CN115323250A - Process for preparing amorphous nanocrystalline magnetic material - Google Patents
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- CN115323250A CN115323250A CN202210999802.2A CN202210999802A CN115323250A CN 115323250 A CN115323250 A CN 115323250A CN 202210999802 A CN202210999802 A CN 202210999802A CN 115323250 A CN115323250 A CN 115323250A
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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Abstract
The invention relates to the field of magnetic materials, in particular to a preparation process of an amorphous nanocrystalline magnetic material, which comprises the following steps: (1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use; (2) Smelting to obtain a master alloy ingot, and then crushing to obtain crushed materials; (3) carrying out core-cladding treatment on the Si and the composite rare earth by using Al; (4) Putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and obtaining an amorphous alloy strip after rotary quenching treatment; (5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material. According to the invention, si and the composite rare earth are subjected to core-cladding treatment by using Al, and because the Si and the composite rare earth are easy to oxidize, the Si and the composite rare earth are isolated by the core-cladding treatment of Al, the oxidation of the Si and the composite rare earth can be greatly reduced during melting, and the quality of the amorphous nanocrystalline magnetic material is improved, so that the amorphous nanocrystalline magnetic material has high saturation magnetic induction intensity and low coercive force.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a preparation process of an amorphous nanocrystalline magnetic material.
Background
The amorphous magnetic material is a solid material with long-range atomic disorder in structure, ferromagnetism or ferrimagnetism, and is a novel magnetic material which is rapidly developed from 70 s internationally. The amorphous magnetic material is synthesized by the Duwess with the liquid quenching method, and the sensitive functional material is increasingly widely applied nowadays.
In the prior art, when Si and rare earth are added in the preparation of an amorphous nanocrystalline magnetic material, two situations are generally adopted. Firstly, directly smelting Si, rare earth and other components to form a master alloy ingot; secondly, melting Si and other components into a master alloy ingot, and adding rare earth during melting. In the process of adopting the preparation technology, si and rare earth are easy to oxidize, loss is caused, and the overall performance of the amorphous nanocrystalline magnetic material is affected.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process of an amorphous nanocrystalline magnetic material, so as to overcome the problems mentioned in the background technology.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme: a preparation process of an amorphous nanocrystalline magnetic material specifically comprises the following steps:
(1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use.
(2) And repeatedly smelting Fe, cu, mo and Cr in a smelting furnace to obtain a master alloy ingot, and crushing the master alloy ingot to obtain crushed materials.
(3) And (4) carrying out core-covering treatment on the Si and the composite rare earth by using Al to obtain the core-covered wire.
(4) And putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and performing rotary quenching treatment to obtain the amorphous alloy belt.
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material.
Preferably, the magnetic material comprises the following components in percentage by weight: 75% of Fe, 12% of Si, 8% of Al, 1% of Cu, 2% of Mo, 1% of Cr and 1% of composite rare earth.
Preferably, in the step (1), the composite rare earth includes rare earth La and rare earth Ce, wherein the mass ratio of rare earth La to rare earth Ce is 2.2:1.
preferably, in the step (2), during smelting, mo, cr, cu and Fe are sequentially placed on a copper mold of a smelting furnace in sequence, and then smelting is repeatedly performed for 4 times.
Preferably, before smelting, the furnace chamber of the smelting furnace is firstly vacuumized to 4Pa, washed with argon gas for 3 times and then vacuumized to 2 x 10 -3 Pa。
Preferably, in the step (3), before the core-spun treatment, si and the composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
Preferably, in the step (4), the melting temperature in the high-vacuum single-roller rotary quenching furnace is controlled to be 1300-1400 ℃, the injection pressure is controlled to be 0.8-1.2MPa, the distance between the nozzle and the copper roller is adjusted to be 1.5-2mm, and the rotating speed of the copper roller is kept at 35-40m/s.
Preferably, before the copper roller is used for rotary quenching, the rotation speed of the copper roller is controlled to be 2-3m/s, and the copper roller is polished by sand paper with 200 meshes, 500 meshes and 1000 meshes in sequence.
