CN103745791A - Production method of ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core - Google Patents
Production method of ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core Download PDFInfo
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Abstract
The invention belongs to the technical field of alloy soft magnetic powder cores and particularly relates to a production method of an ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core. The production method comprises step 1, performing mechanical crushing treatment on an iron-based nanocrystalline thin belt so as to obtain iron-based nanocrystalline powder; step 2, screening and matching the iron-based nanocrystalline powder and mixing into mixed powder which is formed by coarse powder and fine powder; step 3, performing passivation, coupling and insulation coating treatment on the mixed powder in turn through a passivation agent, a coupling agent, an insulating agent and a binding agent and performing compression forming; step 4, performing annealing treatment and spraying insulation treatment on the formed magnetic powder core in turn. According to the production method of the ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core, the coarse powder and fine powder mixing and coupling treatment is adopted and accordingly the problem of the compression forming of large particle nanocrystalline powder can be effectively solved and the ultrahigh magnetic permeability of iron-based nanocrystalline magnetic powder core can be produced, wherein the magnetic permeability can reach more than 200.
Description
Technical field
The invention belongs to alloy soft magnetic powder core technical field, specifically, relate to a kind of preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity.
Background technology
The development of electronics industry, the application that various Switching Power Supplies are a large amount of, requirement has high magnetic permeability at frequency 10kHz-200kHz, low-loss, the powder core of good alternating current-direct current stack performance is made the iron core of inductance, the iron core that general sendust is made also claims alloy magnetic powder core, its relative permeability is the highest does not surpass 200, as the manufacture method > > of Chinese invention patent application CN 101090019 A < < high magnetic permeability FeSiAl powder cores, the manufacture method that a kind of magnetic permeability reaches 150 FeSiAl powder core is disclosed.
Amorphous, nano-crystal soft magnetic alloy have excellent soft magnet performance, and its thin coiled stock is applied widely around iron core product.But because eddy current loss under high frequency is large, amorphous, nano-crystal soft magnetic alloy strip Wound core are difficult to use under high frequency.Therefore, adopt powder metallurgical technique, amorphous, nanocrystalline magnetic core under research and development high frequency have been inexorable trend.Powder core is a kind of novel composite electron material, and it is by nanocrystalline strip powder, to be mixed a kind of soft magnetic material that compacting forms with dielectric.Along with the application aspect motor, require nanocrystalline magnetic core to there is the magnetic permeability of superelevation.
The magnetic permeability of the nanocrystalline magnetic core of reporting in prior art is up to 90, as Chinese invention patent application CN 102709015 A announce a kind of preparation method of high performance nano-crystal powder core.It comprises the steps: 1, iron-based amorphous thin ribbon is heat-treated and is transformed into nano-crystalline thin ribbon; 2, be broken into iron based nano crystal powder; 3, ball milling shaping; 4, sieve out by the first powder of-200 sieve meshes with by the second powder constituent mixed-powder of-150～+ 200 sieve meshes; 5, add binding agent to mix, compressing, insulation spraying.Adopt this technical scheme can prepare magnetic permeability at 26～90 nanocrystalline magnetic core.
The mode that adopt to increase particle size is conducive to improve the magnetic permeability of powder core, as Chinese invention patent application CN 103219119 A announce the preparation method of a kind of magnetic permeability Fe-based amorphous powder core that is 90.It comprises the steps: 1, iron-based amorphous thin ribbon is carried out to catalytic thermal processing; 2, be broken into iron-based amorphous powder; 3, sieve out and be less than 100 object powder; 4, through phosphoric acid or nital, carry out passivation insulation processing, after oven dry, add organic binder bond, inorganic binder, lubricant to be coated granulation; 5, the powder core after compressing is put into heat-treatment furnace and under moving air, carried out stress relief annealing, temperature is 300-400 ℃, temperature retention time 0.5-1h.
