石墨烯纳米片的简易合成及其超级电容性能研究

以硫代氨基脲(CH₅N₃S)为还原剂, 通过还原氧化石墨(GO)制备了石墨烯纳米片(GNS)。利用XRD, FE-SEM, AFM和UV-Vis光谱对产物的结构和形貌进行分析, 并使用循环伏安和恒流充放电等测试手段来表征其超级电容性能。实验结果表明, 所制备的GNS具有良好的结晶状态, 并且在水溶液中具有良好的分散性。以GNS纳米片为电极材料, 在3 mol/L KOH电解质溶液中, 在500 mA/g电流密度测试条件下所得比电容量为75 F/g。而且GNS纳米片显示出了良好的电化学循环稳定性。     

膨胀石墨/纳米氧化锌/锌复合电极材料的超级电容器性能

以膨胀石墨为原料,与滚压振动磨预处理得到的纳米锌粉混合,超声分散24h制备膨胀石墨-纳米氧化锌及锌的复合电极材料(EG/ZnO/Zn)。采用X射线衍射仪(XRD)、场发射扫描电子显微(SEM)、场发射透射电子显微镜(TEM)、拉曼光谱分析仪(Raman),对材料的微观结构及成分表征。结果表明,复合材料中含锌和氧化锌,纳米锌粉颗粒和氧化锌纳米棒在膨胀石墨表面和层间分散良好,其中氧化锌纳米棒呈现出六方晶系纤锌矿结构,其直径大约为20nm。利用电化学循环伏安和恒电流充放电对材料进行电化学电容性能测试,表明经处理的复合电极材料在0.1A/g的电流密度下有明显的赝电容特性,比电容达147F/g,其赝电容来源不只是欠电位沉积的化学吸附,还有氧化还原反应。     

不同pH值对直接乙醇燃料电池Pt-SnO2/C 电催化性能的影响

采用水热法制备了高分散Pt-SnO2/C电催化剂,对制备工艺进行了最佳优化,考察了不同反应溶液pH值对电催化剂活性的影响。采用XRD、SEM、TEM、比表面积、粒度分析等手段对催化剂进行了结构表征。制备的Pt-SnO2纳米复合颗粒高度分散在活性炭载体表面,其平均粒径约4.5nm。通过循环伏安、计时电流、交流阻抗等技术测试了电极在乙醇体系中的电催化活性。结果表明,随着反应溶液pH值的增加,制备的Pt-SnO2/C催化剂可使乙醇的氧化发生在较低电位。在pH值为9、铂锡原子比为3∶1时,制备的Pt-SnO2/C复合催化剂,可以得到较高的乙醇氧化电催化活性和电化学长期稳定性,氧化峰电流密度高达104.54mA·cm-2。     

NiO@CeO_2纳米花材料的合成及其超级电容器性能

采用乙醇辅助的水热法制备了超级电容器NiO@CeO_2纳米花材料。利用X射线衍射(XRD)和扫描电镜(SEM)分别研究了材料的结构和形貌;采用循环伏安(CV)、恒流充放电测试以及电化学阻抗研究了材料的电化学性能。XRD表明,NiO@CeO_2电极材料与NiO具有相似的结构。SEM显示,NiO@CeO_2电极材料是由纳米片堆积而成。CV结果表明,NiO@CeO_2电极材料具有一对氧化还原峰。充放电测试结果表明,NiO@CeO_2电极材料具有较高的比容量和较好的循环稳定性。电化学阻抗结果表明,NiO@CeO_2电极材料在循环5000次之后阻抗增加是其容量降低的主要原因。     

全钒液流电池用碳纳米管-石墨复合电极的研究

将石墨(GP)和多壁碳纳米管(MWNT)按不同比例压片制成电极,用于全钒氧化还原液流电池电极材料,通过循环伏安、交流阻抗、充放电测试、SEM手段对MWNT-GP复合电极进行表征和分析.研究结果表明,MWNT含量为15wt%的MWNT-GP复合电极性能最佳,对组装成的静态电池在电流密度20~80mA/cm2进行充放电性能比较,电流效率均在93%以上,电压效率随着电流密度的增加而有所下降.     

