Fabrication and characterization of zinc oxide nanoparticle coated magnetic iron oxide: Effect of S-layers adsorption on surface of oxide

Mixed zinc oxide nanoparticle coated magnetic iron oxide has been prepared by a sol–gel and co-precipitation routes. Magnetic iron oxide nanoparticles were synthesized by co-precipitation of ferric and ferrous ions with ammonia, and then zinc oxide was coated onto the surface of magnetic iron oxide by hydrolysis of zinc precursors. As a result, zinc oxide coated magnetic iron oxide nanoparticles with an average size of 68 nm were obtained. The crystalline bacterial cell surface layer)S-layer (used in this study was isolated from Lactobacillus helveticus ATCC 12046. The S-layer was adsorbed onto the surface of zinc oxide nanoparticle coated magnetic iron oxide. The nanoparticles were analyzed by X-ray powder diffractometry (XRD), infrared spectroscopy (FTIR), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FESEM) were used to characterize the structural and the chemical features of the nanocomposites. The infrared spectra indicate that the S-layer-nanoparticle interaction occurs. This novel nanoparticle showed admirable potential in adsorption of S-layers on the surface of oxides for drug delivery.     

五羰基铁雾化-热分解-氧化合成氧化铁纳米粒子

建立了将五羰基铁超声雾化、分段加热分解-氧化及产物收集-修饰一体化的纳米氧化铁合成装置,研究了不同修饰剂对纳米粒子的相组成和形貌的影响。采用XRD、TEM和FTIR对合成的纳米粒子进行了表征。通过在雾化液或收集液中添加不同修饰剂,得到平均粒径11.4～36.5 nm的球形水溶性γ-Fe2O3纳米粒子。     

Effect of silane-modified ZnO on morphology and properties of bionanocomposites based on poly(ester-amide) containing tyrosine linkages

In this study, various optically active poly(ester-amide)/Zinc oxide bionanocomposites (PEA/ZnO BNCs) were synthesized with different amount of modified ZnO nanoparticles using ultrasonic irradiation. To obtain the homogeneous distribution of ZnO in polymer matrix, the surface of nanoparticles was modified to organophile with ??-aminopropyltriethoxyl silane. PEA/ZnO BNCs were characterized by Fourier transform infrared spectra, X-ray diffraction, field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM). The FE-SEM, AFM, and TEM results confirmed that the nanoparticles were dispersed uniformly in PEA matrix at the nanoscale. In addition, thermogravimetric analysis data indicated an improvement of thermal stability of novel BNC materials as compared to the pure polymer.     

A novel thermal decomposition method for the synthesis of ZnO nanoparticles from low concentration ZnSO4 solutions

In this research work, ZnO nanoparticles were prepared by direct thermal decomposition method with Zn₄(SO₄)(OH)₆·0.5 H₂O as a precursor. The precursor was calcinated in air for 1 h at 825 °C. Samples were characterized by X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), infrared spectrum (IR), and scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD, EDS, and IR results indicated that the ZnO nanoparticles were pure. The average crystallite and particle size of the ZnO nanoparticles were estimated to be 87 nm and 92 nm by XRD and TEM, respectively. The SEM and TEM images showed that the ZnO nanoparticles were of spherical shape. The simplicity of the present method suggests its potential application at industrial scale as a cheap and convenient way to produce pure ZnO nanoparticles from low concentration ZnSO₄ solutions.     

Magnetic and electric responsive hydrogel–magnetic nanocomposites for drug‐delivery application

Magnetic and electrically responsive hydrogel networks were developed for drug‐delivery applications. The hydrogel matrices were synthesized by the polymerization of acrylamide monomer in the presence of carboxymethylcellulose (CMC) or methylcellulose (MC) with N,N‐methylenebisacrylamide, a crosslinker with the redox initiating system ammonium persulfate/tetramethylethylenediamine. The magnetic nanoparticles were generated throughout these hydrogel matrices by an in situ method by the incorporation of iron ions and their subsequent reduction with ammonia. A series of hydrogel–magnetic nanocomposites (HGMNCs) were developed with various CMC and MC compositions. The synthesized HGMNCs were characterized with spectral (Fourier transform infrared and ultraviolet–visible spectroscopy), X‐ray diffraction, thermal, and microscopy methods. These HGMNCs contained iron oxide (Fe₃O₄) nanoparticles with an average particle size of about 22 nm, as observed by transmission electron microscopy. The dielectrical properties of the pure hydrogel (HG); the hydrogel loaded with iron ions, or the hydrogel iron‐ion composite (HGIC); and the HGMNCs were measured. These results suggest that HGMNCs exhibited higher dielectric constants compared to HG and HGICs. The curcumin loading and release characteristics were also measured for HG, HGIC, and HGMNC systems. These data revealed that there was a sustained release of curcumin from HGMNCs because of the presence of magnetic nanoparticles in the hydrogel networks. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Novel flow injection synthesis of iron oxide nanoparticles with narrow size distribution

