EP1579030A1 - Procede de formation d'un revetement anticorrosion mince sur une surface metallique - Google Patents

Procede de formation d'un revetement anticorrosion mince sur une surface metallique

Info

Publication number
EP1579030A1
EP1579030A1 EP03789349A EP03789349A EP1579030A1 EP 1579030 A1 EP1579030 A1 EP 1579030A1 EP 03789349 A EP03789349 A EP 03789349A EP 03789349 A EP03789349 A EP 03789349A EP 1579030 A1 EP1579030 A1 EP 1579030A1
Authority
EP
European Patent Office
Prior art keywords
coating
phosphating
solution
dispersion
process according
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
EP03789349A
Other languages
German (de)
English (en)
Other versions
EP1579030B1 (fr
Inventor
Michael Deemer
Chanard Cooper
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.)
Chemetall GmbH
Original Assignee
Chemetall GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Chemetall GmbH filed Critical Chemetall GmbH
Publication of EP1579030A1 publication Critical patent/EP1579030A1/fr
Application granted granted Critical
Publication of EP1579030B1 publication Critical patent/EP1579030B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • 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
    • 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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • 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
    • C23C22/07—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 phosphates
    • C23C22/08—Orthophosphates
    • C23C22/10—Orthophosphates containing oxidants
    • 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

