CN104841933B - A kind of preparation method of the low magnetic loss soft-magnetic composite material of high frequency - Google Patents
A kind of preparation method of the low magnetic loss soft-magnetic composite material of high frequency Download PDFInfo
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- CN104841933B CN104841933B CN201510237388.1A CN201510237388A CN104841933B CN 104841933 B CN104841933 B CN 104841933B CN 201510237388 A CN201510237388 A CN 201510237388A CN 104841933 B CN104841933 B CN 104841933B
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Abstract
The invention discloses a kind of preparation method of the low magnetic loss soft-magnetic composite material of high frequency.Benzocyclobutene is dissolved in 1,3,5 trimethylbenzenes and acetone mixed solvent, then Deca ethanol, is stirred simultaneously, be not further added by until observing to precipitate, stop Deca ethanol；Metal or alloy is mixed with products therefrom, with the concussion of ultrasonic vibration instrument, uses mechanical agitation simultaneously, metal or alloy is coated, form the precipitation of composite；The precipitation of composite is dried, obtains pressed powder；Pressed powder is compressing, then solidify, obtain soft-magnetic composite material.Under the conditions of 10mT, 5MHz, power attenuation density is 300mW/cm3；Applying frequency at least improves 100 times；Preparation temperature is relatively low, process is simple, and preparation efficiency is high, and material is thermally-stabilised good, and in the air can keep 300 DEG C for a long time.
Description
Technical field
The present invention relates to a kind of preparation method of the low magnetic loss soft-magnetic composite material of high frequency, belong to advanced material preparation and passive
Components and parts advanced manufacture field.
Background technology
21 century industrial development while improving people's daily life and global economy, also make environment and the energy face huge
Big challenge.At present, the focus of industrial development is turned to " energy-saving and environmental protection and sustainable development " by countries in the world, " energy-conservation
Consumption reduction, sustainable development " is also the national strategy of China.And the important technical as energy conversion, using advanced electricity
Power electronic system, reduce defeated, become, the energy loss in process of distributing electricity imperative.Therefore, in order to improve efficient energy conversion,
This requires that China needs badly in the design of the efficient power transmission and transformation power electronic system with transformator as core, material and manufacture view
Make a breakthrough and autonomous innovation.
The fast development of the third generation (SiC/GaN) power electronic devices so that power electronic system will towards high power,
Lighting, the direction of miniaturization are developed, and senior engineer's working frequency is to realize one of important technical of this target.Although at present
The operating frequency of high-power transformer can reach a megahertz level, but drastically increases because frequency improves the high-frequency loss bringing
Plus, be easily caused magnetic core caloric value excessive and cause rupture.At present still mainly to force to cool down using increasing heat sink size, this with
Future electrical energy electronic system lightweight, the target of miniaturization run in the opposite direction.The warp of power electronic system design, life-time service and maintenance
Test and show, core loss be impact high power power electronic equipment work efficiency principal element, and using have low-coercivity,
The soft magnetic materials of narrower area of hysteresis loop and raising soft magnetic materials resistivity, are to reduce gap hysteresis loss and eddy-current loss
Effective means.Therefore, develop the novel magnetic core material of the ultralow core loss of novel high-frequency, to high electric energy conversion efficiency, ensure
Following high-power electric and electronic system high-frequency Effec-tive Function is significant.
Especially frequency applications when (f=3～30MHz), the eddy-current loss (We) due to magnetic material become with resistivity (ρ)
Inverse ratio (We=CB2f2d2/ ρ), the resistivity therefore improving material becomes the effective ways reducing high frequency eddy current losses.Traditional
Although metal soft magnetic material has a high pcrmeability, high saturation magnetization, due to having low resistivity, in high frequency
Eddy-current loss increases, and energy loss is higher, and serious reduces its serviceability；Though Ferrite Material has high resistivity,
High-frequency loss is relatively low, but it belongs to ferrimagnetic material, and saturation magnetization is relatively low.Therefore they are not well positioned to meet
The frequency applications demand of the development of modern power electronic industry, especially Future third generation semiconductor device.Therefore exploitation has
The high frequency low magnetic loss soft magnetic materials of the advantages of high initial magnetoconductivity, low-coercivity, high resistivity is very necessary.
Content of the invention
The present invention be directed to the exploitation of the high frequency small of high frequency electric source, high conversion efficiency requires, aim at power supply unit
Rectifier part, makes it to meet the high power density output under upper frequency, the magnetic loss simultaneously solving transformator/inductance is asked
Topic.
Technical scheme is as follows：
A kind of preparation method of the low magnetic loss soft-magnetic composite material of high frequency：Benzocyclobutene is dissolved in 1，3，5-trimethyl-benzene
In acetone mixed solvent, then Deca ethanol, it is stirred simultaneously, be not further added by until observing to precipitate, stop Deca wine
Essence；Metal or alloy is mixed with products therefrom, with the concussion of ultrasonic vibration instrument, uses mechanical agitation, to metal or alloy simultaneously
Coated, formed the precipitation of composite；The precipitation of composite is dried, obtains pressed powder；By pressed powder
Compressing, then solidify, obtain soft-magnetic composite material.
