Transformation of sputtered calcium copper titanate thin film into nanorods by sequential annealing

Rapid synthesis of long calcium copper titanate (CCTO) nanorods was carried out by sequential annealing. CCTO thin films have been deposited on p-Si substrate by RF sputtering technique and afterwards, the samples were thermally treated using a preheated furnace by varying the annealing temperature from 850 °C to 1100 °C. CCTO nanorods of 12 µm lengths and 400–600 nm diameters were synthesized at 1100 °C. Based on the FESEM observations, a plausible growth mechanism has been proposed to explain the formation of nanorods. The (220) XRD peak of the CCTO film became prominent for the annealing temperature of 950 °C. The presence of nanoscale crystals in amorphous matrix has been observed by HRTEM studies. The elemental mapping of CCTO nanorod has shown a spatial variation of elements throughout the nanorod. The oxide and interface charge density was found to be increased with the rise in annealing temperature.     

Binder jetting additive manufacturing of aluminum nitride components

In this work, we report on the novel fabrication of aluminum nitride (AlN) components using Binder Jetting (BJT) additive manufacturing (AM). The AlN constructs were subjected to post-fabrication thermal treatment by hot isostatic pressing (HIPing) for 8 hours at a pressure of 206 MPa and temperature of 1900 °C. This treatment resulted in a 60.1% relative density maximum densification for AlN. The BJT printed AlN specimens were analyzed using various characterization techniques. The purity, microstructure, and polycrystallinity of the AlN phase formed were confirmed by techniques that included x-ray diffraction (XRD), scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), and high-resolution transmission electron microscopy (HRTEM). Second harmonic generation (SHG) microscopy showed polarization dependence and second harmonic signal at 470 nm, indicating the potential to produce thermal and optical-mechanical devices. Mechanical properties obtained by nanoindentation resulted in an elastic modulus of ~251 GPa when measured in fully dense, contiguous crystalline regions, corresponding to an apparent, porous bulk stiffness of ~90 GPa for the final, 60.1 % dense products. Finally, the laser flash method (LFM) was used to measure the thermal conductivity of the material as a function of temperature resulting in values from 4.82 W/mK to 3.17 W/mK for the temperature range from 23 °C to 500 °C, respectively.     

Surfactant-free electrochemical synthesis of fluoridated hydroxyapatite nanorods for biomedical applications

Fluoridated hydroxyapatite (FHA) [Ca₁₀(PO₄)₆F_x(OH)_2−x, x = 0–2] is believed to be a promising calcium phosphate (CaP) to replace pure hydroxyapatite (HA) for next-generation implants, owing to its better biocompatibility, higher antibacterial activity, and lower solubility. Notably, the shape and size of the CaP crystals play key roles in their performance and can influence their applications. One-dimensional (1D) FHA nanorods are important CaP materials which have been widely used in regenerative medicine applications such as restorative dentistry. Unfortunately, the traditional synthesis methods for FHA nanorods either employ surfactants or take a relatively long time. In this study, we aimed to propose a facile synthesis route to fabricate FHA nanorods without any surfactants using an electrochemical deposition method for the first time. This study focused on preparing FHA nanorods without the assistance of any surfactant, unlike the traditional synthesis methods, to avoid chemical impurities. FHA nanorods with lengths of 124–2606 nm, diameters of 28–211 nm, and aspect ratios of 4.4–21.8 were synthesized using the electrochemical method, followed by a heat treatment. For the as-synthesized FHA nanorods, the Ca/P ratio was 1.60 and the atomic concentration of F was 2.06 at.%. An ultrastructure examination revealed that each FHA nanorod possessed long-range order, good crystallinity, and a defect-free lattice with a certain crystallographic plane orientation along the whole rod. In short, we propose a novel, surfactant-free, cost-saving, and more efficient route to synthesize FHA nanorods which can be widely applied in multiple biomedical applications, including drug delivery, bone repair, and restorative dentistry.     

Preparation and characterization of heteroepitaxial Zn2SnO4 single crystalline films prepared on MgO (100) substrates

Zinc stannate (Zn₂SnO₄) films were deposited on MgO (100) substrates by pulsed laser deposition, and Zn₂SnO₄ monocrystalline films were obtained by postannealing process. The structures, surface morphologies, and optical properties of the Zn₂SnO₄ films annealed at different temperatures were investigated in detail. Crystal structure analyses showed that the film annealed at 800°C was single crystal Zn₂SnO₄ with an inverse-spinel structure. The heteroepitaxial mechanism was further clarified by a schematic diagram, and the epitaxial relationships between the film and substrate were Zn₂SnO₄ (400) || MgO (200) with Zn₂SnO₄ [001] || MgO [001]. The obtained Zn₂SnO₄ films exhibited excellent transparency. The optical band gap of the 800°C-annealed Zn₂SnO₄ film was about 3.97 eV. The extinction coefficients and refractive indexes of the Zn₂SnO₄ films annealed at different temperatures as a function of wavelength were analyzed in detail.     

