CN114150126A - Copper-containing general oriented silicon steel and preparation method thereof - Google Patents

Copper-containing general oriented silicon steel and preparation method thereof Download PDF

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CN114150126A
CN114150126A CN202111463911.4A CN202111463911A CN114150126A CN 114150126 A CN114150126 A CN 114150126A CN 202111463911 A CN202111463911 A CN 202111463911A CN 114150126 A CN114150126 A CN 114150126A
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steel
oriented silicon
copper
decarburized
annealing
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许光
朱业超
杨秀枝
王自荣
熊智威
龙明建
李江波
蔡苗
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Lysteel Co Ltd
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Lysteel Co Ltd
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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
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
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    • 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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    • 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
    • C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
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    • C21D6/00—Heat treatment of ferrous alloys
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    • 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
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling
    • 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
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    • C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
    • 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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    • 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
    • C21D8/1288—Application of a tension-inducing coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/10—Oxidising
    • C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
    • C23C8/18—Oxidising of ferrous surfaces
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25

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Abstract

The present invention provides a general orientation of copperThe silicon steel and the preparation method thereof comprise the following steps: performing decarburization annealing on the steel plate to obtain a decarburized steel, wherein the oxygen content of the decarburized steel is controlled within the range calculated by the following formula: psiO＝(0.0504×ωSi×H2±0.00005)×106Wherein ψOThe oxygen content of the decarburized steel is ppm; omegaSiIs the weight percentage content of Si in the steel plate; h is the thickness of the steel plate, and the unit is mm; cold rolling the decarburized steel, coating a magnesium oxide coating, curling and coiling annealing to obtain an annealed steel coil; and uncoiling the annealed steel coil, coating a tensile stress coating, and stretching, flattening and annealing to obtain the copper-containing general oriented silicon steel. According to the actual content of Si in the steel plate and the thickness of the steel plate, the oxygen content of the decarburized steel is adjusted so as to obtain a copper-containing general oriented silicon steel product with good surface quality and stable magnetic level.

Description

Copper-containing general oriented silicon steel and preparation method thereof
Technical Field
The application relates to the technical field of steel preparation, in particular to copper-containing general oriented silicon steel and a preparation method thereof.
Background
Oriented silicon steel is an important soft magnetic material, is mainly used for manufacturing transformer cores and is classified according to magnetic polarization strength, and the oriented silicon steel is divided into general oriented silicon steel (CGO) and high magnetic induction oriented silicon steel (HGO). Copper-containing general oriented silicon steel was originally developed by russian new-rietz foundries, and is general oriented silicon steel using AlN as a main inhibitor and an intermetallic compound of copper as an auxiliary inhibitor. Compared with other common oriented silicon steel taking MnS as a main inhibitor, the hot-rolled high-strength oriented silicon steel has the characteristics of low hot-rolling heating temperature and high magnetic polarization strength, so that the hot-rolled high-strength oriented silicon steel is rapidly popularized in the field of common oriented silicon steel manufacturing.
At present, the magnetic level and the surface quality of a common oriented silicon steel product containing copper often fluctuate greatly, and the requirements of equipment such as a transformer, an electric reactor and the like on iron core materials are difficult to meet.
Disclosure of Invention
In order to solve the technical problems, the application provides copper-containing general oriented silicon steel and a preparation method thereof, and aims to provide copper-containing general oriented silicon steel with stable magnetic level and good surface quality.
On one hand, the application provides a preparation method of copper-containing general oriented silicon steel, which comprises the following steps:
(1) performing decarburization annealing on the steel plate to obtain a decarburized steel, wherein the oxygen content of the decarburized steel is controlled within the range calculated by the following formula:
ψO＝(0.0504×ωSi×H2±0.00005)×106，
wherein psiOThe oxygen content of the decarburized steel is ppm; omegaSiIs the weight percentage content of Si in the steel plate; h is the thickness of the steel plate, and the unit is mm;
(2) cold rolling the decarburized steel, coating a magnesium oxide coating, curling and coiling annealing to obtain an annealed steel coil;
(3) and uncoiling the annealed steel coil, coating a tensile stress coating, and stretching, flattening and annealing to obtain the copper-containing general oriented silicon steel.
