CN116037914A - Preparation method of high-temperature-resistant metal soft magnetic composite material - Google Patents
Preparation method of high-temperature-resistant metal soft magnetic composite material Download PDFInfo
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- 239000002184 metal Substances 0.000 title claims abstract description 61
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000006247 magnetic powder Substances 0.000 claims abstract description 112
- 238000002161 passivation Methods 0.000 claims abstract description 53
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 36
- 238000009413 insulation Methods 0.000 claims abstract description 35
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- 238000005260 corrosion Methods 0.000 claims abstract description 21
- 230000005764 inhibitory process Effects 0.000 claims abstract description 20
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 19
- 230000008878 coupling Effects 0.000 claims abstract description 18
- 238000010168 coupling process Methods 0.000 claims abstract description 18
- 238000005859 coupling reaction Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000009736 wetting Methods 0.000 claims abstract description 18
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- 238000002156 mixing Methods 0.000 claims description 27
- 239000003822 epoxy resin Substances 0.000 claims description 23
- 229920000647 polyepoxide Polymers 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000007822 coupling agent Substances 0.000 claims description 11
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 10
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- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000003960 organic solvent Substances 0.000 claims description 10
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 235000015393 sodium molybdate Nutrition 0.000 claims description 8
- 239000011684 sodium molybdate Substances 0.000 claims description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 8
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 7
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 7
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- TZYRSLHNPKPEFV-UHFFFAOYSA-N 2-ethyl-1-butanol Chemical compound CCC(CC)CO TZYRSLHNPKPEFV-UHFFFAOYSA-N 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 5
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- -1 glycidyl ester Chemical class 0.000 claims description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 150000004645 aluminates Chemical class 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- BIOOACNPATUQFW-UHFFFAOYSA-N calcium;dioxido(dioxo)molybdenum Chemical compound [Ca+2].[O-][Mo]([O-])(=O)=O BIOOACNPATUQFW-UHFFFAOYSA-N 0.000 claims description 3
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 3
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 239000005696 Diammonium phosphate Substances 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 2
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 2
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 2
- 239000006012 monoammonium phosphate Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 claims description 2
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- 150000008065 acid anhydrides Chemical class 0.000 claims 1
- 125000001931 aliphatic group Chemical group 0.000 claims 1
- 230000002401 inhibitory effect Effects 0.000 claims 1
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 claims 1
- 238000007873 sieving Methods 0.000 abstract description 9
- 239000000696 magnetic material Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 56
- 230000000052 comparative effect Effects 0.000 description 9
- 230000035699 permeability Effects 0.000 description 9
- 238000000576 coating method Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004844 aliphatic epoxy resin Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910015372 FeAl Inorganic materials 0.000 description 1
- 229910002555 FeNi Inorganic materials 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004845 glycidylamine epoxy resin Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
Classifications
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/02—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions
- C23C22/03—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using non-aqueous solutions containing phosphorus compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention belongs to the technical field of metal soft magnetic materials, and discloses a preparation method of a metal soft magnetic composite material with strong high-temperature magnetic stability, which comprises the following steps: 1) Adding metal soft magnetic powder into a passivation corrosion inhibition solution for treatment, washing with water, and drying to obtain soft magnetic powder material A with an inorganic passivation insulating coating layer formed on the surface; 2) Adding the soft magnetic powder into the coupling wetting solution for treatment, and taking out and drying after finishing interface modification to obtain soft magnetic powder B; 3) Adding the soft magnetic powder B into an insulation additive solution containing superfine inorganic oxide particles for organic insulation treatment to prepare soft magnetic powder slurry; 4) Granulating the slurry serving as a raw material, drying and sieving after preparing magnetic powder coarse materials to obtain the high-temperature-resistant metal soft magnetic composite material. The high-temperature magnetic stability and mechanical property of the soft magnetic composite material are improved, and the components taking the soft magnetic composite material as the material have excellent mechanical property and high-temperature magnetic stability.
Description
Technical Field
The invention belongs to the technical field of metal soft magnetic materials, and particularly relates to a preparation method of a high-temperature-resistant metal soft magnetic composite material with high-temperature magnetic stability.
Background
The metal soft magnetic material has the characteristics of low coercive force, high magnetic permeability and low eddy current loss, so that the metal soft magnetic material is easy to magnetize and demagnetize, and is widely applied to electrical equipment such as electronics, communication, power switches and the like, and electronic terminal products continuously develop towards miniaturization, integration, high frequency, high power and the like, and higher requirements are put forward on the performance of the soft magnetic material.
