CN110176338A - A kind of high resistant iron-resistant method for preparing silicon material and the integrated inductor containing the iron silicon materials - Google Patents

A kind of high resistant iron-resistant method for preparing silicon material and the integrated inductor containing the iron silicon materials Download PDF

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CN110176338A
CN110176338A CN201910265631.9A CN201910265631A CN110176338A CN 110176338 A CN110176338 A CN 110176338A CN 201910265631 A CN201910265631 A CN 201910265631A CN 110176338 A CN110176338 A CN 110176338A
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iron
resistant
powder
added
silicon
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CN110176338B (en
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郭宾
丁卫坡
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/20Magnets 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
    • H01F1/22Magnets 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
    • H01F1/24Magnets 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12Magnets 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
    • H01F1/14Magnets 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
    • H01F1/20Magnets 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
    • H01F1/22Magnets 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
    • H01F1/24Magnets 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
    • H01F1/26Magnets 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F17/00Fixed inductances of the signal type 
    • H01F17/04Fixed inductances of the signal type  with magnetic core
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00Details of transformers or inductances, in general
    • H01F27/24Magnetic cores
    • H01F27/255Magnetic cores made from particles
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0206Manufacturing of magnetic cores by mechanical means
    • H01F41/0246Manufacturing of magnetic circuits by moulding or by pressing powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Spectroscopy & Molecular Physics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

A kind of integrated inductor the invention discloses high resistant iron-resistant method for preparing silicon material and containing the iron silicon materials, a kind of high resistant iron-resistant method for preparing silicon material include the following steps: to select the water atomization iron silicon powder material of 400-500 mesh to carry out ball milling;Powder after ball milling is added in covering liquid and carries out insulating wrapped, covering liquid is dissolved in acetone by two or more in phosphoric acid, aluminium dihydrogen phosphate, chromic acid, potassium water glass to be made;Powder after insulating wrapped is added in secondary covering liquid and carries out secondary cladding, secondary covering liquid is dissolved in acetone by the one or more of silicone resin and liquid glue to be made;Powder after secondary cladding is successively granulated, is dried and is toasted;Auxiliary material is added after being cooled to room temperature to be stirred, be sieved.A kind of integrated inductor is made by above-mentioned high resistant iron-resistant silicon materials and coil compression moulding and after toasting.The present invention is effectively improved the granule-morphology of powder, greatly promotes the insulating properties between powder, reduces the loss of magnetic core.

Description

A kind of high resistant iron-resistant method for preparing silicon material and the integral type containing the iron silicon materials Inductance
Technical field
The present invention relates to inductance fields, more particularly, to a kind of high resistant iron-resistant method for preparing silicon material and contain the iron silicon material The integrated inductor of material.
Background technique
Current many manufacturers can all use alloy powder come the formula inductance that is made into one, and so-called integrated inductor is exactly Inductance after magnetic core made of powder and coil are integrally formed.Wherein, magnetic core is that alloy powder is mixed pressure with dielectric A kind of compound soft magnetic material made of system, due to one layer of dielectric insulating film of the coated with uniform in alloy powder particle, magnetic The resistivity of core is high, thus eddy-current loss is very low, is suitable for upper frequency application.Coil be with made of enamel covered wire coiling, In integrated inductor die cast, the coat of paint of the enameled wire on coil is easy breakage, so as to cause layer short circuit phenomenon.Cause This, generation to avoid short circuit guarantees the performance of integrated inductor, requires the insulating properties powder particles very high.
Magnetic core in the prior art is generally made using the aerosolization powder for having carried out insulating wrapped, for example, in " manufacturing methods of a kind of iron silicon materials and 75 iron silica magnetic particle core of μ " disclosed on state's patent document, notification number CN102294476B, including alloy melting, powder processed, powder reduction, powder classification, grain size proportion, powder passivation, insulating wrapped, Compression molding, heat treatment and surface covering step, a small amount of V and Nb element is added to during alloy melting, improves iron The magnetic property of silicon alloy.
But the mouldability of aerosolization powder is poor, and insulating coating method in the prior art and covering material also can not be in powder Material surface forms preferable insulating bag overlay film, causes the insulation performance between powder poor, core loss is larger.And integrated inductor In production, transport and use process, under the action of electricity, heat and mechanical stress, inside is also easy to produce micro-crack, shortens one The service life of body formula inductance.
