Co-Al spinel-based nanoparticles synthesized by flame spray pyrolysis for glycerol conversion

The catalytic properties of Co-Al spinel nanoparticles prepared by liquid-feed flame spray pyrolysis (L-F FSP) were investigated in the glycerol conversion in gas phase in an atmosphere of hydrogen. Reduction at 1123?K of the as-synthesized spinel nanoparticles induced the formation a new phase containing metallic cobalt species. Although, the reducibility of cobalt oxides is greatly decreased due to interaction with aluminium species, this strong interaction may prevent the aggregation of Co particles under the harsh reduction conditions. X-ray photoelectron spectroscopy (XPS) of the reduced spinel nanoparticles at 1123?K revealed that the Co/Al atomic ratio has decreased to Co/Al?=?0.11, which may indicate a redistribution of the aluminum and cobalt species at the surface of the sample submitted to the reduction in a flow of hydrogen at 1123?K. X-ray diffraction (XRD) and high resolution electron microscopy (HRTEM) also reinforced the formation of metallic cobalt species after reduction of cobalt from the spinel nanoparticles at 1123?K. The main products obtained from the conversion of glycerol in the gas phase were hydroxyacetone, pyruvaldehyde, lactic acid and lactide. FSP ensured uniform dispersion of the active metal on a support material.     

Characteristics of spray flames and the effect of group combustion on the morphology of flame-made nanoparticles

Characteristics of burning and non-burning sprays generated by a coaxial air-assist nozzle, previously used for the synthesis of ceramic nanoparticles by flame spray pyrolysis (FSP), are studied using phase Doppler anemometry. Also, the effect of droplet interaction on the overall combustion behavior of the spray (group combustion) and, consequently, on the characteristics of flame-made ceramic particles is investigated. A physical model is proposed which correlates the formation of inhomogeneous mixtures of micron-sized hollow particles and solid nanoparticles to the combustion mode: the precursor droplets which entirely evaporate in the hot flame are responsible for the formation of nanoparticles. The vapor species react, forming intermediate and product molecules and clusters that quickly grow to nanosized ceramic particles. On the other hand, under certain conditions, a small number of the droplets, particularly with large initial sizes, escape from the spray boundaries and become extinguished, producing large hollow ceramic particles. It is also possible that some of the large droplets, which lie within the spray core, do not entirely evaporate. These surviving droplets then form large particles which are usually hollow but can collapse to solid particles at sufficiently high temperatures. Also, a criterion for the formation of homogeneous ceramic nanoparticles is presented.     

双介质喷嘴雾化特性数值模拟研究

目的 双介质喷嘴雾化效果直接影响烟卷加料工艺的进一步提升，通过对雾化过程进行数值模拟，方便对雾化特性进行透彻的分析，提升雾化效果。方法 采用数值模拟方法构建两相流连续相流场与DPM离散态双向耦合的数值模型，研究蒸汽压力、液体流量以及双介质喷嘴结构对喷嘴雾化特性的影响。结果 适当增加蒸汽压力，可以在不影响最大流速、颗粒粒径均匀度及颗粒中值粒径的情况下，减小雾化扩散角，小幅度地增加喷射距离，雾化细度变好，进而提高雾化效果。随着有机液流量的增加，雾化扩散角增大，喷射距离增加，雾化粒径均匀度变好，从而使雾化效果变好。液体路通流面积越大喷雾的贯穿距离越小，气路通流面积越大喷雾的雾化扩散角度越大。若需要得到较好的雾化效果，需要保证较小的蒸汽路通流面积，与此同时液路侧保持正常开度。结论 适当地提高有机液流量或者蒸汽压力，以及采用较小蒸汽路通流面积，同时液路侧保持正常开度的结构，有利于提高料液喷洒的均匀性，减少了料液的浪费，提高了烟丝制备的工艺水平。     

热喷涂液相合成粉末的雾化喷嘴设计

为了形成尺寸基本一致且在空间呈均匀分布的雾滴,以利于制备均匀性好、粒径分布窄的纳米颗粒,通过对单相流和两相流雾化喷嘴的对比,以及液滴的雾化过程分析,根据相关实验结果和经验公式,设计出了用于热喷涂液相合成粉末的雾化喷嘴,其雾化气输送管径为0.2mm,液料输送管径为2.0mm,二者夹角为90°。此雾化喷嘴在等离子喷涂制备TiO2纳米颗粒的实验中得到了成功应用。     

