CN116313358A - Preparation method of FeSiAl magnetic powder core jointly coated by multiple ferrites - Google Patents
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Abstract
The invention discloses a preparation method of a plurality of ferrite combined coated FeSiAl magnetic powder cores, which relates to a magnetic material technology and comprises the following steps: raw material preparation: preparing NiZn ferrite powder and MnZn ferrite powder, wherein the molecular formula of the NiZn ferrite is Ni x Zn 1‑x Fe 2 O 4 The value range of x is 0.2-0.4; the molecular formula of the MnZn ferrite is Mn x Zn 1‑x Fe 2 O 4 The value range of x is 0.5-0.6; (2) coating: weighing FeSiAl powder, 0.2-1wt% of NiZn ferrite powder and 0.2-1wt% of MnZn ferrite powder by taking the mass of the FeSiAl powder as a reference, adding the three powder into an acetone solution, adding a binder at the same time, continuously stirring, and drying; (3) molding; and (4) annealing. The invention can make the composite magnetic powder core have two characteristics of high magnetic permeability and low loss.
Description
Technical Field
The technology belongs to the technical field of magnetic powder core material preparation, and particularly relates to a FeSiAl magnetic powder combined coating scheme and a preparation method of a magnetic powder core.
Background
The metal magnetic powder core is a soft magnetic material obtained by selecting proper insulating substances to carry out coating treatment on alloy powder, compression molding and annealing treatment. The FeSiAl magnetic powder core has the characteristics of higher saturation magnetic induction intensity, high cost performance and the like, has gradually vigorous market demands, and can be used for manufacturing electronic devices such as high-frequency filters, inductors and the like. The power loss of the magnetic powder core such as FeSiAl mainly consists of two parts, namely eddy current loss and hysteresis loss, and the eddy current loss at high frequency is the main part. Nowadays, more and more high-frequency application scenes exist, and the FeSiAl magnetic powder cores are easy to generate eddy current loss in the high-frequency scenes, so that the resistivity among magnetic particles is effectively improved by using a proper coating substance, and the eddy current loss of the magnetic powder cores is reduced.
Chinese patent publication No. CN112700960A discloses a method for insulating, coating and high-strength bonding of metal soft magnetic powder cores, which adopts gas atomization FeSiAl spherical powder and uses gamma- (2, 3-glycidoxy) propyl trimethoxy silane for coating modification. The performance indexes are as follows: permeability of 30, power loss under 50kHz and 100mT test conditions<180mW/cm 3 . A uniform coating can also be obtained using organic materials,but only plays a role in reducing power loss, and the magnetic permeability of the material can be reduced by introducing non-magnetic substances, and meanwhile, the coating layer is easy to fail in a high-temperature application scene.
Chinese patent publication No. CN109877315A discloses a low-permeability FeSiAl magnetic powder core material and a method for manufacturing a magnetic powder core, wherein gas atomization FeSiAl spherical powder is selected, and chromic acid phosphoric acid boric acid mixed solution is used for reacting with FeSiAl alloy powder. The performance indexes are as follows: the magnetic permeability is 18-20, and the power loss is 45-55mW/cm under the test conditions of 50kHz and 50mT 3 . The acidic material is used for coating, so that the problem of easy failure at high temperature can be solved, a uniform coating layer is obtained, but only the effect of reducing power loss is achieved, and the magnetic performance of the composite magnetic powder core can be reduced due to the introduction of the non-magnetic material.
The Chinese patent publication No. CN112562956A discloses a ferrite coated FeSiAl metal magnetic powder core and a preparation method thereof, wherein a chemical coprecipitation method is used for forming an iron hydroxide layer on the surface of the magnetic powder, and the iron hydroxide layer is converted into a ferrite insulating layer in subsequent high-temperature heat treatment. The performance indexes are as follows: permeability of magnetic material>60, the power loss is 53-56mW/cm under the test conditions of 50kHz and 50mT 3 . The method can obtain a uniform ferrite coating by using a chemical coprecipitation method, plays a role in stabilizing magnetic powder core permeability, but cannot determine converted ferrite components and properties in the process of high-temperature heat treatment, and the obtained ferrite coating is not high-performance and has no obvious effect on reducing power loss.