Summary of the invention
First goal of the invention of the invention is the aerosolization powder in order to overcome in the magnetic core of integrated inductor in the prior art The mouldability of material is poor, and insulating coating method in the prior art and covering material can not also be formed preferably absolutely on powder surface Edge coating film causes the insulation performance between powder poor, and the larger problem of core loss provides a kind of high resistant iron-resistant silicon materials system Preparation Method and integrated inductor magnetic core containing the iron silicon materials, are effectively improved the granule-morphology of powder, and greatly promote powder Between insulating properties, reduce the loss of magnetic core, improve the overall performance of integrated inductor.
Second goal of the invention of the invention be in order to overcome in the prior art integrated inductor in production, transport and use In the process, under the action of electricity, heat and mechanical stress, inside is also easy to produce micro-crack, and shorten integrated inductor uses the longevity The problem of life, provides a kind of high resistant iron-resistant method for preparing silicon material and the integrated inductor magnetic core containing the iron silicon materials, makes one Selfreparing may be implemented in the micro-crack generated in body formula inductance core, improves the service life of integrated inductor.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of high resistant iron-resistant method for preparing silicon material, includes the following steps:
(1) the water atomization iron silicon powder material of 400-500 mesh is selected to carry out ball milling;
(2) the water atomization iron silicon powder material after ball milling is added in covering liquid and carries out insulating wrapped, the covering liquid is by covering material Be dissolved in acetone and being made, the covering material include phosphoric acid, aluminium dihydrogen phosphate, chromic acid, two kinds or two kinds in potassium water glass with On;
(3) the water atomization iron silicon powder material after insulating wrapped is added in secondary covering liquid and carries out secondary cladding, the secondary cladding Liquid is dissolved in acetone by secondary covering material to be made, and the secondary covering material includes one kind or one of silicone resin and liquid glue Kind or more;
(4) the water atomization iron silicon powder material after secondary cladding is successively granulated, is dried and is toasted;
(5) auxiliary material is added after being cooled to room temperature to be stirred, up to high resistant iron-resistant silicon materials after sieving.
The water atomization iron silicon powder material of 400-500 mesh is selected, mouldability is good, can satisfy the Grained Requirements of different inductance value, right Powder carries out ball-milling treatment, can eliminate stress and improve particle sphericity, improve the covered effect of insulating compound.
The present invention uses special insulating coating method: first with including in phosphoric acid, aluminium dihydrogen phosphate, chromic acid, potassium water glass The covering liquid of two or more and acetone the insulating wrapped of first time, the covering liquid ratio are carried out to water atomization iron silicon powder material Merely using phosphoric acid cook insulating compound when insulation effect more preferably;Again with include silicone resin, liquid glue one or more and The secondary covering liquid of acetone carries out secondary cladding, and insulating compound and binder can be made to be uniformly coated on particle surface, added Inorganic insulation powder forms uniform, high adhesion force, high-temperature insulation film as auxiliary material, through low temperature drying, thus significantly It reduces core loss and promotes DC stacked performance, and intergranular insulating properties is greatly improved.
Liquid glue is that a kind of epoxy by high resin content is grafted with silicone oil resin, cooperates special curing agent institute structure At epoxy silicon oil resin, can promote product strength, increase insulating properties between particle.
Preferably, the additive amount of covering material is the 0.2-1.0wt% of water atomization iron silicon powder material, cladding in step (2) Effect is good, and insulating properties is good.
Preferably, the insulating wrapped step in step (2) are as follows: the iron silicon powder material that makes water fogging, which is put into covering liquid, impregnates 5- After 10min, mixing 30min-60min, natural air drying 2-4h, 1-2h is toasted at 90~100 DEG C.Covering liquid can be made equal It is even, be effectively coated on powder surface.
Preferably, further including microcapsules and boron trifluoride ether, micro- glue in secondary covering material in step (3) The preparation method of capsule the following steps are included:
A) neopelex is added in deionized water, stirs 20-30min;
B urea, ammonium chloride and the resorcinol that mass ratio is (10-15): 1:1) are added into acquired solution, is stirred at 70-100 DEG C It mixes to dissolution, pH value of solution is adjusted to 2-3.5;
C bisphenol A type epoxy resin E-54 and trihydroxymethylpropanyltri diglycidyl ether) are added into acquired solution, reacts 10- 20min;
D it) is added and urea quality is than the formaldehyde for 1:1-2:1, filtered after reaction 2-3h at 50-60 DEG C, after vacuum drying to obtain the final product Microcapsules.
