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: Low concentrations of silicon in an etchant solution are analyzed by adding a predetermined concentration of fluoride ions to a test solution comprising a predetermined volume of the etchant solution, and measuring the concentration of fluoride ions in the test solution. Reaction with silicon ions in the test solution reduces the concentration of fluoride ions, which are present in stoichiometric excess, so that the silicon concentration of the etchant solution can be calculated from the difference between the predetermined and measured concentrations of fluoride ions in the test solution. The method is especially suited for analysis of silicon nitride etchants comprising a high concentration of phosphoric acid.

Abstract: The stability of an electroless plating bath for depositing a metal (e.g., nickel) is determined by titrating a sample of the plating bath with a titrant comprising ions of a catalytic metal (e.g., palladium) and detecting hydrogen released at the titration endpoint. The quantity of titrant required to attain the endpoint provides a measure of the stability of the electroless plating bath.

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: The invention provides a device and a method for packaging of one or more neckties for retail display. The device includes a hanger part for hanging neckties on a rack, and a fastener part for holding the neckties together so as to maintain an orderly appearance. The device is inexpensive, convenient to use, and offers enhanced opportunity for brand identification and advertisement.

Abstract: Performance of a flux in a soldering process is assessed by monitoring the activity of the flux via its electrical conductance measured using a probe having interdigitated metallic traces and a temperature sensor. The measured conductance-temperature time profile provides information useful for selecting a suitable flux formulation and soldering conditions for a given application, for determining the cause of soldering process problems, and for developing improved flux formulations.

Abstract: Underfill voids and solder ball defects are detected via laser generation and laser detection of an ultrasonic wave at the top surface of flip chips. High resolution is provided by using small laser spot sizes and closely-spaced laser beams of wavelengths that are absorbed near the surface of the semiconductor. Alternatively, the generation laser beam may be absorbed in the bulk of the semiconductor. Improved spatial resolution and rejection of unwanted scattered waves can be attained by limiting the time frame of the ultrasonic waveform to the time required for the first longitudinal wave reflection from the bottom of the flip chip. The laser beam spacing can be reduced by using overlapping probe and detection beams of different wavelengths. Resolution of less than 100 ?m features was demonstrated for silicon flip chips.

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: Subsurface defects in a processed metal are detected by a laser-ultrasonic method involving generation of a surface acoustic wave at one location on the processed metal surface, and detection of a scattered acoustic wave at another location on the processed metal surface. The method can be used in-line to provide real time monitoring of laser cladding and other metal processing operations.

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: Dynamic vibration monitoring of a cutting tool or workpiece is provided by propagating an ultrasonic carrier beam in a stream of fluid flowing from a probe chamber, which includes a transducer, to the cutting tool or workpiece target area. The modulated ultrasonic beam reflected from the target is detected via a transducer in the chamber, and is demodulated to provide measurements of vibrational surface displacement and velocity. The method is insensitive to the target surface roughness and can be used for dynamic characterization prior to machining, and for monitoring during the machining operation. The device is inexpensive and robust to the machining environment, and can be applied to small cutting tools.

Abstract: A locally distributed electrode is made by placing a conducting metallic oxide layer and a counter electrode in contact with a noble metal electroplating solution and applying a negative potential to the metallic oxide layer relative to the counter electrode, such that the noble metal is electrodeposited from the solution preferentially at defect sites on a surface of the metallic oxide layer. The noble metal nuclei are selectively electrodeposited at the defect sites to form a locally distributed electrode made up of a dot matrix of metallic islands. For reversible electrochemical mirror (REM) devices, the presence of the noble metal renders mirror metal electrodeposition at the defect sites reversible so that the defects become part of the dot matrix electrode and extraneous deposition of the mirror metal on the conducting metallic oxide is avoided.

Abstract: The concentration of citrate complexing agent in an electroless cobalt or nickel plating bath is determined by titrating a sample of the electroless plating bath containing a small concentration of free fluoride ion with a standard lanthanum nitrate solution. During the titration, La3+ ion first reacts preferentially with the citrate complexing agent and then with fluoride ion, which reduces the free fluoride ion concentration. The endpoint for the titration is indicated by a substantial decrease in the free fluoride ion concentration, which is detected via a fluoride ion specific electrode (ISE). The method can be used for analysis of other complexing agents.

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: Reversible electrochemical mirror (REM) devices typically comprise a conductive oxide mirror electrode that is substantially transparent to radiation of some wavelengths, a counter electrode that may also be substantially transparent, and an electrolyte that contains ions of an electrodepositable metal. A voltage applied between the two electrodes causes electrodeposition of a mirror deposit on the mirror electrode and dissolution of the mirror deposit on the counter electrode, and these processes are reversed when the polarity of the applied voltage is changed. Such REM devices provide precise control over the reflection and transmission of radiation and can be used for a variety of applications, including smart windows and automatically adjusting automotive mirrors.

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: The concentration of chloride ion in an acid copper electroplating bath is determined from the effect that chloride exerts on the copper electrodeposition rate in the presence of organic additives. A cyclic voltammetric stripping (CVS) rate parameter is measured, before and after standard addition of a plating bath sample, in an acid copper electrodeposition solution containing little or no chloride and at least one organic additive. Cross contamination and waste disposal issues associated with the reagents and reaction products involved in chloride titration analyses are avoided. The method may also be applied to analysis of other halides (bromide and iodide) and other solutions.

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.