CN111304583A - Oriented silicon steel nitriding device and nitriding method thereof - Google Patents

Oriented silicon steel nitriding device and nitriding method thereof Download PDF

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Publication number
CN111304583A
CN111304583A CN202010146107.2A CN202010146107A CN111304583A CN 111304583 A CN111304583 A CN 111304583A CN 202010146107 A CN202010146107 A CN 202010146107A CN 111304583 A CN111304583 A CN 111304583A
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nitriding
silicon steel
section
treated
steel
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CN111304583B (en
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裴英豪
朱涛
夏雪兰
胡柯
施立发
沈新玉
杜军
张振海
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Maanshan Iron and Steel Co Ltd
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Maanshan Iron and Steel Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/36Solid 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 using ionised gases, e.g. ionitriding
    • C23C8/38Treatment of ferrous surfaces
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/02Pretreatment of the material to be coated

Abstract

The invention provides a nitriding method of oriented silicon steel applied to the technical field of metallurgy, and also relates to a nitriding device of oriented silicon steel, wherein the nitriding method of oriented silicon steel comprises the following nitriding steps: the front conductive sealing roller (7) is electrified to ionize hydrogen in the cleaning and activating section (2), and the surface of the silicon steel (13) to be treated is cleaned and activated; the silicon steel (13) to be treated enters a nitriding section (3), and ions carry out nitriding treatment on the silicon steel (13) to be treated; the silicon steel (13) to be treated enters the sealing chamber (4), the rear conductive sealing roller (8) in the sealing chamber (4) is electrified to remove an oxide layer on the surface of the silicon steel (13) to be treated, and nitriding treatment is completed.

Description

Oriented silicon steel nitriding device and nitriding method thereof
Technical Field
The invention belongs to the technical field of metallurgy, particularly relates to the technical field of oriented silicon steel production devices and processing methods, and more particularly relates to an oriented silicon steel nitriding method and an oriented silicon steel nitriding device.
Background
The oriented silicon steel (oriented electrical steel strip) is produced by smelting qualified molten steel through a converter and RH, continuously casting the molten steel into thick steel billets, and hot-rolling and reducing the thick steel billets to a thickness suitable for cold rolling through high-temperature heating. The hot rolled steel strip is subjected to normalizing, shot blasting, acid pickling, cold rolling, decarburization annealing, coating, long-period high-temperature annealing and hot stretching flattening to obtain the magnetic material with extremely low longitudinal iron loss and extremely high magnetic induction. Generally, in order to obtain magnetic properties of an oriented electrical steel strip having very low longitudinal core loss and very high magnetic induction, under conditions where chemical composition control is very strict (endogenous inhibitors), an external inhibitor (nitriding) is introduced by heating a hot rolled billet before final high temperature annealing, thereby obtaining a great improvement in longitudinal magnetic properties. Nitriding methods generally include gas methods, solid methods, and ion methods, all of which are long-cycle annealing (over 5 hours) of a workpiece. For electrical steel, in order to simplify the production flow, nitriding is carried out on a continuous annealing production line, the nitriding time of a steel strip is very short (the general thickness is 0.15-0.30 mm), the nitriding quality is difficult to control, and the length of the production line and the control difficulty are increased.
In the oriented electrical steel in the prior art, because the thickness is thinner and thinner due to the quality requirement, the decarburization and the nitridation in the production process are finished in a continuous production line. Because the sections of the continuous production line are connected together, the protective atmosphere for preventing oxidation, the decarburization atmosphere containing moisture and the mixed atmosphere of nitriding, hydrogen, nitrogen and ammonia gas need to be isolated from each other, and the difficulty is very high in order to achieve the function purpose. Furthermore, it is very difficult to maintain the surface activity of the steel strip through a continuous production line. Because the surface cleaning and activation of the steel strip are not considered, the induction period of nitriding is longer, and a series of problems (or reduction of the running speed of the production line, reduction of the yield and the quality) such as unstable product quality or increase of the length of the production line are caused.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method is an improvement aiming at the technical problem that the nitriding incubation period is too long and the nitriding effect is not good due to the fact that the surface inert layer exists in the decarburization and nitriding processes of the oriented silicon steel (oriented electrical steel strip and electrical steel) in a continuous production line, and the nitriding effect of the oriented silicon steel is not good.
