CN104028750A - High-bonding-strength insulated coating treatment method of metal soft magnetic composite material - Google Patents
High-bonding-strength insulated coating treatment method of metal soft magnetic composite material Download PDFInfo
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- CN104028750A CN104028750A CN201410245747.3A CN201410245747A CN104028750A CN 104028750 A CN104028750 A CN 104028750A CN 201410245747 A CN201410245747 A CN 201410245747A CN 104028750 A CN104028750 A CN 104028750A
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Abstract
The invention discloses a high-bonding-strength insulated coating treatment method of a metal soft magnetic composite material. The method comprises the following steps: (1) sieving metal magnetic powder, and performing particle size distribution; (2) performing insulated coating on the distributed metal magnetic powder by using a sol-gel method, and then drying the metal magnetic powder; (3) uniformly mixing the dried magnetic powder and an adhesive, adding a release agent, and performing dry pressing to obtain a magnetic ring; (4) performing heat preservation, air cooling and spraying on the magnetic ring in protective atmosphere to obtain a target product. The bonding strength of composite powder prepared by using the sol-gel method and magnetic powder particles is high, the powder is coated uniformly and densely, and a coating layer is controllable in thickness, good, oxidation resistance and high saturation magnetization intensity are achieved, excellent in magnetic property and mechanical property, high in bonding strength, and not prone to disengagement; the coating effect is superior to that of an existing method; the method is high in operability and facilitates batch production; the resistivity of soft magnetic metal particles is effectively improved, and the magnetic core loss of the soft magnetic composite material is greatly reduced.
Description
Technical field
The present invention relates to the preparing technical field of magnetic material, relate in particular to a kind of high bond strength insulating wrapped processing method of soft magnetic metal composite.
Background technology
Soft magnetic metal composite is to mix by having ferromagnetic powder particle a kind of soft magnetic materials that compacting forms with megohmite insulant.Soft magnetic metal composite had both retained a part of good characteristic of soft magnetic metal and ferrite soft magnetic, had overcome again both some defects simultaneously, and combination property is splendid.The conventional preparation process of soft-magnetic composite material comprises: powder passivation, insulating wrapped, compressing and heat treatment etc.Wherein insulating wrapped is an important link in soft-magnetic composite material preparation process, and coated quality directly has influence on the magnetic properties such as frequency characteristic of soft-magnetic composite material, and under high frequency, good insulating wrapped can significantly reduce the eddy-current loss of material.And in compressing process, the easily fragmentation of insulating barrier that associativity is poor, simultaneously because pressing process can produce a large amount of internal stress and defect, cause the increase of magnetic hystersis loss, need to eliminate residualinternal stress by high-temperature heat treatment, thereby require the good thermal stability of insulating wrapped agent, can in annealing process, not decompose.Therefore in the urgent need to preparing densification, associativity is good and have the insulating coating of good thermal stability.
Patent CN100500783C adopts by SiO
2, Al
2o
3, ZrO
2, mica powder mixture of nanoparticles as insulating compound, prepare FeSiAl soft-magnetic composite material; but magnetic and insulating compound even mixes more difficult control; be difficult to magnetic to be evenly coated; and insulated by oxide clad and magnetic bond strength are not high; in pressing process, easily come off, thereby affect covered effect, cause core loss to increase.Japanese patent laid-open 9-74011 and Unexamined Patent 9-125108 disclose employing inorganic insulation binding agent sodium metasilicate and have prepared FeSiAl soft-magnetic composite material, but this soft-magnetic composite material is in heat treatment process, because the decomposition of sodium metasilicate causes cracking even, come off, thereby reduced the insulating properties of magnetic.
The patent No. is that 200910082072.4 Chinese invention patent discloses employing ethyl orthosilicate and ammoniacal liquor etc. as raw material, uses sol-gal process to the coated one deck SiO in FeSiAl magnetic surface
2insulating barrier, and its coated thickness can regulate according to the concentration of ethyl orthosilicate, and this is also the illustration that sol-gal process can be prepared the even and controlled nano particle of size.But in patent, do not provide the magnetic property of prepared soft magnetic metal composite.The patent No. is the preparation method that 201310411806.5 Chinese invention patent discloses ferrite composite magnetic powder core, this technique is prepared ferrite particle by hydro-thermal method, then adopt the mode of mechanical mixture to be coated magnetic, although the shortcoming that while having overcome to a certain extent namagnetic substance as covering, matrix magnetic property reduces, but ferrite particle and magnetic substrate combinating strength are poor, easily come off, be difficult to magnetic to carry out good being coated.
