CA2596825C - Coated steel sheet or strip - Google Patents
Coated steel sheet or strip Download PDFInfo
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- CA2596825C CA2596825C CA2596825A CA2596825A CA2596825C CA 2596825 C CA2596825 C CA 2596825C CA 2596825 A CA2596825 A CA 2596825A CA 2596825 A CA2596825 A CA 2596825A CA 2596825 C CA2596825 C CA 2596825C
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- Prior art keywords
- coating
- weight
- strip
- steel
- melt
- Prior art date
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 38
- 239000010959 steel Substances 0.000 title claims abstract description 38
- 239000011248 coating agent Substances 0.000 claims abstract description 60
- 238000000576 coating method Methods 0.000 claims abstract description 60
- 238000012360 testing method Methods 0.000 claims abstract description 16
- 239000011701 zinc Substances 0.000 claims abstract description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 13
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000155 melt Substances 0.000 claims description 22
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000007921 spray Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000005246 galvanizing Methods 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000002893 slag Substances 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910000765 intermetallic Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000007797 corrosion Effects 0.000 abstract description 14
- 238000003466 welding Methods 0.000 abstract description 12
- 238000010276 construction Methods 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000003618 dip coating Methods 0.000 abstract 1
- 230000035515 penetration Effects 0.000 abstract 1
- 238000005507 spraying Methods 0.000 abstract 1
- 239000003973 paint Substances 0.000 description 9
- 239000011777 magnesium Substances 0.000 description 7
- 229910001335 Galvanized steel Inorganic materials 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000008397 galvanized steel Substances 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000009863 impact test Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000012031 short term test Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
- C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
- C23C2/0222—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating in a reactive atmosphere, e.g. oxidising or reducing atmosphere
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
- C23C2/06—Zinc or cadmium or alloys based thereon
-
- 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
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/14—Removing excess of molten coatings; Controlling or regulating the coating thickness
- C23C2/16—Removing excess of molten coatings; Controlling or regulating the coating thickness using fluids under pressure, e.g. air knives
- C23C2/18—Removing excess of molten coatings from elongated material
- C23C2/20—Strips; Plates
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/30—Fluxes or coverings on molten baths
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
- C23C2/36—Elongated material
- C23C2/38—Wires; Tubes
-
- 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
- C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
- C23C2/34—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the shape of the material to be treated
- C23C2/36—Elongated material
- C23C2/40—Plates; Strips
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Coating With Molten Metal (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
Abstract
The invention relates to a coated steel sheet or coil having a base layer which is composed of steel and to whose at least one top face is applied, by hot dip coating, a zinc coating. In the case of such steel sheets or steel coils, the zinc coating ensures a high level of corrosion resistance. The thicker the coating, the greater this resistance. Thus, in the case of a conventionally alloyed zinc coating, in a spraying test performed on a bright, uncoated sample in accordance with DIN 50021, red rust occurs after just 24 hours in the case of a coat add-on of 25 g/m2 , whereas with a coating add-on of 70 g/m2 red rust is formed only after 120 hours. The thickness of the coating that is needed in the prior art for sufficient corrosion resistance, however, brings problems with it in connection with weldability. This is the case in particular when laser welding at high welding speeds is to be used to produce a penetration weld in the lap joint without a minimum joining gap, of the kind required in particular in the field of the construction of car bodies or in the field of household engineering. The seam produced by such welding ought to be free from through-holes, to possess substantially no craters and to have no open pores.
Description
COATED STEEL SHEET OR STRIP
The invention relates to a coated steel sheet or strip, with a ground coating made of steel, onto at least one upper side of which a zinc coating is applied by hot-dip galvanizing.
On steel sheets or steel strips of this type the zinc coating ensures a high degree of corrosion resistance.
The thicker the coating is, the greater the resistance.
Accordingly, with a conventionally alloyed zinc coating, in a spray test according to DIN 50021 carried out on a bright, unpainted specimen, with a coating of 25 g/m2, red rust already occurs after 24 hours, while with a coating of 70 g/m2 red rust does not occur until after 120 hours.
The thickness of the coating required with the prior art for adequate corrosion resistance does, however, incur problems with regard to weldability. This applies in particular if the intention is that through-welding is to be produced by means of laser welding in the overlap joint without any joint gaps at high welding speeds, such as is required in the motor vehicle chassis construction sector or the domestic engineering sector. The seam produced by such welding should be free of passage holes, should be largely free of cratering, and should not have any open pores.
One possibility for manufacturing hot-dip galvanized steel sheets with increased corrosion resistance with simultaneously reduced coating weight is described in EP
The invention relates to a coated steel sheet or strip, with a ground coating made of steel, onto at least one upper side of which a zinc coating is applied by hot-dip galvanizing.
On steel sheets or steel strips of this type the zinc coating ensures a high degree of corrosion resistance.
