CN104505209B - A kind of soft magnetic metal composite core and preparation method thereof - Google Patents

A kind of soft magnetic metal composite core and preparation method thereof Download PDF

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CN104505209B
CN104505209B CN201410801542.9A CN201410801542A CN104505209B CN 104505209 B CN104505209 B CN 104505209B CN 201410801542 A CN201410801542 A CN 201410801542A CN 104505209 B CN104505209 B CN 104505209B
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iron
powder
insulation
sial
coated
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CN104505209A (en
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苏海林
陈蓉
吴玉程
仝西川
邹中秋
黄礼胜
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JIANGSU RED MAGNETIC MATERIALS Co Ltd
Hefei University of Technology
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JIANGSU RED MAGNETIC MATERIALS Co Ltd
Hefei University of Technology
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Abstract

It is difficult to for prior art while realizing low-loss, high direct current biasing performance, the problem of low cost, the invention provides a kind of inexpensive soft magnetic metal composite core and preparation method thereof.Soft magnetic metal composite core of the present invention, is formed by the metal dust of iron silicon with the metal dust annealing of iron sial, and mass ratio is 2.00~9.00:1.Preparation method of the present invention, including:Prepare the iron silicon insulation pre-feed for being coated with phosphoric acid;Prepare the iron sial insulation pre-feed for being coated with phosphoric acid and boric acid;Prepare the mix insulation powder of iron silicon and iron sial;It is compressing;It is heat-treated 5 steps.Beneficial technique effect:In addition to the present invention is the characteristics of with low-loss, high direct current biasing performance, low noise, also there is low cost, be readily produced and promote.

Description

A kind of soft magnetic metal composite core and preparation method thereof
Technical field
The invention belongs to technical field of magnetic materials, high current low-loss application scenario is mainly used in, and in particular to one Plant soft magnetic metal composite core and preparation method thereof.
Background technology
Metal soft magnetic powder core is the powder being made of metal or alloy soft magnetic materials, is suppressed by special technique A kind of new soft magnetic materials with good combination property.It has metal soft magnetic material high saturated magnetic induction and ferrite concurrently The good characteristic of soft magnetic materials high resistivity, while overcome to greatest extent again, metal soft magnetic material eddy-current loss is big and iron oxygen The low shortcoming of body soft magnetic materials saturation induction density, with permanent magnetic conductivity, saturation induction density be higher, DC stacked ability By force, the advantages of working frequency is wider, becomes so as to meet power electronic devices miniaturization, high frequency, energy-saving, efficient development Gesture, has been widely used in the modern power electronic device such as photovoltaic DC-to-AC converter, reactor, Switching Power Supply, ups power, is used as work( The iron core of the devices such as rate factor correcting inductance, output inductor, resonant inductance, EMI inductance and flyback transformer.
At present, the metal soft magnetic powder core of in the market application is generally single material, including:Ferrocart core, iron Si-Al Magnetic Powder Core, iron silicon Powder core, FeNiCo magnetic core and iron nickel powder core.Iron powder core loss is larger, DC stacked poor-performing, but because cheap application Scope is wider.Fe-Si-Al magnetic core is cheap, and loss is relatively low, but DC stacked poor-performing, it is impossible to for high current occasion. Iron silica magnetic particle core price is relatively low, with excellent DC stacked performance, but is lost very high, it is impossible to for requiring low-loss field Close.FeNiCo magnetic core loss is minimum, but DC stacked performance is general, between iron silica flour core and iron Si-Al Magnetic Powder Core, and its valency Lattice are high, therefore application is less.Iron nickel powder core has the DC stacked performance suitable with iron silica flour core, but loss is far below iron silicon Powder core, thus be the optimal magnetic core for being presently available for high current low-loss occasion, but be equally because its high cost, therefore Application is extremely restricted.In recent years, in order to meet the application scenario of low-loss high current, researcher develops non-again Brilliant nanocrystalline powder core, but preparation cost is very high, and current technique is still immature.In addition, amorphous nano-crystalline powder core and iron sial, iron Silicon, iron nickel powder core are compared, and its maximum shortcoming, which is that the magnetostriction coefficient of alloy is larger, to be caused to produce in alternating electromagnetic field Raw loud noise, does not meet environmental requirement.This problem is not yet resolved at present.It can be seen that, the metal soft magnetic powder of single material Core, due to the limitation of cost or combination property, can not all meet the application demand of high current low-loss low cost.It is prepared by the present invention A kind of soft magnetism composite core based on inexpensive iron silicon and Fe-Si-Al magnetic, disclosure satisfy that had concurrently under high current low-loss and The demand of good DC stacked performance.
