CN114318100A - Silver-doped tungsten-copper composite material and preparation method thereof - Google Patents
Silver-doped tungsten-copper composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 73
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 10
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 60
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- 239000002994 raw material Substances 0.000 claims abstract description 25
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- 238000001764 infiltration Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 16
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 14
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 14
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008117 stearic acid Substances 0.000 claims abstract description 14
- 238000005238 degreasing Methods 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 10
- 229910000881 Cu alloy Inorganic materials 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
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- 238000003892 spreading Methods 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- KYIDJMYDIPHNJS-UHFFFAOYSA-N ethanol;octadecanoic acid Chemical compound CCO.CCCCCCCCCCCCCCCCCC(O)=O KYIDJMYDIPHNJS-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 abstract description 41
- 229910052802 copper Inorganic materials 0.000 abstract description 14
- 229910052721 tungsten Inorganic materials 0.000 abstract description 8
- 238000004100 electronic packaging Methods 0.000 abstract description 6
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 239000010937 tungsten Substances 0.000 abstract description 5
- 239000006104 solid solution Substances 0.000 abstract description 2
- 229910017944 Ag—Cu Inorganic materials 0.000 description 15
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- 238000003756 stirring Methods 0.000 description 9
- 238000005303 weighing Methods 0.000 description 8
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- 229910003460 diamond Inorganic materials 0.000 description 6
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- 229910000831 Steel Inorganic materials 0.000 description 3
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- 239000011521 glass Substances 0.000 description 3
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- 239000011259 mixed solution Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- UYKQQBUWKSHMIM-UHFFFAOYSA-N silver tungsten Chemical compound [Ag][W][W] UYKQQBUWKSHMIM-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- ITZSSQVGDYUHQM-UHFFFAOYSA-N [Ag].[W] Chemical compound [Ag].[W] ITZSSQVGDYUHQM-UHFFFAOYSA-N 0.000 description 1
- BRDCEPWSRLDLST-UHFFFAOYSA-N [W].[Cu].[Ag] Chemical compound [W].[Cu].[Ag] BRDCEPWSRLDLST-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a silver-doped tungsten-copper composite material, which is prepared by doping tungsten-copper alloy with silver, wherein the thermal conductivity is 197-. The invention also discloses a preparation method of the silver-doped tungsten-copper composite material, which adopts pretreated tungsten powder, copper powder and silver powder as raw materials, wherein the pretreated tungsten powder is obtained by adding stearic acid into tungsten powder and heating; the method specifically comprises the following steps: pressing, degreasing and sintering part of the raw materials to obtain a framework, and uniformly paving the rest raw materials on the framework for infiltration to obtain the silver-doped tungsten-copper composite material. According to the invention, silver is added into a tungsten-copper system to form a solid solution with copper, so that the wettability between tungsten and copper is improved, the thermal conductivity of the tungsten-copper composite material is expected to be improved, and the heat dissipation requirement of the tungsten-copper composite material applied to the field of electronic packaging is better met.
Description
Technical Field
The invention relates to the technical field of tungsten-copper composite materials, in particular to a silver-doped tungsten-copper composite material and a preparation method thereof.
Background
Today, as modern industry develops at a high speed, electronic packaging materials realize protection of chips, CPUs (central processing units) and large-scale circuits, the packaging materials can protect components from physical damage and corrosion of harmful gases, and meanwhile, high thermal conductivity ensures heat dissipation of electronic elements. Since the electronic packaging material plays a role in heat dissipation and matrix protection, it is critical to improve the thermal conductivity of the electronic packaging material.
Tungsten (W) has high melting point, high density, high strength, low thermal expansion coefficient, and copper (Cu) has good electrical and thermal conductivity. The W-Cu composite material can integrate the characteristics of W and Cu, has the advantages of higher thermal conductivity, adjustable thermal expansion coefficient and the like, and is an ideal heat dissipation material applied to the field of electronic packaging at present. However, the thermal conductivity of the W-Cu composite material is still not high, and further improvement of the thermal conductivity of the composite material becomes one of the problems to be solved. The element is doped in the W-Cu composite material, so that the wettability between W and Cu can be improved, and the thermal conductivity of the W-Cu composite material can be improved.
