花球状银催化材料的制备及其对4-硝基苯酚的催化加氢性能

通过室温下将硝酸银水溶液与含有硫酸亚铁和柠檬酸的水溶液直接混合,一步合成由银纳米片自组装而成的银花状球结构。结合X射线粉末衍射(XRD)、扫描电子显微镜(SEM)等结构表征手段,考察硝酸银水溶液的滴加速度、柠檬酸添加量等因素对产物形貌及尺寸的影响,并对银花状球的形成机理进行研究。实验结果表明,通过对硝酸银水溶液滴加速度的简单调控可以实现银颗粒形貌由薄片状到花球状的转变。此外,该形貌的微纳米材料在4-硝基苯酚加氢反应中呈现出优异的催化活性。     

复合Ag/ZnO分级结构微球的制备及其光催化性能研究

采用化学沉淀法制备ZnO微球,利用柠檬酸三钠（TCD）避光还原硝酸银在ZnO表面沉积银粒子制备Ag/ZnO复合材料.利用XRD、SEM、TEM、EDS、FTIR、UV-vis DRS、PL、BET等对Ag/ZnO的结构、组分、形貌及光谱性质进行了表征,通过紫外及可见光照降解甲基橙溶液评价样品的光催化性能.结果表明：ZnO纳米微球是由ZnO纳米片相互交错构筑而成的具有丰富孔道的分级结构,Ag纳米粒子均匀沉积在ZnO纳米片上.Ag的沉积显著增加了ZnO的可见光吸收,猝灭了ZnO荧光,提高了ZnO催化活性.     

柠檬酸辅助可控制备花状银粒子及其表面增强拉曼散射性能

以抗坏血酸为还原剂,柠檬酸为结构导向剂,一步还原硝酸银,合成了尺寸和形状可调的花状银颗粒。纳米粒子的粒径可在600～1 200 nm范围内调整,表面突起可达到10～25 nm。柠檬酸的化学性质在银纳米粒子合成多级花状银结构的过程中起着至关重要的作用。通过改变柠檬酸或抗坏血酸溶液的用量,银结构的各向异性形貌可以很容易地调节。以制备的多级花状银颗粒作为表面增强拉曼散射(SERS)基底,对浓度为10~(-10)mol·L~(-1)的罗丹明6G(R6G)仍具有较高的检测灵敏度。     

花状银微纳米结构的合成及SERS性质

通过简便的水溶液方法制备出一种新颖的由纳米片组成的花状银微纳米结构, 采用XRD, SEM, TEM, HRTEM和SAED等手段进行了表征. 考察了反应体系pH值对产物形貌的影响, 并对花状银微纳米结构的形成机理进行了初步探讨. 所制得的微纳米结构由许多纵横交错的纳米片组成. 实验结果表明, 制备的银微纳米结构作为表面增强拉曼散射(Surface-enhanced Raman Scattering, SERS)的基底具有很强的活性.     

核壳结构AlOOH的制备、表征及其生长机制

在柠檬酸钠和硝酸铝水溶液体系中, 通过一步水热法制备了蜷缩刺猬状和核壳结构的AlOOH微球, 并用X射线衍射(XRD)、Fourier变换红外(FTIR)光谱、扫描电镜(SEM)、透射电镜(TEM)、氮气吸脱附和光致发光等分析手段对制备的样品进行了形貌和结构表征. 对反应时间、反应物浓度等影响因素进行了研究. 实验结果表明: 反应时间和反应物柠檬酸钠的浓度对所得AlOOH微球结构的尺寸和形貌具有重要影响; 蜷缩刺猬状和核壳结构AlOOH微球都具有较大的比表面积, 分别为171.5和178.6 m2·g-1; 不同形貌的AlOOH具有不同的荧光发射峰. 并初步探讨了核壳结构AlOOH微球的生长机制.     

