纳米金的制备、表征及应用研究

纳米金材料基于其良好的光学和电子学特性,近年来已成为科学家们研究的热点之一。实验以氯金酸为原料,柠檬酸三钠为还原剂,采用经典的柠檬酸三钠还原法制备出纳米金溶液,利用目测法、紫外-可见分光光度法和扫描探针显微镜法对其进行表征,结果表明:纳米金粒子尺寸均匀、呈球形单分散分布。利用自组装单分子膜原理,通过层层组装将纳米金粒子和DNA探针依次固定到玻碳电极表面制备探针电极,利用电化学工作站检测其信号,结果表明纳米金标记DNA探针可显著增强目标DNA的检测信号,提高检测的灵敏度,并使响应电流增强。     

Novelty phase synthesis mechanism and morphology in resin-bonded Al-Al2O3-TiO2 composites at high temperatures under flowing N2

An Al-AlN core-shell structure is beneficial to the performance of Al-Al₂O₃ composites. In this paper, the phase evolution and microstructure of Al-Al₂O₃-TiO₂ composites at high temperatures in flowing N₂ were investigated after the Al-AlN core-shell structure was created at 853 K for 8 h. The results show that TiO₂ can convert Al into Al₃Ti (~1685 K), which reduces the content of metal Al and rearranges the structure of the composite. Under N₂ conditions, Al₃Ti is further transformed into a novelty non-oxide phase, TiCN. The transformation process can be expressed as follows:Al₃Ti reacts with C and other carbides (Al₄C₃ and Al₄O₄C) to form TiC_x (x < 1). As the firing temperature increases, Al₃Ti transforms into a liquid phase and produces Ti(g) and TiO(g). Finally, Ti(g) and TiO(g) are nitrided and solid-dissolved into the TiC_x crystals to form a TiCN solid solution.     

以ITO导电玻璃为基底电化学法制备纳米金及其表征

本研究采用循环伏安法在ITO玻璃上直接沉积金纳米粒子制备纳米金膜。另外,考察各因素对纳米金膜的影响,并对其进行表征。     

Mechanism of the interaction between Au nanoparticles and polymerase in nanoparticle PCR

Nanoparticle PCR is a novel method to optimize DNA amplification. It performs well in improving specificity, enhancing sensitivity and speed. Several mechanisms were proposed in previous studies: one was based on the interaction between gold nanoparticles (AuNPs) and DNA while the other was attributed to the heat transfer property of AuNPs. In this paper, we propose that the interaction between AuNPs and DNA polymerase can significantly influence PCR. First, the addition of DNA polymerase can eliminate the inhibitory effects of excess AuNPs. Second, the addition of AuNPs will increase yield of the desired PCR product and make the optimum concentration of DNA polymerase move to higher value. Third, while excess polymerase might inhibit amplification efficiency, AuNPs can reverse this process and the yield of PCR amplification. Based on these results we propose a possible mechanism that AuNPs might modulate the activity of polymerase and improve PCR amplification.     

鞭毛辅助的纳米金的控制合成

介绍了一种由细菌鞭毛辅助控制合成纳米金颗粒的新方法,用于优化纳米金颗粒合成过程中的尺寸可控性,并提高金溶胶的稳定性.借助透射电子显微镜(TEM)、Zeta电位仪、紫外可见分光光度计及红外等仪器,探究了溶液p H值对鞭毛分散体系稳定性的影响、金离子与鞭毛的相互作用以及鞭毛辅助的纳米金生长机制.结果表明,鞭毛是纳米金理想的成核位点,同时对纳米金颗粒的聚集和生长有较强的抑制作用.本工作对提高纳米金的稳定性具有借鉴作用.     

Roles of titanium-rich precipitates as inoculants during solidification in low carbon steel

The effect of titanium on the as-cast structure and the growth form of titanium precipitates, and the effect of cooling rate on the size and distribution of titanium precipitates were studied. It is shown that Ti-rich precipitates acting as heterogeneous nucleation sites play an important role in refining the grain size and increasing the equiaxed grain ratio. Cooling rate has a great effect on the size and distribution of precipitates. The number of precipitates increases and the size decreases with the increase of cooling rate. Ti-rich particles acting as heterogeneous nucleation sites at the onset of solidification are observed in the experiment. This result suggests that TiN nucleated on Ti₂O₃ is an effective inoculant for δ-ferrite during solidification in low carbon steel.     

