WO2014007139A1 - 加工性に優れた耐熱・耐食性めっき層を有する配管 - Google Patents

加工性に優れた耐熱・耐食性めっき層を有する配管 Download PDF

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Publication number
WO2014007139A1
WO2014007139A1 PCT/JP2013/067670 JP2013067670W WO2014007139A1 WO 2014007139 A1 WO2014007139 A1 WO 2014007139A1 JP 2013067670 W JP2013067670 W JP 2013067670W WO 2014007139 A1 WO2014007139 A1 WO 2014007139A1
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layer
plating layer
alloy plating
znni alloy
content
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PCT/JP2013/067670
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English (en)
French (fr)
Inventor
康滋 石井
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臼井国際産業株式会社
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Application filed by 臼井国際産業株式会社 filed Critical 臼井国際産業株式会社
Priority to CN201380035210.8A priority Critical patent/CN104428447B/zh
Priority to EP13812803.8A priority patent/EP2871263B1/en
Priority to RU2015103541A priority patent/RU2636423C2/ru
Priority to KR1020147034507A priority patent/KR20150009988A/ko
Priority to US14/408,111 priority patent/US9611972B2/en
Priority to MX2014015473A priority patent/MX360661B/es
Priority to BR112014033111A priority patent/BR112014033111A2/pt
Publication of WO2014007139A1 publication Critical patent/WO2014007139A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/10—Electroplating with more than one layer of the same or of different metals
    • C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
    • C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C28/02—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 only coatings only including layers of metallic material
    • C23C28/023—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 only coatings only including layers of metallic material only coatings of metal elements only
    • C23C28/025—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 only coatings only including layers of metallic material only coatings of metal elements only with at least one zinc-based layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/321—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal alloy layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C28/345—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 with at least one oxide layer
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/38—Chromatising
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/04—Tubes; Rings; Hollow bodies
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L58/00—Protection of pipes or pipe fittings against corrosion or incrustation
    • F16L58/02—Protection of pipes or pipe fittings against corrosion or incrustation by means of internal or external coatings
    • F16L58/04—Coatings characterised by the materials used
    • F16L58/08—Coatings characterised by the materials used by metal
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L9/00—Rigid pipes
    • F16L9/02—Rigid pipes of metal

Definitions

  • the present invention relates to an automobile pipe having a heat-resistant and corrosion-resistant plating layer having excellent workability, and more specifically, a pipe having excellent workability having a ZnNi alloy plating layer as a heat-resistant and corrosion-resistant plating layer on the outer surface of a base steel pipe. It is about.
  • a Ni plating layer is formed as a first layer on the surface of a substrate, and then a chromate film treatment is applied to the surface of the ZnNi alloy plating layer deposited on the Ni plating layer.
  • a heat-resistant / corrosion-resistant multi-layer plated steel material see Patent Document 1, Patent Document 2, etc.
  • a Ni plating layer as a first layer
  • Patent Document 3 that forms a ZnNi alloy plating layer using an alkaline bath as a layer has been proposed.
  • JP-A-2-120034 Japanese Patent Laid-Open No. 10-121267 Japanese Patent Application Laid-Open No. 8-134585
  • the present invention has the above-mentioned problems of the prior art, that is, the problem of deterioration in workability in the case of a pipe in which a ZnNi alloy plating layer is formed alone on a Ni plating layer, and between the Ni plating layer and the ZnNi alloy plating layer during bending.
  • the first layer Ni plating layer is intended to solve the problems of heat resistance and corrosion resistance due to lowering of adhesion and the problem of cost increase when multiple ZnNi alloy plating layers are formed on the Ni plating layer. It is an object of the present invention to provide a high-quality piping having a heat-resistant and corrosion-resistant plating layer that has excellent workability at a low cost without requiring any other material.
  • the present inventor properly determined the Ni content of the ZnNi alloy plating layer without forming the first layer Ni plating layer, The present inventors have found a multilayer ZnNi alloy plating layer exhibiting excellent heat resistance and corrosion resistance even in a bent portion. Although the ZnNi alloy plating layer is excellent in heat resistance and corrosion resistance, the workability is poor, but it is known that, for example, the bent portion of the fuel injection pipe is greatly affected by the plating film thickness and the Ni content.
