Synthesis and characterization of Ag nanoparticles–polyaniline composite powder material

The chemical deposition of silver particles in polyaniline (PANI) powder has been carried out via the reduction of Ag⁺ ions by PANI in various concentrations of AgNO₃ aqueous solutions. It is found that the rate of Ag(I) reduction and the size of the metal particles incorporated were strongly dependent on the reaction medium, the PANI redox form and the stirring method used. Homogeneous distribution of silver nanoparticles into PANI matrix was obtained at low Ag(I) concentration, PANI in emeraldine base form and short reaction time under ultrasonic stirring. The presence of silver particles dispersed into porous polyaniline structures was confirmed using X-ray diffraction, scanning electron microscopy and cavity microelectrode (CME) technique in acidic aqueous electrolyte. The electrochemical study of Ag-PANI composite by CME showed that the redox system of silver depends on the size and the distribution of metal particles incorporated into PANI.     

氧化次数对制备多孔阳极氧化铝膜的影响

在8℃、0.3 mol/L浓度的草酸电解液中,施加40 V直流电压,采用两步阳极氧化法在高纯度铝箔上制备了多孔阳极氧化铝（AAO）膜。用场发射扫描电镜（FESEM）对一次、二次氧化制备的多孔氧化铝膜的表面形貌进行了表征。用XRD对原始铝箔及用二次氧化法制备的氧化铝膜的相结构进行了表征。用TEM观察了扩孔后多孔膜的通透性。结果表明,用二次阳极氧化制备的多孔膜明显比用一次法制得的更规则、有序和更厚,为非晶态的Al2O3。     

CdS nanocrystallites prepared by chemical and physical templates

In this work, a convenient method combining physical and chemical templates is presented to obtain a regular arrangement of CdS nanocrystallites. Poly (ethylene oxide) (PEO) is used to control the crystallite sizes as a chemical template and Si-based anodic aluminum oxide (AAO) act as a physical template to form an ordered arrangement of nanocrystallites. TEM images and SEAD patterns reveal that the CdS/PEO composite deposited into the nanopores of the Si-based AAO films is in a tube shape. In UV/Vis spectra, the absorption onsets of the CdS nanocrystallites shift to a shorter wavelength with decreasing Cd²⁺ concentration in PEO. The corresponding photoluminescence (PL) peaks are all located at about 630 nm due to the sulfur vacancies, while their intensities increase with the increasing mol ratio of Cd²⁺/PEO. This method will provide more choices to prepare optoelectronic materials.     

类银镜法高产量制备高稳定纳米银

以AgNO3为前躯体,葡萄糖为还原剂,十六烷基三甲基溴化铵(CTAB)为络合剂和分散剂,一步法制备纳米银溶胶。利用紫外-可见光分光光度计(UV-Vis)、透射电子显微镜(TEM)和X射线衍射仪(XRD)对银溶胶的形成、颗粒尺寸形貌、稳定性和晶体结构进行了表征。结果表明,CTAB与Ag+和H+发生络合反应,稳定了H+,促进了葡萄糖对Ag+的还原;所制备银纳米粒子以球形为主,分散性良好,粒径分布范围为10～40nm,银浓度高达0.025mol/L,室温条件下能够稳定5个月以上。     

Review of porous anodic aluminium oxide (AAO) applications for sensors,MEMS and biomedical devices

Anodising of aluminium is one of the simplest metal surface finishing processes, and results in a porous anodic aluminium oxide (AAO) which is integral with the parent metal. Pore size, interpore spacing and thickness of the porous oxide film can be controlled by careful selection of the anodising electrolyte (type and concentration), and the operating parameters (voltage, temperature, time) employed. A self-ordered nanoporous AAO can be obtained without the need for expensive or complex processes required for traditional materials employed in microelectronics and MEMS applications (e.g. photolithography in the production of porous silicon). Planar and curved AAO surfaces can be manufactured. The simple and low-cost process for the production of AAO has enabled this material to gain inroads in the manufacture of various sensors and MEMS devices. This review paper discusses the anodising process and the resulting AAO structures tailored for MEMS, sensors, biomedical and nanotechnology fabrication.     

