CN113881910B - Method for regulating immiscible alloy structure by using strong magnetic field - Google Patents
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Abstract
The invention discloses a method for regulating and controlling immiscible alloy structure by using a strong magnetic field, which comprises the following steps: cu to be cut 50 Co 50 Putting the immiscible alloy button ingot into a quartz tube, and covering the surface with a material B 2 O 3 (ii) a To be loaded with cut Cu 50 Co 50 Putting a quartz tube of the immiscible alloy button ingot into a uniform magnetic field in a high-intensity magnetic field material processing device, firstly carrying out non-equilibrium solidification processing in a non-magnetic field to obtain a core-shell structure with 180K-300K high supercooling degree, and then carrying out heat treatment on the alloy obtained by the non-equilibrium solidification processing in a 5-10T high-intensity magnetic field again to obtain a homogeneous tissue structure. The invention is to the existing Cu 50 Co 50 The immiscible alloy is treated by a strong magnetic field, the phase composition of the original alloy is not changed by the magnetic field treatment, and the treated Cu 50 Co 50 The microstructure of the immiscible alloy is obviously changed: the alloy directly subjected to solidification treatment is in a segregated core-shell structure, and can be converted into a homogeneous structure after magnetic field heat treatment.
Description
Technical Field
The invention belongs to the technical field of immiscible alloy treatment, and particularly relates to a method for regulating immiscible alloy structure by using a strong magnetic field.
Background
Immiscible alloys, also known as monotectic alloys, exist in a liquid immiscible region during solidification, and when supercooled in this region, liquid phase separation occurs, from a single liquid phase, into two coexisting liquid phases. However, the density difference of two phases in the alloy is usually large, so that serious gravity segregation is often caused, the development and application of the alloy are limited, and if a small number of phases are dispersed and distributed by a proper method or the alloy is prepared into a composite material with a shell/core structure, the immiscible alloy has special physical and mechanical properties, so that the immiscible alloy has good application prospects in all aspects. Therefore, the immiscible alloy has great value in the aspect of theoretical research and huge development potential in the aspect of industrial application, and is a leading hotspot of research in the field of metal materials at present.
Cu-X (X ═ Fe, Co, Cr, Ta, Nb and the like) is a metastable immiscible alloy, when the supercooling degree of an alloy melt is low, the melt undergoes liquid-solid phase change, and X is enriched and is first precipitated in a solid phase. On the contrary, when the supercooling degree of the alloy melt is larger, the single-phase alloy melt is supercooled and enters a metastable component liquid immiscible region to generate liquid-liquid phase separation, and two mutually immiscible liquid phases are generated: a Cu-rich liquid phase (L1) and an X-rich liquid phase (L2). In the cooling process, the gravity field, the concentration gradient, the temperature gradient in the melt, the interphase interface energy, the melt convection and the like all influence the formation of the phase separation alloy solidification structure. In the search literature, an egg-shaped shell-core structure is obtained in Cu-Fe-based alloy by using atomized powder technology. (C.P.Wang.Formation of immiscile Alloy Powders with Egg-Type MicroStructure. science.2002,297: 990-. The phase field method is utilized to simulate the evolution process of the solidification structure of liquid phase separation type alloys such as Fe-Sn-Si, Fe-Sn and the like under the condition of deep undercooling rapid solidification, and researches show that Marangoni convection is a main factor causing the alloy to form a three-layer core-shell structure. (W.L.Wang, Z.Q.Li, B.Wei.macromolecular integration pattern and microstructure feature of terrestrial Fe-Sn-Si immunological compatibility of free surface Condition. acta Mater.2011,59:5482-5493.W.L.Wang, Y.H.Wu, L.H.Li, N.Yan, B.Wei.Homogeneous nuclear microstructure disposed by phase separation and Rapid solubility of liquid Fe-Sn immunological compatibility. J.Alloys. Comp.2017, 693: 650-. The main problem of limiting the application of immiscible alloy at the present stage is that the microstructure segregation is serious, a great deal of research work has been done on the formation mechanism of a core-shell structure, however, the control means of the microstructure is still single, the regulation and control of the microstructure mainly depends on the alloy design, the shapes of solidified alloy are different, the existing research mostly adopts means of controlling the cooling speed, the supercooling degree and the like, but the regulation and control of different types of shapes in the same alloy system are difficult to realize. The prior art has appeared insurmountable bottleneck in the control of immiscible alloy dispersed structure morphology. Therefore, there is a need to find a new method for effectively controlling segregation structure of immiscible alloy.
