CN117467880A - Sintered tungsten-based material with high strength and high heat conductivity, and preparation method and application thereof - Google Patents
Sintered tungsten-based material with high strength and high heat conductivity, and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 72
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 49
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000010937 tungsten Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 85
- 238000005245 sintering Methods 0.000 claims abstract description 36
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 23
- 239000000956 alloy Substances 0.000 claims abstract description 23
- 238000012216 screening Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 15
- 238000007731 hot pressing Methods 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 3
- 230000001808 coupling effect Effects 0.000 abstract description 5
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 235000013619 trace mineral Nutrition 0.000 abstract description 5
- 239000011573 trace mineral Substances 0.000 abstract description 5
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 238000005275 alloying Methods 0.000 description 16
- 238000005728 strengthening Methods 0.000 description 10
- 238000007792 addition Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 229910001080 W alloy Inorganic materials 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000013001 point bending Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 230000036316 preload Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 238000007545 Vickers hardness test Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 instruments Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007962 solid dispersion Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052722 tritium Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
Abstract
The invention relates to the technical field of powder metallurgy preparation, and particularly discloses a sintered tungsten-based material with high strength and high heat conductivity, a preparation method and application thereof, wherein AKS-W powder and pure W powder are used as raw materials to prepare target alloy, the alloy is sequentially subjected to ball milling, powder screening and vacuum hot-pressing sintering to prepare the target alloy, the sintered tungsten-based material contains Al, si, O and K elements, the particle size is 2-5 mm, and K bubbles with submicron size are dispersed and distributed; the sintered body has a Vickers hardness of 450-500, a thermal conductivity of (160-168) W/mK, and a flexural strength at room temperature exceeding 1.7GPa. The sintering tungsten-based material is doped with micro/trace elements of Al, si, O and K, and the high-strength and high-thermal-conductivity W material is formed by the synergistic effect and the coupling effect of the elements of Al, si, O and K and W.
Description
Technical Field
The invention relates to the technical field of powder metallurgy preparation, in particular to a sintered tungsten-based material with high strength and high heat conductivity, a preparation method and application thereof.
Background
Tungsten has good heat conduction capability and high temperature performance, has the characteristics of low physical sputtering rate, low tritium retention, low neutron activation and the like, and has great application potential in the engineering fields of aerospace, electronic packaging, military equipment, nuclear energy and the like. The high-temperature structural stability and performance optimization of the W material are important points of attention at present.
Alloying is an important means of improving the properties of W materials. However, the addition of alloying elements also causes deterioration of the thermal conductivity of the material. Therefore, in order to obtain a tungsten material having both high thermal conductivity and good strength, people face the dilemma of achieving the strengthening effect and avoiding the deterioration of the thermal conductivity of the W material.
Alloying additions can be largely classified into two major categories, solid solution and dispersion strengthening, depending on the dominant mechanism of material strengthening. Wherein, the solid solution type additive element has the effects of strengthening alloy and improving high temperature and processability of the material; whereas dispersion-strengthened additives (typically oxide, carbide or nitride particles) have significant effects in improving the strength of the alloy. The existing results show that: the additive can only produce the effect of reinforcing material when a certain additive amount (more than 0.1 wt.%) is reached. Accordingly, it has been considered that conventional microalloying is difficult to achieve the strengthening of the W material, and thus little research has been conducted on the trace/microalloying addition of W. Only when preparing WK alloy, the micro/trace doping technology of alloying element is utilized, but the purpose is only to obtain K bubble reinforcement, and other elements such as Al, si, O and the like in the doped carrier are regarded as harmful impurities, and are volatilized and removed as far as possible through high-temperature (above 2100 ℃) hydrogen sintering.
Disclosure of Invention
The invention aims to provide a sintered tungsten-based material with high strength and high heat conductivity, which is doped with micro/trace Al, si, O and K elements, and is a high-strength and high-heat conductivity W material formed by the synergistic and coupling effects of the Al, si, O and K elements and W.
In addition, the invention also provides the sintered tungsten-based material, a preparation method and application thereof.
The invention is realized by the following technical scheme:
the sintered tungsten-based material with high strength and high heat conductivity is characterized in that AKS-W powder and pure W powder are used as raw materials to prepare target alloy, the alloy is sequentially subjected to ball milling, powder screening and vacuum hot-pressing sintering to prepare the sintered tungsten-based material, and the sintered tungsten-based material contains Al, si, O and K elements and is distributed with tiny K bubbles.
