WO2016167343A1 - 容器用鋼板及び容器用鋼板の製造方法 - Google Patents
容器用鋼板及び容器用鋼板の製造方法 Download PDFInfo
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- WO2016167343A1 WO2016167343A1 PCT/JP2016/062103 JP2016062103W WO2016167343A1 WO 2016167343 A1 WO2016167343 A1 WO 2016167343A1 JP 2016062103 W JP2016062103 W JP 2016062103W WO 2016167343 A1 WO2016167343 A1 WO 2016167343A1
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- chemical conversion
- steel plate
- ions
- layer
- treatment
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- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- C—CHEMISTRY; METALLURGY
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
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- B32—LAYERED PRODUCTS
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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Definitions
- the present invention relates to a steel plate for containers and a method for producing a steel plate for containers.
- metal containers made of plated steel sheets such as Ni-plated steel sheets, Sn-plated steel sheets or Sn-based alloy-plated steel sheets are often used.
- a coating may be applied to the surface of such a metal container before or after canning, or a film may be laminated. Paints and films used for surface treatment of metal containers are collectively referred to as coating agents.
- the plated steel sheet used for the base of the coating agent is subjected to a surface treatment using hexavalent chromate or the like (hereinafter referred to as chromate treatment) in order to ensure adhesion and corrosion resistance with the coating agent.
- chromate treatment hexavalent chromate or the like
- the plated steel sheet that has been subjected to chromate treatment has a coating on the film formed by chromate treatment for the purpose of imparting organic solvent resistance, fingerprint resistance, scratch resistance, lubricity, etc., if necessary.
- a coating layer made of an organic resin is formed.
- Patent Literature 2 and Patent Literature 3 below disclose cathode electrolytic treatment using a chemical conversion treatment solution containing Zr ions and F ions as a surface treatment of a plated steel sheet as an alternative to chromate treatment.
- Patent Document 4 discloses a cathodic electrolysis treatment using a chemical conversion treatment solution containing phosphate ions and at least one of Ti ions and Zr ions.
- Patent Document 5 discloses a cathodic electrolytic treatment using a chemical conversion treatment solution containing Zr ions, F ions, and phosphate ions.
- Patent Document 6 discloses a cathodic electrolysis treatment using a chemical conversion treatment solution containing Zr ions and organic substances.
- Patent Document 7 discloses a cathodic electrolysis treatment using a chemical conversion treatment solution containing Zr ions, phosphate ions, and organic substances.
- Patent Document 8 and Patent Document 9 disclose cathode electrolytic treatment using a chemical conversion treatment solution containing Zr ions, phosphate ions, and nitrate ions.
- Patent Document 9 discloses a method for promoting the formation of a film (hereinafter referred to as a chemical conversion film layer) formed by cathodic electrolysis by increasing nitrate ions.
- Patent Documents 2 to 8 have a problem in that suitable productivity cannot be obtained because it takes a long time to form the chemical conversion film layer containing the Zr compound.
- a high concentration of nitrate ions is required, which is not preferable in terms of the environment.
- Patent Documents 2 to 9 do not disclose a method for improving the anti-sulfur blackening resistance.
- the steel plate for containers is used in a food container containing, for example, high-protein food such as fish meat or beans
- the container is subjected to retort treatment (high-temperature heat sterilization treatment in the presence of water vapor) after filling the food.
- retort treatment high-temperature heat sterilization treatment in the presence of water vapor
- at least one of the inner surface and the contents may change to black. This blackening phenomenon is called sulfide blackening.
- S Sulfur contained in food is thermally decomposed by retort treatment, and hydrogen sulfide (H 2 S), thiols (HS ⁇ ) and the like are generated.
- This hydrogen sulfide and thiols react with the constituent metal on the inner surface of the container to produce black metal sulfide, and this blackening of sulfide occurs. Due to this blackening of sulfide, the appearance of the container may deteriorate. Furthermore, the generated black metal sulfide may be misunderstood by consumers as metal corrosion on the inner surface of the container or corrosion of the contents. Therefore, it is necessary to prevent the occurrence of sulfide blackening as much as possible particularly in the steel plate for containers used for food containers.
- the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a steel plate for containers having excellent productivity, environmental friendliness, and resistance to sulfur blackening, and a method for producing a steel plate for containers.
- the present invention adopts the following means in order to solve the above problems and achieve the object.
- a steel plate for a container is provided as a steel plate and an upper layer of the steel plate, and includes an Sn plating layer containing Sn of 560 to 5600 mg / m 2 in terms of metal Sn amount, Provided as an upper layer of the Sn plating layer, 3.0 to 30.0 mg / m 2 of Zr compound in terms of metal Zr amount, and 0.50 to 5.00 mg / m 2 of Mg in terms of metal Mg amount And a chemical conversion film layer containing the compound.
- the Sn plating layer may further include a Fe—Sn alloy.
- the chemical conversion coating layer has a total amount of 1.5 to at least one of phosphoric acid and phosphate converted to P amount. You may employ
- a method for manufacturing a steel plate for containers includes a plating step of forming an Sn plating layer containing 560 to 5600 mg / m 2 on a steel plate in terms of Sn as a metal Sn amount, and the plating After the process, a chemical conversion treatment film layer is formed on the Sn plating layer by performing cathodic electrolysis using a chemical conversion treatment solution containing 100 to 3000 ppm of Zr ions, 120 to 4000 ppm of F ions and 50 to 300 ppm of Mg ions.
- the steel plate on which the Sn plating layer is formed is subjected to a molten tin treatment, and at least a part of Sn in the Sn plating layer and the steel plate A configuration in which at least a part of Fe is alloyed may be employed.
- the chemical conversion treatment solution may further include a phosphate ion of 2000 ppm or less.
- the chemical conversion treatment liquid adopts a configuration further including nitrate ions and ammonium ions in total of 20000 ppm or less. May be.
- the Sn plating layer is formed using water at 10 ° C. or higher and lower than 40 ° C. before the main cleaning step.
- FIG. 1 is a schematic diagram showing a configuration of a container steel plate 10 according to the present embodiment.
- a container steel plate 10 includes a steel plate (original plate) 101 used as a base material, a Sn plating layer 103 formed on the steel plate 101, and a chemical conversion treatment film formed on the Sn plating layer 103.
- a layer 105 is shown in FIG. 1, a container steel plate 10 includes a steel plate (original plate) 101 used as a base material, a Sn plating layer 103 formed on the steel plate 101, and a chemical conversion treatment film formed on the Sn plating layer 103.
- a layer 105 is a layer of the steel plate 10 according to the present embodiment.
- the steel plate 101 is not particularly limited, and a known steel plate 101 that is generally used as a steel plate for containers can be used.
- the manufacturing method and material of these known steel plates 101 are not particularly limited.
- the steel plate 101 manufactured through known steps such as hot rolling, pickling, cold rolling, annealing, temper rolling, etc. from a normal slab manufacturing process can be used.
- an Sn plating layer 103 containing Sn is provided as an upper layer of the steel plate 101.
