EP1022357B1 - Procédé de traitement de surfaces d'aciers inoxydables - Google Patents

Procédé de traitement de surfaces d'aciers inoxydables Download PDF

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Publication number
EP1022357B1
EP1022357B1 EP00101186A EP00101186A EP1022357B1 EP 1022357 B1 EP1022357 B1 EP 1022357B1 EP 00101186 A EP00101186 A EP 00101186A EP 00101186 A EP00101186 A EP 00101186A EP 1022357 B1 EP1022357 B1 EP 1022357B1
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EP
European Patent Office
Prior art keywords
acid
steel
liquid bath
mineral
carried out
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.)
Expired - Lifetime
Application number
EP00101186A
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German (de)
English (en)
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EP1022357A1 (fr
Inventor
Angel Rodriguez Castanedo
Jürgen Salomon
Gerhard Schmidmayer
Bernhard Walter
Frank Dr. Jördens
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.)
BSH Hausgeraete GmbH
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BSH Bosch und Siemens Hausgeraete GmbH
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Publication of EP1022357A1 publication Critical patent/EP1022357A1/fr
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Publication of EP1022357B1 publication Critical patent/EP1022357B1/fr
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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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; 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
    • C23F15/00—Other methods of preventing corrosion or incrustation
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/08—Iron or steel
    • C23G1/083—Iron or steel solutions containing H3PO4

