CN107746929A - High magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced - Google Patents
High magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced Download PDFInfo
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- CN107746929A CN107746929A CN201711181734.4A CN201711181734A CN107746929A CN 107746929 A CN107746929 A CN 107746929A CN 201711181734 A CN201711181734 A CN 201711181734A CN 107746929 A CN107746929 A CN 107746929A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/68—Temporary coatings or embedding materials applied before or during heat treatment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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Abstract
The invention discloses a kind of high magnetic induction grain-oriented silicon steel annealing agent and preparation method thereof and the application on aquation rate is reduced, belong to iron and steel smelting technology field.The annealing agent includes each component of following mass percentage content：MgO：7.64~11.08%, TiO2Or/and B2O3：0.15~0.89%, Sb2(SO4)3：0.007~0.05%, surplus is water；To be made up of high activity MgO and low activity MgO, high activity MgO and low activity MgO mass ratio are MgO：13:7~4:1；High activity MgO granularity D50≤3 μm, CAA values are 30~50s, and low activity MgO granularity D50 is 10~20 μm, and CAA values are 150~250s.The annealing agent can be reduced because of the Surface Defects in Steel Plate caused by high aquation rate the problem of, the large-scale coiled material suitable for being easier to occur temperature change.
Description
Technical field
The present invention relates to a kind of annealing agent of high magnetic induction grain-oriented silicon steel, belong to iron and steel smelting technology field, more particularly to
A kind of high magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced.
Background technology
Orientation silicon steel is mainly used in making the stator battery core of transformation iron core and big generator, be in electric power industry development the most
One of important functional material.Orientation silicon steel presses { 110 }《001》The degree of orientation is divided into common orientation silicon steel and height with magnetic property difference
The class of magnetic induction grain-oriented silicon steel two, wherein high magnetic induction grain-oriented silicon steel have that iron loss is low, magnetic induction intensity compared with common orientation silicon steel
High, the advantages that magnetostriction is small, the power transformer product made of it has the advantages that open circuit loss is low, noise is low, small volume, closely
Nian Lai, the yield of high magnetic induction grain-oriented silicon steel increase year by year with usage amount.
High magnetic induction grain-oriented silicon steel will not only have excellent electromagnetic performance, but also require insulaion resistance height and pile pieces coefficient
High, corrosion resisting property drinks heat resistance is good, coating tack is good, surface color is uniform etc., its quality requirement and technology difficulty ratio
Common orientation silicon steel is high.The coating of high magnetic induction grain-oriented silicon steel is divided into barrier coat, magnesium silicate bottom, 3 kinds of insulating coating, coating
Composition and technique and every quality index of finished product are closely related.
Wherein, barrier coat be high magnetic induction grain-oriented silicon steel after cold rolling and decarburizing annealing, be sent to high temperature bell-type furnace carry out
Before high annealing, it is necessary in steel strip surface roller coat barrier coat and to dry, 1) the acting as of barrier coat is used as annealing separating agent,
Prevent coil of strip from producing adhesive tape in high-temperature annealing process；2) in high-temperature annealing process, the titanium dioxide of magnesia and steel strip surface
Pasc reaction, generate magnesium silicate glass film；3) promote desulfurization, denitrification reaction, improve purification steel effect, 4) improve finished product magnetic
Property.Conventional barrier coat adds appropriate titanium dioxide and a small amount of boride, antimonide, sulfide based on magnesia
Deng additive.
Magnesium silicate bottom is the magnesium silicate of magnesia and the generation of steel strip surface silicon dioxde reaction in high-temperature annealing process
Glass-film, its hardness is higher, is firmly combined with steel band, not only itself has good insulating properties and corrosion resistance, while is also exhausted
The preferable bottom of edge coating.The quality of orientation silicon steel finished product and bottom layer quality have a close relationship, the good then finished product face of bottom
Color is uniform, and with special gloss, coating tack and insulaion resistance are higher, and can produce in insulating coating sintering process compared with
Big tension, reduce the positive effect of iron loss.The purity of magnesia, activity and granularity, the composition of additive in barrier coat
Have an impact to the quality of glass film bottom with content, the moisture content of coating, the temperature curve of high annealing and atmosphere etc..
