CN106356176A - Composite amorphous powder precursor used for magnetic powder core and preparation method of composite amorphous powder precursor - Google Patents
Composite amorphous powder precursor used for magnetic powder core and preparation method of composite amorphous powder precursor Download PDFInfo
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Abstract
The invention belongs to the field of metal-based soft magnetic composite and discloses a composite amorphous powder precursor used for a magnetic powder core and a preparation method of the composite amorphous powder precursor. The preparation method includes the steps of preparing an amorphous alloy ribbon into amorphous alloy powder; subjecting the amorphous alloy powder to screening and compounding to obtain a first product; subjecting the first product to passivation and coupling to obtain a second product; mixing the second product with a ceramic precursor polymer solution with stirring to obtain the composite amorphous powder precursor. The composite amorphous powder precursor and the preparation method has the advantages that by using ceramic precursor polymers as an insulating agent and a binding agent, the step of adding insulating powder is omitted, the problems of poor thermostabilization and poor magnetic performance of a magnetic powder core prepared from an amorphous powder precursor which is obtained by means of subjecting an amorphous ribbon pieces to thermal treating, crushing, screening, compounding, passivating and coupling are solved, production cost is decreased, and the composite amorphous powder precursor can be applied to an electron device requiring high frequency and low consumption.
Description
Technical field
The invention belongs to Metal Substrate soft-magnetic composite material field is and in particular to a kind of composite amorphous powder for powder core
Presoma and preparation method thereof.
Background technology
Non-crystaline amorphous metal is a kind of magnetically soft alloy material of excellent performance, has high resistance, high saturation magnetic flux density, high magnetic conductance
Rate, low-loss, cheap the advantages of, using fast quenching chilling technique preparation amorphous alloy ribbon be widely used in power frequency become
Depressor iron core.But the raising with operating frequency, the eddy-current loss of amorphous alloy ribbon also can become big.Therefore, use for reference powder smelting
Gold and the moulding process of composite, the non-crystaline amorphous metal powder core under exploitation medium-high frequency has become compeling in magnetically soft alloy field
Being essential will.
By by amorphous alloy material powdered, and insulation processing is carried out to amorphous powder granule so that non-crystaline amorphous metal magnetic
Powder core has the low core loss characteristic comparing favourably with mpp powder core and high direct current overlapping features.This makes non-crystaline amorphous metal magnetic
Powder core is highly suitable for the high-performance equipment using high-current inductor, and such as computer, server, industrial power and requirement can be held
Carry the various pfc power circuits of high frequency and high current.
Up to the present, the technique preparing amorphous powdered alloy mainly has convolution current spray art, noble gases spraying
Technique and the technique directly crushing powder processed using amorphous thin ribbon.Wherein, directly prepare amorphous powdered alloy using amorphous thin ribbon
Technique be currently to prepare the prevailing technology of amorphous powdered alloy, its substantially flow process is as follows: first, will be non-below crystallization temperature
Crystal zone material carries out heat treatment so as to embrittlement；Subsequently, amorphous band is made to be deformed using ball-milling method and broken refinement.This preparation
The advantage of technology is that the selectivity to material is not strong, can fully recycle discarded amorphous band, and production efficiency is high, fits
For dry grinding, wet grinding.Shortcoming is directly amorphous thin ribbon to be carried out with brittle annealing it is easy to cause uneven, annealing inequality of annealing
The even crystallization that will result within amorphous thin ribbon change and Stress Release uneven, crushed again after annealing, just very
Easily produce pattern irregularly and have the powder particle of sharp comer it is difficult to insulate.Also it is unfavorable in follow-up Passivation Treatment and bag
Cover and in process, form uniform insulating coating, and then lead to the loss of powder core to raise, reduce material soft magnet performance.
Existing disclosed technical scheme is the prepared amorphous powdered alloy by crushing to amorphous thin ribbon；Again by non-crystaline amorphous metal
Powder obtains being applied to the amorphous powder presoma preparing powder core after processing through transpassivation, coupling, insulating wrapped, but adopts
Disclosed in prior art, the powder core of amorphous powder presoma preparation has that insulating properties is bad, and the asking of heat stability difference
Topic.
