CN101745637B - A kind of insulating coating method and the metal-powder-core prepared according to the method - Google Patents
A kind of insulating coating method and the metal-powder-core prepared according to the method Download PDFInfo
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- CN101745637B CN101745637B CN201010108978.1A CN201010108978A CN101745637B CN 101745637 B CN101745637 B CN 101745637B CN 201010108978 A CN201010108978 A CN 201010108978A CN 101745637 B CN101745637 B CN 101745637B
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Abstract
The metal-powder-core that the invention provides a kind of insulating coating method and prepare according to the method.A kind of insulating coating method is made up of high temperature organic insulation covering doped with nanometer oxide, and doping ratio is 0.01-8wt%.Insulating coating method of the present invention can improve the heat treatment temperature more than 50 DEG C of metal-powder-core, and loss can reduce 50mW/cm
3above, three-point bending strength more than height 5MPa.
Description
Technical field
The invention belongs to Metallic Functional Materials field, the metal-powder-core relating to a kind of insulating coating method and prepare according to the method.
Background technology
The insulating wrapped agent in metal current powder core field generally adopts inorganic insulation covering, and its feature is low price, high temperature heat-resistant process and therefore higher after heat treatment intensity.Inorganic insulation covering generally adopts sodium metasilicate, phosphate and mineral dust, such as bentonite, kaolin etc., and this type of material is oxide, draws materials extensively, decomposition temperature is high, intensity is high afterwards in heat treatment (being greater than 600 DEG C).Along with the development of metallized metal powder core, to iron sial on market, iron silicon, the demand of amorphous metal powder core promotes gradually, this type of material has high rigidity, the feature of plasticity difference, and be fragile material due to the insulating wrapped agent of oxide type, so residual stress is larger after compacting, thus increase the loss of metal-powder-core and reduce the permeability of metal-powder-core, therefore the plasticity improving insulating wrapped agent is needed to make it reduce residual stress, thus improve metal-powder-core performance, especially the comprehensive soft magnet performance of amorphous metal powder core is improved, it is made to compare permalloy, the metal-powder-cores such as iron sial have better cost performance.
But adopt conventional inorganic insulating wrapped agent technique to cause metal-powder-core residual stress large, need higher heat treatment temperature to eliminate residual stress, the raising permeability thus reduction metal-powder-core loss soldier works together; And maximum problem is that organic insulation covering decomposition temperature is low when adopting organic insulation covering technique, insulating wrapped agent generation carbonization phenomenon after heat treatment, finally cause metal-powder-core intensity low and therefore occurred the problem that loss is high, permeability is low, therefore solve the problem that traditional organic binder bond decomposition temperature is low, inorganic binder residual stress is large, thus the intensity of the metal-powder-core that hardness is large, plasticity is poor such as raising amorphous, iron sial etc. and combination property become the focus of current research.
At present, main direction concentrates on the formula improving existing inorganic coating technique, such as adding portion organic binder bond, improve the character etc. of passivating film.But this thinking can't resolve the brittleness problems of main component one inorganic binder.
The present invention is from the feature of the excellent plasticity of organic binder bond, the way trying hard to introduce Inorganic functional groups in organic binder bond improves the decomposition temperature of organic binder bond, thus solves the problem that traditional organic binder bond decomposition temperature is low, inorganic binder residual stress is large.
The object of the invention is for how reducing the residual stress of the metal-powder-core that this hardness is high, plasticity is poor to reduce the wastage, how to improve the problem that traditional organic high-temperature agglomerant annealing temperature is lower, thus the metal-powder-core improving the intensity of the metal-powder-core that this kind of hardness is high, plasticity is poor and performance and provide a kind of insulating coating method and prepare according to the method.
Summary of the invention
For above problem, the metal-powder-core we providing a kind of insulating coating method and prepare according to the method, particular content comprises:
(1) a kind of insulating coating method is formed by high temperature organic insulation covering doped with nanometer oxide, and doping ratio is 0.01-8wt%.The method of doping is: below high temperature organic insulation covering solidification temperature, add corresponding solvent make it be dissolved as uniform liquid, add nano-oxide particles again and stir, then add Magnaglo and make Magnaglo uniformly coated one deck solution film, finally heating makes the solvent of insulating wrapped agent volatilize completely and continues heating until Magnaglo has mobility.Wherein, there is the powder of passivating film on the surface that metal dust can be through passivation, also can add the supplies such as coupling agent in addition before insulating wrapped.
