CN102789860A - Soft magnetic composite with glass xerogel serving as coating layer and method for preparing soft magnetic composite - Google Patents

Soft magnetic composite with glass xerogel serving as coating layer and method for preparing soft magnetic composite Download PDF

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CN102789860A
CN102789860A CN2012103188761A CN201210318876A CN102789860A CN 102789860 A CN102789860 A CN 102789860A CN 2012103188761 A CN2012103188761 A CN 2012103188761A CN 201210318876 A CN201210318876 A CN 201210318876A CN 102789860 A CN102789860 A CN 102789860A
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CN102789860B (en
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武高辉
丁伟
姜龙涛
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention relates to a soft magnetic material and a method for preparing the same, in particular to a soft magnetic composite with glass xerogel serving as a coating layer and a method for preparing the soft magnetic composite. The soft magnetic composite with glass xerogel serving as the coating layer and the method for preparing the soft magnetic composite solve the problems that coefficients of thermal expansion of an inorganic insulating layer and magnetic powder are large in difference and the intrinsic coefficient of thermal expansion of the inorganic insulating layer is unchangeable. The soft magnetic composite with glass xerogel serving as the coating layer is composed of the magnetic powder, a silicon dioxide layer coating the magnetic powder and a glass xerogel layer coating the silicon dioxide layer. The preparation method includes: firstly, preprocessing the magnetic powder; secondly, coating the silicon dioxide layer on the surface of the magnetic powder; thirdly, preparing the glass xerogel; fourthly, coating the glass xerogel layer outside the silicon dioxide layer; fifthly, preparing blanks of the soft magnetic material; and sixthly, preparing the soft magnetic material. The soft magnetic composite with glass xerogel serving as the coating layer and the method for preparing the soft magnetic composite are applicable to the field of switch magnetic resistors, resonance inductors, anti-lock brake sensors, electromagnetic driving devices, brushless direct-current motors, rotary machinery and low-frequency filters.

Description

A kind of is the soft-magnetic composite material and preparation method thereof of coating layer with the glass xerogel
Technical field
The present invention relates to a kind of soft magnetic material and preparation method thereof.
Background technology
Soft-magnetic composite material is meant between magnetic one type of soft magnetic material independent mutually and that couple together through insulating layer material.The outstanding advantage of this soft-magnetic composite material is to have low iron loss and three-dimensional isotropic nature under the AC magnetic field.Therefore can prepare the parts that a lot of conventional soft magnetic materials are difficult to realize, be applied in switching magnetic-resistance, resonant inductance, anti-lock brake sensor, electromagnetic actuator device, brshless DC motor, rotating machinery, fields such as low-frequency filter.The preparation technology of soft-magnetic composite material is normally to metal or alloy Magnaglo surface coated inorganic thing and organic insulating barrier; Or adopt Magnaglo matrix-high resistivity continuous fiber complex method to form the composite soft-magnetic powder, adopt the powder metallurgy compaction process to be prepared into closely knit block soft magnetic material then.Soft-magnetic composite material for existing organic substance coating layer; In its preparation process, need apply pressure greater than 800MPa; Reaching needed compacted density, but satisfy good saturation induction density and magnetic permeability again simultaneously, just need anneal and remove the residual stress of material the soft-magnetic composite material that contains the organic substance coating layer; Because the common non-refractory of organic substance coating layer, so be difficult to effectively remove its residual stress.For the soft-magnetic composite material of existing inorganic matter coating layer, the insulating properties of coating layer does not reach requirement, and the existing coating layer environmental pollution that contains P or S is serious, so SiO occurred using 2, MgO, SiO 2With aqueous mixtures, Al 2O 3Mix with water, ZrO 2Mix with water, the inorganic insulation layer of mica powder and aqueous mixtures preparation is as the inorganic matter coating layer, inorganic insulation layer generally has high-temperature stable, it has overcome the shortcoming of the common non-refractory of organic substance coating layer.But existing inorganic insulation layer also has shortcoming; The own thermal coefficient of expansion that the thermal coefficient of expansion of inorganic insulation layer and magnetic differs big and inorganic insulation layer can not change; Can in magnetic, produce thermal stress at the bigger environment of the temperature difference or in long-time use, cause the soft-magnetic composite material of inorganic matter coating layer can't have good magnetic property.These problems are all restricting the development and the application of soft-magnetic composite material.
Summary of the invention
The present invention will solve in the soft-magnetic composite material of existing inorganic matter coating layer; The thermal coefficient of expansion of inorganic insulation layer and magnetic differs thermal coefficient of expansion big and inorganic insulation layer itself can not be changed, and is the soft-magnetic composite material and preparation method thereof of coating layer with the glass xerogel and provide a kind of.
A kind of with the glass xerogel be the soft-magnetic composite material of coating layer by magnetic, coat the silicon dioxide layer of magnetic and be coated on the outer glass xerogel layer of silicon dioxide layer and form; Wherein, magnetic is a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic.
