自组装功能膜诱导合成铁酸铋薄膜的研究

采用分子自组装技术在玻璃基片表面制备了十八烷基三氯硅烷自组装单层膜(OTS-SAMs),并在功能化的基板表面诱导生成铁酸铋(BiFeO3)薄膜,采用接触角测试仪、X射线衍射(XRD)、扫描电镜(SEM)和能谱分析(EDS)测试手段对OTS膜和BiFeO3薄膜进行了表征.实验结果表明,在SAMs功能化的玻璃基底上所制备的铁酸铋薄膜结晶良好,薄膜表面平整光滑,结构致密均一,而且形成BiFeO3多晶聚集体,多晶聚集体的大小在2μm左右.     

Nanoscale control of exchange bias with BiFeO3 thin films

We demonstrate a direct correlation between the domain structure of multiferroic BiFeO3 thin films and exchange bias of Co 0.9Fe 0.1/BiFeO3 heterostructures. Two distinct types of interactions - an enhancement of the coercive field ( exchange enhancement) and an enhancement of the coercive field combined with large shifts of the hysteresis loop ( exchange bias) - have been observed in these heterostructures, which depend directly on the type and crystallography of the nanoscale ( approximately 2 nm) domain walls in the BiFeO3 film. We show that the magnitude of the exchange bias interaction scales with the length of 109 degrees ferroelectric domain walls in the BiFeO 3 thin films which have been probed via piezoresponse force microscopy and X-ray magnetic circular dichroism.     

BiFeO3 films doped in the A or B sites: effects on the structural and morphological properties

Metal-Organic Chemical Vapor Deposition (MOCVD) has been applied to the fabrication of BiFeO3 films undoped and doped with Ba or Ti on SrTiO3 (100) and YSZ (100) substrates. The films have been deposited using a multi-metal source, consisting of the Bi(phenyl)3, Fe(tmhd)3 and Ba(hfa)2 tetraglyme or Ti(tmhd)2(O-iPr)2 (phenyl = -C6H5, H-tmhd = 2,2,6,6-tetramethyl-3,5-heptandione; O-iPr = iso-propoxide; H-hfa = 1,1,1,5,5,5-hexafluoro-2,4-pentanedione; tetraglyme = CH3O(CH2CH2O)4CH3) precursor mixture. The structural and morphological characterization of films has been carried out using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Chemical compositional studies have been performed by energy dispersive X-ray (EDX) analysis. Structural and morphological characterizations point to the formation of homogeneous and flat surfaces for both undoped and doped BiFeO3 films.     

Ferroelectric behavior in bismuth ferrite thin films of different thickness

The ferroelectric behavior of BiFeO(3) thin films is modified by changing the film thicknesses, where the BiFeO(3) thin films with different thicknesses were grown on SrRuO(3)/Pt/TiO(2)/SiO(2)/Si(100) substrates by radio frequency sputtering. The mixture of (110) and (111) orientations is induced for all BiFeO(3) thin films regardless of their thicknesses, together with the columnar structure and the dense microstructure. Their dielectric behavior is almost independent of the film thickness where all thin films have a low dielectric loss. A giant remanent polarization of 2P(r) ≈ 156.6-188.8 μC/cm(2) is induced for the BiFeO(3) thin films in the thickness range of 190-600 nm. As a result, it is an effective way to improve the ferroelectric behavior of the BiFeO(3) thin film by tailoring the film thickness.     

CSD法在亲水性的FTO基板上制备BiFeO3薄膜及其电性能的研究

利用化学溶液沉积法在亲水性的FTO基板上制备BiFeO3薄膜。利用XRD、FE-SEM、XPS、Agi-lent E4980A精密LCR仪及TF-Analyzer2000等分析手段对BiFeO3薄膜进行表征。结果表明,薄膜为纯相的结晶良好的多晶BiFeO3薄膜,由100～300nm的BiFeO3晶粒紧密的堆积而成,表面均匀平整。薄膜厚度为450nm。Fe的氧化态为Fe3+,并没有Fe2+出现。在10kHz时,介电常数和损耗分别为134和0.005。薄膜的剩余极化率为0.58μC/cm2,在0～250kV/cm的测试电场下漏导电流步伐保持在10-6 A/cm2以下。     

Influences of oxygen pressure on optical properties and interband electronic transitions in multiferroic bismuth ferrite nanocrystalline films grown by pulsed laser deposition

