WO2014038510A1 - Stainless steel sheet and method for producing same - Google Patents
Stainless steel sheet and method for producing same Download PDFInfo
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- WO2014038510A1 WO2014038510A1 PCT/JP2013/073537 JP2013073537W WO2014038510A1 WO 2014038510 A1 WO2014038510 A1 WO 2014038510A1 JP 2013073537 W JP2013073537 W JP 2013073537W WO 2014038510 A1 WO2014038510 A1 WO 2014038510A1
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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
- C21D8/02—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
- C21D8/0226—Hot rolling
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- C—CHEMISTRY; METALLURGY
- 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
- C22C38/48—Ferrous alloys, e.g. steel alloys containing chromium with nickel with niobium or tantalum
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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
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/004—Heat treatment of ferrous alloys containing Cr and Ni
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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
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
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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
- C21D8/02—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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- 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
- C21D8/02—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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- 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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- 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
- C22C38/42—Ferrous alloys, e.g. steel alloys containing chromium with nickel with copper
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- C—CHEMISTRY; METALLURGY
- 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
- C22C38/44—Ferrous alloys, e.g. steel alloys containing chromium with nickel with molybdenum or tungsten
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/001—Austenite
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/008—Martensite
Definitions
- the present invention relates to a stainless steel plate and a method for producing the same. More specifically, a stainless steel plate excellent in corrosion resistance and shape flatness, having a sufficiently fine crystal grain suitable for etching processing and laser processing that require recent precision, and suitable for precision processing, and its It relates to a manufacturing method.
- This application claims priority based on Japanese Patent Application No. 2012-194214 for which it applied to Japan on September 4, 2012, and uses the content here.
- stainless steel plates with fine crystal grains are suitable for fine processing such as photoetching and laser cutting.
- Examples of such stainless steel plates include the following.
- Patent Document 1 C: 0.03% or less, Si: 1.0% or less, Mn: 2.0% or less, P: 0.1% or less, Ni: 4.0% or more and 20.0% or less Cr: 12.0% or more and 25.0% or less, N: 0.20% or less, and Nb: 0.01% or more and 0.3% or less, with the balance being Fe and impurities, average
- a stainless steel plate for photoetching with a crystal grain size of 15 ⁇ m or less and a method for producing the same are disclosed.
- Patent Document 2 as described above, C: 0.08% or less, Si: 1.0% or less, Mn: 2.0% or less, P: 0.045% or less, S: 0.05% or less, Ni: 5.0% or more and 15% or less, Cr: 15% or more and 20% or less, and the balance is made of Fe and inevitable impurities, and the average crystal grain size is 15 ⁇ m or less.
- the manufacturing method is disclosed.
- Patent Documents 3 and 4 disclose a stainless steel plate for photoetching.
- metastable austenitic stainless steel is used, work strain is introduced by cold rolling and work-induced martensitic transformation is promoted, and reverse transformation to austenitic structure is performed at a relatively low temperature. Is known to be effective.
- SUS301 and SUS301L which have low austenite stability and are easy to process-induced martensite transformation, are known as component systems that are relatively easy to refine. These steel plates have been put to practical use in automobile cylinder head gaskets and diaphragm plates for diaphragm compressors. Or the material refined as a base material for photo-etching processing or laser processing is put into practical use.
- the average crystal grain size is 6, 7, 8, 15 ⁇ m.
- the average crystal grain size is 7, 8 ⁇ m.
- the average crystal grain size is 6, 7, and 9 ⁇ m.
- alloy B in Table 2 of Patent Document 4 the average crystal grain size is 6, 9 ⁇ m.
- the conventional stainless steel plate containing 18% or more of Cr and 8% or more of Ni has a problem that the average crystal grain size is too coarse to be used in recent highly integrated metal mask applications. there were.
- the average crystal grain size satisfying 5 ⁇ m or less is a composition range inferior in corrosion resistance of Cr: less than 18% and Ni: less than 8%.
- an average crystal grain size of a stainless steel plate excellent in corrosion resistance containing 18% or more of Cr and 8% or more of Ni should be 5 ⁇ m or less. Can be confirmed to be difficult.
- Patent Documents 1 to 4 described above have the following description as rolling reduction ratios before grain refinement annealing.
- the rolling reduction during cold rolling before the final annealing is not particularly limited and may be a rolling reduction of about 40% or more that is normally performed”. Also, in this document, the experimental conditions for laboratory examples are described in [Table 2]. However, the rolling reduction before annealing is 50% in 13 cases out of 14 cases, and 65% in only one case.
- Claim 3 of Patent Document 4 states that “after cold rolling at a rolling rate of 30% or more, heat treatment is performed at a temperature of 700 ° C. or more and 900 ° C. or less to make the average crystal grain size 10 ⁇ m or less”. Has been. Also, paragraph [0026] of the same document states that “If the rolling rate is less than 30%, sufficient strain that becomes a driving force for recrystallization does not occur, and a mixed grain structure is formed in the subsequent heat treatment, and the etched surface becomes rough. Therefore, the rolling ratio is set to 30% or more. " As described above, this document confirms that the rolling rate is as low as about 30%.
- paragraphs [0030] to [0032] of the same document describe that, as an example, after cold rolling from 2.5 mm thickness to 1 mm thickness, fine grain annealing was performed at low temperature.
- the rolling rate at this time is only 60%.
- Patent Document 3 describes the rolling reduction before the fine grain annealing as in Patent Document 4. However, there is no description that the reduction rate before the grain refinement annealing contributes to the promotion of the grain refinement, and the condition of a very low reduction rate that only requires recrystallization.
- Patent Document 2 does not describe the influence of the rolling reduction before grain refinement annealing on the average crystal grain size after grain refinement annealing. In the example of this document, only 60% of cases rolled from 2.5 mm to 1 mm are described.
- Patent Document 7 and Patent Document 8 have been reported for the adverse effect of the oxide film formed on the stainless steel plate during the bright annealing on the etching processability.
- JP 2003-3244 A Japanese Patent Application Laid-Open No. 2005-314772 JP 2005-320586 A JP 2005-320587 A JP 2009-299171 A JP 2011-1117024 A JP 2002-275541 A JP-A-11-269613
- stainless steel sheets with a product thickness of 150 ⁇ m or less are frequently used in precision machining applications, but it is more difficult to secure a large rolling reduction with such thin sheet thickness, and it is not flat. Since it is difficult to correct the shape with a tension leveler or the like, a solution has been desired.
- the present invention has been made in view of the above situation, and in order to ensure corrosion resistance equivalent to or higher than that of SUS304 that is generally used, it contains 18% or more of Cr and 8% or more of Ni, while maintaining an average.
- An object is to provide a stainless steel plate suitable for precision machining with a crystal grain size of 5 ⁇ m or less.
