CN115831520A - High-thermal-conductivity metal soft magnetic composite material and preparation method and application thereof - Google Patents
High-thermal-conductivity metal soft magnetic composite material and preparation method and application thereof Download PDFInfo
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- CN115831520A CN115831520A CN202211625783.3A CN202211625783A CN115831520A CN 115831520 A CN115831520 A CN 115831520A CN 202211625783 A CN202211625783 A CN 202211625783A CN 115831520 A CN115831520 A CN 115831520A
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Abstract
The invention relates to a high-thermal-conductivity metal soft magnetic composite material, a preparation method and application thereof, and relates to the technical field of soft magnetic material preparation. Adding the heat-conducting flake powder into a coupling agent solution to obtain modified heat-conducting flake powder; adding resin and modified heat-conducting flaky powder into the metal soft magnetic powder, coating the metal soft magnetic powder by an insulating layer, and then adding a volatile organic solvent for mixing and granulating; bridging the metal soft magnetic powder through the heat-conducting flaky powder, and dispersing the resin in pores of the system to obtain metal soft magnetic composite particles; pressing and forming to obtain a metal soft magnetic composite material green body; and curing and annealing the green body to obtain the metal soft magnetic composite material. The invention establishes a heat conduction path from the metal soft magnetic powder to the outer surface of the soft magnetic composite magnetic core, and realizes high heat conductivity.
Description
Technical Field
The invention relates to the technical field of preparation of soft magnetic materials, in particular to a high-thermal-conductivity metal soft magnetic composite material and a preparation method and application thereof.
Background
The integrally formed inductor mainly comprises a soft magnetic composite material (SMC) and an internal coil, and under the actual alternating current and direct current superposition working condition, the internal coil has direct current power loss due to direct current resistance; the alternating current in the winding causes alternating power loss and alternating flux loss in the soft magnetic composite material; the metal soft magnetic particles can generate eddy current loss in a high-frequency alternating magnetic field, and the loss can generate certain heat.
Against the background, the heat dissipation mode that integrated into one piece inductance device field adopted uses outside supplementary heat dissipation to give first place to, but because the heat source is inside production, the binder thermal conductivity is lower simultaneously, can't be more fast with the heat derivation of inside production, therefore integrated into one piece inductance heat accumulation appears and leads to the temperature to rise fast. When the temperature of the device rises, the direct current resistance of the device is increased, the power consumption generated by direct current is further increased, and vicious circle is formed. Therefore, especially for the integrally formed inductor applied in high power, high frequency and high ambient temperature scenes, the heat-conducting property of the soft magnetic composite material becomes more important.
The metal soft magnetic composite material is mainly prepared by mixing metal soft magnetic particles, an insulating coating layer and an adhesive in a mould pressing mode; the insulating coating layer mainly comprises organic thermosetting resin, inorganic oxide, metal oxide and the like, and although the insulating coating layer can realize insulation among particles and reduce eddy current loss, a part of material with lower heat conductivity is introduced at the same time, so that the heat resistance of the soft magnetic composite magnetic core is increased.
The binder is generally composed of a thermosetting organic binder such as an epoxy resin, a silicone resin, or a phenol resin. The organic resin being a poor conductor of heat, e.g. epoxyThe thermal conductivity of the resin is 0.17-0.21 W.m -1 ·K -1 Therefore, the use of a resin as a binder is a key factor for increasing the thermal resistance of the soft magnetic composite core.
The soft magnetic composite material also has the problems that the interface bonding force between the adhesive and the coating layer is not strong, phonon scattering is easy to increase the interface thermal resistance, and the related introduction aiming at the improvement of the thermal conductivity of the soft magnetic composite material is less at present.
Disclosure of Invention
The application provides a high-thermal-conductivity metal soft magnetic composite material and a preparation method thereof, wherein resin-high-thermal-conductivity Al is enhanced in a mode of modifying the surface of high-thermal-conductivity flaky powder 2 O 3 The mutual connection between the insulating coating layer and the high-thermal-conductivity powder reduces the thermal resistance of the adhesive and reduces the interface scattering; the high heat conduction characteristic of the metal soft magnetic composite material is realized, so that the technical problem that the soft magnetic composite material in the prior art is low in heat conductivity is solved from the inside of the material.