水热电化学法制备LiCoO2薄膜和粉末

采用水热电化学法同时制备出LiCoO2粉末和薄膜.LiCoO2粉末是由菊花状晶粒组成,LiCoO2薄膜由0.2～0.4μm左右的颗粒堆积而成.LiCoO2薄膜电极首次循环伏安过程在3.85V和4.3V左右出现强氧化峰,在3.6V左右出现还原峰;LiCoO2粉末的首次循环伏安过程在4.3V左右出现强氧化峰,在3.5V左右出现还原峰;在随后的循环中,氧化和还原峰对应的电位和强度衰减程度小,表明该方法制备的LiCoO2正极材料具有良好的循环伏安性能.     

石墨粉末化学镀Ni-P催化剂表面乙醇的电催化氧化

电催化乙醇氧化的阳极材料易失效.在活性炭(C活性)上化学沉积Ni-P颗粒,制备了Ni-P/C活性催化剂,将其填入213型铂电极凹槽之中,制成Ni-P/C活性电极.采用扫描电镜(SEM)和电化学循环伏安法对Ni-P/C活性催化剂性能进行了研究.结果表明:球状Ni-P颗粒以约为100 nm的大小均匀分布于C活性表面;仅C活性电极能催化乙醇发生氧化,但易失活,而Ni-P/C活性电极可以催化乙醇在-0.24 V发生氧化,在阴极极化扫描过程中,-0.39 V时会出现乙醇氧化中间物的氧化峰,催化乙醇氧化的峰电流随循环使用次数的增加而提高,氧化电位逐渐负移,这与Ni-P在碱性条件下电氧化产生Ni(OH)2和NiOOH有关.     

淀粉还原制备纳米MnO_2超级电容器电极材料

采用氧化交联淀粉还原高锰酸钾制备出了超级电容器纳米MnO2电极材料.通过XRD和SEM对电极材料进行了表征,采用电化学测试手段对电极材料在lmol/L Na2SO4溶液中的电容特性和比容量进行了分析.结果表明,采用该方法所制备的材料为无定型的(а-MnO2,颗粒尺寸在100～150nm左右;循环伏安和恒流充放电试验测试结果表明,а-MnO2电极具有良好的电容特性.在放电电流为100 mA/g时,其比容量高达158 F/g.     

镍钴硫化物/碳微球电极的制备与电化学性能测试

采用水热法通过设置反应物的不同比例制备了不同镍钴比的硫化物,利用X射线衍射仪与扫描电子显微镜对制备产物进行表征。以制备产物为活性物质、碳微球为导电剂、泡沫镍为基体制备出可测电极。通过循环伏安法(CV)与恒电流充放电等电化学方法分析测试了不同电极的电化学性能。反应物中镍含量为50%(质量分数)的电极,其CV曲线表现出较大的氧化还原电流密度,且在测试条件下具有最高的比电容938.7F/g。     

纳米MoS2及MoS2-RGO纳米复合材料的制备与电化学性能研究

高性能电极材料的开发是推广新型储能器件的核心所在。二硫化钼(MoS_2)呈现类石墨烯结构,其二维层间具备良好的电荷储存能力。然而MoS_2本身导电性能较差,用于电极材料时需要与其它材料复合以提升导电性能。采用水热法,并分别选用抗坏血酸和硫脲作还原剂,制备得到两种不同形貌结构的纳米二硫化钼。以石墨烯为模板,采用水热法在石墨烯表面生长纳米结构MoS_2,制备得到二硫化钼-还原氧化石墨烯(MoS_2-RGO)纳米复合材料,通过循环伏安测试(CV)和恒电流充放电测试(CP)考察了复合材料的电化学性能。实验结果表明,MoS_2-RGO纳米复合材料呈现平面双电层电容性能,电流密度为1 A/g时,其比电容值达136.2 F/g。     