- the present inventors paid attention to the fact that the amount of C greatly affects the hardness of the generated martensite structure, and adjusted the component system so as to reduce the amount of C added. Furthermore, the amount of Nb added, which is highly effective in suppressing crystal grain growth, was optimized.
- the present invention based on the above findings is as follows. [1] % By mass, C ⁇ 0.030%, Si ⁇ 0.80%, Mn ⁇ 1.20%, P ⁇ 0.045%, S ⁇ 0.01%, Cu ⁇ 0.60%, Mo ⁇ 0. 60%, Al ⁇ 0.02%, 18.0% ⁇ Cr ⁇ 19.0%, 8.0% ⁇ Ni ⁇ 9.0%, 0.03% ⁇ Nb ⁇ 0.12%, 0.02% ⁇ N ⁇ 0.1%, the balance consists of iron and impurities,
- the Md30 value defined by the formula (1) is 25 to 55, A stainless steel plate having an average crystal grain size of 5 ⁇ m or less.
- the present invention can sufficiently promote the work-induced martensite transformation without carrying out special cold rolling by reviewing all the composition ranges forming the alloy in detail and controlling them to an appropriate range.
- a stainless steel plate suitable for metastable austenitic precision machining with excellent workability, rollability and shape flatness after rolling, suitable for crystal grain refinement, and excellent corrosion resistance is realized.
- the effect of the present invention is remarkable when the thickness tolerance of variation such as thickness is small and the thickness of the product, which is difficult to correct the product shape, is 150 ⁇ m or less.
- C content strongly enhances austenite stability and suppresses martensitic transformation, remarkably increases the strength of the transformed martensite structure, and lowers rolling workability. Therefore, the upper limit of C is limited to 0.030%.
- C produces chromium carbide when annealed at a low temperature, and lowers the corrosion resistance. It also makes the recrystallization behavior unstable. Therefore, it is preferable that it is 0.025% or less. Although there is no particular lower limit, it is 0.003% or more in normal production.
- the upper limit of Si is set to 0.80%. If there is no problem such as insufficient deoxidation in the production process, it is preferably 0.7% or less. Although there is no particular lower limit, it is usually 0.10% or more.
- Mn is an austenite generating element and lowers the Md value. Therefore, the upper limit of Mn is 1.20%.
- a large amount of Mn is preferably 1.0% or less in order to reduce the corrosion resistance. Although there is no particular lower limit, it is preferably 0.30% or more because it also contributes to the strength of the steel.
- the amount of P that impairs hot workability is preferably small, and the upper limit is 0.045%.
- the amount of S that impairs hot workability is preferably small, and the upper limit is 0.01%. More preferably, it is 0.007% or less.
- Cu is an austenite generating element and lowers the Md value. Therefore, the upper limit of Cu is set to 0.60%. It is preferable that it is 0.5% or less. Although a lower limit is not particularly provided, it may be contained by 0.05% or more by bringing in from a scrap raw material or the like.
- ⁇ 18.0% ⁇ Cr ⁇ 19.0% Cr is required to be 18.0% or more from the viewpoint of corrosion resistance. From the viewpoint of increasing the Md value, the upper limit of Cr is 19.0%. From the balance between corrosion resistance and cost, it is preferably 18.5% or less.
- Ni is required to be 8.0% or more from the viewpoint of corrosion resistance. From the viewpoint of increasing the Md value, the upper limit of Ni is limited to 9.0%. Ni increases the austenite stability and is an expensive element, so it is preferably 8.5% or less.
- Mo limits the upper limit to 0.60% from the viewpoint of increasing the Md value. Since Mo is an expensive material, its content is preferably 0.50% or less. Although there is no particular lower limit, 0.05% or more is effective because it contributes to the improvement of corrosion resistance.
- Nb is an indispensable element for suppressing the growth of crystal grains and promoting the refinement, and it is essential to contain more than 0.03%. If it is 0.03% or less, these sufficient effects cannot be exhibited.
- the chemical composition of the present invention is less likely to be finer than the 301L system, it is preferable to contain more than 0.05% Nb. Excess content not only causes an increase in cost, but also inhibits recrystallization, so the upper limit is made 0.12%. In order to ensure a stable recrystallization behavior, the content is preferably 0.10% or less.
- N like C, greatly increases the austenite stability, so its upper limit is limited to 0.1%. N lowers the rollability in hot rolling and increases surface scratches, so 0.08% or less is preferable. However, 0.02% or more is added because it contributes to improving the strength of the steel by solid solution strengthening. From the viewpoint of improving the strength, addition of 0.03% or more is preferable.
- the upper limit of Al is 0.02%. Preferably, it is 0.015% or less.
- Al will reduce diffusion bonding property, and in such a use, it is preferable to set it as 0.01% or less. More preferably, it is 0.008% or less.
- the lower limit is not particularly set, even when no intentional addition is performed and Al is not used as a deoxidizer, it is often contained in an amount of about 0.001%.
- Md30 value 25-55
- the Md30 value indicating the stability of the austenite structure is a value obtained from the chemical composition of steel by the equation (1) (Gladman's equation).
- the Md30 value means the temperature at which 50% martensitic transformation occurs when 30% strain is applied. The higher the Md30 value, the more martensitic transformation is promoted, and the finer graining by reverse transformation becomes easier.
- the Md30 value that can realize an average crystal grain size of 5 ⁇ m or less is not limited to 25 or more, without performing cold rolling with special cooling or cold rolling with significantly multiple passes. From the viewpoint of promoting martensitic transformation, the Md30 value is preferably 28 or more, and more preferably 30 or more. On the other hand, when Md30 is high and the stability of austenite is low, work hardening during cold rolling is large and the rolling load is large, so the upper limit is 55.
- the Md30 value is preferably 48 or less, more preferably 40 or less. It is.
- ⁇ Average crystal grain size ⁇ 5 ⁇ m The average grain size is limited to 5 ⁇ m or less. The reason for the limitation is shown below. It is known that the etched surface and the laser processed surface are affected by the crystal grain size, and the smoother the processed surface, the finer the particle. In recent high performance metal masks, stainless steel plates with a thickness of 150 ⁇ m to 80 ⁇ m are mainly used. For materials provided for high-performance metal masks and precision etching applications, a thickness accuracy of ⁇ 4% is guaranteed, and variations in the thickness of actual products are generally within ⁇ 3%. .
- the plate thickness accuracy of ⁇ 3.2 to 6.0 ⁇ m is guaranteed, and the actual product is limited to plate thickness variations of ⁇ 2.4 to 4.5 ⁇ m. is there.
- the average crystal grain size is preferably 4.5 ⁇ m or less.