According to a first aspect of the present invention, there is provided a method for preparing a metallic soft magnetic composite material, comprising the steps of:
(1) Adding the heat-conducting flake powder into a coupling agent solution to obtain modified heat-conducting flake powder; the heat-conducting flaky powder is nitride, carbide or oxide;
(2) Adding resin and the modified heat-conducting flaky powder obtained in the step (1) into metal soft magnetic powder, wherein the metal soft magnetic powder is coated by an insulating layer, and then adding a volatile organic solvent for mixing and granulating; the metal soft magnetic powder is bridged through heat-conducting flaky powder, and the resin is dispersed in pores of the system to obtain metal soft magnetic composite particles;
(3) Pressing and molding the metal soft magnetic composite particles obtained in the step (2) to obtain a metal soft magnetic composite material green body; and heating and curing the green body to obtain the metal soft magnetic composite material.
Preferably, in step (1), the nitride is BN, alN or Si 3 N 4 (ii) a The carbide is SiC or diamond; the oxide is Al 2 O 3 ZnO or BeO.
Preferably, in the step (1), the metallic soft magnetic powder is at least one of carbonyl iron powder, fe-based amorphous alloy powder, fe-based nanocrystalline powder, feNiMo alloy powder, feSi alloy powder, feSiAl alloy powder, and fesicrcr alloy powder.
Preferably, the resin is at least one of an epoxy resin, a silicone resin, and a phenolic resin.
Preferably, the insulating layer is Al 2 O 3 Or MgO.
Preferably, the coupling agent is at least one of an amino coupling agent, a mercapto coupling agent, a vinyl coupling agent, an epoxy coupling agent, a cyano coupling agent, and a methacryloxy silane coupling agent.
Preferably, in the step (3), the heating temperature is 150-700 ℃.
Preferably, in the step (3), the metal soft magnetic composite particles are compressed into a ring-shaped structure.
According to another aspect of the invention, the metal soft magnetic composite material prepared by any one of the methods is provided.
According to another aspect of the invention, there is provided the use of said metallic soft magnetic composite material for inductors or soft magnetic composite cores.
Generally, compared with the prior art, the above technical solution conceived by the present invention mainly has the following technical advantages:
(1) The invention provides a metal soft magnetic composite material with high heat conduction characteristic, which modifies the surface of high heat conduction flaky powder, so that the flaky powder is better compatible with a resin adhesive, reduces phonon scattering between heat conduction particles and resin components, and increases the heat conductivity of the soft magnetic composite material.
(2) The insulating coating layer of the invention preferably adopts Al with high thermal conductivity 2 O 3 (38-42W·m -1 ·K -1 ) The heat conducting sheet powder is used as a heat conducting network to establish a heat conducting path from the metal soft magnetic powder to the outer surface of the soft magnetic composite magnetic core, so that the heat conducting characteristic of the composite magnetic core is realized. The inherent thermal conductivity of thermally conductive fillers (flakes) is generally difficult to achieve in composite materials because the heat is generally directed along the heatThe transmission of the flaky heat conducting powder with higher heat conductivity is realized, and the organic resin used as the adhesive can slow down the process, so that the filler with a specific shape, size and length-diameter ratio is required to be filled in the resin, the interconnection among the flaky powders is realized under the condition of ensuring low filling as much as possible, and a heat conducting passage is realized, namely a network-shaped passage for maximally constructing rapid heat circulation with lower filling amount.
Drawings
Fig. 1 is a schematic structural view of the high thermal conductivity metal soft magnetic composite material of the present invention.
FIG. 2 is EDS of the surface alumina coating layer of the metal magnetic powder of the present invention.
FIG. 3 is an SEM image of BN flakes used in the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention relates to a preparation method of a metal soft magnetic composite material, which comprises the following steps:
(1) Placing the high-thermal-conductivity flaky powder into a diluted coupling agent solution, and stirring and ultrasonically treating the high-thermal-conductivity flaky powder to obtain modified high-thermal-conductivity flaky powder;
(2) Adding a certain amount of resin into the metal soft magnetic powder, adding a volatile organic solvent into the modified high-thermal-conductivity flaky powder, mixing, granulating, drying and sieving to obtain metal soft magnetic composite particles;
(3) Pressing and molding the metal soft magnetic composite particles by adopting a die pressing process to obtain a soft magnetic composite material green body;
(4) And (3) placing the green body in the atmosphere, and curing at a high temperature to obtain the high-thermal-conductivity soft magnetic composite material.
Preferably, the high thermal conductivity flaky powder in the step (1) is BN, alN, si 3 N 4 、SiC、Al 2 O 3 At least one of ZnO and BeO.