Preferably, in the step (5), the temperature in the heat treatment furnace is controlled to be 480 ℃ and is kept for 100min, then the temperature is increased to 560 ℃ and is kept for 120min, and the primary annealing is completed along with the furnace cooling.
Preferably, the amorphous alloy strip after the primary annealing is reheated to 400 ℃ and kept for 90min, a transverse magnetic field is applied during the heating, the external current is controlled to be 60A, and then the annealing treatment is completed along with furnace cooling.
The invention provides a preparation process of an amorphous nanocrystalline magnetic material, which has the following advantages compared with the prior art:
(1) According to the invention, si and the composite rare earth are subjected to core-cladding treatment by using Al, because the Si and the composite rare earth are easily oxidized, the Si and the composite rare earth are isolated by the core-cladding treatment of Al, the oxidation of the Si and the composite rare earth can be greatly reduced at the beginning of melting, and then the quality of the amorphous nanocrystalline magnetic material is improved, so that the amorphous nanocrystalline magnetic material has high saturation magnetic induction intensity and low coercive force.
(2) By adding Cr and Mo, the binding force of Cr and Mo is higher than that of Cr and Fe, so that Cr is discharged into a residual amorphous phase along with Mo in the growth process of crystal grains, and the growth of the nanocrystalline is facilitated.
(3) The composite rare earth is added, the composite rare earth has stronger affinity to oxygen, and the composite rare earth and the oxygen are preferentially combined to generate a stable compound in an alloy system to be separated out, so that the oxygen concentration in molten steel is obviously reduced, the stability is improved, and the performance of the amorphous nanocrystalline magnetic material can be improved by adding the composite rare earth compared with that of single rare earth.
(4) According to the invention, on the basis of the traditional two-time annealing, the temperature is increased again and the transverse magnetic field is applied to carry out annealing treatment again, so that compared with the traditional two-time annealing, the finally prepared magnetic material has improved overall performance.
Drawings
FIG. 1 is an annealing process diagram of the amorphous nanocrystalline magnetic material of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are described below clearly and completely in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation process of an amorphous nanocrystalline magnetic material specifically comprises the following steps:
(1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use. Wherein the magnetic material comprises the following components in percentage by weight: 75% of Fe, 12% of Si, 8% of Al, 1% of Cu, 2% of Mo, 1% of Cr and 1% of composite rare earth. Specifically, the composite rare earth comprises rare earth La and rare earth Ce, wherein the mass ratio of the rare earth La to the rare earth Ce is 2.2:1.
(2) And repeatedly smelting Fe, cu, mo and Cr in a smelting furnace to obtain a master alloy ingot, and crushing the master alloy ingot to obtain crushed materials. During smelting, sequentially placing Mo, cr, cu and Fe on a copper mold of a smelting furnace in sequence, vacuumizing the furnace chamber of the smelting furnace to 4Pa, washing with argon for 3 times, and vacuumizing to 2 multiplied by 10 -3 Pa, followed by 4 repeated smeltings.
(3) And (3) carrying out core-cladding treatment on the Si and the composite rare earth by using Al to obtain the core-clad wire. Wherein, before the core-spun treatment, si and the composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
(4) And putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and performing rotary quenching treatment to obtain the amorphous alloy belt. Wherein the melting temperature in the high-vacuum single-roller rotary quenching furnace is controlled to be 1300 ℃, the injection pressure is controlled to be 0.8MPa, the distance between the nozzle and the copper roller is adjusted to be 1.5mm, and the rotating speed of the copper roller is kept at 35m/s. Further, before the copper roll was quenched, the rotation speed of the copper roll was controlled to 2m/s, and the copper roll was polished with 200 mesh, 500 mesh, and 1000 mesh sandpaper in this order.
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material. Wherein the temperature in the heat treatment furnace is controlled to be 480 ℃ and is kept for 100min, then the temperature is increased to 560 ℃ and is kept for 120min, and the primary annealing is finished along with the furnace cooling. And reheating the preliminarily annealed amorphous alloy strip to 400 ℃, preserving the heat for 90min, applying a transverse magnetic field during the heating, controlling the applied current to be 60A, and then cooling along with the furnace to finish the whole annealing treatment.
