CN116426783A - Preparation method for improving density of AlxCoCrFeNi series high-entropy alloy - Google Patents
Preparation method for improving density of AlxCoCrFeNi series high-entropy alloy Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention belongs to the technical field of metal materials, and particularly relates to a preparation method for improving the density of an AlxCoCrFeNi series high-entropy alloy, the obtained alloy and application thereof. Firstly, preparing high-purity metal simple substance powder by using an aerosol laminar atomization technology; preparing mixed metal powder by a mechanical alloying method; sintering the mixed metal powder into a block alloy sample by a plasma sintering technology; and finally, carrying out pressing treatment on the sintered and cooled alloy sample by using hot isostatic pressing. The alloy prepared by the invention has uniform and compact microstructure, fine grains and mechanical property superior to that of the AlxCoCrFeNi series high-entropy alloy prepared in an as-cast state, and has wide industrial application value.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a preparation method for improving the density of an AlxCoCrFeNi series high-entropy alloy, the obtained alloy and application thereof.
Background
The high-entropy alloy breaks through the fact that the traditional metal material is composed of several main elements, and the related performance of the alloy is improved by adding other trace elements. The high-entropy alloy is generally composed of five or more elements in equimolar ratio or nearly equimolar ratio, and the ratio of each element is 5% -35%; the high-entropy alloy has special four major effects: thermodynamically high entropy effects, kinetically delayed diffusion effects, structural lattice distortion effects, and performance "cocktail effects", deriving thermodynamically high entropy effects from gibbs' law makes alloys more prone to form simple FCC, BCC, HCP etc. stable and single phases, kinetically delayed diffusion effects mean that the rate of atomic diffusion in a high entropy alloy is less than that in an alloy, so that the rate of atomic diffusion is slowed down, resulting in some improvements in relevant properties; structural lattice distortion refers to the lack of solute and solvent distinction in high entropy alloys, such that atoms with larger radii occupy the junction creating structural distortion that can shift the phase composition of certain high entropy alloys from FCC to BCC structure; the cocktail effect mainly refers to the property that different elements in the high-entropy alloy are mixed together to generate a single element, and the unique four effects lead to the high-entropy alloy having good mechanical property, wear resistance, corrosion resistance, high-temperature oxidation resistance, high-temperature radiation resistance and the like, and are generally superior to the traditional metal materials. According to the existing research, the element types of the high-entropy alloy can be increased, the element content variation can be controlled to be larger, and the composition and the performance of the high-entropy alloy can be predicted by utilizing the first performance principle, thermodynamics, dynamics, machine learning and other modes. In a high-entropy alloy system, the content variability of the variable element is strong, so that the high-entropy alloy is a novel metal structure material with huge development potential, has large development space and strong designability, and becomes one of hot spots in the field of metal material research in recent years.
The high-entropy alloy is conventionally prepared by vacuum arc melting and vacuum induction melting technology, defects such as defects, segregation and air holes are inevitably generated in the melting process, and the existence of the defects affects the properties of the alloy to a certain extent, such as mechanical properties, corrosion resistance, wear resistance, high-temperature irradiation resistance and the like.
Disclosure of Invention
In order to solve the defects in the prior art and reduce the defects existing in the conventional casting method, the invention provides a preparation method for improving the density of an AlxCoCrFeNi series high-entropy alloy, the obtained alloy and application thereof. Based on the technical scheme, the density of the high-entropy alloy can be effectively improved.
The technical scheme provided by the invention is as follows:
a preparation method for improving the compactness of AlxCoCrFeNi series high-entropy alloy comprises the following steps:
1) Firstly, preparing high-purity metal simple substance powder raw materials by using an aerosol laminar atomization technology;
2) Then preparing mixed metal powder by a mechanical alloying method;
3) Sintering the mixed metal powder into a block alloy sample by a plasma sintering technology;
4) And finally, performing pressing treatment on the sintered and cooled alloy sample by using hot isostatic pressing to obtain the high-entropy alloy of the AlxCoCrFeNi system with high density.