The patent No. is the preparation method that 201310212031.9 Chinese invention patent discloses a kind of soft magnetic metal composite, selects nano-oxide dispersion liquid to carry out insulating wrapped to metal magnetic.Because this dispersion stability is poor, and nano particle is not good enough to the adhesiveness of magnetic, is difficult to realize evenly coated, at magnetic, be processed in the process of soft-magnetic composite material simultaneously, the megohmite insulant of magnetic surface adhesion easily comes off, and causes magnetic insulating properties poor, and magnetic core eddy-current loss is bigger than normal.The place that the present invention distinguishes is with it: the present invention carries out insulating wrapped by sol-gal process to metal dust, and clad and magnetic bond strength are high, good uniformity, and there is good heat endurance and good magnetic property.
Summary of the invention
The defect of low, the coated inhomogeneous and poor heat stability of insulating coating bond strength for current soft-magnetic composite material, the invention provides a kind of high bond strength insulating wrapped processing method of soft magnetic metal composite, adopt sol-gal process to the coated TiO with high bond strength of soft magnetic metal composite
2insulating barrier, technical scheme of the present invention is as follows:
The high bond strength insulating wrapped processing method of soft magnetic metal composite comprises the steps:
1) grain size proportion: carry out grain size proportion after metal magnetic is sieved, described metal magnetic is iron-based magnetic, the silica-based magnetic of iron or the Ni-based magnetic of iron;
2) sol-gal process insulating wrapped: dissolve the butyl titanate of ethanol volume 5 ~ 10% in ethanol, at room temperature stir 30 ~ 120min, obtain precursor solution; Deionized water, glacial acetic acid and ethanol by volume 1:2:4 ~ 1:2:7 mix mutually, when stirring, dropwise join in precursor solution; Then after lasting stirring 60 ~ 180min, obtain the TiO of yellow transparent
2colloidal sol; TiO
2colloidal sol is under reflux conditions placed in the environment of 50 ~ 100oC until form gel; By the gel mix and blend of metal magnetic and metal magnetic weight 1.0 ~ 5.0%, until solvent evaporation is completely, the magnetic after being coated; Then the magnetic after coated is placed in to the dry 10 ~ 20h of 50 ~ 100oC environment; Again the magnetic after coated is placed in the tube furnace of atmosphere of inert gases and heats 5 ~ 10h under 500 ~ 700oC; Magnetic after coated adds the binding agent that accounts for the magnetic quality 0.5 ~ 2.5% after being coated, and is stirred well to mixture and is dried, mixes under heating condition; In magnetic after the most backward being coated, add and account for the releasing agent of the magnetic gross weight 0.5 ~ 2.0% after being coated and mix, obtain magnetic to be formed;
3) compressing: magnetic to be formed is compressing under the pressure of 600 ~ 2000MPa;
4) heat treatment: adopt nitrogen or argon gas to make protective atmosphere, soft-magnetic composite material is placed in to 400 ~ 650oC environment and is incubated 30 ~ 120min;
5) surface spraying: surface spraying one deck epoxy resins insulation paint of the soft-magnetic composite material after step 4) is processed, make finished product, obtain soft magnetic metal composite.
The weight of described metal magnetic is 10 ~ 20g, and in described precursor solution, the volume of ethanol is 100 ~ 150mL, and the volume of described deionized water is 5 ~ 20 mL.
Described binding agent is phenolic resins, epoxy resin, silicones, poly-ethylene fluoride, melmac, glass powder with low melting point, SiO
2in one or more.
Described releasing agent is one or more in zinc stearate, barium stearate, calcium stearate or molybdenum bisuphide.
