EP3237648B1 - Verfahren zur oberflächenbehandlung von stahlwerkstücken mittels nitrierung oder nitrocarburierung, oxidierung und folgender imprägnierung - Google Patents
Verfahren zur oberflächenbehandlung von stahlwerkstücken mittels nitrierung oder nitrocarburierung, oxidierung und folgender imprägnierung Download PDFInfo
- Publication number
- EP3237648B1 EP3237648B1 EP15821125.0A EP15821125A EP3237648B1 EP 3237648 B1 EP3237648 B1 EP 3237648B1 EP 15821125 A EP15821125 A EP 15821125A EP 3237648 B1 EP3237648 B1 EP 3237648B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- carried out
- nitriding
- minutes
- impregnation
- treatment
- 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.)
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- 238000005121 nitriding Methods 0.000 title claims description 41
- 238000000034 method Methods 0.000 title claims description 28
- 229910000831 Steel Inorganic materials 0.000 title claims description 19
- 239000010959 steel Substances 0.000 title claims description 19
- 238000004381 surface treatment Methods 0.000 title claims description 5
- 238000011282 treatment Methods 0.000 claims description 113
- 238000005470 impregnation Methods 0.000 claims description 50
- 238000005260 corrosion Methods 0.000 claims description 46
- 230000007797 corrosion Effects 0.000 claims description 46
- 150000003839 salts Chemical class 0.000 claims description 33
- 239000000654 additive Substances 0.000 claims description 18
- 230000000996 additive effect Effects 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 10
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- -1 alkali metal cyanates Chemical class 0.000 claims description 8
- 230000001590 oxidative effect Effects 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000005662 Paraffin oil Substances 0.000 claims description 6
- 150000001913 cyanates Chemical class 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims description 5
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 5
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 5
- 150000002826 nitrites Chemical class 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- 229910001337 iron nitride Inorganic materials 0.000 claims description 4
- 150000002823 nitrates Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 3
- 150000008039 phosphoramides Chemical class 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- WMYJOZQKDZZHAC-UHFFFAOYSA-H trizinc;dioxido-sulfanylidene-sulfido-$l^{5}-phosphane Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([S-])=S.[O-]P([O-])([S-])=S WMYJOZQKDZZHAC-UHFFFAOYSA-H 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 229910001963 alkali metal nitrate Inorganic materials 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 description 66
- 230000003647 oxidation Effects 0.000 description 58
- 239000010410 layer Substances 0.000 description 33
- 239000012071 phase Substances 0.000 description 20
- 239000002609 medium Substances 0.000 description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- 239000001993 wax Substances 0.000 description 9
- 101100126074 Caenorhabditis elegans imp-2 gene Proteins 0.000 description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 101100452131 Rattus norvegicus Igf2bp1 gene Proteins 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 235000013824 polyphenols Nutrition 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 5
- 238000007654 immersion Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 235000010344 sodium nitrate Nutrition 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- 101100455063 Caenorhabditis elegans lmp-1 gene Proteins 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910000727 Fe4N Inorganic materials 0.000 description 3
- 239000012736 aqueous medium Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 239000002344 surface layer Substances 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002608 ionic liquid Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 101150053856 psmb9 gene Proteins 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 230000008685 targeting Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical class O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 229910000288 alkali metal carbonate Inorganic materials 0.000 description 1
- 150000008041 alkali metal carbonates Chemical class 0.000 description 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 230000003042 antagnostic effect Effects 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 238000004320 controlled atmosphere Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019256 formaldehyde Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- INHWXZFVSTUXPN-UHFFFAOYSA-J molybdenum(4+) disulfite Chemical compound [Mo+4].[O-]S([O-])=O.[O-]S([O-])=O INHWXZFVSTUXPN-UHFFFAOYSA-J 0.000 description 1
- 150000002894 organic compounds Chemical group 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001289 polyvinyl ether Polymers 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical class [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/80—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/06—Surface hardening
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/02—Pretreatment of the material to be coated
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/34—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases more than one element being applied in more than one step
-
- 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
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/58—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions more than one element being applied in more than one step
Definitions
- the invention relates to a method of surface treatment of a piece of ferrous metal, in practice made of alloyed steel or not, having good resistance to corrosion by virtue of an impregnation treatment and a piece of steel having a high resistance to wear and corrosion which is dry to the touch.
