WO2014103722A1 - 抗菌性に優れたフェライト系ステンレス鋼板及びその製造方法 - Google Patents

抗菌性に優れたフェライト系ステンレス鋼板及びその製造方法 Download PDF

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WO2014103722A1
WO2014103722A1 PCT/JP2013/083205 JP2013083205W WO2014103722A1 WO 2014103722 A1 WO2014103722 A1 WO 2014103722A1 JP 2013083205 W JP2013083205 W JP 2013083205W WO 2014103722 A1 WO2014103722 A1 WO 2014103722A1
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stainless steel
ferritic stainless
steel sheet
mass
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French (fr)
Japanese (ja)
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智彦 盛田
秦野　正治
石丸　詠一朗
浩一 井内
昭仁 山岸
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新日鐵住金ステンレス株式会社
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Priority to CN201380062495.4A priority Critical patent/CN104884657B/zh
Priority to KR1020157013788A priority patent/KR101762046B1/ko
Priority to IN3729DEN2015 priority patent/IN2015DN03729A/en
Publication of WO2014103722A1 publication Critical patent/WO2014103722A1/ja

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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
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    • 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
    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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    • C21D2201/00—Treatment for obtaining particular effects
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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
    • C21D6/00—Heat treatment of ferrous alloys
    • C21D6/002—Heat treatment of ferrous alloys containing Cr

Definitions

  • the present invention relates to a ferritic stainless steel plate having excellent antibacterial properties and a method for producing the same, and more specifically, a currant such as a handrail and a faucet, a metal coin, a metal container, a metal tableware, a bathtub, a household electric appliance, a toilet seat, and a medical device.
  • the present invention relates to a ferritic stainless steel plate that is suitably used as a material for sanitary instruments such as appliances and heating appliances and building materials for buildings, and a method for producing the same.
  • Ferritic stainless steel sheets have been widely used for home appliances such as kitchen equipment and microwave oven side plates centered on sinks. In recent years, it has been used for medical equipment such as hand-washing bats and interior building materials such as handrails in terms of cleanliness, design, and beauty. That is, the use of stainless steel sheets is increasing in places where germs are likely to occur or where germs are not preferred. On the other hand, in recent years, there is a growing tendency to worry about the adverse effects on the human body caused by the propagation of such bacteria, especially for medical equipment and kitchen equipment where cleanliness is essential, and for building materials where many people gather. Strong antibacterial requirements. From such a flow, attempts have been made to provide antibacterial properties to the ferritic stainless steel itself that is used in sites where these cleanliness is required.
  • Patent Document 1 disclose techniques for providing antibacterial properties by a method in which a resin containing an antibacterial agent is applied and laminated on the surface of stainless steel or a method in which a matrix containing an antibacterial component is plated.
  • Patent Documents 3 to 5 Examples of methods for imparting antibacterial properties to the stainless steel material itself include Patent Documents 3 to 5.
  • Patent Literature 3 and Patent Literature 4 Cu is eluted in the electrolyte by applying a noble potential to the ferritic stainless steel material or austenitic stainless steel material containing Cu by an alternating electrolytic treatment method, and then a base potential is applied. By doing so, Cu is deposited on the surface of the stainless steel material to provide antibacterial properties.
  • the surface of the steel surface layer is obtained by polishing and polishing the surface of a ferritic stainless steel material, austenitic stainless steel plate, or martensitic stainless steel plate containing Cu, and then performing bright annealing or nitric hydrofluoric acid pickling.
  • a method of forming a layer in which Cu is concentrated to 3% by mass or more is disclosed.
  • ferritic stainless steel is often used for metal coins because of its good workability and low cost performance.
  • Ferritic stainless steel with low raw material costs is advantageous from an economical point of view.
  • softening of, for example, about Hv 190 or less may be required for punching or stamping.
  • ferritic stainless steel containing Cu for antibacterial properties often has a problem of hardening due to solid solution strengthening or precipitation strengthening.
  • Patent Document 6 discloses the Hv hardness of ferritic stainless steel containing 0.66% or more of Cu.
  • 16.87Cr-0.66Cu is Hv171
  • 13.57Cr-1.08Cu is Hv166.
  • Patent Document 7 discloses that a cooling rate after hot rolling is reduced by heating at a temperature of 3 ° C./s or more to a coiling temperature of 500 to 300 ° C. after hot rolling.
  • a technique for avoiding toughness defects by controlling the Cu clustering present in the sheet metal to a maximum of 5 nm or less.
  • Patent Document 1 and Patent Document 2 when a resin containing an antibacterial agent is applied to the surface or a plating layer containing an antibacterial component is applied, the surface gloss peculiar to stainless steel is lost. Is called. Therefore, commercial value is lost in applications where surface gloss is required. Furthermore, a plating layer containing an antibacterial resin film or an antibacterial component is easily damaged by cracking or chipping during press working or use. Further, when exposed to a humid atmosphere, the antibacterial components are eluted, the appearance is deteriorated and the original antibacterial action is lost.
  • Patent Document 3 to Patent Document 5 there are problems in Patent Document 3 to Patent Document 5 in which the stainless steel material itself has antibacterial properties.
  • the alternating electrolytic treatment methods disclosed in Patent Document 3 and Patent Document 4 deposit Cu on the surface of stainless steel by electrodeposition. Therefore, Cu is easily peeled off from the steel surface. For example, if the surface is rubbed with a wire brush, a steel scrubber or the like, the Cu on the surface is scraped and the antibacterial property is lowered.
