CN108044097A - A kind of method that powder extruding prepares single-phase Fe-6.5%Si silicon steel - Google Patents

A kind of method that powder extruding prepares single-phase Fe-6.5%Si silicon steel Download PDF

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CN108044097A
CN108044097A CN201711368374.9A CN201711368374A CN108044097A CN 108044097 A CN108044097 A CN 108044097A CN 201711368374 A CN201711368374 A CN 201711368374A CN 108044097 A CN108044097 A CN 108044097A
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powder
sintering
silicon steel
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extrusion
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罗丰华
周浩钧
李益民
白云波
赵甲正
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Central South University
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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
    • 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
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • B22F2003/208—Warm or hot extruding
    • 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
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

A kind of method that powder extruding prepares single-phase Fe 6.5%Si silicon steel, using reduction Fe powder, Si powder is raw material powder, forms Fe 4.5~6.7%Si mixed powders.Squarely base is molded, is heated to 950~1050 DEG C of realization Fe phase austenitizings, slab is hot extruded into the deflection that extrusion ratio is 8~16.Then powder is squeezed into slab and vacuum or protection of reducing atmosphere sintering is carried out at 1080~1180 DEG C; Fe powder particles is made to realize metallurgical binding; and Si and Fe realizations are 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; multiple cold rolling, low temperature diffusion sintering again, are sintered in 1280~1350 DEG C of vacuum or protection of reducing atmosphere, realize the homogeneous alloy of high silicon steel; it is thick to obtain 0.1~0.5mm containing 4.5~6.7%Si, density >=7.37g/cm3High silicon steel band.