Optionally, the steel plate in the step (1) comprises the following components in percentage by weight:
0.02wt％≤C≤0.055wt％，2.81wt％≤Si≤3.60wt％，0.10wt％≤Mn≤0.30wt％，0.008wt％≤Als≤0.030wt％，0.4wt％≤Cu≤0.6wt％，0.006wt％≤N≤0.012wt％，P≤0.050wt％，S≤0.015wt％，95.4wt％≤Fe≤96.5wt％。
optionally, the thickness of the steel plate in the step (1) is 0.5-0.7 mm.
Optionally, in the step (1), the oxygen content of the decarburized steel is regulated by adjusting the water-hydrogen ratio in the decarburization annealing process, wherein the water-hydrogen ratio is the partial pressure ratio of water vapor and hydrogen.
Optionally, the annealing temperature of the decarburization annealing in the step (1) is 800-900 ℃, and the annealing time is 2-10 min.
Optionally, the decarburized steel obtained in step (1) comprises a steel body and an oxide film on the surface of the steel body, wherein the oxide film comprises SiO2FeO and Fe2SiO4。
Optionally, the thickness of the oxide film is 3-10 μm.
Optionally, the annealed steel coil obtained in the step (2) includes a steel coil body and a magnesium silicate layer on the surface of the steel coil body.
Optionally, the method for preparing the copper-containing general oriented silicon steel further comprises the following steps:
smelting the molten steel to obtain a casting blank;
heating, hot rolling, laminar cooling and curling a casting blank to obtain a steel coil;
and (2) carrying out acid pickling and primary cold rolling on the steel coil to obtain the steel plate used in the step (1).
In another aspect, the application also provides the copper-containing general oriented silicon steel prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
according to the actual content of Si in the steel plate and the thickness of the steel plate, the oxygen content of the decarburized steel is adjusted, so that the oxide film structure of the decarburized steel is matched with the Si content, the forming temperature of a magnesium silicate bottom layer and the gaps among all layers of the steel coil are adjusted when the decarburized steel is annealed at a high temperature, and finally, a copper-containing general oriented silicon steel product with good surface quality and stable magnetic level is obtained.
Drawings
Features, advantages and technical effects of exemplary embodiments of the present application will be described below with reference to the accompanying drawings.
FIG. 1 is a surface oxide film morphology of a cross section of a decarburized steel of example 10 of the present application.
Detailed Description
Embodiments of the present application will be described in further detail below with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the application and are not intended to limit the scope of the application, i.e., the application is not limited to the described embodiments.
In the description of the present application, it is to be noted that, unless otherwise specified, "a plurality" means two or more; the terms "upper," "lower," "left," "right," "inner," "outer," and the like, indicate an orientation or positional relationship that is merely for convenience in describing the application and to simplify the description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the application. Furthermore, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. "vertical" does not require vertical in the strict sense, but may include an allowable error. "parallel" does not require parallelism in a strict sense, but may include an allowable error.
The embodiment of the first aspect of the application provides a preparation method of copper-containing general oriented silicon steel, which comprises the following steps:
(1) performing decarburization annealing on the steel plate to obtain a decarburized steel, wherein the oxygen content of the decarburized steel is controlled within the range calculated by the following formula:
ψO＝(0.0504×ωSi×H2±0.00005)×106，
wherein psiOThe oxygen content of the decarburized steel is ppm; omegaSiIs the weight percentage content of Si in the steel plate; h is the thickness of the steel plate, and the unit is mm;
(2) cold rolling the decarburized steel, coating a magnesium oxide coating, curling and coiling annealing to obtain an annealed steel coil;
(3) and uncoiling the annealed steel coil, coating a tensile stress coating, and stretching, flattening and annealing to obtain the copper-containing general oriented silicon steel.
According to the actual content of Si in the steel plate and the thickness of the steel plate, the oxygen content of the decarburized steel is adjusted, so that the oxide film structure of the decarburized steel is matched with the Si content, the forming temperature of a magnesium silicate bottom layer and the gaps among all layers of the steel coil are adjusted when the decarburized steel is annealed at a high temperature, and finally, a copper-containing general oriented silicon steel product with good surface quality and stable magnetic level is obtained.
In some embodiments of the present invention, the thickness of the steel plate in the step (1) is 0.5 to 0.7 mm.