Microcapsules and curing agent boron trifluoride ether are added in secondary covering liquid, make to be surrounded by renovation agent bisphenol type epoxy The microcapsules and curing agent of resin E-54 are dispersed in secondary covering liquid while being coated on water atomization iron silicon powder material, when with the powder When magnetic core made of expecting cracks, crack tip stress, which is concentrated, causes microcapsules rupture, and renovation agent is existing by capillary siphoning As release to cracks filling crackle, and solidify under the action of curing agent, so that cohesive crack, reaches restorer performance Purpose improves the service life of integrated inductor magnetic core.
Using bisphenol A type epoxy resin E-54 as the renovation agent in microcapsules, bisphenol A type epoxy resin E-54 is thermoplastic Property resin, but there is thermosetting property, the excellent solidfied material of multiple performance can be formed with a variety of curing agent, catalyst and additive, it is several It is able to satisfy various requirements;The good manufacturability of resin, when solidification, do not generate small molecule volatile matter substantially, can low pressure at Type can be dissolved in multi-solvents;Solidfied material has very high intensity and adhesive strength;Solidfied material has higher corrosion resistance and electrical property Energy;Solidfied material has certain toughness and heat resistance.But viscosity is larger at normal temperature by bisphenol A type epoxy resin E-54, mobility compared with Difference is not easy filling and improves to cracks so diluent trihydroxymethylpropanyltri diglycidyl ether, which is added, reduces renovation agent viscosity Repairing effect.Using Lauxite as microcapsule wall material, there is good mechanical property, heat resistance and barrier property.
Preferably, the secondary covering material additive amount in step (3) is the 2-8wt% of water atomization iron silicon powder material, cladding Uniformly, bond effect is good.
40-50 mesh net is used preferably, being granulated in step (4), flash-off time 3-8h toasts 1-3h at 60-70 DEG C.It can To meet the Grained Requirements of different inductance value, and be conducive to the addition and cladding of subsequent auxiliary material.
Preferably, the auxiliary material in step (5) include magnesia, zinc stearate, silica, in demoulding powder extremely Few one kind.Inorganic insulation auxiliary material is added, lubricating action can be played, convenient for demoulding.
Preferably, the auxiliary material additive amount in step (5) is 0.3-0.6wt%.Lubrication and stripping result are good, not shadow Ring the impedance function of material.
The present invention also provides a kind of integrated inductors containing above-mentioned high resistant iron-resistant silicon materials, by high resistant iron-resistant silicon materials It is made with after coil compression moulding and baking, reduces the loss of magnetic core in integrated inductor, improve the service life of magnetic core DC stacked performance.
Preferably, briquetting pressure is 6~8T/cm2, baking temperature is 70-160 DEG C, baking time 6-8h.Using this Integrated inductor made from technique has good molding effect and overall performance.
Therefore, the invention has the following beneficial effects:
(1) the water atomization iron silicon powder material of 400-500 mesh is selected, mouldability is good, can satisfy the Grained Requirements of different inductance value, to powder Material carries out ball-milling treatment, can eliminate stress and improve particle sphericity, improve the covered effect of insulating compound;
(2) insulating wrapped of first time, the covering liquid good insulating effect used are first carried out to water atomization iron silicon powder material with covering liquid; Secondary cladding is carried out with secondary covering liquid again, insulating compound and binder can be made to be uniformly coated on particle surface;Then it is added Inorganic insulation powder forms uniform, high adhesion force, high-temperature insulation film as auxiliary material, through low temperature drying, thus significantly It reduces core loss and promotes DC stacked performance, and intergranular insulating properties is greatly improved;
(3) microcapsules and curing agent are added in secondary covering material, are dispersed in the microcapsules for being surrounded by renovation agent and curing agent It is coated on water atomization iron silicon powder material simultaneously in secondary covering liquid, when the magnetic core made of the powder cracks, microcapsules Rupture, renovation agent, which can be discharged to cracks, fills crackle, and solidifies under the action of curing agent, so that cohesive crack, reaches The purpose of restorer performance improves the service life of integrated inductor magnetic core.
Specific embodiment
The present invention will be further described With reference to embodiment.
