CN111029076B - Gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss - Google Patents
Gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss Download PDFInfo
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Abstract
The invention provides a gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss, and belongs to the technical field of magnetic materials. The gas atomized Fe-Si-Al soft magnetic composite material is prepared from three gas atomized Fe-Si-Al powders with different particle size ranges; the grain size of the first-stage gas atomization ferro-silicon-aluminum powder is minus 140 meshes to plus 200 meshes, the grain size of the second-stage gas atomization ferro-silicon-aluminum powder is minus 325 meshes to plus 500 meshes, and the grain size of the third-stage gas atomization ferro-silicon-aluminum powder is minus 600 meshes to plus 1000 meshes; the gas atomized Fe-Si-Al soft magnetic composite material has the magnetic permeability of 100kHz/1V not less than 50, the quality factor of 100kHz/1V not less than 155, the direct current bias performance of 100Oe not less than 57%, the direct current bias performance of 200Oe not less than 28%, and the magnetic core loss of 50kHz/100mT not more than 175mW/cm3. The preparation process is simple, and the problem that the high anti-saturation capacity and the low magnetic core loss of the existing gas atomization Fe-Si-Al soft magnetic composite material cannot be achieved at the same time is effectively solved. On the premise of the same magnetic conductivity and direct current bias performance, the medium-frequency loss of the conventional gas atomization iron-silicon-aluminum soft magnetic composite material is obviously reduced.
Description
Technical Field
The invention belongs to the technical field of magnetic materials, and particularly relates to a gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss.
Background
Currently, the use frequency of most medium and small power switching power supplies is still lower than 20 kHz. With the gradual entrance of wide bandgap semiconductor switching tubes into the civil field, the switching frequency of power electronic devices will gradually increase to the mid-frequency range of 50kHz, even more than hundred kHz. And the loss of the soft magnetic core serving as the core magnetic element of the power electronic equipment is rapidly increased along with the increase of the frequency. How to effectively reduce the loss of the soft magnetic composite material on the premise of considering good anti-saturation capacity is a research hotspot at present.
The Fe-Si-Al soft magnetic composite material has the advantages of low loss and low cost, and is the material type with the highest market share in the field of soft magnetic composite materials at present. However, the soft magnetic composite material prepared by crushing the sendust powder by the conventional ball milling has poor saturation resistance. In order to solve the problem, technical personnel develop spherical gas atomization sendust powder, and the use of the spherical powder to prepare the soft magnetic composite material can greatly avoid the possible direct contact of irregular ball-milling powder at sharp corners, thereby effectively improving the anti-saturation capacity of the sendust soft magnetic composite material. But the problem is that the loss of the soft magnetic composite material prepared by the spherical Fe-Si-Al powder with the conventional grain size ratio is obviously improved compared with the soft magnetic composite material prepared by the common ball-milling Fe-Si-Al powder, and the typical loss value of 50kHz/100mT can reach 250-one-step 300mW/cm3The above.
At present, researches on gas-atomized iron-silicon-aluminum soft magnetic composite materials mainly focus on an insulation coating process of gas-atomized iron-silicon-aluminum powder. It is desirable to find an insulating material having high resistivity and good insulating coating effect to realize effective isolation between the gas-atomized sendust powders, thereby improving the application frequency band and the anti-saturation capacity of the soft magnetic composite material. The loss separation research shows that the loss of the soft magnetic composite material below 100kHz is mainly hysteresis loss. Therefore, the insulation process for reducing eddy current loss cannot achieve the purpose of reducing hysteresis loss of the soft magnetic composite material, and the magnetic circuit is cut off due to the fact that the insulation layer separates the atomized sendust powder, so that hysteresis loss is increased. If the hysteresis loss is to be reduced, the only way to reduce the effective demagnetizing field inside the soft magnetic composite is when the alloying composition of the atomized sendust powder has been determined. Generally, a method for increasing the forming pressure of the soft magnetic composite material is usually adopted in production to reduce the number and width of distributed air gaps in the soft magnetic composite material, so as to reduce the effective demagnetizing field. Therefore, the invention provides a method for reducing the number and the width of distributed air gaps in the soft magnetic composite material by designing the particle size ratio and the mass ratio of the magnetic powder, thereby realizing the reduction of effective demagnetizing field and hysteresis loss.
