CN105344993B - A kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core - Google Patents

A kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core Download PDF

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CN105344993B
CN105344993B CN201510888547.4A CN201510888547A CN105344993B CN 105344993 B CN105344993 B CN 105344993B CN 201510888547 A CN201510888547 A CN 201510888547A CN 105344993 B CN105344993 B CN 105344993B
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magnetic
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CN105344993A (en
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黄钧声
王志远
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GUANGZHOU QIDA MATERIAL TECHNOLOGY Co Ltd
Guangdong University of Technology
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GUANGZHOU QIDA MATERIAL TECHNOLOGY Co Ltd
Guangdong University of Technology
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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
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • B22F1/0003
    • 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
    • B22F1/16Metallic particles coated with a non-metal
    • 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
    • H01F1/147Alloys characterised by their composition
    • H01F1/14766Fe-Si based alloys
    • H01F1/14791Fe-Si-Al based alloys, e.g. Sendust
    • 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
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F2003/023Lubricant mixed with the metal powder

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  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention discloses a kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core, the described method comprises the following steps: (1) using passivator processing is passivated to initial soft-magnetic alloy powder, it is dry;(2) soft-magnetic alloy powder after drying is uniformly mixed with binder;(3) by mixed-powder drying and screening, insulating compound mixing cladding is then added;(4) it by the soft-magnetic alloy powder coated and mix lubricant, and is packed into mold, is then heated while pressurization, temperature and pressure compression moulding;(5) powder core of temperature and pressure compression moulding is made annealing treatment;The weight percentage of the initial soft-magnetic alloy powder are as follows: silicon 8.5~10.5%, aluminium 4.5~6.5%, surplus are iron;Lubricant in step (4) is the mixture of zinc stearate and polyethylene glycol.Method disclosed by the invention can effectively improve the density and magnetic conductivity of preparation gained soft-magnetic powder core, significantly reduce magnetic loss.

Description

A kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core
Technical field
The present invention relates to metal material powder metallurgy manufacturing field, especially a kind of preparation side of iron-silicon-aluminum soft magnet powder core Method and the soft-magnetic powder core being prepared using the method.
Background technique
Powder core is a kind of by powder metallurgical technique, soft-magnetic alloy powder is mixed with dielectric made of suppressing, Novel soft magnetism functional material with magnetoelectricity conversion features.Since granularity of magnet powder is very small, and in ferromagnetic powder particle Coated with uniform one layer of dielectric insulating film, improve the resistivity of powder core, hinder the eddy current effect between magnetic powder, Thus eddy-current loss is very low, is suitable for upper frequency and applies (20kHz or more).In addition, powder core saturation magnetic also with higher Induction, good frequency characteristic, compared with low-coercivity and permanent magnetic conduction and temperature stability the advantages that so that powder core is as electric Feel filter, holds back streamline circle and be widely used in the fields such as telecommunications, radar, power switch, it is important to have become soft magnetic materials Component part.
Fe-Si-Al magnetic core component is Fe- (8~13%) Si- (4~7%) Al, is a kind of to have magnetoelectricity conversion function Novel soft magnetic materials.Because of its superior soft magnet performance and price appropriate, it is widely used in pulse transformer, returns transformation In the electronic device of device, line noise filter, energy storage inductor etc..At present Fe-Si-Al magnetic core be in large-scale application and The further development phase.
In general, pressure is bigger, and the density of green compact is higher, and the magnetic conductivity of magnetic powder is bigger.But increase pressure, to powder core The raising of density has the limit, and pressure is excessive to also result in insulating layer rupture, thus reduced insulation effect.
Powder metal warm compaction forming technique is by the way that traditional powder metallurgy press is transformed, heated using special powder, The heating system of powder conveying and mold, is heated to a spy for the mixed-powder for being mixed with the dedicated lubricant of temperature and pressure, binder Fixed temperature is suppressed, then is sintered using traditional handicraft, to obtain the product of higher density and performance.Currently, warm Pressure improves mechanical property mainly for the preparation of structural material, improves soft-magnetic powder core performance applied to powder magnetic material is developed It studies also rarely found.In terms of published patent, only " a kind of warm-pressing formation prepares metal soft magnetic composite material for Zhejiang University Method (application number CN201410246527.2) " and a kind of Guangdong University of Technology " preparation method (Shen of amorphous soft magnet powder core Please number CN201410013455.7) ".Zhu Tao (Zhu Tao powder warm compactingprocess compounded lubricant and its preparation Fe-Si soft magnetism material The Hefei application study [D] in material: Hefei Polytechnics, 2012) temperature and pressure are had studied applied to Fe-Si magnetically soft alloy to its group The effect for knitting structure and mechanical property, using the mixture of amine based polymer, stearate and ethylene glycol polymer as temperature Pressure lubricating agent.H.Shokrollahi et al. (H.Shokrollahi.et al..Journal of Magnetism and Magnetic Materials.2007,313:182-186) have studied at room temperature pressing parameter to multiple for main soft magnetism with straight iron powder The influence of condensation material powder core magnetic property, is with lubricator zinc stearate, the results showed that, with the increase of pressing pressure, powder The density of core increased, and magnetic conductivity and magnetic induction intensity improve, but pressure increase simultaneously introduce dislocation the defects of and interior answer Power also increases, thus coercivity also increased.
