CN103377785A - Method for preparing metal soft magnetic powder core by adopting inorganic insulation adhesive particles - Google Patents
Method for preparing metal soft magnetic powder core by adopting inorganic insulation adhesive particles Download PDFInfo
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Abstract
The invention discloses a method for preparing metal soft magnetic powder core by adopting inorganic insulation adhesive particles. The method includes steps of 1), matching and mixing the metal soft magnetic powder according to particle size of the powder; 2), adding passivant into the magnetic powder matched in the step 1) and for passivating treatment; 3), mixing the inorganic insulation particles with passivated magnetic powder intensively and directly; 4), adding insulating compound 0-0.1 in weight percentage; 5), moulding mixture obtained in the step 4) at 1200-2500MPa, placing blank samples in a protective atmosphere and subjecting the blank samples to thermal insulation at the temperature of 400-800 DEG C for 0.5-3 hours prior to air cooling and spraying to obtain target products. An inorganic adhesive coating process adopted in the method is pollution-free to environment, passivated films are even and clean, the products after annealing are high in tensile strength with no need for solidification, so that production efficiency is improved. Besides, comprehensive performance of the products is good and above the industry standard.
Description
Technical field
The present invention relates to the manufacturing technology field of magnetic bodies, be specifically related to the method that a kind of inorganic insulation bonded particulate prepares soft magnetic metal powder core.
Background technology
After being mixed with dielectric (forming film) by ferromagnetic metal (or alloy) particle, adopt by soft magnetic metal powder core the manufacturing of powder metallurgy forming technology to form.Most domestic manufacturing enterprise still prepares soft magnetic metal powder core with the organic adhesive cladding process at present.Preparation technology's cycle of its bonding is long, and is large to the potential injury of operating personnel's health in the time of environmental pollution, and a little less than the ageing resistance of the powder core of preparation.
Publication number is the manufacture method that the Chinese invention patent of CN101226804A discloses the Fe-Si-Al magnetic core of a kind of magnetic permeability μ=125, and wherein binding agent is the silicone grease with the alcohol dilution.The weak point of this technical scheme is with the properties of product of this organic binder bond preparation relatively poor; To utilizing the prepared product of this technical scheme to test, find its dc superposition characteristic when 40Oe, effective permeability is magnetic permeability μ and permeability of vacuum μ for the 50%(effective permeability only
0Ratio), at f=50kHz, B
mIron loss P during=1000Gs
CvGreater than 300mW/cm
3, be lower than industry standard, and the tensile strength of product is low.
Publication number is that the Chinese invention patent of CN1967736A discloses a kind of Fe-based amorphous, nanocrystalline magnetic core preparation method, and wherein binding agent is polyvinyl alcohol water solution.Adopt this organic insulation binding agent, although technique is simple, be easy to moulding and the demoulding, the existence of organic substance is so that not environmental protection of preparation process, and the tensile strength of powder core is also low after the heat treatment, needs again to solidify the steps such as processing.Increase production cost, also reduced production efficiency.
Application number is the preparation method that 201210206560.3 Chinese invention patent discloses a kind of high performance nano-crystal powder core, and it uses sodium metasilicate (waterglass) as binding agent in the process of preparation nanocrystalline magnetic core.As a kind of inorganic binder, although the sodium metasilicate environmental protection, the powder core intensity of preparation is high, and comprehensive magnetic can reduce greatly, and particularly power loss promotes greatly, can not satisfy industry standard.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of inorganic insulation bonded particulate to prepare the method for soft magnetic metal powder core, improve powder core preparation efficiency and product combination property.
