几种纳米材料的制备、分析、表征及其应用研究
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摘要
本博士学位论文中,作者利用电化学原子层沉积(EC-ALD)和液相还原法等技术分别制备了CuInS2等几种功能纳米材料,进而采用表面分析、化学成分分析、物理指标分析以及多种电化学分析手段系统表征了所制备的材料,探讨了其在光电催化、有机物降解等领域的应用。主要内容包括：
1.采用EC-ALD法在多晶金基底上成功制备了Ⅰ-Ⅲ-Ⅵ2族的半导体化合物CuInS2(CIS)。具体是首先用循环伏安法(CV)确定了每种元素的最佳沉积电位,然后用计时电流法(I-t)制备了该半导体化合物。接下来利用X-射线粉末衍射仪(XRD)、X-射线光电子能谱仪(XPS)、场发射扫描电子显微镜(FE-SEM)和傅立叶变换红外光谱(FT-IR)等手段表征了所得CIS材料。XRD结果表明,CIS薄膜有(112)择优取向的晶体学性质；XPS分析表明,CIS薄膜中,Cu、In和S的原子比例约为1:1:2; FT-IR结果证明发现CIS材料的半导体带隙为1.50eV。
2.采用EC-ALD法在多晶金基底上制备了Ⅳ-Ⅵ族的半导体化合物Pb1-xSnxSe(x=0.2)薄膜。由CV法和I-t技术确定的各元素沉积顺序为：(Se/Pb/Se/Pb/Se/Pb/Se/Pb/Se/Sn...),即每个沉积周期分别是由四个PbSe和一个SnSe的沉积循环组成。通过FE-SEM观察了其形貌；利用XRD研究了其晶体结构；XPS表明沉积物中Se、Pb和Sn的比例约为1.0：0.8：0.2,与预期的化学计量比基本一致；开路电位技术(OCP)研究表明了该沉积物具有典型的p-型半导体性能,其良好的光电性质使其非常适合于制作光电开关。
3.用一步溶剂热法合成了磁性的ZnFe2O4/石墨烯(ZnFe2O4/rGO)复合物。研究发现在氧化石墨被还原成石墨烯的同时,ZnFe2O4粒子可直接负载在石墨烯的表面;H2O2的存在与分解可产生羟基自由基(·OH),使得ZnFe2O4/rGO体系具有较强的可见光-光催化活性,对有机物罗丹明B(RhB)、甲基橙(MO)和亚甲基兰(MB)能够快速降解；该复合物的磁性使其能在溶液中被磁性分离而循环使用。
4.将还原的氧化石墨(rGO)包覆于胺功能化Fe3O4磁性纳米球(AMs)表面,进而负载贵金属纳米粒子Pt,制得了具催化活性的Pt-rGO-AMs复合纳米材料。首先使Fe3O4表面氨基化使其带正电荷,然后通过静电层-层自组装包覆带负电荷的氧化石墨(GO)；再通过多元醇还原反应将Pt纳米颗粒负载在GO表面,同时GO被还原成rGO。所制备的催化剂Pt-rGO-AMs可以尽可能多的把Pt纳米颗粒暴露于材料的表面,因而对甲醇的催化氧化具有更好的电化学活性和稳定性。
5.在rGO包覆有胺功能化的Fe304磁性纳米球上负载PdPt合金催化层,制得了PdPt-rGO-AMs复合纳米材料。利用XRD、FE-SEM、透射电子显微镜(TEM)、拉曼光谱(Raman)等手段表征了该复合材料。电化学研究表明在相同条件下该材料对甲醇的催化活性比一元金属Pt-rGO-AMs更好、更稳定；当甲醇浓度在0.025到1.40mol/L的范围内时,甲醇的氧化峰电流密度与其浓度呈良好的线性关系,可用于甲醇的检测。
In this thesis, the author prepared CuInS2and several functional nanomaterials by electrochemical atomic layer deposition (EC-ALD) and organic phase synthesis methods. The materials were characterized by the surface analysis, the chemical composition analysis, the physical indicators analysis and a variety methods of the electrochemical analysis. Then their application in the field of photoelectric catalysis, degradation of organic compounds were explored. The contents of this thesis were described as follows:
1. The preparation and characterization of the Ⅰ-Ⅲ-Ⅵ2semiconductor compound CuInS2(CIS) on polycrystalline gold substrate at room temperature by EC-ALD method are reported. The optimum deposition potentials for each element are determined using cyclic voltammetry (CV) technique and Amperometric (I-t) method is used to prepare the semiconductor compound. Then, the thin films were characterized by X-ray diffraction (XRD) analysis, X-ray photoelectron spectroscopy (XPS), Field-emission scanning electron microscope (FE-SEM) and Fourier transform infrared spectroscopy (FT-IR). XRD results indicate that the CIS thin films have a (112) preferred orientation. The XPS analyses of the films reveal that Cu, In and S are present in an atomic ratio of approximately1:1:2. And their semiconductor band gaps are found to be1.50eV by FT-IR.
