Fabrication of Nano Flower‐shaped Platinum on Glassy Carbon Electrode as a Sensitive Sensor for Lead Electrochemical Analysis

Platinum nanoflowers modified glassy carbon electrodes (PtNFs/GCE) was fabricated simply for lead determination in water samples. The modified electrodes were prepared by electrodeposition in hexachloroplatinic acid solution at constant potential. The influence of deposition time and potential on surface morphology, chemical composition, electrochemical properties of electrode were investigated. At ?0.2 V of potential and 150 s of deposition duration, platinum developed as nanoflower shape and scattered densely all over the glassy carbon surface, producing the largest electrochemically active surface areas. The highest differential pulse stripping voltammetry (DPSV) signal of lead was obtained by using the prepared electrode. Under optimized experimental condition of electrolyte, accumulation potential and time, the peak current was found to be linear proportion to lead concentration in range of 1 to 100 μg L^?1 (slope=0.371) with a limit of detection of 0.398 μg L^?1. The method has good repeatability and reproducibility with relative standard deviations of 1.47 % and 4.83 %, respectively. The modified PtNFs/GCE also demonstrated an excellent long‐term stability with only 9 % decrease in Pb peak current over 30 days. Moreover, the performance of the modified PtNFs/GCE in determination of Pb(II) in two industrial wastewaters was good agreement with data obtained by a graphite furnace atomic absorption spectrometry (GFAAS) method.     

Investigation of Fe−Ni Mixed‐Oxide Catalysts for the Reduction of NO by CO: Physicochemical Properties and Catalytic Performance

A series of Fe?Ni mixed‐oxide catalysts were synthesized by using the sol–gel method for the reduction of NO by CO. These Fe?Ni mixed‐oxide catalysts exhibited tremendously enhanced catalytic performance compared to monometallic catalysts that were prepared by using the same method. The effects of Fe/Ni molar ratio and calcination temperature on the catalytic activity were examined and the physicochemical properties of the catalysts were characterized by using XRD, Raman spectroscopy, N₂‐adsorption/‐desorption isotherms, temperature‐programmed reduction with hydrogen (H₂‐TPR), temperature‐programmed desorption of nitric oxide (NO‐TPD), and X‐ray photoelectron spectroscopy (XPS). The results indicated that the reduction behavior, surface oxygen species, and surface chemical valence states of iron and nickel in the catalysts were the key factors in the NO elimination. Fe_0.5Ni_0.5O_x that was calcined at 250 °C exhibited excellent catalytic activity of 100 % NO conversion at 130 °C and a lifetime of more than 40 hours. A plausible mechanism for the reduction of NO by CO over the Fe?Ni mixed‐oxide catalysts is proposed, based on XPS and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) analyses.     

ZIF67衍生硫化钴/多孔碳复合催化剂的制备及其电催化性能

采用离子交换法与热处理相结合的方法,以ZIF67为前驱体,硫代乙酰胺为硫源,制备出硫化钴/多孔碳(CoS/C)复合催化材料,并探讨了硫化时间对复合催化剂的形貌、结构及其氧还原(ORR)性能的影响。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)、N2吸附-脱附测定仪、X射线光电子能谱分析(XPS)、拉曼光谱仪(Raman)和旋转圆盘电极(RDE)技术表征催化剂的物理特征和电催化性能。研究结果显示,在碱性条件下该复合催化剂具有与20%(w/w)的商业Pt/C催化剂相媲美的ORR活性,其半波电位仅比Pt/C催化剂低31 mV。随着硫化时间的增加,硫化钴颗粒逐渐增大,催化剂中碳材料的无序程度出现先减小后增大的趋势。在硫化时间为10 min时,复合催化剂在0.1 mol·L-1KOH中表现出良好的电催化活性,且在ORR过程中复合催化剂的平均转移电子数可达到3.72,接近于4,说明氧气在该催化剂表面发生的是四电子转移过程。     

氮掺杂高比表面多孔碳的一步化学活化法制备及其超电容性能

以聚氨酯发泡剂为碳源和氮源,以氢氧化钾为活化剂,采用一步化学活化法制备了具有高比表面积的氮掺杂活性炭。采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、N_2吸附-脱附、X射线粉末衍射(XRD)、拉曼光谱(Raman)、光电子能谱(XPS)对碳材料的微观形貌、组成、比表面积和孔道结构进行了表征。结果表明,在700℃活化的碳材料FC700具有最高的比表面积(2 740 m~2·g~(-1))和最大的孔容(1.27 cm~3·g~(-1)),这归因于KOH与泡沫的充分相互作用。在以6.0 mol·L~(-1)KOH为电解液的三电极体系中,当电流密度为0.5 A·g~(-1)时,其比电容达到了452 F·g~(-1)。在组装的对称超级电容器中,其比电容达到了344 F·g~(-1),功率密度为247 W·kg~(-1)时对应的能量密度为11.9 Wh·kg~(-1)。在10 000次循环后电容保持率为98.03%,表现出优异的稳定性。FC700的优异电化学性能可能归因于高的比表面积,大的孔体积和氮原子的掺杂。     

