CN108504881B - Method for improving wear resistance of high-entropy alloy - Google Patents
Method for improving wear resistance of high-entropy alloy Download PDFInfo
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- CN108504881B CN108504881B CN201810309819.4A CN201810309819A CN108504881B CN 108504881 B CN108504881 B CN 108504881B CN 201810309819 A CN201810309819 A CN 201810309819A CN 108504881 B CN108504881 B CN 108504881B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/16—Remelting metals
- C22B9/20—Arc remelting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
Abstract
The invention relates to a method for improving the wear resistance of high-entropy alloy, which comprises the following steps of putting a high-purity metal sample into a vacuum arc melting furnace to be melted under the protection of argon: repeatedly smelting to obtain a master alloy ingot with uniform components; obtaining a required sample from the master alloy ingot by a copper mold suction casting method; repeatedly smelting and suction casting the sample to obtain the remelting-state high-entropy alloy. The hardness and wear resistance of the high-entropy alloy prepared by the invention after remelting treatment are obviously improved, the performance requirements of key wear-resistant parts of agricultural machinery are met, the high-entropy alloy can be widely applied to high-end agricultural machinery, and in addition, the high-entropy alloy can also be applied to other fields with high requirements on wear resistance.
Description
Technical Field
The invention relates to a method for improving the wear resistance of a high-entropy alloy.
Background
The high-entropy alloy is formed by mixing at least five and more than five metal elements according to the equal atomic ratio or the method close to the equal atomic ratio, and forms a solid solution alloy with a single phase or two phases of the structure. The high-entropy alloy is a novel material developed in recent years, has excellent mechanical properties and wide application prospects, and is paid more and more attention. The high-entropy alloy has the excellent characteristics of high wear resistance, high corrosion resistance, excellent thermal stability, high strength, high hardness, high-temperature oxidation resistance and the like. The excellent performances meet the key performance requirements of agricultural machinery, and can be widely applied to high-end agricultural machinery.
At present, the research on the high-entropy alloy mainly focuses on the influence of components and heat treatment on the structure and the performance of the high-entropy alloy, and the research on the performance improvement of the high-entropy alloy by utilizing the heat history is little, particularly the influence of remelting treatment on the wear resistance of the high-entropy alloy.
Disclosure of Invention
In order to solve the problems, the invention provides a method for improving the wear resistance of the high-entropy alloy, which can obviously improve the wear resistance of the high-entropy alloy.
A method for improving the wear resistance of high-entropy alloy comprises the following steps:
1. putting a high-purity metal sample into a vacuum arc melting furnace to be melted under the protection of argon: firstly, vacuumizing to 2 x 10-3Pa, then filling argon to the pressure of 0.06-0.08MPa, opening the current, melting the metal sample, continuing to perform electromagnetic stirring melting for 10 seconds after the metal sample is melted, cooling, turning over the metal sample by using a stirring rod, and performing secondary melting according to the conditions;
2. repeatedly smelting for at least four times according to the step 1) to obtain a master alloy ingot with uniform components;
3. obtaining a required sample from the master alloy ingot by a copper mold suction casting method;
4. polishing the surface of the sample obtained in the step 3), removing an oxide film on the surface, placing the sample in absolute ethyl alcohol, and oscillating the sample in an ultrasonic cleaning machine for 5 minutes to remove redundant residues on the surface; then putting the mixture into a vacuum arc furnace crucible again for smelting: and (3) repeating the steps 1) and 3) for four times, and obtaining the suction-cast sample which is the remelted high-entropy alloy.
The innovation points of the invention are as follows:
the invention uses the arc furnace to carry out remelting treatment on the high-entropy alloy by adopting a suction casting method, thereby improving the hardness and the wear resistance of the high-entropy alloy. The high-vacuum arc furnace is utilized to smelt master alloy and prepare as-cast and remelting high-entropy alloy, so that compared with a method of blowing and casting in air, the method greatly reduces the oxidation degree, has more smelting times and more uniform fusion of alloy components.
