Porous indium oxide thin films deposited by electrostatic spray deposition technique

This paper presents the preparation process of porous indium oxide (In₂O₃) films using a novel deposition technique, i.e., electrostatic spray deposition (ESD). The films were deposited on platinum-coated alumina substrates using as precursor solution indium chloride in ethanol and acetic acid. The films were characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM) and Raman spectroscopy. The nanocrystalline structure of the films was evidenced by TEM and also by XRD studies. The Raman spectroscopy and XRD measurements revealed the cubic phase of In₂O₃ films. Considering the obtained results, we conclude that the ESD technique is an efficient, cheap and successful method for the preparation of porous indium oxide films.     

Dense nanostructured calcium phosphate coating on titanium by cold spray

This article deals with the understanding of building-up mechanisms of bioactive nanocrystalline hydroxyapatite coatings by Cold Spray, revealing very promising results in contrast to more conventional techniques such as Plasma Spray. A full characterization of feedstock and coatings is provided. The agglomerated structure of the powder proved to be suitable to obtain successfully thick hydroxyapatite coatings. A crystallite size below ∼20 nm in the powder and the as-sprayed coatings is calculated by the Rietveld X-ray refinement method and agreed by Transmission Electron Microscopy. Some wipe tests were carried out on Ti6Al4V substrates in order to study the deposition of single particles and the nanoscale features were evaluated. The resulting structure indicates that there is no delimitation of particle boundaries and the overall coating has been formed by effective compaction of the original nanocrystallites, leading to consistent and consolidated layers.     

Computational study of particle in-flight behavior in the HVOF thermal spray process

A computational framework is developed for the multiphase flow in a high velocity oxygen-fuel (HVOF) thermal spray coating process with steel powders as the feedstock. The numerical model includes continuum-type differential equations that describe the evolution of gas dynamics and multi-dimensional tracking of particle trajectories and temperature histories in the turbulent reacting flow field. The numerical study shows that the particle temperature is strongly affected by the injection position while the particle velocity is less dependent on this parameter. Moreover, both particle velocity and temperature at impact are strongly dependent on particle size, although the spatial variation of these two variables on the substrate is minimal. It is also found that not all the particles are deposited on the substrate perpendicularly (even if the spray angle is 90°), due to substantial radial fluid velocities near the stagnation point. A statistical distribution of particle velocity, temperature, impinging angle and position on the substrate as well as particle residence time is obtained in this work through independent random tracking of numerous particles by accounting for the distributed nature of particle size in the feedstock and injection position as well as the fluctuations in the turbulent gas flow.     

The use of artificial neural networks in electrostatic force microscopy

ABSTRACT: The use of electrostatic force microscopy (EFM) to characterize and manipulate surfaces at the nanoscale usually faces the problem of dealing with systems where several parameters are not known. Artificial neural networks (ANNs) have demonstrated to be a very useful tool to tackle this type of problems. Here, we show that the use of ANNs allows us to quantitatively estimate magnitudes such as the dielectric constant of thin films. To improve thin film dielectric constant estimations in EFM, we first increase the accuracy of numerical simulations by replacing the standard minimization technique by a method based on ANN learning algorithms. Second, we use the improved numerical results to build a complete training set for a new ANN. The results obtained by the ANN suggest that accurate values for the thin film dielectric constant can only be estimated if the thin film thickness and sample dielectric constant are known.PACS: 07.79.Lh; 07.05.Mh; 61.46.Fg.     

Dynamic characteristics of charged droplets in an electrostatic spraying process with twin capillaries

The experimental and simulated investigations on electrostatic spraying with twin capillaries are carried out. The starting electric voltage required for the cone-jet and the deposition characteristics of the droplets are measured. The whole spraying process, which includes jet and droplet motions, is simulated and the simulated results on the motions of jet and droplet are basically consistent with the experiments. According to the simulated results, the contributions of various electric forces to droplet movement are quantitatively analyzed and the droplet dynamic characteristics, especially the interaction mechanism between two sprays, are revealed. The test results on the droplet deposition characteristics partially support the simulated results on the droplet motion. The present work is useful for a better understanding on the interaction between sprays in double or multi-capillary system.     

Mixing in vibrated granular beds with the effect of electrostatic force

In this study, the DEM (Discrete Elementary Method) is used to simulate the behavior of granular mixing in vibrated beds. First, the velocity fields are simulated by the DEM model to examine the convective currents in a three-dimensional vibrated granular bed. Then, in order to characterize the effect of electrostatic force on the granular flow, the electrostatic number Es is defined as the ratio of the electrostatic force to the particle weight. Also, to quantify the quality of mixing, the mixing degree M is used by the well-known Lacey index. The top–bottom and the side–side initial loading patterns of two groups of glass bead with different colors are employed to investigate the influence of the convective currents on the granular mixing. To simplify the electrostatic effect, these two groups of glass beads are given opposite charges and the charged strength is assumed to be constant. The simulation results demonstrate that the granular temperatures increase linearly with the increasing Es number. Meanwhile, the mixing rate constants, calculated from the time evolutions of mixing degree, increase with the increasing Es number in power law relations. The role of granular temperature in the granular mixing is also discussed in this paper.     

