EP1029940B1 - Verfahren zur Aluminisierung von Stahl zum Erzeugen einer dünnen Grenzflächenschicht - Google Patents

Verfahren zur Aluminisierung von Stahl zum Erzeugen einer dünnen Grenzflächenschicht Download PDF

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Publication number
EP1029940B1
EP1029940B1 EP20000400358 EP00400358A EP1029940B1 EP 1029940 B1 EP1029940 B1 EP 1029940B1 EP 20000400358 EP20000400358 EP 20000400358 EP 00400358 A EP00400358 A EP 00400358A EP 1029940 B1 EP1029940 B1 EP 1029940B1
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Prior art keywords
bath
phase
temperature
steel
workpiece
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Expired - Lifetime
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EP20000400358
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English (en)
French (fr)
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EP1029940A1 (de
Inventor
Philippe Guesdon
Jean-Pierre Godin
Eric Lesueur
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USINOR SA
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USINOR SA
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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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/12—Aluminium or alloys based thereon
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/923—Physical dimension
    • Y10S428/924—Composite
    • Y10S428/926—Thickness of individual layer specified
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9265—Special properties
    • Y10S428/933—Sacrificial component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9335—Product by special process
    • Y10S428/939—Molten or fused coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y10T428/1275—Next to Group VIII or IB metal-base component
    • Y10T428/12757—Fe

