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Inorganic powder analysis by time-wavelength resolved luminescence spectroscopy Paski, Edgar Francis


An investigation into the potential of time-wavelength resolved luminescence spectroscopy for the analysis of inorganic powders was performed. A time-wavelength resolved luminescence spectrometer consisting of an excimer laser, scanning monochromator, and gated integrator was constructed. The spectrometer had wavelength coverage from 265 nm to 800 nm, it was capable of measuring lifetimes between 100 ns and 500 ms. Sample excitation was done at 193 nm and 248 nm. A luminescence system model of first order decay in the time domain and a Gaussian function for the emission band was assumed. The time-wavelength resolved luminescence spectrum was described by the parameters: lifetime, peak maxima, peak halfwidth, and intensity factor. Parameter estimation was done with an algorithm employing a linear algebra construct and simplex optimization. The algorithm's performance on highly overlapped spectra was evaluated. For two component mixtures having a 1 % RSD noise level, overlaps greater than 0.3 halfwidths in the spectral domain and lifetime ratios greater than 1:1.3 were resolved with all parameter estimates having an error of less than ±2%. The luminescence spectra of CaMo0₄, SrMo0₄, BaMo0₄, ZnMoO₄, CdMo0₄, PbMoO₄, CaWO₄, SrW0₄, BaWO₄, ZnWO₄, CdW0₄ and PbWO₄ consisted of broad featureless bands showing simple exponential decay. Mixed crystals of Ca(MOxW₁-x)O₄ and Sr(MOxW₁-x)0₄ were examined. Tungstate emission was quenched by molybdate, the molybdate emission dominated when x was greater than 0.15. The tungstate lifetime was found to be proportional to molybdate concentration. The luminescence spectra of CaZrO₃, SrZr O₃, BaZr O₃ CaHfO₃ SrHfO₃, BaHfO₃, CaO, SrO, and BaO as pure compounds and doped with T1, Pb, Sb, and Bi were studied. The pure zirconates and hafnates showed short lived (<100 ns) luminescence with 248 not excitation; no readily discernible luminescence was observed with 193 nm excitation. Doped compounds tended to show luminescence characteristic of the dopant ion.

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