CN115287419A - Annealing and pickling process method of high-temperature-resistant austenitic stainless steel cold-rolled strip steel - Google Patents
Annealing and pickling process method of high-temperature-resistant austenitic stainless steel cold-rolled strip steel Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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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
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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
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- C21D6/005—Heat treatment of ferrous alloys containing Mn
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- C21D6/00—Heat treatment of ferrous alloys
- C21D6/008—Heat treatment of ferrous alloys containing Si
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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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips of ferrous alloys
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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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
- C21D8/0236—Cold rolling
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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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
- C21D8/0273—Final recrystallisation annealing
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/34—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of silicon
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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
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/40—Ferrous alloys, e.g. steel alloys containing chromium with nickel
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/08—Iron or steel
- C23G1/086—Iron or steel solutions containing HF
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G3/00—Apparatus for cleaning or pickling metallic material
- C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
- C25F1/02—Pickling; Descaling
- C25F1/04—Pickling; Descaling in solution
- C25F1/06—Iron or steel
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Abstract
The invention relates to the technical field of special steel material production, in particular to an annealing and pickling process method of high-temperature-resistant austenitic stainless steel cold-rolled strip steel, which comprises the following steps: the method comprises the following steps: cold rolling and annealing; step two: electrolytic pickling; step three: and (5) mixed acid pickling. The invention develops a high-Si-content high-temperature-resistant austenitic stainless steel cold-rolled strip steel annealing and pickling process, which adopts a lower temperature and short-time annealing system to ensure that the oxide skin of a steel plate has moderate thickness and uniform components, and then is matched with a proper electrolytic pickling process to ensure that the surface of the high-temperature-resistant austenitic stainless steel cold-rolled plate with the Si content of more than 1.5 percent has uniform color and no iron-phosphorus roughness defect, the product has better oxidation resistance and corrosion resistance, and the surface roughness of the steel plate with the thickness of less than 2.0mm is less than or equal to 0.30 mu m.
Description
Technical Field
The invention relates to the technical field of special steel material production, in particular to an annealing and pickling process method of high-temperature-resistant austenitic stainless steel cold-rolled strip steel.
Background
The Si content in the stainless steel is usually about 0.6%, and the addition of a certain amount of Si element into the stainless steel can remarkably improve the high-temperature resistance, high-concentration nitric acid and sulfuric acid corrosion resistance of the stainless steel, and is related to the Si element forming an Si-rich oxide protective film on the surface of the stainless steel. Si element has stronger affinity with oxygen, and can be selectively oxidized at high temperature, and SiO which is dispersed and distributed is formed between the substrate and the oxide skin of the substrate 2 The particle layer and Si-O are combined by strong covalent bonds, the structure is very stable, on one hand, the compactness of oxide skin is increased, and on the other hand, siO 2 The copper-based nickel-based copper alloy can permeate into a crystal boundary to play a role of pinning an oxide film, so that the adhesion of the oxide film is enhanced, and the characteristics are favorable for oxidation resistance, but also increase the difficulty of acid washing.
The high-temperature resistant austenitic stainless steel is a product which takes Cr, ni and Si as main oxidation resistant elements, the design of 1.5-2.0 percent of Si content realizes that the oxidation resistant performance is equivalent to that of 310S stainless steel with higher Cr and Ni content, and the maximum service temperature can reach 1095 ℃.
The high Si content leads to complex surface oxide scale components after the heat treatment of the steel plate, increases the difficulty of pickling the surface of the steel plate, and leads to incomplete removal of the surface oxide scale of the steel plate and rough surface due to improper heat treatment and pickling processes, thereby influencing the service performance of the steel plate.
Therefore, the invention develops a pickling method for a high-temperature resistant austenitic stainless steel cold-rolled sheet with high Si content and higher Cr and Ni content, so that oxide skin generated after annealing of the steel sheet is quickly and uniformly cleaned by acid, and a cold-rolled strip steel product with a high-brightness surface is obtained.
Disclosure of Invention
The invention aims to solve the problems and provides an annealing and pickling process method of high-temperature resistant austenitic stainless steel cold-rolled strip steel.