Chinese invention patent application (application publication number：CN105154646, data of publication of application：2015-12-16) disclose
A kind of high magnetic induction grain-oriented silicon steel annealing separating agent, its raw material composition and weight percent content are：TiO2:1~6%, Sb2
(SO4)3:0.1~2%, remaining is MgO, and external adding water, amount of water is according to MgO:Water=1:8~15；Preparation method：By MgO and water
Mixed, add TiO2And stir full and uniform, addition Sb2(SO4)3And stir, it is further continued for stirring and is no less than 2 hours, treats
With.The present invention not only makes high magnetic induction grain-oriented silicon steel magnetic induction performance and bottom layer quality excellent, and good insulation preformance, suitable for Gao Rong
The requirement of quantitative change depressor, while the concession rate of product can also be reduced.
Chinese invention patent application (application publication number：CN106319174A, data of publication of application：2017-01-11) disclose
A kind of annealing separating agent for improving low temperature casting blank heating high magnetic induction grain-oriented silicon steel bottom layer quality, including following components and quality contain
Amount：9~14% silicon-steel grade magnesium oxide, 0.3~1.0% TiO2, 0.05~1.2% Sb2(SO4)3, surplus is water；It is described
The citric acid activity value of silicon-steel grade magnesium oxide is 50~120sec, and viscosity is 15~60C.P.The annealing separating agent solves at present
Low temperature casting blank heats the greatest problem of high magnetic induction grain-oriented silicon steel, i.e.,：Bottom defect problem, the appearance of coat for being is excellent, tack
Reach more than C levels, interface resistance is big, and then greatly improves the product quality of high magnetic induction grain-oriented silicon steel.
The problem of above-mentioned interleaving agent is present be：They all disclose a kind of high magnetic induction grain-oriented silicon steel annealing separating agent, but
It is the solution method for not proposing a series of defects caused by high aquation rate present in scene, it is warm especially for that may occur
Spend the large-scale coiled material of change, it is easier to produce surface defect, lead to not to form uniform glass-film.
The aquation rate of whole annealing agent can be reduced using the aquation rate of magnesia in itself is reduced in the prior art, still
Approach specific implementation difficulty of getting up is larger, because aquation rate and the originally opposite two indices of activity, reduce oxygen
The decrease of MgO activity can also be caused by changing the aquation rate of magnesium in itself, so to ensure the premise of MgO activity as far as possible
Under, to reduce aquation rate.
The content of the invention
In order to solve the above technical problems, the invention discloses a kind of high magnetic induction grain-oriented silicon steel with annealing agent and preparation method and
Its application on aquation rate is reduced.
To achieve the above object, the invention discloses a kind of annealing agent of high magnetic induction grain-oriented silicon steel, it includes following quality
The each component of degree：MgO：7.64~11.08%, TiO2Or/and B2O3：0.15~0.89%, Sb2(SO4)3：0.007
~0.05%, surplus is water；The MgO is that middle high activity MgO and low activity MgO is formed, the middle high activity MgO and low activity
MgO mass ratio is：13:7~4:1；Granularity D50≤3 μm of the middle high activity MgO, CAA values are 30~50s, the low work
Property MgO granularity D50 be 10~20 μm, CAA values are 150~250s.
Further, weight-loss ratio≤1% after the MgO calcinations, aquation rate≤2.5% of the MgO.
Preferably, the calcination condition for controlling above-mentioned MgO is that calcination temperature is 900 DEG C, and calcination time is 1h with up to gross weight
Amount no longer changes.
Yet further, the mass ratio of the MgO and water are 1:8~12.
