CN112941286A - High-magnetic-induction oriented silicon steel manufacturing method for improving effective nitrogen and bottom layer quality - Google Patents
High-magnetic-induction oriented silicon steel manufacturing method for improving effective nitrogen and bottom layer quality Download PDFInfo
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- CN112941286A CN112941286A CN202110132821.0A CN202110132821A CN112941286A CN 112941286 A CN112941286 A CN 112941286A CN 202110132821 A CN202110132821 A CN 202110132821A CN 112941286 A CN112941286 A CN 112941286A
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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
- 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
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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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
- C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
- C21D3/02—Extraction of non-metals
- C21D3/04—Decarburising
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- 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
- 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
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
A method for manufacturing high magnetic induction oriented silicon steel for improving the quality of effective nitrogen and a bottom layer comprises the following steps: continuously casting into a blank after smelting; heating a casting blank; hot rolling, normalizing and aging cold rolling after acid pickling; decarburizing and annealing in a wet atmosphere; soaking in wet mixed atmosphere; nitriding and annealing under a wet mixed atmosphere; and carrying out the subsequent procedures. Compared with the prior art, the method has the advantages that the nitriding process is reasonably controlled, the ratio of the nitrogen content in the steel plate matrix after nitriding to the total nitrogen content is increased to be more than 80%, no point-shaped crystal exposure is generated, and the bottom layer quality of the finally obtained product is excellent.
Description
Technical Field
The invention relates to a production method of oriented silicon steel, in particular to a manufacturing method of high-magnetic-induction oriented silicon steel for improving effective nitrogen and bottom layer quality.
Background
At present, the manufacturing technology of the nitriding oriented silicon steel after low-temperature slab heating and decarburization annealing becomes the first choice for producing the high-magnetic induction oriented silicon steel. The high magnetic induction oriented silicon steel is heated by the low-temperature plate blank, the heating temperature of the plate blank is 1100-1250 ℃, the problems of high heating temperature, high energy consumption, large burning loss, frequent repair of a heating furnace, high cost and the like of the traditional high-temperature heating at 1350-1400 ℃ are solved, and the hot-rolled coil has no edge crack and high yield; however, this technique is insufficient in that nitriding is performed after decarburization annealing to form a sufficient inhibitor to obtain an inhibition ability.
The low-temperature plate blank is heated to form high-magnetic-induction oriented silicon steel, and after decarburization and annealing, continuous nitriding treatment is carried out by adopting ammonia gas to obtain primary recrystallized grains with proper size and good Gaussian texture so as to obtain secondary recrystallized grains with high orientation degree and excellent magnetic performance. However, the nitriding method requires that the substrate surface after decarburization annealing has a proper oxide layer structure to promote nitriding, improve nitriding efficiency and nitriding depth, and realize excellent magnetic performance and good surface quality which are simultaneously obtained and coordinated and unified. However, in the actual control, the problems of difficult nitriding, uneven distribution of nitrogen on the surface and in the thickness direction of the steel plate and the like not only cause that the formation of the obtained inhibitor in the steel plate is difficult and uneven, further the inhibition capability is insufficient, the secondary recrystallization is incomplete, the magnetic performance of the product is reduced, but also nitrogen is aggregated in a surface oxide layer, cannot completely permeate into the steel plate matrix, and the spot-shaped crystal-exposing defect is generated.
In the prior art, the nitriding condition of the steel plate is described by adopting a total single amount, and the defects exist that the nitrogen amount which actually plays a role in inhibiting the penetration into the steel plate matrix cannot be correctly and objectively reflected, the nitrogen amount which promotes the formation of point-shaped crystal exposure in an oxide layer is included, and even if the effective nitrogen is measured and calculated according to the invention, the effective nitrogen is only below 75 percent, so that not only is the nitrogen resource wasted, but also the point-shaped crystal exposure on the surface quality of the steel plate cannot be well solved.
After retrieval:
the Chinese patent publication No. CN 102758127 discloses a nitriding annealing process, wherein the nitriding temperature is 760-860 ℃, the nitriding time is 20-50 sec, and the oxidation degree P isH2O/PH2：0.045～0.200；NH3: 0.5-4.0%, and the content of the permeated nitrogen is 90-260 ppm. The process can improve the nitriding efficiency, but cannot control the nitrogen amount proportion permeated into the steel plate matrix, and the nitrogen amount which can obtain the inhibitor and has the inhibiting effect is not controllable in the steel plate matrix; in addition, nitriding at 760-860 ℃ easily causes high nitrogen content, more nitrogen is accumulated in an oxide layer, and point-shaped crystal exposure defects are easily generated.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for manufacturing high-magnetic-induction oriented silicon steel, which can improve the ratio of the nitrogen content in a nitrided steel plate matrix to the total nitrogen content by more than 80% through reasonably controlling the nitriding process, so that no point-shaped crystal exposure is generated, and the bottom layer with excellent quality is finally obtained.
