活性模板法制备纳米镍粉体

采用活性模板法制备了高纯纳米镍(Ni)粉体。研究了影响纳米粉体性能的各种因素，通过X射线衍射(xRD)、透射电子显微镜(TEM)和激光粒度分析仪等手段对样品的成分、形貌、粒度及其分布进行了分析，探讨了活性模板的作用机理。结果表明：模板介质炭黑具有微反应器作用、空间位阻效应和较强的还原性，活性模板法制得的纳米Ni粉呈规则的球形链状分布，无明显团聚体，平均粒径为45．7nm，粒径分布窄，粒径范围在16．0nm～59．1nm。     

用多轮置换/生长法调节银纳米盘的SPR吸收峰

以双还原剂法制备的单晶三角形银纳米盘为模板,在室温溶液相与HAuCl4发生多轮置换反应,反应9轮后纳米盘的面内偶极表面等离子体共振峰从初始的700 nm逐步红移到1100 nm,形貌从实心盘状逐渐变为空心纳米环.改变每轮加入的HAuCl4的量即可精细调节面内偶极峰的红移步进量.在只进行一轮反应时,若加入的HAuCl4少于一定量,面内偶极峰会发生小幅度的蓝移.在银纳米盘模板溶液中用抗坏血酸还原AgNO3,银原子沉积到纳米盘上使其生长,若采用多轮还原生长的方法,生长8轮后纳米盘的面内偶极峰逐步蓝移至650 nm,形貌从三角形盘状逐渐变为更大更圆滑的圆盘状.以上方法实现了在温和反应条件下在可见光至近红外光区方便地逐步调节银纳米结构的吸收峰.     

Study on Properties of Conductive Adhesive Prepared with Silver Nanoparticles Modified by Silane Coupling Agent

采用经硅烷偶联剂KH-560表面改性的纳米银粉作为填料,环氧树脂为基体在180℃固化得到银导电胶。借助透射电子显微镜(TEM)、红外光谱(FTIR)、差示扫描量热法(DSC)等测试手段,对改性后纳米银粉和导电胶进行了表征。研究了银粉含量、固化时间对导电胶性能的影响。结果表明:KH-560改性后的纳米银粉平均粒径为20 nm,分散均匀;KH-560以化学键合的方式吸附在纳米银颗粒的表面。银粉含量、固化时间等均会影响导电胶的性能。当银粉含量为55%,固化时间为15 min时,导电胶的体积电阻率达最小值为2.5×10-3Ω·cm。与未做任何表面处理的纳米银粉填充的导电胶相比, KH-560改性后纳米银粉所得导电胶的电导率提高了3-5倍。     

银纳米粒子尺寸对多壁碳纳米管自组装的影响

研究了以胶体银纳米粒子为前体在多壁碳纳米管(MWNTs)表面进行的自组装及其银粒子尺寸对自组装的影响。结果表明:银粒子与MWNTs的平均直径之比≤1/3时,能够获得较好的Ag/MWNTs一维复合物材料,而且透射电镜(TEM)直接观察到银纳米粒子的自组装及其生长优先在MWNTs端头发生;基于各种技术表征,在N,N-二甲基甲酰胺(DMF)存在下MWNTs功能化的表面存在的羧基、羟基与柠檬酸根的多羧基、羟基基团之间的氢键作用以及疏水作用可能是银纳米粒子自组装的主要驱动力。     

Mechanism of Preparing Spherical Nano-sized Silver Particles via o-Phenylenediamine Reduction Process in Water-NMPD Mixed Solution System

室温条件下,在水-NMPD混合溶液中,以邻苯二胺还原硝酸银,通过直接混合的一步反应,实现了球形纳米尺度银颗粒的可控制备。制备的颗粒采用扫描电子显微镜（SEM）和X射线衍射（XRD）技术进行性质表征,反应后的溶液体系采用紫外-可见光谱（UV-Vs）和液相色谱-质谱（LC-MS）技术进行分析。结果表明：制备的纳米银颗粒呈现出良好的球形形态,粒径均匀,平均粒径约 70 nm,银纳米颗粒具有面心立方对称结构,其晶格参数 dhkl,a 和 V 3均略大于标准卡片值,邻苯二胺经银离子氧化后的产物为2,3-二氨基吩嗪。     

