DE2503317A1 - Pretreatment of nickel prior to a plating treatment - using mixt. of sulphuric, phosphoric, nitric and acetic acids - Google Patents
Pretreatment of nickel prior to a plating treatment - using mixt. of sulphuric, phosphoric, nitric and acetic acidsInfo
- Publication number
- DE2503317A1 DE2503317A1 DE19752503317 DE2503317A DE2503317A1 DE 2503317 A1 DE2503317 A1 DE 2503317A1 DE 19752503317 DE19752503317 DE 19752503317 DE 2503317 A DE2503317 A DE 2503317A DE 2503317 A1 DE2503317 A1 DE 2503317A1
- Authority
- DE
- Germany
- Prior art keywords
- vol
- nickel
- acid
- activation
- mixt
- 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
Classifications
-
- 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
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1834—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Chemically Coating (AREA)
Abstract
Description
"Verfahren zur chemischen Aktivierung von Nickeloberflächen" Die Erfindung betrifft ein Verfahren zur chemischen Aktivierung der Oberfläche eines aus Nickel oder einer Nickellegierung bestehenden Körpers als Vorbehandlung vor einer galvanischen oder fremdstromlosen Metallabscheidung, insbesondere Nickelabscheidung unter Verwendung einer Aktivierungslösung. "Process for the chemical activation of nickel surfaces" Die The invention relates to a method for chemical activation of the surface of a made of nickel or a nickel alloy body as a pretreatment a galvanic or external current-free metal deposition, in particular nickel deposition using an activation solution.
Die galvanische oder fremdstromlose chemische Abscheidung von Nickel auf Nickeloferflächen, z. B. zum Zweck der Verstärkungeiner bereits vorhandenen-Nickelschicht, ist nur schwierig durchführbar und gelingt in vielen Fällen überhaupt nicht. Der Grund hierfür liegt in der Eigenschaft des Nickels, im alkalischen und neutralen Bereich sowie an der buft passivierende Deckschichten, z. B. in Form von Oxiden oder Hydroxiden, auszubilden, die während eines späteren Abscheidungsvorgangs nicht ohne weiteres abgebaut werden. Diese ,schichten inhibieren die Oberfläche, so daß eine galvanische oder fremdstromlose chemische Abscheidung von Nickel meist nicht gelingt oder abgeschiedene Niederschläge nur sehr schlecht haften.The galvanic or electroless chemical deposition of nickel on nickelofer surfaces, e.g. B. for the purpose of reinforcing an already existing nickel layer, is difficult to implement and in many cases does not work at all. Of the The reason for this lies in the property of nickel, which is alkaline and neutral Area as well as on the buft passivating cover layers, z. B. in the form of oxides or hydroxides, which do not form during a later deposition process can be dismantled without further ado. These , layers inhibit the surface, so that a galvanic or electroless chemical deposition of nickel mostly does not succeed or deposited precipitates adhere only very poorly.
Um diese Schwierigkeiten zu vermeiden, wurde bereits vorgeschlagen, die zu vernickelnden Nickeloberflächen zu aktivieren, bevor der Abscheidungsprozeß eingeleitet wird. Zur Aktivierung für eine galvanische Abscheidung von Nickel auf Nickel wählt man eine Vorbehandlung mit Säuren, während man bei den fremdstromlosen chemischen Methoden Aktivierungslösungen auf der Basis Zinn (II)-chlorid/Palladiumchlorid benutzt. So werden bei der Säureaktivierung z. B 20-3OVoige Salzsäure bei Raumtemperatur für 5 min oder 25e,0ige Schwefelsäure bei Raumtemperatur 5-10-min oder 30-5O5'oige Perchlorsäure bei Raumtemperatur für 2-60 s angewandt. Zur Aktivierung vor der chemischen Abscheidung von Nickel kann man die Nickeloberflächen zuerst mit einer schwach salzsauren 20 g/l Zinn (II)-chloriddihydrat enthaltenden Lösung und danach mit einer salzsauren 200 mg/l Palladiumchlorid enthaltenden Lösung behandeln.In order to avoid these difficulties, it has already been suggested that activate the nickel surfaces to be nickel-plated before the deposition process is initiated. To activate for a galvanic deposition of nickel on For nickel, one chooses a pretreatment with acids, while with the electroless ones chemical methods Activation solutions based on tin (II) chloride / palladium chloride used. So are in the acid activation z. B 20-3O% hydrochloric acid at room temperature for 5 min or 25% sulfuric acid at room temperature 5-10 min or 30-5O5% Perchloric acid applied at room temperature for 2-60 s. To activate before the chemical The nickel surfaces can be deposited first with a weak hydrochloric acid 20 g / l tin (II) chloride dihydrate containing solution and then with a hydrochloric acid solution Treat 200 mg / l solution containing palladium chloride.