The invention also discloses the method for preparing above-mentioned high magnetic induction grain-oriented silicon steel annealing agent, it comprises the following steps：
1) TiO that mass percentage content is 0.15~0.89% is added into water2Or/and B2O3And mass percent contains
Measure the Sb for 0.007~0.05%2(SO4)3, 1~1.5h is stirred after to be added, control mixing speed is not less than
3000rpm/min, the mixture to be stirred；
2) continue to add the MgO that mass percentage content is 7.64~11.08% into the mixture of the step 1), treat
1~1.5h is stirred after addition, controls mixing speed to be not less than 3000rpm within preceding 0.5h, it is therefore an objective to by each of addition
Individual component is well mixed, and is then adjusted to mixing speed to be less than or equal to 1500rpm, it is therefore an objective to prevents magnesia from excessive water occurs
Change, that is, annealing agent is prepared.
Application of the high magnetic induction grain-oriented silicon steel disclosed by the invention with annealing agent on aquation rate is reduced.
Hot rolling, normalizing, annealing, once cold rolling preferably will be passed through containing the raw material slab that silicone content is 3%~3.25%
The step of, obtain the steel plate of corresponding thickness.
It is further preferred that above-mentioned steel plate is placed in progress decarburizing annealing processing in continuous annealing line so that surface of steel plate
Form oxide-film.
It is further preferred that the annealing agent prepared to be formed to the surface of steel plate of oxide-film coated in surface, high temperature is carried out
Annealing, glass film is formed, continue to coat insulation coating agent in surface of steel plate, and be dried, finally refined magnetic domain and be prepared into
To final product.
The selection principle of each component in present invention annealing agent：
Titanium dioxide：Oxygen is decomposited in high-temperature annealing process, improves the atmosphere between steel band, oxygen can be with diffusing out in steel
Aluminium combine, avoid aluminium destroy silicon dioxide film, so as to ensure to generate good magnesium silicate glass film, improve the attachment of glass-film
Property, and strengthen the ability of glass-film absorbed nitrogen, while the number of bends of steel band can also be improved.
Boride：Strengthen rejection ability, make secondary crystallization more perfect, improve glass film quality and magnetic；
Antimonide：Strengthen restraint, promote subgrain development, increase tension caused by insulating coating, improve magnetic.
Magnesia：Magnesia is the main component of annealing agent, but its aquation rate is higher, is easily aoxidized in whipping process
The hydration reaction of magnesium and water reaction generation magnesium hydroxide, causes water content increase in coiled material, so as to improve the dew point of surface of steel plate,
So that glass film becomes uneven in the vertical or horizontal of coiled material, ultimately result in surface of steel plate and a series of defect occur.Add
Increase two kind different MgOs of the activity with low activity, be on the one hand due to often to have when CAA values are too high compared with high-moisture percentage, make
It is difficult the content of control coil of strip reclaimed water in must producing, often leads to coil of strip surface and be oxidized, can be with by the MgO for adding low activity
The overall CAA values of effective regulation, on the other hand because the MgO particles of low activity are bigger, can effectively increase steel band and steel
Gap between band, improve steel plate MgO permeability, be advantageous to the discharge of steam.
Beneficial effect：
The present invention causes the technical problem of the Surface Defects in Steel Plate of production based on aquation rate higher in annealing agent, it is proposed that
A kind of annealing agent for reducing aquation rate, the annealing agent improve the saturating of magnesia by using the magnesia mixture of size particles
Gas so that the steel plate bottom layer quality handled using the annealing agent is good, does not occur the problems such as brilliant leakage or aberration.
Brief description of the drawings
Fig. 1 is the electron-microscope scanning figure before the steel plate coating insulation coating agent of the embodiment of the present invention；
Fig. 2 is the electron-microscope scanning figure before the steel plate coating insulation coating agent of comparative example of the present invention；
Embodiment
In order to preferably explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
Present disclosure is not limited solely to following examples.