Preferably, the ratio of the diameter (average value of the major diameter and the minor diameter) to the thickness of the high thermal conductivity flake powder described in step (1) should be between 10 and 2000.
Preferably, the coupling agent in step (1) is at least one of an amino, mercapto, vinyl, epoxy, cyano and methacryloxy silane coupling agent.
Preferably, the coupling agent solution in the step (1) is ethanol and H 2 Mixed solution of O, wherein H 2 O: the weight ratio of the coupling agent is 5-40%, wherein the volume ratio of the coupling agent to the ethanol is 50-400%, and the ultrasonic stirring time is 2-24 h.
Preferably, the metallic soft magnetic powder in the step (2) is Al 2 O 3 Coating, wherein the preparation process adopts a common sol-gel method or a gas phase method, and the thickness of the coating is 1-100 nm. The metal soft magnetic powder component is at least one of carbonyl iron powder, fe-based amorphous alloy powder, fe-based nanocrystalline powder, feNiMo alloy powder, feSi alloy powder, feSiAl alloy powder and FeSiCr alloy powder.
Preferably, the volume ratio of the modified high thermal conductivity flaky powder to the resin in the step (2) is between 30% and 70%.
Preferably, the resin in the step (2) is at least one of epoxy resin, silicone resin and phenolic resin, wherein the weight ratio of the resin to the metal soft magnetic powder is between 0.5% and 12%.
Preferably, the volatile organic solvent in step (2) is at least one of acetone, ethyl acetate and toluene.
Preferably, the drying temperature in step (2) should be between 40 ℃ and 200 ℃.
Preferably, the sieving process in the step (2) is to sieve the metal soft magnetic composite powder by using a sieve with 40-400 meshes.
Preferably, the molding pressure in step (3) is 300 MPa-2000 MPa, and the dwell time is 30-300 s.
Preferably, the atmosphere in step (4) is at least one of air, nitrogen, argon and helium, wherein the purity of nitrogen, argon and helium is 99.99%.
Preferably, the high temperature condition in step (4) is 150 to 700 ℃.
The structure schematic diagram of the high-thermal-conductivity metal soft magnetic composite material is shown in the attached figure 1, and the embodiment provides a metal magnetic powder core 1 which comprises metal soft magnetic particles 2, an insulating coating layer 3, flaky thermal-conductivity powder 4 and an organic resin adhesive 5. According to the structure, flaky heat conduction powder 4 with a certain filling amount is dispersed in an organic resin adhesive 5 and is formed, bridged and interconnected to form a heat conduction network, and the metal soft magnetic particles 2 coated with the insulating coating layers 3 are dispersed in the heat conduction network to form the soft magnetic composite material with the network heat conduction structure.
Example 1
The embodiment provides a method for manufacturing the metal magnetic powder core, which comprises the following steps:
(1) Weighing 100g of soft metal powder with D50=40 μm, and preparing Al by gas phase method or liquid phase method 2 O 3 And the insulating coating layer is 10nm in insulating thickness.
(2) 200mg of silane coupling agent is placed in 190ml of ethanol and 10ml of water, 20g of BN flake powder is added, ultrasonic stirring is carried out for 6 hours, and modified BN powder is obtained after filtration and drying.
(3) Adding 1g of epoxy resin and 2.16g of BN flake powder with the diameter-thickness ratio of 1000 (the volume ratio of boron nitride filled in the epoxy resin is 50%) into the metal soft magnetic powder, mixing and granulating 20ml of ethyl acetate, and sieving through 40 meshes and 200 meshes after the organic solvent is completely volatilized to obtain soft magnetic composite powder with the particle size interval of 40 meshes-200 meshes.
(4) And (3) placing the granulated powder in a mould, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(5) And (3) annealing the compression-molded inductor in argon gas at 550 ℃ for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
Example 2
The embodiment provides a method for manufacturing the metal magnetic powder core, which comprises the following steps:
(1) Weighing 100g of soft metal powder with D50=40 μm, and preparing Al by gas phase method or liquid phase method 2 O 3 And the insulating coating layer is 20nm in insulating thickness.
(2) 200mg of silane coupling agent is placed in 190ml of ethanol and 10ml of water, 20g of BN flake powder is added, ultrasonic stirring is carried out for 6 hours, and modified BN powder is obtained after filtration and drying.
