CN107829036A - A kind of powder hot-pressing sintering manufacture method of high silicon steel thin belt material - Google Patents

A kind of powder hot-pressing sintering manufacture method of high silicon steel thin belt material Download PDF

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CN107829036A
CN107829036A CN201711369219.9A CN201711369219A CN107829036A CN 107829036 A CN107829036 A CN 107829036A CN 201711369219 A CN201711369219 A CN 201711369219A CN 107829036 A CN107829036 A CN 107829036A
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sintering
powder
hot
silicon steel
high silicon
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CN107829036B (en
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罗丰华
黄小琴
罗硕
廖相巍
李益民
于童童
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Central South University
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Central South University
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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
    • 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
    • B22F3/02—Compacting only
    • 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
    • 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
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0264—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements the maximum content of each alloying element not exceeding 5%
    • C22C33/0271—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements the maximum content of each alloying element not exceeding 5% with only C, Mn, Si, P, S, As as alloying elements, e.g. carbon steel
    • 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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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

A kind of powder hot-pressing sintering manufacture method of high silicon steel thin belt material, using reduction Fe powder, fine Si contents are 70~80% HIGH-PURITY SILICON iron powder, form Fe Si mixed powders.Be molded squarely base, then using single shaft pressuring method under the conditions of 920~980 DEG C, 100~160MPa 0.5~2h of hot pressed sintering, green density is reached 6.69~7.01g/cm3；Hot pressed sintering base is carried out to vacuum or protection of reducing atmosphere sintering at 1060~1160 DEG C, makes Fe powder particles metallurgical bindings, the high silicon steel blank of heterogeneous structure of Si phases, then multiple low-temperature diffusion-sintering and rolled thickness reduction；High temperature diffusion sintering finally is carried out at 1260~1320 DEG C, realizes homogeneous alloy, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.25g/cm3High silicon steel band.

