CN115074558B - Method for regulating and controlling CoCrCuFeNi high-entropy alloy structure and magnetism by utilizing heat treatment - Google Patents
Method for regulating and controlling CoCrCuFeNi high-entropy alloy structure and magnetism by utilizing heat treatment Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
Hair brushThe invention provides a method for regulating and controlling the structure and magnetism of a CoCrCuFeNi high-entropy alloy by utilizing heat treatment, which comprises the following steps: taking high-purity simple substance elements as raw materials, uniformly mixing the raw materials in proportion, and pretreating; smelting by using an electric arc smelting furnace to obtain a high-entropy alloy ingot; hardened B 2 O 3 Smashing into small powder blocks as a purifying agent; placing a high-entropy alloy ingot sample to be heat-treated in a quartz glass tube, and paving B on the surface of the sample 2 O 3 Purifying agent, until the purifying agent completely covers the high-entropy alloy ingot sample; and carrying out heat treatment, taking out the sample after the specified heat preservation time is reached, and carrying out quenching treatment to obtain the sample. The alloy structure obtained after the CoCrCuFeNi high-entropy alloy is subjected to heat treatment is obviously spheroidized relative to the second phase in an as-cast state, meanwhile, the magnetic property of the alloy obtained after the CoCrCuFeNi high-entropy alloy is greatly improved, the degree of improvement along with the length of the heat treatment time is different, the method is simple and convenient, and the functional application of the high-entropy alloy is expanded.
Description
Technical Field
The invention belongs to the technical field of high-entropy alloy structure heat treatment methods, and particularly relates to a method for regulating and controlling a CoCrCuFeNi high-entropy alloy structure and magnetism by utilizing heat treatment.
Background
High entropy alloys typically consist of 5 or more than 5 elements in equimolar or near equimolar ratios. High entropy alloys, due to their high mixed entropy values, typically form simple Body Centered Cubic (BCC), face Centered Cubic (FCC), and Hexagonal Close Packed (HCP) structures, exhibiting excellent properties such as high strength, high hardness, good high temperature structure stability and high temperature oxidation resistance, corrosion resistance, excellent magnetic properties, and the like. The high-entropy alloy becomes one of hot spots in the field of metal material research at present, and has wide industrial application prospect and research value.
In the current research on the magnetic performance of high-entropy alloys, the magnetic performance of materials is usually changed by increasing the content of certain ferromagnetic elements, adjusting the content of different phases, applying external fields, and the like. The researchers add Cu element in AlNiCo alloy to improve the alloy coercive force, and add ferromagnetic Fe element to enhance the ferromagnetic exchange effect, thereby promoting the soft magnetic behavior of the alloy.
The CoCrFeNiMn high-entropy alloy with the nano multiphase structure is also prepared by an inert gas condensation method (IGC), compared with other methods, the preparation method enables the Curie temperature of the material to be increased by 10 times, and the formation and the structural evolution of the nano phase can be regulated and controlled through the subsequent annealing process, so that the magnetic performance is improved. In addition, feCoNiAl with excellent soft magnetic performance and corrosion resistance is obtained under the condition of rapid solidification by regulating and controlling the solidification speed of the alloy 0.2 Si 0.2 High entropy alloy. Although the effect of improving the structure and the magnetic property of the high-entropy alloy can be achieved by the method, the experimental period is long and the cost is high, so that a method for improving the magnetic property of the CoCrCuFeNi high-entropy alloy at low cost is urgently needed.
The heat treatment furnace is visible everywhere in factories and laboratories, so that the cost is low, and the experimental operability is strong. At present, the method for improving the performance of the high-entropy alloy by changing the phase change process, the solid solubility of the nano-phase structure and the solid solution and the like through regulating and controlling the heat treatment temperature is gradually observed by researchers.