The measures for realizing the aim are as follows:
a method for manufacturing high magnetic induction oriented silicon steel for improving the quality of effective nitrogen and a bottom layer comprises the following steps:
1) continuously casting into a blank after conventional smelting;
2) heating the casting blank, and controlling the heating temperature to 1150-1250 DEG C
3) Carrying out conventional hot rolling, normalizing and acid pickling, then carrying out aging cold rolling, and rolling to the thickness of a finished product;
4) performing decarburization annealing in a wet atmosphere at 778-848 ℃ for 30-40 sec,the dew point is 45-59 ℃, the volume percentage of hydrogen in the mixed atmosphere is 38-48%, and the partial pressure ratio P isH2O/PH20.20 to 0.40;
5) soaking in a wet mixed atmosphere at 787-849 ℃ for 10-20 sec at a dew point of 35-59 ℃, wherein the volume percentage of hydrogen in the mixed atmosphere is 38-48%, and the partial pressure ratio P isH2O/PH20.20 to 0.38;
6) nitriding annealing is carried out in a wet mixed atmosphere, the nitriding temperature is controlled to be 860-930 ℃, the nitriding time is 6-70 sec, and the partial pressure ratio is PH2O/PH2: 0.05 to 0.20% NH in a mixed atmosphere35-25% of the total volume;
7) conventionally carrying out the following procedures: coating a magnesia annealing release agent, and finally annealing at high temperature; coating a tension coating, and stretching to be flat.
Preferably: partial pressure ratio P in the atmosphere during soakingH2O/PH20.22 to 0.34.
The effective nitrogen refers to the proportion of the nitrogen content in the nitrided steel plate matrix to the total nitrogen content, namely the effective nitrogen;
the total nitrogen content is the nitrogen content in the steel plate matrix plus the nitrogen content in the oxide layer.
Mechanism and action of the main process of the invention
The invention controls the decarburization annealing temperature to be 778-848 ℃, the decarburization annealing time to be 30-40 sec, the dew point to be 45-59 ℃, the volume percentage of hydrogen in the mixed atmosphere to be 38-48%, and the partial pressure ratio PH2O/PH20.20-0.40, because the rapid decarburization is realized before the oxide layer is formed, and then the oxide layer structure which is beneficial to nitrogen atoms entering the steel plate matrix during nitriding is formed, the nitriding efficiency is improved.
The invention controls the soaking temperature at 787-849 ℃, the soaking time at 10-20 sec, the dew point at 35-59 ℃, the volume percentage of hydrogen in the mixed atmosphere at 38-48 percent, and the partial pressure ratio PH2o/PH20.20 to 0.38; preferably the partial pressure ratio P in the atmosphere during soakingH2O/PH20.22 to 0.34, because the present invention is oriented at high magnetic inductionAfter decarburization annealing and before nitriding of the silicon steel cold-rolled plate, heat preservation is carried out in an atmosphere with a low partial pressure ratio of 0.20-0.38, so that firstly, the surface oxidation layer of the decarburized steel plate is protected from being stable in structure, and the phenomenon that the surface oxidation layer of the steel plate is continuously oxidized to generate excessive FeO and SiO is avoided2The point-like crystal-exposed defect is not generated; secondly, ensure that the oxide layer has a larger proportion of flaky SiO2When the subsequent nitriding is facilitated, nitrogen directly permeates into the steel plate matrix, and is prevented from being accumulated in an oxide layer; and thirdly, the decarburization annealing atmosphere and the nitridation annealing atmosphere are isolated, so that the mutual gas communication of the mixed gas of the decarburization annealing atmosphere and the nitridation annealing atmosphere is avoided, and the functional effect of each furnace section is influenced.
