GB2212521A - Method for post-treatment of plated steel sheet for soldering - Google Patents
Method for post-treatment of plated steel sheet for soldering Download PDFInfo
- Publication number
- GB2212521A GB2212521A GB8726833A GB8726833A GB2212521A GB 2212521 A GB2212521 A GB 2212521A GB 8726833 A GB8726833 A GB 8726833A GB 8726833 A GB8726833 A GB 8726833A GB 2212521 A GB2212521 A GB 2212521A
- Authority
- GB
- United Kingdom
- Prior art keywords
- post
- treatment solution
- treatment
- steel sheet
- plated 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.)
- Granted
Links
- 238000011282 treatment Methods 0.000 title claims description 62
- 229910000831 Steel Inorganic materials 0.000 title claims description 45
- 239000010959 steel Substances 0.000 title claims description 45
- 238000000034 method Methods 0.000 title claims description 17
- 238000005476 soldering Methods 0.000 title claims description 10
- 150000002148 esters Chemical class 0.000 claims description 26
- 239000000194 fatty acid Substances 0.000 claims description 24
- -1 polyethylene Polymers 0.000 claims description 22
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 21
- 229930195729 fatty acid Natural products 0.000 claims description 21
- 150000004665 fatty acids Chemical class 0.000 claims description 19
- 150000001412 amines Chemical class 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- 239000004166 Lanolin Substances 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229940039717 lanolin Drugs 0.000 claims description 8
- 229920000573 polyethylene Polymers 0.000 claims description 8
- 239000000344 soap Substances 0.000 claims description 8
- 235000019388 lanolin Nutrition 0.000 claims description 7
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001565 benzotriazoles Chemical class 0.000 claims description 4
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 claims description 3
- BTXXTMOWISPQSJ-UHFFFAOYSA-N 4,4,4-trifluorobutan-2-one Chemical compound CC(=O)CC(F)(F)F BTXXTMOWISPQSJ-UHFFFAOYSA-N 0.000 claims description 3
- BQACOLQNOUYJCE-FYZZASKESA-N Abietic acid Natural products CC(C)C1=CC2=CC[C@]3(C)[C@](C)(CCC[C@@]3(C)C(=O)O)[C@H]2CC1 BQACOLQNOUYJCE-FYZZASKESA-N 0.000 claims description 3
- 239000005711 Benzoic acid Substances 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 235000010233 benzoic acid Nutrition 0.000 claims description 3
- 125000001165 hydrophobic group Chemical group 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 235000003441 saturated fatty acids Nutrition 0.000 claims description 3
- 150000004671 saturated fatty acids Chemical class 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 claims description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims 1
- 229940043237 diethanolamine Drugs 0.000 claims 1
- 238000005260 corrosion Methods 0.000 description 29
- 230000007797 corrosion Effects 0.000 description 26
- 229910000679 solder Inorganic materials 0.000 description 18
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 230000032683 aging Effects 0.000 description 10
- 230000007423 decrease Effects 0.000 description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 7
- 230000004907 flux Effects 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 239000012188 paraffin wax Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910020816 Sn Pb Inorganic materials 0.000 description 4
- 229910020922 Sn-Pb Inorganic materials 0.000 description 4
- 229910008783 Sn—Pb Inorganic materials 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical class C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 229910020220 Pb—Sn Inorganic materials 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 229940088990 ammonium stearate Drugs 0.000 description 2
- JPNZKPRONVOMLL-UHFFFAOYSA-N azane;octadecanoic acid Chemical compound [NH4+].CCCCCCCCCCCCCCCCCC([O-])=O JPNZKPRONVOMLL-UHFFFAOYSA-N 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- WHOZNOZYMBRCBL-OUKQBFOZSA-N (2E)-2-Tetradecenal Chemical compound CCCCCCCCCCC\C=C\C=O WHOZNOZYMBRCBL-OUKQBFOZSA-N 0.000 description 1
- QULUVEPNTKJBMR-KTKRTIGZSA-N 2-[(z)-octadec-9-enyl]-4,5-dihydro-1h-imidazole Chemical compound CCCCCCCC\C=C/CCCCCCCCC1=NCCN1 QULUVEPNTKJBMR-KTKRTIGZSA-N 0.000 description 1
- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 description 1
- SDEBYHVDMCQKNZ-UHFFFAOYSA-N 4-methoxy-6-piperazin-1-ylpyrimidine;hydrochloride Chemical compound Cl.C1=NC(OC)=CC(N2CCNCC2)=N1 SDEBYHVDMCQKNZ-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- UJEMOXPSTTXLRE-UHFFFAOYSA-N benzotriazol-1-yl(phenyl)methanone Chemical compound N1=NC2=CC=CC=C2N1C(=O)C1=CC=CC=C1 UJEMOXPSTTXLRE-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229940100242 glycol stearate Drugs 0.000 description 1
- OAKJQQAXSVQMHS-UHFFFAOYSA-O hydrazinium(1+) Chemical group [NH3+]N OAKJQQAXSVQMHS-UHFFFAOYSA-O 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009863 impact test Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229940044654 phenolsulfonic acid Drugs 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000007585 pull-off test Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229950004959 sorbitan oleate Drugs 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/226—Non-corrosive coatings; Primers applied before welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
-
- 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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Chemical Treatment Of Metals (AREA)
- Electroplating Methods And Accessories (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
i 11 11 .2212b2'i 1 - METHOD FOR POST-TREATMENT OF PLATED STEEL SHEET FOR
SOLDERING The present invention relates to the post-treatment of plated steel sheet for soldering and especially to the post-treatment solution which exhibits excellent wettability and adhesive strength to solder, hereafter referred to As solderability, as well as excellent corrosion resistance, formability and durability.
Recently, Sn plated steel-sheet, Pb-Sn plated steel sheet, Cu plated steel sheet or Zn plated steel sheet have been used as a plated steel sheet suitable for soldering. However, without post-treatment these plated steel sheets easily corrode during packing or after assembling. Therefore, post-treatments such as chromate treatment, phosphate treatment or coating with anti-corrosion primer 1.5 are applied to said steel sheets.
In the case of chromate treatment, it is not suitable because more than 0. 1 mg/dm 2 of Cr 6+ is necessary in order to provide sufficient corrosion resistance. However, in the 2 6+ case of more than 0.05 mg/dm of Cr, a strong flux is necessary for soldering. The use of strong flux causes deterioration of the working environment and decrease of corrosion resistance of the soldered surface. Therefore, the amount of Cr 6+ is limited to less than 0.05 mg/dm 2 and does not provide sufficient corrosion resistance.
on the other hand, the application of an anti-corrosion primer causes a decrease in solderability similar to - 2 chromate treatment and also a decrease in the corrosion resistance of the soldered location.
There is some prior art relating to a process for production of plated steel sheet for soldering, for example, Japanese Patent Application Laid-Open No. Sho. 61-19793 and Japanese Patent Application Laid-Open No. Sho. 54-15432.
However, the present invention is different from these inventions with regard to construction and materials used.
Japanese Patent Application Laid-open No. Sho. 61-19793 relates to a plated steel sheet having excellent solderability that is summarized as follows: Sn or Sn-Pb alloy is plated on the Zn or Zn type alloy plated steel 2 sheet with the amount of deposit from 0.1 to 100 g/m However, the price of Sn is so expensive that the cost of production is high and use of Pb is undesirable from the viewpoint of environmental pollution. The present invention is different from this invention with regard to construction and materials used.
on the other hand, Japanese Patent Application Laid-Open No. Sho. 54-15432 relates to a post-treatment that is summarized as follows: Zn plated steel sheet is covered with acrylic resin from 0.5 to 20 jun in thickness or paraffin wax from 2 to 20 = in thickness. The present invention is different from this invention with regard to materials used and effects on solderability and corrosion resistance.
