CN109215924A - A kind of in-situ passivation insulating wrapped processing method of metal soft magnetic composite material - Google Patents
A kind of in-situ passivation insulating wrapped processing method of metal soft magnetic composite material Download PDFInfo
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- CN109215924A CN109215924A CN201811092762.3A CN201811092762A CN109215924A CN 109215924 A CN109215924 A CN 109215924A CN 201811092762 A CN201811092762 A CN 201811092762A CN 109215924 A CN109215924 A CN 109215924A
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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
Abstract
The invention discloses a kind of in-situ passivations of metal soft magnetic composite material to coat processing method.After carrying out insulating wrapped to metal magnetic using in-situ passivation method, through bonding, compression moulding, heat treatment, spraying process, target product is obtained.The present invention generates one layer of fine and close passivating film in magnetic powder surface in situ using in-situ passivation method, and passivating film is evenly coated, thickness is controllable, and resistivity height, thermal stability and bond strength are good, has excellent magnetic property and mechanical property；Using in-situ passivation method in one layer of oxide passivation film of metal magnetic coated with uniform, covered effect is better than existing method, and strong operability, convenient for batch production；The Effective permeability of soft-magnetic composite material is greatly improved, and core loss is effectively reduced.
Description
Technical field
The present invention relates to the preparation technical field of magnetic material more particularly to a kind of original position of metal soft magnetic composite material are blunt
Change insulating wrapped processing method.
Background technique
Metal soft magnetic composite material is to mix metal magnetic with dielectric to suppress.Metal magnetic particle size compared with
Small, skin effect is unobvious, therefore the frequency stability of magnetic conductivity is higher.Metal soft magnetic composite material is also with higher simultaneously
Resistivity can be applied to medium-high frequency, can be processed into various complicated shapes using powder metallurgical technique, have low-coercivity, low
The characteristics of loss, so that soft-magnetic composite material is widely used in telecommunications and electricity as filter, inductor, choking-winding etc.
The fields such as source switch.
The higher eddy-current loss of metal soft magnetic material is the main reason for limiting its frequency applications.By in metal magnetic table
Face uniformly coats the dielectric insulating film of one layer of high resistivity, and the eddy-current loss under high frequency can be effectively reduced.Insulating wrapped is usual
It is divided into organic coating and inorganic coating.Organic coating agent mainly includes epoxy resin, phenolic resin, silicone resin etc., passes through high temperature
Annealing can effectively eliminate a large amount of defects and internal stress that soft-magnetic composite material introduces in pressing process, to reduce magnetic hysteresis damage
Consumption, but organic matter heat resisting temperature is low, is easy to decompose under hot conditions, increases eddy-current loss, therefore have good thermal stability
Inorganic coating material become people research emphasis.And inorganic coating specifically includes that Phosphate coating (aluminum phosphate, ferric phosphate
Deng) and oxide cladding (SiO2、MgO、Al2O3And ferrite) etc..Traditional Phosphate coating is good with magnetic powder associativity, tool
There is higher resistivity, simple process is suitable for industrialized production, but being easy to decompose in high-temperature annealing process causes resistivity
It reduces, loss increases therewith.And the method for coating of current metal oxide, poor with magnetic powder associativity, the brittleness of itself makes
Insulating film is easy cracking.In-situ passivation is to generate one layer of fine and close passivating film, heat-resisting temperature with higher in magnetic powder surface in situ
Degree can satisfy the requirement of high annealing, and resistivity is high, and it is excellent insulating coating method that eddy-current loss is lower under high frequency.
The Chinese invention patent of Patent No. 201310212031.9 discloses a kind of preparation of metal soft magnetic composite material
Method utilizes nanometer Al2O3Dispersion liquid carries out insulating wrapped to metal magnetic.This homogeneous dispersion is poor, is easy deposition,
It is uneven to magnetic powder cladding, and nano particle and the associativity on magnetic powder surface are poor, are easy to fall off, and cause the eddy-current loss of magnetic core inclined
Greatly.Area's otherwise is the present invention therewith: the present invention is directly to react to carry out insulating wrapped with metal magnetic by passivating solution,
Clad and magnetic powder associativity are strong, are evenly coated, and have high thermal stability and excellent magnetic property.
The Chinese invention patent of Patent No. 201310396266.8 discloses compound using phosphorus acid passivation nano-crystal soft-magnetic
The preparation method of material, phosphatic high high-temp stability is poor, therefore is suitable only for low-temperature annealing heat treatment, and core loss is inclined
Greatly, and by the way of mechanical mixture uniform insulating wrapped can not be carried out to magnetic powder.