In patent CN105238983A "a rare earth oxide doped tungsten-copper composite material and a method for preparing the same", lie suo wen et al, the density of the W-Cu composite material is improved by doping rare earth oxide into the W-Cu composite material, so that the electric conductivity and the thermal conductivity of the final W-Cu composite material are improved.
Weichenlong et al in patent CN109175354A "preparation method of a Diamond/W-Cu composite", a W-Cu composite is prepared by doping tungsten-plated diamond to make the thermal conductivity of the final Diamond/W-Cu composite reach 275 W.m-1·K-1。
However, the thermal conductivity of the existing doped W-Cu composite material still cannot meet the actual requirement, and the relationship between the existing doped material and the W-Cu composite material is still unclear, and those skilled in the art cannot guess which material can be used to improve the thermal conductivity of the W-Cu composite material.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a silver-doped tungsten-copper composite material and a preparation method thereof.
A silver-doped tungsten-copper composite material is prepared by doping tungsten-copper alloy with silver, and the thermal conductivity is 197-226W/(m.K).
The preparation method of the silver-doped tungsten-copper composite material adopts the pretreated tungsten powder, the copper powder and the silver powder as raw materials, and the pretreated tungsten powder is obtained by adding stearic acid into the tungsten powder and heating;
the method specifically comprises the following steps: pressing, degreasing and sintering part of the raw materials to obtain a framework, and uniformly paving the rest raw materials on the framework for infiltration to obtain the silver-doped tungsten-copper composite material.
Preferably, the pretreated tungsten powder is prepared by the following steps: and heating the tungsten powder in water bath, adding a stearic acid ethanol solution, continuously heating until ethanol is completely volatilized, and drying by hot air to obtain the pretreated tungsten powder.
Preferably, the tungsten powder has a particle size of 5 μm, and the mass ratio of the tungsten powder to the stearic acid is 100: 2-3, wherein the mass-volume ratio g/mL of stearic acid to ethanol is 1: 21.
preferably, the water bath heating temperature is 58-62 ℃, the hot air drying temperature is 58-62 ℃, and the hot air drying time is 7-9 h.
Specifically, if the partial raw materials are the pretreated tungsten powder and the silver powder, the mass ratio of the pretreated tungsten powder to the silver powder is 7-9: 1-3, and the rest raw materials are copper powder;
if the partial raw materials are pretreated tungsten powder, silver powder and copper powder, the rest raw materials are copper powder, and the ratio of the sum of the total consumption of the silver powder and the copper powder to the total consumption of the tungsten powder is 10-20: 80-90 percent, wherein the amount of the copper powder in the partial raw materials accounts for 10-15 percent of the total amount of the copper powder;
if the partial raw materials are pretreated tungsten powder, the rest raw materials are silver powder and copper powder, and the mass ratio of the silver powder to the copper powder is 1-2: 1-2.
Preferably, the pressing pressure is 200 +/-5 MPa, and the pressing time is 30 +/-5 s; the degreasing temperature is 400 +/-5 ℃, and the degreasing time is 60 +/-5 min.
Preferably, the specific operation of sintering is as follows: placing the degreased material in a tube furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen gas at the flow rate of 0.3-0.5L/min, heating to 1000 ℃ at the speed of 10 +/-0.5 ℃/min, heating to 1300 ℃ at the speed of 5 +/-0.5 ℃/min, preserving heat for 120 +/-5 min, cooling to 500 ℃ at the speed of 5 +/-0.5 ℃/min, and cooling to room temperature along with the furnace.
Preferably, the specific operation of infiltration is as follows: uniformly spreading the rest raw materials on the framework, placing in a tubular furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen gas at a flow rate of 0.3-0.5L/min, heating to 1000 deg.C at 10 + -0.5 deg.C/min, heating to 1250 deg.C at 5 + -0.5 deg.C/min, maintaining the temperature for 120 + -5 min, cooling to 500 deg.C at 5 + -0.5 deg.C/min, and cooling to room temperature with the furnace.