  • the ZnNi alloy plating layer has an advantageous effect on the corrosion resistance when the plating film thickness and the Ni content are large in the unprocessed part (straight pipe part or the like), but the plating peels off when the plating film thickness becomes large in the bent part. "The danger of” increased and the possibility of a decrease in corrosion resistance is increased, and the plating film thickness considering workability does not provide the desired corrosion resistance. Similarly, the Ni content is too high. When the Ni content is lowered in consideration of workability, the desired corrosion resistance cannot be obtained, and on the basis of such technical knowledge, the first layer is formed on the substrate surface.
  • the pipe having a heat-resistant and corrosion-resistant plating layer excellent in workability according to the present invention is formed by ZnNi alloy plating with a Ni content of 5 to 9% and a layer thickness of 3 to 9 ⁇ m formed as the first layer on the surface of the base steel pipe.
  • the first layer formed on the surface of the base steel pipe is a ZnNi alloy plating layer having a low Ni content that is advantageous for workability, and the second layer deposited on the first layer emphasizes corrosion resistance.
  • the ZnNi alloy plating layer With a higher Ni content than the first layer, the second layer of the surface layer is excellent in the initial rust prevention performance, and the adverse effect on the lower first layer during processing can be reduced, For example, it is possible to withstand the processing process of the fuel pipe after the formation of the multilayer plating layer, and even if the Ni plating layer does not exist in the first layer, the same heat resistance and corrosion resistance can be obtained in the bent part of the fuel pipe.
  • the plating bath types and the number of product coating layers used in the production process can be reduced, it is advantageous in terms of complexity and cost of plating solution management.
  • the thickness of the ZnNi alloy plating layer of the first layer formed on the surface of the base steel pipe is limited to 3 to 9 ⁇ m because sufficient heat resistance and corrosion resistance cannot be obtained when the layer thickness is less than 3 ⁇ m. If the layer thickness exceeds 9 ⁇ m, plating peeling that can be visually confirmed in the bent portion may occur, which causes a problem in appearance quality. Further, the reason why the thickness of the ZnNi alloy plating layer of the second layer is limited to 1 to 3 ⁇ m, as in the case of the ZnNi alloy plating layer of the first layer, if the layer thickness is less than 1 ⁇ m, sufficient heat resistance and corrosion resistance cannot be obtained. On the other hand, if the layer thickness exceeds 3 ⁇ m, plating peeling that can be visually confirmed in the bent portion may occur, resulting in a problem in appearance quality.
  • the reason why the Ni contents of the ZnNi alloy plating layers of the first layer and the second layer are limited to 5 to 9% and 10 to 15%, respectively, is as follows. That is, the Ni content of the first layer and the second layer needs to be higher than that of the first layer in consideration of workability and corrosion resistance. This is because the surface layer has a high Ni-containing ZnNi alloy plating layer with excellent corrosion resistance, so it is excellent in the initial rust prevention performance even in the bent part, and it is easy to work on the first layer even if it is adversely affected by processing. This is because the inferior second layer is present, so that the low-Ni-containing ZnNi alloy plating layer of the first layer is hardly affected.
  • the Ni content of the first layer and the second layer needs to be higher than the first layer.
  • the Ni content of the ZnNi alloy plating layer of the first layer is less than 5%, sufficient heat resistance and corrosion resistance cannot be obtained.
  • plating peeling may occur in the bent portion. Therefore, the Ni content of the ZnNi alloy plating layer of the first layer is specified as 5 to 9%.
  • the Ni content of the ZnNi alloy plating layer of the second layer is defined as 10 to 15%, as in the case of the first layer, if less than 10%, sufficient heat resistance and corrosion resistance cannot be obtained, On the other hand, if it exceeds 15%, plating peeling may occur at the bent portion, which causes a problem in appearance quality.
