Cu–Ni nanoalloy phase diagram – Prediction and experiment

The Cu–Ni nanoalloy phase diagram respecting the nanoparticle size as an extra variable was calculated by the CALPHAD method. The samples of the Cu–Ni nanoalloys were prepared by the solvothermal synthesis from metal precursors. The samples were characterized by means of dynamic light scattering (DLS), infrared spectroscopy (IR), inductively coupled plasma optical emission spectroscopy (ICP/OES), transmission electron microscopy (TEM, HRTEM), and differential scanning calorimetry (DSC). The nanoparticle size, chemical composition, and Cu–Ni nanoparticles melting temperature depression were obtained. The experimental temperatures of melting of nanoparticles were in good agreement with the theoretical CALPHAD predictions considering surface energy.     

Au-Ni nanoparticles: Phase diagram prediction,synthesis, characterization,and thermal stability

The Au-Ni nanoparticles (NPs) were prepared by oleylamine solvothermal synthesis from metal precursors. The Au-Ni phase diagram prediction respecting the particle size was calculated by the CALPHAD method. The hydrodynamic size of the AuNi NPs in a nonpolar organic solvent was measured by the dynamic light scattering (DLS) method. The average hydrodynamic sizes of the nanoparticle samples were between 18 and 25 nm. The metallic composition of the AuNi NP samples was obtained by inductively-coupled plasma atomic emission spectroscopy (ICP-OES). The metallic fraction inside AuNi NPs was varied Au-(30–70) wt%Ni. The steric alkylamine stabilization was observed. The individual AuNi NPs were investigated by transmission electron microscopy (TEM). The dry nanopowder was also studied. The structures of the aggregated samples were investigated by scanning electron microscopy (SEM). The AuNi NPs reveal randomly mixed face-centered cubic (FCC) crystal lattices. The phase transformations were studied under inert gas and air. The samples were studied by differential scanning calorimetry (DSC).     

聚乙烯亚胺修饰的银纳米颗粒的制备研究及在肝素检测中的应用

该文利用分子量为600的高支化聚胺高分子PEI,在室温条件下,采用化学还原法,使用还原剂硼氢化钠,合成了银纳米颗粒。该方法具有操作简单、便捷、可重复性高等特点。对合成的颗粒进行了一系列的表征,包括紫外可见光谱的测量,动态光散射测量和透射电镜表征等。并以该银纳米颗粒为基础,建立了比色法传感器用于肝素的快速检测,并获得了较好的检测结果,检测限为1μg／mL。该检测方法具选择性高、灵敏度好,且检测耗时短,便于人眼直接观测等优点。     

Synthesis of novel SnO2/ZnSnO3 core-shell microspheres and their gas sensing properities

Large-scale novel core-shell structural SnO₂/ZnSnO₃ microspheres were successfully synthesized by a simple hydrothermal method with the help of the surfactant poly(vinyl pyrrolidone) PVP. The as-synthesized samples were characterized using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). The results indicate that the shell was formed by single crystalline ZnSnO₃ nanorods and the core was formed by aggregated SnO₂ nanoparticles. The effects of PVP and hydrothermal time on the morphology of SnO₂/ZnSnO₃ were investigated. A possible formation mechanism of these hierarchical structures was discussed. Moreover, the sensor performance of the prepared core-shell SnO₂/ZnSnO₃ nanostructures to ethanol was studied. The results indicate that the as-synthesized samples exhibited high response and quick response-recovery to ethanol.     

Formation and optical properties of silver superlattice using hydrazine hydrate as reducing agent

Superlattice of silver nanoparticles was prepared using a liquid–liquid two-phase method with hydrazine hydrate (N₂H₄·H₂O) as reducing agent. The ordered of silver nanoparticles were formed on carbon films coated on transmission electron microscopy (TEM) copper grids by evaporating a drop of silver colloid. The scanning electron microscope, energy dispersive X-ray spectrometer analyses, X-ray diffraction, and fluorescence spectrometer were used to characterize the superlattice. The formation process of the silver nanoparticles was investigated by UV–visible absorption spectroscopy and TEM. The TEM images show directly the results with obvious structure of superlattice. In addition, the UV–visible spectra of the silver nanoparticles colloidal phase obtained finally showed that the system is monodisperse.     

