Optical characterization of antimony-based bismuth-doped thin films with different annealing temperatures

Antimony-based bismuth-doped thin film,a new kind of super-resolution mask layer,is prepared by magnetron sputtering.The structures and optical constants of the thin films before and after annealing are examined in detail.The as-deposited film is mainly in an amorphous state.After annealing at 170-370℃,it is converted to the rhombohedral-type of structure.The extent of crystallization increased with the annealing temperature.When the thin film is annealed,its refractive index decreased in the most visible region,whereas the extinction coefficient and reflectivity are markedly increased.The results indicate that the optical parameters of the film strongly depend on its microstructure and the bonding of the atoms.     

退火对电子束热蒸发Al2O3薄膜性能影响的实验研究

 用电子束热蒸发方法镀制了Al₂O₃材料的单层膜,对它们在空气中进行了250~400 ℃的高温退火。对样品的透射率光谱曲线进行了测量,计算了样品的消光系数、折射率和截止波长。通过X射线衍射仪（XRD）测量分析了薄膜的微观结构,采用表面轮廓仪测量了样品的表面均方根粗糙度。结果发现随着退火温度的提高光学损耗下降,薄膜结构在退火温度为400 ℃时仍然为无定形态,样品的表面粗糙度随退火温度的升高而增加。引起光学损耗下降起主导作用的是吸收而不是散射,吸收损耗的下降主要是由于退火使材料吸收空气中的氧而进一步氧化,从而使薄膜材料的非化学计量比趋于正常。     

在不同衬底上制备的ZnO薄膜透射率的研究

采用反应磁控溅射在不同结构衬底上生长ZnO薄膜,通过X-ray衍射(XRD)及透射光谱来分析薄膜的成膜情况,并得出在Al₂O₃/AlN复合基上溅射沉积的ZnO薄膜比单独在AlN薄膜衬底的结晶质量好且透过率也较高。而经不同的快速热退火温度验证,发现在400 ℃时,ZnO薄膜的结晶化及在(002)方向上的择优取向达到最好,并在可见光范围内的平均透过率达到88%以上。当退火温度超过450 ℃时,温度过高改变了ZnO薄膜的内部结构,使其氧原子和锌原子发生了较大距离的位移,导致薄膜内部缺陷的增多,从而存在过多的晶界,增加了其薄膜的散射机制,使光的透过性变差,退火温度为500 ℃时,薄膜的平均透过率为80%。     

Effect of thermal annealing on the structure and microstructure of TiO2 thin films

Nanostructured TiO₂ thin films have been prepared through chemical route using sol-gel and spin coating techniques. The deposited films were annealed in the temperature range 400–1000°C for 1 h. The structure and microstructure of the annealed films were characterized by GAXRD, micro-Raman spectroscopy and AFM. The as-deposited TiO₂ thin films are found to be amorphous. Micro-Raman and GAXRD results confirm the presence of the anatase phase and absence of the rutile phase for films annealed up to 700°C. The diffraction pattern of the film annealed at 800 to 1000°C contains peaks of both anatase and rutile reflections. The intensity of all peaks in micro-Raman and GAXRD patterns increased and their width (FWHM) decreased with increasing annealing temperature, demonstrating the improvement in the crystallinity of the annealed films. Phase transformation at higher annealing temperature involves a competition among three events such as: grain growth of anatase phase, conversion of anatase to rutile and grain growth of rutile phase. AFM image of the asdeposited films and annealed films indicated exponential grain growth at higher temperature.      