Description

A kind of method that powder extruding prepares single-phase Fe-6.5%Si silicon steel
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder metallurgy of high silicon steel thin belt material is burnt The method of knot, hot extrusion and rolling deformation.
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 the method that a kind of extruding of powder prepares single-phase Fe-6.5%Si silicon steel, for 4.5~ The problem of Fe-Si alloy thin band materials of 6.7%Si contents are difficult to shape uniformly is mixed with reducing Fe powder with fine simple substance Si powder It closes, extruding green compact is molded into after adding binder, then certain thickness slab is prepared using powder hot-extrusion method, utilize heat The large deformation of extruding, which acts on, causes the raising of extruded stock density, structure refinement, and realizes partially-alloyed, shape under thermal diffusion effect Into the heterogeneous structure of the high Si phases of α-Fe crystal grain and brittleness of the poor Si of plastic deformation ability.Subsequently pass through multi-pass cold rolling-sintering After obtain thin plate, finally using High temperature diffusion be sintered obtain the high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions：Using the reduction Fe powder of irregular pattern, fine Si powder is Raw material powder forms Fe-4.5~6.7%Si mixed powders.By suitable bonding agent, dispersant by fine Si powder mixed It is adhered to during closing in the hole of reduced iron powder surface or filling ferrous powder.Since reduction Fe powder is with the coarse of high-compressibility Particle occupies larger volume ratio in mixed powder, does not significantly reduce its plastic deformation ability after adding Si powder, can pass through mould It is pressed into square base.950~1050 DEG C of realization Fe phase austenitizings are heated to, with the deflection hot extrusion that extrusion ratio is 8~16 Into slab.Then powder is squeezed into slab and carries out vacuum or protection of reducing atmosphere sintering in 1080~1180 DEG C of temperature ranges, made Fe powder particles realize metallurgical binding, and Si and Fe realize it is partially-alloyed, formed it is fine and close, have the poor Si's of plastic deformation ability The high silicon steel blank of heterogeneous structure of α-Fe crystal grain and the high Si phases of brittleness.It is sintered subsequently through multiple cold rolling, low temperature diffusion, slab Density rise, plate thickness are reduced, and the alloying level of Si is also continuously improved.The finally vacuum in 1280~1350 DEG C of temperature ranges Or protection of reducing atmosphere sintering, the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, is obtained containing 4.5~6.7%Si 0.1~0.5mm it is thick, 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 reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is the impurity such as Si, Mn, P, S, middle grain size Positioned at 75~106 μm；With the simple substance Si powder of grain size≤3 μm, purity is more than 97%, mainly containing impurity such as Fe, Al, Ca.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to Fine silica powder, and in follow-up powder extrusion process also being mutually twisted for powder easy to implement and improve the intensity of green compact.
The property of simple substance Si is very crisp, it is easy to be refined by Mechanical Crushing technique.The elemental silicon for choosing 3 μm of grain size ＜ 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 subsequent blank toughness, is squeezing, is not being easily caused in rolling densification process Cracking.But Si is easily absorbing oxygen, and SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder In and follow-up batch mixing, heating, powder hot extrusion process in should use inert gas shielding, used instrument also must be pre- First take dehydration, drying process.
On the premise of oxygen content is controlled, influence of the impurity such as other Al, Ca, Mn to alloy magnetic property is little, in the process The possibility for introducing other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and fine Si powder are weighed；It is used under inert protective atmosphere The low energy mixers such as conical mixer, V-arrangement batch mixer or drum mixer mix, and mixing velocity and time regard and is uniformly mixed Property depending on, should try one's best mitigate Fe powder occurs in mixed process processing hardens.
(3) powder squeezes
Square green compact is prepared using compression-moulding methods, green density is 6.32~6.49g/cm3；Using square extruding Cylinder, extrusion ratio are 8~16, using sintered-carbide die, lubricant are done with machine oil and glass dust, by molding square billet in nitrogen before squeezing Be heated to 950~1050 DEG C under gas shielded effect, keep the temperature 2~4h, extrusion cylinder and extrusion die 400~600 DEG C of preheating insulations 1~ 2h implements hot extrusion, and the density of slab is 6.77~7.09g/cm after hot extrusion3；
(4) it is sintered
Hot extrusion pressing plate is placed on surface to be coated in the support plate of MgO micro mists, is placed into sintering furnace.Using 2~5 DEG C/heating rate of min, it is warming up to 1080~1180 DEG C of 2~4h of heat preservation sintering.Sintered blank density is 7.20~7.32g/cm3。 Compared with extruded stock density, density slightly reduces.
Sintering temperature is too low, is unfavorable for the metallurgical binding of Fe powder particles and Si element thermal diffusions；And sintering temperature is excessively high then Si elements can be caused quickly to spread, cause crystal grain excessive high hardness, embrittlement, follow-up rolling deformation is difficult to realize.
Reproducibility or inert gas shielding is taken to be sintered.Can be used during sintering W, Mo, heat resisting steel etc. as support plate (or Burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity is good, and 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 apparent separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, wherein must Have that the Si contents in a kind of Fe phases are low, there is plastic deformation ability.
(5) cold rolling-sintering densification
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure After lower rate reaches 30~45%, then in 1080~1180 DEG C of 0.5~2h of heat preservation sintering in sintering furnace.After multiple cold rolling-sintering, The thickness of plate reaches 0.1~0.5mm, and density reaches 7.36~7.48g/cm3。
Cold-rolling deformation can be born since there are deformable Fe phases, slab in blank.But there is also more in slab High Si phases, performance is more crisp, therefore for amount not above 8%, accumulation total reduction reaches 30~45%, about needs under every time rolling Want 8~20 passages.
Due to existing hard crisp phase, it is necessary to take and keep the temperature vacuum-sintering or restitutive protection again at 1080 DEG C~1180 DEG C Atmosphere sintering, to realize that the closing of pores and the reparation of crackle and a degree of Si elements are generated in cold-rolled process to be homogenized Diffusion., it is necessary to be sintered 1 time again, from the hot extrusion of 2.5~5.0mm after sintered accumulation drafts reaches 30~45% every time Pressing plate material is rolled down to 0.1~0.5mm, takes around and is sintered 6~10 times again.
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, in thermal diffusion Under effect, the homogenization of Si is realized, form single-phase alloy.The thickness of plate is almost unchanged after densification sintering, be 0.1~ 0.5mm, density reach 7.37~7.49g/cm3。
The simple substance Si powder high-energy ball milling of grain size≤3 μm rushes the methods of rotation method and obtains.
Low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
The square green compact height control of step (3) is in 40mm, and the total output pressure of press is up to 576 tons, corresponding surface pressure For 600MPa, the size of the green compact of acquisition is 40 × 80 × 120mm, using the square extrusion cylinder of 40 × 120mm, extrusion die difference For 5~2.5mm × 120mm, corresponding extrusion ratio is 8~16, implements hot extrusion, 3 points of slab after hot extrusion using 300 tons of press Bend test shows plasticity, and bending strength is 77~230MPa.
Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during mixing, the additive amount total amount of binder is not It more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays 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%.
Support plate described in step (4) using the support plate described in step (4) using molybdenum plate, W plates, heat resisting steel, corundum or Zirconia ceramics plate.
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 means such as normalizing treatment are controlled by.
Essence of the invention is by being with the addition of low volume ratio in the reduction Fe powder of the big volumetric portion with good plasticity The fine Si powder of simple substance of example forms Fe-4.5~6.7%Si mixed powders.High density, high uniformity plate are obtained using hot extrusion Base.The element alloyed degree of slab Si is low, and microscopic structure is had high by high-ductility Fe phases and brittleness richness Si phase compositions Cold deformation ability can be improved structural homogenity and compactness, then High temperature diffusion sintering, realized by multi-pass cold rolling and sintering The homogenization of Si, so as to obtain the high silicon steel band of high quality.This method realizes technical process certainly by technique and equipment Design Dynamicization, 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 three-point bending graph of blank after the powder of the embodiment of the present invention 1 squeezes；
Fig. 2 is metallographic structure figure after powder extruding-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 3 is XRD diffraction curve figures after powder extruding-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 4 is XRD diffraction curve figures after powder extruding-cold rolling-high temperature sintering of the embodiment of the present invention 4.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤3 μm according to 93.3:6.7 ratio mixing, forms Fe- The mixed-powder of 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 according to 200ml/ tons of amount addition.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly 40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is 6.32g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 5 × 120mm, and corresponding extrusion ratio is 8.It will before squeezing Molding square billet is heated to 950 DEG C under nitrogen protective effect, keeps the temperature 4h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.It adopts Implement hot extrusion with 300 tons of press, the density of slab is 6.77g/cm after hot extrusion3, three point bending test shows plasticity, sees Fig. 1, bending strength 77MPa.
Using the heating rate of 2 DEG C/min, 1080 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.20g/cm3.It burns The texture of coarse crystal containing the second phase is formed after knot.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure After lower rate reaches 30~45%, then in 1080 DEG C of heat preservation sintering 2h in sintering furnace.Specifically pressure-annealing schedule is：5mm→ 3.5mm → 2.4mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate Reach 0.49mm, density reaches 7.36g/cm3。
1h finally is sintered in 1350 DEG C of Temperature Vacuums, under the action of thermal diffusion, the homogenization of Si is realized, forms single-phase conjunction Gold obtains the high silicon steel of homogeneous.The thickness of plate is almost unchanged after densification sintering, is 0.49mm, and density reaches 7.37g/cm3。
Embodiment 2
By the reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤3 μm according to 95.5:4.5 ratio mixing, forms Fe- The mixed-powder of 4.5%Si.The zinc stearate of raw material total amount 0.6%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol according to 400ml/ tons of amount addition.Using drum mixer by above-mentioned powder mixing 6h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly 40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is 6.49g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 2.5 × 120mm, and corresponding extrusion ratio is 16.It will before squeezing Molding square billet is heated to 1050 DEG C under nitrogen protective effect, keeps the temperature 2h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h. Implement hot extrusion using 300 tons of press, the density of slab is 7.09g/cm after hot extrusion3, three point bending test shows plasticity, Bending strength is 230MPa.
Using the heating rate of 2 DEG C/min, 1180 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.32g/cm3.It burns The texture of coarse crystal containing the second phase is formed after knot, sees Fig. 2.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) phase, such as Fig. 3 findings, body-centred cubic several characteristic peaks have apparent separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, In must have that the Si contents in a kind of Fe phases are low, there is plastic deformation ability.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure After lower rate reaches 30~45%, then in 1180 DEG C of heat preservation sintering 0.5h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate Degree reaches 0.1mm, and density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is：2.5mm→1.85mm→1.39mm→ 1.15mm → 0.89mm → 0.65mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., through 10 cold rollings and After 9 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.48g/cm3。
4h finally is sintered in 1280 DEG C of Temperature Vacuums, forms the high silicon steel of single-phase homogeneous that Si contents are 4.5%, thickness is 0.1mm, density reach 7.48g/cm3。
Embodiment 3
By the reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤3 μm according to 93.5:6.5 ratio mixing, forms Fe- The mixed-powder of 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.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly 40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is 6.38g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 4 × 120mm, and corresponding extrusion ratio is 10.By mould before squeezing Pressure square billet is heated to 1000 DEG C under nitrogen protective effect, keeps the temperature 3h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.It adopts Implement hot extrusion with 300 tons of press, the density of slab is 6.84g/cm after hot extrusion3, bending strength 120MPa.
Using the heating rate of 3 DEG C/min, 1150 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.24g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, and specific cold rolling-sintering schedule is：4.0mm→2.8mm→ 2.0mm → 1.40mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 7 cold rollings and 6 sintering, the thickness of plate Degree reaches 0.27mm, and density reaches 7.39g/cm3。
For above-mentioned cold rolling made-up belt in 1280 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.40g/cm to obtain thickness3, Si Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤3 μm according to 94.2:5.8 ratio mixing, forms Fe- The mixed-powder of 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 according to 400ml/ tons of amount addition.Using drum mixer by above-mentioned powder mixing 3h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly 40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is 6.30g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 3.2 × 120mm, and corresponding extrusion ratio is 12.5.It squeezes Molding square billet under nitrogen protective effect is heated to 1020 DEG C before pressure, keeps the temperature 4h.Extrusion cylinder and extrusion die are protected in 600 DEG C of preheatings Warm 2h.Implement hot extrusion using 300 tons of press, the density of slab is 6.92g/cm after hot extrusion3, bending strength 160MPa.
Using the heating rate of 4 DEG C/min, 1120 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.40g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure After lower rate reaches 30~45%, then in 1120 DEG C of heat preservation sintering 1h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate Reach 0.22mm, density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is：3.2mm→2.4mm→2.0mm→1.3mm→ 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., after 9 cold rollings and 8 sintering, the thickness of plate reaches 0.21mm, density reach 7.46g/cm3。
For above-mentioned cold rolling made-up belt in 1280 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.41g/cm to obtain thickness3, Si Content is 5.8%, and the XRD analysis figure of final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.