Patent application CN201210389520.7 describes a kind of preparation side of high DC stacked performance Fe-Si-Al magnetic core Method.This method is using iron sial metal dust and iron powder or permalloy powder(Or the mixture of two kinds of powder)Mixed powder The doping powder referred in end, but all embodiments is permalloy(Ni-Fe alloys), this can greatly improve powder core cost, And the DC stacked performance of powder core and bad, for the product of magnetic conductivity 60, only just decline 50% in 105Oe inductance.Patent Application CN201210230453.4 describes a kind of nanocrystalline magnetic core preparation method of magnetic conductivity 60, though the powder core is with relatively low Loss and more high DC stacked performance, but to generally acknowledge that manocrystalline powders prepare cost very high for industry, and containing Ni, Nb etc. in alloy Precious metal element, can greatly improve powder core cost.Patent application CN201210203772.6 describes a kind of nanocrystalline magnetic core Preparation method, uses Fe73.5Cu1Nb3Si13.5B9Nanometer crystal alloy, cost is very high, and and undeclared properties of product.Patent Application CN201310454647.7 and CN201310454203.3 describes the preparation method of modified ferrum-silicon-boron amorphous powder core.Two The preparation method of application is mixed using one or more modified powders of ferrum-silicon-boron amorphous powder and nickel powder, iron nickel powder, iron silica flour Powder after conjunction.Amorphous powder industry generally acknowledges that preparation cost is higher, and can greatly improve powder containing Ni elements in modified powder Core cost, though and two modified powder core noise problems of application have improvement, noise is still suffered from, with the iron without noise The powder cores such as silicon, iron sial, iron nickel, which are compared, has obvious inferior position.Patent CN201110391858.1 describes a kind of iron-based and is combined magnetic The preparation method of powder core.This method is using the non-crystalline flours of FeCuNbSiB and the mixed-powder of carbonyl iron dust, lacking with amorphous core Point, and the product uses the auxiliary material containing chromium, does not meet environmental requirement.Patent application CN201210509456.1 describes a kind of iron The preparation method of silicon soft magnetic alloy powder core.This method is using fast quenching ferro-silicium powder and the mixed powder for being atomized ferro-silicium powder A large amount of organic solvents are used in end, preparation process, cost is higher, though the DC stacked performance of products obtained therefrom is higher, be lost too high And Q values are relatively low.Patent application CN201310414993.2 describes a kind of preparation method of high superposition low-loss metal powder core. This method is using atomization Fe-Si-Al magnetic and the mixed-powder for being atomized iron nickel powder, though products obtained therefrom is with higher DC stacked property Can and relatively low loss, but because higher containing precious metal element nickel cost, the product uses the acid solution containing chromium in addition, is not inconsistent cyclization Guaranteed request.
There is provided a kind of simple to operate, production cost is low and be intended for the magnetic of high current low-loss application scenario in summary Powder core preparation method is those skilled in the art's technical barrier urgently to be resolved hurrily.
The content of the invention
For prior art it is difficult to realize low-loss, high DC stacked performance, the problem of low cost simultaneously, the present invention is provided A kind of inexpensive soft magnetic metal composite core and preparation method thereof.
A kind of soft magnetic metal composite core, is formed by the metal dust and the metal powder sintered of iron sial of iron silicon.Wherein, The mass ratio of iron silicon and iron sial is 2.00~9.00:1.The metal dust of iron silicon and the metal dust of iron sial are by exhausted The particulate of edge processing.
This soft magnetic metal composite core, under the conditions of 100kHz/1V, inductance L is between the μ H of 46.00 μ H~50.00; Under the conditions of 100kHz/1V, quality factor q is between 121.00~125.00;Under the conditions of 100kHz:When DC stacked magnetic field H= During 100Oe, LH/L0Between 62.00%~72.01%;As DC stacked magnetic field H=200Oe, LH/L035.00%~ Between 41.49%;Under the conditions of 50kHz/100mT, magnetic core loss PcvIn 440mW/cm3~590mW/cm3Between.
The preparation method of soft magnetic metal composite core of the present invention, is carried out as follows:
Step 1:Preparation is coated with phosphatic iron silicon insulation pre-feed.
1)Sieving is handled:Take the spherical iron silicon of aerosolization(Fe93.5Si6.5)Powder crosses the screen cloth of 200 mesh, after being sieved Iron Si powder.