  • a steel pipe for fuel piping having a diameter of 8 mm is used, and a ZnNi alloy plating layer having a liquid temperature of 15 to 25 ° C., a current density of 5 A / dm 2 and a Ni content of 5% and a layer thickness of 3 ⁇ m is used as the first layer on the surface of the steel pipe.
  • a ZnNi alloy plating layer having a liquid temperature of 15 to 25 ° C., a current density of 5 A / dm 2 and a Ni content of 10% and a layer thickness of 1 ⁇ m is formed, and PH 4.0 is further formed on the second layer.
  • the chromate film treatment was performed for 60 seconds at a liquid temperature of 30 ° C.
  • Zn 9.0 g / L, Ni: 2.2 g / L, NaOH: 125.6 g / L, a complexing agent and a brightening agent were used.
  • Zn 8.0 g / L, Ni: 1.4 g / L, NaOH: 130.0 g / L, complexing agent and brightening agent A plating solution containing an appropriate amount of each was used.
  • the obtained steel pipe for fuel piping having a multilayer ZnNi alloy plating layer was subjected to bending with R15, and appearance peeling of the bent portion was visually observed. Next, the sample after bending was heated at 150 ° C. for 24 hours, and then the corrosion resistance was evaluated by a salt spray test based on JISZ2371. The test results are shown in Table 1.
  • a ZnNi alloy plating layer having a Ni content of 5% and a layer thickness of 3 ⁇ m was formed as the first layer on the surface of the steel pipe for fuel piping having a diameter of 8 mm, and then Ni as the second layer.
  • a chromate film was formed on the second layer. Table 1 shows the results of the appearance peeling test and the salt spray test on the bent portion of the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer in the same manner as in Example 1.
  • a ZnNi alloy plating layer having a Ni content of 5% and a layer thickness of 5 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer.
  • a ZnNi alloy plating layer having a content rate of 10% and a layer thickness of 1 ⁇ m was formed on the second layer.
  • Table 1 shows the results of the appearance peeling test and the salt spray test on the bent portion of the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer in the same manner as in Example 1.
  • a ZnNi alloy plating layer having a Ni content of 5% and a layer thickness of 5 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer.
  • a ZnNi alloy plating layer having a content rate of 10% and a layer thickness of 3 ⁇ m was formed on the second layer.
  • Table 1 shows the results of the appearance peeling test and the salt spray test on the bent portion of the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer in the same manner as in Example 1.
  • Example 1 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 9% and a layer thickness of 9 ⁇ m was formed as the first layer on the surface of the steel pipe for fuel piping having a diameter of 8 mm, and then Ni as the second layer. After forming a ZnNi alloy plating layer having a content rate of 15% and a layer thickness of 3 ⁇ m, a chromate film was formed on the second layer. Table 1 shows the results of the appearance peeling test and the salt spray test on the bent portion of the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer in the same manner as in Example 1.
  • Example 1 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 4% and a layer thickness of 2 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 9% and a layer thickness of 0.8 ⁇ m, a chromate film was formed on the second layer. For the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer, the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • Example 2 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 10% and a layer thickness of 10 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 16% and a layer thickness of 4 ⁇ m, a chromate film was formed on the second layer. Table 1 also shows the results of an external peel test of the bent portion of the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer by the same method as in Example 1.
  • Example 3 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 10% and a layer thickness of 1 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 5% and a layer thickness of 3 ⁇ m, a chromate film was formed on the second layer. For the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer, the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • Example 4 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 10% and a layer thickness of 3 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 5% and a layer thickness of 3 ⁇ m, a chromate film was formed on the second layer. For the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer, the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • Example 5 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 10% and a layer thickness of 1 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 5% and a layer thickness of 5 ⁇ m, a chromate film was formed on the second layer. For the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer, the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • Example 6 By the same plating layer forming method as in Example 1, a ZnNi alloy plating layer having a Ni content of 10% and a layer thickness of 3 ⁇ m was formed as a first layer on the surface of a steel pipe for fuel piping having a diameter of 8 mm, and then Ni as a second layer. After forming a ZnNi alloy plating layer having a content rate of 5% and a layer thickness of 5 ⁇ m, a chromate film was formed on the second layer. For the steel pipe for fuel piping having the obtained multilayer ZnNi alloy plating layer, the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • a Ni plating layer having a layer thickness of 0.5 ⁇ m is formed as the first layer on the surface of the same steel pipe for fuel piping as in Example 1, and then a ZnNi alloy plating layer having a Ni content of 8% and a layer thickness of 5 ⁇ m is formed as the second layer. Further, after a ZnNi alloy plating layer having a Ni content of 5% and a layer thickness of 5 ⁇ m was formed as a third layer by the same method as in Example 1, a chromate film was formed on the third layer.