电极制备方法对球形Ni(OH)2循环伏安特性的影响

用镍粉和氢氧化镍压片制备了不同质量的氢氧化镍圆片电极进行不同扫描速度的循环伏安(CV)实验并和粉未微电极进行比较研究,结果表明：用压片法制得的圆片电极随质量的减小电极可逆性递增。在同一扫描速度下,不同电极的电流密度大致相同。以0．1gNi 0．03gNi(OH)2配比制得的圆片电极表现出较好的准可逆特性。鏊于其良好的质量可计量性,这种电极在CV测试中的重复性和可对比性好于粉未微电极。     

Electrochemical and morphologic studies of nickel incorporation on graphite electrodes modified with polytyramine

Electrodes modified with electropolymerized films have received considerable attention in the development of catalysts and sensors, and their use is rapidly increasing. This work reports modification of the surface of graphite electrodes by electrochemical polymerization of tyramine. These modified electrodes were used to nickel incorporation and hydrogen evolution. Tyramine electrooxidation, in acid and basic media, yielded polymeric films onto graphite surface. In ferrocyanide/ferricyanide solution, the electrodes modified in acid medium showed higher electron transfer efficiency. Impedance studies indicated higher charge transfer resistance to electrodes modified with Ptyr prepared in basic pH. Scanning electron microscopy showed that the formed films present different morphology for the several pH values studied. Interferometry and scanning electron microscopy analysis showed higher coverage to films formed in acid medium. Polymers produced in more alkaline medium present growth self-limited. Nickel was incorporated in the films through immersion of the modified electrodes in solution of potassium hexafluoronickelate, followed of electrochemical reduction of the metal. The electrocatalytic activity of the modified electrodes with nickel incorporated was tested for hydrogen evolution reaction. The amount of nickel mass incorporated as well as the current density of hydrogen evolution reaction was higher in electrodes modified with polytyramine produced in acid medium.     

超细镍粉的制备及还原生长机理研究

以联氨为还原剂,在硫酸镍水溶液中控制液相还原反应条件制备了超细镍粉,并讨论了超细镍粉的还原生长机理.通过实验分析了工艺参数对还原反应的影响,采用X射线衍射(XRD),扫描电镜(SEM),比表面积测定等分析手段对超细镍粉进行表征,结果表明:超细镍粉的形核和生长独立进行;温度、Ni2+浓度和pH值调控着溶液中镍离子的释放并...     

Preparation of nanostructured NiFe2O4 catalysts by combustion reaction

Nanosize nickel ferrite powders (NiFe₂O₄) have been prepared by combustion reaction using nitrates and urea as fuel. The resulting powders were characterized by X-ray diffraction (XRD), nitrogen physical adsorption (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and catalytic activity. The results showed nanosize nickel ferrite powders with high specific surface area (55.21 m²/g). The powders showed extensive XRD line broadening and the crystallite size calculated from the XRD line broadening was 18.0 nm. The nickel ferrite powder presented significant activity as catalyst for the water gas shift reaction, over the temperature range of 250–450 °C.     

A novel chemical reduction route toward fabrication of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> octahedrons and Fe tubes

Novel Fe₃O₄ octahedrons and Fe microtubes were successfully prepared in different alkaline concentration solutions by the reduction of hematite (α-Fe₂O₃) with hydrazine hydrate. The as-prepared powders were characterized in detail by conventional techniques such as X-ray diffraction and field emission scanning electron microscopy. The role of alkaline concentration during the reaction process is discussed in detail. Compared to the reaction in a water system, the reaction in ethanol required less sodium hydroxide and smaller particles were obtained. In addition, the magnetic properties of the samples were characterized using a vibrating sample magnetometer.     

