EP1865088B1 - Verfahren zum Härten von Edelstahl und Salzschmelze zur Durchführung des Verfahrens - Google Patents
Verfahren zum Härten von Edelstahl und Salzschmelze zur Durchführung des Verfahrens Download PDFInfo
- Publication number
- EP1865088B1 EP1865088B1 EP07010534A EP07010534A EP1865088B1 EP 1865088 B1 EP1865088 B1 EP 1865088B1 EP 07010534 A EP07010534 A EP 07010534A EP 07010534 A EP07010534 A EP 07010534A EP 1865088 B1 EP1865088 B1 EP 1865088B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- weight
- molten salt
- carbon
- chloride
- stainless steel
- 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.)
- Active
Links
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 52
- 239000010935 stainless steel Substances 0.000 title claims abstract description 43
- 150000003839 salts Chemical class 0.000 title claims description 50
- 238000000034 method Methods 0.000 title claims description 30
- 238000005496 tempering Methods 0.000 title 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 34
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 30
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims abstract description 19
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 37
- 239000000126 substance Substances 0.000 claims description 28
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 18
- 229910001626 barium chloride Inorganic materials 0.000 claims description 18
- 239000001103 potassium chloride Substances 0.000 claims description 17
- 235000011164 potassium chloride Nutrition 0.000 claims description 17
- AWDBHOZBRXWRKS-UHFFFAOYSA-N tetrapotassium;iron(6+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+6].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] AWDBHOZBRXWRKS-UHFFFAOYSA-N 0.000 claims description 16
- 229910001631 strontium chloride Inorganic materials 0.000 claims description 15
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 claims description 15
- 239000012190 activator Substances 0.000 claims description 13
- 238000009792 diffusion process Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- -1 tetracyano zinc compound Chemical class 0.000 claims description 6
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- MNWBNISUBARLIT-UHFFFAOYSA-N sodium cyanide Chemical compound [Na+].N#[C-] MNWBNISUBARLIT-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 229910020344 Na2Zn Inorganic materials 0.000 claims 1
- 238000006073 displacement reaction Methods 0.000 claims 1
- VUNCZJSMIYWESS-UHFFFAOYSA-N nickel;tetracyanide Chemical compound [Ni].N#[C-].N#[C-].N#[C-].N#[C-] VUNCZJSMIYWESS-UHFFFAOYSA-N 0.000 claims 1
- 230000002265 prevention Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 6
- 239000012298 atmosphere Substances 0.000 abstract description 3
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 abstract description 2
- 239000012266 salt solution Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 229910000831 Steel Inorganic materials 0.000 description 23
- 239000010959 steel Substances 0.000 description 23
- 238000005260 corrosion Methods 0.000 description 21
- 230000007797 corrosion Effects 0.000 description 21
- 239000011651 chromium Substances 0.000 description 17
- 239000000155 melt Substances 0.000 description 17
- 229910052804 chromium Inorganic materials 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 10
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 10
- 239000002184 metal Substances 0.000 description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 150000002825 nitriles Chemical class 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 7
- 238000005121 nitriding Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 6
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 description 6
- GVEHJMMRQRRJPM-UHFFFAOYSA-N chromium(2+);methanidylidynechromium Chemical compound [Cr+2].[Cr]#[C-].[Cr]#[C-] GVEHJMMRQRRJPM-UHFFFAOYSA-N 0.000 description 6
- 229910003470 tongbaite Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- NAVJNPDLSKEXSP-UHFFFAOYSA-N Fe(CN)2 Chemical class N#C[Fe]C#N NAVJNPDLSKEXSP-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910001566 austenite Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000005255 carburizing Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 150000001247 metal acetylides Chemical class 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 230000018199 S phase Effects 0.000 description 2
