Research Paper

Journal of Nanoparticle Research

, Volume 13, Issue 1, pp 375-384

Synthesis of nickel nanoparticles in silica by alcogel electrolysis

  • Muhammad Z. RanaAffiliated withDepartment of Chemical and Materials Engineering (DCME), National Centre for Nanotechnology (NCN), Pakistan Institute of Engineering and Applied Sciences (PIEAS)
  • , Mazhar MehmoodAffiliated withDepartment of Chemical and Materials Engineering (DCME), National Centre for Nanotechnology (NCN), Pakistan Institute of Engineering and Applied Sciences (PIEAS) Email author 
  • , Jamil AhmadAffiliated withDepartment of Chemical and Materials Engineering (DCME), National Centre for Nanotechnology (NCN), Pakistan Institute of Engineering and Applied Sciences (PIEAS)
  • , Muhammad AslamAffiliated withDepartment of Chemical and Materials Engineering (DCME), National Centre for Nanotechnology (NCN), Pakistan Institute of Engineering and Applied Sciences (PIEAS)
  • , Syed K. HasanainAffiliated withDepartment of Physics, Quaid-i-Azam University
  • , Sohail HameedAffiliated withNational Institute for Biotechnology and Genetic Engineering

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Abstract

We report a novel technique for the formation of metal nanoparticles, based on electrolysis of the alcogels containing metal chlorides. The alcogel was formed from TEOS, water, ethanol, and nickel chloride, and subjected to galvanostatic electrolysis. This resulted in successful formation of Ni nanoparticles inside the silica gel. Average particle size of FCC Ni lies between 18 and 20 nm. The formation of tetragonal nickel (a sub-oxide of nickel) as well as NiO were also detected by XRD and SAED. The resistivity measurements showed that the nickel nanoparticles were separated from each other by Ni(O) present between them. Magnetic studies based on ZFC and FC measurements below room temperature (up to 5 K) and above room temperature (up to 700 K) were conducted using SQUID and Magnetic TGA, respectively, which showed strong magnetic irreversibility as attributable to exchange interaction between metallic and oxide phases and mutual interactions among metallic particles in the network structure. The blocking temperature (~600 K) of the samples was above room temperature. M–H studies based on VSM showed an increase in magnetic coercivity with the formation of NiO. A magnetic transition associated with tetragonal nickel was seen at 10 K.

Keywords

Sol–gel Alcogel electrolysis Nanoparticles Tetragonal nickel Exchange interaction Synthesis at room temperature Magnetism