CN108070777A - A kind of method that powder tape casting prepares Fe-6.5%Si soft magnetic materials thin strips - Google Patents
A kind of method that powder tape casting prepares Fe-6.5%Si soft magnetic materials thin strips Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F2003/1042—Sintering only with support for articles to be sintered
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
A kind of method that powder tape casting prepares Fe 6.5%Si soft magnetic materials thin strips, for the present invention using water-atomized iron powder, Si contents are 70~80% HIGH-PURITY SILICON iron powder, form Fe 4.5~6.7%Si mixed powders.Solvent, dispersant, bonding agent and plasticizer are added in mixed powder again; finely dispersed stable slurry is made; biscuit is made on casting machine again; biscuit carries out vacuum or protection of reducing atmosphere sintering at 1070~1170 DEG C; Fe powder particles is made to realize not exclusively sintering; and Si and Fe realizes partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation.It through multiple cold rolling, not exclusively sintering, is finally sintered in 1270~1340 DEG C of vacuum or protection of reducing atmosphere, realizes the homogeneous alloy of high silicon steel, 0.1~0.5mm of the acquisition containing 4.5~6.7%Si is thick, density >=7.37g/cm3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder of the high silicon steel soft magnetism band of high-performance
Metallurgy sintered and rolling deformation method.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis loop is very narrow, it and fundamental magnetization curve are almost
It overlaps, is mainly used for the iron core of inductance coil, transformer, relay and motor.Fe-Si alloys maximum permeability is sent out with Si contents
Changing, respectively Si mass percent it is (the same below) for 2% and 6.5% nearby there is the peak of two maximum permeabilities
Value, respectively reaches 10000 and 25000.There is no absolute predominances, such as slope in soft magnetic materials for the maximum permeability of Fe-Si alloys
The maximum permeability of alloy can not reach 200000.However the manufacture of the Fe-Si lattens of Si ＜ 4.5% is at low cost, therefore
Silicon steel sheet is also known as electrical sheet or silicon steel thin slice, is a kind of very important magnetic material.
And Si>When 4.5%, below 540 DEG C of temperature B can occur for Fe-Si alloys2The eutectoid decomposition reaction of ordered phase, it is raw
Into the unordered phases of α-Fe and DO3Ordered phase so that alloy becomes fragile and is difficult to deform.
For iron Si system alloy of the Si contents between 4.5~6.7%, commonly referred to as high silicon steel, wherein silicone content 6.5%
High silicon steel it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction increases with Si contents
And reduce, it disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases with Si contents and is increased, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that the iron core of amount or large size is sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is in the military aviations such as spacecraft, submarine and guided missile field, Fe-Si systems alloy plays particularly important role.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared in as transformer material on No. 11 airships of Apollo, are completed the mankind and are landed on the moon for the first time
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze is for the first time the study found that the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In have lower iron loss and higher magnetic conductivity.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It spends for 0.1~0.5mm, width is the No yield point 6.5%Si steel discs of 400mm.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and to alloy diffusion inside alloy is finally made to reach required content by raised furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
It asks, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", and technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just generate huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of method that powder tape casting prepares Fe-6.5%Si soft magnetic materials thin strips,
The problem of being difficult to shape for the Fe-Si alloy thin band materials of 4.5~6.7%Si contents, using water-atomized iron powder and Si contents as 70
~80% HIGH-PURITY SILICON iron powder is raw material, then prepares certain thickness slab using powder curtain coating forming method, in degreasing, is burnt
Porous, heterogeneous blank is formed after knot.Fe crystal grain containing substantial amounts of non-alloying in blank, has good plasticity, warp
Thin plate is obtained after crossing multi-pass cold rolling-sintering, is finally sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous.
The present invention is achieved by the following technical solutions：Using subsphaeroidal water-atomized iron powder, fine Si contents are
70~80% HIGH-PURITY SILICON iron powder forms Fe-4.5~6.7%Si mixed powders.Solvent is added in mixed powder again, is disperseed
The ingredients such as agent, bonding agent, plasticizer are made finely dispersed stable slurry, then certain thickness biscuit are made on casting machine.
