CN115612948A - High-strength high-thermal-conductivity tungsten fiber reinforced tungsten-copper alloy and low-cost preparation method thereof - Google Patents
High-strength high-thermal-conductivity tungsten fiber reinforced tungsten-copper alloy and low-cost preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-strength high-heat-conductivity tungsten fiber reinforced tungsten-copper alloy and a low-cost preparation method thereof, and relates to the technical field of new materials. The tungsten-copper alloy comprises 30-80% of tungsten fiber, 5-60% of tungsten powder and 10-20% of copper powder. The tungsten fiber is in a stress-relief annealed state, and has elongated nano-fiber grains or sub-grains with a width of about 100 nm. The length of the tungsten fiber is 3-5 mm, the diameter is 50-150 mu m, the particle sizes of the tungsten powder are two, one is about 3 mu m, the other is about 10 mu m, the mass ratio of the two particle sizes of the tungsten powder is 3:7; the particle size of the copper powder was 3 μm. Has the advantages that: compared with the traditional tungsten-copper alloy, the tungsten fiber reinforced tungsten-copper alloy of the invention adds the tungsten fiber to form a tungsten skeleton, thereby greatly improving the strength and toughness of the tungsten-copper alloy. Compared with a pure tungsten powder matrix, the copper-based composite material has the advantages that the connection interface with copper is reduced, and the heat conduction performance is improved; meanwhile, the obturator and the defect are greatly reduced, and the density of the tungsten-copper alloy is improved.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a tungsten-copper alloy reinforced by high-strength high-heat-conductivity tungsten fibers and a low-cost preparation method thereof.
Background
The tungsten-copper alloy has the characteristics of high heat conductivity, high electric conductivity, low thermal expansion coefficient and the like, and is widely applied to a plurality of high-tech fields such as electronic packaging, electric processing electrodes, aerospace and the like. Because tungsten copper is not dissolved mutually and has large differences of physical properties such as thermal expansion coefficient, the tungsten copper alloy is produced in batches mainly by an infiltration method in the traditional industry. The infiltration method generally comprises the steps of preparing a tungsten framework, raising the temperature to be higher than the melting point of copper, and infiltrating copper into the tungsten framework by utilizing the capillary phenomenon to obtain the tungsten-copper alloy. The tungsten skeleton is easy to form closed pores in the pressing process, so that copper cannot permeate, and the tungsten-copper alloy cannot be completely compact. How to improve the compactness of the tungsten-copper alloy is always a problem to be solved. At present, the method is mainly overcome by doping a binder or doping other trace metals. However, doping with other metal elements can affect the thermal conductivity of the composite. In addition, the mechanical properties of the tungsten skeleton of the common tungsten-copper alloy are low, so that the mechanical properties of the tungsten-copper alloy are also low, and the requirement for rapid development in high-precision advanced technical fields such as aerospace, national defense, new energy, microelectronics and the like cannot be met.
One of the effective methods for improving the comprehensive performance of the tungsten-copper composite material is to use tungsten fibers to replace part of tungsten powder as a framework, and the Chinese patent application publication with the application number of CN 110343978A discloses a short tungsten fiber reinforced CuW composite material with random distribution and a preparation method thereof. However, the method adopts two sintering modes of hot-pressing infiltration, so that the process is complicated and is not beneficial to large-scale industrial production; the mass ratio of the added tungsten fibers is too small, and tungsten powder is still used as a matrix, so that the tungsten-copper interface is too much, the density of a tungsten-copper material is not high, and the situation of poor heat conduction still exists.
Disclosure of Invention
The invention aims to solve the technical problems of low density, poor heat conductivity and poor comprehensive mechanical property of the existing tungsten-copper alloy.
The invention solves the technical problems through the following technical means:
a tungsten-copper alloy reinforced by high-strength high-heat-conductivity tungsten fibers comprises the following components: 30-80% of tungsten fiber, 5-60% of tungsten powder and 10-20% of copper powder by mass.
Has the advantages that: according to the invention, the tungsten fiber, the tungsten powder and the copper powder in a special proportion are selected to prepare the tungsten-copper alloy with better performance, and the compactness of the tungsten-copper alloy is improved and the thermal conductivity and the comprehensive mechanical property of the tungsten-copper alloy are improved through the synergistic effect of the components.
Preferably, the tungsten fibers have a length of 3 to 5mm and a diameter of 50 to 150 μm.
Preferably, the tungsten fibers are in a stress-relieved annealed state, have elongated nanofiber grains or sub-grains, and have a width of 80-120nm.
