EP0770707A1 - Process for producing cold-rolled strip continuously - Google Patents

Process for producing cold-rolled strip continuously Download PDF

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Publication number
EP0770707A1
EP0770707A1 EP96113439A EP96113439A EP0770707A1 EP 0770707 A1 EP0770707 A1 EP 0770707A1 EP 96113439 A EP96113439 A EP 96113439A EP 96113439 A EP96113439 A EP 96113439A EP 0770707 A1 EP0770707 A1 EP 0770707A1
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EP
European Patent Office
Prior art keywords
pickling
strip
carried out
acid
free
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Granted
Application number
EP96113439A
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German (de)
French (fr)
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EP0770707B1 (en
Inventor
Heinz Dipl.-Ing. Berger
Rolf Dipl.-Ing. Noé
Frank Bärhold
Jörg Dr. Neumann
Andreas Dr. mont. Noé
Ralf Waldmann
Bodo Dr. Block
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BWG Bergwerk und Walzwerk Maschinenbau GmbH
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BWG Bergwerk und Walzwerk Maschinenbau GmbH
Keramchemie GmbH
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • B21B45/04—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for de-scaling, e.g. by brushing
    • B21B45/06—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for de-scaling, e.g. by brushing of strip material
    • 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
    • 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
    • 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
    • C23G1/081—Iron or steel solutions containing H2SO4
    • 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
    • C23G1/085—Iron or steel solutions containing HNO3
    • 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
    • C23G1/086—Iron or steel solutions containing HF
    • 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
    • C23G1/10—Other heavy metals
    • C23G1/106—Other heavy metals refractory metals
    • 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
    • C23G3/00—Apparatus for cleaning or pickling metallic material
    • C23G3/02—Apparatus for cleaning or pickling metallic material for cleaning wires, strips, filaments continuously
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
    • B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
    • B21B1/24—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process
    • B21B1/28—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length in a continuous or semi-continuous process by cold-rolling, e.g. Steckel cold mill
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
    • B21B3/02—Rolling special iron alloys, e.g. stainless steel

