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X-ray diffraction and DSC analysis
To gain an insight into the PFC behaviour of FLA-Cn solids, powder wide-angle X-ray diffraction (PXD) and differential scanning calorimetry (DSC) experiments were conducted on the ground and pristine solids. The PXD patterns of pristine FLA-C3 and FLA-C5 solids show sharp and intense reflections, indicative of their well-ordered microcrystalline structures (Fig. 6a). In contrast, the ground samples display broad and featureless diffractograms reflecting notable amorphous features. This
indicates that grinding has induced the phase transition of FLACn solids between crystalline and amorphous states, which should be responsible for the PFC behaviour of FLA-Cn solids. The formation of amorphous state upon grinding was also confirmed by DSC experiments. As shown in Fig. 6b, no additional thermal transitions could be detected for all pristine solids before the isotropic melt transition (Tm); however, there is clearly one exothermic transition peak at the lower-temperature region for ground FLA-C3 and FLA-C5 solids. This broad exothermic peak (Tc) is ascribed to the cold-crystallization of amorphized FLA-Cn solids upon heating. Amorphized FLA-C3 and FLA-C5 solids have high Tc values, which result in their stable PFC behaviour at room temperature. It is known that the Tc is obviously lower than the Tm of a compound, and the ground FLA-C12 solid could cold-crystallize at or below room temperature since its isotropic melt point is only about 65 C. Thus, the amorphized FLA-C12 solid induced by grinding is in a thermodynamically and dynamically unstable morphology. This is reason why ground FLA-C12 solid exhibits spontaneously recovering fluorescence properties at room temperature.

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1樓 2014-10-21 09:42:56

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yhc0316: 金幣+40, 翻譯EPI+1 2014-10-21 18:22:14

X射線衍射和DSC分析
為深入了解FLA-Cn固體的PFC性能，用粉末廣角X射線衍射（PXD）和差示掃描量熱（DSC）對研磨和原始固體進(jìn)行了實(shí)驗(yàn)。FLA-C3和FLA-C5固體的PXD圖譜呈尖銳和強(qiáng)烈的反射，表明他們?yōu)橹刃蚓坏奈⒕ЫY(jié)構(gòu)（圖6a）。與此相反，研磨樣品呈寬和無特征的衍射圖譜，顯示其非晶狀態(tài)特征。這表明研磨引起了FLACn固體晶態(tài)和非晶態(tài)之間轉(zhuǎn)換，這應(yīng)該是FLA-Cn固體PFC性能的原因。研磨時(shí)引起非晶狀態(tài)形成也由DSC實(shí)驗(yàn)證實(shí)。如圖6b所示，原始固體在等向性熔體轉(zhuǎn)變（Tm）前沒有熱轉(zhuǎn)變; 而研磨FLA-C3和FLA-C5固體在較低溫度區(qū)域有一清楚的放熱轉(zhuǎn)變峰。這種廣泛的放熱峰（TC）是由于非晶FLA-Cn固體在加熱時(shí)發(fā)生的冷結(jié)晶所致。非晶化FLA-C3和FLA-C5固體具有高Tc值，導(dǎo)致其在室溫下具有穩(wěn)定的PFC性能�；衔锏腡c值明顯低于Tm值，研磨FLA-C12固體在室溫或低于室溫時(shí)可冷結(jié)晶，因?yàn)樗牡认蛐匀埸c(diǎn)約僅為65℃。因此，研磨誘導(dǎo)的FLA-C12固體非晶化在熱力學(xué)和動態(tài)學(xué)上是一種不穩(wěn)定形態(tài)。這就是為什么研磨FLA-C12固體在室溫下具有自發(fā)恢復(fù)熒光的性能。

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2樓2014-10-21 10:50:21

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