A novel synthesis method based on a flow injection technique was developed and the synthesis of magnetite nanoparticles was performed to demonstrate the concept. The technique consisted of continuous or segmented mixing of reagents under laminar flow regime in a capillary reactor. Different schemes of the flow injection synthesis were evaluated and the continuous mode was found to be more advantageous for the synthesis of the iron oxide particles. The material was characterised by X-ray diffraction, thermal analysis, electron microscopy, and magnetic susceptometry. The obtained magnetite nanoparticles had a narrow size distribution in the range 2-7 nm. The influence of chemical parameters and conditions on properties of the material was investigated.     

Hexamethylene diamine/carboxymethyl cellulose grafted on magnetic nanoparticles for controlled drug delivery

In this study, chemically modified iron oxide nanoparticles with super paramagnetic behavior and biodegradable properties were prepared through the reaction of a polymeric layer with surface hydroxyl functional groups of magnetic nanoparticles (MNP). For this purpose firstly, MNP was grafted with hexamethylene diisocyanate. Then, carboxymethyl cellulose which was modified with the hexamethylenediamine (mCMC) as a shell was coated and reacted simultaneously on MNP-grafted hexamethylene diisocyanate to form a polymeric core–shell (MNP/mCMC). The structural, morphological, thermal, and magnetic properties of the synthesized magnetite nanocomposite were confirmed by Fourier transform infrared spectrophotometer, thermal gravimetric analysis, X-ray diffraction, vibrating sample magnetometer, and scanning electron microscopy. The size of the resulting MNP/mCMC was approximately between 70 and 120 nm. Doxorubicin (DOX) as a model anticancer drug was used. The in vitro release of DOX from the MNP/mCMC was investigated and indicated that the release speed of the DOX could be well controlled. Release profiles of the DOX and its loading capacity were determined by ultraviolet–visible spectroscopy absorption measurement at λ _max 483 nm. The obtained results suggest that the prepared magnetite nanocomposite would be beneficial as a targeted anti-tumor drug carrier for pharmaceutical applications.     

Materials Characterization of Feraheme/Ferumoxytol and Preliminary Evaluation of Its Potential for Magnetic Fluid Hyperthermia

Feraheme, is a recently FDA-cleared superparamagnetic iron oxide nanoparticle (SPION)-based MRI contrast agent that is also employed in the treatment of iron deficiency anemia. Feraheme nanoparticles have a hydrodynamic diameter of 30 nm and consist of iron oxide crystallites complexed with a low molecular weight, semi-synthetic carbohydrate. These features are attractive for other potential biomedical applications such as magnetic fluid hyperthermia (MFH), since the carboxylated polymer coating affords functionalization of the particle surface and the size allows for accumulation in highly vascularized tumors via the enhanced permeability and retention effect. This work presents morphological and magnetic characterization of Feraheme by transmission electron microscopy (TEM), Energy dispersive X-ray spectroscopy (EDX), and superconducting quantum interference device (SQUID) magnetometry. Additionally, the results of an initial evaluation of the suitability of Feraheme for MFH applications are described, and the data indicate the particles possess promising properties for this application.     

