CN102789863A - Soft magnetic composite material taking glass powder as coating layer and preparation method of soft magnetic composite material - Google Patents
Soft magnetic composite material taking glass powder as coating layer and preparation method of soft magnetic composite material Download PDFInfo
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- CN102789863A CN102789863A CN2012103189209A CN201210318920A CN102789863A CN 102789863 A CN102789863 A CN 102789863A CN 2012103189209 A CN2012103189209 A CN 2012103189209A CN 201210318920 A CN201210318920 A CN 201210318920A CN 102789863 A CN102789863 A CN 102789863A
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- 239000011521 glass Substances 0.000 title claims abstract description 189
- 239000002131 composite material Substances 0.000 title claims abstract description 149
- 239000000843 powder Substances 0.000 title claims abstract description 136
- 239000011247 coating layer Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 42
- 239000010410 layer Substances 0.000 claims abstract description 100
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 93
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 46
- 239000011248 coating agent Substances 0.000 claims abstract description 39
- 238000000576 coating method Methods 0.000 claims abstract description 39
- 238000000137 annealing Methods 0.000 claims abstract description 36
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 239000000428 dust Substances 0.000 claims description 133
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 80
- 239000000203 mixture Substances 0.000 claims description 75
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 65
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 29
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 28
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 28
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 28
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 28
- 239000005642 Oleic acid Substances 0.000 claims description 28
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 28
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 24
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 18
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- 239000002184 metal Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 229910000531 Co alloy Inorganic materials 0.000 claims description 12
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 12
- 229910017052 cobalt Inorganic materials 0.000 claims description 12
- 239000010941 cobalt Substances 0.000 claims description 12
- 238000010348 incorporation Methods 0.000 claims description 12
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 10
- 239000012459 cleaning agent Substances 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 229910000765 intermetallic Inorganic materials 0.000 claims description 9
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- 239000002245 particle Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000003980 solgel method Methods 0.000 claims description 7
- GSOLWAFGMNOBSY-UHFFFAOYSA-N cobalt Chemical compound [Co][Co][Co][Co][Co][Co][Co][Co] GSOLWAFGMNOBSY-UHFFFAOYSA-N 0.000 claims description 6
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 claims description 6
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- 239000000126 substance Substances 0.000 description 4
- 229910020598 Co Fe Inorganic materials 0.000 description 3
- 229910002519 Co-Fe Inorganic materials 0.000 description 3
- 229910020516 Co—V Inorganic materials 0.000 description 3
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 3
- 229910003271 Ni-Fe Inorganic materials 0.000 description 3
- 229910003296 Ni-Mo Inorganic materials 0.000 description 3
- 229910018487 Ni—Cr Inorganic materials 0.000 description 3
- 229910052774 Proactinium Inorganic materials 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910002796 Si–Al Inorganic materials 0.000 description 3
- 229910008423 Si—B Inorganic materials 0.000 description 3
- 229910020900 Sn-Fe Inorganic materials 0.000 description 3
- 229910019314 Sn—Fe Inorganic materials 0.000 description 3
- 238000005253 cladding Methods 0.000 description 3
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Abstract
The invention relates to a soft magnetic composite material taking glass powder as a coating layer and a preparation method of the soft magnetic composite material, relating to the soft magnetic material and the preparation method thereof. In the invention, the problem that in the traditional soft magnetic composite material of an inorganic coating layer, excellent mechanical property of the soft magnetic composite material and excellent magnetic property of the soft magnetic composite material resulting from an annealing mean can not coexist, and the difference of coefficients of thermal expansion between an inorganic insulating layer and magnetic powder is greater is solved. The soft magnetic composite material taking the glass powder as the coating layer consists of the magnetic powder, a silicon dioxide layer coated by the magnetic powder and a glass powder layer coated outside the silicon dioxide layer. The preparation method comprises the following steps: firstly, pre-treating the magnetic powder; secondly, coating the silicon dioxide layer on the surface of the magnetic powder; thirdly, coating the glass powder layer outside the silicon dioxide layer; fourthly, preparing a blank material; and fifthly, annealing the blank material. The soft magnetic composite material taking the glass powder as the coating layer and the preparation method of the soft magnetic composite material are applied to the fields of switch magnetic resistance, resonance inductance, anti-lock brake sensors, electromagnetic driving devices, brushless direct current motors, rotating machinery and low-frequency filters.
