CN112962036A - Preparation method of layered nano heterogeneous precipitation hardening high-entropy alloy - Google Patents
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Abstract
The invention provides a preparation method of a layered nanometer isomeric precipitation hardening high-entropy alloy, which comprises the following steps; preparing Cr, Co, Fe, N i and AI into a high-entropy alloy material according to a predetermined mass percentage, and then carrying out solid solution treatment at a predetermined solid solution high temperature; carrying out hot forging treatment on the high-entropy alloy material subjected to solution treatment at a preset hot forging temperature, immediately cooling to room temperature by water, and carrying out equal-channel corner extrusion of a single path; carrying out multi-pass rolling on the extruded high-entropy alloy material at a preset processing temperature, and then carrying out cooling treatment; then aging treatment is carried out to obtain a state that the microstructure is in a laminated coupling with a non-precipitation elongated grain layer sheet and a residual cold-work hardening layer sheet containing a high-density precipitated phase, and the microstructure is free of precipitation layer sheets and is in a non-continuous layered distribution characteristic along the processing direction. The preparation method realizes the preparation of the high-entropy alloy material by a mature industrialized thermal mechanical processing method, and can be popularized and applied to other precipitation hardening type high-entropy alloy systems.
Description
Technical Field
The invention relates to the field of metal treatment, in particular to a method for realizing layering by using conventional industrial thermo-mechanical treatment process and equipmentChemical composition design formula (CrCoFe) of nano heterogeneous precipitation hardening high-entropy alloyx(NiyAl)100-xAnd a method for designing and preparing a coupling microstructure of a non-uniform layer sheet and a cross-scale aging structure.
Background
When the ultrahigh strength plasticity of the metal structural material is realized, the method has important significance on service safety, long service life, energy conservation, emission reduction and the like, and how to simultaneously improve the strength and the plasticity of the material is always a major scientific problem in the field of structural materials. The multi-principal-element alloy, namely the high-entropy alloy, is a unique alloy system newly developed in recent years, the possibility of research and development of novel alloy materials is greatly enriched due to abundant component and structural changes, and meanwhile, a chance is provided for component design, microstructure regulation and control, high quality and high performance of the alloy structural materials.
In 2014, AlCoCrFeNi was designed and developed by professor Luping university of great courseware2.1The eutectic high-entropy alloy is internationally first reported to be formed from layered face-centered cubic L12A eutectic high-entropy structure formed by alternately arranging phases and body-centered cubic B2, and room-temperature and high-temperature mechanical properties. In 2017, the team designs and provides a process method for preparing the eutectic high-entropy alloy with the Ni atom ratio of 2.0-2.2 by a direct casting method, reports the influence of the nickel content on the eutectic high-entropy structure and the performance thereof, achieves the balance of high breaking strength and high toughness, and effectively solves the defect of poor castability of the high-entropy alloy.
In addition, the professor Lu-Ping cooperates with the professor Zhao Yonghao of Nanjing Ridgeon university, the traditional thermo-mechanical processing method is utilized to refine the eutectic lamellar structure, the excellent comprehensive mechanical properties of the tensile strength of 1351MPa and the elongation after fracture of 15.4 percent are obtained, and the strengthening and toughening mechanism of the eutectic high-entropy alloy is disclosed. Furthermore, a research team of cloud wave professor of Shanghai university clock utilizes an industrial smelting-rolling-heat treatment process to prepare the ultra-fine eutectic lamellar morph genetic structure high-entropy alloy for the first time, and in an eutectic high-entropy alloy system, excellent strength-plasticity matching is firstly realized, namely, the yield strength can reach-1.5 GPa, and meanwhile, the plasticity is kept at-16%, and accordingly, a multi-stage processing and hardening mechanism of a two-phase heterogeneous lamellar structure is provided.
In addition, Ni-rich and Al-rich ordered intermetallic compound precipitated phases with nanometer sizes, dispersion distribution and coherent precipitation are introduced. It has also been widely demonstrated that multi-element alloys can be more effectively strengthened while retaining sufficient tensile plasticity. For example, the university of Beijing technology Luzhao professor group introduces high-density and ultra-low mismatching degree Ni (Al, Fe) ordered nano precipitated phase into the martensitic steel, and develops novel high-performance maraging steel with the strength as high as 2.2GPa and the tensile plasticity of 8 percent. Similarly, the research team of Xuehuifei university of Beijing Physician introduces L1 into the single-phase high-entropy alloy with low-strength face-centered cubic structure2The nano precipitated phase can make the alloy strength as high as 1.9GPa, and simultaneously keep about 9% of tensile plasticity.
