EP0763609A1 - Procédé et dispositif pour le traitement de produits sous forme de bande en acier inoxydable - Google Patents

Procédé et dispositif pour le traitement de produits sous forme de bande en acier inoxydable Download PDF

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Publication number
EP0763609A1
EP0763609A1 EP96250179A EP96250179A EP0763609A1 EP 0763609 A1 EP0763609 A1 EP 0763609A1 EP 96250179 A EP96250179 A EP 96250179A EP 96250179 A EP96250179 A EP 96250179A EP 0763609 A1 EP0763609 A1 EP 0763609A1
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EP
European Patent Office
Prior art keywords
strip
electrolyte
treatment
stainless steel
scale
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
EP96250179A
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German (de)
English (en)
Other versions
EP0763609B1 (fr
Inventor
Franz Gerhard Ing. Pempera
Michael Dipl.-Ing. Haentjes
Andeas Dipl.-Ing. Jaenichen
Rainer Dipl.-Ing. Kilb
Horst Dipl.-Ing. Edel
Jürgen Dr.-Ing. Flügge
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.)
Vodafone GmbH
Original Assignee
Mannesmann AG
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Filing date
Publication date
Priority claimed from DE19537501A external-priority patent/DE19537501A1/de
Application filed by Mannesmann AG filed Critical Mannesmann AG
Publication of EP0763609A1 publication Critical patent/EP0763609A1/fr
Application granted granted Critical
Publication of EP0763609B1 publication Critical patent/EP0763609B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F7/00—Constructional parts, or assemblies thereof, of cells for electrolytic removal of material from objects; Servicing or operating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F1/00—Electrolytic cleaning, degreasing, pickling or descaling
    • C25F1/02—Pickling; Descaling
    • C25F1/04—Pickling; Descaling in solution
    • C25F1/06—Iron or steel
    • 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

