Fe3O4@SiO2磁性复合微球的制备与表征

采用化学共沉淀法制备Fe_3O_4颗粒,在其制备过程中控制Fe_3O_4核的长大时间,加入油酸钠作为表面修饰剂来控制Fe_3O_4核的尺寸,然后加入正硅酸乙酯(TEOS)生成纳米级Fe_3O_4@SiO_2复合纳米粒子和亚微米级Fe_3O_4@SiO_2复合微球。通过X射线衍射、透射电镜、能谱分析和红外光谱分析证实Fe_3O_4颗粒表面包覆有SiO_2,并研究了复合粒子的形貌和成分组成,然后进行了磁性能分析。结果表明,Fe_3O_4纳米颗粒、Fe_3O_4@SiO_2复合纳米粒子和亚微米级Fe_3O_4@SiO_2复合微球的饱和磁化强度分别为79.95、34.85和61.51 A·m2/kg,对应的剩磁分别为1.73、1.05和3.07 A·m2/kg,矫顽力分别为1083、755和2002 A/m,亚微米级复合微球的剩磁和矫顽力都显著增大。     

水热法制备纳米Fe3O4磁性颗粒

通过水热法制备了Fe3O4纳米颗粒,采用TEM、XRD和VSM等测试手段对合成的样品的形貌粒径和结构进行了表征.研究了不同反应温度、反应时间、合成比例因素对样品形貌、尺寸和结晶性的影响,探索出形成高纯度Fe3O4的最佳条件.并借助VSM对合成的样品的磁性能进行了表征,可确定产物有较理想的磁性能.     

Fabrication and characteristics of spindle Fe2O3@Au core/shell particles

The fabrication and characteristics of spindle Fe2O3@Au core/shell particle were investigated, and the effect of the core/shell nanoparticles as the surface enhanced Raman spectroscopy (SERS)-active substrates was studied. By using the seed-catalyzed reduction technique, anisotropic Fe2O3@Au core/shell particles with spindle morphology were successfully prepared. The Fe2O3 particles with spindle morphology were initially prepared as original cores. The Au nanoparticles of 2 nm were attached onto the Fe2O3 particles through organosilane molecules. Uniform Au shell formed onto Fe2O3 core modified by Au nanoparticles through the in-situ reduction of HAuCl4. The shell thickness was controlled through regulating the concentration of HAuCl4 solution. The results of TEM, XRD and UV-vis characterization show that the core/shell particles with the original shape of the Fe2O3 particles are obtained and these surfaces are covered by Au shell completely. The surface enhanced Raman spectrum of the probe molecules adsorbed on these core/shell substrates is strong and the intensity is enhanced with the increase of the thickness of Au shell or the aspect ratio of particles. The spindle Fe2O3@Au core/shell particles exhibit optimum (SERS) activity.     

磁性纳米粒子Fe_3O_4@Au和Fe_3O_4@Ag的制备及表征

利用化学共沉淀法将铁盐和亚铁盐溶液按一定比例混合制备磁性纳米Fe3O4,再用3-巯基丙基三甲氧基硅烷修饰磁性粒子,连接金、银纳米粒子制备了核壳结构的功能性微粒。通过X-射线粉末衍射(XRD)、透射电子显微镜(TEM)及紫外-可见光吸收光谱仪(UV-Vis)对粒子的结构与性质进行表征。结果表明:磁性Fe3O4纳米粒子属立方晶型,Fe3O4@Au和Fe3O4@Ag粒子包裹完全,形状趋近于球形,兼有磁性和金、银纳米粒子的特性,对硝基化合物具有良好的催化性能。     

PVP对FePt纳米颗粒磁性能的影响

以乙酰丙酮铁(Fe(acac)3)和氯铂酸(H2PtCl6·6H2O)作为Fe源和Pt源,硼氢化钠(NaBH4)作为还原剂,PVP作为表面活性剂,通过化学还原法制备出单分散的FePt纳米颗粒,研究PVP对FePt纳米颗粒磁性能的影响。通过X射线衍射(XRD)仪,透射电子显微镜(TEM)和振动样品磁强计(VSM)对纳米颗粒进行表征。结果表明:PVP修饰的FePt纳米颗粒为面心立方(fcc)结构,形状近似球形且分散性良好,矫顽力为零,呈超顺磁性。当PVP与Fe(acac)3的比例为7:1时,经600℃热处理保温30min,FePt纳米颗粒从无序的fcc结构转变为有序的fct结构,矫顽力最大,可达5460A·m-1。     