Description
Technical field
The present invention relates to 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 associativity of magnetic and inorganic insulation layer is bad; The residual stress of effectively removing in the preparation process through the method for annealing can cause the mechanical property of soft-magnetic composite material relatively poor, and the cross-breaking strength of the soft-magnetic composite material that existing inorganic matter coats is less than 70MPa; Simultaneously, the thermal coefficient of expansion of inorganic insulation layer and magnetic differs bigger, can in magnetic, produce thermal stress at the bigger environment of the temperature difference or in long-time use, causes 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; Effectively remove cross-breaking strength that residual stress in the preparation process causes existing soft-magnetic composite material again through the method for annealing and differ bigger problem, and provide with glass dust as soft-magnetic composite material of coating layer and preparation method thereof less than the thermal coefficient of expansion of 70MPa and inorganic insulation layer and magnetic.
Form by the silicon dioxide layer of magnetic, coating magnetic and the glass frit layer that is coated on outside the silicon dioxide layer as the soft-magnetic composite material of coating layer with glass dust; 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.
Preparation method as the soft-magnetic composite material of coating layer accomplishes according to the following steps with glass dust: one, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains magnetic; Add ethanol and oleic acid therein; 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; Stir 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, obtain 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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, the solidliquid mixture that reaction is obtained leaves standstill 10min ~ 30min; Outwell solution, the solid that obtains is cleaned, filter; To clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃, dry 20min ~ 360min; Dried solid is screened 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, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, the mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1; Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer; Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature, constant temperature 30min ~ 180min, and the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards; Promptly accomplish annealing, obtain with the soft-magnetic composite material of glass dust as coating layer; Wherein heat treatment temperature is 500 ℃ ~ 1000 ℃.
Preparation method as the soft-magnetic composite material of coating layer accomplishes according to the following steps with glass dust: one, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains magnetic; Add ethanol and oleic acid therein; 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; Stir 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, obtain 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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; Stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition, reacts 2 hours～4 hours, and the solidliquid mixture that reaction is obtained leaves 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, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, the mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1; Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer; Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature, constant temperature 30min ~ 180min, and the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards; Promptly accomplish annealing, obtain with the soft-magnetic composite material of glass dust as coating layer; Wherein heat treatment temperature is 500 ℃ ~ 1000 ℃.
Advantage of the present invention: the present invention design with the soft-magnetic composite material of glass dust as coating layer, have 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 frit layer that coats of proportioning of each composition in the adjusting glass dust; 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 the glass frit 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; Simultaneously; Material can experience in annealing process greater than the temperature of glass frit layer softening temperature, so magnetic and coating layer to combine no longer be simple mechanical bond, but a kind of diffusion-bonded; Therefore also improved the mechanical property of soft-magnetic composite material, made the cross-breaking strength of soft-magnetic composite material greater than 90MPa.
Three, the annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass dust; Make that the softening point temperature of glass frit layer is adjustable; And the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass frit 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 iron powder in the test one.
Fig. 2 is 50000 times electron scanning micrograph of glass dust in the test one.
Fig. 3 is for coating 200 times electron scanning micrograph of the coating magnetic of glass frit layer outside silicon dioxide layer in the test one.
Fig. 4 for the test one the preparation with the metallograph of glass dust as the soft-magnetic composite material of coating layer.
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: what this execution mode provided is made up of the silicon dioxide layer of magnetic, coating magnetic and the glass frit layer that is coated on outside the silicon dioxide layer as the soft-magnetic composite material of coating layer with glass dust; 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.
This execution mode provide with the soft-magnetic composite material of glass dust as coating layer, can adjust the composition and the proportioning of glass frit 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 dust 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 glass dust thermal coefficient of expansion as glass dust.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 dust 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 glass dust thermal coefficient of expansion 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 glass frit layer.