  • the first Ni plating layer in this conventional example was formed using a Watt bath at a liquid temperature of 52 to 57 ° C. and a current density of 5 A / dm 2 .
  • the ZnNi alloy plating layer of the second layer uses an acidic bath of 100 g / L ZnCl 2 , 130 g / L NiCl 2 .6H 2 O, 200 g / L NH 4 Cl, pH 5.7, liquid temperature It was formed at 34 to 36 ° C. and a current density of 3 A / dm 2 .
  • the results of the appearance peel test and the salt spray test of the bent portion in the same manner as in Example 1 are shown together in Table 1.
  • the first layer is a ZnNi alloy plating layer having a low Ni content, which is advantageous for workability, and the thickness is 3 to 9 ⁇ m.
  • the second layer is a ZnNi alloy plating layer having a higher Ni content than the first layer, which emphasizes corrosion resistance.
  • the steel pipes for fuel piping of Examples 1 to 5 of the present invention formed to 3 ⁇ m have no plating peeling phenomenon in the bent portion, and the corrosion resistance is evident from the time until the occurrence of red rust in the bent portion. Therefore, even if there is no Ni plating layer in the first layer, equivalent heat resistance and corrosion resistance can be obtained at the bent portion of the pipe.
  • the result of the salt spray test is that of Comparative Example 1 (thickness of the specified layer or less) in which the thicknesses of the ZnNi alloy plating layers of the first layer and the second layer deviate from the specified values of the present invention. As is clear from the above time), it is not preferable because it is greatly inferior to Examples 1 to 5 of the present invention.
  • Comparative Example 2 thickness greater than or equal to the specified layer thickness in which the thicknesses of the ZnNi alloy plating layers of the first layer and the second layer deviate from the specified values of the present invention, the fuel pipe is caused by plating peeling at the bent portion. Cannot be used as a steel pipe. (4).
  • Comparative Examples 3 to 6 in which the Ni content in the first layer is higher than the Ni content in the second layer are all in accordance with the present invention, as is clear from the results of the salt spray test (the time until red rust occurs in the bent portion). This is not preferable because it is greatly inferior to Examples 1-5.
  • Conventional examples 1 and 2 in which the first layer is composed of the Ni plating layer and the second layer and the third layer are composed of the ZnNi alloy plating layer can withstand bending, but the result of the salt spray test (red rust is generated in the bent portion) Time) is inferior to that of Examples 1 to 5 of the present invention, which indicates that there is a problem in the structure of the multilayer plating.
  • Example only of the steel pipe for fuel piping was demonstrated here, it cannot be overemphasized that the same effect is acquired even if this invention is applied not only to the steel pipe for fuel piping but to various piping of a motor vehicle. For this reason, examples of automobile pipes other than steel pipes for fuel pipes were omitted.