As Chinese patent literature cn103745791 a discloses a kind of iron based nano crystal magnetic powder with superhigh magnetic conductivity
The preparation method of core.Preparation method disclosed in this patent documentation, discloses following technical characteristics, step one, to iron based nano crystal
Strip carries out mechanical activation comminution process, to obtain iron based nano crystal powder；Step 2, sieves to described iron based nano crystal powder
And proportioning, being then mixed into by the pass through coarse powder of -40～+100 sieve meshes and weight content that weight content is 40～80% is 20
The mixed-powder of～60% fine powder composition passing through -325 sieve meshes；Step 3, is respectively adopted passivator, coupling agent, insulating compound
With binding agent described mixed-powder is passivated successively, is coupled, insulating wrapped process, obtain amorphous powder presoma, then
Compressing.And also disclose described insulating compound and adopt glass powder with low melting point；Described binding agent adopts epoxy resin.This patent
Preparation method disclosed in document solves the problems, such as that bulky grain manocrystalline powders are compressing, be obtained group uniformly, seamless,
Pcrmeability reaches more than 300 nanocrystalline magnetic core.
But preparation method disclosed in above-mentioned patent documentation has following defects that
1) directly iron-based nano-crystalline thin ribbon is carried out preparing magnetic as iron based nano crystal powder after mechanical activation comminution process
Powder core, leads to the loss of powder core to raise, and reduces material soft magnet performance.
2) epoxy resin is used as binding agent, but epoxy resin thermostability is not good, asphalt mixtures modified by epoxy resin when generally more than 300 DEG C
Fat begins to crack, and cracking residue when its 400 DEG C, not as good as the 15% of primary resin weight, does not have the enhanced work of bonding
With.
3) adopt glass powder with low melting point as the binding agent under insulating compound and high temperature, those skilled in the art will know that phosphate
The low melting point glass material of system can not be compatible well with the epoxy resin residue after cracking, is easily caused the glass dust of melting
It is difficult to sprawl between amorphous powdered alloy granule and flows, the generated hole of epoxy resin cracking can not be filled up well,
A lot of pores therefore can be left in insulating bond, reduce the resistivity of non-crystaline amorphous metal powder core.
4) low-melting glass of phosphate system, its glass transformation temperature relatively low it is adaptable to low-temperature sealing, but be unsuitable for
It is suitable for for a long time under high temperature.Its molecular structure is susceptible to rupture, and chemical stability is poor, can produce free acid at high temperature
Property oxide and basic anhydride, can react with amorphous powdered alloy granule, lead to non-crystaline amorphous metal powder core magnetic property to be disliked
Change.
Content of the invention
For this reason, to be solved by this invention be in prior art adopt amorphous powder presoma be obtained powder core heat
The technical problem of stability difference, there is provided before a kind of composite amorphous powder that can effectively improve powder core heat stability and magnetic property
Drive body and preparation method thereof.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
The preparation method of the composite amorphous powder precursor for powder core provided by the present invention, comprises the steps,
Amorphous alloy ribbon is prepared into amorphous powdered alloy；
Described amorphous powdered alloy carried out sieve, compound, obtain the first product；
Described first product is passivated and coupling processing, obtains the second product；
By described second product and Preceramic Polymers solution mix and blend, obtain composite amorphous powder precursor.
Described Preceramic Polymers solution is the mixture of silanes Preceramic Polymers and organic solvent；
Described silanes Preceramic Polymers are 1 with the mass ratio of described organic solvent: (5～10)；
The addition of described silanes Preceramic Polymers is the 0.2%～1% of described second product quality.
Further, described silanes Preceramic Polymers be polysilazane, polysiloxanes, PVDF hollow fiber membrane or poly-
At least one in carbon silane；
Described organic solvent is at least in acetone, dimethylbenzene, 1- methoxy-2-propanol or 2- methoxy-1-propanol
Kind.
Further, the mean molecule quantity of described silanes Preceramic Polymers is 1000～20000.
Described amorphous alloy ribbon is prepared into amorphous powdered alloy step, comprising:
Break process is carried out to amorphous alloy ribbon；
Under an inert atmosphere, heat treatment is carried out to the described amorphous alloy ribbon after break process, and in heat treatment process
In, to described amorphous alloy ribbon continuous stirring；
Described amorphous alloy ribbon after heat treatment is ground process, obtains amorphous powdered alloy.
Described break process is that described amorphous alloy ribbon is broken into the fragment of 50 mesh～200 mesh；
The temperature of described heat treatment is 200 DEG C～350 DEG C.
Further, described amorphous alloy ribbon is Fe-based amorphous alloy strip, described Fe-based amorphous alloy strip composition
For fe80si9b11Or fe78si9b13；
The thickness of described Fe-based amorphous alloy strip is 18～26 μm, carries a width of 2～142mm.