The nitriding temperature is controlled to 860-930 ℃, the nitriding time is controlled to 6-70 sec, and the partial pressure ratio is PH2O/PH2: 0.05 to 0.20% NH in a mixed atmosphere3The nitrogen accounts for 5-25% of the volume percentage, and the nitrogen effectively permeates into the steel plate substrate, so that the stability of the effective nitrogen and the nitrogen can be improved. The effective nitrogen in the steel plate substrate reacts with Als to generate an AlN inhibitor during high-temperature annealing, and the AlN inhibitor plays a full inhibiting role in the steel plate, so that a Gauss texture with high orientation degree and perfect secondary recrystallization grains are formed, and the high-magnetic-induction oriented silicon steel product with excellent magnetic property is obtained. In addition, after the effective nitrogen is increased, the accumulation of nitrogen in an oxide layer on the surface of the steel plate can be reduced, the nitrogen is prevented from escaping in the process of forming a glass film bottom layer by high-temperature annealing to damage the glass film bottom layer, the surface of the obtained steel plate has no point-like crystal exposure defects, and the quality of the bottom layer is good.
Compared with the prior art, the method has the advantages that the nitriding process is reasonably controlled, the ratio of the nitrogen content in the steel plate matrix after nitriding to the total nitrogen content is increased to be more than 80%, no point-shaped crystal exposure is generated, and the bottom layer quality of the finally obtained product is excellent.
Detailed Description
The invention is further described below with reference to specific examples:
table 1 shows the influence of partial pressure ratio before nitriding annealing on magnetic property and bottom layer quality in each example and comparative example of the present invention;
table 2 shows the influence of the nitriding annealing temperature and the amount of hydrogen on the magnetic properties and the quality of the underlayer in each example and comparative example of the present invention.
The production of each embodiment of the invention is carried out according to the following steps:
a method for manufacturing high magnetic induction oriented silicon steel for improving the quality of effective nitrogen and a bottom layer comprises the following steps:
1) continuously casting into a blank after conventional smelting;
2) heating the casting blank, and controlling the heating temperature to 1150-1250 DEG C
3) Carrying out conventional hot rolling, normalizing and acid pickling, then carrying out aging cold rolling, and rolling to the thickness of a finished product; (ii) a
4) Performing decarburization annealing in a wet atmosphere, controlling the decarburization annealing at 778-848 ℃, the decarburization annealing time at 30-40 sec, the dew point at 45-59 ℃, hydrogen accounting for 38-48% by volume in the mixed atmosphere, and the partial pressure ratio PH2O/PH20.20 to 0.40;
5) soaking in a wet mixed atmosphere at 787-849 ℃ for 10-20 sec at a dew point of 35-59 ℃, wherein the volume percentage of hydrogen in the mixed atmosphere is 38-48%, and the partial pressure ratio P isH2O/PH20.20 to 0.38;
6) nitriding annealing is carried out in a wet mixed atmosphere, the nitriding temperature is controlled to be 860-930 ℃, the nitriding time is 6-70 sec, and the partial pressure ratio is PH2O/PH2: 0.05 to 0.20% NH in a mixed atmosphere35-25% of the total volume;
7) conventionally carrying out the following procedures: coating a magnesia annealing release agent, and finally annealing at high temperature; coating a tension coating, and stretching to be flat.
TABLE 1 influence of partial pressure ratio before nitriding annealing on magnetic properties and underlayer quality in examples and comparative examples of the present invention
Description of the drawings: 1. quality of the bottom layer: v represents no dot-shaped crystal defect; x represents a point-like crystal defect;
2. in table 1, the comparative examples were carried out according to the prior art.
As can be seen from the results in Table 1, the partial pressure ratios P in examples 1 to 11 areH2O/PH2: 0.20-0.38 percent, the effective nitrogen after nitriding reaches 80-90 percent, the magnetic performance is better, and the high magnetic induction grain-oriented silicon steel can reach the level of a high magnetic induction grain-oriented silicon steel object (B)8Not less than 1.89T), and the bottom layer has good quality and no point-like crystal-exposing defect. In comparative examples 1 to 2, partial pressure ratio PH2O/PH2: 0.40-0.49, although the effective nitrogen can reach more than 80%, the magnetic performance is better, but the FeO component is increased by peroxidation, the bottom layer quality is poor, and the point-shaped crystal-exposing defect occurs. In comparative examples 3 to 4, partial pressure ratio PH2O/PH2: 0.23 to 0.25, but 38% or less of hydrogen gas, and although the effective nitrogen and magnetic properties were equivalent to those of examples 3 to 6 having the same partial pressure ratio, the quality of the underlayer was deteriorated and the point-like crystal defects were caused.
TABLE 2 influence of nitriding annealing temperature and hydrogen amount on magnetic properties and underlayer quality in examples of the present invention and comparative examples
Description of the drawings: quality of the bottom layer: v represents no dot-shaped crystal defect; and x represents the presence of a point-like crystal defect.
