CN111690863A - High-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and preparation method thereof - Google Patents
High-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and a preparation method thereof, and the alloy comprises the following metal raw materials of Cr, Cu, Fe, Ni and V, wherein each metal raw material is prepared according to the atomic percentage of 17-22% and the like; the preparation method comprises the following steps: firstly melting a metal titanium block in a vacuum arc melting furnace under the protection of argon, then adding metal raw materials according to the proportion, vacuumizing, carrying out arc melting under the protection of argon, carrying out electromagnetic stirring, and cooling to obtain a button sample; repeating the arc melting process for multiple times, removing the surface oxide layer, repeating the arc melting process for one time, and cooling to obtain the high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy; the alloy has a BCC + FCC + Tetragonal three-phase structure in an as-cast state, has the hardness of more than 750HV and the yield strength of more than 1250MPa, and has ultrahigh hardness and good toughness.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and a preparation method thereof.
Background
Traditional alloy systems are based primarily on a simple design: an element with a certain special property is used as a matrix, and a small amount of other elements are added to improve the property of the element. Because of the limited number of metallic elements, the choice of alloy development is limited. Yeh et al propose a concept of high-entropy alloy that greatly expands the possibility of novel multi-element metal alloys, the number of main elements of the high-entropy alloy is not less than 5, and the atomic fraction of each element is at least more than 5% but not more than 35%. The high-entropy alloy has a high-entropy effect, and the effect can inhibit the formation of brittle intermetallic compounds among elements, so that a solid solution with a unique microstructure such as simple face-centered cubic structure, body-centered cubic structure and the like is formed. The high entropy effect is mainly derived from the composition of multiple elements in the high entropy alloy in an equimolar ratio or an approximately equimolar ratio, and as the number of the components is increased, the entropy value of the system is improved, and further the stability of the solid solution is greatly improved. In the last 15 years, a large number of multi-element high-entropy alloys have been developed and reported, and the microstructures of the alloys are different, and the properties of the alloys are also greatly different. The high-entropy alloy has great application potential in the fields of aerospace, petrochemical industry, dies, mechanical parts and the like.
The performance of the alloy is determined by the microstructure, and the microstructure can cause great difference of the phase structure and the performance of the obtained high-entropy alloy along with different compositions of alloy elements, so that the alloy is unpredictable. For example, the reported Cr-Cu-Fe-Ni-Co, Cr-Cu-Fe-Ni-Mn and Cr-Cu-Fe-Ni-Al alloys with equal molar ratios of elements have the same four matrix elements of Cr-Cu-Fe-Ni, only one element is replaced, but the phase structures are obviously different, and the performances are greatly different, so that the high sensitivity of the microstructure of the high-entropy alloy to the composition of alloy elements is demonstrated. Therefore, the improvement of the mechanical properties of the alloy by adjusting the components of the alloy is one of the technical problems to be solved urgently in the field of high-entropy alloy.
Disclosure of Invention
In order to solve the technical problem of improving the mechanical property of the alloy, a high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy and a preparation method thereof are provided. The Cr-Cu-Fe-Ni-V high-entropy alloy has ultrahigh hardness and good obdurability
In order to achieve the purpose, the invention is realized by the following technical scheme:
a high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy comprises the following metal raw materials of Cr, Cu, Fe, Ni and V, wherein each metal raw material is prepared according to the atomic percentage of 17-22% and the like.
Further, each metal raw material is prepared according to the following atomic percentages: 20% of Cr, 20% of Cu, 19% of Fe, 20% of Ni and 21% of V.
Further, each metal raw material is prepared according to the following atomic percentages: 21% of Cr, 18% of Cu, 20% of Fe, 21% of Ni and 20% of V.
Further, each metal raw material is prepared according to the following atomic percentages: 21% of Cr, 17% of Cu, 20% of Fe, 20% of Ni and 22% of V.
Further, the purity of the metal raw material is more than 99.9 wt%.
