CN103730225A - Method for preparing amorphous soft magnetic powder core - Google Patents
Method for preparing amorphous soft magnetic powder core Download PDFInfo
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- CN103730225A CN103730225A CN201410013455.7A CN201410013455A CN103730225A CN 103730225 A CN103730225 A CN 103730225A CN 201410013455 A CN201410013455 A CN 201410013455A CN 103730225 A CN103730225 A CN 103730225A
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Abstract
The invention discloses a method for preparing an amorphous soft magnetic powder core in a warm-pressing forming mode. The method includes the following steps that (1) amorphous soft magnetic alloy powder is passivated and dried through passivator; (2) the dried amorphous soft magnetic alloy powder in the step (1) is evenly mixed with mica, high-temperature resistance organic silicon resin and acetone; (3) after solvent evaporation, the coated amorphous soft magnetic alloy powder in the step (2) and a lubricating agent are mixed and are filled into a mold, so that warm-pressing forming is conducted, and heating is performed while pressurization is conducted; (4) annealing treatment is carried out on the magnetic powder core which is formed in the step (3) in a pressing mode. By the adoption of the method, high density can be obtained through small pressing pressure at a warm-pressing temperature, the internal stress of the magnetic powder core is low, and high magnetic conductivity and low loss can be better obtained; in addition, the pressing pressure can be lowered, mold loss is reduced, and the economic effect is quite obvious.
Description
Technical field
The invention belongs to the metallurgical manufacture of metal material powder field, be specifically related to the preparation method of the Fe-based amorphous soft-magnetic powder core of a kind of warm-pressing formation.
Background technology
Amorphous soft magnetic material is a kind of novel magnetic material, has surmounted the category of traditional crystalline state soft magnetic material.When super condensation is solid, atom has little time ordered arrangement crystallization, obtain the combination of solid alloy atomic arrangement and there is shortrange order, the unordered feature of long-range, there is no crystal grain, the crystal boundary of crystal alloy, there is the different characteristic of property of traditional material, as excellent soft magnet performance, high corrosion resistance, well mechanical property, high resistance to wear, intensity, toughness, hardness, high resistivity etc.
Powder core is a kind of by powder metallurgical technique, soft-magnetic alloy powder is mixed to novel soft magnetism functional material that compacting forms, that have magnetoelectricity conversion features with dielectric.Because granularity of magnet powder is very little, and in the coated with uniform of ferromagnetic powder particle, one deck dielectric insulating film, improved the resistivity of powder core, hindered the eddy current effect between magnetic, thereby eddy current loss is very low, be suitable for upper frequency application (more than 20kHz).In addition, powder core also has higher saturation induction density, good frequency characteristic, compared with low-coercivity, with advantages such as permanent magnetic conduction and temperature stabilities, make powder core as inductance filter, hold back streamline circle and be widely used in the fields such as telecommunications, radar, mains switch, become the important part of soft magnetic material.
(the Wang Hongxia such as Wang Hongxia, Deng. Metallic Functional Materials, 2010,17 (2): 8-12) at research amorphous powder passivation technology, find during on the affecting of its powder core performance, be compared to and all do not improve a lot with processing characteristics and the magnetic property of the powder core of passivator, and comparing three kinds of passivator chromic anhydrides, potassium permanganate and Phosphating Solutions, Phosphating Solution is the most superior.Die forming is the powder core that the magnetic having insulated is pressed into various shapes.Because powder core is without high-temperature sintering process, therefore compacting process just seems particularly important.In general, pressure is larger, and the density of pressed compact is higher, and the magnetic permeability of magnetic is larger.But increase pressure, has the limit to the raising of this magnetic core density, the excessive insulating barrier that also can cause of pressure breaks, thus reduced insulation effect.(ten thousand is beautiful for Wan Juan etc., Deng. electronic component and material .2012,31(10): 45-48) in the at room temperature preparation of ferrocart core and Fe-based amorphous powder core and soft magnet performance research process, pressure at 200MPa to 600MPa is suppressed, carry out subsequently the test of dynamic magnetic performance, found that: along with the increase of pressure, the magnetic conductance of powder core takes the lead in increasing rear minimizing, when 400MPa, reach maximum 26, magnetic loss first reduces rear increase along with the increase of pressure, reaches minimum value 11.1W/kg (50kHz) when 400MPa.