Calphad-type assessment of the Sb–Sn–Zn ternary system

The ternary Sb–Sn–Zn phase diagram was investigated experimentally by scanning electron microscopy (SEM) and differential thermal analysis (DTA) of long-term annealed samples. The overall composition of each sample was measured by energy-dispersive X-ray spectroscopy (EDX). The experimental results, together with additional available literature data, were used to perform a CALPHAD-type thermodynamic assessment of this ternary system. Two calculated isothermal sections (250 and 350 °C), an isopleth (x(Sn)=17.57%) and the Zn activity in liquid ternary Sb–Sn–Zn alloys at 550 °C for the composition ratio Sn/Sb=1/3 and at 650 °C for the ratio Sn/Sb=9 are presented with experimental points superimposed. The liquidus projection for the ternary Sb–Sn–Zn system is also presented. The agreement between calculated and experimental results is reasonable.     

Novel nano polymeric system containing biosynthesized core shell silver/silica nanoparticles for functionalization of cellulosic based material

An innovative strategy for functional finishing of cellulosic based materials is based on the incorporation of a thin layer of surface modifying systems (SMS) in the form of stimuli-sensitive nanogels containing combining metal nanoparticles and silica. The silver–silica core–shell nanoparticles (NPs) were synthesized by simple one pot chemical method. Silica/silver nanoparticles have been synthesized using low concentration of dextran as reducing and stabilizing agent and using ascorbic acid as antioxidant agent. The core–shell NPs were characterized for their structural, morphological, compositional and optical behaviour using X-ray diffraction, scanning electron microscopy and energy dispersive X-ray analysis. Stimuli-responsive nanogel was prepared by copolymerization of poly(N-isopropylacrylamide) with pullulan, results in a nanogel that is responsive to both temperature and pH, the nano-particulate hydrogel of poly-NiPAAm-pullulan copolymer was synthesized using surfactant-free emulsion method. The prepared nano-particles were used during the preparation steps of the pullulan nanogel to obtain nanogel/combining metal/silica NPs to produce a composite materials. The nanoparticle size in dry (collapsed) state is estimated at 250 nm by SEM and TEM, and effect of temperature and pH on gel-nanoparticles was investigated by DLS and UV–vis spectrophotometry. The incorporation of the nanoparticles to cellulosic material was done by a simple pad dry-cure procedure from aqueous nanoparticle dispersion that contained a cross-linking agent. This application method provided sufficient integrity to coating by maintaining the responsiveness of surface modifying system. The stimuli responsiveness of modified cellulosic materials has been confirmed in terms of regulating its water uptake in dependence of pH and temperature.     

Molecular dynamics-based refinement of nanodiamond size measurements obtained with dynamic light scattering

The determination of particle size by dynamic light scattering uses the Stokes–Einstein relation, which can break down for nanoscale objects. Here, we employ a molecular dynamics simulation of fully solvated 1–5 nm carbon nanoparticles for the refinement of the experimental data obtained for nanodiamonds in water by using dynamic light scattering. We performed molecular dynamics simulations in differently sized boxes and calculated nanoparticles diffusion coefficients using the velocity autocorrelation function and mean-square displacement. We found that the predictions of the Stokes–Einstein relation are accurate for nanoparticles larger than 3 nm while for smaller nanoparticles the diffusion coefficient should be corrected and different boundary conditions should be taken into account.     

Re-assessment of the Mg–Zn–Ce system focusing on the phase equilibria in Mg-rich corner

The Mg–Zn–Ce alloys exhibit good creep resistance and strength at elevated temperature due to the formation of intermetallic compounds. However, the ternary compounds and phase equilibria in the Mg-rich corner are still controversial which restrains the development of Mg–Zn–Ce alloys. The present work experimentally investigated the phase equilibria in Mg-rich corner of the Mg–Zn–Ce system at 350 and 465 °C and thermodynamically assessed the Mg–Zn–Ce system. The existence of ternary compounds τ₁ and τ₃ were confirmed by a combination of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The crystal structure of τ₁ was resolved as space group of Cmc21 with a = 0.9852(2)–1.0137(2) nm, b = 1.1361(3)–1.1635(3) nm and c = 0.9651(2)–0.9989(2) nm by Rietveld refinement of the XRD pattern. Three invariant reactions, L→τ₃+CeMg₃+CeMg₁₂, L+CeMg₁₂→α-Mg+τ₁ and L+τ₁→τ₂+α-Mg, were revealed by differential scanning calorimeter (DSC) measurement and microstructure characterization. Then, a set of self-consistent thermodynamic parameters was thereafter constructed by assessing the phase equilibria, solid solubilities of CeMg₁₂, τ₁, CeMg₃ and τ₃, as well as the formation enthalpies of binary and ternary compounds calculated by density functional theory. The comparison of calculated phase diagram with experimental results and the literature were discussed. The calculated isothermal section of Mg–Zn–Ce system at 465 °C agreed with our experimental data. The two three-phase equilibria, τ₁+α-Mg+CeMg₁₂ and CeMg₃+τ₃+CeMg₁₂, were confirmed in the Mg-rich corner. This thermodynamic database can be used for the further alloys design of Mg–Zn–Ce system.     

