Classifications

• • C—CHEMISTRY; METALLURGY
  • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
  • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
  • C23C24/00—Coating starting from inorganic powder
  • C23C24/02—Coating starting from inorganic powder by application of pressure only
  • C23C24/04—Impact or kinetic deposition of particles
• • 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
  • C23C18/1689—After-treatment
• • 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
  • C23C18/54—Contact plating, i.e. electroless electrochemical 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
  • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
  • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
  • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
  • C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors

Definitions

• the plating metal may be applied by either electroplating or mechanical plating, depending on such factors as the thickness required and the end use to which the part will be put. Electroplating requires a heavy capital investment, while mechanical plating employs comparatively simple and inexpensive equipment. Since the rate of electroplating is constant for given conditions, cost is directly proportional to the thickness of the plating. In contrast, mechanical plating requires only slightly more time to apply a thick plate than a thin one, and hence cost increases very little with increasing thickness. Where 0.3 to 3 mils of zinc is to be plated on a ferrous metal part, mechanical plating is generally less expensive than electroplating.
• Parts to be either electroplated or mechanically plated are usually first cleaned in strong acids, commonly having a dissociation constant of at least When highcarbon steel is exposed to strong acids, it almost inevitably absorbs hydrogen, becoming embrittled and prone to fail when subjected to tensile stress.
• the plating process itself is also frequently carried on in acidic solution; in electroplating, hydrogen is generated atand absorbed bythe part being plated, causing further hydrogen embrittlement.
• Mechanically applied platings are somewhat porous, permitting absorbed hydrogen to escape quickly and alleviate the stress, while electroplated platings especially if as thick at l mil-are dense, confining the hydrogen within the ferrous metal lattice. This difference provides a further reason why manufacturers of parts which require a comparatively thick plate find mechanical plating more satisfactory than electroplating, especially where the plated part is to be stressed in use.
• the present invention provides a simple, straight-forward, rapid, and inexpensive way to provide metal parts with mechanical platings of any desired thickness. Even 0.1-0.3 mil layers can be applied more simply than, and as economically as, by electroplating.
• the invention involves the surprising and unexpected discovery that mechanical plating can be carried out in the strongly acidic residue remaining after the degreasing and descaling step. This discovery is particularly surprising in view of the fact that an attempt to electroplate in this residue results in a totally unsatisfactory plating.
• parts to be cleaned and mechanically plated are placed in a barrel and flooded with an aqueous solution containing surfactant and sufficient acid to lower the pH to 4 or less.
• the barrel is then rotated, tumbling the parts and media and agitating the solution, until the parts are essentially cleaned and free from oil and scale.
• plating metal particles are added to the solution, desirably providing in the solution means for dispersing the particles and inhibiting their corrosion by the residual acid.
• the barrel contents are then further agitated until the desired thickness of mechanical plating metal has been applied over the surface of the parts, after which the plated parts are separated from the other contents of the barrel.
• Adhesion of the mechanical plating to the substrate, especially to a ferrous metal substrate, is generally enhanced by applying one or more thin flash plates of a nonferrous metal by displacement and/or galvanomechanical techniques.
• a nonferrous metal by displacement and/or galvanomechanical techniques.
• there is added to the solution remaining after cleaning small amounts of soluble salt of a galvanomechanical plating metal and 3 finely divided particles of a driving metal which is more anodically active in the solution than is the galvanomechanical plating metal as the solution is agitated, the galvanomechanical plating metal is deposited on the substrate.
• the acid may be buffered so that its pH does not fall below about 2.5 during plating; alternatively, the acid may be added successively throughout the plating process to maintain the highest pH which is effective. Generally, however, it is preferred to employ an additive which inhibits corrosion of the plating metal particles without affecting acidity.
• cationic amine inhibitors such as Armohib (Armour Industrial Chemical Co.); cationic inhibitors such as Inhibitor GC (Sinclair Mineral and Chemical Co.); filming amines such as Nalco 353 (Nalco Chemical Company); triphenyl sulfonium chloride, and mixtures of propargyl alcohol and the reaction product of certain amine hydrochloride with ketones and formaldehyde, such as the Rodines (Amchem Products, Inc.).
