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作 者:高晟民[1,2] 许智煌[1] 叶李旺[1] 苏根博[1] 庄欣欣[1]
机构地区:[1]中国科学院光电材料化学与物理重点实验室,福州350002 [2]中国科学院大学,北京100049
出 处:《人工晶体学报》2015年第8期2070-2073,共4页Journal of Synthetic Crystals
基 金:中国科学院光电材料化学与物理重点实验室资助项目
摘 要:六次甲基四胺(C6H12N4,HMTA)部分取代六水合硫酸镍(NSH)晶体结构中的配位水,合成Ni(C6H12N4)2SO4·4H2O(NSH-HMTA)晶体材料。采用称量法测定了NSH-HMTA晶体的溶解度曲线,应用水溶液降温法在温度区间56~44℃之间生长出6 mm×6 mm×2 mm尺寸的晶体,生长速度约为0.5 mm/d。通过等离子发射光谱分析所生长晶体中镍离子含量,X射线单晶衍射用于验证晶体的结构。采用热重法(TGA)和差热分析法(DTA)测定晶体脱水温度和分解温度分别为93℃、114℃。测量晶体的紫外-可见光谱特性,其紫外波段透过峰位于波长为307 nm处,比NSH晶体(287 nm)红移了约20 nm,HMTA与Ni2+配位提高了Ni2+的3A2g光谱项的能级,3A2g→3T1g(P)所需能量更低,导致吸收谱红移。The new material,Ni( C6H12N4)2SO4·4H2O,was synthesized through HMTA molecules substituting for part coordinated water molecules. The content of Ni2 +was determined by ICP while its structure was acquired through X-ray single crystal diffraction,conforming to molecular formula. The solubility curve of title complex was measured at various temperatures by weighing method and bulk single crystals( 6 mm × 6 mm × 2 mm) were obtained from aqueous solution by falling temperature growth technique due to its solubility being directly proportional to temperature( 56-44 ℃). The dehydration( 93℃) and decomposing( 114 ℃) temperatures were determined by Thermo Gravimetric Analyzer( TGA)and Differential Thermal Analysis. The UV transmission peak was red-shifted about 20 nm due to the improving of3A2 gspectral term for Ni2 +.
关 键 词:Ni(C6H12N4)2SO4·4H2O 降温法 溶解度 光谱性质
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