In the present invention, if not refering in particular to, all equipment and raw material is commercially available or the industry is common, Method in following embodiments is unless otherwise noted conventional method in that art.
Embodiment 1:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 400 mesh carries out 30 minutes ball millings;
Insulating wrapped: 30g phosphoric acid, 5g aluminium dihydrogen phosphate and 5g chromic acid are poured slowly into 1.2kg acetone and stir 1 minute with On, completely, covering liquid is made in dilution, and covering liquid is added in 10kg water atomization iron silicon powder material and is stirred evenly, and stirs after impregnating 5min 30min is mixed, 3h natural air drying will be dried under powder ventilated environment after mixing evenly, is sieved with 50 mesh screens, is then placed in 100 1h is toasted in DEG C baking oven;
Secondary cladding: 200g silicone resin, 100g liquid glue are uniformly mixed, and are stood 5min, are stirred for 1min, add 1kg acetone Dilution, which stirs evenly, stands 10min, then by 200 mesh net filtrations of the solution, removes impurity part, secondary covering liquid is made, will Secondary covering liquid is added in the water atomization iron silicon powder material by insulating wrapped, stirs 60min;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 50 mesh net pelletizers, 3h is dried, makes It is sieved with 40 mesh pelletizers and removes agglomeration, 60 DEG C of baking 1h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 40g is added Separating powder (wherein demoulding powder is sieved using 160 mesh screens), stirs 10min, crosses 40 mesh screens again to get high resistant iron-resistant silicon material Material;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 6T/cm2, compacting At 7mm × 6.6mm × 3.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in toasted stage by stage, dry Roasting phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 370 minutes, last blank inductance obtained finished product one by whole clubfoot Body formula inductance.
Embodiment 2:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 500 mesh carries out 60 minutes ball millings;
Insulating wrapped: 15g phosphoric acid and 5g potassium water glass are poured slowly into 1.3kg acetone and are stirred 1 minute or more, it has diluted Entirely, covering liquid is made, covering liquid is added in 10kg water atomization iron silicon powder material and is stirred evenly, stirs 60min after impregnating 10min, 4h natural air drying will be dried under powder ventilated environment after mixing evenly, be sieved, be then placed in 90 DEG C of baking ovens with 50 mesh screens Toast 2h;
Secondary cladding: 100g silicone resin, 100g liquid glue are uniformly mixed, and are stood 15min, are stirred for 1min, add 1.1kg third Ketone dilution, which stirs evenly, stands 10min, then by 200 mesh net filtrations of the solution, removes impurity part, secondary covering liquid is made, Secondary covering liquid is added in the water atomization iron silicon powder material by insulating wrapped, 60min is stirred;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 40 mesh net pelletizers, 8h is dried, makes It is sieved with 40 mesh pelletizers and removes agglomeration, 70 DEG C of baking 3h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 30g is added Demoulding powder (wherein demoulding powder is sieved using 160 mesh screens), stirs 10min, crosses 40 mesh screens again to get high resistant iron-resistant silicon material Material;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 8T/cm2, compacting At 13.3mm × 12.2mm × 5.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in dried stage by stage Roasting, baking phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 400 minutes, last blank inductance was obtained by whole clubfoot Finished product integrated inductor.
Embodiment 3:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 400 mesh carries out 30 minutes ball millings;
Insulating wrapped: 30g phosphoric acid, 5g aluminium dihydrogen phosphate and 5g chromic acid are poured slowly into 1.2kg acetone and stir 1 minute with On, completely, covering liquid is made in dilution, and covering liquid is added in 10kg water atomization iron silicon powder material and is stirred evenly, and stirs after impregnating 5min 30min is mixed, 3h natural air drying will be dried under powder ventilated environment after mixing evenly, is sieved with 50 mesh screens, is then placed in 100 1h is toasted in DEG C baking oven;
Microcapsules preparation: 0.2g neopelex is added in 300mL deionized water, stirs 20min;To acquired solution Middle addition mass ratio is 5g urea, 0.5g ammonium chloride and 0.5g resorcinol, at 70 DEG C stirring to after dissolving, with sodium hydroxide and PH value of solution is adjusted to 2.0 by hydrochloric acid solution;5g bisphenol A type epoxy resin E-54 and 5g trihydroxy methyl third are added into acquired solution Alkane triglycidyl ether reacts 10min;37% formalin 15g is added, filters, is dried in vacuo after reacting 2h at 50 DEG C Afterwards up to microcapsules;
Secondary cladding: 200g silicone resin, 100g liquid glue, 15g microcapsules and 1g boron trifluoride ether are uniformly mixed, quiet 5min is set, 1min is stirred for, adds the dilution of 1kg acetone to stir evenly and stands 10min, then by 200 mesh net filtrations of the solution, remove Secondary covering liquid is made in impurity part, and secondary covering liquid is added in the water atomization iron silicon powder material by insulating wrapped, stirring 60min;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 50 mesh net pelletizers, 3h is dried, makes It is sieved with 50 mesh pelletizers and removes agglomeration, 60 DEG C of baking 1h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 40g is added Separating powder (wherein demoulding powder is sieved using 160 mesh screens), stirs 10min, crosses 40 mesh screens again to get high resistant iron-resistant silicon material Material;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 6T/cm2, compacting At 7mm × 6.6mm × 3.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in toasted stage by stage, dry Roasting phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 370 minutes, last blank inductance obtained finished product one by whole clubfoot Body formula inductance.
