本文關(guān)鍵詞： Pt納米粒子 雜多酸 氧化石墨烯 金屬氧化物 血清　出處：《東北師范大學》2017年碩士論文　論文類型：學位論文

【摘要】：傳感器具有設備簡單、體型小、操作簡單等特點,其中電化學傳感器具有靈敏度高、高效、可多次循環(huán)利用、特異性好、成本低廉、檢測速度快等優(yōu)勢,因此對于實際樣品檢測具有重要意義。目前電化學傳感器的主要發(fā)展方向是制備新材料的修飾電極,以達到檢測速度更快,更精準,且材料更簡單、環(huán)保、易得等效果。本文采用多種復合納米材料來制備新型修飾電極,利用能量色散X射線譜圖(EDX)、掃描電鏡(SEM)、紅外(IR)、X-射線粉末衍射(XRD)、X射線光電子能譜(XPS)、透射電極(TEM)等手段對合成材料及修飾電極的表面形貌進行了表征。運用循環(huán)伏安法(CV)、計時電流法(I-t)、微分脈沖伏安法(DPV)等多種電化學方法對修飾電極的電催化性能進行研究,并對實際樣品人體血清中多種生物物質(zhì)進行測定。首先,Pt/IMo6/GO-GCE的新型多種納米復合材料修飾電極的制備,并對其電化學催化生物物質(zhì)進行研究。我們通過電沉積法將石墨烯(GO)、Na5[IMo6O24]?3H2O雜多酸和Pt納米自組裝制備新型復合納米材料修飾電極(Pt/IMo6/GO-GCE)。通過SEM、IR等方法對材料及修飾電極表面形貌進行表征,同時利用CV、I-t、DPV電化學方法表征修飾電極的電化學行為。結(jié)果表明:該納米材料修飾電極不僅保持了雜多酸電催化活性,同時增大了修飾電極比表面積。與GCE、GO-GCE和IMo6/GO-GCE相比,Pt/IMo6/GO-GCE顯示出響應速度快、穩(wěn)定性好、導電性強、比表面積大、選擇性好等優(yōu)點。在掃速為100 mv/s,電解質(zhì)溶液為0.05 M稀硫酸溶液中,催化抗壞血酸(AA)、多巴胺(DA)和尿酸(UA)表現(xiàn)出較高的電催化活性。結(jié)果表明,三種物質(zhì)的檢測限分別為3.0μM、0.22μM和0.72μM,其對應線性相關(guān)系數(shù)分別為0.999、0.999和0.998。且證明該納米復合材料修飾電極可用于同時測定實際樣品人體血清中AA、DA和UA的含量。其次,研究了非酶電化學傳感器ZnO-MoO3-C/PDDA-GCE對葡萄糖的催化,利用安培法定量測定葡萄糖的含量,并應用于實際樣品的檢測。通過自組裝法利用納米復合材料制備了修飾電極ZnO-MoO3-C/PDDA-GCE。利用IR、TEM、SEM、XPS、XRD、電化學技術(shù)等多種手段對材料及電極表面形貌進行表征。結(jié)果表明復合納米材料及對應修飾電極均制備成功,且表現(xiàn)出良好的催化效果。在100 mv/s掃速,0.1 M NaOH電解質(zhì)溶液中,修飾電極對葡萄糖表現(xiàn)出良好的電催化活性,與ZnO-C/PDDA-GCE和MoO3-C/PDDA-GCE相比ZnO-MoO3-C/PDDA-GCE靈敏度更高,最低檢測限為1.74μM、靈敏度為69.5μAmM-1cm-2、線性范圍為6-700μM�？傊撔揎楇姌O具有電催化活性強、響穩(wěn)定性好、響應速度快等特點,已成功應用于測定人體血清中的葡萄糖含量。
[Abstract]:The sensor has the advantages of simple equipment, small size and simple operation, among which the electrochemical sensor has the advantages of high sensitivity, high efficiency, multiple recycling, good specificity, low cost, fast detection speed and so on. At present, the main development direction of electrochemical sensor is the preparation of new materials modified electrode, in order to achieve faster detection, more accurate, more simple materials, environmental protection. In this paper, a new type of modified electrode was prepared by using a variety of composite nanomaterials. Energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM) and IR (IR) were used to prepare the modified electrode. X ray powder diffractometer XRDX X ray photoelectron spectroscopy (XPS). The surface morphology of the composite and modified electrode was characterized by means of transmission electrode (TEM), cyclic voltammetry (CV) and chronoamperometric method (I-t). Various electrochemical methods such as differential pulse voltammetry (DPVV) were used to study the electrocatalytic properties of the modified electrode and to determine a variety of biomaterials in human serum. The preparation and electrochemical catalytic biomaterials of Pt/IMo6/GO-GCE modified electrode were studied. [IMo6O24]? Preparation of a novel composite nano-material modified electrode PtP / IMo6 / GO-GCEC by self-assembly of 3H2O heteropoly acid and Pt nanocrystalline via SEM. The surface morphology of the modified electrode and the material were characterized by IR and CVFI-t. The electrochemical behavior of the modified electrode was characterized by DPV. The results showed that the modified electrode not only kept the heteropoly acid electrocatalytic activity, but also increased the specific surface area of the modified electrode and GCE. Compared with IMo6/GO-GCE, GO-GCE / IMo6 / GO-GCE shows fast response, good stability, strong conductivity and large specific surface area. The catalytic activity of ascorbic acid (AAA) was obtained in the presence of 100 MV / s sweep speed and 0.05 M dilute sulfuric acid solution. The results showed that the detection limits of the three compounds were 3.0 渭 M 0.22 渭 M and 0.72 渭 M, respectively. The linear correlation coefficients were 0.999 and 0.998.It was proved that the modified electrode could be used for simultaneous determination of AA in human serum. The content of DA and UA. Secondly, the non-enzymatic electrochemical sensor ZnO-MoO3-C/PDDA-GCE was used to catalyze glucose, and the content of glucose was determined by amperometric method. The modified electrode ZnO-MoO3-C / PDDA-GCEwas prepared by self-assembly method, and the modified electrode ZnO-MoO3-C / PDDA-GCEand XPS was used to prepare ZnO-MoO3-C / PDDA-GCE. The surface morphology of materials and electrodes were characterized by XRD and electrochemical techniques. The results showed that the composite nanomaterials and the corresponding modified electrodes were successfully prepared. The modified electrode showed good electrocatalytic activity for glucose in the electrolyte solution of 100 mv/s sweep speed of 0. 1 M NaOH. Compared with ZnO-C/PDDA-GCE and MoO3-C/PDDA-GCE, ZnO-MoO3-C/PDDA-GCE is more sensitive. The lowest detection limit is 1.74 渭 m, the sensitivity is 69.5 渭 AmM-1cm-2, and the linear range is 6-700 渭 M. in short, the modified electrode has strong electrocatalytic activity and good response stability. It has been successfully applied to the determination of glucose in human serum.
【學位授予單位】：東北師范大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TB33;TP212.3

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相關(guān)期刊論文 前1條

1 唐波,葛介超,王春先,張國英,吳長舉,舒春英;金屬氧化物納米材料的制備新進展[J];化工進展;2002年10期

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本文編號：1463399