纳米氧化锌的合成及表面改性

以硫酸锌、尿素为原料,采用均相沉淀法合成了纳米氧化锌.研究了硬脂酸对所制的纳米氧化锌粉体表面改性的机理及其对粉体亲油性的影响.实验结果表明,硬脂酸中的羧基与纳米氧化锌粉体颗粒表面的羟基发生了酯化反应,并在表面形成单分子膜.经过表面改性的纳米氧化锌由亲水性转化为亲油性.同时,就纳米氧化锌粉体硬脂酸表面改性反应,探讨了反应摩尔分数、反应温度和反应时间对产物的影响,从而筛选出粉体亲油性最大的反应条件为:硬脂酸质量分数为7%;反应温度为50℃;反应时间为1h.     

复合掺杂氧化物La0.5Sr0.5CoO2.91的性能和稳定性

采用固相反应法和柠檬酸-硝酸盐溶胶-凝胶低温自蔓延燃烧法（简称柠檬酸法）合成了La0.5Sr0.5CoO2．91（LSC）复合氧化物。借助XRD和SEM对不同制备方法合成粉体的晶体结构和晶粒形貌进行了研究。结果表明：固相反应法可制得均一钙钛矿结构的LSC氧化物，柠檬酸法除制得LSC氧化物外，还有LaSrCoO4相的生成。柠檬酸-硝酸盐溶胶-凝胶低温自蔓延燃烧法合成粉体的粒度相对较小。为研究以Ce0．9Gd0.1O1．95（GDC）为电解质的固体氧化物燃料电池阴极材料的性能，将LSC粉体与GDC粉体按6：4（质量比）制备了固体氧化物燃料电池（SOFC）的阴极片。在空气气氛下使用直流四探针法研究了烧结样品300～800℃的电导率，发现由柠檬酸法得到粉体制备的阴极片的电导率值较高。将制备的样品置于马弗炉中800℃条件下烧结800h，比较失效前后电导率的变化情况，并借助XRD，SEM等测试手段分析样品电导率变化的原因。分析发现，失效后两种样品的电导率值都有所降低，且样品中都有新相生成，晶体形貌有较大的变化。     

低温燃烧法制备Nd:YAG透明激光陶瓷粉体

以硝酸盐和柠檬酸为初始原料，用低温燃烧法制备出掺钕钇铝石榴石（Nd：Y3Al5O2，Nd：YAG）多晶超细粉体，并采用XRD，SEM等测试手段对粉体的结构和形貌进行了表征。结果表明，在950oC煅烧2h得到了结晶性能良好的Nd：YAG超细粉体，该粉体分散均匀、粒级分布窄、平均粒度为50nmo上述粉体加入0．5％正硅酸乙酯成型后，采用SPS于1600℃，30MPa下烧结5min后相对密度达98．5％，晶粒尺寸在1μm左右，显微结构均匀，气孔率低。     

微乳法制备纳米级WO3粉体

以最佳重量比６：４的∈ＣＨ２－ＣＨＯＨ）ｎ和ＣＨ３Ｃ１０Ｈ２２ＣＯＣＨ（ＯＨ）ＣＨ（ＯＨ）ＮＨ２作为混合型乳化剂，在二甲苯／水体系中首次制备了纳米级三氧化钨粉体，确定了最佳反应条件。在不同温度下处理得到的纳米级粉体为分散的规则球形粒子（最小尺寸为１５ｎｍ）。用透射电镜和Ｘ－Ｒａｙ衍射对各种温度处理得到的ＷＯ３粉体进行了分析。所制备的ＷＯ３纯度为９９．９６％。     

低温凝胶燃烧法合成Y2O3∶Er3+，Yb3+纳米晶上转换发光材料

分别以柠檬酸和甘氨酸为燃烧剂,采用低温凝胶燃烧法合成了Er³⁺、Yb³⁺共掺Y₂O₃纳米晶粉体。通过TG-DSC、XRD、SEM等分析手段对两种燃烧剂所对应的反应过程及纳米晶粉体的物理性能进行了分析,结果表明甘氨酸法具有更高的反应效率、更好的粉体分散性及粒径均匀性。在980 nm激光二极管(LD)激发下,对甘氨酸法所得样品的上转换发光性能分析表明,绿光和红光发射谱带分别来自于Er³⁺的⁴S_3/2/ ²H_11/2→ ⁴I_15/2和⁴F_9/2→ ⁴I_15/2跃迁。此外,对Er³⁺和Yb³⁺掺杂浓度、粉体煅烧温度对纳米晶样品上转换发光性能的影响进行了讨论。     

