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UNITED STATES PATENT OFFICE 2,668,795 WHITE Brass PLATING Christian J

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UNITED STATES PATENT OFFICE 2,668,795 WHITE Brass PLATING Christian J Patented Feb. 9, 1954 2,668,795 UNITED STATES PATENT OFFICE 2,668,795 WHITE BRAss PLATING Christian J. Wernlund, Niagara Falls, N. Y., as signor to E. I. du Pont de Nemours and Con pany, Wilmington, Del, a corporation of Dela Wale No Drawing. Application July 28, 1951, Seria No. 239,190 12 Claims. (C. 204-44) 2 This invention relates to the electroplating of The foregoing objects may be attained in ac a White zinc copper alloy from an electrolyte cordance with the present invention by electro containing the cyanides of zinc and copper. plating a white zinc copper alloy from an aque Wernlund U. S. P. 2,181,773 describes the elec ous cyanide-containing electrolyte which con trodeposition of a “white brass' from a cyanide tains a Small amount of a Vanadium compound electrolyte. This white zinc copper alloy elec and preferably also a benzaldehyde-aliphatic trodeposit may be electroplated in accordance ether. Employing both of the above-mentioned With the Wernlund patent to produce a semi addition agents, white brass electrodeposits are bright or bright electrodeposit, which is useful obtained with excellent brightness Over a Wide as undercoating for chromium plating and which, O range of current densities without the addition Without a chromium overdeposit, forms an ex of hydrogen peroxide. For example, by the here cellent, corrosion resistant, decorative finish for in described process I have been able to electro articles made of steel, copper, yellow brass and deposit excellent bright white brass. Within the zinc. As undercoat for chromium plating, the current density range of from 5 to 90 amps. per White brass may be used in place of nickel. 5 Square foot. However, Some difficulty has arisen in produc The invention is illustrated by the following ing a satisfactory bright and smooth white brass examples: electrodeposit suitable, without buffing or polish Eacample 1 ing Operations, to Serve as an undercoat for the production of brilliant chrome plate, because of 20 The following ingredients were dissolved in the relatively narrow current density range with Water at a temperature of 80° C.: in which bright electrodeposits of the white brass Gans may be consistently obtained. This difficulty has per liter limited the utilization of the white brass electro Zinc cyanide ------------ we cais - we a sasar as wes’’a law- - 60 plating method, particularly for electroplating Copper cyanide ------------------------- 15 particles of irregular shape, which have inher 25 Sodium cyanide ------------------------- 52.5 ently areas of low and high current density. Sodium hydroxide ----------------------- 60 An object of the present invention is an in Sodium sulfide -------------------------- 0.5 proved White brass electroplating process. A fur ther object is to improve the process of the above The hot solution was filtered and portions of the mentioned Wernlund patent whereby Smooth, 30 filtered solution were utilized as electrolyte to bright, white brass electrodeposits may be ob electrodeposit white brass onto steel panels. The tained uniformly on irregularly shaped objectS steel specimens were plated from this electrolyte and over a wide range of current density. Still in a conventional Hull cell made of hard rubber. Other objects will be apparent from the following under the following conditions: description of the invention. 35 The Copending application of Robert R. Bair, Wolume of electrolyte -------------- cc 250 S. N. 231910, filed June 15, 1951, now abandoned, Cathode surface area. -----------Sq. in- 8 discloses the electrodeposition of white braSS Anode surface area -------------Sq. in.-- 5 from a cyanide Solution containing Small amounts Electrolyte temperature ------------ C 25-35 of a benzaldehyde-aliphatic ether and a Water 40 Average current density---amps./sq. ft.-- 36 soluble molybdenum compound, together with the Over-all cathode density addition of hydrogen peroxide. In the Bair proc Tailge. ------------------ amps./sq. ft. 4-90 ess, the addition of hydrogen peroxide is required Time of plating --------------minutes. ... 1. to produce a satisfactorily bright electrodeposit over a wide current density range. Without the 45 A separate portion of the plating solution was peroxide, bright electrodeposits are obtained employed to electroplate each steel specimen and Within a rather arrow range of current density. for pating certain Specimens Small amounts of A further object of the present invention is to piperonal bisulfite or Sodium ortho-wana.date obtain bright white brass electrodeposits over a (Na3WO4), or both, were added to the electro wide range of current density without the ne: 50 lyte, as indicated below. The following tabu cessity of adding a peroxide or equivalent oxidiz lation shows the current density range within, ing agent, which excellent bright electrodeposits (indicated 2,668,795 3 4. as "very bright') were obtained for each speci 0.1 gram per liter of Vanadium; and as the con en: centration of vanadium is