CN107900354A - A kind of method that powder extruding prepares high silicon steel thin belt material - Google Patents
A kind of method that powder extruding prepares high silicon steel thin belt material Download PDFInfo
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- CN107900354A CN107900354A CN201711368381.9A CN201711368381A CN107900354A CN 107900354 A CN107900354 A CN 107900354A CN 201711368381 A CN201711368381 A CN 201711368381A CN 107900354 A CN107900354 A CN 107900354A
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- 239000000843 powder Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 43
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 76
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 39
- 238000001125 extrusion Methods 0.000 claims abstract description 34
- 230000009467 reduction Effects 0.000 claims abstract description 21
- 238000009792 diffusion process Methods 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001192 hot extrusion Methods 0.000 claims description 22
- 239000000956 alloy Substances 0.000 claims description 19
- 229910045601 alloy Inorganic materials 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 13
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- 238000004321 preservation Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 229910017082 Fe-Si Inorganic materials 0.000 claims description 10
- 229910017133 Fe—Si Inorganic materials 0.000 claims description 10
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 9
- 238000000280 densification Methods 0.000 claims description 7
- 239000010721 machine oil Substances 0.000 claims description 7
- 239000011863 silicon-based powder Substances 0.000 claims description 7
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- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
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- 239000012535 impurity Substances 0.000 claims description 4
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- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
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- 229910052742 iron Inorganic materials 0.000 abstract description 8
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- 229910005347 FeSi Inorganic materials 0.000 description 4
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- 229910005331 FeSi2 Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 238000005275 alloying Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 229910052721 tungsten Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
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- 235000019441 ethanol Nutrition 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 239000011148 porous material Substances 0.000 description 1
- 238000009704 powder extrusion Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004801 process automation Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910006585 β-FeSi Inorganic materials 0.000 description 1
- 229910006578 β-FeSi2 Inorganic materials 0.000 description 1
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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
-
- 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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
A kind of powder extruding method for making of high silicon steel thin belt material, uses reduction Fe powder and 50~70% HIGH-PURITY SILICON iron powder to form Fe 4.5~6.7%Si mixed powders for raw material.Squarely base is molded, 950~1050 DEG C is heated to and realizes Fe phase austenitizings, slab is hot extruded into the deflection that extrusion ratio is 8~16.Then extruding slab is subjected to vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges; Fe powder particles are made to realize metallurgical binding; and Si and Fe realize it is partially-alloyed; 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; after being sintered again by multiple cold rolling, low temperature diffusion; sintered in 1270~1320 DEG C of Temperature Vacuums or protection of reducing atmosphere; it is thick to obtain 0.1~0.5mm containing 4.5~6.7%Si, density >=7.39g/cm3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder metallurgy of high silicon steel thin belt material is burnt
The method of knot, hot extrusion and rolling deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis 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 is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction contains with Si
Amount increases and reduces, and disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents,
At about 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent in higher frequency operation
Low 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 are oozed a diffusion annealing method, powder metallurgic method, microalloying and are changed
The various methods such as property.
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 business
Be developed with the CVD production lines that can realize continuous siliconising, 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 the method that a kind of extruding of powder prepares high silicon steel thin belt material, for 4.5~6.7%
The Fe-Si alloy thin band materials of Si contents are difficult to the problem of shaping, using reduced iron powder and Si contents as 50~70% high purity ferrosilicon
Powder is raw material, and extruding green compact are molded into after adding binder, then prepares certain thickness slab using powder hot-extrusion method,
Acted on using the large deformation of hot extrusion and cause the raising of extruded stock density, structure refinement, and the achievement unit division under thermal diffusion effect
Aurification, forms the α-Fe crystal grain of the poor Si of plastic deformation ability and the heterogeneous structure of the high Si phases of brittleness.It is subsequently cold by multi-pass
Thin plate is obtained after rolling-sintering, is finally sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions:Using the reduction Fe powder of irregular pattern, fine Si powder is
Material powder, forms Fe-4.5~6.7%Si mixed powders.By suitable bonding agent, dispersant by fine Si powder mixed
Adhered to during conjunction in the hole of reduced iron powder surface or filling ferrous powder.Since reduction Fe powder is with the thick of high-compressibility
Bulky grain, occupies larger volume ratio in mixed powder, does not significantly reduce its plastic deformation ability after adding Si powder, can pass through
It is molded squarely base.It is heated to 950~1050 DEG C and realizes Fe phase austenitizings, with the deflection hot extrusion that extrusion ratio is 8~16
It is pressed into slab.Then powder extruding slab is subjected to vacuum in 1060~1160 DEG C of temperature ranges or protection of reducing atmosphere sinters,
Fe powder particles is realized metallurgical binding, and Si and Fe realize it is partially-alloyed, formed densification, there is the poor Si of plastic deformation ability
α-Fe crystal grain and the high Si phases of brittleness the high silicon steel blank of heterogeneous structure.Sintered subsequently through multiple cold rolling, low temperature diffusion, slab
Density rise, plate thickness reduce, the alloying level of Si is also continuously improved.Finally in 1270~1320 DEG C of temperature ranges
Vacuum or protection of reducing atmosphere sintering, realize the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtain containing 4.5~
0.1~0.5mm of 6.7%Si is thick, density >=7.39g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps:
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is the impurity such as Si, Mn, P, S, middle particle diameter
Positioned at 75~106 μm;Use the Si contents of refining for 50~70% HIGH-PURITY SILICON iron powder, it is this with the ferrosilicon powder of particle diameter≤6 μm
Ferrosilicon powder is in addition to containing 50~70%Si, and major impurity is~0.24%Al ,~0.07%Ca ,~0.02%C, remaining
For 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.
