Synthesis of Ag/SiO2 nanocomposite material by adsorption phase nanoreactor technique

Ag/SiO₂ nanocomposite was synthesized in a nanoreactor formed by adsorption layer on silica surface. Ag nanoparticles were prepared by the reduction of Ag ion with ethanol at alkaline condition. By using TEM and XRD, the effects of NaOH concentration, water and temperature on the appearance and grain size of Ag particles were analyzed, respectively. The adsorption curve of NaOH was measured by electrical conductivity meter. The experiment result revealed that Ag grain size decreased while increasing NaOH concentration or while increasing water in our system. Ag grain size increased with the increase of temperature. And Ag aggregated seriously when temperature is up to 60 °C. Finally, after exploring the optimum conditions of reaction, we successfully obtained the well-distributed Ag nanoparticles on surface of silica, and average grain size of Ag nanoparticles reached 5 nm.     

Preparation and characterization of nanocomposite ZnO–Ag thin film containing nano-sized Ag particles: influence of preheating,annealing temperature and silver content on characteristics

Nanocomposite ZnO–Ag thin film containing nano-sized Ag particles have been grown on glass substrate by spin-coating technique using zinc acetate dihydrate as starting precursor in 2-propanol as solvent and monoethanolamine as stabilizer. Silver nanoparticles were added in the ZnO sol using silver nitrate dissolved in ethanol-acetonitrile. Their structural, electrical, crystalline size and optical properties were investigated as a function of preheating, annealing temperature and silver content. The results indicated that the crystalline phase was increased with increase of annealing temperature up to 550 °C at optimum preheating temperature of 275 °C. Thermal gravimetric differential thermal analysis results indicated that the decomposition of pure ZnO and nanocomposite ZnO–Ag precursors occurred at 225 and 234 °C, respectively with formation of ZnO wurtzite crystals. The scanning electron microscopy and atomic force microscopy revealed that the surface structure (the porosity and grain size) of the ZnO–Ag thin film (the film thickness is about 379 nm) was changed compared to pure ZnO thin film. The result of transmission electron microscopy showed that Ag particles were about 5 nm and ZnO particles 58 nm with uniform silver nanoclusters. Optical absorption results indicated that optical absorption of ZnO–Ag thin films decreased with increase of annealing temperature. Nanocomposite ZnO–Ag thin films with [Ag] = 0.068 M and [Ag] = 0.110 M showed an intense absorption band, whose maximum signals appear at 430 nm which is not present in pure ZnO thin films. The result of X-ray photoelectron spectroscopy revealed that the binding energy of Ag 3d_5/2 for ZnO–Ag shifts remarkably to the lower binding energy compared to the pure metallic Ag due to the interaction between Ag and ZnO.     

Recrystallization of Cu-poor CuInS2 assisted by metallic Cu or Ag

We monitor the recrystallization of Cu-poor CuInS₂ thin films assisted by pure Cu or pure Ag by means of real-time synchrotron-based polychromatic X-ray diffraction. In both cases a new microstructure is formed accompanied by an increase in grain size. In the case of Cu, the onset temperature of the thin-film recrystallization is higher than 370 °C. In the case of Ag, the thin-film recrystallization comes to an end at 270 °C. The Ag-assisted recrystallization occurs in the presence of the body-centered cubic β-Ag₂S phase. We find that domain growth and diffusion of silver into the film occur simultaneously.     

Crystallographic Texture and Domain Structure of Nd3:8Dy0:7Pr3:5Fe86Nb1B5 Nanocomposite Prepared by Direct Rapid Solidification

"Strong crystallographic texture and high performance of Nd3:8Dy0:7Pr3:5Fe86Nb1B5 (containing 30% ff-Fe) nanocomposite permanent magnetic material was prepared by direct rapid solidification. X-ray diffraction analysis and magnetic measurement indicated that the ribbons had preferential orientation. The easy magnetization direction switched from perpendicular to the ribbon plane to parallel to the ribbon plane direction as the wheel speed increased from 10 m/s to 30 m/s. The multigrain domains were observed by scan probe microscope (SPM) in the ribbons prepared at wheel speed of 10-30 m/s. The Henkel plots were employed to investigate the interactions of the grains in the samples. A very fine and uniform microstructure with the average grain size about 16 nm was obtained in the sample prepared at wheel speed of 30 m/s. The sample consisted of highly oriented hard magnetic phase (Nd,Dy,Pr)2(Fe,Nb)14B and soft magnetic phase ff-Fe. High performance of Br=1.29 T, Mr/Ms= 0.76 and (BH)max=158.4 kJ/m3 was achieved due to the strong crystallographic texture, fine and homogeneous microstructure and enhancement of the exchange coupling between the soft and hard magnetic phases in this sample. The mechanism of the formation of the crystallographic texture and the multigrain domains was also discussed."     