The Chinese invention patent of Patent No. 201410684249.9 is disclosed to be given a protective coating to metal objects technique insulating wrapped iron using acidity
Base soft-magnetic composite material generates one layer of Fe in magnetic powder surface in situ3O4Insulating film, associativity is preferable, but Fe3O4Insulating film electricity
Resistance rate is lower, and eddy-current loss is high, simultaneously because preparation process is complicated, condition is harsh, is unfavorable for industrialized production.
Summary of the invention
For current soft-magnetic composite material insulating film bond strength is low, the non-uniform defect of clad, the present invention provides
The in-situ passivation insulating wrapped processing method of metal soft magnetic composite material a kind of coats one on metal soft magnetic composite material surface
Layer has the passivating film of high thermal stability high resistivity, and technical scheme is as follows:
The in-situ passivation insulating wrapped processing method of metal soft magnetic composite material includes the following steps:
1) grain size proportion: grain size proportion is carried out after being sieved to metal magnetic；
2) in-situ passivation method insulating wrapped: dissolution accounts for the concentrated acid of 10 ~ 50 % of dehydrated alcohol weight in dehydrated alcohol, and stirring 10 ~
60 min, obtain passivating solution；Proportioned metal magnetic is added in passivating solution, while 5 ~ 40 min of uniform stirring, then
Filtering, dry, the magnetic powder after being passivated；It is added 0.5 ~ 2.5 %'s of magnetic powder quality after accounting for passivation into the magnetic powder after passivation
It is dry, uniformly mixed to be stirred well to mixture in a heated condition for binder；Finally into the magnetic powder after passivation be added account for it is blunt
It the release agent of 0.5 ~ 2.0 % of magnetic powder gross weight and is uniformly mixed after change, obtains magnetic powder to be formed；
3) compression moulding: by magnetic powder to be formed compression moulding under the pressure of 600 ~ 2000 MPa, soft-magnetic composite material is obtained；
4) it is heat-treated: protective atmosphere being made using nitrogen or argon gas, soft-magnetic composite material is placed in 400 ~ 750 oC environment and is kept the temperature
30~120 min；
5) surface sprays: spraying one layer of epoxy resin insulating varnish on step 4) treated soft-magnetic composite material surface, is made into
Product to get arrive metal soft magnetic composite material.
The weight of the metal magnetic is 10 ~ 30 g, and the quality of concentrated acid is 2 ~ 40 g in the mixed solution, anhydrous
The quality of ethyl alcohol is 20 ~ 80 g.
The metal magnetic is iron powder, iron silicon powder, iron aluminum silicon powder, iron cobalt powder, iron nickel powder, iron nickel molybdenum powder and Fe-based amorphous
One of powder is a variety of.The binder is phenolic resin, epoxy resin, silicone resin, poly- ethylene fluoride, melamine tree
Rouge, glass powder with low melting point, SiO2One of or it is a variety of.The release agent be zinc stearate, barium stearate, calcium stearate or
One of molybdenum disulfide is a variety of.
Soft-magnetic composite material prepared by the present invention, due to being to grow one layer of fine and close passivating film in magnetic powder surface in situ, to material
The saturation flux density of material influences smaller, resistivity height strong with magnetic powder associativity, the excellent magnetic with high magnetic conductivity and low loss
Energy.Preparation process is easy simultaneously, and passivating solution can recycle, and preparation cost is low, is advantageously implemented large-scale industrial production.
Detailed description of the invention
Fig. 1 is the surface topography map of magnetic powder after in-situ passivation processing.
Fig. 2 is the magnetic loss (test of the iron-silicon-aluminum soft magnet composite material of in-situ passivation technique and traditional phosphorus acid passivation preparation
Condition is 100 mT).
Fig. 3 is the Effective permeability of the iron-silicon-aluminum soft magnet composite material of in-situ passivation technique and traditional phosphorus acid passivation preparation
(test condition is 100 mT).
Specific embodiment
Soft-magnetic composite material of the invention is to carry out in-situ passivation processing to magnetic powder, generates one layer of cause in magnetic powder surface in situ
Soft-magnetic composite material is made after then adding binder, compression moulding, annealing heat-treatment and spraying in close oxidation film.Now in conjunction with
Invention is further explained for specific embodiment.