A kind of is that the preparation method of the soft-magnetic composite material of coating layer accomplishes according to the following steps with the glass xerogel:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that obtains of the ethanol of adding and step 1 is (2 ~ 4): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt again add acidic aqueous solution with the pH value of mixed solution be adjusted to 2 ~ 6 or employing add alkaline aqueous solution the pH value of mixed solution be adjusted to 8 ~ 12, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
A kind of is that the preparation method of the soft-magnetic composite material of coating layer can also accomplish according to the following steps with the glass xerogel:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction finishes; In product, add oleic acid, the mass ratio that adds with magnetic be (0.25 ~ 0.6): to be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution for 1 tetraethoxysilane, use mass percentage concentration; The rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition, reacted 2 hours～4 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that the ethanol of adding and step 1 obtain is (2 ~ 4): 1, and the oleic acid of adding and the mass ratio of magnetic are (0.05 ~ 0.1): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt again add acidic aqueous solution with the pH value of mixed solution be adjusted to 2 ~ 6 or employing add alkaline aqueous solution the pH value of mixed solution be adjusted to 8 ~ 12, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
Advantage of the present invention: the soft-magnetic composite material of the present invention's design has the following advantages:
One, the thermal coefficient of expansion of insulating barrier is adjustable; Controlled significantly change takes place in the thermal coefficient of expansion that can pass through the feasible glass xerogel layer that coats of proportioning of each composition in the adjusting glass; Can itself and magnetic be mated on thermal coefficient of expansion; The maximized thermal stress that in magnetic, produces when soft-magnetic composite material uses under temperature-fall period or the alternating temperature condition after annealing of reducing, and then improved the magnetic property of soft-magnetic composite material;
Two, under greater than glass xerogel layer softening temperature, anneal, can eliminate the internal stress in the soft-magnetic composite material effectively, improved the magnetic property of soft-magnetic composite material;
Three, the annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass; Make that the softening point temperature of glass xerogel layer is adjustable; And the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass xerogel layer, and then the annealing temperature of also having regulated soft-magnetic composite material accordingly.
Description of drawings
Fig. 1 is 200 times electron scanning micrograph of test one soft-magnetic composite material for preparing.
Embodiment
Below provide embodiment of the present invention and be further described, yet technical scheme of the present invention but is not limited to following cited embodiment.
Embodiment one: this execution mode provides a kind of with the glass xerogel be the soft-magnetic composite material of coating layer by magnetic, coat the silicon dioxide layer of magnetic and be coated on the outer glass xerogel layer of silicon dioxide layer and form; Wherein, magnetic is a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic.
It is a kind of that this execution mode provides is the soft-magnetic composite material of coating layer with the glass xerogel, can adjust the composition and the proportioning of glass xerogel layer according to thermal coefficient of expansion.The thermal coefficient of expansion of two kinds of materials in a kind of material does not match, and when variations in temperature, is easy to produce internal stress at material internal, and then makes the magnetic property of soft-magnetic composite material descend.So in the selection of coating layer, will make its thermal coefficient of expansion as far as possible and the matched coefficients of thermal expansion of soft magnetism powder.With the straight iron powder is magnetic, and having coated the preparation soft-magnetic composite material that carries out hot pressing behind the glass colloidal sol is example.The thermal coefficient of expansion of pure iron is 12 * 10 -6/ K, the thermal coefficient of expansion of silicon dioxide is 5.5 * 10 -7/ K, both thermal coefficient of expansions differ very big, so select to significantly improve the component of the oxide of thermal expansion coefficient of glass as glass.With reference to Jie Mujinnafa or high bridge Itou Kentaro method thermal expansion coefficient of glass is designed.With high bridge Itou Kentaro method is example; Thermal expansion additive property coefficient with reference to its common oxide that provides (can be interpreted as simply that here thermal expansion additive property coefficient is big more; It can make the thermal coefficient of expansion increase of glass big more); The oxide that thermal expansion additive property coefficient is bigger has: I A family metal oxide, II A family metal oxide and PbO, and the additive property coefficient of I A family metal oxide is maximum, PbO takes second place.Can confirm SiO according to high bridge Itou Kentaro method 266%, CaO4%, Na 2The thermal expansion coefficient of glass that O30% forms is 12 * 10 -6The thermal coefficient of expansion of/K and pure iron is consistent.Can reach the purpose of the matched coefficients of thermal expansion that in the selection of coating layer, will make its thermal coefficient of expansion and soft magnetism powder.Add I A family metal oxide, II A family metal oxide or PbO and be the effective method of the thermal coefficient of expansion that improves the glass xerogel layer.
It is a kind of that this execution mode provides is the soft-magnetic composite material of coating layer with the glass xerogel, according to softening point the composition and the proportioning of glass xerogel layer is adjusted.Because the glass of high softening-point is unfavorable for the densification of material, and the size of material density is directly connected to the magnetic property height of material; Though the glass of low softening point helps the densification of material,, causes material the material softening distortion when being carried out high annealing again easily.Therefore the glass xerogel layer of glass softening point temperature between 400 ℃ and 900 ℃ meets the demands.
