EP0870069A1 - Verfahren zum feuerverzinken eines stahlbleches, das oxidierbare legierungselemente enthält - Google Patents
Verfahren zum feuerverzinken eines stahlbleches, das oxidierbare legierungselemente enthältInfo
- Publication number
- EP0870069A1 EP0870069A1 EP96942384A EP96942384A EP0870069A1 EP 0870069 A1 EP0870069 A1 EP 0870069A1 EP 96942384 A EP96942384 A EP 96942384A EP 96942384 A EP96942384 A EP 96942384A EP 0870069 A1 EP0870069 A1 EP 0870069A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sheet
- atmosphere
- steel
- annealing
- ammonia
- 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
Links
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 69
- 239000010959 steel Substances 0.000 title claims abstract description 69
- 238000005246 galvanizing Methods 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000005275 alloying Methods 0.000 title abstract 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000000137 annealing Methods 0.000 claims abstract description 46
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 24
- 239000010703 silicon Substances 0.000 claims abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004320 controlled atmosphere Methods 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000006104 solid solution Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 20
- 239000011248 coating agent Substances 0.000 description 8
- 238000000576 coating method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 229910000976 Electrical steel Inorganic materials 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 238000005121 nitriding Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 229910001337 iron nitride Inorganic materials 0.000 description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000003631 expected effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
Classifications
-
- 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
- C23C2/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
- C23C2/022—Pretreatment of the material to be coated, e.g. for coating on selected surface areas by heating
Definitions
- the invention relates to a method of galvanizing steel sheets containing oxidizable addition elements, in particular silicon.
- steel grades containing oxidizable addition elements, in particular silicon are used.
- steels containing oxidizable addition elements, in particular silicon, are precisely used for their specific mechanical and / or electrical properties.
- the object of the invention is to provide a process for galvanizing steel sheets with a high content of oxidizable additives, in particular silicon, which is economical, efficient and not detrimental to the mechanical and / or electrical properties of said steel.
- the subject of the invention is a process for galvanizing sheet steel containing oxidizable addition elements, in particular silicon, in which the sheet is annealed under an annealing atmosphere which is non-oxidizing and then the sheet is quenched in a galvanizing bath, characterized in that said annealing atmosphere contains between 0.005% and 1% of ammonia.
- the invention applies to steel sheets containing oxidizable addition elements in proportions such that they prevent wettability of the sheet in the galvanizing bath to ensure a homogeneous coating of galvanization.
- the invention is particularly applicable to steel sheets with more than 0.2% silicon.
- - Said annealing atmosphere contains between 0.02% and 0.5% of ammonia.
- the residence time of said sheet in said atmosphere is less than or equal to 3 minutes.
- Another subject of the invention is a device for galvanizing sheet metal to implement the method according to the invention of the type comprising means for annealing sheet metal under a controlled atmosphere, which lead downstream to means for dipping the annealed sheet metal in a galvanizing bath, and means for controlling said atmosphere, characterized in that the means for atmosphere control are suitable for introducing and maintaining in said atmosphere ammonia at a content of between 0.005 and 1% and in that said ammonia is introduced into said atmosphere near the entry of the sheet in the means of annealed.
- the subject of the invention is also a steel sheet containing oxidizable addition elements, in particular silicon, galvanized by the process according to the invention of the type having an interface layer, between said steel and the galvanizing layer, containing nitrogen in solid solution characterized in that the thickness of said interface layer corresponds to less than 1 gram per square meter of interface surface.
- the invention may also have as an additional characteristic silicon at least 0.2% as an addition element in said steel.
- the galvanizing installation that is used comprises means for annealing the sheet metal strip under a controlled atmosphere, which lead downstream to means for quenching the sheet in a galvanizing bath, and means for controlling the said atmosphere.
- the annealing means can be compartmentalized into several zones corresponding to different temperatures, in particular a cooling zone before entering the galvanizing bath.
- the atmosphere of this cooling zone can communicate with the atmosphere above the surface of the galvanizing bath. In each of these zones, the atmosphere is controlled.
- the annealing means and the sheet dipping means as well as the atmosphere control means are known in themselves.
- the atmosphere control means are adapted in a manner known per se to introduce ammonia into the annealing zone and to control the ammonia content of the annealing atmosphere between 0.005 and 1%.
- the ammonia is introduced into the annealing atmosphere near the entry of the sheet into the annealing means.
- This particular arrangement concerning the galvanizing device goes against conventional designs for supplying gas to annealing atmospheres, according to which, in particular for supplying, for example, nitrogen and hydrogen, the gas is introduced essentially at the outlet of the sheet metal annealing means, so that the gas flows against the current of the sheet in the annealing means.
- the method according to the invention is applicable to steel sheets containing oxidizable addition elements.
