Empyrean intelligent x ray diffractometer

The phase composition of both the mixed powders and the composites were characterized by an Empyrean Intelligent X-ray Diffractometer (Malvern Panalytical, Malvern, UK). The specific test conditions were as follows: accelerating voltage 40 kV, current 40 mA, Cu-Kα radiation, scanning speed 10°/min and scanning angle range 10~90°. Before the collection of the diffraction patterns, the tested powder was evenly and randomly laid on the glass test platform, and the surface of the tested composite block was sandpapered and cleaned with an acetone solution.
The microstructure of the mixed powder and the composites were observed and snapped by a ZEISS459315 (Carl Zeiss A.G., Oberkochen, Cermany) metallographic microscope and Quanta 200FEG (FEI Company, Hillsboro, OR, USA) field-emission scanning electron microscopy (SEM) equipped with energy dispersive spectrometer (EDS). The sample with a dimension of 4 mm × 5 mm × 3 mm was obtained by electro discharge wire cutting. Before this, the observed samples were successively polished, cleaned and etched (400 #, 800 #, 2000 # and 4000 # sandpaper were selected for polishing, and a diamond polishing agent was selected for polishing cloth; the etched solution was Kroll reagent with a ratio of 20 vol%HF + 20 vol%HNO₃ + 60 vol%H₂O).

After the forming of the SLM process, the samples were cut from the substrate by wire cutting, cleaned with ethanol and ultrasonic waves, and dried in a vacuum drying oven. Three densitometric measurements were performed and averaged for each sample using Archimedes’ principle, respectively.
To analyze the microstructure of the samples, 450 mesh, 800 mesh, 1000 mesh, and 2000 mesh sandpapers were used to polish the samples in turn. Then, the samples were polished by an LMP-3S type metallographic polishing machine and diamond polishing spray. Etching was carried out using diluted aqua regia. Observation was conducted using a Zeiss Axio Vert microscope (Zeiss, Oberkochen, Germany). XRD tests were carried out using an Empyrean intelligent X-ray diffractometer (Malvern Panalytical, Almelo, The Netherlands). The device was equipped with a metal ceramic X-ray tube (Cu target) with a maximum power of 2.2 kW, and the parameters taken for the test program in the experiments were a test angle of 20° to 90°, a step size of 0.026°, and a scanning speed of 8°/min.
The microstructure was observed using a LYRA3 GMU type aggregated ion beam scanning electron double beam electron microscope from TESCAN (Brno, Czech Republic). Phase composition was observed using EBSD.