不同醇对溶剂热法制备氧化亚铜形貌的影响

以乙酸铜、三乙醇胺和醇为原料,采用溶剂热法制备出了不同形貌的微米氧化亚铜颗粒。通过SEM和XRD对所制备产物的形貌和物相进行分析表征,结果表明,在适当的反应温度下,不同醇类作还原剂均可生成球形氧化亚铜微晶,但随着醇羟基数量的增加,球形氧化亚铜微晶的反应生成温度逐渐降低。同时,对醇在形成氧化亚铜微晶的反应过程中所起的作用进行了初步探讨。     

乙二醇溶剂热法制备纳米TiO2

用乙二醇溶剂热法制备了锐钛矿相纳米TiO2,用X射线粉末衍射(XRO)、红外光谱仪(FTIR)、热重分析(TG-DTA)和透射电子显微镜(TEM)对制备的样品进行了表征,研究了乙二醇浓度、含水量、反应温度和反应时间对纳米TiO2晶型和晶粒尺寸的影响.结果表明:所得的纳米TiO2粒径分布窄,单分散性好.随着溶剂热反应温度的升高,纳米TiO2的晶粒尺寸逐渐变大,但随着溶剂热反应时间的延长,纳米TiO2的晶粒尺寸却几乎不变.     

层状硫化锌的溶剂热法制备

以乙酸锌Zn(CH3COO)2.2H2O为锌源、硫脲SC(NH2)2为硫源、水与乙二胺的混合溶液为反应溶剂、十二烷基磺酸钠C12H25SO3Na形成的胶束为模板,利用溶剂热法制备了具有层状微观形貌的ZnS粉体材料。利用XRD、SEM、EDS等测试手段进行表征,结果表明,所得ZnS粉体材料结晶良好,层状形貌明显;层状ZnS粉体材料在435nm附近有较宽的发射峰,且发光性能明显优于球状ZnS粉体材料。     

溶剂热法制备氧化锆纳米粉体及其发光性能

以乙醇为反应介质通过溶剂热法合成了氧化锆纳米粉体。采用X射线衍射（XRD）、透射电镜（TEM）及荧光光谱（PL）等测试技术对产物相组成、形貌结构及发光性能进行了表征。XRD结果表明,以KOH为沉淀剂制备的凝胶前躯体经140℃溶剂热反应3小时后所得的产物粉体由单一的四方相ZrO2组成,随着反应温度的升高单斜相ZrO2含量逐渐提高。TEM测试结果表明,不同温度合成的ZrO2纳米粉体形貌没有显著差异。产物粉体均为球形颗粒且可观察到较为明显的团聚现象。PL谱测试结果表明,140℃溶剂热合成的氧化锆粉体在250nm的紫外光激发下在402nm和625nm处分别有一个较强的宽发射峰和一个弱发射峰。     

溶剂热法制备YAG微粉及其机理分析

采用异丙醇溶剂为反应介质,通过溶剂热法低温合成了YAG粉体.利用XRD、TEM、IR对产物微观形态和晶体结构进行了表征.研究证明,在300℃下保温10h可以得到平均粒径为200nm的球形单分散YAG微粉,通过温度对反应进程的影响分析了YAG形成机理即溶解-结晶过程.     

特殊结构纳米γ-AlOOH的溶剂热法制备与机理

选用有机铝盐(异丙醇铝和醋酸铝)为原料,分别以氨水和尿素为沉淀剂,在200℃的乙醇溶剂热条件下,制备出白色前驱物粉末。通过SEM,XRD和BET等分析手段对产物进行了表征,考察原料与沉淀剂对产物的影响。结果表明:不同原料得到不同形貌的纳米γ-AlOOH,微观形貌分别为纳米级棒状和片状物;溶剂和沉淀剂种类会影响产物的比表面,采用尿素可使比表面积达到218.64m2/g。同时进一步从结晶机理方面分析了这一结果的成因。     

溶剂热法制备磷酸铁锂的组织结构与性能

以锂∶铁∶磷摩尔比为1∶1∶1为原料,采用溶剂热法合成了纯的、晶型规则的亚微米级LiFe-PO4;再加入酚醛树脂经高温处理合成了LiFePO4/C复合正极材料,其振实密度高,加工性能好。利用X射线衍射（XRD）、扫描电子显微镜（SEM）及恒电流充放电技术研究了溶剂热温度、时间对产物组织结构及性能的影响。结果表明溶剂热温度为190℃、溶剂热时间为24h合成样品表现出良好的电化学综合性能,振实密度为1.25g/cm3;室温下0.1C倍率充放电,放电比容量达到151.3mAh/g;在1C倍率下放电时,材料放电比容量仍能保持在120.1mAh/g左右。     

溶剂热法制备TiO_2-CuO复合颗粒及其光催化性能

采用溶剂热法制备TiO2-CuO复合颗粒,表征了复合颗粒的形貌、结构并研究其模拟太阳光下光催化还原CO2生成甲醇的性能,探讨了TiO2-CuO光催化还原CO2的机理。结果表明:TiO2-CuO复合颗粒为平均粒径约为4.5μm的空心球形颗粒,硫酸铜在复合颗粒的制备过程中具有模板剂和金属源的作用。CuO质量分数为8%的TiO2-CuO复合颗粒具有较高的光催化还原效率,在异丙醇作用下,甲醇产量达127.8μmol/g;CuO复合及异丙醇的添加能够促进电子和空穴的分离,提高光催化还原CO2效率。     

溶剂热还原法制备纳米Cu2O及其光催化性能

以Cu(CH3COO)2.2H2O为原料,乙二醇为溶剂和还原剂,通过溶剂热还原法制备纳米Cu2O。通过X射线衍射分析(XRD)对产物进行表征。结果表明,反应温度、反应时间和Cu(CH3COO)2初始浓度对产物Cu2O的结晶程度和晶粒大小有着重要的影响。以甲基橙溶液为模拟废水,研究纳米晶Cu2O在可见光照射下的光催化活性。实验表明,制备的Cu2O样品在可见光下具有高的光催化活性,可见光催化活性优于商业P25 TiO2光催化剂。     

溶剂热技术制备硫化镍纳米粉体

分别以硝酸镍和硫脲作镍源及硫源、以乙二醇作溶剂,采用溶剂热技术成功地制备了Ni3S2,α-NiS和NiS2粉体。研究结果显示原料的配比及反应温度能够影响产物的物相组成及形貌。     

Cupric oxide inclusions in cuprous oxide crystals grown by the floating zone method

Abstract

Phase-pure cuprous oxide (Cu₂O) crystals are difficult to grow since cupric oxide can form within the crystal as the crystal is cooled to ambient conditions. Vacancies are the solute which causes precipitation of macroscopic defects. Therefore, even when a mostly phase-pure single crystal is used as a feed rod, cupric oxide inclusions persist in the recrystallized solid. Control of the thermal profile during crystal growth, however, can improve phase-purity; a slow counter-rotation rate of the feed and seed rods results in fewer inclusions. Cupric oxide can be removed by annealing, which produces a factor of 540 ± 70 increase in phase-purity.     

乙二醇体系中纳米Cu2O的制备及其性能研究

以Cu(NO3)2为原料,乙二醇为溶剂和还原剂,制备了不同形貌的纳米Cu2O.通过X射线衍射,透射电子显微镜对产物进行了表征,并用热分析法考察了纳米Cu2O对高氯酸铵热分解的催化作用.结果表明,在乙二醇体系中少量水的加入对产物的形貌有着重要的影响.当加入少量水时,产物形貌由不规则状变为短棒状.不同形貌的纳米Cu2O均能强烈催化高氯酸铵的热分解,分散性较好的Cu2O使高氯酸铵的高温分解温度下降了约104℃,分解放热量由590J/g增至1450J/g.     

A simple single-step approach towards synthesis of nanofluids containing cuboctahedral cuprous oxide particles using glucose reduction

Enhancement of thermal properties of conventional heat transfer fluids has become one of the important technical challenges. Since nanofluids offer a promising help in this regard, development of simpler and hassle free routes for their synthesis is of utmost importance. Synthesis of nanofluids using a hassle free route with greener chemicals has been reported. The single-step chemical approach reported here overcomes the drawbacks of the two-step procedures in the synthesis of nanofluids. The resulting Newtonian nanofluids prepared contained cuboctahedral particles of cuprous oxide and exhibited a thermal conductivity of 2.852 W·m^-1·K^-1. Polyvinylpyrrolidone (PVP) used during the synthesis acted as a stabilizing agent rendering the nanofluid a stability of 9 weeks.     

Preparation and characterization of zeolite framework stabilized cuprous oxide nanoparticles

Zeolite framework stabilized copper(I) oxide nanoparticles (4.8 ± 2.6 nm) were prepared for the first time by using a four step procedure: the ion exchange of Cu²⁺ ions with the extra framework Na⁺ ions in Zeolite-Y, the reduction of the Cu²⁺ ions within the cavities of zeolite with sodium borohydride in aqueous solution, the dehydration of Zeolite-Y with the copper(0) nanoclusters, and the oxidation of intrazeolite copper(0) nanoclusters by O₂ at room temperature. Zeolite stabilized copper(I) oxide nanoparticles were thoroughly characterized by ICP-OES, XRD, HR-TEM, Raman, XPS, UV-vis spectroscopy and N₂ adsorption-desorption technique.     

Study on the effect of annealing on the electrical properties of n-type cuprous oxide

n-Type cuprous oxide was synthesized by controlling the bath pH of the electro-deposition. Thereafter, cuprous oxide films were annealed in nitrogen at different temperatures. The electrical properties of n-type cuprous oxide films before and after annealing were studied by the capacitance-voltage measurements. By analysis of the Mott-Schottky curves, it was found that the carrier concentration of cuprous oxide films varied with the deposition bath pH and the annealing temperature. Also, the flat-band potential shifted with the increasing annealing temperature.     

Characterisation of one-dimensional CdS nanorods synthesised by solvothermal method

One-dimensional (1D) cadmium sulfide nanorods were successfully synthesised using cadmium nitrate and sulfur powder as starting materials and polyvinyl alcohol (PVA, MW = 1 25,000) as a capping agent in ethylenediamine as a solvent by solvothermal method at 200°C for 24 and 72 h. X-ray diffraction patterns (XRD) indicated a single phase of hexagonal wurtzite CdS structure, of which the results are in accordance with those of selected area electron diffraction (SAED). The morphologies of CdS were observed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) which showed 1D nanorods. The length and diameter of CdS nanorods were increased when PVA was added and the reaction times were prolonged. High resolution transmission electron microscopy (HRTEM) showed that growth direction of wurtzite CdS nanorods is along [001] direction or c-axis. Raman spectra presented the 1LO and 2LO at 299.36 and 600.72 cm^?1, respectively. The 2LO/1LO intensity ratios were increased when the length of CdS nanorods became longer.     

Cu2O半导体薄膜在酸性条件下的电化学沉积

在酸性溶液中在透明导电玻璃(ITO)基体上电化学沉积Cu2O薄膜.通过实验研究了电沉积工艺条件对电沉积Cu2O薄膜的影响.X射线衍射(XRD)和扫描电镜(SEM)对薄膜的微观结构和表面形貌进行了分析.结果表明,水浴温度较高时,酸性镀液中Ac-HAc共轭缓冲体系的反应速率提高,可以有效抑制铜单质的生长;镀液中铜离子的浓度...     

Zn含量对溶剂热合成纳米铁氧体颗粒的影响

为研究铁氧体液相合成的生长机理及价态变化,以乙二醇为溶剂,乙酸钠作为碱源,采用溶剂热方法合成尖晶石型Mn1-xZn_xFe₂O₄(x=0、0.5、1)纳米颗粒,通过X射线衍射仪、透射电子显微镜、氮吸附比表面仪和光电子能谱仪对样品的物相、微观形貌、比表面积和离子价态进行分析。结果表明:3组样品均为尖晶石结构,未出现杂相,晶粒度从37.5 nm增大至43.2 nm;存在由Fe^{3+还原而来的Fe2+,Fe3+与Fe2+含量比约为4∶[KG-2mm]1,导致衍射峰均向右偏移。粉末形貌特征为近球形颗粒,其生长依靠纳米晶之间的定向附着(OA)和自整合。增加Zn2+}含量可促进颗粒的整个OA生长过程,粒径95 nm减小至82 nm, 比表面积由45.14 m²/g减小至27.84 m²/g。     

溶剂热合成纳米钛酸钡及其表征

为满足钛酸钡纳米陶瓷的需求,本文用TiCl4和Ba(OH)2作前驱体,乙醇和乙二醇甲醚作混合溶剂,溶剂热合成了钛酸钡纳米粉体,并使用TEM、XRD和Raman光谱对产物进行了表征.结果表明,在本文条件下可以得到粒径为10~80 nm纳米粉体,通过控制反应条件可以达到控制颗粒尺寸的目的,反应时间和反应温度对颗粒尺寸有显著的影响.