- XDOQMROXMLWOHR-UHFFFAOYSA-N [Ba].NC#N Chemical compound [Ba].NC#N XDOQMROXMLWOHR-UHFFFAOYSA-N 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JORQDGTZGKHEEO-UHFFFAOYSA-N lithium cyanide Chemical compound [Li+].N#[C-] JORQDGTZGKHEEO-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- GKKCIDNWFBPDBW-UHFFFAOYSA-M potassium cyanate Chemical compound [K]OC#N GKKCIDNWFBPDBW-UHFFFAOYSA-M 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- IEORSVTYLWZQJQ-UHFFFAOYSA-N 2-(2-nonylphenoxy)ethanol Chemical group CCCCCCCCCC1=CC=CC=C1OCCO IEORSVTYLWZQJQ-UHFFFAOYSA-N 0.000 description 1
- BFSUQRCCKXZXEX-UHFFFAOYSA-N 2-methoxypropan-2-ol Chemical compound COC(C)(C)O BFSUQRCCKXZXEX-UHFFFAOYSA-N 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- RMXTYBQNQCQHEU-UHFFFAOYSA-N ac1lawpn Chemical compound [Cr]#[Cr] RMXTYBQNQCQHEU-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- SJKRCWUQJZIWQB-UHFFFAOYSA-N azane;chromium Chemical compound N.[Cr] SJKRCWUQJZIWQB-UHFFFAOYSA-N 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
- UNLSXXHOHZUADN-UHFFFAOYSA-N barium cyanide Chemical compound [Ba+2].N#[C-].N#[C-] UNLSXXHOHZUADN-UHFFFAOYSA-N 0.000 description 1
- 229910001422 barium ion Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 description 1
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 description 1
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 150000001913 cyanates Chemical class 0.000 description 1
- 238000007333 cyanation reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000011551 heat transfer agent Substances 0.000 description 1
- UETZVSHORCDDTH-UHFFFAOYSA-N iron(2+);hexacyanide Chemical compound [Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] UETZVSHORCDDTH-UHFFFAOYSA-N 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 238000007734 materials engineering Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 239000011833 salt mixture Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
Images
Classifications
-
- 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
- C21D1/34—Methods of heating
- C21D1/44—Methods of heating in heat-treatment baths
- C21D1/46—Salt baths
-
- 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
- C23C8/42—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 only one element being applied
- C23C8/44—Carburising
- C23C8/46—Carburising of ferrous surfaces
-
- 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
- C23C8/42—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 only one element being applied
- C23C8/48—Nitriding
- C23C8/50—Nitriding of ferrous surfaces
-
- 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
- C23C8/52—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 one step
- C23C8/54—Carbo-nitriding
- C23C8/56—Carbo-nitriding of ferrous surfaces
Definitions
- the invention relates to a method for hardening stainless steel and a molten salt for carrying out the method.
- stainless steel Due to its excellent corrosion resistance, stainless steel is used in chemical apparatus engineering, in food technology, in the petrochemical industry, in the offshore sector, in shipbuilding and aircraft construction, in architecture, in building construction and equipment construction and in many other industrial sectors.
- the steel is generally not sufficiently resistant to corrosion to be considered stainless steel.
- the content of metallic chromium in the steel is thus an important criterion for the Corrosion resistance, as in P. Gümpel et al. Stainless Steels, Expert Verlag, Volume 349, Renningen Malmsheim 1998 is executed.
- a major disadvantage of most common stainless steels such as 1.4301, 1.4441, 1.4541 or 1.4575 is that these steels are quite soft and thus susceptible to scratching the surface by hard particles such as dust or sand.
- Most stainless steels - except for the very special martensitic stainless steels - are not hardenable by physical methods such as annealing and quenching. The low surface hardness often hinders the use of stainless steel.
- Another disadvantage of most stainless steels is their strong tendency to seize, i. for welding the surface of two mutually sliding surfaces due to adhesion.
- thermochemical treatment e.g. By nitriding or nitrocarburizing in gas (under ammonia atmosphere), in plasma (under nitrogen / argon) or in molten salt (in molten cyanates), the surface of stainless steel can be enriched with nitrogen to form iron and chromium nitrides.