High temperature organic insulation covering is selected from polyimides, span Lay acid imide, cyanate, silicones wherein one or more mixture; Nano-oxide is selected from silica, aluminium oxide, titanium oxide, magnesia, calcium oxide, barium monoxide, chromium oxide, zinc oxide wherein one or more mixture.Dissolve temperature required below 280 DEG C for cyanate, dissolve temperature required below 320 DEG C for polyimides, dissolve temperature required below 240 DEG C for span Lay acid imide, dissolve temperature required below 200 DEG C for silicones.When temperature is higher, insulating wrapped agent is shorter for hardening time, thus is unfavorable for the preparation of metal-powder-core.
Nano-oxide can be silica, aluminium oxide, titanium oxide, magnesia, calcium oxide, barium monoxide, chromium oxide, zinc oxide, and its particle size is less than 100nm, and doping ratio is 0.01-8wt%, preferred 0.01-5wt%.When ratio is higher, the fragility of insulating wrapped agent itself is comparatively large, thus increases residual stress.Fully stir after adding nano-oxide, principle makes it fully be dissolved in high temperature organic insulation covering.
After this, need heating that its solvent is volatilized completely, and make binding agent itself reach certain state of cure (not necessarily will solidify completely), the principle determined is that the mixture of binding agent and metal dust has mobility at normal temperatures.Thus obtained powder also has the feature of granulation, and namely small particle powder is attached on bulky grain, forms mixture of powders of uniform size.
(2) insulating coating method of the present invention can significantly improve intensity and the heat treatment temperature of metal-powder-core, makes traditional organic high-temperature insulation covering can as the insulating wrapped agent of metal-powder-core and absorbing material; The metal-powder-core strength ratio utilizing the method to prepare exceeds 5MPa when being used alone high temperature organic adhesive, and loss simultaneously reduces 50mW/cm
3more than (test condition is 0.1T, 100kHz).
Accompanying drawing explanation
Fig. 1: there is after insulating wrapped the iron sial powder of granulation feature and the mixture of binding agent
Detailed description of the invention
embodiment 1
The present embodiment powder is the composition adopting atomization to prepare is Fe
80si
16b
4fe-based amorphous soft magnetic powder, BMI and silica are selected in insulating wrapped agent, silica mixed proportion is respectively 0wt%, 0.01wt%, 1wt%, 2wt%, 5wt%, 10wt% of BMI, its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 450 DEG C of vacuum annealings.Loss BH ac resistance analysis instrument test, bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 1 is to the improvement of metal-powder-core intensity and loss
Known by upper table: after being mixed into nano-oxide, metal-powder-core intensity obviously raises, and the larger intensity of ratio is higher, but when raising on the contrary because stress increases loss higher than during 8wt%.
embodiment 2
The present embodiment powder is the composition adopting atomization to prepare is Fe
80si
16b
4fe-based amorphous soft magnetic powder, cyanate and chromium oxide are selected in insulating wrapped agent, chromium oxide mixed proportion is respectively 0wt%, 0.01wt%, 1wt%, 2wt%, 5wt%, 10wt% of cyanate, its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 450 DEG C of vacuum annealings.Loss BH ac resistance analysis instrument test, bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 2 is to the improvement of metal-powder-core intensity and loss
Known by upper table: after being mixed into nano-oxide, metal-powder-core intensity obviously raises, and the larger intensity of ratio is higher, but when raising on the contrary because stress increases loss higher than during 8wt%.
embodiment 3
The present embodiment powder is the composition adopting atomization to prepare is Fe
80si
16b
4fe-based amorphous soft magnetic powder, polyimides and aluminium oxide are selected in insulating wrapped agent, aluminium oxide mixed proportion is respectively 0wt%, 0.01wt%, 1wt%, 2wt%, 5wt%, 10wt% of polyimides, its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 450 DEG C of vacuum annealings.Loss BH ac resistance analysis instrument test, bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 3 is to the improvement of metal-powder-core intensity and loss
Known by upper table: after being mixed into nano-oxide, metal-powder-core intensity obviously raises, and the larger intensity of ratio is higher, but when raising on the contrary because stress increases loss higher than during 8wt%.
embodiment 4
The present embodiment powder is the composition adopting atomization to prepare is Fe
80si
16b
4fe-based amorphous soft magnetic powder, insulating wrapped agent selects BMI and silica, aluminium oxide, titanium oxide, magnesia, calcium oxide, barium monoxide, chromium oxide, zinc oxide, mixed proportion to be 2wt%, its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 450 DEG C of vacuum annealings.Loss BH ac resistance analysis instrument test, bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 4 is to the improvement of metal-powder-core intensity and loss
Known by upper table: after different oxide nano particles mixing, all can to improve intensity simultaneously and reduce the wastage.
