CN114058892A - Wear-resistant corrosion-resistant high-entropy alloy-based composite material and preparation method thereof - Google Patents
Wear-resistant corrosion-resistant high-entropy alloy-based composite material and preparation method thereof Download PDFInfo
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- C22C1/04—Making non-ferrous alloys by powder metallurgy
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- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
The invention discloses a wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof, belonging to the technical field of alloy-based composite materials, wherein the high-entropy alloy-based composite material comprises the following components: fe. Co, Cr, Ni; the method comprises the following steps: the components in equal atomic ratio are as follows: step two: preparing WC-FeCoCrNi composite powder: step three: preparing a block body: step four: testing the prepared composite material: the hardness, mechanical property, abrasion property and the like of the composite material,The corrosion behavior of the composite material in the simulated marine environment is tested, and the obtained WC-HEA composite material is prepared by WC hard particles and CrmCnThe wear resistance of the alloy is greatly improved under the joint strengthening action of the phases, and due to the addition of WC, the WC-HEA composite material can obtain good comprehensive corrosion resistance and pitting corrosion resistance, not only can inherit the characteristics of high plastic deformation capability, good corrosion resistance and the like of the FCC system high-entropy alloy, but also can improve the performances of the high-entropy alloy, such as hardness, strength, wear resistance and the like, by utilizing the strengthening phase.
Description
Technical Field
The invention relates to the technical field of alloy-based composite materials, in particular to a wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof.
Background
The high-entropy alloy (HEAS) is a novel alloy system taking a plurality of elements as main elements, M.H.Tsai (M.H.Tsai et al, Materials Research Letters,2014,2: 107-.
HEAS alloys can form single phase solid solution structures, with Face Centered Cubic (FCC) single phase solid solutions being the most widely studied due to their excellent ductility and toughness. The atomic size difference delta of FeCoCrNi high-entropy alloy system with equal atomic ratio is 1.03%, and the mixed entropy delta Smix1.34R (R: 8.314J/mol · K), enthalpy of mixing Δ HmixThe alloy has the advantages that the simple and single FCC solid solution structure is easily formed, the single-phase alloy has uniform components, no obvious macrosegregation and stable structure, has excellent thermal stability, plasticity and corrosion resistance, and is a typical high-entropy alloy researched at present. The HEAS system with FCC single-phase structure is similar to the traditional alloy, and has limited yield strength and hardness although having higher ductility, thus being difficult to meet the current application requirements. The material is compounded, namely the reinforcement of the metal matrix is realized by introducing the reinforcement, and the material has a series of advantages of high specific strength, good electric and heat conductivity, good dimensional stability and the like, and is expected to obtain more excellent performance.
At present, most researches adopt a vacuum melting method and a powder metallurgy method to prepare a bulk high-entropy alloy-based composite material. Among them, the vacuum melting method is the method used most at present, but because HEAs contain a plurality of elements, and the melting points of the matrix and the reinforcement are greatly different, the composition segregation of the high melting point elements and the volatilization of the low melting point elements are difficult to avoid in the melting process, for example, in the name of CrMoNbTiZr high-entropy alloy material and the preparation method thereof disclosed by patent CN107142410A, the vacuum melting method is adopted to prepare the high-entropy alloy with a solid solution phase and a Laves phase in a Body Centered Cubic (BCC) structure, but the alloy ingot has a coarse dendritic crystal structure, and a certain composition segregation exists in dendrites and dendritic crystal boundaries, which can cause unfavorable influence on the mechanical properties of the sample; in addition, the high-entropy alloy is easy to generate some brittle intermetallic compounds in the smelting process, and the defects of shrinkage porosity, air holes and the like can occur, so that the alloy performance is influenced more badly. Meanwhile, the size of the bulk alloy prepared by the vacuum melting method is limited by the size of the melting furnace, and the industrial application and development of the bulk alloy are limited. The powder metallurgy method is a low-cost and high-efficiency production process and is widely applied to preparation of non-equilibrium materials. In the name of 'preparation method of hard high-entropy alloy composite material' disclosed in patent CN108060322A, the hard high-entropy alloy composite material is prepared by a powder metallurgy method, but the invention prepares the composite material powder by a one-step low-energy ball milling method of 240-280r/min, the one-step ball milling method can lead the super-hard material powder WC, BN and the like to generate chemical reaction with alloy element powder to generate one or more carbides or nitrides with uneven distribution, and the bad influence is caused on the performance of the composite material, and in addition, the invention does not analyze and report the wear resistance and the corrosion resistance of the material.