The thicker the coating is, the greater the resistance.
Accordingly, with a conventionally alloyed zinc coating, in a spray test according to DIN 50021 carried out on a bright, unpainted specimen, with a coating of 25 g/m2, red rust already occurs after 24 hours, while with a coating of 70 g/m2 red rust does not occur until after 120 hours.
The thickness of the coating required with the prior art for adequate corrosion resistance does, however, incur problems with regard to weldability. This applies in particular if the intention is that through-welding is to be produced by means of laser welding in the overlap joint without any joint gaps at high welding speeds, such as is required in the motor vehicle chassis construction sector or the domestic engineering sector. The seam produced by such welding should be free of passage holes, should be largely free of cratering, and should not have any open pores.
One possibility for manufacturing hot-dip galvanized steel sheets with increased corrosion resistance with simultaneously reduced coating weight is described in EP
0 038 904 Bl. According to this prior art, a zinc coating containing 0.2 % by weight Al and 0.5 % by weight Mg is applied on a steel substrate by hot-dip galvanizing. As a result of the magnesium content, the hot-dip galvanized steel strip obtained in this way, with a coating weight of 44 g/m2 per side, in the painted state, had first rust formation only after a spray duration of more than 2,000 hours under a salt spray test in which the individual specimen was sprayed with an NaCl solution under the conditions specified in Japanese Industrial Standard JIS
Z 2371. This long period before the occurrence of rust was achieved thanks to the combined corrosion protection of the zinc coating and painting.
Despite the reduction in the coating weight achieved in accordance with EP 0 038 904 Bl and the simultaneous good corrosion resistance, the hot-dip galvanized steel sheets produced in this way still do not fulfil the requirements imposed in the motor vehicle construction sector with regard to weldability.
The object of the invention was therefore to create a flat steel product which possesses an optimum combination of high corrosion resistance and optimum weldability and which is particularly well-suited for use as a material for motor vehicle chassis construction or for the production of domestic appliances.
This object is resolved according to the invention by a coated steel sheet or strip, which has a ground coating made of steel, onto at least one upper side of which a coating is applied by hot-dip galvanizing, the coating being formed from a melt consisting of 0.05 - 0.30 % by weight Al and 0.2 - 2.0 % by weight Mg, the remainder being zinc and unavoidable impurities, and on each side, with a coating thickness of a maximum of 3.5 pm and a coating weight of a maximum of 25 g/m2, guarantees that the steel sheet, in the salt spray mist test carried out in accordance with DIN 50021-SS, shows the first formation of red rust at the earliest after 250 hours.
A hot-dip galvanized flat steel product according to the invention possesses surprisingly good corrosion resistance with a coating weight minimised in relation to the prior art coating weight of a maximum of 25 g/m2 on each side. The low coating weight and the low thickness of the coating associated with this, of a maximum of 3.5 pm on each side, in combination with the high corrosion resistance, makes sheet or strip according to the invention particularly well-suited for the production of components which are manufactured by the welding of individual sheet elements. Accordingly, with steel sheets produced in accordance with the invention, elements for motor vehicle chassis or domestic appliance technology can be manufactured in particular, in that the individual sheet components formed from sheet or strip according to the invention can be welded to one another by laser beam welding at high welding speeds economically and with optimum results.
The corrosion resistance according to the invention is determined on the basis of a salt spray mist test in accordance with DIN 50021-SS in a corrosion short-term test process on bright unpainted steel sheet, in which a neutral 5% NaCl solution, as the corrosive agent, is sprayed continuously at a temperature of 35 2 C in a chamber. The steel sheet samples are in this situation placed in the chamber at an angle of inclination to the horizontal of 65 to 75 . In the practical test carried out in this manner, it has been demonstrated that sheets and strips coated in accordance with the invention regularly do not show any red rust formation until after a test duration of 300 hours.
The magnesium content in the melt intended for the coating remains essentially unchanged in the coating. The Al content of the coating, in the finished steel strip according to the invention, by contrast, is as a rule 1.8 to 3.2 and in particular 2 to 3 times higher than in the melt. An optimum corrosion protection is attained when the coating has an Mg content of 0.4 - 1.0 % by weight, in particular at least 0.5 % by weight.
If it is intended that the coating of the steel base material is to be carried out in the galvanealed process, the melt contains preferably less than 0.15 % by weight of aluminium. Al contents of the melt which are suitable for standard practice are in this case in the range of 0.12 - 0.14 % by weight.
If, by contrast, a conventionally hot-dip galvanized steel sheet according to the invention is provided, the Al content of the melt is preferably at least 0.15 % by weight.
