Controllable phase connectivity and magnetoelectric coupling behavior in CoFe(2)O(4)-Pb(Zr,Ti)O(3) nanostructured films

Magnetoelectric CoFe(2)O(4)-Pb(Zr,Ti)O(3) nanostructured films with various phase connectivity patterns were prepared by a pulsed laser deposition method. It was found that the microstructure as well as the phase connectivity pattern of the film varied remarkably with the variation of phase content ratio. All composite nanofilms exhibit evident ferromagnetic and ferroelectric characteristics, as well as distinct magnetoelectric coupling behavior upon increasing the magnetic field. The correlation between the phase connectivity pattern and magnetoelectric coupling behavior for the composite nanofilm was revealed. This work provides an efficient avenue to modulate the magnetoelectric coupling behavior for the ferroelectric-ferromagnetic composite nanofilm.     

The enhanced microwave absorption property of CoFe(2)O(4) nanoparticles coated with a Co(3)Fe(7)-Co nanoshell by thermal reduction

CoFe(2)O(4) nanoparticles were fabricated by a sol-gel method and then were coated with Co(3)Fe(7)-Co by means of a simple reduction process at different temperatures under 2% H(2) with the protection of argon to generate the dielectric-core/metallic-shell structure. The optimum reflection loss (RL) calculated from permittivity and permeability of the 80 wt% CoFe(2)O(4)/Co(3)Fe(7)-Co and 20 wt% epoxy resin composites reached - 34.4 dB, which was much lower than that of unreduced CoFe(2)O(4) and epoxy resin composites, at 2.4 GHz with a matching thickness of 4.0 mm. Moreover the RL exceeding - 10 dB in the maximum frequency range of 2.2-16 GHz was achieved for a thickness of composites of 1.0-4.5 mm with 600?°C thermal reduction process. The improved microwave absorption properties are a consequence of a proper electromagnetic match and the enhanced magnetic loss besides its dielectric loss due to the existence of the core/shell structure in CoFe(2)O(4) composites. Thus, the reductive CoFe(2)O(4) nanoparticles have great potential for being a highly efficient microwave absorber.     

Effect of strain on ferroelectric and magnetic behavior in Pb(Zr0.52Ti0.48)O3-based magnetoelectric heterostructures

In this paper, the "sandwich" structured magnetoelectric composite films of Pb(Zr0.52Ti0.48)O3/ NiFe2O4/Pb(Zr0.52Ti0.48)O3 and Pb(Zr0.52Ti0.48)O3/CoFe2O4/Pb(Zr0.52Ti0.48)O3 are epitaxially grown on SrRuO3/SrTiO3 substrates by pulsed-laser deposition. The crystalline quality and microstructures of these heterostructures are investigated by X-ray diffraction technique. The effects of strain on the ferroelectric, magnetic and magnetoelectric coupling properties of these thin films are systematically studied. The results show that the strain effect induced by lattice mismatch between the ferroelectric/ferromagnetic layers plays an important role in the ferroelectric and magnetic properties of these composite films. Compared to the strained Pb(Zr0.52Ti0.48)O3/ CoFe2O4/Pb(Zr0.52Ti0.48)O3 heterostructure, improved ferroelectric properties with an out-of-plane polarization (2P(r)) of 34.2 microC/cm2 and electric coercivity field of 158 kV/cm are obtained in the strain-free Pb(Zr0.52Ti0.48)O3/NiFe2O4/Pb(Zr0.52Ti0.48)O3 heterostructure. The ME measurement results not only show that the strain induced by lattice mismatch has great influence on the ME behavior, but also provide an understanding of the multilayers with full control over the interface structure at the atomic-scale.     

纳米CoFe_2O_4颗粒制备及性能研究

铁酸钴具有很多优良特性,应用广泛,其制备方法多为微乳液法,本文中用化学共沉淀法制备了纳米CoFe2O4颗粒。将Co2+和Fe3+的混合液加入沉淀剂溶液中,选用NaOH作为沉淀剂,探讨了温度、保温时间以及NaOH的加入方式对颗粒粒径的影响。用激光粒度分析仪、SEM、XRD、VSM测试了颗粒的大小、形貌、分散状况及饱和磁化强度。结果表明:在制备过程中,适当降低反应温度,缩短反应时间,快速加入NaOH可减小颗粒的粒径,且用此法制备出的CoFe2O4粉末饱和磁化强度为46.776A·m2/kg。     

Spindly cobalt ferrite nanocrystals: preparation, characterization and magnetic properties