Definitions

  • the alkali metal phosphating coatings are mostly poor, nearly free or totally free of manganese and zinc, if there will not be manganese and/or zinc rich surfaces, to be pretreated or treated. They are typically poor, nearly free or totally free of chromium, cobalt, copper, nickel, tin and/or other heavy metals.
  • the phases mainly generated and/or precipitated during iron phosphating, which is performed by contacting iron-rich metallic surfaces with an alkali metal phosphating solution, are iron phosphates, iron oxides and iron hydroxides like e.g. vivianite and/or magnetite.
  • DE-A1-1 914 052 concerns an alkali metal phosphating process by using a rollcoating application with a solution containing 5 to 20 g/L of phosphate ions and 3 to 12.5 g/L of chlorate at a temperature of 54.5 to 60 °C with an extraordinarily unconventional pH value in the range of 1 to 3.5 contacting a coil less than 30 seconds and squeegeeing.
  • EP-B1 -0 968 320 protects a process for an alkali metal phosphating for radiators by using a surfactant rich solution of a pH value in the range from 4 to 6 at a temperature in the range from 35 to 60 °C and especially of at least 50 °C.
  • the orthophosphoric acid may be added as acid, as monoacid and/or as poly acid salt of an alkali metal and/or of an ammonium group or in a small amount as an iron phosphate.
  • orthophosphoric acid its ester(s) and/or its salt(s)
  • a phosphonic acid and/or other phosphorus containing acid and/or at least one of their salts and/or esters may be added to the solution or dispersion, especially at least one water-soluble ester of phosphoric acid.
  • the cleaning and phosphating may be carried out in the same bath container with the same solution or dispersion, so that in the first time of contacting the metallic components with the phosphating solution or dispersion, the cleaning and pickling effect of the solution or dispersion may prevail, whereas in the further time of the contacting, the coating process with the phosphating coating formation may predominate.
  • nearly all types of surfactants resp. surfactant mixtures are suitable to be added to the phosphating solution or dispersion, especially surfactants resp. surfactant mixtures with low- foaming or non-foaming properties and with a cloud-point in the range from 25 to 40 °C, whereby the surfactant mixtures may be free of further constituents than surfactants.
  • At least two coatings one after the other on the metallic surface whereby at least one of them is applied with an alkali metal phosphating solution resp. dispersion and whereby at least one other coating may optionally be applied with a conversion coating solution like a zinc- and/or manganese-rich phosphating.
  • an alkali metal phosphating coating is generated on a metallic surface and then a coating selected from the group consisting of a conversion coating like a zinc- and/or manganese-rich phosphating coating, a stearate coating and an organic polymer coating is applied thereon, especially for coldforming.
  • Panels of cold rolled steel (CRS) were cleaned with Okemclean ® at 3 % by volume and 54.4 °C for 30 seconds by spraying. The panels were then rinsed and afterwards treated in the phosphating bath A or B for 60 seconds by spraying at various temperatures. This was followed by rinsing and drying with compressed air. The panels were finally painted with a Dupont TGIC polyester powder paint and subjected to a salt spray (fog) test strictly according to ASTM B 117 for 336 hours for the evaluation of the corrosion inhibiting properties strictly according to a ASTM D 1654 rating, with 10 to be the best and 0 the worst.
  • CRS cold rolled steel
  • Group 2 Comparison Examples 11 to 42: The same base bath formulations were used for the following tests with the standard chlorate-SNBS-accelerated system A and with the nitroguanidine- accelerated system B as in Group 1. Panels of cold rolled steel (CRS), hot dipped galvanized steel (HDG), electrogalvanized steel (EG) and aluminum alloy AA 6061 were cleaned with Gardoclean ® S 5206, rinsed, treated in the phosphating baths A or B and then rinsed and dried with compressed air. Based on Group 1 , the temperature range covered was changed to lower temperatures used. The panels were finally painted with Morton Corvel Black powder paint and subjected to salt spray (fog) test for 250 hours according to ASTM B 117. The creepage from scribe was measured according to the rating from 0 to 10 according to ASTM D 1654; the higher the SS values, the better are the results.
  • CRS cold rolled steel
  • HDG hot dipped galvanized steel
  • EG electrogalvanized steel
  • Al alloy AA 6061 were
  • the CRS panels went from grey-brown to blue as temperature increased.
  • the HDG and EG panels showed an etched appearance in all cases, but no colour.
  • the aluminum panels were shiny with no apparently visible coating.
  • the CRS panels went from blue to golden with increasing temperature, the HDG and EG panels had an iridescent appearance and the aluminum panels had a transparent light tan colour.
  • the cold rolled steel panels were treated with aqueous acidic phosphating solutions C containing only a very tiny amount much less of 1 g/L of phosphoric acid only to adapt the pH value of the ready mixed solution to 2.5 resp. 4.5, 0.2 g/L nitroguanidine and 0.2 g/L aminoguanidine bicarbonate. If in all the examples aminoguanidine was added, it was added as bicarbonate, although not always indicated.
  • the panels were cleaned with Gardoclean ® S 5206 and rinsed before the nitro- and the aminoguanidine were added.
  • the panels were contacted with the phosphating solution for the test with a pH value of 2.5 at ambient temperature and for the test with a pH value of 4.5 at 49 °C.
  • the phosphating baths were prepared with varying amounts of the base bath formulations starting from Group 1 and varying the accelerator concentrations of A and B.
  • the conversion coating baths were operated at 26.7 °C and mostly at a pH value 4.5 for 60 second spraying.
  • the last comparison example 79 was the standard chlorate-SNBS-accelerated alkali metal phosphating as outlined in Group 1 , but only this was operated at a pH value of 4.5 and at a temperature of 48.9 °C for 80 seconds of spraying.
  • the salt spray rating was evaluated according to ASTM D 1654 after 500 hours salt spray (fog) test according to ASTM B 117. Table 6: Results of the salt spray test and the coating weight dependent from the accelerator amount of the coating solutions of differently accelerated alkali metal phosphating systems and of the pH value at a temperature of 26.7 °C; * bath without accelerator content
  • the bath solution contained fluoride to treat cold rolled steel, hot dipped galvanized, electrogalvanized and aluminum.
  • the base solution B of Group 1 was used by with an additional content of free fluoride, whereby the content of all components of this bath were varied at a temperature of 38 °C.
  • the panels were painted with a Ferro TGIC polyester powder paint of 38 to 51 ⁇ m thickness and were put into a salt spray (SS) test chamber according to ASTM B 117 for 250 hours, whereby the test results were measured in mm creep from the scribe. Further on, adhesion was tested according to ASTMD 3359, whereby 5B means that no flaking did occur in the cross-cut area which is the best possible test result, whereas e.g. 2B means that there is a certain amount of flaking in the crosscut area.
  • SS salt spray
  • Table 8 Results of the salt spray (fog) test on three CRS panels each dependent from the chemical composition of the coating solutions, the pH value, the contacting time and the temperature; * bath without accelerator content
  • the appearance of the coatings was at least as good as for comparable good alkali metal phosphating coatings used in the market. As best accelerator during all these studies, nitroguanidine was identified.
  • the alkali metal phosphating process with the slightly modified working conditions for the solutions according to the invention are well suited for industrial application of coils, parts and wires.
  • the use of the phosphating solution at a significantly lower temperature than today usual for the contacting of metallic surfaces helps to reduce heating costs considerably.
  • the herein proposed phosphating process is easier than the processes used today as it is quite sufficient to control only total and free acid content, but no other parameters of the bath within short time limits, as the bath behaviour is very stable.
  • this process is not only superior because less heating is needed and therefor is cheaper in comparison to actually used processes as there is a significant lower consumption of all chemical compounds of the solution than usual.
  • the panels showed excellent thin coatings of more or less tan colour and good or even excellent corrosion inhibition.
  • the best standard for an iron phosphate coating coated with a chrome final seal reached a salt spray test rating for 240 h of 0.2 mm creep.
  • the results are excellent.

