CN108044096A - A kind of method that High temperature diffusion sintering prepares Fe-6.5%Si bands with tape casting - Google Patents

A kind of method that High temperature diffusion sintering prepares Fe-6.5%Si bands with tape casting Download PDF

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CN108044096A
CN108044096A CN201711368373.4A CN201711368373A CN108044096A CN 108044096 A CN108044096 A CN 108044096A CN 201711368373 A CN201711368373 A CN 201711368373A CN 108044096 A CN108044096 A CN 108044096A
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sintering
powder
high temperature
bands
mixed
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丁艺
罗丰华
唐琳
吴宁
贾吉祥
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Central South University
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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
    • 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
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
    • 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
    • B22F3/1021—Removal of binder or filler
    • 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
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

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  • Manufacturing & Machinery (AREA)
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Abstract

A kind of method that High temperature diffusion sintering prepares Fe 6.5%Si bands with tape casting, the present invention chooses reduction Fe powder and water atomization Fe powder, according to 4:6~6:4 ratio mixing, then the HIGH-PURITY SILICON iron powder that Si contents are 50~70% is added, form Fe 4.5~6.7%Si mixed powders.Solvent, dispersant, bonding agent and plasticizer are added in mixed powder; finely dispersed stable slurry is made; biscuit is made on casting machine again; biscuit at 1060~1160 DEG C is carried out to vacuum or protection of reducing atmosphere sintering, the high silicon steel blank of incomplete alloying porous, that there is compressibility is formed, through multiple cold rolling, not exclusively sintering; finally in 1250~1320 DEG C of sintering; it realizes the homogeneous alloy of high silicon steel, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.39g/cm3High silicon steel band.

Description

A kind of method that High temperature diffusion sintering prepares Fe-6.5%Si bands with tape casting
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 Metallurgy sintered and rolling deformation method.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis loop is very narrow, it and fundamental magnetization curve are almost It overlaps, is 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.There is no absolute predominances, such as slope in soft magnetic materials for the maximum permeability of Fe-Si alloys The maximum permeability of alloy can not reach 200000.However the manufacture of the Fe-Si lattens of Si ＜ 4.5% is at low cost, 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 increases with Si contents And reduce, it disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases with Si contents and is increased, 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 the iron core of amount or large size is sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially It is in the military aviations such as spacecraft, submarine and guided missile field, Fe-Si systems alloy plays particularly important role.20th century 60 Age Mo, the alloy of Si contents 6.5% are appeared in as transformer material on No. 11 airships of Apollo, are completed the mankind and are landed on the moon for the first time 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 is for the first time the study found that 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 have lower iron loss and higher magnetic conductivity.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 spends for 0.1~0.5mm, width is the No yield point 6.5%Si steel discs of 400mm.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 to alloy diffusion inside alloy is finally made to reach required content by raised 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 It asks, 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 ", and 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, 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 generate huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of sintering of High temperature diffusion Fe-6.5%Si thin strips are prepared with powder tape casting Method, the problem of being difficult to shape for the Fe-Si alloy thin band materials of 4.5~6.7%Si contents, contained with technical pure Fe powder with Si It is raw material to measure as 50~70% HIGH-PURITY SILICON iron powder, then prepares certain thickness slab using powder curtain coating forming method, Porous, heterogeneous blank is formed after degreasing, sintering.Fe crystal grain containing substantial amounts of non-alloying in blank, has good Plasticity obtains thin plate after multi-pass cold rolling-sintering, 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：Reduction Fe powder and two kinds of Industrial iron powders of water atomization Fe powder are chosen, According to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, then it is 50~70% to add fine Si contents HIGH-PURITY SILICON iron powder forms Fe-4.5~6.7%Si mixed powders.Again in mixed powder add in solvent, dispersant, bonding agent, The ingredients such as plasticizer are made finely dispersed stable slurry, then certain thickness biscuit are made on casting machine.Tape casting system Powder particle distributing homogeneity is high in the biscuit obtained, while technical pure Fe powder is the big particle with high-compressibility, is being mixed Occupy larger volume ratio in powder, its change will not be significantly reduced after adding the HIGH-PURITY SILICON iron powder that fine Si contents are 50~70% Shape ability.Powder curtain coating shaping slab is subjected to vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges, is made Fe powder particles realize not