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Chapter IV Thermal Studies of …..<br />

structure at room temperature. The observed change of symmetry of the<br />

crystal suggested a phase transition like phenomenon called HTPT at<br />

characteristic temperature Tp = 430 K. The observed weight loss from TG<br />

curve suggested that Tp marked the onset of partial polymerization taking<br />

place on the surface of the sample such that the phase above 430 K was a<br />

mixed phase consisting of tetragonal ADP in the bulk of the sample and<br />

ammonium polyphosphates (NH4)2H2P2O7 at the surface of the crystal.<br />

Several other authors studied thermogravimetry of pure KDP crystals<br />

[12, 13] and various doped KDP crystals [14-17]. It has been found that<br />

glycine doped KDP crystals starts decomposing at 204.93 o C and KDP<br />

crystal at 207.91 o C [16] this also further supports that amino acid doping<br />

slightly increases thermal destability and reduces the phase transition<br />

temperature.<br />

Moreover, thermal studies on amino acids (L-glutamic acid, L-histidine<br />

and L-valine) doped KDP crystals are reported by Kumaresan [17] using TGA<br />

and DTA. The author [17] observed that L-glutamic acid doped KDP melted at<br />

a 125 o C and undergone irreversible endothermic transition around 210 o C<br />

followed by another endothermic transition around 290-675 o C. The TGA<br />

exhibited a weight loss of about 13 % in the temperature range 190-350 o C<br />

due to liberation of volatile substances. However, the prolonged heating up to<br />

900 o C did not produce any endothermic peaks in the DTA curve and TGA<br />

exhibited a total weight loss of nearly 13 % at 900 o C. Interestingly, the DTA<br />

curve of L-histidine doped KDP revealed two more events at 560 o C and 798<br />

o C reported which did not accompany by weight loss. It has been argued that<br />

this might be due to high temperature phase transition of KDP. Apart from<br />

166

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