CuKα radiation was obtained from a copper X-ray tube operated at 40 kV and 40 mA. Data were collected with
an angular step of 0.02° at 900 s/frame AZD1208 in vitro per step. FULLPROF software based on the Rietveld method was used to refine the unit cell parameters [22, 23]. The particle size was estimated using Scherrer’s equation and assuming spherical particles [24]. The chemical composition of the nanocrystals was examined by electron probe microanalysis (EPMA) in a Cameca SX50 (Gennevilliers Cedex, France) microprobe analyzer operating in wavelength-dispersive mode. The contents of erbium, ytterbium, and lutetium were measured using Lα and LiF as analyzing crystals. A FEI QUANTA 600 (Hillsboro, OR, USA) environmental scanning electronic microscope (ESEM) and a JEOL JEM-1011 transmission electron microscope (TEM) with MegaView III (Soft Imaging System, Olympus, Tokyo, Japan) were used to study particle homogeneity, morphology, and size dispersion. To examine the samples by TEM, the nanocrystals were dispersed in acetone. Ultrasonication was used to reduce and disperse the agglomerates. They were then drop-cast onto a copper grid covered by a porous
carbon film. Cathodoluminescence (CL) experiments were performed at room temperature using Gatan MonoCL3+ selleck screening library system attached on Schottky-type field-emission scanning electron microscope (S4300SE Hitachi, Tokyo, Japan). The CL signal was dispersed by a 1,200-lines/mm grating blazed
Phosphoglycerate kinase at 500 nm, and CL spectra and images were recorded using a Peltier-cooled Hamamatsu R943-02 photomultipler tube. Results and discussion Structural characterization The chemical composition of the synthesized nanocrystals measured by EPMA was Lu0.990Er0.520Yb0.490O3. The crystalline phase and unit cell parameters of the (Er,Yb):Lu2O3 nanocrystals are cubic with space group and are reported in Table 1. FULLPROF software was used to refine the (Er,Yb):Lu2O3 nanocrystals and thus determine their lattice parameters (Table 1). As expected, the unit cell parameters increased by the introduction of Er3+ and Yb3+ to the matrix (erbium and ytterbium ions are larger than lutetium ion: ionic radii, Lu3+, cn = 6, 0.861 Å; ionic radii, Er3+, cn = 6, 0.890 Å; ionic radii, Yb3+, cn = 6, 0.868 Å [25]). In addition, Scherrer’s equation was used to estimate a particle size of about 14.9 nm. Table 1 Unit cell parameters of (Er,Yb):Lu 2 O 3 nanocrystals and of undoped Lu 2 O 3 , Er 2 O 3 , and Yb 2 O 3 as reference Stoichiometric formulaa Active ion (at.%) a (Å) V (Å3) Particle size (nm)b Er Yb Lu2O3 c 10.39 1,121.62 Lu0.990 Er0.520 Yb0.490O3 25 25 10.4417 (4) 1,138.45(8) 14.9 Er2O3 d 10.54800 1,173.57 Yb2O3 e 10.43470 1,136.16 aMeasured by EPMA; bcalculated using Scherrer’s equation; cJCPDS Lu2O3 (43–1021); dJCPDS Er2O3 (43–1007); eJCPDS Yb2O3 (41–1106).