfully dissolved in W crystal lattices in a solid solution mode, and the Zr with high adiabatic flame temperature and high combustion heat value can realize combustion of W, so that the alloy powder prepared in the embodiment is high-energy-density powder and is easy to combust to release energy.
Example 2
In this example, compared with example 1, the method for preparing the supersaturated tungsten/zirconium solid solution alloy powder is similar to example 1 except that 2.0Kg of Zr powder and 8.0Kg of 8.0KgW powder are weighed.
SEM (scanning electron microscope) picture and XRD (X-ray diffraction) spectrum of the alloy powder prepared in the example are shown in figures 3 and 4. As can be seen from FIG. 3, the alloy powder particles are irregularly flat, and are finely dispersed, and the average particle size is 2 to 4 μm. As can be seen from FIG. 4, the diffraction peak of Zr has completely disappeared after 20h ball milling, only the diffraction peak of W is remained, which shows that Zr is gradually dissolved into W crystal lattice during ball milling, and finally W (Zr) single phase exceeding saturated solid solution is formed. The diffraction peak of W gradually broadened due to the reduction of grain size and the introduction of microscopic strain during ball milling. In the preparation method of the embodiment, Zr is successfully dissolved in W crystal lattices in a solid solution mode, and the Zr with high adiabatic flame temperature and high combustion heat value can realize combustion of W, so that the alloy powder prepared in the embodiment is high-energy-density powder and is easy to combust to release energy.
Example 3
In this example, 3.0Kg of Zr powder and 7.0Kg of 7.0KgW powder are weighed, and the other processes are the same as in example 1.
SEM (scanning electron microscope) picture and XRD (X-ray diffraction) pattern of the alloy powder prepared in this example are shown in FIGS. 5 and 6. As can be seen from FIG. 5, the alloy powder particles are irregularly flat, and are finely dispersed, and the average particle diameter is 2.5 to 3.5 μm. As can be seen from FIG. 6, the diffraction peak of Zr has completely disappeared after 20h ball milling, only the diffraction peak of W is remained, which shows that Zr is gradually dissolved into W crystal lattice during ball milling, and finally W (Zr) single phase exceeding saturated solid solution is formed. The diffraction peak of W gradually broadened due to the reduction of grain size and the introduction of microscopic strain during ball milling. In the preparation method of the embodiment, Zr is successfully dissolved in W crystal lattices in a solid solution mode, and the Zr with high adiabatic flame temperature and high combustion heat value can realize combustion of W, so that the alloy powder prepared in the embodiment is high-energy-density powder and is easy to combust to release energy.
Example 4
The embodiment provides a preparation method of tungsten/zirconium supersaturated solid solution alloy powder, which specifically comprises the following steps:
weighing 0.5Kg of Zr powder and 9.5Kg of 9.5KgW powder in a nitrogen atmosphere protective glove box, uniformly mixing, and putting into a stainless steel ball milling tank; adding hard alloy balls according to 5 times of the total mass of the tungsten powder and the zirconium powder, wherein the mass ratio of the hard alloy balls with the diameters of 3mm, 7mm and 9mm is 6:2.5: 1.5; adding normal hexane according to 5 percent of the total mass of the tungsten powder and the zirconium powder, and sealing the ball-milling tank. The ball milling equipment adopts a planetary ball mill, the ball milling mode adopts intermittent ball milling, namely, the ball milling is suspended for 5min and reversed for 5min every time the ball milling is carried out for 5min, the circulation is carried out, and the ball milling is carried out for 5h at the rotating speed of 200r/min in nitrogen atmosphere; adding absolute ethyl alcohol according to 3% of the total mass of the tungsten powder and the zirconium powder, sealing, and continuing to perform ball milling for 5 hours at the rotating speed of 200 r/min; anhydrous ethanol was added once every 5h of ball milling, for a total of 10h in this example. After the ball milling is finished, standing and cooling to room temperature, and taking out alloy powder in a nitrogen atmosphere protective glove box, wherein the average grain diameter of the alloy powder is 1-4 microns.