Effect of TaNx on electrical and optical properties of annealed TaNx/Ag/TaNx films

As‐deposited Ag(10 nm)/glass films exhibited agglomerated nanocrystals with seemingly thick boundaries. Introduction of a TaN_x layer below the Ag films resulted in dense and smooth structures, with a resistance at least three times lower than that of Ag/glass. For TaN_x(10 nm)/Ag(10 nm)/TaN_x(10 nm)/glass multilayer films, Auger electron spectroscopy results indicate that TaN_x acts as an effective barrier restraining the diffusion of Ag. After annealing (up to 573 K), no outward diffusion of Ag through either TaN_x layer was seen. However, partial oxidation of the outermost TaN_x layer to form Ta₂O₅ was observed. The films showed promising optical properties with 73% transmittance in the visible region and ~15% average transmittance in the near‐infrared region. The optical data obtained here was in good agreement with simulated predictions. Copyright © 2013 John Wiley & Sons, Ltd.     

Influence of Thermal Treatments on In-depth Compositional Uniformity of CuIn(S,Se)2 Thin Films

CuIn(S,Se)₂ thin films were prepared by thermal crystallization of co-sputtered Cu-In alloy precursors in S/Se atmosphere. In-depth compositional uniformity is an important prereq-uisite for obtaining device-quality CuIn(S,Se)₂ absorber thin films. In order to figure out the influence of heat treatments on in-depth composition uniformity of CuIn(S,Se)₂ thin films, two kinds of reaction temperature profiles were investigated. One process is "one step profile", referring to formation of CuIn(S,Se)₂ thin films just at elevated temperature (e.g. 500 oC). The other is "two step profile", which allows for slow diffusion of S and Se elements into the alloy precursors at a low temperature before the formation and re-crystallization of CuIn(S,Se)₂ thin films at higher temperature (e.g. first 250 oC then 500 oC). X-ray diffrac-tion studies reveal that there is a discrepancy in the shape of (112) peak. Samples annealed with "one step profile" have splits on (112) peaks, while samples annealed with "two step profile" have relatively symmetrical (112) peaks. Grazing incident X-ray diffraction and en-ergy dispersive spectrum measurements of samples successively etched in bromine methanol show that CuIn(S,Se)₂ thin films have better in-depth composition uniformity after "twostep profile" annealing. The reaction mechanism during the two thermal processing was also investigated by X-ray diffraction and Raman spectra.     

Preparation and Characterization of Thin-Film Solar Cells with Ag/C60/MAPbI3/CZTSe/Mo/FTO Multilayered Structures

New solar cells with Ag/C₆₀/MAPbI₃/Cu₂ZnSnSe₄ (CZTSe)/Mo/FTO multilayered structures on glass substrates have been prepared and investigated in this study. The electron-transport layer, active photovoltaic layer, and hole-transport layer were made of C₆₀, CH₃NH₃PbI₃ (MAPbI₃) perovskite, and CZTSe, respectively. The CZTSe hole-transport layers were deposited by magnetic sputtering, with the various thermal annealing temperatures at 300 °C, 400 °C, and 500 °C, and the film thickness was also varied at 50~300 nm The active photovoltaic MAPbI₃ films were prepared using a two-step spin-coating method on the CZTSe hole-transport layers. It has been revealed that the crystalline structure and domain size of the MAPbI₃ perovskite films could be substantially improved. Finally, n-type C₆₀ was vacuum-evaporated to be the electronic transport layer. The 50 nm C₆₀ thin film, in conjunction with 100 nm Ag electrode layer, provided adequate electron current transport in the multilayered structures. The solar cell current density–voltage characteristics were evaluated and compared with the thin-film microstructures. The photo-electronic power-conversion efficiency could be improved to 14.2% when the annealing temperature was 500 °C and the film thickness was 200 nm. The thin-film solar cell characteristics of open-circuit voltage, short-circuit current density, fill factor, series-resistance, and Pmax were found to be 1.07 V, 19.69 mA/cm², 67.39%, 18.5 Ω and 1.42 mW, respectively.     

