Fe_3O_4/TiO_2纳米异质结构的制备及磁性

以TiO2纳米线和Fe(NO3)3·9H2O为原料,在一缩二乙二醇体系中通过溶剂热反应制备了Fe3O4纳米粒子/TiO2纳米线异质结构.高分辨透射电子显微镜(HRTEM)观测结果表明,Fe3O4纳米粒子均匀地附着在TiO2纳米线上,并与TiO2纳米线之间形成了有效的复合.磁性研究结果表明,与文献报道的同粒径纯相Fe3O4纳米粒子相比,异质结构的阻隔温度点明显降低,异质结构的形成对Fe3O4磁性产生了影响.     

新型磁性纳米金修饰过氧化氢生物传感器的研制

利用共沉淀法合成纳米Fe3O4颗粒,将半胱氨酸吸附到纳米Fe3O4微粒表面,借助半胱氨酸的巯基(-SH)对纳米金的强烈吸附,使纳米金自组装到磁性颗粒上,再通过静电吸附作用自组装辣根过氧化酶(HRP),合成了Fe3O4/Cys/Au/HRP纳米复合粒子,最后通过磁力将其修饰到固体石蜡碳糊电极表面,制得新型过氧化氢生物传感器.以对苯二酚作为电子媒介,用计时电流法对H2O2进行测定,线性范围为2.4 X10-3～6.0×10-6mol/L,检出限(S/N=3)为2.5 X 10-6mol/L,响应时间小于10 s.磁性纳米微粒Fe3O4/Cys/Au能够高效地保持HRP的生物活性.该新型传感器已用于实际样品测定.     

新型磁性纳米粒的制备及分离手性物的初步研究

制备了一种新型的手性磁纳米复合物(Fe3O4/SiO2/CMCD),并初步研究了其手性拆分能力。正硅酸乙酯与制备的Fe3O4磁纳米粒反应制得Fe3O4/SiO2;通过羧甲基-β-环糊精(CM-β-CD)手性选择剂对Fe3O4/SiO2修饰制得Fe3O4/SiO2/CMCD。采用傅立叶变换红外光谱、透射电子显微镜和振动样品磁强计对手性磁性纳米材料进行结构表征,表明磁性纳米复合物呈球形。同时将制得的手性磁纳米复合物应用于拆分外消旋体DL-色氨酸和酪氨酸,显示其具有较好的手性识别能力。     

原位沉析法制备磁性氧化铁羟基磷灰石/壳聚糖棒材

首先通过化学沉淀法制备磁性氧化铁羟基磷灰石(Fe3O4/HA),然后以壳聚糖(CS)为基体,利用原位沉析法将Fe3O4/HA与CS复合,制得磁性Fe3O4/HA/CS复合材料.经XRD、粒径分布和PPMS测试,结果表明了Fe3O4/HA复合物的生成.系统研究了磁性Fe3O4/HA/CS棒材力学性能的影响因素,最终确定Fe3O4与HA质量比为3∶17,磁性Fe3O4/HA与CS质量比为9∶91时,棒材的力学性能最优,弯曲强度可达到87.0 MPa,弯曲模量1.57 GPa.     

PS/Fe_3O_4复合材料的制备及其磁性能

以苯乙烯为单体,四氧化三铁纳米粒子(Fe3O4)为磁性体,采用超声辐照乳液聚合法制备了PS/Fe3O4复合粒子(1,1.0μm~100.0μm),其结构和磁性能经FT-IR,XRD和VSM表征。结果表明,核壳之间发生了相互作用,Fe3O4和PS分别以单一相反尖晶石和无定型态存在于1中;1具有超顺磁性,饱和强度为8.333 3 emu·g-1。     

羧甲基壳聚糖磁性纳米粒子的合成及应用

通过合成油酸修饰的Fe3O4纳米粒子和羧甲基壳聚糖直接包埋油酸修饰的Fe3O4纳米粒子的两步合成法制备了羧甲基壳聚糖磁性纳米粒子。采用透射电子显微镜、傅里叶变换红外光谱、振动样品磁强计和同步热分析测试技术对制备的羧甲基壳聚糖磁性纳米粒子进行了表征。所得磁性纳米粒子呈规则球形,粒径约为10 nm;表面含羧基,且具有很好的顺磁性和稳定性。考察了羧甲基壳聚糖磁性纳米粒子对阿霉素的载药量和对阿霉素在磷酸盐缓冲溶液中的缓释性能。结果表明,磁性纳米粒子对阿霉素展示了较高的载药量(91.8 mg/g),结合了阿霉素的磁性复合物对阿霉素的缓释作用明显,说明制备的羧甲基壳聚糖磁性纳米粒子有望作为治疗肿瘤的纳米磁靶向药物输送载体。     