  • the inventors examined the prior art disclosed that antibacterial properties can be obtained by controlling the surface Cu concentration as in Patent Document 5 to a certain value or more. As a result, it has been found that these conventional techniques may cause a large variation in antibacterial properties in the plate width direction within the same plate surface.
  • the antibacterial stainless steel obtained by the method of the prior art is found to have a portion having good antibacterial properties and a portion having a bad antibacterial property on the plate surface, and is used for a final product imparted with antibacterial properties. , It turns out that the yield will deteriorate.
  • the conventionally disclosed technology for developing antibacterial properties in stainless steel itself has a tendency to decrease the antibacterial properties and remains unsatisfactory in terms of yield.
  • the ferritic stainless steel described in Patent Document 6 has a Cu concentration of 0.66 to 1.08% and Hv of 190 or less.
  • the ferritic stainless steel described in Patent Document 6 does not satisfy the formula (a) of the present invention, which will be described later, and cannot cope with the case where high corrosion resistance is required in addition to softening. It was.
  • Patent Document 7 stipulates that the cooling rate from hot rolling to winding is 3 ° C./s or more in order to control Cu clustering to 5 nm or less and improve toughness. However, no technology relating to softening of the cold-rolled material is disclosed.
  • JP-A-5-228202 Japanese Patent Laid-Open No. 6-10191 JP-A-8-60302 JP-A-8-60303 Japanese Patent Laid-Open No. 11-172380 JP 2003-213378 A International Publication No. 2012/108479
  • An object of the present invention is to provide a ferritic stainless steel sheet having both antibacterial properties and softening and a method for producing the same.
  • the present inventors have intensively studied the difference between the antibacterial and good portions on the plate surface. As a result, the following knowledge was obtained.
  • the Cu maximum concentration of the Cu concentrated layer on the steel surface needs to be at least 10% by mass.
  • control of the Cu concentration on the steel surface is a necessary condition for the development of antibacterial properties, but it is not sufficient. That is, according to the evaluation results of the present inventors, even when the maximum Cu concentration on the steel surface was 10% by mass or more, there were cases where the antibacterial property was poor. This means that an antibacterial expression factor exists in addition to the maximum Cu concentration on the steel surface. In the past, it was speculated that antibacterial variation had increased in the plate surface because they were not grasped. Therefore, the present inventors conducted an investigation by further expanding the field of view to the component composition of the steel surface layer portion in order to investigate the factor.
  • the present inventors have further studied the influence of heat treatment on the hardness of the Cu-containing ferritic stainless steel plate. Specifically, various studies were made on the solid solution / precipitation form of Cu and the heat treatment (heating / cooling conditions) exerted on them, and the following knowledge was obtained.
  • a solution temperature of 900 to 1100 ° C. is considered effective for softening because Cu precipitates are re-dissolved.
  • An average cooling rate of 3 ° C./s or more also suppresses Cu precipitation.
  • Hv ⁇ 40 ⁇ (Cu ⁇ 0.3) +135 (a) In addition, Cu in a formula shows Cu content (mass%). Conversely, when the above formula (a) is not satisfied, Cu precipitates are observed at a high density in the steel. Even if it is softened to Hv 190 or less, the deposited Cu reduces the corrosion resistance.
  • hot-rolled sheet annealing is performed by continuous annealing rather than batch annealing, heated to 800 to 1100 ° C., and then average cooling rate of 1 ° C./s or more to 400 ° C. Cool with.
  • it can soften in the range which satisfy
  • most Cu precipitates defined in the present invention are sufficiently small, and coarse precipitates of about 10 to 1000 nm are only partially observed.
  • the size is almost 10 to 1000 nm and the precipitation density is very high.
  • the present invention has been obtained based on the above knowledge, and the contents thereof are as follows.
  • Cu is contained 0.1% or more and 5.0% or less, a Cu concentrated layer is provided on the surface of the stainless steel plate, and the Cu maximum concentration Cm of the Cu concentrated layer is 10.0 mass.
  • % Ferritic stainless steel sheet having an antibacterial property with an Fe / Cr ratio of 2.4 or more at a depth position from the steel sheet surface showing the maximum Cu concentration Cm.
  • Cu is contained in an amount of 0.1% to 5.0%, a Cu concentrated layer is provided on the surface of the stainless steel plate, and the Cu maximum concentration Cm of the Cu concentrated layer is 18.0 mass.
  • the method further includes a hot-rolled sheet annealing step and a finish annealing step, wherein the stainless steel plate has the component composition according to any one of (3) to (6), and the finish annealing step includes The ferritic stainless steel having excellent antibacterial properties as described in (8) or (9) above, comprising a step of annealing at an annealing temperature of 900 to 1100 ° C.
  • a method of manufacturing a steel sheet (11)
  • the hot-rolled sheet annealing step is performed by continuous annealing, and the continuous annealing is performed by annealing at an annealing temperature of 800 to 1100 ° C., and then cooling to 400 ° C. at an average cooling rate of 1 ° C./second or more.
  • the ferritic stainless steel plate excellent in antibacterial properties of the present invention and the manufacturing method thereof in order to demonstrate good antibacterial properties over the entire area of the plate surface, better antibacterial properties than before can be obtained with a good yield. I can do it.
