CN107900355A - A kind of method that powder warm-rolling prepares high silicon steel thin belt material - Google Patents
A kind of method that powder warm-rolling prepares high silicon steel thin belt material Download PDFInfo
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- CN107900355A CN107900355A CN201711369182.XA CN201711369182A CN107900355A CN 107900355 A CN107900355 A CN 107900355A CN 201711369182 A CN201711369182 A CN 201711369182A CN 107900355 A CN107900355 A CN 107900355A
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- 239000000843 powder Substances 0.000 title claims abstract description 126
- 238000005096 rolling process Methods 0.000 title claims abstract description 53
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 title claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 84
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 49
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 38
- 230000009467 reduction Effects 0.000 claims abstract description 34
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- 238000009792 diffusion process Methods 0.000 claims abstract description 13
- 238000005097 cold rolling Methods 0.000 claims abstract description 12
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims description 16
- 239000000314 lubricant Substances 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 11
- 238000005238 degreasing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
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- 238000000265 homogenisation Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000000713 high-energy ball milling Methods 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000000956 alloy Substances 0.000 abstract description 19
- 229910045601 alloy Inorganic materials 0.000 abstract description 18
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 238000005275 alloying Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 10
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- 229910017082 Fe-Si Inorganic materials 0.000 description 8
- 229910017133 Fe—Si Inorganic materials 0.000 description 8
- 238000009413 insulation Methods 0.000 description 6
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000000137 annealing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
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- 238000002360 preparation method Methods 0.000 description 5
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- 229910005347 FeSi Inorganic materials 0.000 description 4
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- 229910005331 FeSi2 Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000000354 decomposition reaction Methods 0.000 description 2
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- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
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- 238000007670 refining Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- XIVNZHXRIPJOIZ-UHFFFAOYSA-N octadecanoic acid;zinc Chemical compound [Zn].CCCCCCCCCCCCCCCCCC(O)=O XIVNZHXRIPJOIZ-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000008520 organization Effects 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
- 238000004801 process automation Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 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
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe 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
- 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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- 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)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
A kind of method that powder warm-rolling prepares high silicon steel thin belt material; the present invention is using reduction Fe powder; Si contents are 50~70% HIGH-PURITY SILICON iron powder; form Fe 4.5~6.7%Si mixed powders; powder warm-rolling slab is subjected to vacuum or protection of reducing atmosphere sintering in 1050~1150 DEG C of temperature ranges; Fe powder particles are made to realize not exclusively sintering, and Si and Fe realizes partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation.Subsequently through multiple cold rolling, not exclusively sintering; finally vacuum or protection of reducing atmosphere sintering in 1255~1330 DEG C of temperature ranges; the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.34~7.44g/cm of density3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder of the high silicon steel soft magnetism band of high-performance
The metallurgy sintered and method of 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 a kind of method that powder warm-rolling 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, adds compound mixture, forms the powder mixture for being adapted to warm-rolling deformation, then prepare using powder warm rolling method
Certain thickness slab, forms porous, heterogeneous blank after degreasing, sintering, is obtained after multi-pass cold rolling-sintering thin
Plate, is finally sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous.
The present invention is achieved by the following technical solutions：Using the reduction Fe powder of irregular pattern, fine Si contents
For 50~70% HIGH-PURITY SILICON iron powder, Fe-4.5~6.7%Si mixed powders are formed.Using compound mixture in mixed process
HIGH-PURITY SILICON iron powder is adhered in the hole of reduced iron powder surface or filling ferrous powder.Since reduction Fe powder is with high-compressibility
Big particle, occupies larger volume ratio in mixed powder, after adding the HIGH-PURITY SILICON iron powder that fine Si contents are 50~70%
Its deformability will not be significantly reduced.The technological merit of warm-rolling shaping is played, implements the shaping of powder warm-rolling, system at 125~150 DEG C
It is standby go out density is higher, the uniform slab of Tissue distribution.Powder warm-rolling slab is subjected to vacuum in 1050~1150 DEG C of temperature ranges
Or protection of reducing atmosphere sintering, make Fe powder particles realize not exclusively sintering, and Si and Fe realize it is partially-alloyed, formation it is porous,
The high silicon steel blank of incomplete alloying with compressibility.Subsequently through multiple cold rolling, not exclusively sintering, the density of slab
Rise, plate thickness are reduced, and the alloying level of Si is also continuously improved.Finally in 1255~1330 DEG C of temperature ranges vacuum or also
Former gas-protecting sintering, realizes the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtains 0.1 containing 4.5~6.7%Si
~0.5mm is thick, 7.34~7.44g/cm of density3High 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 Si, Mn, P, S and other are inevitable
Impurity, using the Si contents of refining, particle diameter≤6 μm, this ferrosilicon powder is except containing 50 for 50~70% HIGH-PURITY SILICON iron powder
Beyond~70%Si, major impurity is~0.24%Al ,~0.07%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to
Thin and tall pure silicon iron powder, and during follow-up powder warm-rolling also being mutually twisted for powder easy to implement and improve the intensity of pressed compact,
Be conducive to the stabilization of powder warm-rolling technique.