The hardness and the wear resistance of the high-entropy alloy prepared by the remelting treatment are obviously improved, the performance requirements of key wear-resistant parts of agricultural machinery are met, and the high-entropy alloy can be widely applied to high-end agricultural machinery, such as blades of harvesters, hair trimmers, rotary cultivators and the like, spindles of cotton pickers, plough side plates, feed pelleting press dies, feed crushing machine hammer blades, ploughshares, rotary cultivator curved knives and the like. In addition, the wear-resistant rubber can also be applied to other fields with high requirements on wear resistance.
Drawings
FIG. 1 is an XRD diffraction pattern of a high entropy alloy in an as-cast state and a remelted state;
as can be seen from fig. 1: only three sharp peaks appear on the XRD curve, which shows that the alloy in the cast state and the alloy in the remelting state do not have complex phases, and both are simple FCC + BCC solid solutions.
FIG. 2 is a diagram of the gold phase of the as-cast and remelted high entropy alloy;
as seen in fig. 2: the cast-state and the remelting-state high-entropy alloys are distributed in a dendritic crystal structure, the dendritic crystal structure of the remelting-processed alloy is more compact, and the dendritic crystals are uniformly distributed and are equiaxed dendritic crystals.
FIG. 3 is a graph of hardness for the as-cast and remelted high entropy alloys;
as can be seen from fig. 3: the hardness of the re-melted high-entropy alloy is higher than that of the as-cast alloy, which indicates that the re-melting treatment improves the hardness of the high-entropy alloy.
FIG. 4 is a friction coefficient diagram of the as-cast and re-melted high-entropy alloy under the test force of an abrasion tester 20N;
fig. 4 shows: the average friction coefficient of the as-cast high-entropy alloy is about 0.24, and the fluctuation of the friction coefficient is large; the average friction coefficient of the re-melted high-entropy alloy is 0.13, and the fluctuation is small, which shows that the re-melting treatment reduces the friction coefficient of the high-entropy alloy and improves the wear resistance.
Detailed Description
Example 1: preparation of high-entropy alloy sample
Five pure metals of Co, Cr, Fe, Ni and Ti with the purity of 99.99 percent are selected as test materials. The mass percent is calculated according to the atomic ratio of 1:1:1:1:1, the total mass of the prepared alloy is 30g, the mass of each metal (6.47 g, 5.71g, 6.13g, 6.44g and 5.25g of Co, Cr, Fe, Ni and Ti respectively) is determined according to the mass percent, weighing and proportioning are carried out, then the metal raw material is placed in a water-cooled copper crucible of a high vacuum arc melting furnace, and melting is carried out under the protection of argon by adopting a non-consumable arc melting method. Firstly, vacuumizing to 2 x 10-3Pa, introducing argon to make the pressure reach 0.06-0.08MPa, cooling, turning over, smelting for the second time, and repeatedly smelting for at least 4 times to obtain CoCrFe with uniform componentsA NiTi master alloy; suction casting the CoCrFeNiTi master alloy into an as-cast high-entropy alloy by using a high-vacuum electric arc furnace; removing an oxide layer on the surface of the as-cast high-entropy alloy, placing the as-cast high-entropy alloy into absolute ethyl alcohol for an ultrasonic cleaning machine to vibrate and clean, removing impurities, particles and the like on the surface, placing the treated as-cast high-entropy alloy into a water-cooled copper crucible of a high-vacuum electric arc furnace, repeatedly smelting for 4 times, and carrying out suction casting through a copper mold to obtain the remelted high-entropy alloy.
Verification example:
1. analyzing the structure of the as-cast and remelting high-entropy alloy
The phases of the as-cast and remelted alloys were analyzed using an X-ray diffraction analyzer (XRD, Empyrean). The scanning speed is 4deg/min, the step length is 0.02 deg., the Cu target radiation, the working voltage and current are 40kV and 120mA respectively. And (3) analyzing XRD patterns of the as-cast and remelting high-entropy alloy.
FIG. 1 is a comparison graph of XRD energy spectrums of as-cast and re-melted high-entropy alloys, and it can be seen from the graph that only 3 sharper peaks appear in the XRD curve, and the as-cast and re-melted high-entropy alloys are analyzed to be simple FCC + BCC solid solutions.