The technical solution adopted in the present invention is specific as follows:
The method that the inorganic insulation bonded particulate prepares soft magnetic metal powder core comprises the steps:
(1) the soft magnetic metal powder with different meshes mixes, wherein,-100 orders～+ 200 purpose soft magnetic metal powder account for 40～80% ,-400 purpose soft magnetic metal powder that 10～30% ,-200 orders of gross mass～+ 400 purpose soft magnetic metal powder account for gross mass and account for 10～30% of gross mass;
(2) add passivator in the soft magnetic metal powder for preparing to step (1) and carry out Passivation Treatment, described passivator is one or more of hydrogen peroxide, phosphoric acid, chromic acid, nitric acid; The gross mass of passivator is 0.1～5% of Magnaglo total weight;
(3) with the inorganic insulation particle directly with passivation after the soft magnetic metal powder fully mix, the quality of inorganic insulation particle is 0.1～3% of soft magnetic metal powder gross mass;
(4) the adding percentage by weight is 0.01～0.1% insulating compound; Described insulating compound is one or more in kaolin, mica powder or the talcum powder; Add percentage by weight again and be 0.2～1.0% release agent, described release agent is one or more of zinc stearate, barium stearate, calcium stearate, molybdenum bisuphide;
(5) mixture that step (4) is obtained is at the pressure compacted under of 1200～2500MPa, after the base sample is positioned in the protective atmosphere, in 400～800 ℃ of lower insulations 0.5～3 hour, air cooling, spraying obtains soft magnetic metal powder core.
Described metal soft magnetic powder is one or more in iron powder, iron silica flour, iron aluminum silicon powder, iron nickel powder, iron nickel molybdenum powder, iron tantnickel powder, Fe-based amorphous powder or the iron based nano crystal powder.
The mass percent component of described inorganic insulation bonded particulate is 30～55%P
2O
5, 34.9～59.9%ZnO, 10～20%B
2O
3, 0.02～20%CuO, 0.02～10%Bi
2O
3, 0.02～10%SrO
5, 0.01～5%Al
2O
3, 0.01～5%Na
2O, 0.01～5%Li
2O
5, 0.01～5%PbO.
The mass percent component of described inorganic insulation bonded particulate is 30～55%P
2O
5, 35～60%ZnO, 10～20%B
2O
3
The granularity of described inorganic insulation bonded particulate is 5～20um.
Protective atmosphere in the described step (5) is nitrogen, argon gas or hydrogen.
The beneficial effect that the present invention compared with prior art has:
1. make final magnetic product keep good comprehensive magnetic can the time, greatly increase the radially tensile strength of powder core, thereby do not need to be cured processing;
2. the inorganic insulation bonded particulate can be directly mixes with magnetic after the passivation, need not drying, has improved production efficiency;
Embodiment
Embodiment 1
(1) the iron powder powder with different meshes mixes, and wherein ,-100 orders～+ 200 purpose iron powder powder account for 80% ,-400 purpose iron powder powder that 10% ,-200 orders of gross mass～+ 400 purpose iron powder powder account for gross mass and account for 10% of gross mass;
(2) add hydrogen peroxide passivator in the iron powder powder for preparing to step (1) and carry out Passivation Treatment, the hydrogen peroxide quality is 0.1% of Magnaglo total weight;
(3) with the inorganic insulation particle directly with passivation after the iron powder powder fully mix, the quality of inorganic insulation particle is 0.1% of iron powder powder total weight, the mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 60%ZnO, 10%B
2O
3
(4) adding percentage by weight is 0.01% kaolin insulating compound, adds percentage by weight again and be 0.2% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1200MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the nitrogen atmosphere, in 400 ℃ of lower insulations 0.5 hour, air cooling, spraying obtains ferrocart core.
After testing, associated electrical magnetic parameter such as the table 1 of target product:
Embodiment 2
(1) the iron Si powder of different meshes is mixed, wherein ,-100 orders～+ 200 purpose iron Si powder account for 40% ,-400 purpose iron Si powder that 30% ,-200 orders of gross mass～+ 400 purpose iron Si powder account for gross mass and account for 30% of gross mass;
(2) add the phosphorus acid passivation agent in the iron Si powder for preparing to step (1) and carry out Passivation Treatment, the quality of phosphoric acid is 5% of iron Si powder total weight;
(3) with the inorganic insulation particle directly with passivation after the iron Si powder fully mix, the quality of inorganic insulation particle is 3% of iron Si powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 59.9%ZnO, 10%B
2O
3, 0.02%CuO, 0.02%Bi
2O
3, 0.02%SrO
5, 0.01%Al
2O
3, 0.01%Na
2O, 0.01%Li
2O
5, 0.01%PbO;
(4) the adding percentage by weight is 0.1% mica powder insulating compound; Add again percentage by weight and be 1.0% barium stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 2500MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the hydrogen atmosphere, in 800 ℃ of lower insulations 3 hours, air cooling, spraying obtains iron silica flour core.