• Armohib Armour Industrial Chemical Co.
• cationic inhibitors such as Inhibitor GC (Sinclair Mineral and Chemical Co.)
• filming amines such as Nalco 353 (Nalco Chemical Company)
• triphenyl sulfonium chloride and mixtures of propargyl alcohol and the reaction product of certain amine hydrochloride with ketones and formaldehyde, such as the Rodines (Amchem Products, Inc.).
• Additives which serve as effective corrosion inhibitors are related to both the acid and the specific plating metal.
• Armohib 25 prevents the corrosion of lead or cadmium particles, but not zinc particles.
• Nalco 358 inhibits the corrosion of cadmium but not lead.
• Sinclair Inhibitor GC does not inhibit the corrosion of cadmium in sulfuric acid, but does in hydrochloric acid.
• the optimum amount of a given additive is related to the specific system in which it is used. Generally, however, the more acidic or more aerated the liquid, the more inhibitor is required.
• the materials which function as effective means for dispersing at least some plating metal powders in at least some acids are those polyoxyethylene glycols having a cloud point in 1% aqueous solution below 100 C., such as Carbowax 20M (Union Carbide Chemicals Company) or Polyglycol E50,000 (Dow Chemical Company); quaternary aliphatic ammonium salts such as Arquad S-2C, (Armour Industrial Chemical Co.); proteinaceous materials such as Technical Protein Colloids No.
• salts of polymerized alkyl aryl sulfonic acids or higher alkyl adducts of diphenyl oxide such as the Marasperses (Marathon Chemical Company), Orzans (Crown-Zellerbach Compony), Darvans (R. T.
• Additives which function as dispersants are related to both the specific acid and the specific plating metal particles involved.
• effective dispersants for Zinc in sulfuric acid include Carbowax 20M and Orzan AH3; dispersants for zinc or tin particles in hydrochloric acid include Nalquat G811, while lead can be dispersed in the same acid by Orzan P.
• dispersants for Zinc in sulfuric acid include Carbowax 20M and Orzan AH3
• dispersants for zinc or tin particles in hydrochloric acid include Nalquat G811, while lead can be dispersed in the same acid by Orzan P.
• Many other examples could be cited.
• Whether a given material will function as means for either dispersing or inhibiting the corrosion of specific plating metal particles in a specific milieu can be determined by adding 0.25-0.5 gram of the material to 250 ml. of the acid plating solution in a 400 ml. beaker, adding 10 grams of plating metal powder, stirring vigorously, and allowing the beaker and its contents to stand for 5 minutes. An effective dispersant will keep the metal powder in suspension, rendering the acid plating solution opaque. An effective corrosion inhibitor will essentially prevent both gasing and clumping of the plating metal metal powder into tough balls.
• the optimum amount of a given additive is related to the specific system in which it is used. In general, however, large volumes of liquid, open barrels, or highly acidic conditions require more inhibitor than small volumes of liquid, closed barrels, or less acidic conditions. Similarly the optitum amount of dispersant decreases as pH rises or the weight of plating metal particles decr ases.
• Example 1 A 1.2-gallon hexagonal mill provided with a cover was charged with two quarts (3,835 grams) of 1% inch x /8 inch roofing nails, 3,110 grams of glass impact media (3 parts 4-6 mesh spherical, 1 part 8-14 mesh nonspherical, 1 part 12-14 mesh spherical, and 1 /2 parts 31100 mesh spherical), and sufficient F. water to cover the solid materials. To the barrel was then added 20 grams of NaHSO 0.5 gram of the adduct of nonyl phenol and a 9-10 ethylene oxide polyoxyethylene glycol (Surfonic N-95, available from Jefferson Chemical Company), 3.0 grams SnCl and 6.0 grams of 3-micron Zinc powder.
• the barrel was closed and rotated at 54 rpm. for 5 minutes, after which period the nails were found to be not only free from oil and scale, but also provided with a tin flash coat.
• To the barrel was then added 57.5 grams of zinc powder and rotation continued for an additional 20 minutes.
• the pH having risen to about 5, 10 grams of NaHSO was added and rotation continued for an additional 5 minutes.
• the nails were separated from the remaining contents of the barrel and fouiid to have a uniform bright 0.3-0.4 mil zinc plating having excellent adhesion and uniformity.