Be preferably described Fe-based amorphous alloy strip a width of 10～60mm of band.
Described inert atmosphere is nitrogen and/or argon.
Further, described heat treatment step operates in atmosphere rotary furnace and carries out；
The speed of rotation of described atmosphere rotary furnace is 5～60r/min, and atmosphere pressures are 0.1～0.3mpa.
Preferably, the temperature of described heat treatment step is 200 DEG C～350 DEG C, and the time is 30min～60min.
Described milled processed step is the output work of the described fluid energy mill being carried out using fluid energy mill operation
Rate 35～100kw, milling time 20～90min.
Further, described screening is included with compounding step: described amorphous powdered alloy is sieved as several classes as follows: 100
More than～150 mesh, 150～200 mesh, 200～240 mesh, 240～270 mesh and 270 mesh；Wherein, 100～150 mesh account for total mesh number
5%～50%, 150～200 mesh account for the 10%～40% of total mesh number, 200～240 mesh account for the 10%～40% of total mesh number, 240～
270 mesh account for more than the 5%～30% of total mesh number, 270 mesh and account for the 5%～10% of total mesh number.
The passivator of described passivation and coupling processing employing is the acetone soln of phosphoric acid and silicon dioxide colloid, wherein, institute
State phosphoric acid addition be described screening with compounding after the quality of amorphous powdered alloy 0.2%～0.8%, described titanium dioxide
The addition of colloidal silica be described screening with compounding after amorphous powdered alloy quality 0.1%～0.5%；
Described coupling agent be γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and
At least one in the ethanol solution of phosphate ester titanium coupling agent；Wherein, described γ-methacryloxypropyl trimethoxy silicon
The addition of alkane be described screening with compounding after amorphous powdered alloy quality 0.05%～0.3%, described γ-aminopropyl three
The addition of Ethoxysilane be described screening with compounding after amorphous powdered alloy quality 0.05%～0.3%, described phosphorus
The addition of acid esters titanium coupling agent be described screening with compounding after amorphous powdered alloy quality 0.1%～0.4%.
In the preparation process of described composite amorphous powder precursor, also include the step adding powder lubricant；
Described powder lubricant be zinc stearate micropowder, barium stearate micropowder or synthesize cured micropowder at least one；Institute
State powder lubricant addition be described passivation and coupling processing after amorphous powdered alloy quality 0.1%～1%.
Present invention also offers the composite amorphous powder precursor being obtained by above-mentioned preparation method.
Compared with prior art, the invention has the following beneficial effects:
1) preparation method of the composite amorphous powder precursor that the embodiment of the present invention is provided, in preparation process, by adopting
With Preceramic Polymers solution and described second product mix and blend, Preceramic Polymers solution serves wherein
Insulating compound and the effect of binding agent.Because Preceramic Polymers are colloidal state at normal temperatures, dissolve in solvent and formed
Solution.After itself and amorphous powdered alloy combination drying, one layer of uniform ceramic setter can be formed on amorphous powdered alloy surface
Body thin polymer film, you can play the effect of bonding, also functions to the effect insulated simultaneously, and this thin film has good calendering
Property, compressing beneficial to use it for preparing during powder core at normal temperatures；
And by using heat cured Preceramic Polymers, net high-polymer can be formed when 200 DEG C～300 DEG C
Amorphous powdered alloy can be bondd by structure effectively；And the quality when 400 DEG C～450 DEG C for the Preceramic Polymers is damaged
Lose and be less than 5%, the mass loss when 450 DEG C～550 DEG C is less than 15%.Its at high temperature the composition after heat treatment be mainly
The material similar to ceramic structure that the elements such as si, c, b, n, o are combined into, its thermostability is up to 800 DEG C.Avoid existing skill
Epoxy resin is adopted as binding agent in art, when glass powder with low melting point is as insulating compound, prepared non-crystaline amorphous metal presoma, then make
The heat stability of the powder core obtaining is poor, the shortcoming that magnetic property declines.Therefore the composite amorphous powder precursor that the present invention is obtained can use
High temperature resistant in preparing, the excellent amorphous state soft magnetism composite magnetic powder core of magnetic property.