Embodiment 1
The 6 g concentrated sulfuric acids are added in 30 g dehydrated alcohols, 15 min is stirred, obtains passivating solution.15 g iron powders are sieved and are carried out
It is added in passivating solution after grain size proportion, while 20 min of uniform stirring, then filters, dry, the magnetic powder after being passivated.Xiang Dun
The binder of 1.0 % of magnetic powder quality after accounting for passivation is added in magnetic powder after change, is stirred well to mixture in a heated condition
Dry, uniformly mixed, the binder is epoxy resin.Magnetic powder gross weight after accounting for passivation is finally added into the magnetic powder after passivation
The release agent of 0.5 % is simultaneously uniformly mixed, and the release agent is zinc stearate, obtains magnetic powder to be formed.Magnetic powder to be formed is existed
23.4 mm of outer diameter, 14.4 mm of internal diameter are pressed under the pressure of 800 MPa, the annular soft-magnetic composite material of high 8.8 mm uses
Nitrogen makees protective atmosphere, and soft-magnetic composite material is placed in 500 oC environment and keeps the temperature 30 min, soft-magnetic composite material is made, soft
The surface of magnetic composite material sprays one layer of epoxy resin insulating varnish, and finished product is to get arriving iron-based soft magnetic composite material.
0.8 mm of line footpath Ф, the 20 circle inductor wire of enameled wire coiling of 0.9 m of wire length are used on iron-based soft magnetic composite material
Circle, it is specific as follows to measure soft-magnetic composite material electromagnetic performance:
(1) soft-magnetic composite material magnetic conductivity: 95；
Under the conditions of (2) 10 kHz/1 V, the μ of inductance L=47.8 H；
(3) DC stacked performance: when 1 kHz, H=100 Oe, LH/LO = 53.6%；
Under the conditions of (4) 100 kHz/1 V, quality factor q=62；
(5) soft-magnetic composite material is lost: when 50 kHz/100 mT, PCV = 820.3 mW/cm3。
Embodiment 2
5 g concentrated nitric acids are added in 25 g dehydrated alcohols, 20 min is stirred, obtains passivating solution.10 g iron aluminum silicon powders are sieved
It is added in passivating solution after carrying out grain size proportion, while 10 min of uniform stirring, then filters, dry, the magnetic powder after being passivated.
The binder of 0.5 % of magnetic powder quality after accounting for passivation is added into the magnetic powder after passivation, is stirred well in a heated condition mixed
Conjunction object is dry, uniformly mixed, and the binder is phenolic resin.Magnetic powder after accounting for passivation is finally added into the magnetic powder after passivation
The release agent of 1.0 % of gross weight is simultaneously uniformly mixed, and the release agent is calcium stearate, obtains magnetic powder to be formed.By magnetic to be formed
Powder is pressed into 23.4 mm of outer diameter under the pressure of 1800 MPa, 14.4 mm of internal diameter, the annular soft-magnetic composite material of high 8.8 mm,
Protective atmosphere is employed nitrogen as, soft-magnetic composite material is placed in 700 oC environment and keeps the temperature 60 min, soft-magnetic composite material is made,
Soft-magnetic composite material surface spray one layer of epoxy resin insulating varnish, finished product to get arrive iron-silicon-aluminum soft magnet composite material.
0.8 mm of line footpath Ф, the 20 circle inductance of enameled wire coiling of 0.9 m of wire length are used on iron-silicon-aluminum soft magnet composite material
It is specific as follows to measure soft-magnetic composite material electromagnetic performance for coil:
(1) soft-magnetic composite material magnetic conductivity: 153；
Under the conditions of (2) 10 kHz/1 V, the μ of inductance L=65.8 H；
(3) DC stacked performance: when 10 kHz, H=100 Oe, LH/LO = 39.4%；
Under the conditions of (4) 100 kHz/1 V, quality factor q=72；
(5) soft-magnetic composite material is lost: when 50 kHz/100 mT, PCV= 282.5 mW/cm3。
Embodiment 3
The dense nitrous acid of 10 g is added in 40 g dehydrated alcohols, 10 min is stirred, obtains passivating solution.20 g iron nickel powders are sieved
It is added in passivating solution after carrying out grain size proportion, while 15 min of uniform stirring, then filters, dry, the magnetic powder after being passivated.