The technical scheme is as follows:
firstly, adopting an airflow layering technology in an atomization method to prepare metal simple substance powder, ensuring the purity of the metal simple substance, preparing the metal simple substance powder into uniformly mixed metal powder in a ball mill by utilizing mechanical alloying, improving the utilization rate of the metal simple substance powder, thereby reducing unnecessary loss, and ensuring that the mixed metal powder has pores and tiny defects on a microscopic structure to a certain extent relative to massive alloy; the compactness of the sample is improved by adopting the spark plasma sintering technology to prepare the sample, the microstructure and structure are improved, and shrinkage cavities and defects are reduced; finally, the sample of the prepared high-entropy alloy is further pressed by adopting the hot isostatic pressing technology, so that internal holes and microstructures of the uniform alloy are eliminated, the compactness of the high-entropy alloy is enhanced to a greater extent, and the microstructure structure is improved, so that the performance of the alloy is improved;
meanwhile, the formation of intermetallic compounds is inhibited due to the unique high entropy effect of the high entropy alloy, the Gibbs free energy is lower, the system is more stable, the slow diffusion effect on dynamics leads to the slow diffusion rate of atoms in the high entropy alloy system, and the lattice distortion effect and the cocktail effect bring structural change and performance improvement to a certain extent. Therefore, pure metal powder is prepared by adopting an atomization method, and after mixed high-entropy alloy powder is prepared by adopting mechanical alloying, the density is improved by adopting plasma sintering and hot isostatic pressing technologies.
Specifically, the AlxCoCrFeNi high-entropy alloy satisfies the condition Al:1.10 to 19.30at percent, co:21.09 to 25.91at%, cr:18.60 to 22.90at percent, fe:19.90 to 24.50at percent, ni:21.00 to 25.80at%; and satisfies the following: (1) Al: the atomic ratio of (CoCrFeNi) is x, wherein x is 4,0< x is less than or equal to 2; (2) the sum of the atomic percentages of the elements is 100.
Specifically, in the step 1), metal simple substance powder of Al, co, cr, fe and Ni is prepared by an aerosol laminar atomization technology, and the purity of the metal simple substance powder reaches 99.9% or more; the atomization gas adopts high-purity argon, and the pressure of the adopted atomization gas is 2-5 MPa; the initial temperature of the metal simple substance powder is 400 ℃, the superheat degree is 20-50 ℃, the final temperature is not higher than the melting point temperature of the metal simple substance, and the inner diameter of the guide pipe is 2-4 mm.
The laminar flow atomization technology is adopted to prepare the metal powder, the atomization gas is high-purity argon, and the purity of the argon reaches 99.9% or more. The flow speed of the argon is firstly fast and then slow, so that other gases in the equipment are completely removed; the flow rate of argon is 3000ml/min before 70% of argon is introduced, the flow rate of the subsequent argon is 2000ml/min, and the purity of the argon reaches more than 99.9%.
Specifically, in the step 2), the metal powder which is uniformly mixed is prepared by a mechanical alloying method, and the shape of the prepared high-entropy alloy metal simple substance powder tends to be a circular shape or a circular shape; the mechanical alloying ball milling medium is WC, the powder granularity is 20-60 mu m, the ball-material ratio is (5-12): 1, and the materials are mixed for 20-35 h under the protection of high-purity argon at the speed of 300-600 r/min; and adding an ethanol solution with the purity of more than 99.8 percent after the ball milling time is finished, and taking the ethanol solution as a process control agent to prevent cold welding among mixed metal powders from generating other intermetallic compounds.
Specifically, in the step 3), the metal powder which is evenly mixed after mechanical alloying is put into
The graphite mould, the mould and the metal powder are placed in an SPS discharge plasma sintering furnace for sintering; the parameters of the vacuum sintering furnace are respectively as follows: sintering vacuum degree is lower than 5 multiplied by 10 -3 Pa, sintering temperature 720-1120 ℃, heating rate 30-60 ℃/min, applied pressure 30-40 MPa, and heat preservation time 4-10 min.
Specifically, in the step 4), cooling the vacuum sintered sample to room temperature, filling the sample into a die, and performing pressing treatment on the sintered sample by using hot isostatic pressing; the heating speed is 5-10 ℃/min, the hot isostatic pressing temperature is 400-500 ℃, the time is 3-5 h, and the applied pressure is 200-300 MPa.
And after the hot isostatic pressing is finished, unloading the pressure of the hot isostatic pressing, and cooling to the room temperature at a speed of 2-5K/s to finally obtain the hot isostatic pressing massive sample.