Powder particle distributing homogeneity is high in biscuit made from tape casting, while water atomization Fe powder is coarse with high-compressibility
Grain, occupies larger volume ratio in mixed powder, will not be shown after adding the HIGH-PURITY SILICON iron powder that fine Si contents are 70~80%
Writing reduces its deformability.Powder curtain coating shaping slab is subjected to vacuum in 1070~1170 DEG C of temperature ranges or reducing atmosphere is protected
It protects and is sintered, Fe powder particles is made to realize not exclusively sintering, and Si and Fe realizations are partially-alloyed, formation is porous, has compressibility
Incomplete alloying high silicon steel blank.Subsequently through multiple cold rolling, not exclusively sintering, the density rise of slab, plate thickness
It reduces, the alloying level of Si is also continuously improved.Finally vacuum or protection of reducing atmosphere in 1270~1340 DEG C of temperature ranges
The homogeneous alloy of high silicon steel is realized in sintering with the help of thermal diffusion, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si,
Density >=7.37g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining for Si, Mn, P, S and other can not
The impurity avoided uses Si contents as 70~80% HIGH-PURITY SILICON iron powder, grain size≤10 μm, this ferrosilicon powder except contain 70~
Beyond 80%Si, major impurity is~0.25%Al ,~0.08%Ca and~0.02%C, remaining is Fe.
Water atomization Fe powder is a kind of widely used Industrial iron powder, has subsphaeroidal pattern, impurity content is less than reduction Fe
Powder has higher compressibility and mobility, is conducive to the Uniform Flow of powder curtain coating molding process powder.Water atomization
Low impurity content is favourable to the soft magnetic characteristic of high silicon steel in Fe powder.
Fe-70~80%Si high purity ferrosilicons are in process of setting in addition to primary silicon crystal grain, and at 1207 DEG C, there are eutectics
Reaction, forms the β-FeSi with tP3 structures2With Si phase eutectic structures, it is this tissue it is very crisp, it is easy to pass through Mechanical Crushing
Technique refines.Fe-70~80%Si high purity ferrosilicons are crushed to≤10 μm of ferrosilicon powder, Si phases, FeSi in actual tissue2
It is mutually more tiny, be conducive to the thermal diffusion homogenization of Si elements during subsequent high temperature sintering, form homogeneous Fe-6.5%Si single-phase alloys.
Meanwhile 20~30%Fe present in powder can effectively reduce the degree of oxidation of Si, be conducive to improve the product matter of high silicon steel
Amount.
By Fe-70~80%Si high purity ferrosilicons Mechanical Crushing to grain size≤10 μm, be conducive to it and be adhered to reduction Fe powder
Surface is filled in the hole of reduction Fe powder, tiny Si, FeSi2The mutually Dispersed precipitate in blank, plays structure refinement
Strengthening and Toughening acts on, and is conducive to improve subsequent blank toughness, cracking is not easily caused in densification process is rolled.But Fe-70~
There are still more Si phases, Si in 80%Si high purity ferrosilicons to be easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2Film,
Therefore in the preparation, storage and transfer process of Fe-70~80%Si HIGH-PURITY SILICON iron powders and follow-up batch mixing, curtain coating, rolled
Cheng Zhongying uses inert gas shielding, and used instrument must also take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as Al, Ca, Mn to alloy magnetic property is little, introduces in the process
The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, water atomization Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders, shape are weighed
Into metal powder raw material, phosphoric acid and absolute ethyl alcohol are pressed 0.8~2.0:100 ratio is mixed to prepare passivating solution, by passivating solution with
The metal powder raw material weighed is 0.4~0.6 according to quality:1 ratio mixing, after stirring 0.5~2h, it is blunt to be put into baking oven
Change, baking temperature is 40~42 DEG C, and passivation time is 4~6h, obtains passivation powder.
Powder will be passivated with organic solution according to volume ratio 1:0.5~1 ratio mixing, 6~12h is stirred with mixer,
Again with 5~15min of ultrasonic disperse, through screen filtration, the slurry for the even dispersion made after vacuum outgas, the viscosity of slurry for 40~
80MPa.s。
Doctor-blade casting process is commonly called as scraper forming process, is a kind of important forming method for preparing large area film, is used
The species such as organic solvent, dispersant, plasticizer, binding agent it is various, above-mentioned pulping process is a kind of feasible method, not
Represent method.
(3) powder tape casting
During curtain coating environment temperature be 28~32 DEG C, will disperse slurry inject casting machine in, control casting machine speed be 0.1~
0.5cm/s, the height of scraper is 1.2~2.4mm, and width is 100~300mm.