2)Insulating wrapped processing:The mixing liquid of phosphoric acid and alcohol is added into the iron Si powder after sieving, and stirs equal It is even, obtain the iron silicon slurry containing phosphoric acid.Then, the iron silicon slurry containing phosphoric acid is heated to 90-120 DEG C and is stirred continuously, Until being somebody's turn to do the iron silicon slurry drying containing phosphoric acid, acquisition is coated with phosphatic iron silicon insulation powder.
3)Add binding agent:Silicone, zinc stearate are added to being coated with phosphatic iron silicon insulation powder, and is stirred Mix uniform, acquisition is coated with phosphatic iron silicon insulation pre-feed.
Step 2:Preparation is coated with phosphatic iron sial insulation pre-feed.
1)Sieving is handled:Take sheet iron sial(Fe85Si9.6Al5.4)Powder crosses the screen cloth of 200 mesh, the iron after being sieved Sial powder.
2)Insulating wrapped processing:The mixing liquid of phosphoric acid, boric acid and alcohol is added into the iron sial powder after sieving, and Stir, obtain the iron sial slurry containing phosphoric acid and boric acid.Then, the iron sial slurry containing phosphoric acid and boric acid is heated To 90-120 DEG C and be stirred continuously, until should iron sial slurry drying containing phosphoric acid and boric acid, acquisition is coated with phosphatic Iron sial insulation powder.
3)Add binding agent:Phenol resin, zinc stearate are added to being coated with phosphatic iron sial insulation powder, and Stir, acquisition is coated with phosphatic iron sial insulation pre-feed.
Step 3:Prepare the mix insulation powder of iron silicon and iron sial.Will be as being coated with phosphatic iron made from step 1 Silicon insulate pre-feed with as being coated with phosphatic iron sial insulation pre-feed in mass ratio 2.00~9.00 made from step 2:1 Uniform mixing, obtains the mix insulation powder of iron silicon and iron sial.
Step 4:It is compressing.By hydraulic forming machine by the well mixed iron silicon obtained by step 3 and iron sial Mix insulation stamping of powder is molded, and obtains the mix insulation blank of iron silicon and iron sial.Wherein, the compacting pressure of hydraulic forming machine For 18.6~21.7 tons/cm2
Step 5:Heat treatment.Protective atmosphere is employed nitrogen as, the mixing of obtained iron silicon and iron sial will be suppressed by step 4 Insulation blank is placed in insulation 30min~120min in 700 DEG C~780 DEG C of anneal environment, and soft magnetic metal composite core is made.
Beneficial technique effect
Soft magnetic metal composite core of the present invention has low-loss concurrently(Under the conditions of 50kHz/100mT, PcvIt is minimum 445mW/cm3), high DC stacked performance(Under the conditions of 100kHz, during H=100Oe, LH/L0Up to 72.01%.During H=200Oe, LH/L0Up to 41.49%)And low noise, and advantage that is inexpensive, being readily produced and promote.Soft magnetic metal of the present invention The preparation method of composite core, has the advantages that technique is simple, low raw-material cost, suitable industrialized production, by our legal system Have insulating properties height, magnetostriction coefficient small, noiseless in alternating electromagnetic field environment for the soft magnetic metal composite core gone out Outstanding advantages.It is in particular in following aspect:
The Fe that the present invention is used93.5Si6.5Spherical gas-atomised powders and Fe85Si9.6Al5.4Irregular ball-milled powder is used as original Material, two kinds of cost of alloy are cheap.Fe prepared by the gas atomization that the present invention is used93.5Si6.5Globular powder and through ball-milling treatment Edge is in irregular Fe85Si9.6Al5.4Flakelike powder, its magnetostriction coefficient is 0, so as to avoid gold of the present invention Category soft magnetism composite core produces noise problem in alternating electromagnetic field because of magnetostriction deformation.
Fe in the present invention93.5Si6.5Spherical gas-atomised powders carry out insulation processing by the mixed liquor of phosphoric acid and alcohol, and Fe85Si9.6Al5.4Irregular ball-milled powder carries out insulation processing by the mixed liquor of phosphoric acid, boric acid and alcohol, i.e., by different Formula respectively insulate to two kinds of raw materials, makes the insulating barrier that last layer dense uniform is coated around magnetic, it is to avoid using singly The acid solution of one a kind of insulating effect causes the extent of corrosion of magnetic to differ, it is to avoid in conventional method that two kinds of different powder are straight The two kinds of powder for mixing and being run into using same insulating process are connect because insulation degree is different, the insulating barrier coated around magnetic is not The problem of bulk article uniformity is poor caused by enough dense uniforms.Meanwhile, the change that can be matched according to magnetic of separately insulating Change, flexibly adjust properties of product.
