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A series of highly dispersed Ho2O3–Yb2O3/SiO2 nanocomposites was synthesized using a liquid-phase method and examined using Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), nitrogen adsorption–desorption, transmission electron microscopy (TEM), Scanning Electron Microscopy (SEM), and photon correlation spectroscopy (PCS). X-ray fluorescence spectrometry (XRF) confirmed a similar amount of weight percentage of Ho, Yb and Si oxides in the prepared samples. Samples HoYbSi1 (Ho2O3:Yb2O3:SiO2 = 0.5:10:89.5, wt. %), HoYbSi2 (Ho2O3:Yb2O3:SiO2 = 1:10:89, wt. %) and HoYbSi3 (Ho2O3:Yb2O3:SiO2 = 2:10:88, wt. %) calcined at 550 °C are amorphous. TEM and SEM analysis confirm a sphere-like morphology with a quite homogeneous size and shape. As compared with the initial silica, the agglomerated particles of nanocomposites in the aqueous medium are in the range from 200 to 850 nm according to PCS data. The effect of anionic polyacrylic acid (PAA) adsorption on fumed silica (SiO2) and Ho2O3–Yb2O3/SiO2 nanocomposite surfaces on suspension stability was studied. The turbidymetry method was used to monitor the initial silica and triple nanooxides suspensions stability as a function of time. [ABSTRACT FROM AUTHOR]