The purpose of the invention is realized by the following steps: a annealing and pickling process method of high-temperature resistant austenitic stainless steel cold-rolled strip steel comprises the following steps: the method comprises the following steps: cold rolling and annealing: the annealing temperature is 1120 +/-10 ℃, the effective length of an annealing hearth in a high-temperature section is 60m, and the strip steel threading speed is calculated according to the effective length of the hearth in the high-temperature section and the thickness of the strip steel according to the principle that the heat of a steel plate in the high-temperature section is preserved for 1-1.5 min/mm; step two: electrolytic pickling: first stage acid pickling Medium Na 2 SO 4 (ii) a Specific gravity of 1.20-1.30g/cm 3 The electrolysis temperature is 75 +/-5 ℃, and the electrolysis current is 2000-7000A; second stage acid cleaning medium HNO 3 The acid concentration is 70-140g/L, the temperature is 50 +/-5 ℃, and the electrolytic current is 2000-5000A; step three: mixed acid pickling: HF and HNO 3 Mixed, HNO 3 Concentration 120-250g/L, HF concentration 15-30g/L, fe n+ Less than or equal to 40g/L, and the temperature of mixed acid is 45 to 55 ℃.
And calculating the threading speed of the strip steel according to the principle that the heat of the steel plate is kept for 1 to 1.5min/mm in the high-temperature section, specifically the thickness of the high-temperature resistant austenitic stainless steel cold-rolled plate is 1 to 2mm according to the effective length of the hearth in the high-temperature section and the thickness of the strip steel, so that the heat-preserving time is 1 to 3min in the high-temperature section, and the threading speed is 20 to 60m/min.
The invention has the beneficial effects that: the invention develops a high-Si-content high-temperature-resistant austenitic stainless steel cold-rolled strip steel annealing and pickling process, which adopts a lower temperature and short-time annealing system to ensure that the oxide skin of a steel plate has moderate thickness and uniform components, and then is matched with a proper electrolytic pickling process to ensure that the surface of the high-temperature-resistant austenitic stainless steel cold-rolled plate with the Si content of more than 1.5 percent has uniform color and no iron-phosphorus roughness defect, the product has better oxidation resistance and corrosion resistance, and the surface roughness of the steel plate with the thickness of less than 2.0mm is less than or equal to 0.30 mu m.
Detailed Description
An annealing and pickling process method of high-temperature resistant austenitic stainless steel cold-rolled strip steel, which mainly comprises the austenitic stainless steel cold-rolled strip steel with the Si content more than or equal to 1.5 percent, is produced according to the following steps: (1) cold rolling and annealing: the annealing temperature is 1120 +/-10 ℃, and the heat preservation of the steel plate in the high-temperature section is less than or equal to 1.5min/mm according to the principle that the hearth is arranged in the high-temperature sectionCalculating the threading speed of the strip steel by the effective length and the thickness of the strip steel. (2) Electrolytic pickling: first stage acid pickling Medium Na 2 SO 4 (ii) a Specific gravity of 1.20-1.30g/cm 3 The temperature is 75 +/-5 ℃, and the electrolytic current is 2000-7000A; second stage pickling medium HNO 3 The acid concentration is 70-140g/L, the temperature is 50 +/-5 ℃, and the electrolytic current is 2000-5000A. (3) Mixed acid pickling: HF and HNO 3 Mixed, HNO 3 Concentration 120-250g/L, HF concentration 15-30g/L, fe n+ Less than or equal to 40g/L and the temperature of mixed acid is 45 +/-5 ℃.
The technical idea of the invention is as follows:
1. formulation of annealing and pickling process
In order to obtain thinner and more uniform steel plate surface oxide skin, the annealing temperature and the annealing time of the steel plate are controlled according to the lower limit on the premise of ensuring the complete recovery of the steel plate structure.
2. Structural analysis of oxide skin
In the oxide scale, the outer layer is Fe 3 O 4 、Fe 2 O 3 And Cr 2 O 3 The mixed layer of (2) is relatively insoluble in an acid solution, and silicon oxide SiO in oxide scale 2 Can only react with hydrofluoric acid in acid, and needs to be avoided due to SiO 2 The problem of grain boundary over-pickling caused by the nail rolling effect is solved, so that the proper acid solution concentration needs to be designed to achieve the ideal pickling effect.
3. Formulation of pickling Process
(1) Electrolytic pickling process
During electrolytic pickling, cr is mainly generated 2 O 3 The electrolytic reaction of (1) and the function of the sodium sulfate in the electrolytic pickling mainly enhances the conductivity of the solution, so that the electrolytic pickling can be better carried out, and the specific gravity is 1.20 to 1.30g/cm 3 Slightly higher than the concentration of the conventional stainless steel.
