化学还原法制备多形貌银纳米材料

银纳米材料因具有导热导电性能好、光电性能优良及抗菌能力强等优点而引起广泛关注,近年来其制备方法得到广泛研究。已报道的制备方法可分为化学法、物理法和生物法等,其中化学还原法可以通过使用不同的还原剂、包裹试剂及助剂,实现不同形貌及粒径的银纳米材料的快速制备。本文综述了化学还原法制备颗粒状、线形、片状、立方体及其它形貌的银纳米材料的原理及应用,并展望了银纳米材料工业化制备及应用研究的发展趋势。可控制备多形貌银纳米材料对于电子行业、医药生物以及传感器等相关领域的发展具有重要意义。     

化学还原法制备纳米铜

以硼氢化钾为还原剂、硫酸铜为氧化剂并添加PVP等辅助材料,采用还原法成功地制备了改性酚醛树脂用纳米铜.通过XRD和TEM对纳米铜进行了表征.结果显示,纳米铜呈球形,粒径为10～50 nm.探讨了BH₄^-与Cu²⁺的反应历程,认为该反应是分三步进行的:第一步是铜的还原反应;第二步是生成的H⁺分别与BH₄^-和OH^-的反应,这是一对竞争反应;第三步是硼的水解反应.在反应过程中,硼氢化钾与硫酸铜消耗的摩尔比为2:1.     

Preparation of Silver Nanoshells on Silica Particles by a Simple Two-step Process

A simple two-step method was developed to prepare silver nanoshells coated on silica paticles. The method involves two steps: concentration of reaction precursor (AgNO3) on particle surfaces and subsequent reduction by formaldehyde. The obtained composite particles were characterized by TEM, ED, and SEM-EDS measurements. The results show that the silver nanoshell is coated on silica particle surface in the form of a polycrystalline (cubic structure) layer with average thickness of 20 nm and weight percentage of 1.9%.     

生物还原-化学沉淀耦合反应制备纳米硫化镉和硫化铅

本文应用生物还原-化学沉淀耦合反应成功制备了高纯纳米硫化镉和硫化铅,EDTA(Ethylene Diamine Tetraacetic Acid)的加入为高浓度金属离子条件下的生物制备提供了保证。研究表明,在0.012 5~0.037 5 mol·L^-1的较低浓度范围内镉浓度增加促进了硫酸根的生物还原和硫化镉的生物制备;但0.05 mol·L^-1的高浓度镉则抑制了SRB的生物活性并降低了硫化镉的生成量。随着厌氧还原反应的进行,微溶的白色硫酸铅沉淀逐渐转化为不溶的黑色硫化铅沉淀,导致纳米硫化铅的生成。硫化镉微球的一次粒子约为10~20 nm,二次粒子平均粒径400 nm,PAM(polyacrylamide)的加入使得二次粒子分布更为均匀。硫化铅微粒二次粒子约为40 nm,PAM的加入没有改变粒子大小,但使得粒子形态由球形变为方形。生物还原-化学沉淀耦合反应对于金属硫化物的制备具有一定的普适性,因而显示出良好的应用前景。     

纳米硫化锌的生物还原-化学沉淀耦合制备及其性能表征

生物还原-化学沉淀耦合反应法制备了纳米硫化锌,采用XRD、SEM、TEM、EDS、PL、FTIR等测试手段对产物进行了结构形貌性能表征。结果表明,在加入与Zn²⁺等物质的量浓度的EDTA后,Zn²⁺对硫酸盐还原菌(SRB)的毒性消除,SRB的较快生长和SO₄^2-的高效还原得以实现,EDTA修饰的生物转化-化学沉淀耦合系统可制备出高纯的纳米硫化锌晶体。制备的纳米ZnS实心微球体形状规则、分散均匀、大小一致,一次粒子直径10～15 nm,二次粒子直径400 nm左右。光致荧光光谱和红外光谱分析显示,ZnS纳米粒子在396 nm处出现荧光发射峰,在465 nm处出现缺陷发光峰,而且具有良好的红外透过性。分散剂聚丙烯酰胺(polyacrylamide)的加入导致产物ZnS的形貌和粒度改变,二次粒子的平均直径减至100 nm以下,其荧光发射峰强度增强,红外透过性提高。     

Preparation of Silver Nanoparticles through Alcohol Reduction with Organoalkoxysilanes