Example 2
A preparation process of an amorphous nanocrystalline magnetic material specifically comprises the following steps:
(1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use. Wherein the magnetic material comprises the following components in percentage by weight: 75% of Fe, 12% of Si, 8% of Al, 1% of Cu, 2% of Mo, 1% of Cr and 1% of composite rare earth. Specifically, the composite rare earth comprises rare earth La and rare earth Ce, wherein the mass ratio of the rare earth La to the rare earth Ce is 2.2:1.
(2) And repeatedly smelting Fe, cu, mo and Cr in a smelting furnace to obtain a master alloy ingot, and crushing the master alloy ingot to obtain crushed materials. During smelting, sequentially placing Mo, cr, cu and Fe on a copper mold of a smelting furnace in sequence, vacuumizing the furnace chamber of the smelting furnace to 4Pa, washing with argon for 3 times, and vacuumizing to 2 multiplied by 10 -3 Pa, and then melting was repeated 4 times.
(3) And (4) carrying out core-covering treatment on the Si and the composite rare earth by using Al to obtain the core-covered wire. Wherein, before the core-spun treatment, si and the composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
(4) And putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and performing rotary quenching treatment to obtain the amorphous alloy belt. Wherein the melting temperature in the high-vacuum single-roller rotary quenching furnace is controlled to be 1400 ℃, the injection pressure is controlled to be 1.2MPa, the distance between the nozzle and the copper roller is adjusted to be 2mm, and the rotating speed of the copper roller is kept at 40m/s. Further, before the spinning with the copper roll, the rotation speed of the copper roll was controlled to 3m/s, and the copper roll was polished with 200 mesh, 500 mesh, and 1000 mesh sandpaper in this order.
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material. Wherein the temperature in the heat treatment furnace is controlled to be 480 ℃ and is kept for 100min, then the temperature is raised to 560 ℃ and is kept for 120min, and the primary annealing is finished along with the furnace cooling. And reheating the preliminarily annealed amorphous alloy strip to 400 ℃, preserving the heat for 90min, applying a transverse magnetic field during the heating, controlling the applied current to be 60A, and then cooling along with the furnace to finish the whole annealing treatment.
Example 3
A preparation process of an amorphous nanocrystalline magnetic material specifically comprises the following steps:
(1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use. Wherein the magnetic material comprises the following components in percentage by weight: 75% of Fe, 12% of Si, 8% of Al, 1% of Cu, 2% of Mo, 1% of Cr and 1% of composite rare earth. Specifically, the composite rare earth comprises rare earth La and rare earth Ce, wherein the mass ratio of the rare earth La to the rare earth Ce is 2.2:1.
(2) And repeatedly smelting Fe, cu, mo and Cr in a smelting furnace to obtain a master alloy ingot, and crushing the master alloy ingot to obtain crushed materials. During smelting, sequentially placing Mo, cr, cu and Fe on a copper mold of a smelting furnace in sequence, vacuumizing the furnace chamber of the smelting furnace to 4Pa, washing with argon for 3 times, and vacuumizing to 2 multiplied by 10 -3 Pa, followed by 4 repeated smeltings.
(3) And (3) carrying out core-cladding treatment on the Si and the composite rare earth by using Al to obtain the core-clad wire. Wherein, before the core-spun treatment, si and the composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
(4) And putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and performing rotary quenching treatment to obtain the amorphous alloy belt. Wherein the melting temperature in the high-vacuum single-roller rotary quenching furnace is controlled to 1350 ℃, the injection pressure is controlled to be 1MPa, the distance between the nozzle and the copper roller is adjusted to be 1.8mm, and the rotating speed of the copper roller is kept to be 36m/s. Further, before the copper roll was quenched, the rotation speed of the copper roll was controlled to 2.5m/s, and the copper roll was polished with 200 mesh, 500 mesh, and 1000 mesh sandpaper in this order.