Soft magnetic materials is widely applied in field of power electronics, and the application product of alloy mostly uses cold quenching strip at present It is wound into the processing of magnetic core after annealing.But the loss characteristic of high band limits strip core application, and after Overheating Treatment Strip brittleness it is big, in industrial circle, need that the special shape for meeting various needs is made of such material in most cases. Under the premise of not damaging this material this advantage of excellent soft magnet performance, the loss value of magnetic core should be significantly reduced, will be closed Gold ribbon material is broken into magnetic powder, and this purpose can be realized by being pressed into powder core.FeSiAl soft magnetism magnetic is prepared using temperature and pressure at present Powder core has not been reported.
Summary of the invention
It is an object of the invention to provide based on the above background and a kind of prepare soft-magnetic powder core using temperature-pressure formation Method;Meanwhile the present invention also provides the soft-magnetic powder core being prepared using the method, the soft-magnetic powder core has Higher magnetic conductivity and lower magnetic loss.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of temperature and pressure prepare iron-silicon-aluminum soft magnet powder core Method, comprising the following steps:
(1) processing is passivated to initial soft-magnetic alloy powder using passivator, it is dry;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder;
(3) the mixed-powder drying and screening for obtaining step (2) then adds insulating compound mixing cladding;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, temperature and pressure compression moulding;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment;
The weight percentage of the initial soft-magnetic alloy powder are as follows: silicon 8.5~10.5%, aluminium 4.5~6.5%, surplus For iron;
Lubricant in the step (4) is the mixture of zinc stearate and polyethylene glycol.
Temperature and pressure of the present invention are prepared in the method for iron-silicon-aluminum soft magnet powder core, using special lubricant temperature and pressure, Ke Yi great The soft magnet performances such as big magnetic conductivity, the magnetic loss for improving preparation gained powder core, further increase the cost performance of soft-magnetic powder core, have Prestige obtains considerable economic benefit in a short time.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core is prepared as temperature and pressure of the present invention, it is described initial soft The weight percentage of magnetic alloy powder are as follows: silicon 9.9%, aluminium 5.5%, surplus are iron, using the initial magnetically soft alloy of this ingredient When powder, being prepared is FeSiAl soft-magnetic powder core, magnetic conductivity with higher and higher cost performance.Institute of the present invention Stating soft-magnetic alloy powder can be used the acquisition of prior art means, can be directly from market purchase etc..Soft-magnetic alloy powder in the present invention It is preferably but not limited to the soft-magnetic alloy powder of ingredient described above, the soft-magnetic alloy powder acquisition of mentioned component is from a wealth of sources, and And cost performance with higher.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (4) in lubricant, the mass ratio of zinc stearate and polyethylene glycol is (0.02~5): 1.It is prepared as temperature and pressure of the present invention The more preferable embodiment of the method for iron-silicon-aluminum soft magnet powder core, in the lubricant of the step (4), zinc stearate and poly- second two The mass ratio of alcohol is (3~1): 2.The most preferably implementation of the method for iron-silicon-aluminum soft magnet powder core is prepared as temperature and pressure of the present invention Mode, in the lubricant of the step (4), the mass ratio of zinc stearate and polyethylene glycol is 2:3.Temperature and pressure preparation of the present invention The method of iron-silicon-aluminum soft magnet powder core, using special lubricant, i.e., the described lubricant is respectively stearic by two kinds of material compositions Sour zinc and polyethylene glycol, and the mass ratio of the two is (0.02~5): 1.Present inventor by numerous studies find, when When the lubricant uses the zinc stearate and polyethylene glycol of the specific proportion, it is prepared using the method for the invention Iron-silicon-aluminum soft magnet powder core magnetic conductivity with higher and very low magnetic loss.Especially in the lubricant, zinc stearate When mass ratio with polyethylene glycol is 2:3, obtained iron-silicon-aluminum soft magnet powder core has highest magnetic conductivity and minimum magnetic Loss.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (4) mass ratio of lubricant and initial soft-magnetic alloy powder is 0.4~2% in.Iron sial is prepared as temperature and pressure of the present invention The more preferable embodiment of the method for soft-magnetic powder core, the quality of lubricant and initial soft-magnetic alloy powder in the step (4) Than being 0.5~1.5%.Present inventor has found after study, in the application the performance of gained soft-magnetic powder core not only with institute It is related with the ratio of polyethylene glycol but also related with the additive amount of lubricant to state zinc stearate in lubricant, the present application People has found through overtesting, when the mass ratio of the lubricant and initial soft-magnetic alloy powder is 0.4~2%, gained soft magnetism magnetic Powder core density with higher, magnetic conductivity and lower magnetic loss;Especially when the lubricant and initial soft-magnetic powder core When mass ratio is 0.5~1.5%, gained soft-magnetic powder core has better density, magnetic conductivity and lower magnetic loss.
