缩合法合成磁性荧光高分子CdTe@Fe_3O_4/P(NIPAM-co-AA)复合微球及其表征

具有超顺磁性和荧光特性的CdTe@Fe_3O_4/P(NIPAM-co-AA)多功能复合微球是以P(NIPAMco-AA)为模板制备而成.首先,采用溶胀法使模板微球带有磁性;其次,辅助TEOS和APTES两种化学试剂实现对Fe_3O_4/P(NIPAM-co-AA)微球表面的氨基功能化;最后,携带氨基的磁性微球与巯基乙酸修饰的CdTe量子点通过酰胺缩合反应,将量子点键合到磁性微球表面上,最终获得单分散的磁性荧光高分子复合微球.分别采用扫描电子显微镜、透射电子显微镜、倒置荧光显微成像系统、荧光分光光度计以及振动样品磁强计等方法对所获复合材料的结构与性能进行了表征.结果表明:复合微球单分散性良好,平均粒径约为30μm,饱和磁化强度可达5.4emu/g,具有良好的超顺磁性和较高的荧光发光效率.该材料将磁性、荧光结合到微米级高分子共聚物上,不仅解决了纳米粒子分离和处理的困难,而且奠定了多功能材料在生物标记、荧光成像等诸多领域潜在的应用基础.     

Fe3O4/CA@CQDs磁性荧光复合材料的制备及表征

为了制备出低毒且性能优异的磁性荧光复合材料,选用发光稳定且生物相容性高的碳量子点(CQDs)作为荧光探针,分别采用一步水热法和化学共沉淀法制备了荧光性能优异的CQDs和超顺磁性四氧化三铁(Fe_3O_4),再以生物相容性较好的柠檬酸(CA)修饰Fe_3O_4,得到表面富含功能性羟基和羧基的Fe_3O_4/CA,通过偶联剂乙二胺将CQDs与Fe_3O_4/CA连接,成功制得Fe_3O_4/CA@CQDs磁性荧光复合材料。并对其进行红外光谱(FTIR)、荧光光谱、振动样品磁强计(VSM)、X射线衍射仪(XRD)、荧光显微镜及透射电子显微镜(TEM)表征,结果表明:Fe_3O_4/CA@CQDs为核壳结构,粒径为30～40 nm,饱和磁化强度为20.14 A·m~2·kg~(-1),该双功能复合材料具有优良的荧光性能和磁性能,细胞毒性低且生物相容性高,有望取代传统荧光磁性纳米复合材料,并广泛应用于生物医学领域。     

Fe_3O_4@SiO_2@TiO_2复合纳米结构的尺寸与磁性调控

采用共沉淀法和溶剂热法制备了不同尺寸的Fe_3O_4纳米粒子,通过Stber法和溶胶-凝胶法在Fe_3O_4磁核上包覆SiO_2和Ti O2壳层获得不同尺寸的Fe_3O_4@SiO_2@Ti O2复合纳米结构.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)和振动样品磁强计(VSM)等对其结构、形貌和磁性进行了研究.结果表明,大尺寸复合纳米粒子包覆均匀,分散性好,饱和磁化强度较大,有利于TiO_2光催化剂的磁回收与再利用.     

空心Fe_3O_4纳米微球的制备及超顺磁性

采用水热控制合成法,以六水三氯化铁、柠檬酸三钠和尿素为原料,聚丙烯酰胺为稳定剂, 200?C下反应12 h制备得到了超顺磁性空心Fe_3O_4纳米微球.通过X射线衍射仪、扫描电子显微镜、透射电子显微镜对样品的结构和形貌进行表征,并采用振动样品磁强计测试了样品的磁性能.结果表明:所得样品为具有尖晶石结构的Fe_3O_4纳米微球,尺寸为160 nm左右,呈分等级结构,即整个微球由粒径约18 nm的初级晶粒自组装堆叠而成;室温下表现为典型的超顺磁性,且饱和磁化强度为73.3 emu/g (1 emu/g=1 A·m~2/kg),这种高饱和磁化强度可以由其初级晶粒晶化程度高且粒径较大以及这种特殊的二次自组装结构进行解释.这种Fe_3O_4纳米微球为疏松多孔的空心球状结构,具有粒径分布均匀、分散性良好和超顺磁性的特点,在药物靶向输运和肿瘤热疗中有潜在的应用.     

微乳液法SiO2/罗丹明B荧光杂化纳米微球的制备与表征

在甲苯存在下的反相微乳液体系中,将γ-缩水甘油醚氧丙基三甲氧基硅烷(KH560)与罗丹明B进行预反应;再与正硅酸乙酯( TEOS)经原位溶胶-凝胶反应,制备SiO2/罗丹明B荧光杂化纳米微球.通过FTIR、UV-Vis、TEM、TG和光致发光谱对杂化纳米微球进行了表征.结果表明:罗丹明B与KH560间通过酯基形成化学键...     