低温燃烧合成Ce0.8Y0.2O1.9固溶体及烧结性能的研究

以硝酸盐做氧化剂,柠檬酸为燃料,采用低温燃烧法制备纳米级超细Ce0.8Y0.2O1.9 (YDC)固溶体.利用TG-DSC,XRD,SEM,FT-IR和BET等手段对凝胶前驱体的热分解行为、相转化过程和YDC粉体的性能进行表征.TG-DSC结果表明,柠檬酸-硝酸盐干凝胶的点火温度约为263.3℃;经XRD测试,粉体经600℃焙烧即形成了单相立方萤石型结构的固溶体,晶粒度为16 ～23nm.柠檬酸与硝酸盐摩尔比(CA/N)对粉体的微观形貌、比表面积和烧结活性有显著影响.当CA/N为1.5∶1时,粉体粒子间仅有微弱的软团聚,将素坯在1400℃烧结2h,得到相对密度为95.6％,平均粒径约为0.7 μm的陶瓷烧结体.     

纳米固体酸催化合成无毒增塑剂柠檬酸三辛酯的研究

以柠檬酸和正辛醇为原料,采用自制的纳米固体酸S04^2-／SnO2、SO4^2-／ZrO2、SO4^2-／TiO2及SO4^2-／Fe2O3催化剂合成无毒增塑剂柠檬酸三辛酯（trioctylcitrate,TOC）。分别考察了纳米催化剂种类、催化剂用量、醇／酸物质的量比、反应时间、反应温度等因素对合成TOC反应酯化率的影响,对合成的产品进行红外光谱分析。实验结果表明,自制的固体酸SO4^2-／SnO2催化合成无毒增塑剂柠檬酸三辛酯的最佳反应条件：催化剂用量为1．0g,酸醇比为1：6.3,反应时间1．0h,反应温度190℃。在最佳反应条件下,柠檬酸三辛酯的酯化率可达到98．5％。     

固态研磨-燃烧法制CuO-ZnO-ZrO2/HZSM-5二甲醚合成催化剂

以柠檬酸为燃烧剂,采用固态研磨-燃烧法和机械混合法制备了CuO-ZnO-ZrO2/HZSM-5CO2加氢一步合成二甲醚双功能催化剂.采用固定床反应器,在反应温度270℃、压力为3.0 MPa、空速4 200 h-1条件下,考察了催化剂对CO2加氢一步合成二甲醚的反应性能,并采用XRD、BET、H2-TPR、NH3-TPD及XPS对催化剂的结构进行了表征.评价结果表明:随柠檬酸量的增加,二甲醚选择性和收率呈峰形变化趋势;当柠檬酸的量等于化学计量比的100%时,制备的催化剂具有较好的催化性能:CO2单程转化率为24.8%、二甲醚(DME)的选择性和收率分别为35.3%和8.7%.表征结果表明:柠檬酸的量影响催化剂的比表面积、还原性能以及CuO和ZnO的晶粒尺寸等,进而影响催化剂反应性能.     

聚合物前驱体方法低温合成LiTaO3纳米粉体

采用聚合物前驱体方法,以柠檬酸为配位剂,乙二醇为酯化剂,低温合成纳米LiTaO3粉体.以红外光谱和拉曼光谱研究了柠檬酸与金属离子的配位情况.当柠檬酸和金属离子物质的量的比为2.5:1、柠檬酸和乙二醇的物质的量比为1:2时可形成稳定的Li-Ta前驱体溶胶.用差热.热重对凝胶前驱体的热分解历程进行分析,采用X射线衍射和红外光谱对Li-Ta凝胶前驱体及不同温度下煅烧所得粉体的相组成进行分析.结果表明,凝胶前驱体经600℃下煅烧2 h可以得到纯钙钛矿型纳米LiTaO3粉体.平均粒径为60～80 nm.     

锐钛矿型纳米TiO2粉体的精细结构及其光催化降解苯酚的活性

  摘要：以Ti（SO4）2·4H2O和尿素为原料，以聚乙二醇－1000为空间构 造剂，制备了不同粒径的具有高热稳定性的锐钛矿型纳米TiO2粉体，并 用XRD，BET和EXAFS技术对其晶相、粒径大小、比表面积及中心Ti原子 的K－边精细结构进行了表征，对其光催化降解苯酚反应的活性进行了 考察．结果表明，未经任何热处理的TiO2粉体即为锐钛矿型晶相，控制 焙烧温度可以达到控制其粒径及比表面积的目的．经850℃焙烧5h的样 品仍保持锐钛矿型晶相，未出现向金红石型晶相转变的迹象．随着纳米 TiO2晶粒的增大，Ti原子局域结构的有序度增强，边前结构A1，A2和A 3三个特征峰的强度增强，各壳层的配位数均呈增大的趋势．粒径处于 15～20nm的锐钛矿型TiO2粉体对光催化降解苯酚表现出较高的活性．     

Nano‐emulsion use for the synthesis of polyaniline nano‐grains or nano‐fibers

We report that nano‐emulsions can be creatively used as a morphology selective synthesis method to prepare not only nano‐grains but also nano‐fibers with high selectivity. Synthesis of the two different morphological materials was demonstrated using polyaniline synthesis as a model case. Polyaniline nano‐grains were synthesized from aniline molecules in nano‐size aqueous droplets as polymerization sites whose droplets were generated by inverse water‐in‐oil nano‐emulsion use, and polyaniline nano‐fibers were synthesized from aniline in aqueous nano‐dimensional channels as polymerization sites whose channels were generated by direct oil‐in‐water nano‐emulsion use containing high population of oil droplets. Using the approaches, we successfully synthesized nano‐fibers of 60 nm diameter with 0.5 µm length and also nano‐grains having diameter of 60–80 nm. The two different polymerization sites of nano‐scale dimension were made by changing the ratio among surfactant, aqueous aniline/HCl solution, and oil, i.e. organic solvent. We found the nano‐fibers synthesized from the channels formed by the direct oil‐in‐water nano‐emulsion have higher bulk electrical conductivity than the nano‐grains which were synthesized from the droplets formed by the inverse water‐in‐oil emulsion. We also found that the emulsion use allows us to use a room temperature synthesis unlike conventional synthesis methods which require to use ice bath temperature. Physical properties of both nano‐fibers and nano‐grains synthesized were characterized by Fourier transform infrared (FTIR), UV–Vis spectra, scanning electron microscopy (SEM), and four probes conductivity measurement. Copyright © 2009 John Wiley & Sons, Ltd.     

纳米氧化镍的制备及其电容特性研究

Nano-nickel oxide was synthesized by chemical deposition of nano-nickel hydroxide followed by heat-treatment in air at 300 ℃. The structure of the sample was studied by XRD, TEM, etc. The electrochemical characteristics of the sample were studied by Cyclic Voltammetry and constant current charge/discharge. The results showed that the structure of nickel oxide was cubic and the shape was acicular. The specific capacitance of the nickel oxide was about 130 F·g^-1 in the 9.0 mol·L^-1 KOH solution. The effects of scan speed, heating temperature and cycling on the specific capacitance were discussed.     

超声化学制备单分散金属纳米钯

A simple sonochemical technique is used to synthesize palladium nanoparticles in a poly(ethylene glycol) (PEG) solvent at room temperature. The reaction based on chemical reduction of PdCl₂ by ascorbic acid (AA). The as prepared Pd nanoparticles are highly dispersed and uniform in size (with average size of ～20nm). The products were characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM).     

单程直驱超高压纳升泵的研制与评价

随着生命科学的发展，纳升液相色谱系统在生化分析领域有着越来越多的应用。纳升流速输液泵作为系统的关键部件之一，其性能直接影响分析结果的准确性与重复性。该文基于高精度直驱电机和十通切换阀研制了一种单程直驱超高压纳升泵，并对其进行了评价。测试结果表明，该纳升输液泵在500 nL/min下的流速准确性优于1%，稳定性优于0.7%，最大输液压强超过100 MPa，梯度输液偏差低于1%。进一步利用该纳升输液泵构建纳升液相色谱-质谱联用系统，对1 μg牛血清白蛋白（BSA）酶解液进样分析，序列覆盖率可达45%，分析1.25 μg Hela细胞蛋白质酶解液鉴定到2809个蛋白质。说明构建的单程直驱超高压纳升泵能够用于生化分析，尤其是蛋白质组学分析研究中。     

Improvement in gas separation properties of a polymeric membrane through the incorporation of inorganic nano‐particles