To solve the technical problems, the invention adopts the technical scheme that:
the invention relates to a nitriding method of oriented silicon steel, which comprises the following nitriding steps: 1) the front conductive sealing roller guides the silicon steel to be treated to continuously enter the device shell, and the silicon steel passes through the nitriding section and then is guided to leave the device shell through the rear conductive sealing roller; 2) electrifying the front conductive sealing roller to ionize hydrogen in the cleaning and activating section, and cleaning and activating the surface of the silicon steel to be treated; 3) the silicon steel to be treated after cleaning and activation treatment leaves a cleaning and activation section and enters a nitriding section, and active ions formed by decomposing electrified ionized ammonia gas are subjected to nitriding treatment; 4) the silicon steel to be treated after nitriding treatment leaves the nitriding section and enters a sealing chamber, and a rear conductive sealing roller in the sealing chamber is electrified to remove an oxide layer on the surface of the silicon steel to be treated; 5) and removing the oxidation layer on the surface of the shell of the silicon steel output device to be treated to finish nitriding treatment.
When the cleaning and activating section is used for treating the silicon steel to be treated, the vacuum degree of the cleaning and activating section is between 100Pa and 1500 Pa; the hydrogen temperature of the hydrogen pipeline is 400-850 ℃, and the voltage for generating glow is 600-1100V.
When the silicon steel to be treated is subjected to nitriding treatment by active ions formed by electrifying and ionizing ammonia in the nitriding section and decomposing the ionized ammonia, the temperature of the ammonia supplied to the nitriding section by an ammonia supply pipeline is 900-1000 ℃, the nitriding temperature when the nitriding section is subjected to nitriding treatment is 550-580 ℃, the vacuum degree in the nitriding section is 780-820 Pa, and the voltage for generating glow in the nitriding section 3 is 600-1100V.
When the rear conductive sealing roller in the sealing chamber is electrified to remove an oxide layer on the surface of the silicon steel to be treated, the vacuum degree of the sealing chamber is controlled between 780Pa and 820 Pa; the temperature of the hydrogen conveyed by the hydrogen pipeline is 580-620 ℃; the flow rate of hydrogen transported by the hydrogen pipeline is 2 cubic meters per hour, and the voltage for generating glow is between 600V and 1000V.
The method comprises the steps of carrying out vacuum treatment on the continuous casting billet by a converter, an argon station and RH, carrying out soaking, rough rolling and finish rolling, rolling the continuous casting billet into a hot rolled plate, carrying out continuous annealing, slowly cooling to 950-900 ℃, quenching with water, carrying out aging rolling, carrying out decarburization annealing treatment at 830-850 ℃ for 4min to form silicon steel to be treated, and carrying out nitriding treatment in an oriented silicon steel nitriding device.
After the steel strip nitrided by the oriented silicon steel nitriding device is coated with MgO, mixed gas of N2 and H2 is introduced to heat to 1200-1300 ℃, then the temperature is preserved for 20-25 hours in pure H2 atmosphere, the steel strip is cooled to room temperature, and the finished product of the oriented silicon steel is obtained after the steel strip is subjected to stretching and leveling coating treatment.
When the cleaning and activating section treats the silicon steel to be treated, the hydrogen flow conveyed by the front hydrogen pipeline is between 0.1 and 10 cubic meters per hour.
The invention also relates to an oriented silicon steel nitriding device which comprises a device shell, wherein the device shell comprises a cleaning and activating section, a nitriding section and a sealing chamber, the cleaning and activating section is connected with the front hydrogen pipeline, the sealing chamber is communicated with the rear hydrogen pipeline, the nitriding section is communicated with an ammonia gas supply pipeline, a front conductive sealing roller is arranged in the cleaning and activating section, a rear conductive sealing roller is arranged in the sealing chamber, an electrode is arranged in the nitriding section, and the front conductive sealing roller, the rear conductive sealing roller and the electrode are respectively communicated with a power supply.
The silicon steel to be treated is arranged into a structure which can be guided to enter the device shell through the front conductive sealing roller and then to leave the device shell through the rear conductive sealing roller after passing through the nitriding section.
When the silicon steel to be treated is contacted with the front conductive sealing roller, the electrode is arranged to be capable of forming an electric loop structure with ionized ammonia, the silicon steel to be treated, the front conductive sealing roller and the power supply; when the silicon steel to be treated contacts the rear conductive sealing roller, the electrode is set to be a structure which can form an electric loop with ionized ammonia, the silicon steel to be treated, the rear conductive sealing roller and the power supply.