Therefore, the invention hopes to develop a high-entropy alloy-based composite material with excellent comprehensive performance, so that the high-entropy alloy-based composite material not only can inherit the characteristics of high plastic deformation capability, good corrosion resistance and the like of the high-entropy alloy of an FCC system, but also can improve the performances of the high-entropy alloy, such as hardness, strength, wear resistance and the like by utilizing the reinforcing phase.
Disclosure of Invention
The invention aims to provide a wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof are disclosed, and the high-entropy alloy-based composite material comprises the following components: fe. Co, Cr, Ni;
the preparation method comprises the following steps:
the method comprises the following steps: the components in equal atomic ratio are as follows: respectively weighing Fe, Co, Cr and Ni pure metal powder by using an electronic balance, wherein the purity of the original pure metal powder is more than or equal to 99.95 percent, and the particle size is less than or equal to 45 mu m; WC powder is weighed according to the addition amount (10-30 wt%) of WC, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
Step two: preparing WC-FeCoCrNi composite powder:
the preparation of the composite powder adopts a two-step ball milling method, wherein the first step is mechanical alloying of pure metal element powder, the weighed pure metal powder of Fe, Co, Cr and Ni is poured into a vacuum stainless steel tank, a stainless steel ball with a proper proportion is added according to the ball-to-material ratio of 10:1, and a small amount of alcohol is added as a process control agent in order to prevent the powder from sticking to the tank;
carrying out ball milling by adopting an all-directional planetary ball mill, setting the rotating speed to be 300rpm, and setting the ball milling time to be 10-80 h; the second step is mixing high energy ball milling of HEA powder and WC powder (10-30 wt%), wherein the high energy ball milling time is 10 h;
after the ball milling is finished, pouring the powder into a 200-mesh screen to sieve the powder, so that the size of the powder is kept as small and uniform as possible;
step three: preparing a block body:
putting the powder into a high-strength graphite die for sintering in an operation box protected by high-purity argon, and separating a contact surface between a grinding tool and the powder by using graphite paper for the convenience of demoulding and the prevention of the reaction of the powder and the graphite die;
after the powder is loaded, a powder tablet machine is used for prepressing the powder at 15-20MPa, and then a mould is placed in a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: keeping the temperature at 1000 ℃ for 15min, keeping the pressure at 30MPa, releasing the pressure after sintering and cooling along with the furnace;
step four: testing the prepared composite material:
and testing the hardness, mechanical property and wear property of the composite material and the corrosion behavior of the composite material in a simulated marine environment.
Further, the vacuum stainless steel tank in the second step is arranged in an operation box containing high-purity argon protection.
Further, in the second step, graphite paper with the thickness of 2mm is stacked on the inner wall of a graphite die with the inner diameter of phi 30mm through high-energy ball milling, then composite powder is filled into the graphite die in an operation box protected by high-purity argon, the graphite paper is also stacked on the upper end and the lower end of the graphite die, 10 wt% of WC-HEA composite powder is pre-pressed at 15-20MPa by using a powder tablet press after being filled, and then the graphite die is placed into a discharge plasma sintering furnace.
Further, the sintering process comprises the following steps: heating from room temperature to 570 ℃ after 3min, heating from 570 ℃ to 600 ℃ after 10min, heating from 600 ℃ to 900 ℃ after 6min, heating from 900 ℃ to 1000 ℃ after 5min, keeping the temperature at 1000 ℃ for 15min, releasing pressure after sintering, cooling along with the furnace, and keeping constant pressure of 30MPa in the sintering process.
Furthermore, the processes of powder loading, powder taking and screening of the original pure metal powder are all carried out in an operation box protected by high-purity argon.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention prepares the HEA material with a single-phase FCC solid solution structure and good mechanical stability by adopting mechanical alloying (10h-80h) and combining with spark plasma sintering, has wide mechanical alloying time range, reasonable and simple preparation process and strong repeatability of the preparation process, and can realize industrialized mass production.
2. The invention adopts a two-step ball milling method to prepare the composite powder, thereby inhibiting the WC powder and the pure metal element powder from generating chemical reaction in the ball milling process.
3. The WC-HEA composite material can obtain WC particles which are fine and uniformly dispersed, the interface of the matrix and the WC particles is well combined, and the density can reach more than 97%.