It is a kind of that this execution mode provides is that the soft-magnetic composite material of coating layer has the following advantages with the glass xerogel: the thermal coefficient of expansion of insulating barrier is adjustable; Controlled significantly change takes place in the thermal coefficient of expansion that can pass through the feasible glass xerogel layer that coats of proportioning of each composition in the adjusting glass; Can itself and magnetic be mated on thermal coefficient of expansion; The maximized thermal stress that in magnetic, produces when soft-magnetic composite material uses under temperature-fall period or the alternating temperature condition after annealing of reducing, and then improved the magnetic property of soft-magnetic composite material; Under greater than glass xerogel layer softening temperature, anneal, can eliminate the internal stress in the soft-magnetic composite material effectively, improved the magnetic property of soft-magnetic composite material; The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass; Make that the softening point temperature of glass xerogel layer is adjustable; And the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass xerogel layer, and then the annealing temperature of also having regulated soft-magnetic composite material.
Embodiment two: the difference of this execution mode and embodiment one is: magnetic be Fe powder, Ni powder, Co powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.Other is identical with embodiment one.
The described iron alloy powder of this execution mode is the alloy powder that ferro element and one or more elements are formed; The mass fraction maximum that iron is shared, wherein iron alloy powder can be a kind of or wherein several kinds the combination in Fe-Si-Al powder, Fe-Ni-Mo powder, Fe-Ni powder, Fe-Cu-Nb-Si-B powder, Fe-Pt powder, Fe-Ni-Cr powder, Fe-Zn powder, La-Co-Fe powder, Pb-Fe powder, W-Ni-Fe powder and the Zr-Ni-Sn-Fe powder.
The described nickel alloy powder of this execution mode is the alloy powder that nickel element and one or more elements are formed, the mass fraction maximum that nickel is shared, and wherein nickel alloy powder can be 35%～90% permalloy powder for the shared mass fraction of nickel.
The described cobalt alloy powder of this execution mode is the alloy powder that cobalt and one or more elements are formed, the mass fraction maximum that cobalt is shared, and wherein the cobalt alloy powder can be the Fe-Co-V powder.
Embodiment three: it is a kind of that this execution mode provides is the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, specifically accomplishes according to the following steps:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that obtains of the ethanol of adding and step 1 is (2 ~ 4): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt again add acidic aqueous solution with the pH value of mixed solution be adjusted to 2 ~ 6 or employing add alkaline aqueous solution the pH value of mixed solution be adjusted to 8 ~ 12, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
The thickness that outside magnetic, coats silicon dioxide layer that this execution mode step 2 obtains is 50nm ~ 150nm.
The described dried solid of this execution mode step 2 uses electromagnet to carry out method for screening: when iron powder is blown afloat with air blast; Utilize electromagnet to coating the active force of magnetic; To coat magnetic and carry out postsearch screening; The silica xerogel that does not have magnetic is blown out, and has reached the purpose of screening.
The a kind of of this execution mode preparation is the soft-magnetic composite material of coating layer with the glass xerogel, can adjust the composition and the proportioning of glass xerogel layer according to thermal coefficient of expansion.The thermal coefficient of expansion of two kinds of materials in a kind of material does not match, and when variations in temperature, is easy to produce internal stress at material internal, and then makes the magnetic property of soft-magnetic composite material descend.So in the selection of coating layer, will make its thermal coefficient of expansion as far as possible and the matched coefficients of thermal expansion of soft magnetism powder.With the straight iron powder is magnetic, and having coated the preparation soft-magnetic composite material that carries out hot pressing behind the glass colloidal sol is example.The thermal coefficient of expansion of pure iron is 12 * 10 -6/ K, the thermal coefficient of expansion of silicon dioxide is 5.5 * 10 -7/ K, both thermal coefficient of expansions differ very big, so select to significantly improve the component of the oxide of thermal expansion coefficient of glass as glass.With reference to Jie Mujinnafa or high bridge Itou Kentaro method thermal expansion coefficient of glass is designed.With high bridge Itou Kentaro method is example; Thermal expansion additive property coefficient with reference to its common oxide that provides (can be interpreted as simply that here thermal expansion additive property coefficient is big more; It can make the thermal coefficient of expansion increase of glass big more); The oxide that thermal expansion additive property coefficient is bigger has: I A family metal oxide, II A family metal oxide and PbO, and the additive property coefficient of I A family metal oxide is maximum, PbO takes second place.Can confirm SiO according to high bridge Itou Kentaro method 266%, CaO4%, Na 2The thermal expansion coefficient of glass that O30% forms is 12 * 10 -6The thermal coefficient of expansion of/K and pure iron is consistent.Can reach the purpose of the matched coefficients of thermal expansion that in the selection of coating layer, will make its thermal coefficient of expansion and soft magnetism powder.Add I A family metal oxide, II A family metal oxide or PbO and be the effective method of the thermal coefficient of expansion that improves the glass xerogel layer.
