纳米Fe2O3和Fe3O4的制备及其催化高氯酸铵热分解性能的研究——一个仪器分析综合实验

介绍一个仪器分析综合实验——纳米Fe_2O_3和Fe_3O_4的制备及其催化高氯酸铵热分解性能的研究。采用水热法合成纳米Fe_3O_4,进而煅烧得到纳米Fe_2O_3。使用X射线粉末衍射(XRD)对制得的样品结构进行表征,通过透射电镜(TEM)可以发现其为球形颗粒,粒径在10–20 nm范围内。将制得的纳米Fe_2O_3和纳米Fe_3O_4按不同比例加入高氯酸铵(AP)中,通过对混合物进行热分析(TG-DSC),发现纳米Fe_2O_3和纳米Fe_3O_4可以明显促进AP的分解,且Fe_2O_3的催化效果优于Fe_3O_4的催化效果,并对催化机理进行了简单讨论。通过该实验,可以让学生学习水热反应的方法,掌握利用XRD、热分析等多种手段对化合物结构及性能进行表征的技能。     

Au与Fe_3O_4纳米微粒共嵌TiO_2纳米纤维的制备及可见光催化性能

通过静电纺丝法制备出含有Fe3O4纳米微粒的TiO2纳米纤维,再采用浸渍还原法将Au纳米微粒嵌入到TiO2纳米纤维上,制备出一种具有较强磁性和良好可见光响应能力的复合光催化材料.采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和紫外-可见固体漫反射光谱仪(UV-VisDRS)等对样品的结构和形貌进行表征,并以降解罗丹明B(RhB)为模型反应,考察了样品在可见光照射下的光催化性能.结果表明,嵌入Au纳米微粒可使复合纳米纤维在可见光下降解RhB时表现出非常好的降解速率和降解率;同时,将Fe3O4纳米微粒嵌入TiO2纳米纤维内部可以赋予材料较强的磁性,使材料便于分离和重复利用.     

SiO2表面包覆对Fe3O4磁性微球性能的影响

采用化学共沉淀法制备Fe3O4磁性纳米粒子;用柠檬酸钠进行表面修饰得到在水相中稳定分散的Fe3O4溶胶。以Fe3O4磁性纳米粒子为种子,用碱催化正硅酸四乙酯水解、缩合制备了粒径和磁性可控的核壳结构的Fe3O4@SiO2复合微球。通过FT-IR,XRD,TEM,VSM和古埃磁天平对Fe3O4@SiO2复合微球进行表征。研究了SiO2包覆对Fe3O4@SiO2复合微球性能的影响。     

基于碳复合Fe3O4纳米粒子的过氧化氢电化学传感器研究

本文以碳纳米粒子复合Fe₃O₄磁性纳米粒子构建新型过氧化氢电化学传感器,该传感器对过氧化氢有良好的电催化性能,过氧化氢浓度在1.00×10^-6 ~ 1.00×10^-3 mol·L^-1范围内与其氧化峰电流之间呈良好线性关系(R = 0.9980),检出限为6.60×10^-7 mol·L^-1. 该传感器具有良好的抗干扰能力、较高的重现性和稳定性.     

纳米Fe2O3/端羟基聚丁二烯(HTPB)复合粒子的制备与表征

为改善纳米Fe₂O₃在固体推进剂中的分散性, 以端羟基聚丁二烯(HTPB)和异氟尔酮二异氰酸酯(IPDI)为包覆和固化材料, 分别采用直接共混法和分步共混法制得纳米Fe₂O₃/HTPB复合粒子. 采用HRTEM, TGA, FTIR和XRD等手段表征了复合粒子的结构, 对比了复合前后纳米Fe₂O₃的分散性, 测量了HTPB包覆量和包覆层厚度. 结果表明, 这两种方法均能实现HTPB对纳米Fe₂O₃物理包覆, 但分步共混法明显优于直接共混法|在分步共混法制得的纳米Fe₂O₃/ HTPB复合粒子中, 内层的纳米Fe₂O₃分散性好, 外层HTPB厚度均一. 复合粒子亲油性结果表明, 将纳米Fe₂O₃与HTPB进行复合, 可有效改善纳米Fe₂O₃在固体推进剂中的分散性.     