Definitions

  • the invention relates to a method and a device for the continuous treatment of annealed and non-annealed hot strip made of stainless steel, in particular with high alloy proportions of chromium from the AISI 300 and 400 series, in a descaling system consisting of scale breakers, spotlights, brushes or the like.
  • the oxide layers formed on the surfaces in these scaling processes must be removed again and again in the production process, since such layers in the further production steps, in particular in the shaping rolling steps, are not only extremely undesirable and cumbersome, but also because leaving even the smallest amounts of residual scale on the Steel strip surfaces make it impossible to achieve the desired surface qualities of the steel in the production steps.
  • passive layers of the stainless steels which are very efficient with regard to corrosion, consist of only a few atomic layers (1-20 nm) thick oxide and also hydroxide layers in various mixed crystal forms, which only contain the element iron to a small extent and mainly from the chemically very stable oxygen compounds of the for the steels of interest here, the characteristic alloy element is chromium (Cr 2 O 3 ).
  • the element chromium in the steel alloy also plays a special role in the individual scaling processes in the course of the production process and thus, of course, also in the techniques for removing the scale layers, which will be discussed further below.
  • Stainless steel strip products are subjected to rolling processes in which the strip is forcedly reduced Strip thicknesses to greater lengths, that means that larger surfaces are also rolled out.
  • Hot rolling processes Hot rolling processes
  • Cold rolling processes If the primary material, for example the slab, is heated to a temperature of around 1,250 ° C for the rolling process, the resulting product is referred to as hot strip; however, if the steel strip is subjected to a rolling process at room temperature, the product is referred to as a cold strip.
  • hot strip with larger strip thicknesses with cold strip naturally smaller strip thicknesses, whereby the thickness ranges of the individual production lines can overlap more or less.
  • the cold strip is initially produced in several multiple hot-rolling passes and, after a certain strip thickness, in subsequent cold-rolling passes with the desired strip thickness and surface quality.
  • the thermal conditions during the shaping hot stitches not only lead to the formation of pronounced scale layers on the steel surfaces, but also to undesired crystal and structure structures of the steel base matrix.
  • a thermal treatment is used to create a completely recrystallized structure in hot strip by converting it from austenitic stainless steel (AISI series 300).
  • the hot strip has elongated, non-recrystallized grains in the middle and partly over the entire cross section, because due to the high proportion of alloys, recrystallization is delayed so much that it can only partially take place during the rolling process and the subsequent cooling in the coil.
  • Soft stabilization is not necessary for stabilized ferritic steels of AISI 409 and 439, for example, which have a ferrite structure in the rolled state (the carbon is stably bound as titanium carbide TiC).
  • This annealing process which is necessary for the production of the desired crystal and structural structures of the steel, in which material temperatures of 800 to 900 ° C for ferrites and of up to 1,200 ° C for austenites have to be achieved if continuous ferritic or austenitic structural structures are achieved, leads to further scaling of the steel surfaces.
  • the oxide formation with regard to its quality and quantity can be influenced within limits by appropriate process management; this will be discussed later.
  • Tinder that is formed on the steel surfaces during hot rolling is referred to as mill scale, and accordingly the scale that forms on the steel surfaces in the aforementioned annealing process is called annealing scale.
  • annealing scale Both of the aforementioned types of scale differ in a characteristic manner, the differences having their origin in the initial and boundary conditions in the formation of scale, which will be discussed in more detail below.
  • oxides wustite () FeO), magnetite (Fe 3 0 4 ) and / or hematite (Fe 2 0 3 ) are formed depending on the temperature range and oxygen pressure.
  • which oxide is stable in equilibrium with the gas phase and what the layer sequence of the oxidation products is can be predicted based on thermodynamic laws and data.
  • the growth of the oxide layers is initially determined by surface reactions and is linearly time-dependent. With a larger thickness of the oxide layer, diffusion processes in the oxides determine the speed and the parabolic time law applies. Diffusion in the oxides is possible due to disorder of the ion lattice, vacancies or interstitial atoms.
  • Protective oxide layers form the alloy elements chromium, aluminum and silicon.
  • the formation of the mixed oxide layer on the metal surface and the associated chromium depletion of the underlying metal matrix can with the high Affinity of chromium can be explained to combine with oxygen to form a stable oxide. It can be seen from thermodynamic stability diagrams that aluminum, silicon, manganese and chromium are oxidized even at very low oxygen pressures and therefore form an oxide layer in atmospheres with a low oxygen content. The oxygen pressures required to form oxide layers on iron and nickel are several powers of ten higher. The oxidation process leads to a sharp gradient in the concentration of chromium in the metal matrix - towards the interface with the oxide phase, which causes chromium to diffuse from the lower layers of the metal matrix towards the interface and the oxidation reaction taking place there.
  • the interfaces between the individual phases, the individual oxide phases and the outside atmosphere during the thermal treatment chromium from the near-surface layers of the metal matrix is reinforced towards the other components of the alloy transporting scale layers, thereby reducing the concentration of the alloying element chromium in the layers of the metal base matrix near the surface below the mixed oxide layer formed.
  • chromium depletion the layers of the metal base matrix near the surface in which this effect has occurred are referred to as the chromium-depleted zone of the metal matrix.
  • a scale layer is formed which consists of two layers - an inner one made of Fe-Cr oxide and an outer one made of Fe oxide.
  • the scale thicknesses are in the range of around 1.0 ⁇ m.
  • the scale thicknesses are only slightly dependent on the annealing time under these conditions.
  • the scale consists essentially of mixed oxide (Cr, Fe) 2 O 3 .
  • the scale thicknesses are in the range of a few ⁇ m and depend on the degree of interference.
  • the scale consists largely of mixed oxide (Cr, Fe) 2 O 3
  • the scale layer grows to a thickness of 5 to 10 ⁇ m.