Abstract

【課題】　加工性に優れた耐熱・耐食性複層めっき層を有する配管を提供する。 【解決手段】　母材鋼管の表面に、第一層として形成したＮｉ含有率５～９％、層厚３～９μｍのＺｎＮｉ合金めっき層と、第一層のＺｎＮｉ合金めっき層上に第二層として被着したＮｉ含有率１０～１５％、層厚１～３μｍのＺｎＮｉ合金めっき層と、該第二層のＺｎＮｉ合金めっき層上に形成したクロメート皮膜とからなる複層めっき層を有することを特徴とする。

Description

加工性に優れた耐熱・耐食性めっき層を有する配管
　本発明は、加工性に優れた耐熱・耐食性めっき層を有する自動車の配管に係り、より詳しくは母材鋼管の外表面に耐熱・耐食性めっき層としてＺｎＮｉ合金めっき層を有する加工性に優れた配管に関するものである。
　従来、自動車の例えば燃料配管では鋼管表面にＺｎめっき層を形成した後にクロメート皮膜を形成した製品が多用されている。しかしながら、めっき層皮膜処理後の製品加工は加工部の耐食性が著しく損なわれ、耐熱性も十分とはいえない。又、低燃費、環境対策面から自動車のエンジンダウンサイジング化（小型化）によるエンジンルーム内の温度の上昇や、それに伴いエンジンルーム内で使用される配管についてもより高耐熱・高耐食性の要求が高まってきている。
　ところで、加工性に優れる耐熱・耐食性めっきとしては、基材の表面に第一層としてＮｉめっき層を形成し、ついで前記Ｎｉめっき層上に被着したＺｎＮｉ合金めっき層の表面にクロメート皮膜処理を施した耐熱・耐食性重層メッキ鋼材（特許文献１、特許文献２等参照）や、第一層としてＮｉめっき層を形成し、ついで中間層として酸性浴使用のＺｎＮｉ合金めっき層を形成し、第三層としてアルカリ性浴使用のＺｎＮｉ合金めっき層を形成する鋼材（特許文献３参照）が提案されている。
　しかしながら、燃料配管等の自動車用配管の製造工程としては、生産性やコスト等の観点から長尺の直管鋼管の状態でめっき及びクロメート処理をした後に製品曲げ加工を行うことが望ましいため、前記した従来技術のようなＮｉめっき層上にＺｎＮｉ合金めっき層を単独で形成する場合は、端部のめっき膜厚が厚くなり加工性が悪化することや、Ｎｉめっき層とＺｎＮｉ合金めっき層間の密着性が曲げ加工時に低下し、耐熱性・耐食性が低下しやすいという問題がある。又、Ｎｉめっき層上にＺｎＮｉ合金めっき層を複数形成する場合も浴管理の煩雑さやコストアップの要因となるという問題がある。
特開平２－１２００３４号公報 特開平１０－１２１２６７号公報 特開平８－１３４６８５号公報
　本発明は、前記した従来技術の問題、即ち、Ｎｉめっき層上にＺｎＮｉ合金めっき層を単独で形成した配管の場合の加工性悪化の問題、曲げ加工時におけるＮｉめっき層とＺｎＮｉ合金めっき層間の密着性の低下による耐熱性・耐食性の低下の問題、及び、Ｎｉめっき層上にＺｎＮｉ合金めっき層を複数形成する場合のコストアップの問題を解決すべくなされたもので、第一層Ｎｉめっき層を必要とせず低コストで優れた加工性を備えた高品質の、耐熱・耐食性めっき層を有する配管を提供しようとするものである。
　本発明者は、加工性に優れた耐熱・耐食性めっき層に関して鋭意研究を重ねた結果、ＺｎＮｉ合金めっき層のＮｉ含有率を適正に定めることにより、第一層Ｎｉめっき層を形成することなく、曲げ加工部でも優れた耐熱・耐食性を示す複層ＺｎＮｉ合金めっき層の構成を見出した。
　ＺｎＮｉ合金めっき層は、耐熱・耐食性に優れる一方、加工性は乏しいが、例えば燃料噴射管の曲げ加工部ではめっき膜厚とＮｉ含有率の影響を大きく受けることが知られている。即ち、ＺｎＮｉ合金めっき層は、未加工部（直管部等）ではめっき膜厚とＮｉ含有率が大きい場合耐食性に有利に作用するが、曲げ加工部ではめっき膜厚が大きくなれば“めっき剥がれ”の危険性が増大し耐食性が低下する可能性が高まり、加工性を考慮しためっき膜厚では所望の耐食性が得られないこと、又、Ｎｉ含有量についても同様で、Ｎｉ含有量が高すぎると加工性が悪化し、加工性を考慮してＮｉ含有量を低くした場合には所望の耐食性が得られないこと、そしてかかる技術的知見に基づいて、基材表面に第一層として形成したＺｎＮｉ合金めっき層上に、当該第一層のＮｉ含有率よりも高いＮｉ含有率のＺｎＮｉ合金めっき層を形成することにより、Ｎｉめっき層を形成しなくても燃料噴射管の曲げ加工部で同等の耐食性を有する複層ＺｎＮｉ合金めっき層の構成を見出したのである。
