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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。
Ni (C6H12N4) 2SO4 · 4H2O (NSH-HMTA) crystal material was synthesized by partially coordinating the coordination water in the crystal structure of nickel sulfate hexahydrate (NSH) with hexamethylenetetramine (C6H12N4, HMTA) The solubility curve of NSH-HMTA crystal was determined by weighing method. The crystal size of 6 mm × 6 mm × 2 mm was grown by aqueous solution cooling method at a temperature range of 56 ~ 44 ℃ with a growth rate of about 0.5 mm / d. The content of nickel ions in the grown crystal was analyzed by plasma emission spectroscopy, and the X-ray single crystal diffraction was used to verify the crystal structure. The dehydration temperature and decomposition temperature of crystal were measured by TGA and DTA respectively at 93 ℃ and 114 ℃. The UV-Vis spectra of the crystals were measured by UV-visible at 307 nm and redshifted by about 20 nm compared with NSH crystals (287 nm). The coordination between HMTA and Ni2 + increased the energy of 3A2g spectra of Ni2 + 3A2g → 3T1g (P) requires lower energy, resulting in a red shift in the absorption spectrum.