CN111676410A - High-strength high-toughness CoFeNiTiV high-entropy alloy and preparation method thereof - Google Patents
High-strength high-toughness CoFeNiTiV high-entropy alloy and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-strength high-toughness CoFeNiTiV high-entropy alloy and a preparation method thereof, wherein the high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: 18-22% of Co, 18-22% of Fe, 18-22% of Ni, 18-22% of Ti and 22-26% of V; the CoFeNiTiV high-entropy alloy prepared by adopting a vacuum arc melting method has a BCC single-phase solid solution structure, the yield strength reaches over 2430MPa, the elongation at break reaches over 18 percent, and the CoFeNiTiV high-entropy alloy has high strength and high toughness.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a high-strength high-toughness CoFeNiTiV high-entropy alloy and a preparation method thereof.
Background
High-entropy alloys (HEA) generally comprise 5 or more than 5 metals as main elements, and the mole fraction of each element is 5-35%, and have a simple solid solution phase structure. The high-entropy alloy has the characteristics of high-entropy effect in thermodynamics, large lattice distortion effect in structure, delayed diffusion effect in kinetics, cocktail effect in performance and the like, so that the high-entropy alloy presents a simple solid solution phase with an FCC or BCC crystal structure on a microstructure. The factor contributing to the formation of this texture is the high entropy of mixing that the multi-elemental alloy has. At the same time, the absolute value of the enthalpy of mixing between the alloy constituents cannot be too high, so as to avoid the formation of intermetallic compounds or the formation of separate multinomial coexisting structures. The performance of the high-entropy alloy is high strength, high hardness, high temperature resistance, oxidation resistance and the like, the comprehensive performance of the high-entropy alloy is obviously superior to that of the traditional unit metal material or conventional alloy, and the application field of the high-entropy alloy is widened.
The high-entropy alloy is mainly prepared by adopting a vacuum arc melting process, under vacuum, utilizing high temperature generated by arc discharge between an electrode and two electrodes of a crucible as a heat source to rapidly heat and melt a high-purity metal raw material, and then rapidly cooling a melt by adopting a water-cooling copper mold to solidify the melt into an ingot in the crucible. The electric arc melting temperature is higher, so that the alloy with higher melting point can be melted, and the good effect on removing a plurality of impurities and certain gases is achieved. However, the prepared alloy is easy to have the phenomena of dendrite segregation and uneven components, and has the problems of coarse grains and low plasticity.
To date, a large number of high entropy alloys of various compositions have been reported, more than 50% of which contain the following five high frequency element groups: AlCrFeNi, CoCrFeNi, AlCoFeNi, AlCoCrNi and AlCoCrFe, which indicates that the research in the field of high-entropy alloys is still in the initial stage. Among the alloy systems that have been reported, a true single phase solid solution structure is observed in only a few alloys, including Co-Fe-Ni-Ti-Al, Co-Fe-Ni-Ti-Cr, and Co-Fe-Ni-Ti-Cu.
Research shows that the element composition is a key factor in alloy design, the alloy components can be obviously changed by adjusting the composition of alloy elements so as to influence the mechanical property of the alloy, even if one element is adjusted, the multielement high-entropy alloy can cause great difference between the phase structure and the performance, and has unpredictability. The problem of how to adjust the alloy components to improve the contradiction between the strength and the toughness of the high-entropy alloy becomes one of the technical problems which are urgently needed to be solved in the field of the high-entropy alloy.
Disclosure of Invention
In order to solve the technical problem of contradiction between strength and toughness of the high-entropy alloy, a high-strength high-toughness CoFeNiTiV high-entropy alloy and a preparation method thereof are provided. The CoFeNiTiV high-entropy alloy prepared by the method has excellent strength and plasticity, and plays an important role in promoting the engineering application of CoFeNiTiV series alloys.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: 18-22% of Co, 18-22% of Fe, 18-22% of Ni, 18-22% of Ti and 22-26% of V.
Further, the high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: 20% of Co, 19% of Fe, 20% of Ni, 20% of Ti and 21% of V.