The a kind of of this execution mode preparation is the soft-magnetic composite material of coating layer with the glass xerogel, can adjust the composition and the proportioning of glass xerogel layer according to softening point.Because the glass of high softening-point is unfavorable for the densification of material, and the size of material density is directly connected to the magnetic property height of material; Though the glass of low softening point helps the densification of material,, causes material the material softening distortion when being carried out high annealing again easily.Therefore the glass xerogel layer of glass softening point temperature between 400 ℃ and 900 ℃ meets the demands.
The soft-magnetic composite material of this execution mode preparation has the following advantages: the thermal coefficient of expansion of insulating barrier is adjustable; Controlled significantly change takes place in the thermal coefficient of expansion that can pass through the feasible glass xerogel layer that coats of proportioning of each composition in the adjusting glass; Can itself and magnetic be mated on thermal coefficient of expansion; The maximized thermal stress that in magnetic, produces when soft-magnetic composite material uses under temperature-fall period or the alternating temperature condition after annealing of reducing, and then improved the magnetic property of soft-magnetic composite material; Under greater than glass xerogel layer softening temperature, anneal, can eliminate the internal stress in the soft-magnetic composite material effectively, improved the magnetic property of soft-magnetic composite material; The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass; Make that the softening point temperature of glass xerogel layer is adjustable; And the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass xerogel layer, and then the annealing temperature of also having regulated soft-magnetic composite material.
Embodiment four: the difference of this execution mode and embodiment three is: the described magnetic of step 1 be Fe powder, Ni powder, Co powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.Other is identical with embodiment three
The described iron alloy powder of this execution mode is the alloy powder that ferro element and one or more elements are formed; The mass fraction maximum that iron is shared, wherein iron alloy powder can be a kind of or wherein several kinds the combination in Fe-Si-Al powder, Fe-Ni-Mo powder, Fe-Ni powder, Fe-Cu-Nb-Si-B powder, Fe-Pt powder, Fe-Ni-Cr powder, Fe-Zn powder, La-Co-Fe powder, Pb-Fe powder, W-Ni-Fe powder and the Zr-Ni-Sn-Fe powder.
The described nickel alloy powder of this execution mode is the alloy powder that nickel element and one or more elements are formed, the mass fraction maximum that nickel is shared, and wherein nickel alloy powder can be 35%～90% permalloy powder for the shared mass fraction of nickel.
The described cobalt alloy powder of this execution mode is the alloy powder that cobalt and one or more elements are formed, the mass fraction maximum that cobalt is shared, and wherein the cobalt alloy powder can be the Fe-Co-V powder.
Embodiment five: this execution mode and embodiment three or four difference are: the described cleaning agent of step 1 is acetone or concentration expressed in percentage by volume greater than 95% ethanol.Other is identical with embodiment three or four.
Embodiment six: it is a kind of that this execution mode provides is the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, specifically accomplishes according to the following steps:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction finishes; In product, add oleic acid, the mass ratio that adds with magnetic be (0.25 ~ 0.6): to be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution for 1 tetraethoxysilane, use mass percentage concentration; The rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition, reacted 2 hours～4 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that the ethanol of adding and step 1 obtain is (2 ~ 4): 1, and the oleic acid of adding and the mass ratio of magnetic are (0.05 ~ 0.1): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt again add acidic aqueous solution with the pH value of mixed solution be adjusted to 2 ~ 6 or employing add alkaline aqueous solution the pH value of mixed solution be adjusted to 8 ~ 12, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
The thickness at magnetic coated silica layer that this execution mode step 2 obtains is 150nm ~ 500nm.
The described dried solid of this execution mode step 2 uses electromagnet to carry out method for screening: when iron powder is blown afloat with air blast; Utilize electromagnet to coating the active force of magnetic; To coat magnetic and carry out postsearch screening; The silica xerogel that does not have magnetic is blown out, and has reached the purpose of screening.
It is a kind of that this execution mode provides is the soft-magnetic composite material of coating layer with the glass xerogel, can adjust the composition and the proportioning of glass xerogel layer according to thermal coefficient of expansion.The thermal coefficient of expansion of two kinds of materials in a kind of material does not match, and when variations in temperature, is easy to produce internal stress at material internal, and then makes the magnetic property of soft-magnetic composite material descend.So in the selection of coating layer, will make its thermal coefficient of expansion as far as possible and the matched coefficients of thermal expansion of soft magnetism powder.With the straight iron powder is magnetic, and having coated the preparation soft-magnetic composite material that carries out hot pressing behind the glass colloidal sol is example.The thermal coefficient of expansion of pure iron is 12 * 10 -6/ K, the thermal coefficient of expansion of silicon dioxide is 5.5 * 10 -7/ K, both thermal coefficient of expansions differ very big, so when selecting the component of glass, should select those oxides that can significantly improve thermal expansion coefficient of glass, with reference to Jie Mujinnafa or high bridge Itou Kentaro method thermal expansion coefficient of glass are designed.With high bridge Itou Kentaro method is example; Thermal expansion additive property coefficient with reference to its common oxide that provides (can be interpreted as simply that here thermal expansion additive property coefficient is big more; It can make the thermal coefficient of expansion increase of glass big more); The oxide that thermal expansion additive property coefficient is bigger has: I A family metal oxide, II A family metal oxide and PbO, and the additive property coefficient of I A family metal oxide is maximum, PbO takes second place.Can estimate SiO according to high bridge Itou Kentaro method 266%, CaO4%, Na 2The thermal expansion coefficient of glass that O30% forms is 12 * 10 -6Thermal coefficient of expansion with pure iron about/K matees basically.So can design the soft-magnetic composite material of multiple coating glass xerogel layer.The common glass forming substance and the thermal coefficient of expansion of intermediate oxide are all quite low, and to add I A family, II A family oxide or PbO be effective method as improving its thermal coefficient of expansion.
