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EP0732425A1 - Passivation treatment of tinplate - Google Patents

Passivation treatment of tinplate Download PDF

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Publication number
EP0732425A1
EP0732425A1 EP96301491A EP96301491A EP0732425A1 EP 0732425 A1 EP0732425 A1 EP 0732425A1 EP 96301491 A EP96301491 A EP 96301491A EP 96301491 A EP96301491 A EP 96301491A EP 0732425 A1 EP0732425 A1 EP 0732425A1
Authority
EP
European Patent Office
Prior art keywords
tinplate
sulphate
titanium
chromium
treatments
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP96301491A
Other languages
German (de)
French (fr)
Other versions
EP0732425B1 (en
Inventor
Ieuan Stephen Rees
John Anthony Mcalister
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Corus UK Ltd
Original Assignee
British Steel PLC
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Filing date
Publication date
Application filed by British Steel PLC filed Critical British Steel PLC
Publication of EP0732425A1 publication Critical patent/EP0732425A1/en
Application granted granted Critical
Publication of EP0732425B1 publication Critical patent/EP0732425B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • 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
    • C23C22/68—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 solutions with pH between 6 and 8
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00—Electrolytic coating other than with metals
    • C25D9/04—Electrolytic coating other than with metals with inorganic materials
    • C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes

Definitions

  • This invention relates to passivation treatments for applying chromium-free passivation films to tin plate.
  • Passivation is a treatment in which chemically active surfaces of tinplate are coated with impervious films of a passive material by anodic or cathodic polarisation significantly to reduce the active state of such surfaces. It is of course extremely important that tinplate used in the canning industry is chemically inactive. In commercial production, strips of blackplate are passed continuously through a series of treatment tanks to clean, plate and chemically treat the plated material prior to use.
  • passivation fluids are chromium-based aqueous solutions, typically sodium dichromate. Like many chromium-based solutions, sodium dichromate is a hazardous fluid which represents a potential health risk to line operatives and is environmentally unfriendly. There is therefore on both health and environmental grounds an increasing need to develop chromium-free passivation treatments.
  • any such treatment must meet a range of performance criteria equivalent to or better than those of chromium based passivation treatments. Also, any such treatment should be capable of application under tinning line conditions similar to those used for chromate-based treatments, these including a typical treatment time of approximately one second.
  • the present invention sets out to provide a chromium-free passivation treatment which meets these and other criteria.
  • the passivating solution is an aqueous solution of a soluble compound selected from potassium titanium oxalate, titanium sulphate and zirconium sulphate.
  • Preferred concentrations of titanium sulphate in solution are from 15 to 30 gms per litre.
  • Preferred concentrations of potassium titanium oxalate in solution are from 5 to 20 gms per litre.
  • Preferred concentrations of zirconium sulphate in solution are from 10 to 30 gms per litre.
  • the invention provides a passivation treatment for tinplate in which the passivating element is either titanium or zirconium.
  • the plating line illustrated in Figure 1 comprises a plurality of guide rollers 1 for transporting a strip of blackplate 2 continuously from a coiled roll 3 to an exit coil 4 via a multiplicity of tanks.
  • These tanks include a cleaning tank 5, rinsing tanks 6, a pickling tank 7, a plating tank 8 and an electrolytic chemical treating tank 9.
  • Towards the centre of the plating line is a reflow 11 to each side of which are positioned a drag-out bath 12 and quenching bath 13.
  • a welding station 15 is positioned between the roll 3 and the entrance to the plating line.
  • the plating line illustrated is generally conventional.
  • strip is passed continuously through the plating line with a thin passivating film being applied to both sides of the tinplate as it passes through the tank 9.
  • the line speed is typically 300-350 metres per minute with a treatment dwell time in tank 9 of one second.
  • Static electrodes are provided in the tank 9, deposition of the passivating film being achieved by cathodic reaction.
  • the width of the strip 2 is typically 1 metre and above and the treatment temperature is typically 65°C.
  • the passivating solution present in the treatment tank 9 has been chromium-based and in particular sodium dichromate.
  • a chromium-free passivating solution is employed, this being selected from aqueous solutions of zirconium sulphate, potassium titanium oxalate and titanium sulphate.
  • zirconium sulphate a solution concentration in the range 10 to 30 gms per litre is preferred, a typical concentration being 21 gms per litre.
  • potassium titanium oxalate a solution concentration in the range 5 to 20 gms per litre is preferred, a typical concentration being 14 gms per litre.
  • titanium sulphate a solution concentration in the range 15 to 30 gms per litre is preferred, a typical concentration being 21 gms per litre.
  • the passivating element is either titanium or zirconium.
  • aqueous solutions of titanium sulphate in a concentration of 21 gm/litre, potassium titanium oxalate in a concentration of 14 gm/litre and zirconium sulphate in a concentration of 21 gm/litre were prepared. These solutions were in turn used in trial passivation treatments of tinplate, the bath temperature, cathodic application and pass time being respectively 65°C, coulomb density 6.4 c/dm 2 and one second. Strip speed for each trial was assumed as 180 metres/minute and the pass time through the passivation bath was one second.
  • the weldability range of tinplate treated in accordance with the invention was generally higher than for that treated using sodium dichromate. No abnormal weld features were observed.
  • tinplate treated in accordance with the invention exhibited less passive film damage than tinplate treated using sodium dichromate.
  • Tinplate produced by all these chromium-free treatments exhibited improved adhesion when compared with tinplate treated with sodium dichromate.
  • the trials show that treatments in accordance with the invention provide effective alternatives to sodium dichromate passivation and can be applied using current tinplate technology; that potassium titanium oxalate, titanium sulphate and zirconium sulphate based treatments meet requirements for alternative chromium-free passivation for tinplate; that it is possible to weld tinplate passivated in accordance with the invention at commercial settings; that treatments in accordance with the invention give improved lacquer adhesion compared to chromium-based treatments; that passive films produced in accordance with the invention provide more abrasion resistance than passive films produced using sodium dichromate; that treatments in accordance with the invention provide treatments of comparable performance to chromium-based treatments; that surface chemistry for treatments in accordance with the invention exhibited reduced amounts of passive film elements compared to chromium-based treatments; and that total oxide film thickness of tinplate treated in accordance with the invention were greater than that produced by chromium-based treatments.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)
  • Electrodes Of Semiconductors (AREA)
  • Chemically Coating (AREA)
  • Printing Plates And Materials Therefor (AREA)
  • Photoreceptors In Electrophotography (AREA)
  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Abstract

A chromium free passivation film for tinplate. The film is produced electrolytically by immersing tinplate in an aqueous solution of a soluble compound selected from potassium titanium oxalate, titanium sulphate and zirconium sulphate. The film so produced has sulphide stain resistance comparable to that produced by conventional chromium bearing passivating solutions.

Description

  • This invention relates to passivation treatments for applying chromium-free passivation films to tin plate.
  • Passivation is a treatment in which chemically active surfaces of tinplate are coated with impervious films of a passive material by anodic or cathodic polarisation significantly to reduce the active state of such surfaces. It is of course extremely important that tinplate used in the canning industry is chemically inactive. In commercial production, strips of blackplate are passed continuously through a series of treatment tanks to clean, plate and chemically treat the plated material prior to use. Conventionally, passivation fluids are chromium-based aqueous solutions, typically sodium dichromate. Like many chromium-based solutions, sodium dichromate is a hazardous fluid which represents a potential health risk to line operatives and is environmentally unfriendly. There is therefore on both health and environmental grounds an increasing need to develop chromium-free passivation treatments.
  • Commercially any such treatment must meet a range of performance criteria equivalent to or better than those of chromium based passivation treatments. Also, any such treatment should be capable of application under tinning line conditions similar to those used for chromate-based treatments, these including a typical treatment time of approximately one second.
  • The present invention sets out to provide a chromium-free passivation treatment which meets these and other criteria.
  • According to the present invention in one aspect there is provided a passivation treatment in which the passivating solution is an aqueous solution of a soluble compound selected from potassium titanium oxalate, titanium sulphate and zirconium sulphate.
  • Preferred concentrations of titanium sulphate in solution are from 15 to 30 gms per litre.
  • Preferred concentrations of potassium titanium oxalate in solution are from 5 to 20 gms per litre.
  • Preferred concentrations of zirconium sulphate in solution are from 10 to 30 gms per litre.
  • In a further aspect the invention provides a passivation treatment for tinplate in which the passivating element is either titanium or zirconium.
  • The invention will now be described by way of example only with reference to the accompanying diagrammatic drawings in which :-
    • Figure 1 is a schematic diagram of a plating line for conducting passivation treatments in accordance with the invention; and
    • Figure 2 is a graph comparing depth profile analyses of passivating elements in accordance with the invention with the conventional passivating element sodium dichromate.
  • The plating line illustrated in Figure 1 comprises a plurality of guide rollers 1 for transporting a strip of blackplate 2 continuously from a coiled roll 3 to an exit coil 4 via a multiplicity of tanks. These tanks include a cleaning tank 5, rinsing tanks 6, a pickling tank 7, a plating tank 8 and an electrolytic chemical treating tank 9. Towards the centre of the plating line is a reflow 11 to each side of which are positioned a drag-out bath 12 and quenching bath 13. A welding station 15 is positioned between the roll 3 and the entrance to the plating line. The plating line illustrated is generally conventional.
  • In use, strip is passed continuously through the plating line with a thin passivating film being applied to both sides of the tinplate as it passes through the tank 9. The line speed is typically 300-350 metres per minute with a treatment dwell time in tank 9 of one second. Static electrodes are provided in the tank 9, deposition of the passivating film being achieved by cathodic reaction. The width of the strip 2 is typically 1 metre and above and the treatment temperature is typically 65°C.
  • Hitherto the passivating solution present in the treatment tank 9 has been chromium-based and in particular sodium dichromate. In the present invention a chromium-free passivating solution is employed, this being selected from aqueous solutions of zirconium sulphate, potassium titanium oxalate and titanium sulphate.
  • For zirconium sulphate a solution concentration in the range 10 to 30 gms per litre is preferred, a typical concentration being 21 gms per litre.
  • For potassium titanium oxalate a solution concentration in the range 5 to 20 gms per litre is preferred, a typical concentration being 14 gms per litre.
  • For titanium sulphate a solution concentration in the range 15 to 30 gms per litre is preferred, a typical concentration being 21 gms per litre.
  • Thus, the passivating element is either titanium or zirconium.
  • Depth profile analyses of each of the passivating elements are shown in the graph of Figure 2. It was found that all three chromium-free treatments produced thicker oxide levels than a conventional chromium-based passivation treatment.
  • By way of example, aqueous solutions of titanium sulphate in a concentration of 21 gm/litre, potassium titanium oxalate in a concentration of 14 gm/litre and zirconium sulphate in a concentration of 21 gm/litre were prepared. These solutions were in turn used in trial passivation treatments of tinplate, the bath temperature, cathodic application and pass time being respectively 65°C, coulomb density 6.4 c/dm2 and one second. Strip speed for each trial was assumed as 180 metres/minute and the pass time through the passivation bath was one second.
  • Sulphide stain resistance of all three treatments was found marginally to be comparable to that of a treatment using sodium dichromate.
  • No discolouration of the tinplate occurred.
  • The weldability range of tinplate treated in accordance with the invention was generally higher than for that treated using sodium dichromate. No abnormal weld features were observed.
  • After two months storage, tinplate treated in accordance with the invention exhibited less passive film damage than tinplate treated using sodium dichromate.
  • Tinplate produced by all these chromium-free treatments exhibited improved adhesion when compared with tinplate treated with sodium dichromate.
  • It was found that surface concentrations of titanium and zirconium were lower than for chromium.
  • All three treatments produced thicker oxide levels than that produced with sodium dichromate.
  • In summary, the trials show that treatments in accordance with the invention provide effective alternatives to sodium dichromate passivation and can be applied using current tinplate technology; that potassium titanium oxalate, titanium sulphate and zirconium sulphate based treatments meet requirements for alternative chromium-free passivation for tinplate; that it is possible to weld tinplate passivated in accordance with the invention at commercial settings; that treatments in accordance with the invention give improved lacquer adhesion compared to chromium-based treatments; that passive films produced in accordance with the invention provide more abrasion resistance than passive films produced using sodium dichromate; that treatments in accordance with the invention provide treatments of comparable performance to chromium-based treatments; that surface chemistry for treatments in accordance with the invention exhibited reduced amounts of passive film elements compared to chromium-based treatments; and that total oxide film thickness of tinplate treated in accordance with the invention were greater than that produced by chromium-based treatments.
  • It will be appreciated that the foregoing is merely exemplary of treatments in accordance with the invention and that modifications can readily be made thereto without departing from the true scope of the invention as set out in the appended claims.

Claims (5)

  1. A passivation treatment for tinplate characterised in that the passivating solution is an aqueous solution of a soluble compound selected from potassium titanium oxalate, titanium sulphate and zirconium sulphate.
  2. A passivation treatment as claimed in Claim 1 wherein the concentration of titanium sulphate in solution is in the range from 15 to 30 gms per litre.
  3. A passivation treatment as claimed in Claim 1 wherein the concentration of potassium titanium oxalate in solution is in the range from 5 to 20 gms per litre.
  4. A passivation treatment as claimed in Claim 1 wherein the concentration of zirconium sulphate in solution is in the range from 10 to 30 gms per litre.
  5. A passivation treatment for tinplate characterised in that the passivating element is either titanium or zirconium.
EP96301491A 1995-03-13 1996-03-05 Passivation treatment of tinplate Expired - Lifetime EP0732425B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB9505041A GB2298870B (en) 1995-03-13 1995-03-13 Passivation treatment of tinplate
GB9505041 1995-03-13

