CN107999758A - A kind of powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip - Google Patents

A kind of powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip Download PDF

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CN107999758A
CN107999758A CN201711369242.8A CN201711369242A CN107999758A CN 107999758 A CN107999758 A CN 107999758A CN 201711369242 A CN201711369242 A CN 201711369242A CN 107999758 A CN107999758 A CN 107999758A
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powder
sintering
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soft magnetic
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罗丰华
李东阳
张立平
李丹阳
白云波
李益民
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Central South University
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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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F1/0003—
    • 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
    • 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
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • 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
    • 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
    • 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
    • B22F3/12—Both compacting and sintering
    • B22F3/14—Both compacting and sintering simultaneously
    • B22F2003/145—Both compacting and sintering simultaneously by warm compacting, below debindering temperature
    • 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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  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention provides a kind of powder hot-pressing sintering preparation method of Fe 6.5%Si soft magnetic materials thin strips, uses water atomization Fe powder, Si powder as raw material, forms Fe Si mixed powders；Be molded squarely base, then using uniaxial compression mode under the conditions of 920~980 DEG C, 100~160MPa 0.5~2h of hot pressed sintering, the density of pressed compact is reached 6.70~7.02g/cm3；Then powder hot-pressing sintered blank is subjected to vacuum at 1080~1180 DEG C or protection of reducing atmosphere sinters; make Fe powder particles metallurgical bindings; and Si and Fe realize it is partially-alloyed; form the α Fe crystal grain of poor Si and the high silicon steel blank of heterogeneous structure of the high Si phases of brittleness, then multiple low-temperature diffusion-sintering and rolled thickness reduction；High temperature diffusion sintering finally is carried out at 1280~1350 DEG C, realizes homogeneous alloy, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.26g/cm3High silicon steel band.

Description

A kind of powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip
Technical field
The present invention principally falls into preparation and the manufacture field of metal material, and in particular to the powder hot-pressing of high silicon steel thin belt material The method of sintering and rolling deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis curve is very narrow, it and fundamental magnetization curve are almost Overlap, be 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.The maximum permeability of Fe-Si alloys does not have absolute predominance, such as slope in soft magnetic materials The maximum permeability of alloy can not reach 200000.But the Fe-Si lattens of Si ＜ 4.5% manufacture cost is low, 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 is with the increase of Si contents And reduce, disappear substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents, 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 amount or large-scale iron core are sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially It is to play particularly important role in the military aviation such as spacecraft, submarine and guided missile field, Fe-Si systems alloy.20th century 60 Age Mo, the alloy of Si contents 6.5% are appeared on No. 11 airships of Apollo as transformer material, are completed the mankind and are landed on the moon first 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 studies discovery first, and 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 there is the magnetic conductivity of lower iron loss and higher.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 is the No yield point 6.5%Si steel discs of 400mm to spend for 0.1~0.5mm, width.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 alloy is reached required content to alloy diffusion inside by elevated 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 Ask, 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 ", its 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, its 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 produce huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip, It is the problem of being difficult to shaping for Fe-4.5~6.7%Si alloy thin band materials, uniform with water atomization Fe powder and fine simple substance Si powder Mixing, green compact are molded into after adding binder, then prepare certain thickness slab using powder hot-pressing sintering method, utilize powder The emollescence to Fe powder of last hot pressed sintering causes green density to improve, and realizes slight alloying under thermal diffusion effect, Form the complex tissue of Fe particles and the high Si phases of brittleness with plastic deformation ability.Subsequently after multi-pass cold rolling-sintering Thin plate is obtained, progressively promotes the alloying of Si, is finally sintered using High temperature diffusion and obtains the fine and close high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions：Subsphaeroidal water atomization Fe powder, fine Si powder are used as original Feed powder end, forms Fe-4.5~6.7%Si mixed powders.Fine Si powder is being mixed by suitable bonding agent, dispersant During adhere to water-atomized iron powder surface.Since water atomization Fe powder is the big particle with high-compressibility, in mixed powder Occupy larger volume ratio, its plastic deformation ability is not significantly reduced after adding Si powder, can be by being molded squarely base.Adopt again With uniaxial compression mode under the conditions of 920~980 DEG C, 100~160MPa 0.5~2h of hot pressed sintering, reach the density of pressed compact 6.70~7.02g/cm3.Then powder hot-pressing sintered blank is subjected to vacuum or reducing atmosphere in 1080~1180 DEG C of temperature ranges Protection sintering, makes Fe powder particles metallurgical bindings, and Si and Fe realize it is partially-alloyed, formed it is fine and close, there is plastic deformation ability The high silicon steel blank of heterogeneous structure of the high Si phases of α-Fe crystal grain and brittleness of the poor Si of power.Burnt subsequently through multiple cold rolling, low temperature diffusion Knot, the density rise of slab, plate thickness are reduced, and the alloying level of Si is also continuously improved.Finally in 1280~1350 DEG C of temperature In the range of vacuum or protection of reducing atmosphere sintering, the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, obtains and contains 4.5 0.1~0.5mm of~6.7%Si is thick, density >=7.26g/cm3High silicon steel band.