Embodiment 4:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 400 mesh carries out 40 minutes ball millings;
Insulating wrapped: 60g phosphoric acid, 20g aluminium dihydrogen phosphate and 10g chromic acid and 10g potassium water glass are poured slowly into 2kg acetone simultaneously Stirring 1 minute or more, completely, covering liquid was made in dilution, and covering liquid is added in 10kg water atomization iron silicon powder material and is stirred evenly, and soaked 45min is stirred after bubble 8min, 2h natural air drying will be dried under powder ventilated environment after mixing evenly, is sieved with 50 mesh screens, It is then placed in 95 DEG C of baking ovens and toasts 1.5h;
Microcapsules preparation: 0.2g neopelex is added in 300mL deionized water, stirs 30min;To acquired solution Middle addition mass ratio is 7.5g urea, 0.5g ammonium chloride and 0.5g resorcinol, and stirring uses hydroxide to after dissolving at 100 DEG C PH value of solution is adjusted to 3.5 by sodium and hydrochloric acid solution;10g bisphenol A type epoxy resin E-54 and tri- hydroxyl of 7g are added into acquired solution Methylpropane triglycidyl ether reacts 20min;37% formalin 40.5g is added, is filtered after reacting 3h at 60 DEG C, Up to microcapsules after vacuum drying;
Secondary cladding: 400g silicone resin, 350g liquid glue, 36g microcapsules and 8g boron trifluoride ether are uniformly mixed, and are stood 5min is stirred for 1min, adds the dilution of 2kg acetone to stir evenly and stands 10min, then by 200 mesh net filtrations of the solution, goes to clean Secondary covering liquid is made in matter part, and secondary covering liquid is added in the water atomization iron silicon powder material by insulating wrapped, stirring 60min;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 50 mesh net pelletizers, 5h is dried, makes It is sieved with 50 mesh pelletizers and removes agglomeration, 65 DEG C of baking 2h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 30g is added Magnesia and 30g separating powder (wherein demoulding powder uses 160 mesh screens to be sieved), stir 10min, cross again 40 mesh screens to get High resistant iron-resistant silicon materials;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 7T/cm2, compacting At 7mm × 6.6mm × 3.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in toasted stage by stage, dry Roasting phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 300 minutes, last blank inductance obtained finished product one by whole clubfoot Body formula inductance.