The soft magnetic composite material is characterized in that a layer of insulating substance is coated on the surface of metal soft magnetic powder, so that the resistance is improved, the eddy current loss is reduced, and the process of coating the insulating layer by the metal soft magnetic powder is a key step in the preparation process of the soft magnetic composite material. In recent years, the application of double insulation coating of inorganic substances and organic substances has been increasing, and the main reasons thereof are as follows: 1) Inorganic materials have excellent high temperature resistance, but have poor formability; 2) The soft magnetic composite material coated by the organic matters is easy to form, but has poor high temperature resistance, poor magnet insulation performance after high temperature annealing and reduced reliability.
Although the double insulation coating of inorganic matters and organic matters can overcome some defects of the inorganic matters and the organic matters, the magnetic performance of the electronic passive component prepared by the soft magnetic composite material prepared by the process at present is still reduced after the reflow soldering temperature (220-280 ℃), the magnetic performance is mainly represented by the reduction of magnetic conductivity, and the insulation performance is poor due to the following reasons: the organic insulating layer of the soft magnetic composite powder can be partially aged and decomposed at high temperature under the high-frequency use condition, so that the magnetic permeability of the organic insulating layer is reduced, the high-temperature stability of the magnetic component is poor, and the use reliability is reduced.
Therefore, on the premise of ensuring the advantages of double insulation cladding of the soft magnetic composite material, how to solve the defects and drawbacks existing in the prior art becomes a technical problem to be solved by the technicians in the field.
Disclosure of Invention
In summary, the invention aims to solve the technical problems that the high-temperature magnetic stability of the metal soft magnetic composite powder prepared by the existing double-insulation coating process is poor, and the organic insulation layer is easy to be partially aged and decomposed due to high temperature under the high-frequency use state, so that the magnetic permeability of the soft magnetic composite powder is reduced, and further the passive electric element manufactured by the organic insulation layer is poor in stability and low in reliability, and provides an improved preparation method of the high-temperature-resistant metal soft magnetic composite material.
In order to solve the technical defects, the invention adopts the technical scheme that the preparation method of the high-temperature-resistant metal soft magnetic composite material is characterized by comprising the following steps:
step 1: according to parts by weight, 100 parts of metal soft magnetic powder is added into passivation corrosion inhibition solution prepared by mixing 0.1-2.5 parts of phosphate, 0.01-1.0 part of molybdate, 0.1-2.5 parts of deionized water and 10-30 parts of organic solvent A, and uniformly stirring is carried out, powder is filtered after passivation reaction is completed, the powder is washed by water until PH=6-7 of supernatant fluid, and then dried, thus obtaining soft magnetic powder A with an inorganic passivation insulating coating layer formed on the surface.
Step 2: and adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.01-1.00 parts of coupling agent, 2.5-7.5 parts of deionized water and 10-30 parts of organic solvent B, uniformly stirring, taking out after finishing interface modification, and drying to obtain the soft magnetic powder B.
Step 3: the prepared soft magnetic powder B is added into an insulating additive solution prepared by mixing 0.50 to 3.00 parts of epoxy resin, 0.01 to 0.06 part of resin curing agent, 0.10 to 0.50 part of superfine inorganic oxide particles and 10 to 30 parts of diluent, and the mixture is stirred uniformly to prepare soft magnetic powder slurry.
Step 4: granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials, wherein the inner layer of the metal soft magnetic powder coarse materials is provided with an inorganic passivation insulating coating layer, and the outer layer of the metal soft magnetic powder coarse materials is provided with an organic insulating coating layer containing superfine inorganic oxide particles, and the metal soft magnetic powder coarse materials are dried and then pass through a standard sieve with more than 300 meshes, so that the high-temperature-resistant metal soft magnetic composite material is obtained.
Further, the metal soft magnetic powder includes, but is not limited to, one or more of carbonyl iron powder, atomized iron powder, feSi-based soft magnetic powder, feSiAl-based soft magnetic powder, feAl-based soft magnetic powder, feNi-based soft magnetic powder, feNiMo-based soft magnetic powder, iron-based amorphous powder, and nanocrystalline powder.