High-rate production of functional nanostructured films and devices by coupling flame spray pyrolysis with supersonic expansion

The fabrication of functional thin films and devices by direct deposition of nanoparticles from the gas phase is a promising approach enabling, for instance, the integration of complex analytical and sensing capabilities on microfabricated platforms. Aerosol-based techniques ensure large-scale nanoparticle production and they are potentially suited for this goal. However, they are not adequate in terms of fine control over the lateral resolution of the coatings, mild processing conditions (avoiding high temperature and aggressive chemicals), low contamination and compatibility with microfabrication processes. Here we report the high-rate and efficient production of functional nanostructured films by nanoparticle assembling obtained by the combination of flame spray pyrolysis and supersonic expansion. Our approach merges the advantages of flame spray pyrolysis for bulk nanopowders such as process stability and wide material library availability with those of supersonic cluster beam deposition in terms of lateral resolution and of direct integration of nanomaterials on devices. We efficiently produced nanostructured films and devices (such as gas sensors) using metal oxide, pure noble metal and oxide-supported noble metal nanoparticles.     

The preparation of hard and super‐hydrophilic MgB2 coating by spray pyrolysis deposition

In this study, we report spray pyrolysis deposition using an alternative precursor solution for the fabrication of MgB₂ films. Polycrystalline MgB₂ films were prepared by spray pyrolysis, a precursor solution of magnesium diboride nanoparticles, sodium hypophosphite, sodium succinate, sodium acetate and dimethyl sulfoxide on AZ91 magnesium alloys. The spray was carried out using argon as carrier gas at a temperature of 150 °C and a spray rate of 5 ml/min for 60 min. After spraying, the deposited samples were annealed at 300 °C for 15, 30 and 45 min in order to investigate morphological changes and crystallization behaviour. The microstructure, hardness and wettability properties of approximately 30 μm coatings were investigated by X‐ray diffraction, scanning electron microscopy, microhardness tester and contact angle meter. Produced coatings showed dense and homogenous structural formation with strong grain connections. As‐deposited MgB₂ films showed the most pronounced preferred orientation with the (101) reflection and the highest hardness value compared to other annealed coatings at different times. Besides, all the synthesized coatings had a super‐hydrophilic surface.     

Spray characteristics and atomization behavior of bio-diesel (Norouzak) and diesel fuel blends

Norouzak oil seeds that are the source of bio-diesel (Norouzak) fuel grow mostly in Gonabad and Kashmar located in Khorasan, north east of Iran. Spray characteristics of Norouzak bio-diesel have been experimentally and theoretically studied in this work. Norouzak fuel is added to the conventional diesel fuel, and mixture formations of several blends have been investigated and compared with each other. Moreover, by varying ambient and injection conditions, behaviors of spray of different blends have been explored. Microscopic and macroscopic properties of spray such as Sauter Mean Diameter (SMD), Ohnesorge number, spray tip penetration, spray cone angle, spray projected area and volume have been examined. To promote mixture formation of the aforementioned sprays, atomization and air entrainment analysis have been performed as well. Furthermore, one can predict experimental results with accuracy of 12% applying suggested theoretical correlations and using error analysis, precision of calculated characteristics has been reported. Results show that increasing injection pressure or adding Norouzak fuel to the blend increases spray tip penetration and reduces spray cone angle. In additions, the results depict that one of the key parameters of improving atomization level of spray is increasing the differences between injection and ambient pressures.     

An experimental study on the spray characteristics of pressure nozzle in a fluid bed granulation

The particles with a narrow size distribution are proper products in a fluid bed granulation and coating. As well, the process efficiency is one of the most important parameters, and the wall deposition of sprayed liquid reduces it. The modality of spray volume distribution is a key parameter in the definition of particle size distribution and process efficiency. This work is done in two steps: In the first step, an experimental study on spray characteristics including spray flux distribution, spray cone angle, and discharge coefficient is conducted. Based on the experimental data, the curves of liquid volume flux versus nozzle pressure and height are obtained. The results indicate that the flux distribution changes significantly with even small pressure and height changes. In the second step, the granulation process is carried out in a semi-industrial conical fluid bed, and the particles size distribution curves and the deposited mass on the bed wall are obtained. The results show that the precise determination of the spray flux distribution is an appropriate way to predict the well-advised nozzle pressure/height in order to achieve the narrow particle size distribution and high efficiency of the process.     