Embodiment 5:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 500 mesh carries out 50 minutes ball millings;
Insulating wrapped: 40g phosphatase 11 0g chromic acid is poured into 1.2kg acetone and stirred 1 minute or more, completely, cladding is made in dilution Covering liquid is added in 10kg water atomization iron silicon powder material and stirs evenly by liquid, stirs 50min after impregnating 6min, will after mixing evenly Powder ventilated environment under dry 4h natural air drying, with 50 mesh screens be sieved, be then placed in 90 DEG C of baking ovens and toast 1h;Microcapsules Preparation: 0.2g neopelex is added in 300mL deionized water, stirs 30min;Quality is added into acquired solution Than for 6g urea, 0.5g ammonium chloride and 0.5g resorcinol, stirring is to after dissolving at 100 DEG C, with sodium hydroxide and hydrochloric acid solution PH value of solution is adjusted to 3.0;14g bisphenol A type epoxy resin E-54 and the contracting of 7g trimethylolpropane tris are added into acquired solution Water glycerin ether reacts 15min;37% formalin 24.3g is added, is filtered after reacting 2.5h at 55 DEG C, after vacuum drying Up to microcapsules;
Secondary cladding: 200g silicone resin, 80g liquid glue, 15g microcapsules and 5g boron trifluoride ether are uniformly mixed, quiet 5min is set, 1min is stirred for, adds the dilution of 1.5kg acetone to stir evenly and stands 10min, then by 200 mesh net filtrations of the solution, go Except impurity part, secondary covering liquid is made, secondary covering liquid is added in the water atomization iron silicon powder material by insulating wrapped, stirring 60min;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 40 mesh net pelletizers, 4h is dried, makes It is sieved with 40 mesh pelletizers and removes agglomeration, 70 DEG C of baking 2h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 20g is added Zinc stearate and 30g silica stir 10min, cross 40 mesh screens again to get high resistant iron-resistant silicon materials;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 6T/cm2, compacting At 7mm × 6.6mm × 3.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in toasted stage by stage, dry Roasting phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 480 minutes, last blank inductance obtained finished product one by whole clubfoot Body formula inductance.
Comparative example 1:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 400 mesh carries out 30 minutes ball millings;
Insulating wrapped: 40g phosphoric acid is poured slowly into 1.2kg acetone and is stirred 1 minute or more, completely, covering liquid is made in dilution, Covering liquid is added in 10kg water atomization iron silicon powder material and is stirred evenly, 30min is stirred after impregnating 5min, by powder after mixing evenly Expect to dry 3h natural air drying under ventilated environment, is sieved with 50 mesh screens, is then placed in 100 DEG C of baking ovens and toasts 1h;
Secondary cladding: add 1kg acetone to dilute 300g epoxy resin, stir evenly and stand 10min, then by 200 mesh of the solution Net filtration removes impurity part, secondary covering liquid is made, and secondary covering liquid is added to the water atomization iron silicon powder for passing through insulating wrapped In material, 60min is stirred;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 50 mesh net pelletizers, 3h is dried, makes It is sieved with 40 mesh pelletizers and removes agglomeration, 60 DEG C of baking 1h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 40g is added Separating powder (wherein demoulding powder is sieved using 160 mesh screens), stirs 10min, crosses 40 mesh screens again to get high resistant iron-resistant silicon material Material;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 6T/cm2, compacting At 7mm × 6.6mm × 3.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in toasted stage by stage, dry Roasting phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 370 minutes, last blank inductance obtained finished product one by whole clubfoot Body formula inductance.
Comparative example 2:
Powder is selected with processing: the water atomization iron silicon powder material for selecting powder size as 500 mesh carries out 60 minutes ball millings;
Insulating wrapped: 20g phosphoric acid is poured slowly into 1.3kg acetone and is stirred 1 minute or more, completely, covering liquid is made in dilution, Covering liquid is added in 10kg water atomization iron silicon powder material and be stirred evenly, stirs 60min after impregnating 10min, it will after mixing evenly 4h natural air drying is dried under powder ventilated environment, is sieved with 50 mesh screens, is then placed in 90 DEG C of baking ovens and toasts 2h;
Secondary cladding: adding 1.1kg acetone to dilute 200g epoxy resin, stirs evenly and stands 10min, then by the solution with 200 Mesh net filtration removes impurity part, secondary covering liquid is made, and secondary covering liquid is added to the water atomization iron silicon for passing through insulating wrapped In powder, 60min is stirred;
It is granulated: the water atomization iron silicon powder material after secondary cladding being granulated under leather hard with 40 mesh net pelletizers, 8h is dried, makes It is sieved with 40 mesh pelletizers and removes agglomeration, 70 DEG C of baking 3h are cooled to room temperature naturally and carry out 40 mesh sievings to powder, and 30g is added Demoulding powder (wherein demoulding powder is sieved using 160 mesh screens), stirs 10min, crosses 40 mesh screens again to get high resistant iron-resistant silicon material Material;
Compression moulding: high resistant iron-resistant silicon materials obtained are pressed together with coil, briquetting pressure 8T/cm2, compacting At 13.3mm × 12.2mm × 5.0mm blank inductance;Blank inductance obtained is placed in and fills N2Baking oven in dried stage by stage Roasting, baking phase temperature is 70 DEG C -100 DEG C -160 DEG C, and baking time 400 minutes, last blank inductance was obtained by whole clubfoot Finished product integrated inductor.