Description

A kind of powder hot-pressing sintering manufacture method of high silicon steel thin belt material
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, and it and fundamental magnetization curve are almost Overlap, be mainly used in 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 (as follows) 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 Si ＜ 4.5% Fe-Si latten manufacturing costs are 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%, wherein commonly referred to as high silicon steel, 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, disappeared substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increased 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 be due to 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.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 lower iron loss and higher magnetic conductivity.Hereafter between many decades, in order to overcome the fragility 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), 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.Japanese NKK companies in 1988 have produced thickness for the first time using CVD technology It is 400mm No yield point 6.5%Si steel discs 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。
CVD principle 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 cost are high, operating environment and its severe, it is impossible to meet ring Guaranteed request.
High silicon steel is " the steel art work ", and its technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and It is the focus of development and exploitation.For the high silicon steel of 6.5%Si, 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 technology and ripe and can be cost-effectively Production, it is that 6.5%Si high silicon steel move towards to be commercialized wide variety of key, the also always emphasis of research work.Once grope Go out simple, economic, effective, ripe preparation technology, will just produce huge economic benefit and social benefit.
The content of the invention
The purpose of the present invention be a kind of high silicon steel thin belt material powder hot-pressing sintering manufacture method, for Fe-4.5~ 6.7%Si alloy thin band materials be difficult to shaping the problem of, using reduce Fe powder with it is equal as 70~80% HIGH-PURITY SILICON iron powder with Si contents Even mixing, green compact are molded into after adding binder, then certain thickness slab is prepared using powder hot-pressing sintering method, utilized The emollescence to Fe powder of powder hot-pressing sintering causes green density to improve, and realizes slight alloy under thermal diffusion effect Change, form the complex tissue of Fe particles and the high Si phases of fragility with plastic deformation ability.Subsequently pass through multi-pass cold rolling-sintering After obtain thin plate, progressively promote Si alloying, finally sintered using High temperature diffusion and obtain the fine and close high silicon strip of homogeneous single phase Material.
The present invention is achieved by the following technical solutions：Using the reduction Fe powder of irregular pattern, fine Si contents It is raw material for 70~80% HIGH-PURITY SILICON iron powder, forms Fe-4.5~6.7%Si mixed powders.By suitable bonding agent, divide Powder adheres to fine HIGH-PURITY SILICON iron powder in the hole of reduced iron powder surface or filling ferrous powder in mixed process.Due to also Former Fe powder is the big particle with high-compressibility, occupies larger volume ratio in mixed powder, is added not notable after ferrosilicon powder Its plastic deformation ability is reduced, can be by being molded squarely base.Again using single shaft pressuring method 920~980 DEG C, 100~ 0.5~2h of hot pressed sintering under the conditions of 160MPa, the density of pressed compact is set to reach 6.69~7.01g/cm3.Then powder hot-pressing is burnt Tie base and carry out vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges, make Fe powder particles metallurgical bindings, and silicon Ferrous powder granules realized with Fe it is partially-alloyed, formed densification, α-Fe crystal grain with the poor Si of plastic deformation ability and fragility it is high The high silicon steel blank of heterogeneous structure of Si phases.Sintered subsequently through multiple cold rolling, low temperature diffusion, the density rise of slab, plate thickness Reduce, Si alloying level also improves constantly.Finally vacuum or protection of reducing atmosphere in 1260~1320 DEG C of temperature ranges Sintering, the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, Density >=7.25g/cm3High silicon steel band.
Methods described 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 Si, Mn, P, S and inevitably miscellaneous Matter, use Si contents as 70~80% HIGH-PURITY SILICON iron powder, particle diameter≤10 μm, this ferrosilicon powder except containing 70~80%Si with Outside, major impurity is~0.25%Al ,~0.08%Ca and~0.02%C, and remaining is Fe.
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 also easily realize being mutually twisted for powder in follow-up powder hot-pressing sintering process and improve the intensity of pressed compact.
In addition to primary silicon crystal grain, eutectic be present at 1207 DEG C in process of setting in Fe-70~80%Si high purity ferrosilicons Reaction, forms the β-FeSi with tP3 structures2It is very crisp with Si phase eutectic structures, this tissue, 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, the Si phases in its actual tissue, FeSi2 It is mutually more tiny, be advantageous to the thermal diffusion homogenization of Si elements during subsequent high temperature sintering, it is single-phase to form homogeneous Fe-4.5~6.7%Si Alloy.Meanwhile 20~30%Fe present in powder can effectively reduce Si degree of oxidation, be advantageous to improve the production of high silicon steel Quality.
By Fe-70~80%Si high purity ferrosilicons Mechanical Crushing to particle diameter≤10 μm, be advantageous 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 advantageous to improve follow-up blank toughness, cracking is not easily caused in densification process is rolled.But Fe-70~ More Si phases are still suffered from 80%Si high purity ferrosilicons, Si is 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, hot pressed sintering, roll Inert gas shielding should be used during system, used instrument must also 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 Fe-4.5~6.7%Si ratio, reduction Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed；Lazy Property protective atmosphere under using low energy mixer mix, mixing velocity and time regarding mixing uniformity depending on, should try one's best mitigation Fe Processing hardening occurs in mixed process for powder.
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.33~6.50g/cm3, using hot pressed sintering Stove, 0.5~2h of hot pressed sintering at 920~980 DEG C, makes the density of pressed compact reach 6.69~7.01g/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 of simple substance Fe particles and rich Si phase compositions after sintering, possesses the high-plastic of pure Fe crystal grain Property characteristic.
(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 1060~1160 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, and after the completion of Si alloyings, strip density brings up to 7.23~7.36g/cm3。