In some embodiments of the present invention, the steel plate in step (1) comprises the following components in percentage by weight:
0.02wt％≤C≤0.055wt％，2.81wt％≤Si≤3.60wt％，0.10wt％≤Mn≤0.30wt％，0.008wt％≤Als≤0.030wt％，0.4wt％≤Cu≤0.6wt％，0.006wt％≤N≤0.012wt％，P≤0.050wt％，S≤0.015wt％，95.4wt％≤Fe≤96.5wt％。
optionally, the thickness of the steel plate in the step (1) is 0.5-0.7 mm.
C, when the important elements for manufacturing the oriented silicon steel are less than 0.02 wt% of C, deformed grains remain after cold rolling and decarburization annealing, secondary crystallization is incomplete after high-temperature annealing, and the magnetic property is reduced; however, when the carbon content is too high, decarburization becomes difficult, so that the carbon content is set to 0.02 wt% or more and 0.055 wt% or less.
Si, which can effectively improve the resistance of the oriented silicon steel, is used for reducing the eddy current loss. When the Si content is less than 2.81 wt%, the effect is not significant; when the Si content is more than 3.60 wt%, processability is lowered. Therefore, the Si content is set to be more than or equal to 2.81 weight percent and less than or equal to 3.60 weight percent.
Mn increases the resistance of the copper-containing general oriented silicon steel, reduces the loss of an iron core, has the function of preventing cracks from appearing in the hot rolling process, and plays a role in inhibiting the growth of crystal grains in the primary recrystallization process. When the manganese content is less than 0.10 wt%, the effect thereof cannot be sufficiently exerted; when the manganese content is more than 0.30 wt%, the magnetic flux density of the oriented silicon steel is reduced, so that the Mn content in the invention is set as follows: mn is more than or equal to 0.10 weight percent and less than or equal to 0.30 weight percent.
Als and N, an element for inhibiting the formation of AlN, and in order to ensure the formation of a sufficient amount of AlN inhibitor and to make the strength of the inhibitor meet the requirements, the content of Als in the invention is set as follows: als is more than or equal to 0.008 wt% and less than or equal to 0.030 wt%, and the content of N is set as follows: n is more than or equal to 0.006 percent and less than or equal to 0.012 percent by weight.
Cu expands an austenite phase region and promotes AlN solid solution; may form ε -Cu or Cu2S and other auxiliary inhibitors can effectively avoid overlarge primary crystal grains and improve the secondary recrystallization crystal grain orientation. The content of Cu in the invention is set as follows: cu is more than or equal to 0.4 weight percent and less than or equal to 0.6 weight percent.
P, a harmful impurity element, is easy to cause brittle fracture of the steel plate in the processing process due to grain boundary segregation, so the content of P is set to be less than or equal to 0.050 wt%.
S, forms MnS, Cu by combining with Mn, S2S, as an auxiliary inhibitor; however, since S is too high and segregation occurs, which affects the stability of the magnetic level, the content of S is set to 0.015 wt% or less.
In some embodiments of the present invention, the decarburized steel obtained in step (1) comprises a steel body, and an oxide film on the surface of the steel body, wherein the oxide film comprises SiO2FeO and Fe2SiO4。
In some embodiments of the present invention, the oxide film has a thickness of 3 to 10 μm.
The decarburization process of the steel plate during decarburization annealing is carried out by the chemical reaction of water vapor and carbon in the atmosphere, and the reaction formula is as follows:
H2O+C＝H2+CO
oxygen in the atmosphere reacts with Si in the steel sheet to produce SiO2Particles; oxygen also reacts with iron to form FeO; FeO can be further mixed with SiO2Synthesis of Fe2SiO4So that a layer of oxide film which is looser than the steel body is formed on the surface of the steel body.
In some embodiments of the present invention, the annealed steel coil obtained in step (2) includes a steel coil body and a magnesium silicate layer on the surface of the steel coil body.
