石墨烯及其组装材料的制备与表征
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摘要
作为碳纳米材料家族中独特的二维晶体结构材料,石墨烯纳米片(GNs)是在2004年被K.S.Novoselov和A.K.Geim等人首次发现并提出的。完美的石墨烯纳米片主要是指具有苯环结构的单个碳原子层。基于其在电学、光学、力学、热学等方面表现的优异性能,石墨烯纳米片已经成为目前材料科学和凝聚态物理研究的一个热点。同时,随着研究人员对石墨烯纳米片相关性能研究的不断深入,石墨烯量子点(GQDs)也以其良好的光致发光性能和在生物成像以及生物探针方面的应用进入研究人员的研究领域中。相应地,石墨烯基组装材料也逐渐成为人们研究的热点。本论文主要研究了石墨烯纳米片的制备及电化学性能研究,石墨烯量子点的制备及光致发光性能的研究以及几类石墨烯组装材料的制备及其性能应用。主要内容如下：
(1)作者分别利用氧化还原的方法和超声波剥离的方法制备出石墨烯纳米片(GNs)。首先,以水合肼作为还原剂把利用传统的hummer方法制备的氧化石墨烯还原为石墨烯纳米片。其次,作者首次利用超声波剥离的方法,选用石墨粉体为原料,以物质的量浓度为0.001M的中性表面活性剂聚乙烯吡咯烷酮(PVP)为分散剂和稳定剂,分别选择去离子水和无水乙醇为溶剂,在不同的功率条件下超声不同的时间制备出了石墨纳米薄片和石墨烯。通过动态光散射仪(DLS)分别测试了氧化石墨烯和石墨烯的Zeta电位及尺寸大小,结果表明氧化石墨烯和石墨烯纳米片表面都呈现出良好的负电性。然后以石英玻璃为基底,采用层层自组装的方法(LBL)实现石墨烯纳米片的层层自组装,形成石墨烯纳米片的均质薄膜。用紫外可见吸收光度计(UV-Vis)表征了组装层数与吸光度的线性关系；以导电玻璃(ITO)为基底,采用电泳沉积的方法(EPD)获得了石墨烯导电薄膜。利用电化学工作站(CHI)初步研究了所制备的石墨烯导电薄膜在超级电容器方面的应用。
(2)作者采用超声法一步简单快捷地合成了颗粒大小均一、分散均匀的光致发光的石墨烯量子点(GQDs),发现其具有良好的发光性能。以超声波剥离法获得石墨烯纳米片为原料,在不加入任何表面活性剂以及稳定剂的条件下,分别选用无水乙醇和N-甲基吡咯烷酮为溶剂,利用强力超声法一步简单快捷地合成了颗粒大小均一、分散均匀的光致发光的石墨烯量子点。
(3)以石墨烯纳米片为模板,以氯化锌和硫脲分别作为锌源和硫源,无水乙醇作为溶剂,在不同锌离子浓度条件下,利用醇热反应在180℃下分别保温12h、14h和16h,最终获得了两种独特的石墨烯/硫化锌量子点组装材料和石墨烯/硫化锌量子片组装材料。在可见光照射下,这两种组装材料均表现出良好的光电反应现象,其最大光电压值分别达到了0.5mV和0.7mV。
(4)分别利用溶剂热的方法和室温搅拌的方法制备了石墨烯纳米片与二氧化钛纳米管以及石墨烯量子点与二氧化钛纳米管的组装材料。然后在可见光照射下,研究并对比了这两种组装材料对有机染料亚甲基蓝(MB)的光催化降解能力,探讨了组装材料对MB光催化降解的简单机理。同时作为对比,作者也考察了单独二氧化钛纳米管作为光催化剂对MB水溶液的光降解效果。结果表明,组装材料的光催化性能明显优越于单独的二氧化钛纳米管。在可见光催化反应过程中,石墨烯充分起到了光敏作用。
(5)以氧化石墨烯和硝酸银为原料,分别选用柠檬酸钠和硼氢化钠为还原剂,在液相体系中原位合成了银/石墨烯组装材料。选用吡啶为目标探测分子,作者首次对银/石墨烯纳米组装材料作为表面增强拉曼活性基底对吡啶分子拉曼信号增强的性能进行了初步研究。
(6)首先,利用2-氨基乙硫醇实现了石墨烯的巯基化共价修饰；其次,以二水合醋酸锌为原料制备了氧化锌量子点；最后,借助于Zn-S键的键合作用成功地实现了氧化锌量子点在石墨烯表面的锚接。在紫外光照射下,以有机染料罗丹明B水溶液模拟工厂污水,氧化锌／石墨烯组装材料为光降解催化剂,测试了所合成氧化锌／石墨烯组装材料的光催化降解性能,分析了其对罗丹明B催化降解的机理过程。同时作为对比,作者也考察了单独氧化锌量子点作为光催化剂对罗丹明B水溶液的光降解效果。结果表明,组装材料的光催化性能优越于单独的氧化锌量子点。
本论文主要以化学纯的石墨粉为原料,分别制备了石墨烯纳米片和石墨烯量子点。然后又在制备的石墨烯纳米片和石墨烯量子点的基础上合成了石墨烯基组装材料,研究了石墨烯纳米片、石墨烯量子点以及石墨烯基组装材料的电性能、荧光性能、光电转化性能、光催化性能以及在表面增强拉曼(SERS)性能等方面的潜在应用。本论文的创新点主要在于：(1)首次在表面活性剂聚乙烯吡咯烷酮存在的条件下,超声制备出了石墨烯纳米片,并以该石墨烯纳米片为原料采用强力超声破碎的方法合成了石墨烯量子点。(2)利用石墨烯纳米片的模板效应,控制一定的反应时间和锌离子浓度,第一次成功可控地实现了硫化锌从量子点到量子片的生长转变；所制备的两种结构独特的ZnS/GNs组装材料都表现出较好的光电响应性能,而ZnSQFs/GNs组装材料的光生电压响应值更优于ZnSQDs/GNs组装材料的光生电压响应值。(3)首次合成了在可见光下具有较高催化性能的石墨烯量子点敏化的二氧化钛纳米管组装材料。(4)首次探索了Ag/GNs组装材料作为表面增强拉曼活性基底对吡啶分子拉曼信号的增强性能,同时也考察了组装材料中银纳米颗粒对石墨烯拉曼信号的增强效果。
As a unique two-dimensional crystal structure material of carbon nanomaterials, graphene nanosheets (GNs) were first discovered and raised in2004by K.S.Novoselov and A.K.Geim. The perfect GNs mainly refer to a single layer of carbon atoms with a benzene ring structure. Based on its excellent performance in the electrical, optical, mechanical and thermal, GNs have become a hot topic in the fields of materials science and condensed matter physics. Meanwhile, with the deepening research about the related properties of GNs, graphene quantum dots (GQDs) gradually appeared in the scope of researchers and attracted much more interests for its good photoluminescence properties and remarkable application in the bio-imaging and bio-probe et al. In view light of this, many researchers have also paid most of their attention to the graphene-based composite materials. In this thesis, preparation and electrochemical properties of the GNs and preparation and photoluminescence properties of the GQDs have been primarily studied, and several types of graphene-based assembled materials and their performance applications have also been discussed. The main contents are as follows:
(1) GNs were prepared respectively with oxidation-reduction method and ultrasonic peeling method. Firstly, using hydrazine hydrate as a reducing agent, graphene oxide prepared via traditional hummer's method was reduced into GNs. Secondly, Slecting graphite powder as raw material and deionized water or ethanol as solvent, using neutral surfactant polyvinyl pyrrolidone (PVP) with concentrations of0.001M as dispersing agents and stabilizers, graphite nanosheets and graphene in the absolute ethanol or deionized water solution were prepared via the ultrasonic peeling method for the first time. Zeta potential and nanosize of graphene oxide and graphene were tested by dynamic light scattering (DLS), the results showed that a good negatively charge of graphene oxide and graphene nanosheets emerged. And then using quartz glass slip as substrate, via the layer by layer self-assembled (LBL) method, a homogeneous GNs film was made. A linear relationship of the assembled layers and the absorbance was characterized by UV-Vis; using electrophoretic deposition (EPD) method with conductive glass (ITO) as the base, graphene conductive thin film was obtained, and their application on the supercapacitor has also been preliminarily studied using electrochemical workstation (CHI).
(2) Employing the GNs prepared by ultrasonic stripping method as raw materials, absolute ethanol and N-methyl pyrrolidone as solvent, the homogeneous GQDs with uniform size and excellent photoluminescence performance were synthesized via the simply and efficiently powerful ultrasonic method. Then its remarkable photoluminescence performance was discussed by fluorescence spectrometer (FL). Morphologies and UV-Vis absorption characteristic peaks of GQDs were performed on the TEM and UV-Vis spectrophotometer.
(3) Selecting GNs as a template, zinc chloride and thiourea as zinc source and sulfur source, anhydrous ethanol as a solvent, the two unique ZnSQDs/GNs and ZnS QFs/GNs assembled materials were obtained with the Zn2+concentration of0.0001M and0.01M. Under visible light irradiation, these two assembled materials showed good photo-voltage response phenomenon, its voltage maximum values have reached respectively0.5mV and0.7mV.
(4) Via solvothermal method and simply mixed/stirred at room temperature, TNTs/GNs assembled materials and TNTs/GQDs assembled materials were synthesized. Their photocatalytic performance about degradation of organic dyes MB under visible light was explored and compared. And meanwhile, as a comparison, the separate TNTs were also investigated for photodegradation of MB aqueous. The results showed that the photocatalytic properties of the composite materials are significantly superior to the individual TNTs. Under the visible light irridation, the GNs acted as a photosensitive.
(5) Using graphene oxide and silver nitrate as raw material, sodium citrate and sodium borohydride as the reducing agent respectively, Ag/GNs assembled materials were in situ synthesized in liquid phase system. Selecting pyridine molecule as target object, the performance of Ag/GNs assembled materials as SERS active substrates for the enhancement of the pyridine molecule Raman signal were preliminary characterized and studied.
(6) Firstly, the graphene thiolated covalent modification was achieved with2-aminoethanethiol; Secondly, the zinc oxide quantum dots (ZnO QDs) were prepared from zinc acetate dihydrate; Finally, ZnO QDs were successfully anchored on the surface of the graphene by means of Zn-S bond in cooperation. Under UV irradiation, using the organic dye rhodamine B (RhB) aqueous solution as analog factory effluent, photocatalytic degradation performance of ZnOQDs/GNs assembled materials photodegradation catalyst was tested, and the catalyzed degradation mechanism on Rhodamine B was also analyzed. The results showed that the photocatalytic properties of the composite materials are significantly superior to the individual ZnO. Under UV irridation, the presence of GNs produced negative effects to the photocatalytic properties.
In brief, this thesis is mainly employing the chemically pure graphite powder as raw materials to synthesize the GNs and GQDs. And then, based on the graphene materials, the graphene-based composite materials were also prepared. The fluorescence properties, optoelectronic conversion performance photocatalytic properties and potential applications of surface-enhanced Raman (SERS) performance of the materials were invesgatied and studied.
(1)作者分别利用氧化还原的方法和超声波剥离的方法制备出石墨烯纳米片(GNs)。首先,以水合肼作为还原剂把利用传统的hummer方法制备的氧化石墨烯还原为石墨烯纳米片。其次,作者首次利用超声波剥离的方法,选用石墨粉体为原料,以物质的量浓度为0.001M的中性表面活性剂聚乙烯吡咯烷酮(PVP)为分散剂和稳定剂,分别选择去离子水和无水乙醇为溶剂,在不同的功率条件下超声不同的时间制备出了石墨纳米薄片和石墨烯。通过动态光散射仪(DLS)分别测试了氧化石墨烯和石墨烯的Zeta电位及尺寸大小,结果表明氧化石墨烯和石墨烯纳米片表面都呈现出良好的负电性。然后以石英玻璃为基底,采用层层自组装的方法(LBL)实现石墨烯纳米片的层层自组装,形成石墨烯纳米片的均质薄膜。用紫外可见吸收光度计(UV-Vis)表征了组装层数与吸光度的线性关系；以导电玻璃(ITO)为基底,采用电泳沉积的方法(EPD)获得了石墨烯导电薄膜。利用电化学工作站(CHI)初步研究了所制备的石墨烯导电薄膜在超级电容器方面的应用。
(2)作者采用超声法一步简单快捷地合成了颗粒大小均一、分散均匀的光致发光的石墨烯量子点(GQDs),发现其具有良好的发光性能。以超声波剥离法获得石墨烯纳米片为原料,在不加入任何表面活性剂以及稳定剂的条件下,分别选用无水乙醇和N-甲基吡咯烷酮为溶剂,利用强力超声法一步简单快捷地合成了颗粒大小均一、分散均匀的光致发光的石墨烯量子点。
(3)以石墨烯纳米片为模板,以氯化锌和硫脲分别作为锌源和硫源,无水乙醇作为溶剂,在不同锌离子浓度条件下,利用醇热反应在180℃下分别保温12h、14h和16h,最终获得了两种独特的石墨烯/硫化锌量子点组装材料和石墨烯/硫化锌量子片组装材料。在可见光照射下,这两种组装材料均表现出良好的光电反应现象,其最大光电压值分别达到了0.5mV和0.7mV。
(4)分别利用溶剂热的方法和室温搅拌的方法制备了石墨烯纳米片与二氧化钛纳米管以及石墨烯量子点与二氧化钛纳米管的组装材料。然后在可见光照射下,研究并对比了这两种组装材料对有机染料亚甲基蓝(MB)的光催化降解能力,探讨了组装材料对MB光催化降解的简单机理。同时作为对比,作者也考察了单独二氧化钛纳米管作为光催化剂对MB水溶液的光降解效果。结果表明,组装材料的光催化性能明显优越于单独的二氧化钛纳米管。在可见光催化反应过程中,石墨烯充分起到了光敏作用。
(5)以氧化石墨烯和硝酸银为原料,分别选用柠檬酸钠和硼氢化钠为还原剂,在液相体系中原位合成了银/石墨烯组装材料。选用吡啶为目标探测分子,作者首次对银/石墨烯纳米组装材料作为表面增强拉曼活性基底对吡啶分子拉曼信号增强的性能进行了初步研究。
(6)首先,利用2-氨基乙硫醇实现了石墨烯的巯基化共价修饰；其次,以二水合醋酸锌为原料制备了氧化锌量子点；最后,借助于Zn-S键的键合作用成功地实现了氧化锌量子点在石墨烯表面的锚接。在紫外光照射下,以有机染料罗丹明B水溶液模拟工厂污水,氧化锌／石墨烯组装材料为光降解催化剂,测试了所合成氧化锌／石墨烯组装材料的光催化降解性能,分析了其对罗丹明B催化降解的机理过程。同时作为对比,作者也考察了单独氧化锌量子点作为光催化剂对罗丹明B水溶液的光降解效果。结果表明,组装材料的光催化性能优越于单独的氧化锌量子点。
本论文主要以化学纯的石墨粉为原料,分别制备了石墨烯纳米片和石墨烯量子点。然后又在制备的石墨烯纳米片和石墨烯量子点的基础上合成了石墨烯基组装材料,研究了石墨烯纳米片、石墨烯量子点以及石墨烯基组装材料的电性能、荧光性能、光电转化性能、光催化性能以及在表面增强拉曼(SERS)性能等方面的潜在应用。本论文的创新点主要在于：(1)首次在表面活性剂聚乙烯吡咯烷酮存在的条件下,超声制备出了石墨烯纳米片,并以该石墨烯纳米片为原料采用强力超声破碎的方法合成了石墨烯量子点。(2)利用石墨烯纳米片的模板效应,控制一定的反应时间和锌离子浓度,第一次成功可控地实现了硫化锌从量子点到量子片的生长转变；所制备的两种结构独特的ZnS/GNs组装材料都表现出较好的光电响应性能,而ZnSQFs/GNs组装材料的光生电压响应值更优于ZnSQDs/GNs组装材料的光生电压响应值。(3)首次合成了在可见光下具有较高催化性能的石墨烯量子点敏化的二氧化钛纳米管组装材料。(4)首次探索了Ag/GNs组装材料作为表面增强拉曼活性基底对吡啶分子拉曼信号的增强性能,同时也考察了组装材料中银纳米颗粒对石墨烯拉曼信号的增强效果。
As a unique two-dimensional crystal structure material of carbon nanomaterials, graphene nanosheets (GNs) were first discovered and raised in2004by K.S.Novoselov and A.K.Geim. The perfect GNs mainly refer to a single layer of carbon atoms with a benzene ring structure. Based on its excellent performance in the electrical, optical, mechanical and thermal, GNs have become a hot topic in the fields of materials science and condensed matter physics. Meanwhile, with the deepening research about the related properties of GNs, graphene quantum dots (GQDs) gradually appeared in the scope of researchers and attracted much more interests for its good photoluminescence properties and remarkable application in the bio-imaging and bio-probe et al. In view light of this, many researchers have also paid most of their attention to the graphene-based composite materials. In this thesis, preparation and electrochemical properties of the GNs and preparation and photoluminescence properties of the GQDs have been primarily studied, and several types of graphene-based assembled materials and their performance applications have also been discussed. The main contents are as follows:
(1) GNs were prepared respectively with oxidation-reduction method and ultrasonic peeling method. Firstly, using hydrazine hydrate as a reducing agent, graphene oxide prepared via traditional hummer's method was reduced into GNs. Secondly, Slecting graphite powder as raw material and deionized water or ethanol as solvent, using neutral surfactant polyvinyl pyrrolidone (PVP) with concentrations of0.001M as dispersing agents and stabilizers, graphite nanosheets and graphene in the absolute ethanol or deionized water solution were prepared via the ultrasonic peeling method for the first time. Zeta potential and nanosize of graphene oxide and graphene were tested by dynamic light scattering (DLS), the results showed that a good negatively charge of graphene oxide and graphene nanosheets emerged. And then using quartz glass slip as substrate, via the layer by layer self-assembled (LBL) method, a homogeneous GNs film was made. A linear relationship of the assembled layers and the absorbance was characterized by UV-Vis; using electrophoretic deposition (EPD) method with conductive glass (ITO) as the base, graphene conductive thin film was obtained, and their application on the supercapacitor has also been preliminarily studied using electrochemical workstation (CHI).