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, the operation of rolling
In should use inert gas shielding, used instrument must also take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as Al, Ca, Mn to alloy magnetic property is little, during introduce
The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed；Lazy
Property protective atmosphere under using low energy mixer mix.During mixing, the lubricant of addition powder total amount 0.4~0.6%.
Powder warm-rolling technique can reduce the interior friction in powder deformation process, improve powder compact density and density, group
Uniformity is knitted, reduces the fretting wear to tool and mould.Lubricant is the key of technique success or not, and the selection principle of lubricant should
When meeting glass transition temperature at 120~150 DEG C or so, the condition such as low friction factor.Common powder warm deformation binder has
Very much.
(3) powder warm-rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
It is 1.2~2.3mm to roll out thickness, and width is 100~200mm, and density is 6.1~6.5g/cm3Powder warm-rolling slab.Roll
Mixed-powder is heated to 125~150 DEG C using powder heating unit before system, and roll is preheating to same temperature.
Go out the difference in roller direction by band, powder warm-rolling can be divided into vertical, horizontal and tilt 3 kinds of forms, and feeding manner has
Dead weight feeding, forced feed, pre-glued feeding etc..The width of blank is related with the width of feeding trough, and the length of blank regards production
Depending on condition is permitted and is actually needed.
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.
2h~4h is kept the temperature respectively using the programming rate of 2~5 DEG C/min, and in 200 DEG C, 400 DEG C.Then will heat up to 1050~1150
DEG C 2~4h of heat preservation sintering.Sintered blank density is 6.15~6.55g/cm3。
Uniform equiaxed grain structure is formed after sintering, matrix grain is about 70~100 μm, and crystal boundary exists about~10 μm
Hole, follow-up rolling and sintering can close.Only a small amount of the second phase about~2 μm is remained in matrix, with base
Body tissue has good interface cohesion, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these richnesses Si
The presence of phase, reduces the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile itself and base
The highly organized interface cohesion of body and Dispersed precipitate are conducive to subsequently homogenization diffusion.
Sintering temperature is too low, the connection being unfavorable between Fe powder particles and Si atoms permeatings, and sintering temperature is excessive then can be by
In the diffusion into the surface of Fe, Si element, there is thick hole, be subsequently difficult to press, rolling densification is difficult to realize.
During sintering can powder warm-rolling blank can be placed with multilayer, but must separate between layers, to avoid plate during sintering
Base, which is shunk, to be caused to crack.Programming rate should not be too fast during sintering, and multistage insulation can be set in temperature-rise period, to realize degassing, take off
The effect of fat.Reproducibility or inert gas shielding degreasing, sintering can also be taken.W, Mo, heat resisting steel etc. can be used during sintering
As support plate (or burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity it is good and beneficial to uniformly
Sintering shrinkage.
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~50%, in sintering furnace, 0.5~2h is re-sintered in 1050~1150 DEG C.After multiple cold rolling-sintering, the thickness of plate reaches
To 0.1~0.5mm, density reaches 7.33~7.43g/cm3。
Since powder batch is porous organization, and there are deformable Fe phases, slab can bear cold-rolling deformation.Palette
There is also more high Si phases in base, its performance is more crisp, therefore not above 8%, accumulation total reduction reaches amount under every time rolling
8~20 passages are taken around to 30~50%.
Due to there are a large amount of holes and hard crisp phase, taking when re-sintering for 1050 DEG C~1150 DEG C, being in vacuum or reduction
Property protective atmosphere sintering, to realize the reparation of the closing of pores and crackle, and the homogenization diffusion of a degree of Si elements.At this time
Programming rate can be very fast, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm, insulation
Time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.The accumulation drafts after sintering reaches 30 every time
, it is necessary to sinter 1 time again after~50%, 0.1~0.5mm is rolled down to from the powder base of 1.2~2.3mm, takes around and sinters again
4~8 times.In addition, in order to make the density of plate reach 7.2g/cm3More than the 95% of solid density (about), it is also desirable to 4 times with
On re-sinter.
