微波辅助共沉淀法制备NiZnCu铁氧体纳米粉体研究

以硝酸铁、硝酸铜、硝酸镍和硝酸锌为原料,采用微波辅助共沉淀法制备了NiZnCu铁氧体纳米粉体,研究了微波的引入对纳米粉体制备的影响,通过XRD、TG-DTG、激光粒度分析和TEM表征了粉体的结晶性能,热性能,粒度以及粉体的形貌.研究表明,微波的引入可以明显加速晶化反应的进行,在较短时间内制得的纳米晶发育好于同温度下传统热处理方式制得的NiZnCu铁氧体纳米晶.研究表明,通过15min的微波辅助加热,可制得粒径在10nm左右的NiZnCu铁氧体纳米晶.     

纳米晶钛酸锶钡(Ba0.5Sr0.5TiO3)粉体的微波水热合成

采用微波水热法合成了纳米晶钛酸锶钡(Ba0.5Sr0.5TiO3)粉体,通过XRD、TEM、SEM等分析手段表征粉体,研究了微波水热合成反应温度、时间和前驱物浓度对反应产物形貌、粒度的影响,获得了制备纳米晶钛酸锶钡粉体的最优工艺参数.实验结果表明:在微波水热反应温度为195℃、反应时间20～30min、前驱物浓度为0.16mol/L时获得的粉体粒径小而且均匀,粉体平均粒度为60nm.     

纳米棒状羟基磷灰石的研究进展

综述了形状纳米羟基磷灰石和棒状纳米羟基磷灰石的常用制备方法、各自的优缺点、研究现状及存在的主要问题,即粒子的几何形状不是很均一,晶相稳定性不好;粉体有团聚;粒子纯度及表面的清洁度很差;粒子粒径及粒度分布范围太宽。针对性地提出了采用微波辅助法合成纳米棒状羟基磷灰石。     

超声振荡法制备纳米TiO_2粉体

以钛酸丁酯为原料,加入适当的模板剂,用超声振荡法制备纳米TiO2粉体,研究分散剂、干燥方式、模板剂等对TiO2粉体粒度分布及结晶性质的影响,借助于X射线衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)、激光粒度分布等测试手段对制备的TiO2粉体的晶体结构及颗粒粒度分布进行表征。结果表明:在80℃真空干燥、加入OP乳化剂和450℃煅烧条件下制备的纳米TiO2粒度较小,平均粒径为15～25nm,获得的纳米TiO2晶型为锐钛矿型,颗粒近似球形,结晶完好。     

化学沉淀法制备纳米氧化铝过程中的防团聚研究

分别以无水乙醇、去离子水为溶剂,以NH3·H2O、NH4HCO3为沉淀剂,采用化学沉淀法制备了纳米Al2O3粉体.利用TEM、XRD、FT-IR和激光粒度仪研究了溶剂、沉淀剂、浓度、前驱体等因素对纳米Al2O3粉体制备过程中的团聚程度的影响.结果表明:当NH4HCO3和Al(NO3)3水溶液浓度分别为3.0mol/L和0.3mol/L时,借助超声分散和微波干燥,得到的纳米Al2O3粉体粒度均匀、分散良好,1100℃煅烧所得粉体平均粒径为20nm.     

GaP纳米复合发光材料的制备和性质

用微波水热方法制备了GaP纳米晶／桑色素复合发充材料，研究了粒度对复合材料发光波长及发光效率的影响。结果表明：在微波水热条件下，GaP纳米晶的晶体结构不发生变化，只是在复合反应后粒度有所长大；与纯CaP纳米晶的发光光谱相比，复合后材料的发光峰变窄，发光强度显著增加，而且发光峰峰位向短波方向移动；另外，复合材料的发光波长和效率与GaP纳米晶的粒度有密切关系，粒度减小时相应的复合材料发光波段蓝移且发光效率提高。     

反相胶束法制备纳米ZrO2粉体

利用NA/煤油-n-C6-OH/NH3@H2O反胶束体系,制备了纳米ZrO2粉体.采用TG-DTA、TEM、XRD等手段对粉体及前驱体进行表征粉体粒度分布均匀,无硬团聚,平均粒度为20～40nm.并且研究了反相胶束中的溶水量对ZrO2粒径的影响以及pH值对ZrO2晶型的影响.并推测20～40nmZrO2的单斜晶(m)与四方晶(t)可能的相转变温度为723℃,比相应的体相材料降低了近450℃.     

