CN113652566B - Preparation method of nanocrystalline refractory high-entropy alloy NbMoTaW-Cu composite material - Google Patents
Preparation method of nanocrystalline refractory high-entropy alloy NbMoTaW-Cu composite material Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 22
- 239000000956 alloy Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 67
- 238000000498 ball milling Methods 0.000 claims abstract description 28
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims description 20
- 239000012071 phase Substances 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000227 grinding Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000002490 spark plasma sintering Methods 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 3
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- 238000002156 mixing Methods 0.000 abstract description 6
- 238000004663 powder metallurgy Methods 0.000 abstract description 2
- 239000002905 metal composite material Substances 0.000 abstract 2
- 239000010949 copper Substances 0.000 description 31
- 229910000881 Cu alloy Inorganic materials 0.000 description 9
- 239000012300 argon atmosphere Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000000713 high-energy ball milling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000003870 refractory metal Substances 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 229910000905 alloy phase Inorganic materials 0.000 description 2
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005551 mechanical alloying Methods 0.000 description 2
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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Abstract
A preparation method of a nanocrystalline refractory high-entropy alloy NbMoTaW-Cu composite material belongs to the technical field of high-entropy alloy and powder metallurgy. The composite material has a NbMoTaW refractory high-entropy phase with a nanocrystalline structure, and has a wide adjustable range of components. The preparation method comprises the following steps: firstly, preparing nanocrystalline NbMoTaW single-phase alloy powder, carrying out planetary ball milling and uniform mixing on micron-sized Cu powder and NbMoTaW alloy powder, and then carrying out pressure sintering. The invention can obtain more excellent mechanical property, expand the application field of the dual-phase metal composite material and prolong the service life of the dual-phase metal composite material.
Description
Technical Field
The invention relates to a method for preparing a refractory high-entropy alloy NbMoTaW-Cu composite material by utilizing mechanical alloying and solid-phase sintering, belonging to the technical field of high-entropy alloy and powder metallurgy.
Background
The W-Cu alloy is formed by uniformly mixing two phases of metal simple substances, and the two phases are not mutually soluble and form intermetallic compounds, and is a typical pseudo alloy. It combines the excellent properties of the two component metals, such as high temperature resistance, high strength, high density characteristic of W and high electric and thermal conductivity, high plasticity and the like of copper. The properties of the W-Cu alloy can also be adjusted by changing the component ratios thereof. The W-Cu alloy has excellent performance and adjustable characteristics, so that the W-Cu alloy has wide application prospects in the fields of electricity, electronics, military and the like. However, tungsten-copper alloy is easy to fail due to deformation in the service process, especially in a high-temperature environment, which seriously affects the service life and limits the application range of the tungsten-copper alloy. The refractory metals in the W-Cu alloy contribute to a greater extent to the mechanical properties, and therefore the ability to increase the resistance of the refractory metals against deformation is critical to mitigating the failure of the composite material to deform.
High entropy alloys differ from conventional alloys in that they contain a number of major elements mixed in equimolar or near-equimolar proportions, each element being present in atomic percentages ranging from about 5% to about 35%. In liquid and solid solution states, the high-entropy alloy has the mixing entropy which is obviously improved compared with the traditional alloy, and can inhibit the generation of various complex intermetallic compounds and intermediate phases. Due to the fact that the multi-principal-element high-entropy alloy has the thermodynamic high-entropy effect, the structural lattice distortion effect, the kinetic delayed diffusion effect and the performance cocktail effect, the multi-principal-element high-entropy alloy has the excellent comprehensive performances of ultrahigh strength, good wear resistance, high work hardening capacity, high temperature softening resistance, oxidation resistance and the like, and particularly the high-entropy alloy with a body-centered cubic structure and composed of refractory metal elements shows very high-temperature strength which cannot be compared with a traditional material prepared through microalloying of various components.