Further, the phosphate in the passivating corrosion inhibition solution includes, but is not limited to, one or more of diammonium phosphate, monoammonium phosphate, sodium dihydrogen phosphate, calcium hydrogen phosphate, zinc phosphate, and phosphoric acid.
Further, the molybdate in the passivating corrosion inhibition solution includes, but is not limited to, one or more of zinc molybdate, calcium molybdate, sodium molybdate.
Further, the organic solvent A in the passivation and corrosion inhibition solution and the organic solvent B in the coupling and wetting solution and the diluent in the insulating additive solution are the same or different in composition, and all the three comprise one or more of alcohol, acetone, butanone and ethyl butanol.
Further, the coupling agent in the coupling wetting solution comprises one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent.
Further, the epoxy resin in the insulation additive solution includes, but is not limited to, one or more of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, and aliphatic epoxy resin.
Further, the resin curing agent in the insulation additive solution includes, but is not limited to, one or more of an anhydride curing agent, an amine curing agent, and an imidazole curing agent.
Further, the ultrafine inorganic oxide particles in the insulation additive solution include, but are not limited to, siO 2 、MgO 2 、TiO 2 One or more of the following.
Further, the granularity of the superfine inorganic oxide particles in the insulating additive solution is selected to be 1-50 nm.
The beneficial effects of the invention are as follows: before organic insulation coating, firstly, metal soft magnetic powder is subjected to passivation and inorganic insulation coating treatment through a passivation corrosion inhibition solution, so that the surface of the metal soft magnetic powder reacts with the passivation corrosion inhibition solution to form a layer of inorganic passivation insulating film, the insulation resistance among powder particles is effectively improved, and hysteresis loss and eddy current loss are greatly reduced. In addition, the soft magnetic powder material A after passivation insulation treatment is easier to be modified and dispersed by the surface of the coupling wetting solution, so that the crosslinking of organic insulation components in the soft magnetic powder material B and an insulation additive solution is obviously improved, the bonding strength between an inorganic passivation insulation coating layer on the inner side of the soft magnetic composite powder material and an organic insulation coating layer on the outer side of the soft magnetic composite powder material is improved, the mechanical property of the organic insulation coating layer on the outer side of the soft magnetic composite powder material under a high-frequency use state is ensured, and the temperature resistance is strong. Moreover, after coupling and wetting, the uniform distribution of the added superfine inorganic oxide particles in the organic insulating layer is promoted, and the superfine inorganic oxide particles have small influence on the magnetic permeability of the soft magnetic composite material, and meanwhile, due to the pinning effect, the high-temperature magnetic stability and the mechanical property of the soft magnetic composite material are remarkably improved. The test and detection prove that the soft magnetic composite material prepared by the method has excellent mechanical property and high-temperature magnetic stability, still has higher magnetic permeability and better insulating property after reflow soldering temperature (220-280 ℃), can completely meet the high-frequency and high-temperature use of passive electric elements of various application metal soft magnetic composite materials, and remarkably improves the high-temperature magnetic stability and use reliability of the soft magnetic composite material.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
Example 1
According to parts by weight, 100 parts of FeSi6.5 soft magnetic powder is added into a passivation corrosion inhibition solution prepared by mixing 0.5 part of sodium dihydrogen phosphate, 0.1 part of sodium molybdate, 1.0 part of deionized water and 30 parts of ethanol, and the mixture is stirred uniformly at a stirring speed of 60r/min for 120min, powder is filtered after the passivation reaction is completed, the powder is washed until the PH value of the upper layer clear solution is between 6 and 7, and then the powder is dried, the baking temperature is 100 ℃ and the baking time is 120min, so that the soft magnetic powder A with the inorganic passivation insulating coating layer formed on the surface is prepared.
Then, adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.5 part of silane coupling agent, 7.5 parts of deionized water and 30 parts of ethanol, uniformly stirring at a stirring speed of 60r/min for 120min, taking out and drying after finishing interface modification, and baking at a temperature of 100 ℃ for 120min to obtain soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture of 1.00 parts of epoxy resin, 0.02 part of epoxy resin curing agent and 0.5 part of superfine SiO with the particle size of 1-50 nm 2 The particles and 20 parts of ethanol are mixed to prepare insulating additive solution, the insulating additive solution is stirred uniformly, the stirring speed is 60r/min, the stirring time is 120min, and the soft magnetic powder slurry is prepared after fully and uniformly mixing.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at the drying temperature of 80 ℃ for 120min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 1.