Preferably, the tungsten powder is a tungsten powder with the particle size of 3 μm and 10 μm, and the mass ratio of the tungsten powder to the powder is 3:7 in a mixture.
Preferably, the particle size of the copper powder is 2-5 μm.
The invention also provides a low-cost preparation method for preparing the high-strength high-thermal-conductivity tungsten fiber reinforced tungsten-copper alloy, which comprises the following steps of:
s1: mixing powder: mixing tungsten fiber, tungsten powder and copper powder according to the mass ratio, adding alcohol dissolved with forming agent stearic acid, and stirring in water bath atmosphere;
s2: profiling: putting the powder processed in the step S1 into a die, and carrying out cold press molding to obtain a green compact body;
s3: and (3) sintering: and (3) sintering the pressed compact obtained in the step (S2) in a hydrogen or vacuum atmosphere to obtain the ceramic material.
Preferably, the adding amount of the stearic acid in the step S1 is 0.5-0.7% of the total mass of the tungsten fiber, the tungsten powder and the copper powder.
Preferably, the temperature of the water bath in the step S1 is 50-70 ℃.
Preferably, the stirring time in the step S1 is 20-40min.
Preferably, the cold pressing pressure in the step S2 is 600-800 MPa, and the cold pressing time is 3-8 min.
Preferably, the sintering temperature in the step S3 is 1100-1200 ℃, and the sintering time is 120-180 min.
The invention has the advantages that:
(1) According to the invention, the tungsten fiber, the tungsten powder and the copper powder in a special proportion are selected to prepare the tungsten-copper alloy with better performance, and the compactness of the tungsten-copper alloy is improved and the thermal conductivity and the comprehensive mechanical property of the tungsten-copper alloy are improved through the synergistic effect of the components.
(2) Compared with the traditional tungsten-copper alloy, the high-strength high-heat-conductivity tungsten fiber reinforced tungsten-copper alloy prepared by the invention is mainly added with tungsten fibers, and plays roles in reinforcing and toughening. Because the tungsten fiber has very high room temperature strength and high temperature strength, the room temperature tensile strength can reach more than 2.8GPa, compared with the tungsten framework prepared by the traditional tungsten powder, the tungsten framework composed of the tungsten fiber has higher strength, and the strength of the tungsten-copper alloy can be further improved. In addition, the tungsten fibers can also play a toughening effect. Therefore, the mechanical property of the tungsten fiber reinforced tungsten-copper alloy prepared by the method is greatly improved compared with that of the traditional tungsten-copper alloy.
(3) Compared with the tungsten framework prepared from pure tungsten powder, the tungsten framework formed by the tungsten fibers and the tungsten powder has smaller contact interface area with copper, the tungsten fibers enhance the heat conduction of the tungsten-copper alloy to be reduced, and the heat conduction performance is better.
(4) The tungsten fibers added in the invention are matched with tungsten powder with different particle sizes, so that the closed porosity of a tungsten framework is reduced, the copper can flow at high temperature, and the density of the tungsten-copper alloy can be effectively improved.
Drawings
FIG. 1 is a schematic structural view of the structure of tungsten fibers added in example 1 of the present invention;
FIG. 2 is a gold phase diagram of a tungsten fiber reinforced tungsten copper alloy of example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of a tungsten fiber reinforced tungsten-copper alloy according to example 1 of the present invention;
FIG. 4 is a gold phase diagram of a tungsten fiber reinforced tungsten copper alloy of example 2 of the present invention;
FIG. 5 is a scanning electron micrograph of a tungsten fiber reinforced tungsten copper alloy according to example 2 of the present invention;
FIG. 6 is a gold phase diagram of a tungsten fiber reinforced tungsten copper alloy of example 3 of the present invention;
FIG. 7 is a SEM of tungsten fiber reinforced tungsten-copper alloy of example 3 of the present invention;
FIG. 8 is a graph showing the stress vs. displacement curves of the W-Cu alloy materials obtained in examples 1-3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
a low-cost preparation method of a high-strength high-heat-conductivity tungsten fiber reinforced tungsten-copper alloy comprises the following steps:
s1: mixing powder: mixing 30g of tungsten fiber, 60g of tungsten powder and 10g of copper powder, adding alcohol dissolved with forming agent stearic acid, heating in water bath at 50 ℃, and stirring for 40min; wherein the tungsten fiber is in a stress relief annealing state, the structure is a slender nanofiber subgrain grain, and the width is 100nm; the length of the tungsten fiber is 3mm, and the diameter of the tungsten fiber is 100 mu m; the tungsten powder is tungsten powder with the particle sizes of 3 mu m and 10 mu m according to the mass ratio of 3:7; the particle size of the copper powder is 3 mu m; the adding amount of stearic acid is 0.5g;
s2: profiling: placing the powder processed in the step S1 in a steel mold, and performing cold press molding at room temperature under the pressure of 800MPa for 2min to obtain a green compact;
s3: and (3) sintering the pressed compact obtained in the step (S2) in a vacuum atmosphere at the temperature of 1200 ℃ for 120min.