Silver nanoparticles of narrow size distribution were prepared through the chemical reduction in an alcohol solution with several organoalkoxysilanes. In this system, organoalkoxysilanes served as a stabilizer, protecting silver nanoparticles from aggregation. The changes in size and morphology of colloidal silver nanoparticles were investigated with the addition of organoalkoxysilanes such as 3-aminopropyltriethoxysilane (APS), methyltriethoxysilane (MTS), phenyltrimethoxysilane (PTS), vinyltriethoxysilane (VTS), and 3-glycidoxypropyltrimethoxysilane (GPS) as stabilizers. The organic functional groups of organoalkoxysilanes interact with silver ions and clusters, which stabilize silver nanoparticles in the system. The silver nanoparticles obtained were characterized with transmission electron microscopy (TEM), UV-vis spectroscopy, etc.     

Preparation of Monodispersed Copper Nanoparticles by an Environmentally Friendly Chemical Reduction

In this paper, highly dispersive nanosized copper particles with a mean particle size of less than 6 nm are prepared by an environmentally friendly chemical reduction method. Non-toxic L-ascorbic acid acts as both reducing agent and antioxidant in ethylene glycol in the absence of any other capping agent. Transmission electron microscopy （TEM） is used to characterize the size and morphology of Cu nanoparticles. The results of UV-Vis spectroscopy （UV-Vis）, energy dispersive spectroscopy （EDS） and high resolution TEM （HRTEM） illustrate that the resultant product is pure Cu nanocrystals. The size of Cu nanoparticles is remarkably impacted by the order of reagent addition, and the investigation reveals the reaction procedure of Cu^2＋ ions and L-ascorbic acid.     

Preparation of Ultrafine Cobalt Powder by Chemical Reduction in Aqueous Solution

IntroductionThe preparation of ultrafine metal powders has been extensively studied in past years due to their scientific interests and potential applications1. Ultrafine particles exhibit novel material properties that differ from those of the bulk solid state because of the size effect2-4. In particular, ultrafine cobalt powders have many important industrial applications. They are commonly used in alkaline rechargeable batteries, magnetic recording media, heterogeneous catalysis, and especi…     

Preparation of Phenolic Resin/Silver Nanocomposites via in-situ Reduction

Polymer/metal nanocomposites have attracted considerable interest because of their potential application in catalysts, electronics, electromagnetics and nonlinear optics1-3. They have been prepared by blending polymer with nanometer metal particles4, reducing polymer-metal ion complexes with reducing agents5, and reducing metal ions in the polymer matrix by high-energy radial irradiation3. In this paper, we report a new approach to phenolic resin/silver nanocomposites, which have potential a…     

几种卟啉在化学还原沉积银膜上的表面增强拉曼光谱特征

应用 Ｊｏｂｉｎ－Ｙｖｏｎ Ｕ—１０００型拉曼光谱仪和ＬＡＢＲＡＭＩ型拉曼光谱系统研究了 ３种卟啉ＴＯＨＰＰ、ＴａｍＰＰ和ＴＳＰＰ在化学还原沉积法制备的银膜上的ＲＳ和ＳＥＲＳ光谱特征。结果表明：化学还原法制备的银膜可以作为这几种卟啉的拉曼增强活性载体。这３种卟啉在获谱的过程中都形成二聚态化合物和发生银离子搀和作用，较长的放置和测谱时间有利于银离子的搀和。     

乙二醇中化学还原合成片状银粉

研究了乙二醇（EG）介质中以聚乙烯吡咯烷酮（PVP）为保护剂，以氯铂酸为催化剂以硝酸银为前驱物经化学还原制备片状银粉的过程,探索与分析影响银粉形貌的主要因素.结果表明,首先被还原出来的铂成为外来晶种,是形成片状银的关键因素.它在原位为随后还原与沉淀的银提供一个平面.PVP与银离子形成络合离子,控制游离银离子的浓度,影响银的成核与生长.同时,PVP被选择性地吸附于银的粒子表面,影响了银成核与生长,最终形成片状银粉.     