Structural characterization of polycrystalline Ag-In-Se thin films deposited by e-beam technique

The Ag-In-Se thin films were deposited by e-beam evaporation of the Ag₃In₅Se₉ single crystal powder under high vacuum without intentional doping. Energy dispersive X-ray analysis (EDXA) showed the decreasing behavior of Se and Ag in the structure depending on the annealing. X-ray diffraction (XRD) analysis showed that as-grown films have amorphous structure while annealing the films under nitrogen environment at 200 °C transformed from the amorphous to polycrystalline structure. The crystallinity of the films improved as annealing temperature increases up to 400 °C by 100 °C-step. The polycrystalline films show mixed binary and ternary crystalline phases. Each phase was determined by comparing XRD patterns with complete data cards as Ag₃In₅Se₉, AgInSe₂, In₄Se₃, In₂Se₃, InSe, Se₆ and Se. The existence of Se segregation was supported by the formation of Se aggregates in crystalline phases of Se₆ and Se. The X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) analysis have been carried out in order to obtain detailed information about the atomic composition, chemical states and morphology of the thin film surface. The decomposition of In 4d, Se 3d and Ag 3d photoelectron peaks revealed the existence of In-In, In-Se, In-Ag, Se-Se and Ag-Ag bondings in as-grown thin films. After annealing the thin films at different temperatures, the concentration of In-Se and In-Ag bonds decreases significantly, which results in an In-rich, but Ag- and Se-deficient thin film structure. The roughness of the film surface as a result of application of post-annealing in between 200 and 400 °C monitored by AFM technique was observed to change from 1.81 to 22.89 nm.     

Phase transformation of nanostructured titanium dioxide thin films grown by sol–gel method

Nanostructured TiO₂ thin films were deposited on quartz glass at room temperature by sol–gel dip coating method. The effects of annealing temperature between 200^∘C to 1100^∘C were investigated on the structural, morphological, and optical properties of these films. The X-ray diffraction results showed that nanostructured TiO₂ thin film annealed at between 200^∘C to 600^∘C was amorphous transformed into the anatase phase at 700^∘C, and further into rutile phase at 1000^∘C. The crystallite size of TiO₂ thin films was increased with increasing annealing temperature. From atomic force microscopy images it was confirmed that the microstructure of annealed thin films changed from column to nubbly. Besides, surface roughness of the thin films increases from 1.82 to 5.20 nm, and at the same time, average grain size as well grows up from about 39 to 313 nm with increase of the annealing temperature. The transmittance of the thin films annealed at 1000 and 1100^∘C was reduced significantly in the wavelength range of about 300–700 nm due to the change of crystallite phase. Refractive index and optical high dielectric constant of the n-TiO₂ thin films were increased with increasing annealing temperature, and the film thickness and the optical band gap of nanostructured TiO₂ thin films were decreased.     

The microstructure investigation of GeTi thin film used for non-volatile memory

GeTi thin film has been found to have the reversible resistance switching property in our previous work. In this paper, the microstructure of this material with a given composition was investigated. The film was synthesized by magnetron sputtering and treated by the rapid temperature process. The results indicate a coexist status of amorphous and polycrystalline states in the as-deposited GeTi film, and the grains in the film are extremely fine. Furthermore, not until the film annealed at 600 °C, can the polycrystalline state be detected by X-ray diffraction. Based on the morphological analysis, the sputtered GeTi has the column growth tendency, and the column structure vanishes with the temperature increasing. The microstructure and thermal property analysis indicate that GeTi does not undergo evident phase change process during the annealing process, which makes the switching mechanism of GeTi different from that of chalcogenide memory material, the most widely used phase change memory material.     

Determination of photocatalytic activity in amorphous and crystalline titanium oxide films prepared using plasma-enhanced chemical vapor deposition

Hydro-oxygenated amorphous titanium oxide (a-TiO_x:OH) films were prepared by plasma-enhanced chemical vapor deposition (PECVD) using precursors of titanium tetraisopropoxide (TTIP) and oxygen. The influences of chemical states and crystal quality on the photocatalytic activity were systematically investigated in the as-deposited and post-annealed films. The degree of the photocatalytic activity was deeply correlated with the porosity related to the hydroxyl (OH) groups in the as-deposited amorphous film. The crystallized anatase structures was observed from the 200 °C-deposited a-TiO_x:OH film after a post-annealing treatment at 400 °C. The photocatalytic activity related to the film with anatase structure was markedly superior to that of an amorphous film with porous structures. The larger the crystal size of the anatase structure, the higher the photocatalytic activity obtained. At elevated annealed temperatures, the inferior anatase structure due to the crystalline transformation led to a low photocatalytic activity. It was concluded that the photocatalytic activity of an amorphous TiO_x film prepared using PECVD was determined by the porosity originating from the functional OH groups in the film, whereas the crystalline quality of anatase phase in the annealed poly-TiO_x film was crucial to the photocatalytic activity.     