At present, the research on the grain size ratio and the mass ratio of the soft magnetic composite material is reported, but the research mostly focuses on screening a series of magnetic powder with different grain sizes without destination, then, the magnetic powder with different grain sizes is freely combined, and the change rule of the magnetic property is analyzed. For example, a literature reports a preparation method of a low-loss high-permeability sendust soft magnetic composite material, which freely mixes magnetic powders with different particle sizes, has no specific design for selection of particle sizes and proportion of the magnetic powders with different particle sizes, and is not beneficial to regulation and control of the proportion of the particle sizes, so that a small air gap is difficult to obtain between the magnetic powder particles, and effective reduction of loss cannot be realized. And if the specific magnetic powder granularity selection and proportion relation are guided, engineering technicians in the field of soft magnetic composite materials can be conveniently guided to rapidly realize the reduction of the width and the quantity of the distributed air gaps in the soft magnetic composite materials in production, so that the extremely low intermediate frequency magnetic core loss is obtained. At present, although many theoretical models for guiding the particle size ratio exist in the field of powder close packing, the soft magnetic composite material is prepared according to the particle size ratio calculated by the models, and the internal air gap ratio of the obtained finished material is far away from the theoretical value, so that the low magnetic core loss can not be realized in the intermediate frequency range of dozens of kHz.
Therefore, the gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss is manufactured on the basis of the scheme that the width and the number of distributed air gaps in the soft magnetic composite material can be effectively reduced in actual production, the specific grain size proportion and the mass proportion of the gas atomization iron-silicon-aluminum powder are low in cost and simple and convenient to operate, and the corresponding preparation process of the soft magnetic composite material is provided, and the difficulty faced by technical personnel in the field at present is the difficulty.
Disclosure of Invention
In order to effectively reduce the hysteresis loss in the medium-frequency range, the invention aims to provide the gas atomization iron-silicon-aluminum soft magnetic composite material with low medium-frequency loss, and the invention also aims to provide the preparation method of the gas atomization iron-silicon-aluminum soft magnetic composite material with low medium-frequency loss.
A gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss is prepared from three gas atomization iron-silicon-aluminum powders with different particle size ranges;
the mass of the first-stage gas atomization ferrum-silicon-aluminum powder is 30-50% of the total mass of the gas atomization ferrum-silicon-aluminum soft magnetic composite material, the mass of the second-stage gas atomization ferrum-silicon-aluminum powder is 25-45% of the total mass of the gas atomization ferrum-silicon-aluminum soft magnetic composite material, and the mass of the third-stage gas atomization ferrum-silicon-aluminum powder is 5-25% of the total mass of the gas atomization ferrum-silicon-aluminum soft magnetic composite material;
the grain size of the first-stage gas atomization ferro-silicon-aluminum powder is minus 140 meshes to plus 200 meshes, the grain size of the second-stage gas atomization ferro-silicon-aluminum powder is minus 325 meshes to plus 500 meshes, and the grain size of the third-stage gas atomization ferro-silicon-aluminum powder is minus 600 meshes to plus 1000 meshes;
the gas atomization iron-silicon-aluminum soft magnetic composite material has the magnetic permeability of 100kHz/1V of not less than 50, the quality factor of 100kHz/1V of not less than 155, the direct current bias performance of 100Oe of not less than 57%, the direct current bias performance of 200Oe of not less than 28%, and the magnetic core loss of 50kHz/100mT of not more than 175mW/cm3。
The operation steps for preparing the gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss are as follows:
(1) uniformly mixing the first-stage gas atomization ferro-silicon-aluminum powder, the second-stage gas atomization ferro-silicon-aluminum powder and the third-stage gas atomization ferro-silicon-aluminum powder according to a formula to obtain mixed powder;
(2) stirring and mixing anhydrous ethanol accounting for 16% of the mass of the mixed powder and silicon dioxide accounting for 1.2% of the mass of the mixed powder uniformly to obtain inorganic insulating coating slurry;
(3) adding the mixed powder into the inorganic insulating coating slurry, stirring for 20-30 minutes at normal temperature, heating to 110-150 ℃, keeping the temperature, stirring for 45-60 minutes, and naturally cooling to room temperature to obtain insulating powder;
(4) sieving the insulated powder with a 80-mesh sieve to obtain sieved granulated powder;
(5) adding organic silicon resin accounting for 0.4 percent of the mass of the granulation powder and zinc stearate accounting for 0.3 percent of the mass of the granulation powder into the granulation powder, and uniformly mixing; performing bidirectional floating pressing in an oil press under 1860MPa to obtain a gas atomized iron-silicon-aluminum soft magnetic composite green body;
(6) and (3) placing the green body in an annealing furnace, heating the green body from room temperature to 200 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, heating the green body to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours, and cooling the green body to room temperature along with the furnace to obtain the gas atomized Fe-Si-Al soft magnetic composite material.