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。     

基于分子动力学仿真的纳米胶体射流抛光材料去除机理

利用分子动力学模拟了纳米Si O2颗粒与单晶硅(100)表面的碰撞过程,以此来分析纳米胶体射流抛光的材料去除机理。仿真结果显示:粒径为7 nm的Si O2颗粒其速度在50 m/s时,与单晶硅工件表面的碰撞作用不会引起工件表面的原子排布的变化;而若要使碰撞对单晶硅工件表面原子排布产生影响,纳米Si O2颗粒的速度需大于250 m/s。以单晶硅工件为加工对象进行了纳米胶体射流抛光加工试验。利用激光拉曼光谱对加工前后单晶硅工件表面原子排布状况进行了比较,其结果与分子动力学仿真结果吻合。利用X射线光电子能谱,研究了加工前后纳米Si O2颗粒与单晶硅工件表面原子之间化学键的变化。通过仿真和试验得出:纳米胶体射流抛光中,纳米颗粒碰撞所产生的机械作用不能直接去除工件材料,材料的去除是纳米颗粒与工件表面之间机械作用和化学作用的共同结果。     

纳米银的分散稳定性和光谱性质研究

采用柠檬酸钠和葡萄糖还原硝酸银制备出平均粒径50nm左右的纳米银溶胶,通过x-射线衍射（XRD）、紫外可见光谱（UV-vis）和荧光光谱（FL）分析了银溶胶的结构和光学性能,最终确定了银溶胶的最佳激发和发射波长值分别为260nm和522nm。详细讨论了溶液pH值、醇／水比例及表面活性剂等因素对纳米银溶胶分散稳定性的影响,并通过透射电镜观察纳米银颗粒的存在状态。结果表明,纳米银溶胶在介电常数较高的溶剂中稳定性提高,体系pH值在5～6时稳定性较高,PVP、阳离子表面活性剂能够提高体系分散稳定性,阴离子表面活性剂则使银粒子发生明显的聚集。     

Preparation of flake AgSnO2 composite powders by hydrothermal method

Silver-tin oxide composite powders and silver powders were synthesized by hydrothermal method using NHs to complex Ag^＋, SO3^2- to reduce Ag（NH3）2^＋ and Na2SnO3 as the source of tin. The powders were characterized by XRD, SEM and EDX. The results show that there are macroscopic and microscopic differences between two kinds of powders. Spherical silver powders are 3μm in diameter, and silver-tin oxide composite powders are mainly flake of about 0.3μm in thickness. Silver crystal in silver-tin oxide composite powders is preferentially oriented in the （111） crystallographic direction and its oriented index is 2.581. Crystal lattice parameter of silver crystal of silver tin-oxide composite powders is 0.409 34 nm, larger than 0.408 68 nm of silver powders. The XPS analysis shows that silver in silver-tin oxide composite powders is metallic silver and tin oxide in silver tin-oxide composite powders has the red shift for Sn^4＋（3d（5/2）） and O^2-（1s）.     

Using nanoparticles as direct-injection printing ink to fabricate conductive silver features on a transparent flexible PET substrate at room temperature

Conductive metallic features that are flexible could have application in integrated circuits, ranging from large-area electronics to low-end applications. This paper shows the creation of conductive silver thin film and wire on the transparent flexible polyethylene terephthalate (PET) substrate by a room-temperature chemical reduction process. One-step synthesis and spectroscopic characterizations of size-controlled silver nanoparticles are also described. Transmission electron microscopy, Fourier transform infrared spectroscopy, thermal gravimetric-mass analysis, X-ray photoelectron spectroscopy and synchrotron radiation X-ray diffraction were used to characterize the dodecanoate-protected silver nanoparticles. Silver metal film and wire were produced by soaking the dodecanoate-protected silver nanoparticle film and wire, which were prepared, respectively, by spin-coating and by directly drawing with a commercial Epson T50 inkjet printer onto the flexible PET substrate using Ag nanoparticles suspended in cyclohexane (10 wt.%) as the ink, in an aqueous solution containing 80% N₂H₄. The resistivities of the Ag films are actually lower compared with the Ag thin films prepared by other conventional chemical routes, such as using silver salts as metallo-organic precursors. It is suggested that the use of nanoparticles as a precursor may be an explanation for the lower resistivity.     