  • the scale consists of (Fe, Cr) 3 O 4 spinel at the phase boundary with the metal and a cover layer made of iron oxide. Above 560 ° C the iron oxide mainly consists of Wüstit FeO; at lower temperatures, the wustite disintegrates into magnetite Fe 3 O 4 and iron particles embedded therein.
  • a covering layer of hematite Fe 2 O 3 can preferably form on the strip edges and on the outer and inner turns of the coils. Cracks form in the tinder during cooling.
  • the chrome-depleted zone on the belt surface has a thickness of ⁇ 1 ⁇ m; the Cr-rich scale layer has a thickness of around 2 ⁇ m. As the reel temperature drops, the thickness of the Cr-rich scale layer and that of the Cr-depleted layer on the metal surface decrease.
  • a surface covered with such hot rolling scale is subjected to long-term annealing (> 20 h) in a bell annealer, diffusion processes lead to an enlargement of the Cr-rich spinel layer at the phase boundary with the metal and to a pronounced Cr depletion on the surface of the metal.
  • the thickness of the spinel layer is about 3 ⁇ m; their Cr content is significantly higher than before the annealing treatment.
  • the Cr-depleted zone can be up to 5 ⁇ m wide.
  • the entire scale layer has a thickness of 10 to 15 ⁇ m. There is often a thin layer of iron (reduced iron oxide) on the oxide layer.
  • the total scale layer thickness also increases to 10 to 15 ⁇ m.
  • the Cr depletion can only take place to a lesser extent, so that the Cr depleted zone has a thickness of approximately 2 ⁇ m and the amount of Cr enrichment in the oxide layer at the phase boundary with the matrix metal is also lower.
  • glow scale layers on hot strip it should be noted that they do not have a continuous mixed oxide layer, as is the case with appropriately annealed cold strip. These scale layers are therefore 10 times thicker than comparable scale layers on cold strip.
  • the scale surface of a hot strip annealed in this way shows a high proportion of iron oxides with embedded Cr-rich oxides.
  • the chemically very stable mixed oxide layer would be permeable to a pickling attack to remove the scale deposit by acid with an economically interesting pickling rate (oxides only dissolve very slowly in acids or acid mixtures) if an electrolyte connection with the chromium-depleted zone or the basic matrix, the local element necessary for chemical pickling with the scale layers and thus the corresponding potential for rapid dissolution of the chromium-depleted zone or the basic matrix in the acid with the associated infiltration and blasting mechanism for the oxide coatings can be formed.
  • the local element happens only very slowly, so that economical pickling rates cannot be achieved with such a hot strip scale in acid.
  • such layers of scale on such surfaces are preferably removed by physical processes such as blasting or / and brushing to such an extent that a sufficient free area of chromium-depleted layer or of the base matrix is exposed in order to achieve an economical pickling rate.
  • the chromium-depleted layer Since mostly in the mechanical descaling process after hot strip annealing, not only the critical but also a very large area of the chromium-depleted layer or the basic matrix is exposed - moreover, the chromium-depleted layer is not as pronounced as in the case of the cold strip, which Thickness of this layer is therefore not very large, - can be pickled with high pickling rates if the concentration of the individual components in the mixed acid is chosen accordingly.
  • Hot strip annealing is performed to recrystallize the metal structure after hot rolling and cooling. This is tantamount to a reduction in the increase in strength values caused by hot rolling and cooling.
  • the increase in strength is only 10 to 20%. These materials could be cold worked without an annealing process (50 - 80%). However, the remaining 20% of the AISI 400 series materials must be annealed before cold working.
  • this system configuration produces strip with a roughness of 4 - 6 Ra ⁇ m.
  • the object of the present invention is to present a method and a system which make it possible to economically pickle stainless steel strip (AISI 300 and 400) -also in material qualities that have to be annealed as hot strip before further treatment, such as Ferrite 430 - to be produced with surface roughnesses of only 1 - 2 ⁇ m Ra and 100% descaling in one pass, depending on the rolling process to reduce 50 - 80% in thickness, to anneal, to descaling and to dress.
  • the tape which is 100% scale-free before cold forming, has a passivation layer in order to ensure that the reflection factor is reduced significantly by a good darkening of the surface.
  • a system for performing the method according to the invention is protected in claim 7.
  • the descaling system consists of a configuration of known individual units paired with a completely new concept of electrolytic pickling.
  • emitters are provided (depending on the strip speed, 1 to n aggregates) in order to generate the free oxide surfaces required for annealed hot strip for the rapid formation of the required potential and thus for economical pickling.
  • the electrolytic pickling that follows now offers in its new concept in cells based on the known system of electrolytic pickling with a switching of the current flow Anode length 1/3 cathode length 2/3 to work. The number (n) of cells depends on the belt speed. After these cells, a cell is installed that contains more than two anodes as current feeders. This is followed by a cell that contains only one cathode. This cathode is connected to one of the anodes from the anode cell via a rectifier.
  • the strip Under the anode, the strip is cathodic and inevitably has a pH value of approx. 14 on the strip surface, which means that only the gas development is effective as a detachment factor for descaling.
  • the tape On the cathodic side, however, the tape is anodic, so that a pH of approx. 0 is established on the tape surface. This corresponds to a 1-molar H 2 SO 4 on the belt. Only this section of the electrolytic pickling is able to ensure descaling down to the pores.
  • the entire electrolytic part is run instead of or in addition to Na 2 SO 4 as an electrolyte with an approx. 3 mol-containing H 2 SO 4 in order to increase the gradient of the descaling effect.
  • the use of a 3-molar H 2 SO 4 forms a dark-colored passive layer only in the cells arranged after the abrasive devices, in addition to the deep pore descaling.
  • the layer thickness of this passive layer is 50-100 nm. In relation to the surface quality of the strip, this does not interfere with the rolling process. However, it has a positive effect on the reflection factor for the glow.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Cleaning By Liquid Or Steam (AREA)
EP96250179A 1995-09-15 1996-08-19 Procédé et dispositif pour le traitement de produits sous forme de bande en acier inoxydable Expired - Lifetime EP0763609B1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE19535844 1995-09-15
DE19535844 1995-09-15
DE19537501A DE19537501A1 (de) 1995-09-15 1995-09-26 Verfahren und Anlage zur Herstellung von Banderzeugnissen aus nichtrostendem Stahl
DE19537501 1995-09-26