Protective properties of Al2O3 + TiO2 coating produced by the electrostatic spray deposition method

Mechanical resistance of Al₂O₃ + TiO₂ nanocomposite ceramic coating deposited by electrostatic spray deposition method onto X10CrAlSi18 steel to thermal and slurry tests was investigated. The coating was produced from colloidal suspension of TiO₂ nanoparticles dispersed in 3 wt% solution of Al₂(NO₃)₃, as Al₂O₃ precursor, in ethanol. TiO₂ nanoparticles of two sizes, 15 nm and 32 nm, were used in the experiments. After deposition, coatings were annealed at various temperatures, 300, 1000 and 1200 °C, and next exposed to cyclic thermal and slurry tests. Regardless of annealing temperature and the size of TiO₂ nanoparticles, the outer layer of all coatings was porous. The first five thermal cycles caused a rapid increase of aluminum content of the surface layer to 30–37 wt%, but further increase in the number of thermal cycles did not affect the aluminum content. The oxidation rate of coating-substrate system was lower during the thermal tests than during annealing. The oxidation rate was also lower for smaller TiO₂ particles (15 nm) forming the coating than for the larger ones (32 nm). The protective properties of Al₂O₃ + TiO₂ coating against intense oxidation of substrate were lost at 1200 °C. Slurry tests showed that coatings annealed at 1000 °C had the best slurry resistance, but thermal tests had weakened this slurry resistance, mainly due to decreasing adhesion of the coating.     

Mechanism of densification of calcium carbonate by cold sintering process

In general, carbonates cannot be easily hardened by the conventional ceramic sintering process due to their thermal decomposition during heating. However, when the cold sintering process (CSP) is selected, carbonates can be hardened at lower temperatures. It has been demonstrated that calcium carbonate can be hardened by CSP, but the detailed densification mechanisms of cold sintering at various temperatures have not been fully clarified. In this study, the vaterite phase of calcium carbonate was selected as the starting material. As the cold sintering temperature for calcium carbonate powder increased, the bulk density of the hardened calcium carbonate body increased. The compressive strength was maximized when cold sintered at 80 °C due to the balance between the solubility of calcium carbonate and the reactivity of cold sintering. Almost no crystal phase transformation from vaterite to calcite occurred during cold sintering, and reprecipitation of the vaterite phase though dissolution-precipitation densified the body.     

Preparation and properties of LiF transparent ceramics by cold sintering process

The development of optoelectronic devices depends on the development of optoelectronic materials such as transparent ceramics. LiF transparent ceramics are photoelectronic ceramics with excellent photoelectric properties. Still, the traditional preparation of LiF transparent ceramics generally needs a high temperature or high-pressure environment, and the cost is high. This paper adopts a cold sintering process to prepare high-density LiF transparent ceramics at low temperatures to reduce the preparation conditions. The effects of different cold sintering temperatures on microstructure, density, hardness, visible and near-infrared transmittance, and electrical properties of transparent ceramics were studied. The results show that using LiOH solution as the solvent, the relative density of LiF ceramics can reach up to 99.64% under the sintering condition of 375 °C/470 MPa, and the Vickers hardness is 1.34 GPa. Vickers hardness is 1.34 GPa. The transmittance in the visible and near-infrared regions is 60.45% and 85.31%, respectively. The dielectric constant and dielectric loss of 13 GHz are 4.36 and 1.11 × 10⁻³, respectively.     

Electrochemical performance of nano-SiO2 modified LiCoO2 thin films fabricated by electrostatic spray deposition (ESD)

With a mixture of a SiO₂ sol and a solution of lithium and cobalt acetates as the precursor, nano-SiO₂ modified LiCoO₂ films were fabricated by the electrostatic spray deposition (ESD) technique. The SiO₂ content of these films was 0, 5, 10, 15 and 20 wt%, respectively. Their structure and electrochemical properties were characterized by means of X-ray diffraction, scanning electron microscopy, galvanostatic cell cycling, AC impedance spectroscopy and cyclic voltammetry. Li₂CoSiO₄ was found formed in the SiO₂-containing films. The film with 15 wt% SiO₂ shows the best cycling stability with the capacity of 130 mAh/g in the voltage range between 2.7 and 4.3 V at the current density of 0.1 mA/cm². Due to its resulted small cell impedance, it has excellent rate capability. A LiCoO₂ (shell)/SiO₂ (core) structure model is proposed to explain the improved properties of these films.     