The present work tries to introduce a high‐performance nano‐composite membrane by using polydimethylsiloxane (PDMS) as its main polymer matrix to meet some specific requirements in industrial gas separations. Different nano‐composite membranes were synthesized by incorporating various amounts of nano‐sized silica particles into the PDMS matrix. A uniform dispersion of nano‐particles in the host membranes was obtained. The nano‐composite membranes were characterized morphologically by scanning electron microscopy and atomic force microscopy. Separation properties, permeability, and ideal selectivity of C₃H₈, CH₄, and H₂ through the synthesized nano‐composite membranes with different nano‐particle contents (0.5, 1, 1.5, 2, 2.5, and 3 wt%) were investigated at different pressures (2, 3, 4, 5, 6, and 7 atm) and constant temperature (35°C). It was found out that a 2 wt% loading of nano‐particles into the PDMS matrix is optimal to obtain the best separation performance. Afterwards, sorption experiments for the synthesized nano‐composite membranes were carried out, and diffusion coefficients of the gases were calculated based on solution‐diffusion mechanism. Gas permeation and sorption experiments showed an increase in sorption and a decrease in diffusion coefficients of the gases through the nano‐composite membranes by adding nano‐particles into the host polymer matrix. Copyright © 2011 John Wiley & Sons, Ltd.     

有机溶剂热生长技术制备硫族化合物及其光学特性的研究

以有机溶剂热生长技术(solvothermaltechnique)制备了半导体硫族化合物(CdS、ZnS、MoS₂)等纳米颗粒,采用XRD、TEM等技术对其结构进行表征.以ITO导电玻璃以及导电聚合物(PANI、PPY)膜为基底,将纳米颗粒涂布其上并以PL法研究其光学特性,实验结果表明:经修饰后,材料的荧光发射位置发生显著的变化.     

水溶性Fe3O4磁性纳米催化剂的合成及应用

利用对氨基苯磺酸氟硼酸重氮盐与Fe₃O₄磁性纳米粒子(MNPs)的偶联反应,非常方便地制备出表面含有磺酸基的Fe₃O₄磁性纳米粒子。 透射电子显微镜(TEM) 测试结果表明,粒子的平均粒径在 20 nm左右。 溶解性实验表明,该纳米粒子具有较好的水溶性,但不溶于常用的有机溶剂,因此可利用其磁性回收并循环使用。 将该纳米粒子用于催化羧酸与醇的酯化反应,产物酯的收率为71%~86%。 催化剂在酯化反应中的最优使用量为1.5%(质量分数)。 同时,该催化剂可催化果糖合成5-羟甲基糠醛(HMF),收率为32%。     

易分离的高效纳米铂氢化催化剂

近年来纳米贵金属的优异催化性能得到了人们的关注,但是纳米粒子在使用、贮藏过程中存在团聚现象。在制备过程中加入稳定剂可以延缓其团聚,但给纳米粒子的分离带来了困难。有献报道利用水溶性表面活性剂聚乙二醇(PEG)的乙二醇链段可以稳定Rh纳米粒子,可是因其分子量过     

Biologically sustainable rubber resin and rubber‐filler promoter: a precursor study

Enthused by the ever growing demand for sustainable and green based materials in responding to applications based on macromolecules, an attempt was made in seeking a bio‐resin (Terpene). Herein, we report the functionalization of bio‐resin with natural rubber (NR) to produce new sustainable and greener functional polymer. Bio‐resin functionalized NR was prepared by melt mixing using di(2‐tert butyl peroxy isopropyl) benzene initiator. Structure elucidation of the bio‐resin functionalized NR was established by proton nuclear magnetic resonance and Fourier transform infrared spectroscopy, respectively. Bio‐resin functionalized NR facilitates the augmented interaction with highly dispersible silica. Amended state of highly dispersible silica dispersion has been achieved in the absence of toxic process oil, expensive silane coupling agent and conventionally used zinc oxide. Remarkable improvement in overall properties corroborated with various meticulous characterization including nanoindentation, rheological, physico‐mechanical and small angle X‐ray scattering using Becauge model, etc. The dynamic mechanical properties of the greener polymer demonstrated low rolling resistance coupled with high traction. More decisively, the macromolecule system toned up sparingly in the presence of the bio‐resin. Our contribution facilitates a novel avenue to develop sustainable high‐performance elastomeric macromolecule. Copyright © 2017 John Wiley & Sons, Ltd.