Preparation for Magnetic Nanoparticles Fe3O4 and Fe3O4@SiO2 and Heterogeneous Fenton Catalytic Degradation of Methylene Blue

Dyestuff textile wastewater treatment has become a research hotspot due to its high chroma, poor biodegradability, and low toxicity characteristics. In this paper, we have synthesized magnetic Fe₃O₄ and core‐shell Fe₃O₄@SiO₂ materials by hydrothermal methods. These materials were characterized by XRD, TEM, N₂ adsorption‐desorption and so on. These materials’ heterogeneous Fenton has been applied to dye wastewater treatment. Methylene blue was used as a typical target of dye wastewater. Decolorization ratios of methylene blue were determined by different nanostructure composites catalysts. A serious of results of study showed that decolorization ratios of magnetic nanoparticles and core‐shell composites arrived at above 90 % under the weakly acidic or neutral conditions and room temperature. When these catalysts were reused, the results show that Fe₃O₄@SiO₂ materials were possessed with good cycle performance.     

羧基化核壳磁性纳米Fe3O4吸附剂的制备及对Cu2+吸附性能

在以共沉淀法制备的磁性纳米Fe3O4粒子(Magnetic nanoparticles, MNP)表面进行了化学修饰, 制备了一种新型富含羧基功能团的核壳磁性纳米吸附剂(Carboxylic functionalized Fe3O4 magnetic nanoparticles, CMNP). 利用透射电子显微镜(TEM)、 X射线衍射仪(XRD)、 X射线能量色散谱(EDS)、 振动样品磁强计(VSM)、 傅里叶变换红外光谱(FIIR)和热重分析仪(TGA)对CMNP的形貌、 结构、 化学组成和磁性能进行了表征, 并考察了吸附剂对Cu2+的吸附性能, 研究了溶液pH值、 吸附时间和Cu2+初始浓度对吸附性能的影响. 结果表明, 羧基化核壳磁性纳米Fe3O4颗粒的平均粒径为15 nm, 具有良好的超顺磁性, 饱和磁化强度为41.84 A·m2/kg, 在10 min中内可达到吸附平衡, 在pH=7.0时吸附量最高, 吸附等温数据符合Langmuir模型, 饱和吸附量qm= 43.48 mg/g.     

基于聚乙烯醇/Fe2O3纳米颗粒的纤维素酶固定化

以聚乙烯醇/Fe2O3磁性纳米颗粒为纤维素酶固定化载体, 通过反复冻融的方法成功地实现了纤维素酶固定化. 采用透射电镜、红外光谱仪、振动样品磁强度计对固定化酶复合体进行了表征, 结果显示, 固定化酶复合体为大小约1 μm的微凝胶团, 内含10 nm左右的Fe2O3纳米颗粒. 研究影响固定化因素后发现, 当pH为6, 固定化时间为11 h, 纤维素酶/PVA质量比为4, PVA/Fe质量比为50时, 固定化纤维素酶效果最好. 通过该方法固定后酶活回收率达42%, 酶水解效率显著提高, 经过5次反应后的固定化酶相对酶活力保留50%以上. 因此, 基于聚乙烯醇/Fe2O3纳米颗粒的纤维素酶固定有利于酶的循环使用并显著提高酶的使用效率, 是一种有效固定化纤维素酶的新方法.     