The present invention uses acid solution(Phosphoric acid, boric acid)Insulating compound is done, the effect of insulation is reached by increasing the usage amount of acid, And without such as other insulating compounds of mica, kaolin, glass dust used in conventional method, can effectively simplify production work Skill, reduces production cost, improves homogeneity of product.
The present invention, only as binding agent, does not play insulating effect using resin, can all be decomposed during the high temperature anneal, will not Any influence is produced on powdered insulation.Resin as insulating compound, therefore can not be carried out high temperature by the conventional method that this is avoided Heat treatment, causes retention large amount of organic in powder core to cause serious aging problem occur during the follow-up use of product.Or because Cause resin decomposition to influence insulation effect to have carried out high-temperature heat treatment, cause loss significantly to raise.
The present invention need not carry out dipping process, it is possible to reduce production link, production cost be reduced, while avoiding impregnation from existing Large amount of organic is introduced in powder core to cause serious aging problem occur during the follow-up use of product.
Brief description of the drawings
Fig. 1 is the soft magnetic metal composite core section X-ray energy spectrum prepared in embodiment 1(EDS)Element area profile.
Fig. 2 is the soft magnetic metal composite core section X-ray energy spectrum prepared in embodiment 2(EDS)Element area profile.
Fig. 3 is the soft magnetic metal composite core section X-ray energy spectrum prepared in embodiment 3(EDS)Element area profile.
Embodiment
Describe the ins and outs of the present invention in detail in conjunction with accompanying drawing.
A kind of soft magnetic metal composite core, is formed by the metal dust of iron silicon with the metal dust annealing of iron sial.Wherein, The mass ratio of iron silicon and iron sial is 2.00~9.00:1.The metal dust of iron silicon and the metal dust of iron sial are by exhausted The particulate of edge processing.
Furtherly, the structural formula of iron silicon particle is Fe93.5Si6.5, and particle diameter is not more than the spherical of 74 μm of aerosolization Powder.The structural formula of iron silicon aluminium particle is Fe85Si9.6Al5.4, and particle diameter is not more than the powder of the sheet of 74 μm of process ball-milling treatment Material.
Furtherly, the Surface coating of iron silicon particle has had the phosphate particulate of insulating effect.The surface of iron silicon aluminium particle It has been coated with the phosphate particulate of insulating effect.
Furtherly, described soft magnetic metal composite core,
Under the conditions of 100kHz/1V, inductance L is between the μ H of 46.00 μ H~50.00;
Under the conditions of 100kHz/1V, quality factor q is between 121.00~125.00;
Under the conditions of 100kHz:As DC stacked magnetic field H=100Oe, LH/L0Between 62.00%~72.01%;When straight During stream superposition magnetic field H=200Oe, LH/L0Between 35.00%~41.49%;
Under the conditions of 50kHz/100mT, magnetic core loss PcvIn 445mW/cm3~590mW/cm3Between.
The preparation method of soft magnetic metal composite core of the present invention, is carried out as follows:
Step 1:Preparation is coated with phosphatic iron silicon insulation pre-feed.
1)Sieving is handled:Take the spherical iron silicon of aerosolization(Fe93.5Si6.5)Powder crosses the screen cloth of 200 mesh, after being sieved Iron Si powder.
2)Insulating wrapped processing:The mixing liquid of phosphoric acid and alcohol is added into the iron Si powder after sieving, and stirs equal It is even, obtain the iron silicon slurry containing phosphoric acid.Then, the iron silicon slurry containing phosphoric acid is heated to 90-120 DEG C and is stirred continuously, Until being somebody's turn to do the iron silicon slurry drying containing phosphoric acid, acquisition is coated with phosphatic iron silicon insulation powder.
3)Add binding agent:Silicone, zinc stearate are added to being coated with phosphatic iron silicon insulation powder, and is stirred Mix uniform, acquisition is coated with phosphatic iron silicon insulation pre-feed.
Step 2:Preparation is coated with phosphatic iron sial insulation pre-feed.
1)Sieving is handled:Take sheet iron sial(Fe85Si9.6Al5.4)Powder crosses the screen cloth of 200 mesh, the iron after being sieved Sial powder.
2)Insulating wrapped processing:The mixing liquid of phosphoric acid, boric acid and alcohol is added into the iron sial powder after sieving, and Stir, obtain the iron sial slurry containing phosphoric acid and boric acid.Then, the iron sial powder containing phosphoric acid and boric acid is heated To 90-120 DEG C and be stirred continuously, until should iron sial slurry drying containing phosphoric acid and boric acid, acquisition is coated with phosphatic Iron sial insulation paste.In this step, boric acid only serves pH effect, does not generate insulating barrier.