The beneficial technical effects of the invention are embodied in the following aspects:
(1) the invention greatly reduces the groups of powder with different particle diameters for mixing the powder, only designs the particle diameter range of three-level powder, effectively simplifies the production process, reduces the cost and is convenient for production and operation.
(2) The invention directly provides the specific quantitative relation among the primary particle size range, the secondary particle size range and the tertiary particle size range of the gas atomized iron-silicon-aluminum powder and a corresponding preparation method of the soft magnetic composite material through a large amount of theoretical calculation and experimental correction.
(3) The gas atomization iron-silicon-aluminum soft magnetic composite material prepared by the invention has the advantages that the frequency loss is obviously reduced on the premise of equal magnetic conductivity and direct current bias performance, and the loss of the soft magnetic composite material with the frequency of 50kHz/100mT is reduced by more than 30% compared with the loss of the conventional gas atomization iron-silicon-aluminum soft magnetic composite material.
(4) The gas atomized iron-silicon-aluminum soft magnetic composite material prepared by the invention has higher density under the condition of a certain granularity ratio, as can be seen from figure 1, the magnetic powder is tightly contacted with the magnetic powder, the arrangement of the three-level grain diameter is clear and visible, and the three-level grain diameter powder is well filled in gaps between the primary powder particles and the secondary powder particles.
(5) The gas atomization iron-silicon-aluminum soft magnetic composite material manufactured by the invention also provides a preparation method of the gas atomization iron-silicon-aluminum soft magnetic composite material with good insulativity, good thermal stability and low loss, and the preparation method is simple and easy for mass production after the powder granularity ratio is finished.
Drawings
FIG. 1 is a cross-sectional scanning view of the gas atomized Fe-Si-Al soft magnetic composite material of the present invention.
Detailed Description
The invention will now be further described by way of example with reference to the accompanying drawings.
Example 1
The operation steps for preparing the gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss are as follows:
(1) through calculation, the grain size range of the first-stage gas atomization ferro-silicon-aluminum powder is determined to be minus 140 meshes to plus 200 meshes, the grain size range of the second-stage gas atomization ferro-silicon-aluminum powder is determined to be minus 375 meshes to plus 400 meshes, and the grain size range of the third-stage gas atomization ferro-silicon-aluminum powder is determined to be minus 800 meshes to plus 900 meshes.
(2) Respectively screening 150g of first-stage gas atomization ferro-silicon-aluminum powder, 135g of second-stage gas atomization ferro-silicon-aluminum powder and 15g of third-stage gas atomization ferro-silicon-aluminum powder, and uniformly mixing the three groups of powder into 300g of powder to be insulated.
(3) 48g of absolute ethyl alcohol and 3.6g of silicon dioxide are fully stirred and uniformly mixed to prepare inorganic insulating coating slurry.
(4) Adding 300g of powder to be insulated into 51.6g of inorganic insulating coating slurry, stirring for 30 minutes at normal temperature, heating to 130 ℃, keeping the temperature, stirring for 50 minutes, and naturally cooling to room temperature to obtain the insulating powder.
(4) And (4) sieving the insulated powder by a 80-mesh sieve, and sieving and granulating to obtain the granulated powder.
(5) And (3) pressing and forming: 200g of granulation powder is weighed, 0.8g of organic silicon resin and 0.6g of zinc stearate are added into the granulation powder and uniformly mixed, and bidirectional floating pressing is carried out in an oil press under the pressure intensity of 1860MPa to obtain a gas atomized iron-silicon-aluminum soft magnetic composite green body.
(6) Annealing treatment: and (3) placing the gas atomized iron-silicon-aluminum soft magnetic composite material green body in an annealing furnace, heating from room temperature to 200 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, then heating to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the finished product of the gas atomized iron-silicon-aluminum soft magnetic composite material.
Referring to fig. 1, a sectional scanning view of the gas atomized sendust soft magnetic composite material.
The magnetic properties of the gas atomized sendust soft magnetic composite material prepared in this example after wire winding test are shown in table 1. Therefore, the prepared gas atomized iron-silicon-aluminum soft magnetic composite material has the magnetic permeability of 52.55 at 100kHz/1V, the quality factor of 160.28 at 100kHz/1V, the 100Oe direct current bias performance of 57.67 percent and the 200Oe direct current bias performance of 29.04 percent, and the loss of 50kHz/100mT is only 168.66mW/cm3. This shows that the intermediate frequency loss is significantly reduced while the good anti-saturation capacity of the gas atomized sendust soft magnetic composite material is maintained.