- the average crystal grain size is more preferably 3.0 ⁇ m or less.
- the stainless steel sheet of the present invention is effective in applications that require corrosion resistance and refinement of crystal grains other than precision processing applications.
- applications include applications where fatigue strength is expected to be improved by refining crystal grains (for example, diaphragm plates for cylinder head gasket diaphragm type compressors for automobiles) or cases where surface roughening does not occur after molding.
- Preferable uses equipment parts such as a stainless steel housing, a mechanical chassis, or a toner blade of a printing apparatus can be mentioned.
- the manufacturing method of the stainless steel plate of this invention is demonstrated.
- the raw material is melted so as to have a predetermined chemical composition, and a static casting or continuous casting is hot-rolled and annealed. Thereafter, the hot-rolled steel sheet from which the oxide scale on the surface is removed is cold-rolled at a predetermined rolling rate and annealed at a predetermined temperature.
- a hot rolled coil as a base material is required to have excellent flatness.
- a plate thickness deviation sheet crown
- the rolling is such that only one side is stretched and the stable rolling becomes difficult.
- a 600 mm wide hot rolled coil is employed from the beginning, cold rolling becomes stable and it is relatively easy to ensure a large reduction ratio.
- a rolling reduction exceeding 65% is essential from the viewpoint of promoting the processing-induced martensitic transformation and introducing sufficient processing strain. From the viewpoint of reducing the grain size after annealing, the higher the rolling reduction, the better.
- a rolling reduction of more than 70% is preferable in order to stably realize fine graining even if there is manufacturing variation during mass production. If the rolling shape does not deteriorate during cold rolling, it is more preferable to set the rolling reduction to 75% or more.
- the thickness before cold rolling is generally 300 ⁇ m or less, and a large reduction ratio is ensured due to the fact that the thickness of the rolled material is thin relative to the work roll diameter. Is particularly difficult.
- the hardness increase of the transformed martensite structure is suppressed, and even the component system in which martensitic transformation is likely to proceed is reduced.
- cold rolling exceeding 70% can be stably performed.
- the upper limit of the rolling reduction is not particularly defined, but is usually 90% or less because the hardness of the material increases with rolling, making rolling difficult.
- -Annealing temperature 810-940 ° C If the annealing temperature is high, crystal grains grow and become coarse, so the upper limit of the annealing temperature is 940 ° C. From the viewpoint of preventing grain growth, 900 ° C. or lower is preferable. In order to make the average particle size 3 ⁇ m or less, 875 ° C. or less is preferable. On the other hand, if the annealing temperature is too low, the number of non-recrystallized regions increases and the molding processability decreases, so the annealing temperature is limited to 810 ° C. or higher. Preferably it is 825 ° C or more. Since the recrystallization behavior changes depending on the selected component system and the rolling reduction before annealing, it is necessary to determine an appropriate annealing temperature within the above temperature range in order to stably secure a refined structure. preferable.
- the influence of the annealing time is relatively small, and recrystallization proceeds in a short time, so the lower limit of the annealing time is not particularly limited. What is necessary is just to implement on general manufacturing conditions, and what is necessary is just to hold
- Example 1 For chemical compositions A to I shown in Table 1, 30 kg test dissolution was performed. The setting concept of each alloy is as follows. In the following table, the underline indicates outside the scope of the present invention. The chemical composition “-” indicates that inclusion is not intended.
- Alloy A invention example, an example of a preferred form of the present invention.
- Alloy B Invention example, within the scope of the present invention, the Md30 value is increased by lowering the C content.
- Alloy C Inventive example, within the scope of the present invention, the Md30 value is lowered by increasing the C content.
- Alloy D Comparative example, a general SUS304 component system in which the C content and Md30 value are outside the scope of the present invention.
- Alloy E Comparative example, alloy D with reduced Cu and Mo contents and Md30 value within the scope of the present invention. C is out of range.
- Alloy F Comparative example, general SUS304L component system. Ni amount and Md30 value are outside the scope of the present invention.
- Alloy G Comparative example, the chemical composition is excessively reduced, and the Md30 value exceeds the range of the present invention.
- Alloy H Comparative example, SUS301L system proven as a fine-grained material. Low Cr and Ni contents are outside the scope of the present invention.
- Alloy I Comparative example, the content of Cr and Ni was too high, and the Md30 value was below the range of the present invention.
- Alloys A to I were melted in a high frequency melting furnace and statically cast into an ingot to obtain an ingot (60 mm ⁇ 200 mm ⁇ 340 mm) of about 30 kg. After the surface of the ingot was carefully treated by mechanical cutting, it was heated to 1150 ° C. and rolled to a thickness of 6 mm by hot rolling. After hot rolling, annealing was performed by holding at 1130 ° C. for 4 minutes, and the thickness of the plate was adjusted to 5 mm while removing the oxide scale on the surface by mechanical grinding. Thereafter, it was cold-rolled to 2 mm with a cold rolling mill to produce 6 cold-rolled steel sheets each exceeding 2 mm ⁇ 180 mm ⁇ 1000 mm and heated to 1100 ° C. in an Ax gas atmosphere (75% hydrogen—25% nitrogen). Annealed by holding for 2 minutes.
- Ax gas atmosphere 75% hydrogen—25% nitrogen
- test piece thus rolled was heat-treated by holding it at temperatures of 800 ° C., 820 ° C., 870 ° C., 920 ° C., and 960 ° C. for 30 seconds in an Ax gas atmosphere.
- test piece after the heat treatment was cut in a direction perpendicular to the rolling, and the average crystal grain size was measured by observing the cross section with an optical microscope.
- Alloy H alone has a particle size of 5 ⁇ m or less even when the rolling reduction is 60%, and it was reconfirmed that it is a component system suitable for refinement.
- alloys A, B, C, E, G, and H are selected and cold-rolled at a rolling reduction exceeding 65% (60 for alloy H). % Or more is acceptable).
- the final judgment of the rolling load was determined that the rolling load was excessive when the maximum current (mill current) consumed by the rolling motor during rolling exceeded 80A.
- Table 4 shows the survey results.
- Alloys A, B, C, E, G, and H were confirmed to have an average grain size of less than 5 ⁇ m when held at an annealing temperature of 820 ° C. to 920 ° C. for 30 seconds.
- Alloys A, B, G, and H were confirmed to have an average particle size of 3.0 ⁇ m or less when held for 30 seconds in the above annealing temperature range.
- the corrosion resistance was evaluated by measuring the pitting potential by the dynamic potential method according to JIS G 0577, using a test piece annealed at 920 ° C. after cold rolling at a rolling reduction of 75%.
- the evaluation was performed based on Vc′100, and it was determined that 300 mV or more passed on the basis of the saturated calomel electrode, and less than that was rejected.