  • concentration of the steel surface can be highly concentrated so that an example is not seen conventionally, and thereby further favorable antibacterial property can be obtained.
  • the ferritic stainless steel sheet of the present invention having these characteristics can be suitably used as, for example, a metal coin.
  • FIG. 1 is a graph showing an example of the concentration distribution of C, O and main elements in the depth direction from the surface of the stainless steel according to the present invention.
  • FIG. 2 is a graph showing an example of the concentration distribution of O and main elements in the depth direction from the surface of the stainless steel according to the present invention.
  • FIG. 3 is a graph showing the relationship between the maximum Cu concentration, Fe / Cr ratio, and antibacterial evaluation for the examples of the present invention (examples of the present invention) and comparative examples.
  • the ferritic stainless steel plate excellent in antibacterial properties and the method for producing the same according to an embodiment of the present invention will be described in detail.
  • the element content% means mass%.
  • the ferritic stainless steel sheet according to the first embodiment contains, by mass%, Cu in a range of 0.1% to 5.0%, and includes a Cu concentrated layer on the surface of the stainless steel sheet, and the maximum Cu in the Cu concentrated layer.
  • the ferritic stainless steel plate of 2nd Embodiment is 0.1% or more and 5.0% or less of Cu by the mass%, comprises the Cu concentrated layer on the surface of the stainless steel plate, This is a ferritic stainless steel sheet having a maximum Cu concentration Cm of 18.0% by mass or more.
  • the ferritic stainless steel sheet of the first embodiment or the second embodiment is in mass%, and C: 0.050% or less, Cr: 10.0 to 30.0%, Si: 2.00% or less, P : 0.030% or less, S: 0.010% or less, Mn: 2.00% or less, N: 0.050% or less, Ni: 2.0% or less.
  • the ferritic stainless steel sheet according to the first embodiment or the second embodiment may be contained by mass%, and may further contain either one or both of Ti: 0.5% or less and Nb: 1.00% or less. Good.
  • the ferritic stainless steel sheet of the first embodiment or the second embodiment is in mass%, and further Sn: 1.00% or less, Mo: 1.00% or less, Al: 1.000% or less, Mg: 0.00. 010% or less, Co: 1.000% or less, V: 0.50% or less, Zr: 0.10% or less, REM: 0.100% or less, La: 0.100% or less, B: 0.0100% 1 or more types selected from below and Ca: 0.010% or less may be contained.
  • the Cu concentrated layer refers to a region having a Cu concentration higher than the average Cu concentration in the ferritic stainless steel plate in the surface layer of the ferritic stainless steel plate.
  • GDS glow discharge emission analysis
  • the Cu concentration from the surface to a depth of 30 nm is larger than the Cu concentration at a depth of more than 30 nm.
  • the Cu concentrated layer in FIG. 2 is a region from the surface to a depth of 30 nm.
  • the Cu enriched layer may be determined in this way.
  • the Cu concentration obtained by GDS analysis is represented by the Cu concentration relative to the total amount of O, Fe, Cr, Si, Mn, Nb, Ti, Al, and Cu.
  • the concentration at which the Cu concentration is maximum is defined as the Cu maximum concentration Cm.
  • the ratio of the Fe concentration and the Cr concentration at the depth from the steel plate surface showing the maximum Cu concentration Cm is referred to as the Fe / Cr ratio in this embodiment.
  • the maximum Cu concentration Cm is 75.0%, and the Fe / Cr ratio is 2.9.
  • P, S, N, and Ni are not considered when calculating the Cu concentration because they do not concentrate on the surface by the pickling process and do not form oxides on the surface.
  • Ti, Nb, and Al are optional added elements in the present embodiment, but are elements that constitute an oxide, and therefore are considered when calculating the Cu concentration. When these elements are not contained, the Cu concentration is calculated assuming that the concentration of these elements is 0%.
  • the Cu concentration is calculated by removing C after detection by GDS analysis.
  • the Cu content of the ferritic stainless steel sheet will be described.
  • Cu is the most important element for improving antibacterial properties in the ferritic stainless steel sheet of the present embodiment.
  • the Cu maximum concentration Cm of the Cu concentrated layer needs to be 10.0% or more.
  • the lower limit of the Cu content of the steel is set to 0.1%.
  • the upper limit is made 5.0% or less.
  • the Cu content of the steel is preferably 0.1 to 1.7%, most preferably 0.2 to 1.5%.
  • the Cu maximum concentration Cm of the Cu concentrated layer on the steel surface needs to be 10.0% or more. When it is less than 10.0%, antibacterial properties are not exhibited even if other regulations are satisfied.
  • the maximum Cu concentration Cm is preferably 11.0% or more, and more preferably 18.0% or more. On the other hand, no matter how high the Cu maximum concentration Cm is, the antibacterial properties are not adversely affected, so the upper limit is not specified.
  • the white circle plot points in the graph of FIG. 3 indicate examples in which antibacterial properties were excellent (examples of the present invention), and the black circle plot points indicate examples in which antibacterial properties were particularly excellent (examples of the present invention).
  • the plot point of the symbol (cross symbol) indicates an example (comparative example) in which the antibacterial property was poor.
  • the Fe / Cr ratio is more preferably 2.6 or more and 9.5 or less, and further preferably 3.0 or more and 9.0 or less.
  • Cu in the Cu enriched layer is presumed to exhibit antibacterial properties because it dissolves into the water as ions from the steel surface and lowers the cell activity of the fungus.
