EP1081252A1 - Procédé de placage sélectif - Google Patents

Procédé de placage sélectif Download PDF

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Publication number
EP1081252A1
EP1081252A1 EP99202857A EP99202857A EP1081252A1 EP 1081252 A1 EP1081252 A1 EP 1081252A1 EP 99202857 A EP99202857 A EP 99202857A EP 99202857 A EP99202857 A EP 99202857A EP 1081252 A1 EP1081252 A1 EP 1081252A1
Authority
EP
European Patent Office
Prior art keywords
plating
stripping
objects
plated
process according
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Withdrawn
Application number
EP99202857A
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German (de)
English (en)
Inventor
Fernando Franciscus Antonius Maria Van Der Pas
Jan Jaques Marie Hendriks
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
MacDermid Enthone BV
Original Assignee
Enthone OMI Benelux BV
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Enthone OMI Benelux BV filed Critical Enthone OMI Benelux BV
Priority to EP99202857A priority Critical patent/EP1081252A1/fr
Priority to PCT/US2000/020808 priority patent/WO2001016404A1/fr
Publication of EP1081252A1 publication Critical patent/EP1081252A1/fr
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F5/00—Electrolytic stripping of metallic layers or coatings
    • 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
    • C25D5/02—Electroplating of selected surface areas
    • C25D5/022—Electroplating of selected surface areas using masking means
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/04—Tubes; Rings; Hollow bodies