Example 2
The operation steps for preparing the gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss are as follows:
(1) by calculation, the grain size range of the first-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 140 meshes to plus 200 meshes, the grain size range of the second-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 450 meshes to plus 500 meshes, and the grain size range of the third-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 900 meshes to plus 950 meshes;
(2) respectively screening 150g of first-stage gas atomization ferro-silicon-aluminum powder, 105g of second-stage gas atomization ferro-silicon-aluminum powder and 45g of third-stage gas atomization ferro-silicon-aluminum powder, and uniformly mixing the three groups of powder into 300g of powder to be insulated;
(3) 48g of absolute ethyl alcohol and 3.6g of silicon dioxide are fully stirred and uniformly mixed to prepare inorganic insulating coating slurry.
(4) Adding 300g of powder to be insulated into 51.6g of inorganic insulating coating slurry, stirring for 30 minutes at normal temperature, heating to 130 ℃, keeping the temperature, stirring for 50 minutes, and naturally cooling to room temperature to obtain the insulating powder.
(4) And (4) sieving the insulated powder by a 80-mesh sieve, and sieving and granulating to obtain the granulated powder.
(5) And (3) pressing and forming: 200g of granulation powder is weighed, 0.8g of organic silicon resin and 0.6g of zinc stearate are added into the granulation powder and uniformly mixed, and bidirectional floating pressing is carried out in an oil press under the pressure intensity of 1860MPa to obtain a gas atomized iron-silicon-aluminum soft magnetic composite green body.
(6) Annealing treatment: and (3) placing the gas atomized iron-silicon-aluminum soft magnetic composite material green body in an annealing furnace, heating from room temperature to 200 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, then heating to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the finished product of the gas atomized iron-silicon-aluminum soft magnetic composite material.
The magnetic properties of the gas atomized sendust soft magnetic composite material prepared in this example after wire winding test are shown in table 2. Therefore, the gas atomization iron-silicon-aluminum soft magnetic composite material prepared from the prepared gas atomization iron-silicon-aluminum soft magnetic composite material has the magnetic permeability of 50.35 at 100kHz/1V, the quality factor of 100kHz/1V of 155.39, the direct current bias performance of 100Oe of 58.02 percent and the direct current bias performance of 200Oe of 29.33 percent, and the loss of 50kHz/100mT is only 172.22mW/cm3. This shows that the intermediate frequency loss is significantly reduced while the good anti-saturation capacity of the gas atomized sendust soft magnetic composite material is maintained.
Example 3
The operation steps for preparing the gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss are as follows:
(1) by calculation, the grain size range of the first-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 140 meshes to plus 200 meshes, the grain size range of the second-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 400 meshes to plus 450 meshes, and the grain size range of the third-stage gas-atomized ferrosilicon aluminum powder is determined to be minus 950 meshes to plus 1000 meshes;
(2) respectively screening 150g of first-stage gas atomization ferro-silicon-aluminum powder, 75g of second-stage gas atomization ferro-silicon-aluminum powder and 75g of third-stage gas atomization ferro-silicon-aluminum powder, and uniformly mixing the three groups of powder into 300g of powder to be insulated;
(3) 48g of absolute ethyl alcohol and 3.6g of silicon dioxide are fully stirred and uniformly mixed to prepare inorganic insulating coating slurry.
(4) Adding 300g of powder to be insulated into 51.6g of inorganic insulating coating slurry, stirring for 30 minutes at normal temperature, heating to 130 ℃, keeping the temperature, stirring for 50 minutes, and naturally cooling to room temperature to obtain the insulating powder.
(4) And (4) sieving the insulated powder by a 80-mesh sieve, and sieving and granulating to obtain the granulated powder.
(5) And (3) pressing and forming: 200g of granulation powder is weighed, 0.8g of organic silicon resin and 0.6g of zinc stearate are added into the granulation powder and uniformly mixed, and bidirectional floating pressing is carried out in an oil press under the pressure intensity of 1860MPa to obtain a gas atomized iron-silicon-aluminum soft magnetic composite green body.
(6) Annealing treatment: and (3) placing the gas atomized iron-silicon-aluminum soft magnetic composite material green body in an annealing furnace, heating from room temperature to 200 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, then heating to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours, and cooling to room temperature along with the furnace to obtain the finished product of the gas atomized iron-silicon-aluminum soft magnetic composite material.