exclusively sintering, and Si and Fe realizations are partially-alloyed, and formation is porous, has not closing completely for compressibility The high silicon steel blank of aurification.Subsequently through multiple cold rolling, not exclusively sintering, the density rise of slab, plate thickness are reduced, the conjunction of Si Aurification degree is also continuously improved.Finally vacuum or protection of reducing atmosphere sintering in 1250~1320 DEG C of temperature ranges, in thermal expansion The homogeneous alloy of high silicon steel is realized with the help of dissipating, 0.1~0.5mm of the acquisition containing 4.5~6.7%Si is thick, density >= 7.39g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitable Impurity, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining for Si, Mn, P, S and other can not The impurity avoided, by reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, and is mixed using conical mixer, V-arrangement Material machine or drum mixer are mixed to form technical pure Fe powder basic materials, and incorporation time is 2~6h；
Using Si contents, grain size≤6 μm, this ferrosilicon powder is except containing 50~70% for 50~70% HIGH-PURITY SILICON iron powder Beyond Si, major impurity is~0.24%Al ,~0.07%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to Fine silica powder, and subsequently curtain coating, in deformation process also being mutually twisted for powder easy to implement and improve intensity.Water atomization Fe powder It is a kind of widely used Industrial iron powder, there is subsphaeroidal pattern, impurity content has higher compressible less than reduction Fe powder Property and mobility, be conducive to the Uniform Flow of powder curtain coating molding process powder, low impurity content in water atomization Fe powder It is favourable to the soft magnetic characteristic of high silicon steel.Fe powder and two kinds of Industrial iron powders of water atomization Fe powder will be reduced, according to 4:6~6:4 ratio Mixing forms technical pure Fe powder basic materials, is conducive to play two kinds of respective advantages of straight iron powder, in industrial production iron-base part And relatively common method.
Fe-50~70%Si high purity ferrosilicons in process of setting there are two eutectic reactions, when rich Si one sides are at 1207 DEG C Form the β-FeSi with tP3 structures2With Si phase eutectic structures, form when rich Fe one 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 subtle 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, Si phases, FeSi in actual tissue2, 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 grain size≤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 subsequent blank toughness, cracking do not easily caused in densification process is rolled.But Fe-50 Still containing 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, curtain coating, rolled Cheng Zhongying uses inert gas shielding, and 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, introduces in the process The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, pre- mixed Fe powder and fine Fe-50~70%Si high purity ferrosilicons are weighed Powder forms metal powder raw material, and phosphoric acid and absolute ethyl alcohol are pressed 0.8~2.0:100 ratio is mixed to prepare passivating solution, will be passivated Liquid and the metal powder raw material that has weighed are according to 0.4~0.6:1 ratio mixing, after stirring 0.5~2h with mixer, is put into baking Case is passivated, and baking temperature is 40~42 DEG C, and passivation time is 4~6h, obtains passivation powder.
Powder will be passivated with organic solution according to volume ratio 1:0.5~1 ratio mixing, 6~12h is stirred with mixer, Again with 5~15min of ultrasonic disperse, through screen filtration, the slurry for the even dispersion made after vacuum outgas, the viscosity of slurry for 40~ 80MPa.s。
Doctor-blade casting process is commonly called as scraper forming process, is a kind of important forming method for preparing large area film, is used The species such as organic solvent, dispersant, plasticizer, binding agent it is various, above-mentioned pulping process is a kind of feasible method, not Represent method.
(3) powder tape casting
During curtain coating environment temperature be 28~32 DEG C, will disperse slurry inject casting machine in, control casting machine speed be 0.1~ 0.5cm/s, the height of scraper is 1.2~2.4mm, and width is 100~300mm.
It is 30~40 DEG C to be cast biscuit drying temperature, and relative humidity is 30~60%, and the thickness of biscuit is after slurry drying 1.0~2.1mm carries out curing process in a nitrogen atmosphere, and solidification temperature is 120~200 DEG C, and hardening time is 1~5h, with stove It is cooled to room temperature, the dry curtain coating slab dense structure of preparation, porosity is low, surfacing, because containing more plasticizer, bonding The organic matters such as agent, density are 6.1~6.5g/cm3。
(4) degreasing, sintering
Curtain coating slab is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, 2h~4h is kept the temperature respectively using the heating rate of 2~5 DEG C/min, and in 200 DEG C, 400 DEG C, then will heat up to 1060~1160 DEG C 2~4h of heat preservation sintering, sintered blank density are 6.2~6.7g/cm3。
Uniform equiaxed grain structure is formed after sintering, matrix grain is about 70~100 μm, and crystal boundary has hole about~10 μm Gap, subsequent rolling and sintering can be closed.Only a small amount of the second phase about~2 μm is remained in matrix, with matrix Tissue has good interface cohesion, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these richness Si phases Presence, reduce the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile with matrix Highly organized interface cohesion 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 excessively high then can be by In the diffusion into the surface of Fe, Si element, there is coarse hole, be subsequently difficult to press, rolling densification is difficult to realize.