Disclosure of Invention
In order to solve the problem of structure segregation generated in the traditional preparation process of the immiscible alloy, the invention provides a method for regulating and controlling the structure of the immiscible alloy by using a strong magnetic field.
The high-intensity magnetic field technology is applied to the material metallurgy process to obtain high-quality metal materials, and the method becomes the key research field. The magnetic field has the advantages of non-contact function, non-contact, stability, large energy and the like, and the magnetic field spans from macro level to micro level and can directly influence the arrangement, migration, matching and other behaviors of atoms in the material, so that the micro structure of the material is influenced, the magnetic field technology is applied to the material metallurgy process, the existing technical bottleneck can be broken through, and the novel material processing mode is formed.
Team selection of Cu 50 Co 50 Immiscible alloy is used as a research object, and the alloy is found to be capable of rapidly and effectively dispersing the segregated second phase through strong magnetic field treatment. Studies on Cu-50 at.% Co immiscible alloys have shown that the minority phase particle size distribution in the alloy structure is bimodal without the application of a strong magnetic field. When the magnetic field strength reaches 2T, the size distribution of the second phase droplets is unimodal, and analysis is believed to be due to the strong applied magnetic field weakening the melt convection caused by electromagnetic suspension conditions. Then, under the magnetic field strength of 4T, the Co-rich liquid drops generated in the liquid phase separation process of the Cu-25 at.% Co alloy The size distribution condition is researched, and the proper magnetic field intensity can effectively inhibit the convection of the melt and weaken the structure segregation of the melt. For Cu 50 Co 50 The immiscible alloy acts a strong magnetic field on the solidification process, and utilizes the special advantages of: 1) avoiding the introduction of other doping elements to pollute an alloy system, 2) carrying out the whole experimental process in a room-temperature environment, not needing vacuum protection, having low cost and simple operation, and 3) having obvious effect, and after being treated by a strong magnetic field, Cu is added 50 Co 50 The immiscible alloy is transformed from a core-shell segregation structure to a homogeneous organizational structure, thereby having stronger industrial application prospect.
The invention is realized by the following technical scheme:
the method for regulating and controlling immiscible alloy structure by using the strong magnetic field comprises the following steps:
cu to be cut 50 Co 50 Putting the immiscible alloy button ingot into a quartz tube, and covering the surface with a material B 2 O 3 ；
To be loaded with said cut Cu 50 Co 50 Putting a quartz tube of the immiscible alloy button ingot into a uniform magnetic field in a high-intensity magnetic field material processing device, and applying a magnetic field of 0T; heating-heat preservation-cooling treatment is carried out, the heating-heat preservation-cooling treatment process is circulated for multiple times to obtain the supercooling degree of 180K-300K, and then the Cu is cooled to 950- 50 Co 50 The non-equilibrium solidification treatment process of the immiscible alloy obtains the Cu with the core-shell structure under large supercooling degree 50 Co 50 Immiscible alloy samples;
cu obtained by the non-equilibrium solidification treatment 50 Co 50 Placing the immiscible alloy sample into a uniform magnetic field in the high-intensity magnetic field material processing device, and applying a magnetic field until the strength of the uniform magnetic field reaches 5-10T; heating and heat preservation treatment are carried out, then the sample is taken out quickly and quenched quickly, and the Cu is finished 50 Co 50 Magnetic field heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
As an originalFurther description of the invention, the Cu 50 Co 50 The smelting preparation process of the immiscible alloy button ingot comprises the following steps:
cu and Co are used as raw materials, a vacuum non-consumable arc melting furnace is adopted for melting, and each sample is repeatedly turned over in the melting process for melting for multiple times to ensure that the components of the alloy are uniform, so that Cu is obtained 50 Co 50 Immiscible alloy button ingot.