Fe_3O_4/P(NaUA-St-BA)核-壳纳米磁性复合粒子的合成与表征

以表面包敷有反应型的表面活性剂NaUA(十一烯酸钠)的Fe3O4磁性胶体粒子为种子,运用无皂乳液聚合方法原位制备出Fe3O4P(NaUAStBA)核壳纳米磁性复合粒子.Fe3O4磁性胶体粒子的粒径为10nm左右.IR和TG结果分析表明,苯乙烯、丙烯酸酯和NaUA在Fe3O4粒子的表面发生了聚合反应,形成P(NaUAStBA);TEM和激光粒度分析仪测试结果显示,Fe3O4P(NaUAStBA)复合粒子具有核壳结构而且粒子分布均匀、平均粒径60nm;TG测试的结果表明,NaUA在Fe3O4粒子的包覆率为13.83%,P(NaUAStBA)共聚物的包覆率71.85%;振动样品磁强仪(VSM)测试的磁滞回线则表明由无皂乳液聚合得到的Fe3O4P(NaUAStBA)复合粒子具有超顺磁性,可避免磁性微球在磁场中的团聚.另外,合成的磁性胶乳可稳定存放数月.     

Fe3O4表面原位引发可控/“活性”聚合制备磁性聚苯乙烯纳米粒子

采用化学共沉淀方法合成了Fe3O4纳米粒子, 用3-甲基丙烯酰氧基丙基三甲氧基硅烷(3-MPS)对其进行表面接枝修饰, 然后以苯乙烯(St)为单体, 过氧化苯甲酰(BPO)为引发剂, 4-羟基-2,2,6,6-四甲基哌啶-1-氧化物自由基(HTEMPO·)为稳定自由基介质, 采用可控/“活性”自由基聚合技术在修饰后的Fe3O4纳米粒子表面原位引发聚合, 制备了粒径小、分布窄、磁含量高的磁性聚苯乙烯（PS）纳米粒子. X射线衍射(XRD)研究表明, 所合成的Fe3O4粒子为尖晶石结构. 凝胶渗透色谱(GPC)分析表明, 聚苯乙烯的分子量与反应时间呈较好的线性关系. 透射电镜(TEM)观察表明, 所制备的磁性聚苯乙烯纳米粒子的粒径在20-30 nm之间. 热重(TG)分析得到磁性聚苯乙烯纳米粒子的磁含量为62.6%. 振动样品磁强计(VSM)测试结果表明, 磁性聚苯乙烯纳米粒子的比饱和磁化强度为31.7 emu·g-1, 呈现单磁畴结构.     

SiO_2表面包覆对Fe_3O_4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。     

用于体外基因转染的氨基硅烷Fe3O4复合纳米粒子的合成及表征

利用2-吡咯烷酮和乙酰丙酮铁为原料制备Fe3O4磁性纳米颗粒, 用XRD和TEM对样品进行了表征. 选择偶联剂γ-氨丙基三乙氧基硅烷[NH2C3H6Si(OC2H5)3]对纳米粒子进行表面修饰, 制得APTTS/Fe3O4复合载体材料. 以此复合粒子作为传递载体, 将CD基因转染U251胶质瘤细胞. 采用RT-PCR, Western blot及免疫荧光等方法检测CD基因的表达及功能. 结果表明, 制备的Fe3O4颗粒粒径为8~10 nm, 结晶度较高; 经表面修饰后, 粒子表面负载—OH, —NH, —NH2, —C—O和—C—OH等多种功能基团. DNA结合分析及DNase-I消化结果表明, APTTS/Fe3O4粒子能够有效地结合和保护DNA. 体外细胞转染实验证实, 该复合纳米颗粒能够高效地传递CD基因进入U251胶质瘤细胞内, 并进行稳定表达.     

磁性Fe_2O_3/Au/Ag复合纳米粒子的制备及其富集作用研究

利用种子生长法制备了磁性Fe2O3/Au/Ag复合纳米粒子,采用UV-vis和SEM对其光学性质以及表面结构的变化进行了表征.通过调节硝酸银的用量,制备了一系列具有不同Ag壳层厚度和表面结构的双金属外壳纳米粒子.以苯硫酚(TP)为探针分子,研究了不同Ag壳厚度的磁性纳米粒子的表面增强拉曼散射(SERS)活性.结果表明其SERS活性与表面结构的改变有关,在同时出现Ag和Au光学性质的Fe2O3/Au/Ag复合纳米粒子表面可观察到最强的SERS效应,这与表面的针孔效应以及Ag和Au之间的耦合增强作用有关.考察了Fe2O3/Au/Ag复合纳米粒子的磁富集作用,并利用SERS原位监测磁富集溶液中低浓度TP的能力,研究结果表明通过磁富集可提高SERS检测限,并且Fe2O3/Au/Ag的磁富集能力较Fe2O3/Au弱,但前者SERS信号较强.     

聚邻甲苯胺的电化学和磁性质

The changes in potentials and pH values of the solution gave rise to variations of colour and electronic absorption spectra of poly-o-methylaniline film. However, its colour did not change with potential and polymer lost its electrochemical activities in the solution of pH 4.13. The g-value was 2.0027 and was not affected by the kinds of doped anions and hydrolysis. The ΔH_(p-p) was 1.6G. It did not depend onthe kinds of doped anions, but was affected by hydrolysis. The magnetic suscepti-billity of poly-o-methylaniline was not measurable at 0.8 to 4 kG magnetic field.     

