超声场对醇/水反应体系制备纳米CeO2粉体影响研究

在超声辐射条件下,以Ce(NO3)3.6H2O和六亚甲基四胺(HMT)为原料,使用醇/水反应体系制备了纳米CeO2粉体。采用透射电子显微镜(TEM)、平衡发射极晶体管(BET)对制备的纳米CeO2粉体进行了表征。研究了超声功率以及醇/水反应体系对纳米CeO2粉体粒径和团聚情况的影响,并探讨了其作用机理。结果表明,使用醇/水反应体系以及适当的超声辐射均有利于制备出粒径更小、分散性更好的纳米CeO2粉体,但过高的超声功率则易导致颗粒间的团聚;而且超声辐射能够显著加快反应速度。制备出的CeO2粉体的平均粒径小于10 nm,粒度分布窄,单分散性好。     

沉淀剂对超声雾化法制备CeO2纳米颗粒的影响

利用硝酸铈为原料,分别以碳酸氢铵和氢氧化钠为沉淀剂,采用超声雾化法制备了CeO2纳米颗粒.在室温将反应液体在超声雾化器中雾化成微滴,然后把微滴作为微反应器,使粒子在体积有限的微液滴内成核、晶化、长大.利用X射线衍射仪、Fourier红外变换仪、透射电镜对所制得样品的物相、结构和形貌进行了表征.结果表明:利用超声雾化法制备CeO2纳米粒子的颗粒均匀且分散性较好;以氢氧化钠为沉淀剂较以碳酸氢铵为沉淀剂制备的CeO2颗粒更均匀,粒径更小,约为3nm.     

水/油微乳液技术制备单分散纳米CeO2

在十六烷基三甲基溴化铵 正丁醇/环己烷/水溶液组成的水/油型微乳液体系中,运用微乳液制备纳米粒子的原理,利用改进的两相液液法,测定了水/油微乳液的区域,并制备了纳米CeO2粉体.对制备得到的CeO2粉末的形貌特征、物相结构、成分等用透射电子显微镜、X射线衍射分析、热重-差示扫描量热法和红外光谱测试进行了表征.结果表明:在测定的微乳液区内能制备出颗粒分散性好,粒度分布均匀的纳米CeO2粒子,所得颗粒尺寸为3 nm左右.     

超声脉冲电沉积镍–氧化锆–氧化铈纳米复合镀层

在超声场中采用脉冲沉积法制备了Ni–ZrO2–CeO2二元纳米复合镀层。镀液组成和基础工艺条件为:氨基磺酸镍300 g/L,H3BO3 30 g/L,NH4Cl 5 g/L,润湿剂0.15 g/L,ZrO2 20 g/L,CeO235 g/L,温度(45±2)°C,pH 3.8±0.1,时间2 h。研究了平均电流密度、占空比和脉冲频率等对Ni–ZrO2–CeO2复合镀层中纳米颗粒含量的影响。采用静态浸泡法研究了不同脉冲参数下制备的纳米复合镀层在10%H2SO4溶液中的耐腐蚀性。结果表明,在平均电流密度4 A/dm2、占空比0.4、频率1 000 Hz条件下脉冲电沉积时,Ni–ZrO2–CeO2复合镀层中纳米颗粒的含量最高,表面最细致。超声波的引入使复合镀层中纳米颗粒的含量有少许降低,但能细化晶粒,提高复合镀层的耐腐蚀性能。Ni–ZrO2–CeO2复合镀层的耐腐蚀性优于相同工艺条件下制备的纯Ni、Ni–ZrO2以及Ni–CeO2镀层。     

超声场中沉淀法纳米氧化锌的制备与表征

将超声辐射应用于以硫酸锌(ZnSO4·7H2O)和草酸(H2C2O4·2H2O)为原料的沉淀法制备纳米氧化锌粉体的工艺过程,制备了平均晶粒尺寸为26nm的氧化锌粉体。通过XRD,DTA—TG和SEM等技术研究了纳米氧化锌的合成过程及粉体性能。结果表明:超声辐射引入普通沉淀法,超声波的空化作用可使前驱体颗粒细化,抑制其团聚并延缓其向凝胶转变,从而可制备出氧化锌纳米粉体。这种方法所得纳米氧化锌粒子外貌为球形,粒度分布均匀,分散性好。     

