Nanocomposites (nanocrystals) of KY(WO4)2 and KY(WO4)2+1% mol Yb were synthesized using a Complex Sol-Gel Process (CSGP). A chemical treatment with concentrated nitric acid and hydrogen peroxide was used to reduce the decarbonisation temperature. The expected monoclinic phase C2/c of the KYW of the nanocomposite powder was confirmed using XDR. From the X-ray diffraction measurements, the unit cell parameters and the size of nanoparticles was determined. Electron spin resonance studies in the X band were carried out on KYW and KYW:Yb nanocrystals. The sintered samples were made with using the high pressure technique at temperatures up to 600oC. In addition chemical analysis, X-ray diffraction measurements and ESR investigations were carried out on the sintered samples.