And measuring the density of the skeleton before infiltration, calculating the porosity according to a theoretical porosity calculation formula of the composite material, and calculating the using amount of the infiltration material according to the porosity calculation formula.
W-Cu composite is a typical pseudo-alloy because tungsten and copper are not solid-soluble with each other and do not form mesophase compounds. Therefore, although the W-Cu composite material has been industrially produced and applied, the poor wettability between W and Cu limits the thermal conductivity thereof.
As mentioned in the background, the relationship between the existing doped material and the W-Cu composite material is still unclear, and those skilled in the art cannot clearly know what kind of material can be used to increase the thermal conductivity of the W-Cu composite material, and even if the same material is used for doping, the doping amount, the doping temperature and the doping process route all affect the performance of the final composite material.
For example, patent CN109175354A "a method for preparing diamond/W-Cu composite" prepares W-Cu composite by doping tungsten-plated diamond, but if diamond is directly doped without metallization pretreatment, its thermal conductivity is reduced; the literature (Yuan, Zhang Jian, Luo Guoqiang, Sun Yi, Shen Qiang, Zhang Lianming, Low-temperature differentiation and microstructure of W-Cu compositions with Sn additions [ J]The Journal of Materials Research and Technology,2021,10:) states that Sn is used (thermal conductivity is only 67 W.m.)-1·K-1) The W-Cu composite material is doped, and the strength and the thermal property of the doped composite material are improved.
The invention adopts silver powder for doping, aiming at improving the thermal conductivity of the silver, and the silver has high thermal conductivity (heat)The conductivity is as high as 429 W.m-1·K-1) The silver-tungsten composite material can form a solid solution with copper to facilitate infiltration, and the wettability of silver-tungsten is superior to that of tungsten-copper, so that the effect of an active sintering aid is achieved, the sintering compactness of the active sintering aid is promoted, the W-Ag-Cu composite material has higher heat-conducting property, and the heat dissipation requirement of the W-Ag-Cu composite material applied to the field of electronic packaging is better met.
Drawings
FIG. 1 is a microstructure of the surface of W-Ag-Cu obtained by the present invention.
FIG. 2 is the EDS total spectrum of the W-Ag-Cu surface obtained by the present invention.
FIG. 3 is an EDS spectrum of tungsten element in W-Ag-Cu obtained by the present invention.
FIG. 4 is an EDS spectrum of copper element in W-Ag-Cu obtained by the present invention.
FIG. 5 is an EDS spectrum of silver element in W-Ag-Cu obtained by the present invention.
FIG. 6 is a graph showing the thermal conductivity of the W-Ag-Cu composite obtained according to the doping amount of silver (mass ratio of silver powder to pretreated tungsten powder in step (2)) in example 1.
