CN110735077B - AlCrFeNiSiTi high-entropy alloy porous material and preparation method thereof - Google Patents
AlCrFeNiSiTi high-entropy alloy porous material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of high-entropy alloy materials, and discloses an AlCrFeNiSiTi high-entropy alloy porous material and a preparation method thereof. The AlCrFeNiSiTi high-entropy alloy porous material comprises the following components in percentage by atom: 10% -20%, Cr: 10% -20%, Fe: 10% -20%, Ni: 10% -20%, Si: 10% -20%, Ti: 10% -20%, the AlCrFeNiSiTi high-entropy alloy porous material is prepared by adopting a reaction synthesis method of element powder, the element powder of each principal element is taken as a raw material, only a small amount of lubricant needs to be added in the preparation process, and the energy consumption and the cost are low; the Kirkendall effect caused by partial diffusion among elements is fully utilized to generate pores, the controllability of the pore structure is good, a pore-forming agent is not required to be added, the problem of subsequent pore-forming agent removal is avoided, and the method has the characteristics of short flow and high performance.
Description
Technical Field
The invention relates to the field of high-entropy alloy materials, in particular to an AlCrFeNiSiTi high-entropy alloy porous material and a preparation method thereof.
Background
The metal porous material is widely used as an inorganic porous material at present, and mainly comprises a FeNiCr stainless steel porous material, a FeCrAl alloy high-temperature resistant porous material, a Ni-based alloy porous material, a Ti-based alloy porous material and the like. The traditional metal porous materials adopt a material design mode of a single principal component and alloying components, for example, FeNiCr stainless steel and FeCrAl alloy take Fe as a principal component, and other elements are alloying components.
High Entropy Alloy (HEA) has significant material advantages over traditional metallic materials. Different from the material design mode of single principal element and alloying component of the traditional metal material, the high-entropy alloy adopts the design of 5 or more multiple principal elements, the content of each principal element is within the range of 5-35 percent, and the high-entropy alloy has typical high-entropy thermodynamic effect. High entropy alloys may exhibit characteristics of single solid solution, or multi-phase alloys, in terms of phase composition. The high-entropy alloy has a structural lattice distortion effect, a kinetic delayed diffusion effect and a performance cocktail effect. Through the research of the material design and the preparation process of the system, the high-entropy alloy can have good mechanical properties including good strength and toughness and excellent high-temperature resistance and corrosion resistance.
At present, the high-entropy alloy is mainly prepared by a fusion casting method, and the method is difficult to prepare the high-entropy alloy porous material. In order to prepare the high-entropy alloy porous material, researchers propose that high-entropy alloy pre-alloy powder is prepared by an atomization method, and then a porous body is prepared by a subsequent pressing and sintering method. The method has the characteristic of high energy consumption because various principal element metals need to be melted and atomized to prepare powder. And the pressing performance of the prealloyed powder is poor, and a large amount of forming agent is often required to be added in the pressing process, so that the problem of large amount of discharge in the removing process is caused. Meanwhile, in the process of preparing the porous material by the method, the formation of pores can only come from interstitial spaces among powder particles, so that a pore-forming agent is often required to be added in the preparation process, the problem of subsequent removal exists, and the method has longer working procedures and higher cost.
Disclosure of Invention
In order to overcome the defects of the background art, the invention provides an AlCrFeNiSiTi high-entropy alloy porous material and a preparation method thereof.
Al and Cr elements in the AlCrFeNiSiTi high-entropy alloy porous material can play a role in enhancing the high-temperature oxidation resistance of the alloy, Fe and Ni elements can play a role in improving the mechanical property of the material, and Si and Ti elements can play a role in enhancing the corrosion resistance of the alloy. The porous high-entropy alloy of the system has good material performance due to the synergistic effect of a plurality of principal elements, and has good application prospect in the filtration field and the electrode field of harsh environments. In addition, the method of the invention takes the element powder of each principal component as the raw material, has low cost and better pressing performance, only needs to add a small amount of lubricant in the preparation process, and has the characteristics of low energy consumption and low cost. Moreover, the alloy material is prepared by adopting the reaction between the element powders, the Kirkendall effect caused by the partial diffusion between the elements can be fully utilized to generate pores, the controllability of the pore structure is better, the pore-forming agent is not required to be added, the problem of subsequent removal of the pore-forming agent is avoided, and the alloy material has the characteristics of short flow and high performance.
In order to achieve the purpose of the invention, the AlCrFeNiSiTi high-entropy alloy porous material comprises the following components in percentage by atom: 10% -20%, Cr: 10% -20%, Fe: 10% -20%, Ni: 10% -20%, Si: 10% -20%, Ti: 10 to 20 percent.