It is a kind of that this execution mode provides is the soft-magnetic composite material of coating layer with the glass xerogel, according to softening point the composition and the proportioning of glass xerogel layer is adjusted.Because the glass of high softening-point is unfavorable for the densification of material, and the size of material density is directly connected to the magnetic property height of material; Though the glass of low softening point helps the densification of material,, causes material the material softening distortion when being carried out high annealing again easily.Therefore the glass xerogel layer of glass softening point temperature between 400 ℃ and 900 ℃ meets the demands.
The soft-magnetic composite material of this execution mode preparation has the following advantages: the thermal coefficient of expansion of insulating barrier is adjustable; Controlled significantly change takes place in the thermal coefficient of expansion that can pass through the feasible glass xerogel layer that coats of proportioning of each composition in the adjusting glass; Can itself and magnetic be mated on thermal coefficient of expansion; The maximized thermal stress that in magnetic, produces when soft-magnetic composite material uses under temperature-fall period or the alternating temperature condition after annealing of reducing, and then improved the magnetic property of soft-magnetic composite material; Under greater than glass xerogel layer softening temperature, anneal, can eliminate the internal stress in the soft-magnetic composite material effectively, improved the magnetic property of soft-magnetic composite material; The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass; Make that the softening point temperature of glass xerogel layer is adjustable; And the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass xerogel layer, and then the annealing temperature of also having regulated soft-magnetic composite material.
Embodiment seven: the difference of this execution mode and embodiment six is: the described magnetic of step 1 be Fe powder, Ni powder, Co powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.Other and embodiment six phase are together.
The described iron alloy powder of this execution mode is the alloy powder that ferro element and one or more elements are formed; The mass fraction maximum that iron is shared, wherein iron alloy powder can be a kind of or wherein several kinds the combination in Fe-Si-Al powder, Fe-Ni-Mo powder, Fe-Ni powder, Fe-Cu-Nb-Si-B powder, Fe-Pt powder, Fe-Ni-Cr powder, Fe-Zn powder, La-Co-Fe powder, Pb-Fe powder, W-Ni-Fe powder and the Zr-Ni-Sn-Fe powder.
The described nickel alloy powder of this execution mode is the alloy powder that nickel element and one or more elements are formed, the mass fraction maximum that nickel is shared, and wherein nickel alloy powder can be 35%～90% permalloy powder for the shared mass fraction of nickel.
The described cobalt alloy powder of this execution mode is the alloy powder that cobalt element and one or more elements are formed, the mass fraction maximum that cobalt is shared, and wherein the cobalt alloy powder can be the Fe-Co-V powder.
Embodiment eight: this execution mode and embodiment six or seven difference are: the described cleaning agent of step 1 is acetone or concentration expressed in percentage by volume greater than 95% ethanol.Other is identical with embodiment six or seven.Other is identical with embodiment six or seven
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of is the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, specifically accomplishes according to the following steps:
One, the ATOMET_1001HP water-atomized iron powder 150g with Quebec, CAN metal dust Co., Ltd puts into ethanol; With the ultrasonic 10min of the frequency of 30KHz; Filtration obtains iron powder, adds ethanol 660mL and oleic acid 10.72g (12mL) therein, and to be 25% ammoniacal liquor be adjusted to 9 with the pH value of solution to the service quality percentage concentration; Rotating speed with 800r/min stirred 1.5 hours, obtained solidliquid mixture;
Two, in the solidliquid mixture that step 1 obtains, add ethanol 2340mL, to use mass percentage concentration be 25% ammoniacal liquor is adjusted to 9 with the pH value of solution, stirs with the rotating speed of 800r/min, by the tetraethoxysilane of 2 adding equivalent; Each 1 hour at interval, the gross mass of the tetraethoxysilane of adding was 44.64g (48mL), after all adding, reacted 2 hours; Reaction is left standstill 20min after accomplishing, and outwells solution, and the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 60 ℃; Dry 300min screens dried solid with electromagnet, promptly obtain the iron powder of coated silica layer;
Three, in the tetraethoxysilane of 23.25g (25mL), add 5mL deionized water, 25mL ethanol, at room temperature,, stir 30min with the mixing speed of 300r/min, obtain organizator solution; To the mass percent concentration of 30mL is in the ethanolic solution of 10% caustic alcohol, adds the Ca (NO of 30mL ethanol, 2.5g 3) 24H 2O obtains solution of additive; Organizator solution is mixed with solution of additive, and to add mass percent concentration be 25% ammoniacal liquor that the pH value of solution is transferred to 9 with the rate of addition of 1mL/min, and with the mixing speed of 300r/min, stirring 180min promptly obtains glass colloidal sol again;
Four, the iron powder with the coated silica layer of 145g is deposited in the surface plate naturally; The even glass colloidal sol of Dropwise 5 mL on the surface of the iron powder of coated silica layer; Put into drying baker,, promptly obtain outside silicon dioxide layer, coating the iron powder of glass xerogel layer at 60 ℃ of dry 120min;
Five, with the cladding iron powder that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 800MPa, constant voltage 2min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 700 ℃ from room temperature with the heating rate of 2 ℃/min, constant temperature 60min, the rate of temperature fall with 2 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
The soft-magnetic composite material that obtains is carried out sem observation; Obtain Fig. 1; Fig. 1 is 200 times electron scanning micrograph of test one soft-magnetic composite material for preparing; The part that from Fig. 1, can observe black crackle shape is an insulating barrier, and the white portion that is being coated by the black crackle is an iron powder, can show and prepare soft-magnetic composite material.