In this paper we describe the preparation of homogeneously needle-shaped cobalt ferrite (CoFe(2)O(4)) nanocrystals on a large scale through the smooth decomposition of urea and the resulting co-precipitation of Co(2+) and Fe(3+) in oleic acid micelles. Furthermore, we found that other ferrite nanocrystals with a needle-like shape, such as zinc ferrite (ZnFe(2)O(4)) and nickel ferrite (NiFe(2)O(4)), can be prepared by the same process. Needle-shaped CoFe(2)O(4) nanocrystals dispersed in an aqueous solution containing oleic acid exhibit excellent stability and the formed colloid does not produce any precipitations after two months, which is of prime importance if these materials are applied in magnetic fluids. X-ray diffraction (XRD) measurements were used to characterize the phase and component of the co-precipitation products, and demonstrate that they are spinel ferrite with a cubic symmetry. Transmission electron microscopy (TEM) observation showed that all the nanocrystals present a needle-like shape with a 22?nm short axis and an aspect ratio of around?6. Varying the concentration of oleic acid did not bring about any obvious influence on the size distribution and shapes of CoFe(2)O(4). The magnetic properties of the needle-shaped CoFe(2)O(4) nanocrystals were evaluated by using a vibrating sample magnetometer (VSM), electron paramagnetic resonance (EPR), and a M?ssbauer spectrometer, and the results all demonstrated that CoFe(2)O(4) nanocrystals were superparamagnetic at room temperature.     

Controlling self-assembled perovskite-spinel nanostructures

We report a discovery that self-assembled perovskite-spinel nanostructures can be controlled simply by selecting single-crystal substrates with different orientations. In a model BiFeO(3)-CoFe(2)O(4) system, a (001) substrate results in rectangular-shaped CoFe(2)O(4) nanopillars in a BiFeO(3) matrix; in contrast, a (111) substrate leads to triangular-shaped BiFeO(3) nanopillars in a CoFe(2)O(4) matrix, irrespective of the volume fraction of the two phases. This dramatic reversal is attributed to the surface energy anisotropy as an intrinsic property of a crystal.     

Fabrication characterization and activity of a solar light driven photocatalyst: cerium doped TiO2 magnetic nanofibers

A novel magnetic separable composite photocatalytic nanofiber consisting of TiO2 as the major phase, CeO(2-y) and CoFe2O4 as the dopant phase was prepared by sol-gel method and electrospinning technique, and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectrum (UV-vis DRS) and vibrating sample magnetometer (VSM). The photocatalytic activity of the resultant CoFe2O4-TiO2 and CeO(2-y)/CoFe2O4-TiO2 nanofibers was evaluated by photodegradation of methylene blue (MB) in an aqueous solution under xenon lamp (the irradiation spectrum energy distribution is similar to sunlight) irradiation in a photochemical reactor. The results showed that the dopant of Ce could affect the absorbance ability and photo-response range. The sample containing 1.0 wt% CeO(2-y) exhibited the highest degradation with 35% for MB under simulate solar light irradiation. Furthermore, the as-synthesized composite photocatalytic nanofibers could be separated easily by an external magnetic field, thus it might hold potential for application in wastewater treatment.     

Preparation and photocatalytic properties of nanometer-sized magnetic TiO2/SiO2/CoFe2O4 composites

Magnetic TiO2/SiO2/CoFe2O4 nanoparticles (TiO2/SCFs) were prepared by a sol-gel process in a reverse microemulsion combined with solvent-thermal technique. TiO2/SCFs were characterized by Fourier transform infrared spectrometry, thermogravimetric analysis-differential scanning calorimetry, X-ray diffraction, Raman spectrometry, TEM, BET specific surface area measurement, and magnetic analysis. Structure analyses indicated that TiO2/SCFs presented a core-shell structure with TiO2 uniformly coating on SiO2/CoFe2O4 nanomagnets (SCFs) and typical ferromagnetic hysteresis. TiO2/SCFs showed larger specific surface area and better photocatalytic activities than TiO2 and TiO2/CoFe2O4 photocatalysts prepared by the same method. The doping interaction between TiO2 and CoFe2O4 reduced thanks to the inert SiO2 mesosphere.     

Stacks of functional oxide thin films patterned by micromolding

Stacks of up to five relief patterned functional oxide thin films were obtained by a low-cost and low-tech soft-lithographic patterning technique. Micromolding was used to pattern a film of a metal-organic precursor solution for Y-stabilized ZrO(2) (YSZO). Subsequent drying and pyrolysis yielded a line-patterned YSZO film. The process was repeated up to four times with a precursor solution for BaTiO(3) on top of the YSZO film, resulting in stacks of YSZO and BaTiO(3) lines with well-defined edges. This approach presents a step forward on the way to a versatile additive micropatterning technique with which simple multi-material device structures can be fabricated in a reliable, fast, and cost-effective manner.     