• Surfonic N is a borderline dispersant for zinc particles in the system, the zinc plating was somewhat rough, which, was considered desirable for roofing nails.
• the plated nails could be chromated in standard fashion.
• Example 2 The mill of Example 1 was charged with 3,835 grams of roofing nails, and 5,099 grams of the impact media, and water as in Example 1. To the barrel was then added 41.54 grams of a cleaner-promoter having the following composition:
• the mill was then run for minutes, at the end of which time the roofing nails had been thoroughly cleaned and had acquired a bright tin plating.
• the barrel was opened, 58 grams of zinc powder added, the barrel reclosed, and rotation continued for an additional minutes.
• the nails were then rinsed, removed from the mill, and found to have a very good zinc plating. Presumably because "()rzan AH-3 is a good dispersant for zinc particles, the plating was somewhat smoother than that obtained in Example 1.
• Example 3 The mill of Example 1 was charged with roofing nails, impact media, and water, all as in Example 1.
• a solid granular cleaner and plating promoter was prepared by blending 35 grams NaHSO 1.7 grams SnSO (water-soluble flash plating salt), 0.7 gram Surfonic N95 (detergent), 0.1 gram of silicone defoamer absorbed on puffed borax (as in Example 2), and 0.75 gram Orzan AH-3 (dispersant).
• a protected driving and mechanical plating metal powder was prepared as follows: 18 grams of a watersoluble binding and coating polymermethylcellulose (Methocel HG, commercial available from Hercules Powder Co.)-was dissolved in 100 cc. of isopropanol, added to 200 cc. water, and stirred to yield a uniform solution. Next 36 grams of powdered zinc was added and stirred vigorously to disperse it throughout the solution. The zinc-containing solution was then poured into a large Petri dish and heated 4 hours at 200 F. to remove the solvent and decrease the water-solubility of the methylcellulose, thereby retarding the rate at which the zinc powder could be subsequently made available. The resultant film was broken into small flakes and shreads and blended with the granular plating promoter described in the preceding paragraph to yield a generally uniform mixture of granular material for use in cleaning, galvanomechanically flash plating and mechanically plating.
• the granular mixture was then added to the mill,- which was then closed and rotated at 30 rpm. for 10 minutes; when opened, it was found that the nails had been uniformly tin plated. The mill was then closed and rotated for an additional 10 minutes, yielding a bright, uniform zinc plate which chromated well.
• Example 4 The mill of Example 1 was charged with 6,500 grams of moderately soiled /3inch mild steel washers and 4,000 grams of the impact media used in Example 1, sufficient water being added to cover the charge.
• Example 5 The mill of Example 1 was charged with 5,020 grams of heavily scaled, soiled -inch hot rolled steel washers (1105 square inches of surface), 4,000 grams of the impact media described in Example 1, and sufficient water to cover the charge. To the mill was then added 20 grams of concentrated H and 8 grams of a cleaner having 'the following composition:
• Additive R seems to combine the features of corrosion inhibition, hydrogen embrittlement prevention, and zinc dispersion in this system, making it an especially interesting additive.
• Example 6 The mill of Example 1 was charged with 6,500 grams of /S-ll'lCh mild steel washers, 4,000 grams of impact media of the type used in Example 1, and sufficient water to cover the solid material. Next 40 grams of an aqueous cleaner-plating promoter chemical (27% H 80 58% NH HSO and 10% ammonium acrylate) was added. The mill was closed and rotated for 15 minutes at F., opened, and 2 grams of SnCl and 3.6 grams of zinc added. The barrel was again closed and rotated for 5 minutes, providing the washers with a thin uniform tin plating. 32.5 grams of zinc was then added and rotation continued for an additional 20 minutes. The washers were found to have a uniform well-adhered 0.2-0.4 mil zinc plating.