铝阳极氧化膜形成过程中离子迁移的规律及对膜形态的影响

用透射电镜、标记原子及等离子体发射光谱定量分析等技术,研究了铝阳极氧化膜生长过程中离子迁移分数及其对膜形态的影响。实验发现,在膜形成过程中,铝和含氧离子沿相反方向漂移穿过膜。在同一电解质溶液中,铝离子的真实迁移分数基本恒定。当电流密度超过某一临界值时,部份铝离子在膜与溶液界面处形成新膜物质,膜的形态为壁垒型。而当电流密度小于临界电流密度时,全部铝离子均进入溶液。这时膜完全由含氧离子在膜与基体界面处形成,由于溶液对膜外表面的侵蚀,形成的膜为多孔型。推导了膜生长效率的理论表达式;表观迁移分数的关系式.用溶解—沉积理论解释了铝离子在膜与溶液界面处形成新膜物质的机理。     

Formation of ZnO nanorod arrays on polytetraflouroethylene (PTFE) via a seeded growth low temperature hydrothermal reaction

ZnO nanorod arrays were formed by a low temperature hydrothermal process on seeded polytetraflouroethylene (PTFE) sheets. The seed layer was formed using thermal oxidation of a thin evaporated Zn film on the PTFE sheet at 300 °C in air for 10 min. The formation of ZnO nanorod arrays in the hydrothermal reactive bath consisting of hexamethylamine (HMT) and Zn ions occurred via the reaction of hydroxyl ions released during the thermal degradation of HMT with the Zn ions. The seed layer provided a template for the nucleation of the ZnO and HMT which also acted as a chelating agent that promoted growth of the ZnO along the c-axis, leading to the formation of exclusively (0 0 2) ZnO nanorods. The effect of exposure time of the seeded PTFE to the reactive solution on the formation of the nanorods was investigated. Well aligned, relatively uniform tapered 300 nm long nanorods can be formed after 8 h of exposure. Longer exposure times to 24 h resulted in the formation of more uniform nanorods with base diameter averaged of ∼100 nm and the tip diameter of ∼50 nm. XRD analysis showed that the ZnO nanorod array had a hexagonal wurtzite structure. This result is in agreement with HR-TEM observations and Raman scattering analysis. Photoluminescence study showed that a strong UV emission peak was obtained at 380 nm and a small peak at 560 nm, which is associated with green emission. The optical band gap measured from these plots was at 3.2 eV on average.     

Ag/Au复合纳米粒子的制备

以柠檬酸化学还原法制备的金纲伙粒子作晶种,在光照的条件下Ag^ 被柠檬酸钠还原成金属银,而均匀地覆盖在金粒子表面,制成具有良好的分散性和较为规则的球形的银／金复合纳米粒子。研究了Ag/Au复合纳米粒子的紫外可见吸收光谱和共振散射光谱特性。     

化学还原法制备纳米银颗粒及纳米银导电浆料的性能

采用化学还原法,在水相中,以硼氢化钠为还原剂,月桂酸为分散剂,通过还原银氨络合物溶液制备了纳米银胶体,之后通过调节胶体的pH值,分离出了纳米银颗粒。TEM和XRD分析表明,该纳米银颗粒的平均粒径大约为17 nm,集中分布于5～30 nm,且无明显的团聚现象;红外光谱分析表明该纳米银颗粒表面包覆有月桂酸,紫外光谱表明制得的纳米银胶体在397 nm处有较强的吸收峰。将分离出的湿纳米银颗粒作为功能相,加入预先配制的载体相中,运用机械搅拌和超声分散等手段,制得了纳米银导电浆料。热重分析表明该浆料含有约67%(质量分数)的金属银,在220℃下烧结2 h后,其电阻率为4.2×10-5Ω.cm。经微细笔直写后,其线条的分辨率可以达到60μm。     

The peculiarities of the kinetics of silver chemical deposition on dielectrics with various technologies of the surface activation

The chemical reduction of single-charged ions of metal (Ar⁺) under the conditions of a hydrodynamic mode on a rotating cylindrical dielectric (D) specimen is first studied. The partial manifestation of the effect of the hydrodynamical rate limitation (HDRL) of silver deposition has been determined. It has been established that the complete manifestation of the HDRL (V _Ag = 0) effect is blocked by the development of the process of the concentration increasing of the electro-active particles in the reactionary zone due to the increase of the amount of collisions of the noncompact silver deposit (growing in the reactor volume) and the oxidation products of the reducer (inverted sugar) with a surface of a compact Ag layer on the D specimen. The results of this research confirm the conceptions concerning the mechanism of the HDRL phenomenondue to the repulsion of electro-active particles of silver from the reactionary layer at high speeds of rotation.     