紫外-可见光谱分析碳纳米管电泳液浓度对阴极场发射性能的影响

将酸化的碳纳米管(CNT)粉末、硝酸镁置于异丙醇溶剂中超声处理,制备成分散均匀的CNT电泳液.采用不同CNT浓度的电泳液在CrCuCr电极上电泳沉积CNT薄膜,并对阴极样品进行场发射性能测试;同时采用紫外-可见光谱仪对CNT电泳液进行光谱分析.结果表明,CNT浓度为0~0.13 g/L的电泳液在258 nm处存在光谱吸收,且其吸光度与相应CNT浓度呈良好的线性关系;当CNT浓度为0.12 g/L时电泳沉积制备的CNT阴极场发射性能较好,其开启电场为0.903 V/μm,当电场强度为1.395 V/μm时场发射电流密度为2.903 mA/cm2.利用紫外-可见光谱可以有效地分析电泳液中CNT浓度,为电泳沉积良好质量的CNT薄膜提供了保证.     

Large-scale and shape-controlled synthesis and characterization of nanorod-like nickel powders under microwave radiation

The nanorod-like nickel powders were fabricated via hydrothermal liquid phase reduction route under microwave irradiation with hydrazine hydrate as a reducing agent as well as polyvinyl alcohol as a dispersant and/or structure directing agent. The morphology and structure of as-prepared products could be easily tuned by adjusting process parameters such as pH value and microwave irradiation time. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscope, transmission electron microscopy and selected-area electron diffraction (SAED). The results demonstrated that pure nickel powders with face-centered cubic (fcc) structure were prepared at relatively mild condition and no characteristic peaks of nickel oxide in the XRD pattern were found. The phenomenon of lattice expansion for Ni powders was explained in details according to the XRD theory. As-prepared Ni sample was of obvious shape anisotropy with length diameter ratio of 5. Magnetic measurements shown that the magnetic properties of nanorod-like (fcc) Ni powders were quite different from those of hexagonal closed-packed (hcp) Ni nanoparticles. Furthermore, it had more strong ferromagnetic properties than that of Ni powders both bulk and nanoparticles.     

电化学研磨法制备超细镍粉

以锂离子电池为微反应器,电化学还原NiO制备了超细镍粉。X射线衍射结果表明所得粉末为纯相Ni,晶粒尺寸约5nm。激光粒度分布测试结果表明Ni粒度分布较窄,中位径集中在200～600nm。透射电镜照片显示颗粒粒径在80～200nm之间;放电电流密度的增加和放电温度的提高都使产物粒径有变大的趋势;在分散过程中加入不同的表面活性剂,可以提高产物Ni的分散性能。     

Microstructure and mechanical properties of nanocrystalline nickel prepared by pulse reverse microelectroforming

Nanocrystalline nickel was produced by pulse reverse microelectroforming. The pulse microelectroforming was also performed for the comparative purposes. The surface morphology and microstructure of electroformed nickel layers were investigated by scanning electron microscopy and X-ray diffractometry. The microhardness of nickel layers was measured with a Vickers microhardness tester. The friction and wear experiments for nickel layers were performed on a friction and wear tester. The results indicate that the nickel layers prepared by pulse reverse microelectroforming exhibit higher density and their grain sizes in the nanometer range. The nickel layers with fine grains, high microhardness and better wear resistance are obtained at positive current density of 20?A/dm² and negative current density of 2?A/dm². The microhardness and wear resistance of nickel layers are improved as the positive and negative current densities are increased.     

电沉积非晶Ni-Fe-P涂层析氢催化性能研究

采用直流电镀技术,通过改变电沉积电流密度制备了不同的非晶Ni-Fe-P涂层。采用稳态极化技术比较不同电流密度下电镀Ni-Fe-P合金涂层电化学催化析氢活性,发现电流密度200A/m2电沉积的Ni-Fe-P合金涂层的电化学催化析氢性能最好。通过XRD分析镀层相结构,SEM观察涂层表面的微观结构及EDX分析表面成分,研究影响非晶Ni-Fe-P合金涂层的析氢电催化活性原因。结果表明,影响非晶Ni-Fe-P合金涂层电催化活性的主要因素是镀层中Fe、P元素含量。当Fe的含量最大18.63%(原子分数),P的含量最小13.14%(原子分数)时,非晶Ni-Fe-P涂层电催化析氢活性最好。2