US3853094A - Electroless plating apparatus - Google Patents

Electroless plating apparatus Download PDF

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US3853094A
US3853094A US00103355A US10335571A US3853094A US 3853094 A US3853094 A US 3853094A US 00103355 A US00103355 A US 00103355A US 10335571 A US10335571 A US 10335571A US 3853094 A US3853094 A US 3853094A
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United States
Prior art keywords
plating
bath
articles
particles
electroless plating
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US00103355A
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Inventor
T Christini
W Flynn
J Inskeep
H Mccauley
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EIDP Inc
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EI Du Pont de Nemours and Co
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Priority to US00103355A priority Critical patent/US3853094A/en
Priority to CA131,852A priority patent/CA962537A/en
Priority to IT19428/72A priority patent/IT946624B/it
Priority to IE69/72A priority patent/IE35988B1/xx
Priority to CH93572A priority patent/CH585277A5/xx
Priority to GB308872A priority patent/GB1382101A/en
Priority to JP769972A priority patent/JPS5624032B1/ja
Priority to AU38157/72A priority patent/AU469973B2/en
Priority to FR7202225A priority patent/FR2123369B1/fr
Priority to BE778401A priority patent/BE778401A/xx
Priority to DE19722203230 priority patent/DE2203230C3/de
Priority to NL7201005A priority patent/NL7201005A/xx
Priority to US05/469,499 priority patent/US3940512A/en
Application granted granted Critical
Publication of US3853094A publication Critical patent/US3853094A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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
    • C23C18/31—Coating with metals
    • C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1619—Apparatus for electroless plating
    • 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
    • C23C18/1601—Process or apparatus
    • C23C18/1633—Process of electroless plating
    • C23C18/1655—Process features
    • C23C18/1662—Use of incorporated material in the solution or dispersion, e.g. particles, whiskers, wires
    • 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
    • C23C18/52—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 using reducing agents for coating with metallic material not provided for in a single one of groups C23C18/32 - C23C18/50

