EP2045364A2 - Déposition galvanique de couches de métaux sur des surfaces en magnésium ou en alliages de magnésium - Google Patents
Déposition galvanique de couches de métaux sur des surfaces en magnésium ou en alliages de magnésium Download PDFInfo
- Publication number
- EP2045364A2 EP2045364A2 EP20080016260 EP08016260A EP2045364A2 EP 2045364 A2 EP2045364 A2 EP 2045364A2 EP 20080016260 EP20080016260 EP 20080016260 EP 08016260 A EP08016260 A EP 08016260A EP 2045364 A2 EP2045364 A2 EP 2045364A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- magnesium
- adhesion
- coated
- promoting layer
- alkaline
- 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.)
- Withdrawn
Links
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 22
- 239000002184 metal Substances 0.000 title claims abstract description 22
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims description 28
- 239000011777 magnesium Substances 0.000 title claims description 28
- 229910052749 magnesium Inorganic materials 0.000 title claims description 28
- 230000008021 deposition Effects 0.000 title description 8
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000000576 coating method Methods 0.000 claims abstract description 17
- 239000003792 electrolyte Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 11
- 239000000853 adhesive Substances 0.000 claims abstract description 8
- 230000001070 adhesive effect Effects 0.000 claims abstract description 8
- 239000000080 wetting agent Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000012487 rinsing solution Substances 0.000 claims abstract 2
- 238000000151 deposition Methods 0.000 claims description 8
- 238000009713 electroplating Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 17
- 229910052802 copper Inorganic materials 0.000 description 17
- 239000010949 copper Substances 0.000 description 17
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 239000013527 degreasing agent Substances 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000007739 conversion coating Methods 0.000 description 2
- DOBRDRYODQBAMW-UHFFFAOYSA-N copper(i) cyanide Chemical compound [Cu+].N#[C-] DOBRDRYODQBAMW-UHFFFAOYSA-N 0.000 description 2
- LEKPFOXEZRZPGW-UHFFFAOYSA-N copper;dicyanide Chemical compound [Cu+2].N#[C-].N#[C-] LEKPFOXEZRZPGW-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 238000004532 chromating Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
-
- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
-
- 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
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/42—Pretreatment of metallic surfaces to be electroplated of light metals
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
- C25D3/40—Electroplating: Baths therefor from solutions of copper from cyanide baths, e.g. with Cu+
Definitions
- the present invention relates to a process for the electrodeposition of metal layers on magnesium or magnesium alloy surfaces.
- Magnesium has been increasingly used in the automotive and commercial aircraft and electronics industries in recent years and decades. Especially in the production of high quality products, magnesium or magnesium alloys are used to save weight.
- magnesium or magnesium alloys have the advantage over other light metals to have excellent casting properties, so that both injection and die castings can be made from appropriate magnesium alloys or magnesium with very good strength properties.
- the production of components by means of magnesium injection molding seems to be of greater interest in the future, especially in the automotive industry. In the injection molding of magnesium or magnesium alloys, these are not heated to complete melting, but only heated to about 100 ° below the melting point. Here then a thixotropic state of magnesium is reached, in which it can be injection-molded accordingly.
- the substrates produced by means of appropriate casting processes generally have to be surface-treated. This can on the one hand serve the corrosion protection of the magnesium or magnesium alloy surface, on the other hand can be correspondingly shiny or matt decorative surfaces are produced by deposition of metal layers on the surface.
- anodising methods, plasma methods or conversion coatings such as, for example, chromating are currently being offered on the market in addition to conventional galvanic coating methods such as the deposition of copper, nickel, chromium, tin and the like.
- galvanic coating processes are suitable for use on decorative surfaces.
- the anodization methods and conversion coatings mentioned above merely serve as corrosion protection and are the basis for a subsequent coating, for example by painting.
- a fundamental problem in the coating of magnesium or magnesium alloys is the oxide film forming on the substrate surface, which must be removed in the prior art by appropriate pretreatments.
- pretreatments by means of an ammonium chloride-containing phosphoric acid solution are known from the cited prior art for the removal of the oxide layer.
- the magnesium or magnesium alloy surfaces to be coated are activated with hydrochloric acid.
- Magnesium alloys commonly used in the industry are those of types AZ31 to AZ91, where AZ is the alloyed aluminum and zinc, and the trailing number indicates how high the proportion of this alloy in magnesium is.
- This object is achieved by a process for the galvanic coating of magnesium or magnesium alloy surfaces, which is characterized in that the surfaces to be coated during the entire coating process until complete coverage with a metal layer of the deposited metal are brought into contact exclusively with process solutions and rinse solutions which have a pH ⁇ pH 7, preferably ⁇ pH 8.
- magnesium is prevented from being dissolved out of the surface of the substrates to be coated. This also reduces the need for levelers, as it exists, for example, in the case of galvanic coating, in particular of high-alloy magnesium alloys such as, for example, AZ91.
- the cleaning of the substrate to be coated can be done by means of a hot degreasing.
- the substrate to be cleaned is treated at a temperature of about 70-80 ° C for 10 minutes with a suitable degreaser solution.
- the combination of different degreasers is provided in particular, the selection of the degreasers to be used being effected as a function of the contaminants present on the substrates or substrate surfaces to be coated.
- the degreasers to be used are alkaline degreasers.
- Kavitec modulus or eductor nozzles can be provided according to the invention.
- Kavitec systems are high-pressure water nozzles that support cleaning by cavitation effects.
- the substrate surface is treated with an alkaline, cyanide-free adhesive dressing.
- a Haftbeize is a Zinkatbeize, which in addition to sodium pyrophosphate (Na 4 P 2 O 7 x 10 H 2 O) zinc sulfate, sodium carbonate and sodium chloride suitable wetting agents for reducing the surface tension of Zinkatbeize.