4. According to the invention, the WC-HEA composite material is prepared by adding WC particles into the HEA matrix, so that high plasticity is ensured and high yield strength and hardness are obtained. The microhardness of the WC-HEA composite material containing 10-30 wt% is 349-465HV, which are all higher than that of the matrix material (295 HV); the yield strength is 913.99-1315.09MPa, and is improved by 47.5% -112.2% compared with the matrix (619.86 MPa).
5. The WC-HEA composite material obtained by the invention is prepared from WC hard particles and CrmCnThe wear resistance of the composite material is greatly improved due to the joint strengthening effect of the phases, and the WC-HEA composite material can obtain good general corrosion resistance and pitting corrosion resistance due to the addition of the WC.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is an XRD pattern of WC-HEA based composite blocks of the present invention at different WC contents;
FIG. 3 shows the mechanical property analysis results of the WC-HEA composite material of the present invention;
FIG. 4 shows the results of the corrosion resistance analysis of the WC-HEA composite material of the present invention;
FIG. 5 shows the results of the wear performance analysis of the WC-HEA composite material of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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. 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.
Referring to fig. 1, the present invention provides a technical solution: a wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof are disclosed, and the high-entropy alloy-based composite material comprises the following components: fe. Co, Cr, Ni;
the preparation method comprises the following steps:
the method comprises the following steps: the components in equal atomic ratio are as follows: respectively weighing Fe, Co, Cr and Ni pure metal powder by using an electronic balance, wherein the purity of the original pure metal powder is more than or equal to 99.95 percent, and the particle size is less than or equal to 45 mu m; WC powder is weighed according to the addition amount (10-30 wt%) of WC, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
Step two: preparing WC-FeCoCrNi composite powder:
the preparation of the composite powder adopts a two-step ball milling method, wherein the first step is mechanical alloying of pure metal element powder, the weighed pure metal powder of Fe, Co, Cr and Ni is poured into a vacuum stainless steel tank, a stainless steel ball with a proper proportion is added according to the ball-to-material ratio of 10:1, and a small amount of alcohol is added as a process control agent in order to prevent the powder from sticking to the tank;
carrying out ball milling by adopting an all-directional planetary ball mill, setting the rotating speed to be 300rpm, and setting the ball milling time to be 10-80 h; the second step is mixing high energy ball milling of HEA powder and WC powder (10-30 wt%), wherein the high energy ball milling time is 10 h;
and after the ball milling is finished, pouring the powder into a 200-mesh screen to sieve the powder, so that the size of the powder is kept as fine and uniform as possible.
The two-step ball milling method is mainly used for inhibiting the reaction of WC powder and pure metal element powder in the ball milling process.
Step three: preparing a block body:
putting the powder into a high-strength graphite die for sintering in an operation box protected by high-purity argon, and separating a contact surface between a grinding tool and the powder by using graphite paper for the convenience of demoulding and the prevention of the reaction of the powder and the graphite die;
after the powder is loaded, a powder tablet machine is used for prepressing the powder at 15-20MPa, and then a mould is placed in a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: keeping the temperature at 1000 ℃ for 15min, keeping the pressure constant at 30MPa, and unloading pressure and cooling along with the furnace after sintering.
Step four: testing the prepared composite material:
and testing the hardness, mechanical property and wear property of the composite material and the corrosion behavior of the composite material in a simulated marine environment.
Example one
(1) Weighing Fe, Co, Cr and Ni powder with equal atomic ratio and 10 wt% of WC nano powder in an operation box under the protection of high-purity argon, wherein the purity of the Fe, Co, Cr and Ni powder is more than or equal to 99.95%, the particle size is less than or equal to 45 mu m, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
(2) In an operation box protected by high-purity argon, weighing pure metal powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder, sequentially adding the pure metal powder, the stainless steel balls and the alcohol into a stainless steel ball milling tank, then installing the sealed stainless steel tank on an omnibearing planetary ball mill for ball milling, setting the rotating speed to be 300rpm, and setting the ball milling time to be 10 hours, thus preparing the HEA powder which is uniformly mixed and pre-alloyed.
(3) Mixing 10 wt% of WC nano powder and the HEA powder prepared in the previous step in an operation box under the protection of high-purity argon gas, performing high-energy ball milling for 10 hours, pouring the powder into a 200-mesh screen to sieve the powder after the ball milling is finished, and keeping the size of the powder as fine and uniform as possible.