Compare with existing soft-magnetic composite material preparation method, the main tool of the present invention has the following advantages:
(1) composite powder and the magnetic powder particle bond strength that adopt sol-gal process to prepare are high, coated even, fine and close, coating thickness is controlled, has good non-oxidizability, high resistivity, high saturation magnetization, has good magnetic property and mechanical property;
(2) adopt sol-gal process at metal magnetic coated with uniform one deck TiO
2insulating barrier, bond strength is high, difficult drop-off, covered effect is better than existing method, and coated treatment temperature is low, workable, is convenient to batch production;
(3) insulating coating has good heat resistance, can the temperature more than 600oC carry out annealing in process and not occur to decompose and destroy;
(4) insulating wrapped layer resistivity is higher, can effectively improve the resistivity of soft-magnetic composite material, significantly reduces the core loss of soft-magnetic composite material.
The specific embodiment
The present invention adopts the butyl titanate with high chemism component to make presoma, glacial acetic acid is made catalyst, ethanol is made solvent, under liquid phase, these raw materials are evenly mixed, and be hydrolyzed, condensation chemical reaction, in solution, form stable vitreosol system, colloidal sol is slowly polymerization through between ageing micelle, the gel that forms three-dimensional space network structure, is further detailed the present invention below in conjunction with embodiment.
Embodiment 1
Get 5mL butyl titanate (TBT) and join in 100mL ethanol, at room temperature stir 30min and obtain precursor solution; Get 5mL distilled water, 10mL glacial acetic acid and 20mL ethanol and mutually mix, when stirring, dropwise join in precursor solution; Then after lasting stirring 1h, obtain the TiO of yellow transparent
2colloidal sol; Solution is under reflux conditions placed in the environment of 80oC until form gel; 20g straight iron powder is sieved and carried out after grain size proportion, iron powder is mixed with the gel that accounts for iron powder weight 2.5%, stir until solvent evaporation is complete magnetic after being coated; Then the magnetic after coated is placed in to the dry 15h of 70oC environment; Again magnetic is placed in the tube furnace of atmosphere of inert gases and heats 5h under 550oC; Magnetic after coated adds the binding agent that accounts for the magnetic quality 0.5% after being coated, and is stirred well to mixture and is dried, mixes under heating condition, and described binding agent is epoxy resin; To being coated in magnetic, adding and account for the releasing agent of coated magnetic gross weight 0.5% and mix, described releasing agent is zinc stearate, obtains magnetic to be formed; Magnetic to be formed is pressed under the pressure of 600MPa to external diameter 23.6mm, internal diameter 14.4mm, the annular soft-magnetic composite material of high 8.89mm; Adopt nitrogen to make protective atmosphere, soft-magnetic composite material is placed in to 400oC environment and is incubated 120min, make soft-magnetic composite material; Surface spraying one deck epoxy resins insulation paint at soft-magnetic composite material, makes finished product, obtains ferrous metals soft-magnetic composite material.
On iron-based soft magnetic composite, adopt wire diameter Ф 0.8mm, the enamel-covered wire coiling 20 circle inductance coils of line length 0.9m, record soft-magnetic composite material electromagnetic performance specific as follows:
(1) soft-magnetic composite material magnetic conductivity: 65;
(2) under 10kHz/1V condition, inductance L=38.5 μ H;
(3) DC stacked performance: 10kHz, during H=100Oe, L
h/ L
o=44.2%;
(4) under 100kHz/1V condition, quality factor q=46;
(5) soft-magnetic composite material loss: during 50kHz/100mT, P
cV=963.6mW/cm
3.
Embodiment 2
Get 10mL butyl titanate (TBT) and join in 120mL ethanol, at room temperature stir 90min and obtain precursor solution; Get 5mL distilled water, 10mL glacial acetic acid and 35mL ethanol and mutually mix, when stirring, dropwise join in precursor solution; Then after lasting stirring 90min, obtain the TiO of yellow transparent
2colloidal sol; Solution is under reflux conditions placed in the environment of 50oC until form gel; 15g Fe-Si-Al magnetic is sieved and carried out after grain size proportion, magnetic is mixed with the gel that accounts for magnetic weight 1.0%, stir until solvent evaporation is complete magnetic after being coated; Then the magnetic after coated is placed in to the dry 20h of 50oC environment; Again magnetic is placed in the tube furnace of atmosphere of inert gases and heats 7h under 500oC; Magnetic after coated adds the binding agent that accounts for the magnetic quality 1.5% after being coated, and is stirred well to mixture and is dried, mixes under heating condition, and described binding agent is phenolic resins; To being coated in magnetic, adding and account for the releasing agent of coated magnetic gross weight 1.0% and mix, described releasing agent is barium stearate and the calcium stearate mixture that 1:1 mixes in mass ratio, obtains magnetic to be formed; Magnetic to be formed is pressed under the pressure of 2000MPa to external diameter 23.6mm, internal diameter 14.4mm, the annular soft-magnetic composite material of high 8.89mm; Adopt argon gas to make protective atmosphere, soft-magnetic composite material is placed in to 600oC environment and is incubated 60min, make soft-magnetic composite material; Surface spraying one deck epoxy resins insulation paint at soft-magnetic composite material, makes finished product, obtains iron sial soft magnetic metal composite.