During sintering can powder curtain coating shaping blank can be placed with multilayer, but must separate between layers, to avoid sintering When slab contraction cause to crack.Heating rate should not be too fast during sintering, and multistage heat preservation can be set in temperature-rise period, de- to realize Gas, the effect of degreasing.Reproducibility or inert gas shielding degreasing, sintering can also be taken.W, Mo, resistance to may be employed during sintering Hot steel etc. can also use the ceramic wafers such as corundum, zirconium oxide, but metallic plate thermal conductivity is good and sharp as support plate (or burning boat) It is shunk in Even Sintering.
(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~45%, in sintering furnace, 0.5~2h is re-sintered in 1060~1160 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches To 0.1~0.5mm, density reaches 7.38~7.49g/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, performance is more crisp, therefore not above 8%, accumulation total reduction reaches amount under every time rolling 8~20 passages are taken around to 30~45%.
Due to there are a large amount of holes and hard crisp phase, selecting when re-sintering for 1060 DEG C~1160 DEG C, in vacuum-sintering or also Atmosphere is sintered under originality protection gas, to realize the reparation of the closing of pores and crackle and the homogenization diffusion of a degree of Si elements. Heating rate can be very fast at this time, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm, Soaking time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.Sintered accumulation drafts reaches every time , it is necessary to be sintered 1 time again after to 30~45%, 0.1~0.5mm is rolled down to from the biscuit of 1.0~2.1mm, is taken around again Sintering 4~8 times.In addition, in order to which the density of plate is made to reach 7.2g/cm3More than (about the 95% of theoretical density), it is also desirable to 4 Secondary above re-sinters.
By the grain structure that 2 cold rollings-sintered matrix is about 100 μm, there is a small amount of tiny hole.Matrix is brilliant Grain is there are two types 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
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1250~1320 DEG C of temperature ranges, in the effect of thermal diffusion Under, it realizes the homogenization of Si, forms single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost unchanged after densification sintering, For 0.1~0.5mm, density reaches 7.39~7.50g/cm3。
Mixing iron powder per ton adds in the absolute ethyl alcohol of 200~500ml in step (1) mixed process.
Organic solution described in step (2) is with 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, with asphalt mixtures modified by epoxy resin Fat is binding agent, and polyethylene glycol is plasticizer, and triethanolamine is dispersant, and the volume ratio of epoxy resin and polyethylene glycol presses 1: 1, then by mixed solvent quality be 50~70%, dispersant quality is 0.1%, the slurry that surplus is formed for binding agent and plasticizer Organic solution.
With high-energy ball milling or rush rotation method acquisition grain size≤6 μm HIGH-PURITY SILICON iron powder.
Step (5) is sintered when re-sintering for 1060~1160 DEG C under vacuum-sintering or restitutive protection's atmosphere, by 5~ 10 DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab is reduced to 0.5 in 0.1~1mm, soaking time ~1h after sintered accumulation drafts reaches 30~40% every time, is sintered 1 time, is rolled from the biscuit of 1.0~2.1mm again To 0.1~0.5mm, it is necessary to be sintered 4~8 times again.
Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo can be used and ceramics are burnt Boat.But plate must tile placement, and tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of elements such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel Large effect can subsequently be annealed by wet hydrogen, the technological means such as normalizing treatment are controlled by.