Based on the method, a method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment is provided.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a method for regulating and controlling the structure and magnetism of a cocrccufeni high-entropy alloy by using heat treatment, so as to solve the problems proposed in the background art.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for regulating and controlling the structure and magnetism of a CoCrCuFeNi high-entropy alloy by utilizing heat treatment comprises the following steps:
s1, taking high-purity simple substance elements as raw materials, uniformly mixing the raw materials in proportion, and pretreating the mixture;
s2, smelting by using an electric arc smelting furnace to obtain a high-entropy alloy cast ingot;
s3, hardening B 2 O 3 Smashing into small powder blocks as a purifying agent;
s4, placing the high-entropy alloy ingot sample to be subjected to heat treatment in a quartz glass tube, and paving B on the surface of the sample 2 O 3 Purifying agent, until the purifying agent completely covers the high-entropy alloy ingot sample;
and S5, placing the quartz glass tube filled with the purifying agent and the high-entropy alloy ingot casting sample in a furnace body of a resistance heating furnace, heating, performing heat preservation treatment, taking out the sample after the specified heat preservation time is reached, and performing quenching treatment to obtain the purifying agent coated sample.
Further, the high-purity elemental elements are specifically solid elemental raw materials of Co, cr, cu, fe, ni, with a purity of 99.95%, and are mixed in an atomic ratio of Co, cr, cu, fe, ni = 1.
Further, the pretreatment is to polish the high-purity elemental raw materials by a grinding wheel machine, remove oxide skin on the surface, perform ultrasonic cleaning for 10min-20min by using alcohol, remove dust and oil stains on the surface of the intermediate alloy, then place the intermediate alloy in a drying box for drying, and place the intermediate alloy in a sample bag for standby after drying.
Further, in S2, the arc melting furnace adopts a non-consumable vacuum arc melting furnace, and high-entropy alloy cast ingots with the mass of about 40-50 g are obtained by melting.
Further, when preparing the high-entropy alloy ingot, firstly wiping the interior of the furnace body of the electric arc melting furnace clean, then putting the raw materials into the melting furnace, keeping the interior of the melting furnace in an atmospheric state at the moment, continuously exhausting and filling argon to keep the interior of the furnace in a vacuum state, finally enabling the interior of the furnace to be vacuumized to be below 0.05MPa, and then filling the furnace body with argon, so that the melting process is in an argon atmosphere, and oxidation in the metal melting process is avoided.
Further, in order to ensure the uniformity of the high-entropy alloy cast ingot, the high-entropy alloy cast ingot is turned and smelted for at least 5 times and more, and finally the button-shaped high-entropy alloy cast ingot is obtained.
Further, hardened B 2 O 3 The size of the small powder block is smaller than the inner diameter of the quartz tube glass, and the sample surface can be covered.
Further, in S5, the temperature rise rate of the resistance heating furnace body during heating is 60K/min, and heat preservation treatment is carried out at 1200 ℃.
Further, the heat preservation treatment time is longer than 2 hours, and the sample is rapidly taken out for quenching treatment after the heat preservation time.
Further, in S4, the size of the high-entropy alloy ingot sample is 4 multiplied by 5mm, and the size of the cut sample is 2 multiplied by 2mm when the magnetic performance test is carried out at the later stage.
Compared with the prior art, the invention has the following advantages:
according to the invention, a high-entropy alloy ingot casting sample is coated by using a purifying agent in an atmospheric environment, the alloy structure obtained after the CoCrCuFeNi high-entropy alloy is subjected to heat treatment is obviously spheroidized relative to the second phase in a casting state, meanwhile, the alloy magnetic property obtained after the CoCrCuFeNi high-entropy alloy is subjected to heat treatment is greatly improved, and the degree of improvement along with the length of heat treatment time is different, so that the method is simple and convenient, and the functional application of the high-entropy alloy is expanded.
Drawings
FIG. 1 is a picture of the texture morphology of a CoCrCuFeNi high-entropy alloy sample after being subjected to heat treatment at 1200 ℃ for 5 hours in an as-cast state in example 1 of the invention, wherein:
(a) Is not subjected to heat treatment and is in an as-cast state;
(b) Heat treatment at 1200 deg.C for 5h.