钛基表面PDLLA/ZnO纳米阵列材料的制备及生物学性能

采用水热生长法,在钛基表面制备高度有序、尺寸可控的氧化锌纳米棒阵列,再通过静电吸附的方法在其表面自组装一层具有良好生物相容性的聚乳酸生物涂层。利用SEM,MTT,LDH方法对细胞形态和生物活性进行表征。结果表明,氧化锌阵列上细胞形态呈圆形,无铺展现象。而经聚乳酸修饰过的材料表面MC3T3细胞外基质铺展较好,细胞分泌的丝状伪足嵌入了阵列结构的空隙中,并且表面细胞数量最多,细胞活性明显高于氧化锌纳米棒及纯钛片。结果表明,聚乳酸涂层提高了氧化锌阵列的生物相容性,为细胞生长提供适宜的微环境,有效促进了细胞的黏附与增殖。     

在柠檬酸盐溶液体系中金核@铂壳纳米粒子的光化学合成

在含有不同Au:Pt摩尔比的双金属离子和单一Pt(Ⅳ)离子的柠檬酸盐溶液体系中,分别利用光化学共还原和Au晶种生长法合成了Au核@Pt壳纳米粒子。借助于透射电子显微镜的表征,研究了在2种制备方法中复合纳米粒子的尺寸变化规律;利用X射线光电子能谱(XPS)分析了复合纳米粒子的表面化学态和它们的结构,证实形成的Au@Pt纳米粒子为核-壳结构。     

阳极氧化铝膜的表面接枝改性及润湿行为

目的通过对阳极氧化铝膜(AAO)表面化学接枝甲基丙烯酸甲酯,改变其表面的粗糙度和分子结构,从而实现AAO膜表面润湿行为的可控。方法采用二步阳极氧化法制备六方柱形的多孔AAO膜,结构高度有序,并对AAO膜表面进行硅烷化(KH-570)处理,采用活性聚合的方法在其表面接枝上甲基丙烯酸甲酯。采用原子力显微镜(AFM)、X射线衍射仪(XRD)和接触角测定仪对AAO膜及改性后的AAO膜进行了结构表征和润湿行为研究。探讨了阳极氧化的工艺条件及接枝甲基丙烯酸甲酯对AAO膜的形貌和润湿性能的影响。结果 AAO膜孔径在100 nm左右,六边形孔洞分布均匀,并且六边形孔洞垂直于AAO膜表面,孔洞与孔洞平行,通过对其表面接枝甲基丙烯酸甲酯,使得AAO膜的表面水接触角先增大后减小。结论 AAO膜表面的润湿行为,可以通过AAO膜表面化学改性和表面粗糙度共同作用而得以调控。     

Synthesis of aligned copper oxide nanorod arrays by a seed mediated hydrothermal method

The synthesis of ordered copper oxide (CuO) nanorod arrays has been obtained using a seed-mediated hydrothermal method. Aligned CuO nanorods were obtained on fluorine doped tin oxide glass substrates over a large scale at low temperature ranging from 75 to 85 °C. It is found the CuO nanoseeds play an important role to facilitate the growth of those aligned CuO nanorods. The band gap energy of the CuO nanorods was estimated by ultraviolet-visible absorption spectroscopy. The growth mechanism of this method was also investigated.     