  • Fe / Cr is preferably 10.0 or less.
  • Fe / Cr is preferably 0.4 or more.
  • Fe / Cr is preferably 0.4 to 10.0, and more preferably 0.5 to 9.5.
  • the Cu content is preferably set to 0.3 to 1.7%. If the Cu content is less than 0.3%, it is well below the Cu solid solubility limit, so that hardening due to Cu precipitation hardly occurs.
  • the precipitation form of Cu is affected by the Cu content and the like, but is 10 to 100 nm granular or rod-shaped.
  • a hard stainless steel plate is characterized in that although the size of Cu precipitates varies, the Cu precipitate density is high.
  • a soft stainless steel plate has a low Cu precipitation density and a small precipitation size. Therefore, Cu precipitation was considered as the main factor of hardening.
  • the cross-sectional hardness of the soft stainless steel plate of this embodiment satisfies the following formula (a) on the Vickers hardness scale.
  • (a) Formula was derived as follows. The measurement results of various Vickers hardnesses were plotted on a graph with Cu concentration and Vickers hardness as axes. The plotted points were classified according to the corrosion resistance evaluation results. As a result, the formula (a) can be derived as a range in which the Vickers hardness (also referred to as Hv hardness or Hv) is 190 or less and also has corrosion resistance. When the formula (a) is not satisfied, even if Hv is 190 or less, the corrosion resistance is deteriorated. This is presumably due to excessive precipitation of Cu. Hv hardness ⁇ 40 ⁇ (Cu ⁇ 0.3) +135 (a) In addition, “Cu” in the formula (a) represents the Cu content (mass%).
  • the essential feature of the present embodiment is the control of the element concentration distribution in the surface layer of the steel sheet as described above.
  • the corrosion resistance, workability and manufacturability, etc. including the component composition of steel that can be used when considering elements other than antibacterial properties, in solving the problems of the present invention as an antibacterial stainless steel plate,
  • the component composition is not limited to the following components.
  • the C is an impurity element that is inevitably mixed in from the dissolved raw material and the like, and it is desirable that the lower limit is not set. If the amount of C exceeds 0.050%, the toughness and cold workability of steel deteriorate, so the upper limit is preferably made 0.050% or less.
  • the amount of C is preferably 0.040% or less, and more preferably 0.020% or less. Moreover, since excessively reducing the amount of C leads to an increase in manufacturing cost, the amount of C is preferably made 0.001% or more.
  • Cr should be added in an amount of 10.0% or more in order to improve corrosion resistance and high temperature oxidation resistance. On the other hand, if the Cr content exceeds 30.0%, the formability may deteriorate, so the Cr content is preferably in the range of 10.0 to 30.0%.
  • the amount of Cr is preferably 12.0 to 27.0%, and most preferably 13.0 to 25.0%.
  • Si acts as a deoxidizing element and improves high-temperature oxidation resistance.
  • Si may be contained by 0.01% or more.
  • the Si content is preferably 2.00% or less.
  • the amount of Si is preferably 0.01 to 1.50%, and more preferably 0.10 to 1.20%.
  • P is an element inevitably mixed from the raw material.
  • P is a grain boundary segregation element, and if it is contained too much, the cold workability and toughness of the steel sheet are deteriorated, so the P content is preferably 0.030% or less.
  • S is an element inevitably mixed in from the raw material as in P. Since S is an element that degrades corrosion resistance and formability, the S content is preferably 0.010% or less.
  • Mn acts as a deoxidizer. Further, grain boundary embrittlement due to segregation of S to the crystal grain boundary can be prevented. In order to obtain these effects, Mn may be contained by 0.10% or more. However, if the amount is too large, the cold workability of the steel sheet is lowered. Therefore, the Mn content should be 2.00% or less. The amount of Mn is preferably 0.10 to 1.80%, more preferably 0.12 to 1.50%.
  • N is preferable to be 0.050% or less because the moldability deteriorates as the content increases.
  • the amount of N is preferably 0.040% or less, and more preferably 0.030% or less.
  • the amount of N is preferably 0.001% or more.
  • Ni improves the hot workability of the ferritic stainless steel sheet of this embodiment.
  • Ni may be contained by 0.1% or more. However, if Ni is contained excessively, the stability of ferrite decreases, so the Ni content should be 2.0% or less.
  • the amount of Ni is preferably 1.5% or less, and more preferably 1.2% or less.
  • the ferritic stainless steel sheets of the first and second embodiments are composed of Fe and impurities inevitably mixed in addition to the above-described component elements.
  • the ferritic stainless steel plates of the first embodiment and the second embodiment may further contain Ti and Nb as optional components.
  • Ti and Nb are carbonitride-forming elements and are elements that improve formability. For this reason, what is necessary is just to contain either one or both among Ti and Nb as needed. In order to obtain the effect of improving the formability, 0.002% or more of Ti and 0.002% or more of Nb may be contained. However, excessive addition of Ti and Nb leads to deterioration of workability and toughness. Therefore, when these are contained, Ti: 0.50% or less and Nb: 1.00% or less are preferable. . More preferably, Ti: 0.45% or less, Nb: 0.95% or less, still more preferably Ti: 0.40% or less, Nb: 0.90% or less.
  • ferritic stainless steel plates of the first embodiment and the second embodiment may contain one or more elements shown below as required.