Low-temperature growth of nanostructured diamond films

Nanostructured diamond films are grown on a titanium alloy substrate using a two-step deposition process. The first step is performed at elevated temperature (820 degrees C) for 30 min using a H2/CH4/N2 gas mixture to grow a thin (approximately 600 nm) nanostructured diamond layer and to improve film adhesion. The remainder of the deposition involves growth at low temperature (< 600 degrees C) in a H2/CH4/O2 gas mixture. The continuation of the smooth nanostructured diamond film growth during low-temperature deposition is confirmed by in situ laser reflectance interferometry, atomic force microscopy, micro-Raman spectroscopy, and surface profilometry. Similar experiments performed without the initial nanostructured diamond layer resulted in poorly adhered films with a more crystalline appearance and a higher surface roughness. This low-temperature deposition of nanostructured diamond films on metals offers advantages in cases where high residual thermal stress leads to delamination at high temperatures.     

Feasibility of TEOS coated CoFe2O4 nanoparticles to a GMR biosensor agent for single molecular detection

Magnetic properties of 200 nm ferrimagnetic CoFe2O4 nanoparticles before and after coating with TEOS were explored and compared to soft ferrimagnetic MgFe2O4 nanoparticles (200 nm) to evaluate the feasibility as an in-vitro GMR SV (giant magnetoresistance spin-valve) biosensor agent for single molecular detection (SMD). It was found that the magnetic degradation (or variation) of TEOS coated CoFe2O4 and MgFe2O4 nanoparticles are dominantly affected by the chemical dispersion process, which is carried out in the oleic acid (OA), oleylamine (OL), or OA+OL surfactant, before starting major coating process. In addition, the TEOS coating thickness controlled by TEOS concentration and pH level in the buffer solution prominently influenced on the magnetic degradation of TEOS coated nanoparticles. According to the experimental analysis results, the magnetic degradation of TEOS coated nanoparticles is mainly attributed to the variation of particle dipole interaction caused by the degree of particle aggregation depending on TEOS coating process conditions. The TEOS coated CoFe2O4 nanoparticles exhibited a higher magnetic stability for a GMR biosensor agent, e.g., small variation of remnant magnetization, saturation magnetization and magnetic coercivity, than that of MgFe2O4 nanoparticles at the different coating process conditions. The physical and chemical analysis confirmed that this is primarily due to its higher magnetic anisotropy. The experimentally verified high biocompatibility as well as the stably maintained magnetic properties of TEOS coated CoFe2O4 nanoparticles demonstrate that CoFe2O4 nanoparticles can be considered as one of the promising ferrimagnetic nanoparticle sensor agent for an SMD GMR SV biosensor.     

RIE对巨磁电阻自旋阀磁性能的影响

对巨磁电阻自旋阀磁场传感器制作中的关键技术之一：自旋阀薄膜的反应离子刻蚀(RIE)工艺,进行了试验研究。自旋阀结构为：Ta(3．5nm)／Cu(0．7nm)／NiFe(4．5nm)／CoFe(1nm)／Cu(3nm)／CoFe(2nm)／Ru(0．7nm)／CoFe(2nm)／MnIr(8nm)／Ta(4nm),刻蚀气体为氢氯碳氟化合物(HCFC：Hydro—chloro—fluoro—carbon),气体流量为10．5seem,RF功率为180W,时间为27min。结果表明：RIE技术可以加工出理想的巨磁电阻自旋阀薄膜图形,且加工过程对自旋阀的磁性能影响不大,这些结果对于巨磁电阻自旋阀型集成磁传感器的批量制作具有积极意义。     

Nanoscale patterning of complex magnetic nanostructures by reduction with low-energy protons