(3) Adding 1g of epoxy resin and 2.16g of BN flake powder with the diameter-thickness ratio of 1000 (the volume ratio of boron nitride filled in the epoxy resin is 50%) into the metal soft magnetic powder, mixing and granulating with 20ml of ethyl acetate, and sieving with 40-mesh and 200-mesh sieves after the organic solvent is completely volatilized to obtain the soft magnetic composite powder with the particle size interval of 40-200 meshes.
(4) And (3) placing the granulated powder in a mould, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(5) And (3) placing the molded inductor in argon gas at 550 ℃ for annealing for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
Example 3
The embodiment provides a method for manufacturing the metal magnetic powder core, which comprises the following steps:
(1) Weighing 100g of soft metal powder with D50=40 μm, and preparing Al by adopting a gas phase method or a liquid phase method 2 O 3 And the insulating coating layer is 20nm in insulating thickness.
(2) Putting 200mg of silane coupling agent into 190ml of ethanol and 10ml of water, adding 20g of BN flake powder, ultrasonically stirring for 6 hours, filtering and drying to obtain modified BN powder;
(3) Adding 1.2g of epoxy resin and 2.57g of BN flake powder with the diameter to thickness ratio of 1000 (the volume ratio of boron nitride filled in the epoxy resin is 40 percent) into the metal soft magnetic powder, mixing and granulating with 20ml of ethyl acetate, and sieving with 40 meshes and 200 meshes after the organic solvent is completely volatilized to obtain soft magnetic composite powder with the grain size interval of 40 meshes-200 meshes.
(4) And (3) placing the granulated powder in a mould, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(5) And (3) placing the molded inductor in argon gas at 550 ℃ for annealing for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
Example 4
The embodiment provides a method for manufacturing the metal magnetic powder core, which comprises the following steps:
(1) Weighing 100g of soft metal powder with D50=40 μm, and preparing Al by gas phase method or liquid phase method 2 O 3 And the insulating coating layer is 20nm in insulating thickness.
(2) Putting 200mg of silane coupling agent into 190ml of ethanol and 10ml of water, adding 20g of BN flake powder, ultrasonically stirring for 6 hours, filtering and drying to obtain modified BN powder;
(3) Adding 0.8g of epoxy resin and 2.57g of BN flake powder with the diameter-thickness ratio of 1000 (the volume ratio of boron nitride filled in the epoxy resin is 60 percent) into the metal soft magnetic powder, mixing and granulating with 20ml of ethyl acetate, and sieving with 40 meshes and 200 meshes after the organic solvent is completely volatilized to obtain soft magnetic composite powder with the grain size interval of 40 meshes-200 meshes.
(4) And (3) placing the granulated powder in a mould, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(5) And (3) placing the molded inductor in argon gas at 550 ℃ for annealing for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
Example 5
The embodiment provides a method for manufacturing the metal magnetic powder core, which comprises the following steps:
(1) Weighing 100g of soft metal powder with D50=20 μm, and preparing Al by gas phase method or liquid phase method 2 O 3 And the insulating coating layer is 20nm in insulating thickness.
(2) Putting 200mg of silane coupling agent into 190ml of ethanol and 10ml of water, adding 20g of BN flake powder, ultrasonically stirring for 6 hours, filtering and drying to obtain modified BN powder;
(3) Adding 0.8g of epoxy resin and 2.57g of BN flake powder with the diameter-thickness ratio of 1000 (the volume ratio of boron nitride filled in the epoxy resin is 60 percent) into the metal soft magnetic powder, mixing and granulating with 20ml of ethyl acetate, and sieving with 40 meshes and 200 meshes after the organic solvent is completely volatilized to obtain soft magnetic composite powder with the grain size interval of 40 meshes-200 meshes.
(4) And (3) placing the granulated powder in a mould, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(5) And (3) placing the molded inductor in argon gas at 550 ℃ for annealing for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
Comparative example 1
(1) Weighing 100g of soft metal powder with D50=20 μm, and preparing Al by gas phase method or liquid phase method 2 O 3 And the insulating coating layer has an insulating thickness of 20nm.
(2) And 2g of epoxy resin and 20ml of ethyl acetate are added into the metal soft magnetic powder for mixing and granulation, and after the organic solvent is completely volatilized, the mixture is sieved by 40-mesh and 200-mesh sieves to obtain soft magnetic composite powder, wherein the particle size interval is 40-200 meshes.
(3) And (3) placing the granulated powder in a mold, adjusting the pressure of equipment to 1800Mpa, and pressing to obtain the soft magnetic composite magnetic powder core.
