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CHEM01200604004 Shri Sanyasinaidu Boddu - Homi Bhabha ...

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transferred into a two-necked RB flask. An aqueous solution (3 ml) of ammonium<br />

dihydrogen phosphate (0.3 g) was added with stirring. The solution was heated at different<br />

temperatures viz. 75, 100, 125 and 185°C for two hours. The precipitate obtained was washed<br />

with methanol and acetone to remove unreacted species and dried under ambient conditions.<br />

The same procedure was followed for the synthesis of other lanthanide ions doped samples.<br />

2.5 Synthesis of gallate nanomaterials:<br />

Synthesis of undoped, In 3+ and Ln 3+ doped ZnGa 2 O 4 nanoparticles: For the preparation<br />

of ZnGa 2 O 4 nanoparticles gallium metal and Zinc acetate were used as starting materials.<br />

Gallium metal (0.2 g) was dissolved in concentrated HCl containing few drops of HNO 3 in a<br />

beaker and the excess acid was removed by repeated evaporation by adding water. This<br />

solution was transferred into a two-necked RB flask, containing appropriate amount of zinc<br />

acetate. Ethylene glycol (25 ml) and distilled water (10 ml) were added to this mixture. The<br />

solution was slowly heated up to 100°C followed by the addition of urea (3.0 g). It was<br />

heated at 120°C whereupon turbidity appeared. Temperature of the reaction was maintained<br />

for 2 hours to complete the reaction. The precipitate was collected by centrifugation and then<br />

washed three times with ethyl alcohol and two times with acetone followed by drying under<br />

ambient conditions. This process was repeated for different ratios of solvent to precursor<br />

concentration as well as ethylene glycol to water. For In 3+ , Eu 3+ and Tb 3+ doped samples<br />

same procedure was followed except addition of appropriate amounts of InCl 3 , Eu 2 O 3 and<br />

Tb 4 O 7 was carried out while dissolving gallium metal in concentrated HCl.<br />

Preparation of In 3+ doped ZnGa 2 O 4 nanoparticles incorporated PMMA matrix: For<br />

incorporating nanoparticles in polymer, the procedure reported by Gonsalves, et al. [115] was<br />

employed. The method is described below. Around 50 mg of ZnGa 2 O 4 nanoparticles was<br />

dispersed in one ml of methyl methacrylate (MMA) by sonicating for one hour under argon<br />

atmosphere. Around 5 mg of azobisisobutyronitrile (AIBN) was added to this mixture and<br />

35

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