embodiment 5
The present embodiment powder is the composition adopting atomization to prepare is Fe
80si
16b
4fe-based amorphous soft magnetic powder, polyimides and aluminium oxide are selected in insulating wrapped agent, and aluminium oxide mixed proportion is respectively 0wt% and 2wt% of polyimides, and its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 200 DEG C, 300 DEG C, 400 DEG C, 450 DEG C, 500 DEG C vacuum annealings.Bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 5 is to the improvement of the intensity after metal-powder-core different heat treatment Temperature Treatment and loss
Known by upper table: after being mixed into nano-oxide, under same heat treatment temperature, metal-powder-core intensity has raising in various degree, and it is higher to be mixed into ratio, the degree improved is more obvious, only in 0.01wt% situation, after its 450 DEG C of heat treatments, intensity is also higher than intensity during unmixed nano-oxide.Mixed proportion more high-temperature improves more.
embodiment 6
The present embodiment powder is the composition adopting atomization to prepare is iron sial powder, cyanate and chromium oxide are selected in insulating wrapped agent, chromium oxide mixed proportion is respectively 0wt%, 0.01wt%, 1wt%, 2wt%, 5wt%, 10wt% of cyanate, its particle size is below 50nm, integral insulation covering accounts for 3% of amorphous powder, and pressing pressure is 1800MPa.Metal-powder-core is afterwards 550 DEG C of vacuum annealings.Loss BH ac resistance analysis instrument test, bending strength adopts the three-point bending method test of universal tensile testing machine.
The different oxide mixed proportion of table 6 is to the improvement of metal-powder-core intensity and loss
Known by upper table: after being mixed into nano-oxide, metal-powder-core loss decreases, and ratio more lossy reduce more, but when higher than during 8wt% due to stress increase loss raise on the contrary.
Claims (2)
1. an insulating coating method, for clad metal powder core, it is characterized in that being formed by high temperature organic insulation covering doped with nanometer oxide, the size of this nano-oxide particles is less than 100nm, and doping ratio is 0.01-5wt%; The method of doping is: below high temperature organic insulation covering solidification temperature, add corresponding solvent make it be dissolved as uniform liquid, add nano-oxide particles again and stir, then add Magnaglo and make Magnaglo uniformly coated one deck solution film, described Magnaglo is the powder having passivating film through the surface of transpassivation, and finally heating makes the solvent of insulating wrapped agent volatilize completely and continues heating until Magnaglo has mobility; High temperature organic insulation covering is selected from wherein one or more the mixture of cyanate, polyimides, span Lay acid imide, silicones; Nano-oxide is selected from wherein one or more the mixture of silica, aluminium oxide, titanium oxide, magnesia, calcium oxide, barium monoxide, chromium oxide, zinc oxide; Magnaglo after insulating wrapped has mobility at normal temperatures, and realizes the granulation to Magnaglo by described insulating coating method.
2. the metal-powder-core prepared of insulating coating method according to claim 1, it is characterized in that: the heat treatment temperature ratio of described metal-powder-core is used alone high temperature organic insulation covering as high more than 50 DEG C during covering, metal-powder-core after process is than three-point bending strength more than height 5MPa when being used alone high temperature organic insulation covering, and loss is comparatively used alone high temperature organic insulation covering and reduces 50mW/cm as during covering
3above.
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| CN103928202B (en) * | 2011-09-26 | 2016-03-02 | 南通大学 | A kind of insulating particle of 3 D electrode reactor and application process |
| JP6864498B2 (en) * | 2017-02-28 | 2021-04-28 | 山陽特殊製鋼株式会社 | A soft magnetic flat powder having high magnetic permeability and high weather resistance and a soft magnetic resin composition containing the same. |
| CN114597050B (en) * | 2022-03-23 | 2023-10-20 | 合肥工业大学 | Preparation method of modified nano oxide/kaolin coated iron-silicon-aluminum-vanadium magnetic powder core |
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Inventor after: Zhang Yanfei Inventor after: Zhang Haibo Inventor after: Guo Feng Inventor after: Jia Chunhong Inventor before: Zhang Yanfei Inventor before: Guo Peng Inventor before: Jia Chunhong |
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Effective date of registration: 20160204 Address after: 215399 No. 16, No. 1, material processing zone, international mould City, 38888 Town Road, Yushan, Kunshan, Jiangsu Applicant after: Chai Xiulan Address before: 100094, Beijing, Haidian District Zhongguancun Yongfeng industrial base, No. 7 Feng Hui Road, new materials building, room 814 Applicant before: Chai Xiulan |
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