CN111354528A - Phosphoric acid-silane co-coated metal soft magnetic composite material and preparation method thereof - Google Patents
Phosphoric acid-silane co-coated metal soft magnetic composite material and preparation method thereof Download PDFInfo
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- CN111354528A CN111354528A CN202010264749.2A CN202010264749A CN111354528A CN 111354528 A CN111354528 A CN 111354528A CN 202010264749 A CN202010264749 A CN 202010264749A CN 111354528 A CN111354528 A CN 111354528A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
- H01F1/26—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated by macromolecular organic substances
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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Abstract
The invention discloses a phosphoric acid-silane co-coated metal soft magnetic composite material, which takes metal soft magnetic powder as a raw material, firstly phosphorizes the soft magnetic powder, and then transfers the soft magnetic powder into silane hydrolysate, thereby forming a metal phosphate and silane co-coated layer on the surface of the powder. According to the invention, the metal phosphate and silane insulation coating layer is generated on the surface of the metal soft magnetic powder through the phosphoric acid and silane co-coating process, so that the temperature resistance of the material can be greatly improved, and compared with the existing material, the material can keep lower loss at higher temperature.
Description
Technical Field
The invention relates to a soft magnetic composite material and a preparation method thereof, in particular to a method for preparing the soft magnetic composite material by pressing and molding after forming an insulating layer on the surface of metal soft magnetic particles through co-coating by phosphoric acid and silane.
Background
Magnetic materials are widely used in the fields of electronics, computers and communications, and now have drastically changed our lives. At present, the magnetic powder core has relatively high magnetic flux density, good temperature stability and mechanical impact adaptability, so that the magnetic powder core is widely applied to micromotors, inductive devices, quick driving and pulse transformers in the fields of aviation, automobiles, household appliances and the like. However, the conventional magnetic materials such as silicon steel sheets have some disadvantages in the use process, and the conventional soft magnetic materials such as silicon steel sheets have high energy loss due to rapid rise of eddy current under a high-frequency condition, so that the temperature of the motor is increased and the efficiency is reduced. Based on the reduction of the eddy current phenomenon and the improvement of the energy efficiency of the soft magnetic material, the development of a novel green energy-saving soft magnetic material as a core of an electric device is imminent. Meanwhile, with the development of electronic components and electronic devices, electrical appliances are increasingly developed in the direction of integration and miniaturization, which requires a magnetic material having higher magnetic permeability and smaller loss. With the trend of miniaturization of electrical equipment and the solution of the above energy problems, the demand for various types of micro magnetic powder cores is increasingly remarkable. In order to develop more energy efficient, smaller volume, and lighter weight powder cores, the development of new soft magnetic composite materials (SMCs) is the current focus. SMCs materials, sometimes referred to as "insulation coated magnetic powder cores", are a new type of iron-based powder soft magnetic materials that have evolved gradually in recent years. The design idea of the material is to combine the two characteristics of high saturation induction density of the iron core and huge resistivity of the insulating substance to exert the advantages of the two characteristics.
The insulating coating layer of SMCs is composed of organic polymer and inorganic oxide, such as organic silicon resin, phenolic resin and phosphate, and the inorganic insulating coating layer is made of MgO or SiO2、Al2O3And the like. However, these materials have their own advantages and disadvantages, such as the inability of the composite materials of the organic insulating layer to operate at high temperatures, or even to be heat treated at higher temperatures. The inorganic insulating layer has poor cohesiveness and poor formability, which results in low mechanical strength of the composite material. At present, a lot of researches are carried out on the materials, and a lot of related scientific research papers and patents are also carried out on the materials, but on the whole, the materials have many unsolved problems, the comprehensive performance of the materials also has a space for further improving, and the materials have wide development and research prospects.
Disclosure of Invention
The invention aims to provide a phosphoric acid-silane co-coated metal soft magnetic composite material with high frequency, low loss and high magnetic induction strength and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
a phosphoric acid-silane co-coated metal soft magnetic composite material is prepared by using metal soft magnetic powder as raw material, firstly phosphorizing the soft magnetic powder, and then transferring the soft magnetic powder into silane hydrolysate, thereby forming a metal phosphate and silane co-coating layer on the surface of the powder.
The preparation method comprises the following steps: adding the cleaned metal soft magnetic powder into a phosphoric acid solution, and drying in a drying oven at 40-80 ℃ to obtain pretreated soft magnetic powder; adding the pretreated soft magnetic powder into silane hydrolysate, drying, adding a binder and a lubricant into the powder, performing compression molding under the condition of 1000-2500 MPa, placing in a nitrogen or argon atmosphere, and standing at the temperature of 200-1000 ℃ for 30-400 min to obtain the phosphoric acid-silane co-coated metal soft magnetic composite material.
