CN105344993A - Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing - Google Patents
Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 67
- -1 iron-silicon-aluminum Chemical compound 0.000 title claims abstract description 60
- 238000003825 pressing Methods 0.000 title claims abstract description 19
- 239000006247 magnetic powder Substances 0.000 title abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 181
- 229910001004 magnetic alloy Inorganic materials 0.000 claims abstract description 85
- 239000000314 lubricant Substances 0.000 claims abstract description 63
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims abstract description 35
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 34
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 34
- 239000000203 mixture Substances 0.000 claims abstract description 32
- 238000000137 annealing Methods 0.000 claims abstract description 30
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 46
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 23
- 239000004115 Sodium Silicate Substances 0.000 claims description 20
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 20
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 19
- 239000005543 nano-size silicon particle Substances 0.000 claims description 14
- 238000002161 passivation Methods 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 9
- 238000012216 screening Methods 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 5
- 230000005291 magnetic effect Effects 0.000 abstract description 60
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- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 239000012212 insulator Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 28
- 238000002360 preparation method Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 6
- 239000000696 magnetic material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
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- 238000005516 engineering process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229910017082 Fe-Si Inorganic materials 0.000 description 2
- 229910017133 Fe—Si Inorganic materials 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000004663 powder metallurgy Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
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- 238000004146 energy storage Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F2003/023—Lubricant mixed with the metal powder
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- Chemical & Material Sciences (AREA)
- 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 invention discloses a method for preparing an iron-silicon-aluminum soft magnetic powder core through warm-pressing. The method comprises the following steps that (1) initial soft magnetic alloy powder is subjected to passivating treatment through a passivator, and drying is conducted; (2) the dried soft magnetic alloy powder is evenly mixed with a binder; (3) the mixed powder is dried and sieved, and then an insulator is added for mixing coating; (4) the coated soft magnetic alloy powder is mixed with lubricant, the mixture is put into a die, then pressurization and heating are conducted simultaneously, and warm-pressing forming is conducted; and (5) the warm-pressing formed magnetic powder core is subjected to annealing treatment. The initial soft magnetic alloy powder comprises, by weight, 8.5%-10.5% of silicon, 4.5%-6.5% of aluminum, and the balance iron. The lubricant in the step (4) is the mixture of zinc stearate and polyethylene glycol. According to the method, the density and the magnetic conductivity of the prepared soft magnetic powder core can be effectively improved, and the magnetic loss is significantly reduced.
Description
Technical field
The present invention relates to the metallurgical manufacture field of metal material powder, the soft-magnetic powder core that especially a kind of preparation method of iron-silicon-aluminum soft magnet powder core and employing the method prepare.
Background technology
Powder core is a kind of by powder metallurgical technique, soft-magnetic alloy powder is mixed with dielectric suppress, there is the novel soft magnetism functional material that magnetoelectricity changes features.Because granularity of magnet powder is very little, and one deck dielectric insulating film in the coated with uniform of ferromagnetic powder particle, improve the resistivity of powder core, hinder the eddy current effect between magnetic, thus eddy-current loss is very low, is suitable for upper frequency application (more than 20kHz).In addition, powder core also has higher saturation induction density, good frequency characteristic, comparatively low-coercivity and the advantage such as permanent magnetic conduction and temperature stability, make powder core as inductance filter, hold back streamline circle and be widely used in the fields such as telecommunications, radar, power switch, become the part that soft magnetic materials is important.
Fe-Si-Al magnetic core composition is Fe-(8 ~ 13%) Si-(4 ~ 7%) Al, is a kind of novel soft magnetic materials possessing magnetoelectricity translation function.The soft magnet performance superior because of it and suitable price, be widely used in pulse transformer, return in the electronic device of transformer, line noise wave filter, energy storage inductor etc.Current Fe-Si-Al magnetic core is in large-scale application and further development phase.
In general, pressure is larger, and the density of pressed compact is higher, and the magnetic conductivity of magnetic is larger.But increase pressure, has the limit to the raising of powder core density, the excessive insulating barrier that also can cause of pressure breaks, thus reduced insulation effect.