By adopting the technical scheme of the invention, the following beneficial effects can be obtained:
according to the nitriding device and the nitriding method of the oriented silicon steel, the cleaning and activating section is arranged at the inlet position of a device shell of the nitriding device of the electrical steel continuous production line, the nitriding section is arranged in the device shell, and the sealing chamber is arranged at the outlet position of the device shell of the nitriding device. When the steel strip is nitrided, the steel strip firstly enters a cleaning and activating section from an inlet, the cleaning and activating section is in a low-pressure and full-hydrogen state, and high-temperature gas is abnormally glowed (the voltage is high) by applying voltage. This condition causes the hydrogen gas entering the cleaning and activating section to be ionized, and the ionized hydrogen cleans and activates the surface of the electrical steel. The nitriding device on the electrical steel continuous production line is additionally provided with a cleaning and activating section, so that the surface of the passing electrical steel is in a metal state and has no oxide layer or foreign matters. Therefore, when the electrical steel enters the nitriding section, the surface of the electrical steel is completely active (the incubation period is close to zero), and the effect is good and the processing quality of the electrical steel is good after the electrical steel enters the nitriding section. After the electrical steel goes out of the cleaning and activating section, the electrical steel enters the nitriding section, so that the induction period in the nitriding process is reduced to be close to zero, and the electrical steel enters the nitriding section to start the nitriding process, namely decarburization. Therefore, on the premise of keeping the mobility of the electrical steel unchanged, the nitriding time is prolonged, and the nitriding effect is improved. The nitriding section is a nitriding cavity, after the electrical steel enters the nitriding cavity, the atmosphere of the nitriding cavity is ammonia gas heated at high temperature, active ions [ N ] are formed after the ammonia gas heated at high temperature is decomposed, the electrical steel after being cleaned and activated is nitrided, and glow voltage is generated at the same time, so that the rapid nitriding of the strip steel is realized. The performance of the oriented silicon steel product obtained after the process is finished is effectively improved. The invention relates to a nitriding device and a nitriding method of oriented silicon steel, which are used for improving the technical problem that the nitriding induction period is too long and the nitriding is unstable due to the existence of a surface inert layer in the decarburization and nitriding processes of the oriented silicon steel in a continuous production line, so that the nitriding effect of the oriented silicon steel is poor.
Drawings
The contents of the description and the references in the drawings are briefly described as follows:
FIG. 1 is a schematic structural view of an apparatus for nitriding oriented silicon steel according to the present invention;
FIG. 2 is a schematic diagram showing the distribution of nitrogen content in thickness (0.265mm product) of an embodiment of the oriented silicon steel nitriding process of the present invention;
FIG. 3 is a chemical composition diagram (wt%) of one embodiment of the hot rolled oriented silicon steel feedstock according to the present invention;
in the drawings, the reference numbers are respectively: 1. a device housing; 2. a cleaning and activating section; 3. a nitriding section; 4. a sealed chamber; 5. a front hydrogen gas conduit; 6. a post-hydrogen pipeline; 7. a front conductive seal roller; 8. a rear conductive seal roller; 9. an electrode; 10. a power source; 11. an ammonia gas supply line; 12. a reversing roller; 13. silicon steel to be treated; 14. a front non-contact seal roller; 15. a rear non-contact seal roller; 16. a front sealed cavity; 17. the rear sealing cavity; 18. and nitriding the cavity.