  • Sn is an effective element for improving the corrosion resistance. In order to obtain this effect, 0.005% or more of Sn may be contained. However, if it exceeds 1.00%, the toughness deteriorates, so the Sn content is made 1.00% or less. Sn amount becomes like this. Preferably it is 0.60% or less, More preferably, it is 0.50% or less.
  • Mo is an effective element for improving the corrosion resistance.
  • Mo may be contained by 0.002% or more. However, if it exceeds 1.00%, the toughness deteriorates, so the Mo amount is made 1.00% or less.
  • the Mo amount is preferably 0.70% or less, and more preferably 0.50% or less.
  • Al like Mo, exhibits an effect of improving corrosion resistance. In order to obtain this effect, 0.002% or more of Al may be contained. However, if it is contained excessively exceeding 1.000%, manufacturability and workability are lowered.
  • the amount of Al is preferably 0.300% or less, and more preferably 0.100% or less.
  • Mg forms Mg oxide in molten steel and acts as a deoxidizer. Moreover, Mg acts as a crystallization nucleus of TiN and can finely produce a ferrite phase during solidification. By refining the solidified structure, the surface defects of the steel sheet due to the coarse solidified structure can be prevented, and the workability is improved. For this reason, Mg is contained as necessary. In order to obtain this effect, 0.001% or more of Mg may be contained. However, if it exceeds 0.010% and is contained excessively, manufacturability and workability are lowered. The amount of Mg is preferably 0.009% or less, and more preferably 0.008% or less.
  • Co like Mo
  • Co exhibits an effect of improving corrosion resistance.
  • 0.002% or more of Co may be contained. However, if it is contained excessively exceeding 1.000%, it leads to an increase in alloy cost and a decrease in manufacturability.
  • the amount of Co is preferably 0.400% or less, and more preferably 0.200% or less.
  • V forms a carbonitride and exhibits the effect of improving the strength of the steel material.
  • V may be contained by 0.002% or more. However, if it exceeds 0.50% and it contains excessively, manufacturability and workability will be reduced.
  • the amount of V is preferably 0.20% or less, and more preferably 0.10% or less.
  • Zr like V, forms carbonitrides and exhibits the effect of improving the strength of the steel material.
  • Zr may be contained by 0.003% or more. However, if it exceeds 0.10% and is contained excessively, manufacturability and workability are lowered.
  • the amount of Zr is preferably 0.08% or less, and more preferably 0.05% or less.
  • REM, La, B, and Ca are all elements that affect the existence form of S in steel, and are included as necessary when improving hot workability.
  • REM: 0.003% or more, La: 0.002% or more, B: 0.0002% or more, Ca: 0.002% or more may be contained.
  • the upper limit of these elements is REM: 0.100% or less, La: 0.100% or less, B: 0.0100% or less, Ca: 0.010% or less, and preferable upper limits are REM: 0.00. 080% or less, La: 0.095% or less, B: 0.0095% or less, Ca: 0.009% or less, and more preferable ranges are REM: 0.050% or less and La: 0.050%, respectively.
  • Ca 0.007% or less.
  • REM in this embodiment means Sc, Y, and elements having atomic numbers 58 to 71.
  • ferritic stainless steel sheet according to the present embodiment described above can be suitably applied to coin applications that require antibacterial properties.
  • softened ferritic stainless steel sheet according to the present embodiment can be applied to cases where further softening is required for coin applications.
  • a hot rolling process, a cold rolling process, and a finish pickling process are sequentially performed on the stainless steel having the above component composition.
  • a first pickling step immersed in a 5.0 to 35.0% by mass sulfuric acid aqueous solution, 1.0 to 15.0% by mass nitric acid, and 0.5 to 5.
  • a second pickling step of immersing in an acid solution containing a 0% by mass hydrofluoric acid aqueous solution is performed.
  • the first pickling step immersed in the sulfuric acid aqueous solution and the second pickling step immersed in the acid solution containing nitric acid and hydrofluoric acid aqueous solution may be performed in this order, or in reverse order.
  • the reason for pickling the surface of the stainless steel sheet is to remove the scale film adhering by heat treatment and to increase the Cu concentration of the surface by preferentially pickling and dissolving Fe and Cr.
  • various acid solutions have been proposed as such acids.
  • first pickling step and a specific concentration nitric hydrofluoric acid pickling step (second pickling step) were performed.
  • first pickling step and a specific concentration nitric hydrofluoric acid pickling step
  • the other surface characteristics described above were also obtained, and it was found that antibacterial properties were exhibited.
  • the acid solution used for pickling must be under the following conditions. That is, the concentration of the sulfuric acid aqueous solution needs to be in the range of 5.0 to 35.0% by mass. When the concentration of the sulfuric acid aqueous solution is less than 5.0% by mass, the dissolution reaction of the scale and the steel by the aqueous acid solution hardly proceeds, so that Cu may not be concentrated on the surface. On the other hand, when the concentration of the sulfuric acid aqueous solution exceeds 35.0% by mass, the dissolution reaction with the acid aqueous solution proceeds remarkably, resulting in significant unevenness due to dissolution. This level of unevenness results in a streak or uneven pattern on the product plate, thus reducing product quality. For this reason, the concentration of the sulfuric acid aqueous solution is preferably 6.0 to 34.0% by mass, and more preferably 8.0 to 33.0% by mass.
  • the nitric hydrofluoric acid aqueous solution needs to have a nitric acid concentration of 1.0 to 15.0 mass% and a hydrofluoric acid concentration of 0.5 to 5.0 mass%.