The temperature and the electrolytic current of the electrolyte have obvious influence on electrolytic pickling, the two parameters are researched, and laboratory simulation pickling parameters are designed as follows:
temperature of the electrolyte: 50. 60, 70, 80 and 90 ℃.
Electrolytic current: 1000. 2000, 4000, 7000A.
Test results show that the higher the temperature of the electrolyte, the shorter the required electrolysis time, and at the temperature of 50 ℃, the time required for electrolysis is twice that of 70 ℃, so that the production requirement cannot be met, and therefore, the temperature of the electrolyte is selected from 70 ℃ to 90 ℃. The parameters selected for the electrolytic current were all effective in removing surface scale, but experiments found that when the area of the sample was increased, the sample surface was likely to exhibit non-uniformity at low current (1000A), and the electrolytic current was selected from 2000 to 7000A because the other electrolytic currents did not greatly affect the electrolytic time.
(2) Mixed acid pickling
The mixed acid pickling is mainly used for removing oxide scales and silicon dioxide on the surface of the steel plate, the concentration of nitric acid pickling is selected to be 120-250g/L, the pickling temperature is 45-55 ℃, the concentration is too low to dissolve residual oxide scales, and the concentration is too high to passivate the surface of the stainless steel, so that the pickling is not facilitated. The acid pickling effect is best when the concentration of hydrofluoric acid is 15 to 30g/L, and SiO can be effectively removed 2 And can avoid local corrosion.
In addition, the concentration of iron salt in the pickling solution has a certain influence on the pickling rate and quality because, in the pickling process, as the iron salt in the solution increases, when the iron salt approaches or exceeds the solubility, hydrate of ferrous salt is precipitated on the surface of the steel plate, so that the contact of the acid solution and the steel plate is prevented, the pickling speed and uniformity are reduced, and therefore, fe is used for producing the steel plate 2+ The concentration of (2) is controlled to be lower than 40g/L.
The following examples are given to illustrate specific embodiments of the present invention, but the present invention is not limited to the following examples.
Example one
The high-Si-content austenitic heat-resistant steel comprises the following components: c: 0.040-0.070, si:1.50 to 2.00, mn:0.80 to 1.20, P: less than or equal to 0.030, S: less than or equal to 0.003, cr:19.20 to 20.00, ni:12.10 to 12.50, N: 0.03-0.06, and the balance of iron and inevitable impurities. The product specification is as follows: 2.0 × 1500 × c (mm).
(1) And controlling the cold wire annealing temperature target at 1110-1115 ℃, calculating the heat preservation time to be 2-3 min according to the thickness of the steel plate being 2.0mm, and finally determining the wire passing speed to be 30m/min.
(2) Electrolytic pickling: na (Na) 2 SO 4 The solution has the specific gravity of 1.25, the temperature of 80 ℃ and the current setting of 5000A;
(3) Mixed acid pickling: HF concentration 30g/l, HNO 3 The concentration of the Fe is 250g/l n+ The concentration is 30g/L, and the mixed acid temperature is 50 ℃;
the cold-rolled sheet product is obtained through the process steps, the performance is qualified, the surface is smooth, and the roughness is 0.25 mu m.
Example two
The high-Si-content austenitic heat-resistant steel comprises the following components: c:0.05 to 0.10, si:1.50 to 1.80, mn:0.50 to 0.80, P: less than or equal to 0.030, S: less than or equal to 0.003, cr: 20.70-21.30, ni: 10.60-11.20, N:0.14 to 0.16, ce:0.03 to 0.05 percent, and the balance of iron and inevitable impurities. The product specification is as follows: 1.2 × 1219 × c (mm).
(1) And controlling the cold wire annealing temperature target at 1110-1115 ℃, calculating the heat preservation time to be 1.2-1.8min according to the thickness of the steel plate of 1.2mm, and finally determining the wire passing speed to be 40m/min.
(2) Electrolytic pickling: na (Na) 2 SO 4 The specific gravity of the solution is 1.20, the temperature is 80 ℃, and the current is set to be 6000A;
(3) Mixed acid pickling: HF concentration 25g/l, HNO 3 Concentration of 200g/l, fe n+ The concentration is 28g/L, and the mixed acid temperature is 50 ℃;
through the process steps, the cold-rolled sheet product is obtained, the performance is qualified, the surface is smooth, and the roughness is 0.20 mu m.