- the resulting layers form out of the material, so they are - unlike galvanic or physical layers - not applied from the outside and therefore extremely adherent.
- hard layers of 5 to 50 ⁇ m thickness are formed. The hardness of such nitrided or nitrocarburized layers on stainless steel reaches over 1000 units on the Vickers hardness scale due to the high hardness of the resulting iron and chromium nitrides.
- nitrided or nitrocarburized layers on stainless steel The problem with the practical use of such nitrided or nitrocarburized layers on stainless steel is that although these layers are hard, they lose their corrosion resistance.
- the reason for this is the relatively high treatment temperature, which is around 580 ° C during nitriding or nitrocarburizing.
- the diffusing elements form nitrogen and carbon with the chromium-stable chromium nitride (CrN) or chromium carbides (Cr 7 C 3 ) in the area of the component surface.
- the corrosion resistance-free free chromium is removed from the stainless steel matrix to a depth of about 50 ⁇ m below the surface and converted into chromium nitride or chromium carbide.
- the surface of the component becomes hard due to the formation of iron and chromium nitride, but it is susceptible to corrosion. In use, such layers are rapidly worn away due to corrosion.
- a hard and at the same time corrosion-resistant layer can be thermochemically produced by the so-called Kolsterizing® on stainless steel.
- This process is for example in Kolster by® - corrosion-resistant surface hardening of austenitic stainless steel - Information Sheet of Bodycote Hardiffbv, Parimariboweg 45, NL-7333 Apeldoorn, info@hardiff.de and M. Wägner Increasing the wear resistance of stainless steels. Steel STEEL No. 2 (2004) 40-43 mentioned.
- the conditions of the process are described neither in the patent literature nor in the generally accessible scientific literature.
- treated components have a hard, wear-resistant layer between 10 and 20 microns thick, the corrosion resistance of the base material remains.
- Kolsterised® components must not be heated above 400 ° C, otherwise they will lose their corrosion resistance.
- the workpiece to be cured is first surface activated by treatment with an acid and then treated in a heated fluidized bed containing active nitrogen and preferably also active carbon capable of diffusing into the workpiece.
- a method for carburizing austenitic metal is described. According to this method, the metal is kept in a fluorine-containing or fluoride-containing guest atmosphere under heating prior to carburizing. The carburizing of the metal is then carried out at a temperature of at most 680 ° C.
- US-A-19996269 discloses a melt for curing iron parts comprising the following components: 50 parts of barium chloride, 25 parts of sodium chloride, 25 parts of potassium chloride, 5-10 parts of sodium cyanide and 3-5% of a mixture of 1 part of strontium chloride and 7 parts of barium chloride.
- JP-A-52123345 discloses a melt for nitriding iron at 690 ° C comprising the following components: 15% potassium chloride, 15% sodium chloride, 80% barium chloride, sodium titanate and potassium hexacyanoferrate.
- the invention has for its object to provide a cost-effective rational method by means of which a hardening of stainless steel is made possible, in which the corrosion resistance of the stainless steel is maintained as much as possible.
- the molten salt according to the invention comprises the following components: 30-60% by weight Potassium chloride (KCL) 20-40% by weight Lithium chloride (LiCl) 15-30% by weight an activator substance consisting of barium chloride (BaCl 2 ) and / or strontium chloride (SrCl 2 ) and / or magnesium chloride (MgCl 2 ) and / or calcium chloride (CaCl 2 ) 0.2-25% by weight a carbon donating substance consisting of a free cyanide and / or a complex cyanide.
- KCL Potassium chloride
- LiCl Lithium chloride
- BaCl 2 barium chloride
- SrCl 2 strontium chloride
- MgCl 2 magnesium chloride
- CaCl 2 calcium chloride
- the present invention avoids high equipment and energy costs and makes use of a light, easy for less qualified personnel easily executable procedure.