BRIEF SUMMARY OF THE INVENTION
The electroplated steel sheet is coated with a post-treatment solution in the range of 0.01 to 2 11m in dry -9 11 m -1 3 - V 1 f.
thickness preferably 0.02 jum or greater. The post-treatment solution contains from 2 to 160 g/l of at least one water-soluble or water-dispersed material such as:
a. fatty alcohols, b. alkylphenols, C. condensates prepared from fatty acids and ethylene oxides, d. polyethylend glycol-alkylamines, e. esters prepared from sorbitan and fatty acids, f. surfactants prepared from polypropylene glycols (as a hydrophobic group) and polyethylene glycols (as a hydrophilic group), 9- amides prepared from fatty acids and diethanol amines, h. esters prepared from fatty acids and sucrose, and i. saponificates prepared from lanolin alcohol or lanolin fatty acids.
Alternatively, there may be employed 2 to 100 g/1 water solubleor waterdispersed halogen-free solder flux such as a. abietic acid, b. benzoic acid, C. saturated fatty acids having 12 to 24'carbon atoms, d. unsaturated fatty acids having 12 to 24 carbon atoms, e. organic alcohols having 2 to 400 carbon atoms, esters of fatty acids, g. derivatives of benzotriazoles and metalates, ammonium salts and amine salts of these materials.
Moreover, there may be employed 5 to 200 g/l of phosphoric esters in the post-treatment solution.
The post-treatment solution may further contain O.bl to 3 g/l of Cr 6+ and/or 10 to 100 g/l of organic amine soap.
DETAILED DESCRIPTION OF THE INVENTION
The detailed method according to the present invention will be described below:
The main components of the present invention are io selected from:
a. water-soluble or water-dispersed fatty al-coh-ol-s, b. alkylphenols, C. condensates prepared from fatty acids and ethylene oxides such as polyethylene glycol alkylphenyl ether, polyethylene glycol alkyl ether and polyethylene glycol-fatty acid esters, d. polyethylene glycol-alkylamines such as N-polyethylene glycol-alkyl amine and polyethylene glycol-alkyl ether, e. esters prepared from sorbitan and fatty acids including sorbitan-fatty acid ester and polyethylene glycol-sorbitan fatty acid ester, f. surfactants prepared from polypropylene glycol (as hydrophobic group) and polyethylene glycol (as hydrophil-ic group) such as polypropylene glycol-polyethylene glycol ether, 9- amides prepared from fatty acid and diethanol amines such as fatty acid-diethanol amides, il h. esters prepared from fatty acids and sucrose such as sucrose-fatty acid esters and i. saponificates prepared from lanolin alcohol or lanolin fatty acid such as polyoxyethylene-lanolin alcohol 5 ester and polyoxyethylene lanolin fatty acid esters.
As the solder flux without halogen there may be mentioned:
a. abietic acid, b. benzoic acid, c. saturated fatty acids which have 12 to 24 carbon atoms, such as stearic acid, lauric acid, palmitic acid, d. unsaturated fatty acids which have 12 to 24 carbon atoms such as oleic acid, e. organic alcohols such as glycerol, ethylene glycol and polyethylene glycol having 4 to 400 carbon atoms, f. esters of fatty acids such as fatty acid-glycerol esters, g. derivatives of benzotriazole such as benzotriazole, azimidole, 1-N-benzoyl-benzotriazole.
Phosphoric esters including soaps with organic amines or mono-basic or di-basic-acids with one or two alkyl groups may be used.
If the alkyl group is large and is not soluble in water, it is possible to add ethylene oxide or neutralize with alkali in order to improve the hydrophilic property. Phosporic esters can be preferably employed in the range of 5 to 200 g/l and at least one is used.
The effects of the present invention are controlled by the amount of posttreatment coating on the plated sheet, 6 - and are not influenced by concentration of post-treatment solution. However, a specified concentration is preferred in order to facilitate operation. Halogen ion is not prefe'ired because it decreases corrosion resistance.
In order to stabilize the post-treatment solution and to improve the corrosion resistance and abrasion resistance, Cr 6+ and/or a soap bf an organic amineare used. A concentration of Cr 6+ oer 3 g/l remarkably decreases solderability and is not suitable.
Soaps of organic amines include dodecylamine, oleoyl imidazoline, aminopropyl beef tallow amine, rosin amine.