Example 2
According to parts by weight, 100 parts of carbonyl iron powder is added into a passivation corrosion inhibition solution prepared by mixing 0.5 part of sodium dihydrogen phosphate, 0.1 part of sodium molybdate, 1.0 part of deionized water and 30 parts of ethanol, the stirring speed is 60r/min, the stirring time is 120min, powder is filtered after the passivation reaction is completed, the powder is washed to the pH value of the upper layer of clear solution between 6 and 7, and then the powder is dried, the baking temperature is 100 ℃ and the baking time is 120min, so that the soft magnetic powder A with the inorganic passivation insulating coating layer formed on the surface is prepared.
Then, adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.5 part of silane coupling agent, 7.5 parts of deionized water and 30 parts of ethanol, uniformly stirring at a stirring speed of 60r/min for 120min, taking out and drying after finishing interface modification, and baking at a temperature of 100 ℃ for 120min to obtain soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture consisting of 1.00 parts of epoxy resin, 0.02 part of epoxy resin curing agent,0.5 part of superfine SiO with the grain diameter of 1-50 nm 2 The particles and 20 parts of ethanol are mixed to prepare insulating additive solution, the insulating additive solution is stirred uniformly, the stirring speed is 60r/min, the stirring time is 120min, and the soft magnetic powder slurry is prepared after fully and uniformly mixing.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at the drying temperature of 80 ℃ for 120min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 2.
Example 3
According to parts by weight, 100 parts of FeSi6.5 soft magnetic powder is added into a passivation corrosion inhibition solution prepared by mixing 0.5 part of sodium dihydrogen phosphate, 0.1 part of sodium molybdate, 1.0 part of deionized water and 30 parts of ethanol, and the mixture is stirred uniformly at a stirring speed of 60r/min for 120min, powder is filtered after the passivation reaction is completed, the powder is washed until the PH value of the upper layer clear solution is between 6 and 7, and then the powder is dried, the baking temperature is 100 ℃ and the baking time is 120min, so that the soft magnetic powder A with the inorganic passivation insulating coating layer formed on the surface is prepared.
Then, adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.5 part of silane coupling agent, 7.5 parts of deionized water and 30 parts of ethanol, uniformly stirring at a stirring speed of 60r/min for 120min, taking out and drying after finishing interface modification, and baking at a temperature of 100 ℃ for 120min to obtain soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture of 1.00 parts of epoxy resin, 0.02 part of epoxy resin curing agent and 0.5 part of superfine TiO with the particle size of 1-50 nm 2 The particles and 20 parts of ethanol are mixed to prepare insulating additive solution, the insulating additive solution is stirred uniformly, the stirring speed is 60r/min, the stirring time is 120min, and the soft magnetic powder slurry is prepared after fully and uniformly mixing.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at the drying temperature of 80 ℃ for 120min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 2.
Example 4
According to parts by weight, 50 parts of FeSiAl soft magnetic powder and 50 parts of atomized iron powder are evenly mixed and added into a passivation corrosion inhibition solution prepared by mixing 2.2 parts of calcium hydrophosphate, 0.03 part of zinc molybdate, 0.4 part of deionized water and 10 parts of acetone, the stirring speed is 120r/min, the stirring time is 60min, powder is filtered after the passivation reaction is completed, the powder is washed to the pH value of an upper layer clear solution between 6 and 7, and then the powder is dried, the baking temperature is 110 ℃ and the baking time is 100min, so that the soft magnetic powder A with the surface provided with a layer of inorganic passivation insulating coating layer is prepared.
Then, adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.05 part of titanate coupling agent, 2.5 parts of deionized water and 25 parts of butanone, uniformly stirring, wherein the stirring speed is 120r/min, the stirring time is 60min, taking out and drying after finishing interface modification, and baking at 110 ℃ for 100min to obtain the soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture of 0.5 part of glycidyl ether epoxy resin, 1.00 parts of aliphatic epoxy resin, 0.01 part of anhydride curing agent and 0.15 part of superfine MgO with the grain diameter of 1-20 nm 2 Uniformly stirring the particles and 15 parts of the insulating additive solution prepared by mixing the ethylbutanol, wherein the stirring speed is 120r/min, the stirring time is 60min, and fully and uniformly mixing to prepare the soft magnetic powder slurry.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at a drying temperature of 100 ℃ for 80min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 4.