Definitions

  • the invention relates to a method for producing a cold-rolled strip from a non-rusting, ferritic or austenitic stainless steel or a titanium alloy, in which in stainless steel or a titanium alloy, in which in one pass a one produced by a hot rolling or casting process and a bundle wound strip is unwound and, if necessary, mechanically descaled, then chemically and / or electrochemically pre-pickled, then cold-rolled to finished dimensions, optionally degreased, annealed, finished pickled and, if necessary, passivated, dressed and stretch-straightened.
  • a relatively thick strip is first produced by a hot rolling process, which is wound up into a bundle after the hot rolling process. This bundle is then transported to another processing point, where it is unwound, annealed, possibly mechanically descaled and pickled.
  • Mechanical descaling mainly consists of a blasting and brushing process, whereby the belt can run through several pairs of brushes.
  • the strip that has not yet been finished is then pickled in one or more baths with different pickling solutions, for example sulfuric acid.
  • the pickled, not yet finished strip is then rewound into a bundle, which is then, again from another processing point, rolled through a cold rolling process to the finished thickness suitable for the finished product. Even after the cold rolling process, the finished strip is rewound into a bundle. This bundle is then - again at another processing point - degreased, annealed and pickled, whereby for economic reasons the same pickling system and thus the same pickling solution as in the treatment of the hot strip is usually used. If necessary, the strip can be passivated, trained and stretch-straightened after the last pickling process.
  • the strip wound on a bundle is unwound and mechanically descaled, cold-rolled, degreased, annealed, pickled and, if necessary, passivated, treated and stretch-straightened.
  • pickling before cold rolling should also be dispensed with, and sufficient blasting and brushing should be used to achieve a surface quality of the strip before cold rolling, which, after the further treatment and processing steps, achieves the specified quality of the finished product Band.
  • the invention is therefore based on the object of demonstrating a method for producing a strip which can be processed into finished products from a stainless steel or a titanium alloy, in which, while maintaining the advantages shown, a so-called integrated line - the strip is chemically and / or electrochemically in one pass Pre-pickled, cold-rolled to the finished size, possibly degreased, annealed, finished pickled and, if necessary, passivated, trained and stretch-straightened - it is excluded that there are any stains on the finished strip that render it unusable.
  • the pickling is carried out by means of a pickling solution containing salt, sulfur and / or nitric acid.
  • the tape is freed from the scale to such an extent that a perfect quality of the finished product or of the finished tape is ensured.
  • the pretreatment can be matched to the final stain in a special way. It is possible to use a different pickling solution or pickling solution combination for the so-called pre-pickling than for the so-called final pickling, so that an optimal pickling result is achieved in a particularly economical manner.
  • the process diagram of a system for producing a strip of stainless steel that can be processed into finished products is shown, in which the strip produced by a rolling process is first wound into a bundle 1, from which it is now unwound again. It is possible to first pass the strip 2 through a descaling unit 3, in which the strip 2 is blasted and brushed.
  • This descaling unit 3 can be of relatively simple design and can even be omitted if necessary.
  • the strip 2 arrives in a pickling device 4, which consists of at least one pickling tank with a pickling solution and which forms the so-called pre-pickling.
  • the pickling device 4 is followed by at least one cold rolling stand 5 in which the strip 2 is reduced to the desired thickness. Then the cold-rolled strip is passed through a Degreasing system 6 and an annealing system 7 performed and then arrives at a further pickling device 8, which consists of at least two flat containers. Here the strip 2 is finish-stained in the usual way. Thereafter, the band 2 is passivated, trained and straightened in a unit 9 as required.
  • samples were also treated with a pickling solution containing nitric acid, which contained about 20% free nitric acid and about 30 g / l free iron.
  • the temperature of the pickling solution was about 60 ° C and the pickling time was about 30 seconds.
  • the nitric acid-containing pickling solution was injected once in these samples, while turbulence was generated in the pickling solution for other samples.
  • the samples had a slightly lightened surface on which, however, scale residues could still be seen. However, these scale residues do not adversely affect the subsequent treatments. After the final pickling, a scale-free, shiny surface was also found.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Laminated Bodies (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
  • Heat Treatment Of Sheet Steel (AREA)

Abstract

A strip of stainless, ferritic or austenitic steel or a titanium alloy produced by hot-rolling or casting is uncoiled and (if required) mechanically descaled. This is followed by chemical and/or electrochemical preliminary pickling, and concluded by cold-rolling to finish dimensions, with possible degreasing, annealing, finish-pickling, passivation, finishing and stretch-straightening. The method is characterised by the fact that preliminary pickling takes place with a solution containing hydrochloric, sulphuric and/or nitric acid.

Description

Die Erfindung bezieht sich auf ein Verfahren zur Herstellung eines kaltgewalzten Bandes aus einem nicht rostenden, ferritischen oder austenitischen Edelstahl oder einer Titanlegierung, bei dem in Edelstahl oder einer Titanlegierung, bei dem in einem Durchlauf ein durch einen Warmwalz- oder Gießvorgang hergestelltes und zu einem Bund gewickeltes Band abgewickelt und bedarfsweise mechanisch entzundert, dann chemisch und/oder elektrochemisch vorgebeizt, anschließend auf Fertigmaß kaltgewalzt, gegebenenfalls entfettet, geglüht, fertig gebeizt und bedarfsweise noch passiviert, dressiert und streckgerichtet wird.The invention relates to a method for producing a cold-rolled strip from a non-rusting, ferritic or austenitic stainless steel or a titanium alloy, in which in stainless steel or a titanium alloy, in which in one pass a one produced by a hot rolling or casting process and a bundle wound strip is unwound and, if necessary, mechanically descaled, then chemically and / or electrochemically pre-pickled, then cold-rolled to finished dimensions, optionally degreased, annealed, finished pickled and, if necessary, passivated, dressed and stretch-straightened.

