Effect of Restricted Geometry on the Structure and Phase Transitions in Potassium Nitrate Nanoparticles

The effect of restricted geometry and thermal prehistory of sample preparation on phase transitions in nanocomposites on base of porous glasses with average pore diameters 7 and 46 nm filled by potassium nitrate have been studied by X-rays and neutron diffraction. The nanoparticle sizes have been determined and phase diagrams (on cooling) for these nanoparticles have been described. It is shown that there is a critical nanoparticle size in the interval from 30 till 20 nm, at which in nanocomposite the ferroelectric phase is realized only regardless of preparation method.     

Application of Graphene as a Sorbent for Simultaneous Preconcentration and Determination of Trace Amounts of Cobalt and Nickel in Environmental Water and Vegetable Samples

A new method using a column packed with graphene as adsorbent was developed for the preconcentration of trace amounts of cobalt (Co) and nickel (Ni) prior to their determinations by flame atomic absorption spectrometry. Several factors influencing the extraction efficiency of Co and Ni and their subsequent determinations, such as pH, amounts of the chelating agent, flow rates of sample and eluent solution, eluent type and its volume, breakthrough volume, and adsorption capacity were established. Under the optimum conditions, the calibration graphs were linear in the range of 4.0‐200.0 μg L^?1 and 5.0‐200.0 μg L^?1 with detection limits of 0.36 μg L^?1 and 0.51 μg L^?1 for Co and Ni, respectively. Good relative standard deviations for ten determinations of 100.0 μg L^?1 of Co and Ni were 3.2 and 3.6%, respectively. The results for determination of Co and Ni in tap water, river water, sea water, vegetable and spiked samples have demonstrated the accuracy and applicability of the proposed method. To validate the proposed method, three certified reference materials of environment water (GSBZ 50030‐94 and GSB 07‐1186‐2000) and tomato leaf (GSBZ 51001‐94) were analyzed, and the determined values were in good agreement with the certified values.     

Facile and green synthesis of Co3O4 nanoplates/graphene nanosheets composite for supercapacitor

Journal of Solid State Electrochemistry - A series of Co3O4 nanoplates/graphene nanosheets (GNS) composites are fabricated using a facile and green method by hydrothermal treatment and subsequent...     

Direct observation of bulk and surface chemical morphologies of Ginkgo biloba leaves by Fourier transform mid- and near-infrared microspectroscopic imaging

Fourier transform infrared microspectroscopy is a powerful tool to obtain knowledge about the spatial and/or temporal distributions of the chemical compositions of plants for better understanding of their biological properties. However, the chemical morphologies of plant leaves in the plane of the blade are barely studied, because sections in this plane for mid-infrared transmission measurements are difficult to obtain. Besides, native compositions may be changed by chemical reagents used when plant samples are microtomed. To improve methods for direct infrared microspectroscopic imaging of plant leaves in the plane of the blade, the bulk and surface chemical morphologies of nonmicrotomed Ginkgo biloba leaves were characterized by near-infrared transmission and mid-infrared attenuated total reflection microspectroscopic imaging. A new self-modeling curve resolution procedure was proposed to extract the spectral and concentration information of pure compounds. Primary and secondary metabolites of secretory cavities, veins, and mesophylls of Ginkgo biloba leaf blades were analyzed, and the distributions of cuticle, protein, calcium oxalate, cellulose, and ginkgolic acids on the adaxial surface were determined. By the integration of multiple infrared microspectroscopic imaging and chemometrics methods, it is possible to analyze nonmicrotomed leaves and other plant samples directly to understand their native chemical morphologies in detail.

Preparation of a new metallomicelle catalyst for the hydrolysis of bis(4-nitrophenyl) phosphate

A new metallomicellar system containing cerium(III), a macrocylic polyamine ligand, and the nonionic surfactant Brij35(polyoxyethylene(23) lauryl ether) was prepared and used as a catalyst in the hydrolysis of bis(4-nitrophenyl) phosphate (BNPP). Catalytic rate of the BNPP hydrolysis was measured kinetically using the UV-VIS spectrophotometric method. The results indicate that the metallomicellar system has relatively high stability and excellent catalytic function in the BNPP hydrolysis; also, the reaction rate of the BNPP catalytic hydrolysis increased by a factor of ca. 1 × 10¹⁰ compared to the BNPP spontaneous hydrolysis due to the catalytic effect of the active species and the local concentration effect of the micelles in the metallomicellar system. Experimental results also showed that the mono-hydroxy complex containing the macrocyclic polyamine ligand and cerium(III) is the real active species in the BNPP catalytic hydrolysis, and that the micelles provide a useful catalytic environment for the reaction. On basis of the research results, the reaction mechanism of BNPP catalytic hydrolysis has been proposed.     

Buildup mechanism of carboxymethyl cellulose and chitosan self-assembled films

Films with different numbers of layers have been built by alternating the adsorption of carboxymethyl cellulose (CMC) and chitosan (CHI) at different pH levels. The adsorption process was recorded by quartz crystal microbalance (QCM). The results showed that under all pH conditions considered, the growth of the films is nonlinear. The film construction performed at pH 4.0 (preferred assembly pH) with different numbers of bilayers (CMC/CHI as one bilayer) was also observed step by step by atomic force microscopy (AFM). Comparing the growth process from QCM with the surface morphological changes from AFM shows the existence of an inhomogeneous structure for the first nine bilayers, and, after a coalescence of islands, an increase in the number of bilayers was demonstrated. The possible growth mechanism was also evaluated.     

