化学共沉淀法制备Fe3O4纳米颗粒的结构和磁性能研究

铁氧体具有优良的磁性能,是一种应用广泛的功能材料.采用化学共沉淀法制备了纳米F33O4颗粒,选用氨水作为沉淀剂,将其加入到Fe2+和Fe3+的混合溶液中.探讨了温度、pH值以及Fe2+/Fe3+物质的量比对颗粒粒径、形貌和磁性能的影响.采用TEM、XRD、VSM和IR对颗粒的结构和性能进行了表征.结果表明,在没有惰性气体保护下为了避免高温氧化,通过增加Fe2+用量和沉淀剂用量,可在较低温度下生成颗粒大小均匀、磁性能好的Fe3O4颗粒,饱和磁化强度达到91.37emu/g.     

纳米Fe3O4/聚苯胺复合粒子的制备及其磁性能研究

用水解沉淀法制备纳米Fe3O4,然后在其溶液中原位合成聚苯胺,得到纳米Fe3O4/聚苯胺复合粒子.通过XRD、TEM、JDM等测试对纳米复合粒子的形态、结构及磁性能进行了研究.实验制备的纳米Fe3O4粒子粒径为30nm左右,在其表面沉积聚苯胺后,复合粒子的粒径达到了50nm左右.与纳米Fe3O4粒子相比,纳米Fe3O4/聚苯胺复合粒子的XRD峰形变得更为明锐.纳米复合粒子的磁性能表现出软磁性,与纳米Fe3O4粒子相比,矫顽力减小为0,这可以大大减小材料的磁滞损耗和退磁难度,性能得到改善.     

纳米Fe3O4/聚乙烯醇磁性水凝胶的制备及性能

利用化学方法制得了纳米Fe3 O4粒子,然后将其与聚乙烯醇(PVA)的胶态溶液共混,通过冻融法制备了纳米Fe3O4/PVA磁性水凝胶.采用综合热分析仪、拉伸试验机及ppms-9综合物性检测系统对磁性水凝胶进行了表征和测试.结果表明,纳米Fe3O4粒子的加入会降低磁性水凝胶的热稳定性;磁性水凝胶的力学性能和磁学性能随纳米Fe3O4含量及冻融次数的改变而显著变化.     

溶胶-凝胶法制备核壳SiO2/Fe3O4复合纳米粒子的研究

采用溶胶-凝胶法,以尺寸约10nm的Fe3O4纳米粒子为种子,碱催化正硅酸已酯(TEOS)水解、缩合,制备了磁性可控的核壳结构SiO2/Fe3O4复合纳米粒子.系统研究了醇水比、NH4OH及TEOS的浓度对复合纳米粒子形貌和性能的影响,并分析了SiO2/Fe3O4复合纳米粒子的生成机理.结果表明,SiO2的生长主要是SiO2初级粒子在Fe3O4表面的聚集生长,醇水比为4∶1、NH4OH浓度为0.3mol/L和TEOS浓度低于0.02mol/L时,随TEOS浓度的增大,SiO2壳层增厚,复合粒子饱和磁化强度下降,矫顽力基本不变,仍具有良好的超顺磁性.     

磁性SiO_2/Fe_3O_4复合粒子的制备研究

采用共沉淀法在硅酸钠溶液中将磁性Fe3O4纳米粒子进行包裹处理,得到表面包覆SiO2薄层的复合粒子,并通过XRD、TEM、穆斯堡尔谱、磁性能测试等手段对包裹样品进行了表征。实验结果表明,共沉淀法制备的复合粒子由磁性Fe3O4粒子核和外部的SiO2包裹层组成,复合粒子的粒径分布为介于20~30nm,包裹后的样品具有典型的铁磁性特征,比饱和磁化强度Ms为23.250emu/g。与单一的Fe3O4纳米颗粒相比,磁性SiO2/Fe3O4复合粒子除了具有良好的磁学性能、较小的矫顽力、较小的剩余磁化强度外,有着非常好的耐酸性和抗氧化性。     

Fe3O4/羧基改性壳聚糖复合纳米粒子的制备、表征及生物学应用

采用氧化水热法,以H2O2为氧化剂制备了磁性Fe3O4纳米颗粒.以磁性Fe3O4为核,通过反相悬浮聚合法对Fe3O4颗粒表面进行改性,在碳二亚胺的活化作用下,与壳聚糖衍生物-α-酮戊二酸缩壳聚糖(KCTS)反应制备了表面含有一定羧基的磁性Fe3O4/KCTS纳米粒子.经XRD、TEM、VSM、IR、TGA等手段对复合材料进行了表征及性能研究.结果表明,该磁性Fe3O4/KCTS纳米粒子的平均粒径为26nm,比饱和磁化强度为24.8A·m2/kg.其性能优良,具备超顺磁性,能很好的应用于生物分离,蛋白吸附等领域.     

