CN110735077A - 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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- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- 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
- B22F3/11—Making porous workpieces or articles
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention belongs to the field of high-entropy alloy materials, and discloses AlCrFeNiSiTi high-entropy alloy porous materials and a preparation method thereof, wherein the AlCrFeNiSiTi high-entropy alloy porous materials comprise, by atomic percentage, 10% -20% of Al, 10% -20% of Cr, 10% -20% of Fe, 10% -20% of Ni, 10% -20% of Si and 10% -20% of Ti.
Description
Technical Field
The invention relates to the field of high-entropy alloy materials, in particular to AlCrFeNiSiTi high-entropy alloy porous materials and a preparation method thereof.
Background
The traditional metal porous materials adopt a single principal component plus alloying component material design mode, for example, FeNiCr stainless steel and FeCrAl alloy use Fe as principal component, and other elements as alloying components.
The High Entropy Alloy has the characteristics of single solid solution or multiphase Alloy in terms of phase composition, has structural lattice distortion effect, kinetic retardation diffusion effect and performance cocktail effect.
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 technology, the invention provides AlCrFeNiSiTi high-entropy alloy porous materials 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 AlCrFeNiSiTi high-entropy alloy porous materials, 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) vacuum sintering after cold pressing and forming, wherein a four-stage sintering process is adopted in the vacuum sintering, the temperature of the th 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.
, mixing the materials in the step (1) according to the atomic percentage of 10-15% of Al, 15-20% of Cr, 15-20% of Fe, 15-20% of Ni, 10-15% of Si and 15-20% of Ti.
, 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.
, adding lubricant in 1-3 wt% of the powder in step (4).
Further , the lubricant in step (4) is stearic acid.
, adding lubricant by alcohol solution of stearic acid in step (4).
And , the drying temperature in the step (4) is 60-70 ℃ for 30-240 minutes.
, pressing in step (5) by mould pressing or cold isostatic pressing at 80-350 MPa.
In the four-stage sintering process, the stage mainly removes oxidizing gas adsorbed on the surfaces of green body powder particles, the second stage mainly removes lubricants and the step purifies the surfaces of the powder particles, the third stage mainly utilizes rapid diffusion of elements such as Al and Si to generate Kirkendall pores in a green body, and simultaneously inhibits high-temperature self-propagating reaction possibly existing in a system, and the fourth stage mainly realizes full diffusion among main elements to complete homogenization of components and phases of materials.
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
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.
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 equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or as a range defined by the series of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pairing of any upper range limit or preferred value with any lower range limit or preferred value, regardless of whether ranges are separately disclosed.
The indefinite articles "" and "" preceding an element or component of the invention are not intended to limit the number of requirements (i.e. number of occurrences) of the element or component, therefore, "" or "" should be read to include or at least , and an element or component in the singular also includes the plural unless the number obviously refers to the singular.
Furthermore, the description of the terms " embodiments," " embodiments," "examples," "specific examples," or " examples," etc., described below, means that a particular feature, structure, material, or characteristic described in connection with the embodiments or examples is included in at least embodiments or examples of the invention.
Example 1
Taking Al, Cr, Fe, Ni, Si and Ti element powder as raw materials, mixing the raw materials according to the following component proportion (according to atom percentage), wherein the Al is 14 percent, the Cr is 18 percent, the Fe is 20 percent, the Ni is 19 percent, the Si is 12 percent, the Ti is 17 percent, the granularity range of the Al and the Ti is-200 meshes, the granularity range of the Cr and the Si is-325 meshes, the granularity range of the Fe and the Ni is-400 meshes, putting the main element powder into a V-shaped mixer for mixing, adopting inert gas for protection in the mixing atmosphere, mixing for 24 hours, adding 2 percent by mass of stearic acid into the mixed powder as a lubricant, adopting a stearic acid alcohol solution, adding the stearic acid into the mixed powder, drying the mixed powder in a vacuum drying box, drying at 70 ℃ for 120 minutes, adopting a mould pressing mode for pressing, adopting a vacuum sintering mode for 150MPa, adopting a four-stage sintering process for heating, controlling the temperature at ℃ for 30 minutes, controlling the heating rate at 20 ℃/min, and controlling the vacuum degree 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. After sintering, cooling toAnd (4) room temperature.