Bei der Herstellung eines Bandes aus Edelstahl, welches anschließend zu Fertigprodukten verarbeitet wird, wird zunächst durch einen Warmwalzvorgang ein verhältnismäßig dickes Band erzeugt, welches nach dem Warmwalzvorgang zu einem Bund aufgewickelt wird. Dieses Bund wird dann zu einer anderen Verarbeitungsstelle transportiert, in der es abgewickelt, geglüht, eventuell mechanisch entzundert und gebeizt wird. Das mechanische Entzundern besteht dabei hauptsächlich aus einem Strahl- und Bürstvorgang, wobei das Band mehrere Bürstenpaare durchlaufen kann. Das Beizen des noch nicht fertigen Bandes erfolgt dann, je nach Werkstoffqualität, in einem Bad oder in mehreren Bädern mit unterschiedlicher Beizlösung, beispielsweise Schwefelsäure, Flußsäure mit Zusätzen ohne Salpetersäure, Mischsäure (Flußsäure-Salpetersäuregemisch) oder in elektrolytischen Bädern mittels Schwefelsäure oder eines neutralen Salzes. Anschließend wird das gebeizte, noch nicht fertige Band wieder zu einem Bund aufgewickelt, welches dann, ebenfalls wieder von einer anderen Verarbeitungsstelle, durch einen Kaltwalzvorgang auf die fertige, für das Fertigprodukt geeignete Dicke gewalzt wird. Auch nach dem Kaltwalzvorgang wird das nun fertige Band wieder zu einem Bund aufgewickelt. Dieses Bund wird dann - wieder an einer anderen Verarbeitungsstelle - entfettet, geglüht und gebeizt, wobei hier aus wirtschaftlichen Gründen meist die gleiche Beizanlage und damit die gleiche Beizlösung wie bei der Behandlung des Warmbandes verwendet wird. Gegebenenfalls kann nach dem letzten Beizvorgang das Band noch passiviert, dressiert und streckgerichtet werden.In the manufacture of a strip made of stainless steel, which is subsequently processed into finished products, a relatively thick strip is first produced by a hot rolling process, which is wound up into a bundle after the hot rolling process. This bundle is then transported to another processing point, where it is unwound, annealed, possibly mechanically descaled and pickled. Mechanical descaling mainly consists of a blasting and brushing process, whereby the belt can run through several pairs of brushes. Depending on the material quality, the strip that has not yet been finished is then pickled in one or more baths with different pickling solutions, for example sulfuric acid. Hydrofluoric acid with additives without nitric acid, mixed acid (hydrofluoric acid-nitric acid mixture) or in electrolytic baths using sulfuric acid or a neutral salt. The pickled, not yet finished strip is then rewound into a bundle, which is then, again from another processing point, rolled through a cold rolling process to the finished thickness suitable for the finished product. Even after the cold rolling process, the finished strip is rewound into a bundle. This bundle is then - again at another processing point - degreased, annealed and pickled, whereby for economic reasons the same pickling system and thus the same pickling solution as in the treatment of the hot strip is usually used. If necessary, the strip can be passivated, trained and stretch-straightened after the last pickling process.

