Abstract: Relative concentrations of active suppressor additive species and suppressor breakdown contaminants in an acid copper electroplating bath are determined by cyclic voltammetric stripping (CVS) dilution titration analysis using two negative electrode potential limits. The analysis results for the more negative potential limit provide a measure of the suppressor additive concentration alone since the suppressor breakdowvn contaminants are not effective at suppressing the copper deposition rate at the more negative potentials. The analysis results for the less negative potential limit provide a measure of the combined concentrations of the suppressor additive and the suppressor breakdown contaminants. Comparison of the results for the two analyses yields a measure of the concentration of the suppressor breakdown contaminants relative to the suppressor additive concentration.

Abstract: In the present invention, the test reference electrode used for voltammetric analysis of a plating bath is calibrated relative to the zero-current point between metal plating and stripping at a rotating platinum disk electrode in the plating bath supporting electrolyte. This calibration is readily performed during the normal course of cyclic voltammetric stripping (CVS) or cyclic pulse voltammetric stripping (CPVS) plating bath analysis the need for additional instrumentation or removal of the test reference electrode from the analysis equipment. Automatic calibration of the reference electrode enabled by the present invention, saves labor, time and expense, and minimizes errors in the plating bath analysis.

Abstract: Relative concentrations of active suppressor additive species and suppressor breakdown contaminants in an acid copper electroplating bath are determined by cyclic voltammetric stripping (CVS) dilution titration analysis using two negative electrode potential limits. The analysis results for the more negative potential limit provide a measure of the suppressor additive concentration alone since the suppressor breakdown contaminants are not effective at suppressing the copper deposition rate at the more negative potentials. The analysis results for the less negative potential limit provide a measure of the combined concentrations of the suppressor additive and the suppressor breakdown contaminants. Comparison of the results for the two analyses yields a measure of the concentration of the suppressor breakdown contaminants relative to the suppressor additive concentration.

Abstract: The concentration of a reducing agent in an electroless bath for plating a first metal is determined from the effect of the reducing agent on the electrodeposition rate of a second metal. For electroless cobalt and nickel baths, a sample of the electroless plating bath is added to an acid copper plating solution and the copper electrodeposition rate is measured by cyclic voltammetric stripping (CVS) analysis. Separate analyses for hypophosphite and dimethylamineborane in baths employing both reducing agents are attained via selective decomposition of the dimethylamineborane in acidic solution.

Abstract: In the present invention, the test reference electrode used for voltammetric analysis of a plating bath is calibrated relative to the zero-current point between metal plating and stripping at a rotating platinum disk electrode in the plating bath supporting electrolyte. This calibration is readily performed during the normal course of cyclic voltammetric stripping (CVS) or cyclic pulse voltammetric stripping (CPVS) plating bath analysis the need for additional instrumentation or removal of the test reference electrode from the analysis equipment. Automatic calibration of the reference electrode enabled by the present invention, saves labor, time and expense, and minimizes errors in the plating bath analysis.

Abstract: Acid copper electroplating baths used to form ultra-fine circuitry features on semiconductor chips contain suppressor, anti-suppressor and leveler additives that must be closely controlled in order to obtain acceptable copper deposits. Cyclic voltammetric stripping (CVS) methods are available to measure the concentrations of the suppressor and anti-suppressor based on the effects of these additives on the copper electrodeposition rate. The present invention is a method that also uses measurements of the copper electrodeposition rate to determine the concentration of the leveler additive. The other two additives are included in the measurement solution at concentrations determined to provide the optimum compromise between minimal interference, high sensitivity and good reproducibility for the leveler analysis.

Abstract: Acid copper electroplating baths used to form ultra-fine circuitry features on semiconductor chips contain suppressor, anti-suppressor and leveler additives that must be closely controlled in order to obtain acceptable copper deposits. Cyclic voltammetric stripping (CVS) methods are available to measure the concentrations of the suppressor and anti-suppressor based on the effects of these additives on the copper electrodepositionrate. The present invention is a method that also uses measurements of the copper electrodepositionrate to determine the concentration of the leveler additive. The other two additives are included in the measurement solution at concentrations determined to provide the optimum compromise between minimal interference, high sensitivity and good reproducibility for the leveler analysis.