The amine may be used as a salt with carbonic acid. The concentration of amine over 100 g/1 has some effects on corrosion resistance but less effect on solderability and is not Preferred.
Moreover, well-known water-soluble or water-dispersible anti-corrosion agents are available, but in this case, it is important to restrict the am6unt ok dddition in o'rder not to decrease the solderability. For example addition of acrylic emulsion increases the abrasion resistance but inversely decreases the solderability.
The PH value of the solution is suitably in the range of from 3 to 10. If the PH of the solution is under 3, the stability of the solution decreases. If the PH of the solution is over 10, drying properties of the post-treatment decrease.
The temperature of the post-treatment is not limited, however, at over 800C, the stability of the post-treatment h - 7 solution decreases, resulting in gelation. An ordinary temperature in the range from 20 to 400C is suitable and economical.
The coating method is not restricted and roll-coating, knife-coating, dipping followed by wringer roll or air-knife treatment are used. The post-treatment product must be sufficiently dry to be handled.
The dry film thickness in the range of 0.01 to 2 jim is suitable. A dry film thickness below 0.01 jim, has no effects on the corrosion resistance. At a dry film thickness above 2 4m, corrosion resistance increases but solderability does not increase.
In the present invention, the post-treatment solution 6+ which may further contain Cr or organic amine soap, can be applied on an Sn plate, Pb-Sn plate, Cu plate or Zn plate.
Solderability and corrosion resistance of said steel sheets increase, even after aging. Steel sheets are not restricted to said steel sheet.
The reason why the properties of the coated steel sheet of the present invention improve, has not been clarified. However, formation of oxides, hydroxides and carbonates is inhibited by coating the present post-treatment solution on said plated steel sheet.
Moreover, it is considered that since the present post-treatment dissolves or reduces the metal oxides which have formed on the plated steel sheet over time, the wetting and diffusion of solder are promoted and solderability is improved. According to said phenomenon, the present - 8 post-treatment film covers the plated steel sheet uniformly and increases the corrosion resistance.
The present invention is based on the above-mentioned concept. By coating the present post-treatment solution on the plated steel sheet uniformly, a plated steel sheet having excellent solderability and corrosion resistance can be continuously produced.
Specific embodiments of the present invention are as follows:
EXAMPLE 1
A cold-rolled steel sheet having thickness of 0.5 mm was used as the substrate and was treated by ordinary alkali cleaning and pickling. After water spraying, the substrates were electroplated.in a sulfuric acid bath at the weight of 5 g/m 2 of Zn deposit and were treated in accordance with the present invention. In this regard, a post-treatment solution containing 10 g/l of ammonium stearate, 20 g/l of glycerol and 5 g/l of. paraffin wax was coated on the Zn plated steel sheet by a dipping method and the thus-coated steel sheet was dried at the temperature of 600C to form a coating of 0.5 jim thickness thereon.
Examples 2-17 of the present invention were treated according to the same procedure as Example 1, except for the type and amount of deposit and post-treatment. COMPARATIVE EXAMPLE I The same substrates as in Example 1 were treated by ordinary alkali cleaning and pickling. After water spraying, the substrate was electroplated in a sulfuric acid h bath at the weight of 10 g/m 2 of Zn deposit and was electroplated in a phenolsulfonic acid bath (400C, 30A/d m 2 according to Japanese Laid-Open Patent Application No. Sho 61-19793. 5 Comparative Example 2 was performed according to Japanese Laid-Open Patent Application No. Sho 54- 15432. Comparative Examples 3-12.were performed according to the same procedure as Comparative Example 2, except for the type and amount of the deposit and post-treatment. The conditions for the post-treatments were summarized in Table 1 and the evaluation of properties was summarized in Tables 2 and 3. As shown in Tables 2 and 3, post-treatment solution of this invention showed excellent effects on corrosion resistance, solderability and aging tests. ordinary chemical treatments such as chromate treatment or phosphate treatment (Comparative Examples 3- 5) showed effects on corrosion resistance but decreased the wettability of the solder particularly after aging. Furthermore, the color of the surface after aging had changed and decreased the corrosion resistance.