Influence of incongruent dissolution-precipitation on 8YSZ ceramics during cold sintering process

The incongruent dissolution-precipitation behaviors of 8YSZ (8 mol% yttria-stabilized zirconia) ceramics during cold sintering process is studied in this paper by changing the pH of liquid media. The different solubility of Y³⁺ and Zr⁴⁺ at the same lattice position causes the disparate dissolution behaviors, and results in incongruent precipitation. Compared with acidic or alkaline solution, neutral solution is more conducive to the incongruent dissolution-precipitation process, and the concentration ratio of dissolved Y³⁺ and Zr⁴⁺ can reach ～6385. The incongruent dissolution-precipitation process facilitates the formation of neck structure and promotes the ionic migration and diffusion at the subsequent high-temperature sintering process, which improves the mechanical properties and electrochemical properties of 8YSZ ceramics. This work reveals the principle of incongruent dissolution-precipitation process of zirconia-based ceramics, and it is of significance for selecting suitable liquid media to control the incongruent dissolution-precipitation behaviors in cold sintering process to prepare high-performance zirconia-based ceramics.     

CPK法在精密仪器喷涂工艺中的应用

精密仪器表面的涂装,除了要求具备一般涂层的性能外,对涂层厚度的控制十分严格.本文采用品质管理中的CPK法对数码相机镜头部件涂装后的尺寸进行分析,以准确判定该涂装工艺在涂层厚度控制方面的有效性,并根据分析结果优化涂装工艺中的各个参数,从而达到精确控制涂层厚度的目的.     

A stochastic simulation for the collection process of fly ashes in single-stage electrostatic precipitators

The dynamic evolution of particle size distribution (PSD) along the longitudinal length of electrostatic precipitator (ESP) quantitatively describes the collection process of ESP, and then is capable of estimating the performance of ESP. The details of the evolution of PSD are obtained by the solutions of population balance equation (PBE) for electrostatic collection. The paper promoted a stochastic method to solve the PBE. The method is based on event-driven technique and introduces the concept of weighted fictitious particles. The halving procedure of number weight of fictitious particle is adopted to restore the statistical samples of the stochastic approach and maintain the computational domain. The method, which is named event-driven constant volume (EDCV) method, is used to simulate the collection process of particles in a small-scale single-stage wire-plate ESP, considering simultaneously the electrostatic force, the convection force and the transverse particle diffusion in the model of collection kernel. The agreement among the results of the Monte Carlo method, the experimental data and the results of method of moments is good.     

Rutile TiO2 microwave dielectric ceramics prepared via cold sintering assisted two step sintering

In this work, a sintering route named cold sintering assisted two step sintering process (CSP-TS) is presented to prepare rutile TiO₂ ceramics with submicron grain sizes. Cold sintering process at 300 °C with tetrabutyl titanate and water as the liquid phase yields a ‘green body’ with a relatively high density of ～80 %, and finally dense (98.5–99.8 %) rutile TiO₂ ceramics with grain sizes of ～600 nm can be obtained in the second sintering process at 950?1000 °C. The microstructural analysis with SEM and TEM indicates that the CSP-TS samples sintered at 950 °C have an obvious phenomenon of recrystallization, accompanying by a decrease of amorphous phases and a formation of clear grain boundaries. Besides, the rutile TiO₂ ceramics prepared by CSP-TS possess excellent microwave dielectric properties with relative permittivity of 92.0–98.4 and Q × f values of 27,800?31,900 GHz. Therefore, it is feasible to utilize CSP-TS to prepare ceramics with small grain sizes at low sintering temperatures.     

Preparation and characterization of reticular SSC cathode films by electrostatic spray deposition

Sm_0.5Sr_0.5CoO_3−δ (SSC) cathode films were deposited on CGO (Gd_0.1Ce_0.9O_1.95) electrolyte substrates by electrostatic spray deposition to prepare SSC/CGO/SSC symmetrical cells. Deposition parameters were changed systematically to examine their effects on film microstructure and electrode performance. A set of deposition parameters including a 0.01 M precursor solution containing metal nitrates in a mixture solvent of de-ionized water (0.6 vol%), ethanol (1.5 vol%) and diethyl butyl carbitol (97.9 vol%), a flow rate of 6 ml/h for precursor solution, a deposition temperature of 350 °C and an imposed electric field of 10 kV/3 cm was identified for preparation of films with a highly porous reticular structure. The superior performance of a reticular SSC electrode was evidenced by its low interfacial resistances of 0.275 and 0.018 Ω cm² measured in 500 and 700 °C, respectively. These values were one-half to one order of magnitude smaller than that of the screen-printed or slurry-painted electrodes.     