Preferably, the AlCrFeNiSiTi high-entropy alloy porous material comprises Al: 10% -15%, Cr: 15% -20%, Fe: 15% -20%, Ni: 15% -20%, Si: 10% -15%, Ti: 15 to 20 percent.
In order to achieve the aim of the invention, the invention also provides a preparation method of the AlCrFeNiSiTi high-entropy alloy porous material, which comprises the following steps:
(1) the component ratio is as follows: al, Cr, Fe, Ni, Si and Ti element powder is adopted as a raw material, and the weight ratio of Al: 10% -20%, Cr: 10% -20%, Fe: 10% -20%, Ni: 10% -20%, Si: 10% -20%, Ti: 10-20% of the mixture in atomic percentage;
(2) the particle size ratio is as follows: in the main element elements, the powder of Al and Ti has the coarsest granularity, and the granularity range is-200 meshes; the powder of Cr and Si has medium granularity, and the granularity range is-325 meshes; fe. The powder of Ni has the finest granularity, and the granularity range is-400 meshes;
(3) mixing materials: putting the powder of each principal element into a mixer for mixing;
(4) adding a lubricant: adding a lubricant into the mixed powder, and drying in a vacuum drying oven after adding;
(5) and (3) vacuum sintering after cold pressing forming: the heating in the vacuum sintering adopts a four-stage sintering process, the temperature of the first stage is 120-250 ℃, the heat preservation time is 30-60 minutes, the temperature rise rate is controlled to be 15-20 ℃/min, and the vacuum degree is controlled to be 10-2-10- 1Pa; the temperature of the second stage is 350--3-10-2Pa; the temperature of the third stage is 550-700 ℃, 1 or more heat-preservation platforms can be arranged in the temperature range of the third stage, the total heat-preservation time is 240-600 min, the temperature-rise rate is controlled to be 1-5 ℃/min, and the vacuum degree is controlled to be 10-3-10-2Pa; the temperature of the fourth stage is 900--3-10-2Pa；
(6) Cooling along with the furnace: and after sintering, cooling to room temperature along with the furnace.
Further, in the step (1), the ratio of Al: 10% -15%, Cr: 15% -20%, Fe: 15% -20%, Ni: 15% -20%, Si: 10% -15%, Ti: 15 to 20 percent of the mixture in percentage by atom.
Further, the mixer in the step (3) is a V-shaped mixer, the mixing atmosphere is protected by inert gas, and the mixing time is 8-72 hours.
Further, a lubricant accounting for 1-3% of the mass of the powder is added in the step (4).
Further, the lubricant in the step (4) is stearic acid.
Further, in the step (4), the lubricant is added in a manner of a stearic acid alcohol solution.
Further, in the step (4), the drying temperature is 60-70 ℃ and the drying time is 30-240 minutes.
Further, the step (5) adopts a mould pressing or cold isostatic pressing mode for pressing, and the pressure is 80-350 MPa.
In the four-stage sintering process, oxidizing gas adsorbed on the surfaces of powder particles of a green body is mainly removed in the first stage, a lubricant is mainly removed in the second stage, the surfaces of the powder particles are further purified, Kirkendall pores are mainly generated in the green body by quickly diffusing Al, Si and other elements in the third stage, high-temperature self-propagating reaction possibly existing in a system is inhibited, and full diffusion among all main element elements is mainly realized in the fourth stage, so that the homogenization of the components and phases of the material is completed.
The beneficial effects of the invention include but are not limited to the following three aspects:
1. the AlCrFeNiSiTi high-entropy alloy porous material is prepared by adopting a reaction synthesis method of element powder, the element powder of each principal element is taken as a raw material, the cost is low, the pressing performance is good, only a small amount of lubricant needs to be added in the preparation process, and the AlCrFeNiSiTi high-entropy alloy porous material has the characteristics of low energy consumption and low cost;
2. pores are generated by fully utilizing the Kirkendall effect caused by partial diffusion among elements, the controllability of the pore structure is good, a pore-forming agent is not required to be added, the problem of subsequent removal of the pore-forming agent is solved, and the method has the characteristics of short flow and high performance;
3. the preparation of the AlCrFeNiSiTi high-entropy alloy porous material is provided, Al and Cr elements can enhance the high-temperature oxidation resistance of the alloy, Fe and Ni elements can improve the mechanical property of the material, Si and Ti elements can enhance the corrosion resistance of the alloy, and a plurality of principal elements act synergistically to endow the porous high-entropy alloy of the system with good material properties, so that the porous high-entropy alloy porous material has good application prospects in the filtration field and the electrode field of harsh environments.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that the following description is only illustrative of the present invention and is not to be construed as limiting the present invention.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
Furthermore, the description below of the terms "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily for the same embodiment or example. Further, the technical features of the embodiments of the present invention may be combined with each other as long as they do not conflict with each other.