水溶性CdTe量子点荧光探针的制备表征及应用

采用水相合成法,在氮气气氛下,以3-巯基丙酸(MPA)为稳定剂制备了水溶性的CdTe量子点,并通过荧光(PL)光谱、紫外可见(UV-Vis)光谱、透射电子显微镜(TEM)和X射线粉末衍射(XRD)对样品进行了表征。XRD结果表明量子点为立方闪锌矿结构,TEM结果表明量子点分散性较好,形状为球形,平均粒径为2.0 nm。进一步考察了回流时间、反应温度和体系pH值对量子点性能的影响,结果表明:回流时间、反应温度和体系pH值对量子点的粒径大小、粒径分布及生长速度均有影响。基于量子点对金属离子具有荧光响应的特性,以CdTe量子点为荧光探针实现了对水溶液中Ni2+的检测。     

α-Fe2O3磁性微球的合成及磁性能

以氯化铁（FeCl3·6H2O）和氨水（NH3·H2O）为原料,以十六烷基三甲基溴化铵（CTAB）为表面活性剂,采用沉淀法制备了氧化铁磁性微球.所得样品用XRD、SEM及SQUID-VSM等手段进行了表征.结果表明,所得氧化铁磁性微球为斜方六面体结构,其粒径大小在0.5-1.5μm范围,其剩余磁感应强度为0.06emu/g,矫顽力为1700Oe,表现出一定的铁磁性.     

Ag@Fe3O4@C-CdTe@SiO2磁性荧光复合微球的制备与光学特征

先采用一步溶剂热法和水热法制备了碳包覆的Ag@Fe₃O₄核壳型磁性纳米粒子,然后通过表面氨基化改性后与巯基乙酸修饰的CdTe量子点反应,将量子点键合到磁性微球上,最后在其表面包覆上一层二氧化硅壳层,制备出具有荧光增强的Ag@Fe₃O₄@C-CdTe@SiO₂磁性荧光复合材料。实验结果表明,该纳米粒子的平均粒径大约为150 nm,磁饱和强度为224 A/g（22.4 emu/g）,在室温下具有较好的磁性能。其中Ag@Fe₃O₄@C-CdTe磁性荧光纳米粒子的荧光强度大于Fe₃O₄@C-CdTe,其主要原因是内核为45 nm的Ag纳米粒子具有表面等离子体共振作用,能够使其表面或附近的量子点荧光得到增强。     

壳核型磁性纳米纤维素微球的超声制备及表征

以纳米级的Fe3 O4液体作为磁核 ,在非水体系的纤维素DMAc(N N二甲基乙酰胺 ) /LiCl溶液中 ,使用包埋法 ,在超声波的辅助下制备得到了纳米尺度的壳核型磁性纤维素微球 .利用FT IR、XRD及AFM/MFM (原子力显微镜 /磁场力显微镜 )对得到的磁性微球进行了表征 ,证实该微球由磁性的核与纤维素的壳组成 ,微球大小为 30～ 5 0nm ,且具有良好的分散性 .并研究了超声条件对磁性微球尺寸的影响 .     

纳米棒状长余辉材料BaAl_2O_4:Eu~(2+),Dy~(3+)的制备与发光性能

利用硝酸铝、硝酸钡、尿素为原料,以一定比例H_2O/正丁醇及H_2O/正丁醇/SBS的混合液作传递压力的介质,进行反应,然后将得到的前驱体在还原气氛下高温煅烧,得到亮度高,余辉时间长的BaAl_2O_4:Eu~(2+),Dy~(3+)纳米棒状长余辉发光材料。TEM和SEM测试表明高温煅烧后得到的BaAl_2O_4:Eu~(2+),Dy~(3+)为棒状结构,其激发光谱和发射光谱均为宽带,主发射峰分别为498 nm,是典型的Eu~(2+)5d→4f跃迁。该方法的特点在于:采用水热法合成的BaAl_2O_4:Eu~(2+),Dy~(3+)长余辉发光材料一般需经过高温煅烧,容易结块,而在合成制得的产品经1 300℃高温煅烧后仍呈现分散性良好的棒状结构,不需球磨,且发光性能良好,可直接应用。同时将2种不同的实验条件进行比较,发现在不使用表面活性剂的条件下依然可得到分散性良好的棒状BaAl_2O_4:Eu~(2+),Dy~(3+)长余辉发光材料。该制备方法有望在其他铝酸盐和硅酸盐系长余辉发光材料的制备中得到应用。     

Synthesis and characteristics of multifunctional Fe3O4-SiO2-CdS magnetic-fluorescent nanocomposites

A luminescent superparamagnetic nanocomposite with an Fe 3 O 4-SiO 2-CdS structure is synthesized.Coated with a silica shell,Fe 3 O 4 nanoparticles and CdS quantum dots (QDs) are successfully assembled together.Analysed from the test results of X-ray diffraction (XRD),transmission electron microscopy (TEM),high resolution transmission electron microscopy (HRTEM),hysteresis loop,and photoluminescence (PL) spectrum,these nanocomposites exhibit superparamagnetic and photoluminescent properties.     