But there is following defect in this method: the nanocrystalline magnetic core magnetic permeability 1, obtaining is still lower, can not meet the instructions for use of motor; 2, adopt and be less than 100 object manocrystalline powders, because powder particle is larger, the gap between particle is larger, is difficult to compressing.
In the manufacture method > > of the Fe-Si-Al magnetic core of Chinese invention patent CN 100541678C < < magnetic permeability μ=125, adopted-150 ~+400 object meal and-400 object fine powders have been mixed, then through roasting, cooling, compressing and heat treatment obtains the method for Fe-Si-Al magnetic core, the visible method for adopting meal and fine powder to mix, can only be increased to 125 by the powder core of the higher material of this magnetic permeability of iron sial.The soft magnetic-powder core of Chinese invention patent application CN 103151134 A < < silicone resin-ferrite compound coatings and preparation method thereof > > discloses a kind of high temperature resistant silicon ketone resin and nano soft magnetic ferrite powder compound coating iron-based powder particle of utilizing to prepare the report of high-performance magnetic core, wherein the preparation method of soft magnetic-powder core comprises the surface modification of soft magnetic metal particle, couplingization is processed, the preparation of nano soft magnetic ferrite powder, insulating wrapped, moulding and heat treatment step, the effect that adds coupling agent in visible coupling treatment step is to be convenient to silicone resin and nano soft magnetic ferrite powder to be coated to soft magnetic metal particle outside.
In sum, in prior art, also do not have magnetic permeability to reach the report of more than 200 nanocrystalline magnetic core and preparation method thereof; In prior art, yet there is no effectively to solve the report of the compressing problem of bulky grain manocrystalline powders.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity, it adopts the method for meal, fine powder mixing and coupling processing, can effectively solve the compressing problem of bulky grain manocrystalline powders, and make magnetic permeability and reach the more than 200 iron based nano crystal powder cores with superhigh magnetic conductivity.
Technical scheme of the present invention is: a kind of preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity, comprises the steps:
Step 1, carries out mechanical crushing processing to iron-based nano-crystalline thin ribbon, to obtain iron based nano crystal powder;
Step 2, sieves and proportioning described iron based nano crystal powder, the mixed-powder that the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that to be then mixed into by weight content be 40 ~ 80% and weight content are 20 ~ 60% forms;
Step 3, adopts respectively passivator, coupling agent, insulating compound and binding agent to carry out successively passivation, coupling, insulating wrapped processing to described mixed-powder, then compressing;
Step 4, carries out annealing in process and spraying insulation processing successively to the powder core of described moulding.
Optimize, the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that mixed-powder described in step 2 is 50 ~ 65% by weight content and weight content are 35 ~ 50% forms.
Optimize, the composition of described iron based nano crystal powder is Fe
73.5cu
1nb
3si
13.5b
9.
Optimize, described coupling agent adopts titanate esters.
Optimize, described passivator adopts water; Described insulating compound adopts glass powder with low melting point; Described binding agent adopts epoxy resin.
Optimize, described Passivation Treatment step is: mixed-powder is joined in the water of 1-8wt%, stir until dry; Described coupling processing step is: mixed-powder is joined in the coupling agent of 1-10wt%, stir until dry; Described insulating wrapped treatment step is: in the mixed liquor of the epoxy resin of the glass powder with low melting point of the 3-10wt% that mixed-powder is joined and 5-12 wt %, stir until dry.
Optimize, pressure compressing described in step 3 adopts 18 ~ 30t/cm
2.
Optimize, annealing in process described in step 4 is carried out 1～4 hour at 500 ~ 600 ℃.
Optimize, described in step 4, spraying insulation processing employing epoxy resin is inorganic agent.
The weight that the weight percentage of passivator of the present invention, coupling agent, insulating compound and binding agent is each reagent accounts for the percentage composition of the total weight of mixed-powder.
