CN111408726A - Heat treatment process of high-performance wave-absorbing powder with ordered superlattice structure - Google Patents
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- CN111408726A CN111408726A CN202010319492.6A CN202010319492A CN111408726A CN 111408726 A CN111408726 A CN 111408726A CN 202010319492 A CN202010319492 A CN 202010319492A CN 111408726 A CN111408726 A CN 111408726A
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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 technical field of magnetic materials, in particular to a heat treatment process of high-performance wave-absorbing powder with an ordered superlattice structure, which comprises the following steps: s1, selecting a certain amount of Fe-Si-Al raw powder for ball milling treatment; s2, placing the mixture into a vacuum annealing furnace for heating treatment; s3, keeping the temperature for 30min, and extracting air and auxiliaries; s4, raising the temperature to 800-1000 ℃ within 0.5-1 h; s5, keeping the temperature to fully heat the magnetic powder; s6, reducing the temperature to 400-500 ℃; and S7, quenching by using liquid nitrogen and a fan, and rapidly cooling to obtain a finished wave-absorbing powder product. The annealing temperature is higher during heat treatment, the heat preservation temperature is 800-.
Description
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a heat treatment process of high-performance wave-absorbing powder with an ordered superlattice structure.
Background
With the rapid development of electronic information technology, high frequency, miniaturization and surface mounting of electronic components bring about serious EMI (electromagnetic interference) problems. The soft magnetic material is widely applied to filtering, noise suppression and near-field and far-field wave absorption. Soft magnetic materials can be classified into soft magnetic ferrites and soft magnetic alloys. The ferrite has lower resonance frequency and sharply reduced magnetic permeability after passing the resonance frequency point due to the limitation of Snoek limit, while the soft magnetic alloy has high saturation magnetization and large initial magnetic permeability, but has high electric conductivity and is limited by skin depth, and the high-frequency magnetic permeability is poor when the soft magnetic alloy is used as a block body alone. The soft magnetic alloy powder is mixed with thermoplastic resin to prepare a flexible composite material in a flattening mode, can effectively inhibit the generation of high-frequency eddy current, improves the magnetic conductivity, and is applied to the field of electromagnetic compatibility.
In the traditional annealing process, the heat treatment temperature is 650 ℃, the temperature is kept for 2 hours, and then the annealing process is cooled along with the furnace. Because the powder particles are small, gaps exist among partial powder, the powder belongs to radiation heat transfer during heating, the temperature rise is slow, the process can not ensure that the powder is completely heated, the annealing temperature is low, the recrystallized grains are difficult to grow, and the order degree is small.
Therefore, the invention provides a heat treatment process for a high-performance electromagnetic wave absorbent with an ordered superlattice structure, researches the relationship of different heat treatment processes on the phase structure and stress distribution of the electromagnetic wave absorbent, finds a proper heat treatment process, improves the order degree, reduces the coercive force and obtains the optimal magnetic performance.
Disclosure of Invention
The invention aims to solve the defects that the powder cannot be completely heated, recrystallized grains are difficult to grow up and the degree of order is small in the prior art, and provides a heat treatment process of high-performance wave-absorbing powder with an ordered superlattice structure.
In order to achieve the purpose, the invention adopts the following technical scheme:
a heat treatment process of high-performance wave-absorbing powder with an ordered superlattice structure comprises the following steps:
s1, selecting a certain amount of Fe-Si-Al raw powder, and putting the Fe-Si-Al raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace and heating to 400-500 ℃;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out the air in the furnace and the auxiliary agents added during ball milling;
s4, continuing to heat the powder, and raising the temperature within 0.5-1 h;
s5, keeping the temperature in the step S4, keeping the temperature, heating the magnetic powder fully, performing recrystallization annealing, increasing the volume of recrystallized grains, and improving the degree of order of the powder;
s6, reducing the temperature to 400-500 ℃ to obtain more DO3 ordered structures in the powder;
and S7, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, keeping the DO3 ordered superlattice structure to a room temperature state, and discharging to obtain a finished wave-absorbing powder product.
Preferably, the vacuum degree in the vacuum furnace in the S2 step is less than 0.008mBar, and the heating time is 0.5-1h
Preferably, the boiling point of the auxiliary agent in the step S3 is 250 ℃.
Preferably, the temperature of the temperature rise in the step S4 is 800-1000 ℃.