Formation and Properties of LBL Films Based on Pectin and Nanocomposite of Pectin–Ag

Ultrathin LbL films based on protamine sulfate and pectins, including silver nanoparticles, have been obtained. Using the methods of quartz crystal microbalance and atomic force microscopy, the characteristics of the formed films are studied. It is shown that films based on pectin–Ag nanocomposites are elastic with a surface roughness of ≤3 nm, water content of <10 wt %, and bilayer thickness of ~5 nm.     

一种中空金/银双金属纳米颗粒的制备及其SERS性能

以银纳米颗粒为牺牲模板,利用Ag和HAu Cl4之间的置换反应,结合柠檬酸钠同步还原的方法制备了一种中空金/银双金属纳米颗粒。通过对颗粒形貌及局域表面等离子体共振(LSPR)的分析,初步研究了此类金/银纳米颗粒的生长机理,并对影响反应的因素进行了探讨。结果表明,通过控制反应条件可以实现对LSPR的精密调控。该类金/银双金属纳米颗粒可用作为SERS基底,苯硫酚在其表面增强因子可达107,并具有良好的信号重现性。该基底用于atto610标记的生物素与亲和素的SERS检测,检测限可达80 pg/m L。     

碳量子点及其功能化与银复合的催化性能研究

采用水热反应釜法制备碳量子点以及氯化亚砜功能化碳量子点,然后分别与用乙二醇还原的银纳米粒子进行复合,利用FTIR、TEM对样品进行表征,利用荧光分光光度计测试荧光谱,紫外-可见分光光度计测试吸收谱和甲基橙浓度。结果表明：碳量子点的平均粒径约3.5nm,类球形银纳米粒子的平均粒径约18nm。银纳米粒子和碳量子点复合催化剂能够使荧光猝灭,使可见光区的吸收增强。复合催化剂比单独的银纳米粒子和碳量子点的催化能力更好。银纳米粒子和碳量子点以1：2的比例复合时催化效率最高。氯化亚砜功能化的碳量子点与银纳米粒子复合能提高降解甲基橙的浓度和降解速率,12分钟内降解完50mL,50mg/L的甲基橙。     

铜基银枝晶的制备和氧还原电催化性能

通过迦尔瓦尼置换反应在不同的Ag+溶液中制备出了铜基银枝晶,采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和电化学工作站分别对样品的结构、微观形貌以及电化学性能进行了表征。结果表明,随着溶液中Ag+浓度和反应时间的增加,银的形貌从团簇状向树枝状转变,氧还原电催化性能也增强;在相同浓度Ag+溶液中,SO42-比NO3-更能促进枝晶的生长,但当阴离子是NO3-时比阴离子是SO42-时所制备的银枝晶的氧还原电催化性能更好;在10 mmol/L AgNO3溶液中,反应时间为1800 s时制备的银枝晶电极使H2O2的还原峰电流最大,在0.1 mol/L Na2SO4+5mmol/L H2O2溶液中,恒电位为-0.32 V时,其稳态电流密度可达2.83 mA/cm2。初步提出了银枝晶的生长机制和H2O2的氧还原催化机制。     

Research on a New Synthesis Technology of La-Mg-Ni System Alloys and Microstructure of La0.67Mg0.33Ni3.0 Alloys

在常温条件下,以硬脂酸银为前驱体,受阻酚为还原剂,三苯基磷为还原促进剂,采用超声化学法制备了银纳米粒子.考察影响银纳米粒子形成的实验因素,并利用透射电子显微镜、紫外可见吸收光谱及X射线衍射仪对银纳米粒子进行了表征.结果表明,在一定条件下所得银纳米粒子的平均粒径为6.8 nm,尺寸分布为6.2 nm至7.4 nm,具有良好的稳定性和均一性.溶剂蒸发后,银纳米粒子可形成二维有序纳米阵列.探讨了银纳米粒子的形成机理.     

Mechanism of polypyrrole and silver nanorod formation in lauric acid–cetyl trimethyl ammonium bromide coacervate gel template: Physical and conductivity properties