- the alloy A was at a pass level, but the alloy H having a low Cr and Ni content was rejected.
- the test piece annealed at 870 ° C. for 30 seconds was confirmed to have a clear etching process with a rectangular shape according to the resist pattern, and was judged to have no problem as a stainless steel plate for precision processing.
- the sample annealed at 800 ° C. for 3600 seconds it was confirmed that the etching processed part was inferior in linearity, and the shape of the processed hole varied from pattern to pattern, and used as a stainless steel plate for precision processing. I decided I could't.
- the measurement result of the slit opening width is that the average value is 102 ⁇ m and the standard deviation is 3 ⁇ m (2.9% with respect to the average value) in the specimen annealed at 870 ° C. for 30 seconds.
- the specimens annealed at 800 ° C for 3600 seconds have a large variation of 104 ⁇ m in average value and 7 ⁇ m in standard deviation (6.7% of the average value), which is not suitable as a material for precision processing. Was confirmed.
- the cause of the deterioration of the linearity of the etched portion is considered to be due to the poor adhesion between the stainless steel plate and the photoresist.
- the cause of the variation in the shape of the processing hole for each pattern is thought to be due to the difference in the amount of dissolution depending on the location because the activation time at the initial stage of etching processing was different due to the presence of a strong coating layer. It is done.
- Alloy J Inventive example, an example of a preferred embodiment of the present invention, which corresponds to alloy A in laboratory tests.
- Alloy K Comparative example, a general SUS304 component system, the amount of C and the Md30 value are out of the scope of the present invention, and correspond to the laboratory test alloy D.
- Alloy L Comparative example, Cu and Mo are reduced from alloy D, and Md30 value is within the range of the present invention.
- C is out of range chemical composition and corresponds to alloy E in the laboratory test.
- Alloy M Comparative example, general SUS304L component system.
- the amount of Ni and the Md30 value are chemical compositions outside the scope of the present invention and correspond to laboratory test alloy F.
- the alloy of each component was melted in the atmosphere of 2.5 tons and continuously cast to obtain a continuously cast slab of 90 mm ⁇ 640 mm ⁇ 5400 mm.
- the surface was cared for by cutting to make it 85 mm ⁇ 640 mm ⁇ 4800 mm.
- the hot-rolled coil was subjected to air annealing at 1150 ° C. and then pickled with a mixed solution of hydrofluoric acid and nitric acid.
- first cold rolling After cold rolling, it was subjected to atmospheric annealing at 1150 ° C. and then pickled with a mixed solution of hydrofluoric acid and nitric acid.
- cold rolling (second cold rolling) was performed to 0.37 mmt using a reversible 6-stage cold rolling mill.
- the rolling reduction at this time is 82%.
- annealing heat treatment was performed at 850 ° C. for 48 seconds in a reducing Ax gas atmosphere (hydrogen 75% -nitrogen 25%).
- finish rolling to 0.15 mm was performed using a reversible 6-stage cold rolling mill.
- heat treatment was performed in the range of 600 to 800 ° C. to reduce residual stress.
- the average crystal grain size was measured by cutting out a small amount of sample after heat treatment in a bright annealing furnace and performing micro observation using an optical microscope in a cross section perpendicular to rolling.
- the manufactured rolled stainless steel plate was cut into 0.15 mm ⁇ 600 mm ⁇ 420 mm and subjected to etching. Etching is performed using a ferric chloride aqueous solution with a liquid temperature of 50 ° C. and a Baume degree of 43 degrees (about 40 mass% in mass percent), pressurized to 0.5 MPa, and sprayed with an etching solution only on one side for 100 seconds from a spray nozzle. And carried out. By measuring the surface roughness of the half-etched surface in which about half of the plate thickness was etched in this way, using a stylus type surface roughness meter, the center line average roughness (Ra) in the direction perpendicular to rolling was measured. The etching processability was evaluated. The measurement length was 4.0 mm, and the cut-off value for removing waviness was 0.80 mm.
- Table 7 shows the number of rolling passes in the second cold rolling in each alloy, the value obtained by dividing the total rolling reduction (82%) by the number of rolling passes, the average crystal grain size after bright annealing, and measurement after finish rolling.
- the centerline average roughness (Ra) of the half-etched surface and the overall judgment result are shown.
- the intended cold rolling with a rolling rate of 82% was carried out for all alloys, but the number of passes and the rolling load at that time varied depending on the alloy.
- the final 4 passes of Alloy K and the final 5 passes of Alloy L are rolled with a large tensile tension and rolling load, but the rolling rate per pass is less than 10%.
- the rolling load is not only high, but the product shape after rolling is apt to be deteriorated, and rolling under a condition of a large load and a low pressure reduction rate is unavoidable.
- alloys J and L the average crystal grain size after grain refinement annealing using a bright annealing furnace was 3.0 ⁇ m or less for alloys J and L. Alloys K and M are also refined to 10 ⁇ m or less by carrying out the large rolling and low-temperature heat treatment, but they are not 5.0 ⁇ m or less, which is the object of the present invention.
- the center line average roughness of the half-etched surface after half-etching in the final product is confirmed to be smoother than that of other alloys in alloys J and L, 0.28 ⁇ m and 0.32 ⁇ m, respectively. .
- alloys K and L are inferior in rolling productivity, and alloys K and M cannot have an average crystal grain size of 5 ⁇ m or less, and as a comprehensive judgment, only alloy J is superior. It was.
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Abstract
Description
[1]
質量%で、C≦0.030%、Si≦0.80%、Mn≦1.20%、P≦0.045%、S≦0.01%、Cu≦0.60%、Mo≦0.60%、Al≦0.02%、18.0%≦Cr≦19.0%、8.0%≦Ni≦9.0%、0.03%<Nb≦0.12%、0.02%≦N≦0.1%、残部が鉄と不純物からなり、
(1)式で定義されるMd30値が25~55であり、
平均結晶粒径が5μm以下である、ステンレス鋼板。
Md30=497-462(C+N)-9.2(Si)-8.1(Mn)-13.7(Cr)-20(Ni+Cu)-18.5(Mo) ・・・ (1)式
ここで、(1)式において、C、N、Si、Mn、Cr、Ni、Cu、Moは、鋼中の各元素の含有量(単位:質量%)を意味する。
[2]
板厚が0.15mm以下である、[1]に記載のステンレス鋼板。
[3]
板厚ばらつきが該板厚の±4%以下である、[2]に記載のステンレス鋼板。
[4]
質量%で、C≦0.030%、Si≦0.80%、Mn≦1.20%、P≦0.045%、S≦0.01%、Cu≦0.60%、Mo≦0.60%、Al≦0.02%、18.0%≦Cr≦19.0%、8.0%≦Ni≦9.0%、0.03%<Nb≦0.12%、0.02%≦N≦0.1%、残部が鉄と不純物からなり、(1)式で定義されるMd30値が25~55であるオーステナイトステンレス鋼板を、65%を超える冷間圧延率で冷間圧延を施した後、810~940℃の焼鈍を行う、ステンレス鋼板の製造方法。 The present invention based on the above findings is as follows.