Definitions

  • the present invention is in the field of steels and Machining or treatment of steels, preferably for the production of Devices e.g. are intended for home use.
  • the present invention such devices and parts or their treatment that the Exposed to heat.
  • the present invention provides a method of treatment of stainless steel available for these applications are intended, the treatment of the invention Steels prevent their yellowing from occurring during daily use.
  • JP-A 52 64 045 This includes the 5-step process described in JP-A 52 64 045, where the surface of the steel is first sandblasted, then in an etchant such as HF, salt, saltpetre or Phosphoric acid immersed, then coated with a resin film and heated is so that the film adheres to the surface in cured form.
  • the JP-A 61 06 693 describes another method which is a sandblast treatment of the steel to make its surface more corrosion resistant do. This process is also followed by an immersion of the steel in a mineral acid before applying a resin layer.
  • Another one Process for the treatment of stainless steel a so-called Chromating process is described in JP-A 52 145 346. Doing so The surface is film-coated by immersing the steel in a hot one aqueous solution containing sulfuric acid, oxidizing agents e.g. based on chrome (such as potassium dichromate) and phosphoric acid.
  • Vollmer et al. (Materials and Corrosion, 46 , 92-97 (1995)) describes a surface treatment process for stainless steels, in which samples are stored in an oven at 600 ° C in order to obtain a uniform oxide layer covering the entire surface. To remove the oxide layer, the samples are treated with non-liquid pickling pastes, which after an exposure time under running water are brushed off together with the oxide layer. Since the thickness of the oxide layer formed on the steel surface depends on the operating temperature during the oxidation, a relatively thick passive layer with a high chromium content protecting against corrosion is formed at the described operating temperature of 600 ° C. after removal of the oxide layer.
  • this passive layer changes the original surface structure of the stainless steel, so that the steel surface is usefully not given a special surface structure (for example a brush cut) before the surface treatment, since this changes optically after the surface treatment has been carried out.
  • US 5,269,957 describes a rust removing agent for stainless surfaces Steel made from phosphoric acid, a polyhydroxymonocarboxylic acid (or one of its salts) and a surfactant.
  • JP-A 62 124 019 discloses a bath for immersing steels at elevated heights Temperatures. This bath is based on an aqueous solution of phosphoric acid, Nitric acid (or nitrate) and an amine group inhibitor.
  • US 4,078,949 describes a method of machining stainless steel surfaces, to e.g. Remove oxides. This is done by heating the steel to a specific one Oxygen potential.
  • JP-A 07 286 215 discloses a method to improve the corrosion resistance of To improve ferrite steels. Two process steps involve exposing the steel (i) compared to a hydrogen or (ii) a hydrogen / nitrogen atmosphere.
  • the object of the present invention is accordingly to provide a simple method by means of which Stainless steel surface resistant to dirt and Discoloration (yellowing) can be made.
  • This procedure includes treatment of the steel with mineral acids, preferably phosphoric acid, especially with aqueous phosphoric acid, the presence of one or of several surfactants is preferred.
  • mineral acids preferably phosphoric acid, especially with aqueous phosphoric acid
  • phosphoric acid particularly suitable as phosphoric acid for the process according to the invention FINOX® DH ISO 9002.
  • concentration of the aqueous phosphoric acid is preferably included 50% (v / v) or less, concentrations in the range are particularly preferred of 25, 30, 35, 40 and 45% (v / v).
  • This steel treatment process according to the invention should generally be carried out beforehand the use of steel in the manufacturing chain of equipment or parts respectively. In any case, this procedure achieves that later Discoloration (yellowing) of the steel can be prevented.
  • the method according to the invention does not require a large outlay on equipment and without sandblasting and coatings of any kind (e.g. with Resins and other polymers).
  • the present invention thus relates to a method for Surface treatment of stainless steels, which is particularly suitable To prevent yellowing after the steel has been exposed to heat.
  • the heated steel becomes immediate immersed in the liquid bath after step (a) (step (b)), i.e. without previous Cooling of the steel.
  • step (a) steel cooled to room temperature or slightly above (30-55 ° C) after immersing it in a hot mineral, preferably phosphoric acid (Temperature greater than approx. 50 ° C, preferably greater than 80 ° C), resistant to Yellowing is or will be.
  • a hot mineral preferably phosphoric acid (Temperature greater than approx. 50 ° C, preferably greater than 80 ° C)
  • a particularly preferred phosphoric acid in step (b) is an aqueous one Phosphoric acid mixed with surfactants such as FINOX® DH ISO 9002.
  • surfactants such as FINOX® DH ISO 9002.
  • the use of a 33% (v / v) aqueous is particularly preferred Solution of FINOX® DH ISO 9002 (Chimiderouil Productos Tamosa, S.A.).
  • FINOX® DH eliminates ISO 9002 by immersion, circulation, Sprinkling or other application of greasy contaminants from Surfaces. It also enables the deoxidation of numerous metals (i.e. the Removal of oxide layers or derusting) such as the carbon and Cast steels, stainless ferritic and martensitic steels, des Aluminum and copper and their two alloys.
  • step (b) is preferably carried out over a period of 1-10 min, preferably 2-8 min, particularly preferably 3-6 min. Another a particularly preferred embodiment provides for a duration of about 5 minutes Step (b) above.
  • Other preferred mineral acids required for the liquid bath in step (b) Can be used are hydrochloric acid, nitric acid, sulfuric acid, chloric acid, Perchloric acid, bromic acid, perbromic acid, iodic acid, periodic acid, Silica, tungstic acid, 12-tungstosilicic acid, 12-tungstophosphoric acid or a mixture of two or more of these or other mineral acids.
  • steps (c) and (d) are to remove any rest of the liquid bath Remove step (b) completely. Otherwise there is the, albeit minor, Possibility of streaked or grained during finishing Form surfaces, making the end product less aesthetically acceptable would.
  • the temperature of the air flow in step (d) is usually 50-150 ° C, in particular at 70-130 ° C or at 80-120 ° C, particularly preferably at 90-110 ° C or at 95-105 ° C, with a temperature of 100 ° C especially suitable is.
  • This treatment prevents the user from using his device subject to mechanical or chemical abrasion to eliminate yellowed surfaces.
  • the result of this is damage of the steel parts and the risk to the user when using them resulting from such aggressive chemical products can be avoided.
  • the device comprises a zone 5 of the entry of water into a cooling and rinsing circuit (shown in Fig. 1 by a line "-----"), a zone of separation 7 between the water and the liquid bath which reprocesses the water from zone 6 for the cooling and rinsing cycle and the separated phosphoric acid 9 in the steam cycle (shown in Fig. 1 by a line "----") for recovery and reprocessing it is fed.
  • This steam cycle also includes a zone for cooling 11, which is common to the cooling and rinsing circuit, and a zone 10 for collecting vapors, which allows the Phosphoric acid attributed to the treatment 2 bath.
  • FIG. 1 In accordance with a preferred embodiment of FIG Invention to be treated stainless steel plates through the zone 8 inserted in the oven 1, where they are heated to 300-400 ° C before be led into bath 2 for a period of 4.5 minutes, the one Contains 33% (v / v) solution of FINOX® DH ISO 9002 in water.
  • the plates are then guided into the rinsing tub 3, where they are one Be rinsed with water by sprinkling. From there they will into a drying chamber with hot air at 105 ⁇ 5 ° C. In connection the plates are then sent into the assembly chain to continue with Continue normal procedures to manufacture the appropriate device.
  • the device From the point of view of environmental protection, the device has how already stated above, via a circuit for reprocessing the Water and phosphoric acid and their return to the system. In addition to saving water and treatment product Avoid waste products that are harmful to the environment.
  • the present invention is further illustrated by the following example shown that in no way intends to limit their reach.
  • the panels to be treated were introduced through zone 8 into oven 1 where they were heated to 375 ° C. After this step, they were in the liquid bath led, which contained the 33% (v / v) solution of FINOX® DH ISO 9002, where they remained for 4.5 minutes. Then they were put in rinsing tub 3, where they have been irrigated with water. Of there they were led into a drying chamber with hot air at 105 ⁇ 5 ° C, from where they were sent to the assembly chain to match the normal Proceed with the processing of the plates to manufacture the equipment.

