CN102658367B - Method and device for preparing high-silicon silicon steel sheet in static magnetic field with powder sintering method - Google Patents
Method and device for preparing high-silicon silicon steel sheet in static magnetic field with powder sintering method Download PDFInfo
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Abstract
The invention relates to a method and device for preparing a silicon steel sheet in a static magnetic field with a powder sintering method. The specific process of the method consists of the following steps of: mixing Fe-Si powder; rolling into a plate blank; and sintering a Fe-6.5 weight percent Si green compact in a static magnetic field. In the method, 6.5 percent by weight of Si high-silicon steel with high density is obtained by using the influence of the magnetic field on the sintering densification and orientation process of a Fe-6.5 weight percent Si powder green compact, and an easily-magnetized axis is oriented along the magnetic field. An atmosphere/vacuum sintering device in a static magnetic field consists of a temperature control device, an exhaust pipe, a thermocouple, a heating element, a corundum crucible, a refractory fiber, a support block, a heat insulating block, a water-cooled bush, a static magnetic field generating device, a sealed corundum pipe, an inert gas inlet valve, a vacuum pumping valve, a Fe-6.5weight percent Si green compact, a thin corundum plate interlayer and a fixing molybdenum wire. The 6.5 percent Si silicon steel sheet prepared with the method has the advantages of near net molding, superior magnetic property, high orientation degree and the like, and has a remarkable industrial application prospect.
Description
Technical field
The present invention relates to powder sintering under a kind of steady magnetic field and prepare method and the device thereof of high-silicon silicon steel sheet, belong to silicon steel fabricating technology field.
Background technology
Silicon steel is that electric power and telecommunication are industrial to manufacture the important magnetic material of generator, motor, transformer, transformer, relay and other electrical instrumentation
,, silicon content is that the high silicon steel magnetostriction coefficient of 6.5 % goes to zero, magnetic conductivity maximum, resistivity is large, turbine loss is little, is the desirable core material of making low noise, low iron loss.Yet due to the raising of silicone content, the fragility of silicon steel sheet increases, and traditional milling method is difficult to processing, and the silicone content of the silicon steel sheet of therefore producing in enormous quantities is at present mostly in 4 %.In today of energy growing tension, especially in high-frequency information field, high-silicon silicon steel sheet is reconsidered the substitution material into ordinary silicon steel disc, and 6.5 %Si high-silicon silicon steel sheet preparation technologies' research has very profound significance for energy-saving and emission-reduction.
The method of preparing at present high-silicon silicon steel sheet mainly contains traditional rolling, rapid solidification method and CVD method.Since the sixties, people attempt improving traditional rolling and prepare high silicon sheet iron, Russia develops a kind ofly rolls method technique three of hot rolling, warm-rolling, cold rolling and corresponding heat treatment phase combination, and this complex technical process, energy consumption is large and lumber recovery is low, is difficult to be applied to industry and becomes to produce.Rapid solidification method refers to and utilizes emergency cooling process to produce high silicon steel thin belt, but have very large problem aspect size and process controllability.CVD method be take ordinary silicon steel disc as substrate; at surface of steel plate and silicide generation high-temperature chemical reaction, Si is enriched on silicon steel sheet; thereby by heat treatment, Si is diffused in whole silicon steel plate again and makes high-silicon steel; at present this is uniquely can realize the preparation method that industrial scale is produced high silicon steel, by Japanese NKK Developed and put into production.But CVD method cost is high, energy consumption is high, the SiCl of employing
4gas is highly corrosive gas, have serious environmental protection hidden danger, so this technology is subject to very large restriction.
Powder sintering is prepared high-silicon silicon steel sheet and is compared with traditional rolling, CVD method, have composition easy to control, can newly net forming, the lower and simple technological process and other advantages of power consumption.Yet the silicon steel that current powder sintering process makes, its density is on the low side, and magnetic property is well below application requirements, and this is also that current powder sintering is prepared high-silicon silicon steel sheet and failed to be widely used in industrial reason.If can break through from powder sintered critical process, in the situation that not significantly improving its cost, effectively improve silicon steel density, can bring into play the advantage of powder sintering process, prepare the high-silicon silicon steel sheet that density is high, magnetic property reaches application requirements.