Polypyrrole (PPy) and silver (Ag) nanorods are synthesized in cetyl trimethylammonium bromide–lauric acid (CTAB–LA) complex coacervate gel template. When PPy–CTAB–LA system is polymerized with AgNO₃, Ag nanorods are produced while use of ammonium persulphate (APS) as initiator yields PPy nanorods. Ag-nanorods are produced from the initial stage while PPy nanorods take a longer time. The average diameter of Ag nanorods varies from 60 to 145 nm by increasing AgNO₃ concentration from 0.27 M to 1.08 M and that of PPy varies from 145 nm to 345 nm by changing pyrrole concentration from 1 × 10^?4 to 2 × 10^?4 M, respectively. Fourier transformed infrared (FTIR) spectra indicate stabilization of Ag nanorods through complexation of PPy with adsorbed Ag⁺ ions. PPy nanoparticles are stabilized by adsorbed sulphate ions and lauric acid, both are acting as dopant to it. FFT pattern and EDX spectra clearly indicate the presence of Ag nanocrystals and PPy on the surface of Ag nanorods, respectively. The mechanism of nanorod formation is attributed from UV–Vis spectra showing a red shift of surface plasmon band of Ag and π–π* transition band of PPy with time. The highest dc conductivity of PPy–Ag composite is found to be 414.2 S/cm, 7 orders higher than that of PPy nanorods (9.3 × 10^?4 S/cm). PPy–Ag systems show Ohmic behavior while PPy nanorods exhibit semi-conducting behavior. The preferential formation of Ag nanorod in AgNO₃ initiated polymerization is attributed to the higher cohesive force of Ag than that of PPy. With two times higher LA and CTAB concentration in the gel the Ag nanorod diameter decreases only 12% while that of PPy nanorod decreases by 50%. Possible reasons are discussed from the hard and soft nature of the two nanorods and from the elasticity of the gel template.     

微波法快速制备单分散纳米银溶胶

不添加任何还原剂,在PVP保护下通过微波辐射[Ag(NH3)2]OH络合物水溶液激发自由电子还原Ag+形成纳米银溶胶。UV-Vis吸收光谱测试表明,胶态纳米银粒子的吸光度随微波辐射时间的延长而增加,但最大吸收波长基本不变。当Ag+/PVP质量比为1:8,微波辐射时间为5min时,吸光度趋于稳定。TEM观测和图像分析结果表明,纳米银粒子的形貌为球形、单分散、平均粒径1.36nm、标准偏差0.54nm。     

化学还原法制备片状纳米银粉

通过化学还原法制备了尺寸约30nm的片状纳米银粉。研究表明,十六烷基三甲基溴化铵(CTAB)的位阻效应防止了粉片的团聚,但是过多的CTAB则阻碍粉片的生长,不利于片状的形成,当CTAB加入量与硝酸银质量比为0.8(wCTAB:AgNO3=0.8)时,可获得片状纳米银粉;反应温度为20°C时,CTAB没有完全溶解,不能有效阻止粉片的团聚,同时反应过程缓慢导致粉片明显长大且分布不均匀,升高温度至40°C时,提高了CTAB的溶解度并促进了反应的进行,但当温度达到60°C时,反应速度过快,形核率增加,最终获得细小的粉片。pH值的升高有利于促进反应的进行,保证Ag+反应完全,但是过高的pH值破坏片状银粉周围的双电层结构,导致粉片的团聚,当pH值为6(弱酸性)时,可获得稳定分散的片状纳米银粉。     

粒径可控高振实密度球银的制备工艺研究

以硝酸银为原料,对苯二酚(C6H4(OH)2)为还原剂,链烷醇胺A为分散剂,用液相化学还原法制备高振实密度超细银粉。用激光粒度分布仪测试银粉的粒度分布与平均粒径,用扫描电子显微镜(SEM)和透射电子显微镜(TEM)分析银粉的形貌、粒径和团聚状态,用多晶X射线衍射(XRD)仪检测粉体的晶相。结果表明：通过调节硝酸银的浓度、硝酸银与还原剂的配比以及分散剂的用量等,可以实现对所制备球银粒径的控制;制备的超细银粉为面心立方晶体结构,呈规则球形,振实密度可达4.0 g/cm3。     

Formation and immobilization of silver nanoparticles onto chromia surface by novel preparation route involving polyol process

Silver nanoparticles were formed and immobilized onto the chromia surface by novel preparation route involving polyol process for the first time. (3-Mercaptopropyl) trimethoxy silane (MPTMS) was employed as a chemical protocol to make a binding between silver nanoparticle and chromia surface. UV-vis absorption spectroscopy, TEM observation and EDS analysis revealed that silver nanoparticles with a size of ∼ 50 nm in diameter were formed and immobilized onto the surface of chromia particles with an average size of 210 nm. It is thought that this novel preparation route can be extended to the preparation of various metal-inorganic heterogeneous composite particles.