2) preparation method of the composite amorphous powder precursor that the embodiment of the present invention is provided, by silanes pottery of making pottery
Preceramic polymer is mixed with organic solvent；And limit both ratios, and silanes Preceramic Polymers and organic
The respective species of solvent, makes Preceramic Polymers solution have suitable viscosity, is easy to and appropriate amorphous powdered alloy
Mixing bonding, obtains that structure is homogeneous effectively, stable composite amorphous powder precursor, thus apply it to preparing powder core
When, can obtain that structure is homogeneous, stable powder core；And the silanes Preceramic Polymers of these species have excellent electricity
Insulating properties, and due to good calenderability and thermostability, can be formed inside amorphous powder core during room temperature compacting
Insulation adhesive Rotating fields, relying on unlike glass powder with low melting point extends after high-temperature fusion forms insulating bond, therefore it can
Thinner insulating bond is obtained, reduces the consumption of namagnetic substance in amorphous powder core, improve inside amorphous powder core
The uniformity of structure is so that the soft magnet performance of amorphous powder core is more stable.
3) preparation method of the composite amorphous powder precursor that the embodiment of the present invention is provided, by amorphous alloy ribbon
First crushed, more uniform heat treatment, finally ground mode, it is possible to obtain the amorphous that particle aspect is uniform, edge is round and smooth closes
Bronze end, efficiently solves the amorphous powdered alloy heterogeneity that in prior art, amorphous alloy ribbon is obtained, the many sharp comer in edge
Problem, and then solve the problems, such as impact non-crystaline amorphous metal powder core insulating properties and soft magnet performance therefrom.
4) preparation method of the composite amorphous powder precursor that the embodiment of the present invention is provided, by using phosphoric acid and dioxy
The acetone soln of SiClx colloid, as the passivator of amorphous powdered alloy, improves the densification of amorphous powder particle surface passivating film
Property and bond strength；The compounding coupling mixing according to a certain percentage by using silane coupler and titanate coupling agent again
Agent, enables the dispersion evenly of varigrained amorphous powder granule, improves amorphous powder granule and gathers with ceramic precursor
The wettability of compound, and improve the adhesion strength of amorphous powder granule and Preceramic Polymers.
5) preparation method of the composite amorphous powder precursor that the embodiment of the present invention is provided, by screening and with compounding,
The pcrmeability of prepared composite magnetic powder core can be regulated and controled according to actual needs, convenient and simple；Eliminate the step adding insulating compound powder
Suddenly, solve the problems, such as that conventional amorphous thin ribbon crushes that pcrmeability when preparing powder core is unstable and heat stability is poor.
6) the composite amorphous powder precursor that the embodiment of the present invention is provided, structure is homogeneous, stable, and has excellent heat
Stable；With its preparation-obtained powder core, there is high temperature resistant and excellent soft magnet performance, and can be with its magnetic conductance of Effective Regulation
Rate, e.g., can control its relative permeability is 60～90, and it records magnetic loss under conditions of f=100khz, b=0.05t
＜ 42w/kg.
Specific embodiment
In order to the object, technical solutions and advantages of the present invention are better described, below in conjunction with specific embodiment to this
Bright it is described further.The present invention can be embodied in many different forms, and should not be construed as limited to set forth herein
Embodiment.On the contrary, provide these embodiments so that the disclosure will be thorough and complete, and the design of the present invention will be filled
Divide and convey to those skilled in the art, the present invention will only be defined by the appended claims.
Silicon dioxide colloid described in each embodiment following and comparative example is purchased from chemistry institute of the Chinese Academy of Sciences；γ-metering system
Acryloxypropylethoxysilane trimethoxy silane, gamma-aminopropyl-triethoxy-silane are purchased from BASF；Polysilazane, PVDF hollow fiber membrane
Can make by oneself with polysiloxanes, also available commercially is commercially available, and homemade method is well known to a person skilled in the art,
This repeats no more；Phosphate ester titanium coupling agent is purchased from Chemical Co., Ltd. of Japanese SHIN-ETSU HANTOTAI；Zinc stearate micropowder, barium stearate micropowder and
Synthesize cured micropowder and be purchased from Nanjing sky Siconnect Ltd..
Coupling agent described in each embodiment following and comparative example is γ-methacryloxypropyl trimethoxy silicon
The volume fraction of the ethanol solution of alkane, gamma-aminopropyl-triethoxy-silane or phosphate ester titanium coupling agent is 0.1%～10%.