Techniques that can produce patterns with nanoscale details on surfaces have a central role in the development of new electronic, optical and magnetic devices and systems. High-energy ion irradiation can produce nanoscale patterns on ferromagnetic films by destroying the structure of layers or interfaces, but this approach can damage the film and introduce unwanted defects. Moreover, ferromagnetic nanostructures that have been patterned by ion irradiation often interfere with unpatterned regions through exchange interactions, which results in a loss of control over magnetization switching. Here, we demonstrate that low-energy proton irradiation can pattern an array of 100-nm-wide single ferromagnetic domains by reducing [Co(3)O(4)/Pd](10) (a paramagnetic oxide) to produce [Co/Pd](10) (a ferromagnetic metal). Moreover, there are no exchange interactions in the final superlattice, and the ions have a minimal impact on the overall structure, so the interfaces between alternate layers of cobalt (which are 0.6?nm thick) and palladium (1.0?nm) remain intact. This allows the reduced [Co/Pd](10) superlattice to produce a perpendicular magnetic anisotropy that is stronger than that observed in the metallic [Co/Pd](10) superlattices we prepared for reference. We also demonstrate that our non-destructive approach can reduce CoFe(2)O(4) to metallic CoFe.     

The Pattern Growth of Carbon Nanotubes by Self-assembled Monolayers Techniques

The well controllable selective growth of carbon nanotubes (CNTs)on the desired area is an important issue for their future applications. In this study, a novel method for selective growth of CNTs was proposed by using the technology of self-assembly monolayers (SAMs) and the Fe-assisted CNTs growth. The Si wafers with the a ： Si/Si3N4 layer patterns were first prepared by low pressure chemical vapor deposition (LPCVD)and lithography techniques to act as the substrates for selective deposition of SAMs. The selectivity of SAMs from APTMS solution (N-(2-aminoethyl)-3-aminopropyltrimethoxsilane) is based on its greater reactivity of head group on a-Si than Si3N4 films. The areas of pattern with SAMs will first chelate the Fe3 ions by their diamine-terminated group. The Fe^3 ions were then consolidated to become Fe-hydroxides in sodium boron hydride solution to form the Fe-hydroxides pattern. Finally, the Fe-hydroxides pattern was pretreated in H plasma to become a well-distributed Fe nano-particles on the surface, and followed by CNTs deposition using Fe as catalyst in a microwave plasma-chemical vapor deposition (MP-CVD) system to become the CNTs pattern. The products in each processing step, including microstructures and lattice images of CNTs, were characterized by contact angle measurements, scanning electron microscopy (SEM), XPS, Auger spectroscopy, transmission electron microscopy (TEM) and high resolution TEM (HRTEM) deposition. The results show that the main process parameters include the surface activation process and its atmosphere, consolidation time and temperature, H plasma pretreatment. The function of each processing step will be discussed.     

The Pattern Growth of Carbon Nanotubes by Self-assembled Monolayers Techniques

The well controllable selective growth of carbon nanotubes (CNTs)on the desired area is an important issue for their future applications. In this study, a novel method for selective growth of CNTs was proposed by using the technology of self-assembly monolayers (SAMs) and the Fe-assisted CNTs growth. The Si wafers with the a: Si/Si3N4 layer patterns were first prepared by low pressure chemical vapor deposition (LPCVD)and lithography techniques to act as the substrates for selective deposition of SAMs. The selectivity of SAMs from APTMS solution (N-(2-aminoethyl)-3-aminopropyltrimethoxsilane) is based on its greater reactivity of head group on a-Si than Si3N4 films. The areas of pattern with SAMs will first chelate the Fe3 ions by their diamine-terminated group. The Fe3 ions were then consolidated to become Fe-hydroxides in sodium boron hydride solution to form the Fe-hydroxides pattern. Finally, the Fe-hydroxides pattern was pretreated in H plasma to become a well-distributed Fe nano-particles on the surface, and followed by CNTs deposition using Fe as catalyst in a microwave plasma-chemical vapor deposition (MP-CVD) system to become the CNTs pattern. The products in each processing step, including microstructures and lattice images of CNTs, were characterized by contact angle measurements, scanning electron microscopy(SEM), XPS, Auger spectroscopy, transmission electron microscopy (TEM) and high resolution TEM (HRTEM)deposition. The results show that the main process parameters include the surface activation process and its atmosphere, consolidation time and temperature, H plasma pretreatment. The function of each processing step will be discussed.     

Soft magnetic properties of hybrid ferromagnetic films with CoFe, NiFe, and NiFeCuMo layers

Two-layered ferromagnetic alloy films (NiFe and CoFe) with intermediate NiFeCuMo soft magnetic layers of different thicknesses were investigated to understand the relationship between coercivity and magnetization process by taking into account the strength of hard-axis saturation field. The thickness dependence of H_EC (easy-axis coercivity), H_HS (hard-axis saturation field), and χ (susceptibility) of the NiFeCuMo thin films in glass/Ta(5 nm)/[CoFe or NiFe(5 nm-t/2)]/NiFeCuMo(t = 0, 4, 6, 8, 10 nm)/[CoFe or NiFe(5 nm-t/2)]/Ta(5 nm) films prepared using the ion beam deposition method was determined. The magnetic properties (H_EC, H_HS, and χ) of the ferromagnetic CoFe, NiFe three-layers with an intermediate NiFeCuMo super-soft magnetic layer were strongly dependent on the thickness of the NiFeCuMo layer.     