Example 5
According to parts by weight, 80 parts of FeNiMo soft magnetic powder and 20 parts of FeAl soft magnetic powder are taken, uniformly mixed and added into a passivation corrosion inhibition solution prepared by mixing 0.3 part of phosphoric acid, 0.4 part of calcium molybdate, 0.6 part of zinc molybdate, 1.5 parts of deionized water and 25 parts of butanone, the stirring speed is 120r/min, the stirring time is 60min, powder is filtered after the passivation reaction is completed, the powder is washed to the pH value of an upper layer of clear solution, and then the solution is dried, the baking temperature is 110 ℃, and the baking time is 100min, so that the soft magnetic powder A with the surface provided with a layer of inorganic passivation insulating coating layer is prepared.
Then, adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.8 part of aluminate coupling agent, 3.5 parts of deionized water and 15 parts of ethyl butanol, uniformly stirring at the stirring speed of 120r/min for 60min, taking out and drying after finishing interface modification, and baking at the temperature of 110 ℃ for 100min to obtain the soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture of 0.5 part of glycidol epoxy resin, 0.06 part of amine curing agent and 0.1 part of superfine TiO with the particle size of 20-40 nm 2 Particles, 0.1 part of superfine SiO with the particle size of 20-40 nm 2 The particles and 10 parts of acetone are mixed to prepare an insulating additive solution, the insulating additive solution is stirred uniformly, the stirring speed is 120r/min, the stirring time is 60min, and the soft magnetic powder slurry is prepared after fully and uniformly mixing.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at a drying temperature of 100 ℃ for 80min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 5.
Example 6
According to parts by weight, 30 parts of nanocrystalline powder and 70 parts of FeNi soft magnetic powder are evenly mixed and then added into passivation corrosion inhibition solution prepared by mixing 1.5 parts of diammonium hydrogen phosphate, 0.2 part of sodium molybdate, 0.1 part of zinc molybdate, 2.3 parts of deionized water and 15 parts of ethyl butanol, the stirring speed is 120r/min, the stirring time is 60min, powder is filtered after passivation reaction is completed, the powder is washed to the pH value of the upper layer of clear solution and then dried, the baking temperature is 110 ℃, and the baking time is 100min, so that the soft magnetic powder A with the surface provided with the inorganic passivation insulating coating layer is prepared.
And then adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.5 part of silane coupling agent, 0.5 part of titanate coupling agent, 5.5 parts of deionized water and 10 parts of acetone, uniformly stirring at the stirring speed of 120r/min for 60min, taking out and drying after finishing interface modification, and baking at the temperature of 110 ℃ for 100min to obtain the soft magnetic powder B with good interface performance and dispersibility.
Then adding the prepared soft magnetic powder B into a mixture of 3 parts of glycidol amine epoxy resin, 0.04 part of imidazole curing agent and 0.15 part of superfine SiO with the particle size of 30-50 nm 2 Particles, 0.2 part of superfine MgO with the particle size of 30-50 nm 2 And uniformly stirring the particles and 25 parts of butanone into an insulating additive solution, wherein the stirring speed is 120r/min, the stirring time is 60min, and the soft magnetic powder slurry is prepared after fully and uniformly mixing.
And granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials with an inorganic passivation insulating coating layer on the inner layer and an organic insulating coating layer containing superfine inorganic oxide particles on the outer layer, and finally drying the prepared soft magnetic powder coarse materials at a drying temperature of 100 ℃ for 80min, and sieving the dried soft magnetic powder coarse materials with a standard sieve of more than 300 meshes to obtain the high-temperature-resistant metal soft magnetic composite material of the embodiment 6.
Comparative example 1
Adding 100 parts of FeSi6.5 metal soft magnetic powder into a passivation corrosion inhibition solution prepared by mixing 0.5 part of sodium dihydrogen phosphate, 0.1 part of sodium molybdate, 1.0 part of deionized water and 30 parts of ethanol, uniformly stirring at a stirring rate of 60r/min for 120min, filtering powder after the passivation reaction is completed, washing the powder until the pH value of the upper layer of clear solution is 6-7, and then drying at a baking temperature of 100 ℃ for 120min; then adding a mixed solution of 0.5 part of silane coupling agent, 7.5 parts of deionized water and 30 parts of ethanol solvent, taking out and drying after stirring completely, wherein the stirring speed is 60r/min, the stirring time is 120min, the baking temperature is 100 ℃, and the baking time is 120min; and adding a mixed solution of 1.00 parts of epoxy resin, 0.02 part of epoxy resin curing agent and 20 parts of ethanol, taking out after stirring completely, granulating, drying, wherein the stirring speed is 60r/min, the stirring time is 120min, the baking temperature is 80 ℃, the baking time is 120min, and sieving through a 300-mesh standard sieve or more after drying to prepare the metal soft magnetic composite material of the comparative example 1.