Landscapes

  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Paints Or Removers (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)
EP03789349A 2002-12-24 2003-12-18 Procede de formation d'un revetement anticorrosion mince sur une surface metallique Expired - Lifetime EP1579030B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US328924 2002-12-24
US10/328,924 US20040118483A1 (en) 2002-12-24 2002-12-24 Process and solution for providing a thin corrosion inhibiting coating on a metallic surface
PCT/EP2003/014577 WO2004059034A1 (fr) 2002-12-24 2003-12-18 Procede de formation d'un revetement anticorrosion mince sur une surface metallique

Publications (2)

Publication Number Publication Date
EP1579030A1 true EP1579030A1 (fr) 2005-09-28
EP1579030B1 EP1579030B1 (fr) 2010-04-14

Family

ID=32594623

Family Applications (1)

Application Number Title Priority Date Filing Date
EP03789349A Expired - Lifetime EP1579030B1 (fr) 2002-12-24 2003-12-18 Procede de formation d'un revetement anticorrosion mince sur une surface metallique

Country Status (13)

Country Link
US (1) US20040118483A1 (fr)
EP (1) EP1579030B1 (fr)
CN (1) CN1754009B (fr)
AT (1) ATE464404T1 (fr)
AU (1) AU2003293945B2 (fr)
BR (1) BR0316881A (fr)
CA (1) CA2511361A1 (fr)
DE (1) DE60332161D1 (fr)
ES (1) ES2344345T3 (fr)
MX (1) MXPA05006897A (fr)
RU (1) RU2358035C2 (fr)
WO (1) WO2004059034A1 (fr)
ZA (1) ZA200505064B (fr)