Im ersten Falle basiert die Aktivierung auf einer Auflösung der Passivschicht, im zweiten Fall auf der Bildung von Palladium-Keimen auf der Passivschicht,- wonach die Nickelabscheidung auf der Passivschicht einsetzt. Diese Verfahren besitzen den Nachteil, daß sie kaum reproduzierbare Ergebnisse liefern und die abgeschiedenen Nickelschichten auf der Unterlage nur schlecht haften.In the first case, the activation is based on a dissolution of the passive layer, in the second case on the formation of palladium nuclei on the passive layer, - after which the Nickel deposition on the passive layer begins. These procedures have the disadvantage that they give hardly reproducible results and the deposited Nickel layers adhere poorly to the substrate.
Der Erfindung lag daher die Aufgabe zugrunde, ein Verfahren anzugeben, mit dessen Hilfe sowohl bei galvanischer als auch stromloser Metallabscheidung, insbesondere Nickel abscheidung, gute reproduzierbare Ergebnisse erhalten werden, wobei eine gute Haftung des abgeschiedenen Metalles gewahrleistet ist.The invention was therefore based on the object of specifying a method with its help for both galvanic and electroless metal deposition, especially nickel deposition, good reproducible results are obtained, good adhesion of the deposited metal is ensured.
Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß als Aktivierungslösung ein Säuregemisch verwendet wird, das 5-15 Vol-% Schefelsäure, 98%ig 5-15 Vol-% o-Phosphorsäure, 89%ig 25-35 Vol-% Salpetersäure, 6Yig und 40-60 zu40-60 Vol-O Essigsäure, 99%ig enthält.This object is achieved according to the invention in that as an activating solution an acid mixture is used that contains 5-15% by volume of sulfuric acid, 98% 5-15% by volume of o-phosphoric acid, 89% 25-35% by volume nitric acid, 6% and 40-60 to 40-60% by volume acetic acid, 99% contains.
Der Vorteil der Erfindung ist darin zu sehen, daß die Lösung die Ausgangsnickeloberfläche bei Raumtemperatur nur sehr eringfigig abträgt und nicht aufrauht. Bei höheren Temperaturen, beispielsweise bei 50-90° C, kann sogar eine Einebung der Nickeloberfläche stattfinden.The advantage of the invention can be seen in the fact that the solution is the starting nickel surface at room temperature only very eringfigig wears away and does not roughen. At higher temperatures, for example at 50-90 ° C, there can even be a leveling the nickel surface take place.
Eine besondere vorteilhafte -Aktivierungslösung besteht aus folgenden Komponenten: 10 Vol-% Schwefelsäure, 98%ig 10 Vol-% o-Phosphorsäure, 89%ig 30 Vol-% Salpetersäure, 65%ig 50 Vol-o Essigsäure, 99%ig Die Behandlungsdauer beträgt bei Raumtemperatur 10-30 s.A particularly advantageous activation solution consists of the following Components: 10% by volume sulfuric acid, 98% 10% by volume o-phosphoric acid, 89% 30% by volume Nitric acid, 65% 50 vol-o acetic acid, 99% The treatment time is at Room temperature 10-30 s.
Nach anschließendem kurzen Spülen mit deionisiertem Wasser wird die entsprechende Probe ohne vorherige Trocknung sofort in den gewünschten Elektrolyten zur galvanischen oder fremdstromlosen chemischen Vernickelung gebracht.After a short rinse with deionized water, the corresponding sample immediately into the desired electrolyte without prior drying brought to galvanic or electroless chemical nickel plating.