  • a nitric acid concentration is less than 1.0% by mass, since the dissolution reaction hardly proceeds as in the case of sulfuric acid, Cu does not concentrate on the surface.
  • the nitric acid concentration exceeds 15.0% by mass, the dissolution reaction proceeds remarkably and the product quality is lowered.
  • hydrofluoric acid for the same reason as sulfuric acid and nitric acid, concentrations of less than 0.5% by mass and more than 5.0% by mass are not suitable as aqueous solution concentrations.
  • the nitric acid concentration is 1.2 to 14.5% by mass
  • the hydrofluoric acid concentration is 0.7 to 4.7% by mass
  • the nitric acid concentration is 1.5 to 14.0% by mass.
  • the concentration is 0.9 to 4.5% by mass.
  • the time for immersing the steel sheet in these acid solutions is appropriately selected within a range of 10 to 1000 seconds for each of the sulfuric acid aqueous solution and the nitric hydrofluoric acid aqueous solution, taking into consideration the maximum Cu concentration Cm and other physical properties in the Cu concentrated layer. do it.
  • the temperature of each acid aqueous solution is not particularly limited as long as it is a general condition. For example, it may be performed in the range of 40 to 80 ° C.
  • the feature of the manufacturing method of this embodiment is that the physical properties of the steel surface layer can be strictly controlled within the above-described range by finishing pickling with an aqueous sulfuric acid solution and an aqueous nitric hydrofluoric acid solution. Therefore, for example, the pickling order of the sulfuric acid aqueous solution and the nitric hydrofluoric acid aqueous solution can be reversed. Moreover, as long as the physical property range of the ferritic stainless steel sheet of this embodiment is not deviated, a third pickling treatment and a fourth pickling treatment may be performed in addition to the sulfuric acid aqueous solution and the nitric hydrofluoric acid aqueous solution.
  • the hot rolling process will be described.
  • the surface layer Cu is concentrated in the hot rolling stage by strictly controlling various conditions of the hot rolling process. Therefore, it was found that by subjecting the cold-rolled sheet in a state where the surface Cu concentration was concentrated by hot rolling to the finish pickling, the surface Cu concentration could be further increased and the antibacterial property could be further improved.
  • the concentration Cm can be increased to 18.0%.
  • the range of finishing temperature and winding temperature will be described.
  • Cu contained in the steel is generated as a Cu precipitate during cooling. For this reason, the amount of Cu dissolved in steel decreases.
  • the finishing temperature at the time of hot-rolled sheet production is 800-1000 ° C, using normal equipment such as water spraying, the hot-rolled sheet is cooled relatively quickly and wound at 600 ° C or less, thereby forming Cu precipitates.
  • the hot-rolled stainless steel sheet thus obtained has been found to be a cold-rolled sheet having a high Cu concentration even with normal pickling, and the maximum Cu concentration Cm is 18.0 by pickling as defined above. It turned out that it becomes a ferritic stainless steel plate which has Cu of the high concentration which is not more than% as a surface layer.
  • the steel plate temperature is 600 ° C. or less, the Cu diffusion rate in the steel is slowed and the formation of Cu precipitates is suppressed, but Cu precipitates are generated when held for a long time, so that the finish It is preferable to perform water injection winding after hot rolling and to cool the coil with water.
  • More preferable conditions in the hot rolling process are heating temperature: more than 1200 ° C., finish rolling temperature: more than 800 ° C., winding temperature: not more than 600 ° C., most preferably heating temperature: 1250 to 1300 ° C., finishing Rolling temperature: 900 to 1000 ° C., winding temperature: 500 ° C. or less.
  • the above-described stainless steel plate having antibacterial properties according to this embodiment is annealed at 900 to 1100 ° C. under the condition of the finish annealing step after cold rolling, and 400 ° C. at an average cooling rate of 3 ° C./second or more. By cooling to a level, it can be softened to a hardness equal to or lower than that specified in the present embodiment.
  • the solution temperature (finish annealing temperature) is equal to or higher than the temperature at which Cu can be dissolved, the influence on hardness is small. Therefore, in order to grasp the influence of the solution temperature on the hardness, solution heat treatment (finish annealing) was performed at various temperatures within a range of 700 to 1100 ° C., and then water cooling was performed. As a result, the hardness hardly changed at a solution temperature of 900 ° C. or higher, and the influence on the hardness was less than Hv10. Moreover, it becomes Hv hardness which satisfy
  • the average cooling rate of 3 ° C./second or more can be controlled by ordinary equipment such as gas blowing.
  • Cu precipitation tends to be suppressed as the cooling rate increases, and is effective for softening. Therefore, the upper limit of the average cooling rate is not particularly set, and may be appropriately determined in consideration of the performance of the cooling equipment to be used.
  • the cooling end temperature is 400 ° C. or less.
  • the cooling control is performed at 900 to 1100 ° C. after solution heat treatment at an average cooling rate of 3 ° C./second or more to various temperatures, and then natural cooling (average cooling rate of 3 ° C. ⁇ / Second).
  • the cooling end temperature was set to 400 ° C. or lower, it was possible to soften the Hv hardness satisfying the above formula (a) defined in the present embodiment.
  • the cooling end temperature was 500 to 700 ° C., significant hardening was confirmed. In this hardened specimen, Cu precipitates of 10 to 100 nm were observed.