Example 1
Al, Cr, Fe, Ni, Si and Ti element powder is used as raw materials, and the raw materials are mixed according to the following component proportionIn atomic percent), Al: 14%, Cr: 18%, Fe: 20%, Ni: 19%, Si: 12%, Ti: 17 percent. The granularity of Al and Ti is-200 meshes; the particle size range of Cr and Si is-325 meshes; fe. The Ni particle size range is-400 meshes. And (3) putting the powder of each principal element into a V-shaped mixer for mixing, wherein the mixing atmosphere is protected by inert gas, and the mixing time is 24 hours. Adding 2% of stearic acid serving as a lubricant into the mixed powder in percentage by mass, adding the stearic acid in an alcohol solution of stearic acid, and drying the stearic acid in a vacuum drying oven at the drying temperature of 70 ℃ for 120 minutes. Pressing by adopting a mould pressing mode, wherein the pressure is 150 MPa. The sintering adopts a vacuum sintering mode, and the heating adopts a four-stage sintering process. The temperature of the first stage is 150 ℃, the heat preservation time is 30 minutes, the heating rate is controlled at 20 ℃/min, and the vacuum degree is controlled at 10 DEG C-2-10-1Pa. The temperature of the second stage is 450 ℃, the heat preservation time is 90 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The temperature of the third stage is 560 ℃ and 620 ℃, the holding time is 180 minutes and 240 minutes respectively, the heating rate is controlled at 2 ℃/min, the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The fourth stage temperature is 1050 ℃, the heat preservation time is 240 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. And after sintering, cooling to room temperature along with the furnace.
Example 2
Al, Cr, Fe, Ni, Si and Ti element powder is used as a raw material, and the raw material is mixed according to the following component proportion (according to atomic percent), wherein Al: 10%, Cr: 20%, Fe: 15%, Ni: 15%, Si: 20%, Ti: 20 percent. The granularity of Al and Ti is-200 meshes; the particle size range of Cr and Si is-325 meshes; fe. The Ni particle size range is-400 meshes. And (3) putting the powder of each principal element into a V-shaped mixer for mixing, wherein the mixing atmosphere is protected by inert gas, and the mixing time is 24 hours. Adding 2% of stearic acid serving as a lubricant into the mixed powder in percentage by mass, adding the stearic acid in an alcohol solution of stearic acid, and drying the stearic acid in a vacuum drying oven at the drying temperature of 70 ℃ for 120 minutes. Pressing by adopting a mould pressing mode, wherein the pressure is 150 MPa. The sintering adopts a vacuum sintering mode and heatingA four-stage sintering process is adopted. The temperature of the first stage is 150 ℃, the heat preservation time is 30 minutes, the heating rate is controlled at 20 ℃/min, and the vacuum degree is controlled at 10 DEG C-2-10-1Pa. The temperature of the second stage is 450 ℃, the heat preservation time is 90 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The temperature of the third stage is 560 ℃ and 620 ℃, the holding time is 180 minutes and 240 minutes respectively, the heating rate is controlled at 2 ℃/min, the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The fourth stage temperature is 1050 ℃, the heat preservation time is 240 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. And after sintering, cooling to room temperature along with the furnace.
Example 3
Al, Cr, Fe, Ni, Si and Ti element powder is used as a raw material, and the raw material is mixed according to the following component proportion (according to atomic percent), wherein Al: 15%, Cr: 15%, Fe: 18%, Ni: 20%, Si: 15%, Ti: 17 percent. The granularity of Al and Ti is-200 meshes; the particle size range of Cr and Si is-325 meshes; fe. The Ni particle size range is-400 meshes. And (3) putting the powder of each principal element into a V-shaped mixer for mixing, wherein the mixing atmosphere is protected by inert gas, and the mixing time is 24 hours. Adding 2% of stearic acid serving as a lubricant into the mixed powder in percentage by mass, adding the stearic acid in an alcohol solution of stearic acid, and drying the stearic acid in a vacuum drying oven at the drying temperature of 70 ℃ for 120 minutes. Pressing by adopting a mould pressing mode, wherein the pressure is 150 MPa. The sintering adopts a vacuum sintering mode, and the heating adopts a four-stage sintering process. The temperature of the first stage is 150 ℃, the heat preservation time is 30 minutes, the heating rate is controlled at 20 ℃/min, and the vacuum degree is controlled at 10 DEG C-2-10-1Pa. The temperature of the second stage is 450 ℃, the heat preservation time is 90 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The temperature of the third stage is 560 ℃ and 620 ℃, the holding time is 180 minutes and 240 minutes respectively, the heating rate is controlled at 2 ℃/min, the vacuum degree is controlled at 10 DEG C-3-10-2Pa. The fourth stage temperature is 1050 ℃, the heat preservation time is 240 minutes, the heating rate is controlled at 5 ℃/min, and the vacuum degree is controlled at 10 DEG C-3-10-2Pa. And after sintering, cooling to room temperature along with the furnace.