Comparative example 2
According to parts by weight, 100 parts of carbonyl iron powder is added into a passivation corrosion inhibition solution prepared by mixing 0.5 part of sodium dihydrogen phosphate, 0.1 part of sodium molybdate, 1.0 part of deionized water and 30 parts of ethanol, and the mixture is stirred uniformly at a stirring speed of 60r/min for 120min, powder is filtered after passivation reaction is completed, the powder is washed to a pH value of an upper layer clear solution at 6-7, and then the solution is dried, wherein the baking temperature is 100 ℃ and the baking time is 120min; then adding a mixed solution of 0.5 part of silane coupling agent, 7.5 parts of deionized water and 30 parts of ethanol solvent, taking out and drying after stirring completely, wherein the stirring speed is 60r/min, the stirring time is 120min, the baking temperature is 100 ℃, and the baking time is 120min; and adding a mixed solution of 1.00 parts of epoxy resin, 0.02 part of epoxy resin curing agent and 20 parts of ethanol, taking out after stirring completely, granulating, drying, wherein the stirring speed is 60r/min, the stirring time is 120min, the baking temperature is 80 ℃, the baking time is 120min, and sieving through a 300-mesh standard sieve or more after drying to prepare the metal soft magnetic composite material of the comparative example 2.
The following describes the embodiments of the above six examples and two comparative examples and their powder sample properties in tabular form.
Table 1: powder component proportions of examples 1-6.
Table 2: powder composition ratio tables of comparative examples 1 to 2.
The acceptable mesh granulation powders in examples 1-6 and comparative examples 1-2 were added with 0.5% lubricant, pressed into rings of D1 x D2 x h=20 x 6 x 1.6mm at 500MP, cured at 180 ℃ for 2 hours, tested for permeability μe1, insulation properties IR1, and mechanical strength, and the above-tested magnetic rings were subjected to reflow treatment and then tested for permeability μe2, insulation properties IR2, and mechanical strength again, with the following test data:
table 3: table of sample performance evaluation for examples and comparative examples.
The table data intuitively show that the formula components of the high-temperature-resistant metal soft magnetic composite material of each embodiment of the invention, compared with comparative example samples, the soft magnetic composite material prepared by adopting the technical scheme of each embodiment of the invention has excellent performance.
In summary, before organic insulation coating, the metal soft magnetic powder is firstly passivated and inorganic insulation coated by the passivation corrosion inhibition solution, so that the surface of the metal soft magnetic powder reacts with the passivation corrosion inhibition solution to form a layer of inorganic passivation insulating film, the insulation resistance among powder particles is effectively improved, and hysteresis loss and eddy current loss are greatly reduced. In addition, the soft magnetic powder material A after passivation insulation treatment is easier to be modified and dispersed by the surface of the coupling wetting solution, so that the crosslinking of organic insulation components in the soft magnetic powder material B and an insulation additive solution is obviously improved, the bonding strength between an inorganic passivation insulation coating layer on the inner side of the soft magnetic composite powder material and an organic insulation coating layer on the outer side of the soft magnetic composite powder material is improved, the mechanical property of the organic insulation coating layer on the outer side of the soft magnetic composite powder material under a high-frequency use state is ensured, and the temperature resistance is strong. Moreover, after coupling and wetting, the uniform distribution of the added superfine inorganic oxide particles in the organic insulating layer is promoted, and the superfine inorganic oxide particles have small influence on the magnetic permeability of the soft magnetic composite material, and meanwhile, due to the pinning effect, the high-temperature magnetic stability and the mechanical property of the soft magnetic composite material are remarkably improved. The test and detection prove that the soft magnetic composite material prepared by the method has excellent mechanical property and high-temperature magnetic stability, still has higher magnetic permeability and better insulating property after reflow soldering temperature (220-280 ℃), can completely meet the high-frequency and high-temperature use of passive electric elements of various application metal soft magnetic composite materials, and remarkably improves the high-temperature magnetic stability and use reliability of the soft magnetic composite material.
