# US 10,480,080 B2 · Method for activating metal surfaces to be phosphated > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,480,080 B2 - Document ID: US10480080B2 - Status: Granted - Kind: B2 - Application number: 15/302,365 - Filed: 2015-04-07 - Published: 2017-02-02 - Granted: 2019-11-19 - Earliest claimed: 2014-04-11 - Assignees: ThyssenKrupp Steel Europe AG; thyssenkrupp AG - Applicants: ThyssenKrupp Steel Europe AG; ThyssenKrupp AG - Inventors: Fabian Junge; Gregor Müller; Nicole Weiher; Heinrich Meyring; Frank Panter - Web page: https://patentgrep.com/patent/US10480080B2 ## CPC - C23C 22/80: with solutions containing titanium or zirconium compounds - C23C 18/30: Activating {or accelerating or sensitising with palladium or other noble metal} - C23C 22/07: containing phosphates - C23C 22/78: Pretreatment of the material to be coated - C23F 17/00: Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25 (coating for obtaining at least two superposed coatings either by methods not provided for in a single one of main groups C23C2/00 - C23C26/00, or by combinations of methods providedfor in subclasses C23C and C25D, C23C28/00) - C25D 3/22: of zinc - 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 (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - C23F: NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE (working metal by laser beams B23K26/00; desurfacing by applying flames B23K7/00; working of metal by electro-erosion B23H; producing decorative effects by removing surface material, e.g. by engraving, by etching, B44C1/22; electrolytic etching or polishing C25F); INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25 - C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR ## Abstract A method of activating a metal surface, such as a galvanized steel sheet, before a phosphating process, may involve bringing the metal surface into contact with an activating bath containing activating particles, which may be based on phosphate and/or titanium, dispersed in water. To alleviate or even eliminate the problems of poor adhesion of surface coatings to preferably electrolytically galvanized, phosphated metal strip, an additive that suppresses or at least slows agglomeration of the activating particles may be added to the activating bath. In some examples, polyethylene glycol (PEG) and/or sodium stearate may be added. Further, the particle size distribution of the activating particles present in the activating bath may be determined and the activating bath may be replaced or taken out of operation as a function of the particle size distribution of the activating particles. ## Claims ### Claim 1 A method for activating a metal surface prior to a phosphating process, the method comprising: adding to an activating bath of activating particles dispersed in water an additive that suppresses or at least slows agglomeration of the activating particles, wherein the activating particles are based on at least one of phosphate or titanium; adding to the activating bath a surfactant for suppressing or slowing agglomeration of the activating particles, wherein the surfactant is at least one of polyethylene glycol or sodium stearate; and bringing the metal surface into contact with the activating bath. ### Claim 2 (depends on 1) The method of claim 1 wherein the metal surface is a coated metal surface. ### Claim 3 (depends on 1) The method of claim 1 wherein the metal surface is a galvanized steel sheet. ### Claim 4 (depends on 1) The method of claim 1 further comprising agitating the activating bath continuously or discontinuously by at least one of stirring, pumped circulation, or ultrasound. ### Claim 5 (depends on 4) The method of claim 4 wherein the agitating occurs at least when the additive is added to the activating bath and when the metal surface is brought into contact with the activating bath. ### Claim 6 (depends on 5) The method of claim 5 further comprising stirring the activating bath by a mechanical stirrer. ### Claim 7 (depends on 1) The method of claim 1 further comprising: determining a particle size distribution of the activating particles in the activating bath; and replacing the activating bath based on the particle size distribution of the activating particles. ### Claim 8 (depends on 7) The method of claim 7 wherein the determining of the particle size distribution of the activating particles occurs either continuously or periodically by way of dynamic light scattering during operation of the activating bath. ### Claim 9 (depends on 7) The method of claim 7 wherein the determining of the particle size distribution of the activating particles occurs either continuously or periodically by way of nanoparticle tracking analysis during operation of the activating bath. ### Claim 10 (depends on 1) The method of claim 1 further comprising adjusting the activating bath to have an activating particle concentration in a range of 0.1 g/l to 10 g/l. ### Claim 11 (depends on 1) The method of claim 1 further comprising adjusting the activating bath to have an activating particle concentration in a range of 0.5 g/l to 3 g/l. ### Claim 12 (depends on 1) The method of claim 1 further comprising adjusting the activating bath to have an activating particle concentration in a range of 0.7 g/l to 1.5 g/l. ### Claim 13 A method for activating a metal surface for a phosphating process, the method comprising: galvanizing the metal surface in an electrolytic cell; adding to an activating bath of activating particles dispersed in water an additive that suppresses or at least slows agglomeration of the activating particles, wherein the activating particles are based on at least one of phosphate, titanium, or metal oxides; determining a particle size distribution of the activating particles in the activating bath; replacing the activating bath based on the particle size distribution of the activating particles; and bringing the metal surface into contact with the activating bath. ### Claim 14 (depends on 13) The method of claim 13 further comprising rinsing the metal surface after the metal surface is galvanized. ### Claim 15 (depends on 13) The method of claim 13 further comprising squeezing, wiping, or blowing the metal surface a liquid film from the metal surface after the metal surface exits the activating bath. ### Claim 16 (depends on 15) The method of claim 15 further comprising spraying a phosphating solution onto the metal surface after the metal surface exits the activating bath. ### Claim 17 (depends on 13) The method of claim 13 further comprising spraying a phosphating solution onto the metal surface after the metal surface exits the activating bath.