This execution mode provide with the soft-magnetic composite material of glass dust as coating layer, according to softening point the composition and the proportioning of glass frit layer are adjusted.Because the glass dust 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 dust 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 frit layer of glass dust softening point temperature between 400 ℃ and 900 ℃ meets the demands.
What this execution mode provided has the following advantages with the soft-magnetic composite material of glass dust as coating layer: 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 frit layer that coats of proportioning of each composition in the adjusting glass dust; 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 the glass frit 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; Simultaneously; Material can experience in annealing process greater than the temperature of glass frit layer softening temperature, so magnetic and coating layer to combine no longer be simple mechanical bond, but a kind of diffusion-bonded; Therefore also improved the mechanical property of soft-magnetic composite material, made the cross-breaking strength of soft-magnetic composite material greater than 90MPa.The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass dust; Make that the softening point temperature of glass frit layer is adjustable, and the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass frit 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.
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: this execution mode provide with the preparation method of glass dust as the soft-magnetic composite material of coating layer, specifically accomplish 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 magnetic; Add ethanol and oleic acid therein; 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, and 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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, the solidliquid mixture that reaction is obtained leaves standstill 10min ~ 30min; Outwell solution, the solid that obtains is cleaned, filter; To clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃, dry 20min ~ 360min; Dried solid is screened 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, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, the mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1;
Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature; Constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing; Obtain with the soft-magnetic composite material of glass dust as coating layer, wherein heat treatment temperature is 500 ℃ ~ 1000 ℃.
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.
This execution mode preparation with the soft-magnetic composite material of glass dust as coating layer, can adjust the composition and the proportioning of glass dust 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 dust 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 glass dust thermal coefficient of expansion as glass dust.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 dust 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 glass dust thermal coefficient of expansion 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 glass frit layer.
This execution mode preparation with the soft-magnetic composite material of glass dust as coating layer, can adjust the composition and the proportioning of glass frit layer according to softening point.Because the glass dust 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 dust 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 frit layer of glass dust softening point temperature between 400 ℃ and 900 ℃ meets the demands.
Having the following advantages with the soft-magnetic composite material of glass dust as coating layer of this execution mode preparation: 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 frit layer that coats of proportioning of each composition in the adjusting glass dust; 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 the glass frit 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; Simultaneously; Material can experience in annealing process greater than the temperature of glass frit layer softening temperature, so magnetic and coating layer to combine no longer be simple mechanical bond, but a kind of diffusion-bonded; Therefore also improved the mechanical property of soft-magnetic composite material, made the cross-breaking strength of soft-magnetic composite material greater than 90MPa.The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass dust; Make that the softening point temperature of glass frit layer is adjustable, and the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass frit 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.
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 the shared mass fraction of nickel is 35%～90% permalloy powder.
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: this execution mode with the difference of one of embodiment three to five is: the described glass dust of step 3 is to use Prepared by Sol Gel Method.
Embodiment seven: this execution mode provide with the preparation method of glass dust as the soft-magnetic composite material of coating layer, specifically accomplish 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 magnetic; Add ethanol and oleic acid therein; 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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; Stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition, reacts 2 hours～4 hours, and the solidliquid mixture that reaction is obtained leaves 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, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, the mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1;
Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature, constant temperature 30min ~ 180min, and the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards; Promptly accomplish annealing, obtain with the soft-magnetic composite material of glass dust as coating layer;
Wherein heat treatment temperature is 500 ℃ ~ 1000 ℃.
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.
This execution mode provide with the soft-magnetic composite material of glass dust as coating layer, can adjust the composition and the proportioning of glass frit 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 dust 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 dust, should select those oxides that can significantly improve the glass dust thermal coefficient of expansion, 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 dust 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 glass dust thermal coefficient of expansion 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 frit layer.The thermal coefficient of expansion that common glass dust forms thing and intermediate oxide is all quite low, is effective method as improving its thermal coefficient of expansion adding I A family, II A family oxide or PbO.