Method the invention discloses high magnetic induction grain-oriented silicon steel with annealing agent, it comprises the following steps：
1) TiO that mass percentage content is 0.15~0.89% is added into water2Or/and B2O3And mass percent contains
Measure the Sb for 0.007~0.05%2(SO4)3, 1~1.5h is stirred after to be added, control mixing speed is not less than
3000rpm, the mixture to be stirred；
2) continue to add the MgO that mass percentage content is 7.64~11.08% into the mixture of the step 1), treat
1~1.5h is stirred after addition, controls mixing speed to be not less than 3000rpm within preceding 0.5h, it is therefore an objective to by each of addition
Individual component is well mixed, and is then adjusted to mixing speed to be less than or equal to 1500rpm, it is therefore an objective to prevents magnesia from excessive water occurs
Change, that is, the slurry of annealing agent is prepared.
The annealing agent prepared using the above method is as shown in table 1；
Each component and content in the annealing agent of the embodiment of table 1 and comparative example
To be containing slab chemical composition (Wt%)：0.055%C, 3.18%Si, 0.035%Mn, 0.024%S,
0.027%Als, 0.008%N, 0.12%Cu remaining be Fe and inevitable impurity high magnetic induction grain-oriented silicon steel by hot rolling,
Annealing and cold rolling, have obtained the steel plate of 0.26mm thickness；Then, above-mentioned steel plate is placed on continuous annealing line, control annealing temperature
Spend for 835 DEG C, annealing time 120s, carry out decarburizing annealing processing so that surface of steel plate generates oxide-film.
The annealing agent of table 1 is respectively coated on the surface of steel plate that above-mentioned surface forms oxide-film, control coated weight be 5~
7g/m2, high annealing is carried out, the high annealing is the gas of hydrogen by steel plate coiled material in about 1170 DEG C of high-temperature annealing furnace
16~19h is incubated under atmosphere and carries out high annealing；Glass film is formed, continues to coat insulation coating agent in surface of steel plate and is done
It is dry, finally refine magnetic domain and final products are prepared, the performance parameter of product is as shown in table 2；
Plate property after the annealing agent processing of the embodiment of table 2 and comparative example
Being understood with reference to Fig. 1 and Fig. 2, wherein Fig. 1 is the electron-microscope scanning figure before the steel plate coating insulation coating agent of embodiment 1,
Fig. 2 is the electron-microscope scanning figure before the steel plate coating insulation coating agent of comparative example 1, it is seen that using the embodiment of the present invention
Annealing agent processing after steel plate, after annealed processing, the magnesium silicate granule of formation is compact and complete, and the sample table in comparative example
Then there is the defects of more in face, and the magnesium silicate granule of formation is bigger, and matrix surface is not fine and close, has more matrix to expose.
Understand that 1~embodiment of embodiment 6 is by the extra light calcined magnesia and heavy-burned magnesia in magnesia with reference to table 1
Content control in suitable scope, that is, ensure high activity MgO and low activity MgO mass ratio be：13:7~4:1, it is most
The product bottom outward appearance obtained eventually is as shown in table 2, understands that the bottom outer tube of product is good, is tightly combined, tack with reference to table 2
Also it is preferable.Conversely, when the content of magnesia of high activity is higher, as shown in comparative example 1, the ratio with reference to water is caused substantially to rise
Height, steam increases the final bottom for causing product and the defects of point-like leakage is brilliant occurs in annular furnace, and when the magnesia of low activity contains
When amount is higher, as shown in comparative example 2, causes the formation temperature of glass-film too high and influence the formation of glass-film, finally cause
The bottom of product forms bad.
Claims (7)
- A kind of 1. high magnetic induction grain-oriented silicon steel annealing agent, it is characterised in that：It includes each component of following mass percentage content： MgO：7.64~11.08%, TiO2Or/and B2O3：0.15~0.89%, Sb2(SO4)3：0.007~0.05%, surplus is water； To be made up of high activity MgO and low activity MgO, the high activity MgO and low activity MgO mass ratio is the MgO：13:7~ 4:1；Granularity D50≤3 μm of the high activity MgO, CAA values are 30~50s, and the granularity D50 of the low activity MgO is 10~20 μm, CAA values are 150~250s.
- 2. high magnetic induction grain-oriented silicon steel according to claim 1 annealing agent, it is characterised in that：Mistake after the MgO calcinations Rate≤1% again, aquation rate≤2.5% of the MgO.