- the Sn plating layer 103 of the present embodiment contains 560 to 5600 mg / m 2 of Sn per side in terms of the amount of metallic Sn.
- Sn has excellent workability, weldability and corrosion resistance, but in order to exert these effects, the Sn content of the Sn plating layer 103 is 560 mg / m 2 or more per side in terms of the amount of metal Sn. It is necessary to be.
- the above effect is improved as the Sn content of the Sn plating layer 103 is increased.
- the Sn content is converted to the amount of metal Sn and exceeds 5600 mg / m 2 , the above effect is saturated. Therefore, from an economical viewpoint, the Sn content of the Sn plating layer 103 is converted to a metal Sn amount to be 5600 mg / m 2 or less per side.
- Sn content of the Sn-plated layer 103 is preferably a single-sided per 700 ⁇ 4500mg / m 2 in terms of metallic Sn amount, more preferably 1200 ⁇ 4000mg / m 2.
- the Sn plating layer 103 may be formed on both surfaces of the steel plate 101, or may be formed only on one surface of the steel plate 101 from the viewpoint of manufacturing cost reduction.
- the steel plate 101 on which the Sn plating layer 103 is formed only on one surface can be manufactured, for example, it is preferable that the surface on which the Sn plating layer 103 is formed be the inner surface of the container. .
- the Sn content of the Sn plating layer 103 can be measured by, for example, a fluorescent X-ray method.
- a calibration curve related to the Sn content is prepared in advance using a sample with a known Sn content, and the Sn content is relatively measured using the calibration curve.
- sulfide blackening the phenomenon in which a black compound such as SnS, SnS 2 , FeS, Fe 2 S 3 , or Fe 2 S is formed is referred to as sulfide blackening. Further, the resistance (characteristic) against sulfide blackening is referred to as sulfide blackening resistance.
- the container steel plate 10 includes a chemical conversion coating layer 105 as an upper layer of the Sn plating layer 103 in order to improve resistance to sulfur blackening.
- Chemical conversion coating layer 105 and in terms of metal Zr content 3.0 ⁇ Zr compound of 30.0 mg / m 2, and in terms of metal Mg content 0.50 ⁇ 5.00mg / m 2 of Mg compound Containing.
- the Zr compound contained in the chemical conversion coating layer 105 has a function of improving sulfide blackening resistance, adhesion and workability.
- Examples of the Zr compound according to this embodiment include oxidized Zr, phosphoric acid Zr, hydroxylated Zr, and fluorided Zr (including hydrates thereof), and the chemical conversion coating layer 105 includes the above-described Zr compound. Contains a plurality.
- the Zr content in the chemical conversion coating layer 105 When the Zr content in the chemical conversion coating layer 105 is increased, the resistance to blackening, adhesion and workability of the steel plate for containers 10 are improved. Specifically, when the Zr content of the chemical conversion coating layer 105 is 3.0 mg / m 2 or more per side in terms of the metal Zr content, practically suitable sulfur blackening resistance is ensured. On the other hand, when the Zr content exceeds 30.0 mg / m 2 per side in terms of the metal Zr content, the chemical conversion coating layer 105 becomes too thick, the adhesion of the chemical conversion coating layer 105 itself deteriorates, and is resistant to sulfuration. Black denaturation is reduced.
- the Zr content of the chemical conversion coating layer 105 is 3.0 to 30.0 mg / m 2 per side in terms of the metal Zr content.
- the lower limit of the Zr content is preferably 5.0 mg / m 2 or more, more preferably 8.0 mg / m 2 or more per side, in terms of metal Zr content.
- the upper limit value of the Zr content is preferably 20.0 mg / m 2 or less, more preferably 15.0 mg / m 2 or less per side in terms of the metal Zr content.
- the chemical conversion film layer 105 contains an Mg compound in addition to the Zr compound.
- the chemical conversion treatment liquid used when forming the chemical conversion treatment film layer 105 contains Mg ions, and the Mg ions in the chemical conversion treatment solution are mixed with the Zr compound as an Mg compound in the chemical conversion treatment film layer 105. It is captured.
- the Mg compound in the chemical conversion coating layer 105 may be partially removed from the chemical conversion coating layer 105 in the cleaning step performed after the chemical conversion coating layer 105 is formed, but the remainder is the chemical conversion coating layer 105. Remains in. The present inventors have found that when the chemical conversion film layer 105 contains a Mg compound, the resistance to sulfur blackening is improved.
- Examples of the Mg compound contained in the chemical conversion coating layer 105 include Mg oxide, Mg hydroxide, Mg fluoride, Mg phosphate (including hydrates thereof), and the chemical conversion coating layer 105 is the above-mentioned.
- a plurality of Mg compounds may be contained. These Mg compounds are generally transparent or white.
- Mg ions combine with thiol ions (HS ⁇ ) or hydrogen sulfide (H 2 S), which are the main component of the sulfide blackening phenomenon, to form a transparent or white compound.
- the Mg compound in the chemical conversion coating layer 105 suppresses the transmission of thiol ions and hydrogen sulfide through the chemical conversion coating layer 105. Moreover, the compound produced
- the chemical conversion coating layer 105 contains 0.50 to 5.00 mg / m 2 of Mg compound per side in terms of the amount of metallic Mg.
- the Mg content in the chemical conversion coating layer 105 is 0.50 mg / m 2 or more per side in terms of the amount of metallic Mg, it has practically suitable sulfur blackening resistance.
- the chemical conversion treatment film layer 105 in order for the chemical conversion treatment film layer 105 to contain Mg compound of more than 5.00 mg / m 2 per side in terms of the amount of metallic Mg, it is necessary to add a large amount of Mg compound to the chemical conversion treatment solution. .
- the chemical conversion treatment film layer 105 may not proceed properly, which is not preferable. Further, since the chemical conversion coating layer 105 contains Mg compound of more than 5.00 mg / m 2 per side in terms of the amount of metal Mg, the adhesion (primary adhesion) with the coating agent is not affected. However, it is not preferable because adhesion (secondary adhesion), rust resistance, or corrosion resistance under the coating film may be deteriorated during high-temperature sterilization treatment in the presence of water vapor such as retort treatment.
- the chemical conversion coating layer 105 contains an Mg compound in excess of 5.00 mg / m 2 per side in terms of the amount of metallic Mg, when the steel plate 10 for containers is used for a food container, the taste or flavor of the contents Is unfavorable because it may damage the process.
- the lower limit of the content of the Mg compound in the chemical conversion film 105 is preferably 0.80 mg / m 2 per side, more preferably 1.00 mg / m 2 in terms of the amount of metallic Mg.
- the upper limit of the amount of the Mg compound of the chemical conversion coating layer 105 is preferably a single-sided per 4.00 mg / m 2 in terms of metallic Mg amount, and more preferably from 3.00 mg / m 2.
- the amount of Zr compound or Mg compound in the chemical conversion coating layer 105 is the total content of metal Zr or metal Mg in the chemical conversion coating layer 105 quantified by, for example, a quantitative analysis method such as fluorescent X-ray analysis, It means the content of the Zr compound or Mg compound remaining in the chemical conversion coating layer 105 after the cleaning step described later.
