EP2147131B1 - Verfahren zum thermochemischen passivieren von edelstahl - Google Patents

Verfahren zum thermochemischen passivieren von edelstahl Download PDF

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Publication number
EP2147131B1
EP2147131B1 EP08715970A EP08715970A EP2147131B1 EP 2147131 B1 EP2147131 B1 EP 2147131B1 EP 08715970 A EP08715970 A EP 08715970A EP 08715970 A EP08715970 A EP 08715970A EP 2147131 B1 EP2147131 B1 EP 2147131B1
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Prior art keywords
stainless steel
process according
heat treatment
weight
salts
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EP08715970A
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German (de)
English (en)
French (fr)
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EP2147131A1 (de
Inventor
Olaf BÖHME
Siegfried Piesslinger-Schweiger
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Poligrat GmbH
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Poligrat GmbH
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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
    • C23C22/73—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
    • 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
    • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/50—Treatment of iron 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
    • 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
    • C23C22/82—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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/02—Pretreatment of the material to be coated

Definitions

  • the present invention relates to a novel method of passivating stainless steel surfaces which provides improved corrosion resistance of the treated surfaces as well as increasing the resistance of these surfaces to thermal discoloration.
  • the process consists of a chemical treatment with an aqueous solution comprising complexing agents, a rinsing and a subsequent thermal treatment in a gaseous, oxygen-containing atmosphere.
  • Stainless steel which is often referred to as stainless steel, is an iron alloy which, in addition to iron, may contain a number of other elements such as chromium, nickel, molybdenum, copper and others.
  • the chromium present in the alloy reacts with oxygen from the environment at the surface and forms an oxide layer on the surface of the material.
  • the resulting chromium oxide can reliably form a dense layer on the surface and thus protects the workpiece from corrosion.
  • This protective layer is also called a passive layer.
  • Such a passive layer is usually about 10 molecule layers thick and contains in addition to the chromium oxide especially iron oxide in a concentration of 10-55 wt .-%.
  • the corrosion resistance of the workpiece depends on the content of chromium and other alloying elements such as nickel and molybdenum. These additional alloying elements are added to the stainless steel alloy to form the Corrosion resistance to further improve, if the addition of chromium alone is not able to give the workpiece the desired degree of corrosion resistance or other characteristics.
  • these other corrosion resistance improving elements are expensive and thus increase the cost of producing the stainless steel to a considerable extent.
  • Another known measure to increase corrosion resistance is to increase the ratio of chromium to iron in the passive layer.
  • treatment of the surface with substances that have a high affinity for iron ions and thus are able to selectively dissolve out and bind iron ions from the passive layer is suitable for this purpose.
  • aqueous solutions of complexing agents and / or chelating agents such as citric acid are frequently used, for example, the chromium / iron ratio on bright-rolled or ground stainless steel surfaces of a value of 0.8 to 1.2 before the treatment to a value of 3.0 can increase to 5.0 after treatment.
  • This increased content of chromium oxide causes a correspondingly improved corrosion resistance of the workpiece.
  • thermally grown oxide layers significantly reduce the corrosion resistance of the stainless steel by either preventing the formation of true passive layers or displacing existing passive layers at higher temperatures.
  • thermally generated oxide layers such as the tarnish or scale described above
  • thermally generated oxide layers such as the tarnish or scale described above
  • no method is known in the prior art, which improves the resistance of stainless steel surfaces against thermal discoloration, ie against the formation of such thermally generated oxide layers.
  • the aim of the present invention is a method for passivation of stainless steel surfaces, which in comparison to known passivation method according to the prior art, a significant increase in the corrosion potential, measured as pitting potential according to DIN 50900 causes.
  • the increase in corrosion potential that can be achieved with the methods described herein ranges from +500 mV to +850 mV from the initial state. This makes it possible in many cases, instead of expensive molybdenum or copper-containing materials cheaper To use stainless steel grades that have the required corrosion resistance due to their passivation according to a method of the present invention.
  • the corrosion resistance of the stainless steel surface can be markedly improved both for workpieces made of stainless steel with ferritic and austenitic structures by targeted heat treatment of the surfaces in an oxygen-containing atmosphere.
  • This heat treatment in an oxygen-containing atmosphere is often referred to below as heat treatment or thermal treatment.