Um das unnötige und vor allem Dingen zeitraubende Ab- und Aufwickeln des Bandes zu vermeiden, wurde vorgeschlagen, mehrere Behandlungsstufen in einem Durchlauf hintereinander zusammenzufassen. Gemäß diesem Vorschlag wird das auf einem Bund gewickelte Band abgewickelt und in einem Durchlauf mechanisch entzundert, kaltgewalzt, entfettet, geglüht, gebeizt und gegebenenfalls noch passiviert, dressiert und streckgerichtet. Durch ein solches Verfahren entfallen unnötige Abwickel- und Aufwickelvorgänge. Ebenso soll auch auf das Beizen vor dem Kaltwalzen verzichtet und durch ausreichendes Strahlen und Bürsten eine Oberflächenqualität des Bandes vor dem Kaltwalzen erreicht werden, die nach den weiteren Behandlungs- und Bearbeitungsschritten die Erreichung einer spezifikationsgerechten Qualität des fertigen Bandes sicherstellt. Dazu werden Strahlanlagen und mehrwellige Bürstmaschinen verwendet, die einen verhältnismäßig hohen Aufwand erfordern. Trotz dieses hohen Aufwandes ist jedoch nicht gänzlich auszuschließen, daß auf dem durch einen Kaltwalzvorgang zu bearbeitenden Band Restzunder verbleibt, der sich nachteilig auf das Fertigprodukt auswirkt.In order to avoid the unnecessary and, above all, time-consuming unwinding and winding of the tape, it has been proposed to combine several treatment stages in a single pass. According to this proposal, the strip wound on a bundle is unwound and mechanically descaled, cold-rolled, degreased, annealed, pickled and, if necessary, passivated, treated and stretch-straightened. Such a process eliminates unnecessary unwinding and winding operations. Likewise, pickling before cold rolling should also be dispensed with, and sufficient blasting and brushing should be used to achieve a surface quality of the strip before cold rolling, which, after the further treatment and processing steps, achieves the specified quality of the finished product Band. Blasting systems and multi-shaft brushing machines are used for this, which require a relatively high outlay. Despite this great effort, it cannot be entirely ruled out that residual scale remains on the strip to be processed by a cold rolling process, which has a disadvantageous effect on the finished product.

Um diesen Restzunder auszuschließen, wurde ferner vorgeschlagen, vor dem Kaltwalzvorgang eine Vorbeizung durchzuführen, die in gleicher Weise wie das Beizen des warmgewalzten Bandes mittels einer Mischsäure durchgeführt wird. Diesbezügliche Versuche haben jedoch ergeben, daß das Band nach der Vorbeize zwar sauber ist, nach dem Fertigbeizen aber Flecken aufweist, die das Band für eine weitere Verarbeitung unbrauchbar macht.In order to exclude this residual scale, it was further proposed to carry out a pre-pickling before the cold rolling process, which is carried out in the same way as the pickling of the hot-rolled strip using a mixed acid. Experiments in this regard, however, have shown that the strip is clean after the pickling, but has stains after the finished pickling, which makes the strip unusable for further processing.

Dre Erfindung liegt deshalb die Aufgabe zugrunde, ein Verfahren zur Herstellung eines zu Fertigprodukten verarbeitbaren Bandes aus einem nicht rostenden Edelstahl oder einer Titanlegierung aufzuzeigen, bei dem unter Beibehaltung der aufgezeigten Vorteile einer sogenannten integrierten Linie - das Band wird in einem Durchlauf chemisch und/oder elektrochemisch vorgebeizt, auf Fertigmaß kaltgewalzt, gegebenenfalls entfettet, geglüht, fertig gebeizt und bedarfsweise noch passiviert, dressiert und streckgerichtet - ausgeschlossen ist, daß auf dem fertig behandelten Band noch irgendwelche Flecken sind, die dasselbe unbrauchbar machen.The invention is therefore based on the object of demonstrating a method for producing a strip which can be processed into finished products from a stainless steel or a titanium alloy, in which, while maintaining the advantages shown, a so-called integrated line - the strip is chemically and / or electrochemically in one pass Pre-pickled, cold-rolled to the finished size, possibly degreased, annealed, finished pickled and, if necessary, passivated, trained and stretch-straightened - it is excluded that there are any stains on the finished strip that render it unusable.

Zur Lösung dieser Aufgabe wird gemäß der Erfindung bei einem Verfahren der eingangs beschriebenen Gattung vorgeschlagen, daß das Vorbeizen mittels einer salz-, schwefel- und/oder salpetersäurehaltigen Beizlösung durchgeführt wird.To achieve this object, it is proposed according to the invention in a method of the type described in the introduction that the pickling is carried out by means of a pickling solution containing salt, sulfur and / or nitric acid.