- Sn plating layer 103 contains Mg
- Mg of steel plate 10 for containers after performing a chemical conversion treatment process The amount of compound can be measured, and the amount of Mg compound in the chemical conversion coating layer 105 can be measured from the difference between the two.
- the chemical conversion film layer 105 may contain at least one of phosphoric acid and phosphate in addition to the Zr compound and the Mg compound.
- the phosphate contained in the chemical conversion coating layer 105 include Zr phosphate and Mg phosphate (including hydrates thereof).
- the chemical conversion film layer 105 may contain a plurality of compounds among compounds composed of phosphoric acid and phosphate.
- the chemical conversion treatment film layer 105 contains at least one of phosphoric acid and phosphate, excellent sulfurization blackening resistance and adhesion can be obtained.
- the total content of phosphoric acid and phosphate is 1.5 mg / m 2 or more per side in terms of the amount of P, practically suitable sulfurization blackening resistance and adhesion can be obtained.
- the sulfur blackening resistance and adhesion are also improved.
- the total content of phosphoric acid and phosphate is converted to P amount by 25. If it exceeds 0 mg / m 2 , the adhesiveness of the phosphoric acid or phosphate in the chemical conversion coating layer 105 is deteriorated, so that the adhesiveness with the coating agent and the corrosion resistance under the coating film are lowered. Further, if the total content of phosphoric acid and phosphate exceeds 25.0 mg / m 2 per side in terms of P amount, the electrical resistance increases and the weldability deteriorates, which is not preferable.
- the chemical conversion treatment film layer 105 preferably contains phosphoric acid and phosphate in a total amount of 1.5 to 25.0 mg / m 2 per side in terms of P amount.
- the lower limit of the total content of phosphoric acid and phosphate is more preferably 2.5 mg / m 2 per side in terms of P amount, and even more preferably 5.0 mg / m 2 .
- the upper limit of the total content of phosphoric acid and phosphate is more preferably 20.0 mg / m 2 per side, more preferably 12.5 mg / m 2 in terms of P amount.
- the total amount of phosphoric acid and phosphate contained in the chemical conversion coating layer 105 is the amount of P contained in the chemical conversion coating layer 105 after the cleaning process, for example, a quantitative analysis method such as fluorescent X-ray analysis. Can be quantified.
- FIG. 2 is a flowchart showing a method for manufacturing the container steel plate 10 according to the present embodiment.
- the manufacturing method of the steel plate 10 for containers has a plating process, a chemical conversion treatment process, and a washing process.
- Sn plating is performed on the surface of the steel plate 101 to form the Sn plating layer 103 (step S101).
- the Sn plating method is not particularly limited, and a known technique such as an electroplating method, a vacuum evaporation method, or a sputtering method can be used.
- As the Sn plating bath a ferrostan bath or the like can be used.
- the molten tin treatment may be performed after the plating step.
- a chemical conversion treatment step is performed to form a chemical conversion treatment film layer 105 on the Sn plating layer 103 (step S103).
- a chemical conversion treatment step cathodic electrolysis using a chemical conversion solution is performed.
- the immersion treatment method is used as the formation method of the chemical conversion treatment film layer 105, since the base is etched, adhesion of the chemical conversion treatment coating layer 105 becomes non-uniform and the time of the chemical conversion treatment step becomes long. This is not preferable for industrial production.
- the cathode electrolytic treatment is preferable because the surface of the chemical conversion treatment film layer 105 to be formed is cleaned by forced charge transfer and hydrogen generation at the interface between the steel plate 101 and the chemical conversion treatment liquid. Further, cathodic electrolysis is preferable because the adhesion of the chemical conversion treatment film layer 105 is promoted by increasing the pH of the chemical conversion treatment solution.
- the conditions for the cathodic electrolysis are not particularly limited.
- the conditions of the temperature of the chemical conversion treatment solution at 10 ° C. to 60 ° C., the current density of 0.1 to 20.0 A / dm 2 , and the treatment time of 0.01 to 30 seconds. Can be done below.
- the pH of the chemical conversion solution is preferably in the range of 3.0 to 4.5. Nitric acid or hydrofluoric acid or the like is added to lower the pH, and ammonia or the like is added to increase the pH. Adjust it.
- the chemical conversion treatment solution used in the chemical conversion treatment step contains 100 to 3000 ppm of Zr ions.
- Zr ions in the chemical conversion treatment liquid are taken into the chemical conversion treatment film layer 105 as a Zr compound.
- the lower limit value of Zr ions in the chemical conversion liquid is preferably 500 ppm, more preferably 1000 ppm.
- the upper limit value of Zr ions in the chemical conversion treatment liquid is preferably 2500 ppm, more preferably 2000 ppm.
- the chemical conversion treatment solution contains 120 to 4000 ppm of F ions.
- F ions form a complex ion with Zr ions, thereby stabilizing Zr ions in the chemical conversion solution.
- the F ions in the chemical conversion solution are also taken into the chemical conversion coating layer 105 in the same manner as the Zr ions, but it is preferable to remove the F compound in the chemical conversion coating layer 105 as much as possible by a cleaning step described later.
- the chemical conversion treatment solution contains 50 to 300 ppm of Mg ions. It is preferable that the chemical conversion treatment solution contains Mg ions because the chemical conversion treatment film layer 105 contains an Mg compound and improves the resistance to sulfur blackening. Further, Mg ions can promote the precipitation of Zr ions. Specifically, when the amount of Zr compound in the chemical conversion treatment film layer 105 formed by the chemical conversion treatment step is compared between the case where the chemical conversion treatment solution contains Mg ions and the case where it does not contain Mg ions, it contains Mg ions. In some cases, the amount of Zr compound is contained in the chemical conversion coating layer 105 more.
- the cause of the Zr precipitation promoting effect by Mg ions is considered as follows.
- the Zr ions exist stably in the state of complex ions such as [ZrF 6 ] 2 ⁇ together with the F ions.
- the pH rises due to forced charge transfer and hydrogen generation at the interface between the steel plate 101 and the electrolysis solution.
- the complex ions are hydrolyzed to become Zr ions and F ions as shown in the above formula (1), and then the chemical conversion coating layer 105 containing the Zr compound is deposited.
- the reaction of the above formula (1) is an equilibrium (reversible) reaction, when the F ions in the chemical conversion solution increase, the rightward reaction of the above formula (1) (reaction in which complex ions decompose) Is significantly inhibited.
- F -] is such that dissociated into F ions and Mg ions, added during the chemical conversion treatment solution It is preferable to adjust the Mg ion concentration. As described above, when the chemical conversion solution contains Mg ions, the precipitation of Zr is promoted. Therefore, the manufacturing method of the steel plate 10 for containers which concerns on this embodiment can shorten the time which a chemical conversion treatment process requires, and has the outstanding productivity.
- the Mg ion concentration added to the chemical conversion solution is preferably 50 to 300 ppm. If the Mg ion concentration is less than 50 ppm, it is insufficient to exhibit the effect of promoting the precipitation of Zr. On the other hand, when the Mg ion concentration is more than 300 ppm, it is not preferable because it becomes easy to form poorly soluble MgF 2 .
