Applications

In this article portable Raman spectroscopy as an effective tool for at-line characterization of carbon black is presented. Raman spectroscopic analysis can be an effective test to characterize carbon black material, including the structural order.

Raman spectroscopy is a valuable tool for the characterization of carbon nanomaterials due to its selectivity, speed, and ability to measure samples nondestructively. Carbon materials typically have simple Raman spectra, but they contain a wealth of information about internal microcrystalline structures in peak position, shape, and relative intensity.

The Restriction of Hazardous Substances (RoHS) Directive 2002/95/EC stipulates maximum limits for the hazardous metals cadmium, lead and mercury as well as the hexavalent chromium and the brominated flame retardants in electrical and electronic products. To ensure compliance, reliable analysis methods are required.This poster deals with the wet-chemical determination of trace concentrations of the six RoHS-restricted substances in a wide variety of materials including metals, electrotechnical components, plastics and wires. After sample preparation according to IEC 62321, the metals lead, cadmium and mercury are best determined by anodic stripping voltammetry (ASV) and the flame retardants PBB and PBDE are quantified by direct-injection ion chromatography (IC) using spectrophotometric detection. Chromium(VI) can be determined either by adsorptive stripping voltammetry (AdSV) or IC. Both methods are very sensitive and meet prescribed RoHS limits.

UV/VIS detection is one of the most sensitive detection techniques in trace-level chromatography. Sometimes, however, spectrophotometric detection lacks sensitivity, selectivity or reproducibility and chemical derivatizations are required. By using Metrohm`s rugged and versatile flow-through reactor, single- or multi-step derivatizations can be done fully automatically, in either pre- or post-column mode at any temperature between 25…120 °C. The variable reactor geometry allows to adjust the reactor residence time of the reactants according to derivatization kinetics. The flexibility of the reactor is demonstrated by optimizing four widespread post-column techniques: the relatively slow ninhydrin reaction with amino acids and the fast derivatizations of silicate, bromate and chromate(VI).

Eco Titrators provide the capability to send PC/LIMS reports directly to a PC. This feature is mainly used to transfer data to an external LIMS system or to simply store the data in a digitally on the PC. Additionally, it is possible to control the Eco Titrator by RS232 commands if the connection is set up according to the procedure described below.The data transfer from the Eco Titrator to a PC can be done by a software- or a hardware-based option. Additional accessories are needed for the hardware-based option whereas for the software-based option two additional softwares must be installed. Both solutions are described in this document.

This Application Bulletin contains installation instructions for the MVA-24 CVS setup used to measure suppressors, brighteners, and levelers in plating solutions.

Cleanliness is indispensable in electronics production. Ionic contaminations in particular lead to a drastic worsening of the quality of the printed circuit boards. The present Application Note describes the determination of cations on printed circuit board surfaces. The intelligent Partial Loop Injection Technique (MiPT) used for this purpose permits the determination of cations and anions in the same sample. The determination of the anions is described in AN-S-317.

Hydrogen peroxide is available in different purity grades depending on its use. High purity H2O2 (electronic grade) requires very low contamination levels, e.g., less than 1 μg/L of trimethylamine (TMA). This application describes the determination of trimethylamine in a high-purity H2O2 solution (30%). Analysis is performed using Inline Preconcentration with Matrix Elimination (MiPCT-ME) applying conductivity detection after sequential cation suppression.

Determination of trace levels of cations and amines in hydrogen peroxide is important in quality determination of high-grade semiconductor chemicals. In particular, some manufactures look for 1 ppb trimethylamine or less in hydrogen peroxide samples. Ion chromatography after MiPCT-ME* with conductivity detection after sequential cation suppression is applied.

A reference electrode has a stable and well-defined electrochemical potential (at constant temperature), against which the applied or measured potentials in an electrochemical cell are referred. A good reference electrode is therefore stable and non-polarizable. In other words, the potential of such an electrode will remain stable in the used environment and also upon the passage of a small current. This application note lists the most used reference electrodes, together with their range of use.

Copper is arguably one of the most technologically relevant metals, especially for the semiconductor industry. The deposition process used in this industry is known as the dual-damascene process and it involves the electrodeposition of copper from an acidic cupric compound, in the presence of additives.This Application Note illustrates the use of the Autolab rotating ring disc electrode (RRDE) for the study of electrodeposition of copper and the detection of the Cu+ intermediate.

The determination of heavy metal ions in a solution is one of the most successful application of electrochemistry. In this application note, anodic stripping voltammetry is used to measure the presence of two analytes, in a sample of tap water.