As a further explanation of the present invention, the Cu: the atomic ratio of Co is 1: 1, and the purity of pure Co and Cu elements is 99.99 wt.%.
As a further illustration of the invention, the incubation temperature of the non-equilibrium solidification treatment is set at 1410-1440 ℃.
As a further illustration of the invention, the incubation time for the non-equilibrium solidification treatment is at least 5 min.
As a further illustration of the invention, the heat preservation temperature of the magnetic field heat treatment is 1280-1370 ℃.
As a further illustration of the invention, the heat preservation time of the magnetic field heat treatment is 6-12 h.
As a further explanation of the invention, the sample is required to be cut, polished and ultrasonically cleaned before being placed in the uniform magnetic field inside the high-intensity magnetic field material processing device.
Specifically, the sample is placed in a uniform magnetic field of an exciting coil inside the high-intensity magnetic field material processing apparatus, and the exciting coil is energized by an exciting power supply to apply a magnetic field.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention is to the existing Cu 50 Co 50 The immiscible alloy is treated by a strong magnetic field, the phase composition of the original alloy is not changed by the magnetic field treatment, and the treated Cu 50 Co 50 The microstructure of the immiscible alloy is obviously changed: the alloy directly subjected to solidification treatment is in a segregated core-shell structure, and can be converted into a homogeneous structure after magnetic field heat treatment.
Drawings
FIG. 1 is a schematic view of the microstructure of an immiscible alloy obtained by the method provided by the present invention;
FIG. 2 shows Cu at 240K supercooling degree obtained under no magnetic field treatment 50 Co 50 The microstructure of the immiscible alloy;
FIG. 3 shows Cu at 290K supercooling degree obtained under magnetic field-free treatment 50 Co 50 The microstructure of the immiscible alloy;
FIG. 4 shows Cu after heat treatment at 1300 ℃ in a 10T magnetic field 50 Co 50 The microstructure of the immiscible alloy;
FIG. 5 is a schematic flow chart of a method for controlling the structure of an immiscible alloy by using a strong magnetic field according to an embodiment of the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a detailed description of the present invention will be given below with reference to the accompanying drawings and specific embodiments. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Fig. 5 is a simplified flow chart of a method for regulating an immiscible alloy structure by using a strong magnetic field according to an embodiment of the present invention, and as shown in fig. 5, the present invention provides a method for regulating an immiscible alloy structure by using a strong magnetic field, including:
Step 1: cu to be cut 50 Co 50 Putting the immiscible alloy button ingot into a quartz tube, and covering the surface with a material B 2 O 3 ；
Step 2: to be loaded with said cut Cu 50 Co 50 Putting a quartz tube of the immiscible alloy button ingot into a uniform magnetic field in a high-intensity magnetic field material processing device, and applying a magnetic field of 0T; performing heating-heat preservation-cooling treatment, and circulating the heating-heat preservation for multiple timesThe temperature-cooling treatment process is carried out to obtain the supercooling degree of 180K-300K, and then the temperature is cooled to 950- 50 Co 50 The non-equilibrium solidification treatment process of the immiscible alloy obtains the Cu with the core-shell structure under large supercooling degree 50 Co 50 Immiscible alloy samples;
and step 3: cu obtained by the non-equilibrium solidification treatment 50 Co 50 Placing the immiscible alloy sample into a uniform magnetic field in the high-intensity magnetic field material processing device, and applying a magnetic field until the strength of the uniform magnetic field reaches 5-10T; heating and heat preservation treatment are carried out, then the sample is taken out quickly and quenched quickly, and the Cu is finished 50 Co 50 Magnetic field heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
In step 1, the Cu 50 Co 50 The smelting preparation process of the immiscible alloy button ingot comprises the following steps:
cu and Co are used as raw materials, wherein Cu: the atomic ratio of Co is 1: 1, converting into mass fraction for batching; the purity of pure Co and Cu elements is 99.99 wt.%.
