CN114717491B - High-toughness W f /W composite material and preparation method thereof - Google Patents
High-toughness W f /W composite material and preparation method thereof Download PDFInfo
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- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
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Abstract
The invention provides a high-toughness W f The material of the/W composite material comprises W f W powder and coating film W f (ii) a The W is f Adopting potassium-doped tungsten fiber with the diameter of 100-300 mu m and the length of 2-4 mm; the W powder is tungsten powder with the particle size of 5-10 mu m; the coating film W f Adopts the potassium-doped tungsten fiber with the surface combined with the BN film, wherein the diameter of the potassium-doped tungsten fiber is 100 to 300 mu m, and the length of the potassium-doped tungsten fiber is 2 to 4mm. The invention also provides a high-toughness W f A preparation method of a/W composite material. The invention utilizes W which can respectively combine with W matrix to generate strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f The strong interface generated by combination with the W matrix can improve the strength of the composite material matrix, and the BN film is plated on the W f The weak interface generated by combination with the W matrix can improve the toughness of the composite matrix.
Description
Technical Field
The invention relates to the field of materials, in particular to a high-toughness W f a/W composite material and a preparation method thereof.
Background
Tungsten is currently considered to be the most promising plasma-facing material in the fusion field because of its high melting point, low vapor pressure, low thermal expansion rate, high strength, and low protium, deuterium, and tritium retention rate. Tungsten itself has its limitations, most notably its intrinsic brittleness.
Taking a tube-through type tungsten target module (W/Cu/CuCrZr) of a divertor in an international thermonuclear fusion experimental reactor (ITER) as an example, the tungsten target module is subjected to 20MW/m 2 When the tungsten target module is subjected to heat load, the surface temperature of the tungsten target module exceeds 2000 ℃, and the temperature difference of about 1500 ℃ is generated between the surface of the tungsten target and the heat sink copper pipe, so that large thermal stress occurs, and the tungsten target module of the divertor can be cracked. The divertor of the Chinese fusion engineering experimental reactor (CFETR) currently in engineering design can bear higher steady-state heat load which can reach 40MW/m 2 The thermal stress generated is greater. Therefore, the design of the component structure of the tungsten to improve the strength and toughness of the tungsten is a precondition for the tungsten to be used as a plasma-facing material of the future fusion reactor, only because the performance of the general pure tungsten is not enough to bear the heat load generated by the future fusion reactor.
Disclosure of Invention
The invention aims to provide a high-toughness W which has both strength and toughness f a/W composite material and a preparation method thereof.
The invention adopts the following technical scheme to solve the technical problems:
high-toughness W f The material of the/W composite material comprises W f W powder and coating film W f (ii) a W is f Adopting potassium-doped tungsten fiber with the diameter of 100-300 mu m and the length of 2-4 mm; the W powder is tungsten powder with the particle size of 5-10 mu m; the coating film W f The potassium-doped tungsten fiber with the surface combined with a BN film (boron nitride film) is adopted, wherein the diameter of the potassium-doped tungsten fiber is 100-300 mu m, and the length of the potassium-doped tungsten fiber is 2-4 mm.
In a preferred embodiment of the present invention, W is W in the raw material f And a coating film W f Is 10 to 50% and wherein W f And a plating film W f The mass ratio of (1).
In a preferred embodiment of the present invention, W is f And a plating film W f The potassium-doped amount of the tungsten fiber doped with potassium is 60-75 ppm.
In a preferred embodiment of the present invention, W is f In the/W composite material, W f Bonding with W substrate to generate strong interface, coating W f Bonding to the W substrate creates a weak interface. Wherein, the strong interface generally means that the interface bonding strength of the fiber matrix is high, when the composite material is acted by external force, the interface is still tightly bonded, the fiber is not debonded and pulled out, and the reinforcing effect can be well achieved. The weak interface, generally refers to the weak bonding strength of the interface of the fiber matrix, when the composite material is subjected to external force, the interface is easy to be damaged, and the fiber is stripped and pulled out, thereby playing a good toughening role.
The high toughness W f The preparation method of the/W composite material comprises the following steps:
(1) Coating film W f Preparation of (2)
(1) Soaking W in concentrated nitric acid f Then ultrasonically cleaning the surface to obtain surface-treated W f ；
(2) Preparing precursor solution by using boric acid and urea as raw materials, and then treating the surface of the W f Dipping, drying and heat treating to obtain W with the surface plated with the BN film f ；
(2)W f Preparation of/W composite material
Coating film W prepared in the step (1) f With W without any treatment f And W powder are uniformly mixed and sintered by hot isostatic pressing to obtain the W required by the target f A/W composite material.
In a preferred embodiment of the present invention, in the step (1) or (1), the concentration of the concentrated nitric acid is 65 to 68%, and W is f The soaking time in the concentrated nitric acid is 0.5 to 3 hours.