  • the stainless steel workpiece is heated to a temperature of at least 80 ° C for a certain period of time.
  • the upper limit of the temperature to be used is given by the temperature at which a thermally induced discoloration of the stainless steel surface begins and varies depending on the quality of stainless steel used.
  • the present invention thus relates to a method for passivating stainless steel, wherein the stainless steel is first subjected to a chemical treatment with an aqueous solution, then rinsed with water and subsequently a heat treatment is carried out.
  • the aqueous solution used in the chemical treatment comprises at least one complexing agent combination and an oxidizing agent.
  • the complexing agent combination consists of those compounds known to complex iron ions in aqueous solution.
  • the invention is based in particular on the observation that only with a combination of the complexing agents a passivation effect is achieved, which satisfies the objectives of the invention.
  • complexing agents are used in particular hydroxcarboxylic acids, phosphonic acids and organic nitrosulfonic acids.
  • the complexing agents used are multidentate complexing agents. These multidentate complexing agents form chelate complexes with the iron ions and therefore contribute to further increasing the ratio of chromium oxide to iron oxide in the passive layer.
  • suitable complexing agents include, for example, hydroxycarboxylic acids which have 2 or 3 hydroxyl groups and 2 or 3 carboxyl groups or salts thereof.
  • a particularly suitable example of such a hydroxycarboxylic acid is citric acid.
  • Another suitable complexing agent is a diphosphonic acid of the general structure R "[- PO (OH) 2 ] 2 , where R" is a divalent alkyl, hydroxyalkyl or aminoalkyl radical.
  • R is a divalent alkyl, hydroxyalkyl or aminoalkyl radical.
  • R is a divalent alkyl, hydroxyalkyl or aminoalkyl radical.
  • a particularly preferred example of such an acid is 1-hydroxyethane-1,1-diphosphonic acid (HEDP) or its salts.
  • HEDP 1-hydroxyethane-1,1-diphosphonic acid
  • nitrosulphonic acids ie the nitroalkylsulphonic acids, nitroarylsulphonic acids or their salts.
  • a particularly preferred nitroarylsulfonic acid is meta- nitrobenzenesulfonic acid.
  • the acid or the salt has sufficient solubility in the aqueous solution.
  • the carbon chains whether linear, branched, cyclic or aromatic, comprise not more than about 12 carbon atoms, more preferably not more than 10 carbon atoms, and most preferably not more than 6 carbon atoms.
  • oxidizing agent Another essential ingredient of the aqueous solution in the chemical treatment is an oxidizing agent.
  • This oxidizing agent must be sufficient to ensure a normal potential of at least +300 mV in the solution.
  • Suitable oxidizing agents include, for example, nitrates, peroxo compounds, iodates and cerium (IV) compounds in the form of the respective acids or the corresponding water-soluble salts.
  • peroxo compounds are peroxides, persulfates, perborates or else percarboxylates, such as peracetate. These oxidizing agents can be used alone or in the form of mixtures.
  • the term "stainless steel” refers to iron alloys containing at least 13 weight percent chromium. Other corrosion resistance improving elements may be included in the alloy.
  • the chemical treatment according to the invention is not to be confused with a conventional pickling process, in which targeted metal from the surface of a metallic Workpiece is removed (see. DE 92 14 890 U1 EP 0596 273 A , and WO 88/00252 A1 ).
  • the inventors of the present application suspect that the special effect of the method according to the invention is attributable to the fact that a passive layer is not first produced, but an already existing passive layer is changed in its composition and structure by the sequence of the method steps according to the invention. But this is rather a theoretical idea that can not be understood in the sense of a limitation of the present method.
  • the aqueous solutions may also comprise one or more wetting agents which reduce the surface tension of the aqueous solution.
  • suitable wetting agents are, for example, the nitroalkyl or nitroaryl sulfonic acids already described in the case of the complexing agents, or also alkyl glycols of the general structure H- (O-CHR-CH 2 ) n -OH, where R is hydrogen or an alkyl radical having 1, 2 or 3 Is carbon atoms, and n is preferably an integer between 1 and 5, for example 2 or 3; or other wetting agents.
  • the at least one hydroxycarboxylic acid comprises citric acid, and / or the at least one diphosphonic acid HEDP, and / or the at least one nitroaryl or nitroalkyl sulfonic acid m- nitrobenzenesulfonic acid, and / or the at least one alkyl glycol, ethylene glycol and / or butyl glycol, and Oxidizing agent nitrate, peroxide, persulfate and / or cerium (IV) ions, in each case in the weight ratios indicated above.
  • compositions may be added to the above compositions in a concentration between 0.02 and 2.0% by weight, preferably between 0.05 and 1.0% by weight.
  • thickening agents may optionally be added to these compositions. These thickening agents, for example diatomaceous earth, can serve to increase the viscosity of the solution.
  • the chemical treatment in aqueous solution is preferably carried out in a dip bath, so that such thickeners can be dispensed with.
  • the aqueous solution preferably has a pH which is less than 7, preferably less than 4. This can be achieved by the aqueous solution containing at least one acid.
