CN108015287A - A kind of method that hot pressed sintering prepares Fe-6.5%Si bands with High temperature diffusion sintering - Google Patents
A kind of method that hot pressed sintering prepares Fe-6.5%Si bands with High temperature diffusion sintering Download PDFInfo
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Classifications
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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
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention provides a kind of method that hot pressed sintering prepares Fe 6.5%Si bands with High temperature diffusion sintering, reduction Fe powder and water atomization Fe powder is chosen, according to 4:6~6:4 ratio mixing, then the HIGH-PURITY SILICON iron powder that Si contents are 70~80% is added, form Fe Si mixed powders.By being molded squarely base, 0.5~2h of hot pressed sintering under the conditions of 920~980 DEG C, 100~160MPa, makes the density of pressed compact reach 6.65~6.98g/cm3；Then powder hot-pressing sintered blank is carried out to vacuum or protection of reducing atmosphere sintering multiple low-temperature diffusion-sintering and rolled thickness reduction again at 1060~1160 DEG C；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 >=7.36g/cm3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder hot-pressing sintering of high silicon steel thin belt material
With the method for 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 and High temperature diffusion sintering to prepare Fe-6.5%Si thin strips
Method, the problem of being difficult to shaping for Fe-4.5~6.7%Si alloy thin band materials, using industrial Fe powder with Si contents as 70~
80% HIGH-PURITY SILICON iron powder uniformly mixes, and is molded into green compact after adding binder, then prepare using powder hot-pressing sintering method
Certain thickness slab, the emollescence to Fe powder sintered using powder hot-pressing cause green density to improve, and in thermal diffusion
Slight alloying is realized under effect, forms the complex tissue of Fe particles and the high Si phases of brittleness with plastic deformation ability.Subsequently
Thin plate is obtained after multi-pass cold rolling-sintering, progressively promotes the alloying of Si, is finally sintered using High temperature diffusion and obtains densification
The high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions：Reduction Fe powder and two kinds of Industrial iron powders of water atomization Fe powder are chosen,
According to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, then it is 70~80% to add fine Si contents
HIGH-PURITY SILICON iron powder is raw material, forms Fe-4.5~6.7%Si mixed powders.Will be fine by suitable bonding agent, dispersant
HIGH-PURITY SILICON iron powder is adhered in mixed process in Industrial iron powder surface or hole.Since industrial Fe powder is with high-compressibility
Big particle, occupies larger volume ratio in mixed powder, its plastic deformation ability is not significantly reduced after adding ferrosilicon powder, can be with
By being molded squarely base.Uniaxial compression mode hot pressed sintering 0.5 under the conditions of 920~980 DEG C, 100~160MPa is used again
~2h, makes the density of pressed compact reach 6.65~6.98g/cm3.Then by powder hot-pressing sintered blank in 1060~1160 DEG C of temperature models
Enclose and carry out vacuum or protection of reducing atmosphere sintering, make Fe powder particles metallurgical bindings, and ferrosilicon powder particles realize alloy part with Fe
Change, form α-Fe crystal grain fine and close, with the poor Si of plastic deformation ability and the high silicon steel blank of heterogeneous structure of the high Si phases of brittleness.
Sintered subsequently through multiple cold rolling, low temperature diffusion, the density rise of slab, plate thickness are reduced, and the alloying level of Si is also continuous
Improve.Finally vacuum or protection of reducing atmosphere sintering in 1260~1320 DEG C of temperature ranges, are realized with the help of thermal diffusion
The homogeneous alloy of high silicon steel, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.36g/cm3High silicon strip
Material.
The method specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitable
Impurity, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining for Si, Mn, P, S and other can not
The impurity avoided, by reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, and is mixed using conical mixer, V-arrangement
Material machine or drum mixer are mixed to form technical pure Fe powder basic materials, and incorporation time is 2~6h.