The electromagnetic performance and the mechanical property of this kind soft-magnetic composite material are as shown in table 1.
The electromagnetic performance and the mechanical performance index of the soft-magnetic composite material of table 1 test one preparation
Figure BDA00002085997400141
In the table 1, μ mMaximum permeability for soft-magnetic composite material; B 5000The magnetic flux density value of soft-magnetic composite material when the expression magnetizing field is 5000A/m; Br representes residual magnetic flux density; Hc representes coercive force; W (50Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 50Hz; W (200Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 200Hz; TRS representes cross-breaking strength.
Test two: a kind of is the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, specifically accomplishes according to the following steps:
One, the ATOMET_1001HP water-atomized iron powder 150g with Quebec, CAN metal dust Co., Ltd puts into ethanol; With the ultrasonic 10min of the frequency of 30KHz; Filtration obtains iron powder, adds ethanol 660mL and oleic acid 10.72g (12mL) therein, and to be 25% ammoniacal liquor be adjusted to 9 with the pH value of solution to the service quality percentage concentration; Rotating speed with 800r/min stirred 1.5 hours, obtained solidliquid mixture;
Two, in the solidliquid mixture that step 1 obtains, add ethanol 2340mL, to use mass percentage concentration be 25% ammoniacal liquor is adjusted to 9 with the pH value of solution, stirs with the rotating speed of 800r/min, by the tetraethoxysilane of 2 adding equivalent; Each 1 hour at interval, the gross mass of the tetraethoxysilane of adding was 44.64g (48mL), after all adding, reacted 2 hours; Reaction is left standstill 20min after accomplishing, and outwells solution, and the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 60 ℃; Dry 300min screens dried solid with electromagnet, promptly obtain the iron powder of coated silica layer;
Three, in the tetraethoxysilane of 23.25g (25mL), add 5mL deionized water, 25mL ethanol, at room temperature,, stir 30min with the mixing speed of 300r/min, obtain organizator solution; To the mass percent concentration of 30mL is in the ethanolic solution of 10% caustic alcohol, and the mass percent concentration that adds 10mL is that the mass percent concentration of methanol solution, the 10mL of 5% calcium methoxide is 5% aluminium secondary butylate Al (OC 4H 9) 3Ethanolic solution, with the mixing speed of 400r/min, stir 30min, obtain solution of additive; Organizator solution is mixed with solution of additive, and to add mass percent concentration be 10% aqueous hydrochloric acid solution that the pH value of solution is adjusted to 4 with the rate of addition of 1mL/min, and with the mixing speed of 300r/min, stirring 120min promptly obtains glass colloidal sol again;
Four, the iron powder with the coated silica layer of 140g is deposited in the surface plate naturally; Evenly drip the glass colloidal sol of 8mL on the surface of the iron powder of coated silica layer; Put into drying baker,, promptly obtain outside silicon dioxide layer, coating the iron powder of glass xerogel layer at 70 ℃ of dry 120min;
Five, with the cladding iron powder that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 1000MPa, constant voltage 2.5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 750 ℃ from room temperature with the heating rate of 2 ℃/min, constant temperature 60min, the rate of temperature fall with 2 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
The electromagnetic performance and the mechanical property of this kind soft-magnetic composite material are as shown in table 2.
The electromagnetic performance and the mechanical performance index of the soft-magnetic composite material of table 2 test two preparations
Figure BDA00002085997400151
In the table 2, μ mMaximum permeability for soft-magnetic composite material; B 5000The magnetic flux density value of soft-magnetic composite material when the expression magnetizing field is 5000A/m; Br representes residual magnetic flux density; Hc representes coercive force; W (50Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 50Hz; W (200Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 200Hz; TRS representes cross-breaking strength.