The AKS-W powder and the pure W powder are both commercial products; the fine K bubbles are specifically K bubbles having a size of less than 0.1 μm.
The AKS-W powder contains micro/trace elements of Al, si, O and K, and the elements of Al, si, O and K are kept through controlling a vacuum hot-pressing sintering process, namely the sintered tungsten-based material prepared by the invention is doped with micro/trace elements of Al, si and O, and the high-strength and high-thermal conductivity W material is formed through the synergistic and coupling effects of the elements of Al, si, O and K and W.
The sintered tungsten-based material prepared by the invention breaks the following conventional thinking and overcomes the technical bias:
1) The effective strengthening of the W material cannot be realized when the addition amount of the alloying elements is less than 0.1wt.%, and the alloying elements (Al, si, O and K elements) in the invention are micro/trace, so that the strengthening effect on the W material can be realized.
2) Al, si and O are always regarded as harmful impurities, and can cause the performance degradation of the W material, and by adding micro/trace alloying elements (Al, si, O and K elements), the thermal conductivity of the prepared sintered tungsten-based material is (160-168) W/m.K, namely the thermal conductivity is close to pure W, the strength is greatly increased, and the Vickers hardness is 450-500; the flexural strength at room temperature exceeds 1.7GPa.
Further, the grain size of the sintered tungsten-based material is 2-5 mm; the K bubbles are submicron in size.
Further, the mass ratio of AKS-W powder in the target alloy is (40-80) wt%.
Further, the particle sizes of AKS-W powder and pure W powder are equivalent; the particle sizes of AKS-W powder and pure W powder are 2.5-3.5mm.
Further, the nominal concentrations of Al, si, O and K elements in the AKS-W powder are all ppm.
Further, the Vickers hardness of the sintered tungsten-based material is 450-500 HV, the thermal conductivity of the sintered tungsten-based material is (160-168) W/m.K, and the bending strength at room temperature is more than 1.7GPa.
A preparation method of a sintered tungsten-based material comprises the following steps:
s1, mixing AKS-W powder and pure W powder in proportion to prepare a target alloy;
s2, performing ball milling treatment on the target alloy obtained in the step S1 to obtain initial powder;
s3, screening the initial powder obtained in the step S2 to obtain final powder;
and S4, carrying out vacuum hot-pressing sintering on the final powder obtained in the step S3 to obtain the sintered tungsten-based material.
Further, in step S3, the initial powder is put into a sieving machine attached with 50 mesh, 100 mesh and 200 mesh sieves, and the sieves are placed from top to bottom in 50 mesh, 100 mesh and 200 mesh.
Further, the process of vacuum hot press sintering includes two stages:
the sintering temperature in the first stage is 1100-1200 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60 min; the sintering temperature in the second stage is 1650-1750 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60-120 min.
The invention ensures that the prepared sintered tungsten-based material retains Al, si and O elements by controlling the sintering process of vacuum hot-pressing sintering, which is different from the prior conventional technology, and volatilizes the Al, si and O which are considered as harmful elements by controlling the sintering process of vacuum hot-pressing sintering.
The application of the sintered tungsten-based material in preparing heat conduction products, wherein the heat conduction products comprise fusion reactor materials and materials with high strength and high heat conduction performance in the engineering fields of aerospace, electronic packaging, military equipment, nuclear energy and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the AKS-W powder is used as a pure W powder additive carrier, so that the uniform addition and distribution of micro/trace alloying elements are realized, and the comprehensive synergistic strengthening effect of the micro/trace alloying elements is finally achieved; the coupling action of the alloying elements of Al, si, O and K with the ppm level content in the W matrix realizes the remarkable strengthening effect of the W material; the micro/trace addition of alloying elements not only realizes the remarkable reinforcement of the W material, but also ensures that the W material maintains the excellent heat conduction performance of nearly pure W, thereby providing a new way for developing the high-strength W material with excellent heat conduction performance.
