CN101665861A - Method for preparing oriented silicon steel by pulse current recovery annealing - Google Patents
Method for preparing oriented silicon steel by pulse current recovery annealing Download PDFInfo
- Publication number
- CN101665861A CN101665861A CN200910196582A CN200910196582A CN101665861A CN 101665861 A CN101665861 A CN 101665861A CN 200910196582 A CN200910196582 A CN 200910196582A CN 200910196582 A CN200910196582 A CN 200910196582A CN 101665861 A CN101665861 A CN 101665861A
- Authority
- CN
- China
- Prior art keywords
- silicon steel
- oriented silicon
- sample
- annealing
- pulse current
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Manufacturing Of Steel Electrode Plates (AREA)
Abstract
The invention discloses a method for preparing oriented silicon steel by pulse current recovery annealing, which has the main technical characteristics by comprising the following steps: first connecting an oriented silicon steel cold rolling sample on two electrodes of an output end of a pulse power supply by a copper fixture with good conductivity; then sending a quartz tube into the oriented silicon steel cold rolling sample; sealing and introducing the oriented silicon steel cold rolling sample into protective atmosphere with 90% N2 plug 10% H2; and then electrifying for pulse current recovery annealing treatment after 1h; adjusting pulse current frequency and peak current according to the different components of the samples; leading the sample to be heated to 550 DEG C; and carrying out heat preservation for 5min; taking out the sample; coating the surface of the sample evenly with magnesium oxide coating; sending the sample into a thermal treatment furnace for high temperature annealing for 12h under the conditions of 1200 DEG C and pure H2 protective atmosphere as well as for hot-leveling annealing treatment for 2h under the conditions of 800 DEG C and pure N2 protective atmosphere; and finally obtaining the oriented silicon steel with high magnetic induction and low iron loss. The method is simple and easy to use as well as easy for industrialization, and the prepared oriented silicon steel sample has excellent performance.
Description
Technical field
The present invention relates to a kind of method of preparing oriented silicon steel by pulse current recovery annealing, belong to the silicon steel technical field.
Background technology
Silicon steel is indispensable important non-retentive alloy in electric power, the electronic industry, also is a kind of important energy saving Metallic Functional Materials.The oriented silicon steel that wherein is mainly used in transformer industry b referred to as the whole world steel " pinnacle of a pagoda product ", and the laudatory title of " special steel artwork " is more arranged.Silicon steel with core loss (iron loss) and magnetic induction density (magnetic strength) as product magnetic guarantee value, how to improve the magnetic property (comprising iron loss and magnetic strength) of oriented silicon steel better, make it have higher magnetic permeability, lower magnetostriction and core loss become one of heat subject of our times.And the complex manufacturing of oriented silicon steel, manufacturing technology strictness, external production technology is all strictly protected with the form of patent, is considered as the life of enterprise.The manufacturing technology of silicon steel and quality product have become one of important symbol of weighing national special steel production and development in science and technology level more.
The Production Flow Chart of oriented silicon steel is generally: molten iron demanganize-smelting-vacuum-treat-continuous casting and hot rolling-normalizing and pickling-cold rolling-decarburizing annealing (recovery annealing)-be coated with magnesium oxide-high temperature annealing-smooth stretching annealing and be coated with insulation layer.As everyone knows, the magnetic property of oriented silicon steel and secondary recrystallization texture are closely related, and recovery annealing technology has directly and significant effects following closely secondary recrystallization process, will be formed with to be beneficial to tissue and the texture that forms goss texture.At present, the main path that improves the oriented silicon steel magnetic property both at home and abroad is that technological improvement is carried out in the smelting and the operation of rolling, thereby improves the secondary recrystallization texture of oriented silicon steel.By optimizing the annealing process of oriented silicon steel, and then the research that improves secondary recrystallization tissue and texture just more and more comes into one's own but in recent years.Because with solidify and the operation of rolling comparatively speaking, annealing process is easier to be controlled and promotes in industrial production and use.