In conclusion, the fine microstructure of the Fe-Co-Cr-Ni-Al multi-principal-element eutectic alloy is adjusted, so that the toughening effect with super-strong high toughness is expected to be obtained. Meanwhile, the size of the ordered intermetallic compound precipitated phase is refined, so that the ordered intermetallic compound precipitated phase is converted into a nano-size dispersed granular precipitated phase from a relatively thick lamellar, and the toughness of the alloy system is further improved. However, in the reported eutectic alloy composition (AlCoCrFeNi)2.0～2.2) On the premise, the spheroidization and refinement of the layered intermetallic compound phase are difficult to realize by the conventional thermal mechanical processing method.
Disclosure of Invention
The invention aims to provide a chemical composition design formula (CrCoFe) for realizing the layered nano isomeric precipitation hardening high-entropy alloy by using a conventional industrial thermo-mechanical treatment process and equipmentx(NiyAl)100-xAnd a method for designing and preparing a coupling microstructure of a non-uniform layer sheet and a cross-scale aging structure.
Specifically, the invention provides a preparation method of a layered nano heterogeneous precipitation hardening high-entropy alloy, which comprises the following steps;
100, preparing Cr, Co, Fe, Ni and AI into a high-entropy alloy material according to a predetermined mass percentage, and then carrying out solid solution treatment at a predetermined solid solution high temperature to ensure that the average grain size of the high-entropy alloy material is about 20-80 mu m and the microstructure is uniform equiaxial coarse crystals;
400, obtaining a high-entropy alloy material with the macroscopic discontinuous layered microscopic characteristics, wherein the microstructure is partially layered and dynamically recovered, the volume fraction of the high-entropy alloy material is 40% -45%, and the average width and the spacing of the layered recovered state grain structure are several micrometers;
The chemical components of the novel hypoeutectic high-entropy alloy limited by the invention form a novel age-hardenable lamellar heterogeneous high-entropy structure after two processes of thermomechanical deformation and subsequent aging treatment, obtain a micro-structure form with no precipitation-return micro-layer (actually, high-return elongated grains) and a residual cold-work hardened layer containing a high-density precipitation phase, which are alternately arranged, and realize the coupling construction of a lamellar heterogeneous matrix and a cross-scale aging structure. By utilizing heterogeneous deformation induced hardening and precipitation hardening effects, the comprehensive performance matching of the tensile strength of more than 1.6-2.0 GPa and the elongation after fracture of 5-10% is realized. The preparation of the high-entropy alloy material is realized only by a mature industrialized thermal mechanical processing method in the whole treatment process, so that the method is extremely easy to popularize and apply to other precipitation hardening type high-entropy alloy systems.
Drawings
FIG. 1 is a schematic flow diagram of a method of making one embodiment of the present invention;
FIG. 2 is a schematic diagram of the processing temperature-time sequence relationship during the execution of the manufacturing method;
FIG. 3 is a photograph of a microstructure of a coupled cross-scale aged structure of a layered nano-heterogeneous matrix in an embodiment of the present invention, wherein a, b are layered nano-heterogeneous matrices, white/dark bands are highly recovered layered grains, and black bands are aged residual cold-hardened layered matrices; c, d is a cold-work hardening matrix layer precipitated at high density and a highly recovered lamellar crystal grain layer without precipitation, and the white and bright particles are a precipitation phase;
FIG. 4 shows the layered nano-isomeric precipitation hardening (PHL (CrCoFe))x(NiyAl)100-x) Schematic drawing of tensile engineering stress-strain curve of the high-entropy alloy. Wherein, the contrast dotted line is eutectic high-entropy alloy (EHEA AlCoCrFeNi)2.1) And (4) stretching the curve.
Detailed Description
The detailed structure and implementation process of the present solution are described in detail below with reference to specific embodiments and the accompanying drawings.
As shown in FIG. 1, in one embodiment of the present invention, a method for preparing a layered nano-isomeric precipitation-hardened high-entropy alloy is disclosed, comprising the steps of;
100, preparing Cr, Co, Fe, Ni and AI into a high-entropy alloy material according to a predetermined mass percentage, and then carrying out solid solution treatment at a predetermined solid solution high temperature to ensure that the average grain size of the high-entropy alloy material is about 20-80 mu m and the microstructure is uniform equiaxial coarse crystals;
the chemical compositions of the hypoeutectic high-entropy alloy consisting of Cr, Co, Fe, Ni and AI are shown in Table 1.