Powder metal warm compaction forming technique is by transforming traditional powder metallurgy press, adopt the heating system of the heating of special powder, powder conveying and mould, by being mixed with the special lubricant of temperature and pressure, the mixed-powder of binding agent is heated to a specific temperature and suppresses, traditional handicraft is adopted to sinter again, to obtain higher density and the product of performance.At present, temperature and pressure improve mechanical property mainly for the preparation of structural material, and being applied to development powder magnetic material, to improve the research of soft-magnetic powder core performance also rarely found.In published patent, Jin You Zhejiang University " a kind of warm-pressing formation prepares the method (application number CN201410246527.2) of soft magnetic metal composite " and Guangdong University of Technology " a kind of preparation method (application number CN201410013455.7) of amorphous soft magnet powder core ".Zhu Tao (Zhu Tao. powder warm compactingprocess compounded lubricant and the application study [D] in preparation Fe-Si soft magnetic materials thereof. Hefei: Hefei Polytechnics, 2012) have studied temperature and pressure and be applied to the effect of Fe-Si magnetically soft alloy to its institutional framework and mechanical property, adopt the mixture of amine based polymer, stearate and ethylene glycol polymer as temperature and pressure lubricant.The people such as H.Shokrollahi (H.Shokrollahi.etal..JournalofMagnetismandMagneticMateria ls.2007,313:182-186) to have studied under room temperature pressing parameter to the impact of straight iron powder for main soft-magnetic composite material powder core magnetic property, it is with lubricator zinc stearate, result shows, along with the increase of pressing pressure, the density of powder core increases to some extent, magnetic conductivity and magnetic induction intensity improve, but the defects such as the dislocation of pressure increase introducing simultaneously and internal stress also increase, and thus coercivity also increases to some extent.
Soft magnetic materials is widely applied in field of power electronics, and the application product of current alloy is mostly coiled into the process of magnetic core after annealing with cold quenching thin coiled stock.But the loss characteristic of high band limits strip core application scenario, and strip fragility after Overheating Treatment is large, in industrial circle, in most cases needs to make with this kind of material the special shape meeting various needs.Under the prerequisite not damaging excellent this advantage of soft magnet performance of this material, the loss value of magnetic core should be reduced significantly, alloy strip steel rolled stock is broken into magnetic, be pressed into powder core and just can realize this purpose.Current employing temperature and pressure are prepared FeSiAl soft-magnetic powder core and be have not been reported.
Summary of the invention
The object of the invention is to provide a kind of method adopting temperature-pressure formation to prepare soft-magnetic powder core based on above-mentioned background; Meanwhile, present invention also offers the soft-magnetic powder core adopting described method to prepare, described soft-magnetic powder core has higher magnetic conductivity and lower magnetic loss.
For achieving the above object, the technical scheme that the present invention takes is: a kind of temperature and pressure prepare the method for iron-silicon-aluminum soft magnet powder core, comprise the following steps:
(1) passivator is utilized to carry out Passivation Treatment to initial soft-magnetic alloy powder, dry;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing;
(3) by the mixed-powder drying and screening that step (2) obtains, insulating compound mixing is then added coated;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then heat while pressurization, temperature and pressure are compressing;
(5) annealing in process is carried out to the powder core that temperature and pressure in step (4) are compressing;
The weight percentage of described initial soft-magnetic alloy powder is: silicon 8.5 ~ 10.5%, aluminium 4.5 ~ 6.5%, surplus are iron;
Lubricant in described 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, adopt special lubricant temperature and pressure, greatly can improve the soft magnet performance such as magnetic conductivity, magnetic loss preparing gained powder core, improve the cost performance of soft-magnetic powder core further, be expected to obtain 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, the weight percentage of described initial soft-magnetic alloy powder is: silicon 9.9%, aluminium 5.5%, surplus are iron, when adopting the initial soft-magnetic alloy powder of this composition, what prepare is FeSiAl soft-magnetic powder core, and it has higher magnetic conductivity and higher cost performance.Soft-magnetic alloy powder of the present invention can adopt prior art means to obtain, can directly from market purchase etc.In the present invention, soft-magnetic alloy powder preferably but be not limited to the soft-magnetic alloy powder of composition described above, and the soft-magnetic alloy powder of mentioned component obtains wide material sources, and has higher cost performance.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (0.02 ~ 5): 1.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (3 ~ 1): 2.Prepare the most preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is 2:3.Temperature and pressure of the present invention prepare the method for iron-silicon-aluminum soft magnet powder core, adopt special lubricant, and namely described lubricant is made up of two kinds of materials, is respectively zinc stearate and polyethylene glycol, and the mass ratio of the two is (0.02 ~ 5): 1.Present inventor finds through large quantity research, and when described lubricant adopts zinc stearate and the polyethylene glycol of described specific proportioning, the iron-silicon-aluminum soft magnet powder core adopting the method for the invention to prepare has higher magnetic conductivity and very low magnetic loss.Especially, when in described lubricant, when the mass ratio of zinc stearate and polyethylene glycol is 2:3, the iron-silicon-aluminum soft magnet powder core obtained has the highest magnetic conductivity and minimum magnetic loss.