Aiming at the MnZn ferrite coated FeSiAl alloy, the university of Anhui (Current Applied Physics,2019,19 (8): 924-927) discloses a research on a metal magnetic powder core material, wherein a ball milling mixing process is used for coating the MnZn ferrite, and the addition amount of the MnZn ferrite is 5wt% of the composite magnetic powder core performance index: permeability >40, and power loss <10W/kg under test conditions of 1000kHz and 5 mT. Although the addition of MnZn ferrite can improve the magnetic permeability of the magnetic powder core, the high-frequency eddy current loss of the magnetic powder core cannot be effectively reduced due to the low resistivity of the MnZn ferrite. Meanwhile, the ball milling mixing process is easy to introduce ball milling media, and the magnetic powder core performance is deteriorated.
In addition, aiming at NiZn ferrite coated alloy powder, the university of south China (Journal of Magnetism and Magnetic Materials,2017, 428:148-153) discloses a research on a metal magnetic powder core material, and NiZn ferrite is coated on the surface of iron powder by using chemical coprecipitation, wherein the composite magnetic powder core performance indexes are as follows: permeability of magnetic material>47, a power loss of 193.3mW/cm under test conditions of 100kHz,20mT 3 . NiZn has high resistivity, is a typical high-frequency soft magnetic material, can effectively reduce the eddy current loss of the magnetic powder core, but the effect of improving the magnetic powder core permeability of the NiZn ferrite is not obvious, and meanwhile, the chemical coprecipitation method is not suitable for large-scale industrial production.
Based on the above, the organic matter or the high-resistivity material is adopted for coating treatment, so that the power loss of the magnetic powder core can be effectively reduced, but when the coating material is a non-magnetic material, the magnetic conductivity of the composite magnetic powder core can be obviously reduced; the NiZn ferrite is singly adopted as a coating agent, and the high-resistance characteristic of the NiZn ferrite is utilized, so that the eddy current loss of the magnetic powder core can be effectively reduced, but the magnetic permeability improvement effect is not obvious; the MnZn ferrite is singly adopted as a coating agent, and the magnetic permeability of the magnetic powder core can be effectively improved by utilizing the high-conductivity characteristic of the MnZn ferrite, but the high-frequency loss characteristic of the magnetic powder core cannot be effectively improved due to the low resistivity of the MnZn ferrite. Based on the above, the invention provides a plurality of ferrite combined coated FeSiAl magnetic powder cores and a preparation method thereof. The composite magnetic powder core performance is improved by adopting two magnetic substances, namely NiZn ferrite with high resistivity and MnZn ferrite with high magnetic conductivity, so that the magnetic powder core magnetic conductivity is improved under the condition of reducing the power loss.
Disclosure of Invention
The invention aims to solve the technical problem that a single coating agent can only stabilize magnetic permeability or reduce power loss, and provides a preparation method of a NiZn and MnZn ferrite combined coating FeSiAl magnetic powder core, which can stabilize and even improve the magnetic permeability of a magnetic powder core material under the condition of meeting the low-loss application requirement.
The technical scheme adopted by the invention for solving the technical problems is that the preparation method for jointly coating FeSiAl magnetic powder cores by a plurality of ferrites comprises the following steps:
(1) Raw material preparation: preparing NiZn ferrite powder and MnZn ferrite powder,
the molecular formula of the NiZn ferrite is Ni x Zn 1-x Fe 2 O 4 The value range of x is 0.2-0.4;
the molecular formula of the MnZn ferrite is Mn x Zn 1-x Fe 2 O 4 The value range of x is 0.5-0.6;
(2) Coating: weighing FeSiAl powder, 0.2-1wt% of NiZn ferrite powder and 0.2-1wt% of MnZn ferrite powder by taking the mass of the FeSiAl powder as a reference, adding the three powder into an acetone solution, adding a binder at the same time, continuously stirring, and drying;
(3) And (3) forming: pressing and forming a green blank;
(4) Annealing: the green blank is annealed at 700-900 ℃ for 1-3h.