TABLE 1 (C)rCoFe)x(NiyAl)100-xChemical composition design table of high-entropy alloy material
The chemical components of the secondary hardening high-entropy alloy are designed as shown in the following formula:
α(Cr)＝α(Co)＝α(Fe)＝x/3， (1)
α(NiyAl)＝100-x， (2)
α(Ni):α(Al)＝y， (3)
wherein, alpha represents the atomic content of chemical elements, and x is the atomic percentage of the chemical elements; the chemical composition design can be characterized by the following characteristics: (1) the non-traditional single component alloy system contains 5 main elements of Cr, Co, Fe, Ni, Al and the like; (2) the contents of the alloy elements Cr, Co and Ni are the same and are all x/3, and the contents of the other elements Ni and Al are 100-x; (3) meanwhile, the atomic ratio of Ni to Al element is y.
In order to realize spheroidization transformation of the high-entropy alloy material in the subsequent aging process and ensure that a large amount of precipitated phases are separated out to obtain a considerable hardening effect, the control conditions of the chemical components meet the following formulas (5) and (6):
50％≤x≤70％， (5)
namely, the sum of the atomic percentages of the three elements of Cr, Co and Fe is between 50% and 70%.
And simultaneously satisfies:
2.0≤y(Ni/Al)≤3.25， (6)
that is, the atomic ratio of the alloying elements Ni/Al is between 2.0 and 3.25.
Predetermined temperature T in this step01100 ℃ -1250 ℃), predetermined holding time t0＝6h～24h。
here predetermined hot forging temperature TF＝1150℃～900℃。
predetermined processing temperature TR550 ℃ to 700 ℃. The predetermined Missels equivalent strain is 0.4-0.6, which is equivalent to the rolling reduction of about 50-90% during multi-pass high-temperature rolling. 5. In the multi-pass rolling process, the heat preservation time of the high-entropy alloy material before each rolling is 4-6 min, and the rolling deformation forming time is 3-10 min.
The high-entropy alloy material after multi-pass rolling can be required to be processed and cleaned: firstly, carrying out mechanical grinding processing on the outer surface of the high-entropy alloy material to obtain better surface quality; and then 5% hydrochloric acid alcohol solution is used for carrying out decontamination treatment on the surface of the high-entropy alloy material, and finally, absolute ethyl alcohol is used for cleaning.
The cooling treatment directly quenches the high-entropy alloy material into liquid nitrogen for cooling.
400, obtaining a high-entropy alloy material with the macroscopic discontinuous layered microscopic characteristics, wherein the microstructure is partially layered and dynamically recovered, the volume fraction of the high-entropy alloy material is 40% -45%, and the average width and the spacing of the layered recovered state grain structure are several micrometers;
Wherein the predetermined holding temperature TAAt 600-800 deg.c for heat preservation time tAIs 4 to 150 hours.
In the above steps, the relationship between temperature and time in the above processing steps is shown in fig. 2. The microscopic photograph of the high-entropy alloy material is shown in fig. 3.
The aging structure of the high-entropy alloy is characterized in that: forming a recovery layer without precipitation and a cold hardening layer with high density precipitation which are alternately arranged; the average particle size distribution of the formed precipitation phase presents a plurality of peaks from nanometer to submicron scale.
The heterogeneous distribution of the precipitated phase is characterized by: only precipitates in the residual cold-work hardening matrix and is in a granular shape with uneven size, little or no precipitates are precipitated in the highly recovered lamellar crystal grains, and finally the microstructure characteristic that lamellar non-precipitated crystal grain strips and high-density precipitated cold-work hardening strips are alternately arranged is formed.
The aging structure of the high-entropy alloy is characterized in that: the size distribution of the precipitated phase spans the range from nano-scale to micron-scale, a recovery layer without precipitation and a cold hardening layer with high-density precipitation are alternately arranged, and the average particle size distribution of the precipitated phase presents a plurality of peak values from nano-scale to submicron-scale.
The chemical components of the novel hypoeutectic high-entropy alloy limited by the embodiment are subjected to thermomechanical deformation and subsequent aging treatment to form a novel aging-hardenable lamellar heterogeneous high-entropy structure, a precipitation-free recovered micro layer (actually, highly recovered lamellar crystal grains) and a residual cold-work hardened layer containing a high-density precipitation phase are obtained, and the microstructure forms are alternately arranged, so that the coupling construction of a lamellar heterogeneous matrix and a cross-scale aging structure is realized. By utilizing heterogeneous deformation induced hardening and precipitation hardening effects, the comprehensive performance matching of the tensile strength of more than 1.6-2.0 GPa and the elongation after fracture of 5-10% is realized. The preparation of the high-entropy alloy material is realized only by a mature industrialized thermal mechanical processing method in the whole treatment process, so that the method is extremely easy to popularize and apply to other precipitation hardening type high-entropy alloy systems.