　即ち、本発明に係る加工性に優れた耐熱・耐食性めっき層を有する配管は、母材鋼管の表面に第一層として形成したＮｉ含有率５～９％、層厚３～９μｍのＺｎＮｉ合金めっき層と、該第一層のＺｎＮｉ合金めっき層上に第二層として被着したＮｉ含有率１０～１５％、層厚１～３μｍのＺｎＮｉ合金めっき層と、該第二層のＺｎＮｉ合金めっき層上に形成したクロメート皮膜とからなる複層めっき層を有することを特徴とするものである。
　本発明は、母材鋼管の表面に形成する第一層を加工性に有利な低Ｎｉ含有率のＺｎＮｉ合金めっき層とし、該第一層の上に被着する第二層には耐食性を重視した、前記第一層より高Ｎｉ含有率のＺｎＮｉ合金めっき層としたことにより、表層の第二層が初期防錆性能に優れ、かつ加工時に下層の第一層への悪影響を軽減できるので、例えば複層めっき層形成後の燃料配管の加工工程にも耐えることが可能となり、第一層にＮｉめっき層が存在しなくても燃料配管の曲げ加工部で同等の耐熱・耐食性を得ることができ、生産工程で使用するめっき浴種や製品被覆層数も少なくできることによりめっき液管理の煩雑さやコスト面でも有利である。
　本発明において、母材鋼管の表面に形成する第一層のＺｎＮｉ合金めっき層の層厚を３～９μｍと限定したのは、層厚が３μｍ未満では十分な耐熱・耐食性が得られず、他方、層厚が９μｍを超えると曲げ加工部で目視確認できるめっき剥離が発生するおそれがあり外観品質上問題となるためである。又、第二層のＺｎＮｉ合金めっき層の層厚１～３μｍと限定したのは、第一層のＺｎＮｉ合金めっき層と同様に、層厚が１μｍ未満では十分な耐熱・耐食性が得られず、他方、層厚が３μｍを超えると曲げ加工部で目視確認できるめっき剥離が発生するおそれがあり外観品質上問題となるためである。
　さらに、前記第一層と第二層のＺｎＮｉ合金めっき層のＮｉ含有率をそれぞれ、５～９％、１０～１５％に限定したのは、以下に記載する理由による。
　即ち、第一層と第二層のＮｉ含有率は、加工性と耐食性を考慮すると第二層が第一層より高Ｎｉ含有率とする必要がある。これは、表層側に耐食性に優れる高Ｎｉ含有のＺｎＮｉ合金めっき層があるため、曲げ加工部でも初期の防錆性能に優れ、かつ加工による悪影響を受けても第一層の上に加工性に劣る第二層が存在するため第一層の低Ｎｉ含有のＺｎＮｉ合金めっき層が悪影響を受けにくいためである。逆に、第一層が第二層より高Ｎｉ含有率である場合は、加工性および表層側の初期防錆性能に劣るため、第一層Ｎｉめっき層を形成した上に第二層ＺｎＮｉめっき層を形成したものに劣る耐食性しか得られない。このため、第一層と第二層のＮｉ含有率は、第二層が第一層より高Ｎｉ含有率である必要がある。具体的には、第一層のＺｎＮｉ合金めっき層のＮｉ含有率が５％未満では、十分な耐熱・耐食性が得られず、他方、９％を超えると曲げ加工部でめっき剥離が発生するおそれがあり、外観品質上問題であるため、第一層のＺｎＮｉ合金めっき層のＮｉ含有率を５～９％と規定したのである。又、第二層のＺｎＮｉ合金めっき層のＮｉ含有率を１０～１５％と規定したのは、前記第一層の場合と同様に、１０％未満では、十分な耐熱・耐食性が得られず、他方、１５％を超えると曲げ加工部でめっき剥離が発生するおそれがあり、外観品質上問題となるためである。
　以下、実施例に基づいて本発明をより具体的に説明する。ただし、本発明は下記実施例によって制限を受けるものではなく、趣旨を逸脱しない範囲で変更・実施することは、全て本発明の技術的範囲に含まれる。
　直径８ｍｍの燃料配管用鋼管を使用し、該鋼管の表面に第一層として、液温１５～２５℃、電流密度５Ａ／ｄｍ２でＮｉ含有率５％、層厚３μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層として液温１５～２５℃、電流密度５Ａ／ｄｍ２でＮｉ含有率１０％、層厚１μｍのＺｎＮｉ合金めっき層を形成し、さらに第二層の上にＰＨ４．０、液温３０℃で６０秒間、クロメート皮膜処理を施した。
　なお、本実施例における第一層のＺｎＮｉ合金めっき層の形成には、Ｚｎ：９．０ｇ／Ｌ、Ｎｉ：２．２ｇ／Ｌ、ＮａＯＨ：１２５．６ｇ／Ｌ、錯化剤及び光沢剤を適量含むめっき液を、同第二層のＺｎＮｉ合金めっき層の形成には、Ｚｎ：８．０ｇ／Ｌ、Ｎｉ：１．４ｇ／Ｌ、ＮａＯＨ：１３０．０ｇ／Ｌ、錯化剤及び光沢剤を適量含むめっき液を、それぞれ使用した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管をＲ１５で曲げ加工を施し、当該曲げ加工部の外観剥離を目視で観察した。次いで、曲げ加工後の試料を１５０℃で２４時間加熱した後、ＪＩＳＺ２３７１に基づく塩水噴霧試験で耐食性を評価した。これらの試験結果を表１に示す。