Preparation and Characterization of Poly(benzimidazole-amide)/ZnO Nanocomposites Using Silane Coupling Agent

Some novel nanocompoites were fabricated via zinc oxide (ZnO) nanoparticles which was modified by 3-aminopropyltriethoxylsilane (KH550) as a coupling agent. Poly(benzimidazole-amide) (PBIA) was synthesized via polymerization reaction of 1,3-bis(5-amino-1H-benzimidazol-2-yl)benzene (3a) with isophthaloyl chloride (4b) and used as a polymer matrix. PBIA/ZnO nanocompoites were characterized by Fourier transform infrared spectra (FT-IR), X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). FE-SEM and TEM analysis showed that the modified ZnO nanoparticles were homogeneously dispersed in polymer matrix. In addition, thermogravimetric analysis (TGA) data indicated an enhancement of thermal stability of nanocomposite compared with the pure polymer.     

Application of magnetic iron oxide nanoparticles prepared from microemulsions for protein purification

BACKGROUND: Magnetic nanoparticles are of immense interest for their applications in biotechnology. This paper reports the synthesis of magnetic iron oxide nanoparticles from two different water‐in‐oil microemulsion systems (ME‐MIONs), their characterization and also their use in purification of coagulant protein. RESULTS: ME‐MIONs have demonstrated to be an efficient binder in the purification of Moringa oleifera protein when compared with the superparamagnetic iron oxide nanoparticles prepared from coprecipitation in aqueous media. The size and morphology of the ME‐MIONs were studied by transmission electron microscopy (TEM) while the structural characteristics were studied by X‐ray diffraction (XRD). The microemulsion magnetic iron oxide nanoparticles (ME 1‐MION and ME 2‐MION) obtained have a size range 7–10 nm. The protein and ME‐MIONs interaction was investigated by Fourier transform infrared spectroscopy (FT‐IR); the presence of three peaks at 2970, 2910 and 2870 cm^?1 respectively, confirms the binding of the protein. The purification and molecular weight of the coagulant protein was 6.5 kDa as analyzed by SDS‐PAGE. CONCLUSION: The ME‐MIONs have the advantage of being easily tailored in size, are highly efficient as well as magnetic, cost effective and versatile; they are, thus, very suitable for use in a novel purification technique for protein or biomolecules that possess similar characteristics to the Moringa oleifera coagulant protein. Copyright © 2011 Society of Chemical Industry     

Synthesis of Highly Dispersed Barium Titanate Nanoparticles by a Novel Solvothermal Method

A novel solvothermal route has been developed to synthesize highly dispersed nanocrystalline barium titanate (BaTiO₃), using a mixture of ethylenediamine and ethanolamine as a solvent. The as-synthesized BaTiO₃ nanoparticles were characterized by X-ray powder diffraction, transmission electron microscopy (TEM), high-resolution TEM, Fourier transform infrared spectroscopy, and thermal analysis. Based on the results of characterizations, the organic solvent was found to influence strongly the crystal growth and dispersibility of BaTiO₃. The BaTiO₃ nanoparticles obtained were highly dispersed and crystalline with a cubic perovskite structure. The particle size derived from the TEM ranged from 5 to 20 nm.     

Synthesis method of novel Gd2O3@Fe3O4 nanocomposite modified by dextrose capping agent

In current study, gadolinium oxide was heterogeneously formed on the surface of iron oxide nanoparticles and further modified with dextrose capping agent to be used in biomedical applications, especially for contrast enhancement in MR images. First, two types of iron oxide nanoparticles were prepared at 25 and 80 ^°C via simple coprecipitaion method. Then, gadolinium oxide nanoparticles were synthesized through a consecutive precipitation process on previously formed iron oxide seeds in an aqueous media and subsequent annealing at 300 ^°C. Finally, dextrose was used as capping agent to stabilize nanocomposites in a colloidal suspension. X-ray diffraction (XRD), Scanning and Transmission electron microscopy, Dynamic Laser Scattering (DLS), Fourier-Transform Infrared Spectroscopy (FTIR), and Magnetometery (VSM) techniques were employed for nanocomposites investigation and MTT-assay method used for viability assessment of colloidal samples. Measurements based on Scherrer equation from XRD patterns showed that increasing coprecipitation temperature resulted bigger iron oxide crystallites. The iron oxide crystallite size was increased from 15.1 to 28.1 nm. Precipitation process led to gadolinium oxide formation with 30.7 and 38.8 nm crystallite sizes, respectively. TEM images revealed that iron oxide agglomerates were encapsulated in gadolinium oxide surroundings. Hydrodynamic size of the coated nanoparticles with dextrose was 208 and 247 nm. In VSM examinations, nanocomposites did not display coercive field and the saturation magnetization was 1.93 emu/g. MTT-assay results showed 80% viability in 285 μg nanocomposites containing 96.9 μg [Fe] and 11.4 μg [Gd].     