Synthesis of Co-Cu-Zn doped Fe3O4 nanoparticles with tunable morphology and magnetic properties

Co-Cu-Zn doped Fe₃O₄ nanoparticles can be successfully synthesized using a simple method. The particles in the size range 20−400 nm with different regular shapes i.e. sphere-like, regular hexane and tetrahedron are controllably achieved by changing the metal ion concentration. Compared to pure Fe₃O₄ without dopants, Co-Cu-Zn doped Fe₃O₄ nanoparticles exhibit better microwave absorbing properties at 2−18 GHz. Among three Co-Cu-Zn doped Fe₃O₄ nanoparticles with different morphologies, tetrahedral Co-Cu-Zn doped Fe₃O₄ nanoparticles represent a better dielectric loss in high frequency range. This work is believed the first known report of Co-Cu-Zn doped Fe₃O₄ nanoparticles with tunable morphology and magnetic properties through the hydrothermal process without using any organic solvents, organic metal salts or surfactants.     

Magnetic properties of prussian blue modified Fe3O4 nanocubes

Size controlled cubic Fe₃O₄ nanoparticles in the size range 90–10 nm were synthesized by varying the ferric ion concentration using the oxidation method. A bimodal size distribution was found without ferric ion concentration and the monodispersity increased with higher concentration. The saturation magnetization decreased from 90 to 62 emu/g when the particle size is reduced to 10 nm. The Fe₃O₄ nanoparticles with average particle sizes 10 and 90 nm were surface modified with prussian blue. The attachment of prussian blue with Fe₃O₄ was found to depend on the concentration of HCl and the particle size. The saturation magnetization of prussian blue modified Fe₃O₄ varied from 10 to 80 emu/g depending on the particle size. The increased tendency for the attachment of prussian blue with smaller particle size was explained based on the surface charge. The prussian blue modified magnetite nanoparticles could be used as a radiotoxin remover in detoxification applications.     

Magnetic and rheological properties of monodisperse Fe3O4 nanoparticle/organic hybrid

Fe₃O₄ nanoparticle/organic hybrids were synthesized via hydrolysis using iron (III) acetylacetonate at ∼80 °C. The synthesis of Fe₃O₄ was confirmed by X-ray diffraction, selected-area diffraction, and X-ray photoelectron spectroscopy. Fe₃O₄ nanoparticles in the organic matrix had diameters ranging from 7 to 13 nm depending on the conditions of hydrolysis. The saturation magnetization of the hybrid increased with an increase in the particle size. When the hybrid contained Fe₃O₄ particles with a size of less than 10 nm, it exhibited superparamagnetic behavior. The blocking temperature of the hybrid containing Fe₃O₄ particles with a size of 7.3 nm was 200 K, and it increased to 310 K as the particle size increased to 9.1 nm. A hybrid containing Fe₃O₄ particles of size greater than 10 nm was ferrimagnetic, and underwent Verwey transition at 130 K. Under a magnetic field, a suspension of the hybrid in silicone oil revealed the magnetorheological effect. The yield stress of the fluid was dependent on the saturation magnetization of Fe₃O₄ nanoparticles in the hybrid, the strength of the magnetic field, and the amount of the hybrid.     

Preparation and microwave absorption properties of Fe-phthalocyanine oligomer/Fe3O4 hybrid microspheres

The novel nano-scale Fe-phthalocyanine oligomer/Fe₃O₄ hybrid microspheres were synthesized from bis-phthalonitrile and FeCl₃·6H₂O through a simple solvent-thermal route. The morphology and structure of the hybrid microspheres were characterized by FTIR, XRD, SEM and TEM. These results showed that the hybrids were monodispersed solid microspheres and the morphology can be adjusted by controlling the addition of bis-phthalonitrile. On the basis of these results, the formation process was discussed. Magnetization measurement indicated that saturation magnetizations decreased linearly with increasing the addition of bis-phthalonitrile, while coercivities increased. The microwave absorption properties were measured by a vector network analyzer. The dielectric loss of the hybrid microspheres was larger and a new magnetic loss peak appeared at high frequency. The microwave absorbing properties enhanced with increasing the addition of bis-phthalonitrile and a maximum reflection loss of −31.1 dB was obtained at 8.6 GHz with 1 g bis-phthalonitrile when the matching thickness was 3.0 mm. The novel hybrid materials are believed to have potential applications in the microwave absorbing performances.     

