A sensitive particle distribution probe uses special processing including
a modified Twomey/Chahine iterative convergence technique and a specially
constructed sample cell to obtain particle size distribution measurements
from optically dense slurries, such as the slurries used in the
semiconductor industry for chemical mechanical planarization. Spectral
transmission data is taken over the spectral range of 0.20-2.5 microns,
utilizing specially constructed, chemically resistant sample cells of
50-2000 microns thickness, and miniature, fixed grating, linear detector
array spectrometers. At wavelengths greater than one micron, the
preferred design utilizes InGaAs linear detector arrays. An ultrasonic
disrupter can be employed to breakup harmless soft agglomerates. In
addition to direct particle size distribution measurement, the invention
described here could be used to detect other fundamental causes of slurry
degradation, such as foaming and jelling. The probe accomplishes
continuous, real time sampling of undiluted slurry. A three-position
chopper allows automated operation in an industrial environment without
the need for frequent reference spectra, which would require taking the
probe off-line. In other embodiments, the invention provides a quality
control and/or particle size measuring system for CMP slurries using
transmission data through an as-used CMP slurry flow. The process of the
invention detects transmission through the flow, at select wavelengths,
and determines changes in the logarithmic slope of transmission versus
wavelength to detect acceptable or unacceptable CMP slurries. The process
can further determine CMP slurry particle size through empirical
extinction data stored in memory.