In situ synthesis of iron oxide nanoparticles in a styrene-divinylbenzene copolymer

Summary Magnetic iron oxide nanoparticles were prepared by in situ within a sulfonated styrene-divinylbenzene copolymer. The magnetic nanocomposite was characterized by X-ray diffraction, transmission electron microscopy and vibrating sample magnetometry. The size distribution of the nanoparticles was relatively narrow with good distribution within the copolymer. Nearly spherical nanoparticles, 7 nm in diameter, were identified as CoFe₂O₄ and had a well-defined crystalline structure. Magnetic measurements revealed that the magnetic nanocomposites are superparamagnetic.     

Size Controlling of L1<Subscript>0</Subscript>-FePt Nanoparticles During High Temperature Annealing on the Surface of Carbon Nanotubes

Mono-size FePt nanoparticles with particles size about 2.5 nm have been prepared by polyol method on the surface of carbon nanotubes (CNTs). The CNTs functinalization time and the mass ratio of nanoparticles to CNTs affects on the CNTs surface coating. The as-synthesis nanocomposites have a superparamagnetic behavior with chemically disordered fcc structure at room temperature and they can be transformed into chemically ordered fct structure after thermal annealing above 600 °C. Their magnetic behavior changes from the superparamagnetic to the ferromagnetic with a large coercivity up to 0.83 T for the nanocomposites which annealed at 800 °C. The CNTs surfaces as a substrate prevent the agglomeration of nanoparticles during high temperature annealing and the FePt nanoparticles after annealing at 800 °C have finite size with an average about 10 nm. The structure, composition and magnetic properties of nanocomposite were characterized by X-ray diffraction, transmission electron microscopy, Fourier transform infrared spectroscopy and vibrating sample magnetometer.     

基于化学方法制备油酸改性超顺磁性氧化铁纳米粒子

目的 油酸改性超顺磁性氧化铁纳米粒子（O-SPION）被应用于制备高品质的MRI T2阴性造影剂或搭载药物的磁靶向分子探针,不同于传统的物理合成方法,本课题组尝试采过化学方法制备O-SPION,并通过体外实验检测其细胞毒性及细胞透过性。方法 通过共沉淀法制备分散性好、磁响应强的超顺磁性纳米粒子。对油酸的羧基进行活化后,利用缩合反应实现油酸改性SPION的化学合成。采用X-Ray衍射仪、红外光谱仪、激光粒度分布测试仪、透射电镜对产物进行表征。MTT法检测其对人肝癌细胞HepG2的毒性作用,普鲁士蓝染色检测其细胞摄取能力。结果 O-SPION的核心粒径为12?.5 nm的,其具有稳定的化学结构和低表面电势,体外实验证明其低毒或无毒性,且在细胞内的摄取量较原始SPION明显增多。结论 利用化学方法成功合成了O-SPION,为进一步制备高品质MRI造影剂提供实验依据。     

The Change of Structural,Optical and Thermal Properties of a PVDF/PVC Blend Containing ZnO Nanoparticles

Nanocomposites consisting of a polyvinylidene fluoride (PVDF)/polyvinyl chloride (PVC) blend containing zinc oxide (ZnO) nanoparticles were prepared. The changes of the structural, optical and thermal properties of the PVDF/PVC blend before and after addition of ZnO were studied. The shift of intensity in IR bands suggested an interaction and compatibility between the blend and ZnO. The structural properties, crystallinity and grain size of the samples were studied using X-ray diffraction. The average grain size was approximately 16 nm confirmed by TEM observations. The X-ray peak positions of ZnO in doped samples were located in the same positions as those of pure ZnO indicating the crystal structure of ZnO was not altered by its incorporation into PVDF/PVC. The estimated values of the optical energy gap from UV/Vis spectra for indirect transition decrease with increasing ZnO due to charge transfer between PVDF/PVC and ZnO nanoparticles. The thermogravimetric analysis curves showed nearly identical behaviors for all samples. Samples that contained ZnO exhibited less weight loss compared to the pure blend attributed to crosslinking formation between the blend and ZnO. Transmission electron microscopy (TEM) images revealed that ZnO was uniformly distributed inside PVDF/PVC polymeric matrices and was superimposed on an amorphous background.     