Preferably, the heat preservation time in the step of S5 is 2-3 h.
Preferably, the cooling rate in the step of S6 is less than 150 ℃/h.
Preferably, the cooling rate in the step of S7 is greater than 350 ℃/h.
The invention has the beneficial effects that:
1. the annealing temperature is higher during heat treatment, the heat preservation temperature is 800-.
2. The invention increases the heat preservation time in the heat treatment process, the heat preservation time is more than 2h, the powder can be ensured to be completely recrystallized, larger recrystallized grains can be obtained, the degree of order is increased, and the magnetic property of the powder is improved.
3. The invention adopts a cooling mode of first slow cooling and then fast cooling, the temperature is firstly slow cooled from 800-plus-one temperature of 1000 ℃ to below 600 ℃, and then the temperature is fast cooled to below 100 ℃ by time quenching, so that the obvious DO3 ordered superlattice structure can be obtained.
Drawings
FIG. 1 is a schematic flow chart of a heat treatment process of a high-performance wave-absorbing powder with an ordered superlattice structure provided by the invention;
FIG. 2 is a schematic diagram of powder magnetic permeability at different annealing temperatures in the embodiment of the present invention;
FIG. 3 is a schematic diagram of powder magnetic permeability at different holding times in the embodiment of the present invention;
FIG. 4 is a schematic diagram of powder magnetic permeability in different cooling modes in the embodiment of the present invention;
FIG. 5 is a schematic diagram of the morphology of the powder before annealing in the embodiment of the invention;
FIG. 6 is a schematic diagram illustrating the morphology of the annealed powder in the embodiment of the present invention;
FIG. 7 is a schematic comparison of ordered structures of DO3 before and after heat treatment as proposed by the present invention.
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.
Embodiment 1, a heat treatment process of a high-performance wave-absorbing powder with an ordered superlattice structure, comprising the following steps:
s1, selecting 100-mesh Fe-Si-Al raw powder, and putting the raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace, and heating to 400 ℃, wherein the vacuum degree in the vacuum annealing furnace is 0.007mBar, and the heating time is 0.5 h;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out air in the furnace and the auxiliary agent added during ball milling, wherein the boiling point of the auxiliary agent is 250 ℃;
s4, continuously heating the powder, and raising the temperature to 800 ℃ within 0.5 h;
s5, keeping the temperature in the step S4 for 2 hours, fully heating the magnetic powder, performing recrystallization annealing, increasing the volume of recrystallized grains, and improving the degree of order of the powder;
s6, reducing the temperature to 400 ℃, wherein the temperature reduction rate is 140 ℃/h, so that more DO3 ordered structures are obtained in the powder;
and S7, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, keeping the DO3 ordered superlattice structure at the room temperature state at the speed of 360 ℃/h, and discharging to obtain the wave-absorbing powder finished product I.
Embodiment 2, a heat treatment process of a high-performance wave-absorbing powder with an ordered superlattice structure, comprising the following steps:
s1, selecting 100-mesh Fe-Si-Al raw powder, and putting the raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace, and heating to 450 ℃, wherein the vacuum degree in the vacuum annealing furnace is 0.007mBar, and the heating time is 0.8 h;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out air in the furnace and the auxiliary agent added during ball milling, wherein the boiling point of the auxiliary agent is 250 ℃;
s4, continuously heating the powder, and heating to 900 ℃ within 0.8 h;
s5, keeping the temperature in the step S4 for 2.5 hours, fully heating the magnetic powder, and carrying out recrystallization annealing to increase the volume of recrystallized grains and improve the degree of order of the powder;
s6, reducing the temperature to 450 ℃, wherein the temperature reduction rate is 140 ℃/h, so that more DO3 ordered structures are obtained in the powder;
and S7, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, keeping the DO3 ordered superlattice structure at the room temperature state at the speed of 360 ℃/h, and discharging to obtain a wave-absorbing powder finished product II.
