CN104036907A - Method for preparing soft magnetic metal composite via warm compaction - Google Patents
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- CN104036907A CN104036907A CN201410246527.2A CN201410246527A CN104036907A CN 104036907 A CN104036907 A CN 104036907A CN 201410246527 A CN201410246527 A CN 201410246527A CN 104036907 A CN104036907 A CN 104036907A
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Abstract
The invention discloses a method for preparing a soft magnetic metal composite via warm compaction.The method comprises the steps of: 1) mixing a passivating agent and a solvent to form passivating liquid, mixing the passivating liquid with magnetic metal powder, stirring, and drying to form passivating powder, 2) dissolving an adhesive in a solvent to prepare an adhesive solution, mixing the adhesive solution and the passivating powder, uniformly stirring, and drying to form insulating coated soft magnetic metal powder, and 3) uniformly mixing the insulating coated soft magnetic metal powder and a lubricant, and loading into a mold for the warm compaction.The method has the advantages that with the adoption of a warm compaction method for preparing the soft magnetic metal composite, adhesive curing can be achieved in a forming process; pressing and curing can be merged into the warm compaction; a technology is simplified; the pressing pressure is reduced significantly; the obtained soft magnetic metal composite has the characteristics of high resistivity, high saturation flux density and low coercivity; and the method has wide application prospects in preparing soft magnetic metal powder cores.
Description
Technical field
The present invention relates to a kind of warm compaction molding and prepare the method for soft magnetic metal composite material, belong to electronic devices and components new material new process field.
Background technology
Warm compaction molding method is by mixed-powder preheating in sealing punching block, then carries out extrusion forming, because the temperature of suppressing is between common room temperature and hot pressing temperature, thereby is referred to as temperature and pressure.Warm-pressing technology can obtain higher green density and intensity with lower pressing pressure, and at high strength iron-based part, the fields such as Agglutinate neodymium-iron-boron magnet exist extensive use.
Along with the development of electronic technology, the ever more important for electronic device of saving energy and reduce the cost, the loss reducing by every means under high frequency is significant.The loss under high frequency of traditional silicon steel disc is too large, has limited its frequency applications, then by Magnaglo carry out passivation, insulating wrapped, the soft magnetic metal composite material that obtains after compressing can effectively solve the loss problem under high frequency.The principal character of soft magnetic metal composite material is that magnetic metallic powder is coated by dielectric, and resistivity is higher than traditional metal soft magnetic material, and saturation flux density is higher than soft magnetic ferrites, and applying frequency is wider.In field of power electronics, the composite material moulded powder core of making of soft magnetic metal is widely used in electronic components such as making transformer, filter, instrument transformer.
But due to insulating wrapped, magnetic metal particle spacing increases, make magnetic metallic powder in compacting, to solidify after processing, the density of base substrate can reduce, and then causes mechanical strength to reduce.And because the internal stress of compressing introducing worsens the magnetic property of material, need to increase stress relief annealing work technique, make production process complicated.Therefore developing a kind of material preparation method that can improve soft magnetic metal composite material forming density is extremely necessary.
Summary of the invention
The object of this invention is to provide a kind of warm compaction molding and prepare the method for soft magnetic metal composite material.
The method that warm compaction molding is prepared soft magnetic metal composite material comprises the steps:
1) powder passivation
Solvent and passivator are made into passivating solution, and the soft magnetic metal powder that is 0.1～250 μ m by particle size mixes, and adds passivating solution, stirs 0.1～2h, puts into baking oven passivation, and passivation temperature is 40～100 ℃, and passivation time is 0.1～4h, obtains passivating powder;
2) insulating wrapped
Binding agent is dissolved in organic solvent, obtains binder solution, add binder solution in passivating powder, stir 0.1～2h, put into oven for drying, baking temperature is 40～100 ℃, and baking time is 0.1～4h, obtains the soft magnetic metal powder of insulating wrapped;
3) warm compaction molding
Lubricant is added in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, soft magnetic metal powder in die cavity is heated and is incubated, heating-up temperature is 60～150 ℃, makes in pressing process, and binding agent occurs to solidify, adopt the pressure of 600～1200Mpa by powder pressing forming, pressurize 5～30min, the demoulding, obtains sample.
