D8 focus powder x ray diffractometer

The crystalline structure of the sample was characterized using a Bruker D8 FOCUS X-ray powder diffractometer (XRD, Cu K_α radiation, Bruker Corporation, Billerica, MA, USA). The size, shape, and nanostructure were investigated on a ZEISS MERLIN Compact scanning electron microscope (SEM, Carl Zeiss AG, Oberkochen, Germany) and a Tecnai G2 F20 transmission electron microscope (TEM, Frequency Electronics Inc., Hillsboro, OH, USA). X-ray photoelectron spectra (XPS) were obtained using a Thermo ESCALAB 250XI electron spectrometer (Thermo Fisher Scientific Inc., Waltham, MA, USA). Raman spectrum was taken by a Renishaw inVia Raman microscope (Renishaw Company, Gloucestershire, UK). Nitrogen adsorption/desorption test was performed on an ASAP 2020/Tristar 3000 instrument (Micromeritics Instrument Corporation, Norcross, GA, USA). The amount of carbon materials in the sample was assessed using SDT Q600 thermal gravimetric analysis (TG, TA Instruments, New Castle, DE, USA).

The synthesized nanoparticles were analysed using Fourier transform infrared (FTIR) spectroscopy using a Bruker Vertex80 spectrophotometer in the wavenumber range 400 and 4000 cm⁻¹. Samples were prepared in the form of pellets using KBr, maintaining the KBr : sample mass ratio at 1 : 10. Scanning electron microscopy (SEM) images and surface elemental analysis of AMNPs and AuPd@AMNPs was conducted using a Hitachi SU6600 FE-SEM. X-ray diffraction analysis of the synthesized AMNPs and AuPd@AMNPs was performed using a Bruker D8 Focus X-ray powder diffractometer using Cu Kα radiation (=0.154 nm) over the 2θ range of 5°–80°, with a step size of 0.02° and a step time of 1 s. Elemental analysis of AMNPs and AuPd@AMNPs was done using inductively coupled plasma mass spectrometry (ICPMS) using the Agilent 7000 ICPMS System. Samples: 25.0 mg were digested in H₂O₂ followed by dissolution in a mixture of HCl and HNO₃, the final volume was made up to 10.0 ml. The products of catalytic reactions were characterized by GC–MS using Agilent 5977A Series GC/MSD System having a 30 m × 250 µm × 0.25 µm HP-5 ms column. The temperature programme was 40–250°C at 30°C min⁻¹ with a final temperature isothermal hold for 12 min. The MS mass limit was set between 50 and 450 Da.

All chemicals were purchased from Sigma–Aldrich without further purification. ¹H and ¹³C nuclear magnetic resonance (NMR) was taken by AVII 400 MHz NMR spectrometer of Bruker. Thermogravimetric analyses (TGA) were performed under a nitrogen atmosphere with a heating rate of 10 °C/min using a TA Instruments Trios V3.1 thermogravimetric analyzer. Differential scanning calorimetry (DSC) scans were performed under a nitrogen atmosphere with a heating rate of 10 °C/min using Mettler-Toledo DSC. The dielectric constant was measured by CVU unit in Keithley-SCS4200 with the pelleted sample. Powder X-ray diffraction (PXRD) patterns were recorded on a Bruker D8 Focus Powder X-ray diffractometer using Cu Kα radiation (40 kV, 40 mA) at room temperature. Ferroelectric P-E curve was measured with Precision Multiferroic II Ferroelectric Test System of the Radiant Technologies with high voltage amplifier. Piezoresponse force microscopy (PFM) tests were performed on Bruker Dimension Icon Atomic Force Microscope with grown crystals or spray-coated samples on ITO.