Publications (2)

Publication Number Publication Date
EP0763609A1 true EP0763609A1 (fr) 1997-03-19
EP0763609B1 EP0763609B1 (fr) 1999-12-15

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EP96250179A Expired - Lifetime EP0763609B1 (fr) 1995-09-15 1996-08-19 Procédé et dispositif pour le traitement de produits sous forme de bande en acier inoxydable

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Country Link
US (1) US5804056A (fr)
EP (1) EP0763609B1 (fr)
JP (1) JPH09137300A (fr)
ES (1) ES2142018T3 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6565735B1 (en) 1998-09-11 2003-05-20 Henkel Kommanditgesellschaft Auf Aktien Process for electrolytic pickling using nitric acid-free solutions
EP2581143B1 (fr) * 1999-01-26 2019-10-30 Nippon Steel & Sumitomo Metal Corporation Procédé pour éliminer et empêcher la formation de calamine
DE102018219198A1 (de) 2018-11-12 2020-05-14 Thyssenkrupp Ag Kathodisches Beizverfahren zur beschleunigten Entzunderung ohne Ausbeizen der Korngrenze
DE102018219199A1 (de) 2018-11-12 2020-05-14 Thyssenkrupp Ag Anodisches Beizverfahren zur Entzunderung und Verminderung der Korngrenzenoxidation
DE102020106353A1 (de) 2020-03-09 2021-09-09 Thyssenkrupp Steel Europe Ag Verfahren zum Entzundern eines Stahlbands und Anlage zum Entzundern eines Stahlbands
EP4455374A1 (fr) * 2023-04-24 2024-10-30 ThyssenKrupp Steel Europe AG Procédé de décapage électrolytique d'un feuillard à chaud

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE511777C2 (sv) * 1998-02-02 1999-11-22 Avesta Sheffield Ab Metod för behandling av en metallprodukt
JP2996245B2 (ja) * 1998-02-23 1999-12-27 住友金属工業株式会社 酸化スケ―ル層付きマルテンサイト系ステンレス鋼材およびその製造方法
AT407755B (de) 1998-07-15 2001-06-25 Andritz Patentverwaltung Verfahren zum beizen von edelstahl
AT408451B (de) 1999-11-18 2001-12-27 Andritz Ag Maschf Verfahren zur herstellung von edelstahlbändern mit verbesserten oberflächeneigenschaften
US6814815B2 (en) 2003-04-07 2004-11-09 The Material Works, Ltd. Method of removing scale and inhibiting oxidation in processed sheet metal
CN1280445C (zh) * 2003-07-17 2006-10-18 住友金属工业株式会社 具有耐渗碳性和耐焦化性的不锈钢和不锈钢管
US8278009B2 (en) * 2004-03-18 2012-10-02 Jfe Steel Corporation Metallic material for conductive member, separator for fuel cell using the same, and fuel cell using the separator
CN108380582A (zh) * 2018-05-08 2018-08-10 河南鑫轴传动机械有限公司 一种传动轴清洗工艺
WO2021105738A1 (fr) * 2019-11-25 2021-06-03 Arcelormittal Décapage électro-assisté de l'acier
CN212293834U (zh) * 2020-04-29 2021-01-05 中冶南方工程技术有限公司 一种节能环保带钢电解酸洗系统
CN113369233A (zh) * 2021-06-15 2021-09-10 洛阳市中心医院（郑州大学附属洛阳中心医院） 一种消毒供应中心用气管内套管清洗装置及方法
KR20240057678A (ko) * 2022-10-25 2024-05-03 주식회사 웨스코일렉트로드 동박 제조용 양극 재생을 위한 리드물질 제거방법
CN122029307A (zh) * 2023-10-20 2026-05-12 杰富意钢铁株式会社 钢板的氧化皮除去设备、钢板的制造设备、钢板的氧化皮除去方法及钢板的制造方法