- the method according to the invention is notably applicable to silicon steel sheets, in particular to more than 0.2% of silicon.
- the silicon sheet to be galvanized is cleaned in a manner known per se, for example by passing the bare sheet through a flame to degrease the surface to be coated.
- the sheet is then annealed in the annealing means of the installation, under conditions of temperature, duration and composition of the annealing atmosphere adapted in a manner known per se to obtain in particular the desired rec ⁇ stalling of the steel and, as necessary, the reduction of iron oxides possibly present on the surface of the sheet after cleaning.
- a condition is added concerning the ammonia content of said atmosphere which must be between 0.005% and 1%, which can be achieved by means of control. previously defined atmospheres.
- said ammonia content is maintained between 0.02% and 0.5%.
- the annealing time that is to say the time taken for the sheet to pass through the annealing means, is preferably less than 3 minutes.
- the annealing temperature is generally between 500 C C and 900 ° C.
- Said annealing conditions also include, as necessary, a cooling step in a zone of the annealing means provided for this purpose, before quenching the sheet in the galvanizing bath.
- the galvanized sheet After annealing under this atmosphere comprising ammonia, said annealing therefore comprising possible cooling of the sheet, the galvanized sheet is properly annealed in a manner known per se.
- the sheet obtained by the process according to the invention has on the surface of the steel sheet after annealing, or at the interface between steel and galvanizing layer, an interface layer composed of steel containing nitrogen in solution. solid and / or composed of iron nitride.
- this interface layer has a thickness corresponding to less than 1 g / m2. This low thickness of the interface layer contributes to maintaining the mechanical and electrical properties of the steel.
- the invention it therefore becomes possible to improve the corrosion resistance and the surface appearance of galvanized silicon steel sheets while maintaining the initial mechanical and / or electrical properties.
- a galvanizing device in which, according to a preferred variant of the invention described above, the ammonia is introduced into the annealing atmosphere near the inlet of the sheet, the wettability is further improved. steel.
- the invention also advantageously applies to steels having other oxidizable addition elements than silicon, in particular titanium, manganese, chromium and aluminum.
- the sample to be galvanized is a steel sheet containing 0.3% silicon.
- the sample is annealed under a reducing atmosphere containing 15% hydrogen, the rest being nitrogen and the inevitable impurities.
- Example 1 The result of this comparative example is that problems of wettability of the sample are observed in the galvanizing bath, which is detrimental to the adhesion and the homogeneity of the coating, therefore to the corrosion resistance that he brings.
- Example 1 The result of this comparative example is that problems of wettability of the sample are observed in the galvanizing bath, which is detrimental to the adhesion and the homogeneity of the coating, therefore to the corrosion resistance that he brings.
- the purpose of this example is to illustrate the galvanizing process according to the invention.
- Example 2 The purpose of this test is to illustrate that, according to the invention, the presence of ammonia at low concentration in the annealing atmosphere before galvanization does not appreciably modify the mechanical properties of the silicon steel sheets, often says "HR" steel, that is to say "High Strength".
- the steel grade used corresponds to the steel called "SOLDUR 490" from the company SOLLAC, which contains between 0.2 and 0.3% of silicon.
- the ammonia content in the annealing atmosphere remains much less than or equal to 1%, there is therefore no significant change in the mechanical properties.
- the purpose of this example is to illustrate the drawbacks associated with the application to a steel sheet of a galvanizing process in which the steel is annealed in an atmosphere containing ammonia in a higher proportion than in invention, as in GB 1 396419.
- the purpose of this example is also to illustrate the drawbacks associated with the application, to steels other than those which contain oxidizable addition elements in high proportions, of a galvanization process in which the steel is annealed under a atmosphere containing ammonia in small proportion as in the present invention.
- Document GB 1 396 419 describes a process for nitriding steel wire, which comprises an annealing treatment under a reducing atmosphere containing high proportions of ammonia (> 15%), which has for effect of nitriding the surface to be coated.
- This particular galvanizing process applies here to wires (and not to sheets), to so-called effervescent steels; the effervescent steels are non "deoxidized” steels; they therefore do not contain oxidizable addition elements and therefore do not pose problems of wettability in a galvanizing bath.
- the effect sought by nitriding the surface of the steel before galvanizing is to improve the adhesion of the galvanizing coating, which is a particularly critical problem on steel wires.
- the means described in this document namely the introduction of ammonia in high proportion into the annealing atmosphere, applies to other steels than those of the field of the present invention and does not provide any particular result. in terms of wettability, since this wettability does not pose any problem for this type of steel.
- Comparative Example 2 therefore goes against that of Example 2 according to the invention, at the level of the evolution of the mechanical properties, well preserved in the case of Example 2 for the weak ammonia contents but significantly deteriorated in the case of Comparative Example 2, including for the low ammonia contents.