Amorphous phase formation of Zr-based alloy coating by HVOF spraying process

This investigation was conducted to clarify the effects of process parameters on the formation of the new amorphous coating using a Zr-based alloy, which is known as bulk metallic glass forming alloy, by a HVOF (High Velocity Oxygen Fuel) spraying process. Powders used for spraying was prepared by vacuum gas atomization and then crushed by a centrifugal mill. HVOF spraying experiments were carried out using a Tafa JP-5000 spraying gun. DTA (Differential Thermal Analysis) measurements have shown that the amorphous content of the coatings was measured up to about 62% depending on the spraying process parameters. The amorphous fraction of the coatings is decreased with increasing the spray distance and the fuel flow rate. Microstructural observations and X-ray diffraction analysis of the spray coated layers reveal that the amorphization behavior during the spraying is attributed to the degree of the solidification of droplets and the oxide (ZrO₂) formation in spray coated layers. Therefore, flame temperature and spray distance that can control the carrier gas temperature and undercooling effects of the droplets are the most crucial factors for the evolution of the amorphous phase using this bulk metallic glass forming alloy.     

溶液雾化焙烧法制备氧化亚镍超细粉体

为研究雾化焙烧法制备氧化亚镍超细粉体过程原理与工艺控制,以六水合氯化镍配制水溶液,以压缩空气为载气,利用双通道内混合气流式喷嘴雾化前驱体溶液,获得微细雾滴直接在竖立管式高温电阻炉内焙烧,制备得到超细氧化亚镍粉体.采用热重-差热分析(TGA-DTA)对NiCl2·6H2O在空气气氛中的热行为进行研究,利用X射线衍射分析(...     

微胶囊红磷和聚苯醚对高抗冲聚苯乙烯的协同阻燃作用

利用微胶囊红磷(MRP)和聚苯醚(PPO)来提高高抗冲聚苯乙烯(HIPS)的阻燃性能, 通过熔融共混法制备了一系列不同组成的MRP-PPO/HIPS复合材料。采用水平燃烧、垂直燃烧、氧指数、锥形量热分析、高温热分解实验等方法研究了复合材料的阻燃性能。研究表明, 阻燃剂用量相同时, 在HIPS基体中同时加入MRP和PPO得到的复合材料比单独加入MRP或PPO得到的复合材料具有更好的阻燃性能。当MRP-PPO/HIPS的质量比为10:20:70时, 复合材料的氧指数为23.9%, 水平燃烧级别达到FH-1级, 垂直燃烧级别达到FV-0级, 阻燃性能达到最佳。MRP用量过多时, 复合材料的阻燃性能下降。研究认为, PPO和MRP对HIPS具有较强的协同阻燃作用。两者以适当比例并用时能够使复合材料在燃烧时的热释放速率和燃烧热大幅度减小, 降低了气相燃烧区的温度, 起到气相阻燃作用。同时, 复合材料在热分解和燃烧时能够生成连续和致密的炭层, 抑制了燃烧过程中的热量传递和物质交换, 起到凝聚相阻燃作用。因此, 复合材料的阻燃性能显著改善。     

A Systematic Approach to Design and Prepare Poly(meth)acrylate Based Solid Dispersions of Poorly Water-soluble Drug by Spray Drying

Objective of present study was to develop formulation which improves solubility of furosemide and stability of spray dried solid dispersion. Various processing parameters were optimized by applying DoE. In first step, screening of poly(meth)acrylates were carried out using solvent casting methods to select appropriate polymer. In second step, solid dispersion was prepared using optimized poly(meth)acrylate via spray drying process and trials were conducted as per DoE. Characterization of spray dried microparticles was carried out using SEM, DSC, XRD, in-vitro dissolution, and stability study. EUDRAGIT® E PO was screened as a suitable polymeric carrier in solvent casting method. In-vitro dissolution showed 100% releases within 20 min for spray dried powder as compared to 9% release for pure drug after 60 min in 0.1 N HCl. SEM analysis revealed conversion of crystalline shape to spherical shape. DSC and XRD confirmed that crystalline form was converted into amorphous form which was stable even after 3 months of storage. Outcome of DoE revealed that, feed rate has significant effect on %LOD while solid content has major effect on the process yield. So, present work indicates that EUDRAGIT® E PO formed a stable spray dried solid dispersion and it has ability to enhance dissolution of furosemide.     