Fe-50~70%Si high purity ferrosilicons in process of setting there are two eutectic reactions, 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;At 982 DEG C and 937 DEG C, also there are β-FeSi2Decomposition 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 conducive 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 the degree of oxidation of Si, be conducive 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 conducive to it and be adhered to reduction Fe powder
Surface is filled in the hole of reduction Fe powder, tiny Si, FeSi2, FeSi phases Dispersed precipitate in blank, it is thin to play tissue
The Strengthening and Toughening effect of change, is conducive to improve follow-up blank toughness, cracking is not easily caused in densification process is rolled.But Fe-
Still contain a small amount of Si phases in 50~70%Si high purity ferrosilicons, Si is easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2It is thin
Film, therefore in the preparation, storage and transfer process of Fe-50~70%Si HIGH-PURITY SILICON iron powders, and follow-up batch mixing, extrude, 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 the ratio of Fe-4.5~6.7%Si, 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;
(3) powder extrudes
Square pressed compact is prepared using compression-moulding methods, green density is 6.39~6.56g/cm3;Using square extruding
Cylinder, extrusion ratio are 8~16, using sintered-carbide die, lubricant are done with machine oil and glass dust, by molding square billet in nitrogen before extruding
Be heated to 950~1050 DEG C under gas shielded effect, keep the temperature 2~4h, extrusion cylinder and extrusion die 400~600 DEG C of preheating insulations 1~
2h, implements hot extrusion, the density of slab is 6.83~7.15g/cm after hot extrusion3。
(4) sinter
Hot extrusion pressing plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into sintering furnace.Using 2~5 DEG C/
The programming rate of min, is warming up to 1060~1160 DEG C of 2~4h of heat preservation sintering.Sintered blank density is 7.26~7.38g/cm3.With
Extruded stock density is compared, and density slightly reduces.
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 sintering.Can be used during sintering W, Mo, heat resisting steel etc. as support plate (or
Burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity is good, and it is 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) cold rolling-sintering densification
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1060~1160 DEG C of 0.5~2h of heat preservation sintering in sintering furnace.After multiple cold rolling-sintering,
The thickness of plate reaches 0.1~0.5mm, and density reaches 7.38~7.50g/cm3。
Cold-rolling deformation can be born since there are deformable Fe phases, slab in blank.But there is also more in slab
High Si phases, its performance is more crisp, therefore for amount not above 8%, accumulation total reduction reaches 30~45%, about needs under every time rolling
Want 8~20 passages.
Due to existing hard crisp phase, it is necessary to take and keep the temperature vacuum-sintering or restitutive protection's gas again at 1060~1160 DEG C
Atmosphere sinters, and the closing of pores and the reparation of crackle are produced in cold-rolled process to realize, and a degree of Si elements homogenization expands
Dissipate., it is necessary to sinter 1 time again, from the hot extrusion of 2.5~5.0mm after the accumulation drafts after sintering reaches 30~45% every time
Plate is rolled down to 0.1~0.5mm, takes around and sinters 6~10 times again.
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1270~1320 DEG C of temperature ranges, in thermal diffusion
Under effect, the homogenization of Si is realized, form single-phase alloy, obtain the high silicon steel of homogeneous.The thickness of plate is almost after densification sintering
It is constant, it is 0.1~0.5mm, density reaches 7.39~7.51g/cm3。
The ferrosilicon powder of particle diameter≤6 μm is by high-energy ball milling or rushes the acquisition of rotation method.
The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
Step (2) adds cellulose, paraffin micro mist or the water-insoluble binder of zinc stearate, the additive amount of binder when mixing
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, viscous
The effect of Fe-Si powder, enhancing powder flowbility and compact strength is connect, the additive amount total amount of passivator is no more than the total matter of mixed-powder
The 2% of amount.
