Study of nanocrystalline VO2 thin films prepared by magnetron sputtering and post-oxidation

Nanocrystalline VO2 thin films were deposited onto glass slides by direct current magnetron sputtering and postoxidation. These films undergo semiconductor-metal transition at 70°C, accompanied by a resistance drop of two magnitude orders. The crystal structures and surface morphologies of the VO2 films were characterized by x-ray diffraction (XRD) and atomic force microscope (AFM), respectively. Results reveal that the average grain size of VO2 nanograins measured by XRD is smaller than those measured by AFM. In addition, Raman characterization indicates that stoichiometric VO2 and oxygen-rich VO2 phases coexist in the films, which is supported by x-ray photoelectron spectroscopy (XPS) results. Finally, the optical properties of the VO2 films in UV-visible range were also evaluated. The optical band gap corresponding to 2p-3d inter-band transition was deduced according to the transmission and reflection spectra. And the deduced value, E opt2p-3d = 1.81 eV, is in good agreement with that previously obtained by theoretical calculation.     

The ferroelectric and ferromagnetic characterization of CoFe2O4/Pb(Mg1/3Nb2/3)O3-PbTiO3 multilayered thin films

The multiferroic (PMN-PT/CFO)_n (n = 1,2) multilayered thin films have been prepared on SiO₂/Si(1 0 0) substrate with LNO as buffer layer via a rf magnetron sputtering method. The structure and surface morphology of multilayered thin films were determined by X-ray diffraction (XRD) and atom force microscopy (AFM), respectively. The smooth, dense and crack-free surface shows the excellent crystal quality with root-mean-square (RMS) roughness only 2.9 nm, and average grain size of CFO thin films on the surface is about 44 nm. The influence of the thin films thickness size, periodicity n and crystallite orientation on their properties including ferroelectric, ferromagnetic properties in the (PMN-PT/CFO)_n multilayered thin films were investigated. For multilayered thin films with n = 1 and n = 2, the remanent polarization Pr are 17.9 μC/cm² and 9.9 μC/cm²; the coercivity H_c are 1044 Oe and 660 Oe, respectively. In addition, the relative mechanism are also discussed.     

基片温度与氧分压对磁控溅射制备氧化钒薄膜的影响

采用磁控溅射工艺制备了V₂O₅薄膜.通过改变制备工艺中基片温度和氧分压两个条件，研究了薄膜的晶相组成、表观形貌以及氧化物中钒和氧元素的化合价态.当基片温度升高时，V₂O₅薄膜中颗粒结晶由细长针状转变为平行于基片的片状，V⁵⁺状态保持不变，但723 K时氧结合能向高键能态移动.氧分压较低时，薄膜表面有部分V⁴⁺态存在，但存在较多的高键能氧，此时薄膜中晶粒尺寸较小.随着氧分压的提 关键词： 氧化钒 磁控溅射 相变薄膜 X射线光电子能谱     

采用泵浦探测技术研究VO2薄膜相变特性

为研究纳秒激光作用下的VO₂薄膜的相变特性,采用泵浦-探测技术进行实验。首先,利用直流磁控溅射法制备VO₂薄膜,经X射线衍射（XRD）和原子力显微镜（AFM）分析表明样品质量较高。然后,测量VO₂薄膜在波长532 nm处的透过率随温度的变化情况,发现透过率随温度升高由32%上升到37%,与红外波段完全相反。在此基础上,选择1 064 nm泵浦光和532 nm探测光研究激光参数中能量密度和重频对VO₂薄膜相变特性的影响,同时结合ANSYS有限元软件对纳秒激光作用下VO₂薄膜的单脉冲温升情况进行分析。结果表明：VO₂薄膜在大于30 mJ/cm²的纳秒激光能量密度作用下,单脉冲温升可达相变温度,最小相变响应时间在14 ns左右。进一步提高纳秒激光能量密度,其相变响应时间略有增加但变化不大。在100 Hz以内改变纳秒激光重频对VO₂薄膜的相变响应基本无影响。VO₂薄膜的相变恢复时间随着纳秒激光能量密度的增大而呈自然指数增加,其变化过程与基底材料和纳秒激光参数密切相关。因此,可以通过优化VO₂薄膜基底材料参数提高其激光防护效果。     