喷雾干燥法制备ZrO_2(3Y)微球

以ZrOCl2.8H2O,Y2O3为原料,NH3.H2O为沉淀剂,聚乙二醇为表面活性剂,采用共沉淀-喷雾干燥法制备出ZrO2(3Y)微球,并应用XRD和SEM等分析方法对所得粉体进行了表征,研究了雾化方式对粒径的影响。结果表明:粉体球化较明显,颗粒为球形,平均粒径在15μm左右,球体为纳米颗粒团聚而成,纳米颗粒粒径在20nm左右。     

沉淀法制备纳米氧化铝粉体的新工艺研究

以（NH4）2CO3为沉淀剂，并采用一种高分子分散剂，研制出沉淀法制备纳米氧化铝粉体的新工艺。制备出球形纳米氧化铝粉体，在800℃煅烧得到的颗粒尺寸为5－6nm，在1100℃煅烧得到的颗粒尺寸约为8nm。研究了沉淀pH、溶液浓度、煅烧温度和分散剂用量对纳米氧化铝粉体性能的影响。     

纳米二氧化锡的多种方法制备、表征及其对比

本文采用共沸蒸馏法、水热法、溶胶-凝胶法分别制备纳米SnO2粉体,所制得的SnO2粉体利用X-射线衍射(XRD)和扫描电子显微镜(SEM)表征。结果表明,3种方法制备得的粉体均为四方金红石结构,共沸蒸馏法所得粉体平均颗粒约为20nm。水热法所得粉体的平均颗粒约为10nm。溶胶-凝胶法所得粉体的平均颗粒约为70nm。研究不同制备方法合成纳米SnO2粉体在合成工艺,生产周期,产物颗粒大小等方面的优缺点。     

纳米CeO2粉体的制备及结构表征

采用水热法,以氯化亚铈(Ⅲ)、硝酸亚铈(Ⅲ)为铈源,合成了CeO2纳米立方体和CeO2中空球。采用X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)对合成的样品进行物相和结构分析。同时,实验还研究了水热反应条件对产物形貌和粒度分布的影响。结果表明,氯化亚铈(Ⅲ)直接水热反应,在不同的温度、时间条件下,均可得到立方CeO2粉体,粉体颗粒的粒径在10~50 nm,且随着时间的延长其晶粒变大,结晶完善。当采用硝酸亚铈(Ⅲ)为铈源时,可得到纳米CeO2中空球。其粒径在300~350 nm,球壁是由大量纳米CeO2颗粒片组装而成,其厚度为80~120 nm。并对纳米CeO2中空球的形成机理进行了初步的探讨。     

CeO2-Y2O3共稳定纳米四方多晶氧化锆粉体的制备与研究

用共沉淀法制备掺杂复合稳定剂CeO2-Y2O3纳米四方多晶氧化锆粉体,并讨论了pH,煅烧温度以及稳定剂的含量对所制备的粉体的组成情况和晶粒尺寸。用XRD、BET和热分析的结果表明pH≥9.5,煅烧温度为700℃左右可以获得细晶、稳定的TZP粉体。     

Effect of atomization methods on the size and morphology of Gd0.1Ce0.9O2−δ powder synthesized by aerosol flame synthesis

Nano-sized gadolinium doped ceria (GDC) powders were successfully synthesized by aerosol flame deposition (AFD) with two different atomization methods; ultrasonic and electrostatic atomization. The effect of the atomization method on the size and morphology of GDC particles were investigated. It was observed that the diameter range of the GDC small primary particles synthesized by the ultrasonic atomization method was 10–50 nm while with the electrostatic method was 5–25 nm. In addition, the size of primary large particle found to be decreased from 200 nm to 50 nm with increasing electric field up to 15 kV. The GDC powder synthesized by the electrostatic atomization exhibited reduced crystallite size, particle size, and similar electrical conductivity compared to GDC powder synthesized by ultrasonic atomization. This work demonstrated the benefits of the electrostatic atomization for producing smaller-sized GDC nanopowders for the application in intermediate temperature solid oxide fuel cells.     