Definitions

  • this invention comprises apparatus for concomitant particulate deposition in electroless plating comprising contacting articles to be plated with a continuously circulating electroless plating solution containing suspended particulate material which it is desired to deposit on said articles, and subjecting the articles to tumbling within the plating solution for a sufficient time to obtain a preselected amount of electroless plating with concomitant deposition of particulate material on the articles, and the product thereof.
  • FIG. 1 is a cross-sectional side elevation view of an apparatus wherein the plating solution is supplied in generally upward vertical flow
  • FIG. 2 is a cross-sectional side elevation view of an apparatus for plating buoyant articles wherein the plating solution is supplied in generally downward vertical flow,
  • FIGS. 3A and 3B are, respectively, plan and side elevation cross-sectional views of a first design of apparatus for conducting plating in sequential stages
  • FIG. 4 is a partially cross-sectional perspective view of a second design of apparatus for conducting plating in sequential stages
  • FIGS. 5A and 5B are, respectively, plan and side elevation cross-sectional views of an apparatus incorporating a continuous spiral baffle for effecting continuous, as distinguished from batch, plating.
  • Electroless metal plating of both electrically conductive and electrically non-conductive articles is known to the prior art; however, there exist serious problems as regards plating bath stability.
  • the soluble nickel salt in this instance dissolved NiCl '6- H O, is reduced by an alkali metal borohydride (NaBI-L) in order to plate out nickel on an object immersed in the bath.
  • NaBI-L alkali metal borohydride
  • the Patent reported prior art difficulties with more or less sudden bath decomposition, during which Ni metal flakes either formed, or a heavy black precipitate dropped out when the concentration of the plating metal in the baths had decreased from to percent in the course of plating.
  • the Patent solution to this problem was to add an organic divalent sulfur compound as stabilizer.
  • Bath compositions suitable for use in this invention can cover a wide range; however, those operating at lower temperatures, e.g., in the range from about 30C. to 60C. are particularly preferred.
  • the best available baths from the standpoint of inherent stability are, of course, preferred, and those of US. Pat. No. 3,234,031
  • Typical metallic-alloy matrices deposited can consist of the Ni-P alloy coatings deposited by the processes taught in U.S. Pat. Nos. 2,532,283; 2,658,841; 2,658,842, and others. Or one can equally well utilize the Ni-B alloy coatings of U.S. Pat. Nos. 3,096,182;
  • Electroless plating which is sometimes referred to as chemical reduction plating, occurs by catalytic reaction between metal ions or compounds and a reducing agent dissolved in an appropriate solvent.
  • electroless Ni-P coating processes hereinabove mentioned typically proceed when aqueous solutions containing the reductant H POf ions exist within a bath containing nickel ions supplied by dissolved nickel salts.
  • the electroless Ni-B coating processes typically proceed when aqueous solutions containing a boron reducing agent, such as BH, ions or dimethylamine borane, are present in the nickel ion bath.
  • All practical electroless plating baths also contain buffers, e.g., salts of weak carboxylic or dibasic acids, to prevent rapid changes of pH, plus at least one ofa large variety of chemical additives which have been found to stabilize against spontaneous bath decomposition.
  • Electroless plating is an autocatalytic process in the sense that the coating deposited serves as a catalyst for continuation of the plating action; Once plating has been initiated on the surface of a metallic, ceramic, or polymeric substrate, it continues as long as the substrate remains in contact with the plating solution. Because a uniform coating of any desired thickness can be applied by direct chemical reaction, without the passage of an electric current, the process was denoted electroless plating by Brenner and Riddell, who developed the first practical Ni-P processes (refer to J. Research, National Bureau of Standards, Vol. 37, p. 31 (1946), Brenner, A. and Riddell, G. E).
  • phase dispersed in the metallic alloy coatings of this invention can consist of a broad variety of particulate materials. Where wear resistance is the desideratum, hard inorganic particles such as oxides, carbides, nitrides, silicides, borides, diamond metallic or various intermetallic compounds are suitable.
  • the particles are preferably approximately equiaxial in shape, with an average size ranging from about 0.1p. to about and a length-to-width ratio ranging from about 2:1 to about 20: 1'.
  • Typical powders are described in the following:
  • Particle settling rate is a function of particle size as well as the viscosity of the plating bath. Settling is also affected by particle concentrations, or loading, and degree of bath agitation.
  • Plating rate is influenced by many factors, which include among others (a) pH of the plating solution, (b) concentration of the reductant, (c) temperature of plating bath, ((1) concentration of metal ions, and (e) ratio of bath volume to plating area.