3)Add binding agent:Phenol resin, zinc stearate are added to being coated with phosphatic iron sial insulation powder, and Stir, acquisition is coated with phosphatic iron sial insulation pre-feed.
Step 3:Prepare the mix insulation powder of iron silicon and iron sial.Will be as being coated with phosphatic iron made from step 1 Silicon insulate pre-feed with as being coated with phosphatic iron sial insulation pre-feed in mass ratio 2.00~9.00 made from step 2:1 Uniform mixing, obtains the mix insulation powder of iron silicon and iron sial.
Step 4:It is compressing.By hydraulic forming machine by the well mixed iron silicon obtained by step 3 and iron sial Mix insulation stamping of powder is molded, and obtains the mix insulation blank of iron silicon and iron sial.Wherein, the compacting pressure of hydraulic forming machine For 18.6~21.7 tons/cm2
Step 5:Heat treatment.Protective atmosphere is employed nitrogen as, the mixing of obtained iron silicon and iron sial will be suppressed by step 4 Insulation blank is placed at insulation 30min~120min in 700 DEG C~780 DEG C of anneal environment, and soft magnetic metal composite core is made.
Furtherly, in step 1, the mass ratio of iron Si powder after sieving, phosphoric acid and alcohol is 1:0.005~ 0.008:0.070.Wherein, the concentration of phosphoric acid is 85% liquid.
Furtherly, in step 1, phosphatic iron silicon insulation powder, silicone, the quality of zinc stearate are coated with Than for 1:0.004~0.006:0.003~0.005.Wherein, silicone is liquid, and zinc stearate is solid state powder.
Furtherly, in step 2, iron sial powder after sieving, phosphoric acid, the mass ratio of boric acid and alcohol are 1: 0.015~0.018:0.001~0.003:0.070.Wherein, the concentration of phosphoric acid is 85%, and boric acid is solid state powder.
Furtherly, in step 2, phosphatic iron sial insulation powder, phenol resin, the matter of zinc stearate are coated with Amount is than being 1:0.006~0.008:0.003~0.005.Wherein, phenol resin and zinc stearate are solid state powder.
Furtherly, in step 4, the mix insulation stamping of powder of iron silicon and iron sial is made to the blank of annular.
Embodiment 1:
The Fe that 1000g crosses the screening of 200 eye mesh screens is weighed respectively93.5Si6.5Spherical gas-atomised powders and 1000g cross 200 mesh sieves The Fe of mesh screen choosing85Si9.6Al5.4Ball-milled powder.Fe is weighed respectively93.5Si6.5The phosphoric acid solution of 85% concentration of powder weight 8 ‰ and Fe93.5Si6.5The alcohol of powder weight 7%, Fe is added after both are well mixed93.5Si6.5Powder simultaneously stirs, Ran Houjia Heat is incubated to 100 DEG C or so and is stirred continuously until magnetic is dried.Fe is weighed respectively85Si9.6Al5.4The 85% of powder weight 18 ‰ Phosphoric acid solution, the Fe of concentration85Si9.6Al5.4The boric acid and Fe of powder weight 1 ‰85Si9.6Al5.4The alcohol of powder weight 7%, Fe is added after three is well mixed85Si9.6Al5.4Powder simultaneously stirs, and is then heated to 100 DEG C or so and is incubated and constantly stirs Mix until magnetic is dried.According to mass ratio 7:3 ratio takes dried Fe respectively93.5Si6.5Powder and Fe85Si9.6Al5.4Powder End.By dried Fe93.5Si6.5Powder is mixed with the silicone of magnetic weight 5.5 ‰ and the zinc stearate of magnetic weight 3 ‰ Close uniform.By dried Fe85Si9.6Al5.4Powder and the phenol resin and the zinc stearate of magnetic weight 3 ‰ of magnetic weight 8 ‰ It is well mixed.To be insulated mixed Fe93.5Si6.5Powder and the mixed Fe that insulate85Si9.6Al5.4Powder is well mixed, and Using hydraulic forming machine in 18.6 tons/cm2Pressure under be pressed into OD26.92 × ID14.73 × H11.18(I.e. external diameter is 26.92mm, internal diameter are 14.73mm, are highly 11.18mm)Annular powder core.Powder core is put into the tubular type that nitrogen makees protective atmosphere 700 DEG C are heated in stove and furnace cooling after 30min is incubated, soft magnetic metal composite core is made.