After the surface oxidation film is coated with the magnesium oxide coating, the surface oxidation film is curled to form a steel coil, and the steel coil forms a magnesium silicate layer (Mg) in the high-temperature annealing process2SiO4) The chemical reaction is as follows:
Fe2SiO4+2MgO＝Mg2SiO4+2FeO
according to the embodiment of the invention, the material is annealed in the form of a steel coil during high-temperature annealing, and the annealing atmosphere is H2、N2The mixed gas of (1). Because the oxide film on the surface of the decarburization plate is loose, the high-temperature annealing atmosphere can enter each layer of the steel coil more easily along with the thickening of the thickness of the oxide film, so that the temperature and the atmosphere of each part of the steel coil are more uniform, and the problems of undersize of each layer of the steel coil, uneven stress release and the like caused by factors such as large coiling tension of a previous process, high Si content and the like can be solved to a certain extent. However, if the thickness of the oxide film is too large, the quality of the glass film formed during high-temperature annealing is deteriorated, and Als in the steel is oxidized in advance, which deteriorates the final surface quality and magnetic level of the product.
In the decarburization annealing process, the water-hydrogen ratio is dynamically adjusted according to the actual content of Si in the steel plate and the thickness of the steel plate, so that the oxygen content of the decarburized steel is controlled within the range calculated by the formula, and the oxide film structure of the decarburized steel is matched with the Si content. The thickness of the steel plate is 0.5-0.7 mm, the Si content is more than or equal to 2.81 wt% and less than or equal to 3.60 wt%, and the thickness of the corresponding oxide film is 3-10 mu m.
In the copper-containing general oriented silicon steel, Si plays a role in increasing the resistivity and reducing the iron loss. However, when the Si content is too high, secondary recrystallization is difficult in high-temperature annealing; meanwhile, the heat conductivity and the plasticity of the steel plate are reduced due to the increase of the Si content, so that the gaps between the steel coil layers are reduced, the heat conduction efficiency is reduced, and the gas flow is not smooth in the high-temperature annealing and heating stage, so that the plate shape defects are increased, the secondary recrystallization is delayed, the secondary recrystallization is incomplete, and the magnetic level is seriously deteriorated. When the Si content is too low, the steel sheet interlayer gap increases, the gas flow rate increases, the AlN inhibitor in the steel decomposes in advance, secondary recrystallization advances, the crystal grain orientation is poor, and the magnetic level deteriorates.
In an embodiment of the present invention, the cold rolling in step (2) may further include a recovery annealing.
According to the actual value of the Si content of the copper-containing general oriented silicon steel plate and the thickness of the steel plate, the water-hydrogen ratio is dynamically adjusted, so that the oxygen content of the decarburized steel is controlled in the range calculated by the formula, the oxide film structure of the decarburized steel is matched with the Si content, the forming temperature of the magnesium silicate bottom layer and the gaps among all layers of the steel coil are adjusted during high-temperature annealing, and finally, the copper-containing general oriented silicon steel product with good surface quality and stable magnetic level is obtained.
The adjustment enables the thickness of an oxide film on the surface of the decarburized steel plate to be matched with the content of Si, and different interlayer gaps are obtained under the same coiling tension condition after magnesium oxide is coated, so that the adaptability of the decarburized annealed plate to the change of a return annealing process and the coiling tension fluctuation is enhanced during high-temperature annealing, and the adaptability of the copper-containing general oriented silicon steel product to production lines with different control capacities can be obviously improved.
The embodiment provided by the invention effectively solves the problems of fluctuation of the magnetic level and the surface quality of the product under severe conditions such as fluctuation of Si content of the copper-containing general oriented silicon steel, fluctuation of coiling tension control capability after magnesium oxide coating, change of a recovery annealing process and the like without increasing production cost and adding new equipment.
In some embodiments of the present invention, in the step (1), the oxygen content of the decarburized steel is controlled by adjusting a water-hydrogen ratio in the decarburization annealing process, wherein the water-hydrogen ratio is a partial pressure ratio of water vapor and hydrogen gas.
In some embodiments of the present invention, the annealing temperature of the decarburization annealing in the step (1) is 800 to 900 ℃, and the annealing time is 2 to 10 min.