Further, the high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: 21% of Co, 18% of Fe, 18% of Ni, 20% of Ti and 23% of V.
Further, the high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: 19% of Co, 19% of Fe, 18% of Ni, 20% of Ti and 24% of V.
Further, the purity of the metal simple substance is 99.9 wt%.
The invention also provides a preparation method of the high-strength high-toughness CoFeNiTiV high-entropy alloy, which comprises the following steps:
(1) removing impurities and oxides on the surfaces of metal simple substances Co, Fe, Ni, Ti and V, and cleaning and drying for later use;
(2) firstly melting a metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas, allowing titanium to adsorb oxygen remaining in a protective atmosphere so as to reduce oxidation behavior during high-entropy alloy melting, then adding the metal simple substance according to a ratio, vacuumizing, and carrying out arc melting under the protection of argon gas, wherein electromagnetic stirring is accompanied 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 difficult mixing and melting is caused;
(3) and (3) repeating the electric arc melting for multiple times on the button sample, overturning the button sample before repeating the electric arc melting for each time, cooling and removing a surface oxide layer of the button sample after the electric arc melting for multiple times is finished, repeating the step (2), and cooling to obtain the high-strength high-toughness CoFeNiTiV high-entropy alloy.
Further, removing the impurities and the oxides in the step (1) and polishing the impurities and the oxides by using a grinder or sand paper; the cleaning process adopts acetone as cleaning solvent to carry out oscillation cleaning for 5min in ultrasonic waves, and the power density of the ultrasonic waves is 0.8W/cm2And the frequency was 33 Hz.
Further, the vacuum pumping in the step (2) 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 (3), the melting state needs to be kept for 2-3 min in the process of repeating the arc melting for multiple times; the number of times is 4.
The beneficial technical effects are as follows:
the CoFeNiTiV high-entropy alloy is obtained by vacuum arc melting, has a BCC single-phase solid solution structure, does not have the phenomena of segregation, uneven components and thick grains by vacuum arc melting, has excellent toughness, has compressive yield strength exceeding that of a series of reported alloys, has yield strength of over 2430MPa, has elongation at break of over 18 percent, and has high strength and high toughness.
Drawings
FIG. 1 shows Co obtained in example 319Fe19Ni18Ti20V24XRD patterns of the high-entropy alloy, the CoFeNiTiCr high-entropy alloy of comparative example 1, the CoFeNiTiAl high-entropy alloy of comparative example 2 and the CoFeNiTiCu high-entropy alloy of comparative example 3.
FIG. 2 shows Co obtained in example 319Fe19Ni18Ti20V24Compression performance of the high entropy alloy and the CoFeNiTiCr high entropy alloy of comparative example 1 are compared.
In the above figures, -AC represents the as-cast high entropy alloy.
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-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: co 20%, Fe 19%, Ni 20%, Ti 20%, V21%, expressed as Co20Fe19Ni20Ti20V21。
Co of the present example20Fe19Ni20Ti20V21The preparation method of the high-entropy alloy comprises the following steps:
(1) grinding with SiC abrasive paper (80) to remove impurities and oxides on the surfaces of metal simple substances Co, Fe, Ni, Ti and V, wherein the purity of each metal simple substance is higher than 99.9 wt%, and then using acetone as a cleaning solvent and the power density is 0.8W/cm2And ultrasonic wave with frequency of 33Hz for 5min, and drying for later use;
(2) firstly melting a metallic titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to ensure that the titanium is remained in the protective atmosphere of adsorptionThe oxygen is used for reducing the oxidation behavior of the high-entropy alloy during smelting, the metal simple substance is added according to the proportion, and the vacuum pumping reaches 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 difficult mixing and melting is caused;
(3) repeating the arc melting for four times on the button sample, turning before repeating the arc melting for each time, keeping the molten alloy liquid for about 2min in the repeated arc melting process, cooling to obtain a button sample with the thickness of about 8mm, the diameter of about 15mm and a bright surface, further grinding off the surface oxide layer of the button sample by using an angle grinder, cutting the button ingot into samples with the weight of about 10 g by using a diamond saw, putting the samples into a non-consumable vacuum arc melting furnace, repeating the arc melting operation of the step 2, sucking the melted liquid alloy into a cylindrical copper mold with the diameter of 4mm and the length of 60mm, and cooling to obtain Co20Fe19Ni20Ti20V21High entropy alloy.
