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WO2024200152A1 - Produit plat en acier revêtu par immersion à chaud et phosphaté pour formage à chaud, composant formé à chaud et procédé de production - Google Patents

Produit plat en acier revêtu par immersion à chaud et phosphaté pour formage à chaud, composant formé à chaud et procédé de production Download PDF

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Publication number
WO2024200152A1
WO2024200152A1 PCT/EP2024/057403 EP2024057403W WO2024200152A1 WO 2024200152 A1 WO2024200152 A1 WO 2024200152A1 EP 2024057403 W EP2024057403 W EP 2024057403W WO 2024200152 A1 WO2024200152 A1 WO 2024200152A1
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Prior art keywords
hot
flat steel
steel product
optionally
temperature
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German (de)
English (en)
Inventor
Maria KÖYER
Fabian JUNGE
Robin Dohr
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ThyssenKrupp Steel Europe AG
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ThyssenKrupp Steel Europe AG
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Publication of WO2024200152A1 publication Critical patent/WO2024200152A1/fr
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
    • C22C38/38—Ferrous alloys, e.g. steel alloys containing chromium with more than 1.5% by weight of manganese
    • 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
    • C23C2/12—Aluminium 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
    • C23C2/26—After-treatment
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
    • C23C22/36—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates
    • C23C22/362—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides containing also phosphates containing also zinc cations
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • C23C22/74—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process for obtaining burned-in conversion coatings

Definitions

  • a “flat steel product” or a “sheet metal product” we mean both rolled products such as steel strips or sheets and “sheet metal blanks” (also called blanks) that are cut from the rolled products.
  • “Sheet metal blanks” also mean parts of a rolled product that have undergone further processing that does not involve hot forming, e.g. punching, etc.
  • “Sheet metal parts” or “sheet metal components” of the type according to the invention are made from such sheet metal blanks by means of hot forming, whereby the terms “sheet metal part” and “sheet metal component” are used synonymously here.
  • a straight line parallel to the surface is placed on the SEM image.
  • the ratio of the total length of the straight line within the phase to the total length of the straight line is determined.
  • the straight line parallel to the surface is placed in such a way that the maximum value of the ratio is obtained. This maximum value of the ratio is called the phase continuity.
  • the martensite start temperature and the AC1 and AC3 temperatures are defined below.
  • the martensite start temperature of a steel that is within the scope of the inventive specifications is according to the formula:
  • the reflectance R in the infrared range is determined in the sense of this application by using a black body radiator as a reference.
  • the spectral radiation power i (T) of the black body radiator at the temperature T is therefore multiplied by the measured spectral reflectivity p ⁇ and integrated over the wavelength range. This integral is standardized to the spectral radiation power integrated over the same wavelength range. The following therefore applies:
  • Hot forming also known as hot press hardening
  • steel blanks also known as sheet metal blanks
  • forming temperature that is generally above the austenitizing temperature of the steel in question and, in the heated state, are placed in the tool of a forming press.
  • the sheet metal blank or the component formed from it undergoes rapid cooling due to contact with the cool tool.
  • the cooling rates are set so that a hardened structure (ie martensitic structure) is produced in the component.
  • Phosphate compounds on anti-corrosive coatings containing aluminum/silicon are also known from WO 2012/120081 Al. It was found that the phosphate compounds can lead to an increased heating rate to preform temperature. However, the heating times for anti-corrosive coatings containing aluminum/silicon are only reduced by 30%.
  • hot-formed components for automotive construction are also phosphated. The phosphating step takes place after hot forming. However, with conventional anti-corrosive coatings made of aluminum and silicon, an aluminum oxide layer forms during hot forming. Due to the high temperatures during hot forming, a thick aluminum oxide layer is formed. During the subsequent phosphating step, the typical process parameters during phosphating are not sufficient to break up the oxide layer, meaning that the conversion process cannot be started. As a result, only a small proportion of the surface of the component can be phosphated. This has a negative impact on the optical appearance before and after corrosion, the roughness of the surface and the paintability.
  • the invention relates to a phosphated flat steel product comprising a steel substrate and a corrosion protection coating, wherein the steel substrate contains, in addition to iron and unavoidable impurities from
  • V ⁇ 0.1%
  • the corrosion protection coating is aluminum-based and has an alloy layer and an Al base layer, characterized in that the reflectance R in the infrared range is ⁇ 0.65, preferably ⁇ 0.55, in particular ⁇ 0.40, particularly preferably ⁇ 0.35.
  • the adjustment of the alloying elements ensures the processability, coatability and final properties.
  • the explanations of the steel substrate apply both to the phosphated flat steel product and to the corresponding manufacturing process as well as to the component and the manufacturing process of the component.