Preparation method provided by the invention has following beneficial effect: 1, adopt the method for meal, fine powder mixing and coupling processing, effectively solved the compressing problem of bulky grain manocrystalline powders; 2, make magnetic permeability and reached the more than 200 iron based nano crystal powder cores with superhigh magnetic conductivity; 3, by adopting suitable passivator, coupling agent, insulating compound and binding agent and consumption thereof, by adopting suitable heat treatment, compressing and annealing in process parameter, can make and form even, seamless, magnetic permeability and reach more than 300 nanocrystalline magnetic cores, can meet the instructions for use of motor; 4, by adopting water, be passivator, can accelerate the passivation of nanocrystal surface, be beneficial to compressing.
Embodiment
Below in conjunction with the preferred embodiment of the present invention, the present invention will be further described.
The iron-based nano-crystalline thin ribbon that embodiments of the invention adopt utilizes single roller utmost point cold process to make, and its composition is Fe
73.5cu
1nb
3si
13.5b
9, thickness is 26～35um, bandwidth is 5-40mm; The powder core specification that embodiments of the invention make adopts Φ 47.2 * 24 * 18(mm).
Embodiment 1
The preparation method of the iron based nano crystal powder core with superhigh magnetic conductivity that the present embodiment provides, comprises the steps:
Step 1, carries out mechanical crushing processing to iron-based nano-crystalline thin ribbon, to obtain iron based nano crystal powder; The composition of described iron-based nano-crystalline thin ribbon is Fe
73.5cu
1nb
3si
13.5b
9;
Step 2, sieves and proportioning described iron based nano crystal powder, the mixed-powder that the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that to be then mixed into by weight content be 40 ~ 80% and weight content are 20 ~ 60% forms;
Step 3, adopts respectively passivator, coupling agent, insulating compound and binding agent to carry out successively passivation, coupling, insulating wrapped processing to described mixed-powder, then compressing; Described coupling agent adopts titanate esters; Described passivator adopts water; Described insulating compound adopts glass powder with low melting point; Described binding agent adopts epoxy resin.Described Passivation Treatment step is: mixed-powder is joined in the water of 5wt%, stir until dry; Described coupling processing step is: mixed-powder is joined in the coupling agent of 5wt%, stir until dry; Described insulating wrapped treatment step is: in the mixed liquor of the epoxy resin of the glass powder with low melting point of the 6wt% that mixed-powder is joined and 8 wt %, stir until dry.Described compressing pressure adopts 25t/cm
2.
Step 4, carries out annealing in process and spraying insulation processing successively to the powder core of described moulding.Described annealing in process is carried out 3 hours at 550 ℃.It is inorganic agent that described spraying insulation processing adopts epoxy resin.
The present embodiment, by changing the composition of mixed-powder in step 2, has made 4 kinds of powder core samples, is designated as sample 1-4, and the composition of its mixed-powder refers to table 1.
Comparative example 1
The difference of this comparative example and embodiment 1 is only that the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that in step 2, mixed-powder is 100% by weight content and weight content are 0% forms.
Whether the powder core sample making in above-described embodiment and comparative example, observing can be compressing if being observed, whether compressing rear surface forms even, and effects on surface forms that uniform powder core carries out performance test and by outcome record in table 1.Performance test scheme: powder core is wound around to (30) circle with enamel-cover copper conductor, then use accurate LCR measuring instrument to measure its inductance, then according to L=(0.4 π μ N2A * 10-2)/l derives magnetic permeability, wherein N represents the number of turns, and A represents the sectional area of magnetic core, and l represents the average length of magnetic circuit, measuring condition is: alternating voltage is 1V, frequency is 1KHz, primary turns 15 circles, secondary 6 circles.