At present, relatively Chang Yong method is to influence its microstructure texture by magnetic-field annealing, to reach the purpose of final its performance of raising.Existing result of study has shown that this method can influence the recrystallized structure texture of oriented silicon steel to a certain extent, as Sha Yuhui etc. at " Northeastern University's journal (natural science edition) " (2004,25 (7): in the paper of delivering 665-667) " recrystallization texture of orientation silicon steel thin belt under the action of a magnetic field ", roll to applying magnetic field along orientation silicon steel thin belt and to carry out anneal and find, magnetic-field annealing can significantly increase the recrystallize Goss texture component of symmetrical rolling strip, reduces the Goss texture component of Asymmetric Rolling strip; Masahashi N etc. are at " J Mater Res " (1998,13 (2): find in the research of the paper of delivering 457-461) " Development ofpreferred orientation in annealing of Fe-3.25% Si in hign magnetic field ", magnetic-field annealing can be strengthened among the cold rolling Fe-3.25%Si＜001〉crystal orientation distribution along outer magnetic field direction, but to not obviously influence or the like of average grain size.But the method for magnetic-field annealing has certain limitation, and this method is subjected to the restriction of the equal Heng Qu in magnetic field, can not handle large-scale sample, and this has directly caused it to be difficult to realize industrialization.
Over nearly 20 years, pulsed current is as a kind of novel method of improving the metal material tissue performance, its Application Areas more and more widely, it is bionical or the like to relate to process of setting, nano-crystallization, material.A series of research has been carried out in the recrystallize behavior of copper under the paired pulses galvanic action such as Conrad H, the result shows, in the metal annealing process, add pulsed current, not only can reduce recrystallize starting temperature, quicken its answer and recrystallize, and obvious refinement recrystal grain.Zhou Yizhou etc. are at " investigation of materials journal " (2002,16 (4): in the paper of delivering 375-378) " pulsed current is to the tissue and the Effect on Performance of cold working brass " in the annealing process of cold working brass the apply pulse electric current handle, also obtained handling more uniform recrystal grain than conventional annealing.But such research at present focuses mostly in the research to pure metal, to steel, particularly the research of the annealing process apply pulse current annealing of oriented silicon steel is not seen as yet both at home and abroad that so far report is arranged.
Summary of the invention
The objective of the invention is to overcome the deficiency and the limitation of optimization annealing way such as existing magnetic-field annealing, provide a kind of pulsed current recovery annealing to prepare the method for high-performance oriented silicon steel.This method connects by the two ends with the positive and negative electrodes in same oriented silicon steel cold-rolled sample of the pulse power, realizes burst process with energising.Utilize the heat effect of pulsed current that sample was reached in very short time and be stabilized in the recovery annealing of finishing oriented silicon steel on the required recovery annealing temperature.Utilize the series of effects such as Lorentz stress effect, skin effect of pulsed current to improve the recovery annealing microstructure texture of oriented silicon steel simultaneously.That this method has is simple, be easy to industrialized characteristics.
The present invention is achieved through the following technical solutions:
A kind of apply pulse current annealing is realized the oriented silicon steel recovery annealing, and then prepares the method for high-performance oriented silicon steel, the rolled samples of oriented silicon steel is placed be connected with 90%N
2+ 10%H
2In the silica tube (volume percent) protective atmosphere, sealing; the copper anchor clamps good by conductivity are terminated at two of oriented silicon steel sample on two electrodes of pulse power output terminal; open pulsed current afterwards; incoming frequency is that 5-1000Hz, peak value are the pulsed current of 10A-5000A; sample temperature is remained near 550 ℃, handled 5 minutes.The sample surfaces that to finish recovery annealing afterwards evenly is coated with to be sent into the resistance heat treatment furnace behind the magnesium oxide barrier coat and carries out 1150～1250 ℃, pure H
2Under the protective atmosphere, 6～12 hours The high temperature anneal, make oriented silicon steel finish secondary recrystallization, afterwards furnace cooling.Send into the resistance heat treatment furnace once more the sample of finishing secondary recrystallization clamps it with clamping plate after and carry out 700～900 ℃, pure N
2Under the protective atmosphere, 1～3 hour hot-leveling anneal.Utilize the MATS-2010M silicon steel measuring apparatus of oriented silicon steel special use that sample is carried out magnetism testing at last.