Smelting by a vacuum non-consumable arc melting furnace, repeatedly turning each sample to smelt for multiple times (for example, 4 times) in the smelting process to ensure that the components of the alloy are uniform, thereby obtaining Cu 50 Co 50 Immiscible alloy button ingot.
In step 1, Cu to be cut 50 Co 50 Before the immiscible alloy button ingot is arranged in the quartz tube, the following cleaning treatment process is carried out:
cutting, polishing and ultrasonically cleaning the button ingot, wherein the mass of each experimental sample is about 2 g. The surface-treated sample was placed in a quartz tube having an inner diameter of 7mm and an outer diameter of 12mm and a length of 600mm, and the surface was covered with a small amount of B 2 O 3 Preventing oxidation.
The non-equilibrium solidification treatment process of the step 2 is specifically as follows:
to be loaded with said cut Cu 50 Co 50 Quartz tube of immiscible alloy button ingotPutting the sample into a high-intensity magnetic field material processing device, and enabling the sample to be in a uniform high-intensity magnetic field of an excitation coil of the device; a magnetic field of 0T is applied.
Heating-heat preservation-cooling treatment process is carried out by a heating power supply according to a programmed rate, the heat preservation temperature is set to be 1410-1440 ℃, the heat preservation time is at least 5min, the heating-heat preservation-cooling treatment process is circulated for a plurality of times to obtain 180-300K of large supercooling degree, and then the temperature is cooled to 950-1000 ℃ to carry out rapid quenching in water to finish the Cu-doped steel 50 Co 50 The non-equilibrium solidification treatment process of the immiscible alloy obtains the Cu with the core-shell structure under large supercooling degree 50 Co 50 Immiscible alloy samples.
The magnetic field heat treatment process of the step 3 is as follows:
the Cu obtained by the non-equilibrium solidification treatment in the step 2 50 Co 50 Placing the immiscible alloy sample into a high-intensity magnetic field material processing device, and electrifying the excitation coil through an excitation power supply to ensure that the intensity of the uniform magnetic field of the excitation coil reaches 5-10T; heating by a heating power supply, setting the heat preservation temperature to 1280-1370 ℃, setting the heat preservation time to 6-12 h, quickly taking out the sample after reaching the heat preservation time, and quickly quenching to finish Cu under a magnetic field 50 Co 50 Magnetic field heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
Preferably, Cu obtained by non-equilibrium solidification treatment 50 Co 50 And cutting the immiscible alloy sample into half parts, polishing and cleaning, and then respectively placing the cut samples into the interior of a high-intensity magnetic field material processing device. The sample is cut into two halves, so that the Cu obtained by the non-equilibrium solidification treatment can be observed more clearly 50 Co 50 Core-shell structure of immiscible alloy.
The following examples are specifically described as preferred embodiments.
Example 1
The embodiment provides a method for regulating and controlling the structure of immiscible alloy by treating the immiscible alloy with a strong magnetic field.
Immiscible solutions as described in this exampleThe alloy being Cu 50 Co 50 The magnetic field intensity used is 0, 5T.
In this example, Cu was controlled by high intensity magnetic field treatment 50 Co 50 The method for preparing the microstructure of the immiscible alloy comprises the following specific processes:
firstly, preparing an alloy: preparing materials, namely selecting Co and Cu with the purity of not less than 99.99 percent; the Co and the Cu are both solid pure raw materials. The Co: 1 of Cu: 1, preparing materials. This ratio is an atomic ratio. Firstly, polishing surface oxide scales of two pure metals on a grinding machine, cleaning, then putting into a copper crucible of a vacuum non-consumable electric arc furnace, adopting a vacuum non-consumable electric arc melting method, and repeatedly turning each sample to melt for 4 times in the melting process to ensure that the components of the alloy are uniform, thereby obtaining the final button ingot.