  • Carbon is contained in the steel according to the invention at a level of at least 0.04% and contributes to the hardenability of the steel by delaying the formation of ferrite and bainite as well as the formation of residual austenite in the structure.
  • a proportion of at least 0.07%, particularly preferably at least 0.10% has proven to be advantageous. Too high a carbon content can lead to the welding properties of the flat steel product deteriorating, so the carbon content is limited according to the invention to 0.45%, preferably to 0.4% and particularly preferably to 0.25%.
  • manganese (“Mn”) By adding manganese (“Mn”), the formation of ferrite and bainite in the flat steel product is delayed. In order to obtain the lowest possible proportion of ferrite and bainite during cooling after hot forming, an addition of 0.5% has proven to be advantageous.
  • a manganese content of at least 0.8%, particularly preferably at least 1.0% can be added to the flat steel product. If the manganese content is too high, the machinability of the steel, therefore the manganese content is limited to 2.6%. In particular, to improve the welding properties, the manganese content should preferably be limited to 1.6% and particularly preferably to 1.30%.
  • Silicon leads to solid solution strengthening in the hot-formed product and thus to a further increase in hardenability.
  • a proportion of at least 0.02% according to the invention has proven to be suitable for this purpose.
  • a proportion of at least 0.06% and particularly preferably at least 0.35% has proven to be particularly advantageous for adjusting hardenability. Too high a silicon content in the flat steel product can have a detrimental effect on coatability. Therefore, according to the invention, the silicon content is limited to 1.2%, preferably 1.1%, particularly preferably 0.9%.
  • Aluminium "AI” can be added to the steel as a deoxidising agent. To do this, at least 0.02% and preferably at least 0.03% aluminium is added to the steel. However, too high an aluminium content can increase the AC3 temperature and thus make hot forming more difficult. It has therefore proven advantageous to limit the aluminium content to 1.0, preferably 0.5% and particularly preferably 0.1%.
  • Phosphorus (“P”) and sulfur (“S”) are impurities in flat steel products that are caused by iron ore.
  • the aim is to keep the contents as low as possible, since mechanical properties can be negatively affected by too high a content.
  • the phosphorus content in the present invention is limited to 0.05%, preferably 0.03%.
  • the sulfur content should be at most 0.02%.
  • unavoidable impurities In addition to contamination by sulfur and phosphorus, other elements can also occur as impurities in the flat steel product. These other elements are summarized as "unavoidable impurities".
  • the content of these unavoidable impurities is preferably a maximum of 0.2% in total and particularly preferably 0.1%.
  • contents below the respective lower limit can also occur as impurities in the flat steel product. In this case, they are also counted as "unavoidable impurities".
  • the elements titanium, niobium, boron, chromium, molybdenum, nickel, copper and vanadium can optionally be alloyed into the steel of the flat steel product according to the invention, either individually or in combination.
  • titanium “Ti” can lead to improved grain refinement.
  • An optional addition of at least 0.01% can help with this.
  • the titanium content should be limited to 0.08%, as excessively high titanium contents negatively affect cold rollability and recrystallizability.
  • Niobium "Nb” influences grain refinement during austenitization in the hot forming process. For this purpose, it has been found to be advantageous to add at least 0.02% Nb to the steel according to the invention. However, niobium leads to impaired recrystallization. Therefore, the maximum niobium content is 0.08%, preferably 0.06%.
  • Boron "B” is added to improve the hardenability of the flat steel product. This effect occurs at a boron content of at least 0.001%, preferably at least 0.002%. If the boron content is too high, boron nitrides or boron carbides can form, so the boron content is limited to a maximum of 0.005%, preferably 0.004%.
  • Chromium "Cr” is added to the steel to enable complete martensite formation at low cooling rates by suppressing the formation of ferrite and pearlite.
  • the positive effect of chromium can be used at contents of at least 0.08%, preferably at least 0.18%. However, if the chromium content is too high, the coatability of the steel is negatively affected. Therefore, the maximum chromium content is limited to 1.0%, preferably 0.5%.
  • Molybdenum "Mo” can also optionally be used to suppress ferrite formation, as molybdenum slows down the phase transformation through carbide formation at the grain boundaries and reduces the nucleation rate of ferrite by lowering the grain boundary energy. The effect is particularly noticeable at a content of at least 0.002%. Due to the high cost of the element molybdenum, the maximum content should be limited to 0.5%.
  • Nickel “Ni” can optionally be added to the steel.
  • the optional addition of at least 0.01% nickel leads to a reduction in the Ac3 temperature and helps the formation of bainite and ferrite.
  • the maximum nickel content should be limited to 0.5%, especially 0.20%.