The section EDS Element area profiles of soft magnetic metal composite core are as shown in Figure 1.It can be seen that, contain iron inside powder core Silica magnetic particle particle and Fe-Si-Al magnetic particle, the periphery of two kinds of magnetic powder particles are more equably coated with one layer and contain P element and O The insulating barrier of element.Using line footpath Φ 0.71mm, line length the 0.9m circle of enamel-covered wire coiling 25 electricity in iron silicon metal soft magnetic powder core Feel coil, measure obtained powder core magnetic electricity performance as follows:
(1)Under the conditions of 100kHz/1V, the μ H of inductance L=49.25;
(2)Under the conditions of 100kHz/1V, Q=124.67;
(3)DC stacked performance:When 100kHz, H=100Oe, LH/L0=62.57%;During H=200Oe, LH/L0=35.09%;
(4)Magnetic core loss:During 50kHz/100mT, Pcv=445mW/cm3
Embodiment 2:
The Fe that 1000g is screened through 200 eye mesh screens is weighed respectively93.5Si6.5Spherical gas-atomised powders and 1000g are through 200 mesh The Fe of screen cloth screening85Si9.6Al5.4Ball-milled powder.Fe is weighed respectively93.5Si6.5The phosphoric acid solution of 85% concentration of powder weight 7 ‰ And Fe93.5Si6.5The alcohol of powder weight 7%, Fe is added after both are well mixed93.5Si6.5Powder simultaneously stirs, then 100 DEG C or so are heated to be incubated and be stirred continuously until magnetic is dried.Fe is weighed respectively85Si9.6Al5.4Powder weight 15 ‰ Phosphoric acid solution, the Fe of 85% concentration85Si9.6Al5.4The boric acid and Fe of powder weight 2 ‰85Si9.6Al5.4The wine of powder weight 7% Essence, Fe is added after three is well mixed85Si9.6Al5.4Powder simultaneously stirs, and is then heated to 100 DEG C or so insulations not Disconnected stirring is until magnetic is dried.According to mass ratio 8:2 ratio takes dried Fe respectively93.5Si6.5Powder and Fe85Si9.6Al5.4Powder.By dried Fe93.5Si6.5Powder and Fe93.5Si6.5The silicone of powder weight 4 ‰ and Fe93.5Si6.5The zinc stearate of powder weight 5 ‰ is well mixed.By dried Fe85Si9.6Al5.4Powder and Fe85Si9.6Al5.4 The phenol resin and Fe of powder weight 7 ‰85Si9.6Al5.4The zinc stearate of powder weight 5 ‰ is well mixed.After insulation mixing Fe93.5Si6.5Powder and the mixed Fe that insulate85Si9.6Al5.4Powder is well mixed, and using hydraulic forming machine 20.1 Ton/cm2Pressure under be pressed into OD26.92 × ID14.73 × H11.18(I.e. external diameter is that 26.92mm, internal diameter are 14.73mm, height Spend for 11.18mm)Annular powder core.Powder core is put into nitrogen to make to be heated to 740 DEG C in the tube furnace of protective atmosphere and be incubated Furnace cooling after 60min, is made soft magnetic metal composite core.
The section EDS Element area profiles of soft magnetic metal composite core are as shown in Figure 2.It can be seen that, contain iron inside powder core Silica magnetic particle particle and Fe-Si-Al magnetic particle, the periphery of two kinds of magnetic powder particles are more equably coated with one layer and contain P element and O The insulating barrier of element.Using line footpath Φ 0.71mm, line length the 0.9m circle of enamel-covered wire coiling 25 electricity in iron silicon metal soft magnetic powder core Feel coil, measure obtained powder core magnetic electricity performance as follows:
(1)Under the conditions of 100kHz/1V, the μ H of inductance L=48.19;
(2)Under the conditions of 100kHz/1V, Q=124.66;
(3)DC stacked performance:When 100kHz, H=100Oe, LH/L0=66.89%;During H=200Oe, LH/L0=38.52%;
(4)Magnetic core loss:During 50kHz/100mT, Pcv=515mW/cm3
Embodiment 3:
The Fe that 1000g is screened through 200 eye mesh screens is weighed respectively93.5Si6.5Spherical gas-atomised powders and 1000g are through 200 mesh sieves The Fe of mesh screen choosing85Si9.6Al5.4Irregular ball-milled powder.Fe is weighed respectively93.5Si6.5The phosphoric acid of 85% concentration of powder weight 5 ‰ Solution and Fe93.5Si6.5The alcohol of powder weight 7%, Fe is added after both are well mixed93.5Si6.5Powder simultaneously stirs, 100 DEG C or so are then heated to be incubated and be stirred continuously until magnetic is dried.Fe is weighed respectively85Si9.6Al5.4Powder weight 16 ‰ 85% concentration phosphoric acid solution, Fe85Si9.6Al5.4The boric acid and Fe of powder