- the Mg ion concentration added to the chemical conversion treatment liquid is more preferably 100 to 200 ppm. In addition, it is preferable to add Mg ion with a water-soluble salt such as Mg nitrate or Mg sulfate.
- the chemical conversion treatment solution may contain 2000 ppm or less of phosphate ions. It is preferable that the chemical conversion treatment liquid contains phosphate ions, because the chemical conversion treatment film layer 105 contains phosphoric acid or a phosphate, which improves sulfurization blackening resistance and adhesion.
- the chemical conversion treatment liquid may contain a total of 20000 ppm or less of nitrate ions and ammonium ions. It is preferable that the chemical conversion treatment solution contains nitrate ions and ammonium ions because the time required for the chemical conversion treatment step can be shortened and productivity is improved. In addition, it is preferable that a chemical conversion liquid contains both a nitrate ion and an ammonium ion instead of any one of a nitrate ion and an ammonium ion. The reason is as follows. When forming the chemical conversion treatment film layer 105 containing Zr, first, H 2 is generated at the cathode by the reaction of the following formula (2), and the pH rises.
- first, cathodic electrolysis using a first chemical conversion treatment liquid is performed, and the first layer (not shown) of the chemical conversion treatment film layer 105 on the Sn plating layer 103 side.
- the second layer (not shown) of the chemical conversion coating layer 105 is formed on the first layer of the chemical conversion coating layer 105 by performing cathodic electrolysis using a second chemical conversion solution. You may let them.
- a 1st chemical conversion liquid and a 2nd chemical conversion liquid contain the same component, and only temperature differs. Examples of the temperature of the first chemical conversion treatment liquid include 10 ° C.
- the temperature of the second chemical conversion treatment liquid examples include 45 ° C. to 60 ° C. Since the first layer of the chemical conversion coating layer 105 is a dense layer, it is suitable for ensuring characteristics such as resistance to sulfur blackening. Since the second layer of the chemical conversion coating layer 105 has a rough surface, it is suitable for ensuring adhesion between the chemical conversion coating layer 105 and the coating agent.
- a cleaning treatment for 0.5 seconds or more is performed with water of 40 ° C. or higher (step S107).
- the upper limit of the temperature of water used in the main cleaning process is not particularly limited, but is, for example, 90 to 100 ° C.
- the upper limit of the cleaning time of the main cleaning process is not particularly limited, but is, for example, 10 seconds.
- the temperature is 10 ° C. or higher and lower than 40 ° C. It is preferable to perform a cleaning process (hereinafter referred to as a preliminary cleaning process) for 0.5 seconds or more with water (step S105).
- a cleaning process hereinafter referred to as a preliminary cleaning process
- the upper limit of the cleaning time in the preliminary cleaning step is not particularly limited, but is, for example, 20 seconds. Examples of the cleaning method in the preliminary cleaning step and the main cleaning step include an immersion process or a spray process.
- the ionic species eluting at a low temperature are removed by the preliminary washing step, and the ionic species eluting at a high temperature are removed by the main washing step.
- the removal effect is improved by increasing the processing time of the preliminary cleaning step and the main cleaning step.
- the removal effect improves the cleaning liquid used for this cleaning process, so that temperature is high. When each processing time is less than 0.5 seconds, it is difficult to reduce the ionic species.
- F ions, nitrate ions, ammonium ions, and the like are preferably removed from the chemical conversion coating layer 105 as much as possible by a cleaning process, but may not be completely removed and may remain unavoidably.
- Example shown below is only an example of the manufacturing method of the steel plate for containers and the steel plate for containers which concerns on embodiment of this invention, The manufacturing method of the steel plate for containers and the steel plate for containers which concerns on embodiment of this invention is However, the present invention is not limited to the following examples.
- the treatment liquids 1-1 to 3-2 in Table 1 are all at the same temperature and pH, and are subjected to cathodic electrolysis under the same current density and treatment time. As shown in Table 1, the addition of Mg ions increased the Zr content of the formed chemical conversion coating layer, indicating that Mg ions have a Zr precipitation promoting effect. .
- Test materials were prepared using a chemical conversion treated steel sheet having a Sn plating layer and a chemical conversion coating layer shown in Table 2, and performance evaluation was performed on the following items (A) to (H). The evaluation results are shown in Table 3.
- the case where the peel area ratio is 0% is “Very Good”, the case where the peel area ratio is more than 0% and 5% or less is “Good”, and the case where the peel area ratio is more than 5% and 30% or less is “ The case where “Fair” and the peeled area ratio exceeded 30% was evaluated as “Poor”.
- (G) Corrosion resistance under coating film An epoxy-phenol resin was applied to the test material, and a baking treatment was performed at a temperature of 200 ° C. for 30 minutes. Thereafter, a grid-like cut having a depth reaching the base iron was made, and immersed in a test solution composed of a 1.5% citric acid-1.5% salt solution at a temperature of 45 ° C. for 72 hours. After washing and drying, the tape was peeled off. The corrosion condition under the coating film and the corrosion condition of the flat plate part were observed at the cut portion, and the corrosion resistance under the coating film was evaluated from the evaluation of the width of the corrosion under the coating film and the corrosion area ratio of the flat plate part.
- the corrosion width under the coating film is less than 0.2 mm and the corrosion area ratio of the flat plate portion is 0% is “Very Good”, the corrosion width under the coating film is 0.2 mm or more and less than 0.3 mm and the flat plate portion.
- (H) Retort rust resistance The test material was retorted at a temperature of 125 ° C. for 30 minutes. Thereafter, the state of rust generation was observed, and the retort rust resistance was evaluated from the rust generation area ratio. Specifically, the case where the rust generation area rate is 0% is “Very Good”, the case where the rust generation area rate is more than 0% and 1% or less is “Good”, and the rust generation area rate is more than 1% and 5% or less. The case was evaluated as “Fair”, and the case where the rust generation area ratio exceeded 5% was evaluated as “Poor”.
- the chemical conversion treatment steel plate was manufactured with the following method.
- the production conditions are shown in Table 4.
- ⁇ Sn plated steel plate> Using the following method (Treatment Method 1) or (Treatment Method 2), an Sn plating layer was formed on a steel plate having a thickness of 0.17 to 0.23 mm to produce an Sn plated steel plate.
- a chemical conversion treatment film layer was formed by dissolving cathode Zr and phosphoric acid and performing a cathodic electrolytic treatment using a chemical conversion treatment solution to which Mg nitrate was added.
- a chemical conversion treatment film layer was formed by dissolving cathode Zr and ammonium nitrate and performing a cathodic electrolytic treatment using a chemical conversion treatment solution to which Mg nitrate was added.
- a chemical conversion treatment film layer was formed by dissolving Zr fluoride, phosphoric acid and ammonium nitrate and performing a cathodic electrolytic treatment using a chemical conversion treatment solution to which Mg nitrate was added.
- a chemical conversion treatment film layer was formed by performing immersion treatment using a chemical conversion treatment solution in which Zr fluoride was dissolved and Mg nitrate was added.