The Si contents of refining are used as 70~80% HIGH-PURITY SILICON iron powder, particle diameter≤10 μm, this ferrosilicon powder except containing
Beyond 70~80%Si, major impurity is~0.25%Al ,~0.08%Ca ,~0.02%C, 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 in follow-up powder extrusion process also being mutually twisted for powder easy to implement and improve the intensity of pressed compact, be conducive to
The stabilization of powder extrusion process.Water atomization Fe powder is also a kind of widely used Industrial iron powder, has subsphaeroidal pattern, and impurity contains
Amount is less than reduction Fe powder, compressibility and mobility with higher, is conducive to the uniform flow of powder extrusion process course powder
Dynamic, low impurity content is favourable to the soft magnetic characteristic of high silicon steel in water atomization Fe powder.Will two kinds of reduction Fe powder and water atomization Fe powder
Industrial iron powder, according to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, and it is each to be conducive to two kinds of straight iron powders of performance
From advantage, be also relatively common method in industrial production iron-base part.
Fe-70~80%Si high purity ferrosilicons are in process of setting in addition to primary silicon crystal grain, and at 1207 DEG C, there are eutectic
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 conducive 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 the degree of oxidation of Si, be conducive 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 conducive to it and be adhered to industrial Fe powder
Surface, tiny Si, FeSi2The mutually Dispersed precipitate in blank, plays the role of the Strengthening and Toughening of structure refinement, is conducive to improve follow-up
Blank toughness, do not easily cause cracking in densification process is rolled.But still suffered from Fe-70~80%Si high purity ferrosilicons more
Si phases, Si is easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2Film, therefore in Fe-70~80%Si HIGH-PURITY SILICONs
In the preparation of iron powder, storage and transfer process, and inert gas should be used to protect in follow-up batch mixing, hot pressed sintering, the operation of rolling
Shield, 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 the ratio of Fe-4.5~6.7%Si, industrial Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powder is 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 6.32~6.49g/cm3, by pressed compact in 920
0.5~2h of hot pressed sintering at~980 DEG C, makes the density of pressed compact reach 6.65~6.98g/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 129~259MPa.
(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, is gradually completing with the alloying of Si, and strip density improves, reach 7.35~
7.49g/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 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 slightly improves, and reaches 7.36~7.50g/cm3。
In step (1) mixed process absolute ethyl alcohol is added in 200~500ml/ tons of ratio.
The HIGH-PURITY SILICON iron powder of particle diameter≤10 μm by high-energy ball milling or rushes the acquisition of rotation method in step (1).
Low energy mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
Step (2) adds cellulose, paraffin micro mist when mixing or zinc stearate is water-insoluble adds as binder, binder
Dosage total amount is no 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 powder, the effect for strengthening powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed powder
The 2% of last gross mass.
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 129~
259MPa。
Support plate described in step (4) uses 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 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 fine Fe-70 in the industrial Fe powder of the big volumetric portion with good plasticity
~80%Si HIGH-PURITY SILICON iron powders, form Fe-4.5~6.7Si% mixtures.After powder hot-pressing sintering, fine and close soft Fe is formd
Grain 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 sintering,
Further improve structural homogenity and compactness, then by similar to CVD high-temperature diffusion process, realizing the homogenization of Si, so that
Obtain the single-phase high silicon steel band of high quality.This method realizes Technics Process Automation, serialization by technique and equipment Design
Production, can be mass-produced 0.1~0.5mm thickness, density >=7.36g/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 curves 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 water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 5:5 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 6h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:8.375
Ratio mixing, form the mixed-powder of Fe-6.7%Si.The paraffin micro mist of addition raw material total amount 0.6% during mixing, 0.1%
Machine oil.Absolute ethyl alcohol is added according to 200ml/ tons of amount.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 6.32g/cm3.The uniaxial compression hot pressed sintering of 100MPa, the hot pressed sintering 2h at 920 DEG C, blank
Thickness is about 36mm, and density reaches 6.68g/cm3.Three point bending test shows plasticity, sees Fig. 1, and bending strength reaches
129MPa。
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 1060 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 7.35g/cm3。
4h is sintered in 1320 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches
7.36g/cm3, Si contents are 6.7%.
Embodiment 2
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 6:4 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 4h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42
Ratio mixes, and forms the mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine are added during mixing
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 400MPa, pressed compact size for 300 × 300 ×
60mm, green density 6.49g/cm3.The uniaxial compression hot pressed sintering of 160MPa, hot pressed sintering 0.5h, blank at 980 DEG C
Thickness be about 54mm, density reaches 7.00g/cm3.Three point bending test shows plasticity, and bending strength reaches 259MPa.
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 7.49g/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 1260 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches
7.50g/cm3, Si contents are 4.5%.