After testing, associated electrical magnetic parameter such as the table 2 of target product:
Embodiment 3
(1) the iron sial powder with different meshes mixes, and wherein ,-100 orders～+ 200 purpose iron sial powder account for 70% ,-400 purpose iron sial powder that 10% ,-200 orders of gross mass～+ 400 purpose iron sial powder account for gross mass and account for 20% of gross mass;
(2) add passivator in the iron sial powder for preparing to step (1) and carry out Passivation Treatment, described passivator is phosphoric acid and hydrogen peroxide; Wherein, the quality of phosphoric acid is 0.3% of iron sial mixed-powder gross mass, and the quality of hydrogen peroxide is 0.5% of iron sial mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after iron sial powder fully mix, the quality of inorganic insulation particle is 0.8% of iron sial powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 20%CuO, 1%Bi
2O
3, 1%SrO
5, 1%Al
2O
3, 1%Na
2O, 0.5%Li
2O
5, 0.5%PbO;
(4) the adding percentage by weight is 0.05% talcum powder insulating compound; Add again percentage by weight and be 0.25% calcium stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1980MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 700 ℃ of lower insulations 1 hour, air cooling, spraying obtains the iron Si-Al Magnetic Powder Core.
After testing, associated electrical magnetic parameter such as the table 3 of target product:
Embodiment 4
(1) the iron nickel magnetic that makes that makes water fogging (contains Ni49.0%, Mn0.3%, Ti0.6%, surplus is Fe) mix, wherein,-100 orders～+ 200 purpose iron nickel by powder account for 55% ,-400 purpose iron nickel by powder that 15% ,-200 orders of gross mass～+ 400 purpose iron nickel by powder account for gross mass and account for 30% of gross mass;
(2) add passivator in the iron nickel by powder for preparing to step (1) and carry out Passivation Treatment, described passivator is chromic acid and hydrogen peroxide; Wherein, the quality of chromic acid is 0.5% of iron nickel mixed-powder gross mass, and the quality of hydrogen peroxide is 0.5% of iron nickel mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after the iron nickel by powder fully mix, the quality of inorganic insulation particle is 0.8% of iron nickel by powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 20%CuO, 1%Bi
2O
3, 1%SrO
5, 1%Al
2O
3, 1%Na
2O, 0.5%Li
2O
5, 0.5%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% molybdenum bisuphide release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1800MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 700 ℃ of lower insulations 1 hour, air cooling, spraying obtains iron nickel powder core.
After testing, associated electrical magnetic parameter such as the table 4 of target product:
Embodiment 5
(1) the iron nickel molybdenum magnetic that makes that makes water fogging (contains Fe17.0%, Mo2.0%, Cu1.0%, Al+Si＜1.0%, surplus is Ni) mix, wherein ,-100 orders～+ 200 purpose iron nickel by powder account for 20% of gross mass, 60% ,-400 purpose iron nickel by powder that-200 orders～+ 400 purpose iron nickel by powder account for gross mass account for 20% of gross mass;
(2) add passivator in the iron nickel by powder for preparing to step (1) and carry out Passivation Treatment, described passivator is chromic acid and hydrogen peroxide; Wherein, the quality of chromic acid is 0.5% of iron nickel molybdenum mixed-powder gross mass, and the quality of hydrogen peroxide is 0.5% of iron nickel molybdenum mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after iron nickel molybdenum powder fully mix, the quality of inorganic insulation particle is 0.8% of iron nickel molybdenum powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 2%CuO, 10%Bi
2O
3, 10%SrO
5, 1%Al
2O
3, 1%Na
2O, 0.5%Li
2O
5, 0.5%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1800MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 700 ℃ of lower insulations 1 hour, air cooling, spraying obtains FeNiCo magnetic core.