The processing of the method is described below with specific examples.
In order (CrCoFe)x(NiyAl)100-xThe high-entropy alloy is taken as an example, and the chemical composition of the high-entropy alloy is characterized in that x is 50, and y is 2. For the high-entropy alloy CrCoFeNi with the composition3.3Al performs the following operations:
1. pre-treating the high-entropy alloy material at a predetermined temperature T0At 1100 deg.C, for a predetermined holding time t0Solution treatment is carried out for 6h, so that the average grain size of the high-entropy alloy material is about 20 mu m, and the microstructure is uniform isometric coarse crystals;
2. at TFCarrying out hot forging treatment with the forging ratio of 8 on the homogenized high-entropy alloy material at 950 ℃, and then immediately cooling to room temperature;
3. at room temperature, carrying out single B treatment on the homogenized high-entropy alloy materialAEqual channel corner extrusion processing treatment of a path and a preset Misses equivalent strain of-2;
4. carrying out mechanical grinding processing on the outer surface of the high-entropy alloy material to obtain better surface quality, and simultaneously processing the outer surface to a preset section size of 20mm multiplied by 20 mm;
5. and then carrying out decontamination treatment: firstly, carrying out decontamination treatment on the surface of the high-entropy alloy material by using a 5% hydrochloric acid alcohol solution, and then cleaning by using absolute ethyl alcohol;
6. at a predetermined temperature TRCarrying out rolling treatment on the extruded high-entropy alloy material for 20-pass with a preset Missels equivalent strain of 0.4 at the temperature of 550 ℃, namely rolling reduction of about 50%, wherein the holding time before rolling is usually 5min, and the rolling deformation forming time is 3-10 min;
7. and finally, cooling the high-entropy alloy material at a preset cooling speed v of about 500-1000 ℃/min to obtain the high-entropy alloy material containing a large amount of lamellar crystal grain structures with the volume fraction of about 40%. The average width and the spacing of the lamellar grain structure are both 5-13 mu m.
8. At a predetermined temperature TAAt 800 deg.C, for passing through a heat engineAnd (4) carrying out aging heat treatment on the machined high-entropy alloy material for 8h to obtain a coupling microstructure of the non-uniform laminated substrate and the cross-scale aging structure.
Wherein, the size distribution of the precipitation phase is in the interval of 7 nm-8 μm, the average particle size distribution of the precipitation phase presents a multimodal distribution characteristic, the average particle size distribution peak of the precipitation phase with smaller size is 20nm, and the average particle size distribution peak of the precipitation phase with larger size is 4.5 μm.
As shown in FIG. 4, the room temperature quasi-static tensile test result shows that the layered nano isomeric precipitation hardening high-entropy alloy CrCoFeNi3.3Al has 1.6GPa tensile strength and 7 percent elongation after fracture, and the tensile property is obviously superior to that of eutectic AlCoCrFeNi2.0～2.2High entropy alloy.
Thus, it should be appreciated by those skilled in the art that while a number of exemplary embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications consistent with the principles of the invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (10)
1. A preparation method of a layered nanometer isomeric precipitation hardening high-entropy alloy is characterized by comprising the following steps;
100, preparing Cr, Co, Fe, Ni and AI into a high-entropy alloy material according to a predetermined mass percentage, and then carrying out solid solution treatment at a predetermined solid solution high temperature to ensure that the average grain size of the high-entropy alloy material is about 20-80 mu m and the microstructure is uniform equiaxial coarse crystals;
step 200, performing hot forging treatment with a forging ratio of 4-12 on the high-entropy alloy material subjected to solution treatment at a preset hot forging temperature, immediately cooling the high-entropy alloy material to room temperature by water, performing equal-channel angular extrusion on the high-entropy alloy material in a single path, processing the high-entropy alloy material to a preset Missels equivalent strain of 2-6 to form a layered cold-work hardening matrix structure, and introducing sufficient deformation energy storage for subsequent aging;
step 300, performing multi-pass rolling with the preset Missels equivalent strain of 0.4-0.6 on the extruded high-entropy alloy material at a preset processing temperature, and then performing cooling treatment with the preset cooling speed of 500-1000 ℃/min on the high-entropy alloy material to form dynamic recovery grain layers which are distributed at intervals and have high recovery rate;
400, obtaining a high-entropy alloy material with the macroscopic discontinuous layered microscopic characteristics, wherein the microstructure is partially layered and dynamically recovered, the volume fraction of the high-entropy alloy material is 40% -45%, and the average width and the spacing of the layered recovered state grain structure are several micrometers;
step 500, carrying out aging treatment on the high-entropy alloy material at a preset heat preservation temperature and for a preset heat preservation time to form a non-uniformly distributed precipitation phase in a macroscopic discontinuous layered matrix in the high-entropy alloy material, and finally obtaining a microstructure form in which a microstructure in the high-entropy alloy material is a precipitation-free high-recovery-state grain layer sheet and is laminated and coupled with a residual cold-work hardening layer sheet containing a high-density precipitation phase, wherein the microstructure form is characterized in that no precipitation layer sheet exists macroscopically and is in discontinuous layered distribution along the processing direction.