It is 30~40 DEG C to be cast biscuit drying temperature, and relative humidity is 30~60%, and the thickness of biscuit is after slurry drying
0.95~1.96mm carries out curing process in a nitrogen atmosphere, and solidification temperature is 120~200 DEG C, and hardening time is 1~5h, with
Stove is cooled to room temperature, and the dry curtain coating slab dense structure of preparation, porosity is low, surfacing, because containing more plasticizer, gluing
The organic matters such as agent are tied, density is 6.2~6.6g/cm3。
(4) degreasing, sintering
Curtain coating slab is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace,
2h~4h is kept the temperature respectively using the heating rate of 2~5 DEG C/min, and in 200 DEG C, 400 DEG C, then will heat up to 1070~1170
DEG C 2~4h of heat preservation sintering, sintered blank density are 6.3~6.7g/cm3。
Uniform equiaxed grain structure is formed after sintering, matrix grain is about 70~120 μm, and crystal boundary has about 10~20 μm
Hole, subsequent rolling and sintering can be closed.A large amount of 1~5 μm of the second phase is evenly distributed in matrix, with matrix group
Good interface cohesion is woven with, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these richness Si phases
In the presence of reducing the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile with matrix group
It knits good interface cohesion and Dispersed precipitate is conducive to subsequently homogenization diffusion.
Sintering temperature is too low, the connection being unfavorable between Fe powder particles and Si atoms permeatings, and sintering temperature is excessively high then can be by
In the diffusion into the surface of Fe, Si element, there is coarse hole, be subsequently difficult to press, rolling densification is difficult to realize.
During sintering can powder curtain coating shaping blank can be placed with multilayer, but must separate between layers, to avoid sintering
When slab contraction cause to crack.Heating rate should not be too fast during sintering, and multistage heat preservation can be set in temperature-rise period, de- to realize
Gas, the effect of degreasing.Reproducibility or inert gas shielding degreasing, sintering can also be taken.W, Mo, resistance to may be employed during sintering
Hot steel etc. can also use the ceramic wafers such as corundum, zirconium oxide, but metallic plate thermal conductivity is good and sharp as support plate (or burning boat)
It is shunk in Even Sintering.
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, in sintering furnace, 0.5~2h is re-sintered in 1070~1170 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
To 0.1~0.5mm, density reaches 7.36~7.48g/cm3。
Since powder batch is porous organization, and there are deformable Fe phases, slab can bear cold-rolling deformation.Palette
There is also more high Si phases in base, performance is more crisp, therefore not above 8%, accumulation total reduction reaches amount under every time rolling
8~20 passages are taken around to 30~45%.
Since there are a large amount of holes and hard crisp phase, it is necessary to take and keep the temperature vacuum-sintering again at 1070 DEG C~1170 DEG C or go back
Originality protective atmosphere is sintered, to realize the reparation of the closing of pores and crackle and the homogenization diffusion of a degree of Si elements.This
When heating rate can be very fast, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm, protects
The warm time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.Sintered accumulation drafts reaches every time
, it is necessary to be sintered 1 time again after 30~45%, 0.1~0.5mm is rolled down to from the biscuit of 0.95~1.96mm, is taken around again
Sintering 4~8 times.In addition, in order to which the density of plate is made to reach 7.2g/cm3More than (about the 95% of theoretical density), it is also desirable to 4
Secondary above re-sinters.
By the grain structure that 2 cold rollings-sintered matrix is about 100 μm, there is a small amount of tiny hole.Matrix is brilliant
Grain is there are two types of different contrasts, this is because Si contents are different and cause to corrode difference, low Si crystal grain is conducive in this kind tissue
Machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1270~1340 DEG C of temperature ranges, in the effect of thermal diffusion
Under, it realizes the homogenization of Si, forms single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost unchanged after densification sintering,
For 0.1~0.5mm, density slightly reduces, and reaches 7.37~7.49g/cm3。
Organic solution described in step (2) is with 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, with asphalt mixtures modified by epoxy resin
Fat is binding agent, and polyethylene glycol is plasticizer, and triethanolamine is dispersant, and the volume ratio of epoxy resin and polyethylene glycol presses 1:
1, then by mixed solvent quality be 50~70%, dispersant quality is 0.1%, the slurry that surplus is formed for binding agent and plasticizer
Organic solution.
With high-energy ball milling or rush rotation method obtain grain size≤10 μm HIGH-PURITY SILICON iron powder.
Step (5) is sintered when re-sintering for 1070~1170 DEG C under vacuum-sintering or restitutive protection's atmosphere, by 5~
10 DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab is reduced to 0.5 in 0.1~1mm, soaking time
~1h after sintered accumulation drafts reaches 30~45% every time, is sintered 1 time, is rolled from the biscuit of 0.95~1.96mm again
It makes to 0.1~0.5mm, it is necessary to be sintered 4~8 times again.
Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo can be used and ceramics are burnt
Boat.But plate must tile placement, and tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of elements such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect can subsequently be annealed by wet hydrogen, the technological means such as normalizing treatment are controlled by.
Essence of the invention be by be with the addition of in the water atomization Fe powder of the big volumetric portion with good plasticity granularity≤
Using organic curtain coating system, it is molding multiple to form a kind of achievable powder curtain coating for 10 μm of Fe-70~80%Si high-purity powders
Condensation material；The uniform slab of density, Tissue distribution is prepared using tape casting；By being not exclusively sintered, make Fe powder particles real
Now not exclusively connection, and Si and Fe realizes partially-alloyed, the high silicon of porous, with compressibility the incomplete alloying of formation
Steel blank；Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved；It is real again by high-temperature diffusion process
The homogenization of existing Si, so as to obtain the high silicon steel band of high quality.This method realizes technical process by technique and equipment Design
Automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.37g/cm3High silicon steel band.
Description of the drawings
Fig. 1 is the sintered metallograph of powder tape casting base of the embodiment of the present invention 2；
Fig. 2 is that the plate of the embodiment of the present invention 3 passes through 2 cold rollings-sintered metallograph；
Fig. 3 is XRD diffraction curve figures after the powder tape casting base high temperature sintering of the embodiment of the present invention 3.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the water atomization Fe powder of -100 mesh and the Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:8.375
Ratio mixes, and forms the mixed-powder of Fe-6.7%Si.Phosphoric acid and absolute ethyl alcohol are pressed 0.8:100 ratio is mixed to prepare passivation
Liquid.By passivating solution and the metal powder raw material weighed according to 0.4:1 ratio mixing, after stirring 0.5h with mixer, is put into
Baking oven is passivated, and baking temperature is 40 DEG C, passivation time 4h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin
Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is
60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1:
0.5 ratio mixing, 6h is stirred with mixer, then with ultrasonic disperse 5min, through screen filtration, made after vacuum outgas uniformly more
Scattered slurry, the viscosity of slurry is 40MPa.s.
Environment temperature is 28 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.5cm/s,
The height of scraper is 2.4mm, and width is about 100mm.
It is 40 DEG C to be cast biscuit drying temperature, relative humidity 30%, and the thickness of biscuit is 1.96mm after slurry drying.
Curing process is carried out under nitrogen atmosphere, solidification temperature is 200 DEG C, hardening time 5h, cools to room temperature with the furnace, and curtain coating slab is close
It spends for 6.2g/cm3。
Curtain coating slab is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating rate of 2 DEG C/min, and 4h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1070 DEG C of heat preservation sintering 4h.It burns
It is 6.3g/cm to tie base density3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1070 DEG C of heat preservation sinterings.With 5 DEG C/min speed continuous warmings, soaking time regards plate
Thickness determines, during thickness of slab >=1mm, soaking time 2h；Thickness of slab is in 0.1~1mm, soaking time 1h.Specific pressure-annealing schedule
For：1.96mm → 1.56mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.49mm, density reaches 7.36g/cm3。
For above-mentioned cold rolling made-up belt in 1340 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.37g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
Embodiment 2
By the water atomization Fe powder of -100 mesh and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42 ratio
Example mixing forms the mixed-powder of Fe-4.5%Si.Phosphoric acid and absolute ethyl alcohol are pressed 2.0:100 ratio is mixed to prepare passivation
Liquid.By passivating solution and the metal powder raw material weighed according to 0.6:1 ratio mixing, after stirring 2h with mixer, is put into baking
Case is passivated, and baking temperature is 42 DEG C, passivation time 6h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin
Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is
60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1:1
Ratio mixing, stir 12h with mixer, then with ultrasonic disperse 15min, through screen filtration, made after vacuum outgas uniformly more
Scattered slurry, the viscosity of slurry is 80MPa.s.
Environment temperature is 32 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.1cm/s,
The height of scraper is 1.2mm, and width is about 300mm.
It is 30 DEG C to be cast biscuit drying temperature, relative humidity 60%, and the thickness of biscuit is 0.95mm after slurry drying.