新型无卤膨胀阻燃聚丙烯的制备及阻燃性能

利用有机杂环磷酸酯1, 2, 3-三(5, 5-二甲基-1, 3-二氧杂环己内磷酸酯基)苯(FR)、聚磷酸铵(APP)和三聚氰胺(MEL)制备新型无卤三源膨胀阻燃聚丙烯(IFR/PP)材料, 通过极限氧指数(LOI)、水平燃烧(UL-94)、热重分析法(TGA)、锥形量热(cone)等方法研究了IFR对聚丙烯阻燃性能影响。结果表明: 当IFR总添加质量分数为30%(FR∶APP∶MEL质量比为4∶8∶3), 阻燃IFR/PP的LOI 达到36.2%, 其热释放速率峰值(pk-HRR)、热释放速率平均值(av-HRR)、有效燃烧热平均值(av-EHC)、比消光面积平均值(av-SEA)、质量损失速率平均值(av-MLR)及一氧化碳释放率平均值(av-CO)相对未阻燃PP分别降低75.9%、71.7%、76.4%、74.6%、58.3%和50.0%, 300 s时CO释放量接近0, 呈现出良好的阻燃、抑烟和抑毒性能; SEM研究表明, IFR催化PP在燃烧初期形成了致密、坚硬的优质炭层。     

多层喷射共沉积制备 SiCP/Al-8.5Fe-1.3V-1.7Si复合材料

采用多层喷射沉积工艺制备SiC_P/Al-8.5Fe-1.3V-1.7Si复合材料, 研究了雾化及沉积工艺参数对沉积坯状态及SiC颗粒捕获的影响。结果表明, 液流直径大、雾化气体压力小、喷射高度小会导致沉积坯组织恶化, 反之则造成收得率低、致密度低。雾化器扫描不均匀则会造成沉积坯形状不均匀, 而且会由于热量集中导致显微组织恶化。SiC颗粒输送压力的提高有利于SiC颗粒的捕获以及颗粒的均匀分布。多层喷射沉积制备SiC_P/Al-8.5Fe-1.3V-1.7Si的优化工艺参数为: 液流直径3.6 mm, 雾化气体压力0.8 MPa, 喷射高度200 mm, SiC 颗粒输送压力0.5 MPa。 沉积坯存在两种SiC-Al界面: 晶态Si界面层与非晶态SiO₂界面层。     

Ultrasound-modulated twin-fluid atomization of a liquid jet

A resonant liquid capillary wave theory which extends Taylor's dispersion relation to include the sheltering effect of liquid surface inclination caused by air flow is presented. The resulting dispersion curves are compared to new experimental results of how drop-size and size distributions vary with surface tension and air velocity in both airblast and ultrasound-modulated twin-fluid atomization of liquids with a constant kinematic viscosity of 2 cSt. Good agreements between the theoretical predictions of relative growth rates of the capillary waves and the experimental results of drop-size and size distributions led to the conclusion that Taylor-mode breakup of capillary waves plays a very important role in twin-fluid (airblast) atomization of a liquid jet. Thus, the ultrasound-modulated twin-fluid atomization not only verifies the capillary wave mechanism but also provides a means for controlling the drop-size and size distributions in twin-fluid atomization, which has a variety of applications in fuel combustion, spray drying, and spray coating.     