Fig. 1 is a schematic structural diagram of the structure of the added tungsten fiber, and it can be seen from the diagram that the tungsten fiber is elongated and has sub-grains with the width of about 100 nm.
Fig. 2 is a metallographic image of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example, and fig. 3 is a scanning electron micrograph of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example. As can be seen from fig. 2-3, the resulting tungsten-copper alloy structure is relatively compact.
The tungsten-copper alloy prepared by the embodiment has the compactness of 99.2 percent, the heat conduction of 198 (W/(m.K)), and the bending strength of 830MPa.
Example 2:
a low-cost preparation method of a high-strength high-heat-conductivity tungsten fiber reinforced tungsten-copper alloy comprises the following steps:
s1: mixing powder: mixing 40g of tungsten fiber, 40g of tungsten powder and 20g of copper powder, adding alcohol dissolved with forming agent stearic acid, heating in water bath at 60 ℃, and stirring for 30min; wherein the tungsten fiber is in a stress relief annealing state, the structure is a slender nano fiber crystal grain, and the width is 80nm; the length of the tungsten fiber is 4mm, and the diameter of the tungsten fiber is 150 mu m; the tungsten powder is tungsten powder with the particle sizes of 3 mu m and 10 mu m according to the mass ratio of 3:7; the particle size of the copper powder is 2 mu m; the adding amount of stearic acid is 0.6g;
s2: profiling: placing the powder treated in the step S1 in a steel mold, and carrying out cold press molding at room temperature under the pressure of 650MPa for 6min to obtain a green compact body;
s3: and (3) sintering the pressed compact obtained in the step (S2) in a vacuum atmosphere at the temperature of 1150 ℃ for 150min.
Fig. 4 is a gold phase diagram of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example, and fig. 5 is a scanning electron micrograph of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example. As can be seen from fig. 4-5, the resulting tungsten-copper alloy structure is relatively compact.
The tungsten-copper alloy prepared in the embodiment is detected to have the compactness of 99.6%, the heat conduction of 226 (W/(m.K)), and the bending strength of 858MPa.
Example 3:
a low-cost preparation method of a high-strength high-thermal-conductivity tungsten fiber reinforced tungsten-copper alloy comprises the following steps:
s1: mixing powder: mixing 80g of tungsten fiber, 5g of tungsten powder and 15g of copper powder, adding alcohol dissolved with forming agent stearic acid, heating in 70 ℃ water bath, and stirring for 20min; wherein the tungsten fiber is in a stress relief annealing state, the structure is a slender nano fiber crystal grain, and the width is 120nm; the length of the tungsten fiber is 5mm, and the diameter of the tungsten fiber is 50 mu m; the tungsten powder is prepared from tungsten powder with the particle sizes of 3 mu m and 10 mu m according to the mass ratio of 3:7; the particle size of the copper powder is 5 mu m; the adding amount of stearic acid is 0.7g;
s2: profiling: placing the powder treated in the step S1 in a steel mold, and carrying out cold press molding at room temperature under the pressure of 600MPa for 8min to obtain a green compact body;
s3: and (3) sintering the pressed compact obtained in the step (S2) in a vacuum atmosphere at the temperature of 1100 ℃ for 180min.
Fig. 6 is a gold phase diagram of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example, and fig. 7 is a scanning electron micrograph of the tungsten fiber reinforced tungsten-copper alloy obtained in the present example. As can be seen from fig. 6-7, the resulting tungsten-copper alloy structure is relatively compact.
The tungsten-copper alloy prepared by the embodiment is detected to have the compactness of 99.9%, the heat conduction of 216 (W/(m.K)), and the bending strength of 800MPa.
FIG. 8 is a graph of stress versus displacement for the tungsten copper alloy materials prepared in examples 1-3, from which it can be seen that the material does not fail immediately after fracture, but instead has undulations and steps, illustrating that the addition of tungsten fibers improves the toughness of the material.
In the above example, copper is filled in the gap between the tungsten fiber and the tungsten powder, which shows that the addition of the tungsten fiber indeed reduces the occurrence of closed pores and improves the compactness; copper flows more easily at high temperature, and agglomeration is avoided.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The high-strength high-heat-conductivity tungsten fiber reinforced tungsten-copper alloy is characterized by comprising the following components: 30-80% of tungsten fiber, 5-60% of tungsten powder and 10-20% of copper powder by mass.