The mass ratio of described 1，3，5-trimethyl-benzene and acetone is 3.5～1.5:1.
The quality of described benzocyclobutene and the mass ratio of solvent are 1:50～65.
Described metal or alloy is 50～35 with the mass ratio of benzocyclobutene:1.
Described metal or alloy is permalloy, Fe, Fe alloy or Ni alloy
Described during drying, baking temperature is 80～100 DEG C
Described briquetting pressure is 200～500MPa, and solidification temperature is 250～280 DEG C.
Embodiment includes but is not limited to the firing equipment such as warm table, baking oven.
The effect of the present invention：
(1) the more original Permalloy resistance rate of the soft-magnetic composite material prepared greatly improves (for original 105), magnetic core
Eddy-current loss be greatly reduced (under the conditions of 10mT, 5MHz, power attenuation density be 300mW/cm3), applying frequency improves, by former
The 100KHz coming improves to 10MHz, and applying frequency at least improves 100 times.
(2) preparation temperature of the present invention is relatively low, process is simple, efficiency high, and material heat stability is good, and (in the air can be protected for a long time
Hold 300 DEG C).
Brief description
Fig. 1：The complex permeability contrast of material before and after the cladding of embodiment 3.
Specific embodiment
The present invention is to prepare the composite wood of nucleocapsid structure using Coated with Organic Matter permalloys such as benzocyclobutenes (BCB)
Material, there is provided a kind of method that under cryogenic conditions, high efficiency prepares composite, function admirable, process is simple, heat stability is good.
Concretely comprise the following steps：
A () is equipped with organic solvent：Appropriate 1，3，5-trimethyl-benzene and acetone are mixed to form organic solvent；
B () dissolves：Take benzocyclobutene (BCB) to be dissolved in step (a) gained solvent, form the weak solution of BCB；
(c) precipitation：In the weak solution of BCB ethanol being added drop-wise to step (b) gained, solution is stirred, directly simultaneously
It is not further added by observing to precipitate, stop Deca ethanol；
D () coats：Permalloy is mixed with step (c) products therefrom, with the concussion of ultrasonic vibration instrument, uses machinery simultaneously
Stirring, coats to permalloy, forms the precipitation of composite；
E () is dried：To be precipitated completely after, supernatant is poured in waste liquid bottle, the composite having coated is dried,
Obtain pressed powder；
(f) forming and hardening：Will be compressing for the dusty material of step (e) gained, then solidify.
Embodiment 1
A () takes 15.26g 1，3，5-trimethyl-benzene and 4.36g acetone to be mixed to form organic solvent.
B () benzocyclobutene (BCB) of 0.38g is dissolved in above-mentioned solvent.
C appropriate ethanol is slowly added drop-wise in the weak solution of BCB of step (b) gained by (), until observing precipitation not
It is further added by, stop Deca ethanol, mechanical agitation is carried out to solution simultaneously.
D () pours 19g permalloy in the product of step (c) gained into, with the concussion of ultrasonic vibration instrument, use machinery simultaneously
Stirring, 350 rpms of rotating speed, continue 30 minutes, realize permalloy is fully coated.
(e) to be precipitated completely after, supernatant is poured in waste liquid bottle, by the composite having coated controllable temperature warm table
It is dried at 80 DEG C, obtain pressed powder.
F (), by the powder of step (e) gained through 200MPa pressure forming, compacting circularizes green compact；And with warm table 250
Solidify 1 hour at DEG C.
Embodiment 2
A () takes 11.82g 1，3，5-trimethyl-benzene and 7.88g acetone to be mixed to form organic solvent.
B () benzocyclobutene (BCB) of 0.3g is dissolved in above-mentioned solvent.
C appropriate ethanol is slowly added drop-wise in the weak solution of BCB of step (b) gained by (), until observing precipitation not
It is further added by, stop Deca ethanol, solution is stirred simultaneously.
D () pours 10.5g permalloy in the product of step (c) gained into, with the concussion of ultrasonic vibration instrument, use machine simultaneously
Tool stirs, and 350 rpms of rotating speed continues 30 minutes, realizes permalloy is fully coated.
(e) to be precipitated completely after, supernatant is poured in waste liquid bottle, by the composite having coated baking oven at 90 DEG C
It is dried, obtain pressed powder.
F (), by the powder of step (e) gained through 300MPa pressure forming, compacting circularizes green compact；And with baking oven at 280 DEG C
Lower solidification 1 hour.
Embodiment 3
A () takes 13.08g 1，3，5-trimethyl-benzene and 6.54g acetone to be mixed to form organic solvent.
B () benzocyclobutene (BCB) of 0.38g is dissolved in above-mentioned solvent.
C appropriate ethanol is slowly added drop-wise in the weak solution of BCB of step (b) gained by (), until observing precipitation not
It is further added by, stop Deca ethanol, solution is stirred simultaneously.