链霉亲和素-异硫氰酸荧光素偶联核壳型Fe3O4/Au纳米晶的合成及性质

采用改进的Polyol合成法,以PEO-PPO-PEO为表面活性剂制备了链霉亲和素-异硫氰酸荧光素偶联的Fe3O4/Au纳米粒子;利用透射电镜和X射线衍射仪分析证实了Fe3O4/Au的核壳型纳米结构,确定了其粒径和分布;采用紫外-可见吸收光谱仪和荧光光谱仪测定了所制备的纳米粒子的光学活性和荧光特性,并采用振动样品磁强计(VSM)测量了其磁化率.结果表明,所制备的Fe3O4/Au纳米粒子具有光学活性和荧光特性,以及优异的磁性.     

Comparison of Cadmium Cd2+ and Lead Pb2+ Binding by Fe2O3@SiO2‐EDTA Nanoparticles – Binding Stability and Kinetic Studies

This study describes the synthesis and characterization of ethylenediaminetetraacetic acid (EDTA) functionalized magnetic nanoparticles of 20 nm in size – Fe₃O₄@SiO₂‐EDTA – which were used as a novel magnetic adsorbent for Cd(II) and Pb(II) binding in aqueous medium. These nanoparticles were obtained in two‐stage synthesis: covering by tetraethyl orthosilicate and functionalization with EDTA derivatives. Nanoparticles were characterized using TEM, FT‐IR, and XPS methods. Metal ions were detected under optimized experimental conditions using Differential Pulse Anodic Stripping Voltammetry (DPASV) and Hanging Mercury Drop Electrode (HDME) techniques. We compared the ability of Fe₃O₄@SiO₂‐EDTA to bind cadmium and lead in concentration of 553.9 μg L^?1 and 647.5 μg L^?1, respectively. Obtained results show that the adsorption rate of cadmium binding was very high. The equilibrium for Fe₃O₄@SiO₂‐EDTA‐Cd(II) was reached within 19 min while for the Fe₃O₄@SiO₂‐EDTA‐Pb(II) was reached within 25 minutes. About 2 mg of nanoparticles was enough to bind 87.5 % Cd(II) and 54.1 % Pb(II) content. In the next step the binding capacity of Fe₃O₄@SiO₂‐EDTA nanoparticles was determined. Only 1.265 mg of Fe₃O₄@SiO₂‐EDTA was enough to bind 96.14 % cadmium ions while 5.080 mg of nanoparticles bound 40.83 % lead ions. This phenomenon proves that the studied nanoparticles bind Cd(II) much better than Pb(II). The cadmium ions binding capacity of Fe₃O₄@SiO₂‐EDTA nanoparticles decreased during storage in 0.5 M KCl solution. Two days of Fe₃O₄@SiO₂‐EDTA storage in KCl solution caused the 32 % increase in the amount of nanoparticles required to bind 60 % of cadmium while eight‐days storage caused further increase to 328 %. The performed experiment confirmed that the storage of nanoparticles in solution without any surfactants reduced their binding capacity. The best binding capacity was observed for the nanoparticles prepared directly before the electrochemical measurements.     

导电聚苯胺与Fe3O4磁性纳米颗粒复合物的合成与表征

对十二烷基苯磺酸(DBSA)掺杂的导电聚苯胺(PAn-DBSA)的氯仿溶液,在pH为中性的条件下,采用“修饰-再掺杂(Modification-re-doped)法”合成了含有Fe₃O₄磁性纳米颗粒的导电聚苯胺复合物的有机溶液.用FTIR,XRD,TEM,UV-Vis和SQUID等对所得复合物进行了表征,结果表明,该复合物呈现超顺磁性和半导体的导电性,并具有较好的透明性.     