Claims (7)

1. a kind of method that powder extruding prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that include the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining for Si, Mn, P, S and other inevitably Impurity；The simple substance Si powder of grain size≤3 μm, purity is more than 97%, containing Fe, Al and Ca and other inevitable impurity；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and fine Si powder are weighed；Low energy is used under inert protective atmosphere Mixer mixes；
(3) powder squeezes
Square green compact is prepared using compression-moulding methods, green density is 6.32~6.49g/cm3；Using square extrusion cylinder, squeeze Pressure ratio is 8~16, and using sintered-carbide die, lubricant is done with machine oil and glass dust, protects molding square billet in nitrogen before squeezing 950~1050 DEG C are heated under shield effect, keep the temperature 2~4h, extrusion cylinder and extrusion die in 400~600 DEG C of 1~2h of preheating insulation, Implement hot extrusion, the density of slab is 6.77~7.09g/cm after hot extrusion3；
(4) it is sintered
Hot extrusion pressing plate is placed on surface to be coated in the support plate of MgO micro mists, is placed into sintering furnace, using 2~5 DEG C/min Heating rate, be warming up to 1080~1180 DEG C of 2~4h of heat preservation sintering, sintered blank density is 7.20~7.32g/cm3；It takes also Originality or inert gas shielding sintering；
(5) cold rolling-sintering densification
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 30~45%, then in 1080~1180 DEG C of 0.5~2h of heat preservation sintering, after multiple cold rolling-sintering, plate in sintering furnace Thickness reach 0.1~0.5mm, density reaches 7.36~7.48g/cm3；
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, in the effect of thermal diffusion Under, it realizes the homogenization of Si, forms single-phase alloy, the thickness of plate is 0.1~0.5mm after densification sintering, and density reaches 7.37~7.49g/cm3。
2. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that described Low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
3. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, characterization step (1) are described Grain size≤3 μm simple substance silica flour using high-energy ball milling or rush rotation method acquisition.
4. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Square pressure Base height is controlled in 40mm, and the total output pressure of press is up to 576 tons, and corresponding surface pressure is 600MPa, the green compact of acquisition Size is 40 × 80 × 120mm, and using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 5~2.5mm × 120mm, right It is respectively 8~16 to answer extrusion ratio, implements hot extrusion using 300 tons of press, slab three point bending test shows to mould after hot extrusion Property, bending strength is 77~230MPa.
5. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Step (2) cellulose, paraffin micro mist or zinc stearate water-insoluble binder are added when mixing, the additive amount total amount of binder, which is no more than, mixes The 0.8% of powder gross mass is closed, while adds grease and absolute ethyl alcohol does passivator, passivation Si powder, bonding Fe-Si powder is played, increases The effect of strong powder flowbility and compact strength, the additive amount total amount of passivator are no more than the 2% of mixed-powder gross mass.
6. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Step (4) support plate described in uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the method that powder extruding as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Step (6) during high temperature sintering described in, overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, placed on plate Tablet weight prevents from deforming in sintering process.
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