- the invention applies to all types of mechanical parts intended to provide a mechanical function in service and having to have a high hardness, a long resistance to corrosion and wear. This is for example the case of many parts used in the automotive or aeronautical field.
- nitriding and nitrocarburizing are thermochemical treatments of nitrogen supply (nitrogen and carbon respectively) by combination-diffusion: there is formed on the surface a combination layer formed of iron nitrides (there are several possible phases), under which nitrogen is present by diffusion.
- the Applicant has itself proposed treatment methods aimed at obtaining even better corrosion resistance.
- oxidizing so as to obtain a nitrided layer comprising a deep and compact sublayer and a surface layer of well controlled porosity and finally to the deposition of a polymer of thickness between 3 and 20 ⁇ m, made of fluoroethylene-propylene (FEP) ), or even polytetrafluoroethylene (PTFE), or even polymers or copolymers of fluorinated or silicone polyurethanes, or polyamides-polyimides.
- FEP fluoroethylene-propylene
- PTFE polytetrafluoroethylene
- BS salt spray
- the parts are preferably nitrided in baths of molten salts based on cyanate ions then oxidized and finally impregnated with a hydrophobic wax.
- Nitriding followed by oxidation leads to the formation of a layer consisting of a compact deep sub-layer and a surface layer whose porosity is well controlled.
- the impregnation wax is an organic compound with a high molecular weight of between 500 and 10,000 and of surface tension, in the liquid state, of between 10 and 73 mN / m.
- the contact angle between the solid phase and the surface layer and the wax in the liquid state is between 0 and 75 degrees.
- the wax is chosen from natural waxes, synthetic polyethylene, polypropylene, polyesters, fluorinated waxes or modified petroleum residues.
- This solution simultaneously improves the corrosion resistance and friction properties of ferrous metal parts.
- the parts thus treated have good corrosion resistance in standard salt spray combined with good friction properties.
- the patent EP - 0 560 641 describes a process for phosphating steel parts to improve the resistance to corrosion and wear, making it possible to obtain specific surface characteristics resulting from a phosphating treatment preceded by a nitriding operation in a bath of molten salts containing sulfur species, from a nitriding operation in a bath of molten salts followed by a conventional sulfurization treatment, or from a metal deposit followed by a conventional sulfurization operation.
- the corrosion resistance values of the parts thus treated, after exposure to salt spray are of the order of 900 to 1200 hours.
- the patent EP - 1,180,552 relates to a method of surface treatment of mechanical parts subjected to both wear and corrosion by having a roughness conducive to good lubrication and according to which nitriding is carried out by immersion between 500 ° C and 700 ° C parts in a nitriding bath of molten salts containing alkaline cyanates and carbonates in precise ranges but free of species sulfur, then an oxidation is carried out in an aqueous oxidizing solution below 200 ° C.
- the document WO2012 / 146839 targeted a nitriding treatment leading to an appropriate roughness without requiring a finishing treatment; he described a bath of molten salts for nitriding mechanical steel parts having specific contents of alkali metal chloride, alkali metal carbonate, alkali metal cyanate and cyanide ions.
- the corrosion resistance measured in salt spray was between 240 and 650 hours.
- finishing treatment deposit of a varnish or of a wax, or phosphating treatment
- nitriding or nitrocarburizing treatment oxidation of mechanical parts made of ferrous material
- certain finishing treatments result in the fact that the surface of the parts thus treated tends to transfer a little oil onto the surfaces with which it can come into contact and tends to collect dust. the surrounding environment; this is hardly compatible with an additional step such as overmolding.
- the object of the invention is to remedy these drawbacks in a simple, safe, efficient and rational manner, while achieving very high levels of resistance to corrosion and to wear, better than with baths. current impregnation.
- the impregnation in a bath in accordance with the invention leads to a substantial improvement in corrosion resistance compared to a conventional bath, based on oils, acids and ethanol.