Durch eine derartige Vorbeizung wird das Band so weit vom Zunder befreit, daß eine einwandfreie Qualität des Fertigproduktes bzw. des fertig behandelten Bandes sichergestellt ist. Dabei kann die Vorbeizung in besondere Weise auf die Endbeize abgestimmt werden. Dabei ist es möglich, für das sogenannte Vorbeizen eine andere Beizlösung bzw. Beizlösungs-Kombination als für das sogenannte Endbeizen zu verwenden, so daß in besonders wirtschaftlicher Weise ein optimales Beizergebnis erzielt wird.By means of such a pre-treatment, the tape is freed from the scale to such an extent that a perfect quality of the finished product or of the finished tape is ensured. The pretreatment can be matched to the final stain in a special way. It is possible to use a different pickling solution or pickling solution combination for the so-called pre-pickling than for the so-called final pickling, so that an optimal pickling result is achieved in a particularly economical manner.

Weitere Merkmale eines Verfahrens gemäß der Erfindung sind in den Ansprüchen 2 bis 15 offenbart.Further features of a method according to the invention are disclosed in claims 2 to 15.

Die Erfindung wird nachfolgend anhand von Ausführungsbeispielen und einer Zeichnung näher erläutert.The invention is explained in more detail below with the aid of exemplary embodiments and a drawing.

In dieser Zeichnung ist das Verfahrensschema einer Anlage zur Herstellung eines zu Fertigprodukten verarbeitbaren Bandes aus Edelstahl gezeigt, bei dem das durch einen Walzvorgang hergestellte Band zunächst zu einem Bund 1 gewickelt ist, von dem es jetzt wieder abgewickelt wird. Dabei ist es möglich, das Band 2 zunächst durch eine Entzunderungseinheit 3 zu führen, in der das Band 2 gestrahlt und gebürstet wird. Diese Entzunderungseinheit 3 kann verhältnismäßig einfach ausgestaltet sein und gegebenenfalls sogar entfallen. Nach dieser Entzunderungseinheit 3 gelangt das Band 2 in eine Beizeinrichtung 4, die zumindest aus einem Beizbehälter mit einer Beizlösung besteht und die die sogenannte Vorbeize bildet.In this drawing, the process diagram of a system for producing a strip of stainless steel that can be processed into finished products is shown, in which the strip produced by a rolling process is first wound into a bundle 1, from which it is now unwound again. It is possible to first pass the strip 2 through a descaling unit 3, in which the strip 2 is blasted and brushed. This descaling unit 3 can be of relatively simple design and can even be omitted if necessary. After this descaling unit 3, the strip 2 arrives in a pickling device 4, which consists of at least one pickling tank with a pickling solution and which forms the so-called pre-pickling.

An die Beizeinrichtung 4 schließt sich mindestens ein Kaltwalzgerüst 5 an, in dem das Band 2 auf die angestrebte Dicke reduziert wird. Danach wird das kaltgewalzte Band durch eine Entfettungsanlage 6 und eine Glühanlage 7 geführt und gelangt dann zu einer weiteren Beizeinrichtung 8, die aus mindestens zwei Flachbehältern besteht. Hier wird das Band 2 in der üblichen Weise fertiggebeizt. Danach wird das Band 2 in einer Einheit 9 bedarfsweise passiviert, dressiert und noch streckgerichtet.The pickling device 4 is followed by at least one cold rolling stand 5 in which the strip 2 is reduced to the desired thickness. Then the cold-rolled strip is passed through a Degreasing system 6 and an annealing system 7 performed and then arrives at a further pickling device 8, which consists of at least two flat containers. Here the strip 2 is finish-stained in the usual way. Thereafter, the band 2 is passivated, trained and straightened in a unit 9 as required.