Curing process is carried out under nitrogen atmosphere, solidification temperature is 120 DEG C, hardening time 1h, cools to room temperature with the furnace, and curtain coating slab is close
It spends for 6.8g/cm3。
Curtain coating slab is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating rate of 5 DEG C/min, and 2h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1170 DEG C of heat preservation sintering 2h.It burns
It is 6.7g/cm to tie base density3。
Uniform equiaxed grain structure is formed after sintering, sees Fig. 1.Matrix grain is about 70~120 μm, and crystal boundary presence about 10~
20 μm of hole, subsequent rolling and sintering can be closed.A large amount of 1~5 μm of the second phase is evenly distributed in matrix, with
Matrix has good interface cohesion, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these are rich
The presence of Si phases reduces the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile with
The good interface cohesion of matrix and Dispersed precipitate are conducive to subsequently homogenization diffusion.
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1170 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is
1h.Specifically pressure-annealing schedule is：0.95mm→0.62mm→0.39mm→0.25mm→0.17mm→0.13mm→
0.10mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.48g/cm3。
For above-mentioned cold rolling made-up belt in 1270 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.49g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
Embodiment 3
By the water atomization Fe powder of -100 mesh and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55 ratio
Example mixing forms the mixed-powder of Fe-6.5%Si.Phosphoric acid and absolute ethyl alcohol are pressed 1.0:100 ratio is mixed to prepare passivation
Liquid.By passivating solution and the metal powder raw material weighed according to 0.5:1 ratio mixing, after stirring 1h with mixer, is put into baking
Case is passivated, and baking temperature is 40 DEG C, passivation time 5h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin
Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is
60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1:
0.6 ratio mixing, 8h is stirred with mixer, then with ultrasonic disperse 7min, through screen filtration, made after vacuum outgas uniformly more
Scattered slurry, the viscosity of slurry is 60MPa.s.
Environment temperature is 30 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.3cm/s,
The height of scraper is 1.4mm, and width is about 250mm.
It is 35 DEG C to be cast biscuit drying temperature, relative humidity 45%, and the thickness of biscuit is 1.2mm after slurry drying.
Curing process is carried out under nitrogen atmosphere, solidification temperature is 160 DEG C, hardening time 3h, cools to room temperature with the furnace, and curtain coating slab is close
It spends for 6.24g/cm3。
Curtain coating slab is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 3 DEG C/min, and 2h, 400 DEG C of heat preservation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1150 DEG C of heat preservations and burn
Tie 3h.Sintered blank density is 6.36g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1150 DEG C of heat preservation sintering 1h.With 6 DEG C/min speed continuous warmings.Specific pressure-
Annealing schedule is：1.6mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate
Thickness reach 0.27mm, density reaches 7.38g/cm3。
See Fig. 2 by 2 cold rollings-sintered metallographic structure, matrix is about 100 μm of grain structure, is existed a small amount of thin
Small hole.Matrix grain is there are two types of different contrasts, this is because Si contents are different and cause to corrode difference, in this kind tissue
Low Si crystal grain is conducive to machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.39g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous, and the XRD analysis figure of final plate is shown in Fig. 3.
Embodiment 4
By the water atomization Fe powder of -100 mesh and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95 ratio
Example mixing forms the mixed-powder of Fe-5.8%Si.Phosphoric acid and absolute ethyl alcohol are pressed 1.2:100 ratio is mixed to prepare passivation
Liquid.By passivating solution and the metal powder raw material weighed according to 0.6:1 ratio mixing, after stirring 1h with mixer, is put into baking
Case is passivated, and baking temperature is 42 DEG C, passivation time 6h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin
Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is
60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1:
0.7 ratio mixing, stirs 9h, then with ultrasonic disperse 10min, through screen filtration, that is made after vacuum outgas is uniform with mixer
The slurry of disperse, the viscosity of slurry is 55MPa.s.
Environment temperature is 30 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.3cm/s,
The height of scraper is 1.8mm, and width is about 120mm.
It is 30 DEG C to be cast biscuit drying temperature, relative humidity 50%, and the thickness of biscuit is 1.6mm after slurry drying.
Curing process is carried out under nitrogen atmosphere, solidification temperature is 160 DEG C, hardening time 4h, cools to room temperature with the furnace, and curtain coating slab is close
It spends for 6.4g/cm3。
Curtain coating slab is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 4 DEG C/min, and 3h, 400 DEG C of heat preservation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of heat preservations and burn
Tie 2h.Sintered blank density is 6.46g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1130 DEG C of heat preservation sintering 0.5h.With 8 DEG C/min speed continuous warmings.Specific pressure
Under-annealing schedule is：1.6mm → 1.22mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm is that is, cold through 7 times
It rolls with after 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.39g/cm3。
For above-mentioned cold rolling made-up belt in 1270 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.40g/cm to obtain thickness3, Si
Content is 5.8%, is the high silicon steel of single-phase homogeneous.