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EP0235595A2 (fr) * 1986-03-01 1987-09-09 Hoesch Stahl Aktiengesellschaft Procédé, installation et dispositif de dégraissage et de nettoyage en continu de bandes de métaux, en particulier de bandes d'acier laminées à froid
EP0367112A1 (fr) * 1988-10-29 1990-05-09 Hitachi, Ltd. Procédé pour l'enlèvement de battitures d'acier inoxydable et dispositif à cet effet
EP0518850A1 (fr) * 1991-06-10 1992-12-16 Andritz-Patentverwaltungs-Gesellschaft m.b.H. Procédé et dispositif de décapage électrolytique d'objets conducteurs électriques transportés en continu
EP0644276A1 (fr) * 1993-09-17 1995-03-22 Hitachi, Ltd. Procédé et dispositif pour la fabrication et le décapage de tôles d'acier laminées à chaud

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US3338809A (en) * 1966-06-23 1967-08-29 United States Steel Corp Method of cleaning ferrous metal strands electrolytically, including moving said strands in a horizontal plane through an electrolyte while under the influence of alternating electrical fields
AT391486B (de) * 1988-09-14 1990-10-10 Andritz Ag Maschf Verfahren zum elektrolytischen beizen von edelstahlband
US5525562A (en) * 1994-01-25 1996-06-11 Matsushita Electric Industrial Co., Ltd. Dielectric ceramic compound

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0235595A2 (fr) * 1986-03-01 1987-09-09 Hoesch Stahl Aktiengesellschaft Procédé, installation et dispositif de dégraissage et de nettoyage en continu de bandes de métaux, en particulier de bandes d'acier laminées à froid
EP0367112A1 (fr) * 1988-10-29 1990-05-09 Hitachi, Ltd. Procédé pour l'enlèvement de battitures d'acier inoxydable et dispositif à cet effet
EP0518850A1 (fr) * 1991-06-10 1992-12-16 Andritz-Patentverwaltungs-Gesellschaft m.b.H. Procédé et dispositif de décapage électrolytique d'objets conducteurs électriques transportés en continu
EP0644276A1 (fr) * 1993-09-17 1995-03-22 Hitachi, Ltd. Procédé et dispositif pour la fabrication et le décapage de tôles d'acier laminées à chaud

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6565735B1 (en) 1998-09-11 2003-05-20 Henkel Kommanditgesellschaft Auf Aktien Process for electrolytic pickling using nitric acid-free solutions
EP2581143B1 (fr) * 1999-01-26 2019-10-30 Nippon Steel & Sumitomo Metal Corporation Procédé pour éliminer et empêcher la formation de calamine
DE102018219198A1 (de) 2018-11-12 2020-05-14 Thyssenkrupp Ag Kathodisches Beizverfahren zur beschleunigten Entzunderung ohne Ausbeizen der Korngrenze
DE102018219199A1 (de) 2018-11-12 2020-05-14 Thyssenkrupp Ag Anodisches Beizverfahren zur Entzunderung und Verminderung der Korngrenzenoxidation
DE102020106353A1 (de) 2020-03-09 2021-09-09 Thyssenkrupp Steel Europe Ag Verfahren zum Entzundern eines Stahlbands und Anlage zum Entzundern eines Stahlbands
EP3879008A1 (fr) 2020-03-09 2021-09-15 ThyssenKrupp Steel Europe AG Procédé de décapage d'une bande d'acier et installation de décapage d'une bande d'acier
EP4455374A1 (fr) * 2023-04-24 2024-10-30 ThyssenKrupp Steel Europe AG Procédé de décapage électrolytique d'un feuillard à chaud

Also Published As

Publication number Publication date
ES2142018T3 (es) 2000-04-01
EP0763609B1 (fr) 1999-12-15
US5804056A (en) 1998-09-08
JPH09137300A (ja) 1997-05-27

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