Bei einem Vorbeizen mit entsprechenden Proben aus Edelstahl wurden dieselben zunächst über einen Zeitraum von etwa 45 Sekunden mit einer Beizlösung behandelt, die etwa 130 g/l freie Salzsäure sowie etwa 90 g/l Gesamteisen, welches als zwei- oder dreiwertiges Eisen vorliegt, enthält und eine Temperatur von etwa 80°C aufweist. Unter diesen Bedingungen wurde eine saubere, vollständige entzunderte, glänzende Oberfläche der Proben erzielt. Nach dem Kaltwalzvorgang und einem anschließenden Glühen erfolgte das Endbeizen, welches in der üblichen Weise zunächst elektrochemisch mittels einer schwefelsäurehaltigen Beizlösung und anschließend mittels Mischsäure durchgeführt wurde. Die endgebeizten Proben waren einwandfrei. Durch eine Veränderung der physikalischen Bedingungen, beispielsweise Aufbringen der Beizlösung durch einen Spritzvorgang oder durch die Kombination von Tauchbeizen und Spritzbeizen, konnte die Behandlungszeit erheblich reduziert werden.When pickling with appropriate stainless steel samples, they were first treated with a pickling solution containing about 130 g / l free hydrochloric acid and about 90 g / l total iron, which is in the form of divalent or trivalent iron, over a period of about 45 seconds has a temperature of about 80 ° C. Under these conditions, a clean, completely descaled, shiny surface of the samples was achieved. After the cold rolling process and a subsequent annealing, the final pickling was carried out, which was first carried out in the usual manner electrochemically using a pickling solution containing sulfuric acid and then using mixed acid. The final pickled samples were flawless. The treatment time could be reduced considerably by changing the physical conditions, for example applying the pickling solution by spraying or by combining immersion pickling and spray pickling.

Bei einem Vorbeizen mit einer schwefelsäurehaltigen Lösung enthielt dieselbe etwa 290 g/l freie Schwefelsäure und ein Eisengehalt von etwa 25 g/l. Die Temperatur dieser Beizlösung betrug etwa 100°C. Nach einer Behandlungszeit von etwa 40 Sekunden hatten die Proben nach dem Vorbeizen eine braune/graue Oberflächenfärbung, die sich in der anschließenden Glühzone vorteilhaft auswirkt. Probleme beim Kaltwalzvorgang traten nicht auf. Das sogenannte Endbeizen wurde dann wieder zunächst elektrochemisch in einer schwefelsäurehaltigen Beizlösung und anschließend in Mischsäure durchgeführt. Auch hier war die Qualtität der Proben einwandfrei.When pickled with a solution containing sulfuric acid, it contained about 290 g / l of free sulfuric acid and an iron content of about 25 g / l. The temperature of this pickling solution was about 100 ° C. After a treatment time of about 40 seconds, the samples had a brown / gray surface color after pickling, which has a beneficial effect in the subsequent annealing zone. There were no problems with the cold rolling process. The so-called final pickling was then again first carried out electrochemically in a pickling solution containing sulfuric acid and then in mixed acid. The quality of the samples was also perfect here.

Schließlich wurden auch noch Proben mit einer salpetersäurehaltigen Beizlösung behandelt, die etwa 20% freie Salpetersäure und etwa 30 g/l freies Eisen enthielt. Die Temperatur der Beizlösung betrug etwa 60°C und die Beizzeit etwa 30 Sekunden. Die salpetersäurehaltige Beizlösung wurde bei diesen Proben einmal durch einen Spritzvorgang zugeführt, während bei anderen Proben in der Beizlösung eine Turbulenz erzeugt wurde. Nach der sogenannten Vorbeizung hatten die Proben eine leicht aufgehellte Oberfläche, auf der jedoch noch Zunderreste zu erkennen waren. Diese Zunderreste wirken sich jedoch auf die nachfolgenden Behandlungen nicht nachteilig aus. Nach dem Endbeizen war ebenfalls eine zunderfreie, glänzende Oberfläche feststellbar.Finally, samples were also treated with a pickling solution containing nitric acid, which contained about 20% free nitric acid and about 30 g / l free iron. The temperature of the pickling solution was about 60 ° C and the pickling time was about 30 seconds. The nitric acid-containing pickling solution was injected once in these samples, while turbulence was generated in the pickling solution for other samples. After the so-called pickling, the samples had a slightly lightened surface on which, however, scale residues could still be seen. However, these scale residues do not adversely affect the subsequent treatments. After the final pickling, a scale-free, shiny surface was also found.

Bei entsprechenden Versuchen mit einer salpetersäurehaltigen Beizlösung die etwa 16 bis 17% Salpetersäure enthält, wurde festgestellt, daß bereits bei einer Zudosierung von 0,75% Flußsäure erste Flecken auf den fertigen Proben zu erkennen waren, die ab etwa 3% Flußsäure regelmäßig auftraten.In corresponding experiments with a nitric acid-containing pickling solution which contains about 16 to 17% nitric acid, it was found that with the addition of 0.75% hydrofluoric acid the first stains were visible on the finished samples, which appeared regularly from about 3% hydrofluoric acid.

Claims (15)

Verfahren zur Herstellung eines kaltgewalzten Bandes aus einem nicht rostenden, ferritischen oder austenitischen Edelstahl oder einer Titanlegierung, bei dem in einem Durchlauf ein durch einen Warmwalz- oder Gießvorgang hergestelltes und zu einem Bund gewickeltes Band abgewickelt und bedarfsweise mechanisch entzundert, dann chemisch und/oder elektrochemisch vorgebeizt, anschließend auf Fertigmaß kaltgewalzt, gegebenenfalls entfettet, geglüht, fertig gebeizt und bedarfsweise noch passiviert, dressiert und streckgerichtet wird,
dadurch gekennzeichnet,
daß das Vorbeizen mittels einer salz-, schwefel- und/oder salpetersäurehaltigen Beizlösung durchgeführt wird.Process for the production of a cold-rolled strip from a rustproof, ferritic or austenitic stainless steel or a titanium alloy, in which a strip produced by a hot rolling or casting process and wound into a bundle is unwound and mechanically descaled, if necessary, then chemically and / or electrochemically pre-pickled, then cold-rolled to finished dimensions, if necessary degreased, annealed, finished pickled and, if necessary, passivated, trained and stretch-straightened,
characterized,
that the pickling is carried out by means of a pickling solution containing salt, sulfur and / or nitric acid. Verfahren nach Anspruch 1,
daß das Vorbeizen in getrennten Beizbehältern mit unterschiedlichen Beizlösungen durchgeführt wird.Method according to claim 1,
that the pickling is carried out in separate pickling tanks with different pickling solutions. Verfahren nach Anspruch 1,
dadurch gekennzeichnet,
daß das Vorbeizen in mindestens einem Beizbehälter mit einem Beizlösungsgemisch durchgeführt wird.Method according to claim 1,
characterized,
that the pickling is carried out in at least one pickling tank with a pickling solution mixture. Verfahren nach mindestens einem der Ansprüche 1 - 3,
dadurch gekennzeichnet,
daß das Vorbeizen mit einer salzsäurehaltigen Beizlösung durchgeführt wird, die bis maximal 25% freie Salzsäure enthält und eine Temperatur von etwa 50° bis 90° C aufweist.Method according to at least one of claims 1-3,
characterized,
that the pickling is carried out with a pickling solution containing hydrochloric acid, which contains up to 25% free hydrochloric acid and has a temperature of about 50 ° to 90 ° C. Verfahren nach Anspruch 4,
dadurch gekennzeichnet,
daß die salzsäurehaltige Lösung 10 bis 17% freie Salzsäure enthält und eine Temperatur von 75° bis 85°C aufweist.Method according to claim 4,
characterized,
that the hydrochloric acid solution contains 10 to 17% free hydrochloric acid and has a temperature of 75 ° to 85 ° C. Verfahren nach mindestens einem der Ansprüche 1 bis 3,
dadurch gekennzeichnet,
daß das Vorbeizen mit einer schwefelsäurehaltigen Beizlösung durchgeführt wird, die bis maximal 45% freie Schwefelsäure enthält und eine Temperatur von etwa 70°C bis kurz unterhalb des Siedepunktes der Schwefelsäure aufweist.Method according to at least one of claims 1 to 3,
characterized,
that the pickling is carried out with a pickling solution containing sulfuric acid, which contains up to 45% free sulfuric acid and has a temperature of about 70 ° C to just below the boiling point of the sulfuric acid. Verfahren nach Anspruch 6,