Powder metal warm compaction forming technique is by transforming traditional powder metallurgy press, adopt the heating system of special powder heating, powder conveying and mould, the mixed-powder that is mixed with the special lubricant of temperature and pressure, binding agent is heated to a specific temperature (general 130-150 ℃) to be suppressed, adopt again traditional handicraft to carry out sintering, to obtain the product of higher density and 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 magnetic property also rarely found." temperature pressure binding permanent magnet material and preparation method thereof " (Shanghai University of Jin You Shanghai University aspect existing patent, Chinese Patent Application No. CN200610025232.8, open day 2006.8.23), and consider theoretically, temperature and pressure will be than more remarkable for permanent magnetic material for the superiority of soft magnetic material.Zhu Tao (Zhu Tao. powder warm compactingprocess compounded lubricant and the application study [D] in preparation Fe-Si soft magnetic material thereof. Hefei: Hefei Polytechnics, 2012) study temperature and pressure and be applied to the effect of Fe-Si magnetically soft alloy to its institutional framework and mechanical property, and this alloy does not belong to non-crystaline amorphous metal, in theory, will there be the feature of himself the effect aspect of the soft magnet performance of temperature and pressure to non-crystaline amorphous metal.The people such as H.Shokrollahi (Shokrollahi.et al..J.Magn.Magn.Mater., 2007,313:182-186) studied and under room temperature, suppressed the impact of parameter on soft-magnetic composite material (not being non-crystaline amorphous metal) magnetic property, result shows, along with the increase of pressing pressure, the density of powder core increases to some extent, and magnetic permeability and magnetic flux density improve, but the defects such as the dislocation that pressure increase is simultaneously introduced and internal stress also increase, thereby coercive force also increases to some extent.
Amorphous soft magnetic material is widely applied in field of power electronics, and the application product of non-crystaline amorphous metal is mostly coiled into the processing of magnetic core after annealing with cold quenching thin coiled stock at present.But the loss characteristic of high band has limited thin coiled stock core application scenario, and the amorphous thin ribbon fragility after Overheating Treatment is large, in industrial circle, in most cases needs to make with this kind of material the special shape of dealing with various requirements.Do not damaging under the prerequisite of excellent this advantage of soft magnet performance of this material, should reduce significantly the loss value of magnetic core, amorphous alloy strips is being broken into magnetic, be pressed into powder core and just can realize this purpose.Therefore amorphous powder core research is nearest study hotspot.Adopt at present temperature and pressure to prepare amorphous soft magnet powder core and there is not yet report.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part and a kind of new method that adopts warm-pressing formation to prepare amorphous soft magnet powder core is provided.
For achieving the above object, the technical scheme that the present invention takes is: a kind of preparation method of amorphous soft magnet powder core, said method comprising the steps of:
(1) utilize passivator to carry out Passivation Treatment to amorphous soft-magnetic alloy powder, dry;
(2) the dried amorphous soft-magnetic alloy powder of step (1) is evenly mixed with mica, high-temperature resistant organic silicon resin, acetone;
(3), after solvent evaporates, by the amorphous soft-magnetic alloy powder and the mix lubricant that have been coated in step (2) and to pack in mould temperature and pressure into compressing, in pressurization, heat;
(4) powder core compressing in step (3) is carried out to annealing in process.