In a preferred embodiment of the present invention, in the steps (1) and (2), the mass ratio of boric acid to urea is 1.
In a preferred embodiment of the present invention, in the step (2), the sintering temperature is 1000 to 1600 ℃, the time is 2 to 4 hours, and the pressure is 150MPa.
Compared with the prior art, the invention has the advantages that:
(1) The invention utilizes W which can respectively combine with W matrix to generate strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f The strong interface generated by combination with the W matrix can improve the strength of the composite material matrix, and the BN film is plated on the W f The weak interface generated by combination with the W matrix can improve the toughness of the composite material matrix, thereby obtaining the W with both strength and toughness f a/W composite material;
(2) In the invention W f The potassium-doped tungsten fiber is adopted instead of the pure tungsten fiber, so that the strength of the composite material in high-temperature preparation can be effectively prevented from being damaged, and the strength of the material is further improved.
Drawings
FIG. 1 shows toughness W of an embodiment of the present invention f A preparation flow chart of the/W composite material;
FIG. 2 shows toughness W in an embodiment of the present invention f A model schematic diagram of the/W composite material.
Detailed Description
The following examples are given for the detailed implementation and the specific operation procedures, but the scope of the present invention is not limited to the following examples.
The various starting materials used in the following examples, unless otherwise specified, are all commercially available products known in the art.
Example 1
A toughness W of this example f The material of the/W composite comprises 10% by weight of f 50% of W powder and 40% of coating W f . Wherein, W f By usingThe potassium-doped tungsten fiber (60 ppm doped with potassium) has the diameter of 100 mu m and the length of 2mm and can be combined with a W matrix to generate a strong interface; w powder is tungsten powder with the particle size of 5 mu m; film coating W f The potassium-doped tungsten fiber (60 ppm of potassium) with the BN film bonded on the surface can be bonded with a W matrix to generate a weak interface, wherein the potassium-doped tungsten fiber has the diameter of 100 mu m and the length of 2mm.
The toughness W f The preparation method of the/W composite material is shown in figure 1 and comprises the following steps:
(1) Film coating W f Preparation of (2)
(1) Will W f Soaking in 65% concentrated nitric acid for 3h, and ultrasonic cleaning with deionized water and acetone for 10min to remove residue in W f Nitric acid on the surface to finally obtain surface-treated W f (ii) a Here, W after surface treatment f The surface energy bonds better with the membrane.
(2) Dissolving boric acid and urea in a mixed solvent of water and ethanol according to a mass ratio of 1; w surface-treated in step (1) f Soaking in the precursor solution for 10min, and drying at 100 deg.C for 50min; after 2 cycles of dip-drying, in N 2 Heat treatment is carried out for 5 hours at 500 ℃ under the atmosphere, and finally the BN coating W is obtained f 。
(2)W f Preparation of/W composite material
Coating film W prepared in the step (1) f With W without any treatment f And W powder are uniformly mixed according to a corresponding proportion, and the mixture is subjected to hot isostatic pressing sintering for 4 hours at 1000 ℃ and 150MPa to obtain the target W f a/W composite material.
Example W f The final model of the/W composite is shown in FIG. 2, which utilizes W that respectively binds to the W matrix to create a strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f The strong interface generated by combination with the W matrix can improve the strength of the composite material matrix, and the BN film is plated on the W f The weak interface generated by combining with the W matrix can improve the toughness of the composite material matrix, thereby obtaining the W with both strength and toughness f A/W composite material.
Example 2
A toughness of this example W f the/W composite material comprises 20% of f 50% of W powder and 30% of coating W f . Wherein, W f The potassium-doped tungsten fiber (70 ppm doped with potassium) is adopted, has the diameter of 200 mu m and the length of 3mm, and can be combined with a W matrix to generate a strong interface; w powder is tungsten powder with the particle size of 8 mu m; coating film W f The use of potassium-doped tungsten fibers (potassium-doped 70 ppm) having a BN film bonded to the surface thereof, wherein the potassium-doped tungsten fibers have a diameter of 200 μm and a length of 3mm, can bond to a W substrate to produce a weak interface.
The toughness W f The preparation method of the/W composite material is shown in figure 1 and comprises the following steps:
(1) Coating film W f Preparation of
(1) Will W f Soaking in concentrated nitric acid with concentration of 66% for 2h, sequentially performing ultrasonic cleaning with deionized water and acetone for 10min to remove residual W f Nitric acid on the surface to finally obtain surface-treated W f (ii) a Here, W after surface treatment f The surface energy bonds better with the membrane.