Comparative Examples 6-8, which lacked the phosphate esters or Cr 6+ from Examples 6-8, showed excellefit solderability, but inferior effects on corrosion resistance and solderability was decreased after aging.
Comparative Examples 9-11, which contained halogen in the fluxes for soldering, showed poor corrosion resistance and inferior effects on solderability after aging compared to the present post-treatment.
- As mentioned in Examples 1-17, in Table 1 and 2, excellent corrosion resistance, solderability and formability were obtained and these properties are retained after aging of plated steel-sheet,.by using the present invention.
Evaluation: The metal substrates which were prepared in Examples 1-17 and Comparative Examples 1-12 were evaluated by the following test methods. The results were shown in Tables 1 and 2.
(1) Spreadability of solder: a sample steel sheet, 50 x 50 mm in size, was floated on the solder-bath at a temperature of 2500C. The amount of 0.4 g of bended wire solder, that is, resin flux cored solder (iIS Z 3283) was placed on the sample steel sheet for 30 seconds. The area of solder spread was measured after cooling.
0: Area of spread solder > 20Omm 2 A: 20Omm 2 > area of spread solder > SOmm 2 2 X: Area of spread solder <5Omm, (2) Combination strength of solder: a bundle of twenty wires (=0.18mm) was placed on the test steel sheet and joined with the resin flux solder (RH 50) and was subjected to a pull off test (Bundle of twenty copper wires and solder steel sheet were pulled in opposite directions and evaluated as to the appearance of separated place).
No separation among wire, solder and soldered 0: steel sheet X: Separation between, wire and solder, or solder and soldered steel sheet 1 11 - (3) Corrosion resistance: a sample steel sheet was subjected to 2 cycles of a salt spray test (JIS Z 2371: salt spray 8 hours and dry 16 hours) and evaluated from generation of red rust.
0: No red rust X: entirely red rust (4) Formability: sample steel sheets were subjected to the Erichsen test (Er=7 mm) and Du Pont impact test (1/211 x lkg x 30 cm) and were evaluated as to formability by the adhesive tape test.
0: No separation between plated steel sheet and post-treatment X: Separation between plated steel sheet and post-treatment (5) Aging: sample steel sheets were subjected to a thermo-hygrostat(600C, RH 95%) for 1,000 hours and evaluated as to the appearance (or color change), corrosion resistance and solderability in the same way as in evaluations M-M.
Table 1 -
12 - Preparation and Condition of Specimens Ell Type of Amount of Post-treatment Solution ihickness Caffple Plating Deposit of This Invention Q/1) CU M) ammonium stearate 10 I In plated 5 glycerol - 20 0.5 paraffin wax 5 derivative of benzotriazole 2 2 Zn plated 10 salt of phosphoric ester and amine 1 0.05 CrO:3 0.2 3 Sn-plated 5 oleic acid 50 phosphoric ester 10 3 ester prepared from fatty acid and 6 4 Cu plated 3glycerol 20 0.2 paraffin wax 10 Sn-Pb 10 ethylene glycol 30 plated CrO:3 1 1 polyethylene glycol alkylphenyl ether 6 Zn.plated 5 (E.,-,iaruzitl.o-16: Daiichikogyo S-!iyaku 0.5 Co.LTD) 10 CrO3 1 polypropylene- 0 lycol polyethylene 7 Zn plated 10 lycol ether (Epan-720:Daiichikogyo 0.5 Q 0 Setyaku Co.LTD) 100 phosphoric ester 5 polyethylene VYcol oleate ester 0 8 Sn plated 2 (Noigen-ES90:Daiichikogyo Seiyaku 2 Co.LTD) 2 CrO3 0.02 polyethylene glycol stearate 0 9 Sn plated 5 (Noniolite-T40:'t%'youeisya yushi 0.02 Co.LTD) 5 phosphoric es-.'-- sorbitan oleate (Noniolite-SPS:
1 0 Cu plated 3 Kyoueisya Yushi Co.LTD) 50 0.2 CrO3 I Sn-Pb polyoxyethylene alkylpropylene diamine 1 1 plated to (Noniolite-DNT -10:Xyoueisya yushi 0.5 Co.LTD) 10 CrO3 I Zn plated 5 phosphoric ester (monobasic) too 1. 2 1 1 2 1 1 1 CrO3 0.02 i - 13 Table 1: Preparation and Condition of Specimens Amount of Post-treatment Solution Thickness E...ple Type of Deposit of This Invention W1) (11 m) 1 0 Plating (.-/M2) Zn plated 10 phosphoric ester (mixture of mono- 0-5 and di-basic) 200 phosphoric ester 5 Sn plated 2 CrO.3 3 0-01 Rosin (amine salt) 10 mono-(di-oleyi)phosphoric ester 1 5 5n plated 5 (amine salt) 10 0.1 cr03 0.2 1 6 CU plated 3 phosphoric ester. so 0.5 dodecylamine 100 17 Sn-Pb phosphoric ester 150 0-2 plated 10 (alkanolamine salt) Compara- tive Zn plated 10 Sn plated (according to Japanese Pat.
