CN100453689C - Process for preparing high silicon stalloy by pack siliconizing process - Google Patents
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- CN100453689C CN100453689C CNB2006100017934A CN200610001793A CN100453689C CN 100453689 C CN100453689 C CN 100453689C CN B2006100017934 A CNB2006100017934 A CN B2006100017934A CN 200610001793 A CN200610001793 A CN 200610001793A CN 100453689 C CN100453689 C CN 100453689C
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Abstract
The present invention discloses a process for preparing high silicon stalloy by a pack siliconizing process. In the process, low stalloy containing 0.3 to 1.0 wt% of silicon is embedded into a siliconizing agent, and the high silicon stalloy having the advantages of low loss, low hysteresis expansion coefficients and low coercivity containing about 6.5% of the silicon is obtained by controlling process parameters of chemical heat treatment. The process comprises the steps that firstly, part of the prepared siliconizing agent is laid at the bottom of a crucible; then, the low stalloy of which the surface is treated is placed into the crucible, the circumference of the low stalloy is filled with the surplus siliconizing agent, and argon is filled; heating rate is adjusted to 17 to 20 DEG C /min, and the low stalloy is insulated after heated to 1000 to 1250 DEG C; subsequently, the low stalloy is heated and diffused after insulated for 1.5 to 4.5 hours at the temperature of 1150 to 1350 DEG C in the crucible at the heating rate of 6 to 8 DEG C /min.
Description
Technical field
The present invention relates to a kind of preparation method of high-silicon electrical steel sheet, more particularly, with silicon content is that 0.3～0.45% low-silicon steel sheet is by the pack cementation silicea, simultaneously the processing parameter of thermo-chemical treatment is controlled effectively, thereby obtained to have low-loss, the silicon content of low magnetic hysteresis coefficient of dilatation, low-coercivity is about 6.5% high-silicon electrical steel sheet.
Background technology
Siliconized plate is the main core material of processing high-speed induction motor, and in order to produce efficient height, volume is little, noise is low high-speed induction motor, the silicone content in the siliconized plate has bigger influence to the magnetic strength and the iron loss characteristic of core material.Show that through correlative study along with the increase of silicone content, intrinsic impedance increases in the steel in siliconized plate, especially eddy-current loss reduces in high-frequency range, shows good magnetic.When silicone content reached 6.5% in the siliconized plate, the core material magnetostriction coefficient was near zero, and therefore, the steel that contain 6.5% silicon amount are to make comparatively ideal core material of low noise, low iron loss.But along with the increase of silicone content in the steel, its extensibility has reduced, and has limited the process for processing of high silicon steel material to a great extent.
Summary of the invention
The objective of the invention is to propose a kind of method that adopts the pack cementation silicon technology to prepare the high-silicon electrical steel sheet, this method is that 0.3～0.45% low-silicon steel sheet is embedded in the siliconizing medium with silicon content, by the processing parameter of control thermo-chemical treatment, thereby obtain to have low-loss, the silicon content of low magnetic hysteresis coefficient of dilatation, low-coercivity is 5.1～6.95% high-silicon electrical steel sheet.
The present invention is a kind of method that adopts the pack cementation silicon technology to prepare the high-silicon electrical steel sheet, and it has the following steps:
The first step, the preparation siliconizing medium
Siliconizing medium is made up of the Sodium Fluoride of 3～4wt%, the silica flour of 10～12wt% and the aluminum oxide of 84～86wt%, and the siliconizing medium that makes is put into 100 ℃ of baking ovens preserve 0.5～1 hour, and is stand-by;
Second step, raw-material pre-treatment
Choose silicone content and be 0.3～1.0% low-silicon steel sheet, and the low-silicon steel sheet is taken out after putting into alcohol to preserve 0.1～1 hour after the polishing, dry up with cold wind, stand-by;
The 3rd step, the thermochemistry embedding treatment
The siliconizing medium of preparing in the first step is put into crucible bottom by 5～15% of gross weight, then the low-silicon steel sheet after handling in second step is put into the crucible middle part, and fill up the siliconizing medium of surplus around it, after covering the crucible lid and reinforcing, it is inserted in the heat treatment furnace;
Charge into shielding gas---argon gas 10～30 minutes;
Regulate 17～20 ℃/min of temperature rise rate of heat treatment furnace, be incubated 1.5～4.5 hours after the temperature to 1000 in the process furnace～1250 ℃; Air cooling to room temperature is taken out, and with ultrasonic cleaning after 0.2～1 hour, cold wind dries up, and makes promptly that element silicon is the high-silicon electrical steel sheet that concentration gradient changes on low-silicon steel sheet cross-wise direction;
The high-silicon electrical steel sheet that above-mentioned element silicon is changed is in gradient put into the Glass tubing of heat treatment furnace, and suction to 2 * 10
-5Pa; Regulate 6～8 ℃/min of temperature rise rate of heat treatment furnace, be incubated 1.5～4.5 hours after the temperature to 1150 in the process furnace～1350 ℃; Air cooling to room temperature is taken out, and promptly makes silicon content and be 5.1～6.95% high-silicon electrical steel sheet.