A large amount of deformable Fe phases in blank be present, slab can bear cold-rolling deformation.But there is also more in slab High Si phases, its performance is more crisp, therefore amount can not be too high under every time rolling, and accumulation total reduction reaches 30~50%, takes around 8 ~25 passages.
Because 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 certain 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 too high then Si elements can be caused quickly to spread, cause crystal grain excessive high hardness, embrittlement, follow-up rolling deformation is difficult to.
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 2 kinds of different Fe phases of Si solid solubility be present, 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 1260~1320 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 7.25~7.39g/cm3。
Described low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
The HIGH-PURITY SILICON iron powder of particle diameter≤10 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 400~600MPa surface 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, 100~160MPa single shaft pressuring method, 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, and bending strength reaches 185~ 427MPa。
Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during mixing, the addition total amount of binder is not 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 addition 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 lay MgO powder, and W, Mo and ceramics can be used to burn Boat.But plate must tile placement, flat board 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, it can subsequently be annealed by wet hydrogen, the technological means such as normalizing treatment is controlled by.
Essence of the invention is by with the addition of certain volume in the reduction Fe powder of the big volumetric portion with good plasticity Fine Fe-70~80%Si HIGH-PURITY SILICONs iron powder of ratio, form Fe-4.5~6.7Si% mixtures.After powder hot-pressing sintering, shape Into fine and close soft Fe particles and the composite of hard crisp rich Si phase compositions, there is higher deformation at room temperature ability.Subsequently through more Passage cold rolling and sintering, structural homogenity and compactness are further improved, then by similar to CVD high-temperature diffusion process, realizing Si homogenization, so as to obtain the single-phase high silicon steel band of high quality.This method realizes technique mistake by technique and equipment Design Process automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.25g/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.
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 Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:8.375 ratio Example mixing, form Fe-6.7%Si mixed-powder.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine are added during mixing Oil.Absolute ethyl alcohol adds according to the amount of 200ml/ tons.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Square pressed compact is prepared using compression-moulding methods, surface pressing 600MPa, pressed compact size is 100 × 100 × 40mm, green density 6.33g/cm3。
100MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 2h at 920 DEG C, the thickness of blank are about 36mm, density Reach 6.69g/cm3.Three point bending test shows plasticity, sees Fig. 1, and bending strength reaches 185MPa.
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., sintered through 13 cold rollings and 12 times.
Multi-pass cold rolling is thick in 1060 DEG C of heat preservation sintering 2h, sheet material to after 30~50%, then in vacuum sintering furnace Degree is thinned to 0.49mm, and density reaches 7.23g/cm3。
1h is sintered in 1320 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches 7.25g/cm3, Si contents are 6.7%.
Embodiment 2
By the reduction Fe powder of -100 mesh and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42 ratio Mixing, form Fe-4.5%Si mixed-powder.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing. Absolute ethyl alcohol adds according to the amount of 400ml/ tons.Using drum mixer by above-mentioned powder mixing 6h.
Square pressed compact is prepared using compression-moulding methods, surface pressing 400MPa, pressed compact size is 300 × 300 × 60mm, green density 6.50g/cm3。
160MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 0.5h at 980 DEG C, the thickness of blank is about 54mm, close Degree reaches 7.01g/cm3.Three point bending test shows plasticity, and bending strength reaches 427MPa.
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 1160 DEG C of insulations 0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.36g/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 to exist 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.
1h is sintered in 1260 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches 7.39g/cm3, Si contents are 4.5%.
Embodiment 3
By the reduction Fe powder of -100 mesh and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55 ratio Mixing, form Fe-6.5%Si mixed-powder.The paraffin micro mist of raw material total amount 0.4% is added during mixing, 0.2% methyl is fine Dimension element, 0.1% machine oil.Absolute ethyl alcohol adds according to the amount of 400ml/ tons.Above-mentioned powder is mixed using drum mixer 6h。
Square pressed compact is prepared using compression-moulding methods, surface pressing 500MPa, pressed compact size is 180 × 180 × 50mm, green density 6.37g/cm3。
150MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 1h at 940 DEG C, the thickness of blank are about 46mm, density Reach 6.72g/cm3.Three point bending test shows plasticity, and bending strength reaches 324MPa.
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., sintered 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 1120 DEG C of insulations 1h is tied, sheet metal thickness is thinned to 0.27mm, and density reaches 7.26g/cm3。
2h is sintered in 1300 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.27mm, density reaches To 7.28g/cm3, Si contents are 6.5%,
Embodiment 4
By the reduction Fe powder of -100 mesh and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95 ratio Mixing, form Fe-5.8%Si mixed-powder.The paraffin micro mist of raw material total amount 0.6%, 0.2% machine oil are added during mixing. Absolute ethyl alcohol adds according to the amount of 400ml/ tons.Using drum mixer by above-mentioned powder mixing 3h.
Square pressed compact is prepared using compression-moulding methods, surface pressing 500MPa, pressed compact size is 220 × 220 × 50mm, green density 6.40g/cm3。
150MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 1.5h at 950 DEG C, the thickness of blank is about 52mm, close Degree reaches 6.76g/cm3.Three point bending test shows plasticity, and bending strength reaches 342MPa.
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 1100 DEG C of insulations 1h is tied, sheet metal thickness is thinned to 0.21mm, and density reaches 7.30g/cm3。
2h is sintered in 1280 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.21mm, density reaches To 7.31g/cm3, Si contents are 5.8%, and the XRD analysis figure of its final sheet material is shown in Fig. 4, is the high silicon steel of single-phase homogeneous.