Drawings
The accompanying drawings, which are included to provide a further understanding of embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiments of the invention. In the drawings:
FIG. 1 is a sectional Scanning Electron Microscope (SEM) topography of a sintered body in example 1 of the present invention;
FIG. 2 is a three-point bending line of a sintered body sample in example 1 of the present invention;
FIG. 3 is a sectional Scanning Electron Microscope (SEM) topography of the sintered body in example 2 of the present invention;
FIG. 4 is a three-point bending line of a sintered body sample in example 2 of the present invention.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be described in further detail with reference to the following examples, which are illustrative embodiments of the present invention and the description thereof are intended to be illustrative of the present invention and not limiting of the present invention, and the examples described below are some, but not all, examples of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that: no such specific details are necessary to practice the invention. In other instances, well-known structures, materials, or methods have not been described in detail in order to avoid obscuring the present invention. Materials, instruments, reagents and the like used in the following examples are commercially available unless otherwise specified. The technical means used in the examples, unless otherwise specified, are conventional means well known to those skilled in the art.
The existing W materials are as follows: (a) The effective strengthening of the W material cannot be realized when the addition amount of the alloying element is less than 0.1 wt.%; (b) Al, si, O have been considered as deleterious impurities, leading to degradation of W material properties; and (c) the existing high-strength W alloy is generally difficult to combine with the problems of high heat conductivity and the like.
In order to solve the problems, the embodiment provides a sintered tungsten-based material with high strength and high heat conductivity, which is prepared by taking AKS-W powder and pure W powder as raw materials to prepare a target alloy, sequentially performing ball milling, powder screening and vacuum hot-pressing sintering on the alloy, wherein the sintered tungsten-based material contains alloying components consisting of Al, si, O and K elements, the nominal total content of the alloying components is 100-500 ppm, and fine K bubbles are distributed. The relative density of the sintered tungsten-based material is 98.0-99.0%; the grain size of the sintered tungsten-based material is 2-5 mm; wherein K bubbles with submicron size are dispersed. The Vickers hardness of the sintered tungsten-based material is 450-500, the thermal conductivity is (160-168) W/m.K, and the bending strength at room temperature is more than 1.7GPa.
Wherein the mass ratio of AKS-W powder in the target alloy is (40-80 wt.%; the nominal concentrations of Al, si, O and K elements in the AKS-W powder are all ppm. The particle sizes of the AKS-W powder and the pure W powder are equivalent; the particle sizes of AKS-W powder and pure W powder are 2.5-3.5mm.
AKS-W powder and pure W powder are both commercial products.
Wherein, the purity of the commercial pure W powder is more than 99.999 percent, the particle size is 2.8 mu m, the particle size of AKS-W powder is 3.1mm, and the commercial pure W powder contains the following chemical components: 50ppm, K:130 ppm, si:300ppm, O:520 ppm.
The preparation method of the sintered tungsten-based material in the embodiment comprises the following steps:
s1, mixing AKS-W powder and pure W powder according to a proportion to prepare a target alloy:
the commercial pure W powder (2.8 mu m, purity > 99.999%) is used as a material matrix raw material, custom AKS-W powder (3.1 mm,Al:50 ppm,K:130 ppm,Si:300ppm,O:520 ppm) with similar particle size is selected as a micro/trace alloying carrier additive, and a target W alloy is weighed and prepared, wherein the general formula of the component is W+ (40-80) wt.% AKS-W.
S2, performing ball milling treatment on the target alloy obtained in the step S1 to obtain initial powder:
and (3) loading the target alloy and grinding balls (the ball-ball ratio is 1:8-1:20) into a ball milling tank, filling argon, sealing, putting into a ball mill, performing ball milling at the rotating speed of 150-200 rpm for 1-2 h so as to uniformly mix the alloy raw material powder, and finally obtaining the initial powder.
S3, screening the initial powder obtained in the step S2 to obtain final powder:
placing the initial powder into a sieving instrument with 50 mesh, 100 mesh and 200 mesh sieves, placing the sieves from top to bottom, placing the powder into the 50 mesh sieves, and fixing the powder and the sieves on the sieving instrument together with the 50 mesh sieves with a cover on the top of the 50 mesh sieves; the screening time of the screening instrument is 10-30min, the interval time is 1-5s, the amplitude is 1-4mm, and the whole screening process is circulated for 3 times, so that the final powder is obtained.