- the invention further enhances the tendency of the stainless steel to eat, i. For cold welding and thus the adhesive wear significantly reduced.
- the hardness of the surface of the stainless steel is increased from 200 - 300 Vickers to values up to 1000 Vickers, which results in a high scratch resistance.
- the use of the molten salt according to the invention makes it possible to harden stainless steel while maintaining its corrosion resistance.
- the method according to the invention is based on the following principle
- these processes using the molten salt of the invention are used as a reactive medium and as a heat transfer agent.
- the molten salt according to the invention contains constituents from which diffusible carbon and / or nitrogen can be liberated and suitable activator substances which cause the release of diffusible nitrogen and / or carbon at low temperatures. It is essential that the treatment temperatures in the molten salt below 450 ° C and are particularly advantageous to lower than the formation temperature of chromium carbide (420 - 440 ° C) or chromium nitride (350 - 370 ° C) to the formation of nitrides and To avoid carbides in the steel matrix completely or as far as possible.
- the concentration of the active carbon or nitrogen donating substances in the form of complex or free cyanides in the molten salt of the invention is very high compared with the concentration of corresponding substances (ammonia, methane, carbon monoxide) in gas atmospheres or in a plasma.
- the relatively long treatment times required for the method according to the invention are based on the fact that the diffusion rate of C and N is a function of the temperature and decreases significantly at temperatures below 450 ° C. At the low temperatures necessary to avoid chromium carbide and chromium nitride formation, long diffusion times of 12 to 60 hours must be used.
- Austenitic stainless steels or so-called duplex steels (ferritic-austenitic steels) are against such long heat treatment times very insensitive and change their other mechanical properties or the structure as good as not.
- the molten salt consists of a salt mixture of potassium chloride, barium chloride and lithium chloride.
- a melt of strontium chloride, potassium chloride and lithium chloride can be used.
- magnesium chloride and / or calcium chloride instead of barium chloride or strontium chloride.
- the melting points of the eutectic mixtures of these salts are from 320 ° C to 350 ° C.
- the salt should be dried for at least 12 to 24 hours at 120-140 ° C before the addition and freed from the water of crystallization, since it contains 3 mol equivalents of water of crystallization in the form supplied.
- the red potassium hexacyanoferrate (III) that is, K 3 Fe (CN) 6 , which contains no water of crystallization, can be added to the melt.
- the amount of complex cyanide added is in the range of 2 to 10% by weight.
- complex metal cyanides can also be used as carbon donors.
- these are tetracyanoxide or tetracyanozinc compounds, for example Na 2 Ni (CN) 4 or Na 2 Zn (CN) 4 .
- complex nontoxic iron cyanides or metal cyanides and sodium and / or potassium cyanide can be added in free form, in an amount of 0.1 to 25 wt.%, Preferably between 3 and 10 wt.%.
- the results are similar to the use of complex cyanides, and mixtures of complex and free cyanides can also be used.
- molten salts with complex cyanides is that it does not handle toxic substances because hexacyanoferrate is non-toxic per se.
- the decay is very slow.
- the carbon formed during the decomposition diffuses into the austenitic stainless steel to be hardened and remains there at temperatures below 420 ° C. in solid, saturated or supersaturated solution.
- Austenite has a high solubility for carbon, a lower one for nitrogen.
- Part of the resulting nitrogen also diffuses into the stainless steel surface. If the treatment temperature is below 350 - 370 ° C, so does the nitrogen - like the carbon - in solid solution, the temperature is between 370 ° C and 420 ° C, so the nitrogen forms with the alloying element chromium chromium nitride and thus potentially reduce the corrosion resistance of stainless steel on the surface. However, even in this temperature range, a formation of chromium carbide is still avoided, so that the alloy matrix of the stainless steel, despite the Chromnitridön given in this temperature range still little chromium is removed, so that reducing the corrosion resistance of the stainless steel may still be acceptable.
