晶种法制备单分散的金纳米粒子及光学性能研究

加入聚乙烯吡咯烷酮(PVP)做稳定化试剂,用硼氢化钾还原氯金酸,结合晶种生长法制备了单分散性、粒径小的胶体金。通过晶种生长法,在反应中加入PVP试剂,用抗坏血酸做还原剂,制备了单分散的金纳米棒。结果表明,PVP试剂对金纳米粒子的形貌有重要的影响;加入PVP试剂得到的金纳米粒子(胶体金和金纳米棒)分散性好,无明显的团聚现象。应用透射电镜,纳米粒度分析仪和紫外-可见分光光度计对不同粒径的纳米金进行了表征。     

反相微乳液中纳米金的可控合成及其机理研究

在AOT/正庚烷/氯金酸反相微乳液中,用水合肼作为还原剂制备了纳米金粒子, 用紫外-可见光谱和透射电镜进行分析,系统地研究了水和表面活性剂摩尔比 (ω=nH2O/nAOT)以及氯金酸浓度对粒径的影响。结果表明, 制备的纳米金粒子粒径在4~12 nm、单分散性好。纳米金粒径与ω值存在线性关系。氯金酸的浓度对粒径的影响比较复杂, 随着浓度增大, 粒径先减小后增大。用FT-IR红外光谱解释了AOT的磺酸基对纳米金粒子表面有强烈的吸附作用,从而对合成的纳米金粒子有着很强的保护作用     

芦荟叶提取物绿色制备单分散纳米金及其性能研究

本文以芦荟叶提取液为还原剂和稳定剂,成功地制备了小粒径、球状的金纳米粒子。在这种方法中,简单的芦荟叶提取液和金源混合,没有使用有毒试剂,因此该方法是一种生态友好的合成纳米金的方法。混合溶液的颜色从浅黄色变到紫色,表明生成了纳米金粒子。采用紫外-可见吸收光谱(UV-vis)、激光粒径分析仪(DLS)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱(FT-IR)、X-射线衍射(XRD)等方法对合成的纳米金粒子进行了表征和性能测试。紫外-可见光谱的吸收峰再次表明金纳米颗粒的形成。XRD分析表明所生成的纳米我金具有高度结晶性。TEM和SEM表明纳米金颗粒呈球形,粒径分布在20 nm到60 nm之间。FT-IR证实了金纳米粒子提取物所保护,使其不发生团聚和氧化。论文研究了反应温度、氯金酸溶液和提取物的用量对纳米金粒径的影响。结果表明,这些参数在金纳米粒子的合成中起着重要的作用。     

金纳米颗粒的制备及其性能研究

以氢氧化铵溶液和2,6-吡啶二羧酸为还原剂,通过两步还原法还原氯金酸溶液制备出金纳米颗粒,用X射线衍射(XRD)、透射电子显微镜(TEM)和紫外可见光谱仪(UV-VIS)对纳米颗粒进行了表征。结果表明,制备的金纳米颗粒具有尺寸小、分散性好的特点,并且具有明显的表面等离基元共振效应,使其在纳米尺度的光学领域具有潜在的应用价值。     

压电驱动脉动混合可控合成金纳米粒子

在用柠檬酸钠作还原剂还原氯金酸的基础上,提出了一种压电驱动式脉动微混合可控合成金纳米粒子的制备方法。分析了金纳米粒子的合成机理及脉动微混合的工作原理。针对不同的浓度比(Na_3C_6H_5O_7:HAuCl_4)和脉动混合频率设计并开展了相关金纳米粒子可控合成试验,利用紫外可见分光光度计和透射电子显微镜对所得样品的光学特性、粒子粒径、粒子偏差及单分散性进行了表征,分析了浓度比和频率对试验结果的影响。结果表明:利用压电驱动式脉动微混合法,通过控制两相制剂的浓度比和脉动混合频率,一定程度上可以实现金纳米粒子的可控合成。     