- 3. high magnetic induction grain-oriented silicon steel according to claim 1 or 2 annealing agent, it is characterised in that：In the annealing agent, The mass ratio of the MgO and water are 1:8~12.
- A kind of 4. preparation method of high magnetic induction grain-oriented silicon steel according to claim 1 annealing agent, it is characterised in that：It is wrapped Include following steps：1) TiO that mass percentage content is 0.15~0.89% is added into water2Or/and B2O3And mass percentage content is 0.007~0.05% Sb2(SO4)3, 1~1.5h is stirred after to be added, control mixing speed is not less than 3000rpm, obtained To the mixture to stir；2) continue to add the MgO that mass percentage content is 7.64~11.08% in the mixture obtained to step 1), it is to be added After stir 1~1.5h, within the preceding 0.5h of stirring control mixing speed be not less than 3000rpm, then by mixing speed It is adjusted to be less than or equal to 1500rpm, that is, annealing agent is prepared.
- 5. the high magnetic induction grain-oriented silicon steel according to claim 4 preparation method of annealing agent, it is characterised in that：The step 2) in, MgO is that mass ratio is：13:7~4:1 high activity MgO and low activity MgO mixture, the mistake after the MgO calcinations Rate≤1% again, aquation rate≤2.5%.
- 6. the high magnetic induction grain-oriented silicon steel according to claim 4 preparation method of annealing agent, it is characterised in that：Moved back described In fiery agent, the mass ratio of the MgO and water are 1:8~12.
- A kind of 7. application of the high magnetic induction grain-oriented silicon steel with annealing agent on aquation rate is reduced described in claim 1.
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Cited By (6)
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| CN108977638A (en) * | 2018-08-24 | 2018-12-11 | 首钢智新迁安电磁材料有限公司 | A kind of orientation silicon steel annealing separating agent and its application method |
| CN109306198A (en) * | 2018-08-22 | 2019-02-05 | 武汉钢铁有限公司 | For improving the masking liquid and preparation method thereof of high magnetic induction grain-oriented silicon steel magnesium silicate bottom layer quality |
| CN111186850A (en) * | 2019-12-27 | 2020-05-22 | 南京宝淳新材料科技有限公司 | Magnesium oxide for oriented silicon steel annealing separant and preparation method thereof |
| CN114635020A (en) * | 2022-03-09 | 2022-06-17 | 山西银圣科技有限公司 | Annealing release agent and preparation method and application thereof |
| CN114645126A (en) * | 2022-03-09 | 2022-06-21 | 山西银圣科技有限公司 | Common oriented silicon steel magnesium oxide separant and preparation method and application thereof |
| CN114854960A (en) * | 2022-03-30 | 2022-08-05 | 武汉钢铁有限公司 | Annealing separant for reducing surface defects of oriented silicon steel and using method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109306198A (en) * | 2018-08-22 | 2019-02-05 | 武汉钢铁有限公司 | For improving the masking liquid and preparation method thereof of high magnetic induction grain-oriented silicon steel magnesium silicate bottom layer quality |
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| CN111186850B (en) * | 2019-12-27 | 2022-12-16 | 南京宝淳新材料科技有限公司 | Magnesium oxide for oriented silicon steel annealing separant and preparation method thereof |
| CN114635020A (en) * | 2022-03-09 | 2022-06-17 | 山西银圣科技有限公司 | Annealing release agent and preparation method and application thereof |
| CN114645126A (en) * | 2022-03-09 | 2022-06-21 | 山西银圣科技有限公司 | Common oriented silicon steel magnesium oxide separant and preparation method and application thereof |
| CN114854960A (en) * | 2022-03-30 | 2022-08-05 | 武汉钢铁有限公司 | Annealing separant for reducing surface defects of oriented silicon steel and using method thereof |
| CN114854960B (en) * | 2022-03-30 | 2023-09-05 | 武汉钢铁有限公司 | Annealing isolating agent for reducing surface defects of oriented silicon steel and use method thereof |
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Application publication date: 20180302 |