- Cyanide ions which resulted from the decomposition of the complex metal salt, are oxidized to cyanate ions by atmospheric oxygen, which is omnipresent in the melt. These can decompose to form carbon monoxide and nitrogen. Cyanations are usually the source of diffusible nitrogen. However, cyanide ions can also be further oxidized to carbonate ions, resulting in carbon monoxide. Carbon monoxide can continue to react with carbon dioxide by releasing diffusible carbon.
- cyanide can react with barium ions of the activator substance contained as barium chloride in the molten salt to barium cyanide Ba (CN) 2 , which turns into barium cyanamide BaNCN. This releases carbon, which can diffuse into the components.
- the barium cyanamide further reacts with atmospheric oxygen to form barium carbonate and nitrogen which is released. Similar reactions are to be expected with strontium, calcium and magnesium, if strontium chloride, calcium chloride or magnesium chloride is used as the activator substance.
- strontium, calcium and magnesium if strontium chloride, calcium chloride or magnesium chloride is used as the activator substance.
- the alkaline earth metals in the form of their halides thus form in the process according to the invention activator substances which bring about the release of diffusible nitrogen and carbon in the temperature range of the process according to the invention. Without the participation of at least one alkaline earth element of the series magnesium, calcium, strontium and barium, the diffusion of the necessary carbon into the stainless steel surface is not possible.
- the other alkali metals Na, K, Rb and Cs do not show this effect.
- An analytical control of the molten salts according to the invention can be carried out as follows:
- the change in the concentration of the active Ingredients can be monitored by potentiometric titration.
- K 4 Fe (CN) 6 can be titrated with cerium (IV) sulfate solution.
- Free cyanide can be determined very well with nickel (II) sulfate. Consumed cyanide or complex cyanide is added accordingly.
- an inert gas such as argon, nitrogen or carbon dioxide may be introduced therein.
- the molten salt can be operated in a closed retort using nitrogen, argon or carbon dioxide as a protective gas.
- a crucible made of heat-resistant steel e.g. from the material 1.4828, 42 kg dry potassium chloride, 34 kg dry lithium chloride and 20 kg barium chloride siccum weighed and mixed loosely. All salts must have a residual moisture content of less than 0.3% by weight.
- the mixture is heated to 400 ° C and gives a water-clear melt.
- 4 kg of potassium hexacyanoferrate (II) are slowly added, which had previously been dried for 12 h at 140 ° C in a muffle furnace.
- the potassium hexacyanoferrate (II) is introduced, a very small amount of carbon deposits on the crucible wall and on the surface of the melt. This carbon is skimmed off with a sifting spoon.
- a water-clear melt is present, which is brought to an operating temperature of 400 ° C.
- V2A stain is a mixture of 100 ml of water and conc. 100 ml of hydrochloric acid. (HCI, 30%) and 0.3% "bird's reagent".
- Vogel's reagent is a mixture of 60% 2-methoxy-2-propanol (H3C-O-CH2Oh-CH3) 5% thiourea (H2N-CS-NH2) 5% nonylphenol ethoxylate residue ethanol.
- the cross section is photographically in FIG. 1 shown in a 500-fold magnification.
- the surface hardness of this layer is determined to be 642 - 715 HV (0.5) or 1100 - 1210 HV (0.025).
- the element distribution within the layer can be determined by glow discharge spectroscopy (GDOES) and is exemplified in FIG. 2 shown.
- GDOES glow discharge spectroscopy
- FIG. 2 is the penetration depth of the elements N, C, Fe, Cr 2 , Ni, Mo shown in the surface of the cured with the molten salt workpiece, that is, the mass concentrations of these elements in percent, depending on the depth in the workpiece in microns.
- FIG. 3 shows the hardness curve as a function of the depth (in ⁇ m) for this workpiece.
- the hardness profile was measured by the Vickers method under a test load of 0.010 kp (10 grams).
- the hardness of the workpiece is significantly increased.
- the result of this treatment is a 10-25 ⁇ m thick diffusion layer on the surface of the treated components and samples. which can be made visible metallographically by a cross-section and etching with the etchant V2A-stain.
