The synthesis of new seed mediated AgNi allied bimetallic nanocomposites was successfully carried out by the successive reduction of the metal ions in diethylene glycol, ethylene glycol, glycerol, and pentaerythritol solutions, with concomitant precipitation of Ag/Ni bimetal sols. The optical measurement revealed the existence of distinct band edge with surface plasmon resonance (SPR) in the region of 400–425？nm and excitonic emission with maximum peak at 382？nm which were reminiscent of cluster-in-cluster surface enriched bimetallic silver-nickel sols. The morphological characterization by transmission electron microscopy, high resolution transmission electron microscopy, and X-ray diffraction analyses complimented by surface scan using X-ray photoelectron spectroscopy strongly supported the formation of intimately alloyed face-centered silver/nickel nanoclusters. 1. Introduction The synthesis of new materials and the investigation of their characteristic properties is a noble aspect of nanochemistry due to the fact that various applications have been found for these materials in electronics, sensor, optical devices, waveguide, and fibre optics to mention a few. As a result, immense effort directed at synthesizing and manipulating the size, size distribution, and shape of these nanoparticles is inexhaustive. In particular, silver nanoparticles have been largely prepared and evaluated for sensor, optical, and antimicrobial properties. However, the nanocomposite silver nickel is being considered due to its synergistic effect which offers a wide range of applications that include catalysis. Monodispersed allied silver/nickel nanoparticles have been prepared using various chemical routes based on hydrolytic reduction of the metal ions followed by polycondensation of the reduced nuclei. The reactions are largely thermodynamically driven with respect to temperature and time to produce uniformly distributed nanosized particles. There are a number of literature reports on AgNi nanoparticles; Xiao and coworkers presented an approach in which laser ablation was used in the deposition silver/nickel bimetallic nanoparticles; the laser was a pulsed Nd:YAG laser source [1, 2]. The effective nonlinear absorption of Ni/Ag nanoparticles was found to be higher than that of pristine Ag nanoparticles. The nanoparticles were synthesized via wet chemical reduction in C19H42BrN (CTAB) matrix, hydrazine hydrate being the reducing agent, and it was found to be a very potent material for optical limiting and photonic applications in the work of Kishore et al., 2012 [3].
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