Embodiment 1
The present embodiment provides a kind of composite amorphous powder precursor for powder core and preparation method thereof, corresponding preparation
Method, comprises the steps:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 18 μm, carry a width of 10mm, composition be fe80si9b11Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in nitrogen protection atmosphere rotary furnace in, heat treatment 1h at 300 DEG C,
During heating treatment, the speed of rotation controlling atmosphere rotary furnace is 5r/min, atmosphere pressures are 0.1mpa, does not stop upset atmosphere and returns
Converter, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
35kw, milled processed 50min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 20% of total mesh number, 200～240
Mesh accounts for the 45% of total mesh number, and 240～270 mesh account for the 20% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.6%, the adding of silicon dioxide colloid
Dosage is 0.3% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.2% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous conjunction after mixing compounds
The 0.1% of golden powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.2%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 2: 3: 5 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 0.8% of amorphous powdered alloy quality, and solvent is third
Ketone, 1- methoxy-2-propanol and 2- methoxy-1-propanol are by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor
Polymer is 1: 5 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dry,
After cooling add powder lubricant, wherein said powder lubricant be mass ratio for 3: 3: 4 zinc stearate micropowder, barium stearate
Micropowder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；Powder is moistened
Lubrication prescription be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains composite amorphous powder precursor.
Embodiment 2
The present embodiment provides a kind of composite amorphous powder precursor for powder core and preparation method thereof, corresponding preparation
Method, comprises the steps:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 20 μm, carry a width of 20mm, composition be fe78si9b13Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in argon protection atmosphere rotary furnace in, heat treatment 1h at 300 DEG C,
During heating treatment, the speed of rotation controlling atmosphere rotary furnace is 10r/min, atmosphere pressures are 0.2mpa, does not stop to overturn atmosphere
Rotary furnace, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
70kw, milled processed 50min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 40% of total mesh number, 200～240
Mesh accounts for the 30% of total mesh number, and 240～270 mesh account for the 15% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.5%, the adding of silicon dioxide colloid
Dosage is 0.3% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.15% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous after mixing compounds
The 0.1% of alloy powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.15%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 3: 3: 4 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 0.65% of amorphous powdered alloy quality, and solvent is third
Ketone, 1- methoxy-2-propanol and 2- methoxy-1-propanol are by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor
Polymer is 1: 6 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dry,
After cooling add powder lubricant, wherein said powder lubricant be mass ratio for 3: 3: 4 zinc stearate micropowder, barium stearate
Micropowder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；Powder is moistened
Lubrication prescription be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains composite amorphous powder precursor.
Embodiment 3
The present embodiment provides a kind of composite amorphous powder precursor for powder core and preparation method thereof, corresponding preparation
Method, comprises the steps:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 25 μm, carry a width of 30mm, composition be fe80si9b11Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in nitrogen protection atmosphere rotary furnace in, heat treatment 1h at 280 DEG C,
During heating treatment, the speed of rotation controlling atmosphere rotary furnace is 20r/min, atmosphere pressures are 0.3mpa, does not stop to overturn atmosphere
Rotary furnace, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
50kw, milled processed 90min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 100～150 mesh are accounted for the 40% of total mesh number, 150～200
Mesh accounts for the 20% of total mesh number, and 200～240 mesh account for the 10% of total mesh number, and 240～270 mesh account for the 10% of total mesh number, more than 270 mesh
Account for the 20% of total mesh number, by said ratio, the amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.4%, the adding of silicon dioxide colloid
Dosage is 0.2% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.1% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous conjunction after mixing compounds
The 0.1% of golden powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.2%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 3: 3: 4 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 0.5% of amorphous powdered alloy quality, and solvent is third
Ketone, 1- methoxy-2-propanol and 2- methoxy-1-propanol are by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor
Polymer is 1: 7 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dry,
After cooling add powder lubricant, wherein said powder lubricant be mass ratio for 3: 3: 4 zinc stearate micropowder, barium stearate
Micropowder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；Powder is moistened
Lubrication prescription be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains composite amorphous powder precursor.
Embodiment 4
The present embodiment provides a kind of composite amorphous powder precursor for powder core and preparation method thereof, corresponding preparation
Method, comprises the steps:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 26 μm, carry a width of 40mm, composition be fe78si9b13Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in argon protection atmosphere rotary furnace in, heat treatment 1h at 200 DEG C,
During heating treatment, the speed of rotation controlling atmosphere rotary furnace is 30r/min, atmosphere pressures are 0.2mpa, does not stop to overturn atmosphere
Rotary furnace, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
100kw, milled processed 60min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 40% of total mesh number, 200～240
Mesh accounts for the 30% of total mesh number, and 240～270 mesh account for the 15% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.8%, the adding of silicon dioxide colloid
Dosage is 0.1% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.05% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous after mixing compounds
The 0.3% of alloy powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.1%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 3: 3: 4 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 1% of amorphous powdered alloy quality, solvent be acetone,
, by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor gathers for 1- methoxy-2-propanol and 2- methoxy-1-propanol
Compound is 1: 8 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dries, cold
But add powder lubricant afterwards, the zinc stearate micropowder being 3: 3: 4, barium stearate are micro- for mass ratio for wherein said powder lubricant
Powder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；Powder is lubricated
Agent be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains composite amorphous powder precursor.