Bismuth ferrite (BiFeO(3)) nanocrystalline films with the crystalline size of 27-40 nm have been grown on c-sapphire substrates under various oxygen pressures of 1 × 10(-4) to 1 Pa by pulsed laser deposition. The X-ray diffraction spectra show that the films are polycrystalline and present the pure rhombohedral phase. It was found that the Raman-active phonon mode E(TO1) shifts towards a higher energy side from 74 to 76 cm(-1) with increasing oxygen pressure, indicating a larger tensile stress in the films deposited at higher oxygen pressure. The X-ray photoelectron spectroscopy analysis suggests that the concentrations of both Fe(2+) ions and oxygen vacancies in the BiFeO(3) films increase with decreasing oxygen pressure. Moreover, the dielectric functions in the photon energy range of 0.47-6.5 eV have been extracted by fitting the transmittance spectra with the Tauc-Lorentz dispersion model. From the transmittance spectra, the fundamental absorption edge is observed to present a redshift trend with increasing the temperature from 8 to 300 K. Note that the optical band gap (E(g)) decreases with increasing the temperature due to the electron-phonon interactions associated with the interatomic distance in the BiFeO(3) films. However, the E(g) decreases from 2.88 to 2.78 eV with decreasing oxygen pressure at 8 K, which can be attributed to the increment of oxygen vacancies leading to the formation of some impurity states between the valence and conduction band. It can be concluded that the oxygen pressure during the film fabrication has the significant effects on microstructure, optical properties, and electronic band structure modification of the BiFeO(3) films.     

Hydrothermal synthesis of perovskite bismuth ferrite crystallites with the help of NH4Cl

Bismuth ferrite nanopowders were hydrothermally synthesized with and without NH4Cl for comparison. The effects of NaOH concentration, reaction temperature and reaction time on the product phases and morphologies were studied in detail. Pure BiFeO3 was synthesized in a wide hydrothermal condition with the help of NH4Cl. Especially, it can be synthesized at low temperature of 140 degrees C. X-ray diffraction and Fourier transform infrared spectra revealed the BiFeO3 products had a perovskite structure. Scanning electron microscopy images showed that different BiFeO3 morphologies were formed under different hydrothermal conditions. NH4Cl played a key role in the BiFeO3 formation and BiFeO3 morphologies. Part BiFeO3 samples exhibited weak magnetic properties.     

Amorphous Terfenol-D films using nanosecond pulsed laser deposition

Thin films of Terfenol-D were produced by nanosecond pulsed laser deposition (PLD) at two fluences. Electron dispersive spectroscopy conducted using scanning electron and transmission electron microscopes showed that the film compositions were similar to that of the PLD target. Contrary to previous assertions that suggested that nanosecond PLD results in crystalline films, X-ray diffraction and transmission electron microscopy analysis showed that the films produced at both fluences were amorphous. Splatters present on the film had similar compositions to the overall film and were also amorphous. Magnetic measurements showed that the films had high saturation magnetization and magnetostriction, similar to high quality films produced using other physical vapor deposition methods.     

Dependence of ferroelectric and magnetic properties on measuring temperatures for polycrystalline BiFeO(3) films

A multiferroic BiFeO(3) film was fabricated on a Pt/Ti/SiO(3)/Si(100) substrate by a chemical solution deposition (CSD) method, and this was followed by postdeposition annealing at 923 K for 10 min in air. X-ray diffraction analysis indicated the formation of the polycrystalline single phase of the BiFeO(3) film. A high remanent polarization of 89 microC/cm(2) was observed at 90 K together with a relatively low electric coercive field of 0.32 MV/cm, although the ferroelectric hysteresis loops could not be observed at room temperature due to a high leakage current density. The temperature dependence of the ferroelectric hysteresis loops indicated that these hysteresis loops lose their shape above 165 K, and the nominal remanent polarization drastically increased due to the leakage current. Magnetic measurements indicated that the saturation magnetization was less than 1 emu/cm(3) at room temperature and increased to approximately 2 emu/cm(3) at 100 K, although the spontaneous magnetization could not appear. The magnetization curves of polycrystalline BiFeO3 film were nonlinear at both temperatures, which is different with BiFeO3 single crystal.     

One-dimensional multiferroic bismuth ferrite fibers obtained by electrospinning techniques

We report the fabrication of novel multiferroic nanostructured bismuth ferrite (BiFeO(3)) fibers using the sol-gel based electrospinning technique. Phase pure BiFeO(3) fibers were prepared by thermally annealing the electrospun BiFeO(3)/polyvinylpyrrolidone composite fibers in air for 1 h at 600?°C. The x-ray diffraction pattern of the fibers (BiFeO(3)) obtained showed that their crystalline structures were rhombohedral perovskite structures. Both scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images revealed that the BiFeO(3) fibers were composed of fine grained microstructures. The grains were self-assembled and self-organized to yield dense and continuous fibrous structures. The magnetic hysteresis loops of these nanostructured fibers displayed the expected ferromagnetic behavior, whereby a coercivity of ～ 250 Oe and a saturation magnetization of ～ 1.34 emu g(-1) were obtained. The ferroelectricity and ferroelectric domain structures of the fibers were confirmed using piezoresponse force microscopy (PFM). The piezoelectric hysteresis loops and polar domain switching behavior of the fibers were examined. Such multiferroic fibers are significant for electroactive applications and nano-scale devices.     