A further surprising property which makes a flat product according to the invention particularly suitable for use in chassis construction becomes apparent when such a sheet or strip is painted. Accordingly, a mandrel bend test carried out on the basis of DIN EN ISO 6860 for sheets or strips according to the invention at room temperature and at -20 C produces good paint adherence -capacity. In particular, at a temperature of -20 C there is no indication of paint flaking or of flaking of the coating from the base material.
For the test carried out to determine the paint adherence capacity, a full paint structure was applied onto a steel sheet specimen after alkaline cleaning and phosphating, this structure comprising a 20 pm thick cathodic dip paint coating, a 32 pm thick filler paint coating applied onto this and a 40 pm thick base coating. The bending carried out over the conical mandrel did not lead to any detachment of the paint coating at room temperature or at -20 C.
In addition to a high corrosion resistance and a good paint adherence capacity, sheets or strips according to the invention have outstandingly good resistance to stone impact. Thus, for example, in the stone impact test carried out in accordance with DIN 65996-1B, it was possible to demonstrate that, with steel sheets according to the invention, stone impact did not cause any flaking of the coating from the base coat.
To manufacture sheets according to the invention, a fine steel strip is subjected to a continuous hot-dip galvanizing process in a galvanizing plant operating at a strip speed of a typical 60 to 150 m/min. To do this, the sheet or strip to be galvanized is firstly annealed in a furnace, such as a DFF furnace (Direct Fired Furnace) or, preferably, an RTF furnace (Radiant Type Furnace).
Following on from the furnace, the sheet or strip runs through the reduction furnace section, in which it is held under a protective gas atmosphere with 3.5 - 75 %
hydrogen. The temperatures attained in the course of the annealing lie in the range from 720 - 850 C.
The sheet or strip annealed in this way is then conducted via what is referred to as a nozzle, with the exclusion of air, into the zinc bath, which is formed from a melt containing 0.05 - 0.30 % by weight Al and 0.2 - 2.0 % by weight Mg, in particular 0.4 - 1.0 % by weight and 0.5 -1.0 % by weight respectively, the remainder being zinc and unavoidable impurities.
After the sheet or strip emerges from the melt bath, the thickness of the coating is restricted in an inherently known manner by means of stripper nozzles to a value of a maximum of 3.5 pm on each side, with the result that, with the flat product obtained according to the invention, the coating weight is restricted to a maximum of 25 g/m2 per side.
In order to prevent an over-proportionate formation of slags and inter-metallic phases on the melt bath, it may be expedient to conduct an inert gas flow over the surface of the bath. This inert gas flow can be derived from the stripper nozzles which are used to adjust the thickness of the coating or can be supplied from separate nozzles, which distribute the inert gas in mist fashion over the surface of the bath. As an alternative, the entire melt bath can be surrounded by a housing enclosure, in which an inert atmosphere is maintained.
Especially suitable as the inert gas for this purpose is nitrogen.
The slag formation can also be reduced by adjusting the bath temperature to a range of 380 - 450 C. For the same purpose, the temperature of the strip can be restricted on immersion to 360 - 500 C in order in particular to minimise the inclination to oxidise in the immersion area.
After emerging from the melt bath the coated strip is cooled at a cooling speed of at least 10 K/s.
By means of subsequent in-line rolling at rolling degrees of 0.3 - 1.5%, if required, the desired texturing of the surface can then be carried out.
Inasmuch as the coated is likewise subjected in-line to subsequent heating in the temperature range of 300 -600 C, either a redistribution takes place inside the ZnMg coating or through-alloying is achieved into a ZnFeMag coating. The melts used to produce such a coating preferably have an Al content of less than 0.15 % by weight, and in particular 0.12 - 0.14 % by weight.
To extend the range of application, it is also possible then to apply in an inherently known manner a thin-film layer on the coating.
The effects achieved by the invention have been confirmed on the basis of an experiment, in which a steel strip, 0.82 mm thick, hard-rolled from conventional IF steel, was initially subjected to an alkaline spray cleaning, a brush cleaning, and an electrolytic cleaning.
This was then followed by annealing, during which the cleaned steel strip was annealed under protective gas (5 % H2, remainder N2) to a temperature of 800 C. The annealing time was 60 s.
The steel strip annealed in this way is then cooled, such that it is immersed at a melt bath immersion temperature of 465 C into the melt bath, contained in a housing enclosure under a protective gas atmosphere containing a maximum of 10 ppm oxygen. The melt bath consisted of a Zn melt, which as well as unavoidable impurities (e.g. Fe contents, which are drawn into the melt bath by the strip), contained 0.2 % by weight Al, and 0.8 % by weight Mg. Immersion time was two seconds.
After being conducted out of the melt bath, the coating thickness on the steel strip applied on both sides was adjusted, while still inside the melt bath housing enclosure, by means of stripper nozzles, likewise arranged in the housing enclosure, to a coating thickness of 3 pm on each side (corresponding to a coating weight of 21 g/m2 per side). The stripping was likewise carried out by means of nitrogen gas.