Described soft magnetic metal powder is reduced iron powder, carbonyl iron dust, sendust powder, Fe-Ni Alloy Powder, iron nickel-molybdenum alloy powder, ferrum-silicon-boron amorphous powder, ferro-silicium powder or iron silicon nickel alloy powder.Described solvent is deionized water, ethanol, methylethylketone, acetone, butanone or ethyl acetate.Described passivator is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid.In described passivating solution, the mass fraction of passivator is 0.1～5%.The mass ratio of described passivating solution and soft magnetic metal powder is 0.01:1～1:1.Described binding agent is epoxy resin, phenolic resins, polyvinyl alcohol, polyvinyl butyral resin or glass dust, and in binder solution, the mass fraction of binding agent is 5～50%.Described binder solution and the mass ratio of metal dust are 0.01:1～1:1.
Described lubricant is zinc stearate, barium stearate, acyl acidic group wax, lithium stearate or six side BN, 0.1～1% of the soft magnetic metal opaque amount that lubricant content is insulating wrapped.Described mold shape is cuboid, cylinder, Elliptic Cylinder or their assembly.
The present invention compared with prior art has the following advantages:
1) by warm compaction molding, can prepare and there is high pressed density, the soft magnetic metal composite material of high mechanical properties;
2) temperature while controlling compacting by warm compaction molding, suppression process and the curing process that traditional shaping method to suppress can be prepared to soft magnetic metal composite material are reduced to a procedure, and production process is simple, and efficiency is high;
3) the soft magnetic metal composite material of preparing has high saturation magnetic flux density, low-coercivity, low-loss, the feature of high resistivity.
Embodiment
Soft magnetic metal composite material and preparation method thereof of the present invention is that magnetic metallic powder after passivation, is mixed with binder solution in passivating solution, stirs, and dries, and adds lubricant to carry out warm compaction molding after insulating wrapped.This kind of soft magnetic metal composite material has high saturation flux density, high resistivity, high density and excellent mechanical strength.
The method that warm compaction molding is prepared soft magnetic metal composite material comprises the steps:
1) powder passivation
Solvent and passivator are made into passivating solution, and the soft magnetic metal powder that is 0.1～250 μ m by particle size mixes, and adds passivating solution, stirs 0.1～2h, puts into baking oven passivation, and passivation temperature is 40～100 ℃, and passivation time is 0.1～4h, obtains passivating powder;
2) insulating wrapped
Binding agent is dissolved in organic solvent, obtains binder solution, add binder solution in passivating powder, stir 0.1～2h, put into oven for drying, baking temperature is 40～100 ℃, and baking time is 0.1～4h, obtains the soft magnetic metal powder of insulating wrapped;
3) warm compaction molding
Lubricant is added in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, soft magnetic metal powder in die cavity is heated and is incubated, heating-up temperature is 60～150 ℃, makes in pressing process, and binding agent occurs to solidify, adopt the pressure of 600～1200Mpa by powder pressing forming, pressurize 5～30min, the demoulding, obtains sample.
Described soft magnetic metal powder is reduced iron powder, carbonyl iron dust, sendust powder, Fe-Ni Alloy Powder, iron nickel-molybdenum alloy powder, ferrum-silicon-boron amorphous powder, ferro-silicium powder or iron silicon nickel alloy powder.Described solvent is deionized water, ethanol, methylethylketone, acetone, butanone or ethyl acetate.Described passivator is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid.In described passivating solution, the mass fraction of passivator is 0.1%～5%.The mass ratio of described passivating solution and soft magnetic metal powder is 0.01:1～1:1.Described binding agent is epoxy resin, phenolic resins, polyvinyl alcohol, polyvinyl butyral resin or glass dust, and in binder solution, the mass fraction of binding agent is 5%～50%.Described binder solution and the mass ratio of metal dust are 0.01:1～1:1.
Described lubricant is zinc stearate, barium stearate, acyl acidic group wax, lithium stearate or six side BN, 0.1%～1% of the soft magnetic metal opaque amount that lubricant content is insulating wrapped.Described mold shape is cuboid, cylinder, Elliptic Cylinder or their assembly.
By the present invention, can prepare high compact density, saturation flux density, low-coercivity, high resistivity, low-loss, excellent mechanical strength soft magnetic metal composite material.
Below in conjunction with instantiation, the present invention will be further described, but the present invention is not limited only to following examples.
