CN109741931A - A kind of preparation method of iron based nano crystal powder core magnet ring - Google Patents
A kind of preparation method of iron based nano crystal powder core magnet ring Download PDFInfo
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- CN109741931A CN109741931A CN201910126788.3A CN201910126788A CN109741931A CN 109741931 A CN109741931 A CN 109741931A CN 201910126788 A CN201910126788 A CN 201910126788A CN 109741931 A CN109741931 A CN 109741931A
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Abstract
The present invention relates to a kind of preparation methods of iron based nano crystal powder core magnet ring, it is compared with prior art, the present invention uses in embrittlement process and directlys adopt horizontal magnetic treatment, rejected product in the band production process for the horizontal magnetic heat treatment that can directly generate in process for producing, it can be combined simultaneously with production, improve production efficiency.Meanwhile the iron loss of prepared 1K107 nanocrystalline magnetic core is small compared with the powder core of conventional embrittlement processing, meets the developing direction of electronic device.
Description
Technical field
The present invention relates to iron-based soft magnetic technical field of function materials, more particularly to a kind of iron based nano crystal powder core magnet ring
Preparation method.
Background technique
Iron-based amorphous nanometer crystalline band is at present with very extensive amorphous series soft magnetism electronic material, due to this kind of material
The preparation of material requires high cooling rate (about 106K/s), and the strip that thickness is about 20-30 μm can only be made, then wind or
Laminated core uses.Its shape limits the shape need of certain special electronic devices, meanwhile, applying frequency is also limited to
100MHz or so, it is difficult to adapt to electronic device in the demand of element and topological structure high frequency.1985, company, alliance, U.S. report
Road uses the Fe-based amorphous powder for being ground to specified particle size range, then is prepared for amorphous powder core in a manner of powder metallurgy cold pressing,
Compared with band, the powder particle surface of powder core with coated insulating medium layer, increase the resistivity of magnetic core, reduce
The eddy-current loss of magnetic core, can adapt to frequency applications.1988, Hitachi Metals company developed Fe73.5Si13.5B9Cu1Nb3
(at.%) nanocrystalline material is named as " FineMET ", and structure is that the nanometer of 20nm or so is uniform-distribution on noncrystal substrate
Jingjing grain, the excellent soft magnet performance of the iron based nano crystal material make it become one of most widely used amorphous based material.
Current nanocrystalline magnetic core is made of to crush raw material, sieve the processes such as powder, proportion, passivation, insulating wrapped, compacting, annealing
Powder core.Generally, due to which band has toughness crushing efficiency low and influences powder particle size, to influence soft magnetic-powder core
Final performance
Therefore, it in the prior art there are problem, leftover pieces is recycled and is used to produce high saturation magnetic it is urgent to provide a kind of
Induction, low iron loss and the nanocrystalline powder core magnet ring technology of preparing of soft magnet performance haveing excellent performance are particularly important.
Summary of the invention
It is an object of the invention to avoid shortcoming in the prior art and provide a kind of leftover pieces being recycled and are used for
Produce the preparation method of high saturated magnetic induction, low iron loss and the nanocrystalline powder core magnet ring of soft magnet performance haveing excellent performance.
The purpose of the present invention is achieved through the following technical solutions:
The preparation method of iron based nano crystal powder core magnet ring, includes following steps:
(1) state that will quench iron-base nanometer crystal alloy band is coiled into magnet ring；
(2) magnet ring is put into horizontal magnetic furnace, is filled with protection gas, keep the temperature 1-2h at a temperature of 450-500 DEG C, use horizontal magnetic magnetic field pair
Magnet ring carries out brittle processing, and horizontal magnetic magnetic field strength is 800 ~ 1200Oe, obtains broken broken band；
(3) broken band is carried out being ground to powder, is put into processing in airflow milling and collects -100 mesh powders；
(4) powder that step (3) obtain is put into phosphating solution and is passivated, organic siliconresin is added after dry and carries out insulating wrapped；
(5) 1.2 ~ 1.8 are addedwt.% zinc stearate powder is pressed into powder core magnet ring；
(6) by powder core magnet ring stress relief annealing: keeping the temperature 0.5 ~ 1.5h at 450 ~ 550 DEG C, and protected using nitrogen atmosphere.
Preferably, in step (3), broken band, which is put into planetary ball mill, to be ground, with Φ 8,4 stainless steel sphere of Φ,
Ratio of grinding media to material is 10:1, and ball grinder revolving speed is 800r/min, and is protected using argon gas.
Preferably, in step (4), the phosphating solution of 0.4wt.% is poured into powder, is evenly stirred until and is completely dried；It is dry
Afterwards, the organic siliconresin acetone soln of 5wt.% is added in the powder completed to passivation, then uniform stirring 1h dries at 80 DEG C
It is dry.
Preferably, in step (6), 1h is kept the temperature at 500 DEG C, and protect using nitrogen atmosphere.
Preferably, in step (2), horizontal magnetic magnetic field strength is 1000Oe.
Preferably, in step (5), powder is pressed by toroidal core using hydraulic press, briquetting pressure is 1.8 ~ 2.0GPa.