Definitions

  • the invention relates to a steel aluminizing process comprising a step of dipping the steel part to be coated in a liquid bath containing mainly aluminum.
  • the internal layer of alloy having a fragile behavior one seeks generally to limit its thickness.
  • Silicon is the most commonly used alloying inhibitor; to be effective, its weight concentration in the soaking bath is generally between 3 and 13%.
  • the soaking baths are saturated in iron, due to the dissolution of the steel in the bath; this saturation leads to the well-known formation of mattes; the liquid bath is then in equilibrium with the solid phase of these mattes.
  • the ⁇ 5 phase has a hexagonal structure and therefore crystallizes in the form of globular grains; it is sometimes called ⁇ H or H; the iron content of this phase is generally between 29 and 36% by weight; the silicon content of this phase is generally between 6 and 12% by weight; the balance consists mainly of aluminum; the chemical composition corresponds approximately to the formula Fe 3 Si 2 Al 12 .
  • the ⁇ 6 phase has a monoclinic structure and therefore crystallizes in the form of flat and elongated grains; it is sometimes called ⁇ or M; the iron content of this phase is generally between 26 and 29% by weight; the silicon content of this phase is generally between 13 and 16% by weight; the balance consists mainly of aluminum; the chemical composition corresponds approximately to the formula Fe 2 Si 2 Al 9 .
  • FIG. 1 represents in three dimensions, in a part of the ternary Al-Si-Fe diagram, the variations - vertical axis - of the equilibrium temperature of a liquid phase with different solid phases called as follows: FeAl 3 ⁇ ⁇ , Fe 3 Si 2 Al 12 ⁇ ⁇ 5 , Fe 2 Si 2 Al 9 ⁇ ⁇ 6 , FeSiAl 3 ⁇ ⁇ 2, FeSi 2 Al 4 ⁇ ⁇ , Al ⁇ aluminum, Si ⁇ silicon, and other less important phases like ⁇ 3, ⁇ 4.
  • Phase ⁇ plays an important role in the invention presented below; its structure is monoclinic; it can contain up to 6% by weight of silicon in solid solution; the chemical composition therefore corresponds approximately to the formula FeAl 3 .
  • Figure 2 is a projection of Figure 1; we deduce approximately the liquid-solid equilibrium temperature using isothermal curves; the temperature interval between each curve is 20 ° C.
  • Table I summarizes the possible composition of phases ⁇ , ⁇ 5 and ⁇ 6.
  • Composition of the bath and the main phases obtained after solidification of the aluminum coating Composition:% by mass al Yes Fe Bath > 86% 3 to 13% saturation ( e.g. 3% ) eutectic 87 12.2 0.8 Phase ⁇ 6 55 to 61 13 to 16 26 to 29 Phase ⁇ 5 55 to 62 6 to 12 29 to 36 Phase ⁇ 52 to 64 0 to 6% 36 to 42
  • the internal interfacial layer of the aluminum-based coating is therefore brittle ; it therefore tends to crack during the shaping of the parts aluminized, especially sheet metal; these cracks cause a decrease protection against corrosion provided by the coating; to get aluminized coatings that are more resistant to both shaping and corrosion, it is therefore sought to limit the thickness of this interfacial layer.
  • the object of the invention is therefore, in an aluminizing process of this type, to limit the thickness of the interfacial layer.
  • Condition 2 leads to the use of baths with a silicon content of greater than 7.5%, preferably of the order of 9% (see FIGS. 1 and 2).
  • Applicant has determined conditions different from those in art which lead to a significantly smaller thickness of interfacial layer and which go against the presuppositions underlying conventional methods of the prior art.
  • the invention relates to a process for aluminizing a piece of steel comprising a step in which the part is dipped in a liquid aluminum-based bath, characterized in that the composition and the average temperature of this bath on the one hand, the temperature of immersion of this part in the bath on the other hand, are adapted to obtain, in the immersion zone of this room, a local temperature and composition of bath allowing an equilibrium with the solid phase called ⁇ whose composition corresponds approximately to the chemical formula FeAl 3 .
  • the invention also relates to an aluminized steel sheet, the aluminized coating includes a layer of Al-Fe-Si alloy and a layer surface of aluminum, capable of being obtained by the process according to the invention, characterized in that said alloy layer comprises, on contact of the steel substrate, an underlay composed essentially of phase ⁇ .
  • the thickness of this alloy layer is less than or equal to 3 ⁇ m.
  • the aluminizing installation conventionally comprises means cleaning, annealing means, soaking means in a bath aluminizing, means for wringing the aluminum-based layer driven by the strip at the exit of the bath, cooling means and means for continuously scrolling the strip in the installation.
  • the temperature of the strip when it returns in the bath, or strip immersion temperature is higher than the average bath temperature.
  • the strip then enters the bath at a higher temperature to that of equilibrium with phase ⁇ 6 or ⁇ 5, it causes heating bath room in the strip immersion zone; this local warm-up causes a dissolution of the surface ferrite of the strip and a iron enrichment of the immersion zone.
  • the temperature and the iron enrichment of the immersion zone must be sufficiently high so that, in this zone, the solid phase capable of being in equilibrium with the liquid phase corresponds to the ⁇ ⁇ FeAl phase. 3 ; in this way, in the immersion zone, the first solid sub-layer depositing on the steel strip corresponds to the FeAl 3 ⁇ ⁇ phase.