Detailed Description
The following detailed description of the embodiments of the present invention, such as the shapes and structures of the components, the mutual positions and connection relations among the components, the functions and operation principles of the components, will be made by referring to the accompanying drawings and the description of the embodiments:
as shown in the attached drawings 1-3, the invention relates to a nitriding method of oriented silicon steel, which comprises the following nitriding steps: 1) the front conductive seal roller 7 guides the silicon steel 13 to be treated to continuously enter the device shell 1, and the silicon steel is guided to leave the device shell 1 through the rear conductive seal roller 8 after passing through the nitriding section 3; 2) the front conductive sealing roller 7 is electrified to ionize hydrogen in the cleaning and activating section 2, and the surface of the silicon steel 13 to be treated is cleaned and activated; 3) the silicon steel 13 to be treated after cleaning and activation treatment leaves the cleaning and activation section 2 and enters the nitriding section 3, and active ions formed by decomposing energized ionized ammonia gas are subjected to nitriding treatment on the silicon steel 13 to be treated; 4) the silicon steel 13 to be treated after nitriding treatment leaves the nitriding section 3 and enters the sealing chamber 4, and the rear conductive sealing roller 8 in the sealing chamber 4 is electrified to remove an oxide layer on the surface of the silicon steel 13 to be treated; 5) and removing the oxidized layer on the surface of the silicon steel 13 to be processed, and outputting the silicon steel 13 to the shell 1 of the device to finish nitriding treatment. In the steps, a cleaning and activating section 2 is arranged at the inlet position of a device shell 1 of a nitriding device of an electrical steel continuous production line, the nitriding section 2 is arranged in the device shell 1, and a sealing chamber is arranged at the outlet position of the device shell 1 of the nitriding device. When the steel strip is nitrided, the steel strip firstly enters the cleaning and activating section 2 from an inlet, the cleaning and activating section is in a low-pressure and full-hydrogen state, and high-temperature gas is abnormally glowed (the voltage is high) by applying voltage. This condition causes the hydrogen gas entering the cleaning and activating section to be ionized, and the ionized hydrogen cleans and activates the surface of the electrical steel. The nitriding device on the electrical steel continuous production line is additionally provided with a cleaning and activating section, so that the surface of the passing electrical steel is in a metal state and has no oxide layer or foreign matters. Therefore, when the electrical steel enters the nitriding section, the surface of the electrical steel is completely active (the incubation period is close to zero), and the effect is good and the processing quality of the electrical steel is good after the electrical steel enters the nitriding section. After the electrical steel goes out of the cleaning and activating section, the electrical steel enters the nitriding section, so that the induction period in the nitriding (decarburization) process is reduced to be close to zero, and the electrical steel enters the nitriding section to start the nitriding process, namely decarburization. Therefore, on the premise of keeping the mobility of the electrical steel unchanged, the nitriding time is prolonged, and the nitriding effect is improved. The nitriding section is a nitriding cavity, after the electrical steel enters the nitriding cavity, the atmosphere of the nitriding cavity is ammonia gas which is heated at high temperature, active ions [ N ] are formed after the ammonia gas which is heated at high temperature is decomposed, the electrical steel (strip steel) which is cleaned and activated is nitrided, glow voltage is generated at the same time, the rapid nitriding of the strip steel is realized, and the distribution condition of the nitrogen content of the electrical steel along the thickness direction after the nitriding is finished is shown in figure 2. The performance of the oriented silicon steel product obtained after the process is finished is effectively improved. The method for nitriding the oriented silicon steel is improved aiming at the technical problem that the nitriding induction period is too long and the nitriding effect is not good due to the fact that the surface inert layer exists in the process of decarburization and nitriding of the oriented silicon steel in a continuous production line, and the surface of the oriented silicon steel before nitriding (decarburization) is cleaned and activated, so that the surface of a steel strip is clean and active, the nitriding process of ammonia gas is rapid and uniform, and the processing quality of the oriented silicon steel is high.
The nitriding method of the oriented silicon steel has the following technical effects: 1) the induction period of the nitriding (decarburizing) process is reduced to nearly zero, so that the steel strip enters the nitriding process and starts to be decarburized (enters the decarburizing section). 2) The nitriding process can be controlled, and the nitriding is uniform. 3) In the production line with the same function and size, due to the arrangement of the cleaning and activating section, the nitriding section and the sealing chamber, the running speed of the nitriding production line is increased by 2-4 times (ion nitriding) or 4-8 times (gas nitriding), and the yield of electrical steel is increased by 2-4 times. 4) Because the nitriding process can be controlled, the nitriding is uniform, and the magnetic property of the electrical steel product is improved and stabilized. 5) The production cost of the electrical steel is reduced.
When the cleaning and activating section 2 is used for treating the silicon steel 13 to be treated, the vacuum degree of the cleaning and activating section 2 is between 100Pa and 1500 Pa; the hydrogen temperature of the hydrogen pipeline 5 is 400-850 ℃, and the voltage for generating glow is 600-1100V. By means of the structure, the process parameters of the electrical steel during cleaning and activating treatment of the cleaning and activating section 2 are set, so that the cleaning and activating of the surface of the electrical steel can be realized within the shortest time, the nitriding of the electrical steel can be efficiently and reliably realized when the electrical steel passes through the nitriding section, and the efficiency and the quality are improved.