氮化硼纳米管-纳米片分级结构的制备及光学和吸附特性

将五硼酸铵、 氨硼烷络合物和氧化镁混合, 球磨均匀后, 在1200 ℃及0.6 L/min流动氨气保护条件下退火6 h, 即可在氧化铝基片上收集到白色毛状产物. 采用X射线衍射(XRD), 红外光谱(FTIR)、 扫描电子显微镜(SEM)、 透射电子显微镜(TEM)、 拉曼光谱(Raman)、 紫外-可见吸收光谱(UV-Vis)和荧光光谱(PL)对产物进行了表征. 结果表明, 样品呈一维线状分级结构, 长度大于5 mm, 中间为竹节状空心结构, 内部管径为50~350 nm, 外径范围为200~800 nm. 分级结构表面负载了大量氮化硼(BN)纳米薄片, 单个薄片厚度约为13 nm. 薄片弯曲褶皱, 相互交织, 构成1个氮化硼片层, 其厚度约为50~200 nm. UV-Vis和PL光谱测试结果表明, 氮化硼纳米管(BNNT)分级结构在紫外光材料领域具有一定的应用潜力, 且对亚甲基蓝具有良好的吸附能力(7 min即可吸附71%, 107 min时可吸附96%). 对比实验结果表明, BNNT的生长机理遵循气-液-固相(VLS)模型, 而表面负载的超薄BN片的生长机理遵循气-固相(VS)模型.     

“蜡烛火焰划分”实验的局限成因分析及改进研究

人教版初中化学首个探究性实验"蜡烛及其燃烧"明确指出火焰的划分方法，但在实际教学中肉眼观察法和火柴梗燃烧法对蜡烛火焰的划分存在一定的局限性。采用文献研究法和实验验证法分析其局限性的成因——燃料的析炭能力强弱、材料结构的不同等，并提出相应的改进建议。     

The direct architecture of carbon fiber‐carbon nanofiber hierarchical reinforcements for superior interfacial properties of CF/epoxy composites

A simple and efficient chemical method was developed to graft directly carbon nanofibers (CNFs) onto carbon fiber (CF) surface to construct a CF‐CNF hierarchical reinforcing structure. The grafted CF reinforcements via covalent ester linkage at low temperature without any usage of dendrimer or catalyst was investigated by FTIR, X‐ray photoelectron spectroscopy, Raman, scanning electron microscopy, atomic force microscopy, dynamic contact angle analysis, and single fiber tensile testing. The results indicated that the CNFs with high density could effectively increase the polarity, wettability, and roughness of the CF surface. Simultaneous enhancements of the interfacial shear strength, flexural strength, and dynamic mechanical properties as well as the tensile strength of CFs were achieved, for an increase of 75.8%, 21.9%, 21.7%, and 0.5%, respectively. We believe the facile and effective method may provide a novel and promising interface design strategy for next‐generation advanced composite structures.     

Enantioselective synthesis of N-heterocycles via intramolecular Pd(0)-catalysed allylic amination

An efficient and stereoselective synthesis of pyrrolidine-, piperidine-, and azepane-type N-heterocycles is described by the intramolecular Pd(0)-catalysed cyclisation of amino allylic carbonates. The use of chiral ligands gave the corresponding heterocyclic derivatives having er values that were from moderate to good.     

碳纤维表面原位SiC纳米纤维的合成与生长

基于化学气相反应法,以高纯Si和SiO₂为反应源材料,在碳纤维表面原位生长β-SiC纳米纤维。采用XRD、SEM和TEM 等分析测试手段对SiC纳米纤维进行了表征分析,研究了不同反应温度和时间对生成β-SiC纳米纤维微观形貌和结构的影响,并探讨了β-SiC纳米纤维的生长机制。研究结果表明：采取化学气相反应法能够制备高质量、高纯度的β-SiC纳米纤维,纳米纤维的直径约为100~300 nm。随着反应温度的提高和时间的延长,纳米纤维的产额增加,且微观组织形貌发生了变化。结合制备过程和纳米纤维微观结构的观察分析,表明气-固(VS)机制是SiC纳米纤维生长的主要机理。