Magnetic properties of monodispersed Ni/NiO core-shell nanoparticles

We have recently developed a method to fabricate monodispersed Ni/NiO core-shell nanoparticles by pulsed laser ablation. In this report, the size-dependent magnetic properties of monodispersed Ni/NiO core-shell nanoparticles were investigated. These nanoparticles were formed in two steps. The first was to fabricate a series of monodispersed Ni nanoparticles of 5 to 20 nm in diameter using a combination of laser ablation and size classification by a low-pressure differential mobility analyzer (DMA). The second step was to oxidize the surfaces of the Ni particles in situ to form core-shell structures. A superconducting quantum interference device (SQUID) magnetometer was used to measure the magnetic properties of nanostructured films prepared by depositing the nanoparticles at room temperature. Ferromagnetism was observed in the magnetic hysteresis loop of the nanostructured films composed of core-shell nanoparticles with core diameters smaller than the superparamagnetic limit, which suggests the spin of Ni core was weakly exchange coupled with antiferromagnetic NiO shell. In contrast, smaller nanoparticles with core diameters of 3.0 nm exhibited superparamagnetism. The drastic change in the hysteresis loops between field-deposited and zero-field-deposited samples was attributable to the strong anisotropy that developed during the magnetic-field-assisted nanostructuring process.     

Magnetic and structural properties of Cr1−tTitAs

The pseudobinary CrAsTiAs system has been investigated by X-ray and neutron diffraction and magnetic susceptibility measurements at temperatures between 10 and 1000 K. The phase diagram includes paramagnetic regions with the MnP-, NiAs-, and TiP-type structures and a low-temperature helimagnetic, MnP-type state for0.00 ≦ t ≦ 0.10 of Cr_1?tTi_tAs. The first-order para- to helimagnetic transition in Cr_1?tTi_tAs is accompanied by a hysteresis of 10–15 K. The results are discussed in relation to the findings for other Cr_1?tT_tAs(T =V, Mn, Fe, Co, Ni) andCrAs_1?xX_x (X = P, Sb, Se) phases.     

Microstructure and Magnetic Properties of Ag/Fe/Ag Pseudo-Sandwich Nanogranular Films

"Nanogranular Ag/Fe/Ag films were prepared by magnetron sputtering from a silver and an iron target onto glass substrates at room temperature and subsequent in situ annealing. The structural and magnetic properties of the films were investigated as a function of silver layer thickness and annealing temperature. X-ray diffraction shows the Fe(110) peak is formed in all the samples. Vibrating sample magnetometer measurements indicate that the magnetic moments lie well perpendicular to the film plane. Coercivityreaches the maximum in the sample annealed at 500 oC for 30 min with 3 nm Ag layer. A scanning probemicroscope was used to scan surface morphology and magnetic domain structures. In as-deposited samplesthe average grain size and the average roughness is smaller than that the annealing samples. After annealing,the grain size is larger and the contrast of domains increases, but the domain size becomes smaller."     

Magnetic and thermoelectric properties of layered LixNayCoO2

The magnetic, thermoelectric, and structural properties of Li_xNa_yCoO₂, prepared by intercalation and deintercalation chemistry from the thermodynamically stable phase Li_0.41Na_0.31CoO₂, which has an alternating Li/Na sequence along the c-axis, are reported. For the high Li-Na content phases Li_0.41Na_0.31CoO₂ and Li_0.40Na_0.43CoO₂, a sudden increase in susceptibility is seen below 50 K, whereas for Li_0.21Na_0.14CoO₂ an antiferromagnetic-like transition is seen at 10 K, in spite of a change from dominantly antiferromagnetic to dominantly ferromagnetic interactions with decreasing alkali content. The Curie constant decreases linearly with decreasing alkali content, at the same time the temperature-independent contribution to the susceptibility increases, indicating that as the Co becomes more oxidized the electronic states become more delocalized. Consistent with this observation, the low alkali containing phases have metallic-like resistivities. The 300 K thermopowers fall between 30 μV/K (x+y=0.31) and 150 μV/K (x+y=0.83).     

Magnetic properties of Ca2F2-xMnxO5

Magnetic susceptibility of Ca₂F_2-xMn_xO₅ members crystallizing in two different structures, one having octahedral (O), tetrahedral (T) and square-pyramidal (SP) coordination of transition metal atoms (OTSP structure) and the other having octahedral and tetrahedral coordination (OT structure), has been investigated. Susceptibility behaviour of the oxides with OTSP structure is different from that of the oxides with OT structure. Ca₂Fe_1-33Mn_0-67O₅ with OTSP structure shows an antiferromagnetic ordering while the corresponding oxide with OT structure shows weak ferromagnetism. Contribution No. 398 from the Solid State and Structural Chemistry Unit