The preferred embodiment of the method for soft-magnetic powder core described in iron sial, the step are prepared as temperature and pressure of the present invention (2) binder in is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin;Insulating compound in the step (3) is nanometer two Silica.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (2) in binder, the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is (4~1): 2.As temperature and pressure system of the present invention The more preferable embodiment of the method for standby iron-silicon-aluminum soft magnet powder core, in the binder of the step (2), sodium metasilicate and high temperature resistant The mass ratio of organic siliconresin is 3:2.In the preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, the binder is used Specific two kinds of material compositions, i.e. sodium metasilicate and high-temperature resistant silicone acid resin, and the mass ratio of the two is (4~1): 2, this Apply for that inventor has found by numerous studies, when the binder uses the sodium metasilicate and high-temperature resistant organic silicon resin of specific proportion When composition, cooperates the lubricant and process conditions of the specific proportion, the iron of higher magnetic permcability and very low magnetic loss can be obtained Silicon-aluminum soft magnet powder core.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (2) mass ratio of binder and initial soft-magnetic alloy powder in is 1~2%;Insulating compound and initial soft magnetism in the step (3) The mass ratio of alloy powder is 0~0.4%.The more excellent of the method for iron-silicon-aluminum soft magnet powder core is prepared as temperature and pressure of the present invention Embodiment is selected, the mass ratio of the binder in the step (2) and initial soft-magnetic alloy powder is 1.5%;The step (3) The mass ratio of middle insulating compound and initial soft-magnetic alloy powder is 0.1~0.4%.It is soft that iron sial is prepared as temperature and pressure of the present invention The more preferable embodiment of the method for magnetic powder core, the mass ratio of insulating compound and initial soft-magnetic alloy powder in the step (3) It is 0.2%.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (1) for the passivator used in for phosphoric acid solution, the mass percentage concentration of the phosphoric acid solution is 0.4~3% (remaining is water), institute The mass ratio for stating phosphoric acid solution and initial soft-magnetic alloy powder is (0.5~1.5): 1.When phosphoric acid solution passivating agent concentration is very low When, in the very thin thickness for the phosphating coat that powder particle surface generates, passivation effect is less complete.With the increase of passivating agent concentration With the intensification of degree of passivation, powder particle surface produces complete, uniform fold phosphating coat.But phosphoric acid solution passivator is dense When spending high, phosphatization film thickness is excessive and it is be easy to cause to crack and fall off.It is soft that iron sial is prepared as temperature and pressure of the present invention The more preferable embodiment of the method for magnetic powder core, for the middle passivator used of the step (1) for phosphoric acid solution, the phosphoric acid is molten The mass percentage concentration of liquid is 0.7%.When the mass percentage concentration of the phosphoric acid solution passivator is 0.7%, can reach Optimal film-forming state.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (4) pressing pressure of temperature and pressure compression moulding is 500~1200MPa in, and press temperature is 60~150 DEG C.When pressing pressure is too small, Powder core density is not high enough, performance is bad, and when pressing pressure is excessive, mold is easily damaged.When press temperature is too low, solid lubrication Agent, which is not yet melted, causes temperature and pressure density improvement effect unobvious;When the temperature is excessively high, lubrication film viscosity reduces temperature and pressure, causes powder Intergranular directly contacts, and density is caused to decline instead, and internal stress is high, is unfavorable for improving soft magnet performance.Soft magnetism of the present invention The preparation method of powder core, can be in temperature and pressure temperature using the pressing pressure and press temperature in the temperature and pressure pressing process Higher density is obtained with lesser pressing pressure under degree, and resulting powder core internal stress is low, help to obtain higher In addition magnetic conductivity and lower loss can reduce pressing pressure, less mold is lost, and economic benefits are significant.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core, the step are prepared as temperature and pressure of the present invention (5) annealing temperature made annealing treatment in is 550~750 DEG C, and annealing time is 0.5~1.5 hour.Annealing temperature is lower, the time Shorter, then it is unobvious to eliminate internal stress effect, is unfavorable for improving magnetic property;Annealing temperature is excessively high, then powder core is easy to aoxidize change Matter, consuming energy, and may also result in the damage layer that insulate between powder particle, deteriorate magnetic property.