Embodiment 5
The present embodiment provides a kind of composite amorphous powder precursor for powder core and preparation method thereof, corresponding preparation
Method, comprises the steps:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 22 μm, carry a width of 60mm, composition be fe80si9b11Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in nitrogen protection atmosphere rotary furnace in, heat treatment at 350 DEG C
0.5h, during heating treatment, the speed of rotation controlling atmosphere rotary furnace is 60r/min, atmosphere pressures are 0.1mpa, does not stop to overturn
Atmosphere rotary furnace, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
80kw, milled processed 20min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 20% of total mesh number, 200～240
Mesh accounts for the 45% of total mesh number, and 240～270 mesh account for the 20% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.2%, the adding of silicon dioxide colloid
Dosage is 0.1% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.3% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous conjunction after mixing compounds
The 0.05% of golden powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.1%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 2: 3: 5 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 0.2% of amorphous powdered alloy quality, and solvent is third
Ketone, 1- methoxy-2-propanol and 2- methoxy-1-propanol are by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor
Polymer is 1: 10 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dries
Dry, add powder lubricant after cooling, wherein said powder lubricant is the zinc stearate micropowder for 3: 3: 4 for the mass ratio, Hard Fat
Sour barium micropowder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；By powder
Last lubricant be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains composite amorphous powder precursor.
Comparative example 1
This comparative example provides a kind of amorphous powder presoma and preparation method thereof, corresponding preparation method, walks including following
Rapid:
S1, the preparation of amorphous powdered alloy:
S11, by thickness be 18 μm, carry a width of 10mm, composition be fe80si9b11Fe-based amorphous alloy strip using machinery
Crusher in crushing is the fragment of 50 mesh～200 mesh；
S12, the fragment of 50 mesh～200 mesh is placed in nitrogen protection atmosphere rotary furnace in, heat treatment 1h at 300 DEG C,
During heating treatment, the speed of rotation controlling atmosphere rotary furnace is 5r/min, atmosphere pressures are 0.1mpa, does not stop upset atmosphere and returns
Converter, makes amorphous fragment thermally equivalent；
S13, the fragment after heat treatment is put in fluid energy mill, control the output of fluid energy mill
35kw, milled processed 50min, further by the corner angle rounding of amorphous powder granule, obtain amorphous powdered alloy；
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 20% of total mesh number, 200～240
Mesh accounts for the 45% of total mesh number, and 240～270 mesh account for the 20% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add passivator, coupling agent, insulating compound and binding agent pair
Described mixed-powder is passivated successively, is coupled, insulating wrapped is processed；Described coupling agent adopts titanate esters；Described passivator is adopted
Use water；Described insulating compound adopts glass powder with low melting point；Described binding agent adopts epoxy resin.Described Passivation Treatment step is: will
Amorphous powdered alloy after above-mentioned mixing compounds is added in the water of 5wt%, stirs until being dried；Described coupling processing step
Suddenly it is: mixed-powder being added in the coupling agent of 5wt%, stirring until being dried；Described insulating wrapped process step is:
In the mixed liquor of the glass powder with low melting point of the 6wt% that mixed-powder is added to and the epoxy resin of 8wt%, stir until
It is dried, obtain amorphous powder presoma；
Comparative example 2
This comparative example provides a kind of amorphous powder presoma and preparation method thereof, corresponding preparation method, walks including following
Rapid:
S1, the preparation of amorphous powdered alloy:
S11, under nitrogen protection atmosphere, by thickness be 18 μm, carry a width of 10mm, composition be fe80si9b11Fe-based amorphous
Alloy thin band is put in atmosphere rotary furnace, and heat treatment 1h at 300 DEG C, during heating treatment, controls the rotation of atmosphere rotary furnace
Rotational speed rate is 5r/min, atmosphere pressures are 0.1mpa, does not stop to overturn atmosphere rotary furnace；
S12, using mechanical crusher, the Fe-based amorphous alloy strip after heat treatment to be crushed to 50 mesh～200 purposes broken
Piece；
S13, amorphous fragment is put in fluid energy mill, control the output 35kw of fluid energy mill, grind
Process 50min, obtain amorphous powdered alloy.