This execution mode provide with the soft-magnetic composite material of glass dust as coating layer, according to softening point the composition and the proportioning of glass frit layer are adjusted.Because the glass dust 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 dust 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 frit layer of glass dust softening point temperature between 400 ℃ and 900 ℃ meets the demands.
Having the following advantages with the soft-magnetic composite material of glass dust as coating layer of this execution mode preparation: 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 frit layer that coats of proportioning of each composition in the adjusting glass dust; 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 the glass frit 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; Simultaneously; Material can experience in annealing process greater than the temperature of glass frit layer softening temperature, so magnetic and coating layer to combine no longer be simple mechanical bond, but a kind of diffusion-bonded; Therefore also improved the mechanical property of soft-magnetic composite material, made the cross-breaking strength of soft-magnetic composite material greater than 90MPa.The annealing temperature of soft-magnetic composite material is adjustable; Can be through regulating the proportioning of each composition in the glass dust; Make that the softening point temperature of glass frit layer is adjustable, and the annealing temperature of soft-magnetic composite material is again greater than the softening point temperature of glass frit layer, and then the annealing temperature of also having regulated soft-magnetic composite material.
Embodiment eight: the difference of this execution mode and embodiment seven 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.
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 the shared mass fraction of nickel is 35%～90% permalloy powder.
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 nine: this execution mode and embodiment seven or eight 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 seven or eight.
Embodiment ten: this execution mode with the difference of one of embodiment seven to nine is: the described glass dust of step 3 is to use Prepared by Sol Gel Method.
Adopt following verification experimental verification effect of the present invention:
Test one:, specifically accomplish according to the following steps with the preparation method of glass dust as the soft-magnetic composite material of coating layer:
One, the ATOMET_1001HP water-atomized iron powder 150g with Quebec, CAN metal dust Co., Ltd puts into 250mL 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 46.5g (50mL); After all adding, reacted 2 hours, the solidliquid mixture that reaction is obtained leaves standstill 30min; Outwell solution, in the solid that obtains, add ionized water and ethanol cleaning 2 times, filter; To clean back and solid and put into drying box, temperature is 60 ℃, dry 240min; Dried solid is screened with electromagnet, promptly obtain the magnetic of coated silica layer;
Three, in the magnetic of the coated silica layer that step 2 obtains, add the 4.5g glycerine, in the V-type batch mixer, stir; Mixing speed 20r/min, duration 5min is in the mixture that obtains; Adding particle diameter is the glass dust 15g of 10nm ~ 300nm, continues in the V-type batch mixer, to stir mixing speed 20r/min; Duration 30min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, glass dust is used Prepared by Sol Gel Method, and glass dust is pressed mass fraction by 30% Na
2O, 4% CaO and 66% SiO2 form;
Four, at room temperature, apply the mechanical pressure of 1000MPa, constant voltage 3min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer with the cladding iron powder that obtains in the step 3;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa, be warmed up to 550 ℃ 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 with the soft-magnetic composite material of glass dust as coating layer.
The iron powder of step 1 is carried out scanning electron microscope test, and as shown in Figure 1, Fig. 1 is 200 times electron scanning micrograph of iron powder in the test one; The glass dust of step 3 is carried out scanning electron microscope test, and as shown in Figure 2, Fig. 2 is 50000 times electron scanning micrograph of glass dust in the test one; The coating magnetic that outside silicon dioxide layer, coats glass frit layer that step 3 is obtained carries out scanning electron microscope test; As shown in Figure 3, Fig. 3 is for coating 200 times electron scanning micrograph of the coating magnetic of glass frit layer outside silicon dioxide layer in the test one; From above-mentioned three figure, can draw, test is undertaken by described step, and has obtained outside silicon dioxide layer, coating the coating magnetic of glass frit layer.Carry out Metallographic Analysis with glass dust as the soft-magnetic composite material of coating layer with what step 5 prepared; As shown in Figure 4; Fig. 4 for the test one the preparation with the metallograph of glass dust as the soft-magnetic composite material of coating layer, from Fig. 4, the part that can obtain black crackle shape is an insulating barrier; The white portion that is being coated by the black crackle is an iron powder, can show to have prepared with the soft-magnetic composite material of glass dust as coating layer.
