基于納米復合材料的光電化學和電化學傳感器的構(gòu)建及應(yīng)用
發(fā)布時間：2018-08-14 15:15
【摘要】：本文制備了CdS量子點、TiO2等納米材料,并分別與石墨烯或氯化血紅素復合,構(gòu)建具有高催化性能的新型光電/電化學傳感器。使用FESEM、XRD、UV-Vis、電化學檢測等方法對納米復合材料的表面形貌、結(jié)構(gòu)、光學和電化學性質(zhì)進行了表征。將新型光電/電化學傳感器應(yīng)用于環(huán)境污染物和H2O2的靈敏檢測,研究了對苯二胺的光伏行為以及催化機理。主要內(nèi)容包括以下兩個方面:1、本部分采用水熱法合成了水溶性CdS量子點,摻雜適量石墨烯(GS)后制備了CdS-GS/FTO膜修飾電極。石墨烯的摻雜使CdS量子點薄膜的光電化學性能得到大幅提高。在可見光照射下,由于光電催化反應(yīng)的存在,對苯二胺(PPD)在CdS-GS/FTO上的循環(huán)伏安圖呈現(xiàn)“S”形,這一響應(yīng)被用于膜材料比例的快速優(yōu)化。掃描速率和pH對PPD光伏行為的影響表明,在光輻照下盡管電化學過程的控制步驟沒有發(fā)生改變,卻有相比質(zhì)子數(shù)目更多的電子可能參與到光電催化過程中。此外,光電活性的膜修飾電極被應(yīng)用于對苯二胺的靈敏檢測。這種光電化學傳感器在最優(yōu)條件下對PPD的線性響應(yīng)范圍為1.0?10-7~3.0?10-6 mol·L-1,檢出限(3S/N)為4.3?10-8 mol·L-1。本部分通過光伏方法研究了PPD在電極上的光誘導電子轉(zhuǎn)移過程,并提出了一種PPD靈敏檢測的光電化學方法。2、采用火焰氣溶膠合成技術(shù)制備的TiO2納米顆粒,與氯化血紅素(Hemin)復合,制備了具有電催化活性和光電活性的雙功能Hemin-TiO2/GCE電極。循環(huán)伏安表征顯示Hemin-TiO2復合膜上清晰地顯現(xiàn)出Hemin的一對氧化還原峰,探討了掃描速率、電解液pH對修飾電極電化學行為的影響。Hemin-TiO2/GCE修飾電極對H2O2有良好的電催化還原活性,在3.0?10-7 mol·L-1至4.7?10-4 mol·L-1范圍內(nèi)對H2O2具有良好的線性關(guān)系,檢出限(3S/N)為7.2?10-8 mol·L-1。同時,Hemin-TiO2復合膜還保留了TiO2的光電化學活性,Hemin的摻雜能夠幫助TiO2吸收一部分的可見光,阻礙了TiO2光生電子空穴對(e-/h+)的復合,從而進一步提高了電極對可見光的光電響應(yīng)�；诖藰�(gòu)建了一種用于對苯二酚定量檢測的光電化學傳感器,線性響應(yīng)范圍是4.0?10-7 mol·L-1到3.0?10-5 mol·L-1,檢出限(3S/N)為9.8?10-8 mol·L-1。該傳感器已成功地用于對苯二酚降解率的測定。
[Abstract]:In this paper, CdS quantum dots TiO2 and other nanomaterials were prepared and combined with graphene or hemin, respectively. A novel photoelectric / electrochemical sensor with high catalytic performance was constructed. The surface morphology, structure, optical and electrochemical properties of the nanocomposites were characterized by Fesemer XRDX UV-Visand electrochemical detection. A novel photoelectric / electrochemical sensor was applied to the sensitive detection of environmental pollutants and H2O2. The photovoltaic behavior and catalytic mechanism of p-phenylenediamine were studied. The main contents include the following two aspects: 1. In this part, water-soluble CdS quantum dots were synthesized by hydrothermal method. CdS-GS/FTO film modified electrode was prepared by doping proper amount of graphene (GS). The photochemical properties of CdS quantum dot films are greatly improved by the doping of graphene. Under visible light irradiation, the cyclic voltammogram of p-phenylenediamine (PPD) on CdS-GS/FTO presents a "S" shape due to the existence of photocatalytic reaction, which is used to optimize the ratio of membrane materials. The effects of scanning rate and pH on the photovoltaic behavior of PPD show that, although the control steps of the electrochemical process have not changed under light irradiation, more electrons than the number of protons may be involved in the photocatalytic process. In addition, photoactive membrane modified electrodes are used for sensitive detection of p-phenylenediamine. Under the optimum conditions, the linear response range of the photochemical sensor to PPD is 1.0 脳 10 ~ (-7) ~ 3.0 ~ (-1) mol ~ (-6) mol L ~ (-1) and the detection limit (3S/N) is 4.3 ~ (-8) mol / L ~ (-1). In this part, photoinduced electron transfer of PPD on the electrode was studied by photovoltaic method, and a photochemical method of PPD sensitive detection was proposed. The TiO2 nanoparticles were prepared by flame aerosol synthesis technology and combined with hemin (Hemin). Two functional Hemin-TiO2/GCE electrodes with electrocatalytic activity and photovoltaic activity were prepared. Cyclic voltammetry analysis showed that a pair of redox peaks of Hemin appeared clearly on Hemin-TiO2 composite film. The effects of scanning rate and pH of electrolyte on electrochemical behavior of modified electrode. Hemin-TiO2 / GCE-modified electrode had good electrocatalytic reduction activity to H2O2. There was a good linear relationship for H2O2 in the range of 3.0 ~ 10 ~ (-7) mol ~ (-1) to 4.7 ~ (-4) mol L ~ (-1). The detection limit (3S/N) was 7.2 ~ (-8) mol L ~ (-1). At the same time, the doping of TiO2 can help TiO2 absorb a part of visible light, which hinders the photo-generated electron hole pair (e-r / h) of TiO2, which further improves the photoresponse of the electrode to visible light. A photochemical sensor for quantitative determination of hydroquinone was constructed. The linear response range was from 4.0 ~ 10 ~ (-7) mol ~ (-1) to 3.0 ~ (-1) ~ 10 ~ (-5) mol L ~ (-1). The detection limit (3S/N) was 9.8 ~ (-8) mol L ~ (-1). The sensor has been successfully used to determine the degradation rate of hydroquinone.