The preparation method of the high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy comprises the following steps:
(1) preparing metal raw materials Cr, Cu, Fe, Ni, V and a metal titanium block according to a ratio, firstly melting the metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas, allowing titanium to adsorb residual oxygen in a protective atmosphere so as to reduce oxidation behavior during high-entropy alloy melting, then putting the metal raw materials according to the ratio, vacuumizing, carrying out arc melting under the protection of argon gas, carrying out electromagnetic stirring in the process of arc melting so as to increase the uniformity of alloy mixing, and cooling to obtain a button sample; if the oxygen content in the argon protective atmosphere is too high in the smelting process, the alloy generates oxide scales, the oxide scales are crushed and enter the alloy in the smelting process, oxide inclusions are introduced into the alloy, or the condition of immiscible is caused;
(2) and repeating the electric arc melting process for the button sample for multiple times, cooling and removing a surface oxide layer of the button sample after the electric arc melting process for multiple times is finished, repeating the electric arc melting process for one more time, and cooling to obtain the high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy.
Further, after the metal raw material is prepared in the step (1), a process of cleaning the metal raw material is also included, so as to remove impurities and oxides on the surface of the metal raw material, and the cleaning process is to grind the metal raw material by using a grinder or sand paperAnd then using acetone as a cleaning solvent to perform oscillation cleaning on the metal raw material in ultrasonic waves for 5min, wherein the power density of the ultrasonic waves is 0.8W/cm2And the frequency was 33 Hz.
Further, in step (1), the vacuum pumping reaches 2 × 10-3Filling argon to 5Pa after Pa; the electric arc melting current is 50A-100A, and the time is 30 s-1 min.
Further, in the step (2), the button sample is turned over before the arc melting process is repeated for each time, and the melting state is required to be kept for 2-3 min in the repeated arc melting process; the number of times is 4.
The beneficial technical effects are as follows: the Cr-Cu-Fe-Ni-V high-entropy alloy has a three-phase structure of BCC + FCC + Tetragonal in an as-cast state, has the hardness of more than 750HV, the yield strength of more than 1250MPa, ultrahigh hardness and good toughness.
Drawings
FIG. 1 shows Cr in example 321Cu17Fe20Ni20V22XRD spectra of the high-entropy alloy, the Cr-Cu-Fe-Ni-Al high-entropy alloy of comparative example 1, the Cr-Cu-Fe-Ni-Mn high-entropy alloy of comparative example 2, and the Cr-Cu-Fe-Ni-Co high-entropy alloy of comparative example 3; in the figure, — AC represents an as-cast state, and-a represents after annealing heat treatment.
FIG. 2 shows Cr in example 321Cu17Fe20Ni20V22High entropy alloy compression performance diagram.
Detailed Description
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 only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
A high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy comprises the following metal raw materials of Cr 20%, Cu 20%, Fe 19%, Ni 20% and V21% in atomic percentage, wherein the metal raw materials are represented by Cr20Cu20Fe19Ni20V21High entropy alloy.
Above Cr20Cu20Fe19Ni20V21The preparation method of the high-entropy alloy comprises the following steps:
(1) preparing the metal raw materials of Cr, Cu, Fe, Ni, V and the metal titanium block according to the proportion, polishing the technical raw materials and the metal titanium block by a grinding machine to remove impurities and oxides on the surface, wherein the purity of each metal raw material is higher than 99.9 wt%, using acetone as a cleaning solvent after polishing, and controlling the power density to be 0.8W/cm2And carrying out oscillation cleaning for 5min in an ultrasonic cleaning machine with the frequency of 33Hz, and drying;
melting metallic titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to make titanium adsorb residual oxygen in protective atmosphere so as to reduce oxidation behavior during melting of high-entropy alloy, adding the above metallic raw materials according to proportion, and vacuumizing to 2 × 10-3Argon is reversely filled to 5Pa after Pa, arc melting is carried out for 1min at a current of 60A under the protection of argon, the uniformity of alloy mixing is increased along with electromagnetic stirring in the process of arc melting, and a button sample is obtained after cooling; if the oxygen content in the argon protective atmosphere is too high in the smelting process, the alloy generates oxide scales, the oxide scales are crushed and enter the alloy in the smelting process, oxide inclusions are introduced into the alloy, or the condition of immiscible is caused;
(2) repeating the arc melting process for 4 times on the button sample, overturning the button sample before repeating the arc melting process for each time, cooling and removing a surface oxide layer of the button sample after the multiple arc melting processes are finished, repeating the arc melting process again, and cooling to obtain high-hardness Cr20Cu20Fe19Ni20V21High entropy alloy.
