WO2009119044A1 - 外面防食管、その製造方法、その管の外面の防食に用いられる合金線材の製造方法 - Google Patents
外面防食管、その製造方法、その管の外面の防食に用いられる合金線材の製造方法 Download PDFInfo
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- WO2009119044A1 WO2009119044A1 PCT/JP2009/001193 JP2009001193W WO2009119044A1 WO 2009119044 A1 WO2009119044 A1 WO 2009119044A1 JP 2009001193 W JP2009001193 W JP 2009001193W WO 2009119044 A1 WO2009119044 A1 WO 2009119044A1
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- Prior art keywords
- wire
- alloy
- mass
- less
- pipe
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- 229910045601 alloy Inorganic materials 0.000 title claims description 118
- 239000000956 alloy Substances 0.000 title claims description 118
- 238000004519 manufacturing process Methods 0.000 title claims description 32
- 238000005536 corrosion prevention Methods 0.000 title abstract description 7
- 238000000034 method Methods 0.000 title description 15
- 238000000576 coating method Methods 0.000 claims abstract description 52
- 239000011248 coating agent Substances 0.000 claims abstract description 50
- 229910020944 Sn-Mg Inorganic materials 0.000 claims abstract description 47
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 25
- 229910007610 Zn—Sn Inorganic materials 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims description 44
- 238000005507 spraying Methods 0.000 claims description 33
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000000498 cooling water Substances 0.000 claims description 15
- 230000005496 eutectics Effects 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 11
- 230000008018 melting Effects 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000009749 continuous casting Methods 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 description 67
- 239000011701 zinc Substances 0.000 description 56
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 29
- 238000010438 heat treatment Methods 0.000 description 26
- 230000000052 comparative effect Effects 0.000 description 25
- 229910052725 zinc Inorganic materials 0.000 description 20
- 238000005260 corrosion Methods 0.000 description 17
- 230000007797 corrosion Effects 0.000 description 16
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 15
- 238000005452 bending Methods 0.000 description 15
- 238000011156 evaluation Methods 0.000 description 14
- 239000007921 spray Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 235000019589 hardness Nutrition 0.000 description 9
- 238000005491 wire drawing Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 229910001018 Cast iron Inorganic materials 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 238000005266 casting Methods 0.000 description 6
- 239000008399 tap water Substances 0.000 description 6
- 235000020679 tap water Nutrition 0.000 description 6
- 238000007751 thermal spraying Methods 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004698 Polyethylene Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910000611 Zinc aluminium Inorganic materials 0.000 description 1
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
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- 235000020188 drinking water Nutrition 0.000 description 1
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- 239000003822 epoxy resin Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
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- 239000007779 soft material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C18/00—Alloys based on zinc
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/005—Continuous casting of metals, i.e. casting in indefinite lengths of wire
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/06—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
- B22D11/0611—Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/013—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of an iron alloy or steel, another layer being formed of a metal other than iron or aluminium
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
- C23C4/08—Metallic material containing only metal elements
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/123—Spraying molten metal
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/131—Wire arc spraying
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/12—All metal or with adjacent metals
- Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
- Y10T428/12771—Transition metal-base component
- Y10T428/12785—Group IIB metal-base component
- Y10T428/12792—Zn-base component
- Y10T428/12799—Next to Fe-base component [e.g., galvanized]
Definitions
- the present invention relates to an outer surface anticorrosion pipe, a method for manufacturing the same, and a method for manufacturing an alloy wire used for anticorrosion of the outer surface of the pipe, and in particular, a surface of a pipe made of an iron-based material such as a cast iron pipe has a corrosion prevention layer by a thermal spray coating.
- the present invention relates to a formed outer surface anticorrosion pipe, a method for producing the same, and a method for producing an alloy wire used for anticorrosion of the outer surface of the pipe.
- Metal pipes that can be put to practical use in a state where they are buried underground have been tar-based or bitumen-based for a long time to prevent corrosion.
- the corrosion of the metal tube proceeds from the scratch.
- a metallic coating with a greater ionization tendency than the metal pipe material is formed on the surface of the metal pipe, and a sacrificial anodic action is generated due to the difference in ionization tendency to prevent corrosion from scratches. Widely done.
- a typical metal having such a sacrificial anode action is zinc.
- a zinc coating is formed on the surface of a metal tube such as an iron tube by plating or thermal spraying.
- This film is used as it is as the outermost surface layer, or is used after further being overcoated.
- Zinc has a high tendency to ionize, for example, when used in combination with an iron-based metal, the electrochemical potential difference between iron and zinc is large, so even if some scratches occur in the coating, the sacrificial anodic action is exhibited, Corrosion at the scratch can be suppressed.
- the anticorrosion effect is further enhanced by covering the coating with a polyethylene sheet called a polyethylene sleeve and blocking it from the external environment. .