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DE102006052919A1 (de) * 2006-11-08 2008-05-15 Henkel Kgaa Zr-/Ti-haltige Phosphatierlösung zur Passivierung von Metallverbundoberflächen
CN101629288B (zh) * 2009-08-21 2011-06-22 攀钢集团钢铁钒钛股份有限公司 热镀铝锌板用钝化处理剂及其制备方法
CN102061464B (zh) * 2009-11-12 2013-05-15 佛山市中国地质大学研究院 一种新型环保钝化剂
JP5852338B2 (ja) * 2010-08-19 2016-02-03 株式会社神戸製鋼所 スケール付着抑制性に優れた表面処理金属材の製造方法および海水蒸発器
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RU2468125C1 (ru) * 2011-05-23 2012-11-27 Федеральное государственное бюджетное учреждение науки Институт физической химии и электрохимии им. А.Н. Фрумкина Российской академии наук (ИФХЭ РАН) Пассивация поверхности металлов для защиты от атмосферной коррозии
CN102560461A (zh) * 2012-01-18 2012-07-11 河北科技大学 一种锆及锆合金锌锰复合磷化液及其磷化方法
WO2015055756A1 (fr) * 2013-10-17 2015-04-23 Chemetall Gmbh Procédé de préparation d'articles façonnés métalliques en vue du formage à froid
CN103498138B (zh) * 2013-10-21 2016-03-30 航天精工股份有限公司 钛合金紧固件涂覆前磷化处理方法
US10513784B2 (en) 2014-04-30 2019-12-24 Rio Verwaltungs Ag Treatment device and treatment method for pickling and phosphating metal parts
CN104372323B (zh) * 2014-11-13 2016-09-07 佛山市科腾铝业制品有限公司 铝合金无铬水性钝化剂及其制备方法
KR20190039560A (ko) * 2016-08-12 2019-04-12 피알시-데소토 인터내쇼날, 인코포레이티드 밀봉 조성물
HUE047403T2 (hu) * 2017-04-21 2020-04-28 Henkel Ag & Co Kgaa Lerakódásmentes foszfátbevonat-képzési módszer fémalkatrész sorozatokhoz
DE102017207591A1 (de) * 2017-05-05 2018-11-08 Federal-Mogul Nürnberg GmbH Stahlkolben mit einer Phosphat-Schicht
CN107488849A (zh) * 2017-08-24 2017-12-19 南通市烨达汽车零部件有限公司 一种汽车冲压件表面处理液
CN108085684B (zh) * 2017-11-23 2019-10-08 中国科学院近代物理研究所 用于去除铜表面铌镀层的化学退镀液和退镀方法
CN107966401A (zh) * 2017-12-26 2018-04-27 华测检测认证集团股份有限公司 材料耐腐蚀性能测试装置
CN107966402A (zh) * 2017-12-26 2018-04-27 华测检测认证集团股份有限公司 金属涂层耐磨耐高温性能测试装置
CN108007806A (zh) * 2017-12-26 2018-05-08 华测检测认证集团股份有限公司 金属涂层耐磨耐高温及成份分析设备
GB201917790D0 (en) * 2019-12-05 2020-01-22 Coated Metallic Tech Limited Protective coatings for metals
CN112011791A (zh) * 2020-08-28 2020-12-01 立邦涂料（重庆）化工有限公司 一种基于磷酸无需表调工序及无需亚钠类促进剂的化成剂及制备方法
CN116497267A (zh) * 2022-01-19 2023-07-28 宝山钢铁股份有限公司 一种具有优良加工性和防腐性能的免涂油带钢及其制造方法
CN115367808B (zh) * 2022-08-23 2023-06-23 湘潭大学 一种黄铁矿表面钝化处理的方法

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Also Published As

Publication number Publication date
DE60332161D1 (de) 2010-05-27
ES2344345T3 (es) 2010-08-25
US20040118483A1 (en) 2004-06-24
EP1579030B1 (fr) 2010-04-14
AU2003293945A1 (en) 2004-07-22
BR0316881A (pt) 2005-10-25
RU2005123323A (ru) 2006-02-10
CN1754009B (zh) 2011-10-19
ATE464404T1 (de) 2010-04-15
CN1754009A (zh) 2006-03-29
AU2003293945B2 (en) 2009-01-22
CA2511361A1 (fr) 2004-07-15
ZA200505064B (en) 2008-09-25
MXPA05006897A (es) 2005-08-18
RU2358035C2 (ru) 2009-06-10
WO2004059034A1 (fr) 2004-07-15

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