• an aqueous cleaner-plating promoter chemical 27% H 80 58% NH HSO and 10% ammonium acrylate
• Example 7 A cleaning powder was prepared by absorbing on 70 grams of Zeo 455D, 148.5 grams of concentrated H 80 and 12 grams of the reaction product of a straight chain alcohol and ethylene oxide (Arosurf EO-66, commercially available from Archer Daniels Midland Co.), and then mixing with 6 grams of Orzan AH-3 and 91.5 grams of (NI-19 80 As used hereinafter, Additive R is a product made as follows: To 23.4 grams of dehydroabietyl amine (Amine D, available from Hercules Chemical Company) was slowly added 7.5 grams of acetophenone, with stirring; 10 grams of 20 B. HCl solution in water was added slowly in the same manner.
• Dehydroabietyl amine Amine D, available from Hercules Chemical Company
• Example 1 The mill of Example 1 was charged with washers, impact media, and water, as in Example 5. To the charge was then added 20 grams of the powdered cleaning material described in the opening paragraph of this example, and the mill closed and rotated at 60 rpm. for minutes at 120 F. The mill was opened, 2 grams of SnCI and 3.5 grams of zinc added, closed, and rotated an additional 5 minutes; the washers had been thoroughly cleaned and provided with a uniform tin flash plate. Next .23 grams of zinc powder was added, and the mill closed and rotated an additional minutes at 90 F., providing the washers with a uniform 0.15-0.2 mil Zinc plating.
• Example 8 The mill of Example 1 was charged with 2,500 grams of As-inch mild steel washers, 3,110 grams of glass impact media (75% 12-14 mesh spherical, 91-100 mesh spherical), sufiicient Water to cover the solid material, and 20 ml. of the following composition:
• the mill was closed and rotated for 10 minutes, steam being supplied to heat the charge.
• the mill was then opened, 2 grams of CL1SO4'H2O and 1 gram of NaCl added, closed, and rotated an additional 5 minutes, providing the washers with copper flash-plated by displace ment.
• 1.2.5 grams of zinc powder and 5 grams phthalic anhydride were added, the mill again closed, and steam used to raise the temperature to 160-180 F.. while rotating for about 10 minutes.
• the washers were plated very effectively, although there was some tendency to roughness. Phthalic anhydride becomes acidic only when the temperature is raised sufficiently above room temperature to cause hydrolysis.
• Example 9 The mill of Example 1 was charged with 3,835 grams of roofing nails, 2,100 grams of glass impact media (3 parts 12-14 mesh spherical, 1 part 20-45 mesh spherical, and 1 part 31-100 mesh spherical), and sufficient water to cover the solid material.
• the diatomaceous earth serving to prevent the Zinc from reacting with the NaHSO A 1.3-gram B pellet was formed by mixing and pressing together at 5,000 p.s.i. parts stannous chloride, 10 parts 58-202, 15 parts Celite Super Floss, and 1.5 parts sifted pine sawdust.
• the two promoter pellets were added to the mill, which was then closed, rotated at 60 rpm. for 5 minutes, opened, and 57.5 grams of Zinc powder added. The mill was again closed and rotated for 20 minutes; no foam developed, and the mill was not subjected to increased pressure. The nails were uniformly plated with zinc, showing good brightness and receptivity to chromating.
• Example 10 The mill of Example 1 was charged with 3,835 grams of roofing nails, 3,000 grams of glass impact media (3 parts 4-6 mesh spherical, 1 part 8-14 mesh nonspherical, 1 part 12-14 mesh spherical, 1 part 20 mesh spherical), and sufiicient water to cover the solid materials.
• a cleaner-promoter chemical pellet was formed by pressing at 5,000 p.s.i. the following materials:
• Citric acid 11.2 Diammonium citrate (buffer) 3.7 Stearic acid 0.3 Polyoxyethylene glycol (Carbowax 20M) 0.3 Stannous sulfate 1.5 Surfonic N-95 0.5 Sifted pine sawdust 0.4 Powdered zinc 2.0
• the mill was closed and rotated for 5 minutes at r.p.m., uniformly tinning the nails without developing any foam or pressure.
• 57.5 grams of zinc was added, the barrel closed, and rotation continued for 20 minutes at 60 r.p.m. and F.
• the nails were then removed, rinsed and examined, revealing a 0.35-mil zinc coating with good adhesion and brightness.
• the diammonium citrate maintained the pH high enough that acid did not significantly attack the zinc plating metal particles.