  • the strip cools down to the average temperature of the bath which corresponds to the equilibrium temperature with the solid phase ⁇ 5 or ⁇ 6; so, on the first phase sublayer ⁇ , the interfacial layer is then formed main classic of the prior art, composed of phase ⁇ 5 or ⁇ 6.
  • the strip running causes a layer which is wrung out and solidifies on cooling; we then obtains the aluminized strip according to the invention, the alloyed layer of which interfacial comprises, in contact with steel, an underlay essentially composed of phase ⁇ .
  • the aluminized strip according to the invention therefore resists a lot better for both corrosion and cracking.
  • phase ⁇ is the fastest at be able to form on the tape at the start of immersion, that this formation fast limits the amount of ferrite that goes into solution in the bath, which also limits the thickness of the alloy layer.
  • the invention adds a suitable condition to form in priority phase ⁇ on the substrate.
  • the steels that can be used can also contain alloying elements as Ti between 0.1% and 1% by weight, and Al between 0.01% and 0.1% by weight, by example ferritic stainless steel referenced AISI 409; other elements of addition adapted to desired properties and / or other elements residuals may be present in these steels; when the steel contains these alloying, addition and / or residual elements, the coating obtained on the sheet is generally enriched with these elements.
  • alloying elements as Ti between 0.1% and 1% by weight, and Al between 0.01% and 0.1% by weight, by example ferritic stainless steel referenced AISI 409; other elements of addition adapted to desired properties and / or other elements residuals may be present in these steels; when the steel contains these alloying, addition and / or residual elements, the coating obtained on the sheet is generally enriched with these elements.
  • the invention makes it possible to limit, within the surface layer to aluminum base of the coating, the appearance of chromium-enriched phases; these phases are related to phase ⁇ 5 already described, contain the same proportion of Si that this phase ⁇ 5, contain more than 5% by weight of chromium, generally between 6% and 17% chromium; the presence of this phase in the surface layer of the coating is detrimental to the quality coating; the invention makes it possible to limit if not to eliminate this phase in the surface layer of the coating.
  • the strip to be coated is at a temperature higher than that of the bath, we can use a strip to warm the bath, to compensate for losses thermal bath, to maintain the bath at the desired temperature.
  • this process is advantageous, since in the succession of stages through which the strip - annealing passes, cooling to immersion temperature, quenching, spinning, cooling for solidification - cooling after annealing less important than in the prior art.
  • a bath is used, the composition and the average temperature are adapted to be in balance with phase ⁇ 6; we see that the mattes that result from these baths are less annoying in terms of the quality of the coating obtained than mattes which result from other baths, especially those whose composition and mean temperature are adapted to be in equilibrium with phase ⁇ 5.
  • the bath naturally saturating with iron until the appearance of solid mattes, the liquid phase of the bath is in equilibrium with the solid phase ⁇ 5 ⁇ Fe 3 Si 2 Al 12 .
  • Table II summarizes the results obtained as a function of the immersion temperature. Thickness as a function of the strip temperature at immersion. Belt temperature: 675 ° C 720 ° C 730 ° C 750 ° C 765 ° C Alloy layer thickness ( ⁇ m) 5-6 6-7 2-3 4-5 7
  • the strip should be soaked at a temperature above 720 ° C and lower 765 ° C, preferably around 730 ° C.
  • Example 2 The procedure is as in Example 1 except that the bath this time contains 8% by weight of silicon and its temperature is maintained at about 650 ° C; the cumulative duration of immersion in the bath and of the solidification of the coating is this time of the order of 11 seconds.
  • Table III summarizes the results obtained as a function of the immersion temperature. Thickness as a function of the strip temperature at immersion. Belt temperature: 650 ° C 680 ° C 720 ° C 730 ° C 740 ° C Alloy layer thickness ( ⁇ m) 4 5 2-3 3 > 3
  • the optimal immersion temperature is between 680 ° C and 740 ° C, preferably close to 720 ° C; according to figure 2, to reach the domain of existence of phase ⁇ , it would be advisable that the temperature is greater than or equal to approximately 700 ° C; the domain of Preferred temperature would therefore correspond to the range 700-740 ° C.
  • Example 2 The procedure is as in Example 1 except that the bath this time contains 9.5% by weight of silicon and its temperature is maintained at about 650 ° C; the cumulative duration of immersion in the bath and of the solidification of the coating is this time of the order of 10 seconds.
  • Table IV summarizes the results obtained as a function of the immersion temperature. Thickness as a function of the strip temperature at immersion. Belt temperature (° C) 650 700 715 740 750 760 Alloy layer thickness ( ⁇ m) 5-6 5-6 7 3 5 7-8
  • the optimal immersion temperature is between 715 ° C and 760 ° C, preferably close to 740 ° C; according to figure 2, to reach the domain of existence of phase ⁇ , it would be advisable that the temperature is greater than or equal to approximately 740 ° C; the domain of Preferred temperature would therefore correspond to the range 740-760 ° C.
  • Table V shows the conclusions of Examples 1 to 3.
  • Immersion temperature as a function of the Si content in the bath.
  • Si content in bath 8% 9% 9.5%