Dielectric properties of continuous composition spreaded MgO-Ta2O5 thin films

The dielectric properties of MgO-Ta₂O₅ continuous composition spread (CCS) thin films were investigated. The MgO-Ta₂O₅ CCS thin films were deposited on Pt/Ti/SiO₂/Si substrates by off-Axis RF magnetron sputtering system, and then the films were annealed at 350 °C with rapid thermal annealing system in vacuum. The dielectric constant and loss of MgO-Ta₂O₅ CCS thin films were plotted via 1500 micron-step measuring. The specific point of Ta₂O₅-MgO CCS thin film (post annealed at 350 °C) showing superior dielectric properties of high dielectric constant (k ∼ 28) and low dielectric loss (tan δ < 0⋅004) at 1 MHz were found in the area of 3-5 mm apart from Ta₂O₅ side on the substrate. The cation's composition of thin film was Mg:Ta = 0.4:2 at%.     

蓝宝石衬底SnO2:Sb薄膜的制备及结构和光致发光性质

用射频磁控溅射法在蓝宝石(0001)衬底上制备出锑掺杂的氧化锡(SnO₂:Sb)薄膜.对制备薄膜的结构和发光性质进行了研究.制备样品为多晶薄膜，具有纯SnO₂的四方金红石结构.室温条件下对样品进行光致发光测量，在334 nm附近观测到紫外发射峰，并对SnO₂:Sb的光致发光机制进行了研究.     

氟化类金刚石薄膜的拉曼和红外光谱结构研究

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Effect of RF power and sputtering pressure on the structural and optical properties of TiO2 thin films prepared by RF magnetron sputtering

TiO₂ thin films were deposited onto quartz substrates by RF magnetron sputtering. The samples deposited at various RF powers and sputtering pressures and post annealed at 873 K, were characterized using X-ray diffraction (XRD), micro Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), UV-vis spectroscopy and photoluminescence (PL) spectroscopy. XRD spectrum indicates that the films are amorphous-like in nature. But micro-Raman analysis shows the presence of anatase phase in all the samples. At low sputtering pressure, increase in RF power favors the formation of rutile phase. Presence of oxygen defects, which can contribute to PL emission is evident in the XPS studies. Surface morphology is much affected by changes in sputtering pressure which is evident in the SEM images. A decrease in optical band gap from 3.65 to 3.58 eV is observed with increase in RF power whereas increase in sputtering pressure results in an increase in optical band gap from 3.58 to 3.75 eV. The blue shift of absorption edge in all the samples compared to that of solid anatase is attributed to quantum size effect. The very low value of extinction coefficient in the range 0.0544-0.1049 indicates the excellent optical quality of the samples. PL spectra of the films showed emissions in the UV and visible regions.     

不同衬底和CdCl2退火对磁控溅射CdS薄膜性能的影响

在科宁7059玻璃, FTO, ITO, AZO四种衬底上磁控溅射CdS薄膜, 并在CdCl₂+干燥空气380 ℃退火, 分别研究了不同衬底和退火工艺对CdS薄膜形貌、结构和光学性能的影响. 扫描电子显微镜形貌表明: 不同衬底原位溅射CdS薄膜的形貌不同, 退火后相应CdS薄膜的晶粒度和表面粗糙度明显增大. XRD衍射图谱表明: 不同衬底原位溅射和退火CdS薄膜均为六角相和立方相的混相结构, 退火前后科宁7059玻璃, FTO, AZO衬底上CdS薄膜有 H(002)/C(111) 最强衍射峰, ITO衬底原位溅射CdS薄膜没有明显的最强衍射峰, 退火后出现 H(002)/(111) 最强衍射峰. 紫外-可见分光光度计分析表明: AZO, FTO, ITO, 科宁7059玻璃衬底CdS薄膜的可见光平均透过率依次减小, 退火后相应衬底CdS薄膜的可见光平均透过率增大, 光学吸收系数降低; 退火显著增大了不同衬底CdS薄膜的光学带隙. 分析得出: 上述结果是由于不同衬底类型和退火工艺对CdS多晶薄膜的形貌、结构和带尾态掺杂浓度改变的结果. 关键词： CdS薄膜 磁控溅射 退火再结晶 带尾态     