After testing, associated electrical magnetic parameter such as the table 3 of target product:
Embodiment 6
(1) the iron tantnickel magnetic that makes of water atomization (contains (atomic percent) Si9.0%, Ni4%, Al+P＜0.5%, surplus is Fe) mix, wherein,-100 orders～+ 200 purpose iron tantnickel magnetic powders account for 60% ,-400 purpose iron tantnickel magnetic powders that 30% ,-200 orders of gross mass～+ 400 purpose iron tantnickel magnetic powders account for gross mass and account for 10% of gross mass;
(2) add passivator in the iron tantnickel magnetic powder for preparing to step (1) and carry out Passivation Treatment, described passivator is phosphoric acid and hydrogen peroxide; Wherein, the quality of phosphoric acid is 0.5% of iron sial boron amorphous magnetic mixed-powder gross mass, and the quality of hydrogen peroxide is 0.5% of iron sial boron amorphous magnetic mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after iron sial boron amorphous magnetic powder fully mix, the quality of inorganic insulation particle is 1% of iron sial boron amorphous magnetic powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 4%CuO, 3%Bi
2O
3, 3%SrO
5, 5%Al
2O
3, 5%Na
2O, 3%Li
2O5,2%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1600MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 600 ℃ of lower insulations 1 hour, air cooling, spraying obtains iron tantnickel powder core.
After testing, associated electrical magnetic parameter such as the table 6 of target product:
Embodiment 7
(1) the Fe-based amorphous magnetic that makes of water atomization (contains (atomic percent) Si9.0%, B13.0%, Al+P＜0.5%, surplus is Fe) mix, wherein,-100 orders～Fe-based amorphous magnetic powder of+200 purposes accounts for the Fe-based amorphous magnetic powder of 60% ,-400 purposes that 30% ,-200 orders of gross mass～Fe-based amorphous magnetic powder of+400 purposes accounts for gross mass and accounts for 10% of gross mass;
(2) add passivator in the Fe-based amorphous magnetic powder for preparing to step (1) and carry out Passivation Treatment, described passivator is phosphoric acid and hydrogen peroxide; Wherein, the quality of phosphoric acid is 1% of Fe-based amorphous magnetic mixed-powder gross mass, and the quality of hydrogen peroxide is 0.5% of Fe-based amorphous magnetic mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after Fe-based amorphous magnetic powder fully mix, the quality of inorganic insulation particle is 1% of Fe-based amorphous magnetic powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 2%CuO, 2%Bi
2O
3, 1%SrO
5, 5%Al
2O
3, 5%Na
2O, 5%Li
2O5,5%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1700MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 450 ℃ of lower insulations 1 hour, air cooling, spraying obtains Fe-based amorphous powder core.
After testing, associated electrical magnetic parameter such as the table 6 of target product:
Embodiment 8
(1) the iron based nano crystal magnetic that makes of water atomization (contains (atomic percent) Fe73.5%, Cu1.0%, Nb3.0%, Si13.5%, B9.0%) mix, wherein ,-100 orders～+ 200 purpose iron based nano crystal magnetic powders account for 30% of gross mass, 60% ,-400 purpose iron based nano crystal magnetic powders that-200 orders～+ 400 purpose iron based nano crystal magnetic powders account for quality account for 10% of gross mass;
(2) add passivator in the iron based nano crystal magnetic powder for preparing to step (1) and carry out Passivation Treatment, described passivator is phosphoric acid and nitric acid; Wherein, the quality of phosphoric acid is 0.5% of iron based nano crystal magnetic mixed-powder gross mass, and the quality of nitric acid is 0.3% of iron based nano crystal magnetic mixed-powder gross mass;
(3) with the inorganic insulation particle directly with passivation after iron sial boron amorphous magnetic powder fully mix, the quality of inorganic insulation particle is 1% of iron sial boron amorphous magnetic powder total weight; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 12%B
2O
3, 5%CuO, 3%Bi
2O
3, 3%SrO
5, 2%Al
2O
3, 3%Na
2O, 3%Li
2O
5, 4%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1700MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 520 ℃ of lower insulations 1 hour, air cooling, spraying obtains the iron based nano crystal powder core.
