水热法制备纳米片组装氧化铜微球的研究

本论文制备了由纳米片组装的粒径3-5μm的球形CuO,并通过XRD、SEM、TEM、TPR和氮气吸附对其结构和性能进行了表征。结果表明：CuO微球为单斜对称晶型,且由CuO纳米片组装而成,比表面积为18．5m2／g,BJH-PSD曲线中最大孔分布在29．6nm。     

基于海藻制备超级电容器用三维多孔石墨烯

以海藻作为固相碳源,利用海藻对金属离子具有吸附性能的特点,在未进行生物质材料改性的条件下,实现海藻生物质材料对催化剂金属离子的均匀吸附.本文结合原位高温金属催化和化学活化的方法制备三维多孔石墨烯,并研究了其作为超级电容器电极材料的电化学性能.通过扫描电镜、透射电镜、X射线衍射、拉曼光谱、氮气吸附等手段对三维多孔石墨烯的形貌与结构进行表征分析.研究结果表明,制备的三维多孔石墨烯具有片层状三维网络结构,且片层较薄,并具有较高的石墨化程度,其比表面积达到1 700 m~2/g,孔径分布主要在2~10 nm.以该三维多孔石墨烯材料作为超级电容器电极材料,进行电化学性能表征,发现在较低的电压扫速下得到的比电容量为90 F/g,同时,该材料还具有较高的能量密度和功率密度.以海藻为固相碳源制备得到的三维多孔石墨烯材料在超级电容器领域具有一定的应用前景.     

NiO/AC非对称电容器电极材料的制备及性能研究

以硫酸镍为原料、氨水为沉淀剂, 采用化学沉积法成功制备出氧化镍纳米颗粒, 分别采用X射线粉末衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、热重分析仪(TGA)、物理吸附仪等测试手段对纳米氧化镍的物相、形貌和结构进行分析和表征。结果表明, 所制得的纳米氧化镍为球形多孔颗粒, 直径大约为200 nm。其中在300℃下热处理得到的氧化镍比表面积最大, 为132 m²/g, 平均孔径为7.3 nm。将其作为正极, 活性炭作为负极, 组装成非对称电容器, 结果表明非对称电容器具有良好的电容性能和循环稳定性, 在25 mA/g电流密度下, 比电容达到1039 F/g, 充放电效率高达98%以上。     

以枫叶为模板合成分级多孔氧化铈材料及其催化性能

以枫叶为生物模板合成了由纳米颗粒构成的分级多孔氧化铈材料. 采用场发射电子显微镜(FESEM)、透射电子显微镜(TEM)和氮气脱吸附技术表征了材料的独特生物形态微结构, 其仿生结构是由复制气孔得到的微米孔和复制细胞孔得到的2~4 nm的小孔构成. 通过广角X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)和BET计算发现多孔氧化铈具有很小的晶粒(6~8 nm)和较大的比表面积(64.4 m²/g). 利用化学储氧量(OSC)评价了样品催化性能, 结果表明: 分级多孔氧化铈比无孔氧化铈含有更多的表面活性氧. 当将材料用于酸性品红脱色反应, 由于分级多孔氧化铈材料的颗粒小, 比表面积大和化学储氧量高, 其在染料废水净化处理时具有较好的催化活性和吸附能力, 到300 min时脱色率可达到100%.     

CuO－SnO_2纳米晶粉料的Sol－Gel制备及表征

不用金属醇盐而以无机盐为起始物质，采用Ｓｏｌ－Ｇｅｋ法得到了平均晶粒尺寸为２１～２２ｎｍ，ＣｕＯ掺杂的ＳｎＯ_２粉料；运用Ｘ射线衍射（ＸＲＤ）、差热—失重分析（ＤＴＡ－ＴＧ）、透射电镜（ＴＥＭ）及ＢＥＴ比表面（ＳＡ）测定等分析手段对粉料进行了表征．实验表明，ＣｕＯ的掺杂抑制了ＳｎＯ_２晶粒的生长；以无机盐为原料，采用Ｓｏｌ－Ｇｅｌ法制取ＳｎＯ_２（ＣｕＯ）纳米级晶料是切实可行的，将有利于产业化．     