(4) Stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then filling composite powder into the graphite mould in an operation box protected by high-purity argon gas, stacking the graphite paper on the upper end and the lower end of the graphite mould, prepressing the powder at 15-20MPa by using a powder tablet press after filling 10 wt% of WC-HEA composite powder, then putting the mould into a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: heating from room temperature to 570 ℃ after 3min, heating from 570 ℃ to 600 ℃ after 10min, heating from 600 ℃ to 900 ℃ after 6min, heating from 900 ℃ to 1000 ℃ after 5min, keeping the temperature at 1000 ℃ for 15min, releasing pressure after sintering, cooling along with the furnace, and keeping constant pressure of 30MPa in the sintering process.
(5) The microstructure of the 10 wt% WC-HEA composite obtained in this example is shown in FIG. 3 (b); the composite had a hardness of 349HV, a yield strength of 913.99MPa, and a compressibility of 30.37%, as shown in fig. 5. The potential of the composite material for corrosion starting is-0.22V; the magnitude of the Vicat current density is 1 multiplied by 10 < -5 > A/cm2, the self-corrosion potential of the composite material after fitting is-0.56V, and the self-corrosion current is 2.6 multiplied by 10 < -6 > A/cm 2; the composite material was abraded to a volume of about 2.1X 106 μm 3.
Example two
(1) Weighing Fe, Co, Cr and Ni powder with equal atomic ratio and 30 wt% of WC nano powder in an operation box under the protection of high-purity argon, wherein the purity of the Fe, Co, Cr and Ni powder is more than or equal to 99.95%, the particle size is less than or equal to 45 mu m, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
(2) In an operation box protected by high-purity argon, weighing pure metal powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder, sequentially adding the pure metal powder, the stainless steel balls and the alcohol into a stainless steel ball milling tank, then installing the sealed stainless steel tank on an omnibearing planetary ball mill for ball milling, setting the rotating speed to be 300rpm, and setting the ball milling time to be 10 hours, thus preparing the HEA powder which is uniformly mixed and pre-alloyed.
(3) And mixing 30 wt% of WC nano powder and the HEA powder prepared in the last step in an operation box under the protection of high-purity argon, performing high-energy ball milling for 10 hours, pouring the powder into a 200-mesh screen to sieve the powder after the ball milling is finished, and keeping the size of the powder as fine and uniform as possible.
(4) Stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then filling composite powder into the graphite mould in an operation box protected by high-purity argon gas, stacking the graphite paper on the upper end and the lower end of the graphite mould, pre-pressing the powder at 15-20MPa by using a powder tablet press after filling 30 wt% of WC-HEA composite powder, then putting the mould into a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: heating from room temperature to 570 ℃ after 3min, heating from 570 ℃ to 600 ℃ after 10min, heating from 600 ℃ to 900 ℃ after 6min, heating from 900 ℃ to 1000 ℃ after 5min, keeping the temperature at 1000 ℃ for 15min, releasing pressure after sintering, cooling along with the furnace, and keeping constant pressure of 30MPa in the sintering process.
(5) The microstructure of the 30 wt% WC-HEA composite obtained in this example is shown in FIG. 3 (b); the composite had a hardness of 465HV, a yield strength of 1315.09MPa, and a compressibility of 16.59%, as shown in FIG. 5. The potential of the composite material for starting corrosion is-0.17V; the magnitude of the Vicat current density is 1.24 multiplied by 10 < -5 > A/cm2, the self-corrosion potential of the composite material after fitting is-0.52V, and the self-corrosion current is 3.24 multiplied by 10 < -6 > A/cm 2; the composite material was abraded to a volume of about 1.4X 105 μm 3.
EXAMPLE III
(1) Weighing Fe, Co, Cr and Ni powder with equal atomic ratio and 20 wt% of WC nano powder in an operation box under the protection of high-purity argon, wherein the purity of the Fe, Co, Cr and Ni powder is more than or equal to 99.95%, the particle size is less than or equal to 45 mu m, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
(2) In an operation box protected by high-purity argon, weighing pure metal powder, stainless steel balls (ball-to-material ratio is 10:1) and alcohol with the mass of 2.5 wt% of the powder, sequentially adding the pure metal powder, the stainless steel balls and the alcohol into a stainless steel ball milling tank, then installing the sealed stainless steel tank on an omnibearing planetary ball mill for ball milling, setting the rotating speed to be 300rpm, and setting the ball milling time to be 80h, and preparing the HEA powder which is uniformly mixed and pre-alloyed.
