CN107999768A - A kind of method that powder extruding prepares high silicon steel band with High temperature diffusion sintering - Google Patents
A kind of method that powder extruding prepares high silicon steel band with High temperature diffusion sintering Download PDFInfo
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- CN107999768A CN107999768A CN201711369205.7A CN201711369205A CN107999768A CN 107999768 A CN107999768 A CN 107999768A CN 201711369205 A CN201711369205 A CN 201711369205A CN 107999768 A CN107999768 A CN 107999768A
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- 238000005245 sintering Methods 0.000 title claims abstract description 91
- 239000000843 powder Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 45
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 42
- 238000009792 diffusion process Methods 0.000 title claims abstract description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 38
- 238000001125 extrusion Methods 0.000 claims abstract description 36
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 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 9
- 238000001192 hot extrusion Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000005096 rolling process Methods 0.000 claims description 14
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- 230000008569 process Effects 0.000 claims description 13
- 230000009467 reduction Effects 0.000 claims description 13
- 238000004321 preservation Methods 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
- 238000009692 water atomization Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 238000000280 densification Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000010721 machine oil Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005452 bending Methods 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
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- 238000013001 point bending Methods 0.000 claims description 5
- 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
- 239000000428 dust Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000000314 lubricant Substances 0.000 claims description 4
- 229910052750 molybdenum Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
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- 239000001913 cellulose Substances 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
- 238000007670 refining Methods 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
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000004519 grease Substances 0.000 claims description 2
- 238000000713 high-energy ball milling Methods 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 238000002161 passivation Methods 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011863 silicon-based powder Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 20
- 229910045601 alloy Inorganic materials 0.000 abstract description 19
- 238000005097 cold rolling Methods 0.000 abstract description 10
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- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000000696 magnetic material Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 229910005347 FeSi Inorganic materials 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 229910005331 FeSi2 Inorganic materials 0.000 description 3
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000008859 change Effects 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
- 239000004033 plastic Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-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
- 230000008901 benefit Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 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
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000010924 continuous production Methods 0.000 description 1
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- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable effect Effects 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
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 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
- 238000003860 storage Methods 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
- 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
- B22F3/20—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)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
The method that a kind of extruding of powder prepares high silicon steel band with High temperature diffusion sintering, it for 50~70% HIGH-PURITY SILICON iron powder is raw material to use water-atomized iron powder and Si contents, formation Fe 4.5~6.7%Si mixed powders.By being molded squarely base; it is heated to 950~1050 DEG C and realizes Fe phase austenitizings; slab is hot extruded into the deflection that extrusion ratio is 8~16; slab is carried out to vacuum or protection of reducing atmosphere sintering at 1060~1160 DEG C; Fe powder particles are made to realize metallurgical binding; Si and Fe realizes partially-alloyed, forms the α Fe crystal grain of poor Si and the multi-phase high-silicon steel blank of the high Si phases of brittleness.Multiple cold rolling, low temperature diffusion sintering again, sinter in 1270~1320 DEG C of vacuum or protection of reducing atmosphere, realize the homogeneous alloy of high silicon steel, obtain 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.41g/cm3High silicon steel band.
