基于可逆脱嵌材料的碱金属离子选择性电极

发布时间：2018-04-03 11:39

  本文选题：可逆脱嵌材料　切入点：离子选择性电极　出处：《华北理工大学》2016年硕士论文

【摘要】：碳糊型离子选择性电极具有容易制备、价格低廉、电极表面易于更新、响应稳定等优点,其中活性材料的选择对离子选择性电极的响应性能至关重要。着重于合成不同的可逆脱嵌材料,并以其作为活性材料制备柱状碳糊型离子选择性电极。通过XRD和SEM对材料的物相组成和微观形貌进行表征,采用不同的电化学方法对电极的响应性能、稳定性、重现性和检测限进行测试。研究了不同原料配比、修饰剂、离子掺杂对电极响应性能的影响。1)以水热法合成的MnO_2为原料采用高温固相法制备LiMn_2O_4,以其作为活性材料制备柱状碳糊型锂离子选择性电极。实验结果表明,该电极对锂离子具有良好的响应,当乙炔黑、液体石蜡、LiMn_2O_4的质量比为5:3:2时电极的响应性能最好,电极的灵敏度为67.0mV/dec.,检测下限为5.16×10-6mol/L。但是由于了JahnTeller效应的影响,出现了电位漂移现象。2)以聚3,4-乙撑二氧噻吩(PEDOT)作为修饰剂,对锰酸锂碳糊电极进行修饰改性。当PEDOT含量为锰酸锂含量的2wt%时,通过将PEDOT与锰酸锂碳糊进行直接混合的方式制备出的电极对锂离子呈现出能斯特响应,电极的灵敏度为59±2mV/dec.,具有良好的稳定性,电极的检测下限也有所下降。3)以碳热还原法制备了磷酸钒锂和掺杂Mg、Cu的Li_3V_(1.8)Mg_(0.3)(PO_4)_3和Li_3V_(1.8)Cu_(0.3)(PO_4)_3,以磷酸钒锂为活性材料的选择性电极对锂离子呈现出能斯特响应,以Li_3V_(1.8)Mg_(0.3)(PO_4)_3和Li_3V_(1.8)Cu_(0.3)(PO_4)_3为活性材料制作的电极对锂离子也具有良好的响应。4)通过碳热还原法制备了磷酸钒钠,制备了以磷酸钒钠为活性材料的钠离子选择性电极。当电极组分为最佳配比时,电极的响应斜率为50.8mV/dec.,电极的检测限为8.32×10-5mol/L。以上基于可逆脱嵌材料的碱金属选择性电极均具有良好的响应能力和抗干扰能力,由此可以说明可逆脱嵌材料具有巨大的应用价值和潜在的市场。
[Abstract]:Carbon paste ion-selective electrode has the advantages of easy preparation, low cost, easy updating of electrode surface and stable response, among which the selection of active materials is very important to the response performance of ion-selective electrode.Different reversible descalation materials were synthesized and used as active materials to prepare columnar carbon paste ion-selective electrode.The phase composition and micromorphology of the materials were characterized by XRD and SEM. The response, stability, reproducibility and detection limit of the electrode were measured by different electrochemical methods.The effect of different raw material ratio, modifier and ion doping on the electrode response was studied. (1) LiMnStat _ 2O _ 4 was prepared by high temperature solid state method from MnO_2 synthesized by hydrothermal method, and the columnar carbon-paste type lithium ion selective electrode was prepared by using it as active material.The experimental results show that the electrode has a good response to lithium ion. When the mass ratio of acetylene black and paraffin wax limn _ 2O _ 4 is 5:3:2, the electrode has the best response performance, the sensitivity of the electrode is 67.0 MV / dec.and the detection limit is 5.16 脳 10 ~ (-6) mol / L.However, due to the effect of JahnTeller effect, the phenomenon of potential shift appeared. 2) the modified lithium manganate carbon paste electrode was modified with poly (3h4- ethylenedioxythiophene) as the modifier.When the content of PEDOT is 2 wt% of lithium manganese oxide, the electrode prepared by direct mixing of PEDOT and lithium manganese oxide carbon paste shows a Nernst response to lithium ion. The sensitivity of the electrode is 59 卤2 MV / dec.It has good stability.鐢垫瀬鐨勬��娴嬩笅闄愪篃鏈夋墍涓嬮檷.3)浠ョ⒊鐑�杩樺師娉曞埗澶囦簡纾烽吀閽掗攤鍜屾幒鏉侻g,Cu鐨凩i_3V_(1.8)Mg_(0.3)(PO_4)_3鍜孡i_3V_(1.8)Cu_(0.3)(PO_4)_3,浠ョ７閰搁拻閿備负娲绘，

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