Definitions

  • the invention relates to a process for providing objects with a metal plating. More specifically it relates to electrolytically plating of objects, which objects have shapes that may result in a non-uniform current density distribution during electrolytic processes.
  • objects can for instance be objects with an inner and an outer surface, for example cylinders, sockets, cup-shaped objects and flat objects comprising holes, but also objects with an outer surface only, such as connector pins, or even flat surfaces such as metal strips where, dictated by geometry, metal(gold) may be plated on unwanted area.
  • the object to be plated is electrically contacted to the cathode, and is immersed in a solution comprising cations of the plating metal.
  • the counter electrode is also immersed in the solution.
  • the distribution factor DF is the ratio of the thickness of the metal layer plated on unwanted areas to the thickness of the metal layer plated on wanted area, and generally is substantially larger than 1, more specifically larger than 2.
  • the plating rate will normally be higher on the areas of the objects where the current density is higher. This can be a problem when it is desired that the thickness of the plating at areas of a low current density is higher than that of areas with a high current density.
  • US-A-5,476,581 relates to a method for producing a weapon barrel having a wear resistant inner coating.
  • the inner surface of a prefabricated weapon barrel is subjected to an electrolytic polishing process, followed by an electrolytic plating process.
  • the cathode is placed inside the barrel in order to obtain the required selectivity, i.c. a coating on the inside of the barrel.
  • US-A-5,372,700 teaches a method for selective electrolytic deposition of a metal such as gold onto the inside surface of a bush type hollow body.
  • the selectivity is obtained by injecting the electrolytic solution inside the hollow body and passing a current between the bush and an electrode in electrical contact with the solution.
  • US-A-5,516,415 and US-A-5,527,445 relate to processes for electroforming a structural layer of metal bonded to an internal wall of a metal tube. Deposition on the inside of the tube is obtained by inserting a probe and moving it to span the desired sections.
  • metal distribution on non-uniform objects can be improved by first forming a plating on the surfaces or selected parts of the surfaces of the objects in an electrolytic plating process yielding a certain DF value, which preferably is as low as possible, followed by stripping of the initial plating in an electrolytic stripping process using a stripping solution under such conditions that the DF value is lowered.
  • the stripping rate depends e.g. on the non-uniform current density distribution on each of said objects, and the chemistry of the stripping solutions.
  • the initial plating will have to result in thicker plating layers than required in the final product.
  • the present invention relates to a process for plating an object, having wanted and unwanted areas to be plated, comprising the steps of
  • the total surface of the non-uniform object is plated yielding a certain DF value, which preferably is close to 1, and subsequently is stripped wherein the DF value is lowered through a difference in current distribution and efficiency during stripping.
  • the DF value preferably is much lower than 1, and more preferably lower than 0.5.
  • the DF value can also be improved or can be further lowered by e.g. controlled immersion stripping of for example connector pins when no deposit is required on the connector tip or by means of masking techniques where only unwanted areas of the originally plated spot are exposed to the stripping solution for example spot plating and subsequent spot stripping yielding a nett improved selectivity for metal deposition.
  • the object is fully or partly immersed in a plating bath and subsequently partly immersed in a stripping solution.
  • This embodiment can suitably be carried out in a so-called reel to reel connector or lead frame line.
  • the immersion of the plated object in the stripping bath is controlled in such a way that only a part of the surface plated is subjected to stripping.
  • the object to be plated is first shielded with a mask creating or defining a specific free area, e.g. in the form of a spot or stripe.
  • the surface with the mask is subjected to a plating step, after which the mask may be removed and subsequently a second mask is applied covering part of the plated surface, whereafter the object is subjected to the stripping solution.
  • the process according to the present invention has several advantages.
  • One advantage is that objects can be obtained with a plating that has a required thickness for there were it is needed and a plating that is thin or even absent on areas where no plating is required.
  • plated objects such as loose parts can be obtained that could otherwise not be produced without controlling the plating rate locally.
  • the plating rate is controlled for example by applying means to the objects to be plated in order to shield the areas on which less plating is desired from the coating process. Applying such means lead to more expensive processes. Moreover, such methods are more cumbersome when the size of the objects to be plated is smaller, and would be very difficult to be carried out with very small objects.
  • the metal to be plated is a precious metal or an alloy thereof. Suitable and preferred precious metals are gold, silver, ruthenium, palladium, rhodium, platinum and iridium, and mixtures thereof, while the alloys of these metals with cobalt, nickel, iron, indium, thallium, copper, cadmium, and so on, are suitable as well.
  • the conditions during the initial plating process are chosen such that the DF value is as low as possible.
