EP0232929B1 - Verfahren zur Erleichterung der Kaltumformung von Edelstahl - Google Patents
Verfahren zur Erleichterung der Kaltumformung von Edelstahl Download PDFInfo
- Publication number
- EP0232929B1 EP0232929B1 EP87200060A EP87200060A EP0232929B1 EP 0232929 B1 EP0232929 B1 EP 0232929B1 EP 87200060 A EP87200060 A EP 87200060A EP 87200060 A EP87200060 A EP 87200060A EP 0232929 B1 EP0232929 B1 EP 0232929B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- water
- stainless steel
- oxalate
- oxalate coating
- coating
- 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.)
- Expired - Lifetime
Links
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000010935 stainless steel Substances 0.000 title claims abstract description 13
- 230000008569 process Effects 0.000 title description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000000576 coating method Methods 0.000 claims abstract description 40
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000314 lubricant Substances 0.000 claims abstract description 8
- 229920003169 water-soluble polymer Polymers 0.000 claims abstract description 8
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 claims abstract description 7
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 7
- 239000000654 additive Substances 0.000 claims abstract description 6
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 6
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 6
- 239000000470 constituent Substances 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 239000004133 Sodium thiosulphate Substances 0.000 claims abstract 2
- 238000005482 strain hardening Methods 0.000 claims abstract 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 239000005018 casein Substances 0.000 claims description 2
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 claims description 2
- 235000021240 caseins Nutrition 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 20
- MVWDJLOUEUAWIE-UHFFFAOYSA-N O=C=O.O=C=O Chemical compound O=C=O.O=C=O MVWDJLOUEUAWIE-UHFFFAOYSA-N 0.000 description 13
- 238000005755 formation reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 238000005260 corrosion Methods 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 239000000344 soap Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 239000011651 chromium Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 238000007602 hot air drying Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000008149 soap solution Substances 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000002730 additional effect Effects 0.000 description 1
- 239000000853 adhesive Substances 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
- 239000010953 base metal Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007739 conversion coating Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/46—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing oxalates
Definitions
- the invention relates to a method for facilitating the cold forming of stainless steel by applying an oxalate coating and then a lubricant.
- the oxalation solutions used to produce the oxalate coating contain, as the main constituent, oxalic acid, additives such as fluoride or chloride, which cause the pickling attack, and sodium thiosulfate or the like, which act as accelerators in the formation of crystals in the layer.
- an oxalate coating of a suitable layer weight can be produced, to which a lubricating layer is applied in a next operation using a metal soap solution or dispersion.
- a layer system is currently the best form of preparation of stainless steels for cold forming, provided that conventional degrees of deformation are intended.
- the high-quality and highly corrosion-resistant stainless steels behave disadvantageously with regard to the formation of oxalate coatings, since the layer formation reaction is severely hindered when using conventional oxalation solutions.
- the content of the bath components causing the pickling attack such as fluoride or chloride, has been increased, but this has the consequence that the treatment time takes longer and the coating formation is unsatisfactory.
- the object of the invention is to provide a method for facilitating the cold forming of stainless steels, with which in particular the problems mentioned above can be remedied and which also leads to adhesive coatings in the case of highly corrosion-resistant stainless steels, so that even in the case of heavy cold forming, seizure or cold welding is avoided.
- Particularly suitable water-soluble polymers are polyvinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol; Polyacrylic acid, casein, glue and the like. Polyvinyl alcohol and polyvinyl pyrrolidone are preferred.
- the concentrations of the active constituents of the oxalation solution are significant in that than with oxalic acid below 20 g / l there is no sufficient reaction with the stainless steel and above 100 g / l no further increase in reactivity can be achieved.
- the oxide film does not dissolve sufficiently from the stainless steel surface at a concentration below 5 g / l, so that the formation of the coating proceeds with difficulty. At concentrations above 50 g / l there is practically no additional effect.
- water-soluble polymer do not lead to an improvement in the coating adhesion at concentrations below the lower limit, and the maximum adhesion is reached at concentrations at the upper limit.
- Metal soaps are particularly suitable as lubricants for application to the oxalate coating.
- iron soaps are formed by reaction with the oxalate coating and the soap solution.
- Calcium, barium, zinc soaps and the like dispersed in water give rise to layers of lubricant of the corresponding soaps on the workpiece surface.
- the oxalate coating is applied by contact with an oxalating solution which has a temperature of 70 to 100 ° C., preferably 85 to 95 ° C.
- hydroxylammonium sulfate in combination with oxalic acid is able to quickly and easily bring about complete removal of the oxide film and also to accelerate the formation of the oxalate coating.
- oxalation solutions which additionally contain fluoride and / or chloride can also be used in the process according to the invention.
- the water-soluble polymer contained in the oxalation solution is firmly incorporated into the oxalate coating during the formation of the coating, so that it is not removed even by water rinsing. As a result of the installation, a high binding and adhesive effect is also achieved.
- Sodium thiosulfate is used primarily for nucleation and is therefore particularly responsible for the fineness of the oxalate coating produced.
- lubricant was applied by treatment with a sodium stearate solution (70 g / l; 75'C; 3 min) before the hot air drying.
- the wire rods treated and weighed with the individual oxalation solutions - as indicated above - were placed in a 5% by weight aqueous solution of chromic acid at 80 ° C. for a period of 15 min. submerged. Then the wire rods were withdrawn and the layer weights converted into g / m 2 .
