Abstract: Methods for measuring total accelerator in a solution, such as an electrodeposition solution, are provided. Methods can include providing a solution containing an accelerator and one or more breakdown products of the accelerator, oxidizing the solution, and measuring the concentration of the accelerator in the solution. Methods can further include determining total accelerator based on the concentration of the accelerator in the solution.

Abstract: The thickness of a palladium coating on copper (or another substrate) is measured by passing a cathodic current through a predetermined area of the coating in contact with an electrolytic solution and measuring the potential as a function of time. Protons from the electrolytic solution are electrochemically reduced to palladium hydride at cathodic potentials less negative than required for evolution of hydrogen. As formation of the PdH0.58 beta-phase throughout the Pd coating is completed, the cathodic potential increases rapidly to a cathodic potential plateau corresponding to evolution of hydrogen gas on the PdH0.58 surface. This step in the cathodic potential provides an endpoint time for the measurement. The absolute thickness of the Pd coating is calculated from the integrated cathodic charge passed up to the endpoint time and the predetermined area of the coating in contact with the electrolytic solution.

Abstract: The thickness of a palladium coating on copper (or another substrate) is measured by passing a cathodic current through a predetermined area of the coating in contact with an electrolytic solution and measuring the potential as a function of time. Protons from the electrolytic solution are electrochemically reduced to palladium hydride at cathodic potentials less negative than required for evolution of hydrogen. As formation of the PdH0.58 beta-phase throughout the Pd coating is completed, the cathodic potential increases rapidly to a cathodic potential plateau corresponding to evolution of hydrogen gas on the PdH0.58 surface. This step in the cathodic potential provides an endpoint time for the measurement. The absolute thickness of the Pd coating is calculated from the integrated cathodic charge passed up to the endpoint time and the predetermined area of the coating in contact with the electrolytic solution.

Abstract: An auxiliary leveler additive that cannot be analyzed by conventional CVS methods for acid copper plating baths is analyzed by cyclic voltammetry at a platinum rotating disk electrode from its effect on the anodic current at very positive potentials.

Abstract: The chloride concentration in an acid copper plating bath is determined from the chloride oxidation current measured under controlled hydrodynamic conditions at a noble metal electrode using specific voltammetric parameters. The measurement is made directly on the undiluted plating bath so that the chloride measurement is fast and no waste stream is generated.

Abstract: A simple titration method involving a single copper ion titrant detected by a copper ion specific electrode provides the concentrations of both copper ions and bath complexing agent (ethylene diamine, for example) in alkaline copper electroplating baths of the type used to deposit or thicken copper seed layers on silicon wafers. Standard addition of an excess of a strong complexing agent (EDTA, for example) and back-titration with the copper ion titrant yields the bath copper ion concentration, and continued titration to a second endpoint, preferably after addition of hydroxide to adjust the pH of the analysis solution, yields the total concentration of bath complexing agent. Based on these analyzes, the concentration of free bath complexing agent may be calculated. The method also provides direct determination of the free bath complexing agent concentration via standard addition of excess bath complexing agent to a sample of the plating bath and titration with the copper ion titrant.

Abstract: An auxiliary leveler additive that cannot be analyzed by conventional CVS methods for acid copper plating baths is analyzed by cyclic voltammetry at a platinum rotating disk electrode from its effect on the anodic current at very positive potentials.

Abstract: An additive breakdown product in an acid copper plating bath sample is detected by performing a voltammetric analysis for the leveler additive in two measurement solutions comprising different volume fractions of the copper plating bath sample in a background electrolyte. When the plating bath sample contains a substantial concentration of the additive breakdown product, the analyses for the first and second measurement solutions indicate different concentrations for the leveler additive in the plating bath sample. A comparison of the leveler additive concentrations indicated by the two analyses provides a measure of the concentration of the additive breakdown product.

Abstract: Low concentrations of fluoride ion in a semiconductor processing solution containing an acid are determined via fluoride ion specific electrode measurements corrected for the effect of the acid concentration. No reagents are used for the fluoride determination.

Abstract: A simple titration method involving a single copper ion titrant detected by a copper ion specific electrode provides the concentrations of both copper ions and bath complexing agent (ethylene diamine, for example) in alkaline copper electroplating baths of the type used to deposit or thicken copper seed layers on silicon wafers. Standard addition of an excess of a strong complexing agent (EDTA, for example) and back-titration with the copper ion titrant yields the bath copper ion concentration, and continued titration to a second endpoint, preferably after addition of hydroxide to adjust the pH of the analysis solution, yields the total concentration of bath complexing agent. Based on these analyzes, the concentration of free bath complexing agent may be calculated. The method also provides direct determination of the free bath complexing agent concentration via standard addition of excess bath complexing agent to a sample of the plating bath and titration with the copper ion titrant.