[1]
% By mass, C ≦ 0.030%, Si ≦ 0.80%, Mn ≦ 1.20%, P ≦ 0.045%, S ≦ 0.01%, Cu ≦ 0.60%, Mo ≦ 0. 60%, Al ≦ 0.02%, 18.0% ≦ Cr ≦ 19.0%, 8.0% ≦ Ni ≦ 9.0%, 0.03% <Nb ≦ 0.12%, 0.02% ≦ N ≦ 0.1%, the balance consists of iron and impurities,
The Md30 value defined by the formula (1) is 25 to 55,
A stainless steel plate having an average crystal grain size of 5 μm or less.
Md30 = 497-462 (C + N) -9.2 (Si) -8.1 (Mn) -13.7 (Cr) -20 (Ni + Cu) -18.5 (Mo) (1) Formula where In the formula (1), C, N, Si, Mn, Cr, Ni, Cu, and Mo mean the content (unit: mass%) of each element in the steel.
[2]
The stainless steel plate according to [1], wherein the plate thickness is 0.15 mm or less.
[3]
The stainless steel plate according to [2], wherein the plate thickness variation is ± 4% or less of the plate thickness.
[4]
% By mass, C ≦ 0.030%, Si ≦ 0.80%, Mn ≦ 1.20%, P ≦ 0.045%, S ≦ 0.01%, Cu ≦ 0.60%, Mo ≦ 0. 60%, Al ≦ 0.02%, 18.0% ≦ Cr ≦ 19.0%, 8.0% ≦ Ni ≦ 9.0%, 0.03% <Nb ≦ 0.12%, 0.02% ≦ N ≦ 0.1%, the balance is iron and impurities, and austenitic stainless steel sheet having an Md30 value defined by equation (1) of 25 to 55 is cold rolled at a cold rolling rate exceeding 65%. A method for producing a stainless steel sheet, which is annealed at 810 to 940 ° C. after being applied.
Cは本特許において重要な意味を持つ元素である。 ・ C ≦ 0.030%
C is an element having an important meaning in this patent.
Siは、製鋼時の脱酸剤として使用される。Siの化合物はエッチング加工時にスマットとなりエッチング速度を低下させる。また、含有量が多いとMd値は低くなり、加工誘起マルテンサイト変態が抑制される。そのため、Siの上限を0.80%とする。製造工程上で脱酸不足などの問題がなければ、0.7%以下であることが好ましい。下限は特に設けないが、通常は0.10%以上である。 ・ Si ≦ 0.80%
Si is used as a deoxidizer during steelmaking. The compound of Si becomes a smut at the time of etching processing and decreases the etching rate. Moreover, when there is much content, Md value will become low and a process induction martensitic transformation will be suppressed. Therefore, the upper limit of Si is set to 0.80%. If there is no problem such as insufficient deoxidation in the production process, it is preferably 0.7% or less. Although there is no particular lower limit, it is usually 0.10% or more.
Mnは、オーステナイト生成元素であり、Md値を低くする。そのため、Mnの上限を1.20%とする。多量のMnは、耐食性を低下させるため、1.0%以下であることが好ましい。下限は特に設けないが、鋼の強度への寄与もあるため、0.30%以上であることが好ましい。 ・ Mn ≦ 1.20%
Mn is an austenite generating element and lowers the Md value. Therefore, the upper limit of Mn is 1.20%. A large amount of Mn is preferably 1.0% or less in order to reduce the corrosion resistance. Although there is no particular lower limit, it is preferably 0.30% or more because it also contributes to the strength of the steel.
熱間加工性を損なうPは少ない方が好ましく、0.045%を上限とする。 ・ P ≦ 0.045%
The amount of P that impairs hot workability is preferably small, and the upper limit is 0.045%.
熱間加工性を損なうSは少ない方が好ましく、0.01%を上限とする。より好ましくは、0.007%以下である。 ・ S ≦ 0.01%
The amount of S that impairs hot workability is preferably small, and the upper limit is 0.01%. More preferably, it is 0.007% or less.
Cuは、オーステナイト生成元素であり、Md値を低くする。そのため、Cuの上限を0.60%とする。0.5%以下であることが好ましい。下限は特に設けないが、スクラップ原料等から持ち込みにより0.05%以上含有することがある。 ・ Cu ≦ 0.60%
Cu is an austenite generating element and lowers the Md value. Therefore, the upper limit of Cu is set to 0.60%. It is preferable that it is 0.5% or less. Although a lower limit is not particularly provided, it may be contained by 0.05% or more by bringing in from a scrap raw material or the like.
Crは、耐食性の観点から18.0%以上を必須とする。Md値を高くする観点から、Crの上限は19.0%とする。耐食性とコストのバランスから、18.5%以下であることが好ましい。 ・ 18.0% ≦ Cr ≦ 19.0%
Cr is required to be 18.0% or more from the viewpoint of corrosion resistance. From the viewpoint of increasing the Md value, the upper limit of Cr is 19.0%. From the balance between corrosion resistance and cost, it is preferably 18.5% or less.
Niは、耐食性の観点から8.0%以上を必須とする。Md値を高くする観点から、Niの上限を9.0%に限定する。Niはオーステナイト安定度を高め、しかも高価な元素であることから、8.5%以下であることが好ましい。 ・ 8.0 ≦ Ni ≦ 9.0%
Ni is required to be 8.0% or more from the viewpoint of corrosion resistance. From the viewpoint of increasing the Md value, the upper limit of Ni is limited to 9.0%. Ni increases the austenite stability and is an expensive element, so it is preferably 8.5% or less.
Moは、Md値を高くする観点から、その上限を0.60%に限定する。Moは高価な材料であるため、その含有量は0.50%以下とすることが好ましい。下限は特に設けないが、耐食性の向上に寄与するため、0.05%以上の添加が有効である。 ・ Mo ≦ 0.60%
Mo limits the upper limit to 0.60% from the viewpoint of increasing the Md value. Since Mo is an expensive material, its content is preferably 0.50% or less. Although there is no particular lower limit, 0.05% or more is effective because it contributes to the improvement of corrosion resistance.
Nbは、結晶粒の成長を抑制し、細粒化を進めるために必須な元素であり0.03%を超える含有を必須とする。0.03%以下では、これらの十分な効果を発揮することができない。 ・ 0.03% <Nb ≦ 0.12%
Nb is an indispensable element for suppressing the growth of crystal grains and promoting the refinement, and it is essential to contain more than 0.03%. If it is 0.03% or less, these sufficient effects cannot be exhibited.