To conclude, the steel strip was dressed. The melt bath-coated steel strip obtained had Ra values of 1.8 pm, with Pc values of 46 cm-1 determined in accordance with the StahlEisen Test Datasheet SEP 1940.
The ball impact hardness test in accordance with the StahlEisen Test Datasheet SEP 1931 was carried out on specimens taken from the finished coated steel strip in order to determine the adherence of the coating and its formability. The result could be classified as Stage 1, which corresponds to good adherence and likewise good ability to forming.
In a deep drawing test, in which a hat-shaped component was drawn in a suitable mould out of a round steel sheet blank, a very low friction value was achieved, of a maximum of 0.45 g/m2.
The evaluation of weldability produced, for a laser-beam welded seam, a very good result in each case. Thus, for example, with laser beam welding with a joint gap "0"
with welding speeds of up to 5 m/min, error-free results are achieved.
The salt spray test in accordance with DIN 50021 SS
carried out on an unpainted bright specimen, coated in the manner explained above, did not have first red rust formation until after a spray duration of 312 hours. With a conventional Zn coating on a sheet with a coating weight of 25 g/m2 per side, red rust formation already appeared after 24 hours.
The paint adherence on samples coated according to the invention, in the conical mandrel bending test based on DIN EN ISO 6860, was good both at room temperature as well as at -20 C. The stone impact test according to DIN
55996-1B likewise did not result in any flaking of the coating from the steel base layer.
Z 2371. This long period before the occurrence of rust was achieved thanks to the combined corrosion protection of the zinc coating and painting.
Despite the reduction in the coating weight achieved in accordance with EP 0 038 904 Bl and the simultaneous good corrosion resistance, the hot-dip galvanized steel sheets produced in this way still do not fulfil the requirements imposed in the motor vehicle construction sector with regard to weldability.
The object of the invention was therefore to create a flat steel product which possesses an optimum combination of high corrosion resistance and optimum weldability and which is particularly well-suited for use as a material for motor vehicle chassis construction or for the production of domestic appliances.
This object is resolved according to the invention by a coated steel sheet or strip, which has a ground coating made of steel, onto at least one upper side of which a coating is applied by hot-dip galvanizing, the coating being formed from a melt consisting of 0.05 - 0.30 % by weight Al and 0.2 - 2.0 % by weight Mg, the remainder being zinc and unavoidable impurities, and on each side, with a coating thickness of a maximum of 3.5 pm and a coating weight of a maximum of 25 g/m2, guarantees that the steel sheet, in the salt spray mist test carried out in accordance with DIN 50021-SS, shows the first formation of red rust at the earliest after 250 hours.
A hot-dip galvanized flat steel product according to the invention possesses surprisingly good corrosion resistance with a coating weight minimised in relation to the prior art coating weight of a maximum of 25 g/m2 on each side. The low coating weight and the low thickness of the coating associated with this, of a maximum of 3.5 pm on each side, in combination with the high corrosion resistance, makes sheet or strip according to the invention particularly well-suited for the production of components which are manufactured by the welding of individual sheet elements. Accordingly, with steel sheets produced in accordance with the invention, elements for motor vehicle chassis or domestic appliance technology can be manufactured in particular, in that the individual sheet components formed from sheet or strip according to the invention can be welded to one another by laser beam welding at high welding speeds economically and with optimum results.
The corrosion resistance according to the invention is determined on the basis of a salt spray mist test in accordance with DIN 50021-SS in a corrosion short-term test process on bright unpainted steel sheet, in which a neutral 5% NaCl solution, as the corrosive agent, is sprayed continuously at a temperature of 35 2 C in a chamber. The steel sheet samples are in this situation placed in the chamber at an angle of inclination to the horizontal of 65 to 75 . In the practical test carried out in this manner, it has been demonstrated that sheets and strips coated in accordance with the invention regularly do not show any red rust formation until after a test duration of 300 hours.
The magnesium content in the melt intended for the coating remains essentially unchanged in the coating. The Al content of the coating, in the finished steel strip according to the invention, by contrast, is as a rule 1.8 to 3.2 and in particular 2 to 3 times higher than in the melt. An optimum corrosion protection is attained when the coating has an Mg content of 0.4 - 1.0 % by weight, in particular at least 0.5 % by weight.
If it is intended that the coating of the steel base material is to be carried out in the galvanealed process, the melt contains preferably less than 0.15 % by weight of aluminium. Al contents of the melt which are suitable for standard practice are in this case in the range of 0.12 - 0.14 % by weight.
If, by contrast, a conventionally hot-dip galvanized steel sheet according to the invention is provided, the Al content of the melt is preferably at least 0.15 % by weight.