Capacitors are electronic components necessary for the success of the electronics industry. They have also become essential components of both electric and hybrid vehicles. Electrochemical tests, such as potentiostatic cyclic voltammetry, are used to check the performance of capacitors. VIONIC powered by INTELLO can perform both staircase and linear cyclic voltammetries (CV). This Application Note gives a comparison between the linear and the staircase potentiostatic cyclic voltammetries and highlights the necessity of using the linear CV to best study the performance of capacitors.

In this Application Note, hydrogen permeation experiments are conducted following the procedure described in the ASTM standard G148.

The Devanathan-Stachurski cell (or «H cell») is successfully used to evaluate the permeation of hydrogen through sheets or membranes. As small amounts of hydrogen pass through the sheet or membrane, a very sensitive potentiostat is required for its detection. A study of the hydrogen permeation properties of different iron sheets is discussed in this Application Note while taking the instrumental requirements into account.

In the application note AN-EIS-004 on equivalent circuit models, an overview of the different circuit elements that are used to build an equivalent circuit model was given. After identifying a suitable model for the system under investigation, the next step in the data analysis is estimation of the model parameters. This is done by the non-linear regression of the model to the data. Most impedance systems come with a data-fitting program. In this application note, the way NOVA is uses to fit the data is shown.

In this application note, the advantage of recording the raw time domain data for each individual frequency during an electrochemical impedance measurement is described.

Electrochemical impedance spectroscopy (EIS) is a powerful technique which provides information about the processes occurring at the electrode-electrolyte interface. The data collected with EIS are modeled with a suitable electrical equivalent circuit. The fitting procedure will change the values of the parameters until the mathematical function matches the experimental data within a certain margin of error. In this Application Note, some suggestions are given in order to get acceptable initial parameters and to perform an accurate fitting.

This Application Note presents the Mott-Schottky measurement, an extension of electrochemical impedance spectroscopy (EIS), on a popular semiconducting material.

This Application Note explains how fluoride determination in acid etching baths can be performed with thermometric titration.

Determination of hydrofluoric acid in mixed acid etchant solutions.

This Application Note describes the determination of fluoride in silicon etch solutions with thermometric titration.

Determination of concentrated potassium hydroxide solutions which had been used for the etching of substrates containing silicon.

Determination of the total acids concentration in mixtures of nitric-hydrofluoric acid intended for etching silicon substrates.

Two separate titration sequences are required to analyze the mixture:- titration of the HF content with Al(NO3)3 (the «elpasolite» reaction)- titration of the H2SO4 with BaCl2 followed by titration with NaOH to determine the «total acids» contentThe HF, H2SO4, and «total acids» contents are converted to a HNO3 equivalent, with the HNO3 content found by subtracting the HF and H2SO4 from the «total acids» content.

Thermometric titration can be used for the ready determination of sulfuric acid and phosphoric acid in acid mixtures. An endpoint for each acid appears on the titration curve that can be used to quantify the respective acid.

Thermometric titration is used for the determination of hydrochloric acid and phosphoric acid in acid mixtures. Two endpoints appear on the titration curve that are used for the determination of the two acids.

Thermometric titration is used for the determination of hydrochloric acid and nitric acid in acid baths. The entire acid content is titrated with caustic soda in the initial titration; the hydrochloric acid content is then determined in a second titration using silver nitrate solution.

Thermometric titration is used to determine hydrochloric acid and hydrofluoric acid (hydrogen fluoride) in etching baths containing ethanol and acetonitrile. Two endpoints appear on the titration curve that are used individually for the quantification of the respective acid.

Thermometric titration is used to determine hydrofluoric acid and nitric acid in etching baths containing ethanol and acetonitrile. Two endpoints appear on the titration curve that are used individually for the quantification of the respective acid.

Determination of nitrate in a copper plating bath after conversion of nitrate to ammonium. Direct potentiometric measurement using the NH3-ISE.

Determination of fluoride in a chromium plating bath by direct potentiometry using the F-ISE.

In the semiconductor industry, thermoset resins combined with fabric or paper are used as an intermediate layer between substrates of printed circuit boards (PCB). These polymer-based sheets (laminates) are chosen depending on thickness and their thermomechanical and electrical characteristics. Near infrared spectroscopy (NIRS) is a fast, non-destructive and easy-to-use analytical method which allows the measurement of multiple key quality parameters in less than a minute. The following Application Note describes the determination of the transition time of PCB laminates by NIRS, a parameter correlating with the thickness, glass transition temperature, and tensile strength of the material.

Fast and reliable detection of phosphoric, sulfuric, nitric, and hydrofluoric acids with near-infrared spectroscopy in under one minute.

This application note discusses an alternative near-infrared (NIR) spectroscopy method that can reliably determine all parameters within a minute, even in complex acid mixtures.