- the Zr adhesion promoting rate obtained by dividing the Zr content of each test material by the Zr content of the steel sheet for Mg-free containers.
- the Zr adhesion promoting rate is 1.3 or more is “Very Good”, the case where it is less than 1.3 to 1.2 or more is “Good”, the case where it is less than 1.2 to 1.1 or more The case where “Fair” was less than 1.1 was evaluated as “Poor”.
- Inventive Examples B1 to B26 all have an effect of promoting Zr adhesion by adding Mg ions, and have excellent sulfur blackening resistance, workability, weldability, film adhesion, primary paint adhesion, and secondary paint adhesion. And had corrosion resistance and corrosion resistance under the coating film. Furthermore, when the chemical conversion coating layer contains 1.5 mg / m 2 or more of phosphoric acid or phosphate as the amount of P, film adhesion (including processability) and undercoat corrosion resistance are further improved.
- Comparative Examples b1 to b8 have no effect of promoting Zr adhesion, and are also resistant to sulfur blackening, weldability, workability, weldability, film adhesion, primary paint adhesion, secondary paint adhesion, coating film. At least some of the properties of undercorrosion resistance and corrosion resistance were inferior.
- Comparative Example b6 since the amount of Mg ions in the chemical conversion treatment solution was excessive, poorly soluble MgF 2 was formed, Mg ions did not function sufficiently as a scavenger, and the effect of promoting the precipitation of Zr by Mg ions is preferable. Probably not.
- Comparative Example b8 immersion treatment was used instead of cathodic electrolysis treatment, and the amount of Zr compound in the chemical conversion treatment film layer was small even when the chemical conversion treatment solution contained Mg ions. For this reason, it is considered that the effect of promoting the precipitation of Zr by Mg ions was not suitable.
Abstract
Description
本願は、2015年4月16日に、日本に出願された特願2015-83984号に基づき優先権を主張し、その内容をここに援用する。
コーティング剤の下地に用いられるめっき鋼板には、コーティング剤との密着性及び耐食性を確保するために、6価クロム酸塩等を用いた表面処理(以下、クロメート処理と呼称する)が施されることが多い(例えば、下記の特許文献1を参照。)。さらに、クロメート処理が施されためっき鋼板は、必要に応じて、耐有機溶剤性、耐指紋性、耐傷つき性又は潤滑性等を付与することを目的として、クロメート処理により形成された皮膜の上に、有機樹脂からなる被覆層が形成される。
例えば、下記の特許文献2及び特許文献3には、クロメート処理の代替となるめっき鋼板の表面処理として、Zrイオン及びFイオンを含む化成処理液を用いた陰極電解処理が開示されている。
下記の特許文献5には、Zrイオン、Fイオン及びリン酸イオンを含有する化成処理液を用いた陰極電解処理が開示されている。
下記の特許文献6には、Zrイオン及び有機物を含む化成処理液を用いた陰極電解処理が開示されている。
下記の特許文献8及び特許文献9には、Zrイオン、リン酸イオン及び硝酸イオンを含む化成処理液を用いた陰極電解処理が開示されている。特に、下記の特許文献9では、硝酸イオンを増加することにより、陰極電解処理により形成される皮膜(以下、化成処理皮膜層と呼称する)の形成を促進させる方法が開示されている。
容器用鋼板を、例えば、魚肉又は豆類等の高蛋白質食品を内容物とする食品用容器に用いた場合には、食品充填後のレトルト処理(水蒸気存在下での高温加熱滅菌処理)により、容器内面と内容物との少なくとも一方がまれに黒色に変色する場合がある。このような黒変現象を硫化黒変という。
食品中に含まれる硫黄(S)が、レトルト処理により熱分解して、硫化水素(H2S)及びチオール類(HS-)等が発生する。この硫化水素及びチオール類と、容器内面の構成金属とが反応を起こし、黒色の金属硫化物が生成するため、この硫化黒変が生じる。
この硫化黒変が原因となり、容器の外観が悪くなる場合がある。さらに、発生した黒色の金属硫化物を、消費者が容器内面の金属腐食又は内容物の腐食と誤解する場合がある。そのため、特に食品用容器に用いる容器用鋼板では、硫化黒変を極力発生しないようにする必要がある。
(容器用鋼板)
最初に、容器用鋼板10について説明する。
図1は、本実施形態に係る容器用鋼板10の構成を示す模式図である。図1に示すように、容器用鋼板10は、母材として用いられる鋼板(原板)101と、鋼板101上に形成されたSnめっき103層と、Snめっき層103上に形成された化成処理皮膜層105と、を備える。
Snは優れた加工性、溶接性及び耐食性を有するが、これらの効果を発揮するためには、Snめっき層103のSn含有量が、金属Sn量に換算して片面当たり560mg/m2以上であることが必要である。