The binder was 0.5wt% PVB and 0.5wt% silicone.
The NiZn ferrite powder is prepared by the following steps:
iron oxide, nickel oxide and zinc oxide are mixed according to a molecular formula Ni x Zn 1-x Fe 2 O 4 Proportioning, pre-sintering at 800-900 ℃ after mixing, adding 0.05-0.20wt% of calcium carbonate and 0.05-0.20wt% of bismuth oxide, performing primary ball milling, sintering at 1050-1200 ℃ in air atmosphere, performing secondary ball milling, and finally obtaining the particle size of 0.4-1.5 mu m.
The MnZn ferrite powder is prepared by the following steps:
ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 Proportioning, wherein the value range of x is 0.5-0.6, pre-sintering at 800-900 ℃, adding 0.01-0.05wt% of calcium carbonate, 01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide, performing primary ball milling, sintering at 1350-1420 ℃, performing secondary ball milling on the sintered powder, and finally obtaining the particle size of 1.2-2.5 mu m.
An air atmosphere is adopted in the sintering heating stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, and the oxygen content is 0.1-5.0%.
The invention provides a simple and effective combined coating scheme, less NiZn ferrite and MnZn ferrite are added, and the ferrite with high resistivity and ferrite with high magnetic conductivity are combined, so that non-magnetic substances are not introduced, and the composite magnetic powder core has two characteristics of high magnetic conductivity and low loss; the preparation process of the magnetic powder core is simple and quick, does not need to carry out chemical reaction for a long time or use organic coating substances which are not resistant to high temperature, and is popularized on a large scale in a market.
The invention is further described below with reference to the drawings, tables and detailed description.
Drawings
FIG. 1 is a graph showing the change in permeability with the amount of coating of the magnetic core material of comparative examples 1 to 7.
Fig. 2 is a bar graph of magnetic permeability of the magnetic powder core material of comparative examples 1, 2, and 5, example 1.
Detailed Description
In the present invention, the numerical ranges indicated by the "-" symbols all include the endpoints.
The core idea of the invention is as follows: based on the application requirements of the magnetic powder core on the aspects of high frequency and improvement of magnetic permeability, the application requirement is achieved by adopting a combined coating mode. The NiZn ferrite has higher resistivity>10 6 Omega.m, simultaneous permeability>2000, has good high frequency characteristics; the MnZn ferrite has high magnetic permeability, the magnetic permeability of the high-conductivity MnZn ferrite is up to 15000 by adjusting Zn element in the formula, but the resistivity is high<10Ω·m. The particle size of the NiZn ferrite powder subjected to coating modification is smaller than that of the MnZn ferrite powder, and the two ferrites can form particle grading to achieve the effect of alternate coating, so that a coating layer is formed among FeSiAl particles more uniformly; the NiZn ferrite and the MnZn ferrite are spinel structures, belong to equiaxed crystal systems, are magnetic materials, are cubic crystal systems with FeSiAl, and have similar anisotropism. Therefore, the NiZn and MnZn ferrite are combined for coating, on one hand, the high resistivity characteristic of the NiZn ferrite can be utilized, the resistivity of FeSiAl metal magnetic powder cores is improved, the high frequency characteristic of the magnetic powder cores is improved, and on the other hand, the MnZn ferrite and the NiZn ferrite are utilizedHigh magnetic permeability, stability and high magnetic permeability of the composite magnetic powder core.
The invention comprises the following steps:
(1) Raw material preparation
The raw materials comprise FeSiAl alloy powder and a coating agent. The FeSiAl powder is heat treated at 650 ℃ and has a particle size of 20-40 mu m. The coating agent is selected from NiZn ferrite and MnZn ferrite, and the ferrite is prepared as follows.