FIG. 2 is a diagram of the gold phase of the as-cast and remelted high entropy alloy. As can be seen, the gold phase diagram of the as-cast and remelted high entropy alloys are both typical dendrite distributions. The dendritic crystal and the dendrite of the re-melted high-entropy alloy are distributed more uniformly, the structure is more compact, the grain boundary area is obviously distributed, and the grains are refined.
2. Testing the hardness of as-cast and re-melted high-entropy alloy by using MH-5 Vickers hardness tester
Measuring the hardness values of the as-cast and remelting high-entropy alloys by using an MH-5 Vickers hardness tester; the load of MH-5 Vickers hardness tester was set to 9.8N, and the loading time was set to 15 s. And selecting 7 points at different positions with the distance of 2mm on the center line of the sample for measurement, recording data, removing the maximum value and the minimum value of the obtained data, and finally calculating the average value of the remaining 5 points, wherein the value is the microhardness value of the alloy.
As can be seen from FIG. 3, the hardness of the remelted high-entropy alloy is higher than that of the as-cast high-entropy alloy, indicating that the remelting treatment increases the hardness of the alloy.
3. Abrasion resistance of as-cast and remelting high-entropy alloy is tested by abrasion tester
And performing a friction and wear test on the as-cast and remelting high-entropy alloy under a test force of 20N by using an MMS-2A wear tester, drawing a friction coefficient diagram by using origin to obtain data, and analyzing the wear resistance of the as-cast and remelting high-entropy alloy according to the comparison of the friction coefficients.
FIG. 4 shows the friction coefficients of the as-cast high-entropy alloy and the re-melted high-entropy alloy, and the re-melted high-entropy alloy has a more stable friction coefficient and a lower friction coefficient (0.13) than the as-cast high-entropy alloy (average value of 0.24). The friction coefficients of the two samples are smaller at the initial stage of friction, and because the surfaces of the samples are smoother at the initial stage of friction, the abrasion loss is reduced less, and the contact force of friction is also smaller; the coefficient of friction increases slowly with time. With the increase of the friction time, a small amount of oxide film is generated on the surface of the sample, adhesive abrasion is generated, the contact between a friction pair and the surface of the sample is reduced, and the friction coefficient fluctuates. The as-cast alloy has a large fluctuation in friction coefficient, and as the wear occurs, the wear gradually changes to wear by the abrasive grains, and the wear increases during the friction, thereby increasing the friction coefficient. The friction coefficient of the re-melted high-entropy alloy is stable and is related to the hardness of the alloy, and the abrasion mode is mainly frictional abrasion and enters a stable abrasion stage along with the increase of time.
5. And weighing the abrasion loss of the as-cast high-entropy alloy and the remelting high-entropy alloy after the frictional abrasion test by using an electronic balance.
The weighing results are shown in table 1, and compared with the as-cast high-entropy alloy, the wear loss of the remelting high-entropy alloy is obviously reduced, the wear rate is reduced, and the remelting treatment improves the wear resistance of the high-entropy alloy by combining the results of the friction coefficient.
TABLE 1 high entropy alloy Mass wear
Table 1 shows the comparison of the wear of the as-cast and the as-remelted high-entropy alloys. As can be seen from the table: the abrasion loss of the high-entropy alloy after remelting is obviously reduced, and the abrasion rate is reduced, so that the abrasion resistance of the high-entropy alloy can be effectively improved after remelting.
In the high-entropy alloy prepared in this example, the selected alloy component is CoCrFeNiTi. However, the metal material aimed at by the invention is not limited to the components, and the size of the sample can be changed by changing the size of the copper mould, and can be changed and adjusted according to the actual needs of tests and production; the alloy components can be determined according to the high-entropy alloy components and proportions disclosed in the prior literature, high-purity metals are selected, and the mass of each metal sample required is determined according to the atomic ratio. The invention can meet the requirements of different fields in production and life on wear-resistant materials.