The binder of 1.5 % of magnetic powder quality after accounting for passivation is added into the magnetic powder after passivation, is stirred well in a heated condition mixed
Conjunction object is dry, uniformly mixed, and the binder is silicone resin.It is total that magnetic powder after accounting for passivation is finally added into the magnetic powder after passivation
It weighs the release agent of 0.5 % and is uniformly mixed, the release agent is barium stearate, obtains magnetic powder to be formed.By magnetic powder to be formed
23.4 mm of outer diameter, 14.4 mm of internal diameter are pressed under the pressure of 1400 MPa, the annular soft-magnetic composite material of high 8.8 mm is adopted
Make protective atmosphere with nitrogen, soft-magnetic composite material be placed in 600 oC environment and keeps the temperature 120 min, soft-magnetic composite material is made,
Soft-magnetic composite material surface spray one layer of epoxy resin insulating varnish, finished product to get arrive the Ni-based soft-magnetic composite material of iron.
0.8 mm of line footpath Ф, the 20 circle inductance of enameled wire coiling of 0.9 m of wire length are used on the Ni-based soft-magnetic composite material of iron
It is specific as follows to measure soft-magnetic composite material electromagnetic performance for coil:
(1) soft-magnetic composite material magnetic conductivity: 132；
Under the conditions of (2) 10 kHz/1 V, the μ of inductance L=67.2 H；
(3) DC stacked performance: when 10 kHz, H=100 Oe, LH/LO = 46.3%；
Under the conditions of (4) 100 kHz/1 V, quality factor q=65；
(5) soft-magnetic composite material is lost: when 50 kHz/100 mT, PCV= 570.6 mW/cm3。
Claims (6)
1. a kind of in-situ passivation insulating wrapped processing method of metal soft magnetic composite material, which comprises the steps of:
1) grain size proportion: grain size proportion is carried out after being sieved to metal magnetic；
2) in-situ passivation method insulating wrapped: dissolution accounts for the concentrated acid of 10 ~ 50 % of dehydrated alcohol weight in dehydrated alcohol, and stirring 10 ~
60 min, obtain passivating solution；Proportioned metal magnetic is added in passivating solution, while 5 ~ 40 min of uniform stirring, then
Filtering, dry, the magnetic powder after being passivated；It is added 0.5 ~ 2.5 %'s of magnetic powder quality after accounting for passivation into the magnetic powder after passivation
It is dry, uniformly mixed to be stirred well to mixture in a heated condition for binder；Finally into the magnetic powder after passivation be added account for it is blunt
It the release agent of 0.5 ~ 2.0 % of magnetic powder gross weight and is uniformly mixed after change, obtains magnetic powder to be formed；
3) compression moulding: by magnetic powder to be formed compression moulding under the pressure of 600 ~ 2000 MPa, soft-magnetic composite material is obtained；
4) it is heat-treated: protective atmosphere being made using nitrogen or argon gas, soft-magnetic composite material is placed in 400 ~ 750 oC environment and is kept the temperature
30~120 min；
5) surface sprays: spraying one layer of epoxy resin insulating varnish on step 4) treated soft-magnetic composite material surface, is made into
Product to get arrive metal soft magnetic composite material.
2. metal magnetic according to claim 1 is iron powder, iron silicon powder, iron aluminum silicon powder, iron cobalt powder, iron nickel powder, iron nickel molybdenum
One of powder and Fe-based amorphous powder are a variety of.
3. concentrated acid according to claim 1 is one of sulfuric acid, nitric acid, nitrous acid, permanganic acid, chloric acid or a variety of.
4. the in-situ passivation insulating wrapped processing method of metal soft magnetic composite material according to claim 1, feature exist
In: the weight of the metal magnetic is 10 ~ 30 g, and the quality of concentrated acid is 2 ~ 40 g, dehydrated alcohol in the mixed solution
Quality be 20 ~ 80 g.
5. the in-situ passivation insulating wrapped processing method of metal soft magnetic composite material according to claim 1, feature exist
In: the binder is phenolic resin, epoxy resin, silicone resin, poly- ethylene fluoride, melamine resin, low-melting glass
Powder, SiO2One of or it is a variety of.
6. the in-situ passivation insulating wrapped processing method of metal soft magnetic composite material according to claim 1, feature exist
In: the release agent be one of zinc stearate, barium stearate, calcium stearate or molybdenum disulfide or a variety of.
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| CN110303152A (en) * | 2019-07-31 | 2019-10-08 | 深圳市麦捷微电子科技股份有限公司 | A kind of metal soft magnetic powder high-insulativity cladding processing method |
| CN112247143A (en) * | 2020-10-27 | 2021-01-22 | 佛山市中研非晶科技股份有限公司 | Amorphous nanocrystalline powder coating method and inductor preparation method |
| CN112420371A (en) * | 2020-10-27 | 2021-02-26 | 佛山市中研非晶科技股份有限公司 | Inductor preparation method |
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