Snめっき層103のSn含有量が増加するほど上記の効果は向上するが、Sn含有量が金属Sn量に換算して片面当たり5600mg/m2超過では、上記の効果は飽和する。従って、経済的な観点から、Snめっき層103のSn含有量を金属Sn量に換算して片面当たり5600mg/m2以下とする。
Snめっき層103の形成後に溶融溶錫処理を行なうことにより、Snめっき層103の少なくとも一部が、鋼板中の少なくとも一部のFeとFe-Sn合金を形成する。これにより、耐食性及び表面の外観品質(鏡面仕上げ品質等)をより一層向上できる。
また、Snめっき層103に複数の微細な孔からなるめっき欠陥部位が存在する場合には、硫黄と鋼板101に含まれるFeとが結合し、黒色のFeS、Fe2S3、又はFe2Sが形成される場合がある。本実施形態では、SnS、SnS2、FeS、Fe2S3、又はFe2S等の黒色の化合物が形成される現象を、硫化黒変と呼称する。また、硫化黒変に対する耐性(特性)を、耐硫化黒変性と呼称する。
化成処理皮膜層105は、金属Zr量に換算して3.0~30.0mg/m2のZr化合物と、金属Mg量に換算して0.50~5.00mg/m2のMg化合物とを含有する。
本実施形態に係るZr化合物としては、例えば、酸化Zr、リン酸Zr、水酸化Zr及びフッ化Zr等(それぞれの水和物を含む)が挙げられ、化成処理皮膜層105は上述のZr化合物を複数含有する。
一方、Zr含有量が金属Zr量に換算して片面当たり30.0mg/m2を超えると、化成処理皮膜層105が厚くなり過ぎ、化成処理皮膜層105自体の密着性が劣化し、耐硫化黒変性が低下する。また、Zr含有量が金属Zr量に換算して片面当たり30.0mg/m2を超えると、化成処理皮膜層105の電気抵抗が上昇し、溶接性が低下する場合がある。
従って、化成処理皮膜層105のZr含有量は、金属Zr量に換算して片面当たり3.0~30.0mg/m2とする。Zr含有量の下限値は、好ましくは、金属Zr量に換算して片面当たり5.0mg/m2以上であり、より好ましくは、8.0mg/m2以上である。Zr含有量の上限値は、好ましくは、金属Zr量に換算して片面当たり20.0mg/m2以下であり、より好ましくは、15.0mg/m2以下である。
本発明者らは、化成処理皮膜層105がMg化合物を含有することにより、耐硫化黒変性が向上することを知見した。
また、Mgイオンは、硫化黒変現象の主体であるチオールイオン(HS-)又は硫化水素(H2S)と結合し、透明あるいは白色の化合物を形成する。Mgイオンがチオールイオン又は硫化水素と結合することにより、Fe又はSnとチオールイオン又は硫化水素との結合を抑制することができる。
つまり、化成処理皮膜層105がMg化合物を含有することにより、Sn又はFeとチオールイオン又は硫化水素とが反応する可能性を低減することができるため、硫化黒変現象を抑制することができる。
化成処理皮膜層105中のMg含有量が、金属Mg量に換算して片面当たり0.50mg/m2以上であることで、実用上好適な耐硫化黒変性を有する。
また、化成処理皮膜層105が、金属Mg量に換算して片面当たり5.00mg/m2超のMg化合物を含有するためには、化成処理液中にMg化合物を大量に添加する必要がある。化成処理液に大量のMg化合物が含まれると、化成処理皮膜層105の形成が好適に進行しない場合があるため好ましくない。また、化成処理皮膜層105が金属Mg量に換算して片面当たり5.00mg/m2超のMg化合物を含有することにより、コーティング剤との密着性(一次密着性)には影響が生じないが、レトルト処理などの水蒸気存在下高温殺菌処理時の密着性(二次密着性)、耐錆性又は塗膜下腐食性を劣化させる場合があるため好ましくない。さらに、化成処理皮膜層105が金属Mg量に換算して片面当たり5.00mg/m2超過のMg化合物を含有すると、容器用鋼板10を食品用容器に用いたとき、内容物の味又は風味を損ねる場合があるため、好ましくない。
なお、Snめっき層103がMgを含有する場合には、化成処理工程を行う前のSnめっき層103のMg化合物量を測定した上で、化成処理工程を行った後の容器用鋼板10のMg化合物量を測定し、両者の差分から、化成処理皮膜層105中のMg化合物量を測定することができる。
化成処理皮膜層105がリン酸とリン酸塩との少なくとも一方を含有することにより、優れた耐硫化黒変性及び密着性を得ることができる。リン酸とリン酸塩との合計の含有量が、P量に換算して片面当たり1.5mg/m2以上であれば、実用上好適な耐硫化黒変性及び密着性を得ることができる。
リン酸とリン酸塩との合計含有量が増加すると、耐硫化黒変性及び密着性も向上するが、リン酸とリン酸塩との合計の含有量がP量に換算して片面当たり25.0mg/m2を超えると、化成処理皮膜層105におけるリン酸又はリン酸塩の密着性が劣化することにより、コーティング剤との密着性及び塗膜下腐食性が低下するため好ましくない。また、リン酸とリン酸塩との合計含有量がP量に換算して片面当たり25.0mg/m2を超えると、電気抵抗が上昇し溶接性が劣化するため好ましくない。
リン酸とリン酸塩との合計の含有量の下限値は、より好ましくは、P量に換算して片面当たり2.5mg/m2であり、更に好ましくは、5.0mg/m2である。
リン酸とリン酸塩との合計含有量の上限値は、より好ましくは、P量に換算して片面当たり20.0mg/m2であり、更に好ましくは、12.5mg/m2である。
次に、容器用鋼板10の製造方法について、図2を参照して説明する。
図2は、本実施形態に係る容器用鋼板10の製造方法を示すフローチャートである。図2に示すように、容器用鋼板10の製造方法は、めっき工程、化成処理工程及び洗浄工程を有する。
まず、鋼板101の表面にSnめっきを施し、Snめっき層103を形成する(ステップS101)。Snめっきの方法は、特に限定されず、電気めっき法、真空蒸着法又はスパッタリング法などの公知技術を用いることができる。Snめっき浴としては、フェロスタン浴等を用いることができる。
上述したように、めっき工程後に溶融溶錫処理を行ってもよい。
次に、化成処理工程を行い、Snめっき層103の上層に、化成処理皮膜層105を形成する(ステップS103)。
化成処理工程では、化成処理液を用いた陰極電解処理を行う。
一方、陰極電解処理では、強制的な電荷移動及び鋼板101と化成処理液との界面における水素発生により、形成される化成処理皮膜層105の表面が清浄化されるため好ましい。また、陰極電解処理では、化成処理液のpHが上昇することにより、化成処理皮膜層105の付着が促進されるため好ましい。
化成処理液のpHは、3.0~4.5の範囲が好ましく、pHを下げる場合には硝酸又はフッ化水素酸等を添加し、pHを上げる場合にはアンモニア等を添加することにより適宜調整すればよい。
化成処理液中のZrイオンの下限値は、好ましくは500ppmであり、より好ましくは1000ppmである。化成処理液中のZrイオンの上限値は、好ましくは2500ppmであり、より好ましくは2000ppmである。
なお、化成処理液中のFイオンもZrイオンと同様に化成処理皮膜層105中に取り込まれるが、化成処理皮膜層105中のF化合物は後述する洗浄工程によりできるだけ取り除くことが好ましい。