石墨烯/银复合薄膜的制备及表征

采用静电自组装技术,通过交替沉积聚(二烯丙基二甲基氯化铵)(PDDA)(或硝酸银)和氧化石墨烯,制备氧化石墨烯/PDDA薄膜和氧化石墨烯/硝酸银复合薄膜。然后在600℃下通入氩气和氢气进行气氛还原得到石墨烯薄膜和石墨烯/银复合薄膜。采用AFM、SEM、XPS、UV-Vis以及四探针电阻仪等对薄膜结构及性质进行表征。结果表明,通过静电自组装法可以获得生长均匀的薄膜。对比于相同自组装次数的石墨烯薄膜,石墨烯/银复合薄膜具有更好的透光性和更低的薄膜方块电阻。在λ=500 nm时,四层石墨烯/银复合薄膜的透过率为85%左右,而石墨烯薄膜的透过率为72%左右;石墨烯薄膜的方阻为161.39 kΩ.□-1,而石墨烯/银复合薄膜的方阻为99.11 kΩ.□-1。     

Electrical Properties of Ag Thin Films Deposited by the Improved SILAR Method

Ag films were deposited on glass substrates using the successive layer adsorption and reaction (SILAR) method and characterized with XRD and AFM. The I‐V curves of the thicker Ag films obeyed ohmic law because of the formation of the continuous films. After annealing at 300°C in N₂, the conductance increased due to the removal of imperfections. Compared with the thicker film, the thinner Ag films showed nonlinear I‐V curves. After annealing, these films were inconductible. This may be ascribed to the destruction of the junction, that existed between the Ag islands. The absorption spectra of the films proved the formation of the Ag islands after annealing. With the thickness of the films further decreasing, the Ag films became insulated.     

A comparative studyof heat‐treated Ag:SiO2 nanocomposites synthesized by cosputtering and sol‐gel methods

In this work, we compared formation and properties of heat‐treated Ag nanoparticles in silica matrix synthesized by RF‐reactive magnetron cosputtering and sol–gel methods separately. The sol–gel and sputtered films were annealed at different temperatures in air and in a reduced environment, respectively. The optical UV‐visible spectrophotometry have shown that the absorption peak appears at 456 and 400 nm wavelength indicating formation of silver nanoparticles in SiO₂ matrix for both the sol–gel and sputtering methods at 100 and 800 °C, respectively. XPS measurements showed that the metallic Ag⁰ nanoparticles can be obtained from both the techniques at these temperatures. According to XPS and AFM analysis, by increasing annealing temperature, the concentration of the Ag nanoparticles on the surface decreased and the nanoparticles diffused into the substrate for the sol–gel films, while for the films deposited by cosputtering method, the Ag surface concentration increased by increasing the temperature. Based on AFM observations, the size of nanoparticles on the surface were obtained at about 25 and 55 nm for sputtered and sol–gel films, respectively, supporting our optical data analysis. In comparison, the sputtering technique can produce Ag metallic nanoparticles with a narrower particle size distribution relative to the sol–gel method. Copyright © 2008 John Wiley & Sons, Ltd.     

Ag/PANI/Fe_2O_3复合纳米粒子的合成与催化性能

借助于PANI的还原性质,PANI/Fe2O3复合载体与AgNO3发生表面氧化还原反应,合成了Ag/PANI/Fe2O3复合纳米粒子。TEM和XRD结果表明,立方晶系纳米银的平均粒径10nm。FTIR结果表明,Ag与PANI及Fe2O3复合载体之间不存在化学键合作用,但由于PANI与Ag之间的电子相互作用,Ag/PANI/Fe2O3复合纳米粒子的FTIR吸收峰发生蓝移。Ag/PANI/Fe2O3复合纳米粒子对于间硝基苯磺酸钠的硼氢化钠还原反应表现出良好的催化活性,30min内间硝基苯磺酸钠的转化率达到86.77%。     