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in described step (4), the mass ratio of lubricant and initial soft-magnetic alloy powder is 0.4 ~ 2%.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in described step (4), the mass ratio of lubricant and initial soft-magnetic alloy powder is 0.5 ~ 1.5%.Present inventor finds through research, in the application, the performance of gained soft-magnetic powder core is not only relevant with the ratio of zinc stearate in described lubricant and polyethylene glycol, but also it is relevant with the addition of lubricant, present inventor finds through overtesting, when the mass ratio of described lubricant and initial soft-magnetic alloy powder is 0.4 ~ 2%, gained soft-magnetic powder core has higher density, magnetic conductivity and lower magnetic loss; Especially, when the mass ratio of described lubricant and initial soft-magnetic powder core is 0.5 ~ 1.5%, gained soft-magnetic powder core has better density, magnetic conductivity and lower magnetic loss.
Prepare the preferred embodiment of the method for soft-magnetic powder core described in iron sial as temperature and pressure of the present invention, the binding agent in described step (2) is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin; Insulating compound in described step (3) is nano silicon.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in the binding agent of described step (2), the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is (4 ~ 1): 2.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in the binding agent of described step (2), the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is 3:2.In the preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, described binding agent adopts specific two kinds of materials composition, i.e. sodium metasilicate and high-temperature resistant silicone acid resin, and the mass ratio of the two is (4 ~ 1): 2, present inventor finds through large quantity research, when described binding agent adopts sodium metasilicate and the high-temperature resistant organic silicon resin composition of specific proportioning, coordinate lubricant and the process conditions of described specific proportioning, the iron-silicon-aluminum soft magnet powder core of higher magnetic permcability and very low magnetic loss can be obtained.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, the binding agent in described step (2) and the mass ratio of initial soft-magnetic alloy powder are 1 ~ 2%; In described step (3), the mass ratio of insulating compound and initial soft-magnetic alloy powder is 0 ~ 0.4%.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, the binding agent in described step (2) and the mass ratio of initial soft-magnetic alloy powder are 1.5%; In described step (3), the mass ratio of insulating compound and initial soft-magnetic alloy powder is 0.1 ~ 0.4%.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in described step (3), the mass ratio of insulating compound and initial soft-magnetic alloy powder is 0.2%.
The preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core is prepared as temperature and pressure of the present invention, the passivator adopted in described step (1) is phosphoric acid solution, the mass percentage concentration of described phosphoric acid solution is 0.4 ~ 3% (all the other are water), and the mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is (0.5 ~ 1.5): 1.When phosphoric acid solution passivator concentration is very low, in the very thin thickness of the phosphating coat that powder particle surface generates, passivation effect is not too complete.Along with the increase of passivator concentration and the intensification of degree of passivation, powder particle surface can generate phosphating coat that is complete, uniform fold.But during phosphoric acid solution passivator excessive concentration, phosphating coat thickness is excessive easily to be caused again its cracking and comes off.Prepare the more preferably embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, the passivator adopted in described step (1) is phosphoric acid solution, and the mass percentage concentration of described phosphoric acid solution is 0.7%.When the mass percentage concentration of described phosphoric acid solution passivator is 0.7%, best film-forming state can be reached.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, the pressing pressure that in described step (4), temperature and pressure are compressing is 500 ~ 1200MPa, 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, mould easily damages.When press temperature is too low, kollag not yet melts and causes temperature and pressure density to improve DeGrain; When temperature and pressure temperature is too high, lubricating film viscosity reduces, and causes between powder particle and directly contacts, cause density to decline on the contrary, and internal stress is high, be unfavorable for improving soft magnet performance.The preparation method of soft-magnetic powder core of the present invention, in described temperature and pressure pressing process, pressing pressure described in employing and press temperature, higher density can be obtained with less pressing pressure at temperature and pressure temperature, and the powder core internal stress of gained is low, is conducive to obtaining higher magnetic conductivity and lower loss, can pressing pressure be reduced in addition, less mould loss, economic benefits are remarkable.
Prepare the preferred embodiment of the method for iron-silicon-aluminum soft magnet powder core as temperature and pressure of the present invention, in described step (5), the annealing temperature of annealing in process is 550 ~ 750 DEG C, and annealing time is 0.5 ~ 1.5 hour.Annealing temperature is lower, the time is shorter, then eliminate internal stress DeGrain, be unfavorable for improving magnetic property; Annealing temperature is too high, then powder core is easy to oxidation deterioration, expends the energy, but also insulating barrier between powder particle may be caused to destroy, and worsens 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, and for realizing this object, the technical scheme that the present invention takes is: a kind of iron-silicon-aluminum soft magnet powder core, and it adopts method described above to prepare.
The preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, by the preparation of powder metallurgy warm-pressing New technical use in amorphous soft magnet powder core, groped by lot of experiments, the combination of the described specific lubricant of final selection and other reinforced selections and charging sequence, pressing pressure, press temperature etc., these overall method and technology schemes combining composition, the amorphous soft magnet powder core prepared has higher density and lower internal stress, and gained powder core has higher magnetic conductivity and very low magnetic loss.The preparation method of soft-magnetic powder core of the present invention, compared with existing soft-magnetic powder core technology of preparing, the inventive method can obtain higher density with less pressing pressure at temperature and pressure temperature, and powder core internal stress is low, thus be conducive to magnetic domain wall moving and domain rotation, the magnetic conductivity that favourable acquisition is higher and lower loss.And method of the present invention can reduce pressing pressure, reduce mould loss, there are more significant economic benefits.
Detailed description of the invention
For better the object, technical solutions and advantages of the present invention being described, below in conjunction with specific embodiment, the invention will be further described.
In following examples, the weight percentage of described initial soft-magnetic alloy powder is: silicon 8.5 ~ 10.5%, aluminium 4.5 ~ 6.5%, surplus are iron.More preferably, in following examples, the weight percentage of described initial soft-magnetic alloy powder is: 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 0.4% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 0.5:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 2%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 2:1;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.1%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 500MPa, temperature be 150 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 1%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 0.02:1;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 550 DEG C, and annealing time is 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 1% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 0.6:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 1.8%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 3:2;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.15%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 800MPa, temperature be 90 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 2%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 0.4:1;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 600 DEG C, and annealing time is 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 2% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 0.8:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 1.6%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 3:2;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.2%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 600MPa, temperature be 120 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 0.5%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 1:2;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 630 DEG C, and annealing time is 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 0.7% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 1:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 1.5%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 3:2;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.2%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 1100MPa, temperature be 100 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 1.3%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 2:3;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 680 DEG C, and annealing time is 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 3% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 1.2:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 1.2%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 2:3;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.3%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 1000MPa, temperature be 80 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 1.5%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 3:2;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 700 DEG C, and annealing time is 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, and described in the present embodiment, the preparation method of soft-magnetic powder core comprises the following steps:
(1) utilize mass percentage concentration be 1.5% phosphoric acid solution Passivation Treatment is carried out to initial soft-magnetic alloy powder, dry; The mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is 1.5:1;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing, the mass ratio of described binding agent and initial soft-magnetic alloy powder is 1%, described binding agent is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin, and the mass ratio of described sodium metasilicate, high-temperature resistant organic silicon resin is 1:2;
(3) by the mixed-powder drying and screening that step (2) obtains, then add nano silicon mixing coated, the mass ratio of described nano silicon and initial soft-magnetic alloy powder is 0.4%;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then pressurization while heat, pressure be 1200MPa, temperature be 60 DEG C at temperature and pressure compressing; The mass ratio of described lubricant and initial soft-magnetic alloy powder is 0.4%, and described lubricant is the mixture of zinc stearate and polyethylene glycol, and the mass ratio of described zinc stearate and polyethylene glycol is 5:1;
(5) carry out annealing in process to the powder core that temperature and pressure in step (4) are compressing, annealing temperature is 750 DEG C, and annealing time is 1.5h.
Embodiment 7
The performance test of the iron-silicon-aluminum soft magnet powder core that the method for the invention prepares
Respectively the performance of the iron-silicon-aluminum soft magnet powder core that embodiment 1 ~ 6 prepares is tested, test density, magnetic conductivity when 1000kHz (during 50kHz and), the magnetic loss (50kHz/0.05T) of often organizing gained iron-silicon-aluminum soft magnet powder core respectively, test result is in table 1.
The results of property of table 1 iron-silicon-aluminum soft magnet powder core
Can be found out by the above results, the iron-silicon-aluminum soft magnet powder core that above-described embodiment 1 ~ 6 prepares, have higher density, higher magnetic conductivity and lower magnetic loss, especially the iron-silicon-aluminum soft magnet powder core for preparing of embodiment 4, has extra high magnetic conductivity and very low magnetic loss.
Embodiment 8
In preparation method of the present invention, in lubricant, the mass ratio of zinc stearate and polyethylene glycol is tested the performance impact of gained iron-silicon-aluminum soft magnet powder core
The present embodiment test establishes 9 groups altogether, and in the lubricant often organized, the mass ratio of zinc stearate and polyethylene glycol is shown in Table 2.
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 all adopts the method for the invention to prepare iron-silicon-aluminum soft magnet powder core, and in test group 1 ~ 9, except the mass ratio difference of zinc stearate, polyethylene glycol in lubricant, all the other conditions are all identical.
The density of the iron-silicon-aluminum soft magnet powder core for preparing of testing experiment group 1 ~ 9, magnetic conductivity when 1000kHz (during 50kHz and), magnetic loss (50kHz/0.05T) respectively, test result is shown in Table 3.
The performance test results of table 3 iron-silicon-aluminum soft magnet powder core
Can be found out by table 3 result, in the preparation method of iron-silicon-aluminum soft magnet powder core of the present invention, in lubricant, the mass ratio of zinc stearate and polyethylene glycol has direct impact to the density of gained soft-magnetic powder core, magnetic conductivity and magnetic loss.When in described lubricant, the mass ratio of zinc stearate and polyethylene glycol is (3 ~ 1): when 2, and gained iron-silicon-aluminum soft magnet powder core has higher density, higher magnetic conductivity and lower magnetic loss.Especially, when in described lubricant, when the mass ratio of zinc stearate and polyethylene glycol is 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 is tested the performance impact of gained iron-silicon-aluminum soft magnet powder core
The present embodiment test establishes 7 groups altogether, and in the lubricant often organized, the mass ratio of zinc stearate and polyethylene glycol is 2:3.In the present embodiment, test group 1 ~ 7 all adopts the method for the invention to prepare iron-silicon-aluminum soft magnet powder core, and in test group 1 ~ 7, except lubricant is different from the mass ratio of initial soft-magnetic alloy powder, all the other conditions are all identical.Often in group, the mass ratio of lubricant and initial soft-magnetic 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 for preparing of testing experiment group 1 ~ 7, magnetic conductivity when 1000kHz (during 50kHz and), magnetic loss (50kHz/0.05T) respectively, test result is shown in Table 5.
The performance test results of table 5 soft-magnetic powder core
Can be found out by table 5 result, in the preparation method of soft-magnetic powder core of the present invention, the consumption of lubricant also has direct impact to the density of soft-magnetic powder core, magnetic conductivity and magnetic loss.When the mass ratio of described lubricant and initial soft-magnetic alloy powder is 0.5 ~ 1.5%, gained soft-magnetic powder core has higher density, magnetic conductivity and lower magnetic loss.Especially, when the mass ratio of described lubricant and initial soft-magnetic alloy powder is 1.3%, gained soft-magnetic powder core has higher density, magnetic conductivity and lower magnetic loss.
Finally to should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention but not limiting the scope of the invention; although be explained in detail the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. temperature and pressure prepare a method for iron-silicon-aluminum soft magnet powder core, it is characterized in that, comprise the following steps:
(1) passivator is utilized to carry out Passivation Treatment to initial soft-magnetic alloy powder, dry;
(2) by step (1) dried soft-magnetic alloy powder and binding agent Homogeneous phase mixing;
(3) by the mixed-powder drying and screening that step (2) obtains, insulating compound mixing is then added coated;
(4) by good soft-magnetic alloy powder coated in step (3) and mix lubricant, and load in mould, then heat while pressurization, temperature and pressure are compressing;
(5) annealing in process is carried out to the powder core that temperature and pressure in step (4) are compressing;
The weight percentage of described initial soft-magnetic alloy powder is: silicon 8.5 ~ 10.5%, aluminium 4.5 ~ 6.5%, surplus are iron;
Lubricant in described step (4) is the mixture of zinc stearate and polyethylene glycol.
2. temperature and pressure as claimed in claim 1 prepare the method for iron-silicon-aluminum soft magnet powder core, and it is characterized in that, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (0.02 ~ 5): 1; Preferably, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is (3 ~ 1): 2; More preferably, in the lubricant of described step (4), the mass ratio of zinc stearate and polyethylene glycol is 2:3.
3. temperature and pressure as claimed in claim 1 or 2 prepare the method for iron-silicon-aluminum soft magnet powder core, it is characterized in that, in described step (4), the mass ratio of lubricant and initial soft-magnetic alloy powder is 0.4 ~ 2%; Preferably, in described step (4), the mass ratio of lubricant and initial soft-magnetic alloy powder is 0.5 ~ 1.5%.
4. temperature and pressure as claimed in claim 1 prepare the method for iron-silicon-aluminum soft magnet powder core, and it is characterized in that, the binding agent in described step (2) is the mixture of sodium metasilicate, high-temperature resistant organic silicon resin; Insulating compound in described step (3) is nano silicon.
5. temperature and pressure as claimed in claim 4 prepare the method for iron-silicon-aluminum soft magnet powder core, and it is characterized in that, in the binding agent of described step (2), the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is (4 ~ 1): 2; Preferably, in the binding agent of described step (2), the mass ratio of sodium metasilicate and high-temperature resistant organic silicon resin is 3:2.
6. temperature and pressure as claimed in claim 1 prepare the method for iron-silicon-aluminum soft magnet powder core, and it is characterized in that, the binding agent in described step (2) and the mass ratio of initial soft-magnetic alloy powder are 1 ~ 2%; In described step (3), the mass ratio of insulating compound and initial soft-magnetic alloy powder is 0 ~ 0.4%.
7. temperature and pressure as claimed in claim 6 prepare the method for iron-silicon-aluminum soft magnet powder core, and it is characterized in that, the binding agent in described step (2) and the mass ratio of initial soft-magnetic alloy powder are 1.5%; In described step (3), the mass ratio of insulating compound and initial soft-magnetic alloy powder is 0.1 ~ 0.4%.
8. temperature and pressure as claimed in claim 1 prepare the method for iron-silicon-aluminum soft magnet powder core, it is characterized in that, the passivator adopted in described step (1) is phosphoric acid solution, the mass percentage concentration of described phosphoric acid solution is 0.4 ~ 3%, and the mass ratio of described phosphoric acid solution and initial soft-magnetic alloy powder is (0.5 ~ 1.5): 1.
9. temperature and pressure as claimed in claim 1 prepare the method for iron-silicon-aluminum soft magnet powder core, it is characterized in that, the pressing pressure that in described step (4), temperature and pressure are compressing is 500 ~ 1200MPa, and press temperature is 60 ~ 150 DEG C; In described step (5), the annealing temperature of annealing in process is 550 ~ 750 DEG C, and annealing time is 0.5 ~ 1.5 hour.
10. one kind adopt as arbitrary in claim 1 ~ 9 as described in the iron-silicon-aluminum soft magnet powder core for preparing of method.
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