Parameter optimization of ultrasonic vibration polishing K9 optical glass based on ultrasonic atomization

To further improve the surface finish and processing efficiency of optical components, ultrasonic vibration technology is frequently combined with conventional processing and the process parameters that play a critical role in this composite processing are identified. This research proposes an ultrasonic vibration polishing method based on ultrasonic atomization (UA-UVP). The polishing performance of K9 optical glass is increased by ultrasonic atomization (UA) assisted by polishing solvent for ultrasonic vibration polishing (UVP). Orthogonal experiments are used to study the effects and variation laws of the flow rate of ultrasonic atomization (Q), the gap distance between the polishing tool and workpiece (G), ultrasonic electro spindle speed (W), abrasive particle size (D) and ultrasonic amplitude (A) on surface roughness (SR) and material removal rate (MRR), respectively. When these two polishing characteristics are considered together, the optimization of polishing parameters becomes complicated. Therefore, the principal component analysis (PCA) and grey relational analysis (GRA) methods were employed to the optimal experimental combination as Q:18 ml/min, G: 5 μm, W: 4000 r/min, D: 0.5 μm, A: 8 μm. The experimental results showed that Ra and MRR were measured as 10.466 nm and 0.473*10^8 μm³/min, respectively. Compared with the best experimental combination of orthogonal experiments, the improvement rates of SR and MRR were 26.65% and 25.80%, respectively. Overall, the application of ultrasonic vibration technology contributes to enhancing the uniform distribution of polished abrasive particles and improving the polishing characteristics.     

超声均质微悬浮聚合制备亚微米级聚苯乙烯胶粒

以苯乙烯St为代表性单体,以聚乙烯醇PVA为分散剂,以十六烷HD为助稳定剂,以亚硝酸钠NaNO₂为水相阻聚剂,通过基于超声均质化的微悬浮聚合制得了一系列亚微米级聚苯乙烯胶粒。对亚微米级单体液滴的均质化产生及后续聚合过程中分散相尺寸的变化进行了考察。发现超声均质化和高分子分散剂的结合有利于制备粒径小、分布窄的稳定微悬浮液滴,而吸附于液滴表面的高分子分散剂、油相内的助稳定剂及水相中的阻聚剂的协同作用能使聚合过程较好地保持分散相原有的粒径大小及分布。因而通过改变超声均质强度,可较容易地在0.5～3.5 μm范围内自由调节胶粒的平均粒径。相对于常规的剪切均质微悬浮聚合,超声均质微悬浮聚合可更好地填补（细）乳液聚合与悬浮聚合在粒径分布范围上的间隙,有望高效、高容量地微胶囊化包裹亚微米级目标内容物。     

Experimental investigation of ultrasonic-vibration polishing of K9 optical glass based on ultrasonic atomization

K9 optical glass has an important position in the field of optical material because of its excellent chemical stability and optical projection. The hard and brittle characteristics of K9 optical glass make conventional processing difficult and time-consuming. A non-conventional hybrid polishing system combining ultrasonic atomization (UA) spraying method and axial ultrasonic vibration was developed for processing K9 optical glass. This system utilizes the high-frequency vibration characteristics of ultrasonic vibration technology: On the one hand, the ultrasonic atomization spraying method is used to generate evenly distributed atomized droplets for polishing, on the other hand, the axial ultrasonic vibration of the polishing tool provides impact kinetic energy for the free abrasive particles. Mechanical polishing (MP), ultrasonic-assisted polishing (UVP), mechanical polishing under ultrasonic atomization spraying (UA-MP) and ultrasonic vibration polishing under ultrasonic atomization spraying (UA-UVP) were carried out on K9 optical glass. The material removal rate (MRR), material removal depth (MRD), surface quality and surface micromorphology of the polished workpieces were also analyzed and compared. The experimental results showed that the best surface was obtained at UA-UVP (A_Ⅰ = 9 μm) with MRR of 0.0994 mm³/min, material removal depth of 26.816 μm, the Ra and Sa values were 0.028 μm and 0.033 μm respectively. Meanwhile, no obvious pits and scratches were observed on the micromorphological surface. Ultrasonic atomization contributes to even material removal from the polished surface and axial ultrasonic vibration of the polishing tool has a significant effect in improving the polishing characteristics, which provides the experimental basis for applying ultrasonic vibration technology in polishing.     

Enhancement of fine particle filtration with efficient humidification

Filtration is one of the most effective methods to remove suspended fine particles from air. In filtration processes,pressure drop of compact dust cake causes problems in efficiency and economy, which has received increasing attention and still remains challenging. In this study, we developed a novel technique to intensify the filtration of fine particles with efficient humidification. Two strategies for humidification, including ultrasonic atomization and steam humidification(controlling of ambient humidity), were employed and proved to be both effective. The regeneration frequency of the filter could be reduced by 55% with ultrasonic atomization, while steam humidification could lead to a 78% reduction in regeneration frequency. The effect of operating conditions on pressure drop and the mass loading during filtration were investigated. The dust cake showed a loose and porous structure with an optimized droplet-to-particle ratio. With the ratio of 1.53 and 0.0282, the maximum mass loading was 552 g·m-2upon the ultrasonic atomization and 720 g·m-2upon the steam humidification. The results show that humidification could slow down the increase of pressure drop during filtration and improve the efficiency of process.     