Example 2
A high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: co 21%, Fe 18%, Ni 18%, Ti 20%, V23%, expressed as Co21Fe18Ni18Ti20V23。
Co of the present example21Fe18Ni18Ti20V23The preparation method of the high-entropy alloy comprises the following steps:
(1) grinding by a grinding wheel machine to remove impurities and oxides on the surfaces of the metal simple substances of Co, Fe, Ni, Ti and V, wherein the purity of each metal simple substance is higher than 99.9 wt%, and then using acetone as a cleaning solvent and the power density of 0.8W/cm2And ultrasonic wave with frequency of 33Hz for 5min, and drying for later use;
(2) firstly melting a metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to ensure that the titanium adsorbs residual oxygen in protective atmosphere so as to reduce the oxidation behavior of the high-entropy alloy during melting, then adding the metal simple substance according to the proportion, and vacuumizing to 2 × 10-3Argon is reversely filled to 5Pa after Pa, arc melting is carried out for 45s 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 difficult mixing and melting is caused;
(3) repeating the arc melting for four times, turning before repeating the arc melting for each time, keeping the alloy molten liquid state for about 2.5min in the process of repeating the arc melting, cooling to obtain a button sample with the thickness of about 8mm, the diameter of about 15mm and a bright surface, further grinding off the surface oxide layer of the button sample by using an angle grinder, cutting the button ingot into samples with the weight of about 10 g by using a diamond saw, putting the samples into a non-consumable vacuum arc melting furnace, repeating the arc melting operation in the step 2, sucking the melted liquid alloy into a cylindrical copper mold with the diameter of 4mm and the length of 60mm, and cooling to obtain Co21Fe18Ni18Ti20V23High entropy alloy.
Example 3
A high-strength high-toughness CoFeNiTiV high-entropy alloy comprises the following metal simple substances in atomic percentage: co 19%, Fe 19%, Ni 18%, Ti 20%, V24%, expressed as Co19Fe19Ni18Ti20V24。
Co of the present example19Fe19Ni18Ti20V24The preparation method of the high-entropy alloy comprises the following steps:
(1) grinding with SiC sand paper of 80 # to remove impurities and oxides on the surfaces of the metallic simple substances of Co, Fe, Ni, Ti and V, wherein the purity of each metallic simple substance is higher than 99.9 wt%, and then using acetone as a cleaning solvent,The power density is 0.8W/cm2And ultrasonic wave with frequency of 33Hz for 5min, and drying for later use;
(2) firstly melting a metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon gas to ensure that the titanium adsorbs residual oxygen in protective atmosphere so as to reduce the oxidation behavior of the high-entropy alloy during melting, then adding the metal simple substance according to the 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 difficult mixing and melting is caused;
(3) repeating the arc melting for four times on the button sample, turning before repeating the arc melting for each time, keeping the molten alloy liquid state for about 3min in the repeated arc melting process, cooling to obtain a button sample with the thickness of about 8mm, the diameter of about 15mm and a bright surface, further grinding off the surface oxide layer of the button sample by using an angle grinder, cutting the button ingot into samples with the weight of about 10 g by using a diamond saw, putting the samples into a non-consumable vacuum arc melting furnace, repeating the arc melting operation of the step 2, sucking the melted liquid alloy into a cylindrical copper mold with the diameter of 4mm and the length of 60mm, and cooling to obtain Co19Fe19Ni18Ti20V24High entropy alloy.
For Co of this example19Fe19Ni18Ti20V24The high-entropy alloy adopts a Rigaku X-ray diffractometer to perform phase analysis, the working voltage and the current are respectively 40KV and 190mA, the X-ray source is CuK α (lambda is 0.1542nm) ray, the scanning angle 2 theta is 20-120 degrees, and the specific XRD result is shown in figure 1, and as can be seen from figure 1, the Co prepared by the method is19Fe19Ni18Ti20V24The high entropy alloy is a single phase solid solution with a structure of BCC ordered structure, denoted as B2 phase. For example 1 Co21Fe18Ni18Ti20V23And Co of example 221Fe18Ni18Ti20V23XRD phase analysis was also performed and the structure was consistent with that of example 3.