Example 2
A high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy comprises the following metal raw materials of Cr 21%, Cu 18%, Fe 20%, Ni 21% and V20% in atomic percentage, wherein the metal raw materials are represented by Cr21Cu18Fe20Ni21V20High entropy alloy.
Above Cr21Cu18Fe20Ni21V20The preparation method of the high-entropy alloy comprises the following steps:
(1) preparing Cr, Cu, Fe, Ni, V and a metallic titanium block as metal raw materials according to a ratio, polishing the technical raw materials and the metallic titanium block by using SiC sand paper with the reference number of 80 to remove impurities and oxides on the surface, wherein the purity of each metal raw material is higher than 99.9 wt%, using acetone as a cleaning solvent after polishing, and performing cleaning at the power density of 0.8W/cm2And carrying out oscillation cleaning for 5min in an ultrasonic cleaning machine with the frequency of 33Hz, and drying;
melting metallic titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to make titanium adsorb residual oxygen in protective atmosphere so as to reduce oxidation behavior during melting of high-entropy alloy, adding the above metallic raw materials according to proportion, and vacuumizing to 2 × 10-3Argon is reversely filled to 5Pa after Pa, arc melting is carried out for 40s under the protection of argon at a current of 80A, the uniformity of alloy mixing is increased along with electromagnetic stirring in the process of arc melting, and a button sample is obtained after cooling; if the oxygen content in the argon protective atmosphere is too high in the smelting process, the alloy generates oxide scales, the oxide scales are crushed and enter the alloy in the smelting process, oxide inclusions are introduced into the alloy, or the condition of immiscible is caused;
(2) repeat on the button sample 4And in the secondary arc melting process, the button sample is turned over before the arc melting is repeatedly carried out each time, after the multiple arc melting processes are finished, the surface oxide layer of the button sample is cooled and removed, the arc melting process is repeated again, and the high-hardness Cr is obtained after cooling21Cu18Fe20Ni21V20High entropy alloy.
Example 3
A high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy comprises the following metal raw materials of Cr 21%, Cu 17%, Fe 20%, Ni 20% and V22% in atomic percentage, wherein the metal raw materials are represented by Cr21Cu17Fe20Ni20V22High entropy alloy.
Above Cr21Cu17Fe20Ni20V22The preparation method of the high-entropy alloy comprises the following steps:
(1) preparing the metal raw materials of Cr, Cu, Fe, Ni, V and the metal titanium block according to the proportion, polishing the technical raw materials and the metal titanium block by a grinding machine to remove impurities and oxides on the surface, wherein the purity of each metal raw material is higher than 99.9 wt%, using acetone as a cleaning solvent after polishing, and controlling the power density to be 0.8W/cm2And carrying out oscillation cleaning for 5min in an ultrasonic cleaning machine with the frequency of 33Hz, and drying;
melting metallic titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to make titanium adsorb residual oxygen in protective atmosphere so as to reduce oxidation behavior during melting of high-entropy alloy, adding the above metallic raw materials according to proportion, and vacuumizing to 2 × 10-3Argon is reversely filled to 5Pa after Pa, arc melting is carried out for 30s under the protection of argon at the current of 100A, the uniformity of alloy mixing is increased along with electromagnetic stirring in the process of arc melting, and a button sample is obtained after cooling; if the oxygen content in the argon protective atmosphere is too high in the smelting process, the alloy generates oxide scales, the oxide scales are crushed and enter the alloy in the smelting process, oxide inclusions are introduced into the alloy, or the condition of immiscible is caused;
(2) repeating the arc melting process 4 times on the button sample, and repeating the arc each timeTurning the button sample before smelting, cooling and removing a surface oxide layer of the button sample after multiple electric arc smelting processes are finished, repeating the electric arc smelting processes again, and cooling to obtain high-hardness Cr21Cu17Fe20Ni20V22High entropy alloy.