- the result of this treatment is an approx. 10 ⁇ m thick diffusion layer on the surface of the treated components and samples, which can be made visible metallographically by cross-sectioning and etching with the etchant V2A-stain.
- the hardness of this layer is determined to be 620 HV (0.5).
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PL07010534T PL1865088T3 (pl) | 2006-06-09 | 2007-05-26 | Sposób hartowania stali szlachetnej oraz stopiona sól do realizacji tego sposobu |
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US (1) | US7909943B2 (pt) |
EP (1) | EP1865088B1 (pt) |
JP (1) | JP5101173B2 (pt) |
KR (1) | KR20070118008A (pt) |
CN (1) | CN101235477B (pt) |
AT (1) | ATE443163T1 (pt) |
BR (1) | BRPI0702568B1 (pt) |
CA (1) | CA2591244A1 (pt) |
DE (2) | DE102006026883B8 (pt) |
ES (1) | ES2331383T3 (pt) |
MX (1) | MX2007006969A (pt) |
PL (1) | PL1865088T3 (pt) |
ZA (1) | ZA200704591B (pt) |
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DE202005008582U1 (de) * | 2005-05-31 | 2005-07-28 | Arnold & Stolzenberg Gmbh | Rollenkette |
JP5148209B2 (ja) * | 2007-08-28 | 2013-02-20 | 学校法人同志社 | 溶融塩電気化学プロセスを用いた表面窒化処理方法 |
DE102007051949B3 (de) | 2007-10-31 | 2009-03-12 | Durferrit Gmbh | Verfahren zum Härten von Oberflächen von Werkstücken aus Edelstahl und Verwendung einer Salzschmelze zur Durchführung des Verfahrens |
DE102007059229A1 (de) * | 2007-11-19 | 2009-05-20 | Konrad Damasko | Verfahren zum Herstellen eines Bauteils mit gehärteter Oberfläche |
US9101896B2 (en) * | 2010-07-09 | 2015-08-11 | Sri International | High temperature decomposition of complex precursor salts in a molten salt |
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 |
DE102011087960A1 (de) * | 2011-12-08 | 2013-06-13 | Witzenmann Gmbh | Flexibles Metallelement und Verfahren zum Herstellen eines flexiblen Metallelements |
DE102012018551A1 (de) * | 2012-09-20 | 2014-03-20 | Wika Alexander Wiegand Se & Co. Kg | Edelstahlrohr mit Randhärtung |
EP2886668B1 (de) | 2013-12-19 | 2018-12-12 | Groz-Beckert KG | Textilwerkzeug und dessen Herstellungsverfahren |
CN104060216A (zh) * | 2014-06-12 | 2014-09-24 | 江苏海纳机电集团有限公司 | 一种不锈钢表面获得过饱和固溶体的盐浴硬化处理方法 |
DE102016215709A1 (de) * | 2015-08-28 | 2017-03-02 | Tsubakimoto Chain Co. | Kettenkomponente und Kette |
US11352508B2 (en) * | 2018-01-19 | 2022-06-07 | Dynalene Inc. | Molten salt inhibitor and method for corrosion protection of a steel component |
WO2020004667A1 (ja) | 2018-06-29 | 2020-01-02 | ワークソリューション株式会社 | 医療器具、医療装置、医療器具の製造方法、及び、金属製物品 |
EP3620408A1 (en) | 2018-08-31 | 2020-03-11 | John Bean Technologies Corporation | Hardened components in a conveyor drive system |
JP7178832B2 (ja) * | 2018-08-31 | 2022-11-28 | 日本パーカライジング株式会社 | 表面硬化材料の製造方法 |
US10889448B2 (en) | 2018-10-30 | 2021-01-12 | John Bean Technologies Corporation | Systems and methods for chain wear elongation measurement and drive compensation |