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率５％、層厚３μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率１０％、層厚３μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に示す。
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率１０％、層厚１μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に示す。
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率１０％、層厚３μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に示す。
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率９％、層厚９μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率１５％、層厚３μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に示す。
（比較例１）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率４％、層厚２μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率９％、層厚０．８μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（比較例２）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率１０％、層厚１０μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率１６％、層厚４μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験を行った結果を表１に併せて示す。
（比較例３）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率１０％、層厚１μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率５％、層厚３μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（比較例４）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率１０％、層厚３μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率５％、層厚３μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（比較例５）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率１０％、層厚１μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（比較例６）
　実施例１と同様のめっき層形成方法により、直径８ｍｍの燃料配管用鋼管の表面に第一層としてＮｉ含有率１０％、層厚３μｍのＺｎＮｉ合金めっき層を形成し、次いで第二層としてＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成した後、第二層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（従来例１）
　実施例１と同じ燃料配管用鋼管の表面に第一層として層厚０．５μｍのＮｉめっき層を形成し、次いで第二層としてＮｉ含有率８％、層厚５μｍのＺｎＮｉ合金めっき層を形成し、さらに第三層として実施例１と同様の方法によりＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成した後、第三層の上にクロメート皮膜を形成した。