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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)
  • Coating With Molten Metal (AREA)
  • Chemically Coating (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Chemical Treatment Of Metals (AREA)

Claims (14)

  1. Verfahren zum Aluminieren eines Werkstücks aus Stahl, umfassend einen Schritt, bei dem man das Werkstück in ein schmelzflüssiges Aluminiumbad taucht, dadurch gekennzeichnet, dass zur Bildung einer ersten Unterschicht aus der Feststoffphase , deren Zusammensetzung in etwa der chemischen Formel FeAl3 entspricht, einerseits die Zusammensetzung und die mittlere Temperatur des Bades, andererseits die Tauchtemperatur des Werkstücks in das Bad entsprechend angepasst werden, um in der Tauchzone des Werkstücks eine örtliche Temperatur und Zusammensetzung des Bades zu erhalten, die ein Gleichgewicht mit der Phase  ermöglichen, und dass man eine Grenzflächenschicht bestehend aus der Phase τ5 oder der Phase τ6 auf der ersten Schicht aus der Phase bildet, indem die Führung des Werkstücks im Bad nach der Tauchzone fortgesetzt wird, derart, dass die Zusammensetzung und die mittlere Temperatur des Bades entsprechend angepasst werden, um mit der Phase τ5 oder der Phase τ6 im Gleichgewicht zu sein.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass sich die Tauchzone wie folgt erstreckt:
    dickenmäßig in einem Abstand von bis zu etwa 30 µm von der Oberfläche des Werkstücks,
    längenmäßig längs der Oberfläche des Werkstücks, zwischen dem beginnenden direkten Kontakt zwischen dem Stahl der Oberfläche und dem schmelzflüssigen Bad einerseits und der beginnenden Erstarrung einer Grenzflächenschicht aus der Phase τ5 oder τ6 andererseits.
  3. Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, dass die Zusammensetzung und die mittlere Temperatur des Bades entsprechend angepasst werden, um mit der Phase τ6 im Gleichgewicht zu sein.
  4. Verfahren nach irgendeinem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das schmelzflüssige Bad eisengesättigt ist.
  5. Verfahren nach irgendeinem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die Tauchtemperatur des Werkstücks höher ist als die Temperatur des Bades.
  6. Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass bei einem Siliziumgehalt des Bades von etwa 8 % die Tauchtemperatur 700 bis 740°C, vorzugsweise etwa 720°C beträgt.
  7. Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass bei einem Siliziumgehalt des Bades von etwa 9 % die Tauchtemperatur 720 bis 765°C, vorzugsweise etwa 730°C beträgt.
  8. Verfahren nach irgendeinem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass bei einem Siliziumgehalt des Bades von etwa 9,5 % die Tauchtemperatur 740 bis 760°C, vorzugsweise etwa 740°C beträgt.
  9. Verwendung des Verfahrens nach irgendeinem der Ansprüche 1 bis 8 zum Aluminieren eines Werkstücks aus Kohlenstoffstahl.
  10. Verwendung des Verfahrens nach irgendeinem der Ansprüche 1 bis 8 zum Aluminieren eines Werkstücks aus rostfreiem Stahl.
  11. Aluminiertes Stahlblech, dessen aluminierter Überzug eine Al-Fe-Si-Legierungschicht sowie eine Deckschicht auf Basis von Aluminium aufweist, welche mit dem Verfahren nach irgendeinem der Ansprüche 1 bis 8 hergestellt werden kann, dadurch gekennzeichnet, dass die Legierungsschicht eine mit dem Stahlsubstrat in Kontakt stehende Unterschicht aufweist, die im wesentlichen aus der Phase  besteht.
  12. Blech nach Anspruch 11, dadurch gekennzeichnet, dass die Dicke der Legierungsschicht kleiner oder gleich 3 µm ist.
  13. Blech nach irgendeinem der Ansprüche 11 bis 12, dadurch gekennzeichnet, dass der Stahl ein Kohlenstoffstahl ist.
  14. Blech nach irgendeinem der Ansprüche 11 bis 12, dadurch gekennzeichnet, dass der Stahl ein rostfreier Stahl ist.
EP20000400358 1999-02-18 2000-02-09 Verfahren zur Aluminisierung von Stahl zum Erzeugen einer dünnen Grenzflächenschicht Expired - Lifetime EP1029940B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9902050 1999-02-18
FR9902050A FR2790010B1 (fr) 1999-02-18 1999-02-18 Procede d'aluminiage d'acier permettant d'obtenir une couche d'alliage interfaciale de faible epaisseur

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EP1029940A1 EP1029940A1 (de) 2000-08-23
EP1029940B1 true EP1029940B1 (de) 2004-10-27

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US (1) US6309761B1 (de)
EP (1) EP1029940B1 (de)
JP (1) JP4629180B2 (de)
AT (1) ATE280846T1 (de)
BR (1) BR0000843B1 (de)
CA (1) CA2298312C (de)
DE (1) DE60015202T2 (de)
ES (1) ES2231130T3 (de)
FR (1) FR2790010B1 (de)

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JP4751168B2 (ja) * 2005-10-13 2011-08-17 新日本製鐵株式会社 加工性に優れた溶融Ａｌ系めっき鋼板及びその製造方法
DE102008006771B3 (de) * 2008-01-30 2009-09-10 Thyssenkrupp Steel Ag Verfahren zur Herstellung eines Bauteils aus einem mit einem Al-Si-Überzug versehenen Stahlprodukt und Zwischenprodukt eines solchen Verfahrens
WO2011104443A1 (fr) * 2010-02-24 2011-09-01 Arcelormittal Investigación Y Desarrollo Sl Procédé de fabrication d'une pièce a partir d'une tôle revêtue d'aluminium ou d'alliage d'aluminium
DE102010014267A1 (de) 2010-04-08 2011-10-13 H.C. Starck Gmbh Dispersionen, sowie Verfahren zur deren Herstellung und deren Verwendung
KR101569505B1 (ko) 2014-12-24 2015-11-30 주식회사 포스코 내박리성이 우수한 hpf 성형부재 및 그 제조방법
KR101858863B1 (ko) * 2016-12-23 2018-05-17 주식회사 포스코 내식성 및 가공성이 우수한 용융 알루미늄계 도금강재

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CA2298312A1 (fr) 2000-08-18
EP1029940A1 (de) 2000-08-23
CA2298312C (fr) 2009-02-03
DE60015202D1 (de) 2004-12-02
ES2231130T3 (es) 2005-05-16
BR0000843A (pt) 2000-09-26
DE60015202T2 (de) 2005-11-10
ATE280846T1 (de) 2004-11-15
FR2790010B1 (fr) 2001-04-06
JP2000239819A (ja) 2000-09-05
JP4629180B2 (ja) 2011-02-09
FR2790010A1 (fr) 2000-08-25
BR0000843B1 (pt) 2010-04-06
US6309761B1 (en) 2001-10-30

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