The magnetic properties of the gas atomized sendust soft magnetic composite material prepared in this example after wire winding test are shown in table 2. Therefore, the magnetic permeability of the gas-atomized Fe-Si-Al soft magnetic composite material prepared from the prepared gas-atomized Fe-Si-Al soft magnetic composite material is 54.35 at 100kHz/1V, the quality factor of 100kHz/1V is 176.44, the direct current bias performance of 100Oe reaches 57.25%, the direct current bias performance of 200Oe reaches 28.44%, and the loss of 50kHz/100mT is only 163.26mW/cm3. This indicates that the gas atomized sendust soft magnetic compositeThe material can keep good anti-saturation capacity, and simultaneously, the intermediate frequency loss is obviously reduced.
The above description is only exemplary of the present invention, and is not intended to limit the present invention, and any modifications and equivalents of the method according to the present invention may still fall within the scope of the present invention.
Claims (2)
1. A gas atomization iron-silicon-aluminum soft magnetic composite material with low intermediate frequency loss is characterized in that: is prepared by gas atomized ferrosilicon aluminum powder with three different particle size ranges;
respectively screening 150g of first-stage gas atomization ferrosilicon aluminum powder, 75-135 g of second-stage gas atomization ferrosilicon aluminum powder and 15-75 g of third-stage gas atomization ferrosilicon aluminum powder, and uniformly mixing the three groups of powder to 300g of powder to be insulated;
the grain size of the first-stage gas atomization ferro-silicon-aluminum powder is minus 140 meshes to plus 200 meshes, the grain size of the second-stage gas atomization ferro-silicon-aluminum powder is minus 325 meshes to plus 500 meshes, and the grain size of the third-stage gas atomization ferro-silicon-aluminum powder is minus 600 meshes to plus 1000 meshes;
the gas atomization iron-silicon-aluminum soft magnetic composite material has the magnetic permeability of 100kHz/1V of not less than 50, the quality factor of 100kHz/1V of not less than 155, the direct current bias performance of 100Oe of not less than 57%, the direct current bias performance of 200Oe of not less than 28%, and the magnetic core loss of 50kHz/100mT of not more than 175mW/cm3。
2. The preparation method of the gas atomized sendust soft magnetic composite material with low intermediate frequency loss according to claim 1, is characterized by comprising the following operation steps:
(1) uniformly mixing the first-stage gas atomization ferro-silicon-aluminum powder, the second-stage gas atomization ferro-silicon-aluminum powder and the third-stage gas atomization ferro-silicon-aluminum powder according to a formula to obtain mixed powder;
(2) stirring and mixing anhydrous ethanol accounting for 16% of the mass of the mixed powder and silicon dioxide accounting for 1.2% of the mass of the mixed powder uniformly to obtain inorganic insulating coating slurry;
(3) adding the mixed powder into the inorganic insulating coating slurry, stirring for 20-30 minutes at normal temperature, heating to 110-150 ℃, keeping the temperature, stirring for 45-60 minutes, and naturally cooling to room temperature to obtain insulating powder;
(4) sieving the insulated powder with a 80-mesh sieve to obtain sieved granulated powder;
(5) adding organic silicon resin accounting for 0.4 percent of the mass of the granulation powder and zinc stearate accounting for 0.3 percent of the mass of the granulation powder into the granulation powder, and uniformly mixing; performing bidirectional floating pressing in an oil press under 1860MPa to obtain a gas atomized iron-silicon-aluminum soft magnetic composite green body;
(6) and (3) placing the green body in an annealing furnace, heating the green body from room temperature to 200 ℃ at the heating rate of 5 ℃/min under the protection of nitrogen, preserving heat for 2 hours, heating the green body to 760 ℃ at the heating rate of 5 ℃/min, preserving heat for 2 hours, and cooling the green body to room temperature along with the furnace to obtain the gas atomized Fe-Si-Al soft magnetic composite material.
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| CN112435822B (en) * | 2020-11-05 | 2023-04-07 | 青岛云路先进材料技术股份有限公司 | Preparation method of high-efficiency Fe-Si-Al magnetic powder core and prepared Fe-Si-Al magnetic powder core |
| CN113441714B (en) * | 2021-06-24 | 2023-08-08 | 安徽瑞德磁电科技有限公司 | Method for improving strength of aerosolized Fe-Si-Al soft magnetic composite material |
| CN116288007B (en) * | 2023-03-22 | 2024-04-02 | 龙门金南磁性材料有限公司 | Low-loss high-molding-strength Fe-Si-Al powder and preparation method and application thereof |
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