According to the embodiment of the present invention, during the decarburization annealing, carbon is diffused from the inside of the steel sheet to the surface while CO is continuously discharged out of the furnace in a flowing atmosphere. The main factors affecting the decarburization rate and the oxygen content of the steel sheet are the decarburization temperature, the decarburization time, and the partial pressure ratio of steam to hydrogen, i.e., the water-hydrogen ratio (P)H2O/PH2). The decarburization temperature and time also affect precipitated phases, grain sizes, and the like, and are also closely related to the production line structure. Therefore, the embodiment of the application can adjust the hydrogen proportionAnd the water-hydrogen ratio and further the oxygen content are controlled by the dew point of the water vapor. That is, the water-hydrogen ratio is dynamically adjusted so that the oxygen content always falls within the target range, targeting the target oxygen content calculated by the above formula.
Meanwhile, the water-hydrogen ratio distribution in the length direction of the hearth can be adjusted according to different structures of the decarburization annealing production line, so that the oxygen content of the material in the specified distribution range corresponds to the thickness of the surface oxide film in the specified distribution range; thereby realizing that the material characteristics adapt to corresponding working conditions and finally obtaining the copper-containing general oriented silicon steel product with excellent magnetism and surface quality.
In some embodiments of the present invention, the method for preparing the copper-containing generally oriented silicon steel further comprises the following steps:
smelting the molten steel to obtain a casting blank;
heating, hot rolling, laminar cooling and curling a casting blank to obtain a steel coil;
and (2) carrying out acid pickling and primary cold rolling on the steel coil to obtain the steel plate used in the step (1).
In some embodiments of the invention, smelting includes desulfurization, converter, vacuum treatment, and continuous casting.
In some embodiments of the present invention, the heating temperature is controlled to 1250 to 1350 ℃.
In some embodiments of the invention, the finishing temperature is controlled to be 850-1000 ℃.
According to the embodiment of the invention, the pickling is used for removing the iron oxide scale on the surface of the steel coil.
In a second aspect, the invention provides a copper-containing generally oriented silicon steel prepared by the above method.
The copper-containing general oriented silicon steel comprises a steel body, a magnesium silicate layer attached to the surface of the steel body and a tensile stress coating on the surface of the magnesium silicate layer, has good surface quality and good magnetic property, and can be applied to iron cores of equipment such as transformers, reactors and the like.
First set of examples and comparative examples
Examples 1 to 3 and comparative examples 1 to 2 general oriented silicon steel containing copper was prepared in the following manner. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 1 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 2 is higher than the control range of the present invention.
The method comprises the following steps of steelmaking by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.033% of C, Si: 2.82%, Mn 0.15%, Als 0.0150%, Cu 0.46%, N0.010%, P: 0.011 percent, 0.005 percent of S and the balance of Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
the strip steel is subjected to acid pickling, then is subjected to cold rolling to the thickness of 0.63mm, and then is subjected to decarburization annealing at 840 ℃ according to the conditions shown in table 1, wherein the decarburization time is 4min, the water-hydrogen ratio is dynamically adjusted within the range of 0.30-0.80 according to the production line structure and the target values of carbon and oxygen contents, and decarburized steel is obtained;
then, carrying out secondary cold rolling to obtain a finished product with the thickness of 0.26mm, and selecting whether to carry out recovery annealing and coating an MgO coating according to the table 1; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 1 Experimental conditions and results for examples 1-3 and comparative examples 1-2
Figure BDA0003389604890000081
The adhesion measurement adopts GB/T2522-2017 standard, and the test sample is tightly bent by 180 degrees step by step around a brass cylindrical tower, and then the cracking and peeling appearance of the coating on the inner surface of the steel sheet is checked and judged according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The final magnetic level of the product of the embodiment 1-3 is obviously superior to that of the comparative example 1-2; the surface coatings of the examples 1-3 have good and uniform appearance and B-grade adhesion, which is superior to that of the comparative example 1.
In the decarburization annealing, the oxygen content of the decarburized steel is controlled to be in the range calculated by the formula according to the method provided by the invention, the decarburized steel is not subjected to the recovery annealing step after cold rolling and before coating of the magnesium oxide coating, and the magnetic performance of the decarburized steel is still better than that of the decarburized steel in comparative examples 1-2.
Second set of examples and comparative examples
Examples 4 to 6 and comparative examples 3 to 4 general oriented silicon steel containing copper was prepared according to the following method. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 3 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 4 is higher than the control range of the present invention.