基于苯基功能化纤维状Fe3O4@SiO2@KCC-1的磁性固相萃取-高效液相色谱测定环境水样中的邻苯二甲酸酯

本文采用共聚法制备了一种新型苯基功能化纤维状Fe₃O₄@SiO₂@KCC-1(Fe₃O₄@SiO₂@KCC-1-phenyl)材料,用于环境水样中邻苯二甲酸酯的磁性萃取. 制备的Fe₃O₄@SiO₂@KCC-1-phenyl展现了单分散的球形纤维状、较强的磁性(29 emu/g)和一个丰富的π电子体系. 研究和优化了洗脱溶剂的种类、吸附剂的用量、萃取时间和可重复使用性等因素对分析物萃取效率的影响. 在最佳条件下,用高效液相色谱方法,采用Fe₃O₄@SiO₂@KCC-1-phenyl萃取分离及测定环境水样中的邻苯二甲酸酯类化合物. 结果表明,本方法具有良好的线性(0.1∽20 ng/mL)、低的检测限(7.5∽29 μg/L, S/N=3). 将该方法应用于不同环境水样中邻苯二甲酸酯类化合物的测定,回收率为93%∽103.4%,相对标准偏差为0.8%∽8.3%.     

Fabrication and characterization of magnetic Fe3O4-CNT composites

Carbon nanotubes (CNTs) decorated with magnetite nanoparticles on their external surface have been fabricated by in situ solvothermal method, which was conducted in benzene at 500 °C with ferrocene and CNTs as starting reagents. The as-prepared composites were characterized using XRD, FTIR, SEM and TEM. It has been found that the amount of magnetite nanoparticles deposited on the CNTs can be controlled by adjusting the initial mass ratio of ferrocene to CNTs. The Fe₃O₄-CNT composites display good ferromagnetic property at room temperature, with a saturation magnetization value (M_s) of 32.5 emu g⁻¹ and a coercivity (H_c) of 110 Oe.     

Structural and magnetic studies of Fe2O3/SiO2 granular nanocomposites

Fe₂O₃/SiO₂ nanocomposites were synthesized by mechanical alloying, using Fe and SiO₂ powders as precursors. After 340 h milling, the sample essentially consists of hematite and amorphous silica. TEM images show hematite particles embedded in and surrounded by an amorphous silica matrix. A broad size distribution—5–50 nm—of hematite particles is found, and other group of very small—2–3 nm—unidentified particles are observed. Room temperature Mössbauer spectra show a paramagnetic doublet, which may correspond to a non-crystalline phase in the sample (probably the small unidentified particles), and a sextet corresponding to hematite. Magnetic properties were investigated by measuring hysteresis curves at different temperatures (5–300 K) and by zero-field-cooled (ZFC) and field-cooled (FC) magnetization curves (10 mT). The hysteresis loops were well fitted by a ferromagnetic contribution. No evidence of Morin transition is found down to 5 K.     

Magnetoresistance of Fe3O4/Au/Fe3O4 and Fe3O4/Au/Fe spin-valve structures

A detailed study of the in-plane magnetotransport properties of spin valves with one and two Fe₃O₄ electrodes is presented. Fe₃O₄/Au/Fe₃O₄ spin valves exhibit a clear anisotropic magnetoresistance in small magnetic fields but no giant magnetoresistance (GMR). The absence of GMR in these structures is due to simultaneous magnetization reversal in the two Fe₃O₄ layers. By contrast, a negative GMR effect is measured on Fe₃O₄/Au/Fe spin valves. The negative GMR is attributed to an electron spin scattering asymmetry at the Fe₃O₄/Au interface or an induced spin scattering asymmetry in the Au interfacial layers.     

海藻酸改性的空心Fe3O4纳米颗粒的制备与应用

不使用任何模板一步制得空心Fe₃O₄纳米颗粒,然后将海藻酸钠嫁接在氨基化的空心Fe₃O₄表面,再利用海藻酸盐与钙离子的作用,在空心Fe₃O₄表面形成一个凝胶化层,制得海藻酸盐凝胶化的空心Fe₃O₄纳米颗粒,粒径约为400～500 nm．采用TEM、XRD、XPS、VSM等手段对纳米微球进行表征．VSM表征结果表明在室温下样品磁性材料为超顺磁性．改性Fe₃O₄纳米颗粒成功地用于柔红霉素的载负和缓释,最大载负率和载药量分别为28.4%和14.2%．缓释结果表明,海藻酸盐凝胶化层的存在,能更有效控制柔红霉素缓慢地释放．