Cm 20 super twin microscope

Titania nanoparticles were synthesized from TiBALDH (purchased from Sigma Aldrich, CAS No. 65104-06-5) through a simple precipitation method described in Seisenbaeva G. et al. 201319 (link) and from titanium tetraethoxide (CAS No. 3087-36-3) by the techniques of the Captigel patent no. WO07145573. The particles were washed by centrifugation at 4000 rpm three times in anhydrous ethanol and then washed in water four times. They were analysed by Thermo Gravimetric Analysis (TGA) in a Perkin-Elmer Pyris 1, X-Ray Powder Diffraction in Bruker SMART Apex-II multipurpose diffractometer operating with MoKα radiation λ = 0.71073, Energy-Dispersive X-ray Spectroscopy (EDS) and scanning electron microscopy (SEM) with an Hitachi TM-1000-μDeX. Transmission electron microscopy was used to determine the size of the particles using a Philips CM-20 Super Twin microscope, operating at 200 kV. The particle size in solution, both deionized water and M9-minimal salts, was investigated with nano tracking analysis with Nanosight 300 and additional investigation into the different aggregation-states of the particles analysed by dynamic light scattering (DLS) using Microtrac NANO-flex. The zeta potentials were measured on a Malvern Nano ZS.

Evolution of crystal structure was followed using the XRD technique by collecting patterns in 2θ range of 5°–120° with X’Pert PRO X-ray diffractometer (Cu, Kα1: 1.54060 Å) (PANalytical, Almelo, The Netherlands). The morphology and microstructure of nanoparticles were investigated by high-resolution transmission electron microscopy (HRTEM) using a Philips CM-20 Super Twin microscope (Eindhoven, The Netherlands), operated at 200 kV. Samples for measurements were prepared by dispersing of powders in methanol. Afterwards, a droplet of suspension was deposited on a copper microscope grid covered with perforated carbon. ICP-OES elemental analysis was done using an Agilent 720 apparatus (Santa Clara, CA, USA). Calibration curves were measured using ICP standard solution for determination of the Ca²⁺ and P⁵⁺ ions content. Prior to elemental analysis, the nHAP samples were digested using HNO₃ with spectral purity.

The
crystal structure of synthesized materials was characterized by the
X-ray Diffraction (XRD) technique using an X’Pert PRO X-ray
diffractometer (Cu Kα1, 1.54060 Å) (PANalytical). Measured
XRD patterns were compared to standards of YVO₄ (no. 78074)
and YPO₄ (no. 79754) found in the Inorganic Crystal Structure
Database (ICSD). Microstructural analyses (particle size, morphology)
were performed by electron microscopy. SEM was carried out using an
FEI Nova NanoSEM 230. High resolution transmission electron microscopy
(HR-TEM) was performed using a Philips CM-20 Super Twin microscope.
ICP-OES measurements were conducted on Thermo Scientific ICAP 7000
SERIES.