Nは、Cと同様にオーステナイト安定度を大きく高めるため、その上限は0.1%に制限する。Nは熱間圧延での圧延性を低下させ、表面キズを増加させるので、0.08%以下が好ましい。ただし、固溶強化により鋼の強度向上に寄与するので、0.02%以上を添加する。強度向上の観点からは、0.03%以上の添加が好ましい。 ・ 0.02% ≦ N ≦ 0.1%
N, like C, greatly increases the austenite stability, so its upper limit is limited to 0.1%. N lowers the rollability in hot rolling and increases surface scratches, so 0.08% or less is preferable. However, 0.02% or more is added because it contributes to improving the strength of the steel by solid solution strengthening. From the viewpoint of improving the strength, addition of 0.03% or more is preferable.
Alは脱酸剤として使用されるが、圧延で破砕され難い硬質の介在物を生成して、最終製品に悪影響を及ぼすことがある。そのため、Alの上限は0.02%とする。好ましくは、0.015%以下である。また、エッチング加工されたステンレス鋼板を拡散接合により積層する用途では、Alが拡散接合性を低下させることが知られており、このような用途では0.01%以下とすることが好ましい。より好ましくは、0.008%以下である。下限は特に設定しないが、意図的な添加をせずかつ脱酸剤としてAlを使用しない場合でも、0.001%程度は含有していることが多い。 ・ Al ≦ 0.02%
Al is used as a deoxidizer, but it may produce hard inclusions that are not easily crushed by rolling, and may adversely affect the final product. Therefore, the upper limit of Al is 0.02%. Preferably, it is 0.015% or less. Moreover, in the use which laminates | stacks the etched stainless steel plate by diffusion bonding, it is known that Al will reduce diffusion bonding property, and in such a use, it is preferable to set it as 0.01% or less. More preferably, it is 0.008% or less. Although the lower limit is not particularly set, even when no intentional addition is performed and Al is not used as a deoxidizer, it is often contained in an amount of about 0.001%.
オーステナイト組織の安定度を示すMd30値は、(1)式(Gladmanの式)によって鋼の化学組成から求められる値である。 Md30 value: 25-55
The Md30 value indicating the stability of the austenite structure is a value obtained from the chemical composition of steel by the equation (1) (Gladman's equation).
ここで、(1)式におけるC、N、Si、Mn、Cr、Ni、Cu、Moは鋼中の各元素の含有量(単位:質量%)を意味する。 Md30 = 497-462 (C + N) -9.2 (Si) -8.1 (Mn) -13.7 (Cr) -20 (Ni + Cu) -18.5 (Mo) (1) Formula where C, N, Si, Mn, Cr, Ni, Cu, and Mo in the formula (1) mean the content (unit: mass%) of each element in the steel.
平均結晶粒径は5μm以下に限定する。その限定理由を以下に示す。エッチング加工面やレーザー加工面は結晶粒径の影響を受け、細粒であればあるほど平滑な加工面が得られることが知られている。最近の高性能メタルマスクでは、板厚150μm~80μmのステンレス鋼板が主に採用されている。高性能なメタルマスクや精密なエッチング加工用途に提供される材料では、±4%の板厚精度が保証され、実製品の板厚ばらつきは±3%以内に収まっていることが一般的である。 ・ Average crystal grain size ≦ 5μm
The average grain size is limited to 5 μm or less. The reason for the limitation is shown below. It is known that the etched surface and the laser processed surface are affected by the crystal grain size, and the smoother the processed surface, the finer the particle. In recent high performance metal masks, stainless steel plates with a thickness of 150 μm to 80 μm are mainly used. For materials provided for high-performance metal masks and precision etching applications, a thickness accuracy of ± 4% is guaranteed, and variations in the thickness of actual products are generally within ± 3%. .
本発明では、所定の化学組成となるように原料を溶解し、静止鋳造または連続鋳造したものを熱間圧延して焼鈍する。その後、表面の酸化スケールを除去した熱延鋼板について、所定の圧延率で冷間圧延を行い、所定の温度で焼鈍する。 Next, the manufacturing method of the stainless steel plate of this invention is demonstrated.
In the present invention, the raw material is melted so as to have a predetermined chemical composition, and a static casting or continuous casting is hot-rolled and annealed. Thereafter, the hot-rolled steel sheet from which the oxide scale on the surface is removed is cold-rolled at a predetermined rolling rate and annealed at a predetermined temperature.
本発明のステンレス鋼板では、材料の平坦度が強く要求される。そのため、母材の熱間圧延コイルにも平坦度に優れたものが要求される。一般に熱間圧延コイルでは、幅方向中央部の板厚が厚く端部が薄いという板厚偏差(シートクラウン)が存在する。本発明では、製品幅と同様な幅を有する熱間圧延コイルを用いることが有効である。例えば、600mm幅の製品を製造する場合、1200mm幅の熱間圧延コイルを母材とし、幅方向で半分に分割して使用すると、600mm幅の圧延時に初期状態での左右の板厚(母材での幅中央部と端部の板厚)が異なるため片側だけが伸びる圧延となり、安定した圧延は困難となる。この逆に、始めから600mm幅の熱間圧延コイルを採用すれば、冷間圧延は安定し、大きな圧下率を確保することも比較的容易となる。本発明の精密加工用ステンレス鋼板では、製品幅と同様な幅を有する熱間圧延コイルを母材とすることが望ましい。 -Hot rolling In the stainless steel plate of this invention, the flatness of material is requested | required strongly. Therefore, a hot rolled coil as a base material is required to have excellent flatness. Generally, in a hot-rolled coil, there is a plate thickness deviation (sheet crown) in which the plate thickness at the center in the width direction is thick and the end is thin. In the present invention, it is effective to use a hot rolled coil having a width similar to the product width. For example, when manufacturing a product having a width of 600 mm, when a hot rolled coil having a width of 1200 mm is used as a base material and divided in half in the width direction, the left and right plate thicknesses in the initial state (base material) when rolling the width of 600 mm are used. In this case, the rolling is such that only one side is stretched and the stable rolling becomes difficult. On the other hand, if a 600 mm wide hot rolled coil is employed from the beginning, cold rolling becomes stable and it is relatively easy to ensure a large reduction ratio. In the stainless steel plate for precision processing of the present invention, it is desirable to use a hot rolled coil having a width similar to the product width as a base material.