Claims (12)

  1. Procédé de traitement d'aciers inoxydables, qui comprend les étapes suivantes :
    a) oxydation de la surface de l'acier par chauffage dans un four, et
    b) élimination de la couche d'oxyde, et
    caractérisé en ce que l'oxydation se réalise par échauffement de l'acier à une température de 300 à 400°C et l'élimination de la couche d'oxyde se réalise par immersion de l'acier dans un bain liquide à base d'acide minéral.
  2. Procédé selon la revendication 1, caractérisé en ce que l'acide minéral est un acide phosphorique.
  3. Procédé selon la revendication 2, caractérisé en ce que l'acide minéral est une solution aqueuse d'acide phosphorique.
  4. Procédé selon la revendication 1, caractérisé en ce que, l'acide minéral est l'acide chlorhydrique, l'acide nitrique, l'acide sulfurique, l'acide chlorique, l'acide perchlorique, l'acide bromique, l'acide perbromique, l'acide iodique, l'acide periodique, l'acide silicique, l'acide tungstique, l'acide 12-tungstato-silicique, l'acide 12-tungstato-phosphorique ou un mélange de deux ou plusieurs de ceux-ci ou d'autres acides minéraux.
  5. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le traitement dans l'étape (b) se réalise pendant une durée de 1 à 10 minutes.
  6. Procédé selon la revendication 5, caractérisé en ce que, le traitement dans l'étape (b) se réalise pendant une durée d'environ 5 minutes.
  7. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que le bain liquide contient outre un acide minéral, également une ou plusieurs substances tensio-actives (tensio-actifs).
  8. Procédé selon la revendication 7, caractérisé en ce que le bain liquide de l'étape (b) contient FINOX® DH ISO 9002, en particulier une solution aqueuse de FINOX® DH ISO 9002 à 33% (v/v).
  9. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que l'acier chauffé est immergé directement après l'étape (a) à savoir sans refroidissement préalable de l'acier, dans le bain liquide, ou bien que l'acier chauffé parvient à se refroidir à une température de 20 à 55°C, puis il est immergé dans un bain liquide chauffé à > 50°C.
  10. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que les étapes (c) et/ou (d) supplémentaires font suite aux étapes (a) et (b) :
    c) rinçage de l'acier traité, par de l'eau; et
    d) séchage de l'acier rincé, en particulier au moyen d'un courant d'air.
  11. Procédé selon l'une quelconque des revendications précédentes, caractérisé en ce que la température du courant d'air dans l'étape (d) est autour de 50 à 150°C.
  12. Procédé selon la revendication 11, caractérisé en ce que la température du courant d'air est autour de 90 à 110°C ou de 95 à 105°C.
EP00101186A 1999-01-22 2000-01-21 Procédé de traitement de surfaces d'aciers inoxydables Expired - Lifetime EP1022357B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ES9900126 1999-01-22
ES009900126A ES2162546B1 (es) 1999-01-22 1999-01-22 Metodo e instalacion para el tratamiento superficial del acero inoxidable.

Publications (2)

Publication Number Publication Date
EP1022357A1 EP1022357A1 (fr) 2000-07-26
EP1022357B1 true EP1022357B1 (fr) 2004-06-30

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EP00101186A Expired - Lifetime EP1022357B1 (fr) 1999-01-22 2000-01-21 Procédé de traitement de surfaces d'aciers inoxydables

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EP (1) EP1022357B1 (fr)
AT (1) ATE270353T1 (fr)
DE (1) DE50006912D1 (fr)
ES (2) ES2162546B1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10064134A1 (de) * 2000-12-19 2002-06-27 Bsh Bosch Siemens Hausgeraete Verfahren zum Veredeln von metallischen Oberflächen zur Vermeidung von thermischen Anlauf-Farben
CN106835162B (zh) * 2017-02-14 2020-05-08 江苏金环球建设有限公司 一种不锈钢表面锈迹的清除方法

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE763760A (fr) * 1971-03-03 1971-09-03 Centre Rech Metallurgique Procede pour ameliorer la resistance a la corrosion d'aciers inoxydables.
US4078949A (en) * 1976-09-02 1978-03-14 United States Steel Corporation Method for improving the surface quality of stainless steels and other chromium-bearing iron alloys
JPS6233785A (ja) * 1985-08-02 1987-02-13 Honda Motor Co Ltd 鋼材の塗装前処理方法
JPS62124019A (ja) * 1985-11-22 1987-06-05 Ishikawajima Harima Heavy Ind Co Ltd 鋼材のスケ−ル除去方法
JP3052213B2 (ja) * 1991-02-18 2000-06-12 タイホー工業株式会社 ステンレス鋼表面の錆除去剤
US5279707A (en) * 1992-10-23 1994-01-18 Time Savers Die discoloration remover solution and method
JP3073370B2 (ja) * 1993-08-20 2000-08-07 三菱重工業株式会社 鉄鋼表面の塗装下地処理剤
JPH07286215A (ja) * 1994-04-19 1995-10-31 Kawasaki Steel Corp ステンレス鋼板の製造方法
WO1998036044A1 (fr) * 1997-02-13 1998-08-20 Crown Technology, Inc. Adjuvant de rinçage pour acier inoxydable et procede afferent

Also Published As

Publication number Publication date
ES2162546A1 (es) 2001-12-16
EP1022357A1 (fr) 2000-07-26
ES2162546B1 (es) 2003-05-01
ES2223321T3 (es) 2005-03-01
ATE270353T1 (de) 2004-07-15
DE50006912D1 (de) 2004-08-05

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