Essence of the invention is by being with the addition of granularity≤6 in the technical pure Fe powder of the big volumetric portion with good plasticity μm Fe-50~70%Si high-purity powders, using organic curtain coating system, it is molding compound to form a kind of achievable powder curtain coating Material；The uniform slab of density, Tissue distribution is prepared using tape casting；By being not exclusively sintered, realize Fe powder particles Not exclusively connection, and Si and Fe realizes partially-alloyed, the high silicon steel of porous, with compressibility the incomplete alloying of formation Blank；Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved；Again by high-temperature diffusion process, realize The homogenization of Si, so as to obtain the high silicon steel band of high quality.This method realizes technical process certainly by technique and equipment Design Dynamicization, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.39g/cm3High silicon steel band.
Description of the drawings
Fig. 1 is the sintered metallograph of powder tape casting base of the embodiment of the present invention 2；
Fig. 2 is that the plate of the embodiment of the present invention 3 passes through 2 cold rollings-sintered metallograph；
Fig. 3 is XRD diffraction curve figures after the powder tape casting base high temperature sintering of the embodiment of the present invention 4.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 4:6 ratio is prepared, and is mixed using drum-type Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 2h, is added in mixed process according to 200ml/ tons of ratio anhydrous Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-70%Si high-purity powders of granularity≤6 μm according to 90.43:9.57 Ratio mixes, and forms the mixed-powder of Fe-6.7%Si.Phosphoric acid and absolute ethyl alcohol are pressed 0.8:100 ratio is mixed to prepare passivation Liquid.By passivating solution and the metal powder raw material weighed according to 0.4:1 ratio mixing, after stirring 0.5h with mixer, is put into Baking oven is passivated, and baking temperature is 40 DEG C, passivation time 4h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is 60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1: 0.5 ratio mixing, 6h is stirred with mixer, then with ultrasonic disperse 5min, through screen filtration, made after vacuum outgas uniformly more Scattered slurry, the viscosity of slurry is 40MPa.s.
Environment temperature is 28 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.5cm/s, The height of scraper is 2.4mm, and width is about 100mm.
It is 40 DEG C to be cast biscuit drying temperature, relative humidity 30%, and the thickness of biscuit is 2.1mm after slurry drying. Curing process is carried out under nitrogen atmosphere, solidification temperature is 200 DEG C, hardening time 5h, cools to room temperature with the furnace, and curtain coating slab is close It spends for 6.1g/cm3。
Curtain coating slab is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts With the heating 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 1060 DEG C of heat preservation sintering 4h.It burns It is 6.2g/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~45%, then in vacuum sintering furnace, in 1060 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：2.5mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches 0.49mm, density reach 7.38g/cm3。
For above-mentioned cold rolling made-up belt in 1320 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.39g/cm to obtain thickness3, Si Content is the 6.7% high silicon steel of single-phase homogeneous.
Embodiment 2
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 5:6 ratio is prepared, and is mixed using drum-type Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 3h, is added in mixed process according to 400ml/ tons of ratio anhydrous Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-50%Si high-purity powders of granularity≤10 μm according to 91:9 ratio is mixed It closes, forms the mixed-powder of Fe-4.5%Si.Phosphoric acid and absolute ethyl alcohol are pressed 2.0:100 ratio is mixed to prepare passivating solution.It will Passivating solution and the metal powder raw material that has weighed are according to 0.6:1 ratio mixing, after stirring 2h with mixer, it is blunt to be put into baking oven Change, baking temperature is 42 DEG C, passivation time 6h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is 60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1:1 Ratio mixing, stir 12h with mixer, then with ultrasonic disperse 15min, through screen filtration, made after vacuum outgas uniformly more Scattered slurry, the viscosity of slurry is 80MPa.s.
Environment temperature is 32 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.1cm/s, The height of scraper is 1.2mm, and width is about 300mm.
It is 30 DEG C to be cast biscuit drying temperature, relative humidity 60%, and the thickness of biscuit is 1.0mm after slurry drying. Curing process is carried out under nitrogen atmosphere, solidification temperature is 120 DEG C, hardening time 1h, cools to room temperature with the furnace, and curtain coating slab is close It spends for 6.5g/cm3。
Curtain coating slab is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts With the heating 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 1160 DEG C of heat preservation sintering 2h.It burns It is 6.7g/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, it is subsequent rolling and sintering can be closed.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 Interface cohesion good with matrix and Dispersed precipitate are conducive to subsequently homogenization diffusion.
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction After~45%, then in vacuum sintering furnace, in 1160 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is 1h.Specifically pressure-annealing schedule is：1.0mm → 0.65mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, I.e. after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.49g/cm3。
For above-mentioned cold rolling made-up belt in 1320 DEG C of vacuum-sintering 1h, it is about 0.10mm, density 7.50g/cm to obtain thickness3, Si Content is the 4.5% high silicon steel of single-phase homogeneous.