In the method for above-mentioned preparing oriented silicon steel by pulse current recovery annealing, the direction that applies pulsed current is the rolling direction of oriented silicon steel, and the separant that is adopted is for being the separant of main component with magnesium oxide.
In the aforesaid method, selected pulsed current parameter area is: incoming frequency is that 100～500Hz, current peak are 400～1100A.
Description of drawings
Fig. 1 is an experimental installation synoptic diagram of the present invention.1 is tongued and grooved flanges among the figure, and 2 is sample, and 3 is the copper anchor clamps, and 4 is silica tube.
Embodiment
After now embodiments of the invention specifically being described in.
Below in conjunction with drawings and Examples technical scheme of the present invention is described further.Performing step of the present invention is as follows: (1) sample is prepared: get industrial rolled samples 300mm * 30mm * 0.3mm sample 2, dry up after sample 2 surface cleaning with acetone or alcohol after with weak base aqueous solution surface and oil contaminant being cleaned again; (2) the one side polishing that copper anchor clamps 3 is contacted with sample 2, and clamp sample 2 as far as possible, to keep good electrical conductivity, in case sparking; (3) with thermopair by spring application on sample 2, so that the steady temperature of sample 2 during measuring pulsed current and handling; (4) will be connected the sample 2 that finishes with the pulse power and send into silica tube 4 reposefully, and with tongued and grooved flanges 1 with its sealing; (5) feed 90%N to silica tube 4
2+ 10%H
2Protective atmosphere, kept about 1 hour; (6) make pulse electric current is adjusted parameters such as current peak, frequency and is carried out the recovery annealing processing, and writing time; (7) pulsed current is replied the back that disposes and is taken out sample 2, and removes anchor clamps 3; (8) sample 2 surfaces evenly are coated with the magnesium oxide separant; (9) sample 2 that will coat magnesium oxide coating is sent into the resistance heat treatment furnace and is carried out 1200 ℃, pure H
2Under the protective atmosphere, 12 hours The high temperature anneal, make oriented silicon steel finish secondary recrystallization; (10) send into the resistance heat treatment furnace once more after the sample 2 usefulness clamping plate that will finish secondary recrystallization clamp and carry out 800 ℃, pure N
2Under the protective atmosphere, 2 hours hot-leveling anneal; (11) last oriented silicon steel finished product being carried out magnetic property measures.
The material of present embodiment is the rolled samples of oriented silicon steel in the industrial production, and its main component is C:＜30ppm, Si :～3.15%.Specimen size is 300mm * 30mm * 0.3mm, gets 2 samples, is numbered Q1 and Q2 respectively.During experiment, the rolled samples of 2 oriented silicon steels is placed be connected with 90%N successively
2+ 10%H
2In the silica tube (volume percent) protective atmosphere, sealing; the copper anchor clamps good by conductivity are terminated at two of oriented silicon steel sample on two electrodes of pulse power output terminal; the received current peak value is 1070A respectively; frequency is that 100Hz and current peak are 550A; frequency is the pulsed current of 400Hz; two groups of parameters all can make sample temperature be stabilized near 550 ℃, and be 5 minutes conduction time.Taking out sample afterwards evenly sends into heat treatment furnace behind coating magnesium oxide coating on its surface and carries out 1200 ℃, pure H
2Under the protective atmosphere, 12 hours The high temperature anneal, make oriented silicon steel finish secondary recrystallization.Send into the resistance heat treatment furnace once more after the sample that will finish secondary recrystallization at last clamps with clamping plate and carry out 800 ℃, pure N
2Under the protective atmosphere, 2 hours hot-leveling anneal.
