石墨烯基納米薄膜復(fù)合材料的制備及在電化學(xué)傳感器上的應(yīng)用
發(fā)布時(shí)間：2019-03-27 08:43
【摘要】：石墨烯(GR)是一種獨(dú)特二維空間尺寸的納米材料,具有獨(dú)特的電學(xué)性質(zhì)、熱學(xué)性質(zhì)、機(jī)械強(qiáng)度、較大的比表面積、原料易得等特點(diǎn),近年來引起了科學(xué)研究人員的廣泛關(guān)注。自2004年英國(guó)科學(xué)家Geim等人首次制備了單層二維片狀石墨烯,立即引起了科學(xué)界的研究和探索。石墨烯的出現(xiàn)填補(bǔ)了碳家族中二維結(jié)構(gòu)材料的空缺,使得碳納米材料從零維、一維、二維到三維形成了一個(gè)完整的體系�；谑┎牧弦言诠怆妼W(xué)、催化儲(chǔ)能、傳感器等諸多領(lǐng)域的應(yīng)用。本論文采用優(yōu)化Hummer法對(duì)石墨粉進(jìn)行化學(xué)剝離,得到親水的氧化石墨烯(graphene oxide,GO)。以氧化石墨烯為前驅(qū)體,通過化學(xué)合成法制備了基于石墨烯基的復(fù)合材料,并對(duì)得到的產(chǎn)物性能進(jìn)行表征;同時(shí)通過實(shí)驗(yàn)的分析和探討復(fù)合材料的優(yōu)勢(shì)并將其用于電化學(xué)傳感器領(lǐng)域,制備了基于石墨烯基的復(fù)合物傳感器。其主要內(nèi)容如下:(1)通過高錳酸鉀(KMnO_4)、濃硫酸(H_2SO_4)及硝酸鈉(NaNO_3)作氧化劑,對(duì)石墨粉進(jìn)行化學(xué)氧化切割,使其表面和邊緣修飾上羥基、羧基、環(huán)氧等親水性基團(tuán)。通過過濾、洗滌、透析等方法,最后將得到氧化石墨烯GO。再以氧化石墨烯(GO)為前驅(qū)體與氯化亞銅(CuCl)在堿性溶液下,通過單模微波反應(yīng)器,形成穩(wěn)定三維多孔結(jié)構(gòu)的CuO/r-GO復(fù)合材料。該復(fù)合材料用掃描電鏡(SEM),透射電鏡(TEM)表征形貌,X射線衍射儀(XRD)表征晶格結(jié)構(gòu),吸附-脫附等溫測(cè)試(BET)表征材料的孔隙。CuO/r-GO復(fù)合物修飾電極應(yīng)用于葡萄糖的電化學(xué)傳感器具有較高的靈敏度和穩(wěn)定性,寬的線性范圍和低的檢出限等優(yōu)點(diǎn)。(2)利用高溫加熱的方法合成了碳量子點(diǎn)(CDs),再通過化學(xué)還原制備了碳量子點(diǎn)功能化的石墨烯(CDs/r-GO)。掃描電鏡(SEM),透射電鏡(TEM)表征形貌,原子力顯微鏡(AFM)研究表面結(jié)構(gòu)和厚度,紅外光譜(FT-IR)、紫外光譜(UV-vis)和熒光探討材料的光學(xué)特性。由于在CDs和r-GO之間存在強(qiáng)的電子轉(zhuǎn)移,通過層與層之間的π-π堆積和電子之間的轉(zhuǎn)移作用能夠加速電子轉(zhuǎn)移,使復(fù)合材料具有高的電導(dǎo)性、電催化和氧化還原能力等性能。該復(fù)合材料可作為電化學(xué)傳感器定量分析對(duì)苯二酚(HQ)、鄰苯二酚(CC)和間苯二酚(RC)。此外,CDs/r-GO/GCE進(jìn)一步用于實(shí)際檢測(cè),得到較為滿意的效果。(3)硫化鎘/還原氧化石墨烯(CdS/r-GO)復(fù)合物通過水熱反應(yīng)合成,CdS/r-GO復(fù)合物被成功用來檢測(cè)苯二酚異構(gòu)體。通過對(duì)轉(zhuǎn)移系數(shù)(α)和電子遷移速率(ks)等進(jìn)行了電荷的轉(zhuǎn)移原理的探究,循環(huán)伏安法和差分脈沖伏安法等測(cè)試了CdS/r-GO復(fù)合物的電化學(xué)性能。此外,該傳感器成功的對(duì)苯二酚異構(gòu)體進(jìn)行定量檢測(cè),進(jìn)一步的實(shí)際應(yīng)用也得到滿意的效果。
[Abstract]:Graphene (GR) is a kind of special two-dimensional space-size nanomaterials with unique electrical properties, thermal properties, mechanical strength, large specific surface area, easy availability of raw materials, and so on. In recent years, it has attracted wide attention of scientific researchers. Single-layer two-dimensional flake graphene has been prepared for the first time by British scientist Geim et al in 2004, which has aroused the scientific research and exploration immediately. The appearance of graphene fills the gap of two-dimensional structural materials in the carbon family, which makes the carbon nanomaterials form a complete system from zero-dimensional, one-dimensional, two-dimensional to three-dimensional. Graphene-based materials have been applied in many fields such as photoelectricity, catalytic energy storage, sensors and so on. In this paper, the hydrophilic graphene oxide (graphene oxide,GO) was obtained by chemical stripping of graphite powder by optimized Hummer method. Graphene-based composites were prepared by chemical