Example 1 Application No Sho 61-19793) 0.5 --- 2 Zn plated 10 paraffin wax(according to Japanese Pat.
Application No Sho 54-15432) 100 3 3 Sn plated 5 phosphate treatment 2 g/m 2 1 1 as p a Sn plated 5_ chromate treatment 0.0-'--mgldmz as er Cu plated 3 chromate treatment 0.05m,-c>ldml as CZ 6 Zn plated 5 same as example 6 except CrO3 0-5 7 Z n plated 10 same as example 7 except phosphoric 2 CS ter 8 5n plated 2 same as example 8 except CrO: 0.02 9 Zn-plated 5 an i 1 i ne hydrochloride 20 _d ipping (1 see-) 1 0 Zn plated 10 substituted by hydrazinium hydrochlo- 0.02 ride for benzotriazole in example 2 1 1 Zn plated 2 substituted by Sn(IV)chloride 0. 05mgIdm" for paraffin wax as Cr 1 2 Zn plated 10 ------ 14 - Table 2: Evaluation of Character Sample Corrosion Solde rability Change of Number Resistance Spreadability Strength Formability Color FY;;M., I 1 0 1 0 1 0 0 2 0 0 0 0 0 3 0 0 0 0 0 0 0 0 0 0 01- 0 0 0 6 0 0- 0 0 0 7 0 0 0' 0 0 8 0 0 0- 0 0 9 0 0 0 0 0 1 0 0 0 -0 0 0 I 1 0 0 0 0 0 1 2 0 0 0 0 0 1 3 0 0 0 0 0 14 0 0.0 0 0 0 0 0 0 0 1 6 0 0 0 0 0 17 1 0 0 1 0 1 0 1 0 Comparat ive ExamplE
2 L I 'L 1 0 0 3 x I x 1 0 L-0 0 0 0 L 0 0 0 x 6 1 - x 1 0 1 0 1 0 1 -- x - 7. 0 0 0 x 8 0 c 0 x i 0 1 0 Table 2:
- Evaluation of Characteristics Sample Corrosion Solderability I I Number Resistance Formability Change of Spread ability I Strength Color ComparativE Example
9 X 0 0 0 X 1 X 1 0 1 (3 1 0 1 X 11 1 X 0 0 0 12 1 X 0 0 '0 16 - Table 3: Evaluation of Characteristics After 1,000 Hours Aging Sample Corrosion Solderability Numbe r Resistance Spreadability IStrength Formability EXaMP I e 0 0 0 0 2 0 0 0 0 3 0 0 0 0 0 0 0 0 0 0 0 0 0' 0 0 0 7 0 0 0 0 8 0 0 0 0 9 0 0 0 0 1 0 0 0 0 0 1 1 0 0 0 0 1 2 0 0 0 0 1 3 0 0 0 0 14 0 0 0 0 1 0 1 - a 1 0 1 0 16 1 0 0 0 0 17 0 0 0 0 Comparativial X 0 Example
1 2 X X 0 3 X X 0 4 X-A 0 X- 0 6 1 'Y I I A 1 0 7 1 Y I L I. L 1 0.
