摘要： Nowadays, nano hybrid materials (NHMs) with latent applications have been employed in different fields, particularly for sensor applications. Among NHMs, GO based - upconversion NHMs system is an emerging area for the rapid detection of different hazardous materials either as an aptamer based or free-labeled sensing techniques. For the detection of Pb(II) in water, NaYF4@Yb,Ho,Au/GO-NaYF4@Yb,Ho,Au NHMs system was developed. The synthesized NHMs were characterized by XRD, FT-IR, SEM with EDS, TEM and Raman characterization techniques for observation and confirmation. NaYF4@Yb,Ho,Au/GO-NaYF4@Yb,Ho,Au NHMs fabricated sensors were observed to detect and quantify on real-time basis Pb(II) via surface-enhanced-Raman spectroscopy within the dynamic linear range of 98 – 99%, with detection limits of 1.16 × 10-9 g/mL and 1.15×10-8 g/mL obtained respectively for NaYF4@Yb,Ho,Au and GO- NaYF4@Yb,Ho,Au NHMs.. The relative standard deviation (RSD) value achieved for both were less than ~10%, indicative of reproducibility in the quantification results for Pb(II) traces in water when combined with genetic algorithm partial least square (GA-PLS). Results suggest that the GO-NHMs better enhanced the SERS Pb (II) vis-à-vis NaYF4@Yb,Ho,Au. The GO-wrapped NHMs exhibited a further better SERS performance because the heterostructure of GO-NHMs could be potentially useful for SERS-based immunoassay due to the much easier charge transfer between graphene and the metal ions and molecules so the homogeneity of the SERS probe was improved simultaneously (chemical enhancement) by GO-NHMs.