synthesis using graphene oxide as precursor and their properties were characterized. At the same time, the advantages of the composites were analyzed experimentally and applied to the field of electrochemical sensors, and the composite sensors based on graphene group were prepared. The main contents are as follows: (1) by using potassium permanganate (KMnO_4), concentrated sulfuric acid (H_2SO_4) and sodium nitrate (NaNO_3) as oxidants, the graphite powder was chemically oxidized to modify the hydroxyl and carboxyl groups on its surface and edge. Hydrophilic groups such as epoxy. Finally, graphene oxide GO. can be obtained by filtration, washing, dialysis, etc. Then, using graphene oxide (GO) as precursor and cuprous chloride (CuCl) in alkaline solution, a stable three-dimensional porous CuO/r-GO composite was formed through a single-mode microwave reactor. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM), and the lattice structure was characterized by X-ray diffraction (XRD). Adsorption-desorption isotherms were used to characterize the pores of the material by (BET). The CuO/r-GO complex modified electrode has high sensitivity and stability when applied to the electrochemical sensor of glucose. The advantages of wide linear range and low detection limit were obtained. (2) carbon quantum dots (CDs),) were synthesized by high temperature heating and then functionalized graphene (CDs/r-GO) was prepared by chemical reduction. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM). The surface structure and thickness were studied by atomic force microscopy (AFM). The optical properties of the materials were investigated by infrared spectroscopy (FT-IR), ultraviolet spectroscopy (UV-vis) and fluorescence. Due to the strong electron transfer between CDs and r-GO, the electron transfer can be accelerated by 蟺-蟺 stacking and electron transfer between layers, which makes the composites have high conductivity. Electrocatalysis and redox ability. The composite can be used as electrochemical sensor for quantitative analysis of hydroquinone (HQ), catechol (CC) and resorcinol (RC). In addition, CDs/r-GO/GCE was further applied to the detection of cadmium sulfide / reduced graphene oxide (CdS/r-GO). (3) cadmium sulfide / reduced graphene oxide (CdS/r-GO) composite was synthesized by hydrothermal reaction. The CdS/r-GO complex was successfully used to detect the isomers of catechol. The charge transfer principle was investigated by the transfer coefficient (偽) and electron transfer rate (ks). The electrochemical properties of CdS/r-GO complex were tested by cyclic voltammetry and differential pulse voltammetry. In addition, the sensor has been successfully used for the quantitative detection of hydroquinone isomers, and its further practical application has also achieved satisfactory results.