金纳米粒子二维有序阵列的构筑和电化学性质

在水溶液中用柠檬酸钾还原氯金酸的方法合成了粒径为30～40nm的金纳米粒子,并用透射电镜和紫外可见光谱进行了表征;然后在表面经PVP修饰的导电玻璃上以自组装的方式构筑了金纳米粒子的二维有序阵列,并用扫描电镜和紫外可见光谱进行了表征;以所制备的金纳米粒子二维有序阵列作为电极,对硝基苯酚的电化学响应得到明显提高,金纳米有序阵列电极有望成为检测废水中对硝基苯酚的电化学传感器.     

Fabrication and characterization of anodic oxide films on a Ti-10V-2Fe-3Al titanium alloy

Anodic oxide films of the titanium alloy Ti-10V-2Fe-3Al in ammonium tartrate electrolyte without hydrofluoric acid or fluoride were fabricated. The morphology, components, and microstructure of the films were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results showed that the films were thick, uniform, and nontransparent. Such films exhibited sedimentary morphology, with a thickness of about 3 μm, and the pore diameters of the deposits ranged from several hundred nanometers to 1.5 μm. The films were mainly titanium dioxide. Some coke-like deposits, which may contain or be changed by OH, NH, C-C, C-O, and C=O groups, were doped in the films. The films were mainly amorphous with a small amount of anatase and rutile phase.     

基于纳米金和碳纳米复合材料的辣根过氧化物酶生物传感器的研究

合成了碳纳米粒子(CNs)和多壁碳纳米管(MWCNTs)复合材料,并通过X射线衍射仪(XRD)、透射电子显微镜(TEM)对材料进行表征.并以玻碳电极为基底,修饰上MWCNTs-CNs复合材料,再用电沉积法将金修饰在MWCNTs-CNs表面后,固定过氧化物酶,成功制备出一种新的生物传感器用于检测过氧化氢.实验表明,该生物传感器对过氧化氢具有良好的电催化性能,过氧化氢的浓度在2.91~980.00μmol/L范围内与其峰电流呈良好线性关系,检出限为0.48μmol/L.同时,该传感器具有灵敏度高、重现性和稳定性好的特点.     

镍-磷/金纳米粒子复合化学镀层的研究

在化学镀镍磷溶液中添加金纳米粒子，在基体钢铁上沉积得到镍-磷/金纳米粒子复合镀层. 金纳米粒子在镀液中的浓度为1.0?μmol•L-1. 用扫描电子显微镜，能谱仪，示差扫描热量分析仪，X 射线衍射仪，显微硬度计等仪器对镀层性能进行了分析. 通过EDS分析表明，Ni P镀层中P的质量分数为9.72%，而Ni P/Au镀层中P质量分数为9.29%，金的质量分数为0.93%. 与镍-磷合金镀层相比，纳米复合镀层具有较高的硬度，并且镀层组织致密，孔隙率小，对基体具有更好的保护作用.     

生物法合成纳米金的研究进展

纳米金以它独特的光学、电学和催化性质受到人们越来越多的关注.目前,生物合成的纳米金具有经济、无毒、环境友好等特点而成为研究热点.综述了利用细菌、真菌、放线菌、酵母菌以及各种植物材料合成纳米金的方法,并将各种方法进行了比较,讨论了每种方法的特点、尺寸和形貌的控制以及合成机理.最后,展望了生物合成纳米金的应用以及未来的发展方向.     

纳米金修饰电极上苯二酚的电催化及分析应用

利用恒电位沉积方法将HAuCl4直接还原成纳米金并沉积到玻碳电极表面。制备了对苯二酚异构体具有不同电催化作用纳米金修饰电极。在PBS缓冲溶液中,通过循环伏安法研究了苯二酚异构体及其混合物在纳米金修饰电极上的电化学行为,结果表明。苯二酚异构体在纳米金修饰电极上具有不同的电化学性质。对苯二酚和邻苯二酚在纳米金修饰电极上出现峰型良好的氧化还原峰,而间苯二酚几乎不产生氧化还原峰。比较对苯二酚和邻苯二酚在纳米金电极的的氧化还原峰。两者峰电位有较大区别,相互之间没有干扰,据此建立同时测定苯二酚混合物中的对苯二酚和邻苯二酚分析方法。     

纳米金光度法测定维生素B_1

采用柠檬酸钠还原氯金酸的方法制得粒径约为13 nm的纳米金.在酸性环境中纳米金与维生素B1发生相互作用,纳米金产生凝聚,使其最大吸收峰发生红移,由此建立维生素B1的比色测定方法.优化了溶液pH、纳米金的浓度以及反应时间.在最佳条件下,方法的线性范围为5~60 ng/mL,检测限为0.74 ng/mL.用此方法成功分析了维生素B1片剂和注射液中维生素B1的含量.     