Using the square extrusion cylinder of 40 × 120mm in step (3), extrusion die is 5~2.5mm × 120mm, corresponding extrusion ratio
Respectively 8~16;Using sintered-carbide die, lubricant is done with machine oil and glass dust, implements hot extrusion using 300 tons of press,
Three point bending test shows plasticity, and bending strength is 106~196MPa.
Molybdenum plate, W plates, heat resisting steel, corundum or the zirconia ceramics plate that support plate described in step (4) uses.
Placement sintering plate can be overlapped during step (6) high temperature sintering, but interlayer must be laid with MgO powder, can use W, Mo
Boat is burnt with ceramics.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 means such as normalizing treatment are controlled by by wet hydrogen.
Essence of the invention is by with the addition of granularity≤6 in the reduction Fe powder of the big volumetric portion with good plasticity
μm Fe-50~70%Si high-purity powders, formed Fe-4.5~6.7%Si mixed powders.High density, height are obtained using hot extrusion
Uniformity slab.The element alloyed degree of slab Si is low, its microscopic structure by high-ductility Fe phases and brittleness richness Si phase compositions,
With high cold deformation ability, structural homogenity and compactness can be improved by multi-pass cold rolling and sintering, then High temperature diffusion is burnt
Knot, realizes the homogenization of Si, so as to obtain the high silicon steel band of high quality.This method realizes work by technique and equipment Design
Skill process automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.39g/cm3High silicon steel band.
Brief description of the drawings
Fig. 1 is the three-point bending curve map of blank after the powder of the embodiment of the present invention 1 extrudes;
Fig. 2 is metallographic structure figure after powder extruding-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 3 is XRD diffraction curve figures after powder extruding-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 4 is XRD diffraction curve figures after powder extruding-cold rolling-high temperature sintering of the embodiment of the present invention 4.
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, forms the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine oil are added during mixing.
Absolute ethyl alcohol is added according to 200ml/ tons of amount.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Square pressed compact is prepared using compression-moulding methods, the length and width of pressed compact is respectively 120mm and 80mm, is highly
40mm, uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.39g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 5 × 120mm, and corresponding extrusion ratio is 8.Before extruding
Molding square billet is heated to 950 DEG C under nitrogen protective effect, keeps the temperature 4h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.
Implement hot extrusion using 300 tons of press, the density of slab is 6.83g/cm after hot extrusion3, three point bending test shows to mould
Property, see Fig. 1, bending strength 106MPa.
Using the programming rate of 2 DEG C/min, 1080 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.26g/cm3。
The texture of coarse crystal containing the second phase is formed after sintering.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1080 DEG C of heat preservation sintering 2h in sintering furnace.Specifically pressure-annealing schedule is:5mm→
3.5mm → 2.4mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate
Degree reaches 0.49mm, and density reaches 7.38g/cm3。
1h finally is sintered in 1270 DEG C of Temperature Vacuums, under the action of thermal diffusion, the homogenization of Si is realized, forms single-phase conjunction
Gold, obtains the high silicon steel of homogeneous.The thickness of plate is almost unchanged after densification sintering, is 0.49mm, and density reaches 7.39g/cm3。
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 the mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing.Anhydrous second
Alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 6h.
Square pressed compact is prepared using compression-moulding methods, the length and width of pressed compact is respectively 120mm and 80mm, is highly
40mm, uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.56g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 2.5 × 120mm, and corresponding extrusion ratio is 16.Will before extruding
Molding square billet is heated to 1050 DEG C under nitrogen protective effect, keeps the temperature 2h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.
Implement hot extrusion using 300 tons of press, the density of slab is 7.15g/cm after hot extrusion3, three point bending test shows to mould
Property, bending strength 196MPa.
Using the programming rate of 2 DEG C/min, 1160 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.38g/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 2 kinds of different Fe phases of Si solid solubility,
Must wherein there are the Si contents in a kind of Fe phases low, there is plastic deformation ability.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1160 DEG C of heat preservation sintering 0.5h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate
Degree reaches 0.1mm, and density reaches 7.50g/cm3.Specifically cold rolling-sintering schedule is:2.5mm →1.85mm→1.39mm→
1.15mm → 0.89mm → 0.65mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., through 10 cold rollings
After 9 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.50g/cm3。
4h finally is sintered in 1320 DEG C of Temperature Vacuums, forms the high silicon steel of single-phase homogeneous that Si contents are 4.5%, thickness is
0.1mm, density reach 7.51g/cm3。
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
Example mixing, 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.