Claims (6)
1. a kind of method that powder tape casting prepares Fe-6.5%Si soft magnetic materials thin strips, it is characterised in that including following step
Suddenly：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, use Si contents as 70~80% HIGH-PURITY SILICON iron powder, grain size≤10 μm, major impurity is~0.25%Al ,~
0.08%Ca and~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, water atomization Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed, forms gold
Belong to powder raw material, phosphoric acid and absolute ethyl alcohol are pressed 0.8~2.0:100 ratio is mixed to prepare passivating solution, by passivating solution with weighing
Good metal powder raw material is 0.4~0.6 according to quality:1 ratio mixing after stirring 0.5~2h, is put into baking oven passivation, dries
Roasting temperature is 40~42 DEG C, and passivation time is 4~6h, obtains passivation powder.
Powder will be passivated with organic solution according to volume ratio 1:0.5~1 ratio mixing, stirs 6~12h with mixer, then uses
5~15min of ultrasonic disperse, through screen filtration, the slurry for the even dispersion made after vacuum outgas, the viscosity of slurry for 40~
80MPa.s；
(3) powder tape casting
During curtain coating environment temperature be 28~32 DEG C, will disperse slurry inject casting machine in, control casting machine speed be 0.1~
0.5cm/s, the height of scraper is 1.2~2.4mm, and width is 100~300mm；
It is 30~40 DEG C to be cast biscuit drying temperature, and relative humidity is 30~60%, and the thickness of biscuit is 0.95 after slurry drying
~1.96mm carries out curing process in a nitrogen atmosphere, and solidification temperature is 120~200 DEG C, and hardening time is 1~5h, with furnace cooling
But to room temperature, the dry curtain coating slab density of preparation is 6.2~6.6g/cm3；
(4) degreasing, sintering
Curtain coating slab is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The heating rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, it then will heat up to 1070~1170 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density are 6.3~6.7g/cm3；
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reach 30 through multi- pass rolling to total reduction~
After 45%, in sintering furnace, 0.5~2h is re-sintered in 1070~1170 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
0.1~0.5mm, density reach 7.36~7.48g/cm3；
(6) high temperature sintering is homogenized：
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1270~1340 DEG C of temperature ranges, it is real under the action of thermal diffusion
The homogenization of existing Si forms single-phase alloy, obtains the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering,
Density reaches 7.37~7.49g/cm3。
2. the method that powder tape casting as described in claim 1 prepares Fe-6.5%Si soft magnetic materials thin strips, feature exist
In：Organic solution described in step (2) is with 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is viscous using epoxy resin
Agent is tied, polyethylene glycol is plasticizer, and triethanolamine is dispersant, and the volume ratio of epoxy resin and polyethylene glycol presses 1:1, then press
Mixed solvent quality is 50~70%, and dispersant quality is 0.1%, and surplus is organic molten for the slurry that binding agent and plasticizer are formed
Body.
3. the method that powder tape casting as described in claim 1 prepares Fe-6.5%Si soft magnetic materials thin strips, feature
It is：With high-energy ball milling or rush rotation method obtain grain size≤10 μm HIGH-PURITY SILICON iron powder.
4. the method that powder tape casting as described in claim 1 prepares Fe-6.5%Si soft magnetic materials thin strips, feature
It is：Step (5) is sintered, by 5~10 when re-sintering for 1070~1170 DEG C under vacuum-sintering or restitutive protection's atmosphere
DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab in 0.1~1mm, soaking time is reduced to 0.5~
1h after sintered accumulation drafts reaches 30~45% every time, is sintered 1 time, is rolled from the biscuit of 0.95~1.96mm again
To 0.1~0.5mm, it is necessary to be sintered 4~8 times again.
5. the method that powder tape casting as described in claim 1 prepares Fe-6.5%Si soft magnetic materials thin strips, feature
It is：Overlapping places sintering plate during high temperature sintering, and interlayer is laid with MgO powder.
6. the method that powder tape casting as described in claim 1 prepares Fe-6.5%Si soft magnetic materials thin strips, feature
It is：Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
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| CN114260443A (en) * | 2021-11-25 | 2022-04-01 | 西安汇瑞丰科贸有限公司 | Ultrathin metal porous membrane material and strip for electric heating atomizer and production method |
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