Nickel oxide nanopowder was prepared by a simple method and analyzed by X-ray powder diffraction. A solution of gelatin and NiCl2⋅6H2O salt were prepared and sintered in sequence. Using a synchrotron light source for X-ray powder diffraction analysis, the synthesized material was characterized as a function of temperature in the interval of 375 to 600 °C. Results from thermogravimetric analysis confirm the temperature loss of the organic substance during the sintering process and show that the temperature for NiO attainment is 600 °C.

Atom probe tomography provides a chemical analysis of nanostructured materials with outstanding resolution. However, due to the process of field evaporation triggered by nanosecond high voltage pulses, the method is usually limited to conductive materials. As part of recent efforts to overcome this limitation, it is demonstrated that the analysis of thick NiO and WO3 oxide layers is possible by laser pulses of 500 ps duration. A careful analysis of the mass spectra demonstrates that the expected stoichiometries are well reproduced by the measurement. The reconstruction of lattice planes proves that surface diffusion is negligible also in the case of thermal pulses.