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CHEM01200604004 Shri Sanyasinaidu Boddu - Homi Bhabha ...

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eaction, the precipitate was collected by centrifugation and then washed two times with<br />

acetone and three times with ethyl alcohol followed by drying under ambient conditions.<br />

Samples obtained by above method were dispersible in water and methanol. Same procedure<br />

was also employed for making SbPO 4 samples containing 1 and 2.5 at % Tb 3+ ions (denoted<br />

as SbPO 4 :Tb 3+ (1%) and SbPO 4 :Tb 3+ (2.5%)). For preparing Tb 3+ , Ce 3+ co-doped samples<br />

same procedure was used except that, 0.01 g of Tb 4 O 7 (5 at %) and 0.012 g (2.5 at %) of<br />

Ce(NO 3 ) 3 .6H 2 O were used respectively along with 0.5 g of SbCl 3 (sample is denoted as<br />

SbPO 4 :Ce 3+ (2.5 at %), Tb 3+ (5 at %)).<br />

Preparation of SbPO 4 :Ce 3+ (2.5 at %), Tb 3+ (5 at %) nanomaterials dispersed in silica:<br />

For the preparation of SbPO 4 : Ce 3+ (2.5 at %), Tb 3+ (5 at %) nanomaterials dispersed in silica<br />

(represented as SbPO 4 : Ce 3+ (2.5 at %), Tb 3+ (5 at %)-SiO 2 ), SbCl 3 (0.5 g), Tb 4 O 7 (0.01 g) and<br />

Ce(NO 3 ) 3 .6H 2 O (0.012 g) were dissolved in con. HCl and excess acid was evaporated by<br />

adding distilled water drop wise. To this solution, ethylene glycol (12 ml) and glycerol (8 ml)<br />

were added and it was transferred into a two-necked 100 ml RB flask. The solution was<br />

slowly heated upto 70°C while stirring followed by addition of ammonium dihydrogen<br />

phosphate (0.75 g). Temperature was raised to 120°C resulting in the formation of a turbid<br />

solution. After 10 min, 0.7 ml of tetraethyl orthosilicate (TEOS) was added to this. It was<br />

then refluxed for 2 hours at 120°C. The precipitate was centrifuged, washed with ethanol and<br />

acetone.<br />

Synthesis of undoped and lanthanide doped BiPO 4 nanomaterials: For preparation of<br />

undoped BiPO 4 and lanthanide ions (Tb 3+ , Eu 3+ , Dy 3+ , Sm 3+ ) doped BiPO 4 nanomaterials,<br />

Bi(NO 3 ) 3 .5H 2 O, Tb 4 O 7 , Eu 2 O 3 , Dy 2 (CO 3 ) 3 .xH 2 O, Sm 2 O 3 were used as starting materials. For<br />

the synthesis of Eu 3+ doped BiPO 4 , Bi(NO 3 ) 3 .5H 2 O (1.0 g) and Eu 2 O 3 (0.011 g)(2.5 at %)<br />

were dissolved in concentrated HCl in a beaker and the excess acid was evaporated out<br />

repeatedly by adding water. To this solution, 20 ml of ethylene glycol was added and it was<br />

34

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