Test three: a kind of is the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, specifically accomplishes according to the following steps:
One, the reduced iron powder 150g that the Tianjin roc is reached chemical industry Co., Ltd puts into ethanol; With the ultrasonic 10min of the frequency of 30KHz; Filtration obtains iron powder, adds ethanol 660mL and oleic acid 10.72g (12mL) therein, and to be 25% ammoniacal liquor be adjusted to 9 with the pH value of solution to the service quality percentage concentration; Rotating speed with 700r/min stirred 1.5 hours, obtained solidliquid mixture;
Two, in the solidliquid mixture that step 1 obtains, add ethanol 2340mL, to use mass percentage concentration be 25% ammoniacal liquor is adjusted to 9 with the pH value of solution, stirs with the rotating speed of 700r/min; By the tetraethoxysilane of 2 adding equivalent, each 1 hour at interval, the gross mass of the tetraethoxysilane of adding was 44.64g (48mL); After all adding, reacted 2 hours, after reaction finishes; In product, add oleic acid 12.06g (13.5mL); Add tetraethoxysilane 69.75g (75mL), to use mass percentage concentration be 25% ammoniacal liquor is adjusted to 9 with the pH value of solution, stirs at the rotating speed with 700r/min; Reacted 2 hours, and promptly obtained solidliquid mixture at magnetic surface coated silica layer; Leave standstill 20min, outwell solution, the solid that obtains is cleaned, filter, will clean the back solid and put into drying box, temperature is 60 ℃, and dry 300min screens dried solid with electromagnet, promptly obtain the iron powder of coated silica layer;
Three, in the tetraethoxysilane of 23.25g (25mL), add 5mL deionized water, 25mL ethanol, at room temperature,, stir 30min with the mixing speed of 300r/min, obtain organizator solution; To the mass percent concentration of 30mL is in the ethanolic solution of 10% caustic alcohol, with the mixing speed of 400r/min, stirs 30min, obtains solution of additive; Organizator solution is mixed with solution of additive, with the mixing speed of 300r/min, stir 120min again, promptly obtain glass colloidal sol;
Four, the iron powder with the coated silica layer of 140g is deposited in the surface plate naturally; Evenly drip the glass colloidal sol of 8mL on the surface of the iron powder of coated silica layer; Put into drying baker,, promptly obtain outside silicon dioxide layer, coating the iron powder of glass xerogel layer at 70 ℃ of dry 120min;
Five, with the cladding iron powder that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 950MPa, constant voltage 2.5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ from room temperature with the heating rate of 2 ℃/min, constant temperature 60min, the rate of temperature fall with 2 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
The electromagnetic performance and the mechanical property of this kind soft-magnetic composite material are as shown in table 3.
The electromagnetic performance and the mechanical performance index of the soft-magnetic composite material of table 3 test three preparations
Figure BDA00002085997400171
In the table 3, μ mMaximum permeability for soft-magnetic composite material; B 5000The magnetic flux density value of soft-magnetic composite material when the expression magnetizing field is 5000A/m; Br representes residual magnetic flux density; Hc representes coercive force; W (50Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 50Hz; W (200Hz) be soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 200Hz; TRS representes cross-breaking strength.

Claims (8)

1. one kind is the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that soft-magnetic composite material by magnetic, coat the silicon dioxide layer of magnetic and be coated on the outer glass xerogel layer of silicon dioxide layer and form; Wherein, magnetic is a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic.
2. according to claim 1 a kind of be the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that magnetic be iron powder, nickel powder, cobalt powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.
3. as claimed in claim 1 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that a kind of is that the preparation method of the soft-magnetic composite material of coating layer accomplishes according to the following steps with the glass xerogel:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that obtains of the ethanol of adding and step 1 is (2 ~ 4): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt acidic aqueous solution that the pH value of mixed solution is adjusted to 2 ~ 6 or adopt alkaline aqueous solution that the pH value of mixed solution is adjusted to 8 ~ 12 again, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
4. according to claim 3 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that the described magnetic of step 1 be iron powder, nickel powder, cobalt powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.
5. according to claim 3 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that the described cleaning agent of step 1 is acetone or concentration expressed in percentage by volume greater than 95% ethanol.