S2, amorphous powdered alloy is sieved and is compounded, wherein 150～200 mesh are accounted for the 20% of total mesh number, 200～240
Mesh accounts for the 45% of total mesh number, and 240～270 mesh account for the 20% of total mesh number, more than 270 mesh accounts for the 15% of total mesh number, by said ratio
The amorphous powdered alloy of each mesh number is put into mixing in batch mixer compounding；
S3, compound to above-mentioned mixing after amorphous powdered alloy in add the third of passivator-phosphoric acid and silicon dioxide colloid
The addition of ketone solution, wherein phosphoric acid be mixing compounding after amorphous powdered alloy quality 0.6%, the adding of silicon dioxide colloid
Dosage is 0.3% of the amorphous powdered alloy quality after mixing compounds, passivator is stirred with amorphous powdered alloy and dries
Dry；Add coupling agent-γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
The ethanol solution of ester titanium coupling agent, the wherein addition of γ-methacryloxypropyl trimethoxy silane are that mixing is compounding
The 0.2% of amorphous powdered alloy quality afterwards, the addition of gamma-aminopropyl-triethoxy-silane is the amorphous conjunction after mixing compounds
The 0.1% of golden powder quality, the addition of phosphate ester titanium coupling agent is the amorphous powdered alloy quality after mixing compounds
0.2%, coupling agent and amorphous powdered alloy are stirred post-drying；
S4, in the amorphous powdered alloy of the post-drying that stirs with coupling agent add Preceramic Polymers solution,
Wherein Preceramic Polymers solution for mass ratio be 2: 3: 5 polysilazane, PVDF hollow fiber membrane and polysiloxanes solution,
In Preceramic Polymers solution, Preceramic Polymers gross weight accounts for the 0.8% of amorphous powdered alloy quality, and solvent is third
Ketone, 1- methoxy-2-propanol and 2- methoxy-1-propanol are by volume for 1: 1: 1 mixture being mixed to get, ceramic precursor
Polymer is 1: 5 with the mass ratio of solvent；Preceramic Polymers solution and amorphous powdered alloy are stirred and dry,
After cooling add powder lubricant, wherein said powder lubricant be mass ratio for 3: 3: 4 zinc stearate micropowder, barium stearate
Micropowder and the mixture synthesizing cured micropowder, described powder lubricant gross weight accounts for the 0.5% of amorphous powdered alloy quality；Powder is moistened
Lubrication prescription be can be taken off after being mixed homogeneously with amorphous powdered alloy, obtains amorphous powder presoma.
The magnetic property of the various embodiments described above and comparative example is tested, corresponding method of testing is as follows:
By the amorphous powder presoma obtained by the various embodiments described above and comparative example respectively by leading to composite amorphous powder
Cross powder metallurgy press, and control pressure is 24t/cm2, be compressed into external diameter be 27mm, internal diameter be that 14.6mm, thickness are
The amorphous powder core of 11mm；Compressing amorphous powder core is put in heat-treatment furnace, in a nitrogen atmosphere, with 10 DEG C/min
Ramp to 260 DEG C, and be incubated 1h at 260 DEG C, then with the ramp of 10 DEG C/min to 425 DEG C, and protect at 425 DEG C
Warm 1h, then Temperature fall again；Last amorphous powder core surface spraying last layer thickness after the cooling period is the blue color circle of 0.2mm
Oxygen tree fat is simultaneously dried, and obtains amorphous state soft magnetism composite magnetic powder core.
By the powder core that will be prepared using the amorphous powder presoma obtained by the various embodiments described above and comparative example
After heat treatment different time at 200 DEG C, then test its pcrmeability under conditions of f=100khz, b=0.05t, accordingly
Test effect as shown in table 1 below:
Table 1
Can learn from table 1: the powder core being prepared using the amorphous powder presoma obtained by the embodiment of the present invention
There is higher pcrmeability and relatively low magnetic loss, and after life-time service 2000h at 200 DEG C, its pcrmeability will not change, magnetic
Loss also will not increase.And comparative example then occurs in that pcrmeability declines and magnetic loss increases.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.Right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (10)
1. a kind of preparation method of the composite amorphous powder precursor for powder core is it is characterised in that comprise the steps,
Amorphous alloy ribbon is prepared into amorphous powdered alloy；
Described amorphous powdered alloy carried out sieve, compound, obtain the first product；
Described first product is passivated and coupling processing, obtains the second product；
By described second product and Preceramic Polymers solution mix and blend, obtain composite amorphous powder precursor.