Characteristics of Ag/Bi<Subscript>3.25</Subscript>La<Subscript>0.75</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript>/p-Si heterostructure prepared by sol-gel processing

The metal-ferroelectric-semiconductor (MFS) heterostructure has been fabricated using Bi_3.25La_0.75Ti₃O₁₂ (BLT) as a ferroelectric layer by sol-gel processing. The effect of annealing temperature on phase formation and electrical characteristics of Ag/BLT/p-Si heterostructure were investigated. The BLT thin films annealed at from 500°C to 650°C are polycrystalline, with no pyrochlore or other second phases. The C-V curves of Ag/BLT/p-Si heterostructure annealed at 600°C show a clockwise C-V ferroelectric hysteresis loops and obtain good electrical properties with low current density of below 2×10⁻⁸ A/cm² within ±4 V, a memory window of over 0.7 V for a thickness of 400 nm BLT films. The memory window enlarges and the current density reduces with the increase of annealing temperature, but a annealing temperature over 600°C is disadvantageous for good electrical properties.     

Ag/Au Alloy LSPR Engineering by Co‐deposition of RF‐Sputtering and RF‐PECVD

Silver‐Gold alloy/diamond like carbon (Ag‐Au/DLC) nanocomposite films were prepared by co‐deposition of RF‐sputtering and RF‐PECVD on glass substrates by using acetylene gas and silver‐gold target. The deposition process was carried out at room temperature in one minute with the variable parameters of initial pressures and RF powers. X‐ray diffraction analysis demonstrated the formation of Ag/Au alloy nanoparticles with a face‐centered cubic (FCC) structure. Localized surface plasmon and optical properties of Ag‐Au alloy nanoparticles were studied by UV‐visible spectrophotometry which showed that increasing RF power and initial pressure cause a redshift in all samples. Moreover, the effect of RF power and initial pressure on the size and shape of nanoparticles were studied by 2D Atomic force microscopy images. Energy dispersive X‐ray spectroscopy revealed the formation of Ag‐Au/DLC nanoparticles and the percentages of C, Ag, Au and O in all samples. The applied method for Ag/Au alloy preparation is the one step and low‐cost method which makes the samples ready for sensing application.     

Fabrication of a Simple and Cheap Screen-printed Silver/Silver Chloride (Ag/AgCl) Quasi-reference Electrode

In this work, a silver/silver chloride ink is fabricated using two steps. First the silver ink is prepare using silver, nail polish and acetone. Then the silver ink is painted in a paper substrate and a silver chloride layer is deposited using a bleach solution. The result is the silver/silver chloride conductive ink. The silver ink is cheap ($2.49/g), well-dispersive and very easy to fabricate. The materials were characterized by SEM and XRD. The Ag ink showed the formation of a continuous network throughout the silver ink film with fewer agglomeration. The effective chlorination process was also observed in the Ag/AgCl characterization. Since the Ag/AgCl substrate will be used as a quasi-reference electrode, it is important to investigate the electrical properties. The Ag ink showed an average ohmic resistance of 2.27 Ω. The addition of the AgCl layer decreases the conductivity, as expected. In summary, the Ag/Ag/Cl ink developed is simple, well-dispersed, cheap and with good conductivity. Therefore, it can be used as a conductive ink in the fabrication of quasi-reference electrodes.     

Magnetic and Structural Characterizations of Co-based Heusler Nanoparticles Fabricated via Simple Co-precipitation Method

Nanoparticles of Co₂FeAl magnetic alloy was successfully fabricated in the presence of a well-known capping agent, polyvinyl alcohol, as a polymer template. The magnetic properties were studied using hysteresis curve and first-order reversal curve (FORC) measurements at room temperature. FORC diagrams demonstrated a wide distribution of the coercive field owing to the presence of different particle sizes in products. TEM image also showed that the synthesized samples are composed of some large clusters containing a few smaller particles. The maximum value of magnetization (~76 emu/g) and coercivity (573 Oe) were obtained in the annealed sample with 5 °C/min. A wider distribution of grain size with a smaller average of 20.5 nm as well as lower-degree of crystallinity was observed in the sample annealed with higher rate of 10 °C/min.     