Preparation and characterization of poly(lactic‐co‐glycolic acid) microparticles containing DNA molecules encoding a malaria vaccine candidate

BACKGROUND: A novel ultrasonic atomization approach for the formulation of biodegradable poly(lactic‐co‐glycolic acid) (PLGA) microparticles of a malaria DNA vaccine is presented. A 40 kHz ultrasonic atomization device was used to create the microparticles from a feedstock containing 5 volumes of 0.5% w/v PLGA in acetone and 1 volume of condensed DNA which was fed at a flow rate of 18 ml h^?1. The plasmid DNA vectors encoding a malaria protein were condensed with a cationic polymer before atomization. RESULTS: High levels of gene expression in vitro were observed in COS‐7 cells transfected with condensed DNA at a nitrogen to phosphate (N/P) ratio of 10. At this N/P ratio, the condensed DNA exhibited a monodispersed nanoparticle size (Z‐average diameter of 60.8 nm) and a highly positive zeta potential of 38.8 mV. The microparticle formulations of malaria DNA vaccine were quality assessed and it was shown that the microparticles displayed high encapsulation efficiencies between 82–96% and a narrow size distribution in the range of 0.8–1.9 µm. In vitro release profile revealed that approximately 82% of the DNA was released within 30 days via a predominantly diffusion controlled mass transfer system. CONCLUSIONS: This ultrasonic atomization technique showed excellent particle size reproducibility and displayed potential as an industrially viable approach for the formulation of controlled release particles. Copyright © 2009 Society of Chemical Industry     

盐酸酸洗废液制备α-纳米Fe2O3的工艺优化

以氧化铁皮作为除酸剂,与盐酸酸洗废液反应制得FeCl₂溶液,再采用空气-双氧水双重氧化和沉淀法从中制得α-Fe₂O₃纳米颗粒。分析了FeCl₂质量浓度、氨水质量浓度、超声时间和煅烧温度对产物的的粒径和纯度的影响。采用场发射扫描电子显微镜(SEM)和X射线衍射仪(XRD)对产物的形貌和结构进行了表征。优化实验结果表明,FeCl₂质量浓度为16 g/L,氨水质量浓度为7.5 g/L,超声时间为50 min,煅烧温度为750℃时,制得了分散性虽然一般,但纯度较高的α-Fe₂O₃,其含量高达95.3%,平均晶粒尺寸约为38.2 nm。这为盐酸酸洗废液的资源化利用提供了实验基础。     

制备方法对Al/Fe_2O_3纳米铝热剂性能的影响

分别采用超声共混法、机械球磨法和溶胶-凝胶法制备出Al/Fe2O3纳米铝热剂。研究了3种制备方法对纳米铝热剂晶型、平均粒径、形貌、比表面积和热反应性能的影响。结果表明,超声共混法只能使两组分简单地混合在一起;机械球磨法通过机械作用力使两组分混合均匀,但部分Al颗粒破裂,平均粒径减小;溶胶-凝胶法制备的Fe2O3凝胶均匀包裹着Al颗粒,形成核壳结构的Al/Fe2O3纳米铝热剂,有效地保护了Al颗粒,同时纳米铝热剂具有高的比表面积,固—固反应放热量为896J/g。     

Effect of extensional properties of polymer solutions on the droplet formation via ultrasonic atomization

Ultrasonic atomization was conducted using 2.4 MHz ultrasound generator to produce polymeric particles from the solutions of water‐soluble polymers like poly (ethylene oxide) (PEO), poly(vinyl alcohol) (PVA), and poly(vinyl pyrrolidone) (PVP). In the series of solutions containing these polymers of various molecular weights, the shear viscosity and surface tension were varied; such differences, however, could not account for the observed trends in the atomization behavior. It was found that the availability of droplet formation and size of the droplets depend strongly on the extensional characteristics of polymer solutions along with the apparent extensional viscosities and the longest relaxation times. The extensional properties of polymer solutions were effectively measured by capillary breakup extensional rheometry (CaBER) and provided a rational basis to understand the essential role of fluid viscoelasticity in ultrasonic atomization. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers