新型过渡金属/碳纳米复合材料的制备及分析应用研究
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摘要
本博士学位论文以石墨烯、碳纳米管、介孔碳以及表面活性物质为基本材料,通过自组装、掺杂等步骤,首先制备了石墨烯-碳纳米管、石墨烯-苯胺、聚二烯丙基二甲基氯化铵(PDDA)-介孔碳等复合材料,然后在其表面负载过渡金属纳米材料,进而制得了新型过渡金属/碳纳米复合材料。并对所制备的材料进行了系统的分析与表征,研究了这些材料被用于催化、电化学传感器的可能性。具体工作内容如下：
1.采用原位自组装法制备了三明治层状堆叠结构的氧化石墨烯(Gr)-碳纳米管(CNTs)复合材料,然后利用乙二醇的一步还原法,将Pt纳米粒子负载于Gr/CNTs复合物表面,制得了Pt/Gr-CNTs复合材料。利用扫描电子显微镜(SEM)、X-射线粉末衍射仪(XRD)等手段对Pt/Gr-CNTs进行了系统的表征。进一步研究证明Pt/Gr-CNTs复合材料在中性介质中对甲醇氧化具有高的催化活性。
2.在成功合成了具有夹心结构的Pt/Gr/CNTs复合材料基础上,发展了一种基于该复合材料的电化学传感器,建立了测定热敏纸纸样中双酚A含量的分析方法。以循环伏安法(CV)和微分脉冲伏安法(DPV)为主建立的双酚A分析方法,可在6.0x10-8到8.0×10-5mol/L的浓度范围内进行测定,检测限为4.2×10-8mol/L(S/N=3)。
3.发展了一种基于有机和水相界面相转移的方法,通过电荷转移自组装技术制备了Gr/苯胺(ANI)纳米复合材料；同时以Gr-ANI为原材料,利用原位电聚合法制备了Gr/-聚苯胺(PANI)纳米复合材料；进而将金属钯负载在Gr/pANI基底上用于制作电化学传感的新材料。用可见-紫外光谱法(UV-VIS)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)等手段表征了制备的复合材料。然后利用对苯二酚和邻苯二酚作为探针分子对Pd/Gr-PANI复合材料修饰电极的电催化活性进行了研究。结果表明,该材料对两种探针分子具有良好的电催化作用,可用于对苯二酚和邻苯二酚同分异构体的同时测定。
4.通过原位自组装技术制备了三明治结构的Gr-CNTs纳米复合物,然后将其作为填料制备了导电性好的Gr-CNTs/聚酰亚胺(PI)混合膜。并在此基础上制备了更高导电性的、表面银化的Ag-Gr-CNTs/PI柔性复合膜。所制备的材料性质表明了其有望被应用于太阳能电池以及生物传感器等领域。
5.对介孔碳(MC)进行功能化修饰,然后利用水热反应法将类石墨烯材料MOS2负载于MC表面,制得了MoS2/PDDA-MC复合材料、并将其应用于电化学传感研究。以该复合材料制得的修饰电极对L-半胱氨酸(L-Cys)具有良好的电催化能力,可望用于催化析氢、含硫有机小分子的检测。
In this paper, we studied the electrochemical behavior of several biological molecules on the transition metal/graphene-carbon nanotubes(Gr-CNTs) nanocomposites modified electrodes. The transition metal/Gr-CNTs nanocomposites were synthesized through liquid phase reduction method, several noble metal nanocomposites were successfully synthesized and their morphology and crystalline structures were characterized and analyzed carefully. Additionally, transition metal/Gr-CNTs nanocomposites-based nanocomposites modified electrodes were prepared and applications in electrochemical analysis were also extensively studied. The main contents are as follows:
1. The sandwich lamination structure of Gr-CNTs nanocomposite has been fabricated through in situ facile and green method. Then Pt nanoparticles are fabricated on Gr-CNTs via a simple one-step chemical reduction method in ethylene glycol (EG) and water system. The Pt/Gr-CNTs was further characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD), which indicated that the as-synthesized Pt nanoparticles was successfully dispersed on the surface of Gr-CNTs nanocomposite. Electrochemical study has been proved that the Pt/Gr-CNTs nanocomposite has higher catalytic activity in neutral medium for methanol oxidation, which is hopefully used in variety types of cells and biosensors in physiological medium.
2. Pt/Gr-CNTs nanocomposite based electrochemical sensors for the determination of endocrine disrupter bisphenol A in thermal printing papers. A facile and green method was developed to synthesize the Gr-CNTs nanocomposite with a sandwich lamination structure. Pt nanoparticles were loaded on the assynthesized Gr-CNTs nanocomposite to prepare an electrochemical sensor for determining bisphenol A (BPA) in thermal printing paper. The electrochemical behavior of BPA on the Pt/Gr-CNTs nanocomposite was investigated by cyclic voltammetry (CV) and chronocoulometry (CC). The direct determination of BPA was accomplished by using differential pulse voltammetry (DPV) under optimized conditions. The oxidation peak current was proportional to the BPA concentration in the range from6.0*10"8to 8.0x10-5M. The detection limit was4.2×10-8M (S/N=3). The fabricated electrode showed good reproducibility, stability and selectivity. The proposed method was successfully applied to determine BPA in thermal printing papers samples and the results were satisfact.
3. Anew facile in situ direct synthesis method of graphene-aniline (Gr-aniline) nanocomplex by a chargetransfer self-assembly technology at organic-aqueous interface was developed in this work. The graphene-polyaniline (Gr-PANI) nanocomposite was prepared by simultaneous electropolymerization of Gr-aniline, and palladium nanoparticles were loaded onto the Gr-PANI nanocomposite to be used as a new electrode material for electrochemical sensing. Hydroquinone (HQ) and catechol (CC) were used as probe molecule to evaluate the electrocatalytic activity of Pd/Gr-PANI nanocomposite. The Pd/Gr-PANI nanocomposite shows so excellent electro-catalytic activities toward the oxidation of HQ and CC isomers that the oxidation peaks of the two molecules were well and easily resolved. The excellent reproducibility, stability and selectivity of the Pd/Gr-PANI nanocomposite make it a potential candidate as electrochemical sensor for simultaneous determination of HQ and CC isomers.
4. Silver nanoparticles modified graphene-carbon nanotubes/polyimide (Gr-CNTs/PI) films have been prepared by electrochemical reduction of silver nitrate on potassium hydroxide hydroxylated of Gr-CNTs/PI films surface. The as-prepared nanocomposites were characterized by transmission electron microscopy(TEM), scanning electron microscopy(SEM), X-ray diffraction(XRD) analyzer and semiconductor characterization system. The lower content of Gr-CNTs (10wt.%) doping in PI matrix can improve the conductivity of PI films more clearly than pure CNTs. The conductivity can be regulated by controlling Gr-CNTs content in PI matrix. These silver nanoparticles into Gr-CNTs/PI films presented here can act as deposition seeds which can initiate subsequent electroless silver or copper or electrodeposition other metal.
5. In this work, a simple MoS2/PDDA-MC modified glassy carbon electrode (GCE) sensor has been fabricated. The electrochemical behavior of L-Cys was investigated on MoS2/PDDA-MC modified GCE.
1.采用原位自组装法制备了三明治层状堆叠结构的氧化石墨烯(Gr)-碳纳米管(CNTs)复合材料,然后利用乙二醇的一步还原法,将Pt纳米粒子负载于Gr/CNTs复合物表面,制得了Pt/Gr-CNTs复合材料。利用扫描电子显微镜(SEM)、X-射线粉末衍射仪(XRD)等手段对Pt/Gr-CNTs进行了系统的表征。进一步研究证明Pt/Gr-CNTs复合材料在中性介质中对甲醇氧化具有高的催化活性。
2.在成功合成了具有夹心结构的Pt/Gr/CNTs复合材料基础上,发展了一种基于该复合材料的电化学传感器,建立了测定热敏纸纸样中双酚A含量的分析方法。以循环伏安法(CV)和微分脉冲伏安法(DPV)为主建立的双酚A分析方法,可在6.0x10-8到8.0×10-5mol/L的浓度范围内进行测定,检测限为4.2×10-8mol/L(S/N=3)。
3.发展了一种基于有机和水相界面相转移的方法,通过电荷转移自组装技术制备了Gr/苯胺(ANI)纳米复合材料；同时以Gr-ANI为原材料,利用原位电聚合法制备了Gr/-聚苯胺(PANI)纳米复合材料；进而将金属钯负载在Gr/pANI基底上用于制作电化学传感的新材料。用可见-紫外光谱法(UV-VIS)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)等手段表征了制备的复合材料。然后利用对苯二酚和邻苯二酚作为探针分子对Pd/Gr-PANI复合材料修饰电极的电催化活性进行了研究。结果表明,该材料对两种探针分子具有良好的电催化作用,可用于对苯二酚和邻苯二酚同分异构体的同时测定。
4.通过原位自组装技术制备了三明治结构的Gr-CNTs纳米复合物,然后将其作为填料制备了导电性好的Gr-CNTs/聚酰亚胺(PI)混合膜。并在此基础上制备了更高导电性的、表面银化的Ag-Gr-CNTs/PI柔性复合膜。所制备的材料性质表明了其有望被应用于太阳能电池以及生物传感器等领域。
5.对介孔碳(MC)进行功能化修饰,然后利用水热反应法将类石墨烯材料MOS2负载于MC表面,制得了MoS2/PDDA-MC复合材料、并将其应用于电化学传感研究。以该复合材料制得的修饰电极对L-半胱氨酸(L-Cys)具有良好的电催化能力,可望用于催化析氢、含硫有机小分子的检测。
In this paper, we studied the electrochemical behavior of several biological molecules on the transition metal/graphene-carbon nanotubes(Gr-CNTs) nanocomposites modified electrodes. The transition metal/Gr-CNTs nanocomposites were synthesized through liquid phase reduction method, several noble metal nanocomposites were successfully synthesized and their morphology and crystalline structures were characterized and analyzed carefully. Additionally, transition metal/Gr-CNTs nanocomposites-based nanocomposites modified electrodes were prepared and applications in electrochemical analysis were also extensively studied. The main contents are as follows:
1. The sandwich lamination structure of Gr-CNTs nanocomposite has been fabricated through in situ facile and green method. Then Pt nanoparticles are fabricated on Gr-CNTs via a simple one-step chemical reduction method in ethylene glycol (EG) and water system. The Pt/Gr-CNTs was further characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD), which indicated that the as-synthesized Pt nanoparticles was successfully dispersed on the surface of Gr-CNTs nanocomposite. Electrochemical study has been proved that the Pt/Gr-CNTs nanocomposite has higher catalytic activity in neutral medium for methanol oxidation, which is hopefully used in variety types of cells and biosensors in physiological medium.
2. Pt/Gr-CNTs nanocomposite based electrochemical sensors for the determination of endocrine disrupter bisphenol A in thermal printing papers. A facile and green method was developed to synthesize the Gr-CNTs nanocomposite with a sandwich lamination structure. Pt nanoparticles were loaded on the assynthesized Gr-CNTs nanocomposite to prepare an electrochemical sensor for determining bisphenol A (BPA) in thermal printing paper. The electrochemical behavior of BPA on the Pt/Gr-CNTs nanocomposite was investigated by cyclic voltammetry (CV) and chronocoulometry (CC). The direct determination of BPA was accomplished by using differential pulse voltammetry (DPV) under optimized conditions. The oxidation peak current was proportional to the BPA concentration in the range from6.0*10"8to 8.0x10-5M. The detection limit was4.2×10-8M (S/N=3). The fabricated electrode showed good reproducibility, stability and selectivity. The proposed method was successfully applied to determine BPA in thermal printing papers samples and the results were satisfact.
3. Anew facile in situ direct synthesis method of graphene-aniline (Gr-aniline) nanocomplex by a chargetransfer self-assembly technology at organic-aqueous interface was developed in this work. The graphene-polyaniline (Gr-PANI) nanocomposite was prepared by simultaneous electropolymerization of Gr-aniline, and palladium nanoparticles were loaded onto the Gr-PANI nanocomposite to be used as a new electrode material for electrochemical sensing. Hydroquinone (HQ) and catechol (CC) were used as probe molecule to evaluate the electrocatalytic activity of Pd/Gr-PANI nanocomposite. The Pd/Gr-PANI nanocomposite shows so excellent electro-catalytic activities toward the oxidation of HQ and CC isomers that the oxidation peaks of the two molecules were well and easily resolved. The excellent reproducibility, stability and selectivity of the Pd/Gr-PANI nanocomposite make it a potential candidate as electrochemical sensor for simultaneous determination of HQ and CC isomers.
4. Silver nanoparticles modified graphene-carbon nanotubes/polyimide (Gr-CNTs/PI) films have been prepared by electrochemical reduction of silver nitrate on potassium hydroxide hydroxylated of Gr-CNTs/PI films surface. The as-prepared nanocomposites were characterized by transmission electron microscopy(TEM), scanning electron microscopy(SEM), X-ray diffraction(XRD) analyzer and semiconductor characterization system. The lower content of Gr-CNTs (10wt.%) doping in PI matrix can improve the conductivity of PI films more clearly than pure CNTs. The conductivity can be regulated by controlling Gr-CNTs content in PI matrix. These silver nanoparticles into Gr-CNTs/PI films presented here can act as deposition seeds which can initiate subsequent electroless silver or copper or electrodeposition other metal.
5. In this work, a simple MoS2/PDDA-MC modified glassy carbon electrode (GCE) sensor has been fabricated. The electrochemical behavior of L-Cys was investigated on MoS2/PDDA-MC modified GCE.
引文
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