For comparing, choose the pulsed current recovery annealing experiment that two same rolled samples are carried out the conventional, electric-resistance heat treatment furnace, be numbered Q I and Q II.550 ℃ of recovery temperatures, be 5 minutes turnaround time.Taking out sample afterwards evenly sends into heat treatment furnace behind coating magnesium oxide coating on its surface and carries out 1200 ℃, pure H
2Under the protective atmosphere, 12 hours The high temperature anneal, make oriented silicon steel finish secondary recrystallization.Send into the resistance heat treatment furnace once more after the sample that will finish secondary recrystallization at last clamps with clamping plate and carry out 800 ℃, pure N
2Under the protective atmosphere, 2 hours hot-leveling anneal.
Table 1 is the result that each sample finally carries out magnetism testing.
Each sample magnetism testing result of table 1
Can see according to table 1, adopt the pulsed current recovery annealing, choose suitable pulsed current parameter and can prepare oriented silicon steel with better magnetic property.
Test result in conjunction with two Comparative Examples can be seen, adopts the oriented silicon steel B of pulsed current recovery annealing preparation
8The value outline is better than the sample that adopts common recovery annealing mode to prepare; And P
17/50Value then will be better than Comparative Examples far away.This explanation employing pulsed current annealing can be prepared performance and is better than the oriented silicon steel that the conventional annealing mode prepares.
Claims (6)
1. the method for a preparing oriented silicon steel by pulse current recovery annealing is characterized in that this method has following technological process: the rolled samples of oriented silicon steel is placed be connected with 90%N
2+ 10%H
2In the silica tube (volume percent) protective atmosphere, sealing, the copper anchor clamps good by conductivity are terminated at two of oriented silicon steel sample on two electrodes of pulse power output terminal, open pulsed current afterwards, incoming frequency is that 5～1000Hz, peak value are the pulsed current of 10～5000A, make sample temperature reach near the recovery annealing temperature (550 ℃) of oriented silicon steel, and the pulsed current that keeps finishing the oriented silicon steel sample in 5 minutes is replied processing; Be coated with magnesium oxide afterwards, carry out the annealing of high temperature annealing and hot-leveling.
2. the method for preparing oriented silicon steel by pulse current recovery annealing according to claim 1 is characterized in that, the direction that applies pulsed current is the rolling direction of oriented silicon steel.
3. the method for preparing oriented silicon steel by pulse current recovery annealing according to claim 1 is characterized in that, selected pulsed current parameter area is: incoming frequency is that 100～500Hz, current peak are 400～1100A.
4. the method for preparing oriented silicon steel by pulse current recovery annealing according to claim 1 is characterized in that, described high temperature annealing is under the pure H2 protective atmosphere, temperature is 1150～1250 ℃, 6～12 hours high temperature annealing.
5. the method for preparing oriented silicon steel by pulse current recovery annealing according to claim 1 is characterized in that, described hot-leveling is annealed into pure N
2Under the protective atmosphere, temperature is 700～900 ℃, 1～3 hour hot-leveling annealing.