Surface oxidation of vanadium dioxide films prepared by radio frequency magnetron sputtering

This paper reports that the thermochromic vanadium dioxide films were deposited on various transparent substrates by radio frequency magnetron sputtering, and then aged under circumstance for years. Samples were characterized with several different techniques such as x-ray diffraction, x-ray photoelectron spectroscopy, and Raman, when they were fresh from sputter chamber and aged after years, respectively, in order to determine their structure and composition. It finds that a small amount of sodium occurred on the surface of vanadium dioxide films, which was probably due to sodium ion diffusion from soda-lime glass when sputtering was performed at high substrate temperature. It also finds that aging for years significantly affected the nonstoichiometry of vanadium dioxide films, thus inducing much change in Raman modes.     

磁控溅射制备W掺杂VO2/FTO复合薄膜及其性能分析

为了获得相变温度低且热致变色性能优越的光学材料, 室温下在F:SnO₂ (FTO)导电玻璃基板表面沉积钨钒金属膜, 再经空气气氛下的热氧化处理, 制备了W掺杂VO₂/FTO复合薄膜, 利用X射线光电子能谱、X射线衍射和扫描电镜对薄膜的结构和表面形貌进行了分析. 结果表明: 高温热氧化处理过程中没有生成W, F, V混合氧化物, W以替换V原子的方式掺杂. 与采用相同工艺和条件制备的纯VO₂/FTO复合薄膜相比, W掺杂VO₂薄膜没有改变晶面取向, 仍具有(110)晶面择优取向, 相变温度下降到35 ℃左右, 热滞回线收窄到4 ℃, 高低温下的近红外光透过率变化量提高到28%. 薄膜的结晶程度明显提高, 表面变得平滑致密, 具有很好的一致性, 对光电薄膜器件的设计开发和工业化生产具有重要意义. 关键词： W掺杂 2')" href="#">VO₂ FTO导电玻璃 磁控溅射     

Structural and electrical properties of SrTiO3 thin films as insulator of metal-ferroelectric-insulator-semiconductor （MFIS） structures

SrTiO₃ (STO) thin films were deposited on p-Si(100) substrates at various substrate temperatures from 300℃ to 700℃ by radio frequency (RF) magnetron sputtering technique. Their structure and electrical properties were investigated. It was found that the transition from amorphous phase to polycrystalline phase occurred at the substrate temperatures 300--400℃. Their crystallinity became better when the substrate temperatures further increased. The dielectric and leakage current measurements were carried out by using the Si/STO/Pt metal--insulator--semiconductor (MIS) structures at room temperature. It was found that the fixed charge density decreased and both the interface trap density and the dielectric constant increased when the substrate temperatures were increased. The leakage current mechanisms for STO MIS structures with STO films prepared at 700℃ followed the space charge limited current (SCLC) under the low applied electric field and the Poole--Frenkel emission under the high one. In addition, the resistivity for films prepared at 700℃ was higher than 10¹¹\Omega \cdot cm under the voltage lower than 10V (corresponding to the electric field of 1.54\times 10³kV\cdotcm^-1). It suggested that the STO films prepared at 700℃ were suitable for acting as the insulator of metal--ferroelectric--insulator--semiconductor (MFIS) structures.     