This kind is as shown in table 1 as the electromagnetic performance and the mechanical property of the soft-magnetic composite material of coating layer with glass dust.
Table 1 test one preparation with electromagnetic performance and the mechanical performance index of glass dust as the soft-magnetic composite material of coating layer
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:, specifically accomplish according to the following steps with the preparation method of glass dust as the soft-magnetic composite material of coating layer:
One, the ATOMET_1001HP water-atomized iron powder 150g with Quebec, CAN metal dust Co., Ltd puts into 250mL 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 46.5g (50mL); After all adding, reacted 3 hours, the solidliquid mixture that reaction is obtained leaves standstill 30min; Outwell solution, in the solid that obtains, add ionized water and ethanol cleaning 2 times, filter; To clean back and solid and put into drying box, temperature is 60 ℃, dry 240min; Dried solid is screened with electromagnet, promptly obtain the magnetic of coated silica layer;
Three, in the magnetic of the coated silica layer that step 2 obtains, add the 4.5g glycerine, in the V-type batch mixer, stir; Mixing speed 20r/min, duration 5min is in the mixture that obtains; Adding particle diameter is the glass dust 15g of 10nm ~ 300nm, continues in the V-type batch mixer, to stir mixing speed 20r/min; Duration 30min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, glass dust is used Prepared by Sol Gel Method, and glass dust is pressed mass fraction by 25% Na
2O, 6% Al
2O
3With 69% SiO
2Form;
Four, at room temperature, apply the mechanical pressure of 1000MPa, constant voltage 3min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer with the cladding iron powder that obtains in the step 3;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-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 with the soft-magnetic composite material of glass dust as coating layer.
This kind is as shown in table 2 as the electromagnetic performance and the mechanical property of the soft-magnetic composite material of coating layer with glass dust.
Table 2 test two preparations with electromagnetic performance and the mechanical performance index of glass dust as the soft-magnetic composite material of coating layer
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:, specifically accomplish according to the following steps with the preparation method of glass dust as the soft-magnetic composite material of coating layer:
One, the ATOMET_1001HP water-atomized iron powder 150g with Quebec, CAN metal dust Co., Ltd puts into 250mL 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 46.5g (50mL), after all adding, reacted 3 hours; After reaction finishes, in product, add oleic acid 12.00g (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, reacts 2 hours; The solidliquid mixture that reaction is obtained leaves standstill 30min, outwells solution, in the solid that obtains, adds ionized water and ethanol cleaning 2 times; Filter, will clean back and solid and put into drying box, temperature is 60 ℃; Dry 240min screens dried solid with electromagnet, promptly obtain the magnetic of coated silica layer;
Three, in the magnetic of the coated silica layer that step 2 obtains, add the 4.5g glycerine, in the V-type batch mixer, stir; Mixing speed 20r/min, duration 5min is in the mixture that obtains; Adding particle diameter is the glass dust 15g of 10nm ~ 250nm, continues in the V-type batch mixer, to stir mixing speed 20r/min; Duration 30min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer; Wherein, glass dust is used Prepared by Sol Gel Method, and glass dust is pressed mass fraction by 22% Na
2O, 4.5% Al
2O
3, 4.5% TiO
2With 69% SiO
2Form;
Four, at room temperature, apply the mechanical pressure of 900MPa, constant voltage 3min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer with the cladding iron powder that obtains in the step 3;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-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 with the soft-magnetic composite material of glass dust as coating layer.
This kind is as shown in table 3 as the electromagnetic performance and the mechanical property of the soft-magnetic composite material of coating layer with glass dust.