In an electroless plating bath, the consumed ingredients have to be regularly replenished to ensure an even layer of nickel-phosphorus alloy. This requires online monitoring of the active bath constituents. Parameters to be controlled are pH value (4.5–5.0) as well as nickel (NiSO4 < 10 g/L) and hypophosphite concentration (NaH2PO2: 1–12%). Other measurement options include sulfate, alkalinity, and organic additives (via CVS).

The planarity and smoothness of silicon wafers are fundamental to manufacture optimal semiconductor devices, and Chemical Mechanical Planarization (CMP) is the most common technology used to achieve ultra-flat surfaces. A slurry is used for this purpose, composed of deionized water, a colloidal silicon or alumina liquid dispersion, and hydrogen peroxide, which has to be constantly monitored at all times.Online monitoring of the CMP process is necessary to avoid chemical waste and enhance wafer production yields. Metrohm Process Analytics can measure not only the H2O2 concentration, but also pH, conductivity, and temperature using the multipurpose 2060 Process Analyzer.

Rapid inline monitoring of the major SC1/SC2 bath constituents is possible with reagent-free near-infrared spectroscopy, e.g., the 2060 The NIR-R Analyzer.

Lithium is a soft alkali metal that is typically obtained from salt lake brines. Lithium is used for many applications, but especially for production of lithium-ion batteries in electric cars, mobile phones, and more. This Process Application Note presents a method to monitor lithium as well as other cations in brines by online process ion chromatography (IC), a multiparameter analytical technique that can measure ionic analytes in a wide range of concentrations.

Etching is a vital process in semiconductor fabrication, involving the chemical removal of layers from the wafer substrate. Strict quality control measures are necessary to determine acid etchant concentrations in mixed acid solutions (e.g., SPM, DSP, or DSP+), critical for optimizing etch rate, selectivity, and uniformity during multiple wafer etching steps. This application presents a method to measure sulfuric acid and hydrogen peroxide in etching baths simultaneously using Raman spectroscopy with the PTRam Analyzer from Metrohm Process Analytics.

Monitoring organic additives in copper plating baths is crucial. The 2060 CVS Process Analyzer optimizes copper electroplating by providing precise bath control.

Determination of fluoride, chloride, and nitrate in a solution of NiSO4, ZnSO4 in sulfuric acid using anion chromatography with conductivity detection after chemical suppression.

Determination of fluoride, nitrate, phosphate, and sulfate in an etching reagent using anion chromatography with conductivity detection after chemical suppression.

Determination of bromoacetate, methanesulfonate, chloride, phosphate, and sulfate in an acidic cleaning solution using anion chromatography with conductivity detection and chemical suppression.

Electronic-grade nitric acid may not contain more than the slightest traces of anion contaminations (in the mg/L range). The ion chromatography determination of these kinds of anion traces requires not only a high-capacity column but also an eluent that allows the nitrate to be eluted by the column, although only after all of the other ions of interest have been eluted. This separation is achieved on a column of the Metrosep A Supp 16 - 250/4.0 type with the aid of a strong carbonate/hydrogen carbonate eluent.

Pyrophosphate is used as a stabilizer in aqueous hydrogen peroxide solution. “Reagent grade” solutions may contain pyrophosphate in the higher mg/L range, while “electronic grade” hydrogen peroxide should be free of this stabilizer. Here the determination of pyrophosphate in a high purity H2O2 solution (30%) is performed applying Inline Preconcentration with Matrix Elimination (MiPCT-ME) and a Dose-in Gradient.

Lithium-ion (Li-ion) battery electrolyte quality is essential for performance, stability, and safety reasons. Ion chromatography is an accurate method for electrolyte analysis.

Boehm titration is a quantitative analysis of functional groups on the surface of carbon materials based on their reactions with basic solutions of NaHCO3 (pKa = 6.4), Na2CO3 (pKa = 10.3), and NaOH (pKa = 15.7). This is a cost-efficient method that gives absolute values with high precision of the accessible, mainly oxygen-containing functional groups on the surface. Originally, Boehm titration was developed for carbon materials like conductive carbon black (CCB), activated carbon, porous carbon, and graphite. Modern carbon-based materials like graphene, graphene oxide (GO), or carbon nanotubes can also be analyzed this way.

This Application Note compares the OMNIS Titrator and 888 Titrando for determinations of nitric acid, phosphoric acid, and acetic acid in an aluminum etching bath, as well as the determination of tetramethylammonium hydroxide (TMAH). Identical analysis parameters were used, showing that OMNIS delivers results on par or even better than with other established titration systems.

The pH value in carbon black, an essential additive in modern lithium-ion batteries, is accurately and reliably analyzed in this Application Note by using the 913 pH Meter equipped with a Unitrode easyClean according to ASTM D1512 as well as ISO 787-9 and GB/T 1717-1986.