化学沉淀法制备纳米氧化铝过程中的防团聚研究

分别以无水乙醇、去离子水为溶剂，以NH3·H2O、NH4HCO3为沉淀剂，采用化学沉淀法制备了纳米Al2O3粉体。利用TEM、XRD、nIR和激光粒度仪研究了溶剂、沉淀剂、浓度、前驱体等因素对纳米Al2O3粉体制备过程中的团聚程度的影响。结果表明：当NHaHCO3和Al（NO3）3水溶液浓度分别为3．0mol／L和0．3mol／L时，借助超声分散和微波干燥，得到的纳米Al2O3粉体粒度均匀、分散良好，1100℃煅烧所得粉体平均粒径为20nm。     

微波辅助-水相共沉淀法纳米ITO粉体的制备及其表征

利用微波辅助-水相共沉淀法,在InCl3和SnCl4混和溶液中添加PEG-6000,并滴加体积比1∶4浓度的氨水,并在不同反应温度(35～75℃)下制备了ITO前驱体,在温度800℃煅烧1h后得到纳米ITO粉体。利用SEM对纳米ITO粉体的形貌进行表征,用XRD对其结构、晶粒度和堆垛层数进行了表征,同时用纳米粒度Zeta电位分析仪对相应颗粒度进行了测试。讨论了微波辅助下不同反应体系温度对制备的纳米ITO粉体的形貌和尺寸的影响,并探讨了其机理,研究结果表明,随着反应体系温度的上升,纳米ITO粉体形貌由球形转为棒形,其晶体结构不变,晶粒粒径和颗粒度随着增大;反应体系温度的升高使纳米ITO晶粒不同晶面的晶粒度不同程度地增大,以及不同晶面垂直方向晶面不同程度地增多,是球形ITO晶粒成为棒形ITO晶粒的基础。     

均匀沉淀-水热法制备稳定Y-Ce-ZrO2纳米粉体

以尿素为沉淀剂,采用均匀沉淀-水热法成功地制备了2mol%Y2O3-5.5mol?O2稳定的纳米四方相ZrO2.研究了溶液的浓度、水浴时间、水热时间对ZrO2粉体的晶型和形貌的影响.结果表明在一定工艺条件下可制备平均粒径在10-20nm,粒度分布窄,分散性好的纳米稳定Y2O3-CeO2-ZrO2粉体.     

A new approach to joining of bulk copper using microwave energy

Metallurgical joining of high thermal conductivity materials like copper has been technically challenging. This paper illustrates a novel method for joining of bulk metallic materials through microwave heating. Joining of copper in bulk form has been carried out using microwave energy in a multimode applicator at 2.45 GHz and 900 W. Charcoal was used as susceptor material to facilitate microwave hybrid heating (MHH). Copper in coin and plate forms have been successfully joined through microwave heating within 900 s of exposure time. A sandwich layer of copper powder with approximately 0.5 mm thickness was introduced between the two candidate surfaces. Near complete melting of the powder particles in the sandwich layer does take place during the microwave exposure leading to metallurgical bonding of the bulk surfaces. Characterisation of the joints has been carried out through microstructure study, elemental analysis, phase analysis, microhardness survey, porosity measurement and tensile strength testing. X-ray diffraction (XRD) pattern indicates that some copper powder particles got transformed into copper oxides. XRD analysis also reveals that the dominant orientation (3 1 1) in starting copper powder got transformed into a preferential orientation (1 1 1) in the joint. A dense uniform microstructure with good metallurgical bonds between the sandwich layer and the interface was obtained. The hardness of the joint area was observed to be 78 ± 7 Hv, while the porosity in the joint was observed to be 1.92%. Strength character of the copper joints shows approximately 29.21% elongation with an average ultimate tensile strength of 164.4 MPa.     

Preparation and characterization of nano-NaX zeolite by microwave assisted hydrothermal method

In the present work, nano-NaX zeolite crystals were synthesized via microwave and conventional hydrothermal methods. The effects of reaction time, temperature and heating method on the characteristics of zeolite nanoparticles such as particle size, crystallinity, morphology, size distribution and surface area were investigated. The prepared NaX zeolite nanoparticles were characterized by the XRD, SEM, DLS, BET and XRF analysis. The results showed that both heating methods produced the NaX zeolite crystals with nano-in size. The microwave heating produced smaller zeolite nanoparticles with relatively narrower particle size distribution, required much shorter heating times and did not significantly change composition or crystallinity, compared with the conventional heating method. It was also observed that the time and temperature of microwave heating had significant effects on the prepared zeolite particles and the pure zeolite X nanoparticles or a mixture of zeolite X and A can be synthesized using the microwave heating method by control of the crystallization time and temperature.     

Application of Microwave Melting for the Recovery of Tin Powder

The present work explores the application of microwave heating for the melting of powdered tin. The morphology and particle size of powdered tin prepared by the centrifugal atomization method were characterized. The tin particles were uniform and spherical in shape, with 90% of the particles in the size range of 38–75 μm. The microwave absorption characteristic of the tin powder was assessed by an estimation of the dielectric properties. Microwave penetration was found to have good volumetric heating on powdered tin. Conduction losses were the main loss mechanisms for powdered tin by microwave heating at temperatures above 150 °C. A 20 kW commercial-scale microwave tin-melting unit was designed, developed, and utilized for production. This unit achieved a heating rate that was at least 10 times higher than those of conventional methods, as well as a far shorter melting duration. The results suggest that microwave heating accelerates the heating rate and shortens the melting time. Tin recovery rate was 97.79%, with a slag ratio of only 1.65% and other losses accounting for less than 0.56%. The unit energy consumption was only 0.17 (kW·h)·kg^–1—far lower than the energy required by conventional melting methods. Thus, the microwave melting process improved heating efficiency and reduced energy consumption.     