Meanwhile the present invention also provides a kind of iron-silicon-aluminum soft magnet powder core with higher magnetic permcability and lower magnetic loss, it is Realize this purpose, the technical scheme adopted by the invention is as follows: a kind of iron-silicon-aluminum soft magnet powder core uses method as described above to prepare It obtains.
The preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, powder metallurgy warm-pressing New technical use is soft in amorphous The preparation of magnetic powder core, is groped by a large number of experiments, and specific lubricant described in final choice and other chargings select and feed Sequentially, the combination of pressing pressure, press temperature etc., these integrally combine the method and technology scheme of composition, and the amorphous prepared is soft Magnetic powder core density with higher and lower internal stress, gained powder core magnetic conductivity with higher and very low magnetic loss Consumption.The preparation method of soft-magnetic powder core of the present invention, compared with existing soft-magnetic powder core technology of preparing, the method for the present invention energy Higher density is obtained with lesser pressing pressure at a temperature of temperature and pressure, and powder core internal stress is low, to be conducive to magnetic domain Wall movement and domain rotation, favorably obtain higher magnetic conductivity and lower loss.And method of the invention can reduce compacting Pressure reduces mold loss, has more significant economic benefits.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention It is described further.
In following embodiment, the weight percentage of the initial soft-magnetic alloy powder is equal are as follows: silicon 8.5~10.5%, aluminium 4.5~6.5%, surplus is iron.More preferably, in following embodiment, the weight percentage of the initial soft-magnetic alloy powder is equal Are as follows: silicon 9.9%, aluminium 5.5%, surplus are iron.
Embodiment 1
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 0.4%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 0.5:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 2%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicic acid Sodium, high-temperature resistant organic silicon resin mass ratio be 2:1;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.1%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 500MPa, temperature is 150 DEG C;The lubricant with it is initial soft The mass ratio of magnetic alloy powder is 1%, and the lubricant is the mixture of zinc stearate and polyethylene glycol, and the zinc stearate Mass ratio with polyethylene glycol is 0.02:1;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 550 DEG C, when annealing Between be 0.5h.
Embodiment 2
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 1%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 0.6:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 1.8%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicon Sour sodium, high-temperature resistant organic silicon resin mass ratio be 3:2;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.15%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 800MPa, temperature is 90 DEG C;The lubricant and initial soft magnetism The mass ratio of alloy powder be 2%, the lubricant be zinc stearate and polyethylene glycol mixture, and the zinc stearate and The mass ratio of polyethylene glycol is 0.4:1;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 600 DEG C, when annealing Between be 0.6h.
Embodiment 3
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 2%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 0.8:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 1.6%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicon Sour sodium, high-temperature resistant organic silicon resin mass ratio be 3:2;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.2%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 600MPa, temperature is 120 DEG C;The lubricant with it is initial soft The mass ratio of magnetic alloy powder is 0.5%, and the lubricant is the mixture of zinc stearate and polyethylene glycol, and the stearic acid The mass ratio of zinc and polyethylene glycol is 1:2;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 630 DEG C, when annealing Between be 1h.
Embodiment 4
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 0.7%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 1:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 1.5%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicon Sour sodium, high-temperature resistant organic silicon resin mass ratio be 3:2;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.2%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 1100MPa, temperature is 100 DEG C;The lubricant with it is initial soft The mass ratio of magnetic alloy powder is 1.3%, and the lubricant is the mixture of zinc stearate and polyethylene glycol, and the stearic acid The mass ratio of zinc and polyethylene glycol is 2:3;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 680 DEG C, when annealing Between be 1h.