  • the temperature range of 500 to 700 ° C. is considered to be a nose temperature range for Cu precipitation, and it is effective for softening to pass through this Cu precipitation nose temperature range quickly, that is, to increase the cooling rate.
  • more preferable conditions are: heating temperature (finish annealing temperature): 910 to 1080 ° C., cooling completion temperature: 390 ° C. or less, average cooling rate: 3.2 ° C. /
  • the most preferable conditions are heating temperature: 920 to 1060 ° C., cooling completion temperature: 380 ° C. or lower, and average cooling rate: 3.5 ° C./second or higher, respectively.
  • the hot-rolled sheet annealing conditions after hot rolling.
  • the size of the Cu precipitates is controlled to a size that can be solutionized by finish annealing, which is a subsequent process.
  • the hot-rolled sheet annealing is performed by continuous annealing rather than batch annealing, heating to 800 to 1100 ° C., and then cooling to 400 ° C. at an average cooling rate of 1 ° C./second or more.
  • the cooling end temperature was set to 400 ° C. in order to suppress Cu precipitation. At an average cooling rate of 1 ° C./second or less, Cu precipitates are coarsened, and Cu precipitates cannot be sufficiently solutioned even by subsequent finish annealing.
  • Preferred conditions in the hot-rolled sheet annealing step are heating temperature: 810 to 1090 ° C., cooling temperature: 390 ° C. or less, and average cooling rate: 1.1 ° C./second or more, respectively, and most preferred conditions are heating temperature, respectively. : 820 to 1080 ° C, cooling temperature: 380 ° C or less, average cooling rate: 1.2 ° C / second or more.
  • the ferritic stainless steel sheet and the manufacturing method thereof excellent in antibacterial properties of the first embodiment and the second embodiment good antibacterial properties can be exhibited over the entire area of the plate surface, and conventionally Thus, good antibacterial properties can be obtained with a good yield.
  • the maximum Cu concentration on the steel surface can be increased to an unprecedented level, thereby further improving antibacterial properties. Can be obtained.
  • the Cu content of the Cu-containing ferritic stainless steel is preferably 0.3 to 1.7%.
  • Example 1 Steels having the compositions shown in Table 1A and Table 1B are melted by vacuum melting, hot-rolled at a heating temperature of 1100 to 1350 ° C. and a finishing hot rolling temperature of 700 to 1020 ° C., and at a winding temperature of 400 to 700 ° C. Winded up.
  • atmosphere was performed, and normal pickling was performed.
  • cold rolling was performed and finish annealing was performed to obtain a cold rolled sheet having a thickness of 1.0 to 1.3 mm. Thereafter, it was pickled with sulfuric acid at 40 to 80 ° C. and nitric hydrofluoric acid to produce a ferritic stainless steel sheet.
  • the column labeled “-” indicates that measurement was not performed because the element was not added.
  • evaluation was performed on the obtained ferritic stainless steel sheet.
  • evaluation was performed covering the plate width direction in which a difference in antibacterial properties occurred. That is, a large number of 50 mm square test pieces were cut out in the plate width direction at arbitrary points in the length direction of each steel plate. And all these test pieces were evaluated.
  • the C, O, Fe, Cr, Si, Mn, Nb, Ti, Al, and Cu concentration distribution from the steel surface to about 800 nm was measured by glow discharge emission analysis (GDS).
  • GDS glow discharge emission analysis
  • the Cu, Fe, and Cr concentrations in the Cu enriched layer changed in the depth direction as shown in the example of FIG.
  • the concentration distribution was calculated again excluding C, it changed in the depth direction as in the example shown in FIG. 2, and it was found that a Cu concentrated layer was formed on the stainless steel surface.
  • the maximum Cu concentration of the Cu concentrated layer was Cm.
  • the Fe / Cr ratio obtained from the ratio of the Fe concentration and the Cr concentration at the depth where the maximum Cu concentration Cm was obtained was also obtained.
  • FIG. 2 is an example of the steel of the present invention, and the maximum Cu concentration Cm was 75.0%.
  • concentration Cm is obtained was 2.9.
  • Antibacterial evaluation was in accordance with ISO 22196. 1 ml of the test bacterial solution was applied to each of the above-mentioned test pieces, allowed to stand at 25 ° C. for 36 hours, and then the bacterial solution was wiped off and shaken out into the diluted solution. A predetermined amount of the shake-out solution was mixed with the measurement medium, cultured at 35 ° C. for 24 hours, and then the antibacterial activity value was measured. Steel having an antibacterial activity value of 2.0 or more was evaluated as steel having excellent antibacterial properties to suppress the growth of bacteria, and indicated as “B” (Good) in the antibacterial property evaluation in the table.
  • the antibacterial activity value was 4.0 or more, it was evaluated as steel having particularly excellent antibacterial properties, and indicated as “A” (Excellent) in the antibacterial property evaluation in the table.
  • A Excellent
  • C Breast-C
  • the antibacterial activity value was less than 2.0, the steel was evaluated as being inferior in antibacterial properties, and “C” (Bad) was indicated in the antibacterial properties evaluation in the table.
  • the table there is only one numerical value for each steel material, but among the measured specimens, the one with the lowest antibacterial property in the antibacterial evaluation is described, and the result of the surface component concentration is the most. The measurement result of the test piece with low antibacterial property is shown. This is because, if the antibacterial activity value of the test piece with the lowest antibacterial property among the test pieces in the plate width direction of each steel material is 2.0 or more, the entire plate surface of the steel material has antibacterial properties. It is.