- the adhesion or abrasion resistance of the respective oxalate coatings was tested - also with wire rod.
- the individual wire rods were tested in a reproducible manner and for a certain time that was identical for all samples using an Amsler testing machine (brake pad against wheel principle).
- the friction body KIMWIPE® from Jujo Kimberly K.K.
- the weight of the remaining oxalate coating was then determined using the aforementioned method.
- the pulling speed was 17.8 m / min.
- the oxalation solutions used in the process according to the invention led in all cases to residual coating weights of more than 2 g / m 2 in the adhesion test, as a result of which superior adhesion to conventional oxatation solutions tested according to comparison is demonstrated.
- Tube specimens made of Incolloy 800 (20 Cr, 32 Ni) were used as test objects.
- Example 1 The treatment was carried out according to the procedure of Example 1 (without soaping). The layer weights were then determined, as indicated in Example 1.
- test results show that proper oxalate coatings were formed using the oxalation process used in the invention. Although they differed somewhat in terms of layer weight, they possessed the properties necessary for cold forming to a sufficient extent.
Landscapes
- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Metal Extraction Processes (AREA)
- Lubricants (AREA)
- Chemical Treatment Of Metals (AREA)
- Heat Treatment Of Sheet Steel (AREA)
- Heat Treatment Of Steel (AREA)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| AT87200060T ATE51423T1 (de) | 1986-01-21 | 1987-01-16 | Verfahren zur erleichterung der kaltumformung von edelstahl. |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10752/86 | 1986-01-21 | ||
| JP61010752A JPS62170484A (ja) | 1986-01-21 | 1986-01-21 | ステンレス鋼の冷間加工用潤滑処理方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0232929A1 EP0232929A1 (de) | 1987-08-19 |
| EP0232929B1 true EP0232929B1 (de) | 1990-03-28 |
Family
ID=11759045
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP87200060A Expired - Lifetime EP0232929B1 (de) | 1986-01-21 | 1987-01-16 | Verfahren zur Erleichterung der Kaltumformung von Edelstahl |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP0232929B1 (ru) |
| JP (1) | JPS62170484A (ru) |
| AT (1) | ATE51423T1 (ru) |
| DE (2) | DE3700933A1 (ru) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002088387A (ja) * | 2000-09-14 | 2002-03-27 | Sakai Chem Ind Co Ltd | 非塩素系潤滑油組成物を使用する金属加工 |
| ITMN20060021A1 (it) * | 2006-03-23 | 2007-09-24 | Gilcotubi S R L | Sistema di produzione di strutture tubolari inossidabili e saldabili con alta resistenza meccanica e relativo prodotto ottenuto |
| US11607929B2 (en) | 2018-08-09 | 2023-03-21 | Hanon Systems | Thermal cycle resistant fastening system for refrigerant fitting |
| WO2020165035A1 (de) * | 2019-02-14 | 2020-08-20 | Chemetall Gmbh | Vereinfachtes verfahren zur vorbehandlung von metallischen substraten für die kaltumformung und reaktiver schmierstoff hierzu |
| CN115151627A (zh) | 2020-02-25 | 2022-10-04 | 凯密特尔有限责任公司 | 用于金属冷成型的金属基底的一步预处理方法 |
| US20230106175A1 (en) | 2020-02-25 | 2023-04-06 | Chemetall Gmbh | One-step pretreatment method of metallic substrates for metal cold forming |
| CN111500955B (zh) * | 2020-04-17 | 2021-08-24 | 抚顺特殊钢股份有限公司 | 一种核电蒸发器用n06625合金异型材制造工艺 |
| BR112023019649A2 (pt) | 2021-04-01 | 2023-10-31 | Chemetall Gmbh | Método de pré-tratamento de um substrato metálico, substrato metálico pré-tratado, processo de conformação a frio, e, composição lubrificante aquosa |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2759862A (en) * | 1952-03-11 | 1956-08-21 | Devex Corp | Coating compositions and method of treating ferrous surfaces therewith |
| CA930651A (en) * | 1971-01-12 | 1973-07-24 | Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Energy, Mines, And Resources | Forming oxalate conversion coatings on iron or steel |
| JPS524255B2 (ru) * | 1972-08-26 | 1977-02-02 | ||
| DE2424382A1 (de) * | 1974-05-20 | 1975-12-04 | Metallgesellschaft Ag | Verfahren zur vorbereitung von metallischen werkstuecken fuer die spanlose kaltumformung |
-
1986
- 1986-01-21 JP JP61010752A patent/JPS62170484A/ja active Granted
-
1987
- 1987-01-15 DE DE19873700933 patent/DE3700933A1/de not_active Withdrawn
- 1987-01-16 DE DE8787200060T patent/DE3762053D1/de not_active Expired - Fee Related
- 1987-01-16 EP EP87200060A patent/EP0232929B1/de not_active Expired - Lifetime
- 1987-01-16 AT AT87200060T patent/ATE51423T1/de not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0129872B2 (ru) | 1989-06-14 |
| JPS62170484A (ja) | 1987-07-27 |
| DE3700933A1 (de) | 1987-07-30 |
| DE3762053D1 (de) | 1990-05-03 |
| EP0232929A1 (de) | 1987-08-19 |
| ATE51423T1 (de) | 1990-04-15 |
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