磁性Fe3O4/Pt复合纳米粒子的超声制备与表征

超声条件下,在乙醇分散的3-氨丙基三乙氧基硅烷(APTES)功能化的磁性Fe3O4纳米粒子和氯铂酸的混合溶液中,滴加水合肼成功地制备了磁性Fe3O4/Pt复合纳米粒子。采用紫外吸收可见光谱(UV-Vis),电子能谱仪(EDS),透射电子显微镜(TEM),光电子能谱(XPS),超导量子干涉仪(SQUID)等方法对复合粒子的形态、结构、组成以及磁学性质进行了表征。结果表明:在此条件下制得的复合粒子粒度在50nm左右,室温下磁化强度可达17.2(A·m2)/kg。     

Microstructural evolution of NiFe2O4-10NiO powder prepared by high temperature solid state reaction

1 Introduction The development of inert anode materials for aluminium production has gained considerable attention in recent years[1,2]. The significance of such anodes is the ability to produce environment-friendly O2 gas during electrolysis instead of g…     

高密度煤油基磁性液体的制备及其性能表征

采用化学共沉淀法,通过改变Fe₃O₄纳米颗粒的生长温度、包覆环境pH、清洗、分散方式等工艺参数进行对比试验,得出Fe₃O₄纳米颗粒在生长阶段、包覆阶段、分散阶段的最佳参数条件,优化以往的制备工艺,使油酸包覆的磁性颗粒在煤油中的分散稳定性得到提高。通过XRD、TEM、VSM等对样品进行表征,并使用旋转流变仪对所制煤油基磁性液体的流变性能进行分析。结果表明,改性后的Fe₃O₄纳米颗粒平均粒径约为14nm,呈现较为规则的球形,饱和磁化强度为60 (A·m²)·kg^-1,可制备出质量分数可达60%的高密度煤油基磁性液体,与普通磁液相比,以此制备工艺得的高密度煤油基磁性液体在饱和磁化强度、抗氧化性等方面皆有较大提升,拥有更高的应用价值。     

Inductive heat property of Fe3O4 nanoparticles in AC magnetic field for local hyperthermia

Magnetite (Fe3O4) nanoparticles with different magnetic properties were prepared by coprecipitation of Fe3+ and Fe2+ with aqueous NaOH solution.The inductive heat properties of Fe3O4 nanoparticles in an alternating current (AC) magnetic field were investigated for local hyperthermia. The maximum saunder the optimum conditions of Fe3+:Fe2+ molar ratio at 1.8:1. The Ms of Fe3O4 nanoparticles decreased as the Fe3+ /Fe2+ molar ratio increased. But the coercivity Hc increases with the increasing of Fe3+ /Fe2+ molar ratio. Exposed in the AC magnetic field for 29 min, the temperatures of physiological saline suspension containing Fe3O4 nanoparticles were 42-97.5 ℃.The inductive heat property of Fe3O4 nanoparticles in AC magnetic field decreases as Hc increases, but increases with the increasing of Ms. The Fe3O4 nanoparticles would be useful as good thermoseeds for localized hyperthermia treatment of cancers.     

在有机添加剂存在的情况下共沉淀制备纳米Fe3O4及其性能

在有机添加剂甲基丙烯酸乙酯存在的情况下,采用共沉淀方法从Fe2 与Fe3 的水溶液中制备了Fe3O4纳米粒子.分别通过X射线衍射、透射电镜研究了其结构与形貌.结果表明:当溶液中甲基丙烯酸乙酯浓度为0.015 mol/L时,所制备的纳米粒子为单一的Fe3O4相;粒子呈球形,半径大约为15～30 nm.同时,采用振动样品磁强计对Fe3O4纳米粒子的磁性能进行了表征.结果显示,在不同温度下测得的M-H/T曲线与温度无关,表明该粒子具有典型的超顺磁性.     