8 1 x I - - I Z! -0 w i 17 - Table 3: Evaluation of Characteristics After 1,000 Hours Aging Sample Corrosion Resistancel Number Solderability ISpreadabilitv IStrength I Formability Com Parativ Example
9 I X 0 1 0 1 X 0 1 1 1 X 0 1 2 1 X 0 18 -
Claims (12)
1. A method for post-treatment of plated steel sheet for soldering by coating post-treatment solution in the amount of 0.02 to 2 pm dry thickness on the plated steel sheet, said post-treatment solution containing 2 to 100 g/1 of at least one water-soluble or water-dispersed material comprising:
a.
b.
fatty alcohols, alkylphenols, condensates prepared from fatty acids and ethylene C.
oxides, d. polyethylene glycol-alkylamines, e. esters prepared from sorbitan and fatty acids, f. surfactants prepared from polypropylene glycol as a hydrophobic group and polyethylene glycol as a hydrophilic group, 9. amides prepared from fatty acid and diethanol amine, h. esters prepared from fatty acids and sucrose, and i. saponificates prepared from lanolin alcohol or lanolin fatty acid, and the pH value of said post-treatment solution being from 3 to 10.
2. A method for the post-treatment of plated steel sheet for soldering by coating a post-treatment solution in the amount of 0.02 to 2 pn dry thickness on the plated steel sheet, said post-treatment solution containing 2 to U 1 g/1 of at least one water-soluble or water-dispersed material comprising:
a. abietic acid, b. benzoic acid, C. saturated fatty acids having 12 to 24 carbon atoms, d.
unsaturated fatty acids having 12 to 24 carbon atoms, e. organic alcohols having 2 to 400 carbon atoms, f. esters of fatty acids, g. derivatives of benzotriazoles and metalates, ammonium salts and amine salts of said materials, and 10.
3. sheet for solution the pH of said post-treatment solution being from 3 to A method for the post-treatment of plated steel soldering which comprises coating a post-treatment in the amount of from 0.01 to 2 vim dry thickness, on the plated steel sheet and said post-treatment solution containing from 5 to 200 g/1 of at least one water-soluble or water-dispersed phosphoric ester, and the pH of said post-treatment solution being from 3 to 10.
4. The method according to claim 1, wherein said post-treatment solution contains from 1 to 50 g/1 phosphoric ester or from 0.01 to 3 g/l of Cr 6+ or both.
1
5. The method accor ding to claim 2, wherein said post-treatment solution contains from 1 to 50 g/l of phosphoric ester or from 0.01 to 3 g/l of Cr 6+ or both.
6. The method according to claim 3, wherein said post-treatment solution contains from-0.01 to 3 9/1 of Cr 6+
7. The method according to claim 1, wherein the said post-treatment solution further contains from 10 to 100 g/1 5 of organic amine soap.
8. The method according to claim 2, wherein the said post-treatment solution further contains from 10 to 100 g/1 of organic amine soap.
9. The method according to claim 3, wherein the said 10 post-treatment solution further contains from 10 to 100 g/1 - of organic amine soap.
10. Plated steel sheets coated with a layer 0.01 to 2 pm in thickness comprised of at least one watersoluble or water-dispersed material as defined in any 15 of claims 1 to 3.
11. The method for post-treatment of plated-steel sheet as claimed in any of claims 1 to 3 substantially as herein described with reference to any one of the examples.
12. Coated plated steel sheets as claimed in claim substantially as herein described with reference to any one of the examples.