Preparation of NiZn ferrite: ferric oxide, nickel oxide and zinc oxide according to the formula Ni x Zn 1-x Fe 2 O 4 (x=0.2-0.4), and placing the mixture in a bell jar furnace for presintering at 800-900 ℃. Adding 0.05-0.20wt% of calcium carbonate and 0.05-0.20wt% of bismuth oxide, and ball milling for 3-5h by a planetary ball mill. Placing the powder in a box furnace, sintering at 1050-1200 ℃ in air atmosphere, and ball milling for 20h by using a planetary ball mill, wherein the particle size is 0.4-1.5 mu m. The magnetic permeability of the NiZn ferrite reaches 2200, and the resistivity reaches 10 6 Ω·m。
Preparation of MnZn ferrite: ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 (x=0.5-0.6), and placing the mixture in a bell jar furnace for presintering at 800-900 ℃. Adding 0.01-0.05wt% of calcium carbonate, 0.01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide, and ball milling for 1-2h by a planetary ball mill. And sintering the powder in a tube furnace at 1350-1420 ℃. An air atmosphere is adopted in the sintering heating stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, a certain oxygen partial pressure is maintained, and the oxygen content is 0.1-5.0%. Ball milling the sintered powder for 20h by using a planetary ball mill, wherein the particle size is 1.2-2.5 mu m. The magnetic permeability of the MnZn ferrite reaches about 10000, and the resistivity is 3.72 omega.m.
(2) Coating
Based on the mass of FeSiAl powder, weighing FeSiAl powder, 0.2-1wt% of NiZn ferrite powder and 0.2-1wt% of MnZn ferrite powder, adding the three powders into an acetone solution, adding a commercial binder, and stirring and mixing. Stirring until acetone is volatilized basically, sieving with a 40-mesh sieve, and drying the obtained granulated powder until acetone is volatilized completely. Wherein the binder is 0.5wt% PVB and 0.5wt% silicone.
(3) Shaping
And pressing the powder subjected to the coating treatment by adopting a hydraulic press to form a green part, wherein the forming pressure is 1800-2600MPa.
(4) Annealing
And (3) placing the pressed green blank in an atmosphere sintering device for annealing treatment, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3h. And adopting a vacuum argon annealing mode.
The final technical indexes of the FeSiAl composite magnetic powder core material (coating agent: 0.25wt% NiZn ferrite and 0.25wt% MnZn ferrite) prepared by the invention are as follows: the magnetic permeability is 74.4, and the power loss is 59.57mW/cm under the test conditions of 50kHz and 50mT 3 The power loss is 271.66mW/cm under the test conditions of 50kHz and 100mT 3 。
Examples
Embodiments include the following steps:
(1) Raw material preparation
The raw materials comprise FeSiAl alloy powder and a coating agent. The FeSiAl powder is heat treated at 650 ℃ and has a particle size of 20-40 mu m. The coating agent is selected from NiZn ferrite and MnZn ferrite, and the ferrite is prepared as follows.
Preparation of NiZn ferrite: ferric oxide, nickel oxide and zinc oxide according to the formula Ni x Zn 1-x Fe 2 O 4 (x=0.2-0.4), and placing the mixture in a bell jar furnace for presintering at 800-900 ℃. Adding 0.05-0.20wt% of calcium carbonate and 0.05-0.20wt% of bismuth oxide, and ball milling for 3-5h by a planetary ball mill. Placing the powder in a box furnace, sintering at 1050-1200 ℃ in air atmosphere, and ball milling for 20h by using a planetary ball mill, wherein the particle size is 0.4-1.5 mu m. The magnetic permeability of the NiZn ferrite reaches 2200, and the resistivity reaches 10 6 Ω·m。
Preparation of MnZn ferrite: ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 (x=0.5-0.6), and placing the mixture in a bell jar furnace for presintering at 800-900 ℃. Adding 0.01-0.05wt% of calcium carbonate, 0.01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide, and ball milling for 1-2h by a planetary ball mill. Powder is placed in a tube furnace 1350-14Sintering at 20 ℃. An air atmosphere is adopted in the sintering heating stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, a certain oxygen partial pressure is maintained, and the oxygen content is 0.1-5.0%. Ball milling the sintered powder for 20h by using a planetary ball mill, wherein the particle size is 1.2-2.5 mu m. The magnetic permeability of the MnZn ferrite reaches about 10000, and the resistivity is 3.72 omega.m.