Abstract: The chloride concentration in an acid copper plating bath is determined from the chloride oxidation current measured under controlled hydrodynamic conditions at a noble metal electrode using specific voltammetric parameters. The measurement is made directly on the undiluted plating bath so that the chloride measurement is fast and no waste stream is generated.

Abstract: An additive breakdown product in an acid copper plating bath sample is detected by performing a voltammetric analysis for the leveler additive in two measurement solutions comprising different volume fractions of the copper plating bath sample in a background electrolyte. When the plating bath sample contains a substantial concentration of the additive breakdown product, the analyses for the first and second measurement solutions indicate different concentrations for the leveler additive in the plating bath sample. A comparison of the leveler additive concentrations indicated by the two analyses provides a measure of the concentration of the additive breakdown product.

Abstract: A system and method for producing a barbed taped product is controlled by an electronic controller to provide a predetermined pattern of attachment points. The system automatically clips adjacent loops of product strands together in the predetermined pattern. The system is capable of varying the pattern from roll to roll, within a given roll, and between rolls. The system and method eliminates the need for ceasing production between rolls in order to re-thread.

Abstract: A deployment system and associated products utilize a magazine for holding and dispensing the products. The products may have any of a number of internal and external trusses that may be in tension and/or compression for rigidifying the product in selected directions. Thus the product may be shaped to fit a predetermined contour. The magazine may be supported on a deployment vehicle for ease of deployment of the product.

Abstract: The 3-mercaptopropylsulfonic acid (MPSA) breakdown product of the bis(sodiumsulfopropyl)disulfide (SPS) additive used in acid copper plating baths accelerates copper electrodeposition and can be detected by cyclic voltammetric stripping (CVS) analysis. In the presence of oxygen, MPSA decomposes rapidly in acid copper sulfate baths so that the CVS stripping peak area (Ar) decreases on successive cycles. The slope of a plot of Ar vs. CVS cycle number (or time) or logarithm of the CVS cycle number (or time) provides a measure of the initial MPSA concentration.

Abstract: Suppressor and anti-suppressor additives in an acid copper sulfate plating bath are analyzed by the cyclic voltammetric stripping (CVS) method without cleaning or rinsing the cell between the two analyses. The suppressor analysis is performed first and the suppressor concentration in the resulting measurement solution is adjusted to a predetermined value corresponding to full suppression. This fully-suppressed solution is then used as the background electrolyte for the anti-suppressor analysis. This integrated analysis approach provides results comparable to those obtained with cell cleaning and rinsing between the analyses but significantly reduces the analysis time, consumption of expensive chemicals, and quantity of hazardous waste generated.

Abstract: A deployment system and associated products utilize a magazine for holding and dispensing the products. The products may have any of a number of internal and external trusses that may be in tension and/or compression for rigidifying the product in selected directions. Thus the product may be shaped to fit a predetermined contour. The magazine may be supported on a deployment vehicle for ease of deployment of the product.

Abstract: A barbed tape product as adjacent pairs of loops in which the loops of a pair are attached to each other at an attachment point that is circumferentially offset relative to an attachment point of the adjacent pair of loops. Additional attachment points may be provided in helically progressive positions between the first and second attachment points. The attachment points are positioned on one pair of loops so that each of the attachment points are circumferentially offset relative to all other attachment points on an adjacent pair of loops. The attachment points may be positioned in a predetermined helically progressive pattern on a coil of the product. The pattern may provide a predetermined natural configuration of the product when the product is in a deployed state of use. Attachment elements for attaching strands of the product together are sized and configured for strength and accuracy in automatically attached concertina or other barbed tape products.

Abstract: A system and method for producing a barbed taped product is controlled by an electronic controller to provide a predetermined pattern of attachment points. The system automatically clips adjacent loops of product strands together in the predetermined pattern. The system is capable of varying the pattern from roll to roll, within a given roll, and between rolls. The system and method eliminates the need for ceasing production between rolls in order to re-thread.

Abstract: Suppressor and anti-suppressor additives in an acid copper sulfate plating bath are analyzed by the cyclic voltammetric stripping (CVS) method without cleaning or rinsing the cell between the two analyses. The suppressor analysis is performed first and the suppressor concentration in the resulting measurement solution is adjusted to a predetermined value corresponding to full suppression. This fully-suppressed solution is then used as the background electrolyte for the anti-suppressor analysis. This integrated analysis approach provides results comparable to those obtained with cell cleaning and rinsing between the analyses but significantly reduces the analysis time, consumption of expensive chemicals, and quantity of hazardous waste generated.