不同厚度BiFeO_3薄膜的光电性质

利用溶胶-凝胶法制备BiFeO_3靶材,通过射频磁控溅射法在玻璃衬底上制备不同厚度的BiFeO_3薄膜,并研究不同厚度对其微观结构、铁电性、漏电流特性及薄膜折射率和消光系数的的影响。结果表明,随着薄膜厚度的增加,铁电性变好,薄膜折射率和消光系数增大,当电压较低时(U1/22),Poole-Frenkel机制在漏电特性中起主导作用,当电压较高(1/U0.25)时,FN隧穿起主导作用;通过拟合图谱计算出不同沉积时间的薄膜厚度及表面层厚度,结果与原子力显微镜测的数值基本一致。     

Deposition potential dependence of composition, microstructure, and surface morphology of electrodeposited Ni–Cu alloy films

Composition, microstructure, and surface morphology of Ni–Cu alloy films electrodeposited at different deposition potentials have been investigated. The microstructural analysis carried out by using X-ray diffraction (XRD) confirmed that all Ni–Cu films are polycrystalline in nature and possess face-centered cubic structure. XRD analysis also revealed that the (111) peak of the Ni–Cu alloy films splits into two as Cu-rich and Ni-rich peaks and the peak intensities change depending on the deposition potential and hence the film composition. Compositional analysis of Ni–Cu films carried out by energy dispersive X-ray spectroscopy showed that Ni content within the films increases as the deposition potential becomes more negative. The morphological analysis performed by using a scanning electron microscopy and an atomic force microscopy revealed that the surface morphology changes significantly with applied deposition potential. Furthermore, a direct correlation is observed between the surface roughness and lattice strain.     

低碱浓度下水热合成铁酸铋粉体

以硝酸铋为铋源,硝酸铁或氯化铁为铁源,氨水为沉淀剂,在0．06mol／L氢氧化钠的低碱浓度下水热合成了纯相铁酸铋粉体,采用X射线衍射和红外光谱等分析表征,结果表明,所得产物均为钙钛矿结构铁酸铋粉体;SEM观测显示了随温度升高产物形貌的变化过程。以氯化铁为铁源制得粉体的光催化行为利用可见光分光光度计在亚甲基蓝最大吸收波长（664nm）处测试对应染料上清液吸光度值,表征染料脱色程度,结果表明,采用不同的铁源,所得铁酸铋粉体性能基本一致。     

Surface Morphology, Structural and Magnetic Properties of Electrodeposited NiFeCu/Cu Films

The magnetic and structural properties of the NiFeCu/Cu films electrodeposited on polycrystalline titanium (Ti) substrates and their characterizations were studied. The structural analysis by X-ray diffraction (XRD) has revealed that all films have face-centred cubic (FCC) structure. On the other hand, the XRD analysis showed that the degree of (111) texture is dependent on the Cu content within the film. The composition analysis was carried out by energy-dispersive X-ray spectroscopy (EDX). The result of EDX indicated that the Cu content within the film increases with increasing of non-magnetic Cu layer thickness. The hysteresis loops of the films measured by vibrating sample magnetometer (VSM) showed that all films have a small coercivity typical for soft magnetic materials. The surface morphological structure of the films was investigated by atomic force microscopy (AFM). AFM images indicated that all films have main grains (globular islands) and smaller secondary grains on the main grains with different sizes. The differences observed in the magnetic properties of the films were attributed to the Cu content within the films.     

AZ31镁合金表面磁控溅射Zr(Al,Ti)-SiN_x复合薄膜及其耐蚀性能

镁合金表面沉积薄膜可以提高其耐蚀性,但现有的几种沉积方法得到的膜疏松、与基体结合力差,影响了其耐腐蚀性能.为此,采用磁控溅射法在AZ31镁合金表面制备了Al,Zr,Ti膜及其与SiN_x的复合薄膜.用扫描电镜、X射线衍射、XPS研究了金属膜及其与SiNi_x复合薄膜的晶体结构、表面形貌和化学成分.结果表明:所制备的SiN_x薄膜为非晶态的富N膜;Zr膜的耐腐蚀性最好,Al膜的保护性最差;Zr-SiN_x复合薄膜比AZ31镁合金的腐蚀电流密度降低了3个数量级,Ti-SiN_x复合薄膜在阳极极化区出现了钝化.SiN_x复合薄膜的耐腐蚀性优于AZ31镁合金和单一金属膜.     