  • Some plating of the metal onto the fine particles while they are in suspension can occur, depending upon the nature of the particles and whether they have been made catalytically active. Ordinarily, no preparatory treatment of the fine particles is necessary.
  • the surface of the object to be plated will, in general, have been prepared to receive an adherent coating of metal and occluded particles by a suitable cleaning and chemical pretreatment prior to the electroless plating procedure. In all cases, for nonconductive substrates, the article to be plated will have been given a preliminary metal strike to help secure the particles.
  • the additions of particles to be occluded in the metal matrix can be kept in suspension for the required time periods by agitating the bath solution, which also causes the-particles to be moved into contact with the surface to be plated.
  • the bath agitation resorted to in our process utilizes continuous circulation of the plating bath through a contacting zone of progressively expanding crosssection in order to obtain a tumbling suspension of the articles to be plated at all times during which they are in the plating zone.
  • the process of this invention is concerned with the handling of particle additives in the range of about 0.05p. p. particle size while controlling the bath agitation to maintain these particles in suspension for a time sufficient to effect composite plating of an immersed substrate, during which time bath conditions within which uniform penetration and distribution of the plating bath solution is required.
  • racks prevent complete encapsulation of articles to be plated, since there must be some point of attachment to, or bearing support provided by, the racks.
  • the elimi nation of racks altogether is advantageous for numerous reasons.
  • the mode of agitation of this invention has increased the tolerance of electroless plating baths for particulate solids, so that very high levels, e.g., up to g./l., have been utilized without inducing bath decomposition.
  • very high levels e.g., up to g./l.
  • This is an unexpected benefit, especially in electroless plating, which permits lay-down of very concentrated particulate inclusions.
  • effective particulate suspensions have been maintained over very long time periods, bath lives in excess of 60 hours being routinely obtained using our process.
  • the polymers employed were two varieties of commercially available plating grade acrylonitrilebutadiene-styrene, specifically, Borg Warner Co. EP3510 and the glass-fortified AFl004 of Liquid Nitrogen Processing Corporation.
  • the pretreatment was in the following sequence with a given group of articles placed in a stainless steel wire basket for convenient step-by-step handling:
  • the articles were chemically roughened by immersion in a proprietary chromic-sulfuric acid etch (e.g., Marbon E-), immersion being for 4-6 mins. at
  • step 4 To remove any etch solution carry-over from step 3) the articles were rinsed in hot and cold water for 3 secs. each, followed by an ultrasonic water rinse of 2 mins. and a final rinse with running de-ionized water.
  • steps 2)( 4), inclusive would be substituted for steps 2)( 4), inclusive, to achieve roughening of the ceramic surface.
  • mechanical roughening might be substituted for chemical roughening.
  • a low C steel is prepared for plating by solvent degreasing (e.g., acetone or trichloroethylene), alkaline cleaner and then a rinse in 50 vol. percent HCl solution with rinses in de-ionized water after each step. The parts could then be placed directly in the tumble plating bath.
  • solvent degreasing e.g., acetone or trichloroethylene
  • alkaline cleaner e.g., acetone or trichloroethylene
  • tbmble plater utilizes a large frustoconical funnel l0 coaxially disposed within, and somewhat above, a larger funnel 11 constituting a sump for reception of the gravity exhaust of plating solution 9 I from funnel l0.
  • Peripherally spaced small size ports 12 in funnel 10 permit free overflow of solution (and suspended particulate solids) from this funnel without escape of the articles 14 being plated.
  • the plating solution is continuously recycled from the apex 11a of the lower funnel via pump 15 and recirculating line 16, which latter discharges into the apex 10a of funnel 10.
  • a typical plating bath composition can be as taught in US. Pat. No. 3,234,031 supra, with bath temperatue maintained at about- 55C.
  • Pretreated articles to be plated are dumped into funnel 10 and initially tend'to settle to the bottom under gravitational force. However, as they approach the bottom they encounter the upwardly directed jet stream-of suspended particles recycled by pump 15 via line 16.
  • a very complex article tumbling action results from the turbulence of the jet flow, the gradual deceleration of upward solution travel with progressive cross-sectional increase of funnel l0 and random collisions between the articles being plated. Most of these collisions tend to rotate the articles, causing a random non-directional agitation of the parts.
  • the degree of bath agitation depends on the velocity of plating solution supply and the number of articles charged into the plater, as well as 7.
  • the articles were then placed in a proprietary activation bath (Enthone -440) containing Pd ions. The tin ions are thus further oxidized, under gentle agitation for 1.5 mins., thereupon reducing the Pd ions to metallic state.