Claims (7)

1. the powder hot-pressing sintering manufacture method of a kind of high silicon steel thin belt material, it is characterised in that comprise the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is Si, Mn, P, S and other are inevitably miscellaneous Matter, middle particle diameter are located at 75~106 μm；Use the Si contents of refining for 70~80% HIGH-PURITY SILICON iron powder, with particle diameter≤10 μm Ferrosilicon powder, HIGH-PURITY SILICON iron powder impurity are~0.25%Al ,~0.08%Ca and~0.02%C, and remaining is Fe；
(2) powder mixes
According to Fe-4.5~6.7%Si ratio, reduction Fe powder and fine Fe-70~80%Si HIGH-PURITY SILICONs iron powder are weighed；Lazy Property protective atmosphere under using low energy mixer mix；
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.33~6.50g/cm3, with hot-pressed sintering furnace, in 0.5~2h of hot pressed sintering at 920~980 DEG C, makes the density of pressed compact reach 6.690~7.01g/cm3；
(4) cold rolling-sintering
By above-mentioned hot pressed sintering plate, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through under multi- pass rolling to stagnation pressure After rate reaches 30~50%, then in sintering furnace after 1060~1160 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering, plate The thickness of material reaches 0.1~0.5mm, and density reaches 7.23~7.36g/cm3；
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1320 DEG C of temperature ranges, it is real in the presence of thermal diffusion The existing full alloyings of Si, form single-phase alloy, obtain the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering, Density reaches 7.25~7.39g/cm3。
2. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Described is low Energy hybrid machine is conical mixer, V-arrangement batch mixer or drum mixer.
3. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (1) The high purity iron silica flour of described particle diameter≤10 μm is using high-energy ball milling or rushes the acquisition of rotation method.
4. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (3) Square pressed compact is prepared using compression-moulding methods, using hydraulic press under 400~600MPa surface pressing, obtains square pressure Base, pressed compact length and width are respectively 100~300mm, are highly 40~60mm；The aluminum oxide compacting tool set of same size is put into, is used Hot-pressed sintering furnace, 100~160MPa single shaft pressuring method, under hydrogen shield effect, the hot pressed sintering at 920~980 DEG C 0.5~2h, slab three point bending test shows as plasticity after hot pressed sintering, and bending strength reaches 185~427MPa.
5. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (2) Add cellulose, paraffin micro mist during mixing or zinc stearate is water-insoluble is no more than as binder, the addition total amount of binder The 0.8% of mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, rise passivation Si powder, bonding Fe-Si powder, Strengthen the effect of powder flowbility and compact strength, the addition total amount of passivator is no more than the 2% of mixed-powder gross mass.
6. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (4) Described supporting plate uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the powder hot-pressing sintering manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (5) During described high temperature sintering, overlapping places sintering plate, interlayer laying MgO powder, and plate tiling is placed, and flat board is placed on plate Weight, prevent from deforming in sintering process.
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