Landscapes
- 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)
- Heat Treatment Of Sheet Steel (AREA)
- Manufacturing Of Steel Electrode Plates (AREA)
- Chemical Treatment Of Metals (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR9514835A FR2742449B1 (fr) | 1995-12-14 | 1995-12-14 | Procede de galvanisation de tole d'acier contenant des elements d'addition oxydables |
| FR9514835 | 1995-12-14 | ||
| PCT/FR1996/001978 WO1997021846A1 (fr) | 1995-12-14 | 1996-12-11 | Procede de galvanisation de tole d'acier contenant des elements d'addition oxydables |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0870069A1 true EP0870069A1 (de) | 1998-10-14 |
| EP0870069B1 EP0870069B1 (de) | 2001-07-18 |
Family
ID=9485506
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP96942384A Expired - Lifetime EP0870069B1 (de) | 1995-12-14 | 1996-12-11 | Verfahren zum feuerverzinken eines stahlbleches, das oxidierbare legierungselemente enthält |
Country Status (9)
| Country | Link |
|---|---|
| EP (1) | EP0870069B1 (de) |
| JP (1) | JP4247320B2 (de) |
| KR (1) | KR100441807B1 (de) |
| AT (1) | ATE203284T1 (de) |
| CA (1) | CA2238831C (de) |
| DE (1) | DE69614000T2 (de) |
| ES (1) | ES2158370T3 (de) |
| FR (1) | FR2742449B1 (de) |
| WO (1) | WO1997021846A1 (de) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19758140A1 (de) * | 1997-12-19 | 1999-07-08 | Mannesmann Ag | Verfahren zum Erzeugen von Metallprodukten aus Verbundwerkstoff |
| TWI314955B (en) * | 2002-03-01 | 2009-09-21 | Hot-dip galvanizing steel sheet and method for manufacturing a coated steel sheet | |
| DE10258531B3 (de) * | 2002-12-14 | 2004-04-08 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren und Vorrichtung zur Herstellung korrosionsschutzbeschichteter Stähle |
| EP2009128A1 (de) | 2007-06-29 | 2008-12-31 | ArcelorMittal France | Verzinkter oder Galvanneal-Siliziumstahl |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1552041A (en) * | 1924-05-09 | 1925-09-01 | Frederick M Crapo | Protected metal and process of making it |
| GB424373A (en) * | 1934-01-24 | 1935-02-20 | Rylands Brothers Ltd | Improvements in or relating to methods and apparatus for galvanizing or zinc coating iron or steel articles |
| GB1396419A (en) * | 1972-08-17 | 1975-06-04 | Gkn South Wales Ltd | Hot-dip zinc galvanizing of ferrous articles |
| JPS5974236A (ja) * | 1983-09-05 | 1984-04-26 | Sumitomo Metal Ind Ltd | 成形性のすぐれた深絞り用亜鉛めつき鋼板の製造法 |
| FR2661426B1 (fr) * | 1990-04-27 | 1992-08-07 | Maubeuge Fer | Procede de galvanisation au trempe et en continu. |
-
1995
- 1995-12-14 FR FR9514835A patent/FR2742449B1/fr not_active Expired - Fee Related
-
1996
- 1996-12-11 KR KR10-1998-0704153A patent/KR100441807B1/ko not_active IP Right Cessation
- 1996-12-11 CA CA002238831A patent/CA2238831C/fr not_active Expired - Lifetime
- 1996-12-11 ES ES96942384T patent/ES2158370T3/es not_active Expired - Lifetime
- 1996-12-11 DE DE69614000T patent/DE69614000T2/de not_active Expired - Lifetime
- 1996-12-11 AT AT96942384T patent/ATE203284T1/de active
- 1996-12-11 JP JP52180397A patent/JP4247320B2/ja not_active Expired - Lifetime
- 1996-12-11 WO PCT/FR1996/001978 patent/WO1997021846A1/fr active IP Right Grant
- 1996-12-11 EP EP96942384A patent/EP0870069B1/de not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| See references of WO9721846A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2742449B1 (fr) | 1998-01-09 |
| FR2742449A1 (fr) | 1997-06-20 |
| DE69614000T2 (de) | 2001-11-29 |
| KR19990071869A (ko) | 1999-09-27 |
| EP0870069B1 (de) | 2001-07-18 |
| CA2238831A1 (fr) | 1997-06-19 |
| ATE203284T1 (de) | 2001-08-15 |
| JP2000501787A (ja) | 2000-02-15 |
| DE69614000D1 (de) | 2001-08-23 |
| CA2238831C (fr) | 2004-11-30 |
| KR100441807B1 (ko) | 2004-11-10 |
| ES2158370T3 (es) | 2001-09-01 |
| WO1997021846A1 (fr) | 1997-06-19 |
| JP4247320B2 (ja) | 2009-04-02 |
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