基于Fe3O4@Ag壳核结构磁性纳米复合物的对杀螟硫磷的电化学传感

制备一种壳核结构的Fe3O4@Ag磁性纳米粒子,将该纳米粒子通过壳聚糖（CS）修饰在玻碳电极（GCE）表面,制备了对杀螟硫磷有灵敏电化学传感的Fe3O4@Ag/CS/GCE。应用透射电镜（TEM）和紫外可见光谱（UV-VIS）,对Fe3O4@Ag纳米粒子进行表征。运用电化学交流阻抗（EIS）、循环伏安法（CV）和时间电流法（I-T）来研究杀螟硫磷电化学特性。研究发现,在1.74×10-7～3.27×10–4 mol/L浓度范围内,该传感器可以实现对杀螟硫磷的快速检测,检测限为5.7×10-8 mol/L（S/N=3）     

聚乙烯吡咯烷酮包裹核壳型Fe3O4/Au纳米粒子的制备

采用改进的Polyol合成法,以聚乙烯吡咯烷酮（PVP）为表面活性剂制备PVP包裹的单分散的Fe3O4/Au纳米粒子.透射电镜（TEM）和X射线衍射（XRD）分析证实了Fe3O4/Au的核壳型纳米结构,并确定了纳米粒子的尺寸大小和分布.UV-Vis测定显示了所制备的纳米粒子具有光学活性,而振动样品磁强计（VSM）测量显示纳米粒子具有优异的磁化率.     

Preparation of Formyl Deoxycholic Acid Modified Fe3O4 Nanoparticles and Their Application for Oxytetracycline Loading北大核心CSCD

Formyldeoxycholic acid modified Fe3O4 nanoparticles（FDCA-MNPs）have been successfully constructed. The structure,morphology and magnetic properties of FDCA-MNPs are characterized by Fourier transform infrared spectroscopy（FT-IR）,transmission electron microscopy（TEM）and vibrating sample magnetometer. Oxytetracycline（OTC）is used as a model drug to evaluate the drug loading and release behaviors of FDCA-MNPs. The maximum loading of OTC is 59. 7 mg/g,and the loading behavior follows Freundlich adsorption balance equations with multilayer adsorption．Furthermore,FDCA-MNPs@OTC shows a higher release rate at pH=9 （11. 8%）than that of pH=7（8. 8%）. The bacteriostatic activities of FDCA-MNPs,OTC,FDCA-MNPs@OTC against E. coli are compared in vitro. The results show that FDCA-MNPs have no inhibition-activity for E. coli, meanwhile,FDCA-MNPs@OTC displays better sterilization ability than OTC at the same concentration. The minimum antibacterial concentration is 3 μg/mL,and the antibacterial rate reaches 97. 8%. It is proved that the synergistic effect of drug carrier and drugs reveals good antibacterial properties and reduce the dosage of antibiotics. © 2022, Science Press (China). All rights reserved.     

Fe2O3-TiO2磁性复合材料的制备及可见光催化性能

以FeCl₃和Ti(C₄H₉O)₄为前驱体, 通过复合溶胶法制备了Fe₂O₃-TiO₂磁性复合光催化剂, 并用 XPS, XRD, SEM, EDS及BET进行了表征. 对亚甲基蓝的降解实验证明, Fe₂O₃的引入将复合材料的光响应范围扩展至可见光区, 且掺杂的Fe₂O₃摩尔分数为1.0%时, 样品可见光催化性能最高. 磁强计的测试结果显示, 复合光催化剂具有一定的磁性, 可在反应结束后利用磁场从体系分离, 使催化剂得到回收再利用.     

纳米Al2O3颗粒对纯Fe液诱导凝固过程的分子动力学模拟

采用分子动力学(MD)方法模拟了不同半径大小的纳米Al2O3颗粒夹杂在三个温度下(1750、1730和1710K)对纯Fe液的诱导凝固过程,并分析了作为诱导核心的纳米Al2O3颗粒的结构演变及其对Fe原子体系的凝固过程的影响.发现在诱导过程中,纳米Al2O3颗粒的内部保持较好的晶型结构,仅表面原子有结构变形;诱导凝固的Fe原子主要为面心立方(fcc)和密排六方(hcp)原子;纳米Al2O3颗粒的尺寸越大,发生诱导凝固的温度越高;诱导凝固得到的Fe晶体的晶格取向受纳米Al2O3颗粒在Fe液中的漂移程度影响.     