Comparative example 1
The comparative example is Cr-Cu-Fe-Ni-Al high-entropy alloy, and each metal raw material is prepared according to equal atomic proportion, and each metal element accounts for 20 percent.
Comparative example 2
The comparative example is Cr-Cu-Fe-Ni-Mn high-entropy alloy, and each metal raw material is prepared according to equal atomic proportion, and each metal element accounts for 20 percent.
Comparative example 3
The comparative example is Cr-Cu-Fe-Ni-Co high-entropy alloy, and each metal raw material is prepared according to equal atomic proportion, and each metal element accounts for 20 percent.
Comparative example 4
Cr of this comparative example21Cu17Fe20Ni20V22The high entropy alloy is Cr of example 321Cu17Fe20Ni20V22The high-entropy alloy is obtained after annealing heat treatment for 20 hours at 1673K.
Cr for example 321Cu17Fe20Ni20V22The high-entropy alloy and the high-entropy alloys of comparative examples 1 to 3 were subjected to phase analysis using a Rigaku X-ray diffractometer, the operating voltage and current were 40KV and 190mA, respectively, the X-ray source was CuK α (λ 0.1542nm) radiation, and the scanning angle 2 θ was 20 to 120 °21Cu17Fe20Ni20V22The XRD spectrogram of the high-entropy alloy is shown in figure 1, and as can be seen from figure 1, the phase structures of the Cr-Cu-Fe-Ni-based high-entropy alloy are obviously different after different alloy elements are added, the Cr-Cu-Fe-Ni-Co high-entropy alloy in the comparative example 3 is a single-phase FCC solid solution structure, the Cr-Cu-Fe-Ni-Mn high-entropy alloy in the comparative example 2 is a BCC +2FCC three-phase structure, and the Cr-Cu-Fe-Ni-Al high-entropy alloy in the comparative example 1 is a BCC + FCC + AlFeNi intermetallic compound three-phase structure; book and notebookInvention Cr21Cu17Fe20Ni20V22The phase structure of the high-entropy alloy is BCC + FCC + Tetragonal, and the phase structure of the high-entropy alloy of the comparative example 4 obtained after annealing heat treatment is not changed.
The above examples and comparative examples were subjected to hardness test and compression energy test. The test data are shown in table 1.
The hardness test method comprises the following steps: the samples were placed on an HVS-1000 type digital display microhardness tester, and under a load of 0.5kg, a Vickers microhardness of 30s was measured on the polished cross section using a 136 DEG Vickers diamond pyramid, 10 points were measured on each sample, and finally the data were averaged.
Method for compression testing of cylindrical test piece for compression testing 3.7mm in diameter and 5.6mm in height with axis parallel to the outer surface of the cylinder and upper and lower planes parallel, compression testing was performed at room temperature using a computer controlled Instron (Norwood, MA) mechanical tester (equipped with a silicon carbide die), a thin teflon foil was used between the compression surface and the silicon carbide die to reduce friction, and 5.6 × 10 was applied to the sample-3Constant compression speed of mm/s, corresponding to 10-3s-1The initial strain rate of.
TABLE 1 As-cast Performance data for each of the high entropy alloys of the examples and comparative examples
| Hardness (HV) | Yield strength (MPa) | Elongation at Break (%) | |
| Example 1 | 778 | 1368 | 8.8 |
| Example 2 | 750 | 1256 | 8.2 |
| Example 3 | 768 | 1350 | 8.3 |
| Comparative example 1 | 480 | -- | -- |
| Comparative example 2 | 250 | -- | -- |
| Comparative example 3 | 120 | -- | -- |
Cr of example 321Cu17Fe20Ni20V22FIG. 2 shows the compression behavior of the high-entropy alloy, and FIG. 2 shows that as-cast Cr21Cu17Fe20Ni20V22The yield strength of the high-entropy alloy is 1350MPa, the maximum value of the strength before fracture reaches 1500MPa, the elongation at break is 8.3%, and the high-entropy alloy has high strength and good plasticity.