Table 3 test three preparations with electromagnetic performance and the mechanical performance index of glass dust as the soft-magnetic composite material of coating layer
In the table 3, μ
mThe maximum permeability of expression 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) representes soft-magnetic composite material at maximum magnetic field strength 1T, the iron loss value under the alternative frequency 50Hz; W (200Hz) representes 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 (10)
1. with the soft-magnetic composite material of glass dust, it is characterized in that forming by the silicon dioxide layer of magnetic, coating magnetic and the glass frit layer that is coated on outside the silicon dioxide layer as the soft-magnetic composite material of coating layer with glass dust as coating layer; 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 with the soft-magnetic composite material of glass dust as coating layer, 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 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, it is characterized in that accomplishing according to the following steps with the preparation method of glass dust as the soft-magnetic composite material of coating layer:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains magnetic; Add ethanol and oleic acid therein; 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, and 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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, the solidliquid mixture that reaction is obtained leaves standstill 10min ~ 30min; Outwell solution, the solid that obtains is cleaned, filter; To clean the back solid and put into drying box, temperature is 40 ℃ ~ 80 ℃, dry 20min ~ 360min; Dried solid is screened 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;
Three, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer, wherein; The mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1;
Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer;
Five, in vacuum degree be the condition of 10-1Pa under with glass dust as the blank of the soft-magnetic composite material of coating layer with what obtain in the step 4; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature, constant temperature 30min ~ 180min, and the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards; Promptly accomplish annealing; Obtain with the soft-magnetic composite material of glass dust as coating layer, wherein, heat treatment temperature is 500 ℃ ~ 1000 ℃.
4. according to claim 3 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, 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 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, 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. according to claim 3 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, it is characterized in that the described glass dust of step 3 uses Prepared by Sol Gel Method.
7. as claimed in claim 1 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, it is characterized in that accomplishing according to the following steps with the preparation method of glass dust as the soft-magnetic composite material of coating layer:
One, magnetic is put into cleaning agent with the ultrasonic 10min ~ 20min of the frequency of 24KHz ~ 35KHz; Filtration obtains magnetic; Add ethanol and oleic acid therein; 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, and 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, and stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition; By the tetraethoxysilane of 2 ~ 4 adding equivalent, 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; Stirring pH value with solidliquid mixture at the rotating speed with 600r/min ~ 1200r/min is under 8.5～9.5 the condition, reacts 2 hours～4 hours, and the solidliquid mixture that reaction is obtained leaves standstill 10min ~ 30min; Outwell solution, the solid that obtains is cleaned, filter; To clean the back solid and put into drying box; Temperature is 40 ℃ ~ 80 ℃, and 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, in the magnetic of the coated silica layer that step 2 obtains, add glycerine, in batch mixer, mix; Mixing rate 15r/min～60r/min, incorporation time 20min～90min is in mixture; Adding particle diameter is the glass dust of 10nm ~ 500nm, continues in batch mixer, to mix mixing rate 15r/min～60r/min; Incorporation time 20min～90min promptly obtains outside silicon dioxide layer, coating the coating magnetic of glass frit layer, wherein; The mass ratio of glycerine and magnetic is (0.01 ~ 0.05): 1, and the mass ratio of glass dust and magnetic is (0.05 ~ 0.25): 1;
Four, with the coating magnetic that obtains in the step 3 at room temperature, apply the mechanical pressure of 600MPa～1500MPa, constant voltage 1min ~ 5min removes pressure, promptly obtains with the blank of glass dust as the soft-magnetic composite material of coating layer;
Five, be 10 as the blank of the soft-magnetic composite material of coating layer in vacuum degree with glass dust with what obtain in the step 4
-1Under the condition of Pa; Heating rate with 1 ℃/min ~ 5 ℃/min is warmed up to heat treatment temperature from room temperature; Constant temperature 30min ~ 180min, the rate of temperature fall with 1 ℃/min ~ 5 ℃/min is cooled to room temperature afterwards, promptly accomplishes annealing; Obtain with the soft-magnetic composite material of glass dust as coating layer, wherein heat treatment temperature is 500 ℃ ~ 1000 ℃.
8. according to claim 7 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, 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.
9. according to claim 7 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, 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.
10. according to claim 7 with the preparation method of glass dust as the soft-magnetic composite material of coating layer, it is characterized in that the described glass dust of step 3 uses Prepared by Sol Gel Method.
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| CN113674983A (en) * | 2021-08-20 | 2021-11-19 | 合肥工业大学 | Preparation method of compact alumina-coated soft magnetic powder |
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