Step two, sample treatment: the button ingot is cut, polished and ultrasonically cleaned, and the mass of each experimental sample is about 2 g. The cleaned sample is placed in a quartz tube with an inner diameter of 7mm and an outer diameter of 12mm and a length of 600mm, and a small amount of boron trioxide glass is placed on the surface of the sample to prevent oxidation.
Step three, nonequilibrium solidification treatment: fixing the quartz tube filled with the sample by a copper mold clamp, placing the quartz tube into a high-intensity magnetic field treatment device, enabling the sample to be in the highest temperature zone of a heating body, and carrying out solidification treatment on the sample placed in the magnetic field treatment device. The specific process is that a heating power supply is turned on, and a repeated circulation experiment is carried out according to the heating rate, the heat preservation temperature, the heat preservation time and the cooling rate set by the program to finish the Cu 50 Co 50 And (3) solidifying the immiscible alloy. The magnetic field intensity of the uniform magnetic field of the excitation coil is 0T, the excitation coil is heated to the heat preservation temperature of 1425 ℃, the heat preservation time is 5min, the excitation coil is cooled, then repeated circulation is carried out to obtain the large supercooling degree, the supercooling degree is judged to be 190K according to a cooling curve, the excitation coil is cooled to 950 ℃ and quenched in water to obtain Cu 50 Co 50 And (3) solidifying the immiscible alloy under a 0T magnetic field. The microstructure is a core-shell structure.
Fourthly, magnetic field heat treatment: grinding and cleaning the alloy sample subjected to non-equilibrium solidification treatment by half-and-half cutting, and putting the cut sample into a high-intensity magnetic field materialInside the material processing device. Energizing the excitation coil through an excitation power supply to enable the strength of a uniform magnetic field of the excitation coil to reach 5T; setting a liquid-solid two-phase region at the sample heat preservation temperature, heating by a heating power supply and setting a program, wherein the heat preservation temperature is 1370 ℃, the heat preservation time is 8 hours, and quickly taking out the sample for quenching treatment after reaching the heat preservation time so as to finish Cu under a magnetic field 50 Co 50 Heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
Example 2
The embodiment provides a method for regulating and controlling the structure of immiscible alloy by treating the immiscible alloy with a strong magnetic field.
The immiscible alloy in the embodiment is Cu 50 Co 50 The magnetic field intensity used is 0, 5T.
In this example, Cu was controlled by high intensity magnetic field treatment 50 Co 50 The method for preparing the microstructure of the immiscible alloy comprises the following specific processes:
firstly, preparing an alloy: preparing materials, namely selecting Co and Cu with the purity of not less than 99.99 percent; the Co and the Cu are both solid pure raw materials. The Co: 1 of Cu: 1, preparing materials. This ratio is an atomic ratio. Firstly, polishing surface oxide scales of two pure metals on a grinding machine, cleaning, then putting into a copper crucible of a vacuum non-consumable electric arc furnace, adopting a vacuum non-consumable electric arc melting method, and repeatedly turning each sample to melt for 4 times in the melting process to ensure that the components of the alloy are uniform, thereby obtaining the final button ingot.
Step two, sample treatment: the button ingot is cut, polished and ultrasonically cleaned, and the mass of each experimental sample is about 2 g. The cleaned sample is placed in a quartz tube with an inner diameter of 7mm and an outer diameter of 12mm and a length of 600mm, and a small amount of boron trioxide glass is placed on the surface of the sample to prevent oxidation.