Beneficial effects of the present invention:
The step of preparation method of iron based nano crystal powder core magnet ring of the invention (1) and (2) iron based nano crystal embrittlement handle when,
Then the state that will quench iron-base nanometer crystal alloy band coiling applies a transverse magnetic circlewise to be conducive to improve horizontal magnetic heat treatment efficiency
, make magnetic moment in band gradually longitudinally be difficult to magnetize to magnetic direction rotation.Horizontal magnetic treatment makes to generate biggish sense in band
Raw anisotropy.Horizontal magnetic heat treatment changes the anisotropy of material, changes domain structure to make the shape of hysteresis loop generate
Change, to make band that there is permanent magnetic conductivity and coercivity reduction after horizontal magnetic embrittlement processing, even if material is with stable
Magnetic conductivity and low-loss.Step (4) is passivated powder using phosphating solution, and the wedge angle of powder may make to become round and smooth, is added
The adhesive property of powder part can be improved in organic siliconresin insulating wrapped.The present invention can be improved in the zinc stearate powder of step (5)
Magnetic core powder mobility with preferably compression moulding.Step (6) stress relief annealing can eliminate answering for pressing process generation
Power.
Compared with prior art, the present invention is using directlying adopt horizontal magnetic treatment in embrittlement process, can be directly in process for producing
Rejected product in the band production process of the horizontal magnetic heat treatment generated, while can be combined with production, improve production efficiency.
Meanwhile the iron loss of prepared 1K107 nanocrystalline magnetic core is small compared with the powder core of conventional embrittlement processing, meets the hair of electronic device
Open up direction.
Specific embodiment
The invention will be further described with the following Examples.
Embodiment 1
The preparation method of the iron based nano crystal powder core magnet ring of the present embodiment includes following steps:
(1) it selects band: choosing the state 1K107 alloy strip steel rolled stock of quenching of industrial making method, bandwidth 10mm, with a thickness of 25-30um；
(2) horizontal magnetic embrittlement: being wound into 40mm*25mm*10mm magnet ring for band, be put into horizontal magnetic furnace and be heat-treated, temperature 450
DEG C, 1h, horizontal magnetic magnetic field 800Oe are kept the temperature, and be filled with N2Atmosphere protection is carried out, after the completion of heat treatment, is broken into the band of 5 ~ 10mm long
Material；
(3) band is ground using planetary ball mill, with Φ 8,4 stainless steel sphere of Φ, ratio of grinding media to material 10:1, ball grinder revolving speed is
800r/min, and protected using argon gas, milling time 8h, then secondary grinding, grinding pressure 6MPa are carried out using airflow milling；
(4) 0.4 is admixed into powderwt.% phosphating solution stirs to being completely dried, 5 is then admixed into powderwt.% organic
Silicone resin acetone soln, uniform stirring 1h are dried in 80 DEG C of baking oven；
(5) 1.2 are added into powderwt.% zinc stearate powder, molded, the magnetic suppressed that powder is cooled down with hydraulic press
Ring size is 30mm*17.5mm*14mm, briquetting pressure 1.8GPa；
(6) 1h is kept the temperature at 500 DEG C in heat-treatment furnace, and employs nitrogen as protective atmosphere.
The preparation method simple process and low cost of iron based nano crystal powder core magnet ring of the invention is suitable for industrial metaplasia
It produces.The iron loss of the product nanocrystalline magnetic core of preparation is small compared with processed conventionally powder core, adapts to electronic component miniaturization, high frequency
Change, the growth requirement of energy-saving.
Embodiment 2
The main technical schemes of the present embodiment are substantially the same manner as Example 1, the feature not laid down a definition in the present embodiment, using reality
The explanation in example 1 is applied, is no longer repeated herein.The present embodiment difference from example 1 is that,
The horizontal magnetic embrittlement of step (2): temperature is 480 DEG C, keeps the temperature 1.5h, horizontal magnetic magnetic field 1000Oe；
In step (4), 0.3 is admixed into powderwt.% phosphating solution is stirred to being completely dried, is then admixed into powder
8wt.% organic siliconresin acetone soln, uniform stirring 1.2h are dried in 85 DEG C of baking oven；
In step (5), 1.5 are added into powderwt.% zinc stearate powder, molded, molding that powder is cooled down with hydraulic press
Pressure is 1.9GPa；
In step (6), 1.2h is kept the temperature at 480 DEG C in heat-treatment furnace, and employ nitrogen as protective atmosphere.
Embodiment 3
The main technical schemes of the present embodiment and embodiment 1 or embodiment 2 are essentially identical, do not lay down a definition in the present embodiment
Feature is no longer repeated herein using the explanation in embodiment 1 or embodiment 2.The difference of the present embodiment and embodiment 1
Place is,
The horizontal magnetic embrittlement of step (2): temperature is 500 DEG C, keeps the temperature 2h, horizontal magnetic magnetic field 1200Oe；
In step (4), 0.6 is admixed into powderwt.% phosphating solution is stirred to being completely dried, is then admixed into powder
10wt.% organic siliconresin acetone soln, uniform stirring 1.5h are dried in 90 DEG C of baking oven；
In step (5), 1.8 are added into powderwt.% zinc stearate powder, molded, molding that powder is cooled down with hydraulic press
Pressure is 2.0GPa；
In step (6), 1.3h is kept the temperature at 520 DEG C in heat-treatment furnace.