Orientation silicon steel is compared with non-orientation silicon steel, and its magnetic has strong directionality, has high magnetic permeability and low loss characteristic in direction of easy axis, is mainly used in the manufacture of transformer.According to the data of China's power system statistics, annual national power consumption accounts for the 6-10% of gross generation, and the iron loss loss of silicon steel sheet accounts for the more than 40% of electrical power trans mission/distribution system total losses in transformer, therefore improve transformer significant for saving the energy with the magnetic property of silicon steel sheet.If can make high-silicon silicon steel sheet there is certain degree of orientation by certain technique, can further improve product magnetic property, and at present not yet have technique to prepare to have 6.5% high-silicon silicon steel sheet of high-orientation.
Summary of the invention
The object of this invention is to provide a kind of powder sintering process and prepare the method for silicon content 6.5% high-silicon silicon steel sheet of high-compactness, high magnetic characteristics, and the silicon steel sheet making has certain degree of orientation.
for reaching above-mentioned requirements, the present invention conceives as follows:
The subject matter that powder sintering is prepared high silicon sheet iron is that silicon steel density cannot reach application requirements, and magnetic field is often used in the process of materials processing to improve material property, physical field as a kind of cleaning, it both can obviously affect the thermodynamics and kinetics process of material processing, can material not introduced and be polluted again simultaneously.The present invention adds additional steady magnetic field in sintering process, utilizes the facilitation of magnetic field to the sintering densification process of Fe-Si powder compact, obtains the high high silicon steel of 6.5%Si of density.
Silicon steel is a kind of ferrimagnet simultaneously, adds steady magnetic field can affect the grain growth orientation of material in its sintering process.<100> crystal orientation is the easy axis of silicon steel, the magnetic anisotropy that this side up can be minimum, if add steady magnetic field in sintering process, the <100> crystal orientation crystal grain parallel with magnetic direction has lower magnetic anisotropy as extra crystal boundary migration driving force, to impel the gross area of this orientation crystal grain to increase.Silicon steel sheet is being parallel to the raising of the <100> degree of orientation on sintering magnetic direction, the energy of magnetization that causes silicon steel sheet to make progress the party is lower than other direction, thereby the magnetic property in this direction is improved, therefore makes the silicon steel with certain degree of orientation.
the present invention adopts following technical proposals:
A kind of powder sintering is prepared the method for 6.5wt%Si high-silicon silicon steel sheet, it is characterized in that adding steady magnetic field in sintering process, utilize the impact of magnetic field on the sintering densification process of Fe-Si powder compact, obtain the high 6.5wt%Si high-silicon silicon steel sheet of density, and its easy magnetizing axis is improved along the degree of orientation of magnetic direction.
According to the proportioning of silicone content 6.5wt%Si, take respectively iron powder and silica flour, mixed, the Fe of employing, Si powder can be both micro-meter scales, can be also nanoscales, can be also the mixtures of different grain size powder.In addition, iron powder or silica flour that this place adopts, can also be micron order or the nano level ferro-silicon alloy powder that adopts variable concentrations or same concentrations, and in ferro-silicon alloy powder, the content of silicon is 6.5-99wt%.Mixed-powder both can adopt V-type batch mixer also can adopt planetary ball mill to carry out, and batch mixing rotating speed is 5-1000r/min, and mixing time is 0.5-240h, and batch mixing process is carried out under the protection of inert gas or reducibility gas.The Fe-Si powder pressure rolling mixing is become to Fe-Si powder square billet or slab.Fe-Si powder compact is put into the burner hearth of atmosphere/vacuum protection agglomerating plant, be positioned in the magnetic field space of the steady magnetic field generating means that magnetic induction intensity can adjust within the scope of 0.01 ~ 20T, high temperature sintering under inert gas or reducibility gas protection, inert gas can be pure nitrogen gas, pure argon, pure helium or its mist, or the gas that passes into reproducibility is as hydrogen, methane, carbon monoxide etc.; It can also be the mist that reducibility gas and above-mentioned inert gas form.The 6.5%Si high-silicon silicon steel sheet of cooling rear acquisition high-compactness, high-orientation, rate of temperature fall is 0.1-300 ℃/min.The high-orientation high-silicon steel square billet or the slab that make, the mode that adopts line cutting or inner circle cutting or cylindrical to cut cuts into the thin slice of 0.05-1mm thickness, insulating coating in existing low-silicon steel band preparation technology is processed again, can obtain the high silicon of finished product, high orientation silicon steel sheet material.Sintering temperature is 600-1300 ℃, and temperature retention time is 0.5-100h, and heating rate is 0.1-300 ℃/min.The magnetic field mode that adds both can add magnetic field in whole sintering process, also can only in temperature-rise period, insulating process, temperature-fall period, add magnetic field, can also in intensification, cooling and insulating process, set different magnetic induction intensity, or magnetic induction intensity with sintering temperature difference monotone variation.The steady magnetic field applying is the steady magnetic field that superconductor technology or resistance magnet produce, and can also be the steady magnetic field of superconduction-resistance hybrid magnet generation, and its magnetic induction intensity can be in 0.01-20T range, and the room temperature bore of magnet is 50mm-800mm; Magnetic line of force direction can be rolled to parallel or vertical with slab.