Description
Technical field
The present invention principally falls into preparation and the manufacture field of metal material, and in particular to the powder metallurgy of high silicon steel thin belt material
The method of sintering, 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 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 method for preparing high silicon steel band is sintered with High temperature diffusion the object of the present invention is to provide a kind of extruding of powder, for
The Fe-Si alloy thin band materials of 4.5~6.7%Si contents are difficult to the problem of shaping, using water-atomized iron powder and Si contents as 50~
70% HIGH-PURITY SILICON iron powder is raw material, is molded into extruding green compact after adding binder, then prepare using powder hot-extrusion method
Certain thickness slab, is acted on using the large deformation of hot extrusion and causes the raising of extruded stock density, structure refinement, and is made in thermal diffusion
Realized under partially-alloyed, form the α-Fe crystal grain of the poor Si of plastic deformation ability and the heterogeneous structure of the high Si phases of brittleness.Afterwards
It is continuous to obtain thin plate after multi-pass cold rolling-sintering, finally sintered using High temperature diffusion and obtain the high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions：Use subsphaeroidal water-atomized iron powder and fine Si contents for
50~70% HIGH-PURITY SILICON iron powder is raw material, forms Fe-4.5~6.7%Si mixed powders.By suitable bonding agent, disperse
Fine HIGH-PURITY SILICON iron powder is adhered to water-atomized iron powder surface by agent in mixed process.Since water atomization Fe powder is with high pressure
The big particle of contracting, occupies larger volume ratio in mixed powder, and the change of its plasticity is not significantly reduced after adding HIGH-PURITY SILICON iron powder
Shape ability, can be by being molded squarely base.Be heated to 950~1050 DEG C and realize Fe phase austenitizings, with extrusion ratio for 8~
16 deflection is hot extruded into slab.Then powder extruding slab is subjected to vacuum or reduction in 1060~1160 DEG C of temperature ranges
Gas-protecting sintering, makes Fe powder particles realize metallurgical binding, and Si and Fe realize it is partially-alloyed, formed densification, there is modeling
α-Fe the crystal grain of the poor Si of property deformability and the high silicon steel blank of heterogeneous structure of the high Si phases of brittleness.Subsequently through multiple cold rolling, low
Warm diffusion-sintering, the density rise of slab, plate thickness are reduced, and the alloying level of Si is also continuously improved.Finally 1270~
Vacuum or protection of reducing atmosphere sintering in 1320 DEG C of temperature ranges, realize the homogeneous alloy of high silicon steel with the help of thermal diffusion
Change, obtain 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.4g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining is the impurity such as Si, Mn, P, S, in
Particle diameter is located at 45~150 μm；The Si contents of refining are used as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, this HIGH-PURITY SILICON
Iron powder is in addition to containing 50~70%Si, and major impurity is~0.24%Al ,~0.07%Ca and~0.02%C, remaining is
Fe。
Water atomization Fe powder is a kind of widely used Industrial iron powder, has subsphaeroidal pattern, impurity content is less than reduction Fe
Powder, has the compressibility and mobility of higher, is conducive to the Uniform Flow of powder extrusion process course powder.Water atomization Fe powder
In low impurity content it is favourable to the soft magnetic characteristic of high silicon steel.
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 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 conducive 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, powder hot extrusion,
Inert gas shielding should be used in the operation of rolling, 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, water atomization Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders 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 6.32~6.49g/cm3；Using square extruding
Cylinder, extrusion ratio are 8~16, using sintered-carbide die, lubricant are done with machine oil and glass dust, by molding square billet in nitrogen before 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 7.37~7.49g/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/programming rate of min, it is warming up to 1060~1160 DEG C of 2~4h of heat preservation sintering.Sintered blank density is 7.35~7.42g/cm3。
Compared with extruded stock density, density slightly reduces.
Used sintering range is actually the sintering process of current powder metallurgical ferrous alloy, has been had been subjected to wide
General practical proof.Sintering temperature is too low, is unfavorable for metallurgical binding and the Si element thermal diffusions of Fe powder particles；And sintering temperature mistake
High it will cause Si elements quickly to spread, and causes 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 30~40%, 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 7.36~7.43g/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 30~40%, 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 30~40% 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 slightly reduces, and reaches 7.42~7.46g/cm3。
The HIGH-PURITY SILICON iron 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 the high Si iron of passivation
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) uses the square extrusion cylinder of 40 × 120mm, and 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, protects molding square billet in nitrogen before extruding
950~1050 DEG C are heated under shield effect, 2~4h, extrusion cylinder and extrusion die are kept the temperature in 600 DEG C of preheating insulation 2h, using 300 tons
Press implements hot extrusion, and the density of slab is 7.37~7.49g/cm after hot extrusion3, three point bending test shows plasticity, curved
Qu Qiangdu is 72~197MPa.
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 granularity≤6 in the water atomization 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 >=7.4g/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 water atomization Fe powder of -100 mesh and the Fe-70%Si high-purity powders of granularity≤6 μm according to 90.43:9.57 ratio
Example mixing, forms the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine are added during mixing
Oil.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
6.32g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 5 × 120mm, and corresponding extrusion ratio is 8.Will 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.Adopt
Implement hot extrusion with 300 tons of press, the density of slab is 7.37g/cm after hot extrusion3, three point bending test shows plasticity, sees
Fig. 1, bending strength 72MPa.