- the described zincate pickling to be used according to the invention has a pH value determined photometrically at 30 ° C. in the range between pH 10 and 11, preferably in the range between pH 10 and 10.5.
- the substrate surface to be treated of the magnesium or magnesium alloy substrate to be coated is contacted with the zincate stain at a temperature between 60 and 80 ° C, preferably between 65 and 75 ° C.
- the exposure time is between 5 and 15 minutes, preferably between 9 and 11 minutes.
- zincate stain 100-300 g / l sodium pyrophosphate ⁇ 10 H 2 O 25-75 g / l zinc sulfate x 7 H 2 O. 3 - 6 g / l sodium carbonate 2 - 5 g / l sodium chloride 0,5 - 3 g / l wetting agent
- a wetting agent known as Nonpitter 62 A or a wetting agent known as EnPREP TTM WA can advantageously be used as wetting agent.
- combinations of different wetting agents can be used.
- the surface tension of the zincate pickling used according to the invention is ⁇ 55 mN / m.
- the specified surface tension is determined as the dynamic surface tension by means of a bubble pressure tensiometer.
- the bubble life for this determination is ⁇ 500 ms.
- a suitable measuring instrument for determining the dynamic surface tension is the Scienceline T60 from Sita-Messtechnik GmbH.
- a first metal layer is then deposited on the surface to be coated in the inventive method described here by way of example, with the optional interposition of a rinsing step Substrate surface.
- a rinsing step Substrate surface.
- different electrodeposited metal layers such as copper, nickel or chrome layers may be provided.
- the substrate surface of the magnesium or magnesium alloy substrate to be coated with a zincate layer in the manner described above is contacted with a cyanide bright copper electrolyte, for example, a CUPRALYTE 1545 electrolyte from Enthone Inc. at a temperature between 40 and 55 ° C.
- a current density between 0.5 and 2.0 A / dm 2 is set.
- a lower current density is to be provided than when using copper pieces in corresponding anode baskets.
- the voltage to be applied is in a range between 2.0 and 12.0 volts, depending on the anodes used and the substrates or substrate surfaces to be coated.
- the cyanide copper electrolyte used in the embodiment of the process according to the invention described here has a photometrically determined pH in the range between pH 11.0 and pH 12.0.
- the concentration of copper in the copper electrolyte to be used according to the invention is between 20 g / l and 50 g / l.
- the concentration of free potassium cyanide in the cyanide copper electrolyte to be used here is between 20 g / l and 35 g / l.
- the electrolyte has a maximum potassium carbonate of 120 g / l.
- the density of an electrolyte as described above is about 1.15 g / cm 3 .
- this can be supplemented according to the invention with copper (1) cyanide in order to replace the copper from the electrolyte consumption.
- copper (1) cyanide in order to replace the copper from the electrolyte consumption.
- a metered addition of potassium cyanide in the order of about 2 g per g of copper supplemented can be provided in the electrolyte used here.
- copper layers can be deposited at a deposition rate of the order of about 0.4 ⁇ m / min at a set current density of 1 A / dm 2 .
- the deposited copper layers are adherent and show a uniform gloss.
- metal layers can be applied to the thus deposited copper layers, the subsequent deposition of metal layers in both acidic and alkaline coating electrolytes being possible, insofar as the underlying magnesium or magnesium alloy layer is completely covered by a corresponding copper layer.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE200710048043 DE102007048043A1 (de) | 2007-10-05 | 2007-10-05 | Galvanische Abscheidung von Metallschichten auf Magnesium- oder Magnesiumlegierungsoberflächen |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2045364A2 true EP2045364A2 (fr) | 2009-04-08 |
Family
ID=40113008
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP20080016260 Withdrawn EP2045364A2 (fr) | 2007-10-05 | 2008-09-16 | Déposition galvanique de couches de métaux sur des surfaces en magnésium ou en alliages de magnésium |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP2045364A2 (fr) |
| DE (1) | DE102007048043A1 (fr) |
| WO (1) | WO2009046328A1 (fr) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102010062357B4 (de) | 2010-12-02 | 2013-08-14 | Innovent E.V. | Vorrichtung und Verfahren zur Herstellung eines mit zumindest einer Korrosionsschutzschicht beschichteten magnesiumhaltigen Substrats |
| CN105543919B (zh) * | 2015-12-18 | 2017-11-10 | 沈阳理工大学 | 镁合金表面通过物理气相沉积形成电镀用导电涂层的方法 |
| DE102018216317A1 (de) * | 2018-09-25 | 2020-03-26 | Thyssenkrupp Ag | Verfahren zur Modifikation von feuerverzinkten Oberflächen |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4351713A (en) * | 1979-08-22 | 1982-09-28 | Thomas Steel Strip Corp. | Electro-co-deposition of corrosion resistant nickel/zinc alloys onto steel substrates |
| DE4136442A1 (de) * | 1991-11-06 | 1993-05-13 | Henkel Kgaa | Verfahren zum entfetten und reinigen metallischer oberflaechen und vorrichtung zu dessen durchfuehrung |
| JP3715743B2 (ja) * | 1997-04-15 | 2005-11-16 | 株式会社神戸製鋼所 | Ｍｇ合金部材の製造方法 |
-
2007
- 2007-10-05 DE DE200710048043 patent/DE102007048043A1/de not_active Withdrawn
-
2008
- 2008-09-16 EP EP20080016260 patent/EP2045364A2/fr not_active Withdrawn
- 2008-10-03 WO PCT/US2008/078792 patent/WO2009046328A1/fr not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| WO2009046328A1 (fr) | 2009-04-09 |
| DE102007048043A1 (de) | 2009-04-23 |
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| 18W | Application withdrawn |
Effective date: 20100921 |