S4, carrying out vacuum hot-pressing sintering on the final powder obtained in the step S3 to obtain a sintered tungsten-based material:
the preload pressure is 30MPa, and the vacuum degree is (1-2) multiplied by 10 -2 Pa, heating rate is 15 ℃/min; the sintering temperature in the first stage is 1100-1200 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60 min; the sintering temperature in the second stage is 1650-1750 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60-120 min. And then furnace cooling to room temperature, taking out a sintered body sample, and carrying out density, morphology, composition, hardness, three-point bending and heat conduction performance characterization.
The AKS-W powder of the embodiment contains micro/trace elements of Al, si, O and K, and the elements of Al, si, O and K are kept through controlling the vacuum hot-pressing sintering process, namely the sintered tungsten-based material prepared by the invention is doped with micro/trace elements of Al, si and O, and the high-strength and high-thermal conductivity W material is formed through the synergistic and coupling effects of the elements of Al, si, O and K and W.
Example 1:
preparing a W-50wt.% AKS-W sintered tungsten-based material comprising the steps of:
s1, weighing commercial pure W powder (2.8 mu m, purity is more than 99.999%) and AKS-W powder (3.1 mm,Al:50 ppm,K:130 ppm,Si:300ppm,O:520 ppm) serving as raw materials according to the proportion of W to AKS-W=1:1, and preparing the target W alloy with the composition of W+50wt.% AKS-W.
S2, loading the powder raw materials and grinding balls (the ball ratio is 1:20) into a ball milling tank, filling argon, sealing, putting into a ball mill for ball milling, wherein the rotation speed of the ball mill is 200rpm, and the ball milling time is 2h, so as to obtain initial powder.
S3, placing the initial powder into a sieving instrument with 50-mesh, 100-mesh and 200-mesh sieves, placing the sieves from bottom to top, placing the powder into the 50-mesh sieves, and fixing the powder and the sieve together on the sieving instrument, wherein the top of the 50-mesh sieves is provided with a cover; the screening time of the screening instrument is 20min, the interval time is 2s, the amplitude is 1mm, and the whole screening process is circulated for 3 times, so that the final powder is obtained.
S4, placing the final powder into a vacuum hot-pressing sintering furnace for sintering. The preload pressure is 30MPa, and the vacuum degree is 1 multiplied by 10 -2 Pa. In the first stage, the temperature is raised to 1200 ℃ and is kept for 60 min; and in the second stage, the temperature is raised to 1650 ℃, the temperature is kept for 120min, and the pressure during the two-stage heat-preservation sintering is 70MPa. The heating rate in the whole process is 15 ℃/min. And then furnace cooling to room temperature, taking out a sintered body sample, and carrying out density, morphology, hardness and mechanical property characterization.
The density of the sintered W sample is 98.0% by a drainage method; the measured K, al, si and O contents in the samples were 60ppm, 23ppm, 110ppm and 286ppm, respectively, which are close to the nominal addition. FIG. 1 shows a Scanning Electron Microscope (SEM) morphology of a sintered body section, from which it can be seen that the average size of the matrix W grains is about 2-4 μm, in which fine (0.1 μm) K bubbles are uniformly distributed;
the results of the vickers hardness test at room temperature show that: the hardness (HV 30) of the sintered body is 500 HV, which is far higher than that of the known pure W (< 350) and various W alloy (< 400) sintered bodies; the room temperature three-point bending strength of the sample is up to 1784MPa, as shown in figure 2; further room temperature heat conduction experiment results show that: the thermal conductivity of this sample was 163W/mK, which was close to that of commercially pure W (172W/mK).
Example 2:
preparing a W-40wt.% AKS-W sintered tungsten-based material comprising the steps of:
s1, weighing commercial pure W powder (2.8 mu m, purity is more than 99.999%) and AKS-W customized powder (3.1 mm,Al:50 ppm,K:130 ppm,Si:300ppm,O:520 ppm) serving as raw materials according to the proportion of W to AKS-W=3:2, and preparing a target W alloy with the composition of W+40wt.% AKS-W.
S2, loading the powder raw materials and grinding balls (the ball ratio is 1:12) into a ball milling tank, filling argon, sealing, putting into a ball mill for ball milling, wherein the rotation speed of the ball mill is 180rpm, and the ball milling time is 1.5h, so as to obtain initial powder.