Using the programming rate of 2 DEG C/min, 1060 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.35g/cm3.Burn
The texture of coarse crystal containing the second phase is formed after knot.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~40%, then in 1060 DEG C of heat preservation sintering 2h in sintering furnace.Specifically pressure-annealing schedule is：5mm→
3.5mm → 2.4mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate
Reach 0.49mm, density reaches 7.36g/cm3。
1h finally is sintered in 1320 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 7.42g/cm3。
Embodiment 2
By the water atomization Fe powder of -100 mesh and the Fe-50%Si high-purity powders of granularity≤10 μm according to 91:9 ratio is mixed
Close, 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.Nothing
Water-ethanol 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
6.49g/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 7.49g/cm after hot extrusion3, three point bending test shows plasticity,
Bending strength is 197MPa.
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 7.42g/cm3.Burn
The texture of coarse crystal containing the second phase is formed after knot, sees Fig. 2.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) phase, such as
Fig. 3 findings, body-centred cubic several characteristic peaks have obvious separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, its
In must have 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 30~40%, 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 7.43g/cm3.Specifically cold rolling-sintering schedule is：2.5mm→1.85mm→1.39mm→
1.15mm → 0.89mm → 0.65mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., through 10 cold rollings and
After 9 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.43g/cm3。
4h finally is sintered in 1270 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 7.46g/cm3。
Embodiment 3
By the water atomization 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% methyl are added during mixing
Cellulose, 0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Above-mentioned powder is mixed using drum mixer
Close 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 7.40g/cm after hot extrusion3, bending strength 120MPa.
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 7.38g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, and specific cold rolling-sintering schedule is：4.0mm→2.8mm→
2.0mm → 1.40mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 7 cold rollings and 6 sintering, the thickness of plate
Degree reaches 0.27mm, and density reaches 7.41g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.42g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the water atomization 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
6.40g/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 7.42g/cm after hot extrusion3, bending strength 126MPa.
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 7.40g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~40%, then in 1120 DEG C of heat preservation sintering 1h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate
Reach 0.22mm, density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is：3.2mm→2.4mm→2.0mm→1.3mm→
0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., after 9 cold rollings and 8 sintering, the thickness of plate reaches
0.21mm, density reach 7.46g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.46g/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 method that powder extruding prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that comprise the following steps：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, use the Si contents of refining as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, the major impurity of HIGH-PURITY SILICON iron powder
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, water atomization Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed；In inertia
Mixed under protective atmosphere using low energy mixer；
(3) powder extrudes
Square pressed compact is prepared using compression-moulding methods, green density is 6.32~6.49g/cm3；Using square extrusion cylinder, squeeze
Pressure ratio is 8~16, 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 7.37~7.49g/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, sintering slab density is 7.35~7.42g/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 30~40%, 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 7.36~7.43g/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 7.42~7.46g/cm3。
2. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
The HIGH-PURITY SILICON iron powder of particle diameter≤6 μm is by high-energy ball milling or rushes the acquisition of rotation method.
3. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
It is water-insoluble as binder, the additive amount total amount of binder that step (2) adds cellulose, paraffin micro mist or zinc stearate when mixing
No more than the 0.8% of mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, play high Si iron powders of passivation, 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.
5. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
Using the square extrusion cylinder of 40 × 120mm in step (3), extrusion die is 5~2.5mm × 120mm, and corresponding extrusion ratio is respectively 8
~16；Using sintered-carbide die, lubricant is done with machine oil and glass dust, implements hot extrusion using 300 tons of press, after hot extrusion
The density of slab is 7.37~7.49g/cm3, three point bending test shows plasticity, and bending strength is 72~197MPa.
6. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the method that powder extruding as claimed in claim 1 prepares high silicon steel band with High temperature diffusion sintering, it is characterised in that：
During high temperature sintering described in step (6), overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, on plate
Tablet weight is placed, prevents from deforming in sintering process.
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