weight 3 ‰85Si9.6Al5.4Powder weight 7% Alcohol, Fe is added after three is well mixed85Si9.6Al5.4Powder simultaneously stirs, and is then heated to 100 DEG C or so insulations simultaneously It is stirred continuously until magnetic is dried.According to mass ratio 9:1 ratio takes dried Fe respectively93.5Si6.5Powder and Fe85Si9.6Al5.4Powder.By dried Fe93.5Si6.5Powder and Fe93.5Si6.5The silicone of powder weight 6 ‰ and Fe93.5Si6.5The zinc stearate of powder weight 5 ‰ is well mixed.By dried Fe85Si9.6Al5.4Powder and Fe85Si9.6Al5.4Powder The phenol resin and Fe of last weight 6 ‰85Si9.6Al5.4The zinc stearate of powder weight 5 ‰ is well mixed.It will insulate mixed Fe93.5Si6.5Powder and the mixed Fe that insulate85Si9.6Al5.4Powder be well mixed, and using hydraulic forming machine 21.7 tons/ cm2Pressure under be pressed into OD26.92 × ID14.73 × H11.18(I.e. external diameter is that 26.92mm, internal diameter are 14.73mm, height For 11.18mm)Annular powder core.Powder core is put into nitrogen to make to be heated to 780 DEG C in the tube furnace of protective atmosphere and be incubated Furnace cooling after 120min, is made soft magnetic metal composite core.
The section EDS Element area profiles of soft magnetic metal composite core are as shown in Figure 3.It can be seen that, contain iron inside powder core Silica magnetic particle particle and Fe-Si-Al magnetic particle, the periphery of two kinds of magnetic powder particles are more equably coated with one layer and contain P element and O The insulating barrier of element.Using line footpath Φ 0.71mm, line length the 0.9m circle of enamel-covered wire coiling 25 electricity in iron silicon metal soft magnetic powder core Feel coil, measure obtained powder core magnetic electricity performance as follows:
(1)Under the conditions of 100kHz/1V, the μ H of inductance L=46.61;
(2)Under the conditions of 100kHz/1V, Q=121.43;
(3)DC stacked performance:When 100kHz, H=100Oe, LH/L0=72.01%;During H=200Oe, LH/L0=41.49%;
(4)Magnetic core loss:During 50kHz/100mT, Pcv=590mW/cm3
Furtherly, insulated by adjusting iron silicon with being coated with phosphatic iron sial in the mix insulation powder of iron sial The mass ratio of pre-feed, inductance, DC stacked performance and the magnetic core loss of linear regulation this soft magnetic metal composite core:
When the mass percent for being coated with phosphatic iron sial insulation pre-feed increases to 30% by 10%, institute of the present invention The inductance value for stating soft magnetic metal composite core rises to 49.25 μ H by 46.61 μ H, during superposition 100Oe D.C. magnetic fields, LH/L0By 72.01% is reduced to 62.57%, during superposition 200Oe D.C. magnetic fields, LH/L0Be reduced to 35.09% by 41.49%, magnetic core loss by 590mW/cm3It is reduced to 445mW/cm3

Claims (6)

1. a kind of preparation method of soft magnetic metal composite core, it is characterised in that:The soft magnetic metal composite core is by iron silicon The metal dust annealing of metal dust and iron sial is formed;Wherein, the mass ratio of iron silicon and iron sial is 2.00~9.00:1;Iron The metal dust of silicon and the metal dust of iron sial are the particulate by insulation processing;This soft magnetic metal composite core,
Under the conditions of 100kHz/1V, inductance L is between the μ H of 46.00 μ H~50.00;
Under the conditions of 100kHz/1V, quality factor q is between 121.00~125.00;
Under the conditions of 100kHz:As DC stacked magnetic field H=100Oe, LH/L0Between 62.00%~72.01%;When direct current is folded Plus during magnetic field H=200Oe, LH/L0Between 35.00%~41.49%;
Under the conditions of 50kHz/100mT, magnetic core loss PcvIn 445mW/cm3~590mW/cm3Between;
The Surface coating of iron silicon particle has had the phosphate particulate of insulating effect;The Surface coating of iron silicon aluminium particle has had insulation to make Phosphate particulate;
The operating procedure for preparing soft magnetic metal composite core is as follows:
Step 1:Preparation is coated with phosphatic iron silicon insulation pre-feed;
1)Sieving is handled:The spherical iron Si powder of aerosolization is taken to cross the screen cloth of 200 mesh, the iron Si powder after being sieved;