Embodiment 3
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 6:4 ratio is prepared, and is mixed using drum-type Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 4h, is added in mixed process according to 500ml/ tons of ratio anhydrous Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-60%Si high-purity powders of granularity≤6 μm according to 89.17:10.83 Ratio mixes, and forms the mixed-powder of Fe-6.5%Si.Phosphoric acid and absolute ethyl alcohol are pressed 1.0:100 ratio is mixed to prepare passivation Liquid.By passivating solution and the metal powder raw material weighed according to 0.5:1 ratio mixing, after stirring 1h with mixer, is put into baking Case is passivated, and baking temperature is 40 DEG C, passivation time 5h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is 60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1: 0.6 ratio mixing, 8h is stirred with mixer, then with ultrasonic disperse 7min, through screen filtration, made after vacuum outgas uniformly more Scattered slurry, the viscosity of slurry is 60MPa.s.
Environment temperature is 30 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.3cm/s, The height of scraper is 1.4mm, and width is about 180mm.
It is 35 DEG C to be cast biscuit drying temperature, relative humidity 45%, and the thickness of biscuit is 1.2mm after slurry drying. Curing process is carried out under nitrogen atmosphere, solidification temperature is 160 DEG C, hardening time 3h, cools to room temperature with the furnace, and curtain coating slab is close It spends for 6.15g/cm3。
Curtain coating slab is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns Knot.Using the heating rate of 3 DEG C/min, and 2h, 400 DEG C of heat preservation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1150 DEG C of heat preservations and burn Tie 3h.Sintered blank density is 6.21g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction After~45%, then in hydrogen tube furnace, in 1150 DEG C of heat preservation sintering 1h.With 6 DEG C/min speed continuous warmings.Specific pressure- Annealing schedule is：1.2mm → 0.92mm → 0.66mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate Thickness reach 0.27mm, density reaches 7.39g/cm3。
See Fig. 2 by 2 cold rollings-sintered metallographic structure, matrix is about 100 μm of grain structure, is existed a small amount of thin Small hole.Matrix grain is there are two types 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 7.40g/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 the reduction Fe powder of -100 mesh and -100 mesh according to 5:5 ratio is prepared, and is mixed using drum-type Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 6h, is added in mixed process according to 500ml/ tons of ratio anhydrous Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-62%Si high-purity powders of granularity≤10 μm according to 90.64:9.36 Ratio mixes, and forms the mixed-powder of Fe-5.8%Si.Phosphoric acid and absolute ethyl alcohol are pressed 1.2:100 ratio is mixed to prepare passivation Liquid.By passivating solution and the metal powder raw material weighed according to 0.6:1 ratio mixing, after stirring 1h with mixer, is put into baking Case is passivated, and baking temperature is 42 DEG C, passivation time 6h, obtains passivation powder.
With 10:1.0 methyl ethyl ketone and absolute ethyl alcohol is mixed solvent, is increasing by binding agent, polyethylene glycol of epoxy resin Agent is moulded, triethanolamine is dispersant.The volume ratio of epoxy resin and polyethylene glycol presses 1:1, the addition of mixed solvent is 60%, the addition of dispersant is 0.1%, forms the organic solution of slurry.Powder will be passivated with organic solution according to volume ratio 1: 0.7 ratio mixing, stirs 9h, then with ultrasonic disperse 10min, through screen filtration, that is made after vacuum outgas is uniform with mixer The slurry of disperse, the viscosity of slurry is 55MPa.s.
Environment temperature is 30 DEG C during curtain coating, and disperse slurry is injected in casting machine, controls casting machine speed as 0.3cm/s, The height of scraper is 1.8mm, and width is about 200mm.
It is 30 DEG C to be cast biscuit drying temperature, relative humidity 50%, and the thickness of biscuit is 1.6mm after slurry drying. Curing process is carried out under nitrogen atmosphere, solidification temperature is 160 DEG C, hardening time 4h, cools to room temperature with the furnace, and curtain coating slab is close It spends for 6.3g/cm3。
Curtain coating slab is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns Knot.Using the heating rate of 4 DEG C/min, and 3h, 400 DEG C of heat preservation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of heat preservations and burn Tie 2h.Sintered blank density is 6.36g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction After~45%, 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：1.6mm → 1.26mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm is that is, cold through 7 times It rolls with after 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.42g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.43g/cm to obtain thickness3, Si Content is 5.8%, and the XRD analysis figure of final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.