Described employing pack cementation silicon technology prepares the method for high-silicon electrical steel sheet, and in the 3rd step, polylith low-silicon steel sheet adopts stack to be positioned in the crucible, needs the filling siliconizing medium to do to isolate between each low-silicon steel sheet and uses.
The advantage that the present invention adopts the pack cementation silicon technology to prepare the method for high-silicon electrical steel sheet is: (1) solved stalloy in process for processing because of the cold rolling difficulty in process of bringing; (2) make the high-silicon electrical steel sheet that obtains and have the iron loss of 0.005～0.15W; (3) the magnetic hysteresis coefficient of dilatation of making the high-silicon electrical steel sheet that obtains is 42ppm under the 200mT magnetic field condition, is 84ppm under the 600mT magnetic field condition; (4) coercive force of making the high-silicon electrical steel sheet that obtains is 0.37～0.57O
e
Description of drawings
Fig. 1 is the cross section shape appearance figure of the high-silicon electrical steel sheet that changes in gradient of element silicon that the present invention prepares.
Fig. 2 is the high-silicon electrical steel sheet cross section shape appearance figure after diffusion heat treatments of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention a kind ofly carries out improved its preparation process by the pack cementation silicea to the low-silicon steel sheet, and by hot chemical treatment process the low-silicon steel sheet being carried out embedding, heating, heat diffusion treatment in the method, to obtain to have silicon content be 5.1～6.95% high-silicon electrical steel sheet material.
The present invention is a kind of method that adopts the pack cementation silicon technology to prepare the high-silicon electrical steel sheet, and it has the following steps:
The first step, the preparation siliconizing medium
Siliconizing medium is made up of the Sodium Fluoride of 3～4wt%, the silica flour of 10～12wt% and the aluminum oxide of 84～86wt%, and the siliconizing medium that makes is put into 100 ℃ of baking ovens preserve 0.5～1 hour, and is stand-by;
Moisture, make in the course of processing under hot environment siliconizing medium to the corrosion of low-silicon steel sheet;
Second step, raw-material pre-treatment
Choose silicone content and be O.3～1.0% low-silicon steel sheet, and the low-silicon steel sheet is taken out after putting into alcohol to preserve 0.1～1 hour after the polishing, dry up with cold wind, stand-by;
The low-silicon steel sheet is perishable getting rusty under physical environment, so it is deposited in spirituous solution;
The 3rd step, the thermochemistry embedding treatment
The siliconizing medium of preparing in the first step is put into crucible bottom by 5～15% of gross weight, then the low-silicon steel sheet after handling in second step is put into the crucible middle part, and fill up the siliconizing medium of surplus around it, after covering the crucible lid and reinforcing, it is inserted in the heat treatment furnace;
Charge into shielding gas---argon gas 10～30 minutes;
(heat treatment furnace is chosen model SG-3-1O to regulate heat treatment furnace, Beijing Electric Stove Factory's production) 17～20 ℃/min of temperature rise rate, be incubated 1.5～4.5 hours after the temperature to 1000 in the process furnace～1250 ℃, air cooling to room temperature is taken out, with ultrasonic cleaning after 0.2～1 hour, cold wind dries up, and promptly makes on low-silicon steel sheet cross-wise direction element silicon and is the high-silicon electrical steel sheet that concentration gradient changes;
The high-silicon electrical steel sheet that above-mentioned element silicon is changed is in gradient put into the Glass tubing of heat treatment furnace, and suction to 2 * 10
-5Pa; Regulate 6～8 ℃/min of temperature rise rate of heat treatment furnace, be incubated 1.5～4.5 hours after the temperature to 1150 in the process furnace～1350 ℃; Air cooling to room temperature is taken out, and promptly makes silicon content and be 5.1～6.95% high-silicon electrical steel sheet.