CN113106381B (zh) * | 2020-12-28 | 2023-05-02 | 上海锐力医疗器械有限公司 | 一种奥氏体不锈钢医用缝合针盐浴氮化配方及其加工方法 |
CN113897579A (zh) * | 2021-09-30 | 2022-01-07 | 成都工具研究所有限公司 | 一种316l不锈钢工件低温qpq处理工艺 |
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US1996269A (en) * | 1930-06-07 | 1935-04-02 | Degussa | Method of case-hardening iron articles |
US2248732A (en) * | 1939-05-16 | 1941-07-08 | Degussa | Process for the hardening of steel |
DE1007795B (de) * | 1955-04-27 | 1957-05-09 | Degussa | Verfahren zum Aufkohlen von Eisen und Stahl und Salzgemisch |
JPS5848026B2 (ja) * | 1976-04-09 | 1983-10-26 | 芳夫 和仁 | 低温窒化法 |
DE3048607C2 (de) * | 1980-12-23 | 1983-07-07 | Goerig & Co GmbH & Co KG, 6800 Mannheim | Cyanidfreies Verfahren zum Aufkohlen von Stahl und Zugabesalz zur Durchführung des Verfahrens |
JPS60215756A (ja) | 1984-01-27 | 1985-10-29 | プロセダイン コ−ポレイシヨン | ステンレス鋼の硬化方法 |
CN85103190A (zh) * | 1985-04-22 | 1986-01-10 | 云南工学院 | 金属表面强化盐浴热处理工艺 |
JPS62256957A (ja) * | 1986-05-01 | 1987-11-09 | Kazuto Takamura | 低温塩浴軟窒化剤 |
DE69510719T2 (de) | 1994-04-18 | 1999-12-09 | Daido Hoxan Inc., Sapporo | Verfahren zur Aufkohlung von austenitischem Metall |
US6093303A (en) * | 1998-08-12 | 2000-07-25 | Swagelok Company | Low temperature case hardening processes |
TW557330B (en) * | 2000-11-29 | 2003-10-11 | Parker Netsushori Kogyo Kk | Improved salt bath nitrogenating method for corrosion-resistant iron material and iron units |
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2006
- 2006-06-09 DE DE102006026883A patent/DE102006026883B8/de not_active Expired - Fee Related
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2007
- 2007-05-26 PL PL07010534T patent/PL1865088T3/pl unknown
- 2007-05-26 ES ES07010534T patent/ES2331383T3/es active Active
- 2007-05-26 AT AT07010534T patent/ATE443163T1/de active
- 2007-05-26 EP EP07010534A patent/EP1865088B1/de active Active
- 2007-05-26 DE DE502007001522T patent/DE502007001522D1/de active Active
- 2007-06-05 CA CA002591244A patent/CA2591244A1/en not_active Abandoned
- 2007-06-05 KR KR1020070054825A patent/KR20070118008A/ko not_active Application Discontinuation
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JP5101173B2 (ja) | 2012-12-19 |
ATE443163T1 (de) | 2009-10-15 |
ZA200704591B (en) | 2008-08-27 |
PL1865088T3 (pl) | 2010-01-29 |
CN101235477B (zh) | 2011-05-18 |
MX2007006969A (es) | 2008-10-30 |
JP2007332459A (ja) | 2007-12-27 |
EP1865088A1 (de) | 2007-12-12 |
BRPI0702568B1 (pt) | 2015-10-13 |
US7909943B2 (en) | 2011-03-22 |
KR20070118008A (ko) | 2007-12-13 |
BRPI0702568A (pt) | 2008-02-19 |
DE102006026883B8 (de) | 2007-10-04 |
ES2331383T3 (es) | 2009-12-30 |
DE102006026883B3 (de) | 2007-08-16 |
US20080099108A1 (en) | 2008-05-01 |
CA2591244A1 (en) | 2007-12-09 |
CN101235477A (zh) | 2008-08-06 |
DE502007001522D1 (de) | 2009-10-29 |
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