三维多枝雪花状银粉的制备及催化性能

室温下,以聚乙烯醇为保护剂,采用抗坏血酸还原硝酸银,于水相中一步合成出三维多枝雪花状银粉。结合X射线粉末衍射（XRD）、扫描电子显微镜（SEM）等结构表征手段,对三维多枝雪花状银粉的微观结构进行详细分析,在此基础上提出其可能的形成机理。此外,三维多枝雪花状银粉在4-硝基苯酚催化加氢反应中还表现出优异的催化活性。     

聚乙烯醇基热致导电复合膜的制备

以硝酸银和聚乙烯醇(PVA)为原料,将不同浓度的硝酸银溶解在PVA水溶液中,通过溶液成膜法制备了含有硝酸银的薄膜。对薄膜加热,硝酸银在聚乙烯醇羟基作用下还原成银粒子,从而使薄膜具有导电性。通过热失重分析仪、差示扫描量热仪、扫描电子显微镜、X射线衍射等方法研究了薄膜热性能和热处理后薄膜表面形貌和结构分析。结果表明,AgNO_3/PVA复合薄膜在150~200℃之间出现一个放热峰,表明硝酸银在此温度区间被还原成银粒子。通过热处理方式制备出纳米银,平均尺寸在100 nm左右。由于银粒子的存在,使薄膜具有导电性,当热处理温度从150℃升至175℃,薄膜表面电导率从3.16×10~(-9)S·cm~(-1)增加至1.76×10~(-4)S·cm~(-1),增加了5个数量级,表明热处理时间和处理温度的提高使银粒子的还原更加充分,粒子之间彼此靠近导致导电性提高。     

共聚物核-银壳复合微球的制备及其结构表征

在银氨溶液中利用原位还原的方法制备出共聚物(PS/PMAA)-银核壳微球。共聚物核平均粒径约为260nm, Ag壳层厚度可通过缓慢滴加不同浓度的银氨溶液控制在15-45 nm.利用TEM、TG、XRD、XPS等分析手段对样品的形貌、结构进行了表征。结果表明银氨溶液滴加速度及溶液浓度为控制复合微球形貌的关键因素。复合微球的形成机理可解释为：Ag纳米微晶首先在共聚物表面形成晶核，随后Ag纳米粒子在晶核表面生长并形成不同厚度的Ag壳层。     

气相扩散法制备的碳酸钙的形貌控制和机理

采用不同质量比的柠檬酸作为晶型控制剂制备碳酸钙,研究了在气相扩散体系中柠檬酸对所制备的碳酸钙微晶的粒度、形貌的影响.结果表明,随着柠檬酸浓度的增大,碳酸钙在溶液中结晶成为纳米小单晶体的二次聚集体,其晶粒度逐步变小,其形态呈现从疏松结构的球体、密实球体、花生状颗粒、大长径比针状到密集针状球体有规律的转变,晶型从0.24%和0.72%的球霰石到更大浓度的方解石.通过对柠檬酸在溶液中的聚集状态和柠檬酸分子与碳酸钙微晶的相互作用初步解释了柠檬酸对碳酸钙微晶形貌控制作用的机理.     

细乳液法制备聚硅氧烷-Ag纳米复合微球及其抗菌性

首先以苯乙烯(St)及3-甲基丙烯酰氧基三甲氧基硅烷(MPS)为反应单体,通过细乳液聚合制备表面功能化聚硅氧烷微球,然后利用该微球表面的硅羟基及硅氧烷基团对Ag+的吸附及还原作用原位制备聚硅氧烷-Ag纳米复合微球。采用透射电镜(TEM)、紫外(UV-Vis)、热重分析(TG)及X射线衍射(XRD)等对聚硅氧烷-Ag纳米复合微球的形貌和组成进行了表征。研究表明:改变MPS和硝酸银的用量可调控聚硅氧烷-Ag纳米复合微球的形貌及表面银含量;抗菌实验结果表明,聚硅氧烷-Ag纳米复合微球具有较好的抑菌性。     