A further surprising property which makes a flat product according to the invention particularly suitable for use in chassis construction becomes apparent when such a sheet or strip is painted. Accordingly, a mandrel bend test carried out on the basis of DIN EN ISO 6860 for sheets or strips according to the invention at room temperature and at -20 C produces good paint adherence -capacity. In particular, at a temperature of -20 C there is no indication of paint flaking or of flaking of the coating from the base material.
For the test carried out to determine the paint adherence capacity, a full paint structure was applied onto a steel sheet specimen after alkaline cleaning and phosphating, this structure comprising a 20 pm thick cathodic dip paint coating, a 32 pm thick filler paint coating applied onto this and a 40 pm thick base coating. The bending carried out over the conical mandrel did not lead to any detachment of the paint coating at room temperature or at -20 C.
In addition to a high corrosion resistance and a good paint adherence capacity, sheets or strips according to the invention have outstandingly good resistance to stone impact. Thus, for example, in the stone impact test carried out in accordance with DIN 65996-1B, it was possible to demonstrate that, with steel sheets according to the invention, stone impact did not cause any flaking of the coating from the base coat.
To manufacture sheets according to the invention, a fine steel strip is subjected to a continuous hot-dip galvanizing process in a galvanizing plant operating at a strip speed of a typical 60 to 150 m/min. To do this, the sheet or strip to be galvanized is firstly annealed in a furnace, such as a DFF furnace (Direct Fired Furnace) or, preferably, an RTF furnace (Radiant Type Furnace).
Following on from the furnace, the sheet or strip runs through the reduction furnace section, in which it is held under a protective gas atmosphere with 3.5 - 75 %
hydrogen. The temperatures attained in the course of the annealing lie in the range from 720 - 850 C.
The sheet or strip annealed in this way is then conducted via what is referred to as a nozzle, with the exclusion of air, into the zinc bath, which is formed from a melt containing 0.05 - 0.30 % by weight Al and 0.2 - 2.0 % by weight Mg, in particular 0.4 - 1.0 % by weight and 0.5 -1.0 % by weight respectively, the remainder being zinc and unavoidable impurities.
After the sheet or strip emerges from the melt bath, the thickness of the coating is restricted in an inherently known manner by means of stripper nozzles to a value of a maximum of 3.5 pm on each side, with the result that, with the flat product obtained according to the invention, the coating weight is restricted to a maximum of 25 g/m2 per side.
In order to prevent an over-proportionate formation of slags and inter-metallic phases on the melt bath, it may be expedient to conduct an inert gas flow over the surface of the bath. This inert gas flow can be derived from the stripper nozzles which are used to adjust the thickness of the coating or can be supplied from separate nozzles, which distribute the inert gas in mist fashion over the surface of the bath. As an alternative, the entire melt bath can be surrounded by a housing enclosure, in which an inert atmosphere is maintained.
Especially suitable as the inert gas for this purpose is nitrogen.
The slag formation can also be reduced by adjusting the bath temperature to a range of 380 - 450 C. For the same purpose, the temperature of the strip can be restricted on immersion to 360 - 500 C in order in particular to minimise the inclination to oxidise in the immersion area.
After emerging from the melt bath the coated strip is cooled at a cooling speed of at least 10 K/s.
By means of subsequent in-line rolling at rolling degrees of 0.3 - 1.5%, if required, the desired texturing of the surface can then be carried out.
Inasmuch as the coated is likewise subjected in-line to subsequent heating in the temperature range of 300 -600 C, either a redistribution takes place inside the ZnMg coating or through-alloying is achieved into a ZnFeMag coating. The melts used to produce such a coating preferably have an Al content of less than 0.15 % by weight, and in particular 0.12 - 0.14 % by weight.
To extend the range of application, it is also possible then to apply in an inherently known manner a thin-film layer on the coating.
The effects achieved by the invention have been confirmed on the basis of an experiment, in which a steel strip, 0.82 mm thick, hard-rolled from conventional IF steel, was initially subjected to an alkaline spray cleaning, a brush cleaning, and an electrolytic cleaning.
This was then followed by annealing, during which the cleaned steel strip was annealed under protective gas (5 % H2, remainder N2) to a temperature of 800 C. The annealing time was 60 s.
The steel strip annealed in this way is then cooled, such that it is immersed at a melt bath immersion temperature of 465 C into the melt bath, contained in a housing enclosure under a protective gas atmosphere containing a maximum of 10 ppm oxygen. The melt bath consisted of a Zn melt, which as well as unavoidable impurities (e.g. Fe contents, which are drawn into the melt bath by the strip), contained 0.2 % by weight Al, and 0.8 % by weight Mg. Immersion time was two seconds.
After being conducted out of the melt bath, the coating thickness on the steel strip applied on both sides was adjusted, while still inside the melt bath housing enclosure, by means of stripper nozzles, likewise arranged in the housing enclosure, to a coating thickness of 3 pm on each side (corresponding to a coating weight of 21 g/m2 per side). The stripping was likewise carried out by means of nitrogen gas.