Effect of Ta buffer and NiFe seed layers on pulsed-DC magnetron sputtered Ir20Mn80/Co90Fe10 exchange bias

A systematic investigation has been done on the correlation between texture, grain size evolution and magnetic properties in Ta/Ni₈₁Fe₁₉/Ir₂₀Mn₈₀/Co₉₀Fe₁₀/Ta exchange bias in dependence of Ta buffer and NiFe seed layer thickness in the range of 2-10 nm, deposited by pulsed DC magnetron sputtering technique. A strong dependence of 〈1 1 1〉 texture on the Ta/NiFe thicknesses was found, where the reducing and increasing texture was correlated with exchange bias field and unidirectional anisotropy energy constant at both NiFe/IrMn and IrMn/CoFe interfaces. However, a direct correlation between average grain size in IrMn and H_ex and H_c was not observed. L1₂ phase IrMn₃ could be formed by thickness optimization of Ta/NiFe layers by deposition at room temperature, for which the maximum exchange coupling parameters were achieved. We conclude finally that the coercivity is mainly influenced by texture induced interfacial effects at NiFe/IrMn/CoFe interfaces developing with Ta/NiFe thicknesses.     

纳米TiO_2薄膜的拉曼光谱

本文测量了纳米TiO2 薄膜的Raman散射谱 ,并用B1g模计算了不同厚度的纳米TiO2薄膜的粒度。结果表明 ,随着膜厚的增加 ,粒度也在增加 ,膜厚达到一定程度后 ,粒度的增加量减少     

Crystallization and electrical properties of V2O5 thin films prepared by RF sputtering

V₂O₅ thin films were prepared under various conditions by using reactive RF sputtering technique. The microstructure and electrical properties of the films are have been investigated. X-ray diffraction data revealed the films deposited at low O₂/Ar ratio are amorphous. The orthorhombic structure of film improved after post annealing at 873 K. The microstructure parameters (crystallite/domain size and macrostrain) have been evaluated by using a single order Voigt profile method. Using the two-point probe technique, the dark conductivity as a function of the condition parameters such as film thickness, oxygen content and temperature are discussed. It was also found that, the behaviour of ρd versus d was found to fit properly with the Fuchs-Sondheimer relation with the parameters: ρ_o = 2.14 × 10⁷ Ω cm and ?_o = 112 ± 2 nm. At high temperature, the electrical conductivity is dominated by grain boundaries, the values of activation energy and potential barrier height were 0.90 ± 0.02 eV and 0.92 ± 0.02 V, respectively.     

基于VO2薄膜非致冷红外探测器光电响应研究

VO₂薄膜是非致冷微测辐射热红外探测器热敏电阻材料.研究中应用微电子工艺制备了VO₂溅射薄膜红外探测器,在296K的环境中测试了该探测器在不同的直流偏置、光调制频率下对873K标准黑体源8—12μm红外辐射的光电响应以及器件的噪声电压,在10和30Hz的调制频率下其响应率分别大于17kV/W和接近10kV/W.该探测器实现了探测率D大于1.0×10⁸cm (Hz)^1/2/W,热时间常量为0.011s的8—12μm非致冷 关键词： 非致冷测辐射热探测器 红外探测器 二氧化钒 薄膜     

二氧化钒薄膜低温制备及其太赫兹调制特性研究

针对二氧化钒(VO2)薄膜在可调谐太赫兹功能器件中的应用,利用低温磁控溅射技术,在太赫兹和光学频段透明的BK7玻璃上制备出高质量的VO2薄膜.晶体结构和微观形貌分析显示薄膜为单相VO2单斜金红石结构,具有明显的(011)晶面择优取向,结构致密,表面平整.利用四探针技术和太赫兹时域光谱系统分析了薄膜的绝缘体-金属相变特性,发现相变过程中薄膜电阻率变化达到4个数量级,同时对太赫兹透射强度具有强烈的调制作用,调制深度高达89％.通过电学相变和太赫兹光学相变特性的对比研究,证实薄膜的电阻率突变主要与逾渗通路的形成有关,而太赫兹幅度的调制则来源于薄膜中载流子浓度的变化.该薄膜制备简单,成膜质量高,太赫兹调制性能优异,可应用于太赫兹开关和调制器等集成式太赫兹功能器件.     