Large-area Raman enhancement substrates using spontaneous dewetting of gold films and silver nanoparticles deposition

We present a cost-effective method for making large-area surface enhanced Raman scattering (SERS) substrates by using spontaneous dewetting of ultrathin gold film. The dewetting of 5-nm-thick gold film formed high-density gold islands ranged from 40 nm to 80 nm. The measured SERS signal was 5 times stronger than synthesised gold nanoparticles. The SERS signals can be further increased by depositing small silver nanoparticles on the dewetted film. The experimental results showed 5-nm-thick silver coating increased SERS signals up to 10 times. The calculations by finite-difference time-domain method verified such SERS enhancement originated from enhanced electric fields between gold islands and silver nanoparticles. In the application, we demonstrated an all-optical measurement of pH values in microfluidic devices by using SERS signals of para-mercaptobenzoic acid.     

Experimental investigation and thermodynamic assessment of the Mn–Zr system

The Mn–Zr binary system has been investigated via experimental measurements and thermodynamic calculations. In order to investigate phase equilibria in the Mn–Zr system, five alloys were prepared by arc melting under vacuum. All alloys were examined by means of X-ray diffraction, scanning electron microscopy and electron probe microanalysis after annealing at 650 °C for 70 days or 950 °C for 30 days. The homogeneity range of ZrMn₂ was determined to be from 25.0 to 33.2 at.% Zr at 950 °C and from 26.7 to 34.3 at.% Zr at 650 °C. The solubility of Mn in (αZr) was 1.6 at.% Mn, while that of Zr in (αMn) was 0.2 at.% Zr at 650 °C. The invariant reaction temperatures of liquid → ZrMn₂ + (βZr) and (βZr) → ZrMn₂ + (αZr) were determined to be 1131 and 785 °C, respectively. A thermodynamic assessment of the Mn–Zr system was conducted by taking into account the present experimental results and reliable literature data. The calculated results using the presently obtained parameters can well reproduce the experimental data.     

One-step preparation of carbon nanotubes with nickel as the core

CNTs with core-shell structure were successfully synthesized by a microwave-assisted polyol method,and magnetic Ni nanoparticles were employed as a catalyst. The preparation method is fast and simple. The structures,morphology and magnetic properties of the as-synthesized samples were investigated using Raman spectrometer,X-ray diffraction (XRD),transmission electron microscopy (TEM),vibrating sample magnetometer (VSM),respectively. The XRD results suggested that Ni particles used as a catalyst in our exper...     

Spectroscopic and photoluminescence properties of MgO:Cr3+ nanosheets for WLEDs

This work explores the synthesis of nanocrystalline MgO:Cr³⁺ (1–9 mol%) nanophosphors via solution combustion route at 400 °C. The nanophosphors were well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infra-Red (FTIR) spectroscopy. PXRD results confirm cubic phase and SEM micrographs indicate that the particles are highly porous and agglomerated. The TEM images show that the powder consists of spherical particles of size ∼5–15 nm. Upon 356 nm excitation the emission profile of MgO:Cr³⁺ exhibits an emission peak at 677 nm due to ²E_g → ⁴A_2g transition. It was observed that PL intensity increases with increase in Cr³⁺ concentration and highest PL intensity was observed for 3 mol% doped sample and afterward it decreases, attributed to concentration quenching. The resultant CIE chromaticity co-ordinates in the white region make the present phosphor highly useful for display applications and also for white light-emitting diodes (WLEDs).     

Crystallization in Zr_(60)Al_(15)Ni_(25) bulk metallic glass subjected to rolling at room temperature

The microstructure evolution of Zr60Al15Ni25 bulk metallic glass during rolling at room temperature is investigated by differential scanning calorimetry(DSC),high-resolution transmission electron microscopy(HRTEM) and selected area electronic diffraction(SAED).The HRTEM images show that shear bands are produced in the rolled specimens,indicating the essence of inhomogeneous deformation due to rolling,and that there exist nanocrystals with size of about 5-10 nm in the transition regions between the shear ban...     