Example 2
Taking Al, Cr, Fe, Ni, Si and Ti element powder as raw materials, mixing the raw materials according to the following component proportion (in atom percentage), wherein the Al accounts for 10 percent, the Cr accounts for 20 percent, the Fe accounts for 15 percent, the Ni accounts for 15 percent, the Si accounts for 20 percent, the Ti accounts for 20 percent, the granularity ranges of the Al and the Ti accounts for-200 meshes, the granularity ranges of the Cr and the Si accounts for-325 meshes and the granularity ranges of the Fe and the Ni accounts for-400 meshes, putting the main element powder into a V-shaped mixer for mixing, adopting inert gas for protection in the mixing atmosphere, mixing for 24 hours, adding stearic acid with the mass percentage of 2 percent into the mixed powder as a lubricant, adding the stearic acid into an alcohol solution, drying the mixture in a vacuum drying box, drying at the drying temperature of 70 ℃ for 120 minutes, pressing in a mould pressing mode, sintering at the pressure of 150MPa, adopting a four-stage sintering process for heating, controlling the temperature of stage at the heat preservation time at 30 minutes, controlling the heating rate at 20 ℃/min and controlling the vacuum-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% stearic acid as lubricant into the mixed powder, dissolving with stearic acid alcoholAdding the raw materials in a liquid mode, drying in a vacuum drying oven at 70 ℃ for 120 minutes, pressing in a mould pressing mode, wherein the pressure is 150MPa, sintering in a vacuum sintering mode, heating in a four-stage sintering process, wherein the temperature of th 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-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 (10)
1, AlCrFeNiSiTi high-entropy alloy porous materials, characterized in that, the AlCrFeNiSiTi high-entropy alloy porous materials contains 10% -20% of Al, 10% -20% of Cr, 10% -20% of Fe, 10% -20% of Ni, 10% -20% of Si, and 10% -20% of Ti according to atom percentage.
2. The AlCrFeNiSiTi high entropy alloy porous material of claim 1, wherein the AlCrFeNiSiTi high entropy alloy porous material comprises, in atomic percent, Al: 10% -15%, Cr: 15% -20%, Fe: 15% -20%, Ni: 15% -20%, Si: 10% -15%, Ti: 15 to 20 percent.
3, AlCrFeNiSiTi high entropy alloy porous material preparation method, characterized by that, the said method includes 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) vacuum sintering after cold pressing and forming, wherein a four-stage sintering process is adopted in the vacuum sintering, the temperature of the th 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.
4. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, 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.
5. The preparation method of the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein 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.
6. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein a lubricant accounting for 1-3% of the powder by mass is added in the step (4).
7. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein the lubricant in the step (4) is stearic acid.
8. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein a lubricant is added in the step (4) by using a stearic acid alcohol solution.
9. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein the drying temperature in the step (4) is 60-70 ℃ and the drying time is 30-240 minutes.
10. The method for preparing the AlCrFeNiSiTi high-entropy alloy porous material as claimed in claim 3, wherein the step (5) is carried out by pressing in a mould pressing or cold isostatic pressing mode, and the pressure is 80-350 MPa.
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CN113046590A (en) * | 2021-02-04 | 2021-06-29 | 江苏大学 | High-entropy alloy/aluminum composite foam type wave-absorbing material and preparation method thereof |
CN115141984A (en) * | 2021-11-23 | 2022-10-04 | 燕山大学 | High-entropy austenitic stainless steel 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 |
CN114914454A (en) * | 2022-07-01 | 2022-08-16 | 北京理工大学重庆创新中心 | High-entropy alloy current collector and preparation method and application 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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