Sol-gel制备PLCT薄膜的结晶特性与电畴结构研究

运用sol-gel技术制备了(Pb,La,Ca)TiO3(简写为PLCT)铁电薄膜;利用XRD、SEM、AFM和EDAX分析了PLCT薄膜的结构、表面形貌和组分。XRD衍射结果表明,PLCT薄膜呈钙钛矿结构。随着退火时间的增加,PLCT薄膜的XRD衍射峰的强度也随之增加。SEM、AFM分析表明,PLCT铁电薄膜表面平整、致密、无裂缝。EDAX分析表明,PLCT薄膜的实际组分十分接近设计组分。利用PFM分析了PLCT薄膜的电畴结构,发现随着退火时间的增加,PLCT薄膜的电畴由细小圆点状逐渐增大并形成片状电畴。     

Adsorption-Controlled Growth of BiFeO3 by MBE and Integration with Wide Band Gap Semiconductors

BiFeO3 thin films have been deposited on (001) SrTiO3, (101) DyScO3, (011) DyScO3, (0001) AlGaN/GaN, and (0001) 6H-SiC single crystal substrates by reactive molecular beam epitaxy in an adsorption-controlled growth regime. This is achieved by supplying a bismuth over-pressure and utilizing the differential vapor pressures between bismuth oxides and BiFeO₃ to control stoichiometry in accordance with thermodynamic calculations. Four-circle x-ray diffraction and transmission electron microscopy reveal phase-pure, epitaxial films with rocking curve full width at half maximum values as narrow as 7.2 arc seconds (0.002°). Epitaxial growth of (0001)-oriented BiFeO3 thin films on (0001) GaN, including AlGaN HEMT structures, and (0001) SiC has been realized using intervening epitaxial (111) SrTiO₃ / (100) TiO₂ buffer layers. The epitaxial BiFeO3 thin films have 2 in-plane orientations: [1120] BiFeO>sub>3 || [1120] GaN (SiC) plus a twin variant related by a 180° in-plane rotation. This epitaxial integration of the ferroelectric with the highest known polarization, BiFeO3, with high bandgap semiconductors is an important step toward novel field-effect devices.     

Material and sensing properties of Pd-deposited WO3 thin films

The physicochemical and electrical properties of Pd-deposited WO3 thin films were investigated as a function of Pd thickness, annealing temperature, and operating temperature for application as a hydrogen gas sensor. WO3 thin films were deposited on an insulating material using a thermal evaporator. X-ray diffractometry (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) were used to evaluate the crystal structure, microstructure, surface roughness, and chemical property of the films, respectively. The deposited films grew into polycrystalline WO3 with a rhombohedral structure after annealing at 500 degrees C. Adding Pd had no effect on the crystallinity, but suppressed the growth of WO3 grains. The Pd was scattered as isolated small spherical particles of PdO2 on the WO3 thin film after annealing at 500 degrees C, while it agglomerated as irregular large particles or diffused into the WO3 after annealing at 600 degrees C. PdO2 reduction under H2 and reoxidation under air were dependent on both the Pd deposition thickness and annealing conditions. The WO3 thin film with a 2-nm-thick Pd deposit showed a good response and recovery to H2 gas at a 250 degrees C operating temperature.     

Spray pyrolyzed β-In2S3 thin films: Effect of postdeposition annealing

Indium sulfide thin films prepared using spray pyrolysis, with In/S ratio 2/3 in the solution, were annealed in vacuum at 300 and 400 °C. The effect of this treatment on properties of the films was studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, optical absorption, transmission and electrical measurements. Optical constants of the films were calculated using the envelope method. Annealing did not affect the optical properties of the film much, but the resistivity of the films showed a drastic decrease and the grain size increased. In₂S₃ thin films have potential use as buffer layer in photovoltaic heterojunction devices.     

Electrochromic performance of hybrid tungsten oxide films with multiwalled-CNT additions

In this study, tungsten oxide films were prepared by sol–gel technique. Various amounts of multiwalled carbon nanotubes (MWCNTs) were added during sol–gel process to obtain hybrid WO₃/MWCNT films. The original and hybrid films were characterized by thermogravimetric analysis, X-ray diffraction analysis, and scanning electron microscopy analysis, whereas the electrochromic performance was evaluated by measuring changes in the optical transmittance caused by potentiostatic charge–discharge intercalation. The influence on the structure and properties of tungsten oxide film due to MWCNT addition was also investigated. The results showed that all of the films were amorphous and exhibited porous microstructure. The electrochromic performance of pristine WO₃ film was improved by adding MWCNTs that served as a template for the growth of WO₃ and resulted in more porous microstructure. The hybrid tungsten oxide films with 0.1 wt.% MWCNT addition exhibited the best electrochromic performance.