分级介孔结构组成的ZnO微球及光催化性能

以硝酸锌、脲素及酒石酸为反应物, 采用水热法制备碱式碳酸锌前驱体微球, 通过煅烧前驱体制备了介孔氧化锌微球。通过扫描电子显微镜(SEM)可以观察到, 氧化锌微球的直径约为2~4 μm, 由大量厚度约为10 nm的介孔纳米片组装而成。X 射线衍射(XRD)和透射电镜(TEM)结果表明: ZnO微球为六方纤锌矿结构, 并结晶较好。比表面积测试(BET)表明ZnO微球为介孔材料, 孔径为20~50 nm, ZnO微球比表面积约为29.8 m²/g。以亚甲基蓝为目标降解物, 对介孔氧化锌微球进行了光催化降解实验。实验结果表明, 所合成的介孔ZnO微球对亚甲基蓝的光催化性能较好。     

聚苯胺/氧化铜纳米复合材料的制备及抗菌性能

通过水热法制得长2μm,直径100 nm~200 nm的氧化铜纳米棒,然后以此纳米棒采用原位聚合法得到了聚苯胺/氧化铜纳米复合材料。并用傅立叶红外光谱（FT-IR）、扫描电镜（SEM）、热重分析（TG）等测试方法对所得复合材料进行了表征。结果表明,聚苯胺对纳米氧化铜表面包覆,得到了棒状核壳结构的复合材料,当氧化铜添加质...     

Preparation and photocatalytic property of porous CuO hollow microspheres via carbon sphere templates

Porous copper oxide (CuO) hollow microspheres have been successfully fabricated by using carbon spheres as templates. The products were characterized by scanning electron microscopy (SEM), X-ray diffractometry (XRD) and Fourier transform infrared spectroscopy (FTIR). The influences of different experimental parameters on the morphology of CuO structures have been investigated in detail and the possible formation mechanism of porous CuO hollow microspheres has also been proposed. The specific surface area of the hollow spheres with 74.805 m2/g is measured by BET method. Barrett-Joyner-Halenda (BJH) calculations for the pore size distribution, derived from desorption data, reveal that the average pore radius is 8.56 nm, and the total pore volume (r = 1686.1 A, P/P0 = 0.994296) is 0.107257 cc/g. UV-vis absorption spectrum shows quantum size effect of porous CuO hollow microspheres. Furthermore, the porous CuO hollow microspheres exhibit high efficiency for photodegradation of a sample organic dye, Rhodamine B (RhB), under UV light.     

CuO nanoparticle decorated ZnO nanorod sensor for low-temperature H2S detection

CuO nanoparticle decorated porous ZnO nanorods were synthesized via a two-stage solution process. First, porous ZnO nanorods were fabricated by a low-temperature hydrothermal method. Afterward, the porous ZnO nanorods were used as supports to load CuO nanoparticles by a non-aqueous solution method. The morphology and structure of the prepared samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). To demonstrate the practical application of the synthesized heterostructured porous CuO/ZnO nanorod hybrid, the sensing properties for H₂S at low operating temperatures were investigated. The high sensitivity, reversible response and good selectivity indicated its potential application as a chemical sensor.     

Preparation and magnetic properties of spindle porous iron nanoparticles

Spindle porous iron nanoparticles were firstly synthesized by reducing the pre-synthesized hematite (α-Fe₂O₃) spindle particles with hydrogen gas. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption/desorption isotherms and vibrating sample magnetometry (VSM). A lattice shrinkage mechanism was employed to explain the formation process of the porous structure, and the adsorbed phosphate was proposed as a protective shell in the reduction process. N₂ adsorption/desorption result showed a Brunauer-Emmett-Teller (BET) surface area of 29.7 m²/g and a continuous pore size distribution from 2 nm to 100 nm. The magnetic hysteresis loop of the synthesized iron particles showed a saturation magnetization of 84.65 emu/g and a coercivity of 442.36 Oe at room temperature.     

Ultrasound assisted one pot synthesis of nano-sized CuO and its nanocomposite with poly(vinyl alcohol)

The ultrasound (US) assisted one pot method has used to synthesize CuO nanoparticles. The fourier transform infrared spectroscopy (FTIR) spectrum shows a characteristic peak of metal–oxygen bond at 535 cm⁻¹, which confirms the CuO formation. The high resolution transmission electron microscope (HRTEM) images of the synthesized nano-CuO confirms the size of nanorods with the length of approximately 25–30 nm, and its breadth is less than one nanometer. X-ray diffraction (XRD) pattern of CuO can be readily assigned to those of crystalline CuO, indicating the formation of single-phase CuO with monoclinic structure. The synthesized nano-CuO is mixed with poly(vinyl alcohol) (PVA) to prepare the PVA/CuO nanocomposite to improve the thermal stability of PVA. Their physico-chemical properties are examined by means of FTIR, XRD, differential scanning calorimetry, thermogravimetric analysis, HRTEM, and scanning electron microscope (SEM) techniques.     