- a zinc-aluminum alloy may be used (WO94 / 19640). By adding aluminum, ionization is relaxed and the holding period of the sacrificial anodic action is prolonged.
- the present invention aims to solve the above-mentioned technical problems without significantly increasing the coating amount or using aluminum.
- the outer surface anticorrosion pipe of the present invention has an anticorrosion layer formed on the surface of the pipe made of an iron-based material, and this anticorrosion layer has Sn exceeding 1 mass% and less than 50 mass%.
- the alloy sprayed coating of the anticorrosion layer contains at least one of Ti, Co, Ni, and P, each of which exceeds 0.001% by mass and 3 It is preferable that it is less than mass%.
- the manufacturing method of the outer surface anticorrosion pipe of the present invention is characterized in that, when the outer surface anticorrosion pipe is manufactured, the alloy sprayed coating is heat-treated at a temperature higher than the eutectic temperature of the alloy and lower than the melting point.
- Another method of manufacturing the outer surface anticorrosion pipe of the present invention is to manufacture the above-mentioned outer surface anticorrosion pipe by using a Zn—Sn wire or a Zn—Sn—Mg wire, or at least one of Ti, Co, Ni, and P.
- a wire rod containing one of these is used as a first wire rod, and a Zn wire rod is used as a second wire rod, and arc spraying is performed simultaneously.
- the method for producing an alloy wire of the present invention dissolves a material in which Sn exceeds 1% by mass and less than 50% by mass, Mg exceeds 0.01% by mass and less than 5% by mass, and Zn is the balance. Then, the molten metal obtained by melting was solidified by a continuous casting machine so as to form a linear cast body, and the molten metal during solidification was changed from the eutectic temperature of the Zn—Sn—Mg alloy to 20 ° C./second. It cools to 50 degrees C or less with the above cooling rate, It is characterized by the above-mentioned.
- the outer anticorrosion layer of the pipe made of the iron-based material contains the Zn—Sn alloy sprayed coating or the Zn—Sn—Mg alloy sprayed coating, it is merely zinc sprayed.
- the anticorrosion performance can be remarkably improved as compared with that using a coating.
- Al since Al is not used, the problem of a hygiene side does not arise.
- soft Sn since soft Sn is used, it can be easily processed into a Zn—Sn-based wire or a Zn—Sn—Mg-based wire, and a sprayed material can be formed without any trouble.
- the sprayed alloy coating contains a predetermined amount of at least one of Ti, Co, Ni, and P, the anticorrosion performance can be further improved.
- the anticorrosion performance can be further improved by heat-treating the alloy sprayed coating at a temperature not lower than the eutectic temperature of the alloy and lower than the melting point.
- a Zn—Sn wire or a Zn—Sn—Mg wire, or a wire containing at least one of Ti, Co, Ni, and P as the first wire is used as the first wire.
- the solidified molten metal is rapidly cooled from the eutectic temperature of the Zn—Sn—Mg alloy to 50 ° C. or lower. Therefore, the zinc crystal can be made finer, and therefore the mechanical properties of the alloy wire can be improved. As a result, a Zn—Sn—Mg alloy wire that is difficult to break in the wire drawing process can be produced.
- the outer surface anticorrosion pipe of the present invention is such that an anticorrosion layer containing an alloy spray coating is formed on the surface of a pipe made of an iron-based material such as a cast iron pipe.
- the alloy sprayed coating is composed of a Zn—Sn-based alloy sprayed coating in which Sn exceeds 1 mass% and less than 50 mass%, and the balance is Zn.
- Sn exceeds 1 mass% and less than 50 mass%
- Zn the balance is Zn.
- the alloy sprayed coating has Sn exceeding 1 mass% and less than 50 mass%, Mg exceeding 0.01 mass% and less than 5 mass%, with the balance being Zn Zn—Sn—Mg-based thermal spray coating.
- the anticorrosion performance can be improved as compared with the sprayed coating using only Zn.
- the anticorrosion performance can be equal to or higher than that of Zn-15Al (Zn is 85 mass%, Al is 15 mass%).
- the alloy sprayed coating according to the first and second aspects of the present invention can contain at least one of Ti, Co, Ni, and P. That is, any one or two to four can be included together. It is preferable that each content is 0.001 mass% or more and 3 mass% or less. By including these elements in addition to Sn and Sn—Mg, the amount of the remaining Zn decreases accordingly.
- the anticorrosion performance can be further improved by containing these elements.
- the respective contents are less than 0.001% by mass, it is not possible to obtain a substantial effect of improving the anticorrosion performance by adding them.
- each content exceeds 3 mass%, the improvement effect of the substantial anti-corrosion performance by adding these cannot be acquired similarly.
- the anticorrosion layer contains the above-described alloy sprayed coating. It is particularly preferable that the anticorrosion layer is formed by laminating another coating such as a top coat on the alloy sprayed coating in addition to the alloy sprayed coating.