Embodiment 1:
1) phosphoric acid and acetone being made into mass fraction is 0.6% passivating solution, in the mass ratio of 3:1:1, get that particle diameter is respectively the reduced iron powder of 150 μ m, 75 μ m, 45 μ m and ratio that passivating solution is 1:0.1 according to mass ratio is carried out passivation, in mixer, stir 0.5h, put into baking oven passivation, passivation temperature is 70 ℃, passivation time is 1h, obtains passivating powder;
2) epoxy resin and ethanol being made into epoxy resin mass fraction is 10% binder solution, the ratio that is 0.1:1 according to mass ratio by binder solution and passivating powder is mixed, mixer stirs 0.5h, stir, in 80 ℃ of baking ovens, toast 2h, dry, the soft magnetic metal powder that obtains insulating wrapped is stand-by.
3) lubricant stearic acid zinc is added according to mass fraction 0.3% in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, magnetic in die cavity is heated and is incubated, heating-up temperature is 100 ℃, adopt the pressure of 800Mpa by powder pressing forming, pressurize 10min, the demoulding, obtains sample.
The sample tissue of preparing is fine and close, and porosity is low, and density is 7.2g/cm
3, tensile fracture is 37kg, and sample is carried out to soft magnet performance and electrical performance testing, result is as follows: saturation flux density Bs=1.5T, coercivity H=130A/m, electricalresistivityρ=1.3 * 10
5Ω cm, loss is 330mW/cm
3/ (50KHz/0.05T), and the mechanical performance of sample, magnetics and electric property are excellent.
Embodiment 2:
1) phosphoric acid and ethanol being made into mass fraction is 0.1% passivating solution, in the mass ratio of 3:2:1, get that particle diameter is respectively the Fe-Ni Alloy Powder of 150 μ m, 75 μ m, 45 μ m and ratio that passivating solution is 1:0.01 according to mass ratio is carried out passivation, in mixer, stir 0.1h, put into baking oven passivation, passivation temperature is 40 ℃, passivation time is 4h, obtains passivating powder.
2) epoxy resin and acetone being made into epoxy resin mass fraction is 50% binder solution, the ratio that is 1:1 according to mass ratio by binder solution and passivating powder is mixed, mixer stirs 2h, stir, in 40 ℃ of baking ovens, toast 4h, dry, the soft magnetic metal powder that obtains insulating wrapped is stand-by.
3) lubricant stearic acid zinc is added according to mass fraction 0.1% in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, magnetic in die cavity is heated and is incubated, heating-up temperature is 60 ℃, adopt the pressure of 1200Mpa by powder pressing forming, the pressurize 5min demoulding, obtains sample.
The sample tissue of preparing is fine and close, and porosity is low, and density is 8g/cm
3, tensile fracture is 43kg, and sample is carried out to soft magnet performance and electrical performance testing, result is as follows: saturation flux density Bs=1.6T, coercivity H=150A/m, electricalresistivityρ=3.7 * 10
5Ω cm, loss is 120mW/cm
3/ (50KHz/0.05T), and the mechanical performance of sample, magnetics and electric property are excellent.
Embodiment 3:
1) phosphoric acid and acetone being made into mass fraction is 5% passivating solution, in the mass ratio of 3:2:1, get that particle diameter is respectively the sendust powder of 250 μ m, 75 μ m, 45 μ m and ratio that passivating solution is 1:1 according to mass ratio is carried out passivation, in mixer, stir 2h, put into baking oven passivation, passivation temperature is 100 ℃, passivation time is 0.1h, obtains passivating powder.
2) phenolic resins and ethanol being made into epoxy resin mass fraction is 5% binder solution, the ratio that is 0.01:1 according to mass ratio by binder solution and passivating powder is mixed, mixer stirs 0.1h, stir, in 100 ℃ of baking ovens, toast 0.1h, dry, the soft magnetic metal powder that obtains insulating wrapped is stand-by.
3) lubricant stearic acid barium is added according to mass fraction 1% in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, magnetic in die cavity is heated and is incubated, heating-up temperature is 150 ℃, adopt the pressure of 600Mpa by powder pressing forming, the pressurize 30min demoulding, obtains sample.