Embodiment 3, a heat treatment process of a high-performance wave-absorbing powder with an ordered superlattice structure, comprising the following steps:
s1, selecting 100-mesh Fe-Si-Al raw powder, and putting the raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace, and heating to 500 ℃, wherein the vacuum degree in the vacuum annealing furnace is 0.007mBar, and the heating time is 1 h;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out air in the furnace and the auxiliary agent added during ball milling, wherein the boiling point of the auxiliary agent is 250 ℃;
s4, continuously heating the powder, and raising the temperature to 1000 ℃ within 1 h;
s5, keeping the temperature in the step S4 for 3 hours, fully heating the magnetic powder, performing recrystallization annealing, increasing the volume of recrystallized grains, and improving the degree of order of the powder;
s6, reducing the temperature to 500 ℃, wherein the temperature reduction rate is 140 ℃/h, so that more DO3 ordered structures are obtained in the powder;
and S7, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, keeping the DO3 ordered superlattice structure at the room temperature state at the speed of 360 ℃/h, and discharging to obtain a wave-absorbing powder finished product III.
The heat treatment process of the high-performance wave-absorbing powder with the ordered superlattice structure comprises the following steps of:
s1, selecting 100-mesh Fe-Si-Al raw powder, and putting the raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace, and heating to 500 ℃, wherein the vacuum degree in the vacuum annealing furnace is 0.007mBar, and the heating time is 1 h;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out air in the furnace and the auxiliary agent added during ball milling, wherein the boiling point of the auxiliary agent is 250 ℃;
s4, continuously heating the powder, and heating to 600 ℃ within 1 h;
s5, keeping the temperature in the step S4 for 3 hours, fully heating the magnetic powder, performing recrystallization annealing, increasing the volume of recrystallized grains, and improving the degree of order of the powder;
and S6, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, wherein the temperature reduction rate is 360 ℃/h, and discharging to obtain a wave-absorbing powder finished product IV.
And detecting the four wave-absorbing powder finished products, wherein the detection results are as follows:
the method has the advantages that the annealing temperature and the heat preservation time are increased, the cooling mode of the powder is changed, the powder can be uniformly heated, the magnetic performance of a finished product is improved, the powder is completely recrystallized, larger recrystallized grains are obtained, the degree of order is increased, the magnetic performance of the powder is improved, and an obvious DO3 ordered superlattice structure can be obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A heat treatment process of high-performance wave-absorbing powder with an ordered superlattice structure is characterized by comprising the following steps:
s1, selecting a certain amount of Fe-Si-Al raw powder, and putting the Fe-Si-Al raw powder into a high-energy ball mill for flaking treatment to obtain flaky powder;
s2, putting the flaky powder obtained in the step S1 into a vacuum annealing furnace and heating to 400-500 ℃;
s3, keeping the temperature in the step S2, heating for 30min, and pumping out the air in the furnace and the auxiliary agents added during ball milling;
s4, continuing to heat the powder, and raising the temperature within 0.5-1 h;
s5, keeping the temperature in the step S4, keeping the temperature, heating the magnetic powder fully, performing recrystallization annealing, increasing the volume of recrystallized grains, and improving the degree of order of the powder;
s6, reducing the temperature to 400-500 ℃ to obtain more DO3 ordered structures in the powder;
and S7, quenching by using liquid nitrogen and a fan, reducing the temperature to 80 ℃, keeping the DO3 ordered superlattice structure to a room temperature state, and discharging to obtain a finished wave-absorbing powder product.
2. The heat treatment process of the high-performance wave-absorbing powder with the ordered superlattice structure as claimed in claim 1, wherein the vacuum degree in the vacuum furnace in the step S2 is less than 0.008 mBar.
3. The heat treatment process of the ordered superlattice structure high-performance wave-absorbing powder as claimed in claim 1, wherein the boiling point of the auxiliary agent in the step S3 is 250 ℃.
4. The heat treatment process for the ordered superlattice structured high-performance wave-absorbing powder as claimed in claim 1, wherein the temperature rise in the step S4 is 800-1000 ℃.
5. The heat treatment process of the high-performance wave-absorbing powder with the ordered superlattice structure as claimed in claim 1, wherein the heat preservation time in the step S5 is 2-3 h.
6. The heat treatment process of the high-performance wave-absorbing powder with the ordered superlattice structure as claimed in claim 1, wherein the cooling rate in the step S6 is less than 150 ℃/h.
7. The heat treatment process of the high-performance wave-absorbing powder with the ordered superlattice structure as claimed in claim 1, wherein the cooling rate in the step S7 is greater than 350 ℃/h.
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CN112207283A (en) * | 2020-10-22 | 2021-01-12 | 合肥工业大学 | Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112207283A (en) * | 2020-10-22 | 2021-01-12 | 合肥工业大学 | Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology |
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Application publication date: 20200714 |