Example 5
The embodiment provides a preparation method of tungsten/zirconium supersaturated solid solution alloy powder, which specifically comprises the following steps:
weighing 4.0Kg of Zr powder and 6.0Kg of 6.0KgW powder in an argon atmosphere protective glove box, uniformly mixing, and putting into a stainless steel ball milling tank; adding a mixed grinding ball of a hard alloy ball and a stainless steel ball according to 20 times of the total mass of the tungsten powder and the zirconium powder, wherein the mass ratio of the grinding balls with the diameters of 3mm, 5mm, 7mm and 10mm is 5:3:1: 1; adding methanol according to 4 percent of the total mass of the tungsten powder and the zirconium powder, and sealing the ball milling tank. The ball milling equipment adopts a planetary ball mill, the ball milling mode adopts intermittent ball milling, namely, the ball milling is suspended for 5min and reversed for 5min every time the ball milling is carried out for 5min, the circulation is carried out, and the ball milling is carried out for 5h at the rotating speed of 250r/min under the argon atmosphere; adding absolute ethyl alcohol according to 3% of the total mass of the tungsten powder and the zirconium powder, sealing, and continuing to perform ball milling for 5 hours at the rotating speed of 250 r/min; anhydrous ethanol was added once every 5h of ball milling, for a total of 30h in this example. After the ball milling is finished, standing and cooling to room temperature, and taking out alloy powder in an argon atmosphere protective glove box, wherein the average grain diameter of the alloy powder is 1-4 microns.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A tungsten/zirconium supersaturated solid solution alloy powder, wherein said alloy powder consists of tungsten and zirconium; the mass fraction of zirconium in the alloy powder is 5-40%.
2. The tungsten/zirconium supersaturated solid solution alloy powder according to claim 1 wherein the average particle diameter of said alloy powder is 1 to 4 μm.
3. A preparation method of tungsten/zirconium supersaturated solid solution alloy powder is characterized by comprising the following steps:
s1: according to the mass ratio (60-95): (5-40) weighing tungsten and zirconium as raw materials, uniformly mixing, and putting into a ball milling tank;
s2: adding grinding balls according to the ratio (5:1) - (20:1) of the mass of the grinding balls to the total mass of the raw material tungsten and the raw material zirconium, adding a process control agent according to 3-5% of the total mass of the raw material tungsten and the raw material zirconium, and sealing a ball milling tank;
s3: and ball-milling for 10-30 h at the rotating speed of 200-250 r/min in an inert atmosphere to obtain the tungsten/zirconium supersaturated solid solution alloy powder.
4. The method for producing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 1, wherein in S1, the purity of the raw material tungsten is more than 99.0%, and the particle diameter is 1 to 4 μm; the purity of the raw material zirconium is more than 99.0%, and the particle size is 35-40 mu m.
5. The method for producing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 1, wherein in said S2, said grinding balls are at least one of cemented carbide balls and stainless steel balls.
6. The method for producing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 1 or 5, wherein the grinding balls comprise grinding balls having different particle diameters, and the mass ratios of the grinding balls having different particle diameters are different from each other.
7. The method of preparing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 6 wherein the process control agent is an organic solvent.
8. The method for producing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 7, wherein the organic solvent is at least one of absolute ethyl alcohol, n-hexane, methanol and acetone.
9. The method for preparing the tungsten/zirconium supersaturated solid solution alloy powder according to claim 1, wherein in the step S3, the ball milling is performed by a batch ball milling method, specifically:
ball milling is carried out for 5min, the suspension is carried out for 5min, and then the ball milling is carried out for 5min in the reverse direction.
10. The method for preparing a tungsten/zirconium supersaturated solid solution alloy powder according to claim 9 wherein the process control agent is added in the same amount as in S2 every 5 hours of ball milling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911263343.6A CN111826566B (en) | 2019-12-11 | 2019-12-11 | Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911263343.6A CN111826566B (en) | 2019-12-11 | 2019-12-11 | Tungsten/zirconium supersaturated solid solution alloy powder and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111826566A true CN111826566A (en) | 2020-10-27 |
| CN111826566B CN111826566B (en) | 2021-10-29 |
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| CN112877577A (en) * | 2021-01-12 | 2021-06-01 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
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| CN112877577A (en) * | 2021-01-12 | 2021-06-01 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
| CN112877577B (en) * | 2021-01-12 | 2022-02-08 | 中国人民解放军国防科技大学 | Tungsten/zirconium-zinc alloy and preparation method thereof |
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