基于镍复合材料的无酶电化学传感器研究
发布时间：2018-07-17 20:46
【摘要】：镍及氧化镍具有稳定的物化性能、很好的生物相容性、良好的电催化性能,被广泛用于无酶电化学传感器。然而纯镍及其氧化物存在一定缺陷,导致其在无酶电化学传感器的应用上受到了一定的限制。本论文通过镍及其氧化物结合其它材料的掺杂制备出基于镍的复合材料,从而提高了镍基复合材料的电催化活性,并构建新型无酶电化学传感器。本论文主要研究内容如下:(1)碳-氮/氧化镍复合材料(C-N/Ni O)的制备及双氧水(H_2O_2)无酶电化学传感器的构建。首先通过溶剂热法制备氧化镍微球(Ni O),然后氧化镍微球与二嵌段共聚物(PHEMA_(200)-b-PDMAEMA_(100))混合物在高温下煅烧,得到C-N/Ni O复合材料。通过扫描电镜(SEM)、X射线衍射(XRD)、循环伏安(CV)、安培计时(i-t)等方法对其形貌结构和电催化性能进行了表征。实验结果发现C-N/Ni O复合材料具有较高的比表面积,对H_2O_2具有良好的电催化性能:响应时间快(3 s)、反应灵敏度高(322μA·m M~(-1)·cm~(-2))、检出限低(0.042μM)。因此C-N/Ni O复合材料对医药、环境和食品中的H_2O_2的检测具有实际的应用价值。(2)银(Ag)掺杂氧化镍空心球(Ni O HS)复合材料(Ag/Ni O HS)的制备及葡萄糖无酶电化学传感器的构建。首先通过水热法合成Ni O HS,然后以种子诱导生长法将Ag掺杂到Ni O HS得到Ag/Ni O HS;并通过SEM、XRD、CV等方法对其结构和电催化性能进行了表征。结果表明,在Ag和Ni O HS的协同作用下,Ag/Ni O HS修饰玻碳电极对葡萄糖表现出良好的电催化性能,比如具有超高的灵敏度(2300μA·m M~(-1)·cm~(-2))、较低的检出限(0.007μM)和较宽的线性范围等特点,此外该复合材料修饰的玻碳电极对尿酸和丙烯酸存在优异抗干扰能力,因此,Ag/Ni O HS复合材料在无酶葡萄糖传感器领域具有一定的应用潜力。(3)镍掺杂石墨相氮化碳(g-C_3N_4)复合材料(Ni/g-C_3N_4)的制备及双酚A(BPA)无酶电化学传感器的构建。首先通过煅烧三聚氰胺和氯化镍(Ni Cl_2·6H_2O)的混合物制备出Ni/g-C_3N_4;并通过SEM、XRD、红外(IR)、交流阻抗(EIS)、差分脉冲伏安法(DPV)等方法对其形貌结构和电催化性能进行了表征。结果发现Ni/g-C_3N_4复合材料组装的传感器对BPA具有良好的电催化性能:检测线性范围为0.01μM-1μM和1μM-100μM,检出限为4.34 n M(信噪比为3),因此,Ni/g-C_3N_4复合材料对于BPA的检测具有一定的实际应用价值。
[Abstract]:Nickel and nickel oxide have been widely used in enzymatic electrochemical sensors because of their stable physical and chemical properties, good biocompatibility and good electrocatalytic performance. However, pure nickel and its oxides are limited in the application of enzymatic electrochemical sensors. In this paper, nickel based composites were prepared by doping nickel and its oxides with other materials, thus the electrocatalytic activity of nickel matrix composites was improved, and a new enzyme free electrochemical sensor was constructed. The main contents of this thesis are as follows: (1) preparation of C-N / Ni _ 2O _ 2 composite and construction of H _ S _ 2O _ 2 enzyme free electrochemical sensor. Nickel oxide microspheres (nio) were prepared by solvothermal method. Then the mixture of nickel oxide microspheres and diblock copolymers (PHEMA200 -b-PDMAEMA100) was calcined at high temperature to obtain C-N- / NiO composites. Scanning electron microscopy (SEM) X-ray diffraction (XRD), cyclic voltammetry (CV) and ammeter time (i-t) were used to characterize their morphology and electrocatalytic properties. The experimental results show that C-N / Ni / Ni O composite has high specific surface area and has good electrocatalytic performance for H _ S _ 2O _ 2: fast response time (3 渭 A m M ~ (-1) cm ~ (-1),) high sensitivity (3 渭 A m M ~ (-1) cm ~ (-2),) and low detection limit (0.042 渭 M). Therefore, C-N / Ni / Ni O composite has practical application value for the detection of H _ s _ 2O _ 2 in medicine, environment and food. (2) preparation of silver (Ag) doped nickel oxide hollow ball (Ag-N- / nio HS) composite and construction of glucose enzyme free electrochemical sensor. First, Ni O HSS was synthesized by hydrothermal method, then Ag was doped into Ni O HS by seed induced growth method to obtain Ag / Ni O HS.The structure and electrocatalytic properties of Ag / Ni O HSS were characterized by SEMX XRDCV and other methods. The results show that the electrode modified with Ag / NiO-HS has good electrocatalytic performance for glucose, such as high sensitivity (2300 渭 A m M-1) cm-2), low detection limit (0.007 渭 M) and wide linear range, and so on. The results show that the electrode modified with Ag / NiOHS has good electrocatalytic activity for glucose, for example, high sensitivity (2300 渭 A m ~ (-1) cm ~ (-1) cm ~ (-2), low detection limit (0.007 渭 M) and wide linear range, etc. In addition, the composite modified glassy carbon electrode has excellent anti-interference ability to uric acid and acrylic acid. Therefore, the Ag-Ni-O-HS composite has some potential applications in the field of non-enzymatic glucose sensors. (3) the preparation of Ni-doped graphite-phase carbon nitride (g-C3N4) composite (Nirg-C3N4) and the construction of bisphenol A (BPA) non-enzymatic electrochemical sensor. Ni- / g-C _ 3N _ 4 was prepared by calcining the mixture of melamine and nickel chloride (NiCl _ 2H _ 2O), and its morphology and electrocatalytic properties were characterized by means of SEMG-XRD, IR, EIS and DPV. The results show that the sensors assembled by the Ni- / g-C3Nder4 composite have good electrocatalytic performance for BPA. The detection linear ranges are 0.01 渭 M-1 渭 M and 1 渭 M-100 渭 M, and the detection limit is 4.34nM (SNR 3). Therefore, Nirg-C3Nstud composite has a certain practical application value for the detection of BPA.