Further, the silane hydrolysate is an alcohol solution, an aqueous solution or an alcohol-water mixed solution of silane.
Further, H in the phosphoric acid solution3PO4The content is 0.05 wt% -2 wt% of the metal soft magnetic powder, and the silane used in the silane hydrolysate is 0.1 wt% -5 wt% of the metal soft magnetic powder.
Further, the silane is one or more of gamma- (2.3 glycidoxy) propyl trimethoxy silane, gamma-glycidoxypropyl trimethoxy silane, gamma-methacryloxypropyl trimethoxy silane, gamma-aminopropyl triethoxy silane and 3-aminopropyl triethoxy silane.
Further, the metal soft magnetic powder is one of the following: one or more of pure iron powder, iron-silicon-aluminum powder, iron-nickel alloy powder, iron-nickel-molybdenum alloy powder, iron-silicon-chromium alloy powder, iron-silicon alloy powder and amorphous powder, and the preferable particle size is 3-500 mu m. Still further, ferrosilicon aluminum powder is preferable.
Furthermore, the binder is one or more of sodium silicate, lithium silicate, aluminum silicate, epoxy resin and silicon resin, the dosage of the binder is 0-4% of the mass of the metal soft magnetic powder, and if 0 is taken, the binder is not added.
Further, the lubricant is one or more of lithium stearate, calcium stearate, magnesium stearate, nickel stearate, zinc stearate, dimethyl polysiloxane, molybdenum disulfide lithium base grease, aluminum calcium complex soap base grease, SPANJAARD chromium grease, SPANJAARD nickel grease and SPANJAARD copper grease.
Furthermore, the addition amount of the lubricant is 0.01 wt% -1 wt% of the metal soft magnetic powder.
Further, the pressing forming is carried out for 20-40 s under the condition of 500-800 MPa, and then for 30-60 s under the condition of 1000-2500 MPa.
Further, the heat treatment is: the heating rate is 2-5 ℃/min, the temperature is raised to 200-.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention generates the metal phosphate and silane insulation coating layer on the surface of the metal soft magnetic powder through the phosphoric acid and silane co-coating process, the coating uniformity is greatly improved, the process is simple, the operation is convenient, the cost is low, the production efficiency is high, and the method is suitable for industrial large-scale production. (2) The SMCs are mainly formed by compression molding, and the shapes of the SMCs can be complicated and diversified, while the conventional silicon steel sheets are mainly formed by lamination, so that the SMCs are relatively easy to process into complicated parts. (3) Many experimental methods show that the loss is difficult to keep low at higher temperature, and the temperature resistance of the coating is greatly improved by introducing a metal phosphate layer and a silane insulating coating layer on the surface of the metal. The composite material of the invention is widely applied to the aspects of inductors, motors, sensors, low-frequency filters, electromagnetic driving devices, magnetic field shielding and the like.
Drawings
FIG. 1 is an SEM image of a phosphated-silane co-coated sendust.
FIG. 2 is a graph of the magnetic loss at 100kHz, 100mT for phosphated-silane co-coated samples treated with heat at 700 deg.C, 720 deg.C, 740 deg.C, and 760 deg.C.
FIG. 3 is SEM image of phosphated-silane co-coated pure iron powder
FIG. 4 is a graph of the magnetic loss at 50mT, 45kHz for phospho-silane co-coated samples at different concentrations of phosphoric acid (phosphoric acid concentrations of 0.05%, 0.1%, 0.15%, and 0.2%).