溶液还原法制备球形超细镍粉

超细镍粉由于表面活性高、导电性和导热性好而被广泛应用于化学催化剂、烧结活化剂、导电浆料门等方面．目前，制备超细镍粉的方法主要有问：真空蒸馏冷凝法、机械粉碎法、电解法、羰基镍热分解法、浆化氢还原法和溶液还原法等．在这些方法中，溶液还原法的工艺简单，所得粉末纯度高，颗粒尺寸小且分布均匀[3]．法国的Figlarz等[4]用弱有机还原剂乙二醇还原粒径小干0．1μm的Ni（OH）2。超细粉末，引入AgNO3。作为成核剂后，制得了粒径＜1μm的超细镍粉，但这种方法需长时间高温回流反应，对原料要求苛刻，且采用有机分散介质成本较高，…     

Microwave Absorption and Infrared Stealth Characteristics of Bamboo Charcoal/Silver Composites Prepared by Chemical Reduction Method

Bamboo charcoal coated with silver (BC/Ag) was prepared by activation and chemical reduction processes at different AgNO₃ contents (10‐30 wt.%). The spectroscopic characterizations of the formation processes of BC/Ag composites were studied using X‐ray diffraction, scanning electron microscopy and transmission electron microscopy. These composites were introduced in epoxy resin to be a microwave absorber and mixed polyethylene to be an infrared stealth plate. Microwave absorbing properties were investigated by measuring complex permittivity, complex permeability and reflection loss in the 2‐18 and 18‐40 GHz microwave frequency range using the free space method. The thermal extinction measurements in the 3‐5 and 8‐12 μm were done to evaluate the shielding affectivity of infrared. The results showed that a significant thermal extinction and a wider absorption frequency range could be obtained by adding silver to bamboo charcoal.     

Silver Nanoparticles by PAMAM-Assisted Photochemical Reduction of Ag(+)

The photochemical synthesis of Ag(0) nanoparticles in the presence of amino- and carboxylate-terminated PAMAM dendrimers is reported. The formation of Ag(0) nanoparticles was followed spectrophotometrically and by transmission electron microscopy (TEM). According to TEM investigations Ag(0) nanoparticles with the average size of about 7 nm in diameter were produced. Based on the present investigation a possible mechanism for the Ag(0) nanoparticles formation is proposed. Copyright 2000 Academic Press.     

沉淀聚合制备聚二乙烯基苯微粒

利用沉淀聚合方法，自由基引发二乙烯苯聚合，制备了具有较窄粒度分布的聚二乙烯基苯直发细微粒，用扫描电镜对其表面形态和粒度进行了表 征；红外光谱表明这种聚合物超微粒仍存在有较多未反应的悬吊双键，可以继续与其它功能基团进一步反应，且粒度均一可控。     

Coating of Nanosize Silver Particles with Silica

The formation of silica shells on core silver particles by a modified St?ber process was investigated and the coated particles were characterized using UV-visible spectroscopy, transmission electron microscopy, and electrophoresis. The deposition conditions, such as reagent concentrations and reaction time, were optimized in order to obtain uniform surface layers of silica and to avoid excess precipitation of the latter. Copyright 2000 Academic Press.     

超声辅助化学还原法制备高活性Co-B非晶态合金催化剂

采用超声辅助KBH4化学还原Co(OH)2胶体法制备了粒径均匀的Co-B非晶态合金.在乙腈液相选择性加氢制取乙胺反应中,与传统化学还原法制备的Co-B非晶态合金催化剂相比,该催化剂具有很高的催化活性.这归因于其Co活性位的高度分散、Co活性位对氢的强吸附,以及Co-B非晶态合金间强电子相互作用.     

On the Chemical Processes Accompanying Silver Reduction from Solutions of Its Salts in Organic Media

Silver reduction from its nitrate has been studied in the media of DGEBA-based and aliphatic epoxy resins. It has been found that, under the experimental conditions that were employed, silver ions can be reduced without chemical interaction with the medium only due to photochemical processes. The reduction rate is determined by the rate of dissolution of the initial silver salt in an organic medium and the possibility of the formation of solvates by the system components. Refractometry has been proposed for use in monitoring the kinetics of silver nitrate dissolution in epoxy resins and the formation of silver nanoparticles. Stable dispersions of silver nanoparticles in epoxy resins have been obtained.     

水合肼还原重量法测定银

样品经过硝酸分解后,用过量的氨水分离铅、铁、铝等金属离子,用EDTA掩蔽铜、锌和其他残留的金属离子,用水合肼作还原剂,将银还原成单质沉淀,过滤,洗涤,灼烧,恒重。该方法用于实际样品测定,结果与其他方法测定值一致,误差均在允许范围内;分别对银含量为2.54%和10.00%的样品重复测定12次,相对标准偏差（RSD）分别为1.50%和0.64%,此方法适用于1%以上银含量的测定。