CN107855532A - A kind of method that powder hot-pressing sintering prepares high silicon steel thin belt material - Google Patents
A kind of method that powder hot-pressing sintering prepares high silicon steel thin belt material Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 52
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 36
- 238000007731 hot pressing Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 title claims abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 61
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- 238000000280 densification Methods 0.000 claims description 4
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- 238000004321 preservation Methods 0.000 claims description 3
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 19
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- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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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
- 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
- B22F3/02—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
- B22F3/10—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
- B22F3/12—Both compacting and sintering
- B22F3/16—Both compacting and sintering in successive or repeated steps
- B22F3/162—Machining, working after consolidation
-
- 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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- 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
Abstract
A kind of method that powder hot-pressing sintering prepares high silicon steel thin belt material, using reduction Fe powder, Si contents are 50~70% HIGH-PURITY SILICON iron powder, form Fe Si mixed powders, by being molded squarely base, single shaft pressuring method 0.5~2h of hot pressed sintering under the conditions of 920~980 DEG C, 100~160MPa is used again, the density of pressed compact is reached 6.72~7.04g/cm3;Then powder hot-pressing sintered blank is carried out into vacuum or protection of reducing atmosphere at 1050~1150 DEG C to sinter, makes Fe powder particles metallurgical bindings, ferrosilicon powder particles realize partially-alloyed, then multiple low-temperature diffusion-sintering and rolled thickness reduction with Fe;High temperature diffusion sintering finally is carried out at 1250~1300 DEG C, realizes homogeneous alloy, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.28g/cm3High silicon steel band.
Description
Technical field
The invention belongs to the preparation of metal material and manufacture field, 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, 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
It is an object of the invention to provide a kind of powder hot-pressing sintering prepare high silicon steel thin belt material method, for Fe-4.5~
6.7%Si alloy thin band materials are difficult to the problem of shaping, are former as 50~70% HIGH-PURITY SILICON iron powder to reduce Fe powder with Si contents
Material, green compact are molded into after adding binder, then certain thickness slab is prepared using powder hot-pressing sintering method, utilize powder
The emollescence to Fe powder of hot pressed sintering causes green density to improve, and realizes slight alloying, shape under thermal diffusion effect
Into the Fe particles with plastic deformation ability and the complex tissue of the high Si phases of fragility.Subsequently obtained after multi-pass cold rolling-sintering
Thin plate is obtained, progressively promotes Si alloying, is finally sintered using High temperature diffusion and obtains the fine and close high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions:Using the reduction Fe powder of irregular pattern, fine Si contents
It is raw material for 50~70% 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 6.72~7.04g/cm3.Then powder hot-pressing is burnt
Tie base and carry out vacuum or protection of reducing atmosphere sintering in 1050~1150 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 1250~1300 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 >=7.28g/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 other are inevitable
Impurity, using Si contents, particle diameter≤6 μm, this ferrosilicon powder is except containing 50~70% for 50~70% HIGH-PURITY SILICON iron powder
Beyond Si, major impurity is~0.24%Al ,~0.07%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.
There are two eutectic reactions in Fe-50~70%Si high purity ferrosilicons, in process of setting when rich Si sides are at 1207 DEG C
Form the β-FeSi with tP3 structures2With Si phase eutectic structures, form when rich Fe sides are at 1212 DEG C and tied with tP3
β-the FeSi of structure2With the FeSi eutectic structures of cP8 structures;β-FeSi also be present in 982 DEG C and 937 DEG C2Decomposition and oC48-
FeSi2Two solid-state phase changes processes of formation of phase.Therefore it is easy in process of setting of the Fe-50~70%Si after refining crisp
Change, form trickle Fe-Si or Si heterogeneous structures, it is easy to refine by Mechanical Crushing technique.Fe-50~70%Si is high-purity
Ferrosilicon is crushed to≤6 μm of ferrosilicon powder, the Si phases in its actual tissue, FeSi2, FeSi phases it is more tiny, be advantageous to subsequent high temperature
The thermal diffusion homogenization of Si elements, forms homogeneous Fe-6.5%Si single-phase alloys during sintering.Meanwhile exist in high purity ferrosilicon powder
30~50%Fe can effectively reduce Si degree of oxidation, be advantageous to improve the product quality of high silicon steel.
By Fe-50~70%Si high purity ferrosilicons Mechanical Crushing to particle diameter≤6 μm, be advantageous to it and be adhered to the table of reduction Fe powder
Face is filled in the hole of reduction Fe powder, tiny Si, FeSi2, FeSi phases Dispersed precipitate in blank, play structure refinement
Strengthening and Toughening effect, be advantageous to improve follow-up blank toughness, cracking do not easily caused in densification process is rolled.But Fe-50
Still contain a small amount of Si phases in~70%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-50~70%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 fine Fe-50~70%Si HIGH-PURITY SILICONs iron powder are weighed;
Mixed under inert protective atmosphere using low energy mixer, mixing velocity and time depending on mixing uniformity, should try one's best and subtract
Processing hardening occurs in mixed process for light Fe powder.