Step three, nonequilibrium solidification treatment: fixing the quartz tube filled with the sample by a copper mold clamp, placing the quartz tube into a high-intensity magnetic field treatment device, enabling the sample to be in the highest temperature zone of a heating body, and carrying out solidification treatment on the sample placed in the magnetic field treatment device. The specific process is to beat Starting a heating power supply, and performing repeated circulation experiments according to the heating rate, the heat preservation temperature, the heat preservation time and the cooling rate set by the program to finish the Cu 50 Co 50 And (3) solidifying the immiscible alloy. The magnetic field intensity of the uniform magnetic field of the excitation coil is 0T, the excitation coil is heated to the heat preservation temperature of 1425 ℃, the heat preservation time is 5min, the excitation coil is cooled, then repeated circulation is carried out to obtain the large supercooling degree, the supercooling degree is judged to be 240K according to a cooling curve, the excitation coil is cooled to 950 ℃ and quenched in water to obtain Cu 50 Co 50 And (3) solidifying the immiscible alloy under a 0T magnetic field. The microstructure is a core-shell structure as shown in FIG. 2.
Fourthly, magnetic field heat treatment: and (3) grinding and cleaning the alloy sample subjected to non-equilibrium solidification by half cutting, and putting the cut sample into the high-intensity magnetic field material processing device. Energizing the excitation coil through an excitation power supply to enable the strength of a uniform magnetic field of the excitation coil to reach 5T; setting the sample heat preservation temperature in a liquid-solid two-phase region, heating by a heating power supply and a program, wherein the heat preservation temperature is 1350 ℃, the heat preservation time is 6h, and quickly taking out the sample for quenching treatment after reaching the heat preservation time so as to finish Cu under a magnetic field 50 Co 50 Heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
Example 3
The embodiment provides a method for regulating and controlling the structure of immiscible alloy by treating the immiscible alloy with a strong magnetic field.
The immiscible alloy in the embodiment is Cu 50 Co 50 The magnetic field intensity used was 0, 10T.
In this example, Cu was controlled by high intensity magnetic field treatment 50 Co 50 The method for preparing the microstructure of the immiscible alloy comprises the following specific processes:
firstly, preparing an alloy: preparing materials, namely selecting Co and Cu with the purity of not less than 99.99 percent; the Co and the Cu are both solid pure raw materials. The Co: 1 of Cu: 1, preparing materials. This ratio is an atomic ratio. Firstly, polishing surface oxide scales of two pure metals on a grinding machine, cleaning, then putting into a copper crucible of a vacuum non-consumable electric arc furnace, adopting a vacuum non-consumable electric arc melting method, and repeatedly turning each sample to melt for 4 times in the melting process to ensure that the components of the alloy are uniform, thereby obtaining the final button ingot.
Step two, sample treatment: the button ingot is cut, polished and ultrasonically cleaned, and the mass of each experimental sample is about 2 g. The cleaned sample is placed in a quartz tube with an inner diameter of 7mm and an outer diameter of 12mm and a length of 600mm, and a small amount of boron trioxide glass is placed on the surface of the sample to prevent oxidation.
Step three, nonequilibrium solidification treatment: fixing the quartz tube filled with the sample by a copper mold clamp, placing the quartz tube into a high-intensity magnetic field treatment device, enabling the sample to be in the highest temperature zone of a heating body, and carrying out solidification treatment on the sample placed in the magnetic field treatment device. The specific process is that a heating power supply is turned on, and a repeated circulation experiment is carried out according to the heating rate, the heat preservation temperature, the heat preservation time and the cooling rate set by the program to finish the Cu 50 Co 50 And (3) solidification process of the immiscible alloy. The magnetic field intensity of the uniform magnetic field of the excitation coil is 0T, the excitation coil is heated to the heat preservation temperature of 1425 ℃, the heat preservation time is 5min, the excitation coil is cooled, then repeated circulation is carried out to obtain the large supercooling degree, the supercooling degree is judged to be 180K according to a cooling curve, the excitation coil is cooled to 950 ℃ and quenched in water to obtain Cu 50 Co 50 And (3) solidifying the immiscible alloy under a 0T magnetic field.