化成処理液がMgイオンを含有することにより、化成処理皮膜層105にMg化合物が含まれ、耐硫化黒変性が向上するため好ましい。さらに、Mgイオンは、Zrイオンの析出を促進することができる。具体的には、化成処理液がMgイオンを含有する場合と含有しない場合とで、化成処理工程により形成される化成処理皮膜層105中のZr化合物量を比較した場合に、Mgイオンを含有する場合の方がより多く化成処理皮膜層105中にZr化合物量が含まれる。
上記の式(1)の反応は平衡(可逆)反応であるが、化成処理液中のFイオンが増加することにより、上記の式(1)の右向きの反応(錯イオンが分解する反応)が、著しく阻害される。
上述のように、化成処理液がMgイオンを含有することにより、Zrの析出が促進される。そのため、本実施形態に係る容器用鋼板10の製造方法は、化成処理工程に要する時間を短縮することができ、優れた生産性を有する。
化成処理液に添加されるMgイオン濃度は、より好ましくは、100~200ppmである。
なお、Mgイオンは、硝酸Mg又は硫酸Mg等の易水溶性の塩で添加することが好ましい。
化成処理液がリン酸イオンを含有することにより、化成処理皮膜層105がリン酸又はリン酸塩を含有し、耐硫化黒変性及び密着性が向上するため好ましい。
なお、化成処理液は、硝酸イオンとアンモニウムイオンとのいずれか一方ではなく、硝酸イオンとアンモニウムイオンとの両方を含むことが好ましい。その理由は以下の通りである。
Zrを含有する化成処理皮膜層105を形成する際には、まず、下記の式(2)の反応により、陰極においてH2が発生し、pHが上昇する。
なお、化成処理液がMgイオン、硝酸イオン及びアンモニウムイオンを含有することにより上述の好適な効果を有する点は、本発明により初めて明らかになった。
なお、第一化成処理液と第二化成処理液とは同一の成分を含有し、温度だけが異なる。第一化成処理液の温度の例としては10℃以上40℃未満が挙げられ、第二化成処理液の温度の例としては45℃~60℃が挙げられる。
化成処理皮膜層105の第一層は、緻密な層であるため、耐硫化黒変性等の特性の確保に好適である。化成処理皮膜層105の第二層は、粗度の粗い表面を有するので、化成処理皮膜層105とコーティング剤との密着性の確保に好適である。
Fイオン、硝酸イオン及びアンモニウムイオン等の水溶性イオン種は化成処理液中に含まれるため、Zr化合物と共に化成処理皮膜層105に取り込まれる。化成処理皮膜層105中の上記イオン種は、コーティング剤との密着性(一次密着性)には影響を及ぼさないが、二次密着性、耐錆性又は塗膜下腐食性を劣化させる原因となる。これは、水蒸気や腐食液に化成処理皮膜層105中の上記イオン種が溶出し、化成処理皮膜層105とコーティング剤との結合を分解、或いは、鋼板101を腐食することが原因と考えられる。
そのため、本実施形態では、化成処理工程を行った後、少なくとも、40℃以上の水で0.5秒以上の洗浄処理(以下、本洗浄工程と呼称する)を行う(ステップS107)。なお、本洗浄工程で用いる水の温度の上限は特に限定されないが、例えば90~100℃である。また、本洗浄工程の洗浄時間の上限も特に限定されないが、例えば10秒である。
予備洗浄工程及び本洗浄工程の洗浄方法としては、浸漬処理又はスプレー処理が挙げられる。
それぞれの処理時間が0.5秒を下回ると、上記イオン種を減少させることが難しい。
なお、表1の処理液1-1~3-2はいずれも同じ温度及びpHであり、同じ電流密度及び処理時間の条件下で陰極電解処理が施されている。表1に示されているように、Mgイオンを添加することにより、形成される化成処理皮膜層のZr含有量が増加しており、MgイオンはZrの析出促進効果を有することが示された。
試験材を60mm×60mmLの大きさに切り出し、5mmの長さで端部(剪断によって鋼板端面が露出した部分)をテープでマスキングした。1質量%Na2S水溶液(乳酸でpH=7に調整)に浸漬し、125℃の温度下でレトルト処理を60分間施した。レトルト処理後の各試験材の外観を目視で評価した。
具体的には、クロメート処理材より良好な結果であった場合を「Very Good」、クロメート処理材より若干良好な結果であった場合を「Good」、クロメート処理材と同等の変色があった場合を「Average」、クロメート処理材より若干変色度合いが大きかった場合を「Fair」、クロメート処理材より変色度合いが大きかった場合を「Poor」と評価した。
試験材の両面に、厚さ20μmのPETフィルムを200℃の温度下で貼り付け、絞り加工及びしごき加工による製缶加工を段階的に行った。フィルムの疵、浮き及び剥離を観察し、それらの面積率から加工性を評価した。
具体的には、フィルムの疵、浮き及び剥離が全く観察されなかった場合を「Very Good」、フィルムの疵、浮き及び剥離の面積率が0%超0.5%以下であった場合を「Good」、フィルムの疵、浮き及び剥離の面積率が0.5%超15%以下であった場合を「Fair」、フィルムの疵、浮き及び剥離の面積率が15%超又は破断し加工不能であった場合を「Poor」と評価した。
なお、面積率は、フィルムの疵、浮き及び剥離が観察された部分の面積を、貼り付けたPETフィルムの全体の面積で除することにより求めた。
ワイヤーシーム溶接機を用いて、溶接ワイヤースピード80m/minの条件で、電流を変更して試験材を溶接した。十分な溶接強度が得られる最小電流値とチリ及び溶接スパッタなどの溶接欠陥が目立ち始める最大電流値とからなる適正電流範囲から総合的に判断し、溶接性を評価した。
具体的には、二次側の適正電流範囲が1500A以上の場合を「Very Good」、二次側の電流適正電流範囲が800A以上1500A未満の場合を「Good」、二次側の電流適正電流範囲が100A以上800A未満の場合を「Fair」、二次側の電流適正電流範囲が100A未満の場合を「Poor」と評価した。
試験材の両面に、厚さ20μmのPETフィルムを200℃の温度下で焼付け、絞りしごき加工を行い、缶体を作製した。125℃の温度下でレトルト処理を30分間行い、フィルムの剥離状況を観察し、剥離面積率からフィルム密着性を評価した。
具体的には、剥離面積率が0%の場合を「Very Good」、剥離面積率が0%超2%以下の場合を「Good」、剥離面積率が2%超10%以下の場合を「Fair」、剥離面積率が10%超の場合を「Poor」と評価した。
試験材にエポキシ-フェノール樹脂を塗布し、200℃の温度下で焼付け処理を30分間行った。1mm間隔で地鉄に達する深さの格子状の切れ目を入れ、テープで剥離した。剥離状況を観察し、剥離面積率から一次塗料密着性を評価した。
具体的には、剥離面積率が0%の場合を「Very Good」、剥離面積率が0%超5%以下の場合を「Good」、剥離面積率が5%超30%以下の場合を「Fair」、剥離面積率が30%超の場合を「Poor」と評価した。
試験材にエポキシ-フェノール樹脂を塗布し、200℃の温度下で焼付け処理を30分間行った。1mm間隔で地鉄に達する深さの格子状の切れ目を入れ、その後、125℃の温度下でレトルト処理を30分間行った。乾燥後、テープで塗膜を剥離し、剥離状況を観察し、剥離面積率から二次塗料密着性を評価した。
具体的には、剥離面積率が0%の場合を「Very Good」、剥離面積率が0%超5%以下の場合を「Good」、剥離面積率が5%超30%以下の場合を「Fair」、剥離面積率が30%超の場合を「Poor」と評価した。
