US3843417A - Method for hot dipping aluminium-killed steel sheet - Google Patents

Method for hot dipping aluminium-killed steel sheet Download PDF

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US3843417A
US3843417A US00309890A US30989072A US3843417A US 3843417 A US3843417 A US 3843417A US 00309890 A US00309890 A US 00309890A US 30989072 A US30989072 A US 30989072A US 3843417 A US3843417 A US 3843417A
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hot
steel sheet
sheet
dipping
steel
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M Ohbu
K Asakawa
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Nippon Steel Corp
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Nippon Steel Corp
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • C23C2/10—Lead or alloys based thereon
    • 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
    • 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
    • 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
    • C23C2/024—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by cleaning or etching
    • 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

Definitions

  • ABSTRACT OF THE DISCLOSURE A method for hot dipping an aluminium-killed steel sheet in a hot dipping line involving a reduction annealing process as a pretreatment step wherein an aluminiumkilled steel sheet containing less than 0.05% of soluble aluminium and more than 0.02% of carbon is wound up at a temperature higher than 650 C. after hot rolling to obtain a steel sheet composed of crystals having a grain size number less than 9.5 and an axial ratio smaller than 1.5, descaled by acid pickling, cold rolled, and then degreased in hot dipping equipment, subjected to reduction annealing, cooled to a suitable dipping temperature and is then immersed in a hot dipping bath.
  • the present invention relates to an improvement in the plateability of aluminium-killed steel sheet by hot dipping.
  • a detailed investigation was made particularly directed to an improvement in hot zinc dipping, and the result was applied for other hot dippings. Accordingly, problems and the improvement with the hot dipping of aluminium-killed steel with zinc will be explained first.
  • the object of the present invention is limited only for steel sheets refined by deoxidation with aluminium before casting in a mold. This does not include steel sheets obtained by producing a rimmed layer after casting in a mold and refining the core part with aluminium, because they already possess excellent plateability.
  • the nitrogen content steels for which the present invention is suitable is more than 0.003%.
  • the method for hot dipping of steel sheet with zinc commonly used in recent years is: a steel sheet is subjected to a so-called pretreatment process, such as, the Sendzimir process or a non-oxidizing furnace process, an oxidation or non-oxidation e.g., degreasing, surface cleansing and a reduction annealing, and then after cooling, to a suitable zinc dipping temperature, is immersed in a zinc dipping bath.
  • a so-called pretreatment process such as, the Sendzimir process or a non-oxidizing furnace process
  • an oxidation or non-oxidation e.g., degreasing, surface cleansing and a reduction annealing
  • an aluminium-killed steel used as a base metal for hot dipping does not possess the excellent deep-drawing and non-ageing properties which it would possess with cold rolling. Therefore, a rimmed or capped steel, which is cheap and possesses excellent plateability, is used.
  • the present inventors found that the plateability of aluminium-killed steel is very inferior in hot dipping, and then studied in detail the behavior of aluminium in steel in hot zinc dipping as well as the effect of the conditions in various processes, after hot rolling, on the adhesiveness of plating. As a result, it was ascertained that, by controlling the conditions in the amount of aluminium in steel as well as in each of the processes after proper hot rolling, the zinc plateability of aluminium-killed steel sheet can be remarkably improved.
  • the surface condition of steel sheet is influenced by the oxidation-reduction condition in the pretreatment process of the zinc dipping and also by the steel components in the base metal used for hot dipping and by the winding temperature in the hot rolling.
  • the plateability in hot dipping of aluminium-killed steel is improved remarkably by controlling the winding temperature in the hot rolling adequately. It was ascertained that the degree of crystallization, the condition of the precipitate of AlN, Fe C and others and the amount of AlN precipitated are altered according to the winding temperature in the hot rolling. This results in differences in the surface condition of the steel sheet, and consequently, the winding temperature in the hot rolling has a great influence on the reaction between iron and zinc as well as the adhesiveness of the plating to the base metal.
  • FIG. 1 is a graph showing the relation between the amount of soluble aluminium (hereinafter referred to as Sol.Al) in the steel sheet, wound up at 550 C., and the adhesiveness thereto as well as the thickness of the alloy layer in hot zinc dipping.
  • FIG. 2 is a graph showing the grain size in the steel as a base metal for hot zinc dipping and the adhesiveness of the plating.
  • FIG. 3 is a graph showing the relation between the winding temperature of the base metal for hot dipping after hot rolling and the plating adhesiveness after hot zinc dipping.