FIG. 2 is a hysteresis loop of a CoCrCuFeNi high-entropy alloy sample under different conditions in example 1 of the invention, and the test temperature is room temperature.
FIG. 3 is a picture of the structure morphology of a CoCrCuFeNi high-entropy alloy sample after being subjected to heat treatment at 1200 ℃ for 30h in an as-cast state in example 2 of the invention, wherein:
(a) Without heat treatment, as-cast;
(b) Heat treatment at 1200 deg.C for 30h.
FIG. 4 is a hysteresis loop of a CoCrCuFeNi high-entropy alloy sample after heat treatment at 1200 ℃ for 30h in example 2 of the invention, and the test temperature is room temperature.
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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Embodiment 1, the present invention provides a technical solution: a method for regulating and controlling the structure and magnetism of a CoCrCuFeNi high-entropy alloy by using heat treatment comprises the following steps:
s1, selecting high-purity Co, cr, cu, fe and Ni with the purity of 99.95% as raw materials, preparing the raw materials by using an atomic ratio of Co to Cr to Cu to Fe to Ni = 1.
S2, wiping the inside of the vacuum arc melting furnace clean, then putting the raw materials into a crucible of a vacuum induction melting furnace, filling argon into the melting chamber, closing an argon filling valve after the pressure in the furnace reaches 0.05MPa, circulating for three times in such a way to ensure that the gas in the furnace is pure, then starting to melt, and carrying out turnover melting for 5 times to obtain the button-shaped high-entropy alloy ingot casting of 45 +/-2 g.
S3, hardening the pretreated B 2 O 3 And smashing into small powder blocks, wherein the size of each powder block is smaller than the inner diameter of the quartz tube glass, and the powder blocks can be placed in a sample bag for later use after covering the surface of a sample.
S4, covering a layer B prepared in the step S3 on the inner bottom of a quartz glass tube with the outer diameter of 7mm and the inner diameter of 5mm 2 O 3 A purifying agent, a CoCrCuFeNi high-entropy alloy ingot sample with the thickness of 4 multiplied by 5mm is placed in the quartz glass tube, and the purifying agent is paved on the quartz glass tube again, so that the CoCrFeNi high-entropy alloy ingot sample is treated by the purifying agentThe entropy alloy ingot sample is completely coated.
S5, placing the quartz glass tube filled with the purifying agent and the high-entropy alloy ingot casting sample in a furnace body of a resistance heating furnace, carrying out heat preservation treatment after heating at the temperature rising speed of 60K/min, carrying out heat preservation at 1200 ℃ for 5h, quickly taking out the sample after reaching the specified heat preservation time, and carrying out quenching treatment to finally obtain the purifying agent coated sample.
After the surface of a heat-treated CoCrCuFeNi high-entropy alloy sample is wiped clean, grinding and polishing are carried out to observe the microstructure of the sample, then a square block with the size of 2 multiplied by 2mm is cut, and the magnetization curve test of the square block is carried out by PPMS (positive displacement mass spectrometry) and the test temperature is room temperature. The test results are shown in fig. 1 and fig. 2, fig. 1 is a picture of the structure morphology of a CoCrCuFeNi high-entropy alloy sample after being subjected to heat treatment at 1200 ℃ for 5h in an as-cast state, and in the picture: (a) is in an as-cast state without heat treatment; (b) heat treatment at 1200 ℃ for 5h; FIG. 2 is a hysteresis loop of a CoCrCuFeNi high-entropy alloy sample under different conditions, and the test temperature is room temperature.
The result shows that white phase in the CoCrCuFeNi high-entropy alloy structure subjected to heat treatment at 1200 ℃ for 5 hours is spheroidized, and meanwhile, the magnetic property is obviously improved after heat treatment at 1200 ℃ for 5 hours.
s1, selecting high-purity Co, cr, cu, fe and Ni with the purity of 99.95% as raw materials, preparing the raw materials by using an atomic ratio of Co to Cr to Cu to Fe to Ni = 1.