Matrix after 2 cold rolling-sintering is about 100 μm of grain structure, there is a small amount of tiny hole.Matrix is brilliant
Grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, low Si crystal grain is conducive in this kind tissue
Machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1255~1330 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 7.34~7.44g/cm3。
The HIGH-PURITY SILICON iron powder high-energy ball milling of particle diameter≤6 μm rushes the acquisition of rotation method.
The low energy batch mixer is conical mixer, V-arrangement batch mixer or drum mixer.
Powder gross mass is added when step (2) mixes and is 0.4~0.6% lubricant, while adds powder gross mass
0.1% glycerine, the lubricant are compounded lubricant, are made of zinc stearate and vinyl bis-stearamides, stearic acid
Zinc:EBS is 4:6~2:8, using absolute ethyl alcohol as solvent, added according to the amount of 400~600ml of mixed-powder per ton.
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 μm in the reduction Fe powder of the big volumetric portion with good plasticity
Fe-50~70%Si high-purity powders, form a kind of composite material of achievable powder warm-rolling；Prepared using warm-rolling shaping
Density is higher, the uniform slab of Tissue distribution；By not exclusively sintering, Fe powder particles is realized not exclusively and connect, and Si and Fe
Realize partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation；Subsequently through multi-pass
Cold rolling and sintering, improve structural homogenity and compactness；Again by high-temperature diffusion process, the homogenization of Si is realized, so as to obtain
The high silicon steel band of high quality.This method realizes Technics Process Automation, continuous production by technique and equipment Design, can
It is thick to produce 0.1~0.5mm in enormous quantities, 7.34~7.44g/cm of density3High silicon steel band.
Brief description of the drawings
Fig. 1 is the metallograph after the powder warm-rolling base sintering of the embodiment of the present invention 2；
Fig. 2 is metallograph of the plate of the embodiment of the present invention 3 after 2 cold rolling-sintering；
Fig. 3 is XRD diffraction curve figures after the powder warm-rolling base 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.During mixing total amount of adding be 0.4% compounded lubricant, and 0.1% it is sweet
Oil mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.It is composite lubricated
Agent is made of zinc stearate and EBS, zinc stearate:EBS is 2:8.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Mixed-powder is heated to 140 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 2.3mm
Last warm-rolling slab, the width of slab is 100mm.The density of pressed compact is 6.1g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming rate of 2 DEG C/min, and 4h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1050 DEG C of heat preservation sintering 4h.Burn
It is 6.15g/cm to tie base density3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~50%, then in vacuum sintering furnace, in 1050 DEG C of heat preservation sinterings.With 5 DEG C/min speed continuous warmings, soaking time regards plate
Thickness determines, during thickness of slab >=1mm, soaking time 2h；Thickness of slab is in 0.1~1mm, soaking time 1h.Specific pressure-annealing schedule
For：2.3mm → 1.56mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.50mm, density reaches 7.33g/cm3。
For above-mentioned cold rolling made-up belt in 1330 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.34g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
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.Total amount of adding is 0.5% compounded lubricant during mixing, and 0.1% glycerine subtracts
The oxidation of calomel mercurous chloride end heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by hard
Resin acid zinc and EBS compositions, zinc stearate:EBS is 4:6.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 125 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 1.2mm
Last warm-rolling slab, the width of slab is 200mm.The density of pressed compact is 6.5g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming rate of 5 DEG C/min, and 2h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1150 DEG C of heat preservation sintering 2h.Burn
It is 6.55g/cm to tie base density3。
Uniform equiaxed grain structure is formed after sintering, sees Fig. 1.Matrix grain is about 70~100 μm, and crystal boundary exists about~10
μm hole, follow-up rolling and sintering can close.Only a small amount of the second phase about~2 μm is remained in matrix,
There is good interface cohesion with matrix, i.e., the face divided do not occur.These obvious second phases are certain richness Si phases, these
The presence of rich Si phases, reduces the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile its
Good interface cohesion and Dispersed precipitate are conducive to subsequently homogenization diffusion with matrix.