- the parts are dry to the touch (this is understood to mean the absence of oil transfer to an antagonistic surface), hence the absence of tendency to pick up surrounding dust and the ability to undergo post-treatment such as overmolding.
- a part according to the invention obtained by the process of the invention, namely a steel part having a high resistance to wear and corrosion, comprising a combination layer. at least 8 micrometers, a layer of oxides of thickness between 0.1 and 3 micrometers and an impregnation layer which is dry to the touch.
- ambient temperature does not designate a precise temperature but the fact that the treatment is done without temperature control (it is therefore neither necessary to heat the bath nor to cool it), and that it can be do at the temperature induced by the environment, even if it varies in proportions that can be significant during the year, for example between 15 ° C and 50 ° C.
- the nitriding / nitrocarburizing step is carried out so that the thickness of the combination layer obtained is at least 10 micrometers.
- the synthetic phenolic additive is a compound of formula C 15 H 24 0.
- the impregnation bath further comprises at least one additive chosen from the group consisting of calcium or sodium sulfonate, phosphites, diphenylamines, zinc dithiophosphate, nitrites, phosphoramides.
- the content of such additives is advantageously at most equal to 5%.
- the bath is preferably formed from 90% +/- 0.5% by weight of solvent, 10% +/- 0.5% by weight of paraffin oils and between 0.01% and not more of 1% +/- 0.1% of synthetic phenolic additive of formula C 15 H 24 O.
- the impregnation is carried out by soaking for a period of approximately 15 minutes.
- This soaking step is advantageously followed by a natural or accelerated drying operation by steaming.
- the nitriding / nitrocarburizing step is carried out in a bath of molten salts containing from 14% to 44% by weight of alkaline cyanates at a temperature of 550 ° C to 650 ° C for at least 45 minutes; preferably, this nitriding / nitrocarburizing bath contains from 14% to 18% by weight of alkaline cyanates.
- this treatment is carried out at a temperature of 590 ° C for 90 minutes to 100 minutes; according to a variant, also advantageous, the nitriding / nitrocarburizing treatment in salt baths melted is carried out at a temperature of 630 ° C for about 45 minutes to 50 minutes.
- the nitriding / nitrocarburizing step is carried out in a gaseous medium between 500 ° C and 600 ° C containing ammonia.
- the nitriding / nitrocarburizing step is carried out in an ionic medium (plasma) in a medium comprising at least nitrogen and hydrogen under reduced pressure.
- the oxidation step is carried out in a bath of molten salts containing carbonates, nitrates and alkali hydroxides.
- the molten oxidation salt bath contains alkaline nitrates, alkali carbonates and alkali hydroxides.
- the oxidation step is carried out at a temperature of 430 ° C to 470 ° C for 15 to 20 minutes.
- the oxidation is carried out in an aqueous bath containing alkali hydroxides, alkaline nitrates and alkaline nitrites.
- the oxidation step it is advantageous for the oxidation step to be carried out at a temperature of 110 ° C to 130 ° C for 15 to 20 minutes.
- the oxidation step is carried out in a gaseous medium mainly consisting of water vapor, at a temperature of 450 ° C. to 550 ° C. for 30 to 120 minutes.
- these tests were carried out by combining several types of nitriding or nitrocarburizing treatments, known per se, several types of oxidation treatment, known per se, and several types of impregnation. These tests were carried out on ferrous metal parts with smooth areas and sharp edges. More particularly, tests were carried out on grooved axes in annealed and rectified XC45 steel, having a smooth bearing and a threaded bearing.
- NITRU1 to NITRU3 treatments in molten salt baths.
- EP - 1,180,552 with: * the NITRU1 treatment located in the preferred low temperature range and the preferred average treatment time (from 45 minutes to 50 minutes), * the NITRU2 treatment located in the same preferred low temperature range but with the maximum treatment time (outside the preferred zone, ie from 90 minutes to 100 minutes) and * the NITRU3 treatment located in the preferred high temperature range with the preferred average treatment time (45 minutes to 50 minutes).
- the parameters of these treatments are summarized in the table below.