2)Insulating wrapped processing:The mixing liquid of phosphoric acid and alcohol is added into the iron Si powder after sieving, and is stirred, is obtained Iron silicon slurry that must be containing phosphoric acid;Then, the iron silicon slurry containing phosphoric acid is heated to 90-120 DEG C and be stirred continuously, until should Iron silicon slurry drying containing phosphoric acid, acquisition is coated with phosphatic iron silicon insulation powder;
3)Add binding agent:Silicone, zinc stearate are added to being coated with phosphatic iron silicon insulation powder, and stirs equal Even, acquisition is coated with phosphatic iron silicon insulation pre-feed;
Step 2:Preparation is coated with phosphatic iron sial insulation pre-feed;
1)Sieving is handled:Sheet iron sial powder is taken to cross the screen cloth of 200 mesh, the iron sial powder after being sieved;
2)Insulating wrapped processing:The mixing liquid of phosphoric acid, boric acid and alcohol is added into the iron sial powder after sieving, and is stirred Uniformly, the iron sial slurry containing phosphoric acid and boric acid is obtained;Then, the iron sial slurry containing phosphoric acid and boric acid is heated to 90-120 DEG C and be stirred continuously, until should iron sial slurry drying containing phosphoric acid and boric acid, acquisition is coated with phosphatic iron Sial insulation powder;
3)Add binding agent:Phenol resin, zinc stearate are added to being coated with phosphatic iron sial insulation powder, and is stirred Uniformly, obtain and be coated with phosphatic iron sial insulation pre-feed;
Step 3:Prepare the mix insulation powder of iron silicon and iron sial;Will be exhausted as being coated with phosphatic iron silicon made from step 1 Edge pre-feed with as being coated with phosphatic iron sial insulation pre-feed in mass ratio 2.00~9.00 made from step 2:1 is uniform Mixing, obtains the mix insulation powder of iron silicon and iron sial;
Step 4:It is compressing;By hydraulic forming machine by the mixing of well mixed iron silicon Yu the iron sial obtained by step 3 Insulating powder compression molding, obtains the mix insulation blank of iron silicon and iron sial;Wherein, the compacting pressure of hydraulic forming machine is 18.6~21.7 tons/cm2
Step 5:Heat treatment;Protective atmosphere is employed nitrogen as, the mix insulation of obtained iron silicon and iron sial will be suppressed by step 4 Blank is placed in insulation 30min~120min in 700 DEG C~780 DEG C of anneal environment, and soft magnetic metal composite core is made.
2. the preparation method of soft magnetic metal composite core as claimed in claim 1, it is characterised in that:In step 1, after sieving Iron Si powder, the mass ratio of phosphoric acid and alcohol be 1:0.005~0.008:0.070.
3. the preparation method of soft magnetic metal composite core as claimed in claim 1, it is characterised in that:In step 1, it is coated with Phosphatic iron silicon insulation powder, silicone, the mass ratio of zinc stearate are 1:0.004~0.006:0.003~0.005.
4. the preparation method of soft magnetic metal composite core as claimed in claim 1, it is characterised in that:In step 2, after sieving Iron sial powder, phosphoric acid, the mass ratio of boric acid and alcohol be 1:0.015~0.018:0.001~0.003:0.070.
5. the preparation method of soft magnetic metal composite core as claimed in claim 1, it is characterised in that:In step 2, it is coated with Phosphatic iron sial insulation powder, phenol resin, the mass ratio of zinc stearate are 1:0.006~0.008:0.003~ 0.005。
6. the preparation method of soft magnetic metal composite core as claimed in claim 1, it is characterised in that:By in regulating step 3 Iron silicon and the mass ratio that phosphatic iron sial insulation pre-feed is coated with the mix insulation powder of iron sial, linear regulation sheet The inductance of soft magnetic metal composite core, DC stacked performance and magnetic core loss:Insulated when being coated with phosphatic iron sial When the mass percent of pre-feed increases to 30% by 10%, the inductance value of soft magnetic metal composite core of the present invention is by 46.61 μ H rises to 49.25 μ H, during superposition 100Oe D.C. magnetic fields, LH/L062.57% is reduced to by 72.01%, 200Oe D.C. magnetic fields are superimposed When, LH/L035.09% is reduced to by 41.49%, magnetic core loss is by 590mW/cm3It is reduced to 445mW/cm3
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