The present invention compared with prior art has following evident characteristic and advantage:
1) adopt powder sintering to prepare high-silicon silicon steel sheet, having advantages of can newly net forming, can accurately control the silicone content in silicon steel;
2) compare with conventional powder sintering process, under the magnetic field that the present invention adopts, the method for sintering can obtain that density is higher, the better silicon steel of magnetic property;
3) by method powder sintered under magnetic field, make the high-silicon silicon steel sheet with certain degree of orientation, the magnetic property in a direction of silicon steel sheet is further improved;
4) different from traditional magnetic field orientating heat treatment, the present invention is in the diffusion-sintering of iron powder and silica flour, forms Fe
3in the process of Si solid solution, apply stationary magnetic field, in its lattice restructuring procedure, impel its orientation, therefore can obtain the higher degree of orientation and anisotropy;
The steady magnetic field adopting is a kind of physical field of cleaning, and environment is not polluted, and can not introduce new pollution to silicon steel, can guarantee its degree of purity.
Accompanying drawing explanation
Fig. 1 is the structural representation of atmosphere/vacuum protection high temp sintering device under steady magnetic field in the inventive method.
To be the high silicon steel that makes of the inventive method be parallel to magnetic direction and hysteresis curve comparison diagram perpendicular to magnetic direction to Fig. 2.
The specific embodiment
Below in conjunction with embodiment, the present invention is described in detail:
embodiment mono-
Below specific embodiments of the invention.
A preferred embodiment of the present invention is: referring to accompanying drawing 1.
According to the proportioning of silicon weight content 6.5%, take respectively micron order iron powder 18700g and nanoscale pure silicon powder 1300g, put it in V-type batch mixer and mix, batch mixing speed is 70r/min, and mixing time is 10h, logical argon shield in batch mixer in batch mixing process.Batch mixing finishes the Fe-Si powder that rear taking-up mixes, and pressure rolling becomes the Fe-6.5wt%Si powder slab of multi-disc 80mm * 80mm * 50mm size.
Described under steady magnetic field the method for powder sintered preparation 6.5% high-silicon silicon steel sheet, its sintering process is realized by atmosphere/vacuum protection high temp sintering device under steady magnetic field.Referring to Fig. 1.Under steady magnetic field, atmosphere/vaccum sintering device is by temperature regulating device 1, blast pipe 2, thermocouple 3, heating element heater 4, corundum crucible 5, refractory fibre 6, back-up block 7, heat insulation block 8, water cold sleeve 9, steady magnetic field generating means 10, sealing alundum tube 11, inert gas air intake valve 12, vacuum extraction valve 13, Fe-6.5wt%Si pressed compact 14, thin corundum plate interlayer 15, fixedly molybdenum filament 16 forms.Implement when of the present invention; a plurality of Fe-6.5wt%Si pressed compacts 14 use thin corundum plate interlayer 15 intervals of above-mentioned preparation are stacked; and keep the rolling to parallel with gravitational field direction of Fe-6.5wt%Si pressed compact 14; with fixing molybdenum filament 16, tie; put under steady magnetic field in the corundum crucible 5 in the sealing alundum tube 11 in atmosphere/vacuum protection high temp sintering device, corundum crucible 5 use back-up blocks 7 and heat insulation block 8 support fixing.Open vacuum extraction valve 13, adopt mechanical pump in sealing alundum tube 11, to be pumped into 10
-1pa, closes vacuum extraction valve 13, opens inert gas air intake valve 12, in sealing alundum tube 11, is filled with high-purity argon gas to 1atm.Again open vacuum extraction valve 13, will in sealing alundum tube 11, be pumped into 10
-1pa, and then inflate-bleed circulation 4 times, finally close vacuum extraction valve, will in sealing alundum tube 11, be filled with high-purity argon gas to 0.8atm, then close inert gas air intake valve 12.Open steady magnetic field generating means 10, make magnetic induction intensity wherein reach 6 teslas, and the direction that guarantees the magnetic line of force 17 is for straight up.Give in water cold sleeve 9 and pass into cooling water, open temperature regulating device 1, by heating element heater 4 and refractory fibre 6, the temperature in sealing alundum tube 11 is heated to 1200 ℃ with the speed of 10 ℃/min, by thermocouple 3, carry out monitor temperature.When temperature arrives 1200 ℃, be incubated 50 hours, then by temperature regulating device 1, make to seal temperature in alundum tube 11 and be cooled to room temperature with the cooling velocity of 10 ℃/min, then close temperature regulating device 1 and steady magnetic field generating means 10, from sealing alundum tube 11, take out the Fe-6.5wt%Si pressed compact 14 sintering, adopt the mode of inner circle cutting further Fe-6.5 wt % Si pressed compact 14 to be cut into the thin slice that 0.2mm is thick along parallel magnetic field direction or rolling direction, again through cleaning and conventional insulation processing, can obtain high silicon, the Fe-6.5wt%Si silicon steel sheet of high orientation.