6. the method for preparing oriented silicon steel by pulse current recovery annealing according to claim 1 is characterized in that, the separant that is adopted is for being the separant of main component with magnesium oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101965824A CN101665861B (en) | 2009-09-27 | 2009-09-27 | Method for preparing oriented silicon steel by pulse current recovery annealing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101965824A CN101665861B (en) | 2009-09-27 | 2009-09-27 | Method for preparing oriented silicon steel by pulse current recovery annealing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101665861A true CN101665861A (en) | 2010-03-10 |
| CN101665861B CN101665861B (en) | 2011-06-08 |
Family
ID=41802638
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101965824A Active CN101665861B (en) | 2009-09-27 | 2009-09-27 | Method for preparing oriented silicon steel by pulse current recovery annealing |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101665861B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127622A (en) * | 2011-01-18 | 2011-07-20 | 北京科技大学 | Method for improving magnetic characteristics of orientated silicon steel by heat treatment of pulse electric field |
| CN102220460A (en) * | 2011-05-27 | 2011-10-19 | 河北联合大学 | Evenly diffusion annealing method for raising diffusion speed of element |
| CN102424898A (en) * | 2011-12-16 | 2012-04-25 | 哈尔滨工业大学 | Amplitude-modulated variable-frequency pulse current annealing treatment device for amorphous metal fibers |
| CN102553797A (en) * | 2012-01-30 | 2012-07-11 | 无锡华精新型材料有限公司 | Coating process of insulated paint on surface of oriented silicon steel strip |
| CN104141101A (en) * | 2013-05-10 | 2014-11-12 | 贵州大学 | Pulse current assisted aluminum alloy homogenization heat treatment method |
| CN104831026A (en) * | 2015-05-25 | 2015-08-12 | 马钢(集团)控股有限公司 | Adjustable electrical steel annealing and heating device and annealing and heating method thereof |
| CN105543745A (en) * | 2015-12-18 | 2016-05-04 | 燕山大学 | Device for conducting medium frequency induction heating treatment on copper pipe with assistance of pulse currents |
| CN105886727A (en) * | 2016-05-05 | 2016-08-24 | 北京科技大学 | Method for promoting graphitization of hypoeutectoid steel through adopting pulse current |
| CN111590076A (en) * | 2020-06-01 | 2020-08-28 | 吉林大学 | Electric pulse post-processing method and device for improving performance of metal component |
| CN115058560A (en) * | 2022-04-14 | 2022-09-16 | 太原理工大学 | Post-processing device for plate strip pulse current and using method |
-
2009
- 2009-09-27 CN CN2009101965824A patent/CN101665861B/en active Active
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127622A (en) * | 2011-01-18 | 2011-07-20 | 北京科技大学 | Method for improving magnetic characteristics of orientated silicon steel by heat treatment of pulse electric field |
| CN102127622B (en) * | 2011-01-18 | 2012-12-26 | 北京科技大学 | Method for improving magnetic characteristics of orientated silicon steel by heat treatment of pulse electric field |
| CN102220460A (en) * | 2011-05-27 | 2011-10-19 | 河北联合大学 | Evenly diffusion annealing method for raising diffusion speed of element |
| CN102220460B (en) * | 2011-05-27 | 2013-04-10 | 河北联合大学 | Evenly diffusion annealing method for raising diffusion speed of element |
| CN102424898A (en) * | 2011-12-16 | 2012-04-25 | 哈尔滨工业大学 | Amplitude-modulated variable-frequency pulse current annealing treatment device for amorphous metal fibers |
| CN102424898B (en) * | 2011-12-16 | 2013-04-03 | 哈尔滨工业大学 | Amplitude-modulated variable-frequency pulse current annealing treatment device for amorphous metal fibers |
| CN102553797A (en) * | 2012-01-30 | 2012-07-11 | 无锡华精新型材料有限公司 | Coating process of insulated paint on surface of oriented silicon steel strip |
| CN102553797B (en) * | 2012-01-30 | 2014-07-30 | 无锡华精新材股份有限公司 | Coating process of insulated paint on surface of oriented silicon steel strip |
| CN104141101A (en) * | 2013-05-10 | 2014-11-12 | 贵州大学 | Pulse current assisted aluminum alloy homogenization heat treatment method |
| CN104141101B (en) * | 2013-05-10 | 2017-02-22 | 贵州大学 | Pulse current assisted aluminum alloy homogenization heat treatment method |