Microwave enhanced stabilization of heavy metal sludge

A microwave process can be utilized to stabilize the copper ions in heavy metal sludge. The effects of microwave processing on stabilization of heavy metal sludge were studied as a function of additive, power, process time, reaction atmosphere, cooling gas, organic substance, and temperature. Copper leach resistance increased with addition of aluminum metal powder, with increased microwave power, increased processing time, and using a gaseous environment of nitrogen for processing and air for cooling [N2/air]. The organic in the sludge affected stabilization, whether or not the organic smoldered. During heating in conventional ovens, exothermic oxidation of the organic resulted in sludge temperatures of about 500 degrees C for oven control temperatures of 200-500 degrees C. After microwave heating dried the sludge, the sludge temperature rose to 500 degrees C. The reaction between copper ions and metal aluminum in the dried sludge should be regarded as a solid phase reaction. Adding aluminum metal powder and reaction temperature were the key parameters in stabilizing copper in the heavy metal sludge, whether heated by microwave radiation or conventional oven. The mass balance indicates insignificant volatization of the copper during heating.     

Glycerol valorization by base-free oxidation with air using platinum–nickel nanoparticles supported on activated carbon as catalyst prepared by a simple microwave polyol method

Biodiesel is one of the most common biofuels, and its production yields a large amount of glycerol as a by-product. It is necessary to develop new technologies for the use of this by-product, adding value to the biodiesel production chain. In this work we investigated glycerol oxidation under mild reaction conditions (air as oxidizing agent and base-free medium) promoted by suitable catalysts. We prepared mono- and bimetallic catalysts of platinum, copper and nickel in the form of nanoparticles by conventional heating and by an alternative method using microwave heating. The nanoparticles were dispersed in activated carbon and tested in glycerol oxidation aiming its valorization into molecules with high added value. Copper and nickel monometallic materials were not active in glycerol oxidation. Platinum monometallic and platinum–copper and platinum–nickel bimetallic materials showed catalytic activity, with platinum–nickel prepared by microwave heating being the most active material in reactions tested. This catalyst presented glycerol conversion of approximately 20% with a turnover number of 9465 in a reaction time of 6 h and 58% of selectivity to glyceric acid, the main product obtained. The best performance of platinum–nickel prepared by microwave heating catalyst was attributed to the probable formation of a metallic alloy between Pt and Ni, as evidenced by the decrease in the lattice parameter for PtNi bimetallic nanoparticles. The results showed that it was possible to obtain an active catalyst in glycerol oxidation reaction under mild conditions via a simple methodology using microwave heating, which demands 94% less time in comparison with conventional heating.     

Fast synthesis of nanostructured ZnO particles from an ionic liquid precursor tetrabutylammonium hydroxide

Microwave irradiation could allow a more efficient and homogeneous heating of the reaction mixture to result in a fast synthesis. We propose a facile route for the synthesis of ZnO particles from an ionic liquid precursor with the assistance of microwave heating in which the ionic liquid has multifunctions (adsorbing microwave and acting as solvent, reactant, template) in the particle formation process. It demonstrates that ZnO particles with uniform size and morphology could be synthesized from tetrabutylammonium hydroxide ionic liquid precursor by the microwave heating method. Room temperature photoluminescence spectroscopy is measured to reveal the optical property of the as-obtained products. Moreover, the photocatalytic activity of the synthesized ZnO particles for the degradation of Rhodamine B is investigated.     

SAPO-34分子筛的微波合成实验研究

分别利用传统的水热法及微波合成两种方法制备SAPO-34分子筛，并通过XRD、SEM分析手段对产物进行了表征，结果表明，微波合成法得到的产物与水热法相比，结晶程度高、晶粒尺寸分布均匀，且略显粗大，与水热法的分散不同，后者晶粒易于团聚。从效率上比较，水热法一个合成周期长达60h以上，而微波合成仅需100min，前者耗能约为后者的72倍，说明，微波加热合成SAPO-34分子筛具有高效、节能的巨大优势。     

微波对物料微结构的影响

本文介绍了微波加热在陶瓷烧结、木材干燥、食品膨化、超细粉体干燥等过程中对物料微结构的影响。指出，微波加热具有抑制微结构垮塌、膨化食品微结构、抑制纳米粒子团聚等作用。认为微波加热可为纳米粉体干燥和纳米材料制备提供一种潜在处理方法。应当充分研究微细粒子传热传质特性和物料微细粒子介电行为，从而深入认识微波加热对物料微结构的影响。     

纳米相铁红粒子的液相制备

由０．２ｍｏｌ·Ｌ^－１Ｆｅ^３＋采用微波诱导加热制备了纳米尺寸的准立方形和纺锤形α－Ｆｅ_２Ｏ_３粒子,与常规加热方式比较微波加热制得的α－Ｆｅ_２Ｏ_３粒子粒径小且分布均匀,实验证明无机离子加 Ｈ^＋、ＯＨ^－和 Ｎａ^＋等的加入可明显加速反应速率．