Cleaning the block-shaped ingot alloy after hot isostatic pressing cooling, and then drying; firstly, ultrasonic cleaning is carried out by adopting a propanol solution, and then the ultrasonic cleaning is carried out by using an ethanol solution with the concentration of 75 percent; the drying temperature is 30-100 ℃.
The invention also provides the AlxCoCrFeNi series high-entropy alloy prepared by the method and application thereof. The AlxCoCrFeNi high-entropy alloy provided by the invention has high compactness and mechanical property, and can be used as a welding base metal or a welding wire to connect dissimilar materials, such as a metal material and a metal material, and a metal material and a non-metal material.
The main elements of the invention are selected as follows:
al: the Al element is a typical main element capable of forming high-entropy alloy, and the addition of Al can enhance the strength of the alloy and reduce the density of the alloy; al is a common alloying element and is easily oxidized to form an oxide film, but the atomic size of Al is larger than the size of Co, cr, fe, ni elements in quaternary alloy CoCrFeNi, the mixing enthalpy is negative, the addition of the Al is easy to cause lattice distortion on a microstructure, the transformation of an alloy phase structure is promoted, and the transformation of a high-entropy alloy from FCC to FCC+BCC to a BCC structure is promoted;
co: the Co element is a classical main element which is easy to form high-entropy alloy, is generally uniformly distributed in an alloy structure in the high-entropy alloy, and can be mutually dissolved with other elements;
cr: cr element is a typical main element which is easy to form high-entropy alloy, improves the strength and hardness of the alloy, has little influence on the plasticity and toughness of the alloy, and improves the overall mechanical properties of the alloy. Cr element and Fe element are infinitely miscible, can inhibit the formation of brittle intermetallic compounds, and can be mutually miscible with other elements, and the formation of BCC phase is promoted;
fe: the Fe element is a principal element, is a classical principal element which is easy to form high-entropy alloy, and can be mutually dissolved with other elements;
ni: the element is a principal element, is a classical principal element which is easy to form high-entropy alloy, tends to promote the formation of FCC phase, and Ni element and Fe element are infinitely miscible, so that the formation of brittle intermetallic compounds can be inhibited, and the element can be mutually dissolved with other elements.
Compared with the prior art, the invention improves the density of the prepared alloy and has the following advantages:
1. on one hand, high-purity powder is prepared by adopting a laminar flow atomization technology in an atomization method, and the density and the utilization rate of the high-entropy alloy are improved by preparing high-entropy alloy mixed powder by using mechanical alloying of the high-purity powder;
2. on the other hand, the vacuum plasma sintering technology is utilized to prepare a blocky high-entropy alloy block, so that the microstructure of the high-entropy alloy is improved, and meanwhile, the purity of a high-entropy alloy sample is also improved;
3. finally, the hot isostatic pressing technology is adopted to press the sintered and cooled high-entropy alloy sample, so that casting defects are reduced to the greatest extent, and uniformity and compactness of microstructure are improved.
The preparation method for improving the density of the AlxCoCrFeNi series high-entropy alloy can improve the microstructure of the AlxCoCrFeNi series high-entropy alloy and improve the density of an alloy system. The method for improving the compactness, improving the microstructure and improving the mechanical property can expand the application of the AlxCoCrFeNi series high-entropy alloy.
Drawings
FIG. 1 is an XRD analysis chart of an AlxCoCrFeNi-based high-entropy alloy prepared in example 1.
FIG. 2 is an SEM microstructure of the AlxCoCrFeNi-based high-entropy alloy prepared in example 1.
Detailed Description
The principles and features of the present invention are described below with examples only to illustrate the present invention and not to limit the scope of the present invention.
The purity of the raw materials used in the embodiment of the invention is as follows: fe. Al, ni, co, cr, nb purity is more than or equal to 99.9 percent.
Table 1 below shows comparative chemical compositions of examples of the present invention;
table 2 below shows the aerosol method parameter values according to the embodiment of the present invention;
table 3 below is a table of values of mechanical alloying parameters according to an embodiment of the present invention;
the following table 4 is a table of plasma sintering parameter values according to an embodiment of the present invention;
table 5 below is a table of values of parameters of hot isostatic pressing according to an embodiment of the present invention;
table 6 below shows the results of the main mechanical property test in the examples of the present invention.