药用壳聚糖磁性复合微球的制备及特性

采用化学共沉淀法,以FeCl2·4H2O和FeCl3·6H2O为原料,氨水为沉淀剂制备出磁性Fe3O4纳米粒子;然后采用化学交联法,在分散有纳米Fe,04的壳聚糖乳液中,加入适量的戊二醛交联剂制得包覆有纳米Fe3O4的壳聚糖复合微球载体.该复合磁性微球成球性好,分散均匀,平均粒径达到10βμm左右,具有较好的磁响应性及生物可降解特性.该复合磁性微球可作为载体材料应用于磁性靶向药物的制备.     

高稳定性导热油基磁性流体的制备

以氨水为沉淀剂、油酸为表面改性剂制备了高稳定性导热油基磁性流体.研究了所制备的Fe3O4粒子和磁性流体的各项性能.结果表明,制备的Fe3O4粒子晶型完整、粒径均一,具有很高的饱和磁化强度.通过表面改性油酸成功地包覆到Fe3O4粒子表面.所制备的导热油基磁性流体具有强磁性和高稳定性.     

共沉淀法制备纳米Fe3O4及其对橙黄Ⅱ的降解

通过共沉淀法制备Fe3O4纳米颗粒,采用X射线衍射(XRD)、扫描电子显微镜(SEM)和比表面孔隙分析(BET)对样品进行表征。以合成的纳米Fe3O4催化H2O2氧化降解橙黄Ⅱ,考察了共沉淀法制备过程中的Fe2+/Fe3+的摩尔比、反应温度、pH值、Fe离子浓度等因素对Fe3O4催化性能的影响。结果表明在Fe2+/Fe3+的摩尔比为3∶4、反应温度80℃、pH值为10、Fe离子浓度为0.1mol·L-1的条件下制备出的Fe3O4纳米颗粒催化活性最高,其粒径为20nm左右。并且未干燥的磁流体对橙黄Ⅱ的降解效率明显高于Fe3O4粉体。     

磁性羧甲基化壳聚糖纳米粒子的制备与表征

以化学共沉淀法制备了Fe3O4纳米粒子,壳聚糖经羧甲基化改性后接枝在Fe3O4颗粒表面,得到了磁性羧甲基化壳聚糖(Fe3O4/CMC)纳米粒子.利用透射电镜(TEM)、X射线衍射(XRD)、傅立叶红外光谱(FT-IR)及磁性测试对产物进行了表征.TEM表明Fe3O4纳米粒子被CMC包覆,粒径约10 nm;XRD分析表明复合纳米粒子中磁性物质为Fe3O4;FT-IR表明壳聚糖发生羧甲基反应以及在Fe3O4表面的接枝反应.Fe3O4/CMC纳米粒子具有超顺磁性,比饱和磁化强度25.73 emu/g,有良好的磁稳定性.     

The one-pot synthesis of dextran-based nanoparticles and their application in in-situ fabrication of dextran-magnetite nanocomposites

The dextran-based nanoparticles containing carboxyl groups were synthesized by a one-pot approach, without using any organic solvents and surfactants. The resultant dextran-based nanoparticles was used as a host for the growing and organization of Fe(3)O(4) nanoparticles. The approach consists of the mixture of ferrous/ferric ions aqueous solution and host nanoparticles and subsequent coprecipitation of ferrous/ferric ions in basic medium. The magnetic nanocomposite material obtained was characterized using transmission electron microscopy (TEM), dynamic light scattering (DLS), thermogravimetric analysis (TGA), X-ray diffraction techniques (XRD) and vibrating sample magnetometry (VSM). The data demonstrate that the carboxyls which can capture cationic ferrous/ferric by electronic interaction in the dextran-based hosts plays a crucial role in fabricating nanocomposites with a homogeneous spatial distribution of magnetite nanoparticles. The magnetic nanocomposites exhibit comparable saturation magnetizations to that of reported Fe(3)O(4) nanoparticles, and therefore display great potential in a large scope of biomedical fields.     