The foregoing examples are merely for the purpose of illustrating the technical solution of the present invention and are not intended to limit the embodiments of the present invention. Various modifications and alterations of this invention will be apparent to those skilled in the art without departing from the spirit and substance of this invention, and it is intended to cover all such modifications and alterations as fall within the true scope of this invention.
Claims (10)
1. The preparation method of the high-temperature-resistant metal soft magnetic composite material is characterized by comprising the following steps of:
step 1: adding 100 parts of metal soft magnetic powder into a passivation corrosion inhibition solution prepared by mixing 0.1-2.5 parts of phosphate, 0.01-1.0 part of molybdate, 0.1-2.5 parts of deionized water and 10-30 parts of organic solvent A by weight, uniformly stirring, filtering powder after passivation reaction is completed, washing the powder to PH=6-7 of supernatant, and drying to obtain soft magnetic powder A with an inorganic passivation insulating coating layer formed on the surface;
step 2: adding the prepared soft magnetic powder A into a coupling wetting solution prepared by mixing 0.01-1.00 parts of coupling agent, 2.5-7.5 parts of deionized water and 10-30 parts of organic solvent B, uniformly stirring, taking out and drying after finishing interface modification to prepare soft magnetic powder B;
step 3: adding the prepared soft magnetic powder B into an insulating additive solution prepared by mixing 0.50-3.00 parts of epoxy resin, 0.01-0.06 parts of resin curing agent, 0.10-0.50 parts of superfine inorganic oxide particles and 10-30 parts of diluent, and uniformly stirring to prepare soft magnetic powder slurry;
step 4: granulating the prepared soft magnetic powder slurry serving as a raw material to obtain metal soft magnetic powder coarse materials, wherein the inner layer of the metal soft magnetic powder coarse materials is provided with an inorganic passivation insulating coating layer, and the outer layer of the metal soft magnetic powder coarse materials is provided with an organic insulating coating layer containing superfine inorganic oxide particles, and the metal soft magnetic powder coarse materials are dried and then pass through a standard sieve with more than 300 meshes, so that the high-temperature-resistant metal soft magnetic composite material is obtained.
2. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the metal soft magnetic powder is one or more selected from carbonyl iron powder, atomized iron powder, feSi-based soft magnetic powder, fesai-based soft magnetic powder, feai-based soft magnetic powder, feNi-based soft magnetic powder, feNiMo-based soft magnetic powder, iron-based amorphous powder and nanocrystalline powder.
3. The method for preparing a high-temperature-resistant metal soft magnetic composite material according to claim 1, wherein the phosphate in the passivation and corrosion inhibition solution is one or more selected from the group consisting of diammonium phosphate, monoammonium phosphate, sodium dihydrogen phosphate, calcium hydrogen phosphate, zinc phosphate and phosphoric acid.
4. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the molybdate in the passivation and corrosion inhibiting solution is one or more selected from zinc molybdate, calcium molybdate and sodium molybdate.
5. The method for preparing the high-temperature-resistant metal soft magnetic composite material according to claim 1, wherein the organic solvent A in the passivation and corrosion inhibition solution and the organic solvent B in the coupling and wetting solution and the diluent in the insulating additive solution are the same or different in composition, and all the organic solvent A, the organic solvent B and the diluent in the coupling and wetting solution are one or more selected from alcohol, acetone, butanone and ethyl butanol.
6. The method for preparing a high-temperature-resistant metal soft magnetic composite material according to claim 1, wherein the coupling agent in the coupling wetting solution is one or more selected from silane coupling agents, titanate coupling agents and aluminate coupling agents.
7. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the epoxy resin in the insulating additive solution is one or more selected from the group consisting of glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, and aliphatic type epoxy resin.
8. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the resin curing agent in the insulation additive solution is one or more selected from the group consisting of acid anhydride curing agents, amine curing agents and imidazole curing agents.
9. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the ultrafine inorganic oxide particles in the insulation additive solution are selected from the group consisting of SiO 2 、MgO 2 、TiO 2 One or more of the following.
10. The method for preparing a high temperature resistant metal soft magnetic composite material according to claim 1, wherein the ultrafine inorganic oxide particles in the insulating additive solution have a particle size selected in a range of 1 to 50nm.
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