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1
Weighing 12g of iron-silicon-aluminum powder, adding 0.05 wt% of phosphoric acid into the iron-silicon-aluminum powder, uniformly performing ultrasonic treatment, and drying in a drying oven at 60 ℃ for 30min to obtain pretreated 12g of iron-silicon-aluminum powder; adding the pretreated Fe-Si-Al powder into hydrolysate containing 0.1 wt% of silane, ultrasonically treating for 1min, uniformly mixing, and drying in a drying oven at 60 deg.C for 30min to obtain 12g of finally-treated FeAdding 0.05g of zinc stearate into the silicon aluminum powder, grinding and uniformly mixing the silicon aluminum powder and the zinc stearate, then pressing the mixture into a ring (9.7mm OD × 5.6mm ID × 3.4.4 mm tall) at the temperature of 25 ℃ and 1900MPa, carrying out heat treatment on the compression ring for 60 minutes at the temperature of 720 ℃ in a nitrogen atmosphere to obtain a soft magnetic composite material, subsequently carrying out performance test on the winding of the compression ring, wherein 18 turns of each of a primary coil and a secondary coil are measured by a radio frequency impedance analyzer to obtain a real part of complex permeability of about 56 under the condition of 1MHz, and the total loss of 380kW/m is measured by an alternating current B-H instrument under the conditions of 1003。
Example 2
Weighing 12g of ferrosilicon aluminum powder, adding 1 wt% of phosphoric acid into the ferrosilicon aluminum powder, uniformly performing ultrasonic treatment, placing the mixture in a drying box for drying at 60 ℃ for 30min to obtain 12g of pretreated ferrosilicon aluminum powder, adding the pretreated ferrosilicon aluminum powder into hydrolysate containing 3 wt% of silane, uniformly mixing the mixture by ultrasonic treatment for 1min, placing the mixture in the drying box for drying at 60 ℃ for 30min to obtain 12g of finally-treated ferrosilicon aluminum powder, adding 0.05g of zinc stearate, uniformly grinding and mixing the mixture, pressing the mixture into a ring (9.7mm OD × 5.6.6 mm ID × 3.4.4 mm tall) at 25 ℃ and 1900MPa, performing heat treatment on a pressure ring at 720 ℃ for 60 min in a nitrogen atmosphere to obtain a soft magnetic composite material, performing performance test on subsequent winding of the pressure ring, measuring 18 turns of a primary coil and a secondary coil, measuring a complex permeability real part of about 43 MHz under 1MHz by using a radio frequency impedance analyzer, and measuring the total loss of 150 kW/m/kHz by using an alternating current B3。
Example 3
Weighing 12g of ferrosilicon aluminum powder, adding 2 wt% of phosphoric acid into the ferrosilicon aluminum powder, uniformly performing ultrasonic treatment, drying the mixture in a drying oven at 60 ℃ for 30min to obtain 12g of pretreated ferrosilicon aluminum powder, adding the pretreated ferrosilicon aluminum powder into hydrolysate containing 5 wt% of silane, uniformly mixing the mixture by ultrasonic treatment for 1min, drying the mixture in the drying oven at 60 ℃ for 30min to obtain 12g of finally-treated ferrosilicon aluminum powder, adding 0.05g of zinc stearate, grinding and uniformly mixing the mixture, pressing the mixture into a ring (9.7mm OD × 5.6.6 mm ID × 3.4.4 mm tall) at 25 ℃ and 1900MPa, performing heat treatment on a pressure ring at 720 ℃ in a nitrogen atmosphere for 60 min to obtain a soft magnetic composite material, and performing performance test on winding wires of the pressure ring to obtain 18 turns of a primary coil and a secondary coil, wherein the complex permeability real part under 1MHz of a radio frequency impedance analyzer is 3532.4About 33, and the total loss is 234kW/m measured by an alternating current B-H instrument under the conditions of 100mT and 100kHz3。
Example 4
Weighing 12g of iron powder, adding 0.05 wt% of phosphoric acid into the iron powder, performing ultrasonic homogenization, then placing the mixture in a drying box for drying at 60 ℃ for 30min to obtain pretreated 12g of iron powder, adding the pretreated sendust powder into hydrolysate containing 0.3 wt% of silane, performing ultrasonic homogenization for 1min, then placing the mixture in the drying box for drying at 60 ℃ for 30min to obtain finally treated 12g of iron powder, then adding 0.05g of zinc stearate, grinding and mixing the mixture uniformly, then pressing the mixture into rings at 25 ℃ and 1200MPa (12.7mm OD × 7.6.6 mm ID × 3.4.4 mm tall), performing heat treatment on a pressure ring at 500 ℃ in a nitrogen atmosphere for 60 min to obtain a soft magnetic composite material, and performing performance test on subsequent pressure rings to obtain 20 turns of a primary coil and a secondary coil, wherein the effective permeability is about 126 by using an LCR meter, and the total loss is 90W/Kg by using an alternating current B-H instrument under the conditions of 50mT and 100 kHz.
Example 5
Weighing 12g of iron powder, adding 0.1 wt% of phosphoric acid into the iron powder, performing ultrasonic homogenization, then placing the mixture in a drying box for drying at 60 ℃ for 30min to obtain pretreated 12g of iron powder, adding the pretreated sendust powder into hydrolysate containing 0.3 wt% of silane, performing ultrasonic homogenization for 1min, then placing the mixture in the drying box for drying at 60 ℃ for 30min to obtain finally treated 12g of iron powder, then adding 0.05g of zinc stearate, grinding and mixing the mixture uniformly, then pressing the mixture into rings at 25 ℃ and 1200MPa (12.7mm OD × 7.6.6 mm ID × 3.4.4 mm tall), performing heat treatment on a pressure ring at 500 ℃ in a nitrogen atmosphere for 60 min to obtain a soft magnetic composite material, and performing performance test on subsequent pressure rings to obtain 20 turns of a primary coil and a secondary coil, wherein the effective permeability is about 115 by using an LCR meter, and the total loss is 249W/Kg by using an alternating current B-H instrument under the conditions of 50mT and 100 kHz.