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material. Wherein the temperature in the heat treatment furnace is controlled to be 480 ℃ and is kept for 100min, then the temperature is increased to 560 ℃ and is kept for 120min, and the primary annealing is finished along with the furnace cooling. And reheating the preliminarily annealed amorphous alloy strip to 400 ℃, preserving the heat for 90min, applying a transverse magnetic field during the heating, controlling the applied current to be 60A, and then cooling along with the furnace to finish the whole annealing treatment.
Comparative example 1
Compared with the embodiment 3, only the steps (2), (3) and (4) are changed in the preparation process of the amorphous nanocrystalline magnetic material, and the specific steps are as follows:
(2) And (2) putting Fe, cu, mo, al and Cr into a smelting furnace for repeated smelting to obtain a master alloy ingot, and then crushing the master alloy ingot to obtain crushed materials. Wherein, during smelting, mo, cr, cu, al and Fe are sequentially placed on a copper die of a smelting furnace according to the sequence,firstly, the furnace chamber of the smelting furnace is vacuumized to 4Pa, and is washed by argon gas for 3 times, and then the furnace chamber is vacuumized to 2 multiplied by 10 -3 Pa, and then melting was repeated 4 times.
(3) Si and composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
(4) And (4) putting the crushed materials and the powder in the step (3) into a high-vacuum single-roller rotary quenching furnace for melting, and performing rotary quenching treatment to obtain the amorphous alloy belt. Wherein the melting temperature in the high-vacuum single-roller rotary quenching furnace is controlled to 1350 ℃, the jetting pressure is controlled to be 1MPa, the distance between the nozzle and the copper roller is adjusted to be 1.8mm, and the rotating speed of the copper roller is kept at 36m/s. Further, before the spinning with the copper roll, the rotation speed of the copper roll was controlled to 2.5m/s, and the copper roll was polished with 200 mesh, 500 mesh, and 1000 mesh sandpaper in this order.
As can be seen from comparison of the detection data of example 3 and this comparative example, the magnetic material subjected to the core-cladding treatment with Al is more excellent than the magnetic material not subjected to the core-cladding treatment, so that the performance of the magnetic material is greatly improved.
Comparative example 2
Compared with example 3, only the composite rare earth is replaced by a single rare earth La.
As can be seen from comparison of the detection data of example 3 and the comparative example, the performance of the magnetic material of example 3 is better than that of the magnetic material of the comparative example compared with the case of only using the rare earth La.
Comparative example 3
Compared with the embodiment 3, only the step (5) is changed in the preparation process of the amorphous nanocrystalline magnetic material, which comprises the following specific steps:
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material. Wherein the temperature in the heat treatment furnace is controlled to be 480 ℃ and is kept for 100min, then the temperature is increased to 560 ℃ and is kept for 120min, and the annealing is completed along with the furnace cooling.
As can be seen from comparison of the test data of example 3 with that of the present comparative example, the performance of the magnetic material after the transverse magnetic field application treatment is superior to that of the conventional magnetic material annealed twice.
Performance detection
1. Saturation magnetic induction: the amorphous nanocrystalline magnetic materials prepared in examples 1-3 and comparative examples 1-3 were tested for saturation induction at room temperature using a Vibrating Sample Magnetometer (VSM). Specific detection results are shown in table 1.
TABLE 1 saturation induction
2. Coercive force: the coercive force of the amorphous nanocrystalline magnetic materials prepared in each of examples 1-3 and comparative examples 1-3 was tested at room temperature using a soft magnetic dc magnetic property measurement system instrument. Specific detection results are shown in table 2.
TABLE 2 coercive force
Group of | Coercive force (A/m) |
Example 1 | 2.2 |
Example 2 | 2.3 |
Example 3 | 2.1 |
Comparative example 1 | 3.6 |
Comparative example 2 | 2.7 |
Comparative example 3 | 2.5 |
3. Residual magnetization: the amorphous nanocrystalline magnetic materials prepared in examples 1-3 and comparative examples 1-3 were tested for remanent magnetization according to the standard of GB/T3217-95. Specific detection results are shown in table 3.