Disclosure of Invention
The invention provides a method for preparing a novel refractory high-entropy alloy NbMoTaW-Cu composite material aiming at the problem that the W-Cu alloy is easy to deform and lose efficacy in the service process, so that the composite material has more excellent mechanical properties, the application field of the composite material is expanded, and the service life of the composite material is prolonged.
The invention provides a method for preparing NbMoTaW-Cu composite material, which is characterized by comprising the following steps:
(1) taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, performing high-energy vibration ball milling according to equal atomic ratio ingredients, wherein the mass ratio of grinding balls to powder is 15: 1-25: 1, the rotating speed is 410-500 r/min, and the ball milling time is 6-18 h, so as to obtain NbMoTaW single-phase alloy powder, performing planetary ball milling on micron-sized Cu powder and the NbMoTaW alloy powder obtained in the step (1), wherein the rotating speed is 260-400 r/min, and performing ball milling for 3-12 h, so as to obtain NbMoTaW-Cu composite powder;
(2) putting the NbMoTaW-Cu composite powder obtained in the step (1) into a graphite die, completing sintering in a spark plasma sintering furnace, and vacuumizing until the vacuum degree reaches 2 multiplied by 10 -2 And (2) starting to heat up by electrifying current below Pa, wherein the heating rate is 70-100 ℃/min, increasing the pressure while heating to enable the pressure to rise from 30-35MPa, the boosting rate is 8-10 MPa/min, keeping the pressure constant after the pressure reaches 90-100 MPa, keeping the temperature for 5-15 min when the temperature rises to 900-950 ℃, cooling the sample to room temperature along with the furnace after the temperature is kept, and then releasing the pressure to remove the product.
In the step (2), the Cu content in the composite material is 18-40 wt%, and the composite material has a wide adjustable range.
The refractory high-entropy phase in the composite material prepared by solid-phase sintering can keep the size close to the particle size of powder, and can be regulated and controlled by different matching of process parameters of ball-material ratio, ball-milling rotating speed and ball-milling time, and the adjustable range of the average size is about 1-10 mu m.
The Cu phase in the composite material prepared by the invention reduces the sintering densification temperature, and fine grain size can still be remained in the refractory high-entropy phase obtained by mechanical alloying after sintering, and can be reduced to less than 100 nm.
The characteristics and technical advantages of the technology are as follows:
compared with the high-entropy alloy phase prepared by the smelting method, the high-entropy alloy phase can eliminate coarse dendritic structures, improve the structural uniformity of the material, retain the fine nanocrystalline structure of the refractory high-entropy phase, and further improve the performance of the material. The preparation method is convenient for regulating and controlling the relative contents of the high entropy and the Cu phase of the refractory material so as to obtain different degree matching of the high-temperature mechanical property and the thermal and electric conduction characteristics. The process route of the invention has wide applicability, and can be popularized to the preparation of various high-entropy alloy and Cu composite materials with different principal elements and different principal element proportions. The NbMoTaW-Cu composite material prepared by the method is expected to have more excellent high-temperature hardness and strength than W-Cu alloy in the service process, especially in the high-temperature environment, and the application of the NbMoTaW-Cu composite material in extreme service conditions such as aerospace is expanded.
Drawings
FIG. 1 is a micrograph of the NbMoTaW-Cu bulk composite obtained in example 1;
FIG. 2 is a nanocrystalline structure of a refractory high-entropy phase in the NbMoTaW-Cu bulk composite of example 1;
FIG. 3 shows the phase of the NbMoTaW-Cu composite powder before and after sintering in example 1;
FIG. 4 is a micrograph of the NbMoTaW-Cu bulk composite obtained in example 2;
FIG. 5 is a micrograph of the NbMoTaW-Cu bulk composite obtained in example 3;
FIG. 6 is a graph showing changes in phase of powder with ball milling time in the ball milling process in comparative example 1 at a ball to material ratio of 5: 1;
fig. 7 shows the increase in the shot to shot ratio of 15 in comparative example 1: 1, changing the phase of powder along with the ball milling time in the ball milling process;
table 1 shows the hardness of the NbMoTaW-Cu bulk composite materials obtained in examples 1 to 3.