  • FIG. 4 is a graph showing the relation between the amount of Sol.Al in the steel sheet, wound up at 650 C., and the adhesiveness of the plating.
  • FIG. 1 is a graph showing the relation between the amount of soluble aluminium (hereinafter referred to as Sol.Al) in the steel sheet, wound up at 550 C., and the adhesiveness thereto as well as the thickness of the alloy layer in hot zinc dipping.
  • FIG. 2
  • FIG. 5 is a graph showing the effects of SoLAl in the steel sheet as well as the winding temperature in the hot rolling on the occurrence of pinholes in the hot dipping with terne metal.
  • FIG. 6 is a graph showing the effects of Sol.Al in the steel sheet as well as the winding temperature in the hot rolling on the occurrence of pinholes in the hot dipping with tin.
  • FIG. 7 is a graph showing the effects of Sol.Al in the steel sheet as well as the winding temperature in the hot rolling on the occurrence of pinholes in the hot dipping with tin.
  • FIG. 10 shows the relation between the winding temperature in the hot rolling and the grain size in the continuous and batch annealings.
  • FIG. 8 shows the relation between the winding temperature in the hot rolling and the crystal structure.
  • FIG. 9 is a graph showing the relation between the amount of carbon in the steel and the adhesiveness under varying winding temperature.
  • FIG. 10, a and b are the photographs showing the change of alloy layer in hot zinc dipping according to the amount of Sol.Al in the steel sheet.
  • FIG. 11, a and b are the photographs showing the change of alloy layer in the vincinity of base metal in hot zinc dipping according to the amount of Sol.Al in the steel sheet.
  • FIG. 12, a, b and c are the photographs showing the elfects of the amount of Sol.Al in the steel sheet and the Winding temperature on the condition of alloy layer in the hot dipping with terne metal.
  • FIG. 1 is the experimental result on the effect of Sol.Al in an aluminium-killed steel on the average thickness of the alloy layer and the adhesiveness of the plating to the base metal in hot zinc dipping.
  • the result shows that, while the thickness of alloy layer is nearly constant when the amount of Sol.Al in the steel is less than 0.02%, the average alloy layer becomes thinner in increasing Sol.Al above 0.02%, and there is the tendency that the thickness reaches a nearly constant value when Sol.Al is 0.07- 0.08%.
  • Such a tendency means that the reactivity between iron and zinc decreases in accordance with the content of Sol.Al in the steel in the range where Sol.Al is larger than 0.02%. It is thought that aluminium dissolved as a solid solution in the steel reacts with the atmospheric gases in the oxidation-reduction process used as a pretreatment of plating, forming aluminium oxide, aluminium nitride and others on the surface of the base metal, which hinder the wettability of the base metal to fused zinc as well as the re action between iron and zinc, preventing the formation of the alloy layer.
  • the plating adhesiveness is excellent in the range where Sol.Al in the steel is less than 0.02%, and deteriorates rapidly with increasing the amount of Sol.Al.
  • the relation is quite reversed against the average thickness of the alloy layer.
  • FIG. 10 shows the condition of the alloy layers formed when steel sheets containing trace and 0.080% of Sol.Al are hot dipped with zinc (in the photograph, the alloy layer is thicker in accordance with the blackness). While the alloy layer is formed uniformly all over the total surface when Sol.Al is trace, the formation of alloy layer is very scattered, having some portions with almost no formation of alloy layer (white in the photograph), when the Sol.Al is 0.080%.
  • the base metal is not plated uniformly thin all over the total surface, but has locally unplated parts, and as a result, it is seen that the average thickness of the layer is thin.
  • the adhesiveness of the plating can be improved still more when the formation of the alloy layer is accelerated by decomposing the thin film of aluminium oxide, aluminium nitride and others, which is considered to be formed on the surface of steel sheet in the pretreatment process of hot zinc dipping.
  • various treatments such as insufficient cooling of the base metal after reduction annealing and immersion in a hot dipipng bath at a temperature higher than the bath temperature, or reducing the amount of aluminium in the hot dipping bath to control the restricting effect of the alloy layer, may be considered.
  • the alloy layer consisting of fine grains is formed all over the surface when the amount of Sol.Al in the steel is a trace, the alloy layer is of large plate-like crystals when Sol.Al in the steel is 0.080%. The reason may be considered as due to the shortage of active points to initiate the reaction in the formation of the alloy layer.
  • the adhesiveness of the plating becomes inferior.
  • increasing the active points of the reaction is effective.
  • to elevate the temperature of the steel sheet above 850 C. in the reduction annealing was found to have a tolerable effect, but was insufficient to give a satisfactory adhesiveness suitable to withstand subsequent working.
  • the alloy layer When the alloy layer is developed to a thickness about 23 the unreacted part in Fe-Zn reaction and the shape effect in the alloy layer are removed, and the plating adhesiveness becomes good. However, when the alloy layer is developed to above 3n, the plating adhesiveness becomes inferior owing to the brittleness of the alloy layer itself. Moreover, to control the alloy layer at 2-3 in the industrial production of galvanized steel sheet is difi'rcult.