【學(xué)位授予單位】：閩南師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.1
[Abstract]:Graphene (GR) is a kind of special two-dimensional space-size nanomaterials with unique electrical properties, thermal properties, mechanical strength, large specific surface area, easy availability of raw materials, and so on. In recent years, it has attracted wide attention of scientific researchers. Single-layer two-dimensional flake graphene has been prepared for the first time by British scientist Geim et al in 2004, which has aroused the scientific research and exploration immediately. The appearance of graphene fills the gap of two-dimensional structural materials in the carbon family, which makes the carbon nanomaterials form a complete system from zero-dimensional, one-dimensional, two-dimensional to three-dimensional. Graphene-based materials have been applied in many fields such as photoelectricity, catalytic energy storage, sensors and so on. In this paper, the hydrophilic graphene oxide (graphene oxide,GO) was obtained by chemical stripping of graphite powder by optimized Hummer method. Graphene-based composites were prepared by chemical synthesis using graphene oxide as precursor and their properties were characterized. At the same time, the advantages of the composites were analyzed experimentally and applied to the field of electrochemical sensors, and the composite sensors based on graphene group were prepared. The main contents are as follows: (1) by using potassium permanganate (KMnO_4), concentrated sulfuric acid (H_2SO_4) and sodium nitrate (NaNO_3) as oxidants, the graphite powder was chemically oxidized to modify the hydroxyl and carboxyl groups on its surface and edge. Hydrophilic groups such as epoxy. Finally, graphene oxide GO. can be obtained by filtration, washing, dialysis, etc. Then, using graphene oxide (GO) as precursor and cuprous chloride (CuCl) in alkaline solution, a stable three-dimensional porous CuO/r-GO composite was formed through a single-mode microwave reactor. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM), and the lattice structure was characterized by X-ray diffraction (XRD). Adsorption-desorption isotherms were used to characterize the pores of the material by (BET). The CuO/r-GO complex modified electrode has high sensitivity and stability when applied to the electrochemical sensor of glucose. The advantages of wide linear range and low detection limit were obtained. (2) carbon quantum dots (CDs),) were synthesized by high temperature heating and then functionalized graphene (CDs/r-GO) was prepared by chemical reduction. The morphology was characterized by scanning electron microscopy (SEM),) and transmission electron microscopy (TEM). The surface structure and thickness were studied by atomic force microscopy (AFM). The optical properties of the materials were investigated by infrared spectroscopy (FT-IR), ultraviolet spectroscopy (UV-vis) and fluorescence. Due to the strong electron transfer between CDs and r-GO, the electron transfer can be accelerated by 蟺-蟺 stacking and electron transfer between layers, which makes the composites have high conductivity. Electrocatalysis and redox ability. The composite can be used as electrochemical sensor for quantitative analysis of hydroquinone (HQ), catechol (CC) and resorcinol (RC). In addition, CDs/r-GO/GCE was further applied to the detection of cadmium sulfide / reduced graphene oxide (CdS/r-GO). (3) cadmium sulfide / reduced graphene oxide (CdS/r-GO) composite was synthesized by hydrothermal reaction. The CdS/r-GO complex was successfully used to detect the isomers of catechol. The charge transfer principle was investigated by the transfer coefficient (偽) and electron transfer rate (ks). The electrochemical properties of CdS/r-GO complex were tested by cyclic voltammetry and differential pulse voltammetry. In addition, the sensor has been successfully used for the quantitative detection of hydroquinone isomers, and its further practical application has also achieved satisfactory results.
【學(xué)位授予單位】：閩南師范大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：O657.1
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