The present invention adopts temperature and pressure to prepare amorphous soft magnet powder core first, can at temperature and pressure temperature, with less pressing pressure, obtain higher density, and the powder core internal stress of gained is low, is conducive to obtain higher magnetic permeability and lower loss; Can reduce in addition pressing pressure, reduce mould loss, economic benefits are more remarkable.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (1), amorphous soft-magnetic alloy powder is amorphous soft-magnetic alloy powders that atomic percentage conc is silicon 8.5～9.5%, boron 9～14%, all the other are iron.Amorphous soft-magnetic alloy powder of the present invention can adopt prior art means to obtain, for example, directly from market, buy (for example, purchased from Beijing Antai Science and Technology Co., Ltd) etc.Preferably but be not limited to adopt the amorphous soft-magnetic alloy powder of described composition, the amorphous soft-magnetic alloy powder of composition described above is the powder of relatively commonly using, and obtains wide material sources, and has higher cost performance in the present invention.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (1), passivator is Phosphating Solution.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (1), the volumetric concentration of Phosphating Solution is 6%.When Phosphating Solution passivator concentration is very low, the very thin thickness of the phosphating coat generating at amorphous powder particle surface, passivation effect is not too complete.Along with the increase of passivator concentration and the intensification of degree of passivation, amorphous powder particle surface can generate phosphating coat complete, uniform fold.But during Phosphating Solution passivator excessive concentration, phosphating coat thickness is excessive easily to be caused again its cracking and comes off.During volumetric concentration 6%, can reach best one-tenth membrane stage.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (3), lubricant is zinc stearate.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (3), pressing pressure is 500～1200MPa.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.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (3), press temperature is 60～150 ℃.When press temperature is too low kollag not yet melting cause temperature and pressure density improve DeGrain; During temperature and pressure excess Temperature, lubricating film reduced viscosity causes between powder particle directly contact, causes density to decline on the contrary, and internal stress is high is unfavorable for improving soft magnet performance.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (4), annealing temperature is 350 ℃, and annealing time is 1h.Annealing temperature is lower, the shorter internal stress DeGrain of eliminating of time, is unfavorable for improving magnetic property; The too high powder of annealing temperature core is easy to oxidation deterioration, expends the energy, but also may cause noncrystal crystallization, worsens magnetic property.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (1), the ratio of the volume of passivator and the molal quantity of amorphous soft-magnetic alloy powder is 25:16L/mol.
As the preparation method's of amorphous soft magnet powder core of the present invention preferred implementation, in described step (2), the ratio of the quality of mica and the molal quantity of amorphous soft-magnetic alloy powder is 15:4g/mol, the quality of high-temperature resistant organic silicon resin is 25:8g/mol with the ratio of the molal quantity of amorphous soft-magnetic alloy powder, and the volume of acetone is 75:32L/mol with the ratio of the molal quantity of amorphous soft-magnetic alloy powder.
Mica, high-temperature resistant organic silicon resin and acetone in the method for the invention all can directly be purchased from market.
The preparation method of amorphous soft magnet powder core of the present invention, compared with existing amorphous soft magnet 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, be conducive to obtain higher magnetic permeability and lower loss; Can reduce in addition pressing pressure, reduce mould loss, economic benefits are more remarkable.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the amorphous soft magnet powder core prepared of the present invention.
Fig. 2 is the fracture scanning electron microscope (SEM) photograph of the amorphous soft magnet powder core prepared of the present invention.
Fig. 3 is that the loss of the amorphous soft magnet powder core prepared of the present invention is with the curve of frequency change.
Fig. 4 is that the magnetic permeability of the amorphous soft magnet powder core prepared of the present invention is with the curve of frequency change.
Embodiment
For the object, technical solutions and advantages of the present invention are better described, below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
Taking 50ml volumetric concentration and be 6% Phosphating Solution and 0.032mol atomic percentage conc is silicon 8.5%, boron 9%, all the other are the amorphous soft-magnetic alloy powder mixing of iron, then be dried, again by dried amorphous soft-magnetic alloy powder and 0.12g mica, 0.1g high-temperature resistant organic silicon resin, 75ml acetone evenly mixes, after the dry 60min volatilization of vacuum drying chamber that is positioned over 120 ℃ until solvent, by the amorphous soft-magnetic alloy powder being coated and mix lubricant and pack temperature and pressure in mould into and be pressed into the powder core that is of a size of external diameter 16mm × internal diameter 9mm × high 5mm annular, in pressurization, heat, pressing pressure is 500MPa, press temperature is 60 ℃, finally 350 ℃ of annealing 1 hour.
Embodiment 2
Taking 50ml volumetric concentration and be 6% Phosphating Solution and 0.032mol atomic percentage conc is silicon 9%, boron 11%, all the other are the amorphous soft-magnetic alloy powder mixing of iron, then be dried, again by dried amorphous soft-magnetic alloy powder and 0.12g mica, 0.1g high-temperature resistant organic silicon resin, 75ml solvent acetone is evenly mixed, after the dry 60min volatilization of vacuum drying chamber that is positioned over 120 ℃ until solvent, by the amorphous soft-magnetic alloy powder being coated and mix lubricant and pack temperature and pressure in mould into and be pressed into the powder core that is of a size of external diameter 16mm × internal diameter 9mm × high 5mm annular, in pressurization, heat, pressing pressure is 800MPa, 90 ℃ of press temperatures, finally 350 ℃ of annealing 1 hour.