- the top coat can be applied with an acrylic resin-based paint or an epoxy resin-based paint.
- a method for manufacturing the outer surface anticorrosion pipe of the present invention that is, a method for forming an alloy sprayed coating will be described.
- a known spraying method that is, a Zn—Sn wire, a Zn—Sn—Mg wire, or at least one of Ti, Co, Ni, and P is used.
- a method of performing arc spraying using a wire rod containing selenium can be mentioned.
- thermal spraying using an alloy powder can be performed instead of the wire.
- the Zn—Sn alloy sprayed coating uses a Zn—Sn wire, or a wire containing at least one of Ti, Co, Ni, and P as the first wire. It can also be obtained by performing arc spraying simultaneously using the wire as the second wire.
- the Zn—Sn—Mg alloy film uses a Zn—Sn—Mg wire or a wire containing at least one of Ti, Co, Ni, and P as the first wire, It can also be obtained by performing arc spraying simultaneously using a Zn wire as the second wire.
- Zn-25Sn— instead of simultaneous arc spraying using two 0.5 Mg wires, arc spraying can be performed simultaneously using equal amounts of Zn-50Sn-1.0 Mg wire and Zn wire.
- the anticorrosion performance can be further improved.
- the amount of Zn—Sn—Mg wire used can be halved, the cost required for its preparation can be reduced.
- (A) For example, when arc spraying is simultaneously performed using a Zn—Sn—Mg alloy wire and a Zn wire, a Zn—Sn—Mg alloy and Zn are respectively formed in the sprayed coating formed thereby. Will be distributed. At this time, since the potential of the Zn—Sn—Mg alloy is lower than that of Zn, when these act as a sacrificial anode, the Zn—Sn—Mg alloy is preferentially melted. The dissolved Zn—Sn—Mg alloy forms another relatively stable coating on the surface of the coating, which suppresses the consumption or dissolution of the remaining Zn—Sn—Mg alloy and Zn. It can be considered that this is because.
- Zn present in the coating acts as a physical obstacle to suppress the dissolution of the Zn—Sn—Mg alloy, and when the Zn—Sn—Mg alloy is dissolved, the corrosion product is Zn. It can be considered that this is because dissolution is suppressed.
- the porosity of the Zn-25Sn-0.5Mg sprayed coating obtained by using two Zn-25Sn-0.5Mg wires is about 15%. there were.
- the porosity of the Zn-25Sn-0.5Mg sprayed coating obtained by using equal amounts of Zn-50Sn-1.0Mg wire and Zn wire was about 12%. That is, since the latter has a lower porosity, it can be considered that the anticorrosion performance is improved.
- the low porosity may be due to the fact that the Zn-50Sn-1.0Mg wire is softer than the Zn wire, so that the use of wires with different hardnesses may have an effect.
- the outer surface anticorrosion pipe of the present invention it is preferable to form an alloy sprayed coating on the cast iron pipe and heat-treat it at a temperature not lower than the eutectic temperature (198 ° C.) of the alloy and lower than the melting point.
- the heat treatment By performing the heat treatment in this way, the anticorrosion performance can be further improved.
- the reason is that only Sn is melted by heat treatment at a temperature exceeding the eutectic temperature of Zn—Sn alloy or Zn—Sn—Mg alloy, thereby filling the fine voids generated in the sprayed coating.
- the heat treatment time is not particularly limited, but is preferably 1 second to 60 minutes. If the heat treatment time is shorter than this range, the treatment time is insufficient and the necessary heat treatment cannot be performed.
- alloy wires used for metal spraying include a wire drawing step in which a wire having a predetermined cross-sectional shape is drawn and processed into an alloy wire having a predetermined wire diameter. In other words, it includes a processing step of reducing the diameter of the wire. At this time, if the material for the wire has no strength or ductility, it may break. In order to cope with this, heat treatment or the like may be performed depending on the material of the wire. In particular, the Zn—Sn—Mg alloy wire becomes slightly brittle when the amount of Sn is small, so that the workability is lowered and the wire may be broken in the wire drawing step as described above.
- the method for producing a Zn—Sn—Mg alloy wire of the present invention is a production method that is difficult to break in the wire drawing step.
- this manufacturing method dissolves a material in which Sn exceeds 1 mass% and less than 50 mass%, Mg exceeds 0.01 mass% and less than 5 mass%, and Zn is the balance. Then, while the molten metal obtained by melting is solidified by a continuous casting machine so as to form a linear cast body, the molten metal being solidified is changed from the eutectic temperature of the Zn—Sn—Mg alloy to 20 ° C. / Cool to 50 ° C. or lower at a cooling rate of at least 2 seconds. If it carries out like this, a zinc crystal can be refined
- FIG. 1 shows the configuration of a manufacturing apparatus for carrying out this manufacturing method.
