超声波辅助固液反应球磨制备ZnFe2O4纳米晶的研究

以α-Fe2O3和ZnO粉体为原料,在超声波辅助高能球磨作用下通过诱发固液相反应,并在低温下烧结合成了ZnFe2O4纳米晶粉末.采用X射线、透射电镜(TEM)对前驱体和烧结产物进行了表征,分析了球磨过程对粉体晶粒尺寸的影响和znFe2O4的形成过程.实验结果表明:超声波辅助固液球磨能在低温下烧结合成ZnFe2O4纳米晶,纳米晶的晶粒尺寸为15～25 nm;相比无超声波辅助下的固液球磨,超声波球磨降低znFe2O4烧结温度约50℃;同一烧结温度下,球磨时间越长,ZnFe2O4转化率越高,晶粒尺寸越小.     

超声辅助乙酸溶液球磨法制备SnO2纳米粉末

采用超声波辅助乙酸溶液球磨法制备了金红石型的SnO2纳米粉末.采用X射线衍射仪(XRD)、傅氏转换红外线光谱分析仪(FT-IR)、透射电镜(TEM)对反应产物进行表征,研究了不同液体介质(乙酸溶液、纯水、乙醇溶液)、乙酸浓度、超声波频率对合成SnO2纳米颗粒的影响.结果表明,当反应进行到21 h,SnO2已经完全形成.合成的SnO2纳米粒子的平均粒径为10 nm左右,并且粒子形态统一、尺寸均匀.合成的SnO2纳米颗粒具有良好的光催化性能.锡粉在乙酸溶液中球磨21 h可以合成SnO2,而在水和乙醇溶液中球磨40h,仍不能合成SnO2;乙酸浓度越高,合成SnO2的反应速率越快;超声波频率越低,在超声辅助乙酸溶液体系中的反应速度越快.     

低温球磨制备5083超细铝合金及性能研究

本文采用低温球磨的方法制备了5083纳米晶铝合金,并用XRD、SEM和DSC等检测手段对样品粉末的微观结构、组织的变化过程和热稳定性进行了研究。结果表明:随着球磨的进行,球磨混合料中Mg相逐渐减少并逐渐固溶于Al中形成合金,粉末颗粒尺寸不断减小;球磨时间和球磨转速是影响合金结构和性能的主要因素,采用低温高速球磨能使合金纳米晶粒更加均匀,有利于Mg固溶于Al中;能谱分析和DSC分析表明,低温液氮球磨过程中形成的氧化物和氮氧化物颗粒对晶粒的钉扎一定程度的提高了5083铝合金的热稳定性。     

Al-Fe3O4体系在机械力化学过程中的物理化学变化

将纳米磁性粒子嵌入到绝缘基体中形成的磁性复合粒子,在许多方面具有重要意义.本文利用Al-Fe3O4通过机械力化学方法原位生成Fe/Al2O3 磁性复合粒子.通过对球磨不同时间的Al-Fe3O4粉末进行X射线衍射(XRD)和示差扫描量热(DSC)分析,结果表明Al-Fe3O4混合粉末通过机械力化学方法可获得Fe/Al2O3复合粒子.同时较为详细地研究了上述体系在机械力化学过程中的物理化学变化,并提出了机械力化学过程中Al-Fe3O4体系固相反应的方式.     

微波固相反应前驱体热分解法制备纳米氧化铜粉体

将固体CuSO4·5H2O和Na2CO3混合均匀后溶于适量乙醇中,然后进行微波辐照,立即反应生成泥浆状固体,将该泥浆状固体洗涤后干燥即可得到粉状前驱体.然后在600 ℃加热1 h分解该前驱体,即可制得纳米氧化铜粉体.在加热速率为10 ℃/min的条件下,对该前驱体进行表征,发现其热分解和晶体化温度约为550 ℃.对制得的纳米氧化铜粉体进行XRD、SEM、TEM和IR分析,结果表明制得的产物为纳米氧化铜粉体,其粉体粒径在30～50 nm,平均粒径约为40 nm.     

自分散、抗老化纳米氧化铜制备方法的研究

本文以硫酸铜和氢氧化钠为原料,分别用溶胶-凝胶法和自行开发的压力-热液法制备了氧化铜超细粉末,并采用SEM 、TEM、电子衍射、红外等测试手段对所制得的超细粉末的性能进行了表征,同时对两种方法纳米粒子形成的不同机理进行了初步探讨.结果表明,溶胶-凝胶法制得的氧化铜粉末呈类球形,团聚严重,易老化;而压力-热液法制得的氧化铜具有疏松的、薄片状的外观结构,粒子厚度约为20nm,分散性较好、抗老化能力强.     

固相合成YAG微晶粉体的XRD研究

以高纯Al_2O_3和Y_2O_3超微粉为原料,通过高能球磨和固相反应法制备了Y_3Al_5O_(12)(YAG)微晶;采用X射线衍射法(XRD)研究了球磨时间、煅烧温度、保温时间等对合成YAG微晶相组成的影响.结果表明:原料粉体的粒度随研磨时间延长而降低;随煅烧温度的提高,产物的物相由Y_4Al_2O_9和YAlO_5 逐渐向YAG相转变;延长保温时间有利于Y~(3+)和Al~(3+)的扩散以及Al_2O_3和Y_2O_3的固相反应.当Al_2O_3和Y_2O_3的摩尔比为5 ∶ 3,混合粉体经过15 h的机械球磨并于1300 ℃煅烧40 min即可得到单一物相的YAG微晶粉末.     