热水解法制备Fe2O3纳米粒子及其在Si表面的分散

用快速热水解的方法,制备直径小于10 nm的单分散Fe(OH)3胶体粒子。X射线衍射(XRD)和透射电镜(TEM)衍射分析表明:Fe(OH)3胶体粒子脱水后转变为Fe2O3纳米粒子。用离心分散的方法,胶体粒子在干燥过程中避免了团聚现象,实现其在Si表面的单层均匀分散覆盖。研究了胶体溶液浓度对胶体粒子尺寸及表面覆盖度的影响:改变胶体溶液的浓度,可以调节胶体粒子在Si表面的覆盖度,但对胶体粒子尺寸的影响不明显。     

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．     

富铁铁酸钴的室温合成和Mossbauer表征

采用氧化-沉淀法在室温下合成了不同钴含量的铁酸盐. 不同反应时间样品的IR和XRD谱图分析表明, 富铁铁酸钴是通过中间体绿锈形成的. 通过调节初始溶液中Co/Fe比(Co/Fe分别为: 1/20、1/15、1/10、1/7、1/5、1/3)合成了钴含量分别为Co/Fe=0.05、0.06、0.08?、0.12、0.17、0.18的富铁铁酸钴, 并通过XRD和化学测定分析了上述铁酸盐的化学计量和结构, 并结合Mossbauer谱进一步分 析了产物形成的过程. 实验结果表明: 在室温条件下, 随初始溶液中钴含量的增加, 钴在尖晶石结构中占据八面体空隙中Fe{3+的位置, 且钴含量的增加不利于尖晶石结构的形成, 游离 于绿锈结构以外的钴的化合物中包含了非磁性Fe(Ⅲ)的氧化物.     

Oxidation of dichlorvos with hydrogen peroxide using ferrous ion as catalyst.

This study examines how Fenton's reagent (Fe2+ and H2O2) decomposed dichlorvos insecticide. Results showed that dichlorvos decomposed in a two-stage reaction. The first stage is a Fe2+/H2O2 reaction in which dichlorvos swiftly decomposed. In the second stage, dichlorvos decomposed somewhat less rapidly, and it is a Fe3+/H2O2 reaction. The detection of ferrous ions also supports the theory of the two-stage reaction for the dichlorvos oxidation with Fenton's reagent. The dissolved oxygen of the solution decreased rapidly in the first stage reaction, but it slowly increased in the second stage with a zero-order kinetics. The Fenton system decomposed dichlorvos most rapidly when the initial pH in the solution is 3-4. In addition, increasing the concentration of hydrogen peroxide or ferrous ions can enhance the decomposition of dichlorvos. Consequently, the relationship of rate constant (kobs), [H2O2] and [Fe2+] at initial pH 3 is determined as kobs = 2.67 x 10(4)[H2O2]0.7[Fe2+]1.2.     

Hydrothermal synthesis of magnetite nanoparticles via sequential formation of iron hydroxide precipitates

A novel method for preparing fine magnetite nanoparticles without using any additives and organic solvents has been developed. In this method, a sequential precipitates formation method, ferrous and ferric hydroxides are not coprecipitated but sequentially formed in an alkaline solution, and then the resulting suspension is subjected to a hydrothermal treatment. The obtained magnetite nanoparticles were characterised through scanning electron microscopy observation and X-ray diffraction analysis, and the particle size and magnetic properties were measured with a dynamic light scattering particle size analyser and a superconducting quantum interference device magnetometer, respectively. In order to prepare fine magnetite nanoparticles with a uniform size, both the formation sequence of ferrous and ferric hydroxide precipitates and the supersaturation of ferric hydroxide in the solution were essential. The ferromagnetic magnetite nanoparticles with a median size 8.5?nm were relatively easily obtained in the formation process in which a ferric sulphate solution was rapidly poured into a suspension of ferrous hydroxide particles prepared beforehand using ferric chloride and sodium hydroxide, whereas the median size of magnetite nanoparticles prepared via conventional coprecipitation route was 38.6?nm.     