2. The preparation and characterization of IV-VI semiconductor Pb1-xSnxSe (x=0.2) thin films on polycrystalline gold substrate by EC-ALD method at room temperature are reported. CV and I-t technique are used to determine approximate deposition potentials for each element and prepare the semiconductor compound. The elements are deposited in the following sequence:(Se/Pb/Se/Pb/Se/Pb/Se/Pb/Se/Sn...), each period is formed using four ALD cycles of PbSe followed by one cycle of SnSe. The morphology of the deposit is observed by FE-SEM; XRD pattern is used to study its crystalline structure; XPS of the deposit indicates an approximate ratio1.0:0.8:0.2of Se, Pb and Sn, as the expected stoichiometry for the deposit. Open-circuit potential (OCP) studies indicate a good p-type property, and the good optical activity makes it suitable for fabricating a photoelectric switch.
3. Magnetic ZnFe2O4/graphene composites (ZnFe2O4/rGO) have been successfully synthesized by a facile one-pot solvothermal method. Graphene oxide (GO) was reduced to graphene and the ZnFe2O4particles were simultaneously grown on the graphene sheets under the conditions generated in the solvothermal system. Importantly, the ZnFe2O4/rGO composites show powerful visible-light-photocatalytic activity for the degradation of Rhodamine B (RhB), methyl orange (MO) and methylene blue (MB) in the presence of H2O2. Since it can generate a strong oxidant hydroxyl radical (OH) via photoelectrochemical decomposition. Due to the excellent magnetic properties such that they can easily be separated and recycled in the solution.
4. rGO-encapsulated amine functionalized Fe3O4magnetic nanospheres (AMs), were used to support Pt NPs. And the corresponding catalysts (Pt-rGO-AMs) also be prepared. The Pt-rGO-AMs were fabricated by modifying positively-charged aminopropyltrimethoxysilane on the surface of Fe3O4nanoparticles (NPs) to form functionalized Fe3O4NPs. Then negatively-charged graphene oxide (GO) was coated on the surface of the functionalized Fe3O4nanospheres by electrostatic layer-by-layer self-assembly. Finally, Pt NPs were uniformly anchored on the surface of GO by a polyol reduction reaction and the GO was simultaneously reduced to rGO. The electrochemical activity of the catalyst for methanol oxidation is significantly improved compared to Pt NPs absorbed on a rGO sheet and has better stability. The superior performance of this Pt-rGO-AMs catalyst is attributed both to the structure, which improve the accessibility of the Pt NPs by exposing them on the surface of the support, and to the greatly improved electronic conductivity of the support.
5. PdPt alloy nanoparticles anchored on graphene-encapsulated Fe3O4magnetic nanospheres (PdPt-rGO-AMs) were synthesized via a simple one-step chemical reduction method. The composites were characterized by XRD analysis, FE-SEM, TEM and Raman. Then the composites were used as catalysts for methanol oxidation in alkaline. The electrochemical results showed that the higher catalytic activity and stability than Pt-rGO-AMs under the same conditions. In addition, methanol electrooxidation process at the PdPt-rGO-AMs electrode was proved to be a diffusion process. Moreover, the anodic peak current was proportional to the concentration of methanol in the range of0.025-1.40M, which can be used for the detection of methanol. This study implies that the prepared catalysts are a promising catalyst for fuel cells.
1.采用EC-ALD法在多晶金基底上成功制备了Ⅰ-Ⅲ-Ⅵ2族的半导体化合物CuInS2(CIS)。具体是首先用循环伏安法(CV)确定了每种元素的最佳沉积电位,然后用计时电流法(I-t)制备了该半导体化合物。接下来利用X-射线粉末衍射仪(XRD)、X-射线光电子能谱仪(XPS)、场发射扫描电子显微镜(FE-SEM)和傅立叶变换红外光谱(FT-IR)等手段表征了所得CIS材料。XRD结果表明,CIS薄膜有(112)择优取向的晶体学性质；XPS分析表明,CIS薄膜中,Cu、In和S的原子比例约为1:1:2; FT-IR结果证明发现CIS材料的半导体带隙为1.50eV。
2.采用EC-ALD法在多晶金基底上制备了Ⅳ-Ⅵ族的半导体化合物Pb1-xSnxSe(x=0.2)薄膜。由CV法和I-t技术确定的各元素沉积顺序为：(Se/Pb/Se/Pb/Se/Pb/Se/Pb/Se/Sn...),即每个沉积周期分别是由四个PbSe和一个SnSe的沉积循环组成。通过FE-SEM观察了其形貌；利用XRD研究了其晶体结构；XPS表明沉积物中Se、Pb和Sn的比例约为1.0：0.8：0.2,与预期的化学计量比基本一致；开路电位技术(OCP)研究表明了该沉积物具有典型的p-型半导体性能,其良好的光电性质使其非常适合于制作光电开关。
3.用一步溶剂热法合成了磁性的ZnFe2O4/石墨烯(ZnFe2O4/rGO)复合物。研究发现在氧化石墨被还原成石墨烯的同时,ZnFe2O4粒子可直接负载在石墨烯的表面;H2O2的存在与分解可产生羟基自由基(·OH),使得ZnFe2O4/rGO体系具有较强的可见光-光催化活性,对有机物罗丹明B(RhB)、甲基橙(MO)和亚甲基兰(MB)能够快速降解；该复合物的磁性使其能在溶液中被磁性分离而循环使用。
4.将还原的氧化石墨(rGO)包覆于胺功能化Fe3O4磁性纳米球(AMs)表面,进而负载贵金属纳米粒子Pt,制得了具催化活性的Pt-rGO-AMs复合纳米材料。首先使Fe3O4表面氨基化使其带正电荷,然后通过静电层-层自组装包覆带负电荷的氧化石墨(GO)；再通过多元醇还原反应将Pt纳米颗粒负载在GO表面,同时GO被还原成rGO。所制备的催化剂Pt-rGO-AMs可以尽可能多的把Pt纳米颗粒暴露于材料的表面,因而对甲醇的催化氧化具有更好的电化学活性和稳定性。
5.在rGO包覆有胺功能化的Fe304磁性纳米球上负载PdPt合金催化层,制得了PdPt-rGO-AMs复合纳米材料。利用XRD、FE-SEM、透射电子显微镜(TEM)、拉曼光谱(Raman)等手段表征了该复合材料。电化学研究表明在相同条件下该材料对甲醇的催化活性比一元金属Pt-rGO-AMs更好、更稳定；当甲醇浓度在0.025到1.40mol/L的范围内时,甲醇的氧化峰电流密度与其浓度呈良好的线性关系,可用于甲醇的检测。
In this thesis, the author prepared CuInS2and several functional nanomaterials by electrochemical atomic layer deposition (EC-ALD) and organic phase synthesis methods. The materials were characterized by the surface analysis, the chemical composition analysis, the physical indicators analysis and a variety methods of the electrochemical analysis. Then their application in the field of photoelectric catalysis, degradation of organic compounds were explored. The contents of this thesis were described as follows:
1. The preparation and characterization of the Ⅰ-Ⅲ-Ⅵ2semiconductor compound CuInS2(CIS) on polycrystalline gold substrate at room temperature by EC-ALD method are reported. The optimum deposition potentials for each element are determined using cyclic voltammetry (CV) technique and Amperometric (I-t) method is used to prepare the semiconductor compound. Then, the thin films were characterized by X-ray diffraction (XRD) analysis, X-ray photoelectron spectroscopy (XPS), Field-emission scanning electron microscope (FE-SEM) and Fourier transform infrared spectroscopy (FT-IR). XRD results indicate that the CIS thin films have a (112) preferred orientation. The XPS analyses of the films reveal that Cu, In and S are present in an atomic ratio of approximately1:1:2. And their semiconductor band gaps are found to be1.50eV by FT-IR.