  • Copper “Cu” can optionally be added to the alloy with a content of at least 0.01% to increase hardenability.
  • the maximum Cu content should be limited to 0.2%, preferably 0.1%, as the hot rolling properties deteriorate if the copper content is too high.
  • Vanadium “V” can optionally be added to the alloy with a minimum of 0.001%.
  • the maximum vanadium content is limited to 0.1% for cost reasons.
  • the flat steel product is provided with an anti-corrosion coating which is aluminium-based and has an alloy layer and an Al-base layer.
  • Such a corrosion protection coating is preferably produced by hot-dip coating the flat steel product.
  • the flat steel product is passed through a liquid melt which consists of at least 3%, preferably at least 7%, particularly preferably at least 12% and a maximum of 15%, preferably a maximum of 12% silicon (Si), as well as up to 4.0% iron (Fe), preferably 1 - 3.5% Fe, particularly preferably 2 - 3.5% Fe, preferably 0.2 - 0.7% magnesium, and optionally up to 15% zinc (Zn), preferably up to 10% Zn and optionally further components, the total contents of which are limited to a maximum of 2.0%, and the remainder being aluminum.
  • a liquid melt which consists of at least 3%, preferably at least 7%, particularly preferably at least 12% and a maximum of 15%, preferably a maximum of 12% silicon (Si), as well as up to 4.0% iron (Fe), preferably 1 - 3.5% Fe, particularly preferably 2 - 3.5% Fe, preferably 0.2 - 0.7% magnesium, and optional
  • the thickness of the anti-corrosive coating applied to the flat steel product is typically 10 - 40 pm per side.
  • the coating weight is typically 30 - 100 g/m 2 , preferably 40 - 80 g/m 2 per side.
  • the phosphated flat steel product according to the invention is characterized in that the alloy layer consists of Fe: 35% - 90%,
  • Si 0.1% - 10%, optionally up to 0.5% Mg and optional further components, the total contents of which are limited to a maximum of 2.0%, and the remainder is aluminium and the Al base layer consists of Si: 1.0 - 15%, and optionally Fe: 1 - 4%,
  • Zn up to 15% and optional additional components, the total contents of which are limited to a maximum of 2.0%, and the remainder being aluminium.
  • the alloy layer has one boundary layer to the steel substrate and the other boundary layer to the Al base layer. Due to the diffusion of iron into the coating, iron is enriched in the alloy layer.
  • the alloy layer preferably consists of at least 35% iron.
  • the maximum content of iron in the alloy layer is preferably 90%, particularly preferably 55%.
  • the silicon content in the alloy layer is preferably at least 0.1% and in particular a maximum of 10%.
  • the alloy layer can contain magnesium.
  • the magnesium content should be limited to 0.5%.
  • a magnesium content of at least 0.1% has proven to be particularly advantageous.
  • the alloy layer optionally consists of other components, the content of which is limited to a maximum of 2.0% and the remainder being aluminum.
  • the optional other components include in particular the optional components of the melt, e.g. zinc.
  • the Al base layer is directly adjacent to the alloy layer.
  • the composition of the Al base layer preferably corresponds to the composition of the melt.
  • diffusion processes can lead to different contents.
  • the silicon content in the Al base layer is at least 1.0%, preferably 7.0%, particularly preferably 9.0% and the maximum silicon content is 15%, preferably 12%, particularly preferably 10%.
  • the proportion of iron in the Al base layer can be 1%, preferably 2%.
  • the maximum proportion of iron should be limited to 4%, particularly preferably 3.5%.
  • magnesium can be present in the Al base layer in proportions of up to 0.7%, preferably 0.4%.
  • the minimum proportion of magnesium in the Al base layer is 0.2%.
  • the Al base layer can contain zinc with a maximum proportion of 15%, optionally other components whose total contents are limited to a maximum of 2.0% and the remainder being aluminum.
  • the flat steel product is phosphated.
  • Commercial phosphating solutions such as Gardobond 26 T with the additive H7255 are used as the phosphating solution.
  • the phosphating solutions contain zinc, nickel, manganese, phosphoric acid and fluorides.
  • the phosphated flat steel product is characterized in that the degree of coverage with metal phosphates on the surface of the flat steel product is at least 10%, preferably 25%, particularly preferably 30%.
  • the degree of coverage is at least 72%, preferably 80%, particularly preferably 85%.
  • the degree of coverage can be limited to a maximum of 90%, preferably 79%, particularly preferably 72%, if the flat steel product is a rolled product during the application of the phosphating solution.
  • the high degree of coverage promotes homogeneous heating of the flat steel product to the forming temperature. With a lower degree of coverage, local differences in temperature can occur for a short time during heating, as the local reflectivity in areas not covered with metal phosphates is lower than in areas covered with metal phosphates. In addition, a high degree of coverage on the flat steel product ensures that the hot-formed component is later completely phosphated.