  • the preplate treatment is the same as hereinbefore described, except that a different treatthe size and degree of loading of suspended particles.
  • tumble plating is positively advantageous, because it favors the formation of uniform surface topography free from burrs and massive nodules. Moreover, there is obtained a more uniform dispersion of occluded particles in the plate coat. Elimination of article-holding racks permits easy inspection of individual articles in process by simply scooping them out as An extremely important advantage of tumble plating is the increased throwing power thereby obtained. This results from the impingement-of a high-velocity stream of plating solution, containing suspended particles, which impacts all surfaces of the substrate plated in random manner within the bath. This unique action distinguishes tumble plating from conventional prior art barrel plating methods used in electroplating composites, affording the following advantages:
  • a high volume percentage of particles is incorporated into the plate coat at relatively low bath loading factors of weight of powder/liter plating solution.
  • FIG. 2 For buoyant articles 14, the apparatus of FIG. 2 can be employed, which utilizes an inverted frustoconical funnel 10' provided with ports 18 at its upper, constricted, end through which the articles can be conveniently introduced. With this design a cylindrical sump 19 is provided in open communication at its lower end with funnel l, recirculation of plating solution being obtained by pump 15 having its intake connected via line 16' to the bottom of sump l9 and its discharge to the upwardly disposed apex a of funnel 10'.
  • pump 15 having its intake connected via line 16' to the bottom of sump l9 and its discharge to the upwardly disposed apex a of funnel 10'.
  • Apparatus can be constructed from a wide variety of materials, such as Pyrex brand glassware, stainless steel, or stainless steel coated with a suitable corrosionresistant polymer coating. Frequently, cleaning with nitric acid solution is desirable, and appropriate corrosion. resistance must then be provided.
  • FIG. I A specific apparatus constructed generally according to FIG. I utilized a frustoconical plating chamber 10 of 7 inches top diameter, the interior angle of the chamber being 48. A 2 inch high cylindrical rim was adhered to the top of the funnel and this was provided with twelve A inch dia. liquid overflow holes spaced equaly around the periphery.
  • the diameter of feed and outlet tubes was /s inch id. and the pump utilized was a Cole-Parmer 1/35 l-l.P. sealess magnetic drive centrifugal pump with polypropylene body and impeller.
  • the elbow connecting with orifice 10a was inch vertical dimension.
  • the plating bath composition employed in the following examples was a standard DMAB (i.e., dimethylamine borane) reductant bath, as follows:
  • Solution 1 The bath was prepared from a number of stock solutions which are numbered as follows for convenient reference:
  • TDGA i.e. thiodiglycolic acid
  • Solution 1V DMAB i.e., dimethylamine borane
  • the DMAB bath was operated under the following conditions:
  • the acrylonitrile-butadiene-styrene EP3510 articles consisted of five rectangles of dimensions /a inch X inch X 4 inch, with a hole A; inch diameter, /8 inch long, and a hole 1/16 inch diameter, /8 inch long, together with five rectangles of dimensions Vs inch inch X 4 inch with a hole 1/32 inch diameter, /a inch long, and a hole 1/64 inch diameter, /s inch long.
  • the articles were first taken through the standard polymer preplate line hereinbefore described.
  • EXAMPLE 1 One lot of specimens as described, was taken from the polymer preplate line and placed-for 10 mins. in a 4- liter beaker which contained a standard DMAB plating bath, with gentle agitation being provided to the parts by manually imparting an up-and-down motion to the stainless steel basket in which they were contained. The specimens, plated with a thin nickel strike, were then transferred by dumping from the basket into the plating chamber of the tumble plater (FIG. 1), which also contained the standard DMAB plating bath. Plating ensued for 1 hr. in this bath, free of any hard-particle additions. Then a quantity of aAl O of hexagonal crystal structure and an equiaxed shape with average particle size of 0.31.1.
  • Metallographie and X-ray examination confirmed the presence of composite aAl O -electroless Ni-B deposit on the polymer substrates. Also, metallographic examination confirmed the presence of a composite coating in all hole diameters.
  • Quantimet analysis i.e., the Quantimet Image Analyzing Computer marketed by Metals Research, Ltd, Hertz, England
  • 13.1 vol. percent of otAl O was present in the composite layer.
  • EXAMPLE 2 A second lot of specimens was taken from the polymer preplate line and placed for.10 mins. in a 4-liter beaker which contained the standard DMAB plating bath. Gentle agitation was provided to the parts by manually imparting an up-and-down motion to the stainless steel basket in which they were contained. The specimens were then emptied from the stainless steel basket into the tumble plater (FIG. 1 design) and allowed to plate for 1 hr. in this bath. The tumble plater bath was the same one as used in Example 1, except that it had been carefully filtered at the end of the preceding fun in order to remove'any suspended hard particles. At the end of the 1-hr.