- a continuous casting machine 101 and a winder 102 are provided.
- a groove 112 having a U-shaped cross section is formed on the outer periphery of a rotary casting wheel 111.
- a crucible 115 is disposed above the casting wheel 111.
- the crucible 115 can store a molten metal 103 of Zn—Sn—Mg alloy in the crucible 115 and has a hot water outlet 116 formed at the bottom thereof.
- a spray nozzle 113 is provided in the vicinity of the crucible 115, and the spray nozzle 113 is provided with an outlet 114 for spraying cooling water.
- the molten metal 103 is supplied from the crucible 115 to the portion of the groove 112 positioned at the top of the casting wheel 111 while slowly rotating the casting wheel 111. Then, the molten metal 103 starts to solidify when heat is taken away by the casting wheel 111. Immediately thereafter, cooling water is sprayed from the spray nozzle 113 toward the molten metal 104 in the groove 12 that is solidifying.
- the molten metal 104 being solidified is rapidly cooled, and the alloy wire 105 is manufactured. Since this alloy wire 105 is formed by rapid cooling of the molten metal 104 during solidification, the crystal becomes fine, and therefore the ductility can be improved.
- the obtained alloy wire 105 is wound up by the winder 102.
- Rapid cooling by spraying cooling water from the spray nozzle 113 toward the molten metal 104 being solidified is preferably performed immediately after pouring the molten metal 103 into the groove 102 as much as possible.
- cooling is performed by cooling from a eutectic temperature of Zn—Sn—Mg-based alloy from 198 ° C. to 50 ° C. at a cooling rate of 20 ° C./second or more. It is necessary to adopt conditions.
- the cooling method may be air cooling with cold air, or cooling using other fluid, in addition to the water cooling described above.
- the alloy wire 105 wound by the winder 102 is then subjected to a wire drawing process.
- the workability to wire was evaluated by preparing an alloy lump having a diameter of 47 mm and a length of 350 mm and measuring the Vickers hardness.
- the alloy lump after the hardness was measured was forged to a diameter of 10 mm and further drawn to a diameter of 1.6 mm, and the workability was evaluated according to the following criteria.
- red rust the period until red rust occurs in the salt spray test in the case where only Zn is sprayed and heat treatment is not performed is set to “1”. In the case where only the Zn—Sn—Mg alloy was sprayed, the period until red rust occurred in the salt spray test was evaluated numerically for the test sample when not subjected to heat treatment.
- Examples 1 to 6, Comparative Examples 1 to 4 A Zn—Sn alloy having the component composition shown in Table 1 was sprayed onto a test piece to obtain test samples of Examples 1 to 6 and Comparative Examples 1 to 4. The evaluation results for these test samples are shown in Table 1. Comparative Example 3 was sprayed only with Zn, and Comparative Example 4 was sprayed with Sn only.
- Example 1 to 6 and Comparative Examples 1 to 4 when Ti, Co, Ni, and P were added and a salt spray test was performed, when Ti, Co, Ni, and P were added alone, The same evaluation results were obtained for the period until red rust was generated when the addition amount was changed. Therefore, in Table 1, only one representative example is shown for simplicity. Specifically, Table 1 shows that in Examples 1 to 6 and Comparative Examples 1 to 4, the addition amount of each of Ti, Co, Ni, and P is 0.001, 0.01, 0.1, 1 This means that the same evaluation result was obtained when the content was changed to 3% by mass.
- Examples 7 to 42, Comparative Examples 5 to 18 Zn—Sn—Mg alloys having the composition shown in Table 2 were sprayed onto the test pieces to obtain test samples of Examples 7 to 42 and Comparative Examples 5 to 14.
- the evaluation results for the test samples of Examples 7 to 30 are shown in Table 2, and the evaluation results for the test samples of Examples 31 to 42 and Comparative Examples 5 to 14 are shown in Table 3.
- Comparative Examples 3 and 4 are shown again in Tables 2 and 3.
- Examples 7 to 42 and Comparative Examples 5 to 18 when Ti, Co, Ni, and P are added individually and a salt spray test is performed, red rust is generated when the addition amount is changed. The same evaluation results were obtained for all the periods up to. Therefore, in Tables 2 and 3, only one representative example is shown for simplicity as in Table 1. Specifically, in Examples 7 to 42 and Comparative Examples 5 to 18, when any of Ti, Co, Ni, and P is added, the amount added is 0.001, 0.01, 0.1, 1, When changed to 3% by mass, the same evaluation results were obtained as shown in Tables 2 and 3.
- Example 43 to 53 As shown in Table 4, arc spraying was simultaneously performed using a Zn—Sn—Mg wire as the first wire and a Zn wire as the second wire. The results are shown in Table 4. At this time, similarly to the above-described examples, in Examples 43 to 53, when Ti, Co, Ni, and P were added and a salt spray test was performed, any of Ti, Co, Ni, and P was used alone. Even when added, the same evaluation results were obtained for the period until red rust was generated when the amount added was changed. Therefore, in Table 4, only one representative example is shown for simplicity.