Ferromagnetic behavior of copper oxide-nanowire-covered carbon fibre synthesized by thermal oxidation

Copper oxide nanowires were synthesized on carbon fibre surfaces by annealing of copper thin films at 400 °C for 4 h in air. The nanowires were characterized with field emission scanning electron microscope (FESEM), transmission electron microscope (TEM) and X-ray diffraction (XRD). The magnetic properties of CuO nanowires were measured with a vibrating sample magnetometer (VSM). Its diameters range covered 40–100 nm and lengths range covered 1–3 μm. It is interesting that the CuO nanowires on the carbon fibres showed ferromagnetism at room temperature.     

Hierarchical meso–macroporous titania-supported CuO nanocatalysts: preparation,characterization and catalytic CO oxidation

Hierarchically mesoporous–macroporous titanium dioxide (MMTD) was synthesized by the hydrolysis of tetrabutyl titanate in the absence of surfactant and autoclaving at 60 °C, which exhibits a porous hierarchy of wormhole-like mesostructure in the framework of macrochannels. Different contents of CuO nanoparticles were supported on the MMTD by a deposition–precipitation (DP) method, retaining the high surface areas and hierarchical porosity. The prepared MMTD support and the resulting CuO/MMTD nanocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N₂ adsorption analysis, temperature-programmed reduction (TPR), and X-ray photoelectron spectroscopy (XPS) techniques. Their catalytic behavior for low-temperature CO oxidation was studied by using a microreactor–GC system, and the CuO/MMTD catalyst with 8 wt% CuO content and calcined at 400 °C was found to have the highest catalytic activity. The catalytic activity depended on the CuO loading amount, the precalcination temperature, the meso–macroporous framework, the surface area, and the particle size of the CuO/MMTD catalysts.     

碳化铈水解氧化法制备CeO2纳米粉

提出了一种可大规模制备CeO2纳米粉的有效方法.用碳化铈水解氧化制得颗粒大小为3~5 nm的CeO2纳米粉.研究了各种实验参数包括水解温度、反应时间和投料比对CeO2纳米粉比表面积的影响.结果表明:较低的水解温度(室温附近),较高的投料比(1:20(g/mL))和适当的反应时间(18 h)可得到比表面积为149 m2/g的CeO2纳米粉.优化实验参数(水解温度为30℃,水解时间为18 h,投料比为1:20(g/mL),滤饼在空气中80℃烘干4 h)得到中间产物Ce(OH)3和目标产物CeO2,并用XRD、TEM、SAED及紫外可见光分光光度计进行测试表征.发现Ce(OH)3是由大量长为50~100 nm,直径为5~20 nm的纳米棒组成.CeO2纳米粉具有较高的紫外吸收性能和较好的催化CO性能.     

An efficient chemical precipitation route to fabricate 3D flower-like CuO and 2D leaf-like CuO for degradation of methylene blue

A facile and eco-friendly way for fabrication of CuO is developed based on an one-step chemical precipitation route without calcination procedure or use of surfactant. The structure features of as-prepared CuO are characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and N₂ adsorption-desorption experiment. X-ray diffraction analysis shows that CuO with particle size of 13.5–19.2 nm and crystallinity of 67.0–72.9% can be fabricated by the transformation of Cu(OH)₂ precursor at bath temperature above 50 °C. By adjusting the oil bath temperature and the content of ammonium hydroxide, we demonstrate a formation mechanism to control CuO to be 2D leaf-like structure with large specific surface area of 33.4 m²/g and pore volume of 0.226 cm³/g, or 3D flower-like ones with specific surface area of 7.45–18.7 m²/g and pore volume of 0.0249–0.0850 cm³/g. The catalytic performances of as-prepared CuO are evaluated by monitoring degradation of methylene blue in the presence of hydrogen peroxide. Almost 100% methylene blue degradation rate can be reached after reaction for 210 min on 3D flower-like CuO synthesized with 10 mL ammonia content in oil bath of 50 °C. The high activity can be correlated with the morphology and pore volume of CuO. The present synthetic strategy is an inexpensive and convenient way suitable for large-scale fabrication of copper oxides, which are potential catalysts for organic compounds degradation.     