  • the pH of the phosphating solution is at least 2.0, preferably 2.5, particularly preferably 2.8, and at most 3.5, preferably 3.4, particularly preferably 3.3, in particular 3.2. If the pH is too low, a continuous phosphating layer cannot be formed because the pH change on the surface is not sufficient for crystallization to occur. If the pH is too high, the solution is not stable and metal phosphates precipitate and no continuous layer is formed. This can lead to a pickling attack on the surface.
  • the zinc concentration in the phosphating solution is at least 1 g/l. The maximum zinc concentration is 15 g/l. The nickel concentration is at least 0.5 g/l and a maximum of 10 g/l in the phosphating solution.
  • the zinc concentration and/or the nickel concentration can be increased by adding water-soluble salts, so that the sum of the zinc concentration and the nickel concentration in the phosphating solution is at least 2.4 g/l, preferably at least 7.5 g/l, particularly preferably at least 7.8 g/l.
  • the nickel concentration in the phosphating solution after the optional addition is at least 4 g/l, preferably 5 g/l, particularly preferably at least 6 g/l.
  • the increased zinc concentration and/or nickel concentration means that the zinc phosphate coating weight (or nickel phosphate coating weight) increases by at least 100% for the same phosphating time. Conversely, shorter phosphating times are required to obtain a closed phosphating layer, which enables a higher throughput during phosphating.
  • Fluorides are contained in the phosphating solution at a level of at least 0.5 g/l F-.
  • the fluoride concentration is at least 1.25 g/l F-, preferably 1.66 g/l F-, which leads to an increase in the layer weight of at least 100% compared to phosphating with lower fluoride concentrations.
  • the fluoride content in the present invention is a maximum of 3.8 g/l F-, preferably 3 g/l F-, particularly preferably 2.7 g/l F-.
  • the phosphating solution can contain oxidizing agents such as dimethyl sulfoxide or nitrates.
  • the nitrate concentration is at least 3 g/l, preferably at least 10 g/l, particularly preferably at least 12 g/l.
  • polyethylene glycol can be added to the phosphating solution as an additive. If it is added so that a concentration of at least 0.05 g/l, in particular 0.1 g/l is achieved, the layer weight also increases for the same phosphating time. The concentration should be limited to 5 g/l, in particular 1 g/l, since too high a concentration has negative properties on the phosphating quality.
  • copper can be added to the phosphating solution. The copper can be added in the form of water-soluble copper salts, in particular copper carbonate and/or copper nitrate. The copper concentration in the phosphating solution is then at least 0.01 g/l, preferably 0.05 g/l.
  • the Si-rich phases act as crystallization sites, since the Si-rich phases function as so-called microcathodes.
  • the copper particles can also act as additional microcathodes. These additional microcathodes are now also located between the areas with the Si-rich phases on the surface. This leads to the formation of a more homogeneous phosphating layer and shorter phosphating times being sufficient for complete phosphating.
  • the addition of copper should be limited to a maximum concentration of 0.5 g/l, since at higher concentrations the Cu deposition prevents effective phosphate deposition. In particular, the addition of copper should also be limited to a maximum of 0.1 g/l for resource reasons.
  • the flat steel product according to the invention has a reflectance R in the infrared range of ⁇ 0.65, preferably ⁇ 0.55, in particular ⁇ 0.40, preferably ⁇ 0.35.
  • the degree of reflection is adjusted during the production of the flat steel product.
  • the method for producing a phosphated flat steel product comprises the following steps: a) Providing a previously described steel substrate b) Hot-dip coating the steel substrate with an aluminum-based anti-corrosion coating, wherein the anti-corrosion coating has an alloy layer and an Al base layer c) Tempering the flat steel product d) Optionally cleaning the flat steel product e) Optionally activating the flat steel product f) Phosphating the flat steel product with a phosphating solution g) Optional alkaline cleaning of the flat steel product h) Optional oiling of the flat steel product
  • step a a steel substrate according to the invention with the specified alloy is provided.
  • the steel substrate is manufactured using conventional methods.
  • One possible embodiment is the following:
  • a slab or thin slab is provided, which can be produced by means of continuous slab casting or thin slab casting.
  • This slab or thin slab is heated through, optionally pre-rolled, hot rolled and optionally coiled.
  • the steel substrate is then descaled, optionally cold rolled and optionally annealed.
  • step b) the steel substrate is hot-dip coated with a corrosion protection coating.
  • the hot-dip coating preferably takes place in a continuous process.
  • step c) the flat steel product is skin-passed to improve the surface roughness.