- the NITRU1 treatment results in a combination layer of thickness less than 8 micrometers
- the NITRU2 and NITRU3 treatments result in a layer whose thickness exceeds this threshold, and is preferably even at least 10 micrometers. In practice, it seems unnecessary to seek to exceed 25 micrometers, so that an effective range for the thickness of the layer appears to be 10 to 25 micrometers.
- these three treatments correspond to a treatment in a bath of molten salts containing from 14% to 44% by weight of alkaline cyanates (preferably from 14% to 18%) at a temperature of 550 ° C to 650 ° C (preferably from 590 ° C to 630 ° C) for at least 45 minutes (it does not seem useful to exceed 120 minutes, even 90 minutes).
- NITRU4 a gaseous medium
- NITRU5 a conventional treatment in ionic medium (plasma), NITRU5 (targeting a thickness of combination layer of at least 8 ⁇ m and advantageously between 10 and 25 ⁇ m).
- the NITRU4 treatment in a gaseous medium was carried out in an oven between approximately 500 and 600 ° C. under a controlled atmosphere comprising ammonia.
- the processing time has been established to guarantee a combination layer thickness of at least 8 micrometers, preferably greater than 10 micrometers.
- the NITRU5 treatment it was carried out in an ionic medium (plasma) in a mixture comprising at least nitrogen and hydrogen, under reduced pressure (that is to say under a pressure below atmospheric pressure , typically less than 0.1 atmosphere).
- the processing time has also been established to guarantee a combination layer thickness of at least 8 micrometers, preferably at least 10 micrometers.
- the thickness of the treatment layer indicated does not take into account the diffusion layer (for nitrogen as well as for carbon).
- Oxidations Ox1 and Ox2 correspond substantially, respectively, to the oxidation in salt bath and to the aqueous oxidation of the document EP1180552 cited above, while the nitrocarburizing (NITRU5) and Ox3 oxidation treatment parameters, in an ionized medium, correspond substantially to Example 9 of the document EP0497663 .
- the oxidations were carried out so as to obtain oxidation layers of thickness between 0.1 and 3 micrometers.
- impregnation treatment 1 did not induce dimensional variation.
- the surface of the parts was dry to the touch; this implies that, on the one hand, the surface of these parts does not tend to collect dust and that, on the other hand, these parts are compatible with an after-treatment such as overmolding.
- NITRU 1 NITRU 2 NITRU 3 NITRU 4 NITRU 5 Treatment 1 Ox1 + Imp2 96h 360h 912h 792h 384h 72h Treatment 2 Ox1 + lmp1 96h 960h 1368h 1368h 1008h 576h Treatment 3 Ox2 + lmp2 96h 312h 576h 792h 504h 72h Treatment 4 Ox2 + lmp1 96h 360h 1056h 1056h 720h 360h Treatment 5 Ox3 + lmp2 96h 192h 456h 552h 312h 24h Treatment 6 Ox3 + lmp1 96h 264h 888h 792h 552h 72h Treatment 7 Ox0 + Imp2 96h 96h 456h 384h 48h 48h Treatment 8 Ox0 + Imp1 96h 120h 504h 624h 360h 336h
- the oxidation-impregnation treatment does not matter when there is no nitriding / nitrocarburizing (the corrosion resistance remains at 96 h, in the first column).
- the increase in corrosion resistance is at least of the order of 200 hours.
- the new impregnation results in an increase in the corrosion resistance of the order of 300 hours; in the case of NITRU5 combined with oxidation in an ionic liquid medium (oxidation 1 - treatments 1 and 2), the increase is even of the order of 500 hours.
- the improvement in corrosion resistance is, for type 2 and 3 oxidations (treatments 3 to 6) of at least 250 hours for the NITRU3 treatment and even 450 hours for the treatment NITRU2. With type 2 oxidation (treatments 3 and 4) corrosion resistance exceeding the threshold of 1000 hours is obtained.
- the impregnation bath 1 has a surprising synergistic effect with the nitriding / nitrocarburizing treatments NITRU2 and NITRU3 provided that the nitriding / nitrocarburizing is followed by a type 1 or 2 oxidation. , an optimum seems to be obtained when the oxidation treatment is type 1.