Nano-to-macroporous TiO2 (anatase) by cold sintering process

Cold Sintering Process (CSP) was applied on commercial nanopowders to produce nanostructured TiO₂ anatase with nano-to-macro porosity. Nanoporous TiO₂ based materials were obtained by applying CSP at 150 °C and pressures up to 500 MPa on three TiO₂ nanopowders with different specific surface area (s.s.a. = 50, 90 and 370 m²/g), using water as transient aqueous environment. Although TiO₂ is insoluble in water, a density of 68% and s.s.a. = 117 m²/g were achieved from the powder with the highest specific surface area. A post annealing process at 500 °C increased the density up to 73% with a s.s.a. = 59 m²/g, and the crystallites dimensions passed from 110 Å in the powder to 130 Å in CSP material and 172 Å after post annealing. Finally, macroporosity was produced by using thermoplastic polymer beads as sacrificial templates within TiO₂ nanopowder during CSP, followed by a debonding at 500 °C.     

Particle formation of hydroxyapatite precursor containing two components in a spray pyrolysis process

The particle formation mechanism of hydroxyapatite precursor containing two components, Ca(OOCCH₃)₂ and (NH₄)₂HPO₄ with a ratio of Ca/P = 1.67, in a spray pyrolysis process has been studied by computational fluid dynamics (CFD) simulation on the transfer of heat and mass from droplets to the surrounding media. The focus included the evaporation of the solvent in the droplets, a second evaporation due to crust formation, the decomposition reaction of each component of the precursor, and a solid-state reaction that included the kinetic parameters of the precursor regarding its two components that formed the hydroxyapatite product. The rate of evaporation and the reacted fraction of the precursor both increased with temperature. The predicted average size of the hydroxyapatite particles agreed well with the experimental results. Therefore, the selected models were also suitable for predicting the average size of particles that contain two components in the precursor solution.     

大型喷雾粒径分布的图像法测量

雾化技术在能源、化工等领域应用广泛,研究雾化机理和优化雾化喷嘴性能的前提是对其雾化液滴尺寸及粒度分布进行准确有效的测量和表征。目前常用的雾化液滴粒度测量技术,如基于光散射或衍射原理的激光粒度仪和相位多普勒分析仪等,能够较准确地测量粒径分布比较窄、最大粒度在2000 μm以下的喷雾,但对含特大颗粒且粒径分布很宽的喷雾,往往难以得到可靠结果甚至不可能进行测量。本文提出了用图像法测量这类大流量喷雾,构建了图像法测量系统,编写了图像处理程序,经标定实验后,采用该系统对某喷嘴喷雾液滴粒径分布及规律进行了测量研究。研究结果表明图像法可用于大型喷雾液滴粒度及分布的测量。     

烟气脱硫喷淋塔的数值模拟

以计算流体力学为基础,在三维坐标系下采用标准k-ε双方程模型求解动量、能量和组分方程,结合浆滴蒸发模型及简化的浆滴脱硫反应模型,以Eu ler-Lagrange方法建立了喷淋塔内烟气脱硫的数值计算模型,模型计算结果与孔华的试验数据符合较好。模型计算结果表明,对于粒径小的喷淋液滴,其烟气脱硫反应和液滴蒸发主要发生在烟气进口附近,而随着液滴粒径的增大,液滴在塔内蒸发和脱硫反应的过程延长。同时,增加烟气温度、降低烟气中SO2的入口质量浓度以及增加液气比均有利于提高脱硫效率。文中模型相对于一维柱塞流模型,能够直观地显示出喷淋塔内的流场、温度场和组分质量浓度场的空间分布。     

Grain size effect on microwave dielectric properties of Na2WO4 ceramics prepared by cold sintering process

In this work, cold sintering was adopted to prepare Na₂WO₄ ceramics with different grain sizes ranging from 0.632 μm to 17.825 μm. Their microstructures, complex impedance, and microwave dielectric properties were studied in-depth. It was found that samples with relative densities higher than 92% can be successfully synthesized by cold sintering process at a low temperature of 240 °C. However, their electrical properties have strong dependence on the grain size. Specifically, the resistance of grain boundaries decreases dramatically with the increase of grain sizes, while the quality factor has a positive correlation with the grain sizes of Na₂WO₄ ceramics. Excellent microwave dielectric properties, including permittivity = 5.80, Q × f = 22,000 GHz, and TCF = −70 ppm/°C, are obtained for Na₂WO₄ ceramics with a grain size of 4.477 μm prepared by cold sintering process.