NiCrAlFe精密电阻合金中的L12有序结构研究

有序结构的形成是决定NiCrAlFe精密电阻合金电学性能的关键因素。本文利用第一性原理赝势平面波方法，计算了合金处于无序固溶体结构和形成L12型有序结构时的结合能、态密度、晶格常数等参数，并利用高分辨透射电子显微镜（HRTEM）对合金进行了结构表征，还测试了固溶态和时效态的电阻率。从结合能来看，该合金形成L12有序结构时比无序固溶体更加稳定；态密度以及部分态密度计算结果则表明，在L12有序结构中，Ni、Cr、Al、Fe会强烈成键而使得整个合金体系变得稳定；HRTEM分析结果证明固溶态合金经过和时效处理后出现了L12有序结构，而且该有序结构的晶格常数与计算值基本一致。对比无序固溶体与L12型有序结构费米能级处的态密度值发现，当形成L12有序结构时合金的导电能力较无序固溶体下降，电阻率升高，与实际测试结果吻合。     

Carbon nanotube–polyaniline composites

The last decade has seen a growing interest in hybrid electrically conducting nanocomposites. This article aims to provide a detailed overview of the present status of research in carbon nanotube–polyaniline (CNT/PANI) composites, from processing to structural and property evaluations. CNT/PANI are synthesized by electrochemical and chemical processing. When chemical methods are used, the main challenge is to obtain processable CNT/PANI in the emeraldine salt (ES) form composites. Stable dispersions of ES–CNT in organic media are prepared using the post doping method, inverse emulsion polymerization, or ex situ polymerizations. On the contrary, stable water dispersions of CNT/ES are prepared using hydrophilization of a preformed CNT/ES composite, direct synthesis of micelle–CNT hybrid templates, interfacial polymerization, covalent functionalization of CNT with a water soluble polymer, or using electrostatic interactions between two oppositely charged ES and CNT aqueous colloids. Moreover, the strategies for the synthesis of ternary CNT/PANI composites incorporating noble metal nanoparticles, metal oxide, or graphene sheets are also presented and analyzed in depth. Finally, we give a review of potential applications, including chemical sensors, capacitors, fuel cells and electronic devices.     

Synthesis,structural and morphological characteristics,magnetic and optical properties of Co doped ZnO nanoparticles

Zn_1−xCo_xO (x==0.05, 0.10, 0.15) nanoparticles have been synthesized by an alternative wet-chemical synthesis route using the SimAdd technique. The as-obtained powders were investigated by FT-IR spectroscopy, X-ray diffraction and thermal analysis correlated with evolved gas analysis (TG–DTA–FT-IR) in order to determine their chemical nature, crystalline structure and to establish the decomposition sequences. The precipitates are generally amorphous, but low-intensity reflection peaks assigned both to the zinc oxalate dihydrate, and zinc hydroxide can be observed in the recorded patterns, indicating that hydroxy-oxalate precipitates were obtained. The structure, morphology and magnetic properties of the thermally treated samples have been investigated by X-ray diffraction, FT-IR, HRTEM, SAED, UV–vis and EPR. XRD studies reveal a hexagonal wurtzite-type structure for all Zn_1−xCo_xO samples. TEM investigations show particle size between 28 and 37 nm, with spherical and polyhedral shapes and with tendency to form aggregates. The presence of a Co₃O₄ secondary phase was evidenced by XRD, UV–vis and EPR for the Zn_0.85Co_0.15O sample. The ferromagnetic behavior of the samples was revealed. The paper highlights that by varying the cobalt concentration it is possible to modulate the structural, morphological, optical and magnetic properties.     

Suppression of dislocations by Sb spray in the vicinity of InAs/GaAs quantum dots

The effect of Sb spray prior to the capping of a GaAs layer on the structure and properties of InAs/GaAs quantum dots (QDs) grown by molecular beam epitaxy (MBE) is studied by cross-sectional high-resolution transmission electron microscopy (HRTEM). Compared to the typical GaAs-capped InAs/GaAs QDs, Sb-sprayed QDs display a more uniform lens shape with a thickness of about 3 ~ 4 nm rather than the pyramidal shape of the non-Sb-sprayed QDs. Particularly, the dislocations were observed to be passivated in the InAs/GaAs interface region and even be suppressed to a large extent. There are almost no extended dislocations in the immediate vicinity of the QDs. This result is most likely related to the formation of graded GaAsSb immediately adjacent to the InAs QDs that provides strain relief for the dot/capping layer lattice mismatch.

PACS

81.05.Ea; 81.07.-b; 81.07.Ta     

Characterisation and sintering studies of mechanically milled nano tungsten powder

Abstract

Elemental tungsten powder was mechanically milled by planetary mill for 100 h. Particles were thinned down to nanometre scale. The shape of the milled powders was flat cylindrical with average diameter and length 12˙5 and 46˙5 nm respectively. The corresponding crystallite size obtained by X-ray diffraction (XRD) was 26˙96 nm. The results obtained by XRD and small angle X-ray scattering were well supported by transmission electron microscopy and high resolution transmission electron microscopy results. The maximum shrinkage of the compact has been observed at ～1500 K, which has been used as a guideline for sintering experiments. The powders sintered at 1773 K have resulted in 96% relative density.     

Soft x-ray reflectometry,hard x-ray photoelectron spectroscopy and transmission electron microscopy investigations of the internal structure of TiO2(Ti)/SiO2/Si stacks

Abstract

We developed a mathematical analysis method of reflectometry data and used it to characterize the internal structure of TiO₂/SiO₂/Si and Ti/SiO₂/Si stacks. Atomic concentration profiles of all the chemical elements composing the samples were reconstructed from the analysis of the reflectivity curves measured versus the incidence angle at different soft x-ray reflection (SXR) photon energies. The results were confirmed by the conventional techniques of hard x-ray photoelectron spectroscopy (HXPES) and high-resolution transmission electron microscopy (HRTEM). The depth variation of the chemical composition, thicknesses and densities of individual layers extracted from SXR and HXPES measurements are in close agreement and correlate well with the HRTEM images.