Comparative example
Comparative example and embodiment 1 to 3 the difference is that, use conventional hard force broken without using horizontal magnetic embrittlement in step (2)
The broken band for making 5 ~ 10mm long, and powder core, the magnetic that embodiment 1 to 3 and comparative example obtain are prepared using conventional method
Powder core is made differential mode inductance, is surveyed using LCR digital electric bridge and soft magnetism measuring instrument using 50 circle of copper wire winding of QZY-2 Φ 1.2
Determine inductance and loss, specific measurement result is shown in Table 1, and according to formula μe=103*L*le/(4*3.14*N2* Ae) magnetic conductivity is calculated,
Wherein, L: inductance (unit: μ H), le: effective magnetic circuit length (unit: cm), N: convolute coil the number of turns, Ae: effective sectional area is (single
Position: cm2), calculate the Effective permeability μ of magnetic coree。
Table 1
Finally it should be noted that the above examples are only used to illustrate the technical scheme of the present invention explanation rather than to claim protect
Protect the limitation of range.Those skilled in the art should be appreciated that referring to preferred embodiment and can be to technology of the invention
Scheme is modified or replaced equivalently, but belongs to the substantially identical and protection scope of technical solution of the present invention.
Claims (6)
1. the preparation method of iron based nano crystal powder core magnet ring, which is characterized in that include following steps:
(1) state that will quench iron-base nanometer crystal alloy band is coiled into magnet ring；
(2) magnet ring is put into horizontal magnetic furnace, is filled with protection gas, keep the temperature 1-2h at a temperature of 450-500 DEG C, use horizontal magnetic magnetic field pair
Magnet ring carries out brittle processing, and horizontal magnetic magnetic field strength is 800 ~ 1200Oe, obtains broken broken band；
(3) broken band is carried out being ground to powder, is put into processing in airflow milling and collects -100 mesh powders；
(4) powder that step (3) obtain is put into phosphating solution and is passivated, organic siliconresin is added after dry and carries out insulating wrapped；
(5) 1.2 ~ 1.8 are addedwt.% zinc stearate powder is pressed into powder core magnet ring；
(6) by powder core magnet ring stress relief annealing: keeping the temperature 0.5 ~ 1.5h at 450 ~ 550 DEG C, and protected using nitrogen atmosphere.
2. the preparation method of iron based nano crystal powder core magnet ring according to claim 1, which is characterized in that broken in step (3)
Band is put into planetary ball mill and is ground, and with Φ 8,4 stainless steel sphere of Φ, ratio of grinding media to material 10:1, ball grinder revolving speed is
800r/min, and protected using argon gas.
3. the preparation method of iron based nano crystal powder core magnet ring according to claim 1, which is characterized in that, will in step (4)
The phosphating solution of 0.4wt.% pours into powder, is evenly stirred until and is completely dried；After drying, added into the powder of passivation completion
Then the organic siliconresin acetone soln of 5wt.%, uniform stirring 1h are dried at 80 DEG C.
4. the preparation method of iron based nano crystal powder core magnet ring according to claim 1, which is characterized in that in step (6),
1h is kept the temperature at 500 DEG C, and is protected using nitrogen atmosphere.
5. the preparation method of iron based nano crystal powder core magnet ring according to claim 1, which is characterized in that horizontal in step (2)
Magnetic magnetic field strength is 1000Oe.
6. the preparation method of iron based nano crystal powder core magnet ring according to claim 1, which is characterized in that in step (5), adopt
Powder is pressed into toroidal core with hydraulic press, briquetting pressure is 1.8 ~ 2.0GPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110453156A (en) * | 2019-08-13 | 2019-11-15 | 广东咏旺新材料科技有限公司 | Iron-based micro-nano magnetic powder material and preparation method thereof |
| CN112746146A (en) * | 2020-12-29 | 2021-05-04 | 佛山市中研非晶科技股份有限公司 | Reworking method of nanocrystalline alloy magnetic core |
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| CN1050109A (en) * | 1989-09-03 | 1991-03-20 | 首都钢铁公司冶金研究所 | Method for making amorphous constant-permeability core |
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Cited By (3)
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| CN110453156A (en) * | 2019-08-13 | 2019-11-15 | 广东咏旺新材料科技有限公司 | Iron-based micro-nano magnetic powder material and preparation method thereof |
| CN110453156B (en) * | 2019-08-13 | 2021-10-15 | 广东咏旺新材料科技有限公司 | Iron-based micro-nano magnetic powder material and preparation method thereof |
| CN112746146A (en) * | 2020-12-29 | 2021-05-04 | 佛山市中研非晶科技股份有限公司 | Reworking method of nanocrystalline alloy magnetic core |
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Application publication date: 20190510 |