S3, placing the initial powder into a sieving instrument with 50-mesh, 100-mesh and 200-mesh sieves, placing the sieves from bottom to top, placing the powder into the 50-mesh sieves, and fixing the powder and the sieve together on the sieving instrument, wherein the top of the 50-mesh sieves is provided with a cover; the screening time of the screening instrument is 20min, the interval time is 2s, the amplitude is 2mm, the whole screening process is circulated for 3 times, and finally the final powder is obtained.
S4, placing the final powder into a vacuum hot-pressing sintering furnace for sintering. The preload pressure is 30MPa, and the vacuum degree is 1 multiplied by 10 -2 Pa. In the first stage, the temperature is raised to 1150 ℃ and the temperature is kept for 60 min, and the pressure is 70MPa; in the second stage, the temperature is raised to 1750 ℃, the temperature is kept for 90min, and the pressure during heat preservation and sintering is 70MPa. The heating rate in the whole process is 15 ℃/min. And then furnace cooling to room temperature, taking out a sintered body sample, and carrying out density, morphology, hardness and mechanical property characterization.
The density of the sintered W sample is 98.5% measured by a drainage method; the measured K, al, si and O contents in the samples were 50ppm, 16ppm, 90ppm and 245ppm, respectively, which are close to the nominal addition. FIG. 3 shows that the average size of the matrix W grains in the scanning electron microscope is about 3-5 μm, and fine K bubbles (0.1 μm) are distributed in the matrix W grains; the sintered body has a vickers hardness (HV 30) of 475 HV measured at room temperature, and the sample has a room temperature three-point bending strength of up to 1700MPa shown in fig. 4; the thermal conductivity of the sample was found to be 166W/mK, which is close to that of commercially pure W (172W/mK).
The above results indicate that: the invention successfully prepares the high-strength sintered W material with excellent heat conduction capacity by utilizing the micro/trace alloying technology and the vacuum hot-pressing sintering technology.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (10)
1. The sintered tungsten-based material with high strength and high heat conductivity is characterized in that AKS-W powder and pure W powder are used as raw materials to prepare target alloy, the alloy is sequentially subjected to ball milling, powder screening and vacuum hot-pressing sintering to prepare the sintered tungsten-based material, and the sintered tungsten-based material contains Al, si, O and K elements and K bubbles are distributed.
2. The sintered tungsten-based material with high strength and high heat conductivity according to claim 1, wherein the sintered tungsten-based material has a grain size of 2-5 mm; the K bubbles are submicron in size.
3. The sintered tungsten-based material with high strength and high heat conductivity according to claim 1, wherein the mass ratio of AKS-W powder in the target alloy is (40-80 wt.%).
4. The sintered tungsten-based material with both high strength and high thermal conductivity according to claim 1, wherein the particle size of AKS-W powder and pure W powder is 2.5-3.5mm.
5. The sintered tungsten-based material with high strength and high thermal conductivity according to claim 1, wherein the nominal concentrations of Al, si, O and K elements in the AKS-W powder are ppm.
6. The sintered tungsten-based material with high strength and high heat conductivity according to any one of claims 1 to 5, wherein the sintered tungsten-based material has a vickers hardness of 450 to 500 HV, a thermal conductivity of (160 to 168) W/m-K, and a flexural strength at room temperature of more than 1.7GPa.
7. A method of preparing a sintered tungsten based material according to any one of claims 1 to 6, comprising the steps of:
s1, mixing AKS-W powder and pure W powder in proportion to prepare a target alloy;
s2, performing ball milling treatment on the target alloy obtained in the step S1 to obtain initial powder;
s3, screening the initial powder obtained in the step S2 to obtain final powder;
and S4, carrying out vacuum hot-pressing sintering on the final powder obtained in the step S3 to obtain the sintered tungsten-based material.
8. The method according to claim 7, wherein in step S3, the initial powder is put into a sieving machine with 50 mesh, 100 mesh and 200 mesh sieves attached thereto for sieving treatment, and the sieves are placed from top to bottom in 50 mesh, 100 mesh and 200 mesh.
9. The method according to claim 7, wherein the vacuum hot press sintering process in step S4 comprises two stages:
the sintering temperature in the first stage is 1100-1200 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60 min; the sintering temperature in the second stage is 1650-1750 ℃, the sintering pressure is 70MPa, and the heat preservation time is 60-120 min.
10. Use of a sintered tungsten based material according to any of claims 1-6 for the preparation of a heat conductive product.
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