To conclude, the steel strip was dressed. The melt bath-coated steel strip obtained had Ra values of 1.8 pm, with Pc values of 46 cm-1 determined in accordance with the StahlEisen Test Datasheet SEP 1940.
The ball impact hardness test in accordance with the StahlEisen Test Datasheet SEP 1931 was carried out on specimens taken from the finished coated steel strip in order to determine the adherence of the coating and its formability. The result could be classified as Stage 1, which corresponds to good adherence and likewise good ability to forming.
In a deep drawing test, in which a hat-shaped component was drawn in a suitable mould out of a round steel sheet blank, a very low friction value was achieved, of a maximum of 0.45 g/m2.
The evaluation of weldability produced, for a laser-beam welded seam, a very good result in each case. Thus, for example, with laser beam welding with a joint gap "0"
with welding speeds of up to 5 m/min, error-free results are achieved.
The salt spray test in accordance with DIN 50021 SS
carried out on an unpainted bright specimen, coated in the manner explained above, did not have first red rust formation until after a spray duration of 312 hours. With a conventional Zn coating on a sheet with a coating weight of 25 g/m2 per side, red rust formation already appeared after 24 hours.
The paint adherence on samples coated according to the invention, in the conical mandrel bending test based on DIN EN ISO 6860, was good both at room temperature as well as at -20 C. The stone impact test according to DIN
55996-1B likewise did not result in any flaking of the coating from the steel base layer.
Claims (5)
1. Method for the manufacture of a steel sheet or strip coated on at least one of its sides with a coating consisting of 0.05 - 0.30 % by weight Al and 0.2 - 2.0% by weight Mg, the remainder being zinc and unavoidable impurities, which in the state provided with the coating, in a salt spray mist test carried out in accordance with DIN 50021-SS, shows the first red rust formation at the earliest after 250 hours, in which, in a continuous sequence:
an uncoated steel strip is annealed, following the annealing the steel strip is guided through a reduction furnace section, in which it is held under a protective gas atmosphere with 3.5 - 75 % hydrogen, the temperatures attained in the course of the annealing lying in the range from 720 - 850°C, the annealed steel strip is conducted through a galvanizing bath consisting of 0.05 - 0.30 % by weight Al and 0.2 - 2.0% by weight Mg, the remainder being zinc and unavoidable impurities, the speed of the strip being 60 to 150 m/min and the layer thickness on the steel strip emerging from the melt bath is adjusted by means of a stripper nozzle, characterised in that the surface of the melt bath is kept under an inert gas flow in relation to the surrounding atmosphere, in order to avoid the formation of slag or the occurrence of inter-metallic phases, the inert gas flow being derived from the stripper nozzles, which are used to adjust the thickness of the coating, or being supplied from separate nozzles, which distribute the inert gas in mist fashion over surface of the bath, and the layer thickness of the coating is adjusted by means of the stripper nozzle to a maximum of 3.5 µm on each side and a coating weight of a maximum of 25 g/m2 on each side.
an uncoated steel strip is annealed, following the annealing the steel strip is guided through a reduction furnace section, in which it is held under a protective gas atmosphere with 3.5 - 75 % hydrogen, the temperatures attained in the course of the annealing lying in the range from 720 - 850°C, the annealed steel strip is conducted through a galvanizing bath consisting of 0.05 - 0.30 % by weight Al and 0.2 - 2.0% by weight Mg, the remainder being zinc and unavoidable impurities, the speed of the strip being 60 to 150 m/min and the layer thickness on the steel strip emerging from the melt bath is adjusted by means of a stripper nozzle, characterised in that the surface of the melt bath is kept under an inert gas flow in relation to the surrounding atmosphere, in order to avoid the formation of slag or the occurrence of inter-metallic phases, the inert gas flow being derived from the stripper nozzles, which are used to adjust the thickness of the coating, or being supplied from separate nozzles, which distribute the inert gas in mist fashion over surface of the bath, and the layer thickness of the coating is adjusted by means of the stripper nozzle to a maximum of 3.5 µm on each side and a coating weight of a maximum of 25 g/m2 on each side.
2. Method according to claim 1, characterised in that the coating contains 0.4 - 1.0 % by weight Mg.
3. Method according to claim 2, characterised in that the coating contains more than 0.5 % by weight Mg.
4. Method according to any one of claims 1 to 3, characterised in that the Al content of the melt amounts to 0.12 - 0.14 % by weight.