Fourthly, magnetic field heat treatment: and (3) grinding and cleaning the alloy sample subjected to non-equilibrium solidification by half cutting, and putting the cut sample into the high-intensity magnetic field material processing device. Energizing the excitation coil through an excitation power supply to enable the strength of a uniform magnetic field of the excitation coil to reach 10T; setting the sample heat preservation temperature in a liquid-solid two-phase region, heating by a heating power supply and setting a program, wherein the heat preservation temperature is 1320 ℃, the heat preservation time is 8h, and quickly taking out the sample for quenching treatment after reaching the heat preservation time so as to finish Cu under a magnetic field 50 Co 50 Heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
Example 4
The embodiment provides a method for regulating and controlling the structure of immiscible alloy by treating the immiscible alloy with a strong magnetic field.
The immiscible alloy in the embodiment is Cu 50 Co 50 The magnetic field intensity used was 0, 10T.
In this example, Cu was controlled by high intensity magnetic field treatment 50 Co 50 The method for preparing the microstructure of the immiscible alloy comprises the following specific processes:
firstly, preparing an alloy: preparing materials, namely selecting Co and Cu with the purity of not less than 99.99 percent; the Co and the Cu are both solid pure raw materials. The Co: 1 of Cu: 1, preparing materials. This ratio is an atomic ratio. Firstly, polishing surface oxide scales of two pure metals on a grinding machine, cleaning, then putting into a copper crucible of a vacuum non-consumable electric arc furnace, adopting a vacuum non-consumable electric arc melting method, and repeatedly turning each sample to melt for 4 times in the melting process to ensure that the components of the alloy are uniform, thereby obtaining the final button ingot.
Step two, sample treatment: the button ingot is cut, polished and ultrasonically cleaned, and the mass of each experimental sample is about 2 g. The cleaned sample is placed in a quartz tube with an inner diameter of 7mm and an outer diameter of 12mm and a length of 600mm, and a small amount of boron trioxide glass is placed on the surface of the sample to prevent oxidation.
Thirdly, nonequilibrium solidification treatment: fixing the quartz tube filled with the sample by a copper mold clamp, placing the quartz tube into a high-intensity magnetic field treatment device, enabling the sample to be in the highest temperature zone of a heating body, and carrying out solidification treatment on the sample placed in the magnetic field treatment device. The specific process is that a heating power supply is turned on, and a repeated circulation experiment is carried out according to the heating rate, the heat preservation temperature, the heat preservation time and the cooling rate set by the program to finish the Cu 50 Co 50 And (3) solidifying the immiscible alloy. The magnetic field intensity of the uniform magnetic field of the excitation coil is 0T, the excitation coil is heated to the heat preservation temperature of 1425 ℃, the heat preservation time is 5min, the excitation coil is cooled, then repeated circulation is carried out to obtain the large supercooling degree, the supercooling degree is judged to be 290K according to a cooling curve, the excitation coil is cooled to 950 ℃ and quenched in water to obtain Cu 50 Co 50 And (3) solidifying the immiscible alloy under a 0T magnetic field. The microstructure is a core-shell structure as shown in FIG. 3.
Fourthly, magnetic field heat treatment: and (3) grinding and cleaning the alloy sample subjected to non-equilibrium solidification by half cutting, and putting the cut sample into the high-intensity magnetic field material processing device. Energizing the excitation coil through an excitation power supply to enable the strength of a uniform magnetic field of the excitation coil to reach 10T; setting the sample heat preservation temperature in a liquid-solid two-phase region, heating by a heating power supply and setting a program, wherein the heat preservation temperature is 1300 ℃, the heat preservation time is 6 hours, and quickly taking out the sample for quenching treatment after reaching the heat preservation time so as to finish Cu under a magnetic field 50 Co 50 Heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 The structure of the immiscible alloy sample is shown in fig. 4.