Element silicon is the concentration gradient change profile: adopt electron-microscope scanning low-silicon steel sheet section after heat treatment, find that by analysis the element silicon concentration distribution has the trend of successively decreasing to central part from the surface, the silicon concentration of its surface is 6.11～14.71wt%, the centre portions silicon concentration for O.3～1.0wt%.The high-silicon electrical steel sheet that above-mentioned element silicon is changed in gradient passes through the scanning electron fractograph analysis after heat diffusion treatment, element silicon is evenly distributed in the low-silicon steel sheet, and its silicone content reaches 5.1～6.95%.The shortcoming of having avoided the big standard of high-silicon electrical steel sheet fragility to roll effectively, and can obtain the good stalloy of electromagnetic performance equally.This working method has broken through high-silicon steel sheet material can't have great industrial application value by the limitation of roll compacting processing treatment.
Embodiment 1:
The 80g siliconizing medium is by the silicon Si powder (Si powder degree 200 orders) of Sodium Fluoride NaF, the 9g of 3g and the aluminium oxide Al of 68g
2O
3Form, and the siliconizing medium that makes is put into 100 ℃ of baking ovens preserved 1 hour, stand-by;
Choose two of low-silicon steel sheets that do not have the thick silicon content 0.5% of orientation " EI " type 0.5mm, and it is taken out after alcohol is preserved 1 hour through putting into after the polishing, dry up with cold wind, stand-by;
The 10g siliconizing medium is put into crucible bottom, puts into a slice low-silicon steel sheet then, and around it, top evenly sprinkles the 10g siliconizing medium; Put into another sheet low-silicon steel sheet again, and around it, top evenly fills up the siliconizing medium of surplus, after covering the crucible lid and reinforcing, it is inserted in the heat treatment furnace;
Charge into shielding gas---argon gas 10 minutes;
Regulate the 20 ℃/min of temperature rise rate of heat treatment furnace, insulation 4.5 hours after the temperature to 1040 ℃ in the process furnace, air cooling to room temperature is taken out this two low-silicon steel sheets, uses ultrasonic cleaning half an hour, cold wind dries up, and promptly obtains the high-silicon electrical steel sheet that element silicon changes in gradient.It is carried out its element silicon of electron-microscope scanning cross-section analysis is the concentration gradient change profile and is: adopt electron-microscope scanning low-silicon steel sheet section after heat treatment, find that by analysis the element silicon concentration distribution has the trend of successively decreasing to central part from the surface, the silicon concentration of its surface A is 8.74wt%, the silicon concentration of transition position B is 6.31wt%, the silicon concentration of the C of place, centre is 0.61wt%, and the silicon concentration graded sees also shown in Figure 1.
A slice high-silicon electrical steel sheet wherein that element silicon is changed is in gradient put into the Glass tubing of heat treatment furnace, and suction to 2 * 10
-5Pa; Regulate the 8 ℃/min of temperature rise rate of heat treatment furnace, insulation 2 hours after the temperature to 1200 ℃ in the process furnace, air cooling takes out to room temperature, promptly makes silicon content after tested and be 6.5% high-silicon electrical steel sheet, sees also shown in Figure 2ly, and element silicon is evenly distributed among the figure.
To silicon content is that 6.5% high-silicon electrical steel sheet carries out performance test: adopt the B-H survey meter based on the voltammetry principle of Chinese quantitative study institute development, measuring its coercive force is 0.57Oe, is 25% of original low-silicon steel sheet; Wattful power is reduced to 0.01w by the 0.27w of original low-silicon steel sheet; Adopt YJK4500 type resistance strain meter to measure the magnetic hysteresis telescopicing performance of the high-silicon electrical steel sheet that the present invention prepares, the foil gauge model is BX120-1AA, bonding use 502 glue of foil gauge, under the 200mT magnetic field condition, its magnetic hysteresis coefficient of dilatation of original siliconized plate is 67ppm, its magnetic hysteresis coefficient of dilatation of the resulting stalloy of the present invention is 42ppm, reduces nearly 40%.