  • Tables 2-14 Evaluation results are shown in Tables 2-14.
  • Tables 2 to 7 (Test Nos. 1 to 276) show the evaluation results when pickling in this order using nitric hydrofluoric acid as the first pickling solution and sulfuric acid as the second pickling solution.
  • Tables 8 to 14 (Test Nos. 277 to 551) show the results when the pickling order is changed and the first pickling solution is sulfuric acid and the second pickling solution is nitric hydrofluoric acid. It is an evaluation result.
  • the column labeled “-” indicates that the processing was not performed.
  • Test No. which is an example of the present invention manufactured by the method of this embodiment. 1-180, no. Steel plates Nos. 277 to 456 showed a stable antibacterial property when the antibacterial activity value after culturing was 2.0 or more (the antibacterial property evaluation is “B”, which is a white dot plot point in FIG. 3). Furthermore, test No. manufactured with the manufacturing method which satisfy
  • Test No. which is a comparative example manufactured under conditions outside the pickling conditions defined by the method of this embodiment. 207-276, no. In the steel sheets of 482 to 551, the antibacterial activity value was less than 2.0 (the antibacterial evaluation is “C”, which is the plot point of the multiplication symbol (cross symbol) in FIG. 3). In particular, test no. 207-221 and test no. In the steel plates of 497 to 511, only the nitric hydrofluoric acid treatment was performed as the pickling treatment, so the maximum Cu concentration Cm was less than 10%, and the antibacterial property was lower than that of the present invention.
  • Example 2 Next, in order to confirm the softening effect of the present embodiment, the conditions of the hot-rolled sheet annealing step and the finish annealing step were changed to the conditions shown in Table 15 when manufacturing some of the steel types in Table 1A and Table 1B.
  • the hot rolling process, the cold rolling process, and the finish pickling process were performed under conditions within the range of the present embodiment.
  • the cross-sectional hardness was measured by the following method. Five locations were arbitrarily selected in the vicinity of the center of the plate thickness, a Vickers hardness test was performed at the selected locations, and the average value was taken as the measured value of the cross-sectional hardness. Corrosion resistance was tested in accordance with JISZ2371 by continuously spraying 308K, 5% NaOH solution for 72 hours, and the rusting condition was observed. The evaluation results are shown in Table 15.
  • the cross-sectional Hv hardness exceeds 190, or the result of not satisfying the formula (a) is obtained.
  • Test No. which is an example of the present invention manufactured under the preferable finish annealing conditions of this embodiment.
  • the Hv hardness of the steel plates 552, 555, 556, 559, 560, 563, 564, 567, 568, 571, 572, 575, 576, 579, 580, 583 is 190 or less, and the formula (a) Met.
  • the rusting was significantly less and the corrosion resistance was further improved. From this result, it was found that a steel sheet that can be applied even when softening and high corrosion resistance are required, for example, for coins, under the preferable manufacturing conditions of the present embodiment.
  • the ferritic stainless steel plate of the present embodiment exhibits good antibacterial properties over the entire area of the plate surface. Further, both softening and excellent antibacterial properties can be achieved. For this reason, the ferritic stainless steel plate of this embodiment is a handrail, a faucet or other currant, a metal coin, a metal container, a metal tableware, a bathtub, a household appliance, a toilet seat, a medical instrument, a heating instrument, or a sanitary instrument or a construction It is suitably used as a material for building materials for goods.

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WO2016035235A1 (ja) * 2014-09-05 2016-03-10 Ｊｆｅスチール株式会社 ステンレス冷延鋼板用素材
JP5924459B1 (ja) * 2014-09-05 2016-05-25 Ｊｆｅスチール株式会社 ステンレス冷延鋼板用素材
EP3181714A4 (en) * 2014-09-05 2017-07-12 JFE Steel Corporation Material for cold-rolled stainless steel sheets
US10633730B2 (en) 2014-09-05 2020-04-28 Jfe Steel Corporation Material for cold-rolled stainless steel sheet
WO2019188601A1 (ja) * 2018-03-30 2019-10-03 日鉄ステンレス株式会社 耐塩害腐食性に優れたフェライト系ステンレス鋼
JP2019178364A (ja) * 2018-03-30 2019-10-17 日鉄ステンレス株式会社 耐塩害腐食性に優れたフェライト系ステンレス鋼
US11286547B2 (en) 2018-03-30 2022-03-29 Nippon Steel Stainless Steel Corporation Ferritic stainless steel having excellent salt corrosion resistance
JP7058537B2 (ja) 2018-03-30 2022-04-22 日鉄ステンレス株式会社 耐塩害腐食性に優れたフェライト系ステンレス鋼
US20240084470A1 (en) * 2020-01-21 2024-03-14 Nippon Steel Stainless Steel Corporation Stainless steel material having antibacterial properties and antiviral properties and method for manufacturing same
CN115948635A (zh) * 2023-03-09 2023-04-11 太原科技大学 一种含铜抗菌不锈钢及其表面处理工艺
CN115948635B (zh) * 2023-03-09 2023-05-09 太原科技大学 一种含铜抗菌不锈钢及其表面处理工艺

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KR101762046B1 (ko) 2017-07-26
IN2015DN03729A (ko) 2015-09-18
CN104884657A (zh) 2015-09-02
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