Synthesis of solid NMC622 particles by spray drying,post-annealing and lithiation

Layered lithium-nickel-manganese-cobalt oxide (NMC) cathode materials are widely used in Li-ion batteries that require high energy densities, such as those used in plug-in hybrid electric vehicles (PHEVs) and electric vehicles (EVs). Here we studied the synthesis of NMC622 particles by spray pyrolysis, which is a simple one-step process for production of spherical particles. However, synthesising NMC powder using spray pyrolysis has a tendency to produce hollow NMC particles. To gain insight into the mechanism behind the formation of the hollow particles, one dimensional numerical simulation of the physical and chemical phenomena taking place during spray drying were carried out. The effects of several process parameters, including drying air temperature, drying air mass flow rate, and liquid feed mass flow rate, on the evaporation and particle formation process were studied. The increased evaporation rate at higher temperatures was found to result in crust formation on the droplet surface during the particle formation, and thus, in lower solid volume fractions in the dried particles. However, by optimizing the process parameters production of solid NMC622 sulphate particles by spray drying was achieved. The produced NMC622 sulphate particles were then oxidised and lithiated in air at 850 °C via the conventional thermal treatment process. Four lithium precursors, LiOH, Li₂CO₃, Li₂SO₄ and LiNO_3, were tested for the lithiation of the oxidized NMC particles. The degree of lithiation and the crystalline phase of the powders were determined using ICP-OES and XRD, respectively.     

Continuous Coaxial Electrohydrodynamic Atomization System for Water‐Stable Wrapping of Magnetic Nanoparticles

An electrohydrodynamic atomization (EHDA) system that generates an electrospray can achieve particle formation and encapsulation by accumulating an electric charge on liquid flowing out from the nozzle. A novel coaxial EHDA system for continuous fabrication of water‐stable magnetic nanoparticles (MNPs) is established, based on a cone‐jet mode of electrospraying. Systemic variables, such as flow rates from dual nozzles and inducing voltages, are controlled to enable the preparation of water‐soluble MNPs coated by polysorbate 80. The PEGylated MNPs exhibit water stability. The magnetic resonance imaging potential of these MNPs is confirmed by in vivo imaging using a gastric cancer xenograft mouse model. Thus, this advanced coaxial EHDA system demonstrates remarkable capabilities for the continuous encapsulation of MNPs to render them water‐stable while preserving their properties as imaging agents.     

基于二值化灰度图像的大豆蛋白液喷雾相对雾化程度的研究

目的 为了更直观的评估大豆蛋白液喷雾雾化程度,辅助筛选出有效扇形面积更大、缺陷更少的喷雾,有助于研究喷雾场的雾化均匀性,以期得到均匀一致的大豆蛋白膜。方法 选取合适的阈值后,对粒子图像速度场仪（Particle Image Velocimetry,PIV）拍摄的图像进行二值化处理,划定喷涂有效区域,利用二值化图像计算喷涂雾化场区域在喷涂有效区域内的点位数占比,将数值定义为相对雾化程度,改变稠度系数、喷涂参数,研究相对雾化程度的变化趋势。结果 低稠度系数的大豆蛋白液喷雾相对雾化程度受喷涂参数的影响较小,并保持在90%以上;中高稠度系数的大豆蛋白液喷雾相对雾化程度随着喷涂流量的增加而减小,随着液压、气压的增大有增大的趋势,随着气液比的增加先增大后减小。结论 基于二值化的PIV图像处理可以有效地辅助评估大豆蛋白液喷雾场的均匀性。     

蔬菜复合纸的大豆蛋白喷涂液雾化角度研究

目的研究蔬菜复合纸的大豆蛋白喷涂液雾化角的计算方法,及喷涂过程中工艺参数对大豆蛋白喷涂液雾化角度的影响。方法运用MATLAB软件,通过图像处理方法计算蔬菜复合纸的大豆蛋白喷涂液的雾化角度,并利用响应面分析法研究喷涂参数对大豆蛋白喷涂液雾化角的影响。结果单个因素中喷涂流量和气压对大豆蛋白喷涂液的雾化角有显著影响,喷涂流量、气压及液压三者的交互作用对喷雾角度有极显著影响(0.00080.05)。通过分析软件建立了雾化角与喷涂工艺参数之间的关系模型,并得到了最佳喷涂条件。结论当喷涂流量为48.04 mL/min,气压为199 Pa,液压为151 Pa时,大豆蛋白喷涂液的雾化角最大值为138.2637°。