細粒化の焼鈍を実施する直前の冷間圧延では、加工誘起マルテンサイト変態の促進と十分な加工歪を導入する観点から65%を超える圧下率を必須とする。焼鈍後の粒径を微細化する観点からは、この圧下率は高ければ高い程良い。量産時に製造ばらつきがあっても安定して細粒化を実現するためには、70%超の圧下率が好ましい。冷間圧延時に圧延形状が悪化しないのであれば、75%以上の圧下率とすることが、さらに好ましい。 ・ Cold rolling ratio (rolling ratio)> 65%
In the cold rolling immediately before the refinement annealing is performed, a rolling reduction exceeding 65% is essential from the viewpoint of promoting the processing-induced martensitic transformation and introducing sufficient processing strain. From the viewpoint of reducing the grain size after annealing, the higher the rolling reduction, the better. A rolling reduction of more than 70% is preferable in order to stably realize fine graining even if there is manufacturing variation during mass production. If the rolling shape does not deteriorate during cold rolling, it is more preferable to set the rolling reduction to 75% or more.
焼鈍温度が高いと結晶粒が成長・粗大化してしまうので、焼鈍温度の上限は940℃とする。粒成長を防止する観点から、900℃以下が好ましい。平均粒径を3μm以下とするためには、875℃以下が好ましい。一方、焼鈍温度が低すぎると未再結晶領域が多くなり成形加工性が低下するため、焼鈍温度は810℃以上に限定する。好ましくは825℃以上である。再結晶挙動は選択した成分系と焼鈍前の圧下率に依存して変化するため、微細化した組織を安定して確保するためには、上記の温度範囲内で適切な焼鈍温度を定めることが好ましい。 -Annealing temperature: 810-940 ° C
If the annealing temperature is high, crystal grains grow and become coarse, so the upper limit of the annealing temperature is 940 ° C. From the viewpoint of preventing grain growth, 900 ° C. or lower is preferable. In order to make the average particle size 3 μm or less, 875 ° C. or less is preferable. On the other hand, if the annealing temperature is too low, the number of non-recrystallized regions increases and the molding processability decreases, so the annealing temperature is limited to 810 ° C. or higher. Preferably it is 825 ° C or more. Since the recrystallization behavior changes depending on the selected component system and the rolling reduction before annealing, it is necessary to determine an appropriate annealing temperature within the above temperature range in order to stably secure a refined structure. preferable.
表1に示す化学組成A~Iについて、30kgの試験溶解を実施した。各合金の設定思想は以下の通りである。以下の表において、アンダーラインは、本発明の範囲外を示す。化学組成の「-」は、含有を意図していないことを示す。 (Example 1)
For chemical compositions A to I shown in Table 1, 30 kg test dissolution was performed. The setting concept of each alloy is as follows. In the following table, the underline indicates outside the scope of the present invention. The chemical composition “-” indicates that inclusion is not intended.
・焼鈍条件を870℃×30秒保持に固定して、各成分系での圧下率の影響を確認した。表2に細粒化焼鈍前に行った冷間圧延の圧下率と、焼鈍後の平均結晶粒径の関係を示す。 <Examination of rolling reduction before fine grain annealing>
-The annealing condition was fixed at 870 ° C. × 30 seconds, and the influence of the rolling reduction in each component system was confirmed. Table 2 shows the relationship between the rolling reduction of the cold rolling performed before the refined annealing and the average crystal grain size after the annealing.
・合金D、F、およびIでは、粒径が5μm以下となることがなかった。 -In all component systems, the higher the rolling reduction before annealing, the finer the particles.
In Alloys D, F, and I, the particle size did not become 5 μm or less.
冷間圧延は、1パスの圧延荷重が40トンを超えない範囲で、徒にパス回数が増加しないようなパススケジュールを各々選択して実施された。表3に調査結果を示す。 <Investigation of rolling load>
Cold rolling was performed by selecting each pass schedule that would not increase the number of passes within a range where the rolling load of one pass did not exceed 40 tons. Table 3 shows the survey results.
圧下率75%で冷間圧延を実施したサンプルを用いて、焼鈍温度を800℃、820℃、870℃、920℃および960℃に変化させて30秒間保持したときの平均結晶粒径を調査した。また、焼鈍温度を800℃として3600秒間保持したときの平均結晶粒径を調査した。表5に調査結果を示す。 <Investigation of annealing temperature and annealing time>
Using a sample that was cold-rolled at a rolling reduction of 75%, the average grain size when the annealing temperature was changed to 800 ° C., 820 ° C., 870 ° C., 920 ° C. and 960 ° C. and held for 30 seconds was investigated. . In addition, the average crystal grain size was investigated when the annealing temperature was 800 ° C. and held for 3600 seconds. Table 5 shows the survey results.
一方、焼鈍温度が800℃で3600秒間保持した場合には、全ての合金で再結晶が確認された。
合金A、B、C、E、GおよびHでは、800℃の焼鈍温度で3600秒間保持することによって平均結晶粒径が3μmを下回ることが確認された。 When the annealing temperature was kept at 800 ° C. for 30 seconds, the structure of non-recrystallized was dominant in all alloys.
On the other hand, when the annealing temperature was held at 800 ° C. for 3600 seconds, recrystallization was confirmed in all alloys.
In alloys A, B, C, E, G and H, it was confirmed that the average grain size was less than 3 μm by holding at an annealing temperature of 800 ° C. for 3600 seconds.
合金AとHについて、圧下率75%で冷間圧延後に920℃で焼鈍した試験片を用いて、JIS G 0577に準じて動電位法による孔食電位測定を行って耐食性の評価を実施した。
試験面積は1cm2とし、pH=7.0に調整された200mol/m3の塩化ナトリウム水溶液を用いて、60℃の環境中で0.3mV/s の電位掃引速度で実施した。評価はVc’ 100により行い、飽和カロメル電極基準で300mV以上を合格、それ未満を不合格と判断した。 <Evaluation of corrosion resistance>
For the alloys A and H, the corrosion resistance was evaluated by measuring the pitting potential by the dynamic potential method according to JIS G 0577, using a test piece annealed at 920 ° C. after cold rolling at a rolling reduction of 75%.
The test area was 1 cm 2 and a 200 mol / m 3 aqueous sodium chloride solution adjusted to pH = 7.0 was used in a 60 ° C. environment at a potential sweep rate of 0.3 mV / s. The evaluation was performed based on Vc′100, and it was determined that 300 mV or more passed on the basis of the saturated calomel electrode, and less than that was rejected.