It will be understood by those skilled in the art that the foregoing is only exemplary of the present invention, and is not intended to limit the invention, which is intended to cover any variations, equivalents, or improvements therein, which fall within the spirit and scope of the invention.
Claims (5)
1. A preparation method of an AlCrFeNiSiTi high-entropy alloy porous material is characterized by comprising the following steps:
(1) the component ratio is as follows: al, Cr, Fe, Ni, Si and Ti element powder is adopted as a raw material, and the weight ratio of Al: 10% -20%, Cr: 10% -20%, Fe: 10% -20%, Ni: 10% -20%, Si: 10% -20%, Ti: 10-20% of the mixture in atomic percentage;
(2) the particle size ratio is as follows: in the main element elements, the powder of Al and Ti has the coarsest granularity, and the granularity range is-200 meshes; the powder of Cr and Si has medium granularity, and the granularity range is-325 meshes; fe. The powder of Ni has the finest granularity, and the granularity range is-400 meshes;
(3) mixing materials: putting the powder of each principal element into a mixer for mixing;
(4) adding a lubricant: adding a lubricant into the mixed powder, and drying in a vacuum drying oven after adding;
(5) and (3) vacuum sintering after cold pressing forming: the heating in the vacuum sintering adopts a four-stage sintering process, the temperature of the first stage is 120-250 ℃, the heat preservation time is 30-60 minutes, the temperature rise rate is controlled to be 15-20 ℃/min, and the vacuum degree is controlled to be 10-2-10-1Pa; the temperature of the second stage is 350--3-10-2Pa; the temperature of the third stage is 550-700 ℃, 1 or more heat-preservation platforms can be arranged in the temperature range of the third stage, the total heat-preservation time is 240-600 min, the temperature-rise rate is controlled to be 1-5 ℃/min, and the vacuum degree is controlled to be 10-3-10- 2Pa; the temperature of the fourth stage is 900-1-5 deg.C/min, vacuum degree controlled at 10-3-10-2Pa；
(6) Cooling along with the furnace: after sintering, cooling to room temperature along with the furnace;
the lubricant in the step (4) is stearic acid, and is added in a stearic acid alcohol solution mode; and (5) pressing by adopting a mould pressing or cold isostatic pressing mode, wherein the pressure is 80-350 MPa.
2. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 1, wherein the ratio of Al: 10% -15%, Cr: 15% -20%, Fe: 15% -20%, Ni: 15% -20%, Si: 10% -15%, Ti: 15 to 20 percent of the mixture in percentage by atom.
3. The preparation method of the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 1, wherein a mixer in the step (3) is a V-shaped mixer, the mixing atmosphere is protected by inert gas, and the mixing time is 8-72 hours.
4. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 1, wherein a lubricant accounting for 1-3% of the powder by mass is added in the step (4).
5. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 1, wherein the drying temperature in the step (4) is 60-70 ℃ and the drying time is 30-240 minutes.
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| CN111633218A (en) * | 2020-06-17 | 2020-09-08 | 西北有色金属研究院 | High-entropy alloy powder and oxygen-free sintering preparation method thereof |
| CN112322957B (en) * | 2020-11-10 | 2022-03-29 | 中南大学 | Corrosion-resistant high-strength-and-toughness Fe-rich multi-component alloy and preparation method thereof |
| CN113046590B (en) * | 2021-02-04 | 2022-05-20 | 江苏大学 | High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof |
| CN115141984B (en) * | 2021-11-23 | 2023-02-24 | 燕山大学 | High-entropy austenitic stainless steel and preparation method thereof |
| CN114914454B (en) * | 2022-07-01 | 2023-05-26 | 北京理工大学重庆创新中心 | High-entropy alloy current collector and preparation method and application thereof |
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