After testing, associated electrical magnetic parameter such as the table 7 of target product:
Embodiment 9
(1) the make water fogging Fe-based amorphous magnetic that makes (contain (atomic percent) Si9.0%, B13.0%, Al+P＜0.5%, surplus is Fe) and iron powder mixes, and obtains mixing magnetic powder, and wherein, Fe-based amorphous magnetic powder accounts for 50%, and the iron powder powder accounts for 50%;-100 orders～+ 200 purposes mix 30% ,-200 orders that magnetic powder accounts for gross mass～+ 400 purposes and mix 60% ,-400 purposes that magnetic powder accounts for gross mass and mix magnetic powder and account for 10% of gross mass;
(2) add passivator in the mixing magnetic powder for preparing to step (1) and carry out Passivation Treatment, described passivator is phosphoric acid and nitric acid; Wherein, the quality of phosphoric acid is for mixing 1% of magnetic powder quality, and the quality of nitric acid is for mixing 0.5% of magnetic powder quality;
(3) with the inorganic insulation particle directly with passivation after fully mix for mixing magnetic powder, the quality of inorganic insulation particle is 1% of mixing magnetic powder quality; The mass percent component of inorganic insulation bonded particulate is 30%P
2O
5, 35%ZnO, 10%B
2O
3, 2%CuO, 2%Bi
2O
3, 1%SrO
5, 5%Al
2O
3, 5%Na
2O, 5%Li
2O5,5%PbO;
(4) the adding percentage by weight is 0.05% kaolin insulating compound; Add again percentage by weight and be 0.25% zinc stearate release agent;
(5) mixture that step (4) is obtained is pressed into ring-like base sample under the pressure of 1600MPa, the external diameter of magnet ring is 22.90mm, and internal diameter is 14.20mm, and height is 7.60mm.After the base sample is positioned in the argon gas atmosphere, in 450 ℃ of lower insulations 1 hour, air cooling, spraying obtains mixing powder core.
After testing, associated electrical magnetic parameter such as the table 6 of target product:
Claims (6)
1. an inorganic insulation bonded particulate prepares the method for soft magnetic metal powder core, it is characterized in that comprising the steps:
(1) the soft magnetic metal powder with different meshes mixes, wherein,-100 orders ~+200 purpose soft magnetic metal powder account for 40 ~ 80% ,-400 purpose soft magnetic metal powder that 10 ~ 30% ,-200 orders of gross mass ~+400 purpose soft magnetic metal powder account for gross mass and account for 10 ~ 30% of gross mass;
(2) add passivator in the soft magnetic metal powder for preparing to step (1) and carry out Passivation Treatment, described passivator is one or more of hydrogen peroxide, phosphoric acid, chromic acid, nitric acid; The gross mass of passivator is 0.1 ~ 5% of Magnaglo total weight;
(3) with the inorganic insulation particle directly with passivation after the soft magnetic metal powder fully mix, the quality of inorganic insulation particle is 0.1 ~ 3% of soft magnetic metal powder gross mass;
(4) adding percentage by weight is the insulating compound of 0.01 ~ 0.1 %; Described insulating compound is one or more in kaolin, mica powder or the talcum powder; Add the release agent that percentage by weight is 0.2 ~ 1.0 %, described release agent is one or more of zinc stearate, barium stearate, calcium stearate, molybdenum bisuphide again;
(5) mixture that step (4) is obtained is at the pressure compacted under of 1200 ~ 2500MPa, after the base sample is positioned in the protective atmosphere, in 400 ~ 800 ℃ of lower insulations 0.5 ~ 3 hour, air cooling, spraying obtains soft magnetic metal powder core.
2. method according to claim 1 is characterized in that, described metal soft magnetic powder is one or more in iron powder, iron silica flour, iron aluminum silicon powder, iron nickel powder, iron nickel molybdenum powder, iron tantnickel powder, Fe-based amorphous powder or the iron based nano crystal powder.
3. method according to claim 1 is characterized in that, the mass percent component of described inorganic insulation bonded particulate is 30 ~ 55% P
2O
5, 34.9 ~ 59.9% ZnO, 10 ~ 20% B
2O
3, 0.02 ~ 20% CuO, 0.02 ~ 10% Bi
2O
3, 0.02 ~ 10% SrO
5, 0.01 ~ 5% Al
2O
3, 0.01 ~ 5% Na
2O, 0.01 ~ 5% Li
2O
5, 0.01 ~ 5% PbO.
4. method according to claim 1 is characterized in that, the mass percent component of described inorganic insulation bonded particulate is 30 ~ 55% P
2O
5, 35 ~ 60% ZnO, 10 ~ 20% B
2O
3
5. method according to claim 1 is characterized in that, the granularity of described inorganic insulation bonded particulate is 5 ~ 20um.
6. method according to claim 1 is characterized in that, the protective atmosphere in the described step (5) is nitrogen, argon gas or hydrogen.
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