2. The preparation and characterization of IV-VI semiconductor Pb1-xSnxSe (x=0.2) thin films on polycrystalline gold substrate by EC-ALD method at room temperature are reported. CV and I-t technique are used to determine approximate deposition potentials for each element and prepare the semiconductor compound. The elements are deposited in the following sequence:(Se/Pb/Se/Pb/Se/Pb/Se/Pb/Se/Sn...), each period is formed using four ALD cycles of PbSe followed by one cycle of SnSe. The morphology of the deposit is observed by FE-SEM; XRD pattern is used to study its crystalline structure; XPS of the deposit indicates an approximate ratio1.0:0.8:0.2of Se, Pb and Sn, as the expected stoichiometry for the deposit. Open-circuit potential (OCP) studies indicate a good p-type property, and the good optical activity makes it suitable for fabricating a photoelectric switch.
3. Magnetic ZnFe2O4/graphene composites (ZnFe2O4/rGO) have been successfully synthesized by a facile one-pot solvothermal method. Graphene oxide (GO) was reduced to graphene and the ZnFe2O4particles were simultaneously grown on the graphene sheets under the conditions generated in the solvothermal system. Importantly, the ZnFe2O4/rGO composites show powerful visible-light-photocatalytic activity for the degradation of Rhodamine B (RhB), methyl orange (MO) and methylene blue (MB) in the presence of H2O2. Since it can generate a strong oxidant hydroxyl radical (OH) via photoelectrochemical decomposition. Due to the excellent magnetic properties such that they can easily be separated and recycled in the solution.
4. rGO-encapsulated amine functionalized Fe3O4magnetic nanospheres (AMs), were used to support Pt NPs. And the corresponding catalysts (Pt-rGO-AMs) also be prepared. The Pt-rGO-AMs were fabricated by modifying positively-charged aminopropyltrimethoxysilane on the surface of Fe3O4nanoparticles (NPs) to form functionalized Fe3O4NPs. Then negatively-charged graphene oxide (GO) was coated on the surface of the functionalized Fe3O4nanospheres by electrostatic layer-by-layer self-assembly. Finally, Pt NPs were uniformly anchored on the surface of GO by a polyol reduction reaction and the GO was simultaneously reduced to rGO. The electrochemical activity of the catalyst for methanol oxidation is significantly improved compared to Pt NPs absorbed on a rGO sheet and has better stability. The superior performance of this Pt-rGO-AMs catalyst is attributed both to the structure, which improve the accessibility of the Pt NPs by exposing them on the surface of the support, and to the greatly improved electronic conductivity of the support.
5. PdPt alloy nanoparticles anchored on graphene-encapsulated Fe3O4magnetic nanospheres (PdPt-rGO-AMs) were synthesized via a simple one-step chemical reduction method. The composites were characterized by XRD analysis, FE-SEM, TEM and Raman. Then the composites were used as catalysts for methanol oxidation in alkaline. The electrochemical results showed that the higher catalytic activity and stability than Pt-rGO-AMs under the same conditions. In addition, methanol electrooxidation process at the PdPt-rGO-AMs electrode was proved to be a diffusion process. Moreover, the anodic peak current was proportional to the concentration of methanol in the range of0.025-1.40M, which can be used for the detection of methanol. This study implies that the prepared catalysts are a promising catalyst for fuel cells.
引文
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