The method 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, the simple substance Si powder of particle diameter≤3 μm, purity be more than 97%, mainly containing Fe, Al, Ca and other inevitably it is miscellaneous Matter.
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 the compressibility and mobility of higher, is conducive to the Uniform Flow of powder extrusion process course powder.Water atomization Fe powder In low impurity content it is favourable to the soft magnetic characteristic of high silicon steel.
The property of simple substance Si is very crisp, it is easy to is refined by Mechanical Crushing technique.The elemental silicon for choosing 3 μm of particle diameter ＜ is favourable In the realization of subsequently homogenization diffusion-sintering；And hole that tiny Si is formed in blank, brittle interface are also tiny, play The Strengthening and Toughening effect of structure refinement, is conducive to improve follow-up blank toughness, is not easily caused in extruding, rolling densification process Cracking.But Si is easily absorbing oxygen, SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder In, and inert gas shielding should be used in follow-up batch mixing, heating, powder hot-pressing sintering process, used instrument is also necessary Take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as other Al, Ca, Mn to alloy magnetic property is little, during The possibility for introducing 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 Si powder are weighed；Using low under inert protective atmosphere Energy hybrid machine mixes, and mixing velocity and time, the mitigation Fe powder that should try one's best occurred in mixed process depending on mixing uniformity Processing hardening.
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.34~6.51g/cm3.By pressed compact in 920 0.5~2h of hot pressed sintering at~980 DEG C, makes the density of pressed compact reach 6.70~7.02g/cm3。
Decline the plasticity of plate after hot pressed sintering in order to avoid alloying, relatively low heating is have selected before hot pressed sintering Temperature.Alloy is regarded as the composite material of simple substance Fe particles and richness Si phase compositions after sintering, possesses the high-plastic of pure Fe crystal grain Property characteristic, three point bending test show plasticity, and bending strength reaches 120~227MPa.
(4) cold rolling-sintering
By above-mentioned hot pressed sintering plate cold rolling-sintering, progressively it is thinned, single pass rolling reduction≤8%, through multi- pass rolling to always After reduction ratio reaches 30~50%, then in 1080~1180 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering in sintering furnace Afterwards, the thickness of plate reaches 0.1~0.5mm.It is gradually completing with the alloying of Si, strip density improves, reach 7.24~ 7.38g/cm3。
There are a large amount of deformable Fe phases in blank, slab can bear cold-rolling deformation.But there is also more in slab High Si phases, its performance is more crisp, therefore amount cannot be too high under every time rolling, and accumulation total reduction reaches 30~50%, takes around 8 ~25 passages.
Since existing hard crisp phase, cold deformation process can form some micro-cracks.In order to realize the closing of pores and crackle Repair, and the homogenization diffusion of a degree of Si elements.Cold rolling reduction accumulation needs to sinter 1 again to a certain extent afterwards It is secondary, 0.1~0.5mm is rolled down to from 36~54mm hot pressed sintering plates, takes around and sinters 12~20 times again.
Sintering temperature is too low, is unfavorable for metallurgical binding and the Si element thermal diffusions of Fe powder particles；And sintering temperature is excessive then Si elements can be caused quickly to spread, cause crystal grain excessive high hardness, embrittlement, follow-up rolling deformation is difficult to realize.
Take reproducibility, inert gas shielding or vacuum-sintering.W, Mo, heat resisting steel etc. can be used during sintering as support Plate (or burning boat), can also use the ceramic wafers such as corundum, zirconium oxide, but metallic plate thermal conductivity is good, and be beneficial to Even Sintering.
The texture of coarse crystal containing the second phase is formed after sintering.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) Phase, body-centred cubic several characteristic peaks have obvious separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, wherein must There are the Si contents in a kind of Fe phases low, there is plastic deformation ability.
(5) full alloying high temperature sintering：
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, in the effect of thermal diffusion Under, to realize the full alloyings of Si, form 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 brings up to 7.26~7.40g/cm3。
The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
The simple substance silica flour of particle diameter≤3 μm described in step (1) is by high-energy ball milling or rushes the acquisition of rotation method.