吸附相反应技术制备Ag纳米粒子的反应机理

利用吸附相反应技术在SiO2表面制备Ag粒子, 研究了温度变化对载体表面NaOH的吸附、生成Ag的反应过程以及产物Ag粒子形貌的影响. NaOH的吸附率测定结果表明, 吸附平衡时间随着温度升高而增加. 温度升高加快了NaOH与Si—O—Si的反应, 使得NaOH的平衡吸附率不随吸附层的破坏而减少. 采用实时在线UV-Vis光谱研究了Ag粒子的生成过程, 发现温度超过40 ℃时, 反应体系中Ag出现的时间、Ag粒子的浓度和粒径分布范围都发生较大变化. 样品的TEM和XRD分析也表明, 当体系温度超过40 ℃时SiO2表面Ag粒子出现了团聚, 其晶粒粒径也出现了突变. 温度升高导致表面吸附层破坏, 使得Ag的生成场所从吸附层转移到SiO2表面, 最终导致Ag的反应机理和粒子形貌的变化.     

Selective dissolution of the silver component in colloidal Au and Ag multilayers: a facile way to prepare nanoporous gold film materials

Colloidal Au/Ag multilayer films were prepared by alternate assembly of Au nanoparticles with a size of 5 +/- 1.2 nm and Ag nanoparticles with a size of 10 +/- 2.4 nm by using 1,5-pentanedithiol as cross-linker. Nanoporous gold films with a ligament size of 26.7 +/- 4.6 nm were then prepared by selective dissolution of sacrificial templates of silver particles in colloidal Au/Ag multilayers. The complete dissolution of Ag particles in colloidal Au/Ag multilayers in a mixture solution of 3.0 mM HAuCl(4) and 3 M NaCl took place at room temperature without damage of the colloidal Au film. This method to prepare nanoporous gold films was further extended to the preparation of nanoporous gold nanotubes by depositing colloidal Au/Ag film on the inner wall of anodic aluminum oxides (AAO) followed by dissolution of colloidal Ag and removal of AAO templates.     

Synthesis of Ag and Ag/SiO2 sols by solvothermal method and their bactericidal activity

Ag and Ag/SiO₂ sols containing nanocrystalline silver particles can be advantageously prepared by solvothermal methods using an autoclave with conventional thermal or microwave heating. In this process, the reduction of silver salts can be realized with alcohols like ethanol in the presence of polyvinylpyrrolidone at temperatures of more than 120 °C. Furthermore a combination of silver salt reduction with hydrolysis of alkoxysilanes during the solvothermal process can yield Ag/SiO₂ composite sols. Particle size and crystallinity of as-prepared particles are analyzed by means of X-ray diffraction and high-resolution transmission electron microscopy. Nanosized silver particles gained by this process exhibit antimicrobial properties that are investigated in detail after application on textile fabrics.     

Novel fabrication of Ag thin film on glass for efficient surface-enhanced Raman scattering

This paper describes a very simple electroless-plating method used to prepare optically tunable nanostructured Ag films. Very stable Ag films can be reproducibly fabricated simply by soaking glass substrates in ethanolic solutions of AgNO3 and butylamine. The grain size of silver can be readily controlled to range from 20 to 150 nm, and these nanostructural features correlated well with their UV/vis absorption characteristics, as well as with their surface-enhanced Raman scattering (SERS) activities. It is also very advantageous that the Ag films prepared exhibit very even SERS activity over an area up to hundreds thousand square-micrometers, and the enhancement factor estimated using benzenethiol as a prototype adsorbate reaches approximately 2 x 10(5). Since the proposed method is cost-effective and is suitable for the mass production of diverse Ag films irrespective of the shapes of the underlying substrates, it is expected to play a significant role in the development of surface plasmon-based analytical devices.     

超声膜扩散法制备纳米银粒子

采用超声膜扩散(Ultrasound-assisted reaction method, UAMR)的方法, 以NaBH4还原溶液中的银离子, 在聚乙烯吡咯烷酮(PVP)为稳定剂的条件下, 制备出了平均粒度为4.7 nm的银纳米粒子. 与超声滴加法(Ultrasound-assisted dropping reaction method, UADR)相比, 超声膜扩散法制备出来的银纳米粒子的粒径小, 且尺寸分布较窄.