  • the present inventors found that the grain size in the base metal for plating is, as shown in FIG. 2, one of the most important factors on the plating adhesiveness, having the tendency of deteriorating the plating adhesiveness with increasing the grain size number.
  • the increase in grain size i.e., to reduce the grain size number
  • the mechanism is not yet known in detail
  • the alloy layer formed at the brain boundary is poor in adhesiveness and the peeling of plating starts from the rupture in the neighbourhood of grain boundary.
  • the grain boundary being the starting point of rupture, is diminished as the grain size becomes larger and consequently the plating adhesiveness is improved.
  • the conditions under which growing the grain size is also to be considered.
  • the difference in the winding temperature after hot rolling relates to the difference in the state of the alloy elements in the steel, dissolved as a solid solution or precipitated, particularly in the vicinity of the surface layer.
  • the difference in the high temperature cycle and the holding period in the reduction annealing changes the behavior of the alloy elements in the steel in its precipitation, and thus the activity of steel surface in the Fe-Zn reaction may be improved.
  • the precipitation state or the grain size of alloy elements (particularly aluminium) in the steel can easily be controlled according to the conditions of the processes before the hot zinc dipping, particularly in the hot rolling process.
  • the precipitation of aluminium nitride is controlled by a low temperature winding (below 600 C.) after hot rolling, and the precipitation of aluminium nitride and the formation of pancake grains are accelerated by controlling properly the heating rate and the heating temperature in the annealing process after cold rolling (batch annealing), and thus an excellent workability is obtained.
  • the present inventors investigated, paying attention to the easiness of controlling the grain size by the winding temperature in the hot rolling, the relation between the winding temperature in the hot rolling and the plating adhesiveness.
  • the result is as shown in FIG. 3, From the result, it is obvious that the plating adhesiveness is improved by elevating the winding temperature in the hot rolling, and sufiiciently high adhesiveness suitable for the practical working can be obtained when the winding temperature is above 65 C.
  • FIG. 4 shows the relation between the amount of Sol.Al in the steel sheet and the plating adhesiveness when the winding temperature after hot rolling is 650 C.
  • the winding temperature is 550 C.
  • the plating adhesiveness is improved remarkably, and it is clear that sufficient plating adhesiveness is obtained by applying a high temperature winding when the amount of Sol.Al in the steel lies in the range of 0.010.05
  • FIG. 5 shows the effect of Sol.Al in the steel sheet as well as the winding temperature in the hot rolling thereof on the occurrence of pinholes in the hot dipping with socalled tenne alloy comprising 15% of tin and 85% of lead, in which an aluminium-killed steel sheet is batch annealed (at 700 C., with a heating rate of C./hr. and a holding period of 5 hrs.) and hot dipped by a usual flux method (dipping bath temperature 350 C., immersed for 20 seconds).
  • pinholes increase remarkably when 'Sol.Al in the steel exceeds 0.01% in winding at 550 C. after hot rolling, showing that the plateability with terne metal becomes inferior, pinholes diminish in winding at 650 C.
  • FIG. 6 shows the effect of Sol.Al in the steel sheet as well as the winding temperature in the hot rolling on the occurrence of pinholes in the hot dipping with tin.
  • pinholes increase remarkably when Sol.Al in the steel exceeds 0.02% in winding at 550 C. after hot rolling showing that the tin plateability is deteriorated, pinholes diminish in winding at 650 C., and the effect is particularly distinct in the range where SoLAl in the steel is less than 0.05%, showing a similar tendency as in the hot zinc and terne metal dipping.
  • the carbon content in the steel sheet of this invention is restricted to larger than 002%.
  • the crystal structure may possibly be a measure for improving the plateability of aluminiumkilled steel sheet.
  • the draft in the cold rolling is preferably larger than 50%. Below 50%, the workability is apt to be deteriorated owing to the formation of an abnormal structure, such as, mixed grains. From the standpoint of general industrial manufacture, the content of nitrogen in the steel is defined as larger than 0.003%.
  • a method for hot dipping an aluminium-killed steel sheet in a hot dipping line involving a reduction annealing pretreatment process which includes the steps of hot rolling said steel sheet, descaling the sheet by acid pickling, cold rolling the sheet, and then degreasing the sheet in hot dipping equipment, reduction annealing the sheet, cooling the sheet to a suitable dipping temperature and immersing the sheet in a hot dipping bath, the improvement which comprises winding said aluminiumkilled steel sheet at a temperature higher than 650 C. after the hot rolling.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating With Molten Metal (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
US00309890A 1971-12-01 1972-11-27 Method for hot dipping aluminium-killed steel sheet Expired - Lifetime US3843417A (en)