- the anticorrosion effect is improved by heat treatment for 30 minutes. I was able to.
- the corrosion resistance when immersed in tap water and the corrosion resistance when immersed in sulfuric acid were also excellent.
- Comparative Example 1 since the blending ratio of Sn was lower than the range of the present invention, the blending ratio of Zn was correspondingly high, and accordingly, the occurrence of white rust corresponding thereto was observed. In addition, since the blending ratio of Sn was lower than the range of the present invention, it is difficult for Sn to exert the function of suppressing the elution of Zn. Therefore, the period until red rust is generated is extremely compared with Examples 1 to 6. It was short.
- Comparative Example 3 was sprayed only with Zn, white rust was generated more than Comparative Example 1, and the period until red rust was also shorter.
- Comparative Example 4 was obtained by spraying only Sn, the period until red rust was generated was shorter than that of Comparative Example 2.
- Example 7 to 42 the occurrence of white rust was small, and the period until red rust was generated was long and had sufficient anticorrosion performance.
- the period until red rust was generated was as excellent as that of the known Zn-15Al alloy.
- the corrosion resistance could be further improved.
- heat treatment specifically, when heat treatment is performed at a temperature in the range of 198 ° C. or higher which is the eutectic temperature of the alloy constituting the thermal spray coating and less than the melting point of the alloy thermal spray coating, the anticorrosion effect is improved by heat treatment for 30 minutes. I was able to.
- the corrosion resistance when immersed in tap water and the corrosion resistance when immersed in sulfuric acid were also excellent.
- Comparative Example 5 had no problem with the proportion of Mg, but the proportion of Sn was lower than the range of the present invention, so the proportion of Zn was high accordingly, and accordingly Corresponding white rust was observed. Also, the period until red rust was generated was shorter than in Examples 7 to 42.
- Example 43, 44, 45, 46, 47, 48, 49, and 50 in order to obtain a film having the same composition as in Examples 7, 12, 13, 18, 19, 24, 25, and 30, Sn amount and Mg A Zn—Sn—Mg line whose amount was doubled and a Zn line containing only Zn were used.
- Sn amount and Mg A Zn—Sn—Mg line whose amount was doubled and a Zn line containing only Zn were used.
- At least one of Ti, Co, Ni, and P is added to a Zn—Sn alloy or Zn—Sn—Mg alloy, and a sprayed coating is formed after spraying.
- the heat treatment was performed at a temperature in the range of 198 ° C. or higher which is the eutectic temperature of the alloy and less than the melting point of the alloy sprayed coating, the corrosion resistance could be further improved.
- Example 54 Hereinafter, the Example of the manufacturing method of the alloy wire of this invention is described.
- an alloy wire 105 having a diameter of 10 mm in which the crystal became fine and the ductility was improved under the conditions described later was obtained.
- the alloy wire 105 was processed into an alloy wire having a diameter of 1.6 mm by a wire drawing machine (not shown).
- the cooling water was sprayed at different times. More specifically, as shown in Table 5, the test pieces 1 to 4 were manufactured by changing the timing of spraying the cooling water (hereinafter referred to as “water cooling timing”).
- the water cooling timing was changed based on the timing at which the molten metal 103 discharged from the outlet 116 of the crucible 115 shown in FIG. 1 reached the groove 102 (hereinafter referred to as “arrival timing”). Specifically, the position of the spray nozzle 113 shown in FIG. 1 was adjusted along the direction of rotation of the casting wheel 111 so that the required water cooling timing was reached.
- the obtained specimens 1 to 4 were subjected to a tensile test to measure the tensile strength and elongation. Further, a bending test was performed to measure the load and the break angle. Further, the Vickers hardness Hv was measured. The average value of the results of six measurements was taken as the measurement result.
- the bending test was performed according to JIS Z 2248 “Metal material bending test method”. Specifically, as shown in FIG. 2, a test piece 150 having a diameter of 1.6 mm with the axial direction set in the horizontal direction is placed on a pair of supports 161 and 162 having a diameter of 10 mm and spaced apart in the horizontal direction. I placed it. A load 170 was applied to the test piece 150 in the vertical direction between the support 161 and the support 162 by a pressing member 163 having a semicircular shape with a radius of 5 mm at the tip end.
- the test piece 150 was deformed into a V shape as shown in FIG.
- the bending angle ⁇ generated by the intersection of the extension line of the part 151 in contact with one support 161 and the extension line of the part 152 in contact with the other support 162 in the test piece 150 It was measured.
- the bending angle ⁇ is an angle when the load 170 is applied, and is not an angle after the load is removed. At this time, the presence or absence of tears, scratches and other defects in the outer portion of the curved portion 153 of the test piece 150 was investigated.
