CN109754979B - Multilayer coated soft magnetic composite material and preparation method thereof - Google Patents
Multilayer coated soft magnetic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a multilayer coated soft magnetic composite material and a preparation method thereof. The compoundThe composite material is of a core-shell structure, takes iron-based alloy powder as a core, and is sequentially coated with a passivation layer and Al on the surface of the iron-based alloy powder2O3And (4) coating. The preparation method comprises the following steps: reacting iron-based alloy powder in a passivation solution to obtain powder A; preparation of Al2O3A colloid; powder A, Al2O3Performing colloid ball milling reaction; and (3) calcining the ball-milled powder at high temperature to obtain the multilayer coated soft magnetic composite material with high magnetic conductivity and low loss. Compared with the prior art, the invention has the advantages that the composite material has lower magnetic loss under the condition of high-frequency application by coating the insulating substance with high resistivity in multiple layers, and the insulating coating layer with better uniformity and accurately controllable thickness can be obtained; al (Al)2O3The sol-gel has strong thermal stability, can improve the density of magnetic powder to the maximum extent and improve the magnetic conductivity of the magnetic powder.
Description
Technical Field
The invention relates to a soft magnetic composite material in the field of functional materials, in particular to a multilayer coated soft magnetic composite material and a preparation method thereof.
Background
With the rapid development of electronic information technology, people have developed the development requirements of miniaturization, intellectualization, high integration and high-energy and high-power input for various electronic components. SMCs, which are one of core materials of electromagnetic conversion devices, are required to be developed toward high Bs, high Ms, high Tc, low Pc, low Hc, high frequency, miniaturization, and thinning. The iron-based soft magnetic composite material is a metal soft magnetic composite material with high cost performance, and has wide application space in the fields of power factor correction circuits, pulse flyback transformers, energy storage filter inductors, line filters and the like. But eddy current losses increase with increasing frequency of its application. Eddy current losses cause a significant heating of the magnetic core, thereby reducing the associated magnetic properties of the soft magnetic composite material. Statistically, about 9% of the power loss is due to joule heat generated in the electromagnetic conversion. Therefore, how to reduce the eddy current loss and develop an energy-saving iron-based soft magnetic composite material is a hotspot and difficulty of current research.
Generally, the main measures for reducing the eddy current loss of the soft magnetic composite material are to block the eddy current conduction path between magnet particles and increase the resistivity of the material itself, and generally, magnetic powder is mixed with an insulating agent, the magnetic powder is isolated by an insulating coating agent, the conduction path between the magnetic powder is blocked, and the rho value of the soft magnetic composite material is increased, so that the eddy current loss is reduced. The insulating agent is generally divided into an organic insulating material and an inorganic insulating material, wherein the organic material has larger resistivity and lower magnetic loss, but the organic matter has low thermal stability, can be aged and decomposed at overhigh temperature and can only be used at lower temperature, and the organic insulating material mainly comprises epoxy organic silicon resin, acrylic resin and polyester. The inorganic material mainly comprises Al2O3、MgO、SiO2And the like, which have high resistivity, can effectively reduce magnetic loss, have high thermal stability and can stand high temperature, but the self-material is a non-magnetic material and can reduce the magnetic performance of the composite material, such as Ms, Bs and the like. In order to ensure good magnetic properties of SMCs, therefore, ferrites having a large specific resistance come into the sight of researchers, Mn — Zn ferrites, Ni — Zn ferrites, and the like are all used as coating materials, but ferrites are difficult to be uniformly coated on the surface of magnetic powder, and thus eddy current loss thereof is large.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a multi-layer coated soft magnetic composite material and a preparation method thereof. The multilayer coated soft magnetic composite material has high magnetic conductivity, low loss and excellent comprehensive magnetic performance, and the preparation process of the soft magnetic composite material has implementation property.
The purpose of the invention can be realized by the following technical scheme:
a multilayer coated soft magnetic composite material is of a core-shell structure, iron-based alloy powder is taken as a core, and a passivation layer and Al are sequentially coated on the surface of the iron-based alloy powder2O3And (4) coating.
The passivation layer is a metal salt layer generated by the reaction of iron-based alloy powder and a passivating agent, and the passivating agent is phosphoric acid, nitric acid or glacial acetic acid.
The iron-based alloy powder includes Fe powder.
The preparation method of the multilayer coated soft magnetic composite material comprises the following steps:
(a) reacting the iron-based alloy powder in a passivation solution to obtain powder A, namely passivation powder;
(b) preparation of Al2O3A colloid;
(c) powder A, Al2O3Performing colloid ball milling reaction;
(d) and calcining the ball-milled powder at high temperature to obtain multilayer coated powder, namely the multilayer coated soft magnetic composite material.
