基于鎳復(fù)合材料的無酶電化學(xué)傳感器研究
發(fā)布時間：2018-07-17 20:46
【摘要】：鎳及氧化鎳具有穩(wěn)定的物化性能、很好的生物相容性、良好的電催化性能,被廣泛用于無酶電化學(xué)傳感器。然而純鎳及其氧化物存在一定缺陷,導(dǎo)致其在無酶電化學(xué)傳感器的應(yīng)用上受到了一定的限制。本論文通過鎳及其氧化物結(jié)合其它材料的摻雜制備出基于鎳的復(fù)合材料,從而提高了鎳基復(fù)合材料的電催化活性,并構(gòu)建新型無酶電化學(xué)傳感器。本論文主要研究內(nèi)容如下:(1)碳-氮/氧化鎳復(fù)合材料(C-N/Ni O)的制備及雙氧水(H_2O_2)無酶電化學(xué)傳感器的構(gòu)建。首先通過溶劑熱法制備氧化鎳微球(Ni O),然后氧化鎳微球與二嵌段共聚物(PHEMA_(200)-b-PDMAEMA_(100))混合物在高溫下煅燒,得到C-N/Ni O復(fù)合材料。通過掃描電鏡(SEM)、X射線衍射(XRD)、循環(huán)伏安(CV)、安培計時(i-t)等方法對其形貌結(jié)構(gòu)和電催化性能進(jìn)行了表征。實(shí)驗結(jié)果發(fā)現(xiàn)C-N/Ni O復(fù)合材料具有較高的比表面積,對H_2O_2具有良好的電催化性能:響應(yīng)時間快(3 s)、反應(yīng)靈敏度高(322μA·m M~(-1)·cm~(-2))、檢出限低(0.042μM)。因此C-N/Ni O復(fù)合材料對醫(yī)藥、環(huán)境和食品中的H_2O_2的檢測具有實(shí)際的應(yīng)用價值。(2)銀(Ag)摻雜氧化鎳空心球(Ni O HS)復(fù)合材料(Ag/Ni O HS)的制備及葡萄糖無酶電化學(xué)傳感器的構(gòu)建。首先通過水熱法合成Ni O HS,然后以種子誘導(dǎo)生長法將Ag摻雜到Ni O HS得到Ag/Ni O HS;并通過SEM、XRD、CV等方法對其結(jié)構(gòu)和電催化性能進(jìn)行了表征。結(jié)果表明,在Ag和Ni O HS的協(xié)同作用下,Ag/Ni O HS修飾玻碳電極對葡萄糖表現(xiàn)出良好的電催化性能,比如具有超高的靈敏度(2300μA·m M~(-1)·cm~(-2))、較低的檢出限(0.007μM)和較寬的線性范圍等特點(diǎn),此外該復(fù)合材料修飾的玻碳電極對尿酸和丙烯酸存在優(yōu)異抗干擾能力,因此,Ag/Ni O HS復(fù)合材料在無酶葡萄糖傳感器領(lǐng)域具有一定的應(yīng)用潛力。(3)鎳摻雜石墨相氮化碳(g-C_3N_4)復(fù)合材料(Ni/g-C_3N_4)的制備及雙酚A(BPA)無酶電化學(xué)傳感器的構(gòu)建。首先通過煅燒三聚氰胺和氯化鎳(Ni Cl_2·6H_2O)的混合物制備出Ni/g-C_3N_4;并通過SEM、XRD、紅外(IR)、交流阻抗(EIS)、差分脈沖伏安法(DPV)等方法對其形貌結(jié)構(gòu)和電催化性能進(jìn)行了表征。結(jié)果發(fā)現(xiàn)Ni/g-C_3N_4復(fù)合材料組裝的傳感器對BPA具有良好的電催化性能:檢測線性范圍為0.01μM-1μM和1μM-100μM,檢出限為4.34 n M(信噪比為3),因此,Ni/g-C_3N_4復(fù)合材料對于BPA的檢測具有一定的實(shí)際應(yīng)用價值。
[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.
【學(xué)位授予單位】：湘潭大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：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.
【學(xué)位授予單位】：湘潭大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TB33;O657.1
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