Example 6
Weighing 12g of iron powder, adding 0.2 wt% of phosphoric acid into the iron powder, performing ultrasonic homogenization, then placing the mixture in a drying box for drying at 60 ℃ for 30min to obtain pretreated 12g of iron powder, adding the pretreated sendust powder into hydrolysate containing 0.3 wt% of silane, performing ultrasonic homogenization for 1min, then placing the mixture in the drying box for drying at 60 ℃ for 30min to obtain finally treated 12g of iron powder, then adding 0.05g of zinc stearate, grinding and mixing the mixture uniformly, then pressing the mixture into rings at 25 ℃ and 1200MPa (12.7mm OD × 7.6.6 mm ID × 3.4.4 mm tall), performing heat treatment on a pressure ring at 500 ℃ in a nitrogen atmosphere for 60 min to obtain a soft magnetic composite material, and performing performance test on subsequent pressure rings to obtain a winding wire, wherein the effective permeability is about 103 according to the measurement of 20 turns of a primary coil and a secondary coil, and the total loss is 365W/Kg according to the measurement of an alternating current B-H instrument under the conditions of 50mT and 100 kHz.
Claims (7)
1. The phosphoric acid-silane co-coated metal soft magnetic composite material is characterized in that metal soft magnetic powder is used as a raw material of the soft magnetic composite material, the soft magnetic powder is firstly phosphorized, and then the soft magnetic powder is transferred into silane hydrolysate, so that a metal phosphate and silane co-coated layer is formed on the surface of the powder.
2. The phosphoric acid-silane co-coated metal soft magnetic composite material according to claim 1, wherein the specific preparation method comprises: adding the cleaned metal soft magnetic powder into a phosphoric acid solution, and drying in a drying oven at 40-80 ℃ to obtain pretreated soft magnetic powder; adding the pretreated soft magnetic powder into silane hydrolysate, drying, adding a binder and a lubricant into the powder, performing compression molding under the condition of 1000-2500 MPa, placing in a nitrogen or argon atmosphere, and standing at the temperature of 200-1000 ℃ for 30-400 min to obtain the phosphoric acid-silane co-coated metal soft magnetic composite material.
3. The phosphoric acid-silane co-coated metal soft magnetic composite material according to claim 2, wherein the silane hydrolysate is an alcohol solution, an aqueous solution or an alcohol-water mixed solution of silane.
4. The phosphoric acid-silane co-coated metal soft magnetic composite material according to claim 2, wherein H is contained in the phosphoric acid solution3PO4The content is 0.05 wt% -2 wt% of the metal soft magnetic powder, and the silane used in the silane hydrolysate is 0.1 wt% -5 wt% of the metal soft magnetic powder.
5. The phosphoric acid-silane co-coated metal soft magnetic composite material according to claim 2, wherein the silane is one or more of gamma- (2.3 glycidoxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, and 3-aminopropyltriethoxysilane.
6. The phosphoric acid-silane co-coated metal soft magnetic composite material according to claim 2, wherein the metal soft magnetic powder is one of the following: one or more of pure iron powder, iron-silicon-aluminum powder, iron-nickel alloy powder, iron-nickel-molybdenum alloy powder, iron-silicon-chromium alloy powder, iron-silicon alloy powder and amorphous powder, and the preferable particle size is 3-500 mu m.
7. The phosphoric acid-silane co-coated metal soft magnetic composite material as claimed in claim 2, wherein the binder is one or more of sodium silicate, lithium silicate, aluminum silicate, epoxy resin and silicone resin, and the amount of the binder is 0-4% of the mass of the metal soft magnetic powder.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112475288A (en) * | 2020-09-30 | 2021-03-12 | 东睦新材料集团股份有限公司 | Preparation method of soft magnetic composite material for stator |
| CN112908677A (en) * | 2021-02-08 | 2021-06-04 | 浙江工业大学 | Preparation method of high-permeability low-loss integrated inductance material |
| CN112958779A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of FeBP amorphous soft magnetic powder and magnetic powder core thereof |
| CN113380483A (en) * | 2021-06-10 | 2021-09-10 | 横店集团东磁股份有限公司 | Composite soft magnetic material and preparation method thereof |
| CN113470916A (en) * | 2021-07-05 | 2021-10-01 | 中国科学院宁波材料技术与工程研究所 | Fe-Si-Al soft magnetic powder core and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112475288A (en) * | 2020-09-30 | 2021-03-12 | 东睦新材料集团股份有限公司 | Preparation method of soft magnetic composite material for stator |
| CN112958779A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of FeBP amorphous soft magnetic powder and magnetic powder core thereof |
| CN112908677A (en) * | 2021-02-08 | 2021-06-04 | 浙江工业大学 | Preparation method of high-permeability low-loss integrated inductance material |
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Application publication date: 20200630 |