  • aAl O of hexagonal crystal structure and an acicular shape with average particle size of 20 X 10 p. was introduced into the tumble plater. Over a period of 4% hrs., 12 g. of ozAl O was added to the bath at half-hour to hour intervals in 1.2 g. or 2.4 g. increments.
  • Metallographic and'X-ray examinations confirmed the presence of a composite aAl O electroless Ni-B deposit. Also, metallographic examination confirmed the presence of a composite coating in'all hole diameters. Quantimet analysis indicated that 10.1 vol. percent of aAl O was present in the composite layer.
  • Yam-line wear testing for a period of 6 hrs. using 15- denier dull monofilament with conditions of 5 break angle, 10 g. load, and 1,000 yd./min. running velocity indicatedthat the wear was 0.0163 X 10 cm lhr. Since the tumble plater bath volume was 6 liters, the aAl,O loading factor at the end of the run was 2 g./l.
  • EXAMPLE 3 A third lot of specimens was taken from the polymer preplate line and then placed in a 4-liter beaker which contained the standard DMAB plating bath for 10 mins. Gentle agitation was provided to the parts by manually imparting an up-and-down motion to the stainless steel basket in which they were contained. The specimens were then emptied from the stainless steel basket into the tumble plater (FIG. 1 design) and allowed to plate for 1 hr. in this bath. The tumble plater bath was the same one used in Example 2, except that it had been carefully filtered at the end of the preceding run in order to remove any suspended hard particles. At the end of the l-hr.
  • acicular rutile TiO of tetragonal crystal structure, and with a fiber diameter of 0.2 microns and a fiber length of 3 microns, was introduced into the tumble plater.
  • the addition was 6 g., corresponding to a loading factor of 1 g./l.
  • the composite plating period was 3% hrs.
  • Metallographic and X-ray examination confirmed the presence of a composite acicular rutile-Ni-B deposit. Also, metallographic examination confirmed the presence of a composite coating in all hole diameters.
  • EXAMPLE 4 A small wear article fabricated from glass-filled AF-1004 polymer was formed with an injection molded flared entrance-through slot measuring 7 mils wide X 40 mils long X 200 mils deep.
  • Weirs 39a and 39d define the individual plater via line 31 connected to the intake of pump 28.
  • FIG. 4 A somewhat similar design is depicted in FIG. 4, the platers 38-38d being, in this instance, trough-like in the Shipley Co., Boston, Mass. 5 stages.
  • a single pump 40 discharges into a common TABLE 11 Description of Article Substrate Holes or Particulate Total Particle Size Material Cavities Material g./l. and Shape Remarks A1 2 equiaxed no composite observed 0.3 1.
  • EP 3510 polymer size Va", H16" and shape X 1/32", and A1 0 5 equiaxed composite coating all X W) l/64" diam. 0.3;. areas, 9.1 vol.
  • FIGS. platers Transfer of articles from one plater to the next 35, inclusive. in sequence is readily effected by periodic manual ma-
  • FIGS 3 A and 3 illustrate a Series arrange nipulation of the individual valves 43a-43d, inclusive.
  • Fompanmellti Serves merely as a 2 connected at their upper ends in Order from right collector for articles 45 having finished plate coatings, to left, so that articles 25 to be plated can be impelled alftomam amok removal belng obtafned; y an in sequence from one plater to the next by appropriate cleated belt conveyor Much manipulation of valves 26 and 27 after preselected resitFmly Operated y a (not Show") to carry the dence times in each plater.
  • pump 28 is Operated to recir Compartment 38e 15 provided with an mclmed funnel culate plating solution continuously via lines 32 and 33, covered, through without transfer of the articles, but, of course, mainwhlch lmmedlately wlthqrawn vla taming tumbling at all times pump intake line 48, so that suspended particles have n l h 30 no opportunity to settle out during solution recycle.
  • a modification in this design entails cutting vertically across e g f f t (lian oriented alternately arranged slots in weirs 39a-39c 6 remove at w l at e p atmg so recyc ed (with, optionally, a shallower slot in weir 39d), so that there is continuous flow of plating solution and articles being plated through the apparatus.
  • This has the disadvantage that certain articles might dwell longer within given plating cells than others, with corresponding variation in plating coats.
  • acceptance by visual inspection cures this difficulty.
  • FIGS. A and 5B show a single funnel continuous plater 53 provided with a spiral baffle 54 defining a continuous plating path from the outside periphery to the center.
  • Baffle 54 is open at the bottom, so that a single jet 55 connected to the funnel apex 53a provides tumbling action throughout the entire plating path. Discharge of plating bath solution (and articles 57) is effected via drain connection 56 communicating with the terminal center of baffle 54.
  • Apparatus for concomitant particulate deposition in electroless plating comprising, in combination, a vertically oriented frusto-conical vessel, an electroless plating solution pump connected with discharge port in communication with the small diameter end of said frusto-conical vessel, a receiving vessel connected in open fluid communication with the large end of said frusto-conical vessel, and means connecting said receiving vessel to the intake side of said pump.