Further, step (d) is followed by step (e) and step (f),
(e) the method comprises the following steps Pressing the coated powder in the step (d) into a magnetic core;
(f) the method comprises the following steps Heat treating the magnetic core obtained in the step (e).
The particle size of the iron-based alloy powder is 100-200 um, the iron-based alloy powder comprises Fe powder, the passivation solution is a mixed solution of a passivator and alcohol, the passivator is phosphoric acid, nitric acid or glacial acetic acid, and the volume ratio of the passivator to the alcohol is 0.6-1.2: 98.8-99.4; the adding amount ratio of the iron-based alloy powder to the passivation solution is 40-60 g: 15-25 ml. The reaction conditions of the iron-based alloy powder in the passivation solution are as follows: stirring the iron-based alloy powder in a passivation solution in a constant-temperature water bath kettle at 65 ℃ until the solution is completely evaporated to dryness to obtain powder A.
The Al is2O3The preparation of the colloid comprises the following steps: mixing aluminum isopropoxide and ethylene glycol ethyl ether, stirring, adding acetylacetone, stirring, raising the temperature of the mixed system, adding acetic acid, continuing stirring, evaporating, cooling to room temperature, and obtaining a clear transparent substance, namely Al2O3The colloid is a precursor.
The adding amount ratio of the aluminum isopropoxide to the ethylene glycol monoethyl ether to the acetylacetone to the acetic acid is 2.1-4.5 g: 40-60 ml: 1-3 g: 5-15 ml.
Mixing aluminum isopropoxide and ethylene glycol ethyl ether, magnetically stirring at 60 ℃ for 30min, adding acetylacetone, magnetically stirring at 60 ℃ for 30min, raising the temperature of the mixed system to 80 ℃, adding acetic acid, continuously magnetically stirring for 30min, evaporating, and cooling to room temperature.
The conditions of the ball milling reaction are as follows: powder A, Al2O3Adding the colloid into a ball milling tank, mixing, uniformly stirring, adding steel balls, and putting into a ball mill for ball milling, wherein the time for spheroidal graphite is 10-20 min, and the rotating speed is 100-150 rap/min;
the high-temperature calcination conditions are as follows: keeping the temperature at 600 ℃ for 30 min.
The pressing conditions are as follows: pressing under the condition of 800MP-1000MP,
the conditions of the heat treatment are as follows: under the condition of inert gas, heat treatment is carried out at 500-700 ℃ for 0.5-2h to reduce the residual stress generated in the pressing process.
Further, the present invention provides a specific preparation process comprising the following steps, wherein the following steps are characterized by a certain amount of numerical values, and the process of the present invention can be reproduced by the enlargement of the same proportion.
(1) Weighing a certain amount of Fe powder, and putting the Fe powder into a beaker;
(2) respectively measuring a certain amount of passivant and alcohol, and slowly adding the passivant into the alcohol to prepare a passivation solution with a certain concentration;
(3) weighing a certain volume of passivation solution, adding the passivation solution into a beaker, putting the beaker into a constant-temperature water bath kettle at 65 ℃, and stirring until the solution is completely evaporated to dryness to obtain powder A;
the preparation of the Al2O3 colloid comprises the following steps:
(4) weighing a certain amount of aluminum isopropoxide (grinding), and putting the ground aluminum isopropoxide into a beaker A after weighing;
(5) measuring a certain amount of ethylene glycol ethyl ether by a measuring cylinder, adding the ethylene glycol ethyl ether into a beaker A, and magnetically stirring for 30min at 60 ℃;
(6) measuring a certain amount of acetylacetone by a measuring cylinder, slowly adding into a beaker A, and magnetically stirring for 30min at 60 ℃;
(7) measuring a certain amount of acetic acid, heating to 80 deg.C, adding at one time, stirring for 30min, and evaporating to 60-65 ml;
(8) cooling to room temperature, and obtaining a clear and transparent precursor B;
the multilayer cladding soft magnetic composite material comprises the following steps:
(9) weighing a certain amount of powder A and a certain volume of precursor B, adding the powder A and the precursor B into a ball milling tank, mixing, uniformly stirring, adding steel balls, and putting the mixture into a ball mill for ball milling, wherein the ball milling time is 10-20 min, and the rotating speed is 100-150 rap/min;
(10) putting the ball-milled powder into a tube furnace, and preserving the heat for 30min at the temperature of 600 ℃ to obtain multilayer coated powder;
(11) pressing the coated powder in the step 10) into a magnetic core under the condition of 800MP-1000 MP;
(12) under the condition of inert gas, the heat treatment temperature is 500-700 ℃ for heat treatment for 0.5-2h, so as to reduce the residual stress generated in the pressing process.
In the step (1), the particle size of the iron powder is 100-200 um, and the weight of the weighed Fe powder is 40-60 g.
In the step (2), the passivating agent is phosphoric acid, nitric acid or glacial acetic acid, the volume of the measured passivating agent is 0.6-1.2 ml, and the volume of the alcohol is 98.8-99.4 ml. Preferably, the passivating agent is phosphoric acid, and the concentration of the passivating solution is 0.01 g/ml-0.2 g/ml, preferably 0.012 g/ml;
in the step (3), the volume of the passivation solution is 15-25 mL, and preferably, in the step (3), the ratio of the volume of the passivation solution to the mass of the iron powder is 2-3 g/mL, and preferably 2.5 g/mL.
In the step (4), the mass of the aluminum isopropoxide is 2.1-4.5 g, preferably 4.0048 g.
In the step (5), the volume of the ethylene glycol ethyl ether is measured to be 40-60 ml, preferably 50 ml.
In the step (6), the mass of acetylacetone is weighed to be 1-3 g, preferably 2.0048 g.
In the step (7), the volume of the acetic acid is measured to be 5-15 ml, preferably 10 ml.
Preferably, in the step (4), the inert gas atmosphere is argon or nitrogen.
The invention takes the improvement of magnetic conductivity, the reduction of loss, the optimization and the improvement of the magnetic performance of the soft magnetic composite material as the starting point, takes iron-based alloy powder as the raw material, and respectively adopts the passivating agent passivation and the chemical cladding method to prepare the passivation layer/Al2O3The iron-based alloy core-shell structure powder is coated in a double-layer mode, and then the composite powder is sintered at a high temperature to prepare the high-density iron-based composite soft magnetic composite material with high resistivity, low loss and inter-particle insulation. Due to the single phosphoric acid passivation layer or Al2O3The insulating layer of the magnetic powder of the coating layer is likely to break under high pressure, and the integrity of the insulating layer is reduced, so that the magnetic performance of the magnetic powder core is reduced; the magnetic powder with the phosphatized double-layer coating layer can firstly destroy the structural integrity of the outer insulating layer under high pressure, the inner insulating layer still keeps complete, eddy current can be effectively blocked, eddy current loss is reduced, and the insulating coating layer with better uniformity and accurately controllable thickness can be obtained by a chemical coating method and phosphoric acid passivation. In addition, the density of the magnetic powder property can be improved to the maximum extent by adopting high-temperature sintering treatment, and the magnetic conductivity of the magnetic powder property is improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts chemical coating and passivation technology to obtain the insulating coating layer with better uniformity and accurately controllable thickness, and can effectively improve the heat treatment temperature.
(2) The invention can bear higher compression pressure and effectively relieve a single passivation layer or Al2O3The insulating layer of the coated magnetic powder may be broken under a high pressing force, thereby reducing the magnetic properties of the magnetic powder core.
(3) The invention has lower eddy current loss without affecting the excellent magnetic performance of the soft magnetic composite material.
Drawings
FIG. 1 is a graph of loss versus frequency for the material made in example 1;
FIG. 2 is a graph of the real part of permeability versus frequency for the material prepared in example 2;
FIG. 3 is a graph of the imaginary part of permeability versus frequency for the material made in example 2;
FIG. 4 is a graph of magnetic loss versus frequency for the material made in example 2.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The invention provides the following specific implementation scheme, discloses examples with different reaction temperatures and reaction times, and contrasts and analyzes the performances under different reaction temperatures and reaction times. Therefore, it is considered that this patent specifically states all possible ways of coating that the solution described is disclosed.
Example 1:
a method for preparing a multilayer coated soft magnetic composite material comprises the following steps:
(1) weighing 50g of Fe powder, and putting the Fe powder into a beaker;
(2) respectively measuring 0.7ml of phosphoric acid and 99.3ml of alcohol, and slowly adding a passivating agent into the alcohol to prepare a passivating solution with the concentration of 0.012 g/ml;
(3) weighing 15ml of phosphoric acid passivation solution, adding the solution into a beaker, putting the beaker into a constant-temperature water bath kettle at 65 ℃, and stirring until the solution is completely evaporated to dryness to obtain powder A;
the Al is2O3The preparation of the colloid comprises the following steps:
(4) 4.0048g of aluminum isopropoxide is weighed (ground), and the weighed aluminum isopropoxide is placed into a beaker A;
(5) measuring 50ml of ethylene glycol ethyl ether in a measuring cylinder, adding the ethylene glycol ethyl ether into a beaker A, and magnetically stirring the mixture for 30min at the temperature of 60 ℃;
(6) 2.0024g of acetylacetone is weighed and slowly added into a beaker A, and magnetic stirring is carried out for 30min at 60 ℃;
(7) measuring 10ml of acetic acid, raising the temperature to 80 ℃, adding the acetic acid at one time, continuously stirring for 30min, and evaporating to 60-65 ml;
(8) cooling to room temperature, and obtaining a clear and transparent precursor B;
the multilayer cladding soft magnetic composite material comprises the following steps:
(9) adding 10g of the powder A and 0.03g of the precursor B into a ball milling tank for mixing, uniformly stirring, adding steel balls, and putting into a ball mill for ball milling, wherein the ball milling time is 10-20 min, and the rotating speed is 100-150 rap/min;
(10) putting the ball-milled powder into a tube furnace, and preserving the heat for 30min at the temperature of 600 ℃ to obtain multilayer coated powder;
(11) pressing 3.5g of the coating powder in the step 10) into a magnetic core with the outer diameter of 20mm, the inner diameter of 12mm and the thickness of 2.5mm under the condition of 800 MP;
(12) and (3) carrying out heat treatment for 0.5h at the heat treatment temperature of 600 ℃ under the inert gas condition to reduce the residual stress generated in the pressing process.
The above prepared sample was tested as follows:
and (3) measuring magnetic performance parameters such as magnetic permeability, magnetic loss and the like of the sample by adopting an MATS-2010SA soft magnetic material dynamic measuring device (LCR meter for short).
The loss of the material prepared in example 1 is shown in fig. 1.
Example 2:
a method for preparing a multilayer coated soft magnetic composite material comprises the following steps:
(1) weighing 50g of Fe powder, and putting the Fe powder into a beaker;
(2) respectively measuring 0.7ml of nitric acid and 99.3ml of alcohol, and slowly adding a passivating agent into the alcohol to prepare a passivating solution with the concentration of 0.012 g/ml;
(3) weighing 15ml of nitric acid passivation solution, adding the nitric acid passivation solution into a beaker, putting the beaker into a constant-temperature water bath kettle at 65 ℃, and stirring until the solution is completely evaporated to dryness to obtain powder A;
the Al is2O3The preparation of the colloid comprises the following steps:
(4) 4.0048g of aluminum isopropoxide is weighed (ground), and the weighed aluminum isopropoxide is placed into a beaker A;
(5) measuring 50ml of ethylene glycol ethyl ether in a measuring cylinder, adding the ethylene glycol ethyl ether into a beaker A, and magnetically stirring the mixture for 30min at the temperature of 60 ℃;
(6) 2.0024g of acetylacetone is weighed and slowly added into a beaker A, and magnetic stirring is carried out for 30min at 60 ℃;
(7) measuring 10ml of acetic acid, raising the temperature to 80 ℃, adding the acetic acid at one time, continuously stirring for 30min, and evaporating to 60-65 ml;
(8) cooling to room temperature, and obtaining a clear and transparent precursor B;
the multilayer cladding soft magnetic composite material comprises the following steps:
(9) adding 10g of the powder A and 0.03g of the precursor B into a ball milling tank for mixing, uniformly stirring, adding steel balls, and putting into a ball mill for ball milling, wherein the ball milling time is 10-20 min, and the rotating speed is 100-150 rap/min;
(10) putting the ball-milled powder into a tube furnace, and preserving the heat for 30min at the temperature of 600 ℃ to obtain multilayer coated powder;
(11) pressing 3.5g of the coating powder in the step 10) into a magnetic core with the outer diameter of 20mm, the inner diameter of 12mm and the thickness of 2.5mm under the condition of 800 MP;
(12) and (3) carrying out heat treatment for 0.5h at the heat treatment temperature of 600 ℃ under the inert gas condition to reduce the residual stress generated in the pressing process.
The above prepared sample was tested as follows:
and (3) measuring magnetic performance parameters such as magnetic permeability, magnetic loss and the like of the sample by adopting an MATS-2010SA soft magnetic material dynamic measuring device.
The material prepared in example 2 had permeability real part, imaginary part and loss, and the results are shown in fig. 2, 3 and 4.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. The multilayer coated soft magnetic composite material is characterized in that the multilayer coated soft magnetic composite material is of a core-shell structure, iron-based alloy powder is taken as a core, and a passivation layer and Al are sequentially coated on the surface of the iron-based alloy powder2O3A coating layer;
the passivation layer is a metal salt layer generated by reacting iron-based alloy powder with a passivating agent, and the particle size of the iron-based alloy powder is 100-200 um;
the preparation method of the multilayer coated soft magnetic composite material comprises the following steps:
(a) reacting iron-based alloy powder in a passivation solution to obtain powder A;
(b) preparation of Al2O3A colloid;
(c) powder A, Al2O3Performing colloid ball milling reaction;
(d) and calcining the ball-milled powder at high temperature to obtain multilayer coated powder, namely the multilayer coated soft magnetic composite material.
2. A multi-layer coated soft magnetic composite material according to claim 1, wherein said passivating agent is phosphoric acid, nitric acid or glacial acetic acid.
3. A multi-layer coated soft magnetic composite according to claim 1, wherein the iron-based alloy powder comprises Fe powder.
4. A multi-layer coated soft magnetic composite material according to claim 1, wherein step (d) is followed by steps (e) and (f),
(e) the method comprises the following steps Pressing the coated powder in the step (d) into a magnetic core;
(f) the method comprises the following steps Heat treating the magnetic core obtained in the step (e).
5. A multi-layer coated soft magnetic composite material according to claim 1 or 4, wherein the iron-based alloy powder comprises Fe powder,
the passivation solution is a mixed solution of a passivator and alcohol, the passivator is phosphoric acid, nitric acid or glacial acetic acid, and the volume ratio of the passivator to the alcohol is 0.6-1.2: 98.8-99.4;
the adding amount ratio of the iron-based alloy powder to the passivation solution is 40-60 g: 15-25 ml.
6. A multi-layer coated soft magnetic composite material according to claim 1 or 4, wherein the Al is2O3The preparation of the colloid comprises the following steps:
mixing aluminum isopropoxide and ethylene glycol ethyl ether, stirring, adding acetylacetone, stirring, raising the temperature of the mixed system, adding acetic acid, continuing stirring, evaporating, cooling to room temperature, and obtaining a clear transparent substance, namely Al2O3And (3) colloid.
7. The multilayer coated soft magnetic composite material according to claim 6, wherein the ratio of the addition amount of the aluminum isopropoxide, the ethylene glycol monoethyl ether, the acetylacetone and the acetic acid is 2.1-4.5 g: 40-60 ml: 1-3 g: 5-15 ml.
8. A multilayer coated soft magnetic composite according to claim 1 or 4, characterized in that the ball milling reaction conditions are: powder A, Al2O3Adding the colloid into a ball milling tank, mixing, uniformly stirring, adding steel balls, and putting into a ball mill for ball milling, wherein the time for spheroidal graphite is 10-20 min, and the rotating speed is 100-150 rap/min;
the high-temperature calcination conditions are as follows: keeping the temperature at 600 ℃ for 30 min.
9. A multilayer coated soft magnetic composite material according to claim 4, characterized in that the pressing conditions are: pressing under the condition of 800MP-1000MP,
the conditions of the heat treatment are as follows: heat treatment is carried out for 0.5-2h at the temperature of 500-700 ℃ under the inert gas condition.
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| CN111785470B (en) * | 2020-07-22 | 2023-05-23 | 北京铁路信号有限公司 | Magnetic bead powder and preparation method thereof, laminated magnetic bead and preparation method thereof |
| CN112185642A (en) * | 2020-09-23 | 2021-01-05 | 江西艾特磁材有限公司 | Method for coating magnetic powder core with ball milling modified sol-gel |
| CN112420371A (en) * | 2020-10-27 | 2021-02-26 | 佛山市中研非晶科技股份有限公司 | Inductor preparation method |
| CN112247143A (en) * | 2020-10-27 | 2021-01-22 | 佛山市中研非晶科技股份有限公司 | Amorphous nanocrystalline powder coating method and inductor preparation method |
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| CN113450988B (en) * | 2021-05-18 | 2023-07-21 | 深圳市华控科技集团有限公司 | Soft magnetic powder raw material lamination treatment method for high-permeability inductor |
| CN113744989A (en) * | 2021-09-02 | 2021-12-03 | 横店集团东磁股份有限公司 | Metal magnetic powder core and preparation method and application thereof |
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