Comparative example 1
The comparative example is CoFeNiTiCr high-entropy alloy, each metal simple substance is prepared according to equal atomic proportion, and each metal element accounts for 20 percent. XRD phase analysis was performed on the CoFeNiTiCr high-entropy alloy of the present comparative example, and as shown in FIG. 1, it can be seen from FIG. 1 that the CoFeNiTiCr high-entropy alloy has a single-phase FCC structure.
Comparative example 2
The comparative example is CoFeNiTiAl high-entropy alloy, and each metal simple substance is prepared according to equal atomic proportion, and each metal element accounts for 20 percent. XRD phase analysis is carried out on the CoFeNiTiAl high-entropy alloy of the comparative example, as shown in figure 1, the CoFeNiTiAl high-entropy alloy is a single-phase B2 structure as can be seen from figure 1.
Comparative example 3
The comparative example is a CoFeNiTiCu high-entropy alloy, each metal simple substance is prepared according to equal atomic proportion, and each metal element accounts for 20 percent. XRD phase analysis was performed on the CoFeNiTiCu high-entropy alloy of the present comparative example, and as shown in FIG. 1, it can be seen from FIG. 1 that the CoFeNiTiCu high-entropy alloy has a single-phase FCC structure.
The high-entropy alloys of the above examples and comparative examples were subjected to hardness test and compression property test. The test results 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.
The compression performance test method comprises the following steps: the diameter of the cylindrical sample for the compression test is 3.7mm, the height of the cylindrical sample is 5.6mm, the axis of the sample is parallel to the outer surface of the cylinder, and the upper plane and the lower plane of the sample are parallel; compression testing was performed at room temperature using a computer controlled Instron (Instron, Norwood, MA) mechanical tester (fitted with a silicon carbide die). Between the compression surface and the silicon carbide mould in order to reduce frictionUsing a thin teflon foil, 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 Properties of CoFeNiTiV high entropy alloys of examples 1-3
Co of example 319Fe19Ni18Ti20V24FIG. 2 shows the compression performance of the high-entropy alloy, and it can be seen from FIG. 2 that Co19Fe19Ni18Ti20V24Compared with the CoFeNiTiCr high-entropy alloy of comparative example 1, the Co of the invention19Fe19Ni18Ti20V24The yield strength of the high-entropy alloy in an as-cast state is 2730MPa, the elongation at break is 21.3%, and the strength reaches a maximum value of 3909MPa before breaking; the CoFeNiTiCr high-entropy alloy has the yield strength of 1500MPa and the elongation at break of 9 percent. Compared with CoFeNiTiCr high-entropy alloy of single-phase FCC solid solution, the Co of the single-phase BCC solid solution of the invention19Fe19Ni18Ti20V24The yield strength of the high-entropy alloy is improved from 1500MPa to 2730MPa, the improvement amplitude exceeds 80%, and the elongation at break is improved from 9% to 21.3%. The CoFeNiTiV high-entropy alloy has excellent obdurability.
The CoFeNiTiV quinary high-entropy alloy system prepared by the invention is a BCC single-phase solid solution structure, and the number of the slippage systems in the BCC lattice structure is much less than that in FCC or HCP, so that the high-entropy alloy with the BCC structure has higher strength; meanwhile, the solid solution strengthening of V atoms and the firm combination among main elements of Co, Fe, Ni and Ti play an important role in improving the strength and toughness of the CoFeNiTiV five-element high-entropy alloy system.
The high-entropy alloy system has a single-phase solid solution structure, and has high strength and toughness and excellent obdurability. The preparation method is simple and reliable, and the selected elements are nontoxic and convenient to obtain, and have the advantages of good safety, 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-strength high-toughness CoFeNiTiV high-entropy alloy is characterized by comprising the following metal simple substances in atomic percentage: 18-22% of Co, 18-22% of Fe, 18-22% of Ni, 18-22% of Ti and 22-26% of V.