Smelting steel by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.041% of C, Si: 2.95%, Mn 0.21%, Als 0.0170%, Cu 0.48%, N0.010%, P: 0.012 percent and 0.004 percent of S; the balance of Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
after the strip steel is subjected to acid pickling and then is subjected to cold rolling to the thickness of 0.65mm, decarburization annealing is carried out at 845 ℃ according to the conditions shown in the table 2, the decarburization time is 4.5min, the water-hydrogen ratio is dynamically adjusted within the range of 0.30-0.80 according to the production line structure and the target values of carbon and oxygen content, and decarburized steel is obtained;
then, second cold rolling is carried out, the thickness of a finished product is 0.285mm, and whether recovery annealing and MgO coating oxidation are carried out or not is selected according to the table 2; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 2 Experimental conditions and results for examples 4-6 and comparative examples 3-4
Figure BDA0003389604890000091
The adhesion measurement was carried out by bending the test piece only around a brass cylinder tower by 180 degrees in steps using the GB/T2522-2017 standard, and then inspecting the cracking and peeling morphology of the coating on the inner surface of the steel sheet and judging the grade according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The final magnetic level of the products of the examples 4 to 6 is obviously superior to that of the products of the comparative examples 3 to 4; the surface coatings of the examples 4 to 6 are good and uniform in appearance, and are superior to those of the comparative examples 3 to 4; the adhesion levels of examples 4-6 are comparable to those of comparative examples 3-4.
Third group of examples and comparative examples
Examples 7 to 9 and comparative examples 5 to 6 copper-containing general oriented silicon steel was prepared in the following manner. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 5 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 6 is higher than the control range of the present invention.
Smelting steel by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.045% of C, Si: 3.07%, Mn 0.21%, Als 0.0130%, Cu 0.53%, N0.011%, P: 0.015 percent of the total weight of the alloy, 0.009 percent of the total weight of the alloy and the balance of Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
after the strip steel is subjected to acid pickling and then is subjected to cold rolling to the thickness of 0.58mm, decarburization annealing is carried out at 845 ℃ according to the conditions in the table 3, the decarburization time is 3.8min, the water-hydrogen ratio is dynamically adjusted within the range of 0.30-0.80 according to the production line structure and the target values of carbon and oxygen content, and decarburized steel is obtained;
then, second cold rolling is carried out, the thickness of a finished product is 0.22mm, and whether recovery annealing and MgO coating oxidation are carried out or not is selected according to the table 3; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 3 Experimental conditions and results for examples 7-9 and comparative examples 5-6
Figure BDA0003389604890000101
The adhesion measurement was carried out by bending the test piece only around a brass cylinder tower by 180 degrees in steps using the GB/T2522-2017 standard, and then inspecting the cracking and peeling morphology of the coating on the inner surface of the steel sheet and judging the grade according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The final magnetic level of the products of examples 7-9 is significantly better than that of comparative examples 5-6; the surface coatings of examples 7-9 have good and uniform appearances, which are superior to those of comparative examples 5-6; the adhesion of examples 7 to 9 is superior to that of comparative examples 5 to 6.
Example 9 in decarburization annealing, the oxygen content of the decarburized steel is controlled within the range calculated by the formula according to the method provided by the invention, and the magnetic performance and the adhesion of the decarburized steel are still obviously better than those of comparative examples 5-6 without a recovery annealing step after cold rolling and before coating a magnesium oxide coating.
Fourth group of examples and comparative examples
In examples 10 to 12 and comparative examples 7 to 8, a copper-containing general oriented silicon steel was prepared in the following manner. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 7 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 8 is higher than the control range of the present invention.
Smelting steel by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.049% of C, Si: 3.18%, Mn 0.28%, Als 0.0190%, Cu 0.42%, N0.009%, P: 0.013% of S, 0.011% of S and the balance of Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
after the strip steel is subjected to acid pickling and then is subjected to cold rolling to the thickness of 0.68mm, decarburization annealing is carried out at 840 ℃ according to the conditions shown in the table 4, the decarburization time is 5.0min, the water-hydrogen ratio is dynamically adjusted within the range of 0.30-0.80 according to the production line structure and the target values of carbon and oxygen contents, and decarburized steel is obtained;
then, second cold rolling is carried out, the thickness of a finished product is 0.34mm, and whether recovery annealing and MgO coating oxidation are carried out or not is selected according to the table 4; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 4 Experimental conditions and results for examples 10 to 12 and comparative examples 7 to 8
Figure BDA0003389604890000111
The adhesion measurement was carried out by bending the test piece only around a brass cylinder tower by 180 degrees in steps using the GB/T2522-2017 standard, and then inspecting the cracking and peeling morphology of the coating on the inner surface of the steel sheet and judging the grade according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The structure of the oxide layer of the decarburized steel obtained in example 11 was observed under a scanning electron microscope, and as shown in fig. 1, the oxide layer contained much granular and lamellar oxides, which were more loose than the steel body.