  • a preferred method is that at least one of the complexing agents and / or at least one of the oxidizing agents is at least partially added in the form of an acid to the solution.
  • the first step of the treatment according to the present invention in a preferred embodiment, is in an aqueous solution having a temperature of at most about 70 ° C. It is further preferred that the treatment takes place in aqueous solution at a temperature between room temperature and 60 ° C.
  • the chemical treatment in aqueous solution is preferably carried out over a period of at least 60 minutes, for example, the chemical treatment can be carried out with an aqueous solution over a period of 1-4 hours.
  • the workpiece is rinsed with water, preferably deionized water, to remove the passivating solution, and optionally dried, before the workpiece enters the passivation solution
  • Water preferably deionized water
  • Temperature treatment is subjected. This rinsing can be done by spraying or by (possibly repeated) immersion in a dipping bath or by combinations of these rinsing methods.
  • the step of heat treatment is carried out at a temperature of at least 80 ° C in an oxygen-containing atmosphere.
  • the heat treatment is preferably carried out at a temperature in the range between 80 ° C and 280 ° C, in particular at a temperature above 100 ° C and at most 260 ° C.
  • the oxygen-containing atmosphere of the thermal treatment may be air in a preferred embodiment.
  • the oxygen-containing atmosphere is primarily water vapor or a mixture of water vapor and air.
  • Such a steam-containing atmosphere is preferably used at a temperature of at least 100 ° C.
  • the optimum temperature range for the heat treatment depends essentially on the type of stainless steel to be treated. However, this optimum range can easily be determined by a person of ordinary skill in trial experiments.
  • a suitable temperature in a range between 100 ° C and 270 ° C, preferably between 150 ° C and 260 ° C, in particular between 220 ° C and 260 ° C, when the stainless steel is an austenitic steel having a content of about 16-20 wt .-% chromium and about 7-10 wt .-% nickel, such as stainless steel grade 1.4301 (see. FIG. 1 ).
  • the term "essentially none" means that the elements in question, if present at all, are present in a concentration of less than 1% by weight, generally between 0 and 0.1% by weight, in the alloy.
  • This heat treatment should take place over a period of at least 2 minutes (cf. FIG. 3 for quality 1.4301 stainless steel). Preferably, the heat treatment takes place over a period of 15-45 minutes, for example for about 30 minutes. Depending on the quality of the stainless steel, too long a thermal treatment, for example over several hours, can lead to a fall in the corrosion resistance of the treated workpiece.
  • a stainless steel of quality 1.4016 when heated to 140 ° C, ie at a temperature which is in the optimum range for the heat treatment first shows a rapid increase in the pitting potential to values around +1000 mV (cf. FIG. 4 ). However, if such a workpiece is exposed to this temperature for longer periods, the pitting potential drops again to values of about +700 mV. It is therefore important for some types of stainless steel that the heat treatment is carried out no longer than about 90 minutes, preferably not longer than about 60 minutes.
  • Another important advantage of the method described here is that it is not only suitable for significantly increasing the corrosion resistance, measured as the pitting potential according to DIN 50900, compared with the starting state, but that the method is also suitable for the resistance of stainless steel workpieces to increase thermal discoloration.
  • Such an increase in the resistance of stainless steel workpieces or their surfaces against thermal discoloration in their use by a passivation process has not been described and represents a further significant advantage of the invention described herein.
  • the prior art discloses, inter alia, also a method for cleaning and passivating a stainless steel surface, in which a hydroxyacetic acid or citric acid is applied to the surface in an aqueous solution (cf. EP 0 776 256 B1 ).
  • a hydroxyacetic acid or citric acid is applied to the surface in an aqueous solution
  • the content of hydroxycarboxylic acid in this process is well below 3.0 wt .-%.
  • the complexes used easily precipitate and are incorporated into the oxide film over the workpiece (see. Paragraph [0032] of the aforementioned EP 0 776 256 B1 ).
  • Example 1 Stainless steel of quality 1.4301
  • the chemical treatment was carried out at 40 ° C for 180 min. Subsequently, the sheet was rinsed with deionized water and dried in air.
  • the pitting potential of plate B was measured at +750 mV, an increase of +200 mV compared to the initial state.
  • sheet D was treated in a passivation solution whose composition is described in Example 1. The treatment takes place at room temperature (+ 22 ° C) for a duration of 2.5 h. Subsequently, the plate was rinsed clean with deionized water, dried in air and the pitting potential measured at +520 mV, an increase from the initial state by +150 mV.
  • this example shows that when exceeding the optimal temperature range for a certain quality stainless steel corrosion resistance decreases again, but still higher than before the passivation treatment.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
EP08715970A 2007-03-05 2008-02-22 Verfahren zum thermochemischen passivieren von edelstahl Active EP2147131B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL08715970T PL2147131T3 (pl) 2007-03-05 2008-02-22 Sposób termochemicznej pasywacji stali szlachetnej