Die folgenden Beispiele sollen die Erfindung noch näher erläutern.The following examples are intended to explain the invention in more detail.
Beispiel 1: Ein sauber entfettetes Nickelblech oder ein entsprechend behandeltes Blech aus einer Nickel-Eisen-Legierung wird 10 s lang bei Raumtemperatur in eine Aktivierungslöung getaucht, die sich wie folgt zusammensetzt: 10 Vol-% Schwefelsäure 98%ig, 10 Vol-% o-Phosphorsäure 89%ig, 30 Vol-% Salpetersäure 65%ig und 50 Vol-Vo Essigsäure 99%ig.Example 1: A cleanly degreased nickel sheet or an equivalent treated sheet of nickel-iron alloy is for 10 s at room temperature immersed in an activation solution, which is composed as follows: 10% by volume sulfuric acid 98%, 10% by volume o-phosphoric acid 89%, 30% by volume nitric acid 65% and 50 vol% acetic acid 99%.
Anschließend wird die Probe zwei Sekunden lang unter langsam fließendem Wasser gespült und danach in einem handelsüblichen, schwefelsauren Nickelsulfatelektrolyten 10 min lang bei 500 C und 2 A/dm2 vernickeln Die Stärke der abgeschiedenen Nickelschicht beträgt 5,5/um. Ihre Haftung auf der Nickelunterlage genügt allen Anforderungen.Then the sample is poured under slowly flowing water for two seconds Rinsed with water and then in a commercially available, sulfuric acid nickel sulfate electrolyte Nickel plating for 10 minutes at 500 C and 2 A / dm2 The thickness of the deposited nickel layer is 5.5 / µm. Their adhesion to the nickel backing meets all requirements.
Beispiel 2: Ein mit Nickel bedampfter, gläserner Objektträger wird nach Aktivierung mit einer Aktivierungslösung gemäß Beispiel 1 60 min bei 88-91° C in ein handelsübliches Bad zur stromlosen chemischen Vernickelung getaucht. Die Stärke der abgeschiedenen, gut haftenden Nickelschicht beträgt 11 um Beispiel 3: Der Aktivierungslösung gemäß Beispiel 1 wird 0,1 g>Palladiumchlorid pro Liter zugesetzt. Nach einer Abscheidungsdauer von 60 min bei 900 C in einem handelsüblichen Bad zur stromlosen chemischen Vernickelung entsteht auf einer Unterlage entsprechend Beispiel 1 oder 2 eine haftfeste Schicht von 16/um Dicke.Example 2: A glass slide coated with nickel is made after activation with an activating solution according to Example 1, 60 min at 88-91 ° C immersed in a commercially available bath for electroless chemical nickel plating. the The thickness of the deposited, well-adhering nickel layer is 11 to Example 3: The activation solution according to Example 1 becomes 0.1 g> palladium chloride per liter added. After a deposition time of 60 minutes at 900 ° C. in a commercially available Bath for electroless chemical nickel plating is created accordingly on a base Example 1 or 2 an adhesive layer 16 µm thick.
Beispiel 4: Der Aktivierungslösung gemäß Beispiel 1 wird 0,1 g Silbernitrat pro Liter zugesetzt. Nach einer Abscheidungsdauer von 30 min bei 500 C und 2A/dm2 Stromdicke in einem handelsüblichen, schwefelsauren Nickelsulfatelektrolyten wird auf einer Unterlage entsprechend Beispiel 1 oder 2 eine 17/um dicke, gut haftende Nickelschicht erzielt.Example 4: The activation solution according to Example 1 is 0.1 g of silver nitrate added per liter. After a deposition time of 30 min at 500 C and 2A / dm2 Current thickness in a commercially available, sulfuric acid nickel sulfate electrolyte on a base according to example 1 or 2 a 17 / µm thick, well adhering Nickel layer achieved.