The Ji Li of thermo-chemical treatment in the present invention: the Sodium Fluoride NaF as catalyzer generates fluorosilicone compound with the reaction of silicon Si powder under hot conditions, this compound under hot conditions with the low-silicon steel sheet in iron reaction, the fluorochemical that generates iron evaporate in the middle of the penetration enhancer, the silicon that iron cements out is attached to surface of silicon steel, simultaneously at high temperature to the matrix internal divergence.
6.5% high-silicon electrical steel sheet (silicon-iron soft magnetic alloy) is because its low core loss and low magnetic hysteresis coefficient of dilatation are the more satisfactory iron core soft magnetic materialss of low noise, low-loss.Along with the development of electronic industry and energy-conservationly become the importance that the world economizes on resources, require electric installation to high frequency, efficient, miniaturization development, silicon steel as important electrical material is faced with great challenge, necessarily requires the electrician just to develop to low-loss, lower noise, high magnetic conductance and high saturation and magnetic intensity direction.
Claims (3)
1, a kind of method that adopts the pack cementation silicon technology to prepare the high-silicon electrical steel sheet is characterized in that having the following steps:
The first step, the preparation siliconizing medium
Siliconizing medium is made up of the Sodium Fluoride of 3～4wt%, the silica flour of 10～12wt% and the aluminum oxide of 84～86wt%, and the siliconizing medium that makes is put into 100 ℃ of baking ovens preserve 0.5～1 hour, and is stand-by;
Second step, raw-material pre-treatment
Choose silicone content and be 0.3～1.0% low-silicon steel sheet, and the low-silicon steel sheet is taken out after putting into alcohol to preserve 0.1～1 hour after the polishing, dry up with cold wind, stand-by;
The 3rd step, the thermochemistry embedding treatment
The siliconizing medium of preparing in the first step is put into crucible bottom by 5～15% of gross weight, then the low-silicon steel sheet after handling in second step is put into the crucible middle part, and fill up the siliconizing medium of surplus around it, after covering the crucible lid and reinforcing, it is inserted in the heat treatment furnace;
Charge into shielding gas---argon gas 10～30 minutes;
Regulate 17～20 ℃/min of temperature rise rate of heat treatment furnace, be incubated 1.5～4.5 hours after the temperature to 1000 in the process furnace～1250 ℃; Air cooling to room temperature is taken out, and with ultrasonic cleaning after 0.2～1 hour, cold wind dries up, and makes promptly that element silicon is the high-silicon electrical steel sheet that concentration gradient changes on low-silicon steel sheet cross-wise direction;
The high-silicon electrical steel sheet that above-mentioned element silicon is changed is in gradient put into the Glass tubing of heat treatment furnace, and suction to 2 * 10
-5Pa; Regulate 6～8 ℃/min of temperature rise rate of heat treatment furnace, be incubated 1.5～4.5 hours after the temperature to 1150 in the process furnace～1350 ℃; Air cooling to room temperature is taken out, and promptly makes silicon content and be 5.1～6.95% high-silicon electrical steel sheet.
2, employing pack cementation silicon technology according to claim 1 prepares the method for high-silicon electrical steel sheet, it is characterized in that: in the 3rd step, polylith low-silicon steel sheet adopts stack to be positioned in the crucible, needs the filling siliconizing medium to do to isolate between each low-silicon steel sheet and uses.
3, employing pack cementation silicon technology according to claim 1 prepares the method for high-silicon electrical steel sheet, it is characterized in that: in the 3rd step, element silicon is the concentration gradient change profile: the silicon concentration of surface is 6.11～14.71wt%, and the centre portions silicon concentration is 0.3～1.0wt%.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102162104A (en) * | 2010-10-29 | 2011-08-24 | 东北大学 | Method for preparing high silicon steel thin plate |
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| CN114231835B (en) * | 2021-11-09 | 2023-03-03 | 马鞍山钢铁股份有限公司 | Wide-frequency low-iron-loss non-oriented electrical steel and preparation method thereof |
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