2. preparation method according to claim 1 is it is characterised in that described Preceramic Polymers solution is silanes
Preceramic Polymers and the mixture of organic solvent；
Described silanes Preceramic Polymers are 1 with the mass ratio of described organic solvent: (5～10)；
The addition of described silanes Preceramic Polymers is the 0.2%～1% of described second product quality.
3. preparation method according to claim 2 is it is characterised in that described silanes Preceramic Polymers are poly- silicon
At least one in azane, polysiloxanes, PVDF hollow fiber membrane or Polycarbosilane；
Described organic solvent is at least one in acetone, dimethylbenzene, 1- methoxy-2-propanol or 2- methoxy-1-propanol.
4. preparation method according to claim 3 it is characterised in that described silanes Preceramic Polymers average
Molecular weight is 1000～20000.
5. the preparation method according to any one of claim 1-4 is it is characterised in that described prepare amorphous alloy ribbon
Become amorphous powdered alloy step, comprising:
Break process is carried out to amorphous alloy ribbon；
Under an inert atmosphere, heat treatment is carried out to the described amorphous alloy ribbon after break process, and in heat treatment process, right
Described amorphous alloy ribbon continuous stirring；
Described amorphous alloy ribbon after heat treatment is ground process, obtains amorphous powdered alloy.
6. preparation method according to claim 5 is it is characterised in that described break process is by described amorphous alloy ribbon
It is broken into the fragment of 50 mesh～200 mesh；
The temperature of described heat treatment is 200 DEG C～350 DEG C.
7. preparation method according to claim 6 is it is characterised in that described amorphous alloy ribbon is that Fe-based amorphous alloy is thin
Band, described Fe-based amorphous alloy strip composition is fe80si9b11Or fe78si9b13；
Described heat treatment step operates in atmosphere rotary furnace and carries out；
Described milled processed is carried out using fluid energy mill operation.
8. the preparation method according to any one of claim 1-7 is it is characterised in that described screening and compounding step bag
Include: described amorphous powdered alloy is sieved as several classes as follows: 100～150 mesh, 150～200 mesh, 200～240 mesh, 240～270
More than mesh and 270 mesh；Wherein, 100～150 mesh account for the 5%～50% of total mesh number, 150～200 mesh account for total mesh number 10%～
40%th, 200～240 mesh account for the 10%～40% of total mesh number, 240～270 mesh and account for more than the 5%～30% of total mesh number, 270 mesh and account for
The 5%～10% of total mesh number.
9. the preparation method according to any one of claim 1-8 is it is characterised in that described passivation and coupling processing adopt
Passivator be phosphoric acid and silicon dioxide colloid acetone soln, wherein, the addition of described phosphoric acid be described screening with compounding
The 0.2%～0.8% of the quality of amorphous powdered alloy afterwards, the addition of described silicon dioxide colloid is described screening and compounds
The 0.1%～0.5% of amorphous powdered alloy quality afterwards；
Described coupling agent is γ-methacryloxypropyl trimethoxy silane, gamma-aminopropyl-triethoxy-silane and phosphoric acid
At least one in the ethanol solution of ester titanium coupling agent；Wherein, described γ-methacryloxypropyl trimethoxy silane
Addition be described screening with compounding after amorphous powdered alloy quality 0.05%～0.3%, described γ-aminopropyl three ethoxy
The addition of base silane be described screening with compounding after amorphous powdered alloy quality 0.05%～0.3%, described phosphate ester
The addition of titanium coupling agent be described screening with compounding after amorphous powdered alloy quality 0.1%～0.4%；
In the preparation process of described composite amorphous powder precursor, also include the step adding powder lubricant；
Described powder lubricant be zinc stearate micropowder, barium stearate micropowder or synthesize cured micropowder at least one；
The addition of described powder lubricant be described passivation and coupling processing after amorphous powdered alloy quality 0.1%～
1%.
10. the composite amorphous powder precursor that the preparation method any one of a kind of claim 1-9 is obtained.
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| CN115613013A (en) * | 2022-10-31 | 2023-01-17 | 中国科学院化学研究所 | Composite insulating layer and preparation method thereof |
| CN115613013B (en) * | 2022-10-31 | 2024-06-04 | 中国科学院化学研究所 | Composite insulating layer and preparation method thereof |
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