S2, wiping the inside of the vacuum arc melting furnace clean, then putting the raw materials into a crucible of a vacuum induction melting furnace, filling argon into the melting chamber, closing an argon filling valve after the pressure in the furnace reaches 0.05MPa, circulating for three times in such a way to ensure that the gas in the furnace is pure, then starting to melt, and carrying out turnover melting for 5 times to obtain the button-shaped high-entropy alloy ingot casting of 45 +/-2 g.
S3Hardening the pretreated B 2 O 3 And smashing into small powder blocks, wherein the size of each powder block is smaller than the inner diameter of the quartz tube glass, and the powder blocks can be placed in a sample bag for later use after covering the surface of a sample.
S4, paving a layer of B prepared in the step S3 on the inner bottom of a quartz glass tube with the outer diameter of 7mm and the inner diameter of 5mm 2 O 3 The purifying agent is characterized in that a CoCrCuFeNi high-entropy alloy ingot sample with the thickness of 4 multiplied by 5mm is placed in a quartz glass tube, and the purifying agent is paved on the quartz glass tube again, so that the CoCrFeNi high-entropy alloy ingot sample is completely coated by the purifying agent.
S5, placing the quartz glass tube filled with the purifying agent and the high-entropy alloy ingot casting sample in a furnace body of a resistance heating furnace, carrying out heat preservation treatment after heating at the temperature rising speed of 60K/min, carrying out heat preservation at 1200 ℃ for 30h, quickly taking out the sample after reaching the specified heat preservation time, and carrying out quenching treatment to finally obtain the purifying agent coated sample.
After the surface of a heat-treated CoCrCuFeNi high-entropy alloy sample is wiped clean, grinding and polishing are carried out to observe the microstructure of the sample, then a square block with the size of 2 multiplied by 2mm is cut, and the magnetization curve test of the square block is carried out by PPMS (positive displacement mass spectrometry) and the test temperature is room temperature. The test results are shown in fig. 3 and fig. 4, fig. 3 is a picture of the structure morphology of a cocrccufeni high-entropy alloy sample after being subjected to heat treatment at 1200 ℃ for 30h in an as-cast state, wherein: (a) as-cast without heat treatment; (b) heat treatment at 1200 ℃ for 30h; FIG. 4 is a hysteresis loop of a CoCrCuFeNi high-entropy alloy sample after heat treatment at 1200 ℃ for 30 hours, and the test temperature is room temperature.
The result shows that the white phase in the CoCrCuFeNi high-entropy alloy structure which is subjected to heat treatment at 1200 ℃ for 30h is spheroidized, and the size of the spheroidized phase is increased. Meanwhile, after heat treatment for 30 hours of 1200, the magnetic property is obviously improved, and compared with an as-cast state, the magnetic property is improved by 15 times.
Therefore, the heat treatment is directly acted on the CoCrCuFeNi high-entropy alloy to regulate and control the microstructure and the performance of the alloy, and the alloy has the following advantages:
1. the equipment required by the experiment is simple, the experiment period is short, the heat treatment process can be carried out under the condition of glass cladding, and a complex tube sealing process and the like are not needed.
2. The magnetic property can be improved without changing alloy components, the magnetic property of the material can be changed only by heat treatment, the process is simple, the cost is low, and the energy consumption is low.