水相法制备小粒径金溶胶

采用柠檬酸三钠还原氯金酸法制备金溶胶.研究了还原剂用量、试剂加入顺序、反应时间、搅拌速度等因素对金溶胶浓度、粒径、形貌和分散性的影响,使用紫外-可见分光光度计和透射电子显微镜对金溶胶的光学特性、粒径、形貌及结构进行表征.结果表明:制备小粒径金溶胶的最优条件为柠檬酸三钠(0.034 mol/L)与氯金酸(0.024 mol/L)溶液体积比为3:1,将氯金酸加入柠檬酸三钠溶液中为宜,反应时间6 min,搅拌速度约650 r/min;在此最优条件下可成功制备出形貌均一、分散性好、稳定性佳的金溶胶,其平均粒径约6～7 nm.     

棒状金纳米粒子的制备及其光谱特性

以银离子为辅助粒子,十六烷基三甲基溴化铵(CTAB)为表面活性剂,抗坏血酸为弱还原剂,利用晶种法制备棒状金纳米粒子,着重研究晶种用量与氯金酸量的比例对棒状纳米粒子形状和产率的影响。利用透射电子显微镜（TEM）和X射线衍射（XRD）仪对纳米粒子的形貌及晶体结构进行分析,利用紫外可见光谱（UV-Vis）对产物进行光谱表征。结果表明,纳米棒为面心立方结构,其UV-Vis出现位于530 nm处的短波吸收和970~980 nm的长波吸收,随着晶种与氯金酸用量比例的增加,纳米棒的长径比出现先增大后减小的趋势,并最终形成球形颗粒。最后探讨晶种用量影响金纳米棒生长的机制。     

Green Synthesis of Colloidal Gold by Ethyl Alcohol and NaOH at Normal Temperature

在乙醇和碱性环境下合成了金纳米粒子,并通过电子显微镜进行表征。紫外可见光谱计研究了胶体金吸收的吸收光谱及其不同的影响因子对合成过程的影响,氢氧化钠的量对于最终胶体产物的形成是重要的影响因子。通过X射线衍射分析表明,该金纳米粒子的晶体结构是面心立方结构。另外,讨论了该反应的机理及其氢氧化钠在还原反应中的作用,对于室温下仅仅几分钟内就产生金纳米粒子,乙醇和氢氧根离子是缺一不可的     

金纳米粒子在云母表面组装行为的研究

在超声场作用下,以氯金酸为前驱物,经柠檬酸钠和单宁酸还原,在云母基底上组装分散均匀的金纳米粒子单层膜。利用扫描探针显微镜、扫描电子显微镜和X射线衍射等技术对制备的金胶体进行表征。结果表明：超声场分布和超声功率对金纳米粒子形貌影响较大,驻波场下制备的金粒子为纺锤形,而且随超声波功率的增大,纺锤形金粒子的平均长径比减小;而在扩散场中得到单分散的球形金纳米颗粒,XRD和SEM测试表明金的平均晶粒尺寸为25 nm。金纳米粒子在处理前后的云母表面均能组装成膜,但在处理后的云母表面覆盖度更大     

液相还原法制备纳米铂粉研究

采用液相还原法，以硼氢化钾(KBH₄)作为还原剂，聚乙烯吡咯烷酮(PVP)、聚乙二醇(PEG)等作为分散剂，将还原剂、分散剂及其他添加剂混合制成还原液，加入到处理过的氯铂酸(H₂PtCl₆)溶液中制备电子浆料用纳米铂粉。研究了还原过程中氯铂酸浓度、还原液p H值、分散剂种类等对铂粉粒度大小及形貌的影响。采用扫描电子显微镜(SEM)和X射线衍射仪(XRD)对铂粉进行表征。结果表明，通过控制反应条件可制备平均粒径在20～100 nm的高纯纳米铂粉。对上述铂粉制备的铂浆料指标进行分析后表明，其可应用于制备催化铂电极。     

胶束性质对光化学制备金纳米粒子的影响

研究了阴离子表面活性剂疏水链的长度对光化学制备金纳米粒子的影响。结果发现，疏水链越长，获得的金纳米粒子的尺寸越小；特别是苯环的引入使诱导和自催化现象越加不明显。在十二烷基磺酸钠体系中获得的金纳米粒子的λmax位于540．7nm，TEM表征的平均粒径为47．1nm；十二烷基苯磺酸钠体系的λmax位于526．5nm，平均粒径为6．7nm。探讨了胶束性质对光化学制备金纳米粒子的影响。     

金银复合纳米微粒的光学吸收特性

以NaHB4做还原剂,利用一步共还原氯金酸(HAuCl4)和硝酸银(AgNO3)制备了金银复合结构的纳米颗粒。用透射电子显微镜对所制备的金银复合纳米微粒的形貌和尺寸进行了表征。紫外可见光学吸收光谱的研究表明:通过一步共还原法所制备的金银复合纳米微粒的光学吸收谱具有单峰的等离子体吸收特征,其吸收峰介于纯金和纯银纳米颗粒特征吸收峰之间,且随着反应液中金离子和银离子的摩尔比的增加而向长波方向移动。Mie散射理论的定量计算结果同样说明了实验所观察到的金银复合纳米微粒的光学吸收的组分可剪裁性。     

Room-temperature synthesis of gold nanoparticles — Size-control by slow addition

We report a simple and rapid process for the roomtemperature synthesis of gold nanoparticles using tannic acid, a green reagent, as both the reducing and stabilising agent. We systematically investigated the effect of pH on the size distribution of nanoparticles synthesized. Based on induction time and σ-potential measurements, we show that particle size distribution is controlled by a fine balance between the rates of reduction (determined by the initial pH of reactants) and coalescence (determined by the pH of the reaction mixture) in the initial period of growth. This insight led to the optimal batch process for size-controlled synthesis of 2–10 nm gold nanoparticles — slow addition (within 10 minutes) of chloroauric acid into tannic acid.     

Growing and stability of gold nanoparticles and their functionalization by cysteine

Gold nanoparticles in aqueous dispersion were prepared using the trisodium citrate reduction method to control the size of particles by changing the concentration of HAuCl₄. The average particle size measured by DLS is higher than that obtained by TEM at a zeta potential of -40 mV. When trisodium citrate concentration is kept constant, the particle size increases with gold concentration. The kinetics of growth was studied and apparent kinetic rate constants were determined at various gold/citrate ratios. Gold nanoparticles were attached to silanized glass surfaces; Au rods were grown (ca. 200 nm) by adding more precursors and the rods’ growth rate was monitored by UV-Vis spectroscopy as well as by AFM. Surface functionalization of gold surface was influenced by cysteine. The surface modification by cysteine at pH=6.0 results in aggregation and the red shift of absorption maximum is nearly 200 nm. When glutathione molecules are bound onto the cysteinelinked Au rods on the glass surface, the spectral shift reaches only an amount of 5–10 nm, because the surface attachment hinders the tendency to aggregate.     

Effects of the DC pulse duty ratio on the characteristics of nanoparticles in gold nanofluids

Gold nanoparticles were synthesized using various unipolar DC pulse duty ratios using solution plasma processing (SPP), and their effects on the size distribution and the shape of gold nanoparticles were investigated. The results demonstrated that the power characteristics used for the synthesis of the gold nanoparticles have a strong effect on the fabrication of Au nanoparticles. Generally spherical shaped nanoparticles were fabricated by SPP and as the unipolar DC pulse power increased from 55−40 % duty ratio to 100−0 % duty ratio, the size as well as size distribution of the fabricated nanoparticles decreased, resulting in an average particle size of approximately 18.1±5.0 nm in diameter at 100−0 % duty ratio. Also, the zeta-potential of the gold nanoparticles synthesized at 100−0 % duty ratio was the highest and was measured at −50.8±1.5 mV, which suggested the dispersion of nanoparticles fabricated at 100−0 % duty ratio was more stable than under other conditions. This confirmed the previously reported results, in that increased electrical energy provided from the solution plasma not only made the nanoparticles even smaller in size, but also facilitated good dispersion stability by charging up the nanoparticles negatively.     