Embodiment 3
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 5:6 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 3h, is added in mixed process according to 400ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55
Ratio mixes, and forms the mixed-powder of Fe-6.5%Si.The paraffin micro mist of raw material total amount 0.4%, 0.2% first are added during mixing
Base cellulose, 0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder
Mix 6h.
Prepare square pressed compact using compression-moulding methods, surface pressing 400MPa, pressed compact size for 120 × 120 ×
50mm, green density 6.36g/cm3.The uniaxial compression hot pressed sintering of 150MPa, hot pressed sintering 1.5h, blank at 950 DEG C
Thickness be about 46mm, density reaches 6.72g/cm3.Three point bending test shows plasticity, and bending strength reaches 132MPa.
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 1120 DEG C of insulations
1h is tied, sheet metal thickness is thinned to 0.27mm, and density reaches 7.36g/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 7.37g/cm3, Si contents are 6.5%,
Embodiment 4
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 4:6 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 2h, is added in mixed process according to 200ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95
Ratio mixes, and forms the mixed-powder of Fe-5.8%Si.The paraffin micro mist of raw material total amount 0.6%, 0.2% machine are added during mixing
Oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.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 6.40g/cm3.The uniaxial compression hot pressed sintering of 145MPa, hot pressed sintering 0.8h, blank at 960 DEG C
Thickness be about 52mm, density reaches 6.76g/cm3.Three point bending test shows plasticity, and bending strength reaches 135MPa.
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 7.42g/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 7.43g/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 (8)
1. a kind of method that hot pressed sintering prepares Fe-6.5%Si bands with High temperature diffusion sintering, it is characterised in that including following step
Suddenly：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitably miscellaneous
Matter；Using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, will reduction Fe powder and water atomization Fe powder according to 4:6~6:4 mass ratio is prepared, using conical mixer, V-arrangement batch mixing
Machine or drum mixer are mixed to form technical pure Fe powder basic materials, and incorporation time is 2~6h；
The Si contents for using refining are for 70~80% HIGH-PURITY SILICON iron powder, particle diameter≤10 μm, the major impurity of HIGH-PURITY SILICON iron powder
~0.25%Al ,~0.08%Ca and~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, pre- mixed technical pure Fe powder and simple substance Si powder are weighed；In inert protective atmosphere
It is lower to be mixed using low energy mixer；
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.32~6.49g/cm3, pressed compact is in 920~980 DEG C
0.5~2h of lower hot pressed sintering, makes the density of pressed compact reach 6.65~6.98g/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 1060~1160 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering, plate
Thickness reach 0.1~0.5mm, density reaches 7.35~7.49g/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 under the action 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 7.36~7.50g/cm3。
2. the method that hot pressed sintering as claimed in claim 1 prepares Fe-6.5%Si bands with High temperature diffusion sintering, its feature
It is：The HIGH-PURITY SILICON iron powder of particle diameter≤10 μm is by high-energy ball milling or rushes the acquisition of rotation method.
3. the method that hot pressed sintering as claimed in claim 1 prepares Fe-6.5%Si bands with High temperature diffusion sintering, its feature
It is：The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the method that hot pressed sintering as claimed in claim 2 prepares Fe-6.5%Si bands with High temperature diffusion sintering, its feature
It is：In step (1) mixed process 200~500ml absolute ethyl alcohols are added by ton mixed-powder.
5. the method that hot pressed sintering as claimed in claim 2 prepares Fe-6.5%Si bands with High temperature diffusion sintering, its feature
It is：It is water-insoluble as binder, the addition of binder that step (2) adds cellulose, paraffin micro mist or zinc stearate when mixing
Measure total amount is no more than mixed-powder gross mass 0.8%, while add grease and absolute ethyl alcohol does passivator, rise passivation Si powder,
The effect of Fe-Si powder, enhancing powder flowbility and compact strength is bonded, the additive amount total amount of passivator is total no more than mixed-powder
The 2% of quality.
6. the method that hot pressed sintering as claimed in claim 1 prepares Fe-6.5%Si bands with High temperature diffusion sintering, 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 129~
259MPa。
7. the method that hot pressed sintering as claimed in claim 1 prepares Fe-6.5%Si bands with High temperature diffusion sintering, its feature
It is：Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
8. the method that hot pressed sintering as claimed in claim 1 prepares Fe-6.5%Si bands with High temperature diffusion sintering, 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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