(3) And mixing 20 wt% of WC nano powder and the HEA powder prepared in the last step in an operation box under the protection of high-purity argon, performing high-energy ball milling for 10 hours, pouring the powder into a 200-mesh screen to sieve the powder after the ball milling is finished, and keeping the size of the powder as fine and uniform as possible.
(4) Stacking graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then filling composite powder into the graphite mould in an operation box protected by high-purity argon gas, stacking the graphite paper on the upper end and the lower end of the graphite mould, pre-pressing the powder at 15-20MPa by using a powder tablet press after filling 20 wt% of WC-HEA composite powder, then putting the mould into a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: heating from room temperature to 570 ℃ after 3min, heating from 570 ℃ to 600 ℃ after 10min, heating from 600 ℃ to 900 ℃ after 6min, heating from 900 ℃ to 1000 ℃ after 5min, keeping the temperature at 1000 ℃ for 15min, releasing pressure after sintering, cooling along with the furnace, and keeping constant pressure of 30MPa in the sintering process.
(5) The microstructure of the 20 wt% WC-HEA composite obtained in this example is shown in FIG. 3 (b); the composite had a hardness of 485HV, a yield strength of 1204.18MPa, and a compressibility of 20.73%, as shown in FIG. 5. The potential of the composite material for starting corrosion is-0.15V; the magnitude of the Vicat current density is-1.15 multiplied by 10 < -5 > A/cm2, the self-corrosion potential of the composite material is-0.49V after fitting, and the self-corrosion current is 3.2 multiplied by 10 < -6 > A/cm 2; the composite material was abraded to a volume of about 5X 105 μm 3.
In the above example, the hardness of the composite material was measured using a digital display microhardness tester of DIIV-1000Z manufactured by Shanghai Shang materials testing machine, Inc.; testing the mechanical property of the composite material by adopting an electronic universal testing machine which is manufactured by American Instron corporation and has the model number of INSTRON 3382; testing the abrasion performance of the composite material by adopting a friction abrasion tester with the model number of LMT-100 manufactured by American Rtec instruments ltd; an electrochemical workstation which is manufactured by German armek company and is of a model of Versa STAT 4 is adopted, a potentiodynamic polarization experiment is utilized to research the corrosion behavior of the composite material in a simulated marine environment (NaCl solution), the higher the self-corrosion potential is, the lower the tendency of the sample to generate overall corrosion is, the lower the Victorian current density is, the higher the pitting potential is, and the lower the tendency of the sample to generate pitting corrosion is.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A wear-resistant corrosion-resistant high-entropy alloy-based composite material and a preparation method thereof are characterized in that: the high-entropy alloy-based composite material comprises the following components: fe. Co, Cr, Ni;
the preparation method comprises the following steps:
the method comprises the following steps: the components in equal atomic ratio are as follows: respectively weighing Fe, Co, Cr and Ni pure metal powder by using an electronic balance, wherein the purity of the original pure metal powder is more than or equal to 99.95 percent, and the particle size is less than or equal to 45 mu m; WC powder is weighed according to the addition amount (10-30 wt%) of WC, the purity of the WC powder is more than or equal to 99.9%, and the particle size is less than or equal to 300 nm.
Step two: preparing WC-FeCoCrNi composite powder:
the preparation of the composite powder adopts a two-step ball milling method, wherein the first step is mechanical alloying of pure metal element powder, the weighed pure metal powder of Fe, Co, Cr and Ni is poured into a vacuum stainless steel tank, a stainless steel ball with a proper proportion is added according to the ball-to-material ratio of 10:1, and a small amount of alcohol is added as a process control agent in order to prevent the powder from sticking to the tank;
carrying out ball milling by adopting an all-directional planetary ball mill, setting the rotating speed to be 300rpm, and setting the ball milling time to be 10-80 h; the second step is mixing high energy ball milling of HEA powder and WC powder (10-30 wt%), wherein the high energy ball milling time is 10 h;
after the ball milling is finished, pouring the powder into a 200-mesh screen to sieve the powder, so that the size of the powder is kept as small and uniform as possible;
step three: preparing a block body:
putting the powder into a high-strength graphite die for sintering in an operation box protected by high-purity argon, and separating a contact surface between a grinding tool and the powder by using graphite paper for the convenience of demoulding and the prevention of the reaction of the powder and the graphite die;
after the powder is loaded, a powder tablet machine is used for prepressing the powder at 15-20MPa, and then a mould is placed in a discharge plasma sintering furnace, wherein the sintering process comprises the following steps: keeping the temperature at 1000 ℃ for 15min, keeping the pressure at 30MPa, releasing the pressure after sintering and cooling along with the furnace;
step four: testing the prepared composite material:
and testing the hardness, mechanical property and wear property of the composite material and the corrosion behavior of the composite material in a simulated marine environment.