Detailed Description
The following examples further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
The method comprises the steps of taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, mixing according to an equal atomic ratio, wherein the mass of the powder is 10g, the mass ratio of grinding balls to the powder is 15:1, putting the grinding balls and the powder into a ball milling tank in an argon atmosphere glove box, and carrying out ball milling by using a GN-2 type high-energy ball mill at the rotating speed of 470r/min for 12h, scraping the powder once every 6h, and avoiding cold welding. After high-energy ball milling, 4.5g of micron-sized Cu powder is added into a glove box, and the mixture is uniformly mixed by planetary ball milling at the rotating speed of 320r/min for 12 h. The obtained NbMoTaW-Cu composite powder is put into a graphite die and then is put into a spark plasma sintering furnace for sintering. Before applying current, the sintering pressure was set to 34MPa, and the degree of vacuum in the sintering chamber reached 2X 10 -2 And (2) starting to heat up with current below Pa, wherein the heating rate is 93 ℃/min, the sintering pressure is increased while the heating is carried out, the boosting rate is 9MPa/min, the pressure is kept constant after the pressure reaches 100MPa, the temperature is continuously raised to 950 ℃ and kept for 5min, and the current is closed after the heat preservation is finished, so that the sample is cooled to the room temperature along with the furnace. The microstructure morphology of the NbMoTaW-Cu bulk composite material prepared in this example is shown in fig. 1, the refractory high-entropy phase has a nanocrystalline structure, as shown in fig. 2, the phase composition of the powder and the bulk is shown in fig. 3, and the hardness of the sintered bulk is shown in table 1. The high-temperature hardness test is carried out, and the hardness of the alloy is 177.9 +/-5.5 HV at the temperature of 900 DEG C 30 And the volume fraction of the W-Cu composite material is 31.7 percent higher than that of the W-Cu composite material with the same volume fraction.
Example 2
The method comprises the steps of taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, preparing the raw materials according to an equal atomic ratio, wherein the mass of the powder is 7.5g, the mass ratio of a grinding ball to the powder is 20:1, putting the grinding ball and the powder into a ball milling tank in an argon atmosphere glove box, and carrying out ball milling by using a GN-2 type high-energy ball mill at the rotating speed of 410r/min for 6h. After high-energy ball milling, 1.7g of micron-sized Cu powder is added into a glove box, and the mixed powder is uniformly ball-milled by using a planetary ball mill at the rotating speed of 260r/min for 3 h. And (3) loading the obtained NbMoTaW-Cu composite powder into a graphite die, and then placing the graphite die into a spark plasma sintering furnace for sintering. Before applying current in the sintering process, the sintering pressure was set to 34MPa, and the degree of vacuum in the spark plasma sintering chamber was 2X 10 - 2 And (2) starting to electrify to heat under the condition of Pa, wherein the heating rate is 70 ℃/min, the sintering pressure is increased while the heating is carried out, the boosting rate is 10MPa/min, the pressure is kept constant after the pressure reaches 100MPa, the temperature is continuously raised to 950 ℃, the temperature is kept for 15min, and the current is closed after the temperature is kept, so that the sample is cooled to the room temperature along with the furnace. The microstructure morphology of the NbMoTaW-Cu bulk composite material prepared in this example is shown in fig. 4, and the hardness is shown in table 1.