The Cr-Cu-Fe-Ni-V five-element high-entropy alloy system prepared by the invention has a phase structure of FCC phase + hard BCC phase + Tetragonal phase, so that the as-cast high-entropy alloy, especially the hardness, is remarkably improved compared with other reported Cr-Cu-Fe-Ni-based high-entropy alloys, and meanwhile, good plasticity is maintained. With the difference of one element, the high-entropy alloy has obvious difference of phase structure, and finally, the great difference of performance is caused. This provides beneficial hint for controlling the generated phase by changing the alloy elements, and further improving the alloy performance.
Cr prepared by the invention21Cu17Fe20Ni20V22The alloy is a BCC + FCC + Tetragonal three-phase structure in an as-cast state, has the hardness of 768HV, the yield strength of 1350MPa, the breaking strength of 1500MPa and the breaking elongation of 8.3 percent, and has ultrahigh hardness and good toughness. The preparation method is simple and reliable, and the selected elements are nontoxic and convenient to obtain, and have the advantages of good economical efficiency, good alloy performance and high application value.
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 (9)
1. The high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy is characterized by comprising the following metal raw materials of Cr, Cu, Fe, Ni and V, wherein each metal raw material is prepared according to the atomic percentage of 17-22% and the like.
2. The high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy according to claim 1, wherein each of the metal raw materials is prepared from the following atomic percentages: 20% of Cr, 20% of Cu, 19% of Fe, 20% of Ni and 21% of V.
3. The high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy according to claim 1, wherein each of the metal raw materials is prepared from the following atomic percentages: 21% of Cr, 18% of Cu, 20% of Fe, 21% of Ni and 20% of V.
4. The high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy according to claim 1, wherein each of the metal raw materials is prepared from the following atomic percentages: 21% of Cr, 17% of Cu, 20% of Fe, 20% of Ni and 22% of V.
5. A high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy as claimed in claim 1, wherein the purity of the metallic starting material is greater than 99.9 wt%.
6. A preparation method of the high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) preparing metal raw materials of Cr, Cu, Fe, Ni and V and a metal titanium block according to a ratio, firstly melting the metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon, then putting the metal raw materials according to the ratio, vacuumizing, and then carrying out arc melting under the protection of argon, wherein the process of arc melting is accompanied with electromagnetic stirring, and cooling to obtain a button sample;
(2) and repeating the electric arc melting process for the button sample for multiple times, cooling and removing a surface oxide layer of the button sample after the electric arc melting process for multiple times is finished, repeating the electric arc melting process for one more time, and cooling to obtain the high-hardness Cr-Cu-Fe-Ni-V high-entropy alloy.
7. The method according to claim 6, wherein the step (1) further comprises a step of cleaning the raw metal material after preparing the raw metal material, wherein the cleaning step comprises grinding the raw metal material by using a grinder or sand paper, and then washing the raw metal material by using acetone as a cleaning solvent in an ultrasonic wave with a power density of 0.8W/cm for 5min2And the frequency was 33 Hz.
8. The method according to claim 6, wherein the evacuation in step (1) is performed to a vacuum level of 2 × 10- 3Filling argon to 5Pa after Pa; the electric arc melting current is 50A-100A, and the time is 30 s-1 min.
9. The preparation method according to claim 6, wherein in the step (2), the button sample is turned over before repeating the arc melting process for each time, and the melting state is kept for 2-3 min during repeating the arc melting process for multiple times; the number of times is 4.
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| CN115404367A (en) * | 2022-08-29 | 2022-11-29 | 南京理工大学 | Superhard as-cast NiAlCoFeNb two-phase high-entropy alloy and preparation method thereof |
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