(2) Coating
Based on the mass of FeSiAl powder, weighing FeSiAl powder, 0.25-1wt% of NiZn ferrite powder and 0.25-1wt% of MnZn ferrite powder, adding the three powders into an acetone solution, adding a commercial binder, and stirring and mixing by using a stirrer. Stirring until acetone is volatilized basically, sieving with 40 mesh sieve twice, and oven drying the obtained granulated powder until acetone is volatilized completely. Wherein the binder is 0.5wt% PVB and 0.5wt% silicone.
(3) Shaping
And (3) pressing and forming the coated powder into a green part by using a hydraulic press, wherein the pressure maintaining time is 20s, and the forming pressure is 1800-2600MPa.
(4) Annealing
And (3) placing the pressed green body in a tube furnace for annealing treatment, wherein the annealing temperature is 700-900 ℃, and the heat preservation time is 1-3h. And adopting a vacuum argon annealing mode. Vacuum argon annealing is divided into:
4.1, vacuumizing for 40min, and introducing argon until the pressure gauge approaches 0MPa;
4.2, vacuumizing for 30min, and introducing argon until the pressure gauge is close to minus 0.05MPa;
4.3, starting annealing;
4.4, the temperature in the furnace is up to 500 ℃, and the step (2) is carried out.
(5) Testing
And (3) testing the magnetic property of the sample prepared in the step (4).
The resistivity and the magnetic conductivity of the material are tested by adopting a TH2826 high-frequency LCR digital bridge of Changzhou Homeou electronics limited company, the power loss of the material is tested by adopting a SY-8218BH analyzer of IWAtsU company, and the hysteresis loss and the eddy current loss of the material are obtained by adopting a Jordan loss separation method.
To verify the core idea of the invention, 5 sets of examples, 7 sets of comparative examples, and the coating scheme is as follows:
table 1: example ferrite content
| Examples | NiZn ferrite (wt%) | MnZn ferrite (wt%) |
| 1 | 0.25 | 0.25 |
| 2 | 0.25 | 0.50 |
| 3 | 0.25 | 0.75 |
| 4 | 0.50 | 0.25 |
| 5 | 0.75 | 0.25 |
Table 2: comparative example ferrite content
| Comparative example | NiZn ferrite (wt%) | MnZn ferrite (wt%) |
| 1 | 0 | 0 |
| 2 | 0.25 | 0 |
| 3 | 0.50 | 0 |
| 4 | 0.75 | 0 |
| 5 | 0 | 0.25 |
| 6 | 0 | 0.50 |
| 7 | 0 | 0.75 |
Examples 1-5, comparative examples 1-7 all used a 2200M forming pressure with an annealing temperature of 750 ℃.
The composite magnetic powder cores were prepared by the above process, examples 1-5, comparative examples 1-7, and the performance parameters were as follows:
table 3: performance parameters
| Permeability of magnetic material | Permeability of magnetic material | ||
| Example 1 | 74.4 | Comparative example 2 | 73.9 |
| Example 2 | 78.7 | Comparative example 3 | 71.9 |
| Example 3 | 79.0 | Comparative example 4 | 70.2 |
| Example 4 | 72.8 | Comparative example 5 | 77.5 |
| Examples5 | 71.4 | Comparative example 6 | 81.4 |
| Comparative example 1 | 75.2 | Comparative example 7 | 86.8 |
As shown in fig. 1, the NiZn ferrite can stabilize the magnetic permeability of the magnetic powder core, the decrease amplitude is not large, and the magnetic permeability of the composite magnetic powder core with the coating amount of 0.75wt% is more than 70; the MnZn ferrite is added to effectively improve the magnetic permeability of the magnetic powder core, and the magnetic permeability of the composite magnetic powder core with the cladding amount of 0.75wt% is more than 86;
as can be seen from fig. 2, the magnetic powder core adopting the combined cladding treatment can maintain the magnetic permeability above 70;
TABLE 4 Table 4
Table 4 shows the power loss of the magnetic powder core materials of examples 1 to 3, comparative examples 1 to 2: (1) 50kHz,50mT; (2) 50kHz,100mT; (3) 50kHz,50mT; (4) 50kHz,50mT. The MnZn ferrite of example 1 plays a role in reducing loss while keeping the amount of added NiZn ferrite unchanged. With the addition of MnZn ferrite, the power loss gradually increases, which shows that the excessive addition of MnZn ferrite can deteriorate the loss characteristics of the composite magnetic powder core.