Example 3
The method comprises the steps of taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, mixing according to an equal atomic ratio, wherein the mass of the powder is 6g, the mass ratio of grinding balls to the powder is 25:1, putting the grinding balls and the powder into a ball milling tank in an argon atmosphere glove box, and carrying out ball milling by using a GN-2 type high-energy ball mill at the rotating speed of 500r/min for 6 h. After high-energy ball milling, 4.1g of micron-sized Cu powder is added into a glove box, and the mixed powder is uniformly ball-milled by using a planetary ball mill at the rotating speed of 400r/min for 12 h. And (3) loading the obtained NbMoTaW-Cu composite powder into a graphite die, and then placing the graphite die into a spark plasma sintering furnace for sintering. Before applying current in the sintering process, the sintering pressure was set to 34MPa, and the degree of vacuum in the spark plasma sintering chamber was 2X 10 -2 And under the condition of Pa below, starting to heat up by electrifying current, wherein the heating rate is 100 ℃/min, increasing the sintering pressure while heating, the boosting rate is 8MPa/min, keeping the pressure constant after the pressure reaches 90MPa, continuously heating to 900 ℃, keeping the temperature for 10min, and closing the current after the heat preservation is finished so as to cool the sample to the room temperature along with the furnace. The microstructure morphology of the NbMoTaW-Cu bulk composite material prepared in this example is shown in fig. 5, and the hardness is shown in table 1.
Comparative example 1
The method comprises the steps of taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, mixing according to an equal atomic ratio, wherein the mass of the powder is 30g, the mass ratio of a grinding ball to the powder is 5:1, putting the grinding ball and the powder into a ball milling tank in an argon atmosphere glove box, carrying out ball milling by using a GN-2 type high-energy ball mill at the rotating speed of 470r/min for 18h, scraping the powder in a vacuum glove box every 6h to prevent cold welding, and simultaneously taking out a proper amount of powder test phase. The test results are shown in fig. 6, and it was found that a single solid solution was not formed at the ball milling time of 18 h. When the other parameters are unchanged and the ball-to-material ratio is increased from 5:1 to 15:1, the test results are shown in fig. 7, and a single solid solution can be formed in the ball milling time of only 6 hours, so that the four-element powder is completely alloyed.
TABLE 1
| Test specimen | Hardness at room temperature/HV 30 |
| Example 1 | 393±5.5 |
| Example 2 | 636±8.9 |
| Example 3 | 267±4.9 |
Claims (2)
1. A preparation method of a nanocrystalline refractory high-entropy alloy NbMoTaW-Cu composite material is characterized by comprising the following steps: (1) taking micron-sized Nb powder, Mo powder, Ta powder and W powder as raw materials, carrying out high-energy vibration ball milling according to equal atomic ratio ingredients, wherein the mass ratio of grinding balls to powder is 15: 1-25: 1, the rotating speed is 410-500 r/min, and the ball milling time is 6-18 h, so as to obtain NbMoTaW single-phase alloy powder, then carrying out planetary ball milling on the micron-sized Cu powder and the obtained NbMoTaW alloy powder at the rotating speed of 260-400 r/min, and carrying out ball milling for 3-12 h, so as to obtain NbMoTaW-Cu composite powder;
(2) putting the NbMoTaW-Cu composite powder obtained in the step (1) into a graphite die, completing sintering in a spark plasma sintering furnace, and vacuumizing until the vacuum degree reaches 2 multiplied by 10 -2 Heating with current below Pa, wherein the heating rate is 70-100 ℃/min, increasing the pressure while heating to enable the pressure to rise from 30-35MPa, the pressure rise rate is 8-10 MPa/min, keeping the pressure constant when the pressure reaches 90-100 MPa, keeping the temperature for 5-15 min when the temperature rises to 900-950 ℃, cooling the sample to room temperature along with the furnace after the temperature is kept, and then releasing the pressure to take out the product;
in the step (2), the Cu content in the composite material is 18-40 wt%, and the composite material has a wide adjustable range;
the size of a refractory high-entropy phase in the composite material prepared by solid-phase sintering can be kept close to the particle size of powder, and can be regulated and controlled by different matching of process parameters of ball-material ratio, ball-milling rotating speed and ball-milling time, wherein the adjustable range of the average size is 1-10 mu m;
the fine grain size is kept in the refractory high-entropy phase and is less than 100 nm.
2. The nanocrystalline refractory high-entropy alloy NbMoTaW-Cu composite material prepared according to the method in claim 1.
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