巯基功能化离子液体作稳定剂制备纳米金

利用绿色的、稳定的巯基功能化室温离子液体作为稳定剂,在室温条件下制备出相当稳定的Au纳米粒子.对制备的金粒子用紫外可见吸收光谱、透射电子显微镜和X-射线衍射进行了表征.结果表明在555 nm处有强而锐的吸收峰并且金粒子的平均直径为2~3 nm,X-射线衍射结构表征进一步说明产物是纳米级立方面心的单质金.     

量子点荧光增强和纳米金光度法测定链霉素

首次建立了Cd Te量子点荧光增强法和纳米金紫外可见分光光度法检测链霉素的两种新方法,并将两种方法进行了比较.结果表明,量子点的荧光强度与链霉素浓度在2.75×10-7~1.65×10-5mol/L之间呈线性关系;纳米金吸收光谱的变化与链霉素浓度在1.89×10-7~5.46×10-6mol/L之间呈现良好的线性关系.两种方法用于样品中链霉素含量的测定,回收率均在97.5%~103.75%之间,结果令人满意.     

基于纳米金表面等离子体的高灵敏过氧化氢光学检测方法

在酸性2-吗啉乙磺酸介质中,建立基于纳米金表面等离子体的微量过氧化氢(H2O2)的比色检测体系,探讨裸眼检测途径下的分辨极限,提高体系稳定性并利用光谱分析精确定量H2O2浓度(c).结果表明,当c100μmol/L时,纳米金为团聚态,呈现蓝色;c120μmol/L时,纳米金为分散态,呈现红色.该方法的裸眼检测极限可分辨浓度差为20μmol/L.反应溶液的显色结果并不稳定,在反应后45 min内变化较快,c为60~100μmol/L的反应溶液也将逐渐由蓝色变为红色.溶液在570 nm处的吸光度(OD570)检测证明,反应体系在检测后3 h内仍持续变化.反应10 min后,加入适量半胱甘肽终止反应,可使反应溶液的显色结果稳定,提高体系稳定性.实验测定不同浓度H2O2反应产物的吸收光谱发现,c100μmol/L的反应孔产物在波长约550 nm处有吸收峰,且吸收强度与c成正相关.而c120μmol/L的反应产物吸收峰逐渐往短波长方向偏移,最终峰值约为540 nm.分析反应体系吸收光谱结果证明,各反应产物在630 nm和545 nm处吸光度的比值(OD630/545)与c呈良好的线性关系.实验对c为100~120μmol/L的H2O2溶液进行检测,定量浓度差为2μmol/L的H2O2溶液,降低裸眼检测途径下该方法的分辨极限,为微量样品检测提供更好的平台.     

纳米金-铂/碳纤维复合材料的制备及其修饰电极性能研究

通过静电纺丝法制备聚丙烯腈纤维(PANF)并高温碳化以获得碳纳米纤维(CNF),利用水热法将纳米铂(PtNPs)负载于CNF表面得到Pt/CNF复合材料,将其固定于电极表面之后进一步利用电沉积法将纳米金(AuNPs)形成于Pt/CNF表面得到修饰电极(Au/Pt/CNF/CILE)。通过扫描电镜考察复合材料的形貌结构,利用电化学方法研究修饰电极的电化学性能,求解其有效面积。结果表明CNF呈网状结构,PtNPs稳定附着在纤维表面,电沉积的AuNPs均匀分布在Pt/CNF/CILE表面,所制备的修饰电极的导电性能增强、有效面积增大且表面丰富的电活性位点促进了电子的有效转移。     

分光光度法研究纳米金溶胶和DNA的相互作用

本文采用分光光度法研究了纳米金溶液、ＣＴ－ＤＮＡ及两者混合液高速离心前后的吸收值的变化情况,发现纳米金溶胶和ＤＮＡ之间存在相互作用,并进一步证明了两者有定量的结合关系。