Square pressed compact is prepared using compression-moulding methods, the length and width of pressed compact is respectively 120mm and 80mm, is highly
40mm, uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.42g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 4 × 120mm, and corresponding extrusion ratio is 10.By mould before extruding
Pressure square billet is heated to 1000 DEG C under nitrogen protective effect, keeps the temperature 3h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.Adopt
Implement hot extrusion with 300 tons of press, the density of slab is 6.86g/cm after hot extrusion3, bending strength 141MPa.
Using the programming rate of 3 DEG C/min, 1150 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.28g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, and specific cold rolling-sintering schedule is:4.0mm→2.8mm →
2.0mm → 1.40mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 7 cold rollings and 6 sintering, plate
Thickness reaches 0.27mm, and density reaches 7.39g/cm3。
For above-mentioned cold rolling made-up belt in 1290 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.41g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the reduction Fe powder of -100 mesh and the Fe-62%Si high-purity powders of granularity≤10 μm according to 90.64:9.36 ratio
Example mixing, 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.
Square pressed compact is prepared using compression-moulding methods, the length and width of pressed compact is respectively 120mm and 80mm, is highly
40mm, uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.43g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 3.2 × 120mm, and corresponding extrusion ratio is 12.5.Squeeze
Molding square billet is heated to 1020 DEG C under nitrogen protective effect before pressure, keeps the temperature 4h.Extrusion cylinder and extrusion die are protected in 600 DEG C of preheatings
Warm 2h.Implement hot extrusion using 300 tons of press, the density of slab is 6.86g/cm after hot extrusion3, bending strength 148MPa.
Using the programming rate of 4 DEG C/min, 1120 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.29g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1120 DEG C of heat preservation sintering 1h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate
Reach 0.22mm, density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is:3.2mm →2.4mm→2.0mm→1.3mm
→ 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., after 9 cold rollings and 8 sintering, the thickness of plate reaches
To 0.21mm, density reaches 7.41g/cm3。
For above-mentioned cold rolling made-up belt in 1310 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.42g/cm to obtain thickness3, Si
Content is 5.8%, and the XRD analysis figure of its final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.
Claims (7)
1. a kind of powder extruding method for making 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 50~70% HIGH-PURITY SILICON iron powder, with the silicon of particle diameter≤6 μm
Iron powder, ferrosilicon powder in addition to containing 50~70%Si, major impurity for~0.24%Al ,~0.07%Ca and~0.02%C,
Remaining is Fe;
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, 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 extrudes
Square pressed compact is prepared using compression-moulding methods, green density is 6.39~6.56g/cm3;Using square extrusion cylinder, squeeze
Pressure ratio is 8~16, using sintered-carbide die, does lubricant with machine oil and glass dust, protects molding square billet in nitrogen before extruding
950~1050 DEG C are heated under shield effect, keep the temperature 2~4h, extrusion cylinder and extrusion die in 400~600 DEG C of 1~2h of preheating insulation,
Implement hot extrusion, the density of slab is 6.83~7.15g/cm after hot extrusion3;
(4) sinter
Hot extrusion pressing plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into sintering furnace, using 2~5 DEG C/min
Programming rate, be warming up to 1060~1160 DEG C of 2~4h of heat preservation sintering, sintered blank density is 7.26~7.38g/cm3;
(5) cold rolling-sintering densification
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to total reduction
After reaching 30~45%, then in 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 7.38~7.50g/cm3;
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1270~1320 DEG C of temperature ranges, it is real under the action of thermal diffusion
The homogenization of existing Si, forms single-phase alloy, obtains the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering,
Density reaches 7.39~7.51g/cm3。
2. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that:Particle diameter≤6 μm
Ferrosilicon powder is by high-energy ball milling or rushes the acquisition of rotation method.
3. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that the low energy
Mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that:Step is adopted in (3)
With the square extrusion cylinder of 40 × 120mm, extrusion die is 5~2.5mm × 120mm, and corresponding extrusion ratio is respectively 8~16;Using hard
Matter alloy mold, lubricant is done with machine oil and glass dust, implements hot extrusion using 300 tons of press, three point bending test is shown
Plasticity, bending strength are 106~196MPa.
5. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that:Add fiber during mixing
Element, paraffin micro mist or the water-insoluble binder of zinc stearate, the additive amount total amount of binder are no more than mixed-powder gross mass
0.8%, while add grease and absolute ethyl alcohol does passivator, rise passivation Si powder, bonding Fe-Si powder, enhancing powder flowbility and
The effect of compact strength, the additive amount total amount of passivator are no more than the 2% of mixed-powder gross mass.
6. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that:Step (4) is described
Support plate use molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the powder extruding method for making of high silicon steel thin belt material as claimed in claim 1, it is characterised in that:Step (6) is described
High temperature sintering when, overlapping place sintering plate, interlayer be laid with MgO powder, plate tiling place, on plate place tablet weight
Thing, prevents from deforming in sintering process.
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