The sample tissue of preparing is fine and close, and porosity is low, and density is 6.3g/cm
3, tensile fracture is 32kg, and sample is carried out to soft magnet performance and electrical performance testing, result is as follows: saturation flux density Bs=1.1T, coercivity H=35A/m, electricalresistivityρ=6.3 * 10
6Ω cm, loss is 120mW/cm
3/ (50KHz/0.05T), and the mechanical performance of sample, magnetics and electric property are excellent.
Embodiment 4:
1) phosphoric acid and acetone being made into mass fraction is 0.8% passivating solution, in the mass ratio of 3:1:1, get that particle diameter is respectively the ferrum-silicon-boron amorphous powder of 150 μ m, 75 μ m, 0.1 μ m and ratio that passivating solution is 1:0.08 according to mass ratio is carried out passivation, in mixer, stir 0.5h, put into baking oven passivation, passivation temperature is 80 ℃, passivation time is 1.5h, obtains passivating powder.
2) phenolic resins and ethanol being made into epoxy resin mass fraction is 10% binder solution, the ratio that is 0.1:1 according to mass ratio by binder solution and passivating powder is mixed, mixer stirs 0.5h, stir, in 80 ℃ of baking ovens, toast 2h, dry, the soft magnetic metal powder that obtains insulating wrapped is stand-by.
3) six side BN are added according to mass fraction 0.3% in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, the magnetic in die cavity is heated and is incubated, heating-up temperature is 170 ℃, adopt the pressure of 900Mpa by powder pressing forming, the pressurize 20min demoulding, obtains sample.
The sample tissue of preparing is fine and close, and porosity is low, and density is 6.1g/cm
3, tensile fracture is 30kg, and sample is carried out to soft magnet performance and electrical performance testing, result is as follows: saturation flux density Bs=1.0T, coercivity H=5A/m, electricalresistivityρ=8.5 * 10
6Ω cm, loss is 30mW/cm
3/ (50KHz/0.05T), and the mechanical performance of sample, magnetics and electric property are excellent.
Claims (9)
1. warm compaction molding is prepared a method for soft magnetic metal composite material, it is characterized in that comprising the steps:
1) powder passivation
Solvent and passivator are made into passivating solution, and the soft magnetic metal powder that is 0.1～250 μ m by particle size mixes, and adds passivating solution, stirs 0.1～2h, puts into baking oven passivation, and passivation temperature is 40～100 ℃, and passivation time is 0.1～4h, obtains passivating powder;
2) insulating wrapped
Binding agent is dissolved in organic solvent, obtains binder solution, add binder solution in passivating powder, stir 0.1～2h, put into oven for drying, baking temperature is 40～100 ℃, and baking time is 0.1～4h, obtains the soft magnetic metal powder of insulating wrapped;
3) warm compaction molding
Lubricant is added in the soft magnetic metal powder of insulating wrapped and stir, pack in mould, soft magnetic metal powder in die cavity is heated and is incubated, heating-up temperature is 60～150 ℃, makes in pressing process, and binding agent occurs to solidify, adopt the pressure of 600～1200Mpa by powder pressing forming, pressurize 5～30min, the demoulding, obtains sample.
2. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described soft magnetic metal powder is reduced iron powder, carbonyl iron dust, sendust powder, Fe-Ni Alloy Powder, iron nickel-molybdenum alloy powder, ferrum-silicon-boron amorphous powder, ferro-silicium powder or iron silicon nickel alloy powder.
3. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described solvent is deionized water, ethanol, methylethylketone, acetone, butanone or ethyl acetate.
4. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described passivator is hydrogen peroxide, potassium permanganate, phosphoric acid or chromic acid.
5. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that the mass fraction of passivator in described passivating solution is 0.1～5%.
6. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described passivating solution and the mass ratio of soft magnetic metal powder are 0.01:1～1:1.
7. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described binding agent is epoxy resin, phenolic resins, polyvinyl alcohol, polyvinyl butyral resin or glass dust, in binder solution, the mass fraction of binding agent is 5～50%.
8. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described binder solution and the mass ratio of metal dust are 0.01:1～1:1.
9. a kind of warm compaction molding according to claim 1 is prepared the method for soft magnetic metal composite material, it is characterized in that described lubricant is zinc stearate, barium stearate, acyl acidic group wax, lithium stearate or six side BN, 0.1～1% of the soft magnetic metal opaque amount that lubricant content is insulating wrapped.
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