- Test piece 1 An alloy wire manufactured under conditions without water cooling was designated as test piece 1.
- the test piece 1 was broken when the tensile strength was 125 N / mm 2 , the elongation was 1%, the load when the bending test was performed was 20 N, and the bending angle ⁇ was 40 degrees.
- the Vickers hardness Hv was 26.
- Table 5 shows the evaluation results for the test piece 1.
- Test piece 2 An alloy wire produced under conditions with water cooling was designated as test piece 2.
- the water cooling timing was 30 seconds after the arrival timing at which the molten metal 103 shown in FIG. During cooling, normal temperature cooling water was continuously sprayed for 5 to 10 seconds.
- the temperature of the molten metal 104 before water cooling was 200 to 250 ° C.
- the temperature of the wire 105 after water cooling was 20 to 40 ° C.
- the test piece 2 was fractured when the tensile strength was 154 N / mm 2 , the elongation was 10%, the load during the bending test was 25 N, and the bending angle ⁇ was 150 degrees.
- the Vickers hardness Hv was 35.
- Table 5 shows the evaluation results for the test piece 2.
- Test piece 3 An alloy wire manufactured under conditions with water cooling was used as a test piece 3.
- the water cooling timing was 15 seconds after the above arrival timing. During cooling, normal temperature cooling water was continuously sprayed for 5 to 10 seconds.
- the temperature of the molten metal 104 before water cooling was 250 to 300 ° C.
- the temperature of the wire 105 after water cooling was 30 to 50 ° C.
- This test piece 3 had a tensile strength of 150 N / mm 2 and an elongation of 14%. As a result of the bending test, even when the load was 25 N and the bending angle was 180 degrees, it did not break.
- the Vickers hardness Hv was 35.
- Table 5 shows the evaluation results for the test piece 3.
- Test piece 4 An alloy wire manufactured under conditions with water cooling was used as a test piece 4. The water cooling timing was 5 seconds after the arrival timing. During cooling, normal temperature cooling water was continuously sprayed for 5 to 10 seconds. The temperature of the molten metal 104 before water cooling was 300 to 350 ° C., and the temperature of the wire 105 after water cooling was 30 to 50 ° C. This test piece 4 had a tensile strength of 155 N / mm 2 and an elongation of 16%. As a result of the bending test, even when the load was 25 N and the bending angle was 180 degrees, it did not break. The Vickers hardness Hv was 35.
- Table 5 shows the evaluation results for the test piece 4.
- FIG. 3 shows the result of observing the structure of the test piece 1 manufactured under conditions without water cooling with an optical microscope. As shown in the figure, a dendritic structure formed by precipitation of zinc crystals in a dendritic shape was observed. In FIG. 3, a black part is a zinc crystal and a white part is a eutectic.
- FIG. 4 shows the result of observing the structure of the test piece 4 manufactured under conditions with water cooling with an optical microscope. As shown in the figure, an acicular structure formed by precipitation of zinc crystals in an acicular shape was observed. Furthermore, the zinc crystal was finer than the alloy wire of FIG. 3 manufactured under the condition without water cooling.
- the mechanical properties of the alloy wire were improved. Furthermore, the earlier the timing of spraying the cooling water, the better results were obtained. Specifically, as is apparent from the measurement results of the tensile test, the test pieces 2 to 4 manufactured under the condition with water cooling are higher in tensile strength than the test piece 1 manufactured under the condition without water cooling. Improved by about 20%, and the growth improved significantly. Moreover, it was shown that it was hard to fracture
- test piece 3 with the earlier timing of injecting the cooling water than the test piece 2 was harder to break.
- test piece 4 whose timing of injecting the cooling water was earlier than that of the test piece 3 was larger in elongation.
- the zinc crystals could be refined and the mechanical properties of the alloy wire could be improved. Furthermore, by increasing the timing of spraying the cooling water, it was possible to promote the refinement of zinc crystals and improve ductility in particular.