The final magnetic level of the products of examples 10-12 is obviously superior to that of comparative examples 7-8; the surface coatings of the examples 10 to 12 are good and uniform in appearance, and are superior to those of the comparative examples 7 to 8; the adhesion of examples 10 to 12 is superior to that of comparative examples 7 to 8.
In the decarburization annealing, the oxygen content of the decarburized steel is controlled to be within the range calculated by the formula according to the method provided by the invention, the decarburized steel is not subjected to a recovery annealing step after cold rolling and before coating of a magnesium oxide coating, and the magnetic performance and the surface quality of the decarburized steel are still better than those of the decarburized steel in comparative examples 7-8.
Fifth set of examples and comparative examples
Examples 13 to 15 and comparative examples 9 to 10 copper-containing general oriented silicon steel was prepared in the following manner. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 9 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 10 is higher than the control range of the present invention.
Smelting steel by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.054% of C, Si: 3.33%, Mn 0.17%, Als 0.0270%, Cu 0.47%, N0.009%, P: 0.016 percent, 0.008 percent of S and the balance of Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
after the strip steel is subjected to acid pickling and then is subjected to cold rolling to the thickness of 0.55mm, decarburization annealing is carried out at 845 ℃ according to the conditions shown in the table 5, the decarburization time is 3.5min, the water-hydrogen ratio is dynamically adjusted within the range of 0.30-0.80 according to the production line structure and the target values of carbon and oxygen contents, and decarburized steel is obtained;
then, second cold rolling is carried out, the thickness of a finished product is 0.19mm, and whether recovery annealing and MgO coating oxidation are carried out or not is selected according to the table 5; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 5 Experimental conditions and results for examples 13-15 and comparative examples 9-10
Figure BDA0003389604890000131
The adhesion measurement was carried out by bending the test piece only around a brass cylinder tower by 180 degrees in steps using the GB/T2522-2017 standard, and then inspecting the cracking and peeling morphology of the coating on the inner surface of the steel sheet and judging the grade according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The final magnetic level of the products of examples 13-15 is superior to that of comparative examples 9-10; the surface coatings of examples 13-15 have good and uniform appearance, which is superior to that of comparative example 10; examples 13-15 have better adhesion than comparative example 9.
Sixth set of examples and comparative examples
Examples 16 to 18 and comparative examples 11 to 12 copper-containing general oriented silicon steel was prepared in the following manner. In examples 1 to 3, the oxygen content of the decarburized steel was controlled according to the method provided by the present invention. While comparative example 11 has an oxygen content lower than the control range required by the present invention; the oxygen content of comparative example 12 is higher than the control range of the present invention.
Smelting steel by using a converter, refining by using a vacuum furnace, and continuously casting into a slab, wherein the slab comprises the following chemical components in percentage by weight: 0.036% of C, Si: 3.54%, Mn 0.13%, Als 0.0220%, Cu 0.54%, N0.010%, P: 0.012%, S0.005%, and the balance Fe and inevitable impurities;
heating the component plate blank to 1290 ℃, preserving heat for 100min, carrying out hot rolling at the final rolling temperature of 920-;
the strip steel is subjected to acid pickling, then is subjected to cold rolling to the thickness of 0.64mm, and then is subjected to decarburization annealing at 840 ℃ according to the conditions shown in the table 1, wherein the decarburization time is 4.3min, the water-hydrogen ratio is within the range of 0.30-0.80, and the target values of carbon and oxygen contents are dynamically adjusted according to the structure of a production line, so that decarburized steel is obtained;
then, second cold rolling is carried out, the thickness of a finished product is 0.26mm, and whether recovery annealing and MgO coating oxidation are carried out or not is selected according to table 6; then, carrying out high-temperature annealing on the steel strip coil in a mixed atmosphere of nitrogen and hydrogen to form a bottom layer and finish secondary recrystallization to obtain an annealed steel coil;
and (3) coating a tensile stress coating after uncoiling, and carrying out stretching flattening annealing to obtain the copper-containing general oriented silicon steel.