Published 1989 at The Patent Office, StateHouse, 6671 High Holbom.Londz)n WClR4TP. Further copies maybe obtalnedfrom The Patent Office. Sales Branch, St Mary Cray, Orpington, Kent BR5 3RD. Printed by Multiplex techniques ltd, St Mary Cray, Kent, Con. 1/87 k t 4
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB9125633A GB2249320B (en) | 1987-11-17 | 1991-12-02 | Metod for post-treatment of plated steel sheet for soldering |
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61233323A JPS6388085A (en) | 1986-10-02 | 1986-10-02 | Post-treatment of plated steel sheet |
| JP62201023A JPH0611920B2 (en) | 1986-10-02 | 1987-08-13 | Multi-layer plated steel sheet with excellent solderability |
| CA000551642A CA1332130C (en) | 1986-10-02 | 1987-11-12 | Method for post-treatment of plated steel sheet for soldering |
| FR8715773A FR2623212B1 (en) | 1986-10-02 | 1987-11-16 | POST-TREATMENT SOLUTION OF A PLATED STEEL SHEET FOR WELDING, AND METHOD FOR ITS APPLICATION |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8726833D0 GB8726833D0 (en) | 1987-12-23 |
| GB2212521A true GB2212521A (en) | 1989-07-26 |
| GB2212521B GB2212521B (en) | 1992-07-22 |
Family
ID=39365786
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8726833A Expired - Lifetime GB2212521B (en) | 1986-10-02 | 1987-11-17 | Method for post-treatment of plated steel sheet for soldering |
Country Status (5)
| Country | Link |
|---|---|
| JP (2) | JPS6388085A (en) |
| CA (1) | CA1332130C (en) |
| DE (1) | DE3740177A1 (en) |
| FR (1) | FR2623212B1 (en) |
| GB (1) | GB2212521B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0631444B2 (en) * | 1989-06-07 | 1994-04-27 | 東洋鋼板株式会社 | Multi-layer plated steel sheet for solder |
| US5011711A (en) * | 1989-07-18 | 1991-04-30 | Toyo Kohan Co., Ltd. | Method for post-treatment of electroplated steel sheets for soldering |
| JPH03153883A (en) * | 1989-11-13 | 1991-07-01 | Nkk Corp | Multi-ply plated steel sheet having superior lubricity, corrosion resistance and suitability to coating |
| US5069730A (en) * | 1991-01-28 | 1991-12-03 | At&T Bell Laboratories | Water-soluble soldering paste |
| FR2683475B1 (en) * | 1991-11-08 | 1995-07-21 | Geb | BRAZING FLOW. |
| FR2742364B1 (en) * | 1995-12-14 | 1998-01-09 | Lorraine Laminage | METHOD FOR THE SURFACE TREATMENT OF A METAL SHEET FOR STAMPING |
| CN119447320B (en) * | 2024-11-26 | 2025-09-12 | 江阴纳力新材料科技有限公司 | A composite current collector electrode welding method for laminated battery |
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- 1987-11-12 CA CA000551642A patent/CA1332130C/en not_active Expired - Fee Related
- 1987-11-16 FR FR8715773A patent/FR2623212B1/en not_active Expired - Fee Related
- 1987-11-17 GB GB8726833A patent/GB2212521B/en not_active Expired - Lifetime
- 1987-11-26 DE DE19873740177 patent/DE3740177A1/en active Granted
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| GB525597A (en) * | 1938-05-16 | 1940-08-30 | Pope S Metaaldraadlampenfabrie | Improved method of soft-soldering insulated flexible electric conductors |
| GB807660A (en) * | 1957-01-30 | 1959-01-21 | Amchem Prod | Improvements in or relating to the surface treatment and cold-working of metals |
| GB1004836A (en) * | 1961-06-13 | 1965-09-15 | Pyrene Co Ltd | Improvements relating to the cold-working of metals |
| GB1125942A (en) * | 1965-12-31 | 1968-09-05 | Borg Holding Ag | Process for the surface treatment of plants containing water and/or steam |
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| GB1421386A (en) * | 1973-09-19 | 1976-01-14 | Pyrene Chemical Services Ltd | Coating compostions |
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Also Published As
| Publication number | Publication date |
|---|---|
| CA1332130C (en) | 1994-09-27 |
| GB2212521B (en) | 1992-07-22 |
| GB8726833D0 (en) | 1987-12-23 |
| DE3740177A1 (en) | 1989-06-08 |
| JPH0611920B2 (en) | 1994-02-16 |
| JPS6388085A (en) | 1988-04-19 |
| JPS6447894A (en) | 1989-02-22 |
| FR2623212A1 (en) | 1989-05-19 |
| FR2623212B1 (en) | 1994-05-13 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19971117 |