2. The high-strength high-toughness CoFeNiTiV high-entropy alloy is characterized by comprising the following metal elements in atomic percentage: 20% of Co, 19% of Fe, 20% of Ni, 20% of Ti and 21% of V.
3. The high-strength high-toughness CoFeNiTiV high-entropy alloy is characterized by comprising the following metal elements in atomic percentage: 21% of Co, 18% of Fe, 18% of Ni, 20% of Ti and 23% of V.
4. The high-strength high-toughness CoFeNiTiV high-entropy alloy is characterized by comprising the following metal elements in atomic percentage: 19% of Co, 19% of Fe, 18% of Ni, 20% of Ti and 24% of V.
5. The CoFeNiTiV high-entropy alloy with high strength and toughness as claimed in claim 1, wherein the purity of the elementary metal is 99.9 wt%.
6. The preparation method of the high-strength high-toughness CoFeNiTiV high-entropy alloy according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) removing impurities and oxides on the surfaces of metal simple substances Co, Fe, Ni, Ti and V, and cleaning and drying for later use;
(2) firstly melting a metal titanium block in a non-consumable vacuum arc melting furnace under the protection of argon, then adding the metal simple substance according to the proportion, vacuumizing, and 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;
(3) and (3) repeating the electric arc melting for multiple times on the button sample, overturning the button sample before repeating the electric arc melting for each time, cooling and removing a surface oxide layer of the button sample after the electric arc melting for multiple times is finished, repeating the step (2), and cooling to obtain the high-strength high-toughness CoFeNiTiV high-entropy alloy.
7. The preparation method of the high-strength high-toughness CoFeNiTiV high-entropy alloy according to claim 6, wherein the impurities and oxides removed in the step (1) are ground by using a grinder or sand paper; the cleaning process adopts acetone as cleaning solvent to carry out oscillation cleaning for 5min in ultrasonic waves, and the power density of the ultrasonic waves is 0.8W/cm2And the frequency was 33 Hz.
8. The method for preparing the CoFeNiTiV high-entropy alloy with high strength and toughness according to claim 6, wherein the vacuum pumping in the step (2) is up to 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 method for preparing the CoFeNiTiV high-entropy alloy with high strength and toughness according to claim 6, wherein the molten state is kept for 2-3 min in the process of repeating the arc melting for multiple times in the step (3); the number of times is 4.
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| CN114231818A (en) * | 2021-12-21 | 2022-03-25 | 中国科学院江西稀土研究院 | Light high-strength corrosion-resistant high-entropy alloy and preparation method thereof |
| CN114774753A (en) * | 2022-03-25 | 2022-07-22 | 江苏理工学院 | Light high-strength high-hardness CoCrNiTiV high-entropy alloy and preparation method thereof |
| CN114774752A (en) * | 2022-03-25 | 2022-07-22 | 江苏理工学院 | High-strength high-toughness TiZrNbMoV refractory high-entropy alloy and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114231818A (en) * | 2021-12-21 | 2022-03-25 | 中国科学院江西稀土研究院 | Light high-strength corrosion-resistant high-entropy alloy and preparation method thereof |
| CN114231818B (en) * | 2021-12-21 | 2023-03-03 | 中国科学院江西稀土研究院 | Light high-strength corrosion-resistant high-entropy alloy and preparation method thereof |
| CN114774753A (en) * | 2022-03-25 | 2022-07-22 | 江苏理工学院 | Light high-strength high-hardness CoCrNiTiV high-entropy alloy and preparation method thereof |
| CN114774752A (en) * | 2022-03-25 | 2022-07-22 | 江苏理工学院 | High-strength high-toughness TiZrNbMoV refractory high-entropy alloy and preparation method thereof |
| CN114774752B (en) * | 2022-03-25 | 2023-12-22 | 江苏理工学院 | High-strength high-toughness TiZrNbMoV refractory high-entropy alloy and preparation method thereof |
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