The corresponding AlxCoCrFeNi high-entropy alloy in the invention meets the condition that: 1.10 to 19.30at percent, co:21.09 to 25.91at%, cr:18.60 to 22.90at percent, fe:19.90 to 24.50at percent, ni:21.00 to 25.80at%; and satisfies the following: (1) Al: the atomic ratio of (CoCrFeNi) is x, wherein x is 4,0< x is less than or equal to 2; (2) The sum of the atomic percentages of the elements is 100
The preparation steps of the embodiment of the invention are as follows:
firstly preparing high-purity metal simple substance powder by an aerosol laminar flow atomization technology,
the mixed metal powder is prepared by a mechanical alloying method,
sintering the mixed metal powder into a block alloy sample by a plasma sintering technology;
and finally, performing pressing treatment on the alloy sample by double hot pressing.
The parameters corresponding to each process are shown in tables 1 to 5 below:
TABLE 1 comparative chemical composition Table (wt.%)
| Element(s) | Al | Fe | Co | Ni | Cr |
| Example 1 | 1.2 | 24.5 | 25.8 | 25.7 | 22.8 |
| Example 2 | 3.5 | 23.9 | 25.2 | 25.1 | 22.3 |
| Example 3 | 6.7 | 23.1 | 24.4 | 24.3 | 21.5 |
TABLE 2 Aerosol method parameter values table of AlxCoCrFeNi series embodiment of the invention
| Examples | Example 1 | Example 2 | Example 3 |
| Atomization pressure/MPa | 3 | 4 | 5 |
| Degree of superheat/. Degree.C | 25 | 36 | 48 |
TABLE 3 mechanical alloying parameter values table for AlxCoCrFeNi series embodiments of the invention
| Examples | Example 1 | Example 2 | Example 3 |
| Powder particle size/. Mu.m | 30 | 40 | 50 |
| Rotational speed/r/min | 400 | 450 | 500 |
| Ball-to-material ratio | 6:1 | 8:1 | 10:1 |
| Mixing time/h | 12 | 18 | 22 |
TABLE 4 plasma sintering parameter values table for AlxCoCrFeNi series embodiments of the invention
| Examples | Example 1 | Example 2 | Example 3 |
| Sintering temperature/DEGC | 750 | 850 | 900 |
| Temperature rise rate/. Degree.C/ |
40 | 45 | 50 |
| Applied pressure/MPa | 30 | 35 | 38 |
| Incubation time/min | 5 | 6 | 8 |
TABLE 5 Dual HIP parameter values table for AlxCoCrFeNi series embodiments of the present invention
TABLE 6 comparative chemical composition Table of AlxCoCrFeNi series examples of the invention
| Examples | Example 1 | Example 2 | Example 3 |
| Yield strength/MPa | 142 | 450 | 500 |
| Tensile strength/MPa | 180 | 620 | 800 |
| Elastic modulus/GPa | 50 | 60 | 80 |
According to the table, the mechanical property of the high-entropy alloy system is improved along with the change of the content of the aluminum element; meanwhile, preparing high-purity powder, and uniformly mixing the high-purity powder by adopting a mechanical alloying method; sintering the powder into a block sample by adopting a discharge plasma method, and finally obtaining the high-entropy alloy system with high density and excellent mechanical property by adopting a hot isostatic pressing technology.
As can be seen from fig. 1, the phase structure of the AlxCoCrFeNi-based high-entropy alloy obtained after hot isostatic pressing is a single FCC structure, which proves the feasibility of the method, and the phase structure of the sample of example 1 in the as-cast condition is also a single FCC structure.
As can be seen from fig. 2, the microstructure of the AlxCoCrFeNi-based high-entropy alloy obtained after hot isostatic pressing is complete and fine precipitates are formed, which demonstrates the improvement of the microstructure and the improvement of the densification.
The AlxCoCrFeNi high-entropy alloy obtained by the method of examples 1 to 3 is compared with a sample obtained by directly carrying out hot isostatic pressing on the simple substance powder without adopting mechanical alloying and plasma sintering technology, so that the microstructure is improved, the microstructure of a precipitate is smaller, the yield strength is improved, and the comprehensive mechanical property is excellent.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The preparation method for improving the compactness of the AlxCoCrFeNi high-entropy alloy is characterized by comprising the following steps of:
1) Firstly, obtaining a high-purity powder raw material of a metal simple substance;
2) Then preparing mixed metal powder by a mechanical alloying method;
3) Sintering the mixed metal powder into a block alloy sample by a plasma sintering technology;
4) And finally, performing pressing treatment on the sintered and cooled alloy sample by using hot isostatic pressing to obtain the high-entropy alloy of the AlxCoCrFeNi system with high density.