Al-Ti基体上纳米网状钙磷陶瓷/多孔Al2O3生物复合涂层的原位生长

先采用PVD法在医用钛金属表面沉积一层Al膜,得到Al-Ti基体材料;而后采用阳极氧化与水热合成复合制备技术在Al-Ti基体上成功构造了由纳米网状磷酸盐组成的钙磷生物陶瓷/Al2O3多孔复合生物涂层.利用扫描电镜(SEM)、透射电镜(TEM)、电子能谱(EDAX)、X射线衍射(XRD)表征了阳极氧化前后铝膜和钙磷生物陶瓷涂层的微观形貌、元素构成以及晶相成分.结果表明:在阳极氧化过程中,钙、磷元素嵌入阳极氧化铝(AAO)膜,并经水热处理反应原位生成钙磷陶瓷;钙磷陶瓷晶体从Al2O3孔洞长出并覆盖于多孔氧化膜的表面;最终获得的钙磷生物陶瓷/多孔Al2O3复合涂层具有纳米网状、多孔的结构特征.分析探讨了钙磷生物陶瓷/多孔Al2O3复合涂层的原位生长过程,浓度梯度与电位差分别是Ca、P元素进入AAO膜的主要推动力.     

纳米银溶胶的固液分离研究

以次磷酸钠液相还原法制备纳米银溶胶,通过添加试剂破坏银溶胶的稳定性,使银粒子产生聚沉或絮凝,分析了纳米银溶胶的稳定条件.考查了加入氨水的工艺条件对从银溶胶中过滤分离纳米银粉的影响,控制溶胶的pH范围可以得到不同粒度的纳米银.用有机碱性混合试剂可使溶胶中的银粒子絮凝,易于固液分离,干燥后的银粉经快速渗透剂T分散后,银粉的粒度小（10 nm～20 nm）、稳定性好.提供了从银溶胶中过滤纳米银粉的新方法,该方法工艺简单、对设备要求低、能耗小、银粉的收率高,易于实现工业化.试样经TEM分析发现,该法制备的纳米银粉粒度小（10nm～40 nm）,分散性好.XRD物相分析证实其为纯的金属银.     

Spectral-Kinetic Analysis of State of Silver Sol Particles During Synthesis in Various Media

Protection of Metals and Physical Chemistry of Surfaces - Silver nanoparticles (Ag NPs) have been synthesized in various media using chemical reduction of silver ions with tannin and absorption...     

间接电还原法合成银纳米颗粒及纳米银粉的抗菌性能

利用Keggin结构的12-磷钨酸（PTA,下同）作为还原剂,采用间接电还原法还原硝酸银制备了银纳米颗粒,考察了12-磷钨酸与Ag+离子不同摩尔配比对Ag纳米颗粒大小的影响。用透射电子显微镜(TEM)、紫外可见吸收光谱(UV-vis)、X射线光电子能谱(XPS)、X射线衍射(XRD)等手段对制备的银纳米颗粒的形貌、组分、粒径和相结构进行了表征。测试了银纳米颗粒对大肠杆菌和金黄色葡萄球菌的抗菌性能,结果表明,制备的Ag纳米颗粒的平均粒径随磷钨酸和硝酸银的摩尔比的减小而增大。纳米银对大肠杆菌和金黄色葡萄球菌生长具有较好的抑制作用,且抗菌性能稳定。     

高质量氧化铝模板的制备及其研究

以5%磷酸为电解液,通过阳极氧化高纯铝片制得了有序性较高的多孔氧化铝模板,结合扫描电镜(SEM)对其结构和行貌进形观察和表征.研究了氧化铝模板的制备工艺,还讨论了氧化铝膜的形成过程,最后比较了一次阳极氧化和二次阳极氧化获得的样品的多孔结构,认为低温下采用二次阳极氧化法可以获得很好的多孔氧化铝模板.     

简易种子调停法制备大小可调的三角形银纳米盘(英文)

通过柠檬酸钠还原银离子,以银纳米粒子为种子,在室温下制备出平均厚度约为5nm,尺寸40到500nm可调的三角形银纳米片。通过种子调停法可实现银纳米盘的面内偶极表面等离子体共振峰(SPR)从最初的520nm红移至1100nm。通过控制实验参数能够很好地理解其生长机制。柠檬酸根离子和增加到生长液里面的银纳米种子是2个重要的参数,可以控制银纳米盘的大小却不改变银纳米盘的厚度以及晶面结构。采用PVP作为包覆剂,其作用机理还不是很清楚,需要进一步的研究。