When the silicon steel 13 to be treated is subjected to nitriding treatment by active ions formed by decomposing the ionized ammonia gas in the nitriding section 3 by electrifying, the temperature of the ammonia gas supplied to the nitriding section 3 by the ammonia gas supply pipeline 11 is 900-1000 ℃, the nitriding temperature when the nitriding section 3 is subjected to nitriding treatment is 550-580 ℃, the vacuum degree in the nitriding section 3 is 780-820 Pa, and the voltage for generating glow in the nitriding section 3 is 600-1100V. According to the process parameters, the nitriding section is of a cavity structure, so that the electrical steel is always in a nitriding state when passing through the nitriding section, the nitriding efficiency and the nitriding quality of the electrical steel are effectively improved, and the overall performance of the electrical steel is improved.
When the rear conductive sealing roller 8 in the sealing chamber 4 is electrified to remove an oxide layer on the surface of the silicon steel 13 to be treated, the vacuum degree of the sealing chamber 4 is controlled between 780Pa and 820 Pa; the temperature of the hydrogen conveyed by the hydrogen pipeline 6 is 580-620 ℃; the hydrogen pipeline 5 delivers hydrogen with the flow rate of 2 cubic meters per hour, and the voltage for generating glow is between 600V and 1000V.
The method comprises the steps of carrying out vacuum treatment on the continuous casting billet by a converter, an argon station and RH, carrying out soaking, rough rolling and finish rolling, rolling the continuous casting billet into a hot rolled plate, carrying out continuous annealing, slowly cooling to 950-900 ℃, quenching with water, carrying out aging rolling, carrying out decarburization annealing treatment at 830-850 ℃ for 4min to form silicon steel to be treated, and carrying out nitriding treatment in an oriented silicon steel nitriding device. After the steel strip nitrided by the oriented silicon steel nitriding device is coated with MgO, mixed gas of N2 and H2 is introduced and heated to 1200-1300 ℃, then the temperature is preserved for 20-25 hours in pure H2 atmosphere, then the steel strip is cooled to room temperature, and the finished product of the oriented silicon steel is obtained after the steel strip is subjected to stretching and leveling coating treatment.
When the cleaning and activating section 2 is used for treating the silicon steel 13 to be treated, the hydrogen flow rate conveyed by the front hydrogen pipeline 5 is between 0.1 cubic meter per hour and 10 cubic meters per hour.
The invention also relates to an oriented silicon steel nitriding device which is simple in structure, aims at solving the technical problems that the nitriding incubation period is too long and the nitriding is unstable due to the existence of a surface inert layer in the decarburization and nitriding processes of the oriented silicon steel (oriented electrical steel strips and electrical steel) in a continuous production line, so that the nitriding effect of the oriented silicon steel is poor, and cleans and activates the surface of the oriented silicon steel before nitriding (decarburization) so that the surface of the steel strip is clean and active, the nitriding process of ammonia gas is rapid and uniform, and the processing quality of the oriented silicon steel is high.
The oriented silicon steel nitriding device comprises a device shell 1, wherein the device shell 1 comprises a cleaning and activating section 2, a nitriding section 3 and a sealing chamber 4, the cleaning and activating section 2 is connected with a front hydrogen pipeline 5, the sealing chamber 4 is communicated with a rear hydrogen pipeline 6, the nitriding section 3 is communicated with an ammonia gas supply pipeline 11, a front conductive sealing roller 7 is arranged in the cleaning and activating section 2, a rear conductive sealing roller 8 is arranged in the sealing chamber 4, an electrode 9 is arranged in the nitriding section 3, and the front conductive sealing roller 7, the rear conductive sealing roller 8 and the electrode 9 are respectively communicated with a power supply 10. According to the structure, the front conductive sealing roller 7 and the rear conductive sealing roller 8 are used for conveying the silicon steel to be treated, so that the silicon steel to be treated can be subjected to nitriding treatment continuously through the nitriding device. When the steel strip is nitrided, the steel strip firstly enters the cleaning and activating section 2 from an inlet, the cleaning and activating section is in a low-pressure and full-hydrogen state, and high-temperature gas is abnormally glowed (the voltage is high) by applying voltage. This condition causes the hydrogen gas entering the cleaning and activating section to be ionized, and the ionized hydrogen cleans and activates the surface of the electrical steel. The nitriding device on the electrical steel continuous production line is additionally provided with a cleaning and activating section, so that the surface of the passing electrical steel is in a metal state and has no oxide layer or foreign matters. Therefore, when the electrical steel enters the nitriding section, the surface of the electrical steel is completely active (the incubation period is close to zero), and the effect is good and the processing quality of the electrical steel is good after the electrical steel enters the nitriding section. After the electrical steel goes out of the cleaning and activating section, the electrical steel enters the nitriding section, so that the induction period in the nitriding (decarburization) process is reduced to be close to zero, and the electrical steel enters the nitriding section to start the nitriding process, namely decarburization. Therefore, on the premise of keeping the mobility of the electrical steel unchanged, the nitriding time is prolonged, and the nitriding effect is improved. The nitriding section is a nitriding cavity, after the electrical steel enters the nitriding cavity, the atmosphere of the nitriding cavity is ammonia gas which is heated at high temperature, active ions [ N ] are formed after the ammonia gas which is heated at high temperature is decomposed, the electrical steel (strip steel) which is cleaned and activated is nitrided, glow voltage is generated at the same time, the rapid nitriding of the strip steel is realized, and the distribution condition of the nitrogen content of the electrical steel along the thickness direction after the nitriding is finished is shown in figure 2. The performance of the oriented silicon steel product obtained after the process is finished is effectively improved.