(2) Dissolving boric acid and urea in a mixed solvent of water and ethanol according to a mass ratio of 1; w surface-treated in step (1) f Soaking in the precursor solution for 10min, and drying at 100 deg.C for 50min; after 2 cycles of dip-drying, in N 2 Heat treatment is carried out for 4 hours at 700 ℃ under the atmosphere, and finally the BN coating W is obtained f 。
(2)W f Preparation of/W composite material
Coating the film W prepared in the step (1) f With W without any treatment f And W powder are uniformly mixed, and the mixture is subjected to hot isostatic pressing sintering for 3 hours at 1200 ℃ and 150MPa to obtain the W required by the target f A/W composite material.
Example W f The final model of the/W composite is shown in FIG. 2, which utilizes W that respectively binds to the W matrix to create a strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f Combined with W substrate to produceThe strong interface of (2) can improve the strength of the composite material matrix, and the BN coating W f The weak interface generated by combination with the W matrix can improve the toughness of the composite material matrix, thereby obtaining the W with both strength and toughness f A/W composite material.
Example 3
A toughness W of this example f a/W composite material comprising 30% of f 50% of W powder and 20% of coating W f . Wherein, W f The potassium-doped tungsten fiber (70 ppm doped with potassium) is adopted, has the diameter of 200 mu m and the length of 3mm, and can be combined with a W matrix to generate a strong interface; w powder is tungsten powder with the particle size of 8 mu m; film coating W f The use of potassium-doped tungsten fibers (potassium-doped 70 ppm) having a BN film bonded to the surface thereof, wherein the potassium-doped tungsten fibers have a diameter of 200 μm and a length of 3mm, can bond to a W substrate to produce a weak interface.
The toughness W f The preparation method of the/W composite material is shown in figure 1 and comprises the following steps:
(1) Film coating W f Preparation of
(1) W is to be f Soaking in 67% concentrated nitric acid for 40min, and ultrasonic cleaning with deionized water and acetone for 10min to remove residue in W f Nitric acid on the surface to finally obtain surface-treated W f (ii) a Here, W after surface treatment f The surface energy bonds better with the membrane.
(2) Dissolving boric acid and urea in a mixed solvent of water and ethanol according to a mass ratio of 1; w surface-treated in step (1) f Soaking in the precursor solution for 10min, and drying at 100 deg.C for 50min; after 2 cycles of dip-drying, in N 2 Heat treatment is carried out for 3 hours at 800 ℃ under the atmosphere, and finally the BN coating W is obtained f 。
(2)W f Preparation of a/W composite
Coating film W prepared in the step (1) f With W without any treatment f And W powder are evenly mixed, and the mixture is subjected to hot isostatic pressing sintering for 3 hours at 1500 ℃ and 150MPa to obtain the target W f A/W composite material.
Example W f The final model of the/W composite is shown in FIG. 2, which utilizes W that respectively binds to the W matrix to create a strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f The strong interface generated by combination with the W matrix can improve the strength of the composite material matrix, and the BN film is plated on the W f The weak interface generated by combination with the W matrix can improve the toughness of the composite material matrix, thereby obtaining the W with both strength and toughness f a/W composite material.
Example 4
A toughness of this example W f The material of the/W composite material comprises 40% of f 50% of W powder and 10% of coating film W f . Wherein, W f The potassium-doped tungsten fiber (doped with potassium of 75 ppm) is adopted, has the diameter of 300 mu m and the length of 4mm, and can be combined with a W matrix to generate a strong interface; w powder is tungsten powder with the particle size of 10 mu m; coating film W f The use of potassium-doped tungsten fibers (potassium-doped 75 ppm) having BN film bonded to the surface thereof, wherein the potassium-doped tungsten fibers have a diameter of 300 μm and a length of 4mm, can bond to a W substrate to produce a weak interface.
The toughness W f The preparation method of the/W composite material is shown in figure 1 and comprises the following steps:
(1) Film coating W f Preparation of
(1) W is to be f Soaking in 68% concentrated nitric acid for 30min, and ultrasonic cleaning with deionized water and acetone for 10min to remove residual W f Nitric acid on the surface to finally obtain surface-treated W f (ii) a Here, W after surface treatment f The surface energy bonds better with the membrane.
(2) Dissolving boric acid and urea in a mixed solvent of water and ethanol according to a mass ratio of 1; w surface-treated in step (1) f Soaking in the precursor solution for 10min, and drying at 100 deg.C for 50min; after 2 cycles of dip-drying, in N 2 Heat treatment is carried out for 2 hours at 500 ℃ under the atmosphere, and finally the BN coating W is obtained f 。
(2)W f Preparation of a/W composite
Coating the film W prepared in the step (1) f And does notW of any treatment f And W powder are evenly mixed, and the mixture is subjected to hot isostatic pressing sintering for 2 hours at 1600 ℃ and 150MPa to obtain the target W f a/W composite material.