(2) Employing the GNs prepared by ultrasonic stripping method as raw materials, absolute ethanol and N-methyl pyrrolidone as solvent, the homogeneous GQDs with uniform size and excellent photoluminescence performance were synthesized via the simply and efficiently powerful ultrasonic method. Then its remarkable photoluminescence performance was discussed by fluorescence spectrometer (FL). Morphologies and UV-Vis absorption characteristic peaks of GQDs were performed on the TEM and UV-Vis spectrophotometer.
(3) Selecting GNs as a template, zinc chloride and thiourea as zinc source and sulfur source, anhydrous ethanol as a solvent, the two unique ZnSQDs/GNs and ZnS QFs/GNs assembled materials were obtained with the Zn2+concentration of0.0001M and0.01M. Under visible light irradiation, these two assembled materials showed good photo-voltage response phenomenon, its voltage maximum values have reached respectively0.5mV and0.7mV.
(4) Via solvothermal method and simply mixed/stirred at room temperature, TNTs/GNs assembled materials and TNTs/GQDs assembled materials were synthesized. Their photocatalytic performance about degradation of organic dyes MB under visible light was explored and compared. And meanwhile, as a comparison, the separate TNTs were also investigated for photodegradation of MB aqueous. The results showed that the photocatalytic properties of the composite materials are significantly superior to the individual TNTs. Under the visible light irridation, the GNs acted as a photosensitive.
(5) Using graphene oxide and silver nitrate as raw material, sodium citrate and sodium borohydride as the reducing agent respectively, Ag/GNs assembled materials were in situ synthesized in liquid phase system. Selecting pyridine molecule as target object, the performance of Ag/GNs assembled materials as SERS active substrates for the enhancement of the pyridine molecule Raman signal were preliminary characterized and studied.
(6) Firstly, the graphene thiolated covalent modification was achieved with2-aminoethanethiol; Secondly, the zinc oxide quantum dots (ZnO QDs) were prepared from zinc acetate dihydrate; Finally, ZnO QDs were successfully anchored on the surface of the graphene by means of Zn-S bond in cooperation. Under UV irradiation, using the organic dye rhodamine B (RhB) aqueous solution as analog factory effluent, photocatalytic degradation performance of ZnOQDs/GNs assembled materials photodegradation catalyst was tested, and the catalyzed degradation mechanism on Rhodamine B was also analyzed. The results showed that the photocatalytic properties of the composite materials are significantly superior to the individual ZnO. Under UV irridation, the presence of GNs produced negative effects to the photocatalytic properties.
In brief, this thesis is mainly employing the chemically pure graphite powder as raw materials to synthesize the GNs and GQDs. And then, based on the graphene materials, the graphene-based composite materials were also prepared. The fluorescence properties, optoelectronic conversion performance photocatalytic properties and potential applications of surface-enhanced Raman (SERS) performance of the materials were invesgatied and studied.
引文
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