The device is characterized in that a plurality of reversing rollers 12 are arranged in the device shell 1, and the silicon steel 13 to be processed is set to be of a structure which can be guided to enter the device shell 1 through the front conductive sealing roller 7 and then be guided to leave the device shell 1 through the rear conductive sealing roller 8 after passing through the nitriding section 3. With the structure, the direction of the silicon steel to be processed in the device shell 1 can be changed by arranging the reversing rollers 12. The reversing rollers 12 are three, the first reversing roller enables the silicon steel to be treated to turn from the inlet to enter the cleaning and activating section 2, the second reversing roller enables the silicon steel to be treated to bypass the nitriding cavity, and the third reversing roller enables the silicon steel to be treated to pass through the sealing chamber from the nitriding cavity 18 to the outlet. Thus, the process that the steel strip passes through the nitriding cavity of the nitriding section is the nitriding process. The steel belt can start nitriding when entering the nitriding section, and the nitriding effect and the nitriding efficiency are effectively improved.
When the silicon steel 13 to be treated is contacted with the front conductive sealing roller 7, the electrode 9 is set to be in a structure which can form an electric loop with ionized ammonia, the silicon steel 13 to be treated, the front conductive sealing roller 7 and the power supply 10; when the silicon steel 13 to be processed contacts the rear conductive sealing roller 8, the electrode 9 is set to be a structure capable of forming an electric loop with ionized ammonia, the silicon steel 13 to be processed, the rear conductive sealing roller 8 and the power supply 9. Above-mentioned structure, preceding electrically conductive seal roller 7 is behind the circular telegram formation electric circuit for the electric steel through clearance and activation section 2 realizes clearance and activation, and electrically conductive seal roller 8 behind the electrically conductive electric circuit that forms of back of seal chamber 4 makes the electric steel surface that passes through be metal state, no oxide layer and foreign matter behind the circular telegram formation electric circuit. Therefore, the overall performance of the electrical steel is effectively improved.
In the structure of the invention, a front non-contact sealing roller 14 is arranged in the cleaning and activating section 2, and a rear non-contact sealing roller 15 is arranged in the sealing chamber 4. A closed front sealing cavity 16 is formed between the front conductive sealing roller 7 and the front non-contact sealing roller 14, so that the vacuum degree of the cleaning and activating section 2 is ensured, and when the oriented silicon steel passes through the front sealing cavity 16, the hydrogen input into the front sealing cavity 16 can be conveniently cleaned and activated. And a sealed rear sealing cavity 17 is formed between the conductive sealing roller 8 and the rear non-contact sealing roller 15, so that the vacuum degree of the sealing chamber is ensured to be kept, and the oxide layer on the surface of the electrical steel can be removed through hydrogen input into the front sealing cavity when the oriented silicon steel passes through the rear sealing cavity. Thus, the overall performance of the electrical steel is improved.