Facile and surfactant-free synthesis of SnO<Subscript>2</Subscript>-graphene hybrids as high performance anode for lithium-ion batteries

A facile microwave-assisted ethylene glycol method is developed to synthesize the SnO₂ nanoparticles dispersed on or encapsulated in reduced graphene oxide (SnO₂-rGO) hybrids. The morphology, structure, and composition of SnO₂-rGO are investigated by scanning electron microscopy, transmission electron microscope, thermo-gravimetric analyzer, X-ray diffraction, Raman spectroscopy, and X-ray photoelectron spectroscopy. The electrochemical performance of SnO₂-rGO as anode materials for lithium-ion batteries was tested by cyclic voltammetry, galvanostatic charge–discharge cycling, and rate capability test. It is found that the SnO₂ nanoparticles with a uniform distribution have p-type doping effect with rGO nanosheets. The as-prepared SnO₂-rGO hybrids exhibit remarkable lithium storage capacity and cycling stability, and the possible mechanism involved is also discussed. Their capacity is 1222 mAhg^?1 in the first cycle and maintains at 700 mAhg^?1 after 100 cycles. This good performance can be mainly attributed to the unique nanostructure, good structure stability, more space for volume expansion of SnO₂, and mass transfer of Li⁺ during cycling.     

基于氮掺杂碳载铁复合物的锌空电池氧阴极催化剂

迫在眉睫的环境和能源问题推动人类探索可行、可靠和可再生的能源技术.锌-空气电池和氢氧燃料电池等器件显示出高能量转换效率,但是仍有许多难题有待克服,例如阴极侧上缓慢的氧还原反应(ORR),以及高昂的成本极大地限制了铂基催化剂在商业上的广泛应用.因此,开发高性能的廉价ORR催化剂具有重要意义.过渡金属碳氮化合物(M-N-C, M=Co, Fe等)成为最有希望替代铂基催化剂的一类材料, M-N-C催化剂可以通过直接热解含有过渡金属、氮和碳物种的前驱体合成.然而热解时金属原子易团聚,多孔结构不能被有效地控制,导致相对较差的催化活性.目前, MOF衍生的催化剂在能源转化和储存技术中得到了广泛的关注,其具有丰富的氮含量、高比表面积和可调的孔道结构等特点.本文报道了一种简便可靠可控的合成铁氮共掺杂碳十二面体纳米结构催化剂的方法,并作为阴极电催化剂用于锌空气电池中,测试结果证实,合成的铁氮共掺杂的纳米碳具有与铂基材料相当的活性和更加优异的稳定性.表面吸附了的邻菲罗啉铁的ZIF-8在碳化过程中,氮基团能够结合铁形成Fe Nx结构单元,因此可得到铁氮共掺杂的电催化剂.粉末X射线衍射,扫描电镜证实ZIF-8的成功合成.经过热解得到的催化剂中Fe Nx或Fe Cx衍射峰较弱,表明样品中铁含量较低,存在部分无定型铁.通过拉曼光谱分析发现,引入的邻菲罗啉在热解过程中诱导了缺陷的形成,所以Fe-NCDNA-0的ID/IG比值明显高于NC.同时ID/IG随着铁含量的增加而减少,这是因为铁可以诱导石墨化,诱导效应随着铁含量的增加而增加.分析氮气吸附-脱附等温线得出,引入邻菲罗啉之后,比表面积增加;而铁的引入因其占据了微孔结构,导致比表面积下降.同时电镜证实Fe-NCDNA-2具有较大的形貌扭曲,使得该材料具有较大的比表面积.系统的电化学研究表明,氮掺杂有利于增强ORR活性,在引入铁之后形成高效的活性中心会进一步提高催化性能.因此, Fe-NCDNA-2在碱性条件下表现出优异的ORR性能.线性扫描伏安法曲线表明,铁氮共掺杂的材料表现出与Pt/C相似的性能,其中Fe-NCDNA-2的半波电位(E1/2)为0.863 V,比商业Pt/C的电位更正(E1/2=0.841 V).同时, Fe-NCDNA-2具有更加优异的稳定性,测试30000 s后的电流保持率为80%(Pt/C:64%).在中性介质中,合成的材料也展示了较高的ORR活性.Fe-NCDNA-2的E1/2=0.715 V,催化30000 s后电流保持率77%,均优于商业Pt/C催化剂.组装的锌空气电池进一步验证其作为氧还原催化剂实际应用的可行性.相比于以Pt/C为催化剂做空气阴极的电池,以Fe-NCDNA-2组装的电池表现出更高的开路电压,更高的功率密度(184 m Wcm^-2),以及更加优异的充放电循环稳定性.该工作也有利于启发研究人员探索类似的氮掺杂过渡金属碳材料在各种催化上的应用.     

紫外熔石英元件高精度低缺陷控形控性制造技术研究进展

传统的紫外熔石英元件加工方法本身会引入各类制造缺陷,需要后期加工来消除前期加工带来的缺陷,限制了熔石英元件的加工质量和加工效率。针对这些问题,课题组提出了采用磁流变、离子束、保形光顺和流体动压抛光等可控柔体加工技术提升熔石英元件的加工效果,并开展了相关研究。主要介绍了课题组在关键技术上取得的重要进展,包括亚纳米精度表面控形制造技术、纳米精度本征表面控性生成方法、熔石英元件高精度低缺陷组合工艺与设备等一系列关键技术。通过探讨关键技术及其发展现状,为未来紫外熔石英元件高精度低缺陷制造技术的发展提供参考。