- the particular composition of the impregnation bath considered in the tests falls into a more general composition, namely a bath formed of at least 70% by weight, to within 1%, of a solvent formed of a mixture of hydrocarbons formed from a cut of C9 to C17 alkanes, from 10% to 30% by weight, to within 1%, of at least one paraffin oil composed of a cut of C16 to C32 alkanes and of minus an additive of the synthetic phenolic additive type at a concentration of between 0.01% and 3% by weight, at room temperature.
- the solvent content is preferably between 80% and 90% by weight; likewise, the content of paraffin oil is preferably between 10% and 20% by weight.
- the cut of alkanes in the solvent is preferably from C9 to C14.
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Claims (25)
- Verfahren zur Oberflächenbehandlung eines Stahlteils, um ihm eine erhöhte Widerstandsfähigkeit gegen Verschleiß und Korrosion zu verleihen, welches umfasst:* einen Nitrier- oder Nitrocarburierschritt, der angepasst ist, um eine Verbindungsschicht von mindestens 8 Mikrometern Dicke zu bilden, die aus Eisennitriden der ε- und/oder γ'-Phasen besteht,* einen Oxidationsschritt, der angepasst ist, um eine Schicht aus Oxiden mit einer zwischen 0,1 und 3 Mikrometern liegenden Dicke zu erzeugen, und* einen Schritt der Imprägnierung durch Eintauchen in ein Imprägnierungsbad während mindestens 5 Minuten, wobei das Bad zu mindestens 70 Gewichts-%, auf 1 % genau, aus einem Lösungsmittel, das aus einem Kohlenwasserstoffgemisch besteht, welches aus einem C9- bis C17-Schnitt von Alkanen besteht, zu mindestens 10 bis 30 Gewichts-%, auf 1 % genau, aus einem Paraffinöl, das sich aus einem C16- bis C32-Schnitt von Alkanen zusammensetzt, und mindestens einem Additiv des synthetischen Phenol-Additiv-Typs in einer zwischen 0,01 und 3 Gewichts-%, auf 0,1 % genau, liegenden Konzentration besteht, bei Raumtemperatur.
- Verfahren nach Anspruch 1, in welchem das synthetische Phenol-Additiv eine Verbindung der Formel C15H24O ist.
- Verfahren nach Anspruch 2, in welchem das Imprägnierungsbad aus 90+/-0,5 Gewichts-% Lösungsmittel, 10+/-0,5 Gewichts-% Paraffinölen und weniger als 1+/-0,1 Gewichts-% synthetischem Phenol-Additiv der Formel C15H24O besteht.
- Verfahren nach einem der Ansprüche 1 bis 3, wobei das Imprägnierungsbad zudem mindestens ein Additiv umfasst, welches aus der Gruppe bestehend aus Calcium- oder Natriumsulfonat, Phosphiten, Diphenylaminen, Zinkdithiophosphat, Nitriten und Phosphoramiden ausgewählt ist.
- Verfahren nach einem der Ansprüche 1 bis 4, in welchem dem Eintauchvorgang ein natürlicher oder durch Heizen beschleunigter Trocknungsvorgang folgt.
- Verfahren nach einem der Ansprüche 1 bis 5, wobei der Nitrier- oder Nitrocarburierschritt bei einer Temperatur von 550 °C bis 650 °C während mindestens 45 Minuten in einem Bad aus geschmolzenen Salzen durchgeführt wird, das 14 bis 44 Gewichts-% Alkalicyanate enthält.
- Verfahren nach Anspruch 6, in welchem das Nitrier- oder Nitrocarburierbad 14 bis 18 Gewichtsprozent Alkalicyanate enthält.
- Verfahren nach Anspruch 6 oder Anspruch 7, in welchem die Nitrier- oder Nitrocarburierbehandlung bei einer Temperatur von 590 °C während 90 Minuten bis 100 Minuten durchgeführt wird.
- Verfahren nach Anspruch 6 oder Anspruch 7, in welchem die Nitrier- oder Nitrocarburierbehandlung bei einer Temperatur von 630 °C während etwa 45 Minuten bis 50 Minuten durchgeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 5, in welchem der Nitrocarburierschritt in einem gasförmigen Medium, das Ammoniak enthält, zwischen 500 °C und 600 °C durchgeführt wird.
