Bath nickel sulfamate

Soluble anode materials are not always a pure metal. In acid, low chloride nickel solutions, pure nickel does not corrode well, and small amounts of specific impurities are added to make the nickel more active, allowing more efficient dissolution. For example, since the early 1960s, nickel anode material containing a small amount of nickel sulfide [16812-54-7] NiS, has been commercially available and important in nickel sulfamate [13770-85-3] Ni(H2N02S)2, plating baths. These anodes corrode at a lower potential then pure nickel or other nickel anode materials (see Nickel and nickel alloys). 

Nickel. Nickel plating continues to be very important. Many plating baths have been formulated, but most of the nickel plating is done in either Watts baths or sulfamate baths. Watts baths contain sulfate and chloride nickel salts along with boric acid, and were first proposed in 1916 (111). Nickel was first plated from sulfamate in 1938 (112) and patented in 1943 (108). The process was brought to market in 1950 (113). Typical bath compositions and conditions are shown in Table 14. 

Nickel sulfamate is more soluble than the sulfate salt, and baths can be operated using higher nickel concentrations and higher currents. Sulfamate baths have been found to have superior microthrowing power, the abiUty to deposit in small cracks or crevices. Using one nickel salt, only a hydrometer and pH paper are needed to control the bath. A small amount of chloride salt was added as a proprietary. Highly purified nickel sulfamate concentrates are commercially available that can be used to make up new plating baths without further purification. 

Palladium and Palladium Alloys. Palladium is used in telephone equipment and in electronics appHcations as a substitute for gold in specific areas. Palladium is plated from ammoniacal and acid baths available along with chelated variations as proprietary processes. One typical alkaline bath uses 8 g/L diammine-dinitropalladium, 100 g/L ammonium nitrate, and 10 g/L sodium nitrite. The pH is adjusted to 9—10 using ammonium hydroxide, and the bath is operated at 100 A/m at 50° C. If ammonium sulfamate, 100 g/L, is used in some baths to replace the nitrate and sodium nitrite salts, the bath is mn at lower temperature, 25—35°C, and a pH of 7.5—8.5. A palladium—nickel alloy, 75% Pd, is plated from a bath having 6 g/L palladium from the same salt, 3 g/L nickel from nickel sulfamate concentrate, and 90 g/L ammonium hydroxide. The bath is operated at 20—40°C with 50-100 A/m/... 

Plating solutions used in nickel electroforming are primarily the Watts bath and the nickel sulfamate bath. Watts baths exhibit higher stress and require additives for stress control, which may affect other properties. Sulfamate baths produce much lower stress and are preferred where purer nickel or nickel—cobalt deposits ate needed. ASTM specifications are available that describe the mandrels and plating solutions (116,162). 

The composition of the codeposition bath is defined not only by the concentration and type of electrolyte used for depositing the matrix metal, but also by the particle loading in suspension, the pH, the temperature, and the additives used. A variety of electrolytes have been used for the electrocodeposition process including simple metal sulfate or acidic metal sulfate baths to form a metal matrix of copper, iron, nickel, cobalt, or chromium, or their alloys. Deposition of a nickel matrix has also been conducted using a Watts bath which consists of nickel sulfate, nickel chloride and boric acid, and electrolyte baths based on nickel fluoborate or nickel sulfamate. Although many of the bath chemistries used provide high current efficiency, the effect of hydrogen evolution on electrocodeposition is not discussed in the literature. 

Fine nickel powder reacts with sulfamic acid in hot aqueous solution under controlled conditions, forming nickel sulfamate tetrahydrate, Ni(S03NH2)2 4H20, used in electroplating baths. 

Nickel Sulfamate. Vltramon, a Thomas and Betts subsidiary, installed a 1 gpm ARO system to recover rinses and recycle nickel bath used to plate electronic capacitors. Previously, Vitramon had used an ion exchange system to remove the nickel. Ion exchange regenerant was shipped to a reclaimer. Water was reused. Ion exchange cost of operation was 4,000 per month. The ARO system maintains the rinse at less than 40 ppm nickel. Savings from nickel recovery and avoided treatment cost will provide a payback of approximately 10 months. 

Plating bath composition Fluorinated pitch 50 g/1 Nickel sulfamate 360 g/1 Nickel chloride 45 g/1 Boric acid 30 g/1... 

Lustrous adhesive nickel layers can be obtained from baths containing nickel sulfamate, nickel chloride, boric acid, or dimethylformamide (DMF). At 60 °C, current densities of 3 A/dm can be reached [152]. 

Fig. 8-32. Analysis of chloride, bromide, and sulfate in a nickel sulfamate bath. - Separator column 2 IonPac AS4A eluent 0.0017 mol/L NaHC03 + 0.0018 mol/L Na2C03 flow rate 1.5mL/min detection suppressed conductivity injection 50 pL sample (1 1000 diluted).

The main component in nickel sulfamate baths — sulfamate - can be determined in a single rim, in addition to the decomposition product sulfate and other bath constituents such as chloride and bromide (see Fig. 8-32). To achieve a sufficient separation between the sulfamate ions and chloride, both of which elute near the void volume, two identical anion exchangers were used in series, even though this increases the total analysis time to about 20 minutes. 

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