FIG. 7 shows the amount of Ag doped and the W-Ag obtained in example 2x-Cu15-xThermal conductivity line graph of the composite.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example 1
A preparation method of a silver-doped tungsten-copper composite material comprises the following specific steps:
(1) powder pretreatment: weighing a certain amount of tungsten powder, placing the tungsten powder in a magnetic stirring type water bath, heating to 60 ℃, and keeping the temperature for 30 minutes; weighing stearic acid, dissolving in 100mL of ethanol, wherein the mass ratio of tungsten powder to stearic acid is 100: 2.5, stirring by a glass rod to fully dissolve; pouring the ethanol mixed solution of stearic acid into preheated tungsten powder, adding a magnetic rotor, stirring at a constant temperature of 60 ℃ until ethanol is basically volatilized, then placing the tungsten powder into a forced air drying oven, and drying for 8 hours at the temperature of 60 ℃ to obtain pretreated tungsten powder;
(2) mixing powder: respectively mixing silver powder and pretreated tungsten powder according to the mass ratio of 1: 9. 2: 8. 3: 7, putting the mixture into a powder mixer, stirring the mixture for 6 hours at a speed of 300 revolutions per minute, and uniformly mixing the mixture to obtain mixed powder;
(3) pressing a green body: pressing the tungsten-silver composite powder obtained in the step 2 into a skeleton green body by adopting a hydraulic press steel die, wherein the pressing pressure is 200MPa, and the pressure maintaining time is 30 s;
(4) degreasing: placing the skeleton green body obtained in the step 3 in a tube furnace, and preserving heat for 1h at 400 ℃ for degreasing;
(5) and (3) sintering: placing the degreased skeleton green body obtained in the step 4 in a tubular furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen atmosphere (the hydrogen flow rate is 0.3-0.5L/min), heating to 1000 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, preserving heat for 120min, cooling to 500 ℃ at 5 ℃/min after preserving heat, and cooling to room temperature along with the furnace to obtain a skeleton with certain density;
(6) infiltration: measuring the density of the skeleton obtained in the step 5, calculating the copper infiltration amount according to a theoretical porosity calculation formula of the composite material, and uniformly paving copper powder with corresponding mass on the skeleton; the infiltration process is carried out in the hydrogen atmosphere of a tubular furnace (the hydrogen flow rate is 0.3-0.5L/min), the temperature is firstly increased to 1000 ℃ at the speed of 10 ℃/min, then is increased to 1250 ℃ at the speed of 5 ℃/min, the temperature is preserved and infiltrated for 120min at the temperature of 1250 ℃, is reduced to 500 ℃ at the speed of 5 ℃/min after infiltration, and is cooled to the room temperature along with the furnace, thus obtaining the compact W-Ag-Cu composite material.
The W-Ag-Cu composite material obtained in this example was subjected to electron microscope scanning, as shown in FIG. 1. As can be seen from fig. 1: it can be seen that the entire sample surface is dense and no apparently continuous large pores are seen. The W-Ag-Cu composite material obtained in this example was further subjected to elemental analysis, as shown in FIGS. 2 to 5. As can be seen from fig. 2-5: the silver in the composite material is uniformly distributed.
The thermal conductivity of the W-Ag-Cu composite material obtained in this example was measured, as shown in FIG. 6. As can be seen from fig. 6: as the doping amount of silver is increased (the doping amount ratio is the mass ratio of the silver powder to the pretreated tungsten powder in the step (2) of the embodiment), the heat conductivity of the W-Ag-Cu composite material is increased and then reduced, and the maximum value is 226 W.m-1·K-1。
Example 2
A preparation method of a silver-doped tungsten-copper composite material comprises the following specific steps:
(1) powder pretreatment: weighing a certain amount of tungsten powder, placing the tungsten powder in a magnetic stirring type water bath, heating to 60 ℃, and keeping the temperature for 30 minutes; weighing stearic acid, dissolving in 100mL of ethanol, wherein the mass ratio of tungsten powder to stearic acid is 100: 2.5, stirring by a glass rod to fully dissolve; pouring the ethanol mixed solution of stearic acid into preheated tungsten powder, adding a magnetic rotor, stirring at a constant temperature of 60 ℃ until ethanol is basically volatilized, then placing the tungsten powder into a forced air drying oven, and drying for 8 hours at the temperature of 60 ℃ to obtain pretreated tungsten powder;
(2) mixing powder: pretreating tungsten powder, copper powder and silver powder, and weighing the tungsten powder, the copper powder and the silver powder according to the proportion of W-0.5 wt% of Ag-14.5 wt% of Cu, W-1.0 wt% of Ag-14 wt% of Cu, W-1.5 wt% of Ag-13.5 wt% of Cu, W-2.0 wt% of Ag-13.0 wt% of Cu and W-2.5 wt% of Ag-12.5 wt% of Cu;
adding 2 wt% of copper powder, pretreated tungsten powder and silver powder into a powder mixer, stirring for 6 hours at 300 revolutions per minute, and uniformly mixing to obtain mixed powder;
(3) pressing a green body: pressing the tungsten-silver-copper composite powder obtained in the step 2 into a framework green body by adopting a hydraulic press steel die, wherein the pressing pressure is 200MPa, and the pressure maintaining time is 30 s;
(4) degreasing: placing the skeleton green body obtained in the step 3 in a muffle furnace, heating to 400 ℃, and preserving heat for 1h for degreasing;
(5) and (3) sintering: placing the degreased skeleton green body obtained in the step 4 in a tubular furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen atmosphere (the hydrogen flow rate is 0.3-0.5L/min), heating to 1000 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, preserving heat for 120min, cooling to 500 ℃ at 5 ℃/min after preserving heat, and cooling to room temperature along with the furnace to obtain a skeleton with certain density;
(6) infiltration: uniformly spreading the rest copper powder on the framework, carrying out infiltration process in a tubular furnace under hydrogen atmosphere (hydrogen flow rate is 0.3-0.5L/min), firstly heating to 1000 deg.C at 10 deg.C/min, then heating to 1250 deg.C at 5 deg.C/min, carrying out heat preservation infiltration at 1250 deg.C for 120min, cooling to 500 deg.C at 5 deg.C/min, and furnace-cooling to room temperature to obtain compact W-Agx-Cu15-xA composite material.
For W-Ag obtained in this examplex-Cu15-xThe thermal conductivity of the composite was measured as shown in fig. 7. As can be seen from fig. 7: W-Ag along with the increase of the doping amount of silverx-Cu15-xThe heat-conducting property of the composite material is firstly increased and then reduced, and the highest heat-conducting property can be up to 205 W.m-1·K-1Is superior to the prior commercial W-15Cu (the thermal conductivity is 160-190 W.m)-1·K-1)。
Example 3
A preparation method of a silver-doped tungsten-copper composite material comprises the following specific steps:
(1) powder pretreatment: weighing a certain amount of tungsten powder, placing the tungsten powder in a magnetic stirring type water bath, heating to 60 ℃, and keeping the temperature for 30 minutes; weighing stearic acid, dissolving in 100mL of ethanol, wherein the mass ratio of tungsten powder to stearic acid is 100: 2.5, stirring by a glass rod to fully dissolve; pouring the ethanol mixed solution of stearic acid into preheated tungsten powder, adding a magnetic rotor, stirring at a constant temperature of 60 ℃ until ethanol is basically volatilized, then placing the tungsten powder into a forced air drying oven, and drying for 8 hours at the temperature of 60 ℃ to obtain pretreated tungsten powder;
(2) pressing a green body: pressing the pretreated tungsten powder obtained in the step 1 into a skeleton green body by adopting a hydraulic press steel die, wherein the pressing pressure is 200MPa, and the pressure maintaining time is 30 s;
(3) degreasing: placing the skeleton green body obtained in the step (2) in a muffle furnace, and preserving heat for 1h at 400 ℃ for degreasing;
(4) and (3) sintering: placing the degreased skeleton green body obtained in the step (3) in a tubular furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen atmosphere (the hydrogen flow rate is 0.3-0.5L/min), heating to 1000 ℃ at 10 ℃/min, heating to 1300 ℃ at 5 ℃/min, preserving heat for 120min, cooling to 500 ℃ at 5 ℃/min after heat preservation, and cooling to room temperature along with the furnace to obtain a tungsten skeleton with certain density;
(5) mixing powder: measuring the density of the tungsten skeleton obtained in the step (4), calculating the porosity of the tungsten skeleton according to a theoretical porosity calculation formula of the composite material, weighing copper powder and silver powder with corresponding mass (the mass ratio is 1: 1, 2: 1 and 1: 2 respectively), placing the copper powder and the silver powder into a powder mixer, stirring for 8 hours at 300 revolutions per minute, and uniformly mixing;
(6) infiltration: and (5) taking out the composite powder obtained in the step (5), and uniformly paving the composite powder on a tungsten framework. The infiltration process is carried out in the hydrogen atmosphere of a tubular furnace (the hydrogen flow rate is 0.3-0.5L/min), the temperature is firstly increased to 1000 ℃ at the speed of 10 ℃/min, then is increased to 1250 ℃ at the speed of 5 ℃/min, the temperature is preserved and infiltrated for 120min at the temperature of 1250 ℃, is reduced to 500 ℃ at the speed of 5 ℃/min after infiltration, and is cooled to the room temperature along with the furnace, thus obtaining the W-Ag-Cu composite material.
The thermal conductivity of the W-Ag-Cu composite material obtained in the embodiment is tested to be up to 197 W.m-1·K-1。
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A silver-doped tungsten-copper composite material is characterized in that silver is adopted to dope a tungsten-copper alloy, and the thermal conductivity is 197-226W/(m.K).
2. The method for preparing the silver-doped tungsten-copper composite material according to claim 1, wherein the raw materials are pretreated tungsten powder, copper powder and silver powder, and the pretreated tungsten powder is obtained by adding stearic acid into tungsten powder and heating;
the method specifically comprises the following steps: pressing, degreasing and sintering part of the raw materials to obtain a framework, and uniformly paving the rest raw materials on the framework for infiltration to obtain the silver-doped tungsten-copper composite material.
3. The method for preparing the silver-doped tungsten-copper composite material according to claim 2, wherein the tungsten powder is pretreated by the following steps: and heating the tungsten powder in water bath, adding a stearic acid ethanol solution, continuously heating until ethanol is completely volatilized, and drying by hot air to obtain the pretreated tungsten powder.
4. The method for preparing the silver-doped tungsten-copper composite material according to claim 3, wherein the water bath heating temperature is 58-62 ℃, and the hot air drying temperature is 58-62 ℃.
5. The method of preparing the silver-doped tungsten-copper composite material according to claim 2, wherein if the partial raw materials are the pretreated tungsten powder and the silver powder, the mass ratio of the pretreated tungsten powder to the silver powder is 7-9: 1-3, and the rest raw materials are copper powder.
6. The method of claim 2, wherein if the partial raw materials are pretreated tungsten powder, silver powder and copper powder, the rest raw materials are copper powder, and the ratio of the total amount of the silver powder and the copper powder to the total amount of the tungsten powder is 10 to 20: 80-90 percent, wherein the amount of the copper powder in the partial raw materials accounts for 10-15 percent of the total amount of the copper powder.
7. The method for preparing the silver-doped tungsten-copper composite material according to claim 2, wherein if the part of the raw materials is the pretreated tungsten powder, the rest raw materials are silver powder and copper powder, and the mass ratio of the silver powder to the copper powder is 1-2: 1-2.
8. The method of preparing the silver-doped tungsten-copper composite material according to claim 2, wherein the pressing pressure is 200 ± 5Mpa, and the pressing time is 30 ± 5 s; the degreasing temperature is 400 +/-5 ℃, and the degreasing time is 60 +/-5 min.
9. The method of preparing the silver-doped tungsten-copper composite material according to claim 2, wherein the sintering is performed by the following steps: placing the degreased material in a tube furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen gas at the flow rate of 0.3-0.5L/min, heating to 1000 ℃ at the speed of 10 +/-0.5 ℃/min, heating to 1300 ℃ at the speed of 5 +/-0.5 ℃/min, preserving heat for 120 +/-5 min, cooling to 500 ℃ at the speed of 5 +/-0.5 ℃/min, and cooling to room temperature along with the furnace.
10. The method of preparing the silver-doped tungsten-copper composite material according to claim 2, wherein the infiltration is performed by the following steps: uniformly spreading the rest raw materials on the framework, placing in a tubular furnace, vacuumizing the furnace chamber at room temperature, introducing hydrogen gas at a flow rate of 0.3-0.5L/min, heating to 1000 deg.C at 10 + -0.5 deg.C/min, heating to 1250 deg.C at 5 + -0.5 deg.C/min, maintaining the temperature for 120 + -5 min, cooling to 500 deg.C at 5 + -0.5 deg.C/min, and cooling to room temperature with the furnace.
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| CN114833348A (en) * | 2022-05-07 | 2022-08-02 | 合肥工业大学 | Large-scale preparation method of controllable high-quality W-Cu composite powder |
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