Linxeye detector

Crystal structures were identified from X-ray powder diffraction (XRD) patterns of the samples using a Bruker D8 Advance diffractometer (Berlin, Germany) equipped with a Bruker LINXEYE detector and a CuKα radiation source. Micro-Raman spectroscopy was performed using a JASCO NRS-5100 Dispersive Micro-Raman (Tokyo, Japan) equipped with a green diode laser of 532 nm, with 30 mW power (Elforlight G4-30; Nd: YAG), with a spectral range from 50 to 8000 cm⁻¹. Thermogravimetric analysis was carried out in a Shimadzu TGA-50H (Kyoto, Japan) with a vertical furnace design, a maximum precision of 0.001 mg, and a temperature range between 25 °C and 950 °C (CIC-UGR).

The relative density of the sintered samples was calculated as the ratio between the experimental density determined by the Archimedes’ method and the composite theoretical density (7.618 g cm⁻³) calculated as the weighted average of PZT (8.006 g cm⁻³) and CFO (5.304 g cm⁻³) crystallographic densities.
The crystalline phases were identified by X-ray powder diffraction using a Bruker D8 Advance X-ray diffractometer (θ-θ equipped with a LINXEYE detector (Bruker, Karlsruhe, Germany), using Cu K_α radiation. Patterns were recorded in the 15° ≤ 2θ ≤ 80° range with 2.4°/min scanning rate.
The microstructure of the sintered samples was investigated by scanning electron microscopy (SEM-FEG, Carl Zeiss Sigma NTS GmbH, Oberkochen, Germany), embedding the cross sections in epoxy resin and then polishing them down to 0.25 µm finish. The grain size distributions of the sintered samples were calculated via image analysis of the SEM micrographs using ImageJ software (Java, ORACLE, Redwood City, CA, USA).

Structural and compositional characterizations of each sample was performed through quantitative analysis by X-ray diffraction (XRD) using the q-XRD Rietveld Refinement method and peak ratio analysis (RIR: reference intensity ratio), allowing the determination of the crystalline and amorphous components in multiphase mixtures. The identification of the most frequent elements was performed by X-ray fluorescence (XRF) using qualitative and quantitative standardless methods. The studies were carried out with the equipment and technicians at the X-ray Division of the Central Services of Science and Technology (Servicios Centrales de Ciencia y Tecnología—SC-ICYT) of the University of Cadiz (UCA): Bruker D8Advance A25 Davinci, with a LINXEYE detector, for XRD and Bruker M4 Tornado for XRF.