Table 1
| Nanocrystalline metal size of powder particles, weight content | Sample 1 | Sample 2 | Sample 3 | Sample 4 | Comparative example 2 |
| -40 ~+100 sieve meshes | 60% | 50% | 65% | 40% | 100% |
| -325 sieve meshes | 40% | 50% | 35% | 60% | 0% |
| High frequency magnetic permeability (1KHz, 1V) | 325 | 314 | 307 | 295 | —— |
| Soft magnetic-powder core surface composition | Surface composition is even | Surface composition is even | Surface composition is even | Surface composition is even | Can not be compressing |
Contrast by upper table is known, comparative example 1 only adopts the meal can not be compressing, sample employing meal in the embodiment of the present invention 1 and granularity and the proportioning of fine powder can be compressing, obtain the uniform powder core of surface composition, so embodiments of the invention are better than comparative example.
In embodiments of the invention 1, sample 1-3 surface composition evenly and have a magnetic permeability of superelevation, its magnetic permeability is higher than sample 4, so the preferred technical scheme of the present invention is: the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that mixed-powder described in step 2 is 50 ~ 65% by weight content and weight content are 35 ~ 50% forms.
Embodiment 2
The preparation method of the iron based nano crystal powder core with superhigh magnetic conductivity that the present embodiment provides, comprises the steps:
Step 1, carries out mechanical crushing processing to iron-based nano-crystalline thin ribbon, to obtain iron based nano crystal powder; The composition of described iron-based nano-crystalline thin ribbon is Fe
73.5cu
1nb
3si
13.5b
9;
Step 2, sieves and proportioning described iron based nano crystal powder, the mixed-powder that the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that to be then mixed into by weight content be 60% and weight content are 40% forms;
Step 3, adopts respectively passivator, coupling agent, insulating compound and binding agent to carry out successively passivation, coupling, insulating wrapped processing to described mixed-powder, then compressing; Described coupling agent adopts titanate esters; Described passivator adopts water; Described insulating compound adopts glass powder with low melting point; Described binding agent adopts epoxy resin.Described Passivation Treatment step is: mixed-powder is joined in the water of 5wt%, stir until dry; Described coupling processing step is: mixed-powder is joined in the coupling agent of 1-10wt%, stir until dry; Described insulating wrapped treatment step is: in the mixed liquor of the epoxy resin of the glass powder with low melting point of the 6wt% that mixed-powder is joined and 8 wt %, stir until dry.Described compressing pressure adopts 25t/cm
2.
Step 4, carries out annealing in process and spraying insulation processing successively to the powder core of described moulding.Described annealing in process is carried out 3 hours at 550 ℃.It is inorganic agent that described spraying insulation processing adopts epoxy resin.
The present embodiment, by changing the addition of coupling agent in step 4, has made 4 kinds of powder core samples, is designated as sample 5-8, and the addition of its coupling agent refers to table 2.
Comparative example 2
This comparative example is only not adopt coupling agent in step 4 with the difference of embodiment 2, does not also carry out coupling processing step.
Whether the powder core sample making in above-described embodiment and comparative example, observing can be compressing if being observed, whether compressing rear surface forms even, and effects on surface forms that uniform powder core carries out performance test and by outcome record in table 2.
Table 2
| Coupling agent kind, addition | Sample 5 | Sample 6 | Sample 7 | Sample 8 | Comparative example 2 |
| Coupling agent | Titanate esters | Titanate esters | Titanate esters | Titanate esters | —— |
| Addition | 1% | 5% | 10% | 20% | —— |
| High frequency magnetic permeability | 314 | 325 | 307 | 279 | —— |
| Soft magnetic-powder core surface composition | Surface composition is even | Surface composition is even | Surface composition is even | Surface composition is even | Can not be compressing |
Contrast by upper table is known, comparative example 2 does not adopt coupling agent, do not carry out coupling processing yet, can not be compressing, sample in the embodiment of the present invention 2 adopts coupling agent to carry out coupling processing can be compressing, obtain the uniform powder core of surface composition, so embodiments of the invention are better than comparative example.
The coupling agent that the present invention adopts can make the powder core making have superhigh magnetic conductivity, so the preferred technical scheme of the present invention is: coupling agent adopts titanate esters.