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Abstract
Description
直径47mm×長さ350mmの合金塊を作製し、ビッカース硬さ測定することによって、線材への加工性を評価した。また硬さを測定した後の合金塊を鍛造して直径10mmに縮径するようにし、さらに直径1.6mmまで伸線するようにして、その加工性を下記の基準により評価した。
×:伸線工程で破断が発生
(2)耐食性
下記の要領で耐食試験を行い評価した。すなわち、150mm×70mm×2mmのサンドブラスト鋼板を試験片として用い、これに、直径1.6mmの線材を用いた電気式アーク溶射方法によって、溶射量130g/m2で、厚さ20~30μmの溶射被膜を形成して供試サンプルとした。腐食試験および評価方法は、次の通りとした。
JIS Z2371に規定される塩水噴霧試験を実施し、Zn-Sn合金のみを溶射した場合またはZn-Sn-Mg合金のみを溶射した場合において、熱処理を施していないときの、白錆の発生程度と、赤錆が発生するまでの期間とにより評価した。白錆の発生程度は、目視にて、下記の基準により評価した。
△:白錆の発生が中程度
×:白錆の発生が多い
(2-2)
赤錆については、Znのみを溶射し熱処理を施していない場合の塩水噴霧試験における赤錆が発生するまでの期間を「1」として、それとの対比のうえで、Zn-Sn合金のみを溶射した場合またはZn-Sn-Mg合金のみを溶射した場合において、熱処理を施していないときの供試サンプルについて塩水噴霧試験における赤錆が発生するまでの期間を数値で評価した。
Ti、Co、Ni、Pのいずれかを単独で添加し、熱処理を施していないときの、塩水噴霧試験の際に赤錆が発生するまでの期間について評価した。詳細には、これらを添加しないZn-Sn合金のみの場合またはZn-Sn-Mg合金のみの場合において、熱処理を施していないときの赤錆が発生するまでの期間を「1」として、それとの対比のうえで、下記の基準により評価した。
○:赤錆が発生するまでの期間が1.0倍以上1.5倍未満に伸びた
△:赤錆が発生するまでの期間はほぼ同じであった
(2-4)
Ti、Co、Ni、Pを添加せずにZn-Sn合金のみを溶射した場合またはZn-Sn-Mg合金のみを溶射した場合において、熱処理を施したときの、塩水噴霧試験の際に赤錆が発生するまでの期間について評価した。詳細には、供試サンプルについて、30分間の熱処理を施した場合において、熱処理を施さない場合に比べて赤錆が発生するまでの期間が伸びて防食効果が向上したと評価できる熱処理温度の範囲を測定した。
Ti、Co、Ni、Pを添加していない供試サンプルであって、熱処理を施していないものを、30℃の水道水中に浸漬して、赤錆が発生するまでの期間について評価した。詳細には、Znのみを溶射した場合の赤錆が発生するまでの期間を「1」として、それとの対比のうえで、供試サンプルについて赤錆が発生するまでの期間を数値で評価した。
Ti、Co、Ni、Pを添加していない供試サンプルであって、熱処理を施していないものを、30℃のpH3の硫酸中に浸漬して、赤錆が発生するまでの期間について評価した。詳細には、Znのみを溶射した場合の赤錆が発生するまでの期間を「1」として、それとの対比のうえで、供試サンプルについて赤錆が発生するまでの期間を数値で評価した。
表1に示す成分組成のZn-Sn合金を試験片に溶射して、実施例1~6、比較例1~4の供試サンプルを得た。これらの供試サンプルについての評価結果を表1に示す。比較例3はZnのみを溶射したものであり、比較例4はSnのみを溶射したものである。
表2に示す成分組成のZn-Sn-Mg合金を試験片に溶射して、実施例7~42、比較例5~14の供試サンプルを得た。実施例7~30の供試サンプルについての評価結果を表2に示し、実施例31~42、比較例5~14の供試サンプルについての評価結果を表3に示す。参考のために、表2および表3に比較例3と比較例4を再掲する。
表4に示すように、Zn-Sn-Mg線材を第1の線材として用いるとともに、Zn線材を第2の線材として用いて、同時にアーク溶射を行った。その結果を表4に示す。このとき、上述の実施例と同様に、実施例43~53において、Ti、Co、Ni、Pを添加して塩水噴霧試験を実施した場合は、Ti、Co、Ni、Pのいずれを単独で添加した場合も、その添加量を変化させたときの赤錆が発生するまでの期間について、すべて同一の評価結果が得られた。そこで、表4でも、簡単のために、代表例一つのみを記載した。
以下、本発明の合金線材の製造方法の実施例を説明する。
水冷なしの条件で製造された合金線材を試験片1とした。この試験片1は、引張強さが125N/mm2、伸びが1%、曲げ試験を行ったときの荷重が20Nで、曲げ角度θが40度となったときに破断した。ビッカース硬さHvは26であった。
水冷ありの条件で製造された合金線材を試験片2とした。水冷タイミングは、図1に示される溶湯103が溝102に到達した到達タイミングから30秒後とした。冷却に際しては、常温の冷却水を連続的に5~10秒間噴霧した。水冷前の溶湯104の温度は200~250℃であり、水冷後の線材105の温度は20~40℃であった。この試験片2は、引張強さが154N/mm2、伸びが10%、曲げ試験を行っときの荷重が25Nで、曲げ角度θが150度となったときに破断した。ビッカース硬さHvは35であった。
水冷ありの条件で製造された合金線材を試験片3とした。水冷タイミングは、上述の到達タイミングから15秒後とした。冷却に際しては、常温の冷却水を連続的に5~10秒間噴霧した。水冷前の溶湯104の温度は250~300℃であり、水冷後の線材105の温度は30~50℃であった。この試験片3は、引張強さが150N/mm2で、伸びが14%であった。曲げ試験を行った結果、荷重が25Nで曲げ角度が180度でも破断しなかった。ビッカース硬さHvは35であった。