2. The tungsten-copper alloy reinforced by high-strength high-thermal-conductivity tungsten fibers as claimed in claim 1, wherein the tungsten fibers have a length of 3 to 5mm and a diameter of 50 to 150 μm.
3. The high strength high thermal conductivity tungsten fiber reinforced tungsten-copper alloy according to claim 1 or 2, wherein the tungsten fiber is in a stress-relieved annealed state with elongated nano-fiber grains or sub-grains and a width of 80-120nm.
4. The high-strength high-thermal-conductivity tungsten fiber-reinforced tungsten-copper alloy according to claim 3, wherein the tungsten powder is a tungsten powder with particle sizes of 3 μm and 10 μm, and the mass ratio of the tungsten powder to the tungsten powder is 3:7 in a mixture.
5. The high strength high thermal conductivity tungsten fiber reinforced tungsten copper alloy of claim 4, wherein the particle size of the copper powder is 2-5 μm.
6. A method for preparing the high-strength high-thermal-conductivity tungsten fiber reinforced tungsten-copper alloy according to claims 1 to 5, which comprises the following steps:
s1: mixing powder: mixing tungsten fiber, tungsten powder and copper powder according to the mass ratio, adding alcohol dissolved with forming agent stearic acid, and stirring in water bath atmosphere;
s2: profiling: putting the powder processed in the step S1 into a die, and carrying out cold press molding to obtain a green compact body;
s3: and (3) sintering: and (3) sintering the pressed compact obtained in the step (S2) under hydrogen or vacuum to obtain the ceramic green compact.
7. The method of the tungsten fiber reinforced tungsten-copper alloy with high strength and high thermal conductivity according to claim 6, wherein the water bath temperature in the step S1 is 50-70 ℃, and the stirring time is 20-40min.
8. The method of claim 6, wherein the amount of stearic acid added in step S1 is 0.5-0.7% of the total mass of the tungsten fiber, tungsten powder and copper powder.
9. The method of claim 6, wherein the cold pressing pressure in step S2 is 600-800 MPa, and the pressing time is 3-8 min.
10. The method of claim 6, wherein the sintering temperature in step S3 is 1100-1200 ℃ and the sintering time is 120-180 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116460295A (en) * | 2023-04-27 | 2023-07-21 | 江苏科融新材料有限公司 | Preparation method of tungsten-lanthanum alloy wire |
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| CN110343978A (en) * | 2019-07-08 | 2019-10-18 | 西安理工大学 | The short tungsten fiber Reinforced Cu W composite material and preparation method of random distribution |
| CN112080676A (en) * | 2020-08-12 | 2020-12-15 | 西安理工大学 | Flaky powder micro-laminated W-based composite material and preparation method thereof |
| CN113333747A (en) * | 2021-06-28 | 2021-09-03 | 江西理工大学 | Tungsten copper functional gradient material with continuously-changed components and preparation method thereof |
| CN114959518A (en) * | 2022-05-30 | 2022-08-30 | 合肥工业大学智能制造技术研究院 | Tungsten fiber and oxide nanoparticle synergistic toughening tungsten-based composite material and preparation method thereof |
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| CN105039876A (en) * | 2015-07-06 | 2015-11-11 | 西安理工大学 | Preparation method for W-Cu composite materials of fiber and particle hybrid structure |
| CN110343978A (en) * | 2019-07-08 | 2019-10-18 | 西安理工大学 | The short tungsten fiber Reinforced Cu W composite material and preparation method of random distribution |
| CN112080676A (en) * | 2020-08-12 | 2020-12-15 | 西安理工大学 | Flaky powder micro-laminated W-based composite material and preparation method thereof |
| CN113333747A (en) * | 2021-06-28 | 2021-09-03 | 江西理工大学 | Tungsten copper functional gradient material with continuously-changed components and preparation method thereof |
| CN114959518A (en) * | 2022-05-30 | 2022-08-30 | 合肥工业大学智能制造技术研究院 | Tungsten fiber and oxide nanoparticle synergistic toughening tungsten-based composite material and preparation method thereof |
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| CN116460295A (en) * | 2023-04-27 | 2023-07-21 | 江苏科融新材料有限公司 | Preparation method of tungsten-lanthanum alloy wire |
| CN116460295B (en) * | 2023-04-27 | 2024-04-12 | 江苏科融新材料有限公司 | Preparation method of tungsten-lanthanum alloy wire |
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