D () pours 15.2g permalloy in the product of step (c) gained into, with the concussion of ultrasonic vibration instrument, use machine simultaneously
Tool stirs, and 350 rpms of rotating speed continues 30 minutes, realizes permalloy is fully coated.
(e) to be precipitated completely after, supernatant is poured in waste liquid bottle, by the composite having coated baking oven at 100 DEG C
Under be dried, obtain pressed powder.
F (), by the powder of step (e) gained through 500MPa pressure forming, compacting circularizes green compact；And with baking oven at 280 DEG C
Lower solidification 1 hour.
The material of preparation is done the test of frequency-changing AC susceptibility, acquired results as shown in figure 1, under the conditions of 10mT, 5MHz,
Power attenuation density is 300mW/cm3.
Embodiment 4
A () takes 13.08g 1，3，5-trimethyl-benzene and 6.54g acetone to be mixed to form organic solvent.
B () benzocyclobutene (BCB) of 0.38g is dissolved in above-mentioned solvent.
C appropriate ethanol is slowly added drop-wise in the weak solution of BCB of step (b) gained by (), until observing precipitation not
It is further added by, stop Deca ethanol, solution is stirred simultaneously.
D () pours 15.2g Fe powder in the product of step (c) gained into, with the concussion of ultrasonic vibration instrument, use machinery simultaneously
Stirring, 350 rpms of rotating speed, continue 30 minutes, realize Fe powder is fully coated.
(e) to be precipitated completely after, supernatant is poured in waste liquid bottle, by the composite having coated baking oven at 100 DEG C
Under be dried, obtain pressed powder.
F (), by the powder of step (e) gained through 500MPa pressure forming, compacting circularizes green compact；And with baking oven at 280 DEG C
Lower solidification 1 hour.
Present invention disclosure and all methods proposing, are described by preferred embodiment, person skilled
Substantially in without departing from present invention, spirit and scope, methods and techniques described herein route can be modified or again
Combination, to realize final technology of preparing.Specifically, all similar replacements and change are to art technology
It is it will be apparent that they are considered as including in present invention spirit, scope and content for personnel.
Claims (6)
1. a kind of low magnetic loss soft-magnetic composite material of high frequency preparation method it is characterised in that：
Benzocyclobutene is dissolved in 1，3，5-trimethyl-benzene and acetone mixed solvent, then Deca ethanol, is stirred simultaneously
Mix, be not further added by until observing to precipitate, stop Deca ethanol；Metal is mixed with products therefrom, with the shake of ultrasonic vibration instrument
Swing, use mechanical agitation simultaneously, metal is coated, form the precipitation of composite；The precipitation of composite is dried,
Obtain pressed powder；Pressed powder is compressing, then solidify, obtain soft-magnetic composite material；Described metal closes for perm
Gold, Fe, Fe alloy or Ni alloy.
2. method according to claim 1, is characterized in that the mass ratio of described 1，3，5-trimethyl-benzene and acetone is 3.5
～1.5:1.
3. method according to claim 1, is characterized in that the described quality of benzocyclobutene and 1，3，5-trimethyl-benzene
Mass ratio with acetone mixed solvent is 1:50～65.
4. method according to claim 1, is characterized in that described metal is 50～35 with the mass ratio of benzocyclobutene:
1.
5. method according to claim 1, it is characterized in that described during drying, baking temperature is 80～100
℃.
6. method according to claim 1, is characterized in that described briquetting pressure is 200～500MPa, solidification temperature is
250～280 DEG C.
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| CN104841933B true CN104841933B (en) | 2017-03-01 |
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| US20100000769A1 (en) * | 2007-01-23 | 2010-01-07 | Tadahiro Ohmi | Composite magnetic body, method of manufacturing the same, circuit board using the same, and electronic apparatus using the same |
| JP5574395B2 (en) * | 2008-04-04 | 2014-08-20 | 国立大学法人東北大学 | Composite material and manufacturing method thereof |
| JP4513131B2 (en) * | 2008-05-23 | 2010-07-28 | 住友電気工業株式会社 | Method for producing soft magnetic material and method for producing dust core |
| CN103632794B (en) * | 2012-08-28 | 2017-04-12 | 有研稀土新材料股份有限公司 | Composite soft magnetic material and method for preparing material |
| CN103862048B (en) * | 2012-12-07 | 2015-12-02 | 中国科学院理化技术研究所 | A kind of method by hot pressing soft magnetic composite material |
| CN104028749B (en) * | 2014-06-05 | 2016-04-27 | 浙江大学 | A kind of high thermal stability insulating wrapped processing method of soft magnetic metal composite |
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Address after: 300350 District, Jinnan District, Tianjin Haihe Education Park, 135 beautiful road, Beiyang campus of Tianjin University Patentee after: Tianjin University Address before: 300072 Tianjin City, Nankai District Wei Jin Road No. 92, Tianjin University Patentee before: Tianjin University |