5. Method according to any one of claims 1 to 3, characterised in that the Al content of the melt amounts to at least 0.15 % by weight.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP05003762.1 | 2005-02-22 | ||
| EP05003762A EP1693477A1 (en) | 2005-02-22 | 2005-02-22 | Coated steel plate |
| PCT/EP2006/050955 WO2006089854A1 (en) | 2005-02-22 | 2006-02-15 | Coated steel sheet or coil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2596825A1 CA2596825A1 (en) | 2006-08-31 |
| CA2596825C true CA2596825C (en) | 2013-03-19 |
Family
ID=34933875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA2596825A Expired - Fee Related CA2596825C (en) | 2005-02-22 | 2006-02-15 | Coated steel sheet or strip |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US20080142125A1 (en) |
| EP (2) | EP1693477A1 (en) |
| JP (1) | JP5270172B2 (en) |
| KR (1) | KR101268570B1 (en) |
| CN (1) | CN101128614B (en) |
| AU (1) | AU2006218005B2 (en) |
| CA (1) | CA2596825C (en) |
| ES (1) | ES2650741T3 (en) |
| WO (1) | WO2006089854A1 (en) |
Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PL1857566T3 (en) * | 2006-05-15 | 2017-10-31 | Thyssenkrupp Steel Europe Ag | Flat steel product provided with a corrosion protection coating and method of its manufacture |
| EP1857567B1 (en) * | 2006-05-15 | 2017-04-05 | ThyssenKrupp Steel Europe AG | Method of manufacturing a flat steel product coated with a corrosion protection system |
| DE102007048504B4 (en) * | 2007-10-10 | 2013-11-07 | Voestalpine Stahl Gmbh | Anti-corrosion coating for steel sheets and method of conditioning a corrosion protection coating |
| EP2055799A1 (en) * | 2007-11-05 | 2009-05-06 | ThyssenKrupp Steel AG | Flat steel product with an anti-corrosion metal coating and method for creating an anti-corrosion metal coating on a flat steel product |
| EP2141255B1 (en) * | 2008-07-04 | 2020-03-18 | Volvo Car Corporation | Improved corrosion inhibiting structure |
| WO2010130883A1 (en) | 2009-05-14 | 2010-11-18 | Arcelormittal Investigacion Y Desarrollo Sl | Method for producing a coated metal band having an improved appearance |
| DE102010037254B4 (en) | 2010-08-31 | 2012-05-24 | Thyssenkrupp Steel Europe Ag | Process for hot dip coating a flat steel product |
| DE102011051731B4 (en) | 2011-07-11 | 2013-01-24 | Thyssenkrupp Steel Europe Ag | Process for the preparation of a flat steel product provided by hot dip coating with a metallic protective layer |
| DE102012101018B3 (en) | 2012-02-08 | 2013-03-14 | Thyssenkrupp Nirosta Gmbh | Process for hot dip coating a flat steel product |
| US9863029B2 (en) * | 2012-08-01 | 2018-01-09 | Dongkuk Steel Mill Co., Ltd. | Apparatus for forming nitrogen cloud to produce hot dip coated steel sheet |
| AU2013209303B2 (en) * | 2012-08-01 | 2015-05-07 | Dongkuk Coated Metal Co., Ltd. | Method and apparatus for producing zinc-aluminum alloy-coated steel sheet with superior workability and corrosion resistance |
| JP6199403B2 (en) | 2012-10-24 | 2017-09-20 | マグナ インターナショナル インコーポレイテッド | Laser metal weld clad of weld seam for automotive parts |
| KR101439694B1 (en) | 2012-12-26 | 2014-09-12 | 주식회사 포스코 | Zn-Mg ALLOY COATED STEEL SHEET AND MEHTDOD FOR MANUFACTURING THE SAME |
| ES2851199T3 (en) | 2013-07-03 | 2021-09-03 | Outokumpu Nirosta Gmbh | Procedure for coating flat steel products with a metallic protective layer |
| GB2521363A (en) * | 2013-12-17 | 2015-06-24 | Eaton Ind Netherlands Bv | Method for producing a housing for medium voltage switchgear and such a housing |
| JP7051436B2 (en) | 2014-12-24 | 2022-04-11 | ポスコ | Zinc alloy plated steel with excellent weldability and corrosion resistance of processed parts and its manufacturing method |
| WO2017020965A1 (en) * | 2015-08-06 | 2017-02-09 | Thyssenkrupp Steel Europe Ag | Method for producing a zinc-magnesium-galvannealed hot-dip coating and flat steel product provided with such a coating |
