In situ diagnostics of the crystal-growth process through neutron imaging: application to scintillators.

Neutrons are known to be unique probes in situations where other types of radiation fail to penetrate samples and their surrounding structures. In this paper it is demonstrated how thermal and cold neutron radiography can provide time-resolved imaging of materials while they are being processed (e.g. while growing single crystals). The processing equipment, in this case furnaces, and the scintillator materials are opaque to conventional X-ray interrogation techniques. The distribution of the europium activator within a BaBrCl:Eu scintillator (0.1 and 0.5% nominal doping concentrations per mole) is studied in situ during the melting and solidification processes with a temporal resolution of 5-7 s. The strong tendency of the Eu dopant to segregate during the solidification process is observed in repeated cycles, with Eu forming clusters on multiple length scales (only for clusters larger than ∼50 µm, as limited by the resolution of the present experiments). It is also demonstrated that the dopant concentration can be quantified even for very low concentration levels (∼0.1%) in 10 mm thick samples. The interface between the solid and liquid phases can also be imaged, provided there is a sufficient change in concentration of one of the elements with a sufficient neutron attenuation cross section. Tomographic imaging of the BaBrCl:0.1%Eu sample reveals a strong correlation between crystal fractures and Eu-deficient clusters. The results of these experiments demonstrate the unique capabilities of neutron imaging for in situ diagnostics and the optimization of crystal-growth procedures.

Transmission electron microscopy specimen preparation method for multiphase porous functional ceramics.

An optimum method is proposed to prepare thin foil transmission electron microscopy (TEM) lamellae of multiphase porous functional ceramics: prefilling the pore space of these materials with an epoxy resin prior to focused ion beam milling. Several advantages of epoxy impregnation are demonstrated by successful preparation of TEM specimens that maintain the structural integrity of the entire lamella. Feasibility of the TEM alignment procedure is demonstrated, and ideal TEM analyses are illustrated on solid oxide fuel cell and solid oxide electrolysis cell materials. Some potential drawbacks of the TEM specimen preparation method are listed for other samples.

Indirect measurement of the magnetocaloric effect using a novel differential scanning calorimeter with magnetic field.

A simple and high-sensitivity differential scanning calorimeter (DSC) unit operating under magnetic field has been built for indirect determination of the magnetocaloric effect. The principle of the measuring unit in the calorimeter is based on Peltier elements as heat flow sensors. The high sensitivity of the apparatus combined with a suitable calibration procedure allows very fast and accurate heat capacity measurements under magnetic field to be made. The device was validated from heat capacity measurements for the typical DSC reference material gallium (Ga) and a La(0.67)Ca(0.33)MnO(3) manganite system and the results were highly consistent with previous reported data for these materials. The DSC has a working range from 200 to 340 K and has been tested in magnetic fields reaching 1.8 T. The signal-to-noise ratio is in the range of 10(2)-10(3) for the described experiments. Finally the results have been compared to results from a Quantum Design(R) physical properties measuring system. The configuration of the system also has the advantage of being able to operate with other types of magnets, e.g., permanent magnets or superconducting coils, as well as the ability to be expanded to a wider temperature range.