• Example 11 The mill of Example 1 was charged with 1,700 grams of golf cleats, 2,000 grams of glass impact media (4 parts 4-6 mesh spherical, 2 parts 14-20 mesh nonspherical, 1 part -100 mesh spherical), and sulficient water to cover the solid materials. To the barrel were then added a watersoluble bag containing 19 grams of chemicals and a 7.2- gram pressed bar. Formulations of these two additives were as follows:
• the contents were preheated with steam to 125 -l30 F., after which the mill was closed and rotated at 60 rpm. for 5 minutes, cleaning and tin flash coating the cleats.
• 17 grams of zinc powder was added, and the mill closed and rotated for 20 minutes maintaining a temperature of approximately F.; the cleats were found to have a good coating of zinc.
• Example 12 The mill of Example 1 was charged with 450 grams of fiat nominally Az-inch copper washers (0.693-inch O.D.), 1,000 grams of glass impact media (3 parts 4-6 mesh spherical, 1 part 8-14 mesh nonspherical, 1 part 12-14 mesh spherical, and 1 part 30-100 mesh spherical), and sufiicient water to cover the solid materials.
• a cleanerpromoter consisting of 5 grams citric acid, 5 grams diammonium citrate, 0.2 gram Carbowax 20M, and 0.1 gram Surfonic N-95, was then added, and the mill closed and rotated at 45 rpm. for 10 minutes to clean Example 13 To a 4.75-ft.
• octagonal horizontal barrel adapted to be closed at both ends, was added 300 lbs. of /s-inch flat mild steel washers, 270 lbs. of glass impact media (3 parts 12-l4 mesh spherical, 1 part 20-45 mesh spherical, 1 part 31100 mesh spherical), and sufficient water to cover the charge.
• glass impact media 3 parts 12-l4 mesh spherical, 1 part 20-45 mesh spherical, 1 part 31100 mesh spherical
• the barrel was closed and rotated 5 minutes to tin the washers, opened, and 1 /2 lbs. Zinc powder added.
• the barrel was again closed and rotated for 30 minutes at 20 r.p.m., providing the washers with a bright, well-adhered 0.150.25 mil zinc plating.
• the NaHCO in the promoter chemical bar reacted with the acid, thereby hastening disintegration of the bar.
• Example 14 Zinc powder and rotation continued for an additional 20 1 minutes. When removed from the barrel and rinsed, the nails were found to have a zinc plating which was extremely well-adhered, uniformly covered and 0.3 mil thick.
• Example 15 To a tulip barrel of the type described in Example 14 was added 1 quart of lock washers (1,107 grams), 1 /2 quarts of spherical glass impact media (8 parts 12-14 mesh, 2 parts 45 mesh, and 1 part 91-100 mesh), sufficient water to cover the charge, and 20 grams of cleaner having the following composition:
• the barrel was rotated for an additional 5 minutes, after which time the lock washers were found to have been uniformly tinned.
• To the barrel was then added 38.7 grams of zinc powder and rotation continued for 30 minutes at 52 r.p.m. An extremely adherent 0.3-mil zinc plating was found to have been applied, of the available zinc powder having been utilized.
• Example 16 To a tulip barrel of the type described in Example 14 was added 1,276 grams of spring wire hose clamps (SAE 1065 steel) having a total surface area of 320 square inches, 10 lbs. of spherical glass impact media (4 parts 4-6 mesh, 1 part 12-14 mesh, 1 part 2045 mesh, 1 part -100 mesh) and one liter of water. To the barrel was then added 12 cc. of one composition containing 24.95% water, 74.71% 52 B. H 80 and 0.34% Additive R (commercial equivalent), and 12 cc. of another composition containing 48.6% water, 27.1% 52 B. H SO 10.0% CuSO -5H O, and 14.3% NaCl. The barrel was rotated at 60 r.p.m.
• Example 17 T o the barrel of Example 14 was added the same load of hose clamps, impact media, and cleaners as in Example 16 for cleaning carried out in the same manner. Next a promoter containing 0.7 gram CdO and 0.136 gram Additive A was added and allowed to dissolve for 5 minutes, and 2 grams of powdered zinc then added. The barrel was again rotated, and a cadmium flat plate obtained after 5 minutes. 8.8 grams of cadmium powder was added and rotation continued for 20 minutes, yielding an excellent cadmium plate.