試験材にエポキシ-フェノール樹脂を塗布し、200℃の温度下で焼付け処理を30分間行った。その後、地鉄に達する深さの格子状の切れ目を入れ、1.5%クエン酸-1.5%食塩混合液からなる試験液に、45℃の温度下で72時間浸漬した。洗浄及び乾燥後、テープ剥離を行った。切れ目を入れた部分の塗膜下腐食状況と平板部の腐食状況とを観察し、塗膜下腐食の幅及び平板部の腐食面積率の評価から、塗膜下耐食性を評価した。
具体的には、塗膜下腐食幅が0.2mm未満かつ平板部の腐食面積率が0%の場合を「Very Good」、塗膜下腐食幅が0.2mm以上0.3mm未満かつ平板部の腐食面積率が0%超1%以下の場合を「Good」、塗膜下腐食幅が0.3mm以上0.45mm未満かつ平板部の腐食面積率が1%超5%以下の場合を「Fair」、塗膜下腐食幅が0.45mm以上又は平板部の腐食面積率が5%超の場合を「Poor」と評価した。
試験材を125℃の温度下でレトルト処理を30分間行った。その後、錆の発生状況を観察し、錆発生面積率からレトルト耐錆性を評価した。
具体的には、錆発生面積率が0%の場合を「Very Good」、錆発生面積率が0%超1%以下の場合を「Good」、錆発生面積率が1%超5%以下の場合を「Fair」、錆発生面積率が5%超の場合を「Poor」と評価した。
<Snめっき鋼板>
以下の(処理法1)又は(処理法2)の方法を用いて、板厚0.17~0.23mmの鋼板上にSnめっき層を形成し、Snめっき鋼板を作製した。
冷間圧延後、焼鈍及び調圧された鋼板を、脱脂及び酸洗した後、その両面に、フェロスタン浴を用いてSnめっき層を形成し、Snめっき鋼板を作製した。
(処理法2)
冷間圧延後、焼鈍及び調圧された鋼板を、脱脂及び酸洗した後、その両面に、フェロスタン浴を用いてSnめっき層を形成した。その後、リフロー処理(溶融溶錫処理)を行い、Sn合金層を有するSnめっき鋼板を作製した。
上記の(処理法1)又は(処理法2)の方法で作製したSnめっき鋼板に対して、以下の(処理法3)~(処理法7)のいずれかの方法を施すことによりSnめっき鋼板の表面にZr化合物及びMg化合物を含む化成処理皮膜層を形成した。なお、処理法3~6では、0.5~30.0A/dm2の電流密度、0.5~5.0秒の陰極電解処理時間及び10~60℃の化成処理液の温度の条件下で陰極電解処理を行った。また、処理法7では、温度が60℃でありpHが3.5である化成処理液に180秒の浸漬時間浸漬した。
フッ化Zrを溶解させ、硝酸Mgを添加した化成処理液を用いて陰極電解処理を行うことにより、化成処理皮膜層を形成した。
上記の処理により化成処理皮膜層を形成した後、鋼板を10℃以上40℃未満の蒸留水中に0.5秒~5.0秒浸漬することにより予備洗浄を行った。
予備洗浄を行った後、表4に示す温度の蒸留水に表4に示す時間鋼板を浸漬することにより本洗浄を行った。
めっき層中の金属Sn量は蛍光X線法によって測定した。また、化成処理皮膜層のZr含有量、Mg含有量及びリン酸又はリン酸塩の含有量(P量に換算)は、蛍光X線分析等の定量分析法により測定した。
測定結果を表5に示す。
上記の処理を行った試験材について、実施例2に挙げた(A)~(H)の項目と、以下に記載する(I)の項目について性能評価を行った。評価結果を表6に示す。
各試験材を作製する際に用いた化成処理液からMgイオンを除去した化成処理液を用い、それ以外の条件は各試験材と同様の条件により容器用鋼板(以下、Mg非含有容器用鋼板と呼称する)を作製した。その後、Mg非含有容器用鋼板のZr含有量を測定した。
各試験材のZr含有量を、Mg非含有容器用鋼板のZr含有量で除算した比率(以下、Zr付着促進率と呼称する)により、Mgイオン添加によるZr付着促進効果を評価した。具体的には、Zr付着促進率が1.3以上の場合を「Very Good」、1.3未満~1.2以上の場合を「Good」、1.2未満~1.1以上の場合を「Fair」、1.1未満の場合を「Poor」と評価した。
更に、化成処理皮膜層がP量として1.5mg/m2以上のリン酸又はリン酸塩を含有することにより、フィルム密着性(加工性を含む)及び塗膜下腐食性が更に向上した。
一方、比較例b1~b8では、Zr付着促進効果を有さないと共に、耐硫化黒変性、溶接性、加工性、溶接性、フィルム密着性、一次塗料密着性、二次塗料密着性、塗膜下腐食性及び耐食性の少なくとも一部の特性が劣っていた。
比較例b2及びb3では、化成処理液中のFイオン量が過剰に存在していたため、MgイオンがFイオンのスカベンジャーとしての機能を十分に発揮できず、MgイオンによるZrの析出促進効果が好適ではなかったと考えられる。
比較例b5では、化成処理液中のMgイオン量が不足していたため、MgイオンによるZrの析出促進効果が好適ではなかったと考えられる。逆に、Fイオンが多い場合には、(ZrF6)2-等の錯イオンが過剰に安定化する事で皮膜形成を困難にする。)
比較例b8は陰極電解処理ではなく浸漬処理を用いており、化成処理液がMgイオンを含む場合であっても化成処理皮膜層中のZr化合物量が少なかった。そのため、MgイオンによるZrの析出促進効果が好適ではなかったと考えられる。
101 鋼板
103 Snめっき層
105 化成処理皮膜層
Claims (8)
- 鋼板と;
前記鋼板の上層として設けられ、金属Sn量に換算して560~5600mg/m2のSnを含有するSnめっき層と;
前記Snめっき層の上層として設けられ、金属Zr量に換算して3.0~30.0mg/m2のZr化合物と、金属Mg量に換算して0.50~5.00mg/m2のMg化合物と、を含有する化成処理皮膜層と;
を備える
ことを特徴とする、容器用鋼板。 - 前記Snめっき層が、Fe-Sn合金を更に含有する
ことを特徴とする、請求項1に記載の容器用鋼板。 - 前記化成処理皮膜層が、リン酸とリン酸塩との少なくとも一方を、P量に換算して合計で1.5~25.0mg/m2更に含有する
ことを特徴とする、請求項1又は2に記載の容器用鋼板。 - 鋼板上に、Snを金属Sn量に換算して560~5600mg/m2含むSnめっき層を形成するめっき工程と;
前記めっき工程後、100~3000ppmのZrイオン、120~4000ppmのFイオン及び50~300ppmのMgイオンを含む化成処理液を用いて陰極電解処理を行うことにより、前記Snめっき層上に化成処理皮膜層を形成する化成処理工程と;
前記化成処理工程後、40℃以上の水を用いて前記Snめっき層及び前記化成処理皮膜層が形成された前記鋼板を0.5秒以上の洗浄処理を行う本洗浄工程と;
を有する
ことを特徴とする、容器用鋼板の製造方法。 - 前記Snめっき層が形成された前記鋼板に溶融溶錫処理を行い、前記Snめっき層の少なくとも一部のSnと前記鋼板中の少なくとも一部のFeとを合金化する
ことを特徴とする、請求項4に記載の容器用鋼板の製造方法。 - 前記化成処理液が、2000ppm以下のリン酸イオンを更に含む
ことを特徴とする、請求項4又は5に記載の容器用鋼板の製造方法。 - 前記化成処理液が、合計で20000ppm以下の硝酸イオン及びアンモニウムイオンを更に含む
ことを特徴とする、請求項4~6のいずれか一項に記載の容器用鋼板の製造方法。 - 前記本洗浄工程の前に、10℃以上40℃未満の水を用いて前記Snめっき層及び前記化成処理皮膜層が形成された前記鋼板を0.5秒以上の洗浄処理を行う予備洗浄工程を更に有する
ことを特徴とする、請求項4~7のいずれか一項に記載の容器用鋼板の製造方法。
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