In embodiments of the invention 2, sample 5-7 surface composition evenly and have a magnetic permeability of superelevation, its magnetic permeability is higher than sample 8, therefore the preferred technical scheme of the present invention is: the step of coupling processing described in step 4 is: mixed-powder is joined in the coupling agent of 1-10wt%, stir until dry.
In sum, the preparation method that present embodiment provides has following characteristics: 1, adopt the method for meal, fine powder mixing and coupling processing, effectively solved the compressing problem of bulky grain manocrystalline powders; 2, make magnetic permeability and reached the more than 200 iron based nano crystal powder cores with superhigh magnetic conductivity; 3, by adopting suitable passivator, coupling agent, insulating compound and binding agent and consumption thereof, by adopting suitable heat treatment, compressing and annealing in process parameter, can make and form even, seamless, magnetic permeability and reach more than 300 nanocrystalline magnetic cores, can meet the instructions for use of motor; 4, by adopting water, be passivator, can accelerate the passivation of nanocrystal surface, be beneficial to compressing.
Claims (9)
1. a preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity, is characterized in that: comprise the steps:
Step 1, carries out mechanical crushing processing to iron-based nano-crystalline thin ribbon, to obtain iron based nano crystal powder;
Step 2, sieves and proportioning described iron based nano crystal powder, the mixed-powder that the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that to be then mixed into by weight content be 40 ~ 80% and weight content are 20 ~ 60% forms;
Step 3, adopts respectively passivator, coupling agent, insulating compound and binding agent to carry out successively passivation, coupling, insulating wrapped processing to described mixed-powder, then compressing;
Step 4, carries out annealing in process and spraying insulation processing successively to the powder core of described moulding.
2. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 1, is characterized in that: the fine powder that passes through-325 sieve meshes that the meal that passes through-40 ~+100 sieve meshes that mixed-powder described in step 2 is 50 ~ 65% by weight content and weight content are 35 ~ 50% forms.
3. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 2, is characterized in that: the composition of described iron based nano crystal powder is Fe
73.5cu
1nb
3si
13.5b
9.
4. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 3, is characterized in that: described coupling agent adopts titanate esters.
5. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 4, is characterized in that: described passivator adopts water; Described insulating compound adopts glass powder with low melting point; Described binding agent adopts epoxy resin.
6. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 5, is characterized in that: described Passivation Treatment step is: mixed-powder is joined in the water of 1-8wt%, stir until dry; Described coupling processing step is: mixed-powder is joined in the coupling agent of 1-10wt%, stir until dry; Described insulating wrapped treatment step is: in the mixed liquor of the epoxy resin of the glass powder with low melting point of the 3-10wt% that mixed-powder is joined and 5-12 wt %, stir until dry.
7. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 6, is characterized in that: pressure compressing described in step 3 adopts 18 ~ 30t/cm
2.
8. the preparation method with the iron based nano crystal powder core of superhigh magnetic conductivity according to claim 7, is characterized in that: annealing in process described in step 4 is carried out 1～4 hour at 500 ~ 600 ℃.
9. according to the preparation method of the iron based nano crystal powder core with superhigh magnetic conductivity described in claim 1-8 any one, it is characterized in that: described in step 4, spraying insulation processing employing epoxy resin is inorganic agent.
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| CN106086770A (en) * | 2016-06-21 | 2016-11-09 | 深圳顺络电子股份有限公司 | A kind of ferrous alloy powder core magnet and manufacture method thereof |
| CN106180674A (en) * | 2015-04-30 | 2016-12-07 | 深圳市麦捷微电子科技股份有限公司 | The manufacture method of alloy powder |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
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| CN106086770A (en) * | 2016-06-21 | 2016-11-09 | 深圳顺络电子股份有限公司 | A kind of ferrous alloy powder core magnet and manufacture method thereof |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
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