• Example 18 A load of hose clamps was cleaned as in Example 16. Next 0.110 gram of Additive R (commercial equivalent), 0.364 gram Additive A (as in Example 16) and 0.45 gram SnCl were added, together with 1.2 grams zinc powder. A uniform tin flash plate was obtained in 5 minutes, after which 11 grams of tin powder was added. Rotation was continued for 20 minutes, yielding a welladhered mechanically applied tin plate; the plating was somewhat rough, indicating the desirability of slightly more dispersant.
• Additive R commercial equivalent
• Additive A as in Example 16
• SnCl 0.45 gram SnCl
• Additive A is the reaction product of 102 parts water, 63 parts Carbowax 20M, S) parts HCL 13 parts o-toluidine, and 13 parts 36% aqueous solutlon of HCHO.
• Example 19 A barrel of the type employed in Example 14 was loaded with hose clamps, impact media, and water as in Example 16. To the barrel was then added a cleaning composition consisting of 8.25 grams 66 B. H 80 0.055 gram Addi tive R, 1.58 grams CuSO -5H O, 2.27 grams NaCl, and 7.7 grams of water. The barrel was then rotated at 60 r.p.m. for 15 minutes to clean the parts, after which promoter chemical consisting of 0.114 gram Additive R, 0.0364 gram Additive A, and 0.45 gram SnCl was added, and the barrel rotated for 5 minutes to effect solution. Next 0.9 gram of powdered zinc was added and the barrel rotated for 5 minutes to provide the hose clamps with a tin flash plate. An additional 11 grams of zinc was then added, and rotation continued for 20 minutes, yielding a uniform zinc plating.
• a cleaning composition consisting of 8.25 grams 66 B. H 80 0.055 gram Addi tive R, 1.58 grams Cu
• Example 20 To a tulip barrel of the type described in Example 14 were added 400 grams of hose clamps, 1,558 grams of glass impact media (3 parts 46 mesh spherical, 1 part 814 mesh spherical, 1 part 12-14 mesh spherical, 1 /2 parts 90-100 mesh spherical), and suflicient water to impart fluidity. The barrel was set in rotation and the following cleaning composition added:
• Example 21 The plating barrel of Example 14 was charged with hose clamps, impact media, and water as in Example 18 and the following cleaner added:
• Additive R (commercial equivalent)0.05 gram Additive A"0.05 gram PbCl 0.5 gram
• the barrel was rotated at 52 r.p.m. for 10 minutes to clean the parts and 1.0 gram of zinc dust then added; after 5 minutes further rotation, it was found that a lead flash plate had been galvanically deposited.
• 3 grams of zinc dust and 0.1 gram of Additive A were added and rotation continued for 20 minutes; a 0.2-mil zinc plating was obtained.
• Example 22 The plating barrel of Example 14 was charged With hose clamps, impact media, and water, and the following cleaner added:
• Additive R (commercial equivalent)--0.05 gram Additive A0.05 gram HgSO 0.S gram Surfonic N-100-0.05 gram
• Additive R (commercial equivalent)--0.05 gram Additive A0.05 gram HgSO 0.S gram Surfonic N-100-0.05 gram
• the barrel was rotated at 52 r.p.m. for 5 minutes to clean the parts and 1 gram of zinc dust then added; after 5 minutes further rotation it was found that a bright mercury coating had been galvanically deposited.
• 3 grams of zinc dust and 0.1 gram Additive A were added to the barrel and rotation continued for min- 12 utes. It was noted that the pH had risen to 5.5, while a fairly bright coating of zinc had been mechanically applied.
• Example 23 To a large open, tapered barrel was added 100 lbs. of 8d nails, and 275 lbs. of glass impact media of the type used in Example 1. Suflicient Water was added to cover the nails, after which cleaner having the following composition was added:
• the barrel was rotated for 15 minutes at 66 F., cleaning and flash-coppering the nails.
• To the barrel was then added 500 grams of zinc powder and rotation continued for 10 minutes, after which an additional 500 grams of zinc powder and 500 grams of NaHSO was added. Rotation was continued for an additional minutes, after which the nails were found to have been provided with a bright uniform zinc plating.