Publications (2)

Publication Number Publication Date
EP0732425A1 true EP0732425A1 (en) 1996-09-18
EP0732425B1 EP0732425B1 (en) 2003-06-18

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EP96301491A Expired - Lifetime EP0732425B1 (en) 1995-03-13 1996-03-05 Passivation treatment of tinplate

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EP (1) EP0732425B1 (en)
AT (1) ATE243269T1 (en)
DE (1) DE69628689T2 (en)
GB (1) GB2298870B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002050341A2 (en) * 2000-12-19 2002-06-27 Centro Sviluppo Materiali S.P.A. Process for the passivation of tinned stainless steel strip with a chrome-free passivation film
EP1394292A2 (en) * 2000-05-06 2004-03-03 Henkel KGaA Electrochemically produced TiO2 layers for providing corrosion protection or wash primers
WO2006136333A2 (en) * 2005-06-22 2006-12-28 Henkel Kommanditgessellschaft Auf Aktien ELECTRODEPOSITION MATERIAL, PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2
EP2180084A4 (en) * 2007-08-23 2016-01-27 Nippon Steel & Sumitomo Metal Corp Environmentally friendly steel sheet for container material, process for producing the same, and environmentally friendly laminated steel sheet for container material and precoated steel sheet for container material each produced from that steel sheet
EP3626862A1 (en) * 2018-09-24 2020-03-25 Tenova S.p.A. Passivation process of a steel tinplate

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4339310A (en) * 1980-11-25 1982-07-13 Hooker Chemicals & Plastics Corp. Method of surface treatment of tin plated cans and tin plated steel sheets

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5468734A (en) * 1977-11-11 1979-06-02 Nippon Packaging Kk Surface treatment of tin plated steel plate and can
JPS5993886A (en) * 1982-11-17 1984-05-30 Katayama Chem Works Co Ltd Anticorrosive for metal

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4339310A (en) * 1980-11-25 1982-07-13 Hooker Chemicals & Plastics Corp. Method of surface treatment of tin plated cans and tin plated steel sheets

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1394292A2 (en) * 2000-05-06 2004-03-03 Henkel KGaA Electrochemically produced TiO2 layers for providing corrosion protection or wash primers
EP1394292A3 (en) * 2000-05-06 2004-06-16 Henkel KGaA Electrochemically produced TiO2 layers for providing corrosion protection or wash primers
WO2002050341A2 (en) * 2000-12-19 2002-06-27 Centro Sviluppo Materiali S.P.A. Process for the passivation of tinned stainless steel strip with a chrome-free passivation film
WO2002050341A3 (en) * 2000-12-19 2003-09-25 Ct Sviluppo Materiali Spa Process for the passivation of tinned stainless steel strip with a chrome-free passivation film
WO2006136333A2 (en) * 2005-06-22 2006-12-28 Henkel Kommanditgessellschaft Auf Aktien ELECTRODEPOSITION MATERIAL, PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2
WO2006136333A3 (en) * 2005-06-22 2007-08-16 Henkel Kommanditgessellschaft ELECTRODEPOSITION MATERIAL, PROCESS FOR PROVIDING A CORROSION-PROTECTIVE LAYER OF TiO2 ON AN ELECTRICALLY CONDUCTIVE SUBSTRATE AND METAL SUBSTRATE COATED WITH A LAYER OF TiO2
EP2180084A4 (en) * 2007-08-23 2016-01-27 Nippon Steel & Sumitomo Metal Corp Environmentally friendly steel sheet for container material, process for producing the same, and environmentally friendly laminated steel sheet for container material and precoated steel sheet for container material each produced from that steel sheet
EP3626862A1 (en) * 2018-09-24 2020-03-25 Tenova S.p.A. Passivation process of a steel tinplate
CN110938852A (en) * 2018-09-24 2020-03-31 特诺恩股份公司 Passivation process of tin-plated steel plate
CN110938852B (en) * 2018-09-24 2023-12-12 特诺恩股份公司 Passivation process of tin-plated steel plate

Also Published As

Publication number Publication date
EP0732425B1 (en) 2003-06-18
GB2298870A (en) 1996-09-18
ATE243269T1 (en) 2003-07-15
GB2298870B (en) 1998-09-30
DE69628689T2 (en) 2004-04-29
GB9505041D0 (en) 1995-05-03
DE69628689D1 (en) 2003-07-24

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