TABLE 6 Experimental conditions and results for examples 16 to 18 and comparative examples 11 to 12
Figure BDA0003389604890000141
The adhesion measurement was carried out by bending the test piece only around a brass cylinder tower by 180 degrees in steps using the GB/T2522-2017 standard, and then inspecting the cracking and peeling morphology of the coating on the inner surface of the steel sheet and judging the grade according to the standard. The judging grades are sorted from superior to inferior, and the sequence is as follows: A. b, C, D, E are provided.
The final magnetic level of the products of examples 16-18 is significantly better than that of comparative examples 11-12; the surface coatings of examples 16 to 18 are good and uniform in appearance, and are superior to those of comparative examples 11 to 12; the adhesion of examples 16-18 was superior to that of comparative example 12.
While the invention has been described with reference to specific embodiments, the scope of the invention is not limited thereto, and those skilled in the art can easily conceive various equivalent modifications or substitutions within the technical scope of the invention. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the copper-containing general oriented silicon steel is characterized by comprising the following steps:
(1) performing decarburization annealing on the steel plate to obtain a decarburized steel, wherein the oxygen content of the decarburized steel is controlled within the range calculated by the following formula:
ψO＝(0.0504×ωSi×H2±0.00005)×106，
wherein psiOThe oxygen content of the decarburized steel is ppm; omegaSiIs the weight percentage content of Si in the steel plate; h is the thickness of the steel plate, and the unit is mm;
(2) cold rolling the decarburized steel, coating a magnesium oxide coating, curling and coiling annealing to obtain an annealed steel coil;
(3) and uncoiling the annealed steel coil, coating a tensile stress coating, and stretching, flattening and annealing to obtain the copper-containing general oriented silicon steel.
2. The method for preparing general oriented silicon steel containing copper according to claim 1, wherein the steel plate in the step (1) comprises the following components in percentage by weight:
0.02wt％≤C≤0.055wt％，2.81wt％≤Si≤3.60wt％，0.10wt％≤Mn≤0.30wt％，0.008wt％≤Als≤0.030wt％，0.4wt％≤Cu≤0.6wt％，0.006wt％≤N≤0.012wt％，P≤0.050wt％，S≤0.015wt％，95.4wt％≤Fe≤96.5wt％。
3. the method for preparing copper-containing generally oriented silicon steel as claimed in claim 1, wherein the thickness of the steel plate in step (1) is 0.5-0.7 mm.
4. The method for preparing general oriented silicon steel containing copper according to claim 1, wherein in the step (1), the oxygen content of the decarburized steel is controlled by adjusting the water-hydrogen ratio in the decarburization annealing process, wherein the water-hydrogen ratio is the partial pressure ratio of water vapor and hydrogen.
5. The method for preparing general oriented silicon steel containing copper according to claim 1, wherein the annealing temperature of the decarburization annealing in the step (1) is 800 to 900 ℃, and the annealing time is 2 to 10 min.
6. The method of claim 1, wherein the decarburized steel obtained in step (1) comprises a steel body and an oxide film on the surface of the steel body, wherein the oxide film comprises SiO2FeO and Fe2SiO4。
7. The method of manufacturing copper-containing generally oriented silicon steel as claimed in claim 6, wherein the oxide film has a thickness of 3 to 10 μm.
8. The method for preparing the copper-containing generally oriented silicon steel as set forth in claim 1, wherein the annealed steel coil obtained in the step (2) includes a steel coil body and a magnesium silicate layer on the surface of the steel coil body.
9. The method of making copper-containing generally oriented silicon steel as set forth in claim 1, further comprising the steps of:
smelting the molten steel to obtain a casting blank;
heating, hot rolling, laminar cooling and curling a casting blank to obtain a steel coil;
and (2) carrying out acid pickling and primary cold rolling on the steel coil to obtain the steel plate used in the step (1).
10. The copper-containing generally oriented silicon steel prepared by the method according to any one of claims 1 to 9.
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