2. The wear-resistant corrosion-resistant high-entropy alloy-based composite material and the preparation method thereof according to claim 1, are characterized in that: and in the second step, the vacuum stainless steel tank is arranged in an operation box containing high-purity argon protection.
3. The wear-resistant corrosion-resistant high-entropy alloy-based composite material and the preparation method thereof according to claim 1, are characterized in that: and step two, mixing high-energy ball milling, namely padding graphite paper with the thickness of 2mm on the inner wall of a graphite mould with the inner diameter of phi 30mm, then filling composite powder into the graphite mould in an operation box protected by high-purity argon, padding the graphite paper on the upper end and the lower end of the graphite mould, pre-pressing the powder at 15-20MPa by using a powder tablet press after 10 wt% of WC-HEA composite powder is filled, and then putting the mould into a discharge plasma sintering furnace.
4. The wear-resistant corrosion-resistant high-entropy alloy-based composite material and the preparation method thereof according to claim 3, are characterized in that: the sintering process comprises the following steps: heating from room temperature to 570 ℃ after 3min, heating from 570 ℃ to 600 ℃ after 10min, heating from 600 ℃ to 900 ℃ after 6min, heating from 900 ℃ to 1000 ℃ after 5min, keeping the temperature at 1000 ℃ for 15min, releasing pressure after sintering, cooling along with the furnace, and keeping constant pressure of 30MPa in the sintering process.
5. The wear-resistant corrosion-resistant high-entropy alloy-based composite material and the preparation method thereof according to claim 1, are characterized in that: the original pure metal powder is filled, taken and sieved in an operation box under the protection of high-purity argon.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752836A (en) * | 2022-03-18 | 2022-07-15 | 郑州大学 | AlN-CoCrFeNi cermet electrothermal material and preparation method thereof |
| CN114807725A (en) * | 2022-05-31 | 2022-07-29 | 中国矿业大学 | High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof |
| CN115401195A (en) * | 2022-09-13 | 2022-11-29 | 中国化学工程第十一建设有限公司 | Particle-reinforced high-entropy alloy powder and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170314097A1 (en) * | 2016-05-02 | 2017-11-02 | Korea Advanced Institute Of Science And Technology | High-strength and ultra heat-resistant high entropy alloy (hea) matrix composites and method of preparing the same |
| CN108060322A (en) * | 2017-12-07 | 2018-05-22 | 中南大学 | The preparation method of hard high-entropy alloy composite material |
| CN109161774A (en) * | 2018-11-23 | 2019-01-08 | 西安工业大学 | Haystellite and preparation method thereof by high-entropy alloy as binder |
-
2021
- 2021-10-27 CN CN202111253697.XA patent/CN114058892A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170314097A1 (en) * | 2016-05-02 | 2017-11-02 | Korea Advanced Institute Of Science And Technology | High-strength and ultra heat-resistant high entropy alloy (hea) matrix composites and method of preparing the same |
| CN108060322A (en) * | 2017-12-07 | 2018-05-22 | 中南大学 | The preparation method of hard high-entropy alloy composite material |
| CN109161774A (en) * | 2018-11-23 | 2019-01-08 | 西安工业大学 | Haystellite and preparation method thereof by high-entropy alloy as binder |
Non-Patent Citations (1)
| Title |
|---|
| JUAN XU等: "Microstructure and Properties of CoCrFeNi(WC) High-Entropy Alloy Coatings Prepared Using Mechanical Alloying and Hot Pressing Sintering", 《COATINGS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752836A (en) * | 2022-03-18 | 2022-07-15 | 郑州大学 | AlN-CoCrFeNi cermet electrothermal material and preparation method thereof |
| CN114807725A (en) * | 2022-05-31 | 2022-07-29 | 中国矿业大学 | High-entropy alloy-based nano superhard composite material enhanced by inlaid particles and preparation method thereof |
| CN115401195A (en) * | 2022-09-13 | 2022-11-29 | 中国化学工程第十一建设有限公司 | Particle-reinforced high-entropy alloy powder and preparation method and application thereof |
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