- Verfahren nach einem der Ansprüche 1 bis 5, in welchem der Nitrier- oder Nitrocarburierschritt in einem ionischen Medium durchgeführt wird, das ein Plasma bildet und mindestens Stickstoff und Wasserstoff unter vermindertem Druck umfasst.
- Verfahren nach einem der Ansprüche 1 bis 11, wobei der Nitrier- oder Nitrocarburierschritt derart durchgeführt wird, dass eine Verbindungsschicht mit einer Dicke gebildet wird, die mindestens gleich 10 Mikrometern ist.
- Verfahren nach einem der Ansprüche 1 bis 12, wobei der Oxidationsschritt in einem Bad aus geschmolzenen Salzen durchgeführt wird, das Alkalinitrate, Alkalicarbonate und Alkalihydroxide enthält.
- Verfahren nach Anspruch 13, in welchem der Oxidationsschritt bei einer Temperatur von 430 °C bis 470 °C während 15 bis 20 Minuten vollzogen wird.
- Verfahren nach einem der Ansprüche 1 bis 12, wobei der Oxidationsschritt in einem wässrigen Bad durchgeführt wird, das Alkalihydroxide, Alkalinitrate und Alkalinitrite enthält.
- Verfahren nach Anspruch 15, in welchem der Oxidationsschritt bei einer Temperatur von 110 °C bis 130 °C während 15 bis 20 Minuten vollzogen wird.
- Verfahren nach einem der Ansprüche 1 bis 12, in welchem der Oxidationsschritt bei einer Temperatur von 450 °C bis 550 °C während 30 bis 120 Minuten in einem überwiegend aus Wasserdampf bestehenden gasförmigen Medium durchgeführt wird.
- Stahlteil, das eine erhöhte Widerstandsfähigkeit gegen Verschleiß und Korrosion aufweist, erhalten durch das Verfahren nach einem der Ansprüche 1 bis 17, welches eine Verbindungsschicht von mindestens 8 Mikrometern, eine Schicht aus Oxiden mit einer zwischen 0,1 und 3 Mikrometern liegenden Dicke und eine Imprägnierungsschicht umfasst, die grifftrocken ist.
- Stahlteil nach Anspruch 18, dadurch gekennzeichnet, dass die Verbindungsschicht aus Eisennitriden der ε- und/oder γ'-Phasen besteht.
- Stahlteil nach einem der Ansprüche 18 oder 19, dadurch gekennzeichnet, dass die Verbindungsschicht eine Dicke von mindestens 10 µm aufweist.
- Stahlteil nach Anspruch 20, dadurch gekennzeichnet, dass die Dicke der Verbindungsschicht zwischen 10 µm und 25 µm liegt.
- Stahlteil nach einem der Ansprüche 18 bis 21, dadurch gekennzeichnet, dass die Imprägnierungsschicht mindestens ein Paraffinöl umfasst, das sich aus einem C16- bis C32-Schnitt von Alkanen zusammensetzt.
- Stahlteil nach einem der Ansprüche 18 bis 22, dadurch gekennzeichnet, dass die Imprägnierungsschicht mindestens ein synthetisches Phenol-Additiv umfasst.
- Stahlteil nach Anspruch 23, dadurch gekennzeichnet, dass das synthetische Phenol-Additiv eine Verbindung der Formel C15H24O ist.
- Stahlteil nach einem der Ansprüche 18 bis 24, dadurch gekennzeichnet, dass die Imprägnierungsschicht zudem mindestens ein Additiv umfasst, welches aus der Gruppe bestehend aus Calcium- oder Natriumsulfonat, Phosphiten, Diphenylaminen, Zinkdithiophosphat, Nitriten und Phosphoramiden ausgewählt ist.