合金Aについて、800℃で3600秒間の焼鈍を実施したものと870℃で30秒間の焼鈍をした試験片を0.1mmまで冷間圧延し、0.1mm×150mm×360mmに切断して、エッチング加工性の評価を実施した。この試験片にアルカリ脱脂をした後に、試験片の両面にアクリル樹脂系のフォトレジストを厚さ10μmで塗布し、幅0.1mm、長さ5mmの長方形のスリット状のパターンを多数形成した。その後、液温50℃でボーメ度が45度(質量パーセントで約42mass%)の塩化第二鉄水溶液を用いて、0.5MPaに加圧してスプレーノズルからエッチング液を両面に噴霧してエッチング加工を実施した。その後、フォトレジスト膜を除去して、スリットパターンの形状を実態顕微鏡を用いて観察すると共に、長方形のスリットパターンの狭い方の開口幅を各々36か所について1μm単位で測定した。測定部位は、各スリットパターンの長手方向中央部に限定した。 <Evaluation of etching processability>
For Alloy A, specimens annealed at 800 ° C. for 3600 seconds and annealed at 870 ° C. for 30 seconds are cold-rolled to 0.1 mm, cut into 0.1 mm × 150 mm × 360 mm, and etched The workability was evaluated. After alkali degreasing the test piece, an acrylic resin photoresist was applied to both sides of the test piece with a thickness of 10 μm to form a large number of rectangular slit-like patterns having a width of 0.1 mm and a length of 5 mm. After that, using an aqueous ferric chloride solution with a liquid temperature of 50 ° C. and a Baume degree of 45 degrees (about 42 mass% in mass percent), pressurizing to 0.5 MPa and spraying the etching liquid on both sides from the spray nozzle for etching processing Carried out. Thereafter, the photoresist film was removed, and the shape of the slit pattern was observed with an actual microscope, and the narrower opening width of the rectangular slit pattern was measured in units of 1 μm at 36 locations. The measurement site was limited to the central portion in the longitudinal direction of each slit pattern.
上記実験室試験によって得られた知見に基づいて、表6に示す合金J~Mについて、スケールアップした試作と評価を実施した。各合金の設定思想は以下の通りである。 <Example 2>
Based on the knowledge obtained by the laboratory test, alloys J to M shown in Table 6 were scaled up and evaluated. The setting concept of each alloy is as follows.
熱間圧延コイルは、1150℃で大気焼鈍をした後に、フッ酸と硝酸の混合液により酸洗された。 It was heated to 1200 ° C. and hot-rolled to obtain a hot-rolled coil having a thickness of 6 mm.
The hot-rolled coil was subjected to air annealing at 1150 ° C. and then pickled with a mixed solution of hydrofluoric acid and nitric acid.
可逆式の20段冷間圧延機を用いて、2mmまで冷間圧延を実施した。(圧下率=67%)この一番最初の冷間圧延を、第1冷間圧延と呼ぶ。冷間圧延後は、1150℃で大気焼鈍をした後に、フッ酸と硝酸の混合液により酸洗された。 Thereafter, coil polishing was performed to remove wrinkles and the like on the coil surface generated during hot rolling.
Using a reversible 20-stage cold rolling mill, cold rolling was performed to 2 mm. (Reduction ratio = 67%) This first cold rolling is called first cold rolling. After cold rolling, it was subjected to atmospheric annealing at 1150 ° C. and then pickled with a mixed solution of hydrofluoric acid and nitric acid.
Claims (5)
- 質量%で、C≦0.030%、Si≦0.80%、Mn≦1.20%、P≦0.045%、S≦0.01%、Cu≦0.60%、Mo≦0.60%、Al≦0.02%、18.0%≦Cr≦19.0%、8.0%≦Ni≦9.0%、0.03%<Nb≦0.12%、0.02%≦N≦0.1%、残部が鉄と不純物からなり、
(1)式で定義されるMd30値が25~55であり、
平均結晶粒径が5μm以下である、ステンレス鋼板。
Md30=497-462(C+N)-9.2(Si)-8.1(Mn)-13.7(Cr)-20(Ni+Cu)-18.5(Mo) ・・・ (1)式
ここで、(1)式において、C、N、Si、Mn、Cr、Ni、Cu、Moは、鋼中の各元素の含有量(単位:質量%)を意味する。 % By mass, C ≦ 0.030%, Si ≦ 0.80%, Mn ≦ 1.20%, P ≦ 0.045%, S ≦ 0.01%, Cu ≦ 0.60%, Mo ≦ 0. 60%, Al ≦ 0.02%, 18.0% ≦ Cr ≦ 19.0%, 8.0% ≦ Ni ≦ 9.0%, 0.03% <Nb ≦ 0.12%, 0.02% ≦ N ≦ 0.1%, the balance consists of iron and impurities,
The Md30 value defined by the formula (1) is 25 to 55,
A stainless steel plate having an average crystal grain size of 5 μm or less.
Md30 = 497-462 (C + N) -9.2 (Si) -8.1 (Mn) -13.7 (Cr) -20 (Ni + Cu) -18.5 (Mo) (1) Formula where In the formula (1), C, N, Si, Mn, Cr, Ni, Cu, and Mo mean the content (unit: mass%) of each element in the steel. - 板厚が0.15mm以下である、請求項1に記載のステンレス鋼板。 The stainless steel plate according to claim 1, wherein the plate thickness is 0.15 mm or less.
- 板厚ばらつきが該板厚の±4%以下である、請求項2に記載のステンレス鋼板。 The stainless steel plate according to claim 2, wherein the plate thickness variation is ± 4% or less of the plate thickness.
- 質量%で、C≦0.030%、Si≦0.80%、Mn≦1.20%、P≦0.045%、S≦0.01%、Cu≦0.60%、Mo≦0.60%、Al≦0.02%、18.0%≦Cr≦19.0%、8.0%≦Ni≦9.0%、0.03%<Nb≦0.12%、0.02%≦N≦0.1%、残部が鉄と不純物からなり、(1)式で定義されるMd30値が25~55であるオーステナイトステンレス鋼板を、65%を超える冷間圧延率で冷間圧延を施した後、810~940℃の焼鈍を行う、ステンレス鋼板の製造方法。 % By mass, C ≦ 0.030%, Si ≦ 0.80%, Mn ≦ 1.20%, P ≦ 0.045%, S ≦ 0.01%, Cu ≦ 0.60%, Mo ≦ 0. 60%, Al ≦ 0.02%, 18.0% ≦ Cr ≦ 19.0%, 8.0% ≦ Ni ≦ 9.0%, 0.03% <Nb ≦ 0.12%, 0.02% ≦ N ≦ 0.1%, the balance is iron and impurities, and austenitic stainless steel sheet having an Md30 value defined by equation (1) of 25 to 55 is cold rolled at a cold rolling rate exceeding 65%. A method for producing a stainless steel sheet, which is annealed at 810 to 940 ° C. after being applied.
- 前記焼鈍が600秒未満である、請求項4に記載のステンレス鋼板の製造方法。 The method for producing a stainless steel plate according to claim 4, wherein the annealing is less than 600 seconds.
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