| CN108018513A (en) * | 2016-10-28 | 2018-05-11 | 宝山钢铁股份有限公司 | A kind of dip galvanized aluminum magnesium clad steel sheet and its manufacture method |
| KR102031466B1 (en) | 2017-12-26 | 2019-10-11 | 주식회사 포스코 | Zinc alloy coated steel having excellent surface property and corrosion resistance, and method for manufacturing the same |
| DE102018212540A1 (en) | 2018-07-27 | 2020-01-30 | Bayerische Motoren Werke Aktiengesellschaft | Method for coating a motor vehicle raw component and motor vehicle raw component |
| DE102019215050B4 (en) * | 2019-09-30 | 2023-09-07 | Thyssenkrupp Steel Europe Ag | Process for producing a laser soldered connection between coated sheet steel components |
| DE102019217912A1 (en) * | 2019-11-20 | 2021-05-20 | Volkswagen Aktiengesellschaft | Process for laser beam soldering |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1446872A (en) | 1964-09-15 | 1966-07-22 | Inland Steel Co | Protective coating made of zinc-based alloys |
| IT1036986B (en) * | 1975-06-13 | 1979-10-30 | Centro Speriment Metallurg | STEEL ALLOY AND COATED ALLOY PRODUCTS |
| AU525668B2 (en) * | 1980-04-25 | 1982-11-18 | Nippon Steel Corporation | Hot dip galvanizing steel strip with zinc based alloys |
| JPS5891162A (en) * | 1981-11-18 | 1983-05-31 | Nisshin Steel Co Ltd | Manufacture of galvanized steel plate |
| JPS6362835A (en) * | 1986-09-02 | 1988-03-19 | Nikko Aen Kk | Zinc alloy for hot dip galvanizing and method for using same |
| KR960004773B1 (en) * | 1991-12-06 | 1996-04-13 | 가와사키 세이데츠 가부시키가이샤 | Method of manufacturing molten zinc plated steel plates |
| JP3357471B2 (en) * | 1994-08-22 | 2002-12-16 | 川崎製鉄株式会社 | Zn-Mg-Al-based hot-dip galvanized steel excellent in corrosion resistance and method for producing the same |
| JP3113189B2 (en) * | 1995-11-15 | 2000-11-27 | 新日本製鐵株式会社 | Hot-dip Zn-Mg-Al-Co plated steel sheet with excellent blackening resistance |
| JP3201469B2 (en) * | 1997-11-04 | 2001-08-20 | 日新製鋼株式会社 | Mg-containing hot-dip Zn-base plated steel sheet |
| JPH11140665A (en) * | 1997-11-11 | 1999-05-25 | Nippon Steel Corp | Coated steel sheet excellent in edge face corrosion resistance and its production |
| JPH11140614A (en) * | 1997-11-13 | 1999-05-25 | Nippon Steel Corp | Weldable coated steel sheet excellent in corrosion resistance |
| JP2000160315A (en) * | 1998-11-27 | 2000-06-13 | Nippon Steel Corp | Hot dip galvannealed steel |
| JP2002322527A (en) * | 2001-04-25 | 2002-11-08 | Nippon Steel Corp | Al-Zn-Mg BASED ALLOY PLATED STEEL PRODUCT |
| JP2004244650A (en) * | 2003-02-10 | 2004-09-02 | Nippon Steel Corp | METHOD OF PRODUCING Zn-Al-Mg BASED ALLOY PLATED STEEL |
-
2005
- 2005-02-22 EP EP05003762A patent/EP1693477A1/en not_active Withdrawn
-
2006
- 2006-02-15 WO PCT/EP2006/050955 patent/WO2006089854A1/en active Application Filing
- 2006-02-15 AU AU2006218005A patent/AU2006218005B2/en not_active Ceased
- 2006-02-15 US US11/816,799 patent/US20080142125A1/en not_active Abandoned
- 2006-02-15 CA CA2596825A patent/CA2596825C/en not_active Expired - Fee Related
- 2006-02-15 ES ES06724846.8T patent/ES2650741T3/en active Active
- 2006-02-15 KR KR1020077021513A patent/KR101268570B1/en active IP Right Grant
- 2006-02-15 CN CN2006800056157A patent/CN101128614B/en active Active
- 2006-02-15 EP EP06724846.8A patent/EP1851352B8/en active Active
- 2006-02-15 JP JP2007556589A patent/JP5270172B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP5270172B2 (en) | 2013-08-21 |
| KR20070105371A (en) | 2007-10-30 |
| EP1851352B1 (en) | 2017-09-06 |
| EP1851352B8 (en) | 2017-10-18 |
| AU2006218005A1 (en) | 2006-08-31 |
| EP1851352A1 (en) | 2007-11-07 |
| US20080142125A1 (en) | 2008-06-19 |
| CN101128614A (en) | 2008-02-20 |
| WO2006089854A1 (en) | 2006-08-31 |
| AU2006218005B2 (en) | 2011-11-17 |
| JP2008531844A (en) | 2008-08-14 |
| ES2650741T3 (en) | 2018-01-22 |
| EP1693477A1 (en) | 2006-08-23 |
| CN101128614B (en) | 2012-07-18 |
| CA2596825A1 (en) | 2006-08-31 |
| KR101268570B1 (en) | 2013-05-28 |
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