Step (3) prepares square pressed compact using compression-moulding methods, is pressed using hydraulic press on the surface of 400~600MPa Under power, square pressed compact is obtained, pressed compact length and width is respectively 100~300mm, is highly 40~60mm；It is put into the oxidation of same size Aluminium compacting tool set, using hot-pressed sintering furnace, the uniaxial compression mode of 100~160MPa, under hydrogen shield effect, in 920~ 0.5~2h of hot pressed sintering at 980 DEG C, slab three point bending test shows as plasticity after hot pressed sintering, bending strength for 120~ 227MPa。
It is water-insoluble total as binder, the additive amount of binder to add cellulose, paraffin micro mist or zinc stearate during mixing 0.8% of amount no more than mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding The effect of Fe-Si powder, enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed-powder gross mass 2%.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo and ceramics can be used to burn Boat.But plate must tile placement, tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of element such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel Large effect, can subsequently be annealed, the technological means such as normalizing treatment is controlled by by wet hydrogen.
Essence of the invention is by with the addition of certain body in the water atomization Fe powder of the big volumetric portion with good plasticity The fine Si powder of simple substance of product ratio, forms Fe-4.5~6.7Si% mixtures.After powder hot-pressing sintering, fine and close soft Fe is formd Particle and the composite material of hard crisp richness Si phase compositions, have higher deformation at room temperature ability.Subsequently through multi-pass cold rolling and burning Knot, further improves structural homogenity and compactness, then by similar to CVD high-temperature diffusion process, realizing the homogenization of Si, from And obtain the single-phase high silicon steel band of high quality.This method realizes Technics Process Automation, continuous by technique and equipment Design Metaplasia is produced, and can be mass-produced 0.1~0.5mm thickness, density >=7.26g/cm3High silicon steel band.
Brief description of the drawings
Fig. 1 is the three-point bending curve map of blank after the powder hot-pressing of the embodiment of the present invention 1 sinters.
Fig. 2 is metallographic structure figure after powder hot-pressing sintering-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 3 is XRD diffraction curve figures after powder hot-pressing sintering-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 4 is XRD diffraction curve figures after powder hot-pressing sintering-cold rolling-high temperature sintering of the embodiment of the present invention 4.
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment
Embodiment 1
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.3:6.7 ratio mixing, forms The mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol is pressed Added according to 200ml/ tons of amounts.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Prepare square pressed compact using compression-moulding methods, surface pressing 600MPa, pressed compact size for 100 × 100 × 40mm, green density 6.34g/cm3。
The uniaxial compression hot pressed sintering of 100MPa, the hot pressed sintering 2h at 920 DEG C, the thickness of blank are about 36mm, density Reach 6.70g/cm3.Three point bending test shows plasticity, sees Fig. 1, and bending strength reaches 120MPa.
By above-mentioned hot pressed sintering plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is：36mm→24mm→ 17mm→12mm→9.5mm→7.2mm→5mm→3.5mm→2.4mm→1.6mm→1.02mm→1.02mm→0.71mm→ 0.49mm, i.e., sinter through 13 cold rollings and 12 times.
Multi-pass cold rolling is thick in 1080 DEG C of heat preservation sintering 2h, plate to after 30~50%, then in vacuum sintering furnace Degree is thinned to 0.49mm, and density reaches 7.22g/cm3。
1h is sintered in 1350 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches 7.24g/cm3, Si contents are 6.7%.
Embodiment 2
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 95.5:4.5 ratio mixing, forms The mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol is pressed Added according to 400ml/ tons of amounts.Using drum mixer by above-mentioned powder mixing 6h.
Prepare square pressed compact using compression-moulding methods, surface pressing 400MPa, pressed compact size for 300 × 300 × 60mm, green density 6.51g/cm3。
The uniaxial compression hot pressed sintering of 160MPa, the hot pressed sintering 0.5h at 980 DEG C, the thickness of blank is about 54mm, close Degree reaches 7.02g/cm3.Three point bending test shows plasticity, and bending strength reaches 227MPa.
By above-mentioned hot pressed sintering plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is：54mm→36mm→ 36mm→24mm→17mm→12mm→9.5mm→7.2mm→5mm→3.5mm→2.4mm→1.6mm→1.02mm→ 1.02mm → 0.71mm → 0.49mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., through 20 cold rollings and 19 sintering.
Multi-pass cold rolling is to after 30~50% total reductions, then is burnt in hydrogen shield sintering furnace in 1180 DEG C of insulations 0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.37g/cm3。
The texture of coarse crystal containing the second phase is formed after sintering, sees Fig. 2.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) phase, as seen in Figure 3, body-centred cubic several characteristic peaks have obvious separating phenomenon, illustrate there are Si solid solubility it is different 2 Kind Fe phases, wherein must have the Si contents in a kind of Fe phases low, have plastic deformation ability.
4h is sintered in 1280 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches 7.40g/cm3, Si contents are 4.5%.
Embodiment 3
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.5:6.5 ratio mixing, forms The mixed-powder of Fe-6.5%Si.The paraffin micro mist of addition raw material total amount 0.4% during mixing, 0.2% methylcellulose, 0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 6h.