3. The effect is obvious, the microstructure of the CoCrCuFeNi high-entropy alloy is obviously changed after heat treatment, and the magnetic property is greatly improved.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
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 (7)
1. A method for regulating and controlling the structure and magnetism of a CoCrCuFeNi high-entropy alloy by utilizing heat treatment is characterized by comprising the following steps of:
s1, taking high-purity simple substance elements as raw materials, uniformly mixing the raw materials in proportion, and pretreating the mixture;
s2, smelting by using an electric arc smelting furnace to obtain a high-entropy alloy cast ingot;
s3, hardening B 2 O 3 Smashing into small powder blocks as a purifying agent;
s4, placing the high-entropy alloy ingot sample to be subjected to heat treatment in a quartz glass tube, and paving B on the surface of the sample 2 O 3 Purifying agent, until the purifying agent completely covers the high-entropy alloy ingot sample; said heightThe size of the entropy alloy cast ingot sample is 4 multiplied by 5mm, and the size of the cut sample is 2 multiplied by 2mm when the magnetic performance test is carried out at the later stage;
s5, placing the quartz glass tube filled with the purifying agent and the high-entropy alloy ingot casting sample in a furnace body of a resistance heating furnace, heating to 1200 ℃ at a heating rate of 60K/min for heat preservation treatment for 30h, and quickly taking out the sample for quenching treatment after the heat preservation time is reached to obtain a sample coated with the purifying agent; after heat treatment at 1200 ℃ for 30h, the magnetic property is obviously improved, and compared with an as-cast state, the magnetic property is improved by 15 times.
2. The method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment as claimed in claim 1, wherein the high-purity elemental elements are solid elemental raw materials of Co, cr, cu, fe, ni, co, cr, cu, fe and Ni with the purity of 99.95%, and the high-purity elemental raw materials are mixed in an atomic ratio of Co, cr, cu, fe, ni = 1.
3. The method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment as claimed in claim 1, wherein the pretreatment comprises the steps of polishing a high-purity elemental raw material by a grinding wheel machine, removing oxide skin on the surface, carrying out ultrasonic cleaning for 10min-20min by using alcohol, removing dust and oil stains on the surface of the intermediate alloy, then placing the intermediate alloy in a drying box for drying, and placing the intermediate alloy in a sample bag for later use after drying.
4. The method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment as claimed in claim 1, wherein in S2, an arc melting furnace adopts a non-consumable vacuum arc melting furnace, and a high-entropy alloy ingot with the mass of 40-50g is obtained by melting.
5. The method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment as claimed in claim 4, wherein when preparing the high-entropy alloy ingot, the interior of a furnace body of an electric arc melting furnace is wiped clean, then raw materials are placed into the melting furnace, the melting furnace is in an atmospheric state at the moment, then air is continuously pumped and argon is continuously filled, the furnace is kept in a vacuum state, finally the furnace is vacuumized to be below 0.05MPa, then the furnace body is filled with argon, and the melting process is prevented from being oxidized in the metal melting process under the argon atmosphere.
6. The method for regulating and controlling the structure and magnetism of the CoCrCuFeNi high-entropy alloy according to claim 5, wherein the high-entropy alloy ingot is turned and smelted at least 5 times or more to ensure the uniformity of the high-entropy alloy ingot, and finally the button-shaped high-entropy alloy ingot is obtained.
7. The method for regulating and controlling the structure and the magnetism of the CoCrCuFeNi high-entropy alloy by utilizing heat treatment as claimed in claim 1, wherein the hardened B is hardened 2 O 3 The size of the small powder block is smaller than the inner diameter of the quartz tube glass, and the sample surface can be covered.
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| US20200109467A1 (en) * | 2018-10-04 | 2020-04-09 | City University Of Hong Kong | High entropy alloy structure and a method of preparing the same |
| CN109402482B (en) * | 2018-12-10 | 2022-07-05 | 北京中辰至刚科技有限公司 | Light high-entropy alloy with high strength and high plasticity and preparation method thereof |
| CN110000515A (en) * | 2019-05-24 | 2019-07-12 | 中国矿业大学 | A kind of high-entropy alloy CoCrCuFeNi laser re cast layer and preparation method thereof |
| CN113025865B (en) * | 2021-03-03 | 2021-12-07 | 北方工业大学 | Preparation method of AlCoCrFeNi series two-phase structure high-entropy alloy |
| CN113278861A (en) * | 2021-05-12 | 2021-08-20 | 南昌大学 | High-strength and high-plasticity high-entropy alloy with nanophase precipitation and preparation method thereof |
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