Example W f The final model of the/W composite is shown in FIG. 2, which utilizes W that respectively bonds to the W matrix to create a strong interface f And a plating film W for producing a weak interface f To jointly compound the W matrix; wherein, W f The strong interface generated by combination with the W matrix can improve the strength of the composite material matrix, and the BN film is plated on the W f The weak interface generated by combination with the W matrix can improve the toughness of the composite material matrix, thereby obtaining the W with both strength and toughness f a/W composite material.
Further, it is noted that the above-described embodiment is strong in toughness W f The raw material composition of the/W composite material can also be "2% f 50% of W powder and 8% of coating W f ”、“4％W f 80% of W powder and 16% of coating W f ”、“8％W f 50% of W powder and 2% of coating W f "and the like.
Example 5
This example was used to test the above example W f Strength and toughness of the/W composite:
according to the national standard GB/T228.1-2010 part 1 of the tensile test of metal materials: room temperature test method for toughness W f The tensile property test at room temperature is carried out on the/W composite material, the obtained results are shown in the table 1, and the results show that: invention W f Compared with pure W (strength: 240Mpa, elongation: 0.3%) prepared by the same process, the strength and toughness of the/W composite material are both improved.
TABLE 1 inventive W f Strength and toughness test results of/W composite
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Strength (MPa) | 313 | 342 | 365 | 371 |
| Elongation (%) | 1.2 | 1.5 | 1.8 | 1.4 |
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (5)
1. High-toughness W f A/W composite material, characterized in that the raw material comprises W f W powder and coating film W f (ii) a W is f Adopting potassium-doped tungsten fibers, wherein the diameter is 100 to 300 mu m, and the length is 2 to 4mm; the W powder is tungsten powder, and the particle size is 5-10 mu m; the coating film W f Adopting potassium-doped tungsten fibers with BN films combined on the surfaces, wherein the diameter of the potassium-doped tungsten fibers is 100-300 mu m, and the length of the potassium-doped tungsten fibers is 2-4 mm; w is f In the/W composite material, W f Bonding with W substrate to generate strong interface, coating W f Bonding to the W substrate to create a weak interface;
meanwhile, in the raw materials, W f And a coating film W f Is 10 to 50 percent, and W is f And a coating film W f 1, 2, 3, 2 or 4, and the balance being W powder; w is f And a plating film W f The potassium doping amount of the potassium-doped tungsten fiber is 60 to 75ppm.
2. Toughness W as claimed in claim 1 f The preparation method of the/W composite material is characterized by comprising the following steps:
(1) Coating film W f Preparation of
(1) Soaking W in concentrated nitric acid f Then ultrasonically cleaning the surface to obtain surface-treated W f ；
(2) Preparing precursor solution by using boric acid and urea as raw materials, and then treating the surface of the W f Dipping, drying and heat treating to obtain W with the surface plated with a BN film f ；
（2）W f Preparation of/W composite material
Coating the film W prepared in the step (1) f With W without any treatment f And W powder are uniformly mixed and sintered by hot isostatic pressing to obtain the W required by the target f A/W composite material.
3. The high toughness W of claim 2 f The preparation method of the/W composite material is characterized in that in the step (1) and the step (1), the concentration of concentrated nitric acid is 65-68%, and W is f The soaking time in concentrated nitric acid is 0.5 to 3h.
4. The high toughness W of claim 2 f The preparation method of the/W composite material is characterized in that in the steps (1) and (2), the mass ratio of boric acid to urea is 1.
5. The high toughness W of claim 2 f The preparation method of the/W composite material is characterized in that in the step (2), the sintering temperature is 1000 to 1600 ℃,the time is 2 to 4 hours, and the pressure is 150MPa.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560292A (en) * | 2012-02-29 | 2012-07-11 | 中国科学院等离子体物理研究所 | Tungsten-based plasma facing material and preparation method thereof |
| CN103924443A (en) * | 2014-03-21 | 2014-07-16 | 南京航空航天大学 | Preparation method of carbon fiber surface antioxidation coating |
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| JP4051141B2 (en) * | 1998-09-25 | 2008-02-20 | 株式会社東芝 | Tungsten, tungsten fiber reinforced composite material and molybdenum, molybdenum fiber reinforced composite material, manufacturing method thereof, and high-temperature component using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560292A (en) * | 2012-02-29 | 2012-07-11 | 中国科学院等离子体物理研究所 | Tungsten-based plasma facing material and preparation method thereof |
| CN103924443A (en) * | 2014-03-21 | 2014-07-16 | 南京航空航天大学 | Preparation method of carbon fiber surface antioxidation coating |
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| Title |
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| Urea route to coat inorganic nanowires, carbon fibers and nanotubes by boron nitride;A. Gomathi等;《Materials Science and Engineering A》;20081231;第29-33页 * |
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