冷冻球磨法制备Al/MnO2复合粉体及其相关性质的研究

利用冷冻球磨法制备Al/MnO2复合粉体,利用XRD和SEM对球磨产物的物相组成及微观形貌进行分析表征,采用差示扫描量热计(DSC)对复合粉体进行热分析.研究表明,相对于室温球磨,冷冻球磨法可以有效抑制球磨过程中Al/MnO2体系的反应,获得具有亚微米级别粉体颗粒和纳米级别晶粒的复合粉体;制备的粉体因机械活化程度更高,反应活性更高,反应放热量也有明显增大.     

球磨固相反应法制备钨青铜K0.27WO3

以钨酸钾和三氧化钨为原料,采用机械球磨后高温固相反应的方法合成了钨青铜.X射线粉末衍射、X射线能谱分析表明,所制备样品为单相的K0.27WO3多晶.低温电阻率测量发现:多晶样品由于大量晶界影响而呈现出异于单晶样品的类半导体行为.     

用聚甲基丙烯酸制备MS(M=Zn,Cd)半导体纳米粉末的研究

本文介绍一种适合制备MS(M=Zn,Cd)半导体纳米粉末的化学合成方法.此方法成本低,易操作,且具有一定的广泛性.本合成通过调节聚合链长和反应循环次数可在1.8nm到5nm范围内对纳米粒径进行很好的控制.透射电镜和X射线粉末衍射对所制得的纳米粉末进行了表征.     

Synthesis and self‐assembled mechanism of CuO peony‐flowers by a composite hydroxide‐mediated approach at low temperature

A composite‐hydroxide mediated (CHM) method was utilized for the synthesis of CuO peony‐flower nanostructures under temperatures ranging between 25 and 160 °C. The CHM mechanism was confirmed through X‐ray Powder Diffraction (XRD) and a Thermo‐Gravimetric Differential Scanning Calorimeter (TG‐DSC). Cu(NO₃)₂ was shown to transform into Cu(OH)₂ in the mixed alkalis (NaOH/KOH); the reaction was facilitated by the solvent properties of the mixed alkalis. Cu(OH)₂ subsequently consumed H₂O in the adsorption of the mixed alkalis at 25∼65 °C. At higher reaction temperatures (>65 °C), the Cu(OH)₂ was seen to decompose at an accelerated rate. Therefore, crystalline CuO could be obtained not only above 65 °C but also at 25 °C. The crystal morphology and structure of CuO were examined through Filed Emission Scanning Electron Microscopy (FE‐SEM) and Transmission Electron Microscopy (TEM). It was determined that the CuO peony‐flower had a polycrystalline structure composed of single crystalline CuO petals. Using the Selected Area Electron Diffraction (SAED) results, the rings were indexed as (002), (111), (112), (202) and (−113), which was in agreement with the XRD results. With increasing temperature, the CuO flower petals self‐assembled through random aggregation and gathered CuO nanorod parts, which led to incomplete CuO flower petals through orientated aggregation. Prolonged reaction time led to the growth of CuO flower petals in the direction of [001]. An ideal CuO flower structure was observed through TEM observation.     

纺锤状CuO微结构的可控合成与表征

以NaOH、尿素为沉淀剂,Cu(NO3)2·3H2O为铜源,采用水热法控制合成了一种纺锤状CuO微结构.采用XRD、SEM、TEM和HRTEM等手段对产物进行了表征和分析,结果表明该CuO呈单斜晶相且具有很高的结晶性.研究了反应体系pH值、尿素浓度、反应温度、反应时间等因素对CuO形貌的影响,结果表明改变NaOH与尿素的相对浓度能显著调变CuO的形貌,使其呈现出空心微球、花状以及纺锤状等结构.提出了纺锤状CuO微结构可能的生长机理.     

Fabrication and photocatalytic property of CuO nanosheets via a facile solution route

Two‐dimensional (2D) CuO nanosheets were fabricated on Cu foils using a solution method. The method was novel, easy and can be completed at room temperature in the absence of any surfactant. The obtained materials were characterized by X‐ray diffraction (XRD), X‐ray Photoelectron Spectroscopy (XPS), scanning electron microscopy (SEM) and ultraviolet‐visible (UV‐Vis) spectroscopy. The effects of reaction time and temperature on the morphology and formation of CuO nanosheets were investigated, and a possible mechanism for the formation of CuO nanosheets was proposed. Experiments demonstrated that the formation of CuO nanosheets were significantly influenced by the growth time, and the reaction temperature was a key factor in determining the size of CuO nanosheets. Photocatalytic performance of CuO nanosheets was evaluated by measuring the decomposition rate of methyl orange solution. About 93% of the methyl orange was degraded after 150 min, which was much more efficient than that of CuO nanoparticles.     