Experimental test analysis:
cu obtained after different magnetic field heat treatments in example 1, example 3 and example 4 50 Co 50 The immiscible alloy is cold-set in a direction parallel to the magnetic field, and is gradually ground to 2000# sandpaper, and then polished on a polishing machine with a 1.5 # diamond paste at a suitable speed until no scratches appear on the surface. The sample was etched with a formulation of ferric chloride (5g), hydrochloric acid (10ml) and ethanol (100ml) and observed for texture by an OLYMPUS optical microscope (GX 71 type) as shown in fig. 2, 3 and 4. By heat treatment in a magnetic field, Cu 50 Co 50 The microstructure of the immiscible alloy is obviously changed, the solidification microstructure is a typical core-shell structure under the condition of no magnetic field, and the microstructure is changed into a homogeneous structure with second phase dispersion distribution along with the setting of the heat treatment temperature in a liquid-solid two-phase region of the alloy after the magnetic field is applied.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A method for regulating and controlling immiscible alloy structure by utilizing a strong magnetic field is characterized by comprising the following steps:
cu to be cut 50 Co 50 Putting the immiscible alloy button ingot into a quartz tube, and covering the surface with a material B 2 O 3 ；
To be filled with the cut Cu 50 Co 50 Putting a quartz tube of the immiscible alloy button ingot into a uniform magnetic field in a high-intensity magnetic field material processing device, and applying a magnetic field of 0T; heating-heat preservation-cooling treatment is carried out, the heating-heat preservation-cooling treatment process is circulated for multiple times to obtain the supercooling degree of 180K-300K, and then the Cu is cooled to 950- 50 Co 50 The non-equilibrium solidification treatment process of the immiscible alloy obtains the Cu with the core-shell structure under large supercooling degree 50 Co 50 Immiscible alloy samples;
cu obtained by the non-equilibrium solidification treatment 50 Co 50 Placing the immiscible alloy sample into a uniform magnetic field in the high-intensity magnetic field material processing device, and applying a magnetic field until the strength of the uniform magnetic field reaches 5-10T; heating and heat preservation treatment are carried out, then the sample is taken out quickly and quenched quickly, and the Cu is finished 50 Co 50 Magnetic field heat treatment process of immiscible alloy to obtain Cu after magnetic field heat treatment 50 Co 50 Immiscible alloy samples.
2. The method for regulating immiscible alloy structure by using strong magnetic field as claimed in claim 1, wherein the Cu is 50 Co 50 The smelting preparation process of the immiscible alloy button ingot comprises the following steps:
cu and Co are used as raw materials, a vacuum non-consumable arc melting furnace is adopted for melting, and each sample is repeatedly turned over in the melting process for melting for multiple times to ensure that the components of the alloy are uniform, so that Cu is obtained 50 Co 50 Immiscible alloy button ingot.
3. The method for regulating and controlling the structure of the immiscible alloy by utilizing the strong magnetic field as claimed in claim 2, wherein the Cu: the atomic ratio of Co is 1: 1, and the purity of pure Co and Cu elements is 99.99 wt.%.
4. The method for regulating and controlling the structure of the immiscible alloy by utilizing the strong magnetic field as claimed in claim 1, wherein the temperature of the non-equilibrium solidification treatment is set to be 1410-1440 ℃.
5. The method for regulating and controlling the structure of immiscible alloy according to claim 1, wherein the temperature holding time of the non-equilibrium solidification treatment is at least 5 min.
6. The method for regulating and controlling the structure of the immiscible alloy by utilizing the strong magnetic field as claimed in claim 1, wherein the temperature for the heat treatment of the magnetic field is 1280 ℃ to 1370 ℃.
7. The method for regulating and controlling the structure of the immiscible alloy by utilizing the strong magnetic field as claimed in claim 1, wherein the heat preservation time of the magnetic field heat treatment is 6-12 h.
8. The method for regulating and controlling the structure of the immiscible alloy by utilizing the strong magnetic field as claimed in claim 1, wherein the sample is subjected to cutting, grinding and ultrasonic cleaning before being placed in the uniform magnetic field inside the strong magnetic field material processing device.
9. The method for controlling the texture of an immiscible alloy according to claim 1, wherein the sample is placed in a uniform magnetic field of an excitation coil inside the high-intensity magnetic field material processing device, and the excitation coil is energized by an excitation power supply to apply a magnetic field.
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