多孔硅/碳复合负极材料的制备及电化学性能

以介孔二氧化硅SBA-15为硅源, 采用镁热还原法和化学气相沉积(CVD)法合成了具有莲藕状结构的多孔硅/碳复合材料。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和氮气吸脱附法研究了原料配比, 混压方式以及反应温度对多孔硅物相组成和结构形貌的影响。多孔硅的最佳合成条件为: 镁粉过量20wt%, 原料经球磨混合均匀后直接在750℃下高温反应4 h。对多孔硅及多孔硅/碳材料进行了电化学性能测试, 在0.5 A/g电流密度下循环70次后仍保持1633.1 mAh/g的可逆容量, 并且在8 A/g下容量达到580.1 mAh/g, 表现出优异的循环稳定性以及倍率性能。     

NiO微球的微波辅助合成及电荷传导能力优化

为了优化电荷传导特性, 提高电极的电化学性能, 本工作采用微波辅助合成了分级多孔结构的氧化镍微球。通过XRD、SEM和TEM对产物的形貌进行了表征。研究结果表明, 开放多孔结构的氧化镍微球是由极薄纳米片自组装而成, 以硫酸镍为镍源, 得到的氧化镍微球的粒径约为2 µm。作为超级电容器电极材料, 在电流密度为0.5 A/g时, 电极的比容量达到455 F/g, 由于NiO微球独特的多孔特性, 使电极表现出良好的阻抗特性, 为法拉第反应过程提供了较多的活性反应点, 从而提高了电极的电容性能。     

Single Crystal Fe Nanowire Arrays Encapsulated by SiO2 Nanotubes

Aligned silicon dioxide nanotubes with diameter of 60-70 nm were synthesized inside the nanoholes of an anodic AI membrane (AAM) template by pressure impregnating the AAM pores with the SiO_2 sol. The Si0_2 nanotubes with different wall thickness were produced by repeating the process. Using the second-order template of porous AAM with silicon dioxide nanotubes, it was fabricated the nanostructure of Fe nanowires encapsulated by SiO_2 nanotubes by electrochemical deposition. Scanning electron microscope (SEM) and transmission electron microscope (TEM) observations show that the nanotubes and nanocables are compact, continuous and uniform. Selected area electron diffraction (SAED) pattern shows the Fe nanowire is a single crystal. The magnetic properties of these samples were checked by a vibrating sample magnetometer (VSM). The coercivities of the samples are greatly improved compared to the corresponding bulk materials.     

纳米钯/铁双金属颗粒对一氯乙酸的脱氯

为了提高零价铁对氯代有机物还原脱氯的性能,采用还原沉淀法制备了纳米钯/铁双金属颗粒.利用X射线衍射(XRD)、X射线荧光光谱(XRF)、扫描电子显微镜(SEM)、透射电镜(TEM)、以及BET-N2比表面积法对纳米钯/铁双金属颗粒进行了表征.结果表明,制备的纳米钯/铁双金属颗粒中Fe主要以α-Fe0形式存在.纳米钯/铁双金属颗粒的直径约为30～50nm,比表面积约51m2/g.纳米钯/铁双金属颗粒对一氯乙酸还原脱氯的脱氯率是还原铁粉和纳米铁粉对一氯乙酸还原脱氯的脱氯率的7.9倍和1.7倍.     

棒状多孔NiCo2O4粉末的可控制备及其电催化性能研究

以NiCl₂·6H₂O, CoCl₂·6H₂O和草酸为原料, 利用氨水为配位剂和溶液pH调节剂, 通过配位共沉淀-热分解法制备了棒状多孔NiCo₂O₄粉末, 采用X射线衍射、扫描电镜、透射电镜以及比表面积仪对前驱体和NiCo₂O₄粉末的形貌和结构进行了表征, 考察了溶液pH对前驱体粉末形貌和分散性的影响; 采用循环伏安法和计时电流法研究了乙醇在棒状多孔NiCo₂O₄粉末修饰的玻碳电极上的电催化性能。结果表明: 前驱体的形貌与溶液的pH有关, 热分解得到的NiCo₂O₄粉末继承了前驱体形貌, 呈多孔棒状, 比表面积为89 m²/g, 平均孔径为12.56 nm。该粉末对乙醇具有良好的电催化活性, 氧化峰电流与乙醇浓度、扫速的平方根均呈直线关系, 表明棒状多孔NiCo₂O₄粉末对乙醇的催化反应机理为扩散控制。