水冷ありの条件で製造された合金線材を試験片4とした。水冷タイミングは、到達タイミングから5秒後とした。冷却に際しては、常温の冷却水を連続的に5~10秒間噴霧した。水冷前の溶湯104の温度は300~350℃であり、水冷後の線材105の温度は30~50℃であった。この試験片4は、引張強さが155N/mm2で、伸びが16%であった。曲げ試験を行った結果、荷重が25Nで曲げ角度が180度でも破断しなかった。ビッカース硬さHvは35であった。
Claims (6)
- 鉄系材料で構成された管の表面に防食層が形成され、この防食層は、Snが1質量%を超えかつ50質量%未満であり、残部がZnであるZn-Sn系合金溶射被膜と、Snが1質量%を超えかつ50質量%未満であり、Mgが0.01質量%を超えかつ5質量%未満であり、残部がZnであるZn-Sn-Mg系合金溶射被膜とのいずれかを含有することを特徴とする外面防食管。
- 防食層の合金溶射被膜が、Ti、Co、Ni、Pのうち少なくともいずれか一つを含み、その含有量は、各々が、0.001質量%を超えかつ3質量%未満であることを特徴とする請求項1記載の外面防食管。
- 請求項1に記載の外面防食管を製造するに際し、合金溶射被膜を合金の共晶温度以上かつ融点未満の温度で熱処理することを特徴とする外面防食管の製造方法。
- 請求項1に記載の外面防食管を製造するに際し、Zn-Sn線材またはZn-Sn-Mg線材、またはこれにTi、Co、Ni、Pのうち少なくともいずれか一つを含ませた線材を第1の線材として用いるとともに、Zn線材を第2の線材として用いて、同時にアーク溶射を行うことを特徴とする外面防食管の製造方法。
- Snが1質量%を超えかつ50質量%未満であり、Mgが0.01質量%を超えかつ5質量%未満であり、Znが残部である素材を溶解し、
溶解により得た溶湯を連続鋳造機で線状の鋳造体となるように凝固させながら、その凝固中の溶湯を、Zn-Sn-Mg系合金の共晶温度以上から、20℃/秒以上の冷却速度で50℃以下まで冷却することを特徴とするZn-Sn-Mg系合金線の製造方法。 - 線状の鋳造体となるように凝固中の溶湯に、冷却水を噴霧することを特徴とする請求項5記載のZn-Sn-Mg系合金線の製造方法。
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EP09725795.0A EP2270250B1 (en) | 2008-03-24 | 2009-03-18 | Pipe provided with corrosion prevention layer on the outside surface and process for production of pipe |
KR1020107008597A KR101512681B1 (ko) | 2008-03-24 | 2009-03-18 | 외면 방식관, 그 제조 방법, 그 관의 외면의 방식에 이용되는 합금 선재의 제조 방법 |
US12/733,569 US8828556B2 (en) | 2008-03-24 | 2009-03-18 | Pipe provided with corrosion prevention layer on the outside surface |
US14/265,468 US20140234158A1 (en) | 2008-03-24 | 2014-04-30 | Pipe provided with corrosion prevention layer on the outside surface, process for production of the same, and process for production of alloy wires used for the corrosion prevention layer |
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JP5572128B2 (ja) * | 2011-02-04 | 2014-08-13 | 株式会社神戸製鋼所 | 耐食性アルミニウム合金部材、および、オープンラック式気化器の伝熱管またはヘッダー管 |
CN102168208A (zh) * | 2011-04-08 | 2011-08-31 | 江苏美特林科特殊合金有限公司 | 一种玻璃镀膜用ZnSn溅射靶材的制造方法 |
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CN104685093A (zh) * | 2012-08-03 | 2015-06-03 | 液态金属涂料有限公司 | 含金属涂层以及其使用和制备方法 |
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Also Published As
Publication number | Publication date |
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CN101809183A (zh) | 2010-08-18 |
TR201006923T1 (tr) | 2011-07-21 |
US20140234158A1 (en) | 2014-08-21 |
EP2270250A4 (en) | 2017-09-13 |
KR101512681B1 (ko) | 2015-04-16 |
KR20100128273A (ko) | 2010-12-07 |
US20140230948A1 (en) | 2014-08-21 |
CN101809183B (zh) | 2012-01-18 |
US20100193063A1 (en) | 2010-08-05 |
US9540713B2 (en) | 2017-01-10 |
EP2270250B1 (en) | 2019-05-22 |
EP2270250A1 (en) | 2011-01-05 |
US8828556B2 (en) | 2014-09-09 |
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