【學位授予單位】：華中科技大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TB33;O657.1
[Abstract]:In this paper, CdS quantum dots TiO2 and other nanomaterials were prepared and combined with graphene or hemin, respectively. A novel photoelectric / electrochemical sensor with high catalytic performance was constructed. The surface morphology, structure, optical and electrochemical properties of the nanocomposites were characterized by Fesemer XRDX UV-Visand electrochemical detection. A novel photoelectric / electrochemical sensor was applied to the sensitive detection of environmental pollutants and H2O2. The photovoltaic behavior and catalytic mechanism of p-phenylenediamine were studied. The main contents include the following two aspects: 1. In this part, water-soluble CdS quantum dots were synthesized by hydrothermal method. CdS-GS/FTO film modified electrode was prepared by doping proper amount of graphene (GS). The photochemical properties of CdS quantum dot films are greatly improved by the doping of graphene. Under visible light irradiation, the cyclic voltammogram of p-phenylenediamine (PPD) on CdS-GS/FTO presents a "S" shape due to the existence of photocatalytic reaction, which is used to optimize the ratio of membrane materials. The effects of scanning rate and pH on the photovoltaic behavior of PPD show that, although the control steps of the electrochemical process have not changed under light irradiation, more electrons than the number of protons may be involved in the photocatalytic process. In addition, photoactive membrane modified electrodes are used for sensitive detection of p-phenylenediamine. Under the optimum conditions, the linear response range of the photochemical sensor to PPD is 1.0 脳 10 ~ (-7) ~ 3.0 ~ (-1) mol ~ (-6) mol L ~ (-1) and the detection limit (3S/N) is 4.3 ~ (-8) mol / L ~ (-1). In this part, photoinduced electron transfer of PPD on the electrode was studied by photovoltaic method, and a photochemical method of PPD sensitive detection was proposed. The TiO2 nanoparticles were prepared by flame aerosol synthesis technology and combined with hemin (Hemin). Two functional Hemin-TiO2/GCE electrodes with electrocatalytic activity and photovoltaic activity were prepared. Cyclic voltammetry analysis showed that a pair of redox peaks of Hemin appeared clearly on Hemin-TiO2 composite film. The effects of scanning rate and pH of electrolyte on electrochemical behavior of modified electrode. Hemin-TiO2 / GCE-modified electrode had good electrocatalytic reduction activity to H2O2. There was a good linear relationship for H2O2 in the range of 3.0 ~ 10 ~ (-7) mol ~ (-1) to 4.7 ~ (-4) mol L ~ (-1). The detection limit (3S/N) was 7.2 ~ (-8) mol L ~ (-1). At the same time, the doping of TiO2 can help TiO2 absorb a part of visible light, which hinders the photo-generated electron hole pair (e-r / h) of TiO2, which further improves the photoresponse of the electrode to visible light. A photochemical sensor for quantitative determination of hydroquinone was constructed. The linear response range was from 4.0 ~ 10 ~ (-7) mol ~ (-1) to 3.0 ~ (-1) ~ 10 ~ (-5) mol L ~ (-1). The detection limit (3S/N) was 9.8 ~ (-8) mol L ~ (-1). The sensor has been successfully used to determine the degradation rate of hydroquinone.
【學位授予單位】：華中科技大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：TB33;O657.1
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