超声辅助均匀沉淀法由前躯体ZnS制备ZnO纳米颗粒及其表征

前躯体ZnS在超声辅助60℃的低温条件下,采用醋酸锌为锌源、硫代乙酰胺为硫源来制备,然后采用在空气中热处理前躯体ZnS的方法制备了直径约为20~40 nm的ZnO纳米颗粒。所得产物分别采用红外光谱(FTIR)、热重-差热分析(TGA-DTA)、X射线衍射(XRD)、场发射扫描电镜(FE-SEM)、透射电镜(TEM)、电子能谱(EDS)和荧光光谱(PL)进行表征。实验结果表明,所得产物ZnO为六方纤锌矿结构,且结晶性很好,并且随着超声时间的延长其粒径有所降低。室温PL光谱表明,样品在400~550 nm内有3个较强的荧光发射峰。     

Study on Composition Distribution and Ferromagnetism of Monodisperse FePt Nanoparticles

Monodisperse FePt nanoparticles with size of 4.5 and 6.0 nm were prepared by simultaneous reduction of platinum acetylacetonate and thermal decomposition of iron pentacarbonyl in benzylether. The crystallography structure, size, and composition of the FePt nanoparticles were examined by X-ray diffraction and transmission electron microscopy. Energy dispersive X-ray spectrometry measurements of individual particles indicate a broad compositional distribution in both the 4.5 and 6 nm FePt nanoparticles. The effects of compositional distribution on the phase-transition and magnetic properties of the FePt nanoparticles were investigated.     

Novel iron oxide–silica coreshell powders compacted by using pulsed electric current sintering: Optical and magnetic properties

The properties of the bulk materials consolidated of silica coreshell powders with iron oxide core have been studied. Iron oxide nanoparticles smaller than 20 nm in size were synthesized by a reverse co-precipitation process in ambient atmosphere. Coreshell structures with various amounts of iron oxide were prepared via a modified Stöber method. The powders were compacted by using pulsed electric current sintering (PECS) at 1373 K. The morphologies, microstructures, phases, optical, and magnetic properties of the samples were studied by using transmission electron microscope (TEM), scanning electron microscope (SEM), X-ray diffraction (XRD), UV–visible spectroscopy (UV–Vis), and vibrating sample magnetometer (VSM). Transmittance values in the 250–800 nm range varied with the amount of iron oxide. Sample with the lower content was transparent while the sample with the highest content was opaque with microporosity. The compact with the highest iron oxide content showed the ferromagnetic behaviour at 300 K. The phase transformations in the coreshell powders during the sintering process are discussed.     

Preparation and corrosion resistance of nanostructured PVC/ZnO–polyaniline hybrid coating

ZnO–polyaniline nanocomposite with core–shell nanostructure was prepared by in situ polymerization of aniline monomer in the presence of ZnO nanoparticles. Fourier transform infrared spectroscopy, X-ray diffraction patterns, field emission scanning electron microscopy and transmission electron microscopy techniques were used to characterize the composition and structure of ZnO–polyaniline nanocomposite. d.c. electrical conductivity measurement showed that the electrical conductivity of ZnO–polyaniline nanocomposite pellets is higher than that of pristine polyaniline and ZnO nanoparticles pellets. The addition of ZnO nanoparticles causes to the increasing of polyaniline electrical conductivity. ZnO–polyaniline nanocomposite was mixed with polyvinyl chloride (PVC) through a solution mixing method and the three components PVC/ZnO–polyaniline hybrid material was applied as coating on iron coupon by the solution casting method. Corrosion protection efficiency of PVC/ZnO–polyaniline hybrid coating on iron coupons was studied by open circuit potential and Tafel techniques in 3.5% NaCl solution as corrosive environment. According to the results, PVC/ZnO–polyaniline hybrid nanocomposite coating showed dramatically increased corrosion protection effect on iron samples compared to that of uncoated iron coupon and pure polyaniline anticorrosive coating. It was found that ZnO nanoparticles improve the barrier and electrochemical anticorrosive properties of polyaniline and the addition of polyvinyl chloride increases the barrier effect of polyaniline coating.