| CN104831026A (en) * | 2015-05-25 | 2015-08-12 | 马钢(集团)控股有限公司 | Adjustable electrical steel annealing and heating device and annealing and heating method thereof |
| CN105543745A (en) * | 2015-12-18 | 2016-05-04 | 燕山大学 | Device for conducting medium frequency induction heating treatment on copper pipe with assistance of pulse currents |
| CN105886727A (en) * | 2016-05-05 | 2016-08-24 | 北京科技大学 | Method for promoting graphitization of hypoeutectoid steel through adopting pulse current |
| CN111590076A (en) * | 2020-06-01 | 2020-08-28 | 吉林大学 | Electric pulse post-processing method and device for improving performance of metal component |
| CN111590076B (en) * | 2020-06-01 | 2021-07-23 | 吉林大学 | Electric pulse post-processing method and device for improving performance of metal component |
| CN115058560A (en) * | 2022-04-14 | 2022-09-16 | 太原理工大学 | Post-processing device for plate strip pulse current and using method |
| CN115058560B (en) * | 2022-04-14 | 2023-10-24 | 太原理工大学 | Post-processing device for plate and strip pulse current and application method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101665861B (en) | 2011-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101665861B (en) | Method for preparing oriented silicon steel by pulse current recovery annealing | |
| CN104388951B (en) | A kind of grain boundary decision method for improving sintered NdFeB magnetic property | |
| KR101404101B1 (en) | Method for manufacturing non-oriented silicon steel with high-magnetic induction | |
| JP6884875B2 (en) | Laser scribed directional silicon steel for stress relief annealing and its manufacturing method | |
| CN102361993B (en) | Process for producing grain-oriented magnetic steel sheet, grain-oriented magnetic steel sheet for wound core, and wound core | |
| CN101886215B (en) | Short-flow high-efficiency preparation method of thin high-silicon electrical steel strip | |
| CN108486453A (en) | A kind of preparation method of low-iron loss high-magnetic strength non-oriented silicon steel plate | |
| CN104404396B (en) | High-magnetic-strength no-orientation silicon steel free from normalizing and production method of sheet billets | |
| CN103695791B (en) | A kind of high magnetic induction grain-oriented silicon steel and production method | |
| CN111057820B (en) | Efficient annealing method for improving comprehensive performance of iron-based amorphous alloy iron core | |
| CN107109583B (en) | Non-oriented electromagnetic steel sheet and its manufacturing method | |
| CN105039758B (en) | Precipitation strengthening type high-strength and high-conductivity CuZr alloy and preparing method thereof | |
| CN104937118A (en) | Production method for semi-processed non-oriented electromagnetic steel sheet exhibiting superior magnetic properties | |
| CN103074476B (en) | Method for producing high-magnetic-induction oriented silicon strips through three-stage normalizing | |
| CN102212671B (en) | Method for promoting growth of GOSS textures of silicon steel strips by using pulse current | |
| CN109252102A (en) | A method of improving low silicon non-oriented silicon-steel magnetic can | |
| WO2018227792A1 (en) | Iron-based amorphous alloy having low stress sensitivity, and preparation method therefor | |
| CN201265027Y (en) | Direct switch-on heating annealing apparatus of hot rolled plate | |
| CN104046758A (en) | Short-process efficient cold-rolling preparation method of high-silicon steel thin strip | |
| CN102220466A (en) | Method for producing semi-processed cold-rolled non-oriented electrical steel | |
| WO2014078977A1 (en) | Oriented silicon steel and method for manufacturing same | |
| CN109182705B (en) | Method for rapidly preparing oriented thin strip electrical steel at room temperature by pulse current | |
| CN102127622B (en) | Method for improving magnetic characteristics of orientated silicon steel by heat treatment of pulse electric field | |
| KR101633611B1 (en) | High silicon electrical steel sheet with superior magnetic properties, and method for fabricating the high silicon electrical steel | |
| CN104018061B (en) | Easy processing, big magnetostriction FeAl alloy strip steel rolled stock and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |