CN113046615B - Preparation method of HCP (host-P) phase high-entropy alloy with high strength - Google Patents
Preparation method of HCP (host-P) phase high-entropy alloy with high strength Download PDFInfo
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- CN113046615B CN113046615B CN202110271484.3A CN202110271484A CN113046615B CN 113046615 B CN113046615 B CN 113046615B CN 202110271484 A CN202110271484 A CN 202110271484A CN 113046615 B CN113046615 B CN 113046615B
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention relates to a high-strength HCP phase high-entropy alloy and a preparation method thereof, and is characterized in that: high-purity metal powder Co, Cr, Fe, Ni, Ta and Nb are used as raw materials, firstly, single powder is mechanically mixed in a high-energy ball mill according to a certain proportion and then is put into a vacuum drying oven for drying, and then, the high-entropy alloy is obtained by layer-by-layer accumulation by adopting a powder plasma arc additive manufacturing technology; after XRD identification and precipitated phase mechanical property test are carried out on the high-strength HCP-phase high-entropy alloy, the high-strength HCP-phase high-entropy alloy containing Ta and Nb has higher-strength HCP-phase and mechanical property, and under the condition that the substitution scheme of substituting partial Ta by Nb provided by the scheme does not change the precipitated phase type and phase components of the high-entropy alloy, the technical scheme is adopted, so that the performance of the high-entropy alloy is ensured, and the material cost is greatly saved by substituting Ta with relatively less reserve.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a preparation method of a high-strength HCP (host-P) phase high-entropy alloy.
Background
Ta and Nb occur in symbiotic form in nature, with the average content of Nb in the earth being 0.002%, while Ta is only 0.000006%. The tantalum alloy and the niobium alloy are widely applied to engineering bridges, superconducting materials, biological metals and the like, and have great development potential. Therefore, it is urgently needed to find a new substance capable of realizing higher mechanical property on the basis of retaining the property of Ta, and the problem to be solved by researchers at present is solved. Taking CoCrFeNi-based high-entropy alloy which is widely researched in recent years and has application potential as an example, the strength and hardness of CoCrFeNi can be obviously improved by adding Ta and Nb, and the effect of improving the corrosion resistance of CoCrFeNi is also obvious. Research shows that Ta and Nb with the same components are added, and Ta can promote the improvement of the mechanical property of the CoCrFeNi alloy. Considering that both can produce precipitates of the same crystal structure, the applicant tried to replace part of Ta in cocrfenita0.4 with Nb to achieve higher strength in a lower cost manner.
The factors influencing the mechanical properties of the alloy are more, but the types of precipitated phases, volume fractions and sizes of crystal grains are mainly used. The grain size determination is mainly suitable for the same metal, and the volume fraction and hardness of precipitated phases are particularly important for metals with different components. And increasing the volume fraction of precipitated phase inevitably leads to alloy brittle fracture, which is suitable for the contrary. On the premise of certain phase volume fraction distribution, improving the hardness of a precipitated phase undoubtedly becomes an effective method for improving the comprehensive performance of the alloy. However, what kind of preparation method is adopted, and how to select proper process parameters and preparation method, the high-entropy alloy with higher strength is produced by using a cheaper technology becomes a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength HCP phase high-entropy alloy, which provides a high-entropy alloy with similar phase volume fraction and higher phase hardness by adjusting the content and atomic percentage of elements in the high-entropy alloy, and the alloy has higher Vickers hardness and provides a basis for preparing the high-strength high-toughness high-entropy alloy.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a high-strength HCP-phase high-entropy alloy is characterized in that the high-entropy alloy comprises high-entropy alloy powder consisting of elementary substance powder of Co, Cr, Fe, Ni, Ta and Nb, and the atomic percentage of the high-entropy alloy powder is 1: 1: 1: 1: 0.2: 0.3, the preparation method comprises the following steps:
s1, mixing the single-component powder in a vacuum glove box according to a certain proportion, putting the mixture and alumina grinding balls into a ball milling tank, wherein the mass ratio of the powder balls is 1:3, and the high-energy ball mill runs in a mode of rotating forwards for 5 minutes, stopping for 5 minutes, then rotating backwards for 5 minutes and stopping for 5 minutes, and the running time is 12 hours in total:
s2: drying the uniformly mixed high-entropy alloy powder in a vacuum drying oven for 5 hours, and storing the dried high-entropy alloy powder in a closed container for later use;
s3: polishing a substrate used in plasma deposition by using an angle grinder, and then cleaning the substrate by using alcohol and acetone in sequence to remove oil stains on the surface;
s4: performing layer-by-layer deposition on the dried high-entropy alloy powder by adopting powder plasma arc additive manufacturing equipment, wherein the scanning speed of the powder plasma arc additive manufacturing equipment is 400mm/Min, the deposition current is 110A, the powder feeding rotating speed is 35r/Min, the ionic gas flow is 3L/Min, the protective gas flow is 9L/Min, the powder feeding gas flow is 4L/Min, the gas types are argon, and the high-entropy alloy is prepared by deposition in a layer-by-layer accumulation manner;
s5: the deposition interval between the deposition layers of the high-entropy alloy is not less than two minutes, and the oxide skin accumulation on the metal surface caused by insufficient protective gas is removed by adopting an angle grinder within the interval time after each deposition layer is completely stacked.
Preferably, in the powder plasma arc additive manufacturing process, the purity of each component of Co, Cr, Fe, Ni, Ta and Nb is more than 99.95%, and the granularity is 150-300 meshes.
Preferably, steps S1, S2 are both performed in a vacuum environment to avoid oxidation of the high entropy alloy powder prior to printing.
Compared with the prior art, the invention has the following advantages:
(1) the invention successfully provides a preparation method of a HCP phase with higher strength on the premise of saving at least 12% of material cost by replacing part of Ta in the CoCrFeNiTa alloy with Nb and designing the proper proportion of Ta and Nb. The prepared high-entropy alloy has higher strength and hardness.
(2) The invention solves the problem of less Ta in nature, provides a replacement scheme for the application of Ta alloy, and the alloy prepared by the invention has no macroscopic defects such as pores, cracks and the like.
(3) The method provided by the invention has the advantages of simplicity and high efficiency, and the plasma arc deposition equipment has higher efficiency and lower equipment price than laser deposition equipment, thereby having higher economic benefit and wide application prospect.
Drawings
FIG. 1 is an XRD pattern of a high entropy alloy prepared by the present invention and a control group;
FIG. 2 is a phase volume fraction diagram of a high entropy alloy prepared according to the present invention and a control group;
FIG. 3 is a diagram showing the phase hardness morphology and the nano-hardness values of the high-entropy alloy prepared by the present invention and a control group.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflicting with each other.
The invention is described in further detail below with reference to figures 1-3.
A high-entropy HCP alloy with high strength, wherein the powder of the high-entropy alloy consists of Co, Cr, Fe, Ni, Ta and Nb, and the atomic percentage is 1: 1: 1: 1: 0.2: 0.3, the purity of each metal powder is more than 99.95 percent, and the granularity is 150-300 meshes.
Example (b):
to illustrate the feasibility of the method, two control groups of CoCrFeNiTa0.4 and CoCrFeNiNb0.4 high-entropy alloys were set.
The preparation method comprises the following steps:
and S1, mixing the monomer powder in a vacuum glove box, and putting the mixture and alumina grinding balls into a ball milling tank, wherein the mass ratio of the powder balls is 1: 3. The high-energy ball mill was operated for a total of 12 hours by rotating forward for 5 minutes, stopping for 5 minutes, and then rotating backward for 5 minutes, stopping for 5 minutes. So as to avoid the metal cold welding caused by overhigh temperature during the rotation.
And S2, drying the uniformly mixed high-entropy alloy powder in a vacuum drying oven for 5 hours, and storing in a closed container for later use.
And S3, polishing the substrate used in plasma deposition by an angle grinder, and then cleaning the substrate by alcohol and acetone in sequence to remove oil stains on the surface.