On iron-silicon-aluminum soft magnet composite, adopt wire diameter Ф 0.8mm, the enamel-covered wire coiling 20 circle inductance coils of line length 0.9m, record soft-magnetic composite material electromagnetic performance specific as follows:
(1) soft-magnetic composite material magnetic conductivity: 96;
(2) under 10kHz/1V condition, inductance L=48.2 μ H;
(3) DC stacked performance: 10kHz, during H=100Oe, L
h/ L
o=41.1%;
(4) under 100kHz/1V condition, quality factor q=67;
(5) soft-magnetic composite material loss: during 50kHz/100mT, P
cV=231.5mW/cm
3.
Embodiment 3
Get 15mL butyl titanate (TBT) and join in 150mL ethanol, at room temperature stir 120min and obtain precursor solution; Get 5mL distilled water, 10mL glacial acetic acid and 30mL ethanol and mutually mix, when stirring, dropwise join in precursor solution; Then after lasting stirring 180min, obtain the TiO of yellow transparent
2colloidal sol; Solution is under reflux conditions placed in the environment of 100oC until form gel; 10g iron nickel magnetic (mass percent of iron, nickel is respectively 50%) is sieved and carried out after grain size proportion, magnetic is mixed with the gel that accounts for magnetic weight 5.0%, stir until solvent evaporation is complete magnetic after being coated; Then the magnetic after coated is placed in to the dry 10h of 100oC environment; Again magnetic is placed in the tube furnace of atmosphere of inert gases and heats 10h under 700oC; To adding the binding agent that accounts for the magnetic mass fraction 2.5% after coated in the magnetic after coated, under heating condition, be stirred well to mixture and be dried, mix, described binding agent is silicones; To being coated in magnetic, adding and account for the releasing agent of coated magnetic gross weight 2.0% and mix, described releasing agent is zinc stearate and the molybdenum bisuphide mixture that 1:1 mixes in mass ratio, obtains magnetic to be formed; Magnetic to be formed is pressed under the pressure of 1600MPa to external diameter 23.6mm, internal diameter 14.4mm, the annular soft-magnetic composite material of high 8.89mm; Adopt nitrogen to make protective atmosphere, soft-magnetic composite material is placed in to 650oC environment and is incubated 30min, make soft-magnetic composite material; Surface spraying one deck epoxy resins insulation paint at soft-magnetic composite material, makes finished product, obtains iron nickel based metal soft-magnetic composite material.
On the Ni-based soft-magnetic composite material of iron, adopt wire diameter Ф 0.8mm, the enamel-covered wire coiling 20 circle inductance coils of line length 0.9m, record soft-magnetic composite material electromagnetic performance specific as follows:
(1) soft-magnetic composite material magnetic conductivity: 156;
(2) under 10kHz/1V condition, inductance L=53.5 μ H;
(3) DC stacked performance: 10kHz, during H=100Oe, L
h/ L
o=74.1%;
(4) under 100kHz/1V condition, quality factor q=83;
(5) soft-magnetic composite material loss: during 50kHz/100mT, P
cV=202.4mW/cm
3.