Fabrication of Fe3O4 Nanoparticles Modified Electrode and Its Application for Voltammetric Sensing of Dopamine

Magnetic nanoparticles of Fe₃O₄ approximately 5nm in size were synthesized and characterized by XRD and TEM. A novel gold electrode modified with Fe₃O₄ nanoparticles was then constructed and was characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The modified electrode exhibited strong promoting effect and high stability toward the electrochemical oxidation of dopamine (DA), which gave reversible redox peaks with a formal potential of 0.192 V (vs. Ag/AgCl) electrode in pH 7.0 phosphate buffer solution (PB). The anodic peak currents (measured by constant potential amperometry) increased linearly with the concentration of dopamine in the range of 1.5×10^?7 to 4.0×10^?4 M. The detection limit (S/N=3) obtained was 3.0×10^?8 M. The relative standard deviation (RSD) of 8 successive scans was 3.41% for 1.5×10^?6 M DA. The interference of ascorbic acid (AA) could be eliminated efficiently. The proposed method showed excellent sensitivity and recovery.     

Fe2O3—TiO2—K2O复合氧化物体系结构与湿敏性能

Ｆｅ２Ｏ３┐ＴｉＯ２┐Ｋ２Ｏ复合氧化物体系结构与湿敏性能储向峰刘杏芹＊王弘（中国科学技术大学材料科学与工程系合肥２３００２６）关键词Ｆｅ２Ｏ３－ＴｉＯ２－Ｋ２Ｏ，复合氧化物，湿度传感器１９９７－０４－３０收稿，１９９７－０９－２９修回Ｆｅ２Ｏ３是一种...     

单分散Fe3O4纳米颗粒的控制合成和表征

以十八烯为溶剂、乙酰丙酮铁为铁源,并在油酸、油胺的辅助作用下,通过热分解法成功合成了单分散Fe3O4纳米颗粒。讨论了实验参数如反应温度、表面活性剂的量和种类、溶剂、油酸、油胺对单分散Fe3O4纳米颗粒的尺寸及形貌的影响。利用X射线衍射（XRD）、透射电子显微镜（TEM）、选区电子衍射（SAED）和高分辨透射电子显微镜（HRTEM）对所得产物的物相、结构、尺寸和形貌进行了表征分析。通过振动样品磁强计（VSM）表征产物磁性能,表明在室温下,Fe3O4纳米颗粒的饱和磁化强度（Ms）和矫顽力（Hc）分别为74.0 emu/g,72.6 Oe。     

Direct Electrochemistry of Hemoglobin Based on Fe3O4@SiO2 Nanoparticles Modified Electrode

A biosensor based on hemoglobin‐Fe₃O₄@SiO₂ nanoparticle bioconjunctions modified indium‐tin‐oxide (Hb/Fe₃O₄@SiO₂/ITO) electrode was fabricated to determine the concentration of H₂O₂. UV‐vis absorption spectra, fourier transform infrared (FT‐IR) spectroscopy, cyclic voltammetry (CV) and high‐resolution transmission electron microscopy (HRTEM) were used to characterize the bioconjunction of Fe₃O₄@SiO₂ with Hb. Experimental results demonstrate that the immobilized Hb on the Fe₃O₄@SiO₂ matrix retained its native structure well. In addition, Fe₃O₄@SiO₂ nanoparticles (NPs) are very effective in facilitating electron transfer of the immobilized enzyme, which can be attributed to the unique nanostructure and larger surface area of the Fe₃O₄@SiO₂ NPs. The biosensor displayed good performance for the detection of H₂O₂ with a wide linear range from 2.03×10^?6 to 4.05×10^?3 mol/L and a detection limit of 0.32 µmol/L. The resulting biosensor exhibited fast amperometric response, good stability, reproducibility, and selectivity to H₂O₂.