【学位授予单位】：湘潭大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB33;O657.1
[Abstract]:Nickel and nickel oxide have been widely used in enzymatic electrochemical sensors because of their stable physical and chemical properties, good biocompatibility and good electrocatalytic performance. However, pure nickel and its oxides are limited in the application of enzymatic electrochemical sensors. In this paper, nickel based composites were prepared by doping nickel and its oxides with other materials, thus the electrocatalytic activity of nickel matrix composites was improved, and a new enzyme free electrochemical sensor was constructed. The main contents of this thesis are as follows: (1) preparation of C-N / Ni _ 2O _ 2 composite and construction of H _ S _ 2O _ 2 enzyme free electrochemical sensor. Nickel oxide microspheres (nio) were prepared by solvothermal method. Then the mixture of nickel oxide microspheres and diblock copolymers (PHEMA200 -b-PDMAEMA100) was calcined at high temperature to obtain C-N- / NiO composites. Scanning electron microscopy (SEM) X-ray diffraction (XRD), cyclic voltammetry (CV) and ammeter time (i-t) were used to characterize their morphology and electrocatalytic properties. The experimental results show that C-N / Ni / Ni O composite has high specific surface area and has good electrocatalytic performance for H _ S _ 2O _ 2: fast response time (3 渭 A m M ~ (-1) cm ~ (-1),) high sensitivity (3 渭 A m M ~ (-1) cm ~ (-2),) and low detection limit (0.042 渭 M). Therefore, C-N / Ni / Ni O composite has practical application value for the detection of H _ s _ 2O _ 2 in medicine, environment and food. (2) preparation of silver (Ag) doped nickel oxide hollow ball (Ag-N- / nio HS) composite and construction of glucose enzyme free electrochemical sensor. First, Ni O HSS was synthesized by hydrothermal method, then Ag was doped into Ni O HS by seed induced growth method to obtain Ag / Ni O HS.The structure and electrocatalytic properties of Ag / Ni O HSS were characterized by SEMX XRDCV and other methods. The results show that the electrode modified with Ag / NiO-HS has good electrocatalytic performance for glucose, such as high sensitivity (2300 渭 A m M-1) cm-2), low detection limit (0.007 渭 M) and wide linear range, and so on. The results show that the electrode modified with Ag / NiOHS has good electrocatalytic activity for glucose, for example, high sensitivity (2300 渭 A m ~ (-1) cm ~ (-1) cm ~ (-2), low detection limit (0.007 渭 M) and wide linear range, etc. In addition, the composite modified glassy carbon electrode has excellent anti-interference ability to uric acid and acrylic acid. Therefore, the Ag-Ni-O-HS composite has some potential applications in the field of non-enzymatic glucose sensors. (3) the preparation of Ni-doped graphite-phase carbon nitride (g-C3N4) composite (Nirg-C3N4) and the construction of bisphenol A (BPA) non-enzymatic electrochemical sensor. Ni- / g-C _ 3N _ 4 was prepared by calcining the mixture of melamine and nickel chloride (NiCl _ 2H _ 2O), and its morphology and electrocatalytic properties were characterized by means of SEMG-XRD, IR, EIS and DPV. The results show that the sensors assembled by the Ni- / g-C3Nder4 composite have good electrocatalytic performance for BPA. The detection linear ranges are 0.01 渭 M-1 渭 M and 1 渭 M-100 渭 M, and the detection limit is 4.34nM (SNR 3). Therefore, Nirg-C3Nstud composite has a certain practical application value for the detection of BPA.
【学位授予单位】：湘潭大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB33;O657.1
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