Claims (8)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19752503317 DE2503317C3 (en) | 1975-01-28 | Process for the chemical activation of nickel surfaces as a pretreatment for galvanic or electroless metal deposition |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19752503317 DE2503317C3 (en) | 1975-01-28 | Process for the chemical activation of nickel surfaces as a pretreatment for galvanic or electroless metal deposition |
Publications (3)
Publication Number | Publication Date |
---|---|
DE2503317A1 true DE2503317A1 (en) | 1976-07-29 |
DE2503317B2 DE2503317B2 (en) | 1976-11-04 |
DE2503317C3 DE2503317C3 (en) | 1977-06-16 |
Family
ID=
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5200272A (en) * | 1988-04-29 | 1993-04-06 | Miles Inc. | Process for metallizing substrate surfaces |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5200272A (en) * | 1988-04-29 | 1993-04-06 | Miles Inc. | Process for metallizing substrate surfaces |
Also Published As
Publication number | Publication date |
---|---|
DE2503317B2 (en) | 1976-11-04 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
DE2630151C2 (en) | ||
DE3031501C2 (en) | ||
DE2014285C3 (en) | Process for preparing aluminum or aluminum alloy surfaces for electroless nickel plating | |
DE4432591A1 (en) | Coating process for a nickel-titanium alloy component | |
DE3317493C2 (en) | ||
DE3030919A1 (en) | COMPOSITION AND METHOD FOR CHEMICAL DETACHING OF METAL DEPOSITS | |
EP1088117B1 (en) | Method for depositing a metallic layer on a polymer surface of a workpiece | |
DE2254857C3 (en) | Process for making wear resistant nickel dispersion coatings | |
EP0183925B1 (en) | Process for etching the walls of through-holes in synthetic-resin boards to be used in the manufacture of printed circuits | |
DE2503317C3 (en) | Process for the chemical activation of nickel surfaces as a pretreatment for galvanic or electroless metal deposition | |
DE2503317A1 (en) | Pretreatment of nickel prior to a plating treatment - using mixt. of sulphuric, phosphoric, nitric and acetic acids | |
DE2512339A1 (en) | PROCESS FOR CREATING AN ADHESIVE METAL LAYER ON AN OBJECT MADE OF ALUMINUM, MAGNESUM OR AN ALUMINUM AND / OR MAGNESIUM BASED ALLOY | |
EP0146723A1 (en) | Process for activating the adhesion properties of polyamide substrates for electroless metallization | |
DE656663C (en) | Process for the electrolytic coating of aluminum and aluminum alloys with metals | |
DE1794029C3 (en) | Process for the pretreatment of the surface of objects made of polyethylene or polypropylene or corresponding copolymers for chemical nickel plating | |
DE2448148C3 (en) | ||
DE2200527A1 (en) | Method for applying a metallic coating to a workpiece made of titanium or titanium alloy and, according to this method, a workpiece made of titanium or titanium alloy provided with a metallic coating | |
DE2259544A1 (en) | METHOD OF ELECTRONICALLY PLATING A PLASTIC SUBSTRATE WITH A METAL | |
DE1771930C3 (en) | Process for the pretreatment of the surfaces of plastic articles for chemical nickel plating | |
DE1947003C (en) | Process for electroless copper plating of aluminum and its alloys | |
DE19815175A1 (en) | Process for the surface metallization of plastic parts used in a galvanic hearth | |
DE1796217C2 (en) | Cyanide-free, bright zinc bath containing sodium zincate | |
DE3925840A1 (en) | METHOD FOR PRODUCING COATS ON ZINC | |
DE1794029B2 (en) | PROCESS FOR PRE-TREATMENT OF THE SURFACE OF OBJECTS MADE OF POLYETHYLENE OR POLYPROPYLENE OR THE APPROPRIATE MIXED POLYMERIZED FOR CHEMICAL NICKEL-PLATING | |
DE1812040C3 (en) | Process for chemical nickel plating of the surfaces of aluminum and aluminum alloys |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C3 | Grant after two publication steps (3rd publication) | ||
E771 | Valid patent as to the heymanns-index 1977, willingness to grant licences | ||
8339 | Ceased/non-payment of the annual fee |