  • skin-pass degrees of up to 3%, preferably up to 2%, are achieved.
  • step d the flat steel product is optionally cleaned. Whether this step is necessary depends on the cleanliness of the strip and the skin-pass agents used. In a special embodiment, cleaning can be carried out with a solution that contains sodium hydroxide and water as its main components.
  • the flat steel product can optionally be activated.
  • the activation solution results in more nucleation nuclei being present on the surface for later phosphating.
  • the activation solution preferably consists of zinc phosphates, as a higher zinc phosphate coating can then be achieved after the subsequent phosphating, compared with activations from other phosphate compounds, such as titanyl phosphates.
  • Commercially available activation solutions can be used, such as the activations ZL 6 or V6513, in particular V6559 from Chemetall.
  • the activation concentration used is at least 1 g/l, in particular at least 3 g/l, in order to apply sufficient nucleation nuclei to the surface.
  • the flat steel product is phosphated with a phosphating solution, in particular with one of the phosphating solutions previously described as advantageous.
  • step g) the flat steel product is optionally cleaned with alkali.
  • the flat steel product can be rinsed. This cleaning step can serve to reduce the fluoride content on the surface. The reduction may be desired in order to prevent the formation of a toxic HF atmosphere during hot forming.
  • step h the flat steel product is optionally oiled.
  • a hot-formed component can be produced from the phosphated flat steel product.
  • the following process steps are necessary for this: a) provision of a previously described flat steel product; b) optional separation of a sheet metal blank from the flat steel product and optional further processing; c) heating the sheet metal blank in such a way that the AC3 temperature of the blank is at least partially exceeded and the temperature T Einig of the blank when inserted into a forming tool intended for hot press forming (work step d)) at least partially has a temperature above Ms+100 °C, where Ms denotes the martensite start temperature; d) inserting the heated sheet metal blank into a forming tool, wherein the transfer time t Tr ans required for removing the blank from the heating device and inserting it is at most 20 s, preferably at most 15 s; e) hot-press forming the sheet metal blank to form the sheet metal part, wherein the blank is cooled to the target temperature T Ziei during the hot-press forming over a period t
  • step a) the previously described flat steel product is provided in step a). If the flat steel product is If the product is a rolled product, it can optionally be divided into sheet metal blanks in step b) and optionally undergo further processing that does not involve hot forming, e.g. punching, etc. If the flat steel product in step a) already consists of sheet metal blanks, step b) is omitted.
  • the flat steel product provided in step a) is heated at least partially to AC3 temperature in step c).
  • the temperature T Einig of the blank when placed in a forming tool intended for hot press forming (step d)) must at least partially be a temperature above Ms+100 °C.
  • partially exceeding a temperature is understood to mean that at least 30%, in particular at least 60%, of the volume of the blank exceeds a corresponding temperature.
  • at least 30% of the blank therefore has an austenitic structure, i.e.
  • the conversion from the ferritic to the austenitic structure does not have to be complete when placed in the forming tool. Rather, up to 70% of the volume of the blank when placed in the forming tool can consist of other structural components, such as tempered bainite, tempered martensite and/or non- or partially recrystallized ferrite. For this purpose, certain areas of the blank can be kept at a lower temperature level than others during heating. To do this, the heat supply can be directed only at certain sections of the blank, or the parts that are to be heated less can be shielded from the heat supply.
  • Maximum strength properties of the resulting sheet metal part can be achieved by ensuring that the temperature reached at least partially in the sheet metal blank is between AC3 and 1000 °C, preferably between 850 °C and 950 °C.
  • the average heating rate r O f e n of the sheet metal blank during heating in step c) is at least 5 K/s, preferably at least 11 K/s, in particular at least 15 K/s.
  • the average heating rate r O f e n is to be understood as the average heating rate from 30 °C to 700 °C.
  • the heating rate depends in particular on the sheet thickness. Therefore, in a preferred embodiment, the product of heating rate and sheet thickness in the temperature range 30 °C to 700 °C is greater than or equal to 12 (K*mm)/s, preferably greater than or equal to 15 (K*mm)/s, particularly preferably greater than or equal to 18 (K*mm)/s.
  • the average heating rate in the temperature range 500 °C to 750 °C is lower than the average heating rate in the temperature range 30 °C to 700 °C.
  • the average heating rate in the range 500 °C to 750 °C is >7 K/s, preferably >9 K/s, particularly preferably >10 K/s.
  • Phosphating on the steel substrate used increases the product of the average heating rate and sheet thickness compared to a non-phosphated steel substrate.
  • the layer with metal phosphates changes the reflectance of the surface.
  • the improvement in the heating rate compared to a non-phosphated steel sheet is at least 40%, preferably 60%, particularly preferably 70%, especially 80%.