Claims (1)
1. The remelting treatment is used for improving the hardness and the wear resistance of the high-entropy alloy CoCrFeNiTi,
the remelting treatment comprises the following steps:
the test material selects five pure metals of Co, Cr, Fe, Ni and Ti with the purity of 99.99 percent, the mass percent is calculated according to the atomic ratio of 1:1:1:1:1 and the like, the total mass of the prepared alloy is 30g, the mass of each metal is determined according to the mass percent, weighing and proportioning are carried out, then the metal raw material is placed in a water-cooled copper crucible of a high-vacuum arc melting furnace, the smelting is carried out under the protection of argon by adopting a non-consumable arc melting method, and the vacuum is firstly pumped to 2 multiplied by 10-3Pa, then filling argon to ensure that the air pressure reaches 0.06-0.08MPa, cooling, then turning over the alloy, carrying out secondary smelting, and repeatedly smelting for at least 4 times in such a way to obtain a CoCrFeNiTi master alloy with uniform components; then, carrying out suction casting on the CoCrFeNiTi master alloy into an as-cast high-entropy alloy by using a high-vacuum arc furnace; removing an oxide layer on the surface of the as-cast high-entropy alloy, placing the alloy into an ultrasonic cleaning machine, and vibrating and cleaning the alloy by using absolute ethyl alcohol to remove impurities and particles on the surface; the treated as-cast high-entropy alloy is put into a water-cooled copper crucible of a high-vacuum electric arc furnace, and is repeatedly smelted for 4 times, and the re-smelted high-entropy alloy with improved hardness and wear resistance is obtained by suction casting through a copper mould;
the hardness of the remelted high-entropy alloy is 911.96 HV; the average friction coefficient of the remelted high-entropy alloy is 0.13.
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| CN109628777B (en) * | 2019-01-23 | 2020-09-22 | 山东农业大学 | Method for improving corrosion resistance of high-entropy alloy |
| CN112210705A (en) * | 2020-09-14 | 2021-01-12 | 西安理工大学 | CuCrCoFeNiZrx high-entropy alloy and preparation method thereof |
| CN113969369A (en) * | 2021-10-22 | 2022-01-25 | 西北工业大学 | Novel Ti-Zr-Hf-Ni-Co-Cu high-entropy shape memory alloy and preparation method thereof |
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| CN101215663B (en) * | 2008-01-04 | 2010-06-16 | 哈尔滨工业大学 | High-entropy alloy-base composite material and preparation method thereof |
| CN102776430B (en) * | 2012-08-20 | 2014-08-06 | 太原理工大学 | AlCoCrFeNiTix high-entropy alloy material and method for preparing same |
| CN104152781B (en) * | 2014-09-04 | 2016-06-22 | 哈尔滨工业大学 | A kind of preparation method of AlCoCuFeNiSi high-entropy alloy |
| CN104674103B (en) * | 2015-03-10 | 2017-01-04 | 西北工业大学 | A kind of CrFeCoNiNbx high-entropy alloy and preparation method thereof |
| CN106756637B (en) * | 2016-12-06 | 2018-06-19 | 太原理工大学 | A kind of high entropy bulk metallic glass matrix composite and preparation method thereof |
| CN107267841B (en) * | 2017-06-14 | 2018-08-14 | 湘潭大学 | A kind of CrMoNbTaV high-entropy alloys and preparation method thereof |
| CN107267842A (en) * | 2017-06-26 | 2017-10-20 | 北京理工大学 | A kind of high-melting-point high-entropy alloy and preparation method thereof |
| CN107739956B (en) * | 2017-09-14 | 2019-10-29 | 北京理工大学 | A kind of Nb microalloying Ni-Co-Fe-Cr-Al high-entropy alloy |
| CN107699822B (en) * | 2017-09-20 | 2019-04-12 | 华中科技大学 | A kind of high entropy block amorphous alloy and preparation method thereof |
| CN108220742B (en) * | 2018-03-14 | 2022-10-18 | 北京中辰至刚科技有限公司 | Microalloyed Ti-Zr-Hf-V-Nb-Ta refractory high-entropy alloy and preparation method thereof |
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