Single step deposition method for nearly stoichiometric CuInSe2 thin films

This paper reports the production of high quality copper indium diselenide thin films using pulsed DC magnetron sputtering from a powder target. As-grown thin films consisted of pin-hole free, densely packed grains. X-ray diffraction showed that films were highly orientated in the (112) and/or (204)/(220) direction with no secondary phases present. The most surprising and exciting outcome of this study was that the as-grown films were of near stoichiometric composition, almost independent of the composition of the starting material. No additional steps or substrate heating were necessary to incorporate selenium and create single phase CuInSe₂. Electrical properties obtained by hot point probe and four point probe gave values of low resistivity and showed that the films were all p-type. The physical and structural properties of these films were analyzed using X-ray diffraction, scanning electron microscopy and atomic force microscopy. Resistivity measurements were carried out using the four point probe and hot probe methods. The single step deposition process can cut down the cost of the complex multi step processes involved in the traditional vacuum based deposition techniques.     

Ellipsometric and Rutherford Back scattering Spectrometry studies of SiO(X)N(Y) films elaborated by plasma-enhanced chemical vapour deposition technique

Silicon oxynitride (SiO(X)N(Y)) thin films were deposited by plasma-enhanced chemical vapour deposition technique (PECVD) from silane (SiH4), nitrous oxide (N2O), ammonia (NH3) and nitrogen (N2) mixture. Spectroscopic ellipsometry (SE), in the range of wavelengths 450-900 nm, was used to define the film thickness and therefore the deposition rate, as well as the refractive index as a function of the N2O gaseous flow. While considering the (Si3N4, SiO2, H2 or void) heterogeneous mixture, Maxwell Garnett (MG) theory allows to fit the SE measurements and to define the volume fraction of the different phases. Finally, Rutherford Backscattering Spectrometry (RBS) results showed that x = O/Si ratio increases gradually with increasing the N2O flow, allowing the correlation of the SiO(X)N(Y) films main parameters.     

平炉尘合成超细铁氧体催化性能研究

平炉尘提纯得到超细Fe2O3, 利用同晶型间的拓扑转化原理, 使平炉尘转化为超细铁氧体MnFe2O4、CoFe2O4催化剂, 并对催化剂进行了BET、XRD、H2-TPR、TEM和电导技术表征, 研究了其对丙烷氧化脱氢制丙烯反应的催化性能.实验结果表明由平炉尘转化得到的超细铁氧体CoFe2O4为p型半导体催化剂,对丙烷氧化脱氢制丙烯反应表现出优异的催化性能,当丙烷转化率在10%和20%时,丙烯的选择性分别为40.34%和35.23%.为资源综合利用及减少环境污染提供了新方法.     

Oscillatory-like relaxation behavior of light transmitted through ferrofluids

An oscillatory-like relaxation process in which there are two valleys in the T-t curve is observed when light is transmitted through binary ferrofluids composed of both ferrimagnetic CoFe(2)O(4) nanoparticles and paramagnetic p-MgFe(2)O(4) nanoparticles in the presence of a high magnetic field and through pure (single) CoFe(2)O(4) ferrofluids in a low magnetic field. This relaxation behavior is explained using a model of a bidispersed system based on both chained and unchained particles. In such a bidispersed system, the variation of the transmitted light results mainly from the motion of the chains, with the polarized unchained particles' gas producing the modulation effect. The oscillatory-like relaxation phenomenon depends on the features of both the chained and unchained particle systems. If either the particle volume fraction of chained particles or of unchained particles is very low, or the degree of polarization of the unchained particles gas is very weak, a simple nonlinear relaxation process, giving only a valley in the T-t curve, will appear for the transmitted light. For pure CoFe(2)O(4) ferrofluids, the number of chained and unchained particles does not remain constant under different values of the magnetic field. According to the analysis of the relaxation behavior of transmitted light, it is known that binary ferrofluids based on strong magnetic CoFe(2)O(4) particles and weak magnetic p-MgFe(2)O(4) particles can be much closer to the theoretical bidispersed system than single ferrofluids containing only strong magnetic particles.