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US00103355A 1971-01-25 1971-01-25 Electroless plating apparatus Expired - Lifetime US3853094A (en)

Priority Applications (13)

Application Number Priority Date Filing Date Title
US00103355A US3853094A (en) 1971-01-25 1971-01-25 Electroless plating apparatus
CA131,852A CA962537A (en) 1971-01-25 1972-01-06 Method and apparatus for concomitant particulate deposition in electroless plating and the product thereof
IT19428/72A IT946624B (it) 1971-01-25 1972-01-15 Metodo ed apparecchiatura per la deposizione concomitante particel lare nel rivestimento per riduzio ne chimica e prodotto in tal modo ottenuto
IE69/72A IE35988B1 (en) 1971-01-25 1972-01-18 Electroless plating
GB308872A GB1382101A (en) 1971-01-25 1972-01-21 Electroless plating
JP769972A JPS5624032B1 (en)) 1971-01-25 1972-01-21
CH93572A CH585277A5 (en)) 1971-01-25 1972-01-21
AU38157/72A AU469973B2 (en) 1971-01-25 1972-01-21 Method and apparatus for concomitant particulate deposition in electroless plating, andthe product thereof
FR7202225A FR2123369B1 (en)) 1971-01-25 1972-01-24
BE778401A BE778401A (fr) 1971-01-25 1972-01-24 Procede et appareil pour le depot concomitant d'une matiere en particules dans une operation de metallisation non electrolytique et produits obtenus par ce procede
DE19722203230 DE2203230C3 (de) 1971-01-25 1972-01-24 Verfahren und Vorrichtung zur Herstellung von metallbeschichteten Trägern durch stromloses Metallisieren
NL7201005A NL7201005A (en)) 1971-01-25 1972-01-25
US05/469,499 US3940512A (en) 1971-01-25 1974-05-13 Method and apparatus for concomitant particulate deposition in electroless plating, and the product thereof

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US00103355A US3853094A (en) 1971-01-25 1971-01-25 Electroless plating apparatus

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US05/469,499 Division US3940512A (en) 1971-01-25 1974-05-13 Method and apparatus for concomitant particulate deposition in electroless plating, and the product thereof

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BE (1) BE778401A (en))
CA (1) CA962537A (en))
CH (1) CH585277A5 (en))
FR (1) FR2123369B1 (en))
GB (1) GB1382101A (en))
IE (1) IE35988B1 (en))
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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4063564A (en) * 1976-08-30 1977-12-20 Francis Theodore R Vibratory cleaning and coating system
US4150180A (en) * 1975-12-08 1979-04-17 Potapov Fedor P Method for chemical nickel-plating of parts having a catalytic surface employing a vessel having an upper heated zone and a lower cooled zone
US4262044A (en) * 1980-05-16 1981-04-14 Kuczma Jr John J Method for the electroless nickel plating of long bodies
US4328266A (en) * 1977-06-06 1982-05-04 Surface Technology, Inc. Method for rendering non-platable substrates platable
US5114751A (en) * 1989-10-24 1992-05-19 Henkel Corporation Application of an organic coating to small metal articles
US5415890A (en) * 1994-01-03 1995-05-16 Eaton Corporation Modular apparatus and method for surface treatment of parts with liquid baths
US5753096A (en) * 1993-10-08 1998-05-19 Tumbleveyor, Inc. Method for the surface treatment of parts
US6193858B1 (en) * 1997-12-22 2001-02-27 George Hradil Spouted bed apparatus for contacting objects with a fluid
US6309583B1 (en) * 1999-08-02 2001-10-30 Surface Technology, Inc. Composite coatings for thermal properties
US20020195333A1 (en) * 1997-12-22 2002-12-26 George Hradil Spouted bed apparatus for contacting objects with a fluid
US20030141018A1 (en) * 2002-01-28 2003-07-31 Applied Materials, Inc. Electroless deposition apparatus
US20050217989A1 (en) * 1997-12-22 2005-10-06 George Hradil Spouted bed apparatus with annular region for electroplating small objects
US20130143031A1 (en) * 2009-11-30 2013-06-06 Francesco Sorbo Electroless ni-composite plated substrate and method

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2443238C3 (de) * 1974-09-10 1987-07-09 FAG Kugelfischer Georg Schäfer KGaA, 8720 Schweinfurt Reibrotor zum Friktionsfalschdrallen von synthetischen Fäden
JPS57200057U (en)) * 1981-06-15 1982-12-20
JPS5874363U (ja) * 1981-11-13 1983-05-19 リコーエレメックス株式会社 回路基板の実装構造
GB2246145A (en) * 1990-07-18 1992-01-22 Nippon Piston Ring Co Ltd Nickel-born alloy composite slidable surface