Embodiment 3
Taking 50ml volumetric concentration and be 6% Phosphating Solution and 0.032mol atomic percentage conc is silicon 9%, boron 13%, all the other are the amorphous soft-magnetic alloy powder mixing of iron, then be dried, again by dried amorphous soft-magnetic alloy powder and 0.12g mica, 0.1g high-temperature resistant organic silicon resin, 75ml solvent acetone is evenly mixed, after the dry 60min volatilization of vacuum drying chamber that is positioned over 120 ℃ until solvent, by the amorphous soft-magnetic alloy powder being coated and mix lubricant and pack temperature and pressure in mould into and be pressed into the powder core that is of a size of external diameter 16mm × internal diameter 9mm × high 5mm annular, in pressurization, heat, pressing pressure is 800MPa, press temperature is 120 ℃, finally 350 ℃ of annealing 1 hour.
Embodiment 4
Taking 50ml volumetric concentration and be 6% Phosphating Solution and 0.032mol atomic percentage conc is silicon 9.5%, boron 13.5%, all the other are the amorphous soft-magnetic alloy powder mixing of iron, then be dried, again by dried amorphous soft-magnetic alloy powder and 0.12g mica, 0.1g high-temperature resistant organic silicon resin, 75ml solvent acetone is evenly mixed, after the dry 60min volatilization of vacuum drying chamber that is positioned over 120 ℃ until solvent, by the amorphous soft-magnetic alloy powder being coated and mix lubricant and pack temperature and pressure in mould into and be pressed into the powder core that is of a size of external diameter 16mm × internal diameter 9mm × high 5mm annular, in pressurization, heat, pressing pressure is 1200MPa, press temperature is 120 ℃, finally 350 ℃ of annealing 1 hour.
Embodiment 5
Taking 50ml volumetric concentration and be 6% Phosphating Solution and 0.032mol atomic percentage conc is silicon 9.5%, boron 14%, all the other are the amorphous soft-magnetic alloy powder mixing of iron, then be dried, again by dried amorphous soft-magnetic alloy powder and 0.12g mica, 0.1g high-temperature resistant organic silicon resin, 75ml solvent acetone is evenly mixed, after the dry 60min volatilization of vacuum drying chamber that is positioned over 120 ℃ until solvent, by the amorphous soft-magnetic alloy powder being coated and mix lubricant and pack temperature and pressure in mould into and be pressed into the powder core that is of a size of external diameter 16mm × internal diameter 9mm × high 5mm annular, in pressurization, heat, pressing pressure is 1200MPa, press temperature is 150 ℃, finally 350 ℃ of annealing 1 hour.
Embodiment 6
The performance test of the amorphous soft magnet powder core that employing the method for the invention prepares
It is upper that the amorphous soft magnet powder core that the method for the invention is prepared is placed on X-ray diffractometer (be called for short XRD), and directly start is tested, and obtains the XRD spectra of the amorphous soft magnet powder core that the method for the invention prepares, as shown in Figure 1.
By accompanying drawing 1, can be found out the visible wider lower amorphous peak of amorphous soft magnet powder core that the method for the invention prepares, rather than the diffraction maximum of very narrow very high crystal.
The amorphous soft magnet powder core preparing from the method for the invention is got fracture sample, be positioned over scanning electron microscopy (abbreviation ESEM) observation, obtain the fracture scanning electron microscope (SEM) photograph of the amorphous soft magnet powder core that the method for the invention prepares, as shown in Figure 2.By accompanying drawing 2, can find out fracture and the powder particle pattern that amorphous soft magnet powder core that the method for the invention prepares is exaggerated.
Adopt alternating magnetism measuring instrument to measure damage curve corresponding to various frequencies and numerical value, obtain the loss of the amorphous soft magnet powder core that the method for the invention prepares with the curve of frequency change, as shown in Figure 3.
Adopt accurate magnetic component analysis instrument to measure permeability curcve corresponding to various frequencies and numerical value, obtain the magnetic permeability of the amorphous soft magnet powder core that the method for the invention prepares with the curve of frequency change, as shown in Figure 4.