S4, performing layer-by-layer deposition on the dried high-entropy alloy powder by adopting powder plasma arc additive manufacturing equipment, wherein the scanning speed is 400 mm/Min; the deposition current is 110A; the powder feeding speed is 35 r/Min; the ionic gas flow is 3L/Min; the protective gas flow is 9L/Min; the flow rate of the powder feeding gas is 4L/Min. The gas type was argon, and high entropy alloys of 150 × 20 × 15mm size were deposited in a layer-by-layer build up.
And S5, the interval between the deposited layers is not less than two minutes, so that the oxide skin accumulation on the metal surface caused by insufficient protective gas can be removed by using an angle grinder, and the comprehensive mechanical property of the alloy is influenced.
The crystal structures of the high-entropy alloy prepared in the example and the control group are shown in FIG. 1. As can be seen from the figure, the cocrfenita0.2nb0.3 alloy has diffraction peaks of Fe7(TaNb)3, Co2Ta, and Fe2Nb, respectively, in addition to the FCC diffraction peak, similar to the cocrfenita0.4 and cocrfeninb0.4 alloys. Further, diffraction spots of the precipitated phases of the alloys were calibrated by a Transmission Electron Microscope (TEM), and the three phases were found to have the same crystal structure (HCP phase).
The high entropy alloys CoCrFeNiTa0.2Nb0.3, CoCrFeNiTa0.4 and CoCrFeNiNb0.4 prepared in the examples were subjected to phase composition and volume fraction measurement as shown in FIG. 2. The results of the examination using a Tescan-Mira-3-XH scanning electron microscope equipped with an EBSD (Oxford-Nordly-Max3) probe revealed that the three had the same Ta and Nb content, both at about 24at%, in the precipitated phase components. The volume fraction of the phases is similar to 20-25%.
The high entropy alloys CoCrFeNiTa0.2Nb0.3, CoCrFeNiTa0.4 and CoCrFeNiNb0.4 prepared in the examples were subjected to phase hardness, respectively, as shown in FIG. 3. The measurement of the phase hardness is carried out by adopting a nano-indenter (G200-Keysight), the test result and the topographic map of nano-indentation are shown in figure 3, and it can be seen that the nano-hardness of the precipitated phase under the combined action of Ta and Nb is higher than that of the precipitated phase in the CoCrFeNiTa0.4 and CoCrFeNiNb0.4 high-entropy alloys. It is worth noting that nano-indentation is not easy to be completely distributed in HCP phase due to the existence of more fine HCP phase in the CoCrFeNiTa0.2Nb0.3 high-entropy alloy, and theoretically, the hardness of HCP phase in the Ta0.2Nb0.3 high-entropy alloy should be higher than 13.3 GPa. For this reason, after the cocrfenita0.2nb0.5 high-entropy alloy was prepared again by the above process and the precipitated phase composition thereof was examined, it was found that the sum of the contents of Ta and Nb in the HCP phase was 25.8at% which was almost the same as the HCP phase composition in the three high-entropy alloys measured previously. The hardness of the HCP phase in ta0.2nb0.5 was 15.8GPa as measured by the phase hardness, and therefore it was concluded that the hardness of the HCP phase in ta0.2nb0.3 was close to 15.8GPa and significantly higher than the phase hardness of Ta and Nb acting alone on CoCrFeNi.
The high-entropy alloys CoCrFeNiTa0.2Nb0.3, CoCrFeNiTa0.4 and CoCrFeNiNb0.4 prepared in the examples are subjected to Vickers hardness and tensile property tests, and the hardness (468 HV) of the CoCrFeNiTa0.2Nb0.3 is remarkably higher than the hardness (382 HV) of the CoCrFeNiTa0.4 and the CoCrFeNiNb0.4; all three alloys have low elongation, which is typical of brittle fracture. The fracture strength (716 MPa) of the CoCrFeNiTa0.2Nb0.3 is higher than that of CoCrFeNiTa0.4 (692 MPa) and CoCrFeNiNb0.4 (505 MPa).