  • the improvement in the heating rate is defined as (heating rate_phosphated - heating rate_unphosphated) / heating rate_unphosphated, whereby all other parameters are not changed. This makes it possible to carry out hot forming with less energy consumption.
  • the dew point in the furnace during the hot forming step is at least -20 °C, preferably at least -15 °C, in particular at least -5 °C, particularly preferably at least 0 °C, in particular at least 5 °C and a maximum of +25 °C, preferably a maximum of +20 °C, in particular a maximum of +15 °C.
  • the atmosphere in the furnace consists of air, i.e. 19 - 22 vol. % oxygen and 77-79 vol. % nitrogen and unavoidable air components (e.g. noble gases).
  • the heating in step c) takes place step by step in areas with different temperatures.
  • the heating takes place in a roller production ovens with different heating zones.
  • Heating takes place in a first heating zone at a temperature (so-called oven inlet temperature) of at least 650 °C, preferably at least 680 °C, in particular at least 720 °C.
  • the maximum temperature in the first heating zone is preferably 900 °C, in particular a maximum of 850 °C.
  • the maximum temperature of all heating zones in the oven is preferably a maximum of 1200 °C, in particular a maximum of 1000 °C, preferably a maximum of 950 °C, particularly preferably a maximum of 930 °C.
  • the total time in the furnace t O fen which consists of a heating time and a holding time, is preferably at least 2 minutes, in particular at least 3 minutes, preferably at least 4 minutes for both variants (constant furnace temperature, gradual heating). Furthermore, the total time in the furnace for both variants is preferably a maximum of 20 minutes, in particular a maximum of 15 minutes, preferably a maximum of 12 minutes, in particular a maximum of 8 minutes. Longer total times in the furnace have the advantage that uniform austenitization of the sheet metal blank is ensured. On the other hand, holding for too long above AC3 leads to grain coarsening, which has a negative effect on the mechanical properties.
  • the blank heated in this way is removed from the respective heating device, which can be, for example, a conventional heating furnace, an induction heating device that is also known per se or a conventional device for keeping steel components warm, and transported into the forming tool so quickly that its temperature when it arrives in the tool is at least partially above Ms+100 °C, preferably above 600 °C, in particular above 650 °C, particularly preferably above 700 °C.
  • Ms refers to the martensite start temperature.
  • the temperature is at least partially above the ACl temperature.
  • the temperature is in particular a maximum of 900 °C.
  • step d) the transfer of the austenitized blank from the heating device used to the forming tool is completed preferably within a maximum of 20 s, in particular within a maximum of 15 s. Such rapid transport is necessary to avoid excessive cooling before deformation.
  • the sheet metal blank is hot-pressed into a sheet metal part.
  • the tool typically has a temperature between room temperature and temperature (RT) and 200 °C, preferably between 20 °C and 180 °C, in particular between 50 °C and 150 °C.
  • the tool can be tempered at least in some areas to a temperature Twz of at least 200 °C, in particular at least 300 °C, in order to only partially harden the component.
  • the tool temperature T W z is preferably a maximum of 600 °C, in particular a maximum of 550 °C. It only has to be ensured that the tool temperature T W z is below the desired target temperature T Z iei.
  • step d) the sheet metal blank is partially cooled to the target temperature T Ziei at a cooling rate r wz of more than 30 K/s and is optionally held there.
  • the residence time in the tool t wz is more than 1 s, preferably at least 2s, in particular at least 3s, particularly preferably at least 5s.
  • the maximum residence time in the tool is preferably 25s, in particular a maximum of 20s.
  • the target temperature T Ziei of the sheet metal part is at least partially below 400 °C, preferably below 300 °C, in particular below 250 °C, preferably below 200 °C, particularly preferably below 180 °C, in particular below 150 °C.
  • the target temperature T Ziei of the sheet metal part is particularly preferably below Ms-50 °C, where Ms denotes the martensite start temperature.
  • the target temperature of the sheet metal part is preferably at least 20 °C, particularly preferably at least 50 °C.
  • the phosphating layer on the flat steel product acts as a forming aid during hot press forming.
  • the phosphate crystals serve as an additional sliding surface.
  • step f the sheet metal part is removed from the tool and cooled to the target temperature.
  • the resulting component can be further phosphated using conventional methods.
  • activation can be carried out before the phosphating step. This step may be necessary if a closed phosphating layer, i.e. coverage >99%, is required for the technical application.
  • the zinc phosphates can also serve as additional crystallization nuclei. This makes it possible to achieve a denser phosphate layer on the AS surface compared to a non-inventive component without a phosphated flat steel product. A non-phosphated flat steel product forms a dense closed oxide layer on the surface after hot forming, so that a large-area subsequent subsequent phosphating is hardly possible. In the subject matter according to the invention, it is helpful for good subsequent phosphating if the degree of coverage with metal phosphate crystals from the phosphating is as high as possible.
  • the hot-formed component obtained comprising a flat steel substrate with the composition according to the invention and an anti-corrosive coating, the anti-corrosive coating being aluminum-based and having an alloy layer and an Al base layer, is characterized in that the degree of coverage with metal phosphates on the surface is preferably at least 10%, in particular 25%, particularly preferably 30%.
  • the degree of coverage is at least 72%, preferably 80%, particularly preferably 85%.
  • the degree of coverage can be limited to a maximum of 90%, preferably 79%, particularly preferably 72%, if the product is a rolled product during the application of the phosphating solution. However, 100% coverage is not technically achievable. Due to the high degree of coverage after hot forming, a further phosphating step may not be necessary.
  • the hot-formed component is characterized in that the alloy layer consists of
  • Si 0.1 - 10%, optionally up to 0.5% Mg, and optional further components, the total contents of which are limited to a maximum of 2.0%, and the remainder being aluminium and the Al base layer comprising silicon-poor and silicon-rich phases, whereby the silicon contents in the phases in relation to the average value of the silicon content in the Al base layer Si ai applies:
  • the phosphating before hot forming causes a change in the Al base layer after hot forming, which lies directly below the oxide layer.
  • the change in the alloy layer is minimal.
  • the alloy layer after hot forming should have the same composition as before hot forming. Only the thickness of the alloy layer has increased during hot forming.
  • the alloy layer after hot forming preferably consists of at least 35% iron.
  • the maximum iron content in the alloy layer is preferably 90%, particularly preferably 55%.
  • the silicon content in the alloy layer after hot forming is preferably at least 0.1% and a maximum of 10%.
  • the alloy layer can contain magnesium.
  • the magnesium content should be limited to 0.5%.
  • a magnesium content of at least 0.1% has proven to be particularly advantageous.
  • the alloy layer after hot forming optionally consists of further components, the content of which is limited to a maximum of 2.0% and the remainder being aluminum.
  • the optional further components include in particular the optional components of the melt, e.g. zinc.
  • the Si-rich phase is more discrete. Discrete means that the Si-rich phases have less permeability.
  • the Al base layer comprises silicon-poor and silicon-rich phases, whereby the silicon content in the phases in relation to the average value of the silicon content in the Al base layer Si ai applies:
  • silicon-rich phases are arranged within the silicon-poor phase and/or the silicon-rich phases have a permeability of at most 90% and are in particular delimited by silicon-poor regions.
  • the permeability is at most 75%, particularly preferably at most 65%.
  • an oxide layer forms on the Al base layer.
  • This oxide layer is a mixture of different oxide types. The oxides formed depend on the composition of the corrosion protection coating. The required free reaction The enthalpy of formation for typical Al oxides, e.g. Al 2 O 3 , is lower than that of typical silicon oxides, e.g. Si 2 O 3 , at hot forming temperatures. Therefore, a large part of the outer oxide layer consists of Al oxides. These are formed by the diffusion of aluminum to the surface, where the aluminum reacts with the oxygen from the environment. The formation of this oxide layer in the present invention is disrupted by the metal phosphates on the surface during hot forming.
  • the Si-rich phases with lower permeability ensure that more aluminum remains in the Al base layer. This means that if the surface of the component is damaged, more free aluminum is available in the Al base layer. This free aluminum diffuses to the surface and forms another external aluminum oxide layer, thus protecting the component against corrosion.
  • This flat steel product was hot-dip coated with different corrosion protection coatings a and g using standard methods (see Table 2).
  • the melt analyses for each sample are given here in weight percent.
  • the coating thickness is also given on one side.
  • the rolled product was then phosphated directly as a coil and then sheet metal blanks were made, or sheet metal blanks were made from the rolled product and then phosphated.
  • the sheet metal blanks produced each had a size of 200x300 m. The respective procedure can be found in the "Process" column in Table 4.
  • the sheet metal blanks were heated to an oven temperature T O f en and held for a total time t O f en .
  • the oven temperature and the total time are given in Table 5.
  • the heating rate in the temperature range 30 °C to 700 °C depending on the sheet thickness is given in Table 6. Different values result depending on the phosphating solution.
  • the heating rate in the range 30 °C to 700 °C and in the range 500 °C to 100 °C were determined. Both are shown in Table 6.
  • the sheet metal blanks heated in this way were then placed in a forming tool with a maximum transfer time of 15 s.
  • the sheet metal blanks had a temperature above Ms+100 °C at least in some cases.
  • the forming tool was tempered to room temperature.