As can be seen from the results in Table 2, examples 1 to 11 had a nitriding temperature of 860 to 930 ℃, a hydrogen gas content of 38 to 48%, and a partial pressure ratio PH2O/PH2: 0.05-0.20 percent, the effective nitrogen after nitriding reaches more than 80 percent, the magnetic performance is better, and the magnetic induction grain-oriented silicon steel can reach the level of a high-magnetic induction grain-oriented silicon steel object (B)8Not less than 1.89T), and the bottom layer has good quality and no point-like crystal-exposing defect. In comparative examples 1 to 2, hydrogen gas was out of 38% to 48%, and although effective nitrogen was more than 81% and magnetic properties were good, excessive oxidation or reduction was observedThe oxide layer structure on the surface of the nitrided steel plate is damaged, the quality of the bottom layer is deteriorated, and the point-like crystal exposure defect appears. In comparative examples 3 to 4, the nitriding temperature was 820 to 840 ℃, and although the effective nitrogen and magnetic properties were equivalent to those of examples 8 to 9 having the same partial pressure ratio, excessive residual nitrogen accumulated in the oxide layer, the quality of the bottom layer was deteriorated, and the point-like crystal defect was caused. In the comparative examples 5-6, the nitriding temperature is 940-950 ℃, although the bottom layer has good quality, the nitriding is difficult, the effective nitrogen is only 57-65%, the magnetic performance index is reduced, and the level of the silicon steel is only up to that of the common oriented silicon steel.
The embodiments of the present invention are merely preferred examples, and are not intended to limit the scope of the claims.
Claims (2)
1. A method for manufacturing high magnetic induction oriented silicon steel for improving the quality of effective nitrogen and a bottom layer comprises the following steps:
1) continuously casting into a blank after conventional smelting;
2) heating the casting blank, and controlling the heating temperature to 1150-1250 DEG C
3) Carrying out conventional hot rolling, normalizing and acid pickling, then carrying out aging cold rolling, and rolling to the thickness of a finished product;
4) performing decarburization annealing in a wet atmosphere, controlling the decarburization annealing at 778-848 ℃, the decarburization annealing time at 30-40 sec, the dew point at 45-59 ℃, hydrogen accounting for 38-48% by volume in the mixed atmosphere, and the partial pressure ratio PH2O/PH20.20 to 0.40;
5) soaking in a wet mixed atmosphere at 787-849 ℃ for 10-20 sec at a dew point of 35-59 ℃, wherein the volume percentage of hydrogen in the mixed atmosphere is 38-48%, and the partial pressure ratio P isH2O/PH20.20 to 0.38;
6) nitriding annealing is carried out in a wet mixed atmosphere, the nitriding temperature is controlled to be 860-930 ℃, the nitriding time is 6-70 sec, and the partial pressure ratio is PH2O/PH2: 0.05 to 0.20% NH in a mixed atmosphere35-25% of the total volume;
7) conventionally carrying out the following procedures: coating a magnesia annealing release agent, and finally annealing at high temperature; coating a tension coating, and stretching to be flat.
2. The method for manufacturing high magnetic induction grain-oriented silicon steel for improving the quality of effective nitrogen and a bottom layer as claimed in claim 1, wherein the method comprises the following steps: partial pressure ratio P in the atmosphere during soakingH2O/PH20.22 to 0.34.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113832322A (en) * | 2021-09-26 | 2021-12-24 | 武汉钢铁有限公司 | High-efficiency decarburization annealing process for high-magnetic-induction oriented silicon steel |
| CN115058682A (en) * | 2021-12-16 | 2022-09-16 | 刘鹏程 | Method for improving nitriding efficiency of high-magnetic induction oriented silicon steel |
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| CN111663081A (en) * | 2020-07-10 | 2020-09-15 | 武汉科技大学 | Niobium-containing oriented silicon steel adopting low-temperature heating plate blank and production method |
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2021
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| CN113832322A (en) * | 2021-09-26 | 2021-12-24 | 武汉钢铁有限公司 | High-efficiency decarburization annealing process for high-magnetic-induction oriented silicon steel |
| CN113832322B (en) * | 2021-09-26 | 2023-04-28 | 武汉钢铁有限公司 | High-efficiency decarburization annealing process for high-magnetic induction oriented silicon steel |
| CN115058682A (en) * | 2021-12-16 | 2022-09-16 | 刘鹏程 | Method for improving nitriding efficiency of high-magnetic induction oriented silicon steel |
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