  • areas of higher current density will generally obtain an initial plating with a higher thickness than the areas of lower current density.
  • the selectivity for example expressed as the ratio of the rate of removal from the areas where the current density is higher and the rate of removal from the areas where the current density is lower, is higher than the ratio of the two corresponding initial plating rates. In this way, the stripping will result in a final plating on the objects that is thinner on the areas where the current density during stripping was higher than on the areas where the current density during stripping was lower.
  • the initial plating is applied using conventional electrolytic plating processes.
  • Loose part plating can be performed using e.g. vibratory equipment or barrel equipment or any other means to plate loose parts. In all cases these loose parts are being completely exposed to the plating solution. In case of other objects selectivity in plating may be obtained with techniques such as controlled immersion, reel to reel applications for connector reels, or spot galvanising by using masks.
  • the electrolytic plating process is carried out using solutions comprising the ion of the metal to be plated and additional ingredients which influence the initial metal distribution required for the specific applications. After all, metal distribution is not only dependent on geometrical factors buts also on chemical and electrochemical factors and compositions.
  • AUTRONEX HSV, AUTRONEX 2910 are the preferred processes for loose part plating, yielding the lowest initial DF values, although also baths containing other ingredients such as potassium and/or ammonium sulphate and/or sulfamates, chelating agents, metal salts such as cobalt and nickel salts and conducting salts, or other processes such as AutronexTM CC and/or OmegaTM C can be used. Additives used in Autronex baths are described in e.g. US-A-5,169,514.
  • the stripping process can be conducted in a similar process step, the important difference being the reversal of the current.
  • the plated object is contacted to the anode and submerged in a solution, esp. in an aqueous solution, comprising phosphates, esp. monophosphates, hydroxides, sulfamates, cyanates and/or thiocyanates of alkali metals, e.g. sodium or potassium, or ammonium; or thiourea or derivatives thereof.
  • Stripping can preferably be conducted in a process like MetalexTM EL-M.
  • the basis of Metalex EL-M is a mixture of sodium thiocyanate and sodium hydroxide.
  • This stripping bath is especially suitable for gold.
  • this stripping bath may contain conventional additives to manipulate the stripping behaviour (e.g. the conductivity, organic adsorbents, etc.) where needed.
  • the main requirement of the material of the objects to be plated by the process of the present invention is that they are electrically conductive. Metal objects will therefore be preferred.
  • the size of the objects to be plated is not a limiting factor. Even small objects, especially smaller than 25 mm and even smaller than 5 mm can be plated in the plating process according to the invention.
  • the substrate material can be any electrolytically plateable metal.
  • the stripped material can be recovered from the stripping solution with economical advantage. Recovering of the material will be especially beneficial when noble metals, such as gold, silver, platinum, palladium or rhodium are used.
  • the shape of loose parts to be used in the process according to the present invention has to be non-uniform, for example objects that comprise an inner and an outer surface.
  • Preferred shapes are open cylinders, cup-shaped objects and flat objects comprising at least one hole.
  • gold plated female connectors are objects that are especially suitable to be manufactured with the process according to the present invention. Due to their small size, such connectors are plated preferably in large amounts simultaneously, for instance several thousands per batch. Since the gold plating is only required on the inside of such connectors, producing these connectors with less gold plating or even no gold plating at all on areas where it is not required can be of great economical advantage. Producing female connectors with a gold plating that is selectively formed on the inside is enabled by the present invention.
  • Small objects such as loose parts
  • a vibrating barrel provided with means to contact each of the objects at least for a part of the plating time or stripping time with an electrode.
  • a suitable example is a vibrobot.
  • a vibrobot barrel is basically an open circular basket with a bottom electrode. The loose parts are put in the basket and the total is immersed in the plating or stripping solution. The basket then is vibrated with such frequency and amplitude, that the parts start rotating around the periphery of the basket.
  • the bottom has a shape of half a turn of a screw so when the parts rotate they tumble and mix every time they fall over the edge.
  • the bottom electrode is the cathode when plating and the anode when stripping.
  • step (b) is generally carried out at temperatures between 10 and 80°C, although these temperature ranges do not give an essential limitation.
  • step (b) is carried out at a temperature of between 30 and 60°C.
  • step (b) is generally performed using a current density of 0.01 - 4A/dm 2 , preferably of 0.1 - 2A/dm 2 .
  • the current density is generally in the range of 1 - 100 A/dm 2 , and preferably between 2 and 50 A/dm 2 when larger objects have a less complicated shape are to be plated. More in particular, these current densities can suitably be used when the controlled immersion technique or the spot stripping technique in accordance with the second and third preferred embodiment of the present invention, is carried out.
  • the duration of the stripping step can vary between 5 seconds and 30 minutes or more, preferably between 30 seconds and 10 minutes. It depends on the applied current density but also on other parameters in the stripping process. In the light of the information given in this specification the person skilled in the art will have the knowledge and tools to find suitable conditions.
  • Electrode-EL-M has proved to be effective for this application.
  • An example of a batch-wise process uses a rotating barrel in which loose parts are placed.
  • the barrel used in the plating process is provided with means to contact the objects with the cathode. This can be obtained for instance by using a basket which comprises holes and by placing the cathode in contact with these loose parts.
  • the anode is in contact with the electrolytic liquid.
  • a similar set-up can be applied, in which the object is contacted to the anode and the stripping liquid to the cathode. Homogeneous mixing of the objects is again obtained by rotating the barrel or the basket.
  • a vibrobot barrel is basically an open circular basket with a bottom electrode.
  • the loose parts are put in the basket and the total is immersed in the plating or stripping solution.
  • the basket then is vibrated with such frequency and amplitude, that the parts start rotating around the periphery of the basket.
  • the bottom has a shape of half a turn of a screw so when the parts rotate they tumble and mix every time they fall over the edge.
  • the bottom electrode is the cathode when plating and the anode when stripping.
  • the current required in the plating process can be advantageously applied as a pulsed current.
  • the duty cycle for pulse plating (on/off) must be optimised for each individual application. Typically, pulses of the type 900 msec on, 100 msec off are used.
  • the process of the present invention can be a continuous controlled immersion plating and stripping process or a continuous spot plating an stripping process.
  • reel to reel connector or lead frame plating a strip of connectors is pulled through a series of process baths. The connector strips are supplied on reels. At the beginning of the process line the strip is unwinded and at the end wound up again.
  • techniques like controlled immersion or spot processing may be used. This embodiment is described in figure 1.
  • FIG 1a connector strips are brought in a gold bath.
  • Figure 1b shows immersion of the gold plated strips in a stripping solution, while figure 1c shows the end result: gold plate on the grey area only.
  • organic additives may be present. These organic additions are electrochemically active in (depending on the additive) high or low CD regions and influence the current density gradients and so the thickness distribution. Current density is not only determined by the geometry of the body and the position and shape of the counter electrode, but also by the chemical composition of the plating/stripper solution (primary respectively secondary current distribution). Examples of such additives are given in US-A-5.169.514.
  • sockets total approximate surface area 30 dm 2 ; the individual sockets having a length of 2.25 mm, the widest diameter (see fig. 2) being 1 mm, the smallest diameter being 0.65 mm, and being made from leaded brass
  • a bath of deionized water having a conductivity of less than 3 ⁇ -Siemens 600 ml/l AutronexTM CC B, 2 g/l PPS (1-(3-sulfopropyl-pyridinium betaine), 16 g/l IQPS (1-(3-sulfopropyl)-isoquinolinium betaine), and 40 g/l (NH 4 )SO 4 .
  • This bath was used with the sockets in a vibrobot set-up having a volume of 5 dm 3 at 35°C for 4 hours at a current density of 0.015 A/dm 2
  • a uniform plating thickness of 2 ⁇ m was obtained, as measured using X-ray fluorescence spectroscopy (XRF).
  • the distribution, factor (DF) which is defined here as the average thickness of the plating on the outside of the object divided by the average thickness of the plating on the inside of the object was 1.
  • Solution 1 7.5 g/l sodium hydroxide and 70 g/l sodium thiocyanate in demineralized water (having a conductivity of less than 4 ⁇ -Siemens).
  • Solution 2 50 g/l potassium mono phosphate, 40 g/l sodium hydroxide and 55 g/l sodium thiocyanate in demineralized water (having a conductivity of less than 4 ⁇ -Siemens).
  • the sockets were subjected to three different stripping procedures:
  • the DF-values are measured by determining the thickness of the plating on 16 randomly chosen places at 16 randomly picked different sockets by using XRF. The results are summarized in Figures 3 - 5.
  • 150 g sockets (surface area 30 dm 2 ) were gold plated using a gold bath (AutronexTM CC (cobalt hardened gold)) having a gold concentration of 1 g/l, in vibratory equipment (see example 1) at a temperature of 35°C and a current density of 0.1 A/dm 2 , for 60 minutes.
  • the plated sockets obtained had an average thickness of 1.15 ⁇ m and a DF of 1.
  • the sockets were subjected to a stripping step using Metalex stripper bath MetalexTM EL-M containing 5 - 40 g/l sodium hydroxide and 55 g/l sodium thiocyanate under the following conditions:
  • Procedure 1 Procedure 2 Measurement No. Thickness Inside ⁇ m Thickness Outside ⁇ m Thickness Inside ⁇ m Thickness Outside ⁇ m 1 0.69 0.56 0.84 0.08 2 0.66 0.39 0.88 0.36 3 0.65 0.49 0.87 0.27 4 0.61 0.37 0.94 0.39 5 0.69 0.54 0.88 0.27 6 0.72 0.44 0.98 0.37 7 0.99 0.44 0.71 0.23 8 0.50 0.49 0.86 0.15 9 0.64 0.31 0.81 0.36 10 0.50 0.52 0.40 11 0.74 0.53 0.26 12 0.58 0.56 0.32 13 0.56 14 0.52 15 0.41 16 0.46 Mean 0.696 0.475 0.863 0.288 DF 0.68 0.33
  • 150 g sockets (surface area 30 dm 2 ) were gold plated by using an AutronexTM HSV (2 g/l Au) plating bath, pH 4.8, room temperature, 0.05 A/dm 2 , 35 minutes. subsequently, the plated sockets were subjected to a stripping step using different versions of METALEX EL-M (as identified in table 2). Plating thickness of Example 3 No.

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  • 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)
EP99202857A 1999-09-02 1999-09-02 Procédé de placage sélectif Withdrawn EP1081252A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP99202857A EP1081252A1 (fr) 1999-09-02 1999-09-02 Procédé de placage sélectif
PCT/US2000/020808 WO2001016404A1 (fr) 1999-09-02 2000-08-31 Procede servant a ameliorer le placage selectif d'objets non uniformes par abaissement du facteur de distribution

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EP99202857A EP1081252A1 (fr) 1999-09-02 1999-09-02 Procédé de placage sélectif

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6887331B2 (en) 2000-07-25 2005-05-03 Firma Carl Freudenberg Method and device for producing a spunbonded nonwoven fabric
EP3059277A1 (fr) * 2015-02-23 2016-08-24 Enthone, Incorporated Composition d'inhibiteur pour racks lors de l'utilisation de gravures exemptes de chrome sur des processus plastiques
US10054286B2 (en) 2014-07-04 2018-08-21 The United States Of America, As Represented By The Secretary Of Commerce, The National Insitute Of Standards And Technology Optical transformer, process for making and use of same

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0410955A1 (fr) * 1989-07-24 1991-01-30 Maschinenfabrik Andritz Actiengesellschaft Procédé pour revêtir les objets plats sur une face par électrodéposition
US5098534A (en) * 1988-10-11 1992-03-24 C. Uyemura & Co., Ltd. Composition and method for electrolytically stripping silver

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2423536A1 (fr) * 1978-04-17 1979-11-16 Interox Compositions et procede pour le lavage et le blanchiment
DE3108358C2 (de) * 1981-03-05 1985-08-29 Siemens AG, 1000 Berlin und 8000 München Vorrichtung zum partiellen Galvanisieren von zu elektrisch leitenden Bändern, Streifen oder dgl. zusammengefaßten Teilen im Durchlaufverfahren
FR2688804A1 (fr) * 1992-03-20 1993-09-24 Souriau & Cie Procede de depot electrolytique selectif d'un metal notamment d'un metal noble tel que l'or sur la face interne de corps creux en forme de douille notamment d'elements de contact de connecteur machine pour la mise en óoeuvre du procede, produit obtenu.
US5268045A (en) * 1992-05-29 1993-12-07 John F. Wolpert Method for providing metallurgically bonded thermally sprayed coatings
DE4335139A1 (de) * 1993-10-15 1995-04-20 Rheinmetall Ind Gmbh Verfahren zur Herstellung eines Waffenrohres mit einer verschleißfesten Innenbeschichtung

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5098534A (en) * 1988-10-11 1992-03-24 C. Uyemura & Co., Ltd. Composition and method for electrolytically stripping silver
EP0410955A1 (fr) * 1989-07-24 1991-01-30 Maschinenfabrik Andritz Actiengesellschaft Procédé pour revêtir les objets plats sur une face par électrodéposition

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6887331B2 (en) 2000-07-25 2005-05-03 Firma Carl Freudenberg Method and device for producing a spunbonded nonwoven fabric
US7191813B2 (en) 2000-07-25 2007-03-20 Firma Carl Freudenberg Method and device for producing a spunbonded nonwoven fabric
US10054286B2 (en) 2014-07-04 2018-08-21 The United States Of America, As Represented By The Secretary Of Commerce, The National Insitute Of Standards And Technology Optical transformer, process for making and use of same
EP3059277A1 (fr) * 2015-02-23 2016-08-24 Enthone, Incorporated Composition d'inhibiteur pour racks lors de l'utilisation de gravures exemptes de chrome sur des processus plastiques

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WO2001016404A1 (fr) 2001-03-08

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