Embodiment 5
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 3%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 1.2:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 1.2%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicon Sour sodium, high-temperature resistant organic silicon resin mass ratio be 2:3;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.3%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 1000MPa, temperature is 80 DEG C;The lubricant with it is initial soft The mass ratio of magnetic alloy powder is 1.5%, and the lubricant is the mixture of zinc stearate and polyethylene glycol, and the stearic acid The mass ratio of zinc and polyethylene glycol is 3:2;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 700 DEG C, when annealing Between be 1.3h.
Embodiment 6
Temperature and pressure of the present invention prepare a kind of embodiment of the method for iron-silicon-aluminum soft magnet powder core, soft-magnetic powder described in the present embodiment The preparation method of core the following steps are included:
(1) processing is passivated to initial soft-magnetic alloy powder using the phosphoric acid solution that mass percentage concentration is 1.5%, done It is dry;The mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is 1.5:1;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder, the binder and initial soft magnetism The mass ratio of alloy powder is 1%, and the binder is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the silicic acid Sodium, high-temperature resistant organic silicon resin mass ratio be 1:2;
(3) the mixed-powder drying and screening for obtaining step (2) then adds nano silica mixing cladding, described The mass ratio of nano silica and initial soft-magnetic alloy powder is 0.4%;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then adding It is heated while pressure, the temperature and pressure compression moulding in the case where pressure is 1200MPa, temperature is 60 DEG C;The lubricant with it is initial soft The mass ratio of magnetic alloy powder is 0.4%, and the lubricant is the mixture of zinc stearate and polyethylene glycol, and the stearic acid The mass ratio of zinc and polyethylene glycol is 5:1;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment, annealing temperature is 750 DEG C, when annealing Between be 1.5h.
Embodiment 7
The performance test for the iron-silicon-aluminum soft magnet powder core that the method for the invention is prepared
The performance for the iron-silicon-aluminum soft magnet powder core that Examples 1 to 6 is prepared respectively is tested, and tests every group respectively Density, magnetic conductivity (when 50kHz and when 1000kHz), the magnetic loss (50kHz/0.05T) of gained iron-silicon-aluminum soft magnet powder core are surveyed Test result is shown in Table 1.
The results of property of 1 iron-silicon-aluminum soft magnet powder core of table
It can be seen that by the above results, the iron-silicon-aluminum soft magnet powder core that above-described embodiment 1~6 is prepared is with higher The iron-silicon-aluminum soft magnet powder core that density, higher magnetic conductivity and lower magnetic loss, especially embodiment 4 are prepared, has Extra high magnetic conductivity and very low magnetic loss.
Embodiment 8
In preparation method of the present invention, the mass ratio of zinc stearate and polyethylene glycol is soft to gained iron sial in lubricant The performance of magnetic powder core influences test
The present embodiment test sets 9 groups altogether, and in every group of lubricant, the mass ratio of zinc stearate and polyethylene glycol is shown in Table 2 institutes Show.
The mass ratio of table 2 zinc stearate and polyethylene glycol
Group Zinc stearate: polyethylene glycol
Test group 1 0.02:1
Test group 2 0.1:1
Test group 3 1:5
Test group 4 2:3
Test group 5 1:1
Test group 6 3:2
Test group 7 3:1
Test group 8 4:1
Test group 9 5:1
In the present embodiment, test group 1~9 is all made of the method for the invention and prepares iron-silicon-aluminum soft magnet powder core, test group 1 In~9, in addition to the mass ratio difference of zinc stearate, polyethylene glycol in lubricant, remaining condition is all the same.
The density of the iron-silicon-aluminum soft magnet powder core that testing experiment group 1~9 is prepared respectively, magnetic conductivity (when 50kHz and When 1000kHz), magnetic loss (50kHz/0.05T), test result is shown in Table 3.
The performance test results of 3 iron-silicon-aluminum soft magnet powder core of table
It can be seen that by 3 result of table, in the preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, stearic acid in lubricant The mass ratio of zinc and polyethylene glycol has direct influence to the density of gained soft-magnetic powder core, magnetic conductivity and magnetic loss.When described In lubricant, the mass ratio of zinc stearate and polyethylene glycol is (3~1): when 2, gained iron-silicon-aluminum soft magnet powder core has higher Density, higher magnetic conductivity and lower magnetic loss.Especially in the lubricant, the matter of zinc stearate and polyethylene glycol When amount is than being 2:3, gained iron-silicon-aluminum soft magnet powder core has higher density, higher magnetic conductivity and lower magnetic loss.
