Abstract: Colloidal dispersions which contain particles predominantly in the submicron size range are ideal candidates for particle size analysis using the combined techniques of dynamic light scattering (DLS) and single particle optical sensing (SPOS). Our new Accusizer 388 hybrid instrument system combines results from both of these systems simultaneously, yielding particle size distribution (PSD) results over a wide size range with unprecedented resolution. The DLS subsystem provides a "broad-brush" description of the overall PSD, often using a simple Gaussian or log-normal shape, where the resolution is limited by the ensemble nature of DLS, requiring data inversion techniques. The resulting mean diameter and standard deviation can be used to identify the end point of the particle manufacturing process (e.g. grinding, homogenization, emulsion polymerization, etc.). The complementary SPOS subsystem provides a precise picture of the outlying, large-diameter tail of the primary particles/aggregates, which often can severely compromise the quality of the final product associated with the dispersion. Proprietary Autodilution (Pat.) and specialized data analysis techniques permit the PSD results from the two subsytems to be coupled quantitatively.

Application Note 158 (AN158) Multiangle Sizing of Proteins and Protein Aggregation

Abstract: Proteins prepared using hot and cold methods were sized at 90, 60, and 20 degrees using the Nicomp 380 Dynamic Light Scattering (DLS) Particle Size Analyzer equipped a multiangle goniometer. This capability was coupled with a high powered 15 mW laser diode and a high gain avalanche photo-diode detector providing a gain increase of 12 over the standard Nicomp 380. Since larger particles scatter relatively more light in the forward direction, low angle DLS has the potential to provide important information on the aggregation of proteins and other macromolecules.
Abstract: Traditionally, blood cells, both red and white, are counted using the electrozone sensing method. This method measures the increase in resistance or inversely, the decrease in conductivity across a small aperture when particles, dispersed in a conductive medium, pass through this aperture. The magnitude of this response is related to the particle’s volume and thus its size. While this technique has worked well for years, this paper demonstrates that particle counting using SPOS (Single Particle Optical Sensing) in conjunction with Autodilution can size both red and white blood cells with greater ease of use and less diluent restrictions than electrozone sensing.
Abstract: Zeta Potential has been used to gauge the stability of colloidal dispersions. The basis for this is that zeta potential is proportional to the charge on the surface of a particle. The larger the zeta potential then, the stronger the repulsive forces between these particles. Such large repulsive forces keep diffusing particles from randomly colliding together to form aggregates. The measurement of zeta potential can be useful in other applications. In this paper, zeta potential was used to test an instrument that separates blood into its various fractions. Red blood cells have a larger surface potential than white blood cells. It was observed that as the concentration of white blood cells increased in each fraction, the average zeta potential decreased.
Abstract: In analyzing the particle size distributions of polymer emulsions, it is common to employ one of the various light scattering methods. Generally, they fall into two categories: Static and Dynamic. Static light scattering, also known as Laser Diffraction, employs the use of spatially arrayed detectors that record the scattered light patterns as a function of angle. Dynamic light scattering measures, over a period of time, the amplitude of the scattered light at one angle. In both techniques, specialized mathematical algorithms are needed to invert either the scattered light patterns or scattered light time profiles to arrive at particle size distributions (PSDs). As a consequence of the ensemble nature of both these light scattering methods, they are low resolution and low sensitivity techniques and they can be susceptible to artifacts and instabilities. The data in this paper demonstrates that the Nicomp algorithm, used only in the Nicomp 380, can provide accurate and realistic PSDs for emulsion samples which have relatively wide distributions and would give other light scattering instruments trouble.
Abstract: Kaolin clay is a naturally occurring mineral used extensively by the paper industry as filler and as a coating. In its natural state, Kaolin clay is white in color. It is this whiteness as well as other properties such a large surface area and good ink retention that makes it an ideal material for use in the manufacturing of paper. Particle size is extremely important in the processing of the clay. The clay particles are classified and the different fractions are used to impart various properties to the paper. It is also important in the processing of Kaolin clay that impurities such as sand and mica be removed. The Accusizer 780, with its high sensitivity and resolution, allows the clay fractions to be more accurately characterized and out-liers to be more readily detected than can be done with Laser Diffraction methods.
Abstract: Chemical Mechanical Polishing (CMP) is an important set of steps in the production of high-density integrated circuits. And because CMPs are used during various points in the process for usually short periods of time, they must be handled extensively and are exposed to many different environments. New batches must be prepared often, from concentrate kept in storage. All of these issues impact the stability of the slurries, which in turn effect the yield levels of chips. What is required is a measurement technique that is sensitive to low levels of out-of- spec particles, which can be the result of contamination from handling or aggregation from applied stress. This technique would need to be used to do quality checks on fresh material and have the ability to be placed online to monitor the slurry in-situ. The goal of this paper is demonstrate the utility of Single Particle Optical Sizing (SPOS) for providing quantitative information about CMP slurry health.
Abstract: The semiconductor industry is moving toward smaller line widths and more layers. One of the most important process considerations that will lead the way to this higher density chip technology is more sophisticated control of the planarization steps. The planerization or polishing steps are effected by the use of colloidally dispersed metal oxide slurries (known as CMPs, which stands for Chemical-Mechanical Planerization), primarily silica and alumina, with mean diameters in the 10-200 nm range. These slurries are applied to spinning polishing pads which rest on the wafers. In the past, Laser Diffraction was most commonly used to characterize the particle size distribution of these slurries. It has always been known that these slurries contain a small volume percentage of particles greater than 1 micron in size. It is believed that these particles can cause scratches and other defects in the wafer surfaces. This paper will demonstrate that by virtue of the nature of the measurement, Laser Diffraction is inadequate to the task of quantitatively determining the concentration of out-of-spec slurry particles. On the other hand, Single Particle Optical Sizing or SPOS, because it counts particles, will be shown to be an excellent tool for characterizing CMP slurries.
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