Effect of O2 gas partial pressure on structures and dielectric characteristics of rf sputtered ZrO2 thin films

Amorphous and polycrystalline zirconium oxide thin films have been deposited by reactive rf magnetron sputtering in a mixed argon/oxygen or pure oxygen atmosphere with no intentional heating of the substrate. The films were characterized by high-resolution transmission electron microscopy (HR-TEM), atomic force microscopy (AFM), spectroscopic ellipsometry (SE), and capacitance versus voltage (C-V) measurements to investigate the variation of structure, surface morphology, thickness of SiO₂-like interfacial layer as well as dielectric characteristics with different oxygen partial pressures. The films deposited at low oxygen partial pressures (less than 15%) are amorphous and dense with a smooth surface. In contrast, the films prepared at an oxygen partial pressure higher than 73% are crystallized with the microstructure changing from the mixture of monoclinic and tetragonal phases to a single monoclinic structure. The film structural transition is believed to be consequences of decrease in the oxygen vacancy concentration in the film and of increase of the energetically neutral particles in the plasma due to an increased oxygen partial pressure. SE measurements showed that significant interfacial SiO₂ growth has taken place above approximately 51%. The best C-V results in terms of relative dielectric constant values are obtained for thin films prepared at an oxygen partial pressure of 15%.     

基于FTO/VO2/FTO结构的VO2薄膜电压诱导相变光调制特性

采用直流磁控溅射和后退火工艺在掺氟的SnO₂(FTO)导电玻璃衬底上制备VO₂薄膜, 研究了不同退火时间和不同比例的氮氧气氛对VO₂薄膜性能的影响, 对VO₂薄膜的结晶取向、表面形貌、表面元素的相对含量和透过率随波长变化进行了测试分析, 结果表明在最佳工艺条件下制备得到了组分相对单一的VO₂薄膜. 基于FTO/VO₂/FTO结构在VO₂薄膜两侧的透明导电膜上施加电压并达到阈值电压时, 观察到了明显的电流突变. 当接触面积为3 mm×3 mm时, 阈值电压为1.7 V, 阈值电压随接触面积的增大而增大. 与不加电压的情况相比, FTO/VO₂/FTO结构在电压作用下高低温的红外透过率差值可达28%, 经反复施加电压, 该结构仍保持性能稳定, 具有较强的电致调控能力.     

Effects of substrate temperature on the efficiency of hydrogen incorporation on the properties of Al-doped ZnO films

Al-doped ZnO (AZO) transparent conducting films were successfully prepared on glass substrates by RF magnetron sputtering at different substrate temperatures in Ar and H₂ + Ar sputtering ambient. The effects of substrate temperature on the effectiveness of hydrogen incorporation in Al-doped ZnO films were investigated. The microstructural, electrical and optical properties of AZO films were systematically analyzed by surface profiler, X-ray diffractometry, scanning electron microscope, four-point probe measurement and UV/vis spectrophotometer. The XRD patterns and SEM pictures indicate that the crystallinity of AZO thin films was markedly improved with hydrogen incorporation at low substrate temperature, while the improvement of crystallinity was not an obvious change at high substrate temperature. The results also indicate that hydrogen incorporation has the stronger effectiveness on the transparent conductive properties of AZO films with the substrate temperature decreasing. The resistivity of the films decreases, especially for lower substrate temperatures, due to the incorporation of hydrogen atoms. These results suggest that substrate temperature should be controlled to the lower level to effectively reduce resistivity without detriment to transmittance of AZO thin films when hydrogen is incorporated.