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102007010538A DE102007010538A1 (de) 2007-03-05 2007-03-05 Verfahren zum thermochemischen Passivieren von Edelstahl
PCT/EP2008/001419 WO2008107082A1 (de) 2007-03-05 2008-02-22 Verfahren zum thermochemischen passivieren von edelstahl

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EP2147131A1 EP2147131A1 (de) 2010-01-27
EP2147131B1 true EP2147131B1 (de) 2011-08-17

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US (1) US8430973B2 (pl)
EP (1) EP2147131B1 (pl)
JP (1) JP5222308B2 (pl)
AT (1) ATE520802T1 (pl)
DE (1) DE102007010538A1 (pl)
ES (1) ES2370088T3 (pl)
PL (1) PL2147131T3 (pl)
WO (1) WO2008107082A1 (pl)

Cited By (1)

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DE102014203412A1 (de) 2013-02-25 2014-08-28 Zschimmer & Schwarz Mohsdorf GmbH &Co.KG. Verfahren und Formulierung zur gleichzeitigen Entschichtung und Passivierung von Edelstahloberflächen

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US8906579B2 (en) * 2009-05-14 2014-12-09 GM Global Technology Operations LLC Low contact resistance coated stainless steel bipolar plates for fuel cells
EP2617866A1 (de) 2012-01-23 2013-07-24 Merz Pharma GmbH & Co. KGaA Verfahren und Zusammensetzung zur Aufbereitung medizinischer Instrumente
DE102012107807A1 (de) * 2012-08-24 2014-02-27 Paul Hettich Gmbh & Co. Kg Verfahren zur Herstellung eines metallischen Bauteils eines Beschlages, Ofenbeschlag und Ofen mit Pyrolysereinigungsfunktion
CN103225087B (zh) * 2013-04-26 2015-04-01 河南师范大学 一种不锈钢酸洗钝化膏及其制备方法
US20160310984A1 (en) * 2013-12-18 2016-10-27 Poligrat Gmbh Method for the production of colored stainless steel surfaces
US9202483B1 (en) * 2015-01-02 2015-12-01 HGST Netherlands B.V. Iron-oxidized hard disk drive enclosure cover
EP3162558A1 (en) 2015-10-30 2017-05-03 Outokumpu Oyj Component made of metallic composite material and method for the manufacture of the component by hot forming
CN106637175B (zh) * 2016-11-09 2019-02-22 深圳市麦滕医疗器械有限公司 外科手术器械用马氏体型抗菌不锈钢的表面钝化处理方法
US10683576B2 (en) * 2017-03-27 2020-06-16 Baker Hughes, A Ge Company, Llc Corrosion inhibitors for passivation of galvanized coatings and carbon steel
JP7299012B2 (ja) * 2018-12-17 2023-06-27 株式会社Ｉｈｉインフラシステム 不動態化処理方法、不動態化処理液及び不動態化処理容器
CN114086189B (zh) * 2021-11-24 2024-03-08 宁波吉海金属科技有限公司 一种环保型不锈钢酸洗钝化液

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Publication number Priority date Publication date Assignee Title
DE102014203412A1 (de) 2013-02-25 2014-08-28 Zschimmer & Schwarz Mohsdorf GmbH &Co.KG. Verfahren und Formulierung zur gleichzeitigen Entschichtung und Passivierung von Edelstahloberflächen

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US20100132844A1 (en) 2010-06-03
ES2370088T3 (es) 2011-12-12
JP2010521581A (ja) 2010-06-24
ATE520802T1 (de) 2011-09-15
JP5222308B2 (ja) 2013-06-26
WO2008107082A8 (de) 2008-11-20
US8430973B2 (en) 2013-04-30
DE102007010538A1 (de) 2008-09-11
PL2147131T3 (pl) 2012-01-31
EP2147131A1 (de) 2010-01-27
WO2008107082A1 (de) 2008-09-12

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