TABLE 3 remanent magnetization
Group of | Remanent magnetization (T) |
Example 1 | 0.23 |
Example 2 | 0.25 |
Example 3 | 0.21 |
Comparative example 1 | 0.65 |
Comparative example 2 | 0.51 |
Comparative example 3 | 0.55 |
It should be noted that, in this document, the terms "comprises", "comprising" or any other variation thereof are intended to cover a non-exclusive inclusion, so that a process, a method, an article or a device including a series of elements includes not only those elements but also other elements not explicitly listed or inherent to such a process, method, article or device. Without further limitation, an element defined by the phrases "comprising a" \8230; "does not exclude the presence of additional like elements in processes, methods, articles or the like that comprise the element.
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation process of an amorphous nanocrystalline magnetic material is characterized by comprising the following steps:
(1) Preparing Fe, si, al, cu, mo, cr and composite rare earth for later use;
(2) Putting Fe, cu, mo and Cr into a smelting furnace for repeated smelting to obtain a master alloy ingot, and then crushing the master alloy ingot to obtain crushed materials;
(3) Carrying out core-spun treatment on the Si and the composite rare earth by using Al to obtain a core-spun yarn;
(4) Putting the crushed materials and the core-spun yarn into a high-vacuum single-roller rotary quenching furnace for melting, and obtaining an amorphous alloy belt after rotary quenching treatment;
(5) And putting the amorphous alloy strip into a heat treatment furnace, and annealing to obtain the amorphous nanocrystalline magnetic material.
2. The process for preparing an amorphous nanocrystalline magnetic material according to claim 1, wherein the magnetic material comprises the following components in percentage by weight: 75% of Fe, 12% of Si, 8% of Al, 1% of Cu, 2% of Mo, 1% of Cr and 1% of composite rare earth.
3. The process for preparing an amorphous nanocrystalline magnetic material according to claim 1, characterized in that: in the step (1), the composite rare earth comprises rare earth La and rare earth Ce, wherein the mass ratio of the rare earth La to the rare earth Ce is 2.2:1.
4. the process according to claim 1, wherein in the step (2), during smelting, mo, cr, cu and Fe are sequentially placed on a copper mold of a smelting furnace in sequence, and then smelting is carried out repeatedly for 4 times.
5. The process of claim 4, wherein the furnace chamber is evacuated to 4Pa, purged with argon for 3 times, and then evacuated to 2X 10 -3 Pa。
6. The process for preparing an amorphous nanocrystalline magnetic material according to claim 1, characterized in that: in the step (3), before the core-spun treatment, si and the composite rare earth are crushed and ground into powder, and the particle size of the powder is controlled to be 0.5-1mm.
7. The process for preparing an amorphous nanocrystalline magnetic material according to claim 1, wherein in the step (4), the melting temperature in the high vacuum single-roller rotary quenching furnace is controlled to be 1300-1400 ℃, the injection pressure is controlled to be 0.8-1.2MPa, the distance between the nozzle and the copper roller is adjusted to be 1.5-2mm, and the rotating speed of the copper roller is kept at 35-40m/s.
8. The process according to claim 7, wherein before the copper roller is rotated and quenched, the rotation speed of the copper roller is controlled to be 2-3m/s, and the surface of the copper roller is polished by 200-mesh, 500-mesh and 1000-mesh sand papers in sequence until the surface of the copper roller is bright and flat.
9. The process according to claim 1, wherein in the step (5), the temperature in the heat treatment furnace is controlled to 480 ℃ and kept for 100min, then the temperature is raised to 560 ℃ and kept for 120min, and the primary annealing is completed after furnace cooling.
10. The process of claim 9, wherein the initially annealed amorphous alloy ribbon is reheated to 400 ℃ and kept at the temperature for 90min, during which a transverse magnetic field is applied, an applied current is controlled to 60A, and then furnace cooling is performed to complete the entire annealing treatment.
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CN110055446A (en) * | 2019-05-23 | 2019-07-26 | 北京乾茂兴业科技发展有限公司 | A kind of wear-resisting spraying powder core wire of iron-based non-crystalline and its preparation |
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