Methods for determining organic component concentrations in an electrolytic solution
First Claim
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1. A method for determining concentration of an organic component in a sample electrolytic solution, said method comprising the steps of:
- (a) applying a potential step to the sample electrolytic solution by using at least a working electrode and a reference electrode;
(b) measuring double layer capacitance of the working electrode in said sample electrolytic solution under the applied potential step;
(c) determining the concentration of the organic component in said sample electrolytic solution, based on the double layer capacitance measured in step (b), and(d) adding organic component when the concentration of organic component falls below effective electrolytic solution levels,wherein the sample electrolytic solution comprises a copper electroplating solution comprising copper ions, and wherein the copper ions do not deposit onto the working electrode;
wherein the double layer capacitance of the working electrode is measured by monitoring current response of the sample electrolytic solution under the potential step over time; and
wherein the current response is measured using at least one measuring device selected from the group consisting of poteniometers, ammeters and ohmmeters.
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Abstract
The present invention relates to a method and apparatus for determining organic additive concentrations in a sample electrolytic solution, preferably a copper electroplating solution, by measuring the double layer capacitance of a measuring electrode in such sample solution. Specifically, the present invention utilizes the correlation between double layer capacitance and the organic additive concentration for concentration mapping, based on the double layer capacitance measured for the sample electrolytic solution.
96 Citations
20 Claims
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1. A method for determining concentration of an organic component in a sample electrolytic solution, said method comprising the steps of:
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(a) applying a potential step to the sample electrolytic solution by using at least a working electrode and a reference electrode; (b) measuring double layer capacitance of the working electrode in said sample electrolytic solution under the applied potential step; (c) determining the concentration of the organic component in said sample electrolytic solution, based on the double layer capacitance measured in step (b), and (d) adding organic component when the concentration of organic component falls below effective electrolytic solution levels, wherein the sample electrolytic solution comprises a copper electroplating solution comprising copper ions, and wherein the copper ions do not deposit onto the working electrode; wherein the double layer capacitance of the working electrode is measured by monitoring current response of the sample electrolytic solution under the potential step over time; and wherein the current response is measured using at least one measuring device selected from the group consisting of poteniometers, ammeters and ohmmeters. - View Dependent Claims (2, 3, 4, 5)
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6. A method for determining concentration of an organic component in a sample electrolytic solution, said method comprising the steps of:
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(a) applying a potential step to the sample electrolytic solution by using at least a working electrode and a reference electrode; (b) measuring double layer capacitance of the working electrode in said sample electrolytic solution under the applied potential step; (c) determining the concentration of the organic component in said sample electrolytic solution, based on the double layer capacitance measured in step (b), and (d) adding organic component when the concentration of organic component falls below effective electrolytic solution levels, wherein the sample electrolytic solution comprises a copper electroplating solution comprising copper ions, and wherein the copper ions do not deposit onto the working electrode; wherein one or more calibration solutions containing said organic component at unique, known concentrations are provided, wherein the double layer capacitance of the working electrode in each of said calibration solutions under the potential step is measured, which is correlated to the concentration of the organic component in respective calibration solution, and wherein the concentration of the organic component in the sample electrolytic solution is determined based on the double layer capacitance measured for said sample electrolytic solution and the capacitance-concentration correlation obtained by measuring the calibration solutions; and wherein the capacitance-concentration correlation data set is stored in a memory of a computational assembly. - View Dependent Claims (7, 8, 9, 10, 11, 12, 13)
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14. A method for determining concentration of an organic component in a sample electrolytic solution, said method comprising the steps of:
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(a) applying a potential step to the sample electrolytic solution by using at least a working electrode and a reference electrode; (b) measuring double layer capacitance of the working electrode in said sample electrolytic solution under the applied potential step; (c) determining the concentration of the organic component in said sample electrolytic solution, based on the double layer capacitance measured in step (b), and (d) adding organic component when the concentration of organic component falls below effective electrolytic solution levels, wherein the sample electrolytic solution comprises a copper electroplating solution comprising copper ions, and wherein the copper ions do not deposit onto the working electrode; and wherein the organic additives contained in the sample electrolytic solution are not consumed during the measurement of the double layer capacitance. - View Dependent Claims (15, 16, 17, 18, 19, 20)
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Specification