Phase‐manipulable synthesis of Cu‐based nanomaterials using ionic liquid 1‐butyl‐3‐methyl‐imidazole tetrafluoroborate

Using the ionic liquid (IL), 1‐butyl‐3‐methyl‐imidazole tetrafluoroborate, and the precursor Cu₇Cl₄(OH)₁₀·H₂O, series of phase‐manipulable Cu‐based nanomaterials were synthesized by hydrothermal and microwave assisted routes, respectively. The structural characters of the as‐prepared CuO, CuO/Cu₂O composites and pure Cu nanoparticles were investigated by XRD, SEM, TEM and HRTEM, and their surface photovoltaic properties were studied by surface photovoltage spectra. Via hydrothermal route Cu²⁺ ions were found to be reduced gradually into Cu⁺ and subsequently Cu⁰ with increasing the IL, and various phase ratio of CuO, Cu₂O and Cu composite nanosheets and pure Cu nanoparticles were obtained. This implies that the IL could function as both a reductant in the oxygen‐starved condition and a template for the nanosheet products. The ¹H‐NMR result of the IL supports it being a reductant. In microwave assisted route, however, only monoclinic single crystalline CuO nanosheets were obtained, which indicates the IL being a template only in oxygen‐rich condition. Therefore, the crystal phase, composition and morphology of the Cu‐based products could be controlled by simply adjusting the quantity of the IL and oxygen in solution routes. The molecular structure of the IL after oxidation reactions was investigated by ¹H‐NMR and a possible reaction mechanism was proposed. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

纳米Al粉体性能及热稳定性研究

本文采用等离子体电弧法制备了纳米Al粉末,用XRD、TEM、TG、DTA、热处理等测试技术研究了纳米Al粉末的组成结构、晶粒大小、晶粒形貌和热稳定性情况.结果表明,该粉体平均粒径是39nm,晶粒形貌为球状,热稳定性好.     

溶胶-凝胶法制备La2CuO4纳米晶生长动力学研究

以硝酸镧和硝酸铜为起始原料,柠檬酸为络合剂,乙二醇为交联剂,采用溶胶-凝胶法制备了La2CuO4纳米晶.通过XRD和FESEM对La2CuO4粉体进行了测试和表征,研究了不同柠檬酸配比对La2CuO4相组成、显微结构以及晶体生长活化能的影响.结果表明:当柠檬酸与金属阳离子总和(La3++Cu2+)的物质的量比为1∶1,600℃煅烧保温2h后,可获得单一正交晶型的La2CuO4,颗粒形貌为球状结构,平均尺寸为65 nm;在制备过程中提高柠檬酸的加入量,能够降低La2CuO4晶体的生长活化能,当物质的量比由0.5∶1增加至1∶1时,生长活化能由67.3 kJ/mol降低到50.5 kJ/mol.     

Controllable one‐step synthesis of CuO,Cu2O and Cu

In the present report, CuO, Cu₂O and Cu have been successfully synthesized through a facile, one‐step hydrothermal method at a relative low temperature by controlling only the concentration of citric acid. Compared with other synthetic methods, the present method is mild, high‐efficient and nontoxic. The crystal structure and morphology of the as prepared samples were characterized by X‐ray diffraction and scanning electron microscopy, respectively. The mechanism for the crystal phase and morphological changes with different citric acid concentrations were discussed. The possible reaction process of the synthesis was also studied on the basis of the experimental results. We hope that this facile, one‐step hydrothermal method could be used in controlling synthesis of other metals and metal oxides under appropriate experimental conditions.     

Facile synthesis and characterization of hierarchical CuO nanoarchitectures by a simple solution route

The controlled synthesis of hierarchical CuO nanomaterials in a solution phase has been realized with high yield at low temperature using copper acetate hydrate and NaOH as starting materials with the assistance of surfactant under hydrothermal conditions. X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and ultraviolet‐visible spectroscopy (UV‐Vis) were used to characterize the products. It was shown that the hierarchical CuO nanoarchitectures were formed through aggregation of tiny single‐crystal CuO nanorods. Experiments demonstrated that the morphology of CuO products was significantly influenced by hydrothermal temperature and reaction time. A rational growth mechanism based on oriented attachment was proposed for the selective formation of the hierarchical CuO nanoarchitectures. Our work demonstrated the growth of hierarchical CuO nanoarchitectures built from one‐dimentional nanorods through a one‐step solution‐phase chemical route under controlled conditions. In addition, The UV‐Vis spectrum of the hierarchical CuO nanoarchitectures showed large blue shift because of the quantum size effect. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis of silica nanopowders in a microwave plasma

In the synthesis of silica nanopowders in a microwave plasma, the rate of feeding precursor materials has no dominant effect on the average size of SiO₂ particles, but varying the precursor material can affect significantly that size. Tetrachlorosilane and tetraethyl orthosilicate served as precursors in the preparation of silica nanopowders. Larger particles resulted when the precursor was altered to TEOS. The SiO₂ nanopowders were characterized with a transmission electron microscope and X-ray diffraction.