Last institute 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 the present invention is explained in detail with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify or be equal to replacement technical scheme of the present invention, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. a preparation method for amorphous soft magnet powder core, is characterized in that, comprises the following steps:
(1) utilize passivator to carry out Passivation Treatment to amorphous soft-magnetic alloy powder, dry;
(2) the dried amorphous soft-magnetic alloy powder of step (1) is evenly mixed with mica, high-temperature resistant organic silicon resin, acetone;
(3), after solvent evaporates, by the amorphous soft-magnetic alloy powder and the mix lubricant that have been coated in step (2) and to pack in mould temperature and pressure into compressing, in pressurization, heat;
(4) powder core compressing in step (3) is carried out to annealing in process.
2. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (1), amorphous soft-magnetic alloy powder is that atomic percentage conc is silicon 8.5～9.5%, boron 9～14%, all the other amorphous soft-magnetic alloy powders for iron.
3. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (1), passivator is Phosphating Solution.
4. the preparation method of amorphous soft magnet powder core as claimed in claim 3, is characterized in that, in described step (1), the volumetric concentration of Phosphating Solution is 6%.
5. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (3), lubricant is zinc stearate.
6. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (3), pressing pressure is 500～1200MPa.
7. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (3), press temperature is 60～150 ℃.
8. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (4), annealing temperature is 350 ℃, and annealing time is 1h.
9. the preparation method of amorphous soft magnet powder core as claimed in claim 1, is characterized in that, in described step (1), the ratio of the volume of passivator and the molal quantity of amorphous soft-magnetic alloy powder is 25:16L/mol.
10. the preparation method of amorphous soft magnet powder core as claimed in claim 1, it is characterized in that, in described step (2), the ratio of the quality of mica and the molal quantity of amorphous soft-magnetic alloy powder is 15:4g/mol, the quality of high-temperature resistant organic silicon resin is 25:8g/mol with the ratio of the molal quantity of amorphous soft-magnetic alloy powder, and the volume of acetone is 75:32L/mol with the ratio of the molal quantity of amorphous soft magnet magnetic alloy powder.
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| CN104036907A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | Method for preparing soft magnetic metal composite via warm compaction |
| CN104190945A (en) * | 2014-08-12 | 2014-12-10 | 宁波韵升股份有限公司 | Method for preparing amorphous metal soft magnetic powder core |
| CN105344993A (en) * | 2015-12-04 | 2016-02-24 | 广东工业大学 | Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing |
| CN106890999A (en) * | 2015-12-21 | 2017-06-27 | 北京中科三环高技术股份有限公司 | A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core |
| WO2019153310A1 (en) * | 2018-02-11 | 2019-08-15 | 深圳市铂科新材料股份有限公司 | Preparation method for iron-based amorphous-state soft magnet powder core and use thereof |
| CN111009371A (en) * | 2019-12-27 | 2020-04-14 | 浙江工业大学 | Preparation method of soft magnetic composite material based on novel phosphating solution process |
| CN111161934A (en) * | 2019-12-30 | 2020-05-15 | 广东工业大学 | Amorphous nano Fe-Ni magnetic powder core and preparation method and application thereof |
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| CN104036907A (en) * | 2014-06-05 | 2014-09-10 | 浙江大学 | Method for preparing soft magnetic metal composite via warm compaction |
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| CN105344993A (en) * | 2015-12-04 | 2016-02-24 | 广东工业大学 | Method for preparing iron-silicon-aluminum soft magnetic powder core through warm-pressing |
| CN105344993B (en) * | 2015-12-04 | 2018-12-28 | 广东工业大学 | A kind of method that temperature and pressure prepare iron-silicon-aluminum soft magnet powder core |
| CN106890999A (en) * | 2015-12-21 | 2017-06-27 | 北京中科三环高技术股份有限公司 | A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core |
| CN106890999B (en) * | 2015-12-21 | 2019-06-28 | 北京中科三环高技术股份有限公司 | A kind of preparation method of amorphous or nano-crystal soft-magnetic powder core |
| WO2019153310A1 (en) * | 2018-02-11 | 2019-08-15 | 深圳市铂科新材料股份有限公司 | Preparation method for iron-based amorphous-state soft magnet powder core and use thereof |
| CN111009371A (en) * | 2019-12-27 | 2020-04-14 | 浙江工业大学 | Preparation method of soft magnetic composite material based on novel phosphating solution process |
| CN111161934A (en) * | 2019-12-30 | 2020-05-15 | 广东工业大学 | Amorphous nano Fe-Ni magnetic powder core and preparation method and application thereof |
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Application publication date: 20140416 |