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~50%, then in vacuum sintering furnace, in 1150 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is
1h.Specifically pressure-annealing schedule is：1.2mm→0.75mm→0.49mm→ 0.32mm→0.19mm→0.14mm→
0.10mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.43g/cm3。
For above-mentioned cold rolling made-up belt in 1255 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.44g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
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.Total amount of adding is 0.6% compounded lubricant during mixing, and 0.1%
Glycerine mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compound profit
Lubrication prescription is made of zinc stearate and EBS, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 125 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 1.6mm
Last warm-rolling slab, the width of slab is 160mm.The density of pressed compact is 6.16g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 3 DEG C/min, and 2h, 400 DEG C of insulation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1120 DEG C of insulations and burn
Tie 3h.Sintered blank density is 6.2g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~50%, then in hydrogen tube furnace, in 1120 DEG C of heat preservation sintering 1h.With 6 DEG C/min speed continuous warmings.Specific pressure-
Annealing schedule is：1.6mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate
Thickness reach 0.27mm, density reaches 7.37g/cm3。
Fig. 2 is shown in metallographic structure after 2 cold rolling-sintering, and matrix is about 100 μm of grain structure, exists a small amount of thin
Small hole.Matrix grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, in this kind tissue
Low Si crystal grain is conducive to machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.38g/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.Total amount of adding is 0.6% compounded lubricant during mixing, and 0.1%
Glycerine mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compound profit
Lubrication prescription is made of zinc stearate and EBS, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 3h.
Mixed-powder is heated to 150 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 2.0mm
Last warm-rolling slab, the width of slab is 120mm.The density of pressed compact is 6.2g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 4 DEG C/min, and 3h, 400 DEG C of insulation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of insulations and burn
Tie 2h.Sintered blank density is 6.26g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~50%, then in hydrogen tube furnace, in 1130 DEG C of heat preservation sintering 0.5h.With 8 DEG C/min speed continuous warmings.Specific pressure
Under-annealing schedule is：2.0mm → 1.3mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm is that is, cold through 7 times
Roll with after 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.38g/cm3。
For above-mentioned cold rolling made-up belt in 1285 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.39g/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 warm-rolling prepares high silicon steel thin belt material, it is characterised in that including including 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, uses Si contents as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, and major impurity is~0.24%Al ,~0.07%Ca
With~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed；Protected in inertia
Protect under atmosphere and mixed using low energy mixer, total amount of adding is 0.4~0.6% lubricant during mixing；
(3) powder warm-rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder, rolled
It is 1.2~2.3mm to go out thickness, and width is 100~200mm, and density is 6.1~6.5g/cm3Powder warm-rolling slab.Before rolling
Mixed-powder is heated to 125~150 DEG C using powder heating unit, and roll is preheating to same temperature；
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The programming rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, then it will heat up to 1050~1150 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density is 6.15~6.55g/cm3；
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reach 30 through multi- pass rolling to total reduction~
After 50%, then in sintering furnace, after 1050~1150 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering, the thickness of plate
Reach 0.1~0.5mm, density reaches 7.33~7.43g/cm3；
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1255~1330 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 7.34~7.44g/cm3。
2. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：The grain
Footpath≤6 μm HIGH-PURITY SILICON iron powder high-energy ball milling rushes the acquisition of rotation method.
3. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：Described is low
Energy batch mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：Step (2)
The lubricant that gross mass is 0.4~0.6%, and the glycerine of gross mass 0.1% are added during mixing, the lubricant is compound
Lubricant, is made of zinc stearate and vinyl bis-stearamides, zinc stearate:EBS is 4:6~2:8, made using absolute ethyl alcohol
For solvent, added according to the amount of 400~600ml of mixed-powder per ton.
5. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：Step (5)
Vacuum-sintering or restitutive protection's atmosphere sintering are taken when being sintered again after cold rolling, programming rate is in 5~10 DEG C/min, continuous liter
Temperature, soaking time determine according to thickness of slab, and during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab subtracts in 0.1~1mm, soaking time
Less to 0.5~1h；After the accumulation drafts after sintering reaches 30~50% every time, sinter 1 time again, from the powder of 1.2~2.3mm
Base is rolled down to 0.1~0.5mm, it is necessary to sinter 4~8 times again.
6. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：Step (4)
The support plate uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the method that a kind of powder warm-rolling as claimed in claim 1 prepares high silicon steel thin belt material, it is characterised in that：High temperature sintering
When overlapping place sintering plate, interlayer be laid with MgO powder, plate tiling place, on plate place tablet weight, prevent sintered
Deformed in journey.
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Inventor after: Luo Fenghua Inventor after: Zhao Jiazheng Inventor after: Li Yimin Inventor after: Jia Jixiang Inventor after: Feng Ziheng Inventor before: Luo Fenghua Inventor before: Wang Hande Inventor before: Li Yimin Inventor before: Jia Jixiang Inventor before: Feng Ziheng |
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Application publication date: 20180413 |
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