Claims (4)
1. a high bond strength insulating wrapped processing method for soft magnetic metal composite, is characterized in that, comprises the steps:
1) grain size proportion: carry out grain size proportion after metal magnetic is sieved, described metal magnetic is iron-based magnetic, the silica-based magnetic of iron or the Ni-based magnetic of iron;
2) sol-gal process insulating wrapped: dissolve the butyl titanate of ethanol volume 5 ~ 10% in ethanol, at room temperature stir 30 ~ 120min, obtain precursor solution; Deionized water, glacial acetic acid and ethanol by volume 1:2:4 ~ 1:2:7 mix mutually, when stirring, dropwise join in precursor solution; Then after lasting stirring 60 ~ 180min, obtain the TiO of yellow transparent
2colloidal sol; TiO
2colloidal sol is under reflux conditions placed in the environment of 50 ~ 100oC until form gel; By the gel mix and blend of metal magnetic and metal magnetic weight 1.0 ~ 5.0%, until solvent evaporation is completely, the magnetic after being coated; Then the magnetic after coated is placed in to the dry 10 ~ 20h of 50 ~ 100oC environment; Again the magnetic after coated is placed in the tube furnace of atmosphere of inert gases and heats 5 ~ 10h under 500 ~ 700oC; Magnetic after coated adds the binding agent that accounts for the magnetic quality 0.5 ~ 2.5% after being coated, and is stirred well to mixture and is dried, mixes under heating condition; In magnetic after the most backward being coated, add and account for the releasing agent of the magnetic gross weight 0.5 ~ 2.0% after being coated and mix, obtain magnetic to be formed;
3) compressing: magnetic to be formed is compressing under the pressure of 600 ~ 2000MPa;
4) heat treatment: adopt nitrogen or argon gas to make protective atmosphere, soft-magnetic composite material is placed in to 400 ~ 650oC environment and is incubated 30 ~ 120min;
5) surface spraying: surface spraying one deck epoxy resins insulation paint of the soft-magnetic composite material after step 4) is processed, make finished product, obtain soft magnetic metal composite.
2. the high bond strength insulating wrapped processing method of soft magnetic metal composite according to claim 1, it is characterized in that: the weight of described metal magnetic is 10 ~ 20g, in described precursor solution, the volume of ethanol is 100 ~ 150mL, and the volume of described deionized water is 5 ~ 20 mL.
3. the high bond strength insulating wrapped processing method of soft magnetic metal composite according to claim 1, is characterized in that: described binding agent is phenolic resins, epoxy resin, silicones, poly-ethylene fluoride, melmac, glass powder with low melting point, SiO
2in one or more.
4. the high bond strength insulating wrapped processing method of soft magnetic metal composite according to claim 1, is characterized in that: described releasing agent is one or more in zinc stearate, barium stearate, calcium stearate or molybdenum bisuphide.
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| CN112251648A (en) * | 2020-09-29 | 2021-01-22 | 绵阳西磁科技有限公司 | High-permeability low-loss FeNiMo magnetic powder core and preparation method thereof |
| CN112366057A (en) * | 2020-10-23 | 2021-02-12 | 浙江工业大学 | Organic-inorganic hybrid nano titanate coated metal soft magnetic composite material and preparation method thereof |
| CN112692276B (en) * | 2020-12-09 | 2024-03-08 | 武汉科技大学 | Iron-based antioxidant magnetic composite powder and preparation method thereof |
| CN112692276A (en) * | 2020-12-09 | 2021-04-23 | 武汉科技大学 | Iron-based antioxidant magnetic composite powder and preparation method thereof |
| CN112700959A (en) * | 2020-12-15 | 2021-04-23 | 安徽工业大学 | Compact insulation coating method for metal soft magnetic powder |
| CN112700960A (en) * | 2020-12-15 | 2021-04-23 | 安徽工业大学 | Method for insulating and coating metal soft magnetic powder core and high-strength bonding |
| CN112863799A (en) * | 2020-12-31 | 2021-05-28 | 莱芜职业技术学院 | Iron-based soft magnetic composite material with mesoporous structure coating layer and preparation method thereof |
| CN114220645A (en) * | 2021-12-16 | 2022-03-22 | 宁波磁性材料应用技术创新中心有限公司 | Preparation method of amorphous composite magnetic powder core |
| CN114220645B (en) * | 2021-12-16 | 2024-07-26 | 宁波磁性材料应用技术创新中心有限公司 | Preparation method of amorphous composite magnetic powder core |
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