(3) powder hot-pressing sinters
Square pressed compact is prepared using compression-moulding methods, green density is 6.34~6.53g/cm3, by pressed compact in 920
0.5~2h of hot pressed sintering at~980 DEG C, makes the density of pressed compact reach 6.72~7.04g/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, three point bending test show plasticity, and bending strength reaches 147~347MPa.
(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 1050~1150 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 Si alloying, and strip density improves, reach 7.26~
7.41g/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 1250~1300 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 7.28~7.42g/cm3。
Described low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
The HIGH-PURITY SILICON iron powder of particle diameter≤6 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 147~
347MPa。
It is water-insoluble total as binder, the addition of binder to add cellulose, paraffin micro mist or zinc stearate during mixing
0.8% of amount no more than mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding
The effect of Fe-Si powder, enhancing powder flowbility and compact strength, the 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-50~70%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 >=7.28g/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-70%Si high-purity powders of granularity≤6 μm according to 90.43:9.57 ratio
Mixing, form Fe-6.7%Si mixed-powder.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine oil are added during mixing.
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 6.36g/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 6.68g/cm3.Three point bending test shows plasticity, sees Fig. 1, and bending strength reaches 147MPa.
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 1050 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 7.26g/cm3。
1h is sintered in 1300 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches
7.28g/cm3, Si contents are 6.7%.
Embodiment 2
By the reduction Fe powder of -100 mesh and the Fe-50%Si high-purity powders of granularity≤10 μm according to 91:9 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.Anhydrous second
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 6.53g/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 7.04g/cm3.Three point bending test shows plasticity, and bending strength reaches 347MPa.
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 1150 DEG C of insulations
0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.41g/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.
4h is sintered in 1250 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches
7.42g/cm3, Si contents are 4.5%.
Embodiment 3
By the reduction Fe powder of -100 mesh and the Fe-60%Si high-purity powders of granularity≤6 μm according to 89.17:10.83 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 120 × 120 ×
50mm, green density 6.40g/cm3。
120MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 1h at 960 DEG C, the thickness of blank are about 46mm, density
Reach 6.76g/cm3.Three point bending test shows plasticity, and bending strength reaches 217MPa.
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 1100 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 1280 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.27mm, density reaches
To 7.32g/cm3, Si contents are 6.5%,
Embodiment 4
By the reduction Fe powder of -100 mesh and the Fe-62%Si high-purity powders of granularity≤10 μm according to 90.64:9.36 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 180 × 180 ×
50mm, green density 6.44g/cm3。
130MPa single shaft pressurization hot pressed sintering, the hot pressed sintering 1.5h at 930 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 271MPa.
By above-mentioned hot pressed sintering plate cold rolling-sintering, specific pressure-annealing schedule, which is progressively thinned, is:52mm→39mm→
26mm→18mm→13mm→10.5mm→8.2mm→5mm→3.2mm→2.4mm→2.0mm→1.3mm→0.90mm→
0.63→0.43mm→0.32mm→0.21mm.Sintered through 17 cold rollings and 16 times.
Multi-pass cold rolling is to after 30~50% total deformations, then is burnt in hydrogen shield sintering furnace in 1120 DEG C of insulations
1h is tied, sheet metal thickness is thinned to 0.21mm, and density reaches 7.32g/cm3。
2h is sintered in 1260 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.21mm, density reaches
To 7.33g/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. a kind of method that powder hot-pressing sintering prepares 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, Si contents are used as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, HIGH-PURITY SILICON iron powder impurity is~0.24%Al ,~
0.07%Ca and~0.02%C, remaining is Fe;
(2) powder mixes
According to Fe-4.5~6.7%Si ratio, reduction Fe powder and fine Fe-50~70%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 6.34~6.53g/cm3, it is hot at 920~980 DEG C
Pressure 0.5~2h of sintering, makes the density of pressed compact reach 6.72~7.04g/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 1050~1150 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 7.26~7.41g/cm3;
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1250~1300 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 7.28~7.42g/cm3。
2. the method that powder hot-pressing sintering as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that:Described is low
Energy hybrid machine is conical mixer, V-arrangement batch mixer or drum mixer.
3. the method that powder hot-pressing as claimed in claim 1 sintering prepares high silicon steel thin belt material, described in its characterization step (1)
The high purity iron silica flour of particle diameter≤6 μm is using high-energy ball milling or rushes the acquisition of rotation method.
4. the method that powder hot-pressing sintering as claimed in claim 1 prepares high silicon steel thin belt material, 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 147~347MPa.
5. the method that powder hot-pressing sintering as claimed in claim 1 prepares high silicon steel thin belt material, 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 method that powder hot-pressing sintering as claimed in claim 1 prepares high silicon steel thin belt material, 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 method that powder hot-pressing sintering as claimed in claim 1 prepares high silicon steel thin belt material, 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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