本文選題：可逆脫嵌材料　切入點(diǎn)：離子選擇性電極　出處：《華北理工大學(xué)》2016年碩士論文

【摘要】：碳糊型離子選擇性電極具有容易制備、價(jià)格低廉、電極表面易于更新、響應(yīng)穩(wěn)定等優(yōu)點(diǎn),其中活性材料的選擇對離子選擇性電極的響應(yīng)性能至關(guān)重要。著重于合成不同的可逆脫嵌材料,并以其作為活性材料制備柱狀碳糊型離子選擇性電極。通過XRD和SEM對材料的物相組成和微觀形貌進(jìn)行表征,采用不同的電化學(xué)方法對電極的響應(yīng)性能、穩(wěn)定性、重現(xiàn)性和檢測限進(jìn)行測試。研究了不同原料配比、修飾劑、離子摻雜對電極響應(yīng)性能的影響。1)以水熱法合成的MnO_2為原料采用高溫固相法制備LiMn_2O_4,以其作為活性材料制備柱狀碳糊型鋰離子選擇性電極。實(shí)驗(yàn)結(jié)果表明,該電極對鋰離子具有良好的響應(yīng),當(dāng)乙炔黑、液體石蠟、LiMn_2O_4的質(zhì)量比為5:3:2時(shí)電極的響應(yīng)性能最好,電極的靈敏度為67.0mV/dec.,檢測下限為5.16×10-6mol/L。但是由于了JahnTeller效應(yīng)的影響,出現(xiàn)了電位漂移現(xiàn)象。2)以聚3,4-乙撐二氧噻吩(PEDOT)作為修飾劑,對錳酸鋰碳糊電極進(jìn)行修飾改性。當(dāng)PEDOT含量為錳酸鋰含量的2wt%時(shí),通過將PEDOT與錳酸鋰碳糊進(jìn)行直接混合的方式制備出的電極對鋰離子呈現(xiàn)出能斯特響應(yīng),電極的靈敏度為59±2mV/dec.,具有良好的穩(wěn)定性,電極的檢測下限也有所下降。3)以碳熱還原法制備了磷酸釩鋰和摻雜Mg、Cu的Li_3V_(1.8)Mg_(0.3)(PO_4)_3和Li_3V_(1.8)Cu_(0.3)(PO_4)_3,以磷酸釩鋰為活性材料的選擇性電極對鋰離子呈現(xiàn)出能斯特響應(yīng),以Li_3V_(1.8)Mg_(0.3)(PO_4)_3和Li_3V_(1.8)Cu_(0.3)(PO_4)_3為活性材料制作的電極對鋰離子也具有良好的響應(yīng)。4)通過碳熱還原法制備了磷酸釩鈉,制備了以磷酸釩鈉為活性材料的鈉離子選擇性電極。當(dāng)電極組分為最佳配比時(shí),電極的響應(yīng)斜率為50.8mV/dec.,電極的檢測限為8.32×10-5mol/L。以上基于可逆脫嵌材料的堿金屬選擇性電極均具有良好的響應(yīng)能力和抗干擾能力,由此可以說明可逆脫嵌材料具有巨大的應(yīng)用價(jià)值和潛在的市場。
[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 鹵2 MV / dec.It has good stability.鐢墊瀬鐨勬嫻嬩笅闄愪篃鏈夋墍涓嬮檷.3)浠ョ⒊鐑繕鍘熸硶鍒跺浜嗙７閰擱拻閿傚拰鎺烘潅Mg,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閰擱拻閿備負(fù)媧繪，

本文編號(hào)：1705053