Manufactured integrated inductor in above-described embodiment and comparative example is tested for the property, the results are shown in Table 1.
Table 1: integrated inductor the performance test results.
Using phosphoric acid as covering material in comparative example 1 and comparative example 2, epoxy resin is implemented as secondary covering material Covering material is mixed using multiple material in example 1 and embodiment 2, and secondary covering material uses insulating properties more preferably and silicon resistant to high temperature Resin and liquid glue, from table 1 it follows that the insulation resistance of integrated inductor obtained is wanted in embodiment 1 and embodiment 2 Much larger than comparative example 1 and comparative example 2.
Microcapsules and curing agent boron trifluoride ether are added in embodiment 3-5 in secondary covering liquid, make obtained one Body formula inductance has self-repair function, and remediation efficiency is up to 75% or more.Remediation efficiency is the fracture toughness and reparation after repairing The ratio of preceding fracture toughness, fracture toughness are surveyed using KQL series universal testing machine according to Unite States Standard (ASTM E399) Examination.

Claims (10)

1. a kind of high resistant iron-resistant method for preparing silicon material, characterized in that include the following steps:
(1) the water atomization iron silicon powder material of 400-500 mesh is selected to carry out ball milling;
(2) the water atomization iron silicon powder material after ball milling is added in covering liquid and carries out insulating wrapped, the covering liquid is by covering material Be dissolved in acetone and being made, the covering material include phosphoric acid, aluminium dihydrogen phosphate, chromic acid, two kinds or two kinds in potassium water glass with On;
(3) the water atomization iron silicon powder material after insulating wrapped is added in secondary covering liquid and carries out secondary cladding, the secondary cladding Liquid is dissolved in acetone by secondary covering material to be made, and the secondary covering material includes one kind or one of silicone resin and liquid glue Kind or more;
(4) the water atomization iron silicon powder material after secondary cladding is successively granulated, is dried and is toasted;
(5) auxiliary material is added after being cooled to room temperature to be stirred, up to high resistant iron-resistant silicon materials after sieving.
2. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1, characterized in that coat material in step (2) The additive amount of material is the 0.2-1.0wt% of water atomization iron silicon powder material.
3. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1 or 2, characterized in that exhausted in step (2) Edge encapsulation steps are as follows: the iron silicon powder material that makes water fogging, which is put into covering liquid, impregnates 5-10min, and 30min-60min is mixed, natural After air-drying 2-4h, 1-2h is toasted at 90 ~ 100 DEG C.
4. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1, characterized in that secondary in step (3) Further include microcapsules and boron trifluoride ether in covering material, the preparation methods of the microcapsules the following steps are included:
A) neopelex is added in deionized water, stirs 20-30min;
B it is (10-15): 1: 1 urea, ammonium chloride and resorcinol, 70-100 that mass ratio) is added into acquired solution PH value of solution is adjusted to 2-3.5 to after dissolving by stirring at DEG C;
C bisphenol A type epoxy resin E-54 and trihydroxymethylpropanyltri diglycidyl ether) are added into acquired solution, reacts 10- 20min;
D it) is added and urea quality is than the formaldehyde for 1:1-2:1, filtered after reaction 2-3h at 50-60 DEG C, after vacuum drying to obtain the final product Microcapsules.
5. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1 or 4, characterized in that two in step (3) Secondary covering material additive amount is the 2-8wt% of water atomization iron silicon powder material.
6. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1, characterized in that being granulated in step (4) makes With 40-50 mesh net, flash-off time 3-8h toasts 1-3h at 60-70 DEG C.
7. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1, characterized in that the auxiliary in step (5) Material includes at least one of magnesia, zinc stearate, silica, demoulding powder.
8. a kind of high resistant iron-resistant method for preparing silicon material according to claim 1 or claim 7, characterized in that auxiliary in step (5) Helping material additive amount is 0.3-0.6wt%.
9. a kind of integrated inductor containing high resistant iron-resistant silicon materials described in claim 1, characterized in that by high resistant iron-resistant silicon It is made after material and coil compression moulding and baking.
10. a kind of integrated inductor according to claim 9, characterized in that the briquetting pressure is 6 ~ 8T/cm2, baking Temperature is 70-160 DEG C, baking time 6-8h.
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