The invention adopts a lower temperature and short time annealing system to ensure that the oxide skin of the steel plate has moderate thickness and uniform components, and then is matched with a proper electrolytic pickling process to ensure that the surface color of the high temperature resistant austenitic stainless steel cold-rolled plate with the Si content of more than 1.5 percent is uniform without the defects of iron phosphorus roughness, the product has better oxidation resistance and corrosion resistance, and the surface roughness of the steel plate with the thickness of less than 2.0mm is less than or equal to 0.30 mu m.
The above description is only an embodiment of the present invention, but the structural features of the present invention are not limited thereto, and any changes or modifications within the scope of the present invention by those skilled in the art are covered by the present invention.
Claims (2)
1. An annealing and pickling process method of high-temperature resistant austenitic stainless steel cold-rolled strip steel is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: cold rolling and annealing: the annealing temperature is 1120 +/-10 ℃, the effective length of an annealing hearth in a high-temperature section is 60m, and the strip steel threading speed is calculated according to the effective length of the hearth in the high-temperature section and the thickness of the strip steel according to the principle that the heat of a steel plate in the high-temperature section is preserved for 1-1.5 min/mm;
step two: electrolytic pickling: first stage acid pickling Medium Na 2 SO 4 (ii) a Specific gravity of 1.20-1.30g/cm 3 The electrolysis temperature is 75 +/-5 ℃, and the electrolysis current is 2000-7000A; second stage pickling medium HNO 3 The acid concentration is 70-140g/L, the temperature is 50 +/-5 ℃, and the electrolytic current is 2000-5000A;
step three: mixed acid pickling: HF and HNO 3 Mixed, HNO 3 Concentration of 120-250g/L, HF concentration of 15-30g/L, fe n+ Less than or equal to 40g/L, and the temperature of mixed acid is 45 to 55 ℃.
2. The annealing and pickling process method of the high-temperature resistant austenitic stainless steel cold-rolled strip steel according to claim 1, characterized by comprising the following steps: and calculating the threading speed of the strip steel according to the principle that the heat of the steel plate is kept for 1 to 1.5min/mm in the high-temperature section, specifically the thickness of the high-temperature resistant austenitic stainless steel cold-rolled plate is 1 to 2mm according to the effective length of the hearth in the high-temperature section and the thickness of the strip steel, so that the heat-preserving time is 1 to 3min in the high-temperature section, and the threading speed is 20 to 60m/min.
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|---|---|---|---|---|
| KR20070045502A (en) * | 2005-10-27 | 2007-05-02 | 주식회사 포스코 | A descaling method for austenite stainless steel |
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| CN110814032A (en) * | 2019-10-18 | 2020-02-21 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Cold rolling method for 2B surface 439 ferritic stainless steel |
| CN113234898A (en) * | 2021-05-19 | 2021-08-10 | 山西太钢不锈钢股份有限公司 | Continuous line annealing and pickling production method for wide iron-chromium-aluminum cold-rolled coil |
| CN114058797A (en) * | 2021-11-18 | 2022-02-18 | 山西太钢不锈钢股份有限公司 | Continuous line annealing and pickling production method of nickel-saving austenitic stainless steel |
| CN114150124A (en) * | 2021-12-09 | 2022-03-08 | 山西太钢不锈钢股份有限公司 | Annealing and pickling process method for high-chromium-nickel stainless steel cold-rolled steel strip |
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- 2022-07-20 CN CN202210848373.9A patent/CN115287419A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070045502A (en) * | 2005-10-27 | 2007-05-02 | 주식회사 포스코 | A descaling method for austenite stainless steel |
| CN105586600A (en) * | 2016-03-16 | 2016-05-18 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Duplex stainless steel cold rolling annealing and pickling process |
| CN110814032A (en) * | 2019-10-18 | 2020-02-21 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Cold rolling method for 2B surface 439 ferritic stainless steel |
| CN113234898A (en) * | 2021-05-19 | 2021-08-10 | 山西太钢不锈钢股份有限公司 | Continuous line annealing and pickling production method for wide iron-chromium-aluminum cold-rolled coil |
| CN114058797A (en) * | 2021-11-18 | 2022-02-18 | 山西太钢不锈钢股份有限公司 | Continuous line annealing and pickling production method of nickel-saving austenitic stainless steel |
| CN114150124A (en) * | 2021-12-09 | 2022-03-08 | 山西太钢不锈钢股份有限公司 | Annealing and pickling process method for high-chromium-nickel stainless steel cold-rolled steel strip |
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