  • the sheet metal blanks were formed in the forming tool.
  • the formed sheet metal blanks were then cooled to room temperature within 20 s and removed from the tool.
  • heating rate_phosphated - heating rate_unphosphated was determined using (heating rate_phosphated - heating rate_unphosphated) / heating rate_unphos- phosphated.
  • the heating rate of reference example 0 was chosen as the unphosphated heating rate.
  • Si phases were determined on the cross-section using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX).
  • SEM scanning electron microscopy
  • EDX energy dispersive X-ray spectroscopy
  • variants 1-18 according to the invention have patencies ⁇ 75%.
  • Figure 1 shows a schematic cross-section of the hot-formed component without prior phosphating.
  • the figure is intended to serve as a reference.
  • On the steel substrate (1) there is an alloy layer (2) and on the alloy layer the Al base layer (3) with the Si-rich phases (4).
  • the Si-rich phases border on each other and this forms a 5-layer layer consisting of Al base layer / layer of Si-rich phases / Al base layer / layer of Si-rich phases / Al base layer.
  • Figure 2 shows a schematic of the hot-formed component according to the invention.
  • the layer structure also shows the alloy layer (2) on the steel substrate (1).
  • the Si-rich phases (4) are not connected to each other and are embedded in the Al base layer (3).
  • Figure 3 shows an SEM image of the surface of the steel product according to the invention at various magnifications.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Coating With Molten Metal (AREA)

Abstract

L'invention concerne un produit plat en acier phosphaté. La réflectance du produit plat en acier phosphaté est ≤ 0,65. L'invention concerne également un composant formé à chaud fabriqué à partir du produit plat en acier phosphaté. La structure en couches du revêtement de protection contre la corrosion sur le substrat en acier (1) du composant formé à chaud selon l'invention est constituée d'une couche d'alliage (2), d'une couche de base d'Al (3) et de phases riches en Si (4), qui ne sont pas liées ensemble et sont incorporées dans la couche de base d'Al (3). Sur la surface, il y a une couche d'oxyde avec du phosphore (6). Le composant formé à chaud peut éventuellement être phosphaté.
PCT/EP2024/057403 2023-03-28 2024-03-20 Produit plat en acier revêtu par immersion à chaud et phosphaté pour formage à chaud, composant formé à chaud et procédé de production Pending WO2024200152A1 (fr)

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EP23164640.7A EP4438757A1 (fr) 2023-03-28 2023-03-28 Produit plat en acier revêtu par immersion à chaud et phosphaté pour le formage à chaud
EP23164640.7 2023-03-28

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Citations (9)

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Publication number Priority date Publication date Assignee Title
JPH04254587A (ja) * 1991-02-04 1992-09-09 Nippon Parkerizing Co Ltd アルミニウム系金属板のプレス成形前処理方法及び塗装前処理方法
JP2007291441A (ja) * 2006-04-25 2007-11-08 Nippon Steel Corp 成形部の塗装後耐食性に優れた高強度自動車部材およびその熱間プレス方法
WO2012120081A2 (fr) 2011-03-08 2012-09-13 Thyssenkrupp Steel Europe Ag Produit plat en acier et procédé de fabrication d'un produit plat en acier
WO2015036151A1 (fr) 2013-09-13 2015-03-19 Thyssenkrupp Steel Europe Ag Procédé de fabrication d'un élément de construction en acier doté d'un revêtement de protection anticorrosion métallique et élément de construction en acier
US20180044774A1 (en) * 2015-02-19 2018-02-15 Arcelormittal Method of producing a phosphatable part from a sheet coated with an aluminum-based coating and a zinc coating
US20200165712A1 (en) * 2017-02-28 2020-05-28 Tata Steel Ijmuiden B.V. Method for producing a hot-formed coated steel product
CN111424212A (zh) * 2020-05-11 2020-07-17 马鞍山钢铁股份有限公司 一种抗拉强度1800MPa级镀铝钢板及其制造方法及热成形零部件
US20220090250A1 (en) * 2019-01-04 2022-03-24 Salzgitter Flachstahl Gmbh Aluminum-based coating for flat steel products for press mold hardening components, and method for producing same
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JPH04254587A (ja) * 1991-02-04 1992-09-09 Nippon Parkerizing Co Ltd アルミニウム系金属板のプレス成形前処理方法及び塗装前処理方法
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WO2015036151A1 (fr) 2013-09-13 2015-03-19 Thyssenkrupp Steel Europe Ag Procédé de fabrication d'un élément de construction en acier doté d'un revêtement de protection anticorrosion métallique et élément de construction en acier
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CN115443350A (zh) * 2020-05-18 2022-12-06 日本制铁株式会社 Al镀覆热冲压钢材

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