固液反应合成铝基自生复合材料

利用Ａｌ－Ｍｇ合金液与Ｆｅ３Ｏ４粉末的反应,获得了细小Ａｌ－Ｆｅ相和Ａｌ２Ｏ３分布于铝基体上的复合材料;在离心铸造过程中,利用Ａｌ－Ｍｇ合金液与Ｆｅ２Ｏ３的反应,获得了外层含有初生Ａｌ－Ｆｅ相、内层不含初生Ａｌ－Ｆｅ相的复合材料。分析了复合材料的组织特征和物相组成。     

Synthesis of Fe3O4-coated silica aerogel nanocomposites

Fe3O4:SiO2 nanocomposite powders were synthesized by a two-step process,which included the precipitation of FeCl2 and FeCl3 and the gelation of silicic acid solution derived from water glass.At first,Fe3O4 nanoparticles having a crystallite size of 20 nm were obtained by controlling the ratio of Fe(II) and Fe(III) precursors.In the second step,Fe3O4 particles were embedded in SiO2 matrix by the hydrolysis and subsequent condensation of the silicic acid solution containing Fe3O4 particles.It was found that the Fe3O4 nanoparticles homogenously disperse in the SiO2 matrix.The Fe3O4:SiO2 nanocomposite exhibited an enhanced thermal stability against oxidation compared with pure Fe3O4.FT-IR analysis indicates the presence of the Si-O-Fe bond in the Fe3O4:SiO2 (1:10,mole fraction) nanocomposite.     

Structural macrokinetics of synthesizing ZnFe2O4 by mechanical ball milling

Powder mixtures of Fe2O3 and ZnO were milled in a high-energy planetary ball mill to synthesize ZnFe2O4 and X-ray powder diffractometry was used to obtain the relative content of phases,crystallite size and microstrain of both Fe2O3 and ZnFe2O4. The lattice constants of Fe2O3 were obtained by cell refinement method.The macrokinetics and the structure evolution of matters were studied and the results show that the dynamics process of mechanochemical synthesis of ZnFe2O4 fits Avrami-Erofe’ev model and is controlled by a nucleation-growth mechanism,and the structural macrokinetics theory in combustion synthesis research area could be used to describe the kinetic process as well.     

载银磁性Fe3O4纳米粒子的制备与催化及抗菌性能的研究

利用磁性纳米粒子Fe3O4表面的聚多巴胺 (PDA) 对银离子的吸附作用,采用种子诱导法制备了载银磁性纳米粒子 (PDA-Fe3O4@Ag)。采用UV-Vis (紫外-可见) 光谱对PDA-Fe3O4@Ag纳米粒子的制备过程进行了分析,采用FTIR (红外光谱)、XRD (X射线衍射仪)、TEM (透射电镜) 和VSM (振动样品磁强计) 等手段对所得的PDA-Fe3O4@Ag粒子进行表征;研究了PDA-Fe3O4@Ag对4-硝基苯酚还原反应的催化作用,还测试了其抗菌性能。结果表明,纳米金种子的存在是制备PDA-Fe3O4@Ag纳米粒子的关键;在外加磁场作用下该磁性催化剂可以容易地从反应体系中分离,经多次循环使用后仍具有良好的催化性能;此外PDA-Fe3O4@Ag纳米粒子具有杀菌性能,且经磁分离回收循环利用5次后仍呈现对金黄色葡萄球菌较好的杀菌效果。     

磁性Fe3O4/Ag复合纳米粒子制备与抗菌性能

采用箔-纤维-箔法和1150℃/150 MPa/30 min的真空热压工艺成功制备了SiCf/Ti-43Al-9V复合材料,并使用金相显微镜、X射线衍射仪、扫描电镜及能谱仪对该复合材料微观组织的形成进行了研究.结果表明,制备过程中SiC纤维与TiAl基体合金发生反应,并形成一定厚度的反应层;基体组织为等轴晶,粒径约为8 μm,与原始合金组织相比明显细化;从反应层到远处的TiAl基体合金,基体合金的组织由全γ相转变为α2/γ片层组织、γ晶粒和晶间B2相的混合组织.其中全γ相区域的厚度为2～4 μm,并围绕纤维分布.根据Ti-Al-V相图、C原子和V原子的扩散,分析了这两个基体区域的形成机理,并结合热压成形过程中的塑性变形和变形储存能,解释了基体合金晶粒大小的变化.     

原位一步法合成Ag/Fe2O3磁性核壳纳米粒子

采用原位法在低温下一步合成Ag/Fe2O3磁性核壳纳米粒子,并采用XRD,TEM和UV光谱研究了Ag-Fe2O3核壳纳米复合材料的结构。结果表明,纳米银粒子表面被Fe2O3层包覆,Ag核的平均粒径大约为35nm,Fe2O3壳层平均厚度约为7.5nm或15nm,形成了核壳结构的电磁复合纳米粒子。在室温下,饱和磁化强度达到0.98(A·m2)·kg-1,矫顽力8.48×103A/m;Ag/Fe2O3核壳粒子的导电率达到0.62S/cm。通过此法可以比较容易的控制核和壳的尺寸以及复合粒子的单分散性,并得到较高的产率,在催化剂、医药、光电等领域有着广阔的应用前景。     

高产率纳米铁粉的制备及表征

采用循环水冷却和循环等离子体工作气体的改进方法，制备出纳米铁粉。当电流为500A，气体总压为0．03MPa，电压为32V，氢气含量为50％，风机转速为2400r／min时，铁粉产率可高达6．2g／min，其平均粒径为50nm。粒子大多呈球形，表面光滑，粒子大小均匀，连接成链状。但是有些大颗粒粒径达到微米级，这主要是团聚所致。实验中制备的纳米铁颗粒为层状结构，由内到外依次是Fe-Fe3O4—Fe2O3，Fe3O4和Fe2O3的含量很低，但起到了对纳米粒子的保护作用。     

Gr/NiFe2O4纳米复合材料的制备与形成机理研究

以氧化石墨烯(GO)、Fe2(SO4)3和NiSO4为初始反应物,利用一步水热法合成了Gr/NiFe2O4纳米复合材料。采用X射线衍射(XRD)、透射电子显微镜(TEM)和拉曼光谱(RS)等分析手段对Gr/NiFe2O4样品进行了表征。结果表明:经过水热反应GO被还原的同时,纳米NiFe2O4成功地负载到石墨烯上,二者之间存在较强的界面相互作用,而且NiFe2O4纳米粒子增加了石墨烯片层间的距离避免了其再次堆垛,实现了石墨烯与NiFe2O4的良好复合。初步讨论了Gr/NiFe2O4纳米复合材料的形成机制,Ni2+、Fe3+在GO的含氧基团处非均相成核,在水热条件下不断长大,其生长过程遵循Ostwald熟化理论,即小尺寸的NiFe2O4粒子由于其较高的表面能而逐渐溶解,被那些尺寸较大的粒子消耗。     

Investigation on Preparation of Tb2Fe17 by Direct Electrochemical Reduction of Tb4O7-Fe2O3 Pellet in Molten Calcium Chloride

在CaCl2熔盐中直接电化学还原固态Tb4O7与Fe2O3(Tb∶Fe=2∶17)的混合 粉末, 一步制得了金属间化合物Tb2Fe17. 结合混合氧化物烧结片在850 ℃的CaCl2 熔盐中3.1 V电解不同时间段产物的成分分析探讨了还原机理：Fe2O3优先还原 成金属Fe, 随后Tb4O7粉末在Fe上还原逐渐生成Tb2Fe17. 采用不锈钢筛网电极 循环伏安法证明了Tb4O7在Fe上的欠电位还原.     

Oxidization mechanism in CaO-FeOx-SiO2 slag with high iron content

Oxidization mechanism in CaO-FeOx-SiO2 slag with high iron content was investigated by blowing oxygen into molten slag so as to oxidize Fe（ Ⅱ）. The relationship between Fe（ Ⅱ ） content and oxidizing time at different temperatures was obtained by chemical analysis. Microstructure of slag was observed by metallographic microscope and SEM. Phases compositions were ascertained by EDXS and XRD. Grain size and crystallizing quantity of magnetite（Fe3O4 ） were determined by image analyzer. The oxidizing kinetic equations were deduced. Confirmed by graphical construction method, Fe（ Ⅱ ） oxidizing reaction in CaO-FeOx-SiO2 slag system is of first order, and the reaction apparent energy Eo is 296. 67 kJ/mol in the pure oxygen and 340. 30 kJ/mol in air. The enrichment and crystal growth mechanism of magnetite（Fe3O4 ） phases were investigated. In oxidizing process, content of fayalite declines, while that of magnetite（Fe3O4 ） increases, and iron resources enrich into magnetite（Fe3O4 ） phase. All these provide a theoretical base for compressive utilizing of those slags.