TABLE 5
Table 5 shows the power loss of the magnetic powder core materials of examples 1, 4, 5 and comparative examples 1, 4, test conditions: (1) 50kHz,50mT; (2) 50kHz,100mT; (3) 50kHz,50mT; (4) 50kHz,50mT. Under the condition that the addition amount of the MnZn ferrite is kept unchanged, the power loss is obviously reduced along with the addition of the NiZn ferrite.
Claims (5)
1. The preparation method of the FeSiAl magnetic powder core jointly coated by a plurality of ferrites is characterized by comprising the following steps:
(1) Raw material preparation: preparing NiZn ferrite powder and MnZn ferrite powder,
the molecular formula of the NiZn ferrite is Ni x Zn 1-x Fe 2 O 4 The value range of x is 0.2-0.4;
the molecular formula of the MnZn ferrite is Mn x Zn 1-x Fe 2 O 4 The value range of x is 0.5-0.6;
(2) Coating: weighing FeSiAl powder, 0.2-1wt% of NiZn ferrite powder and 0.2-1wt% of MnZn ferrite powder by taking the mass of the FeSiAl powder as a reference, adding the three powder into an acetone solution, adding a binder at the same time, continuously stirring, and drying;
(3) And (3) forming: pressing and forming a green blank;
(4) Annealing: the green blank is annealed at 700-900 ℃ for 1-3h.
2. The method for preparing a plurality of ferrite composite coated fesai magnetic powder cores according to claim 1, wherein the binder comprises 0.5wt% pvb and 0.5wt% silicone.
3. The method for preparing the ferrite composite coated fesai magnetic powder core according to claim 1, wherein the NiZn ferrite powder is prepared by the following steps:
iron oxide, nickel oxide and zinc oxide are mixed according to a molecular formula Ni x Zn 1-x Fe 2 O 4 Proportioning, pre-sintering at 800-900 deg.C after mixing, adding 0.05-0.20wt% of calcium carbonate and 0.05-0.20wt% of bismuth oxide, ball milling once, sintering at 1050-1200 deg.C in air atmosphere, secondary ball milling and the mostThe final particle size is 0.4-1.5 μm.
4. The method for preparing the ferrite composite coated fesai magnetic powder core according to claim 1, wherein the MnZn ferrite powder is prepared by the following steps:
ferric oxide, manganic oxide and zinc oxide according to the molecular formula Mn x Zn 1-x Fe 2 O 4 Proportioning, wherein the value range of x is 0.5-0.6, pre-sintering at 800-900 ℃, adding 0.01-0.05wt% of calcium carbonate, 01-0.05wt% of titanium oxide and 0.05-0.20wt% of bismuth oxide, performing primary ball milling, sintering at 1350-1420 ℃, performing secondary ball milling on the sintered powder, and finally obtaining the particle size of 1.2-2.5 mu m.
5. The method for preparing the ferrite-coated FeSiAl magnetic powder core according to claim 4, wherein an air atmosphere is adopted in the sintering temperature-raising stage; the nitrogen atmosphere is adopted in the temperature-reducing stage, and the oxygen content is 0.1-5.0%.
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