According to the nitriding device and the nitriding method of the oriented silicon steel, the cleaning and activating section is arranged at the inlet position of a device shell of the nitriding device of the electrical steel continuous production line, the nitriding section is arranged in the device shell, and the sealing chamber is arranged at the outlet position of the device shell of the nitriding device. When the steel strip is nitrided, the steel strip firstly enters a cleaning and activating section from an inlet, the cleaning and activating section is in a low-pressure and full-hydrogen state, and high-temperature gas is abnormally glowed (the voltage is high) by applying voltage. This condition causes the hydrogen gas entering the cleaning and activating section to be ionized, and the ionized hydrogen cleans and activates the surface of the electrical steel. The nitriding device on the electrical steel continuous production line is additionally provided with a cleaning and activating section, so that the surface of the passing electrical steel is in a metal state and has no oxide layer or foreign matters. Therefore, when the electrical steel enters the nitriding section, the surface of the electrical steel is completely active (the incubation period is close to zero), and the effect is good and the processing quality of the electrical steel is good after the electrical steel enters the nitriding section. After the electrical steel goes out of the cleaning and activating section, the electrical steel enters the nitriding section, so that the induction period in the nitriding process is reduced to be close to zero, and the electrical steel enters the nitriding section to start the nitriding process, namely decarburization. Therefore, on the premise of keeping the mobility of the electrical steel unchanged, the nitriding time is prolonged, and the nitriding effect is improved. The nitriding section is a nitriding cavity, after the electrical steel enters the nitriding cavity, the atmosphere of the nitriding cavity is ammonia gas heated at high temperature, active ions [ N ] are formed after the ammonia gas heated at high temperature is decomposed, the electrical steel after being cleaned and activated is nitrided, and glow voltage is generated at the same time, so that the rapid nitriding of the strip steel is realized. The performance of the oriented silicon steel product obtained after the process is finished is effectively improved. The invention relates to a nitriding device and a nitriding method of oriented silicon steel, which are used for improving the technical problem that the nitriding induction period is too long and the nitriding is unstable due to the existence of a surface inert layer in the decarburization and nitriding processes of the oriented silicon steel in a continuous production line, so that the nitriding effect of the oriented silicon steel is poor.
The present invention has been described in connection with the accompanying drawings, and it is to be understood that the invention is not limited to the specific embodiments disclosed, but is intended to cover various modifications, changes and equivalents of the embodiments of the invention, and its application to other applications without departing from the spirit and scope of the invention.

Claims (10)

1. A nitriding method of oriented silicon steel is characterized by comprising the following steps: the nitriding method of the oriented silicon steel nitriding method comprises the following nitriding steps: 1) the front conductive sealing roller (7) guides the silicon steel (13) to be treated to continuously enter the device shell (1), and the silicon steel is guided to leave the device shell (1) through the rear conductive sealing roller (8) after passing through the nitriding section (3); 2) the front conductive sealing roller (7) is electrified to ionize hydrogen in the cleaning and activating section (2), and the surface of the silicon steel (13) to be treated is cleaned and activated; 3) the silicon steel (13) to be treated after cleaning and activation treatment leaves the cleaning and activation section (2) and enters the nitriding section (3), and active ions formed by decomposing electrified ionized ammonia gas are subjected to nitriding treatment on the silicon steel (13) to be treated; 4) the silicon steel (13) to be treated after nitriding treatment leaves the nitriding section (3) and enters a sealing chamber (4), and a rear conductive sealing roller (8) in the sealing chamber (4) is electrified to remove an oxide layer on the surface of the silicon steel (13) to be treated; 5) and removing the oxidized layer on the surface of the silicon steel (13) to be treated, and outputting the device shell (1) to finish nitriding treatment.
2. The method of nitriding oriented silicon steel of claim 1, wherein: when the cleaning and activating section (2) is used for treating the silicon steel (13) to be treated, the vacuum degree of the cleaning and activating section (2) is between 100Pa and 1500 Pa; the hydrogen temperature conveyed by the front hydrogen pipeline (5) is between 400 and 850 ℃, and the voltage for generating glow is between 600 and 1100V.
3. The method for nitriding oriented silicon steel according to claim 1 or 2, characterized in that: when the silicon steel (13) to be treated is subjected to nitriding treatment by active ions formed by electrifying and ionizing ammonia in the nitriding section (3) and decomposing the ionized ammonia, the temperature of the ammonia supplied to the nitriding section (3) by the ammonia supply pipeline (11) is 900-1000 ℃, the nitriding temperature when the nitriding section (3) is subjected to nitriding treatment is 550-580 ℃, the vacuum degree in the nitriding section (3) is 780-820 Pa, and the voltage for generating glow in the nitriding section (3) is 600-1100V.