2. The production method according to claim 1,
in the step 100, α represents the atomic content of the chemical element, and x is the atomic percentage of the chemical element, which includes:
α(Cr)＝α(Co)＝α(Fe)＝x/3
α(NiyAl)＝100-x
α(Ni):α(Al)＝y
wherein, the contents of the alloy elements Cr, Co and Ni are the same and are all x/3, and the contents of the other elements Ni and Al are 100-x; and the atomic ratio of Ni to Al element is y.
3. The production method according to claim 2,
in order to realize spheroidization transformation of the high-entropy alloy material in the subsequent aging process, ensure that a large amount of precipitate phase is separated out and obtain considerable hardening effect, wherein the sum of the atomic percentage contents of the three elements of Cr, Co and Fe is between 50 and 70 percent; that is, x satisfies:
50％≤x≤70％
and simultaneously satisfies:
2.0≤y(Ni/Al)≤3.25
that is, the atomic ratio of the alloying elements Ni/Al is between 2.0 and 3.25.
4. The production method according to claim 1,
the predetermined solid solution high temperature T01100-1250 ℃; the predetermined hot forging temperature TF1150 ℃ to 900 ℃; the predetermined processing temperature TRIs 550-700 ℃.
5. The production method according to claim 1,
in the step 200, the surface of the extruded high-entropy alloy material is ground, the section size is processed to a preset size, then 5% hydrochloric acid alcohol solution is used for decontamination treatment of the surface, finally, absolute ethyl alcohol is used for cleaning, and then the subsequent rolling process is carried out.
6. The production method according to claim 1,
in the multi-pass rolling process of the step 300, the heat preservation time of the high-entropy alloy material before each rolling is 4-6 min, and the rolling deformation forming time is 3-10 min.
7. The production method according to claim 1,
in the step 300, the cooling treatment is to directly quench the high-entropy alloy material into liquid nitrogen for cooling.
8. The production method according to claim 1,
in step 500, the non-uniform distribution of the precipitation phase is characterized by: only precipitates in the residual cold-work hardening matrix and is in a granular shape with uneven size, little or no precipitates are precipitated in the highly recovered lamellar crystal grains, and finally the microstructure characteristic that lamellar non-precipitated crystal grain strips and high-density precipitated cold-work hardening strips are alternately arranged is formed.
9. The method according to claim 8,
the size distribution of the precipitated phase spans the scale range of several nanometers to several micrometers, and the average particle size distribution of the precipitated phase is characterized by multimodal distribution.
10. The production method according to claim 1,
in the step 500, the temperature T is presetAAt 600-800 deg.c for heat preservation time tAIs 4 to 150 hours.
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| CN104694808A (en) * | 2015-03-26 | 2015-06-10 | 北京科技大学 | High-entropy alloy with dispersion nano-sized precipitate strengthening effect and preparing method thereof |
| KR20190068916A (en) * | 2017-12-11 | 2019-06-19 | 한국기계연구원 | High entropy alloy and method for manufacturing the same |
| CN111826573A (en) * | 2020-06-29 | 2020-10-27 | 华中科技大学 | Precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and preparation method thereof |
| US20200392613A1 (en) * | 2017-12-11 | 2020-12-17 | Korea Institute Of Machinery & Materials | High-entropy alloy, and method for producing the same |
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| CN104694808A (en) * | 2015-03-26 | 2015-06-10 | 北京科技大学 | High-entropy alloy with dispersion nano-sized precipitate strengthening effect and preparing method thereof |
| KR20190068916A (en) * | 2017-12-11 | 2019-06-19 | 한국기계연구원 | High entropy alloy and method for manufacturing the same |
| US20200392613A1 (en) * | 2017-12-11 | 2020-12-17 | Korea Institute Of Machinery & Materials | High-entropy alloy, and method for producing the same |
| CN111826573A (en) * | 2020-06-29 | 2020-10-27 | 华中科技大学 | Precipitation strengthening type high-entropy alloy without sigma phase precipitation tendency and preparation method thereof |
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