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JP9732171A JPS5426497B2 (enrdf_load_stackoverflow) 1971-12-01 1971-12-01

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4067754A (en) * 1975-02-28 1978-01-10 Armco Steel Corporation Cold rolled, ductile, high strength steel strip and sheet and method therefor
US4144379A (en) * 1977-09-02 1979-03-13 Inland Steel Company Drawing quality hot-dip coated steel strip
USRE31306E (en) * 1975-02-28 1983-07-12 Armco Inc. Cold rolled, ductile, high strength steel strip and sheet and method therefor
US5026612A (en) * 1983-05-07 1991-06-25 Alcan International Limited Structures fabricated from aluminum components and processes involved in making these structures
US5074924A (en) * 1989-06-21 1991-12-24 Nippon Steel Corporation Process for producing galvanized, non-aging cold rolled steel sheets having good formability in a continuous galvanizing line
US5127966A (en) * 1990-03-20 1992-07-07 Kawasaki Steel Corporation Method of producing hot-dip galvannealed steel sheet free of ti white-stripe defects
US5139888A (en) * 1983-05-07 1992-08-18 Alcan International Limited Structures fabricated from aluminium components and processes involved in making these structures

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4202921A (en) * 1976-02-24 1980-05-13 Aktiebolaget Garphytte Bruk Process for the preparation of rope and spring wire of carbon steel with an improved corrosion resistance

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4067754A (en) * 1975-02-28 1978-01-10 Armco Steel Corporation Cold rolled, ductile, high strength steel strip and sheet and method therefor
USRE31306E (en) * 1975-02-28 1983-07-12 Armco Inc. Cold rolled, ductile, high strength steel strip and sheet and method therefor
US4144379A (en) * 1977-09-02 1979-03-13 Inland Steel Company Drawing quality hot-dip coated steel strip
US5026612A (en) * 1983-05-07 1991-06-25 Alcan International Limited Structures fabricated from aluminum components and processes involved in making these structures
US5139888A (en) * 1983-05-07 1992-08-18 Alcan International Limited Structures fabricated from aluminium components and processes involved in making these structures
US5074924A (en) * 1989-06-21 1991-12-24 Nippon Steel Corporation Process for producing galvanized, non-aging cold rolled steel sheets having good formability in a continuous galvanizing line
US5127966A (en) * 1990-03-20 1992-07-07 Kawasaki Steel Corporation Method of producing hot-dip galvannealed steel sheet free of ti white-stripe defects

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JPS5426497B2 (enrdf_load_stackoverflow) 1979-09-04
JPS4860028A (enrdf_load_stackoverflow) 1973-08-23
DE2258589A1 (de) 1973-06-14
DE2258589B2 (de) 1978-12-14

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