异丙醇锆电化学合成研究

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以锆板为阳极,不锈钢板为阴极,异丙醇为溶剂,四乙基溴化铵(Et_4NBr)为电解质,通过电化学的方法合成了异丙醇锆(Zr(O~iPr)_4),阳极电流效率97.05%。使用红外光谱,核磁共振对产品进行表征,证明了产品为异丙醇锆。通过循环伏安,线性极化,计时电流电化学手段探究了扫描速率、电解质浓度、阳极电势对锆阳极电化学行为影响。并用扫描电镜对锆表面的形貌进行了表征。结果表明,在0.05 M四乙基溴化铵异丙醇溶液中,由于钝化膜的存在锆阳极在2 V左右低电势下不存在活性溶解区,当电压增加到2.5 V,锆的溶解是以点蚀的形式开始,其与扫描电镜观测的结果一致。点蚀电位随电解质的浓度增加而降低,随着扫描速率减小而减小。点蚀的开始需要一定的诱导时间、电解质浓度和电势下才能发生。 Zr (O ~ iPr) _4) was synthesized by electrochemical method using zirconium plate as anode, stainless steel as cathode, isopropanol as solvent and tetraethylammonium bromide (Et_4NBr) as electrolyte. Anode current efficiency of 97.05%. The product was characterized by infrared spectroscopy and nuclear magnetic resonance, which proved that the product was zirconium isopropoxide. The effects of scan rate, electrolyte concentration and anode potential on the electrochemical behavior of zirconium anode were investigated by cyclic voltammetry, linear polarization and chronoamperometry. The surface morphology of zirconium was characterized by scanning electron microscopy. The results show that in 0.05 M tetraethylammonium bromide isopropanol solution, there is no active dissolution zone at the low potential of 2 V due to the existence of passivation film. When the voltage is increased to 2.5 V, the dissolution of zirconium is Starting with pitting corrosion, which is consistent with the results of scanning electron microscopy. Pitting potential decreases with increasing electrolyte concentration, decreasing with decreasing scan rate. The beginning of pitting requires a certain induction time, electrolyte concentration and potential to happen.
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