Compared with the price of 0.4 of CoCrFeNiTa0.2Nb0.3 per mole of CoCrFeNiTab, the price of the CoCrFeNiTa0.3 per mole of the preparation method saves at least 12% of material cost, and has wide application prospect.
The invention utilizes Ta and a symbiotic element Nb, takes CoCrFeNi-based high-entropy alloy as an example, replaces partial Ta in CoCrFeNiTa0.4, realizes that the hardness of a precipitated phase is obviously improved on the premise of not changing the type, the components, the tissue structure and the volume fraction of the precipitated phase, and realizes the preparation of the high-entropy alloy with higher strength and hardness. Provides practical guidance for improving the mechanical property of the high-entropy alloy. The replaced CoCrFeNiTa0.2Nb0.3 high-entropy alloy saves the use of Ta and has more excellent mechanical property, and provides an effective scheme for partial replacement for the application of Ta alloy in the aspects of aerospace, medical treatment and the like.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (3)
1. A preparation method of a high-strength HCP-phase high-entropy alloy is characterized in that the high-entropy alloy comprises high-entropy alloy powder consisting of elementary substance powder of Co, Cr, Fe, Ni, Ta and Nb, and the atomic percentage of the high-entropy alloy powder is 1: 1: 1: 1: 0.2: 0.3, the preparation method comprises the following steps:
s1, mixing the single-component powder in a vacuum glove box according to a certain proportion, putting the mixture and alumina grinding balls into a ball milling tank together, wherein the mass ratio of the powder balls is 1:3, and the high-energy ball mill runs in a mode of rotating forwards for 5 minutes, stopping for 5 minutes, then rotating backwards for 5 minutes and stopping for 5 minutes, and the running time is 12 hours in total;
s2, drying the uniformly mixed high-entropy alloy powder in a vacuum drying oven for 5 hours, and storing the dried powder in a closed container for later use;
s3, polishing and brightening the substrate used in plasma deposition by an angle grinder, and then cleaning the substrate by alcohol and acetone in sequence to remove oil stains on the surface;
s4, performing layer-by-layer deposition on the dried high-entropy alloy powder by adopting powder plasma arc additive manufacturing equipment, wherein the scanning speed of the powder plasma arc additive manufacturing equipment is 400mm/Min, the deposition current is 110A, the powder feeding rotating speed is 35r/Min, the ionic gas flow is 3L/Min, the protective gas flow is 9L/Min, the powder feeding gas flow is 4L/Min, the gas types are argon, and the high-entropy alloy is deposited and manufactured in a layer-by-layer accumulation mode;
and S5, depositing the high-entropy alloy deposition layers at intervals of not less than two minutes, and removing the oxide skin accumulation on the metal surface due to insufficient protective gas by using an angle grinder within the interval time after each deposition layer is deposited.
2. The method for preparing the HCP phase high-entropy alloy is characterized in that the purity of each of Co, Cr, Fe, Ni, Ta and Nb is more than 99.95% and the grain size is 150-300 meshes in the powder plasma arc additive manufacturing process.
3. A method of producing a high-entropy alloy with high-strength HCP phase according to claim 1, wherein steps S1 and S2 are performed in a vacuum environment to avoid oxidation of the high-entropy alloy powder before printing.
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CN110499445A (en) * | 2019-09-12 | 2019-11-26 | 北京理工大学 | A kind of eutectic high-entropy alloy and preparation method thereof |
CN111663070A (en) * | 2020-06-03 | 2020-09-15 | 上海理工大学 | AlCoCrFeNiSiY high-entropy alloy resistant to high-temperature oxidation and preparation method thereof |
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CN111663070A (en) * | 2020-06-03 | 2020-09-15 | 上海理工大学 | AlCoCrFeNiSiY high-entropy alloy resistant to high-temperature oxidation and preparation method thereof |
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"Factors determining solid solution phase formation and stability in CoCrFeNiX0.4 (X=Al, Nb, Ta) high entropy alloys fabricated by powder plasma arc additive manufacturing";Yupeng Zhang;《Journal of Alloys and Compounds》;20201016;第857卷;第2页、第3页表1、第5页左栏第2段 * |
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