4. The method for nitriding oriented silicon steel according to claim 1 or 2, characterized in that: when the rear conductive sealing roller (8) in the sealing chamber (4) is electrified to remove an oxide layer on the surface of the silicon steel (13) to be treated, the vacuum degree of the sealing chamber (4) is controlled between 780Pa and 820 Pa; the temperature of the hydrogen conveyed by the hydrogen pipeline (6) is 580-620 ℃; the hydrogen pipeline (5) is used for delivering hydrogen with the flow rate of 2 cubic meters per hour, and the voltage for generating glow is between 600V and 1000V.
5. The method for nitriding oriented silicon steel according to claim 1 or 2, characterized in that: the method comprises the steps of carrying out vacuum treatment on the continuous casting billet by a converter, an argon station and RH, carrying out soaking, rough rolling and finish rolling, rolling the continuous casting billet into a hot rolled plate, carrying out continuous annealing, slowly cooling to 950-900 ℃, quenching with water, carrying out aging rolling, carrying out decarburization annealing treatment at 830-850 ℃ for 4min to form silicon steel to be treated, and carrying out nitriding treatment in an oriented silicon steel nitriding device.
6. The method for nitriding oriented silicon steel according to claim 1 or 2, characterized in that: after the steel strip nitrided by the oriented silicon steel nitriding device is coated with MgO, mixed gas of N2 and H2 is introduced and heated to 1200-1300 ℃, then the temperature is preserved for 20-25 hours in pure H2 atmosphere, then the steel strip is cooled to room temperature, and the finished product of the oriented silicon steel is obtained after the steel strip is subjected to stretching and leveling coating treatment.
7. The method of nitriding oriented silicon steel of claim 2, wherein: when the cleaning and activating section (2) treats the silicon steel (13), the hydrogen flow rate conveyed by the front hydrogen pipeline (5) is between 0.1 cubic meter per hour and 10 cubic meters per hour.
8. The utility model provides an orientation silicon steel nitriding device which characterized in that: including device casing (1), device casing (1) is including clearance and activation section (2), nitriding section (3), seal chamber (4), clearance and activation section (2) be connected with preceding hydrogen pipeline (5), seal chamber (4) and back hydrogen pipeline (6) intercommunication, nitriding section (3) and ammonia supply pipeline (11) intercommunication set up preceding electrically conductive seal roller (7) in clearance and activation section (2), set up back electrically conductive seal roller (8) in seal chamber (4), nitriding section (3) in set up electrode (9), preceding electrically conductive seal roller (7), back electrically conductive seal roller (8), electrode (9) communicate with power (10) respectively.
9. The apparatus of claim 8, wherein: the silicon steel processing device is characterized in that a plurality of reversing rollers (12) are arranged in the device shell (1), and the silicon steel (13) to be processed is arranged into a structure which can be guided to enter the device shell (1) through the front conductive sealing roller (7) and then guided to leave the device shell (1) through the rear conductive sealing roller (8) after passing through the nitriding section (3).
10. The apparatus of claim 8 or 9, wherein: when the silicon steel (13) to be treated is contacted with the front conductive sealing roller (7), the electrode (9) is set to be a structure which can form an electric loop with ionized ammonia, the silicon steel (13) to be treated, the front conductive sealing roller (7) and the power supply (10); when treating silicon steel (13) and electrically conductive seal roller (8) contact in back, electrode (9) set up to form the structure of electric loop with ionized ammonia, treating silicon steel (13), electrically conductive seal roller (8) in back, power (9).
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TW201531595A (en) * 2014-02-11 2015-08-16 Univ Nat Taiwan Method for treating stainless steel surface and stainless steel treating system
CN105154816A (en) * 2015-09-22 2015-12-16 华南理工大学 Arc plasma assisted low-pressure nitriding method under different atmospheres
CN105839046A (en) * 2016-05-06 2016-08-10 华南理工大学 Method for conducting low-temperature efficient rapid ion nitriding on surface of steel workpiece

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CN101294268A (en) * 2007-04-24 2008-10-29 宝山钢铁股份有限公司 Nitrogen case hardening method of orientation silicon steel
US20120222777A1 (en) * 2009-11-25 2012-09-06 Tata Steel Ijmuiden B.V. Process to manufacture grain-oriented electrical steel strip and grain-oriented electrical steel produced thereby
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Publication number Priority date Publication date Assignee Title
CN115074655A (en) * 2022-06-13 2022-09-20 无锡晶龙华特电工有限公司 Oriented silicon steel nitriding method based on nitriding device
CN115074655B (en) * 2022-06-13 2023-08-22 无锡晶龙华特电工有限公司 Oriented silicon steel nitriding method based on nitriding device

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