Annealing temperature effect on structural,optical, morphological and electrical properties of CdS/Si(100) nanostructures

CdS nanostructures have grown on p-type silicon (Si) (100) substrates using sol–gel method. The crystalline quality, surface morphology, optical and electrical properties of the deposited CdS nanostructures have been characterized and analyzed using atomic force microscopy, scanning electron microscopy, X-ray diffraction, thermogravimetric analysis, differential thermal analysis, UV–vis spectroscopy and electrical characterization, respectively. The effect of annealing temperature in the range 200–600 °C on the structural, morphological, optical and electrical properties has been elaborated. The XRD analysis shows that the crystalline quality can be improved by increasing the temperature to 400 °C, but further increase to 600 °C leads to degradation of crystalline quality. The bulk modulus is calculated and showed good agreement with experimental and theoretical results. The optical properties of absorption, reflection, energy band gap and extinction coefficient are obtained by UV–vis spectroscopy. The calculated refractive index and optical dielectric constant have shown good agreement with other results. The electrical and thermal properties are studied for antireflection coating applications.     

Hydrothermal synthesis and gas sensing characters of ZnO nanorods

ZnO nanorods are prepared by a hydrothermal process with cetyltrimethylammonium bromide (CTAB) and zinc powder at 182 °C. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The gas sensing properties of the materials have been investigated. The results indicate that the as-prepared ZnO nanorods show much better sensitivity and stability than the conventional materials. The PdO doping can improve the sensitivity and selectivity of the sensors. ZnO nanorods are excellent potential candidates for gas sensors.     

Selectivity of flame-spray-made Nb/ZnO thick films towards NO2 gas

Unloaded ZnO and Nb/ZnO nanoparticles containing 0.25, 0.5 and 1 mol.% Nb were produced in a single step by flame-spray pyrolysis (FSP) technique. The nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The BET surface area (SSA_BET) of the nanoparticles was measured by nitrogen adsorption. FSP yielded small Nb particles attached to the surface of the supporting ZnO nanoparticles, indicating a high SSA_BET. The morphology and accurate size of the primary particles were further investigated by TEM. Nb/ZnO nanoparticles paste composed of ethyl cellulose and terpineol as binder and solvent respectively was coated on Al₂O₃ substrate interdigitated with gold electrodes to form thick films by spin coating technique. After the sensing tests, the morphology and the cross-section of sensing film were analyzed by SEM and EDS analyses. The influence on a low dynamic range of Nb concentration on NO₂ response (0.1-4 ppm) of thick film sensor elements was studied at the operating temperatures ranging from 250 to 350 °C in the presence of dry air. The optimum Nb concentration was found be 0.5 mol.% and 0.5 mol.% Nb exhibited an optimum NO₂ response of ∼1640 and a short response time (27 s) for NO₂ concentration of 4 ppm at 300 °C.     

A novel facile synthesis and electromagnetic wave shielding effectiveness at microwave frequency of graphene oxide paper

Nano-structured graphene oxide (GO) freestanding paper was synthesized by an arc recharge technique in flowing of oxygen for the first time. This technique offers new ways on how e.g. layers structure nanomaterials could be produced. The morphology and structural properties of the as-synthesized GO were examined by means of X-ray diffraction, Fourier transform infrared spectra, scanning electrom microscopy, energy dispersive x-ray spectroscopy, transmission electron microscopy, high resolution transmission electron microscopy and selective area electron diffraction techniques. The structural and morphological characterizations revealed that the synthesized GO were well-defined nanosheets with a thickness of 6 nm. The optical band gap was calculated from the absorption spectrum, and was found to be 3.32 eV. Furthermore, we aim to use GO paper to develop new electromagnetic interference shielding sheets that have a high shielding effectiveness (SE) (over 30 dB) at frequencies in the 1–12 GHz range. The complex permittivity and total shielding effectiveness of as synthesized GO freestanding paper are measured at frequencies from 1 to 12 GHz. Finally, to enhance the performances of the electromagnetic shields effectiveness, five-layered GO sheets were made. Furthermore, the highest SE for the light-weight freestanding GO paper was 50 dB at 1 GHz, indicating commercial use for many industrial or military shielding applications as an attractive candidate for the new type of microwave shielding.     

Dispersive SnO2 nanosheets: Hydrothermal synthesis and gas-sensing properties

SnO₂ nanosheets with the thickness of 10 nm were successfully synthesized by a simple hydrothermal process at 180 °C for 12 h. The samples were characterized by X-ray power diffraction, scanning electron microscopy, transmission electron microscopy, and high-resolution transmission electron microscopy. The sensor performance of the as-prepared SnO₂ nanosheets for ethanol and carbon monoxide was measured. The results indicate that the sensor exhibited high response, quick response-recovery kinetics, and good repeatability.