6. as claimed in claim 1 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that the preparation method of soft-magnetic composite material accomplishes according to the following steps:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains clean magnetic; In clean magnetic, add ethanol and oleic acid; To be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution to the service quality percentage concentration, stirred 1 h ~ 2 hours with ultrasonic dispersion 1 h ~ of the frequency of 24KHz ~ 35KHz 2 hours or with the rotating speed of 600r/min ~ 1200r/min, obtains solidliquid mixture;
Wherein, The mass ratio of oleic acid and magnetic is (0.03 ~ 0.2): 1; The volume ratio of oleic acid and ethanol is 1: (40 ~ 75), magnetic are a kind of or wherein several kinds the combination in the metal powder with magnetic, the metal alloy powder with magnetic and the metallic compound powder with magnetic;
Two, in the solidliquid mixture that step 1 obtains, add ethanol, to use mass percentage concentration be 20% ~ 30% ammoniacal liquor is adjusted to 8.5～9.5 with the pH value of solution, the rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition; Divide the tetraethoxysilane that adds equivalent for 2 ~ 4 times, each 0.5 h ~ at interval 1.5 hours, the gross mass of the tetraethoxysilane of adding and the mass ratio of magnetic are (0.25 ~ 0.4): 1; After all adding, reacted 0.5 h ~ 1.5 hours, after reaction finishes; In product, add oleic acid, the mass ratio that adds with magnetic be (0.25 ~ 0.6): to be 20% ~ 30% ammoniacal liquor be adjusted to 8.5～9.5 with the pH value of solution for 1 tetraethoxysilane, use mass percentage concentration; The rotating speed with 600r/min ~ 1200r/min stir with the pH value be under 8.5～9.5 the condition, reacted 2 hours～4 hours, after reaction is accomplished; Leave standstill 10min～30min, outwell solution, the solid that obtains is cleaned; Filter, will clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃; Dry 20min ~ 360min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Wherein, the volume ratio of the solidliquid mixture that the ethanol of adding and step 1 obtain is (2 ~ 4): 1, and the oleic acid of adding and the mass ratio of magnetic are (0.05 ~ 0.1): 1;
Three, the organizator compound is dissolved in alcoholic solvent, obtains organizator solution; With a kind of in additive compound and the inorganic salts or wherein several kinds combination be dissolved in solvent, obtain solution of additive; Organizator solution is (0.2 ~ 2) by volume with solution of additive: 1 mixes, and under 15 ℃～65 ℃ temperature, with the mixing speed of 180r/min ~ 600r/min, continuous stirring 10min～120min obtains mixed solution; Adopt again add acidic aqueous solution with the pH value of mixed solution be adjusted to 2 ~ 6 or employing add alkaline aqueous solution the pH value of mixed solution be adjusted to 8 ~ 12, promptly obtain glass colloidal sol; Wherein, the organizator compound is boric acid, phosphoric acid, Ge (OC 3H 7) 4, Ti (OC 2H 5) 4, Al (OC 4H 9) 3, Si (OCH 3) 4And Si (OC 2H 5) 4In a kind of or wherein several kinds combination; Alcoholic solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol and the propyl alcohol; Additive compound is for meeting chemical general formula M (OR) xCompound in a kind of or wherein several kinds combination, M is Si, Ti, Be, Mn, In, Ge, Al, Zr, Na, K, Li, Mg, Ca, Mg or Ba, R is C nH 2n+1And n is 1,2,3,4 or 5, and x is 1～5 and M (OR) xCompound be electric neutrality; Inorganic salts are NaNO 3Or Ca (NO 3) 24H 2The combination of one or both among the O; Solvent is a kind of or wherein several kinds the combination in methyl alcohol, ethanol, ethylene glycol, third alcohol and water; Acidic aqueous solution is a kind of or wherein several kinds the combination in aqueous hydrochloric acid solution, aqueous solution of nitric acid and the aqueous acetic acid; Alkaline aqueous solution is an ammoniacal liquor; The gross mass of organizator compound is (50g ~ 700g): 1L with the ratio of the volume of alcoholic solvent; A kind of in additive compound and the inorganic salts or wherein several kinds the ratio of gross mass and the volume of solvent of combination be (10g ~ 600g): 1L; The mass percent concentration of acidic aqueous solution is 1% ~ 20%; The mass percent concentration of alkaline aqueous solution is 10% ~ 30%;
In the magnetic of the coated silica layer that four, in step 2, obtains, drip the glass colloidal sol that obtains in the step 3, after the mixing, under 40 ℃ ~ 100 ℃, dry 60min ~ 500min promptly obtains outside silicon dioxide layer, coating the magnetic of glass xerogel layer;
Wherein, the quality of the magnetic of coated silica layer is (8kg ~ 40kg): 1L with the ratio of the volume of glass colloidal sol;
Five, with the magnetic that outside silicon dioxide layer, coats the glass xerogel layer that obtains in the step 4, put into mould, at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains the blank of soft-magnetic composite material;
Six, the blank with the soft-magnetic composite material that obtains in the step 5 is 10 in vacuum degree -1Under the condition of Pa, be warmed up to 500 ℃ ~ 1000 ℃ from room temperature with the heating rate of 1 ℃/min ~ 5 ℃/min, constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing, obtains soft-magnetic composite material.
7. according to claim 6 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that the described magnetic of step 1 be iron powder, nickel powder, cobalt powder, iron alloy powder, nickel alloy powder, cobalt alloy powder, oxides-containing iron powder, nickeliferous oxidate powder and contain a kind of in the cobalt/cobalt oxide powder or wherein several kinds combination and have magnetic.
8. according to claim 6 a kind of be the preparation method of the soft-magnetic composite material of coating layer with the glass xerogel, it is characterized in that the described cleaning agent of step 1 is acetone or concentration expressed in percentage by volume greater than 95% ethanol.
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