Prepare square pressed compact using compression-moulding methods, surface pressing 500MPa, pressed compact size for 120 × 120 × 50mm, green density 6.39g/cm3。
The uniaxial compression hot pressed sintering of 140MPa, the hot pressed sintering 1.5h at 930 DEG C, the thickness of blank is about 46mm, close Degree reaches 6.75g/cm3.Three point bending test shows plasticity, and bending strength reaches 169MPa.
By above-mentioned hot pressed sintering plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is：46mm→36mm→ 24mm→17mm→12mm→9.5mm→7.2mm→5mm→3.5mm→2.4mm→1.6mm→1.02mm→1.02mm→ 0.71mm → 0.49mm → 0.39mm → 0.27mm, i.e., sinter through 16 cold rollings and 15 times.
Multi-pass cold rolling is to after 30~50% total deformations, then is burnt in nitrogen protective sintering stove in 1150 DEG C of insulations 1h is tied, sheet metal thickness is thinned to 0.27mm, and density reaches 7.29g/cm3。
2h is sintered in 1320 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.27mm, density reaches To 7.31g/cm3, Si contents are 6.5%,
Embodiment 4
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 94.2:5.8 ratio mixing, forms The mixed-powder of Fe-5.8%Si.The paraffin micro mist of raw material total amount 0.6%, 0.2% machine oil are added during mixing.Absolute ethyl alcohol is pressed Added according to 400ml/ tons of amounts.Using drum mixer by above-mentioned powder mixing 3h.
Prepare square pressed compact using compression-moulding methods, surface pressing 500MPa, pressed compact size for 180 × 180 × 50mm, green density 6.43g/cm3。
The uniaxial compression hot pressed sintering of 150MPa, the hot pressed sintering 1h at 950 DEG C, the thickness of blank are about 52mm, density Reach 6.79g/cm3.Three point bending test shows plasticity, and bending strength reaches 196MPa.
By above-mentioned hot pressed sintering plate cold rolling-sintering, specific pressure-annealing schedule, which is progressively thinned, is：52mm→39mm→ 26mm→18mm→13mm→10.5mm→8.2mm→5mm→3.2mm→2.4mm→2.0mm→1.3mm→0.90mm→ 0.63→0.43mm→0.32mm→0.21mm.Sintered through 17 cold rollings and 16 times.
Multi-pass cold rolling is to after 30~50% total deformations, then is burnt in hydrogen shield sintering furnace in 1120 DEG C of insulations 1h is tied, sheet metal thickness is thinned to 0.21mm, and density reaches 7.33g/cm3。
2h is sintered in 1300 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.21mm, density reaches To 7.34g/cm3, Si contents are 5.8%, and the XRD analysis figure of its final plate is shown in Fig. 4, is the high silicon steel of single-phase homogeneous.

Claims (7)

1. a kind of powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip, 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, with the simple substance Si powder of particle diameter≤3 μm, purity is more than 97%, mainly containing Fe, Al, Ca and other inevitable impurity；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, water atomization Fe powder and fine Si powder are weighed；Using low under inert protective atmosphere Energy hybrid machine mixes；
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.34~6.51g/cm3, it is hot at 920~980 DEG C Pressure 0.5~2h of sintering, makes the density of pressed compact reach 6.70~7.02g/cm3；
(4) cold rolling-sintering
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to total reduction After reaching 30~50%, then in sintering furnace after 1080~1180 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering, plate Thickness reach 0.1~0.5mm, density reaches 7.24~7.38g/cm3；
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, it is real under the action of thermal diffusion The existing full alloyings of Si, form single-phase alloy, and the thickness of plate is 0.1~0.5mm after densification sintering, and density reaches 7.26~ 7.40g/cm3。
2. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：The simple substance Si powder of particle diameter≤3 μm is by high-energy ball milling or rushes the acquisition of rotation method.
3. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：Step (3) prepares square pressed compact using compression-moulding methods, using hydraulic press 400~600MPa surface pressing Under, square pressed compact is obtained, pressed compact length and width is respectively 100~300mm, is highly 40~60mm；It is put into the aluminium oxide of same size Compacting tool set, using hot-pressed sintering furnace, the uniaxial compression mode of 100~160MPa, under hydrogen shield effect, in 920~980 0.5~2h of hot pressed sintering at DEG C, slab three point bending test shows as plasticity after hot pressed sintering, bending strength for 120~ 227MPa。
5. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：Add that cellulose, paraffin micro mist or zinc stearate are water-insoluble as binder, and the additive amount total amount of binder is not during mixing More than the 0.8% of mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding Fe-Si The effect of powder, enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed-powder gross mass 2%.
6. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the powder hot-pressing sintering preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature It is：During high temperature sintering described in step (5), overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, in plate Tablet weight is placed on material, prevents from deforming in sintering process.
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