This paper addresses the challenging task of optical characterization of pure, dielectric (nano-)powders with the aim to provide an end-to-end instruction from appropriate sample preparation up to the determination of material remission and absorption spectra. We succeeded in establishing an innovative preparation procedure to reproducibly obtain powder pellet samples with an ideal Lambertian scattering behavior. As a result, a procedure based on diffuse reflectance spectroscopy was developed that allows for (i) performing reproducible and artifact-free, high-quality measurements as well as (ii) a thorough optical analysis using Monte Carlo and Mie scattering simulations yielding the absorption spectrum in the visible spectral range. The procedure is valid for the particular case of powders that can be compressed into thick, non-translucent pellets and neither requires embedding of the dielectric (nano-)powders within an appropriate host matrix for measurements nor the use of integrating spheres. The reduced spectroscopic procedure minimizes the large number of sources for errors, enables an in-depth understanding of non-avoidable artifacts and is of particular advantage in the field of material sciences, i.e., for getting first insights to the optical features of a newly synthesized, pure dielectric powder, but also as an inline inspection tool for massively parallelised material characterization.

Nonlinear diffuse femtosecond-pulse reflectometry is introduced as a powerful experimental tool for the unambiguous characterization of polar and non-polar point symmetry groups of harmonic upconversion nanoparticles. Using intense ultrashort 40 femtosecond laser pulses and an appropriate figure of merit (FOM), second and third harmonic emission serve for the structural characterization of polar Yb-doped lithium niobate and non-polar titanium dioxide nanoparticles. The tool is capable of differentiating these two samples by FOM values that differ by up to 13 orders of magnitude. The general applicability to harmonic upconversion nanoparticles over a broad range of intensities and wavelength spectrum, is discussed.