三维多枝雪花状银粉的制备及催化性能

室温下,以聚乙烯醇为保护剂,采用抗坏血酸还原硝酸银,于水相中一步合成出三维多枝雪花状银粉。结合X射线粉末衍射(XRD)、扫描电子显微镜(SEM)等结构表征手段,对三维多枝雪花状银粉的微观结构进行详细分析,在此基础上提出其可能的形成机理。此外,三维多枝雪花状银粉在4-硝基苯酚催化加氢反应中还表现出优异的催化活性。     

Graft copolymerization onto cellulose-based filter paper and its further development as silver nanoparticles loaded antibacterial food-packaging material

The present work describes ceric ammonium nitrate (CAN) initiated graft copolymerization of acrylamide onto cellulose-based filter paper followed by entrapment of silver nanoparticles. The copolymerization was carried out in aqueous solution, containing 2 M acrylamide monomer and 16 mM N,N’-methylene bisacrylamide (MB) crosslinker. The optimum initiation time and grafting reaction temperature were found to be 15 min and 30 °C, respectively. The silver nanoparticles were loaded into grafted filter paper by equilibration in silver nitrate solution followed by citrate reduction. The formation of silver nanoparticles has been confirmed by TEM and SAED analysis. The novel nano silver loaded filter paper has been investigated for its antimicrobial properties against E.coli. This newly developed material shows strong antibacterial property and thus offers its candidature for possible use as antibacterial food-packaging material.     

Fabrication of flower-like silver nanoparticles for surface-enhanced Raman scattering

The flower-like silver nanoparticles have been synthesized by reducing silver nitrate (AgNO₃) with ascorbic acid (AA) as the reductant and polyvinyl pyrrolidone (PVP) as the capping agent under vigorous stirring. Such flower-like nanoparticles are aggregates of small nanoplates and nanorods. They were tested as substrates for the surface-enhanced Raman scattering (SERS), showing high sensitivity for detecting Rhodamine 6G (R6G) at a concentration as low as 10^-7 mol/L. It has been found that replacing mechanical stirring with ultrasound sonication would drastically change the particle morphology, from flower-like nanoparticles to well-dispersed smaller nanoparticles. Furthermore, when trace amounts of NaCl were added into the reagents, well-dispersed Ag nanoparticles formed even in vigorous stirring. These phenomena can be explained with the diffusion and reactant supply during nucleation and growth of Ag nanoparticles.     

Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 μm, some even more than 100 μm, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silver nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD).     

Morphology transformation of micrometre-sized giant vesicles based on physical conditions for photopolymerisation-induced self-assembly

The physical conditions to vary the morphology of vesicles formed by amphiphilic poly(methacrylic acid)-block-poly(methyl methacrylate-random-methacrylic acid) were determined for the self-assembly induced by the nitroxide-mediated photocontrolled/living radical polymerisation performed in an aqueous methanol solution. The copolymer produced micrometre-sized spherical vesicles in the solution with a 30 wt% water content. The vesicles were transformed into a film-like morphology by decreasing the water content, whereas they were changed into nanometre-sized spherical vesicles by increasing it. The concentration of the growing polymer chain also varied the morphology. Large spherical vesicles formed at a low concentration were transformed into much smaller vesicles, followed by rod-like vesicles as a result of increasing the concentration. Furthermore, the stirring speed during the polymerisation-induced self-assembly dominated the morphology. Large elliptical vesicles produced at a low stirring speed changed into spherical vesicles, but decreased the size as the speed increased.     

Amperometric determination of organic isothiocyanates

An amperometric titration method is described for the determination of 1-5 mg of organic isothiocyanates, based on their quantitative reaction with n-butylamine in dimethylfonnamide to form N,N-disubstituted thioureas which are then titrated amperometrically in aqueous ammonia-ammonium nitrate buffer with silver nitrate (dropping mercury electrode at -0.56V). The end-point corresponds to a silver:thiourea ratio of 2:1, with precipitation of silver sulphide. The method is simple, accurate, widely applicable, and gives reproducible results.