2. The method for improving the compactness of the AlxCoCrFeNi-based high-entropy alloy according to claim 1, which is characterized in that: the AlxCoCrFeNi system high entropy combination meets the condition of Al:1.10 to 19.30at percent, co:21.09 to 25.91at%, cr:18.60 to 22.90at percent, fe:19.90 to 24.50at percent, ni:21.00 to 25.80at%; and satisfies the following: (1) Al: the atomic ratio of (CoCrFeNi) is x, wherein x is 4,0< x is less than or equal to 2; (2) the sum of the atomic percentages of the elements is 100.
3. The method for improving the density of an AlxCoCrFeNi-based high-entropy alloy according to claim 1, wherein in step 1):
adopting an aerosol laminar flow atomization technology to prepare Al, co, cr, fe, ni metal simple substance powder, wherein the purity of the metal simple substance powder is more than 99.9%; the atomization gas adopts high-purity argon, and the pressure is 2-5 MPa; the initial temperature of the metal simple substance powder is 400 ℃, the superheat degree is 20-50 ℃, the final temperature is not higher than the melting point temperature of the metal simple substance, and the inner diameter of the guide pipe is 2-4 mm;
the flow rate of argon is 3000ml/min before 70% of argon is introduced, and the flow rate of the subsequent argon is 2000ml/min;
the purity of the argon reaches more than 99.9 percent.
4. The method for improving the density of an AlxCoCrFeNi-based high-entropy alloy according to claim 1, wherein in step 2):
preparing metal powder which is uniformly mixed by a mechanical alloying method, wherein the shape of the prepared high-entropy alloy metal simple substance powder tends to be round or round; the mechanical alloying ball milling medium is WC, the powder granularity is 20-60 mu m, the ball-material ratio is (5-12): 1, and the materials are mixed for 20-35 h under the protection of high-purity argon at the speed of 300-600 r/min; adding ethanol solution with purity of more than 99.8% after the ball milling time is over as a process control agent for preventing cold welding between mixed metal powders from generating other intermetallic compounds;
the purity of the argon reaches more than 99.9 percent.
5. The method for improving the density of an AlxCoCrFeNi-based high-entropy alloy according to claim 1, wherein in step 3): placing the mixed metal powder obtained by mechanical alloyingPutting the graphite mould into a graphite mould, and then placing the mould and metal powder into an SPS discharge plasma sintering furnace for sintering; the parameters of the vacuum sintering furnace are respectively as follows: sintering vacuum degree is lower than 5 multiplied by 10 - 3 Pa, sintering temperature 720-1120 ℃, heating rate 30-60 ℃/min, applied pressure 30-40 MPa, and heat preservation time 4-10 min.
6. The method for producing an AlxCoCrFeNi-based high-entropy alloy according to claim 1, wherein, in step 4),
cooling the vacuum sintered sample to room temperature, filling the sample into a die, and performing pressing treatment on the sintered sample by using hot isostatic pressing; the heating speed is 5-10 ℃/min, the hot isostatic pressing temperature is 400-500 ℃, the time is 3-5 h, and the applied pressure is 200-300 MPa;
and after the hot isostatic pressing is finished, unloading the pressure of the hot isostatic pressing, and cooling to the room temperature at a speed of 2-5K/s to finally obtain the hot isostatic pressing massive sample.
7. The method for improving the compactness of the AlxCoCrFeNi-based high-entropy alloy according to claim 1, which is characterized in that: cleaning the block-shaped ingot alloy after hot isostatic pressing cooling, and then drying; firstly, ultrasonic cleaning is carried out by adopting a propanol solution, and then the ultrasonic cleaning is carried out by using an ethanol solution with the concentration of 75 percent; the drying temperature is 30-100 ℃.
8. A high-density AlxCoCrFeNi-based high-entropy alloy produced by the production method according to any one of claims 1 to 7.
9. Use of a high-density AlxCoCrFeNi-based high-entropy alloy according to claim 8, characterized in that: can be used as a welding parent metal or a welding wire for connecting dissimilar materials.
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