decreased below that value, the brightening effect becomes correspond Addition Agts. ingly less. While some slight brightening effect (g.f.) Current occurs at concentrations even below 0.01 gram Trial Density Electrodeposit per liter of vanadium, generally Such Small Piperona, (amp's. Appearance amounts of Vanadium have little or no conner NagWO Bisulfite cial importance. The Wanadium concentration generally should not be increased to beyond about 4 to 8------ Gray. 10 0.5 gram per liter, as higher concentrations tend A-------- None None 8 to 20----- Semi bright. to cause exfoliation or blistering of the electro 3.5%.O 3i----- SifrighteInlbright. B-------- 0. A None E. SE ight deposit in the bright areas. Also as the vanadium C-------- None 3 (GSIE.09------ azy gray. oright, concentration is increased above around 0.1 gram 4 to 5------. Dull. per liter, the extent of the bright range tends to D-------- 0. 35 to 78.----| Very bright. 5 decrease. - 78 to.90---- Hazy bright. The aliphatic-aromatic ether aldehydes suit E 0.2 3 { to 5------ Dull. ... -- - - - - - - - - 5 to 90----- Very bright. able as addition agents are benzaldehyde-ali F 0.4 3 { to 5- Du. phatic ethers, that is, ethers having an aliphatic - - - - - - - - o E.I.Y.E.E.o 8- azy bright. group. joined through ether oxygen linkage to a G-------- 1.0 3 { to 90----- Very bright. 20 4 to 9------ Duli. benzene ring With an aldehyde group on the ring. H-------- 1, 6 39 to 47----- Bright. They may be represented by the generic formulas: 47 to 90---- Exfoliated. 4 to 12----- Grayish black. CEO , --------- 2 ---------- 2 to 40---- Dull gray. 40 to 90. Bright but blistered. 25 (O-R). Eacample 2 The process of Example was repeated in a and series of plating tests, employing the Vanadium CEO compounds and aldehyde ethers indicated in the 30 table below. To use vanadium pentoxide, it was dissolved in a caustic Soda solution and the Solu tion added to the electrolyte. Wanadium trioxide Yr (V2O3) (4.grams) was digested in 40 cc. of 10% caustic Soda, Solution at 100° C. and the resulting 35 o/ filtered solution added to the electrolyte. Walnadyl where R is an aliphatic hydrocarbon radical, and Sulfate (VOSO4) was dissolved in the electrolyte. n is a whole number of from 1 to 3. Preferably, The results obtained are tabulated below: R contains a single carbon atom and n is 1 or 2. Addition agents (g/l.) Current Density Electrodeposit Trial (amps.fsq. Appearance Vanadium Compound Aldehyde Ether ft.) 4 to 7------ Bright. A.------ None---------------------------------- Anisaldehyde Bisufte (3 g/l.)------ 26 B - - Egy bright. : . 090-...-- Uiray. 4 to 5------ Gray. B------ 0.20 g/l. WOs dissolved in NaOH---------- do------------------------------- 5 to 20.---- Hazy bright. 20 to 90.--- Very bright. C------ None---------------------------------- Vertraldehyde- Bisulfite (3g.fl.).----- 4 to 6------Go. ModeratelySbright. bright. 090---- Stray. D------ 0.20 g/l. V2O5 dissolved in NaOH----------- do------------------------------- (sia.. Visight. E.------ 0.08 gll. WOSO4----------------------- Piperonal Bisulfite (3 g/l.)----------- (38. E.E. 4 to 12.---- Hazy bright. F------ 0.32g.il. WOSO4------------------------ ----do - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - { to 90---- Very bright. G------ 4.0 g.fl. V2O3 digested in 40 ml. of 10% -----do------------------------------- ESI E. NaOH at 100° C. (filtered). In addition to the vanadium compounds dis Examples are: piperonal, vanillin, Veratralde closed in the foregoing examples, any of the hyde, anisaldehyde, 2,3-dimethoxybenzaldehyde inorganic vanadium compound Which can be dis and o-methoxybenzaldehyde. In order to obtain solved in the electrolyte to the extent stoichio suitable solubility in the electroplating bath, the metrically equivalent to approximately 0.01 gram 60 aldehyde is preferably added in the form of its bi per liter or more of elemental vanadium may be Sulfite compound. The amount of the aldehyde utilized in the practice of my invention. Wana addition agent may vary from 0.2 to 7.5 grams dium compounds soluble in alkaline solutions, in per liter of the bisulfite compound and generally cluding those, like vanadium trioxide, which re best results are obtained at a concentration of quire strong alkali concentration and heating to 65 from 0.4 to 4 grams per liter. effect Solution, are generally suitable. I gen The presence of other addition agents gen erally prefer to dissolve Vanadium pentoxide in erally suitable for electroplating white brass from a solution of sodium or potassium hydroxide and cyanide Solutions ordinarily is not deleterious in add the resulting solution to the electrolyte. As the practice of my invention. More specifically, illustrated by the examples, the concentration a Small amount of a water-soluble molybdenum of the vanadium compound may vary from the compound as described in the aforesaid Bair ap stoichiometrical equivalent of about 0.01 to 0.5 plication, With or Without the addition of a per gram per liter of elemental vanadium. The pre oxide or other oxidizing agent, may be added, if ferred concentration is in the neighborhood of 75 desired; and good results are thereby obtained.
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