Effects of the gap distance on the characteristics of gold nanoparticles in nanofluids synthesized using solution plasma processing

In this study, gold nanoparticles for use in the production of nanofluids were synthesized with various gap distances of 1.0 mm to 16.0 mm between cathode and anode electrodes using Solution Plasma Processing (SPP). The size distribution and the shape of gold nanoparticles in the nanofluids were investigated using a UV-vis nir spectrophotometer and transmission electron microscope (TEM); the dispersion stability of the gold nanofluids was characterized using zeta-potential. The results demonstrate that the distances between electrodes have a strong effect on the formation of Au nanoparticles in nanofluids. The gap distance of 1.0 mm produced the smallest average particle size, 17.7 ± 6.0 nm in diameter, and the most uniform size distribution. In addition, the zeta-potential of the gold nanoparticles synthesized with a gap distance of 1.0 mm was measured at −45.4 ± 1.3 mV, which suggests excellent dispersion stability of nanoparticles in the nanofluids. Possible mechanisms for the formation of nanoparticles in SPP are suggested. The electrons provided from the solution plasma are believed to play a vital role in producing the Au nanoparticles. Also, increased electrical energy from the plasma is responsible not only for increasing the surface areas of the nanoparticles in the solution by making the nanoparticles even smaller in size, but also for facilitating good dispersion stability by negatively charging the nanoparticles.     

Displacement deposition of gold nanoparticles and electroless deposition of nickel films on silicon-carbide (4H-SiC) wafers

Metallisation of silicon carbide (SiC) wafers is a key technology for producing efficient power devices. Conventional autocatalytic electroless deposition cannot produce adherent metal films directly on SiC substrates. The authors applied their recently developed surface-activation process for electroless metal-film deposition on silicon wafers to SiC wafers. Gold nanoparticles were produced on 4H-SiC substrates by displacement deposition after immersing the substrates in a tetrachloroauric(III) acid solution that includes hydrofluoric acid or potassium hydroxide. The size and the particle density of the deposited gold are changed with deposition parameters such as the surface condition of the substrates, the solution composition, and the UV-light illumination. The gold nanoparticles work not only as catalysts to initiate autocatalytic electroless deposition but also as binding-points between the metal film and the SiC surface. Adherent and uniform nickel-phosphorus alloy films are produced on such SiC substrates by autocatalytic electroless deposition without any further treatments.     

Synthesis of metallic copper nanoparticles using copper oxide nanoparticles as precursor and their metal–metal bonding properties

Abstract

This work proposes a method for preparing metallic Cu nanoparticles using CuO nanoparticles as a precursor, and performs metal–metal bonding by using the metallic Cu nanoparticles. Colloid solution of CuO nanoparticles with a longitudinal particle size of 13·0±3·0, a lateral particle size of 8·4±2·2 and a crystal size of 7·8 nm was prepared with salt base reaction using Cu(NO₃)₂ aqueous solution and NaOH aqueous solution. Preparation of the metallic Cu particle colloid solution was performed in water using the CuO nanoparticles, hydrazine and cetyltrimethylammonium bromide, which resulted in production of the metallic Cu nanoparticles with a particle size of 50·6 nm and a crystal size of 30·5 nm. Metallic copper discs could be bonded using the metallic Cu nanoparticles under annealing at 400°C and pressurising at 1·2 MPa for 5 min in H₂ gas. A shear strength required for separating the bonded discs was recorded as high as 39·6 MPa.