dadurch gekennzeichnet,
daß die schwefelsäurehaltige Beizlösung 20 bis 30% freie Schwefelsäure enthält und eine Temperatur von 95 bis 105°C aufweist.Method according to claim 6,
characterized,
that the sulfuric acid-containing pickling solution contains 20 to 30% free sulfuric acid and has a temperature of 95 to 105 ° C. Verfahren nach Anspruch 6 oder 7,
dadurch gekennzeichnet,
daß das Band nach dem Vorbeizen an seiner Oberfläche eine dunkle Belagschicht aufweist.Method according to claim 6 or 7,
characterized,
that the strip has a dark coating on its surface after pickling. Verfahren nach mindestens einem der Ansprüche 1 bis 3,
dadurch gekennzeichnet,
daß das Vorbeizen mit einer salpetersäurehaltigen Beizlösung durchgeführt wird, die bis maximal 30% freie Salpetersäure enthält und eine Temperatur von etwa 30 bis 90°C aufweist.Method according to at least one of claims 1 to 3,
characterized,
that the pickling is carried out with a pickling solution containing nitric acid, which contains up to 30% free nitric acid and has a temperature of about 30 to 90 ° C. Verfahren nach Anspruch 9,
dadurch gekennzeichnet,
daß das Band nach dem Vorbeizen an seiner Oberfläche noch eine Restzunderschicht aufweist.Method according to claim 9,
characterized,
that the strip still has a residual scale layer on its surface after pickling. Vorrichtung nach mindestens einem der Ansprüche 1 bis 10,
dadurch gekennzeichnet,
daß die säurehaltige Beizlösung weniger als 0,75% freie Flußsäure enthält.Device according to at least one of claims 1 to 10,
characterized,
that the acidic pickling solution contains less than 0.75% free hydrofluoric acid. Verfahren nach mindestens einem der Ansprüche 1 bis 11,
dadurch gekennzeichnet,
daß zumindest die salzsäurehaltige Beizlösung dem Band durch mindestens einen Spritzvorgang zugeführt wird.Method according to at least one of claims 1 to 11,
characterized,
that at least the pickling solution containing hydrochloric acid is fed to the strip by at least one spraying operation. Verfahren nach Anspruch 12,
dadurch gekennzeichnet,
daß zwischen zwei aufeinanderfolgenden Spritzvorgängen das Band durch ein Tauchbeizbad geführt wird.Method according to claim 12,
characterized,
that the tape is passed through an immersion pickling bath between two successive spraying operations. Verfahren nach mindestens einem der Ansprüche 1 bis 13,
dadurch gekennzeichnet,
daß bei einem elektrochemischen Vorbeizen die Stromdichte bis 50A/dm2 beträgt.Method according to at least one of claims 1 to 13,
characterized,
that with an electrochemical pickling, the current density is up to 50A / dm 2 . Verfahren nach Anspruch 14,
dadurch gekennzeichnet,
daß die Stromdichte 10 bis 20A/dm2 beträgt.The method of claim 14
characterized,
that the current density is 10 to 20A / dm 2 .
EP96113439A 1995-09-01 1996-08-22 Process for producing cold-rolled strip continuously Revoked EP0770707B1 (en)

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CN103920708A (en) * 2014-03-27 2014-07-16 中冶南方工程技术有限公司 Production method of low-consumption corrosion-resistant high-surface-quality cold-rolled product
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CN110791763A (en) * 2019-12-03 2020-02-14 西安庄信新材料科技有限公司 Titanium plate leveling method
CN111560565A (en) * 2020-06-29 2020-08-21 江苏九天光电科技有限公司 Production method of high-quality special steel thin steel strip for measuring instrument

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JPH09125271A (en) 1997-05-13
DE19532278A1 (en) 1997-03-06
DE19532278B4 (en) 2006-07-27
ATE235584T1 (en) 2003-04-15

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