Adopt high silicon steel prepared by the inventive method along being parallel to magnetic direction and perpendicular to measuring respectively its hysteresis curve on magnetic direction, find that high silicon steel is obviously greater than perpendicular to magnetic direction along the saturation magnetization that is parallel to magnetic direction, as shown in Figure 2, illustrate that silicon steel sheet prepared by the inventive method has had the anisotropy of obvious preferred orientation and magnetic property.In addition the density that adopts drainage to record high silicon steel prepared by this law reaches 97% of solid density, apparently higher than without 94% of sintered specimen under magnetic field, shows that its density also significantly improves.
Claims (9)
1. under steady magnetic field, powder sintering is prepared the method for high silicon sheet iron, it is characterized in that by mixing Fe-Si powder, be rolled into three steps of sintering Fe-6.5wt%Si pressed compact under slab and steady magnetic field and form, utilize the impact of magnetic field on the sintering densification of Fe-6.5wt%Si powder compact and orientation process, obtain the high high silicon steel of 6.5wt%Si of density, and its easy magnetizing axis is orientated along magnetic direction.
2. method according to claim 1, is characterized in that the Fe, the Si powder that adopt can be both micro-meter scales, can be also nanoscale, can be also the mixture of different grain size powder.
3. method according to claim 1, it is characterized in that iron powder or silica flour in material powder, can adopt micron order or nano level straight iron powder and pure silicon powder, also can be micron order or the nano level ferro-silicon alloy powder that adopts variable concentrations or same concentrations, in ferro-silicon alloy powder, the content of silicon be 6.5-99wt%.
4. method according to claim 1; the process that it is characterized in that mixed-powder both can adopt V-type batch mixer also can adopt planetary ball mill to carry out; batch mixing rotating speed is 5-1000r/min, and mixing time is 0.5-240h, and batch mixing process is carried out under the protection of inert gas or reducibility gas.
5. method according to claim 1, it is characterized in that steady magnetic field is the stationary magnetic field that superconductor technology produces, also can be the stationary magnetic field that adopts resistance magnet or superconduction-resistance hybrid magnet to produce, its magnetic induction intensity can be in 0.01-20T range, and the room temperature bore of magnet is 50-800mm; Magnetic line of force direction can be parallel or vertical with Fe-6.5wt%Si pressed compact direction.
6. method according to claim 1, the sintering temperature that it is characterized in that sealing in alundum tube is 600-1300 ℃, and temperature retention time is 0.5-100 hour, and heating rate and rate of temperature fall are 0.1-300 ℃/min.
7. method according to claim 1, is characterized in that both can in whole sintering process, adding stationary magnetic field, also can only in insulating process or in temperature-fall period, add stationary magnetic field.
8. method according to claim 1, it is characterized in that for preventing that sample is oxidized in sintering process, in sealing alundum tube, pass into inert gas or reducibility gas, inert gas can be pure nitrogen gas, pure argon, pure helium or its mist, or pass into the gas of reproducibility, the gas of this reproducibility is hydrogen, methane, carbon monoxide; It can also be the mist that reducibility gas and above-mentioned inert gas form.
9. under steady magnetic field, powder sintering is prepared the special purpose device of the method for high silicon sheet iron, it is characterized in that this device is by temperature regulating device (1), blast pipe (2), thermocouple (3), heating element heater (4), corundum crucible (5), refractory fibre (6), back-up block (7), heat insulation block (8), water cold sleeve (9), steady magnetic field generating means (10), sealing alundum tube (11), inert gas air intake valve (12), vacuum extraction valve (13), Fe-6.5wt%Si pressed compact (14), thin corundum plate interlayer (15), fixedly molybdenum filament (16) forms.
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