• Example 24 This example was carried out in an open-ended cylindrical barrel having an effective axial length of 18 inches, an outer diameter of 36 inches, a 7-inch diameter opening at one end, and a 16-inch diameter opening at the other end.
• To the barrel which was provided with internal lifter bars, was then added 100 lbs. of 8d nails, 275 lbs. of impact media as in Example 23, 706 grams NaHSO 20 grams SnSO 23.6 grams Zinc powder, and enough water to leave a small puddle as the barrel was rotated. The barrel was then rotated for 2 minutes to clean and tin-plate the nails, after which 1.5 grams of Additive R (commercial equivalent) was added and rotation continued for an additional minute.
• Additive R commercial equivalent
• Example This example was carried out in an open-end barrel similar to that of Example 24, except that the effective inner axial length was 24 inches and the outer diameter 48 inches.
• To the barrel was added 191 lbs. of spring washers, having a total area of approximately 572 square feet, 220 lbs. of glass impact media (4 parts 46 mesh spherical, and 1 part 8-14 mesh nonspherical, 2 parts 12-14 mesh spherical, and 1 part 100 mesh spherical), and 2,900 ml. of each of the following cleaner components:
• Additive R (commercial equivalent) 5.0 Additive A 2.0 Pine sawdust 26.0 SnCl 21.0 Stearic acid 1.0
• Example 26 To an open-ended barrel of the type described in the preceding example was added 3 cubic feet (210 lbs.) of Palnut lock washers, and 3 cubic feet of glass impact media (8 parts 12-14 mesh spherical, 2 parts 20-45 mesh spherical, 1 part 31-100 mesh spherical), and 1,368 grams of a cleaner having the following composition:
• the barrel was then rotated for minutes to tin the lock washers, after which 5,900 grams of zinc was added and the barrel rotated an additional 30 minutes at 16 r.p.m.
• the plating was found to be firmly adhered and to have an average thickness of 0.57 mil:7%.
• Example 27 This example was carried out in an open-end barrel similar to that of Example 24 except that the effective inner axial length was 48 inches.
• To the barrel was added 325 lbs. of mild steel washer-type lock nuts having a surface area of 1,040 square feet, 840 lbs. of glass impact media (4 parts 4-6 mesh spherical, 1 part 12-14 mesh spherical, 1 part 8-14 mesh nonspherical, 1 part -100 mesh spherical), and about 15 gallons of water.
• the barrel was rotated at 24 r.p.m. while adding 5 /2 quarts each of Part A and Part B, as described in Example 25. After 15 minutes the parts were found to be clean and provided with a copper flash plate. Eleven 91-gram bars having the following composition were added:
• a method of providing a metal substrate with a firmly adherent uniform plating of a mechanical plating metal comprising the steps of:
• a method of providing a metal substrate with a firmly adherent uniform plating of a mechanical plating metal comprising the steps of:
• a method of providing small metal parts with a firmly adherent uniform coating of a mechanical plating metal comprising the steps of:
• a no-rinse method of providing small ferrous metal parts with a firmly adherent uniform plating of a dif- 0 ferent metal comprising the steps of (l) placing said parts in a rotary treating barrel together with components comprising (a) water (b) impact media (c) surfactant (d) sufiicient acid having a dissociation constant of at least 10 to lower the pH to not more than 4,

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• Organic Chemistry (AREA)
• General Chemical & Material Sciences (AREA)
• Electrochemistry (AREA)
• Chemically Coating (AREA)
• Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
• Detergent Compositions (AREA)

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Cited By (18)

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Citations (4)

• 1967
  • 1967-07-17 US US653657A patent/US3531315A/en not_active Expired - Lifetime
• 1968
  • 1968-07-05 SE SE6809287A patent/SE409882B/xx unknown
  • 1968-07-16 BE BE718128D patent/BE718128A/xx not_active IP Right Cessation
  • 1968-07-16 FR FR1585113D patent/FR1585113A/fr not_active Expired
  • 1968-07-16 CH CH1061368A patent/CH505911A/de not_active IP Right Cessation
  • 1968-07-16 GB GB1230491D patent/GB1230491A/en not_active Expired

Patent Citations (5)

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