(4) And (3) placing the molded inductor in argon gas at 550 ℃ for annealing for 1 hour to obtain the required high-thermal-conductivity soft magnetic composite material.
As shown in fig. 1, which is a schematic structural diagram of the present invention, the flaky thermal conductive powder 4 is uniformly distributed in the organic resin binder 5 and is bridged to form a thermal conductive network, and the thermal conductive network is wrapped around the metal soft magnetic particles 2 coated with the insulating coating layer 3 to form a network-shaped thermal conductive soft magnetic composite material. As shown in FIG. 2, the soft magnetic particles are uniformly coated with a layer of Al 2 O 3 And an insulating coating layer. The sheet-shaped heat-conducting powder used in the present invention is shown in fig. 3.
According to the formula of equivalent medium
The thermal conductivity of the soft magnetic composite material can be calculated, wherein lambda is c Is a composite material heatConductivity, λ 1 Is the resin matrix thermal conductivity, λ 2 Is the magnetic powder thermal conductivity, V is the magnetic powder packing volume fraction, k R Is the thermal resistance factor. According to the calculation result, the soft magnetic composite material prepared by the scheme has the beneficial effect of improving the thermal conductivity.
Table 1 calculation of thermal conductivity results for examples and comparative examples
| Sample (I) | Calculating the thermal conductivity k e (W·m -1 ·K -1 ) |
| Example 1 | 9.2 |
| Example 2 | 9.3 |
| Example 3 | 8.1 |
| Example 4 | 10.7 |
| Example 5 | 9.6 |
| Comparative example 1 | 7.6 |
It will be understood by those skilled in the art that the foregoing is only an exemplary embodiment of the present invention, and is not intended to limit the invention to the particular forms disclosed, since various modifications, substitutions and improvements within the spirit and scope of the invention are possible and within the scope of the appended claims.
Claims (10)
1. The preparation method of the metal soft magnetic composite material is characterized by comprising the following steps:
(1) Adding the heat-conducting flake powder into a coupling agent solution to obtain modified heat-conducting flake powder; the heat-conducting flaky powder is nitride, carbide or oxide;
(2) Adding resin and the modified heat-conducting flaky powder obtained in the step (1) into metal soft magnetic powder, wherein the metal soft magnetic powder is coated by an insulating layer, and then adding a volatile organic solvent for mixing and granulating; the metal soft magnetic powder is bridged by heat-conducting flaky powder, and the resin is dispersed in pores of the system to obtain metal soft magnetic composite particles;
(3) Pressing and molding the metal soft magnetic composite particles obtained in the step (2) to obtain a metal soft magnetic composite material green body; and heating and curing the green body to obtain the metal soft magnetic composite material.
2. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein in the step (1), the nitride is BN, alN or Si 3 N 4 (ii) a The carbide is SiC or diamond; the oxide is Al 2 O 3 ZnO or BeO.
3. The method for preparing a metallic soft magnetic composite material according to claim 1 or 2, wherein in the step (1), the metallic soft magnetic powder is at least one of carbonyl iron powder, fe-based amorphous alloy powder, fe-based nanocrystalline powder, feNiMo alloy powder, feSi alloy powder, feSiAl alloy powder, and fesicror alloy powder.
4. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein the resin is at least one of an epoxy resin, a silicone resin, and a phenol resin.
5. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein the insulating layer is Al 2 O 3 Or MgO.
6. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein the coupling agent is at least one of an amino coupling agent, a mercapto coupling agent, a vinyl coupling agent, an epoxy coupling agent, a cyano coupling agent, and a methacryloxy silane coupling agent.
7. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein the heating temperature in the step (3) is 150 ℃ to 700 ℃.
8. The method for preparing a metallic soft magnetic composite material according to claim 1, wherein in the step (3), the metallic soft magnetic composite particles are compressed into a ring-shaped structure.
9. Metallic soft magnetic composite material obtainable by the process according to any one of claims 1 to 8.
10. Use of the metallic soft magnetic composite material according to claim 9 for inductors or soft magnetic composite cores.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211625783.3A CN115831520A (en) | 2022-12-14 | 2022-12-14 | High-thermal-conductivity metal soft magnetic composite material and preparation method and application thereof |
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| CN202211625783.3A CN115831520A (en) | 2022-12-14 | 2022-12-14 | High-thermal-conductivity metal soft magnetic composite material and preparation method and application thereof |
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