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SI201531209T SI3237648T1 (sl) | 2014-12-23 | 2015-12-15 | Postopek za površinsko obdelavo kosa jekla z nitriranjem ali nitrokarboriranjem, oksidiranjem, potem impregniranjem |
PL15821125T PL3237648T3 (pl) | 2014-12-23 | 2015-12-15 | Sposób obróbki powierzchniowej elementu ze stali poprzez azotowanie albo węgloazotowanie, oksydowanie, a następnie impregnację |
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FR1463252A FR3030578B1 (fr) | 2014-12-23 | 2014-12-23 | Procede de traitement superficiel d'une piece en acier par nitruration ou nitrocarburation, oxydation puis impregnation |
PCT/FR2015/053511 WO2016102813A1 (fr) | 2014-12-23 | 2015-12-15 | Procédé de traitement superficiel d'une pièce en acier par nitruration ou nitrocarburation, oxydation puis imprégnation |
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US (1) | US10774414B2 (de) |
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CN108359785B (zh) * | 2018-03-19 | 2019-12-17 | 盐城工学院 | 一种W6Mo5Cr4V2高速钢拉刀的强韧化处理方法 |
CN110423977B (zh) * | 2019-09-05 | 2021-06-18 | 合肥工业大学 | 一种以化学浸镀铁为预处理的铝材料气体渗氮方法 |
FR3105262B1 (fr) * | 2019-12-24 | 2022-04-15 | Hydromecanique & Frottement | Procédé et installation de traitement d’une pièce en métal ferreux |
RU2736289C1 (ru) * | 2020-03-05 | 2020-11-13 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ростовский государственный университет путей сообщения" (ФГБОУ ВО РГУПС) | Способ азотирования деталей из легированных сталей |
RU2737796C1 (ru) * | 2020-03-05 | 2020-12-03 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ростовский государственный университет путей сообщения" (ФГБОУ ВО РГУПС) | Состав компаунда для азотирования деталей из легированных сталей |
CN111423817A (zh) * | 2020-05-28 | 2020-07-17 | 眉山市三泰铁路车辆配件有限公司 | 一种铸铁制品专用的气体qpq耦合剂及其制备方法 |
US11590485B2 (en) | 2021-01-13 | 2023-02-28 | Saudi Arabian Oil Company | Process for modifying a hydroprocessing catalyst |
CN112935737A (zh) * | 2021-03-25 | 2021-06-11 | 上齿集团有限公司 | 一种新型螺旋锥齿轮干切齿方法 |
FR3141702A1 (fr) * | 2022-11-07 | 2024-05-10 | Hydromecanique Et Frottement | Liquide d’imprégnation, procédé de traitement avec un tel liquide d’imprégnation, et pièce traitée obtenue |
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JPS5977138A (ja) * | 1982-10-26 | 1984-05-02 | Aisin Chem Co Ltd | 車輌用摩擦材 |
GB8310102D0 (en) | 1983-04-14 | 1983-05-18 | Lucas Ind Plc | Corrosion resistant steel components |
JPH0257735A (ja) * | 1988-08-19 | 1990-02-27 | Toyoda Gosei Co Ltd | 防振ゴム |
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FR2672059B1 (fr) * | 1991-01-30 | 1995-04-28 | Stephanois Rech Mec | Procede pour conferer a des pieces en metal ferreux, nitrurees puis oxydees, une excellente resistance a la corrosion tout en conservant les proprietes acquises de friction. |
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FR2679258B1 (fr) * | 1991-07-16 | 1993-11-19 | Centre Stephanois Recherc Meca | Procede de traitement de pieces en metal ferreux pour ameliorer simultanement leur resistance a la corrosion et leurs proprietes de friction. |
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FR2812888B1 (fr) * | 2000-08-14 | 2003-09-05 | Stephanois Rech Mec | Procede de traitement superficiel de pieces mecaniques soumise a la fois a l'usure et a la corrosion |
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RU2230825C2 (ru) * | 2002-08-30 | 2004-06-20 | Общество с ограниченной ответственностью "Борец" | Способ химико-термической обработки материала на основе порошковых сплавов железа и деталь ступени погружного центробежного насоса |
FR2972459B1 (fr) | 2011-03-11 | 2013-04-12 | Hydromecanique & Frottement | Bains de sels fondus pour la nitruration de pieces mecaniques en acier, et un procede de mise en oeuvre |
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