A novel nanostructured iron oxide-gold bioelectrode for hydrogen peroxide sensing

Fe(3)O(4) nanoparticles covalently linked to a gold electrode have been used for immobilizing catalase (CAT) enzyme to sense the presence of various concentrations of H(2)O(2). These nanoparticles ranging from 20 to 30 nm were synthesized by thermal co-precipitation of ferric and ferrous chlorides. SEM and XRD have been used for morphological and structural characterization of Fe(3)O(4) nanoparticles. CAT enzyme was linked covalently to the surface of iron oxide using carbodiimide in phosphate buffer (pH 7.4) at 4?°C. The enzyme-iron oxide link was confirmed by FT-IR spectroscopy. Sensing studies carried out using cyclic voltammetry showed a linear response of the CAT/nano Fe(3)O(4)/Au bioelectrode towards H(2)O(2) between 1.5 and 13.5 μM with a very sharp response time of 2 s.     

均匀沉淀法制备纳米Fe2O3的正交实验研究

为了研制生物质气化用纳米Fe2O3掺杂的铁基催化剂,以Fe(NO3)3·9H2O为原料、尿素为沉淀剂,采用均匀沉淀法制备了纳米Fe2O3.同时,利用正交实验探讨了不同工艺参数对合成纳米Fe2O3的影响,并得出了最佳工艺条件.产品分析表明,在反应物n(尿素):n(硝酸铁)=5:1、铁盐浓度为0.20mol/L、沉淀反应温度为115℃的最佳条件下制得的纳米Fe2O3粒子呈球形,分散性好,纯度较高,属立方晶系结构,平均粒径约为21nm.     

Synthesis and characterization of ultrafine poly(vinylalcohol phosphate) coated magnetite nanoparticles

Nanosized magnetite (Fe3O4) particles showing superparamagnetism at room temperature have been prepared by controlled coprecipitation of Fe2+ and Fe3+ in presence of highly hydrophilic poly(vinylalcohol phosphate)(PVAP). The impact of polymer concentration on particle size, size distribution, colloidal stability, and magnetic property has been extensively studied. The aqueous suspension of magnetite, prepared using 1% PVAP solution is stable for four weeks at pH 5-8. X-ray diffractograms show the formation of nanocrystalline inverse spinel phase magnetite. Transmission Electron Microscopy confirmed well dispersed cubic magnetite particles of size of about 5.8 nm. Dynamic Light Scattering measurement shows narrow distribution of hydrodynamic size of particle aggregates. Infrared spectra of samples show strong Fe--O--P bond on the oxide surface. UV-visible studies show aqueous dispersion of magnetite formed by using 1% PVAP solution is stable at least for four weeks without any detoriation of particle size. Magnetization measurements at room temperature show superparamagnetic nature of polymer coated magnetite nanoparticles.     

Preparation and characterization of Ni-nitrilotriacetic acid bearing poly(methacrylic acid) coated superparamagnetic magnetite nanoparticles

Stable superparamagnetic magnetite (Fe3O4) nanoparticles were synthesized via co-precipitation in the presence of poly(methacrylic acid) (PMAA) in aqueous solution. The polymer coated Fe3O4 nanoparticles were characterized using transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction, thermal analysis, and vibrating sample magnetometry (VSM) techniques. These measurements reveal the presence of magnetite nanoparticles with a size of approximately 8 nm inside the PMAA matrix. The magnetization value of these superparamagnetic nanoparticles at room temperarure and 7 T was measured as about 40 emu/g. PMAA-coated Fe3O4 nanoparticles were further assembled with Ni-chelate through a reaction between a primary amine-bearing NTA (nitrilotriacetic acid) ligand and carboxy-functional groups of PMAA. NTA-PMAA-coated magnetite nanoparticles were then loaded with nickel ions and characterized using FTIR. The average amount of binded Ni on the surface of the NTA-modified PMAA coated Fe3O4 was calculated as 1.65 +/- 0.3 x 10(-6) mol nickel(II) ions per g of the magnetic particles from the inductively coupled plasma optical emission spectroscopy (ICP-OES) measurements.