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2165364A (en) * 1938-01-19 1939-07-11 Fernplas Corp Method of and apparatus for coating articles by dipping
US2908249A (en) * 1957-05-14 1959-10-13 Westinghouse Electric Corp Apparatus for uniformly coating photoflash lamps
US3025828A (en) * 1960-05-05 1962-03-20 Du Pont Coating apparatus
US3336906A (en) * 1965-06-09 1967-08-22 Fairchild Camera Instr Co Apparatus for immersion development

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1621206B2 (de) * 1967-01-18 1971-12-16 Friedr. Blasberg Gmbh & Co, Kg, 5650 Solingen Verfahren zur beschichtung gleitend reibend auf verschleiss beanspruchter werkstuecke
JPS4829695A (en)) * 1971-08-23 1973-04-19

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2165364A (en) * 1938-01-19 1939-07-11 Fernplas Corp Method of and apparatus for coating articles by dipping
US2908249A (en) * 1957-05-14 1959-10-13 Westinghouse Electric Corp Apparatus for uniformly coating photoflash lamps
US3025828A (en) * 1960-05-05 1962-03-20 Du Pont Coating apparatus
US3336906A (en) * 1965-06-09 1967-08-22 Fairchild Camera Instr Co Apparatus for immersion development

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4150180A (en) * 1975-12-08 1979-04-17 Potapov Fedor P Method for chemical nickel-plating of parts having a catalytic surface employing a vessel having an upper heated zone and a lower cooled zone
US4063564A (en) * 1976-08-30 1977-12-20 Francis Theodore R Vibratory cleaning and coating system
US4328266A (en) * 1977-06-06 1982-05-04 Surface Technology, Inc. Method for rendering non-platable substrates platable
US4262044A (en) * 1980-05-16 1981-04-14 Kuczma Jr John J Method for the electroless nickel plating of long bodies
US5114751A (en) * 1989-10-24 1992-05-19 Henkel Corporation Application of an organic coating to small metal articles
US5753096A (en) * 1993-10-08 1998-05-19 Tumbleveyor, Inc. Method for the surface treatment of parts
US5415890A (en) * 1994-01-03 1995-05-16 Eaton Corporation Modular apparatus and method for surface treatment of parts with liquid baths
US6193858B1 (en) * 1997-12-22 2001-02-27 George Hradil Spouted bed apparatus for contacting objects with a fluid
US20020195333A1 (en) * 1997-12-22 2002-12-26 George Hradil Spouted bed apparatus for contacting objects with a fluid
US6936142B2 (en) 1997-12-22 2005-08-30 George Hradil Spouted bed apparatus for contacting objects with a fluid
US20050217989A1 (en) * 1997-12-22 2005-10-06 George Hradil Spouted bed apparatus with annular region for electroplating small objects
US6309583B1 (en) * 1999-08-02 2001-10-30 Surface Technology, Inc. Composite coatings for thermal properties
US20030141018A1 (en) * 2002-01-28 2003-07-31 Applied Materials, Inc. Electroless deposition apparatus
US7138014B2 (en) * 2002-01-28 2006-11-21 Applied Materials, Inc. Electroless deposition apparatus
US20130143031A1 (en) * 2009-11-30 2013-06-06 Francesco Sorbo Electroless ni-composite plated substrate and method

Also Published As

Publication number Publication date
DE2203230A1 (de) 1972-08-03
JPS5624032B1 (en)) 1981-06-03
BE778401A (fr) 1972-07-24
IE35988L (en) 1972-07-25
NL7201005A (en)) 1972-07-27
FR2123369B1 (en)) 1977-04-01
CA962537A (en) 1975-02-11
GB1382101A (en) 1975-01-29
DE2203230B2 (de) 1976-04-15
AU3815772A (en) 1973-07-26
CH585277A5 (en)) 1977-02-28
IE35988B1 (en) 1976-07-21
IT946624B (it) 1973-05-21
FR2123369A1 (en)) 1972-09-08
AU469973B2 (en) 1976-02-26

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