　本従来例における第一層のＮｉめっき層は、ワット浴を使用し、液温５２～５７℃、電流密度５Ａ／ｄｍ２で形成した。又、第二層のＺｎＮｉ合金めっき層は、１００ｇ／ＬのＺｎＣｌ２、１３０ｇ／ＬのＮｉＣｌ２・６Ｈ２Ｏ、２００ｇ／ＬのＮＨ４Ｃｌ、ｐＨ５．７の酸性浴を使用し、液温３４～３６℃、電流密度３Ａ／ｄｍ２で形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
（従来例２）
　実施例１と同じ燃料配管用鋼管の表面に従来例１と同様の方法により、第一層として層厚３μｍのＮｉめっき層を形成し、同じく第二層としてＮｉ含有率８％、層厚５μｍのＺｎＮｉ合金めっき層を形成し、さらに第三層として実施例１と同様の方法によりＮｉ含有率５％、層厚５μｍのＺｎＮｉ合金めっき層を形成した後、第三層の上にクロメート皮膜を形成した。
　得られた複層ＺｎＮｉ合金めっき層を有する燃料配管用鋼管について、実施例１と同様の方法で曲げ加工部の外観剥離試験と塩水噴霧試験を行った結果を表１に併せて示す。
　表１の結果より、以下のように考察することができる。
（１）．第一層に加工性に有利な低Ｎｉ含有率のＺｎＮｉ合金めっき層を層厚３～９μｍ、第二層に耐食性を重視した第一層より高Ｎｉ含有率のＺｎＮｉ合金めっき層を層厚１～３μｍ形成した実施例１～５の本発明の燃料配管用鋼管は、いずれも曲げ加工部のめっき剥離現象は皆無であり、かつ当該曲げ加工部の赤錆発生までの時間より明らかなように耐食性にも優れることから、第一層にＮｉめっき層が存在しなくても同等の耐熱・耐食性が配管の曲げ加工部で得られる。
（２）．第一層及び第二層のＺｎＮｉ合金めっき層の層厚が本発明の規定値より外れた比較例１（規定層厚以下）のものは、塩水噴霧試験の結果（曲げ加工部の赤錆発生までの時間）より明らかのように、本発明の実施例１～５に比べ大きく劣っていることから好ましくない。
（３）．第一層及び第二層のＺｎＮｉ合金めっき層の層厚が本発明の規定値より外れた比較例２（規定層厚以上）のものは、曲げ加工部でめっき剥離が生じたことにより燃料配管用鋼管として採用できない。
（４）．第一層のＮｉ含有率が第二層のＮｉ含有率より高い比較例３～６は、塩水噴霧試験の結果（曲げ加工部の赤錆発生までの時間）より明らかのようにいずれも本発明の実施例１～５に比べ大きく劣っていることから好ましくない。
（５）．第一層をＮｉめっき層、第二層及び第三層をＺｎＮｉ合金めっき層で構成した従来例１、２は、曲げ加工には耐え得るものの、塩水噴霧試験の結果（曲げ加工部の赤錆発生までの時間）が本発明の実施例１～５より劣ることから、複層めっきの構成に問題があることがわかる。
　なお、ここでは燃料配管用鋼管のみの実施例について説明したが、本願発明は燃料配管用鋼管のみならず、自動車の各種配管に適用しても同様の作用効果が得られることはいうまでもないため、燃料配管用鋼管以外の他の自動車用配管については実施例を省略した。
Figure JPOXMLDOC01-appb-T000001

Claims (1)

  1. 　母材鋼管の表面に第一層として形成したＮｉ含有率５～９％、層厚３～９μｍのＺｎＮｉ合金めっき層と、該第一層のＺｎＮｉ合金めっき層上に第二層として被着したＮｉ含有率１０～１５％、層厚１～３μｍのＺｎＮｉ合金めっき層と、該第二層のＺｎＮｉ合金めっき層上に形成したクロメート皮膜とからなる複層めっき層を有することを特徴とする加工性に優れた耐熱・耐食性めっき層を有する配管。
PCT/JP2013/067670 2012-07-04 2013-06-27 加工性に優れた耐熱・耐食性めっき層を有する配管 WO2014007139A1 (ja)

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EP13812803.8A EP2871263B1 (en) 2012-07-04 2013-06-27 Pipe having heat-resistant corrosion-resistant plating layer that has excellent processability
RU2015103541A RU2636423C2 (ru) 2012-07-04 2013-06-27 Трубопровод, имеющий термостойкий и коррозионно-устойчивый плакирующий слой, который имеет превосходную обрабатываемость
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