Claims (7)

1. a kind of method that High temperature diffusion sintering prepares Fe-6.5%Si bands with tape casting, it is characterised in that including following step Suddenly：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitably miscellaneous Matter, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining is Si, Mn, P, S and other are inevitable Impurity, will reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, using conical mixer, V-arrangement batch mixer Or drum mixer is mixed to form technical pure Fe powder basic materials, incorporation time is 2~6h；
Si contents are used as 50~70% HIGH-PURITY SILICON iron powder, grain size≤6 μm, major impurity is~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, pre- mixed Fe powder and fine Fe-50~70%Si HIGH-PURITY SILICONs iron powder are weighed, Metal powder raw material is formed, phosphoric acid and absolute ethyl alcohol are pressed 0.8~2.0:100 ratio is mixed to prepare passivating solution, by passivating solution With the metal powder raw material that has weighed according to 0.4~0.6:1 ratio mixing, after stirring 0.5~2h with mixer, is put into baking oven Passivation, baking temperature are 40~42 DEG C, and passivation time is 4~6h, obtain passivation powder；
Powder will be passivated with organic solution according to volume ratio 1:0.5~1 ratio mixing, stirs 6~12h with mixer, then uses 5~15min of ultrasonic disperse, through screen filtration, the slurry for the even dispersion made after vacuum outgas, the viscosity of slurry for 40~ 80MPa.s；
(3) powder tape casting
During curtain coating environment temperature be 28~32 DEG C, will disperse slurry inject casting machine in, control casting machine speed be 0.1~ 0.5cm/s, the height of scraper is 1.2~2.4mm, and width is 100~300mm；
It is 30~40 DEG C to be cast biscuit drying temperature, and relative humidity is 30~60%, after slurry drying the thickness of biscuit for 1.0~ 2.1mm, carries out curing process in a nitrogen atmosphere, and solidification temperature is 120~200 DEG C, and hardening time is 1~5h, furnace cooling To room temperature, the dry curtain coating slab density of preparation is 6.1~6.5g/cm3；
(4) degreasing, sintering
Curtain coating slab is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2 The heating rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, it then will heat up to 1060~1160 DEG C of guarantors Temperature 2~4h of sintering, sintered blank density are 6.2~6.7g/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 45%, in sintering furnace, 0.5~2h is re-sintered in 1060~1160 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches 0.1~0.5mm, density reach 7.38~7.49g/cm3；
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1250~1320 DEG C of temperature ranges, it is real under the action of thermal diffusion The homogenization of existing Si forms single-phase alloy, obtains the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering, Density reaches 7.39~7.50g/cm3。
2. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：Mixing iron powder per ton adds in the absolute ethyl alcohol of 200~500ml in step (1) mixed process.
3. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：Organic solution described in step (2) is with 10:1.0 methyl ethyl ketone and absolute ethyl alcohol be mixed solvent, using epoxy resin as Binding agent, polyethylene glycol are plasticizer, and triethanolamine is dispersant, and the volume ratio of epoxy resin and polyethylene glycol presses 1:1, then It is 50~70% by mixed solvent quality, dispersant quality is 0.1%, and surplus is organic for the slurry that binding agent and plasticizer are formed Solution.
4. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：With high-energy ball milling or rush rotation method obtain grain size≤6 μm HIGH-PURITY SILICON iron powder.
5. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：Step (5) is sintered, by 5~10 when re-sintering for 1060~1160 DEG C under vacuum-sintering or restitutive protection's atmosphere DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab in 0.1~1mm, soaking time is reduced to 0.5~ 1h after sintered accumulation drafts reaches 30~40% every time, is sintered 1 time, is rolled down to from the biscuit of 1.0~2.1mm again 0.1~0.5mm, it is necessary to be sintered 4~8 times again.
6. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：Overlapping places sintering plate during high temperature sintering, and interlayer is laid with MgO powder.
7. the method that High temperature diffusion sintering as described in claim 1 prepares Fe-6.5%Si bands with tape casting, feature It is：Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
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Application publication date: 20180518