Embodiment 9
In preparation method of the present invention, the content of lubricant influences test to the performance of gained iron-silicon-aluminum soft magnet powder core
The present embodiment test sets 7 groups altogether, and in every group of lubricant, the mass ratio of zinc stearate and polyethylene glycol is 2:3. In the present embodiment, test group 1~7 is all made of the method for the invention and prepares iron-silicon-aluminum soft magnet powder core, in test group 1~7, removes Lubricant is different from the mass ratio of initial soft-magnetic alloy powder outer, remaining condition is all the same.Lubricant and initial soft magnetism in every group The mass ratio of alloy powder is shown in Table 4.
The mass ratio of table 4 lubricant and initial soft-magnetic alloy powder
Group Lubricant: initial soft-magnetic alloy powder
Test group 1 0.4%
Test group 2 0.6%
Test group 3 0.8%
Test group 4 1%
Test group 5 1.3%
Test group 6 1.6%
Test group 7 2%
The density of the soft-magnetic powder core that testing experiment group 1~7 is prepared respectively, magnetic conductivity are (when 50kHz and 1000kHz When), magnetic loss (50kHz/0.05T), test result is shown in Table 5
The performance test results of 5 soft-magnetic powder core of table
It can be seen that by 5 result of table, in the preparation method of soft-magnetic powder core of the present invention, the dosage of lubricant is also to soft magnetism Density, magnetic conductivity and the magnetic loss of powder core have direct influence.When the quality of the lubricant and initial soft-magnetic alloy powder When than being 0.5~1.5%, gained soft-magnetic powder core density with higher, magnetic conductivity and lower magnetic loss.Especially work as institute When the mass ratio for stating lubricant and initial soft-magnetic alloy powder is 1.3%, gained soft-magnetic powder core has higher density, magnetic conductance Rate and lower magnetic loss.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention And range.

Claims (9)

1. a kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core, which comprises the following steps:
(1) processing is passivated to initial soft-magnetic alloy powder using passivator, it is dry;
(2) soft-magnetic alloy powder of step (1) after dry is uniformly mixed with binder;
(3) the mixed-powder drying and screening for obtaining step (2) then adds insulating compound mixing cladding;
(4) soft-magnetic alloy powder and mix lubricant that will have been coated in step (3), and be packed into mold, then in pressurization It is heated simultaneously, temperature and pressure compression moulding;
(5) powder core of temperature and pressure compression moulding in step (4) is made annealing treatment;
The weight percentage of the initial soft-magnetic alloy powder are as follows: silicon 8.5~10.5%, aluminium 4.5~6.5%, surplus are iron;
Lubricant in the step (4) is the mixture of zinc stearate and polyethylene glycol;The matter of zinc stearate and polyethylene glycol Amount is than being (0.02~5): 1;
The mass ratio of lubricant and initial soft-magnetic alloy powder is 0.5~1.5% in the step (4);
The passivator used in the step (1) is phosphoric acid solution;
Binder in the step (2) is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin;
Insulating compound in the step (3) is nano silica;
The pressing pressure of temperature and pressure compression moulding is 500~1200MPa in the step (4), and press temperature is 60~150 DEG C;Institute Stating the annealing temperature made annealing treatment in step (5) is 550~750 DEG C, and annealing time is 0.5~1.5 hour.
2. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (4) Lubricant in, the mass ratio of zinc stearate and polyethylene glycol is (3~1): 2.
3. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (4) Lubricant in, the mass ratio of zinc stearate and polyethylene glycol is 2:3.
4. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (2) Binder in, the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is (4~1): 2.
5. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (2) Binder in, the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is 3:2.
6. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (2) In binder and initial soft-magnetic alloy powder mass ratio be 1~2%.
7. the method that temperature and pressure as claimed in claim 6 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the step (2) In binder and initial soft-magnetic alloy powder mass ratio be 1.5%;Insulating compound and initial magnetically soft alloy in the step (3) The mass ratio of powder is 0.1~0.4%.
8. the method that temperature and pressure as described in claim 1 prepare iron-silicon-aluminum soft magnet powder core, which is characterized in that the phosphoric acid solution Mass percentage concentration be 0.4~3%, the mass ratio of the phosphoric acid solution and initial soft-magnetic alloy powder is (0.5~1.5): 1。
9. a kind of iron-silicon-aluminum soft magnet powder core being prepared using such as any the method for claim 1~8.
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