直流磁控反应溅射法制备的钒氧化物薄膜及其光谱研究

用直流磁控反应溅射法和不同基底温度下在玻璃底上沉积微纳结构的氧化钒薄膜,通过X射线衍射、电子扫描显微镜、UV-Vis透射、红外和拉曼光谱研究了薄膜的结构特性.在低温下制备的薄膜表现出高的光学透过特性,在基底温度低于200℃下制备的薄膜具有无定形结构,而在基底温度高于200℃时制备的薄膜具有多晶结构.薄膜的光学参数使用经...     

Effects of annealing temperature and method on structural and optical properties of TiO2 films prepared by RF magnetron sputtering at room temperature

TiO₂ thin film was deposited on non-heated Si(1 0 0) substrate by RF magnetron sputtering. The as-deposited films were annealed by a conventional thermal annealing (CTA) and rapid thermal annealing (RTA) at 700 and 800 °C, and the effects of annealing temperature and method on optical properties of studied films were investigated by measuring the optical band gaps and FT-IR spectra. And we also compared the XRD patterns of the studied samples. The as-deposited film showed a mixed structure of anatase and brookite. Only rutile structures were found in samples annealed above 800 °C by CTA, while there are no special peaks except the weak brookite B(2 3 2) peak for the sample annealed at (or above) 800 °C by RTA. FT-IR spectra show the broad peaks due to Ti-O vibration mode in the range of 590-620 cm⁻¹ for the as-deposited film as well as samples annealed by both annealing methods at 700 °C. The studied samples all had the peaks from Si-O vibration mode, which seemed to be due to the reaction between TiO₂ and Si substrate, and the intensities of these peaks increased with increasing of annealing temperature. The optical band gap of the as-deposited film was 3.29 eV but it varied from 3.39 to 3.43 eV as the annealing temperature increased from 700 to 800 °C in the samples annealed by CTA. However, it varied from 3.38 to 3.32 eV as the annealing temperature increased from 700 to 800 °C by RTA.     

Characteristics of electron beam evaporated nanocrystalline SnO2 thin films annealed in air

Tin oxide (SnO₂) thin films (about 200 nm thick) have been deposited by electron beam evaporation followed by annealing in air at 350-550 °C for two hours. Optical, electrical and structural properties were studied as a function of annealing temperature. The as-deposited film is amorphous, while all other annealed films are crystalline (having tetragonal structure). XRD suggest that the films are composed of nanoparticles of 5-10 nm. Raman analysis and optical measurements suggest quantum confinement effects that are enhanced with annealing temperature. For instance, Raman peaks of the as-deposited films are blue-shifted as compared to those for bulk SnO₂. Blue shift becomes more pronounced with annealing temperature. Optical band gap energy of amorphous SnO₂ film is 3.61 eV, which increases to about 4.22 eV after crystallization. Two orders of magnitude decrease in resistivity is observed after annealing at 350-400 °C due to structural ordering and crystallization. The resistivity, however, increases slightly with annealing temperature above 400 °C, possibly due to improvement in stoichiometry and associated decrease in charge carrier density.     

Effect of annealing temperature on the optical constants of zinc oxide films

In this paper, the effect of annealing temperature on optical constants was studied. The ZnO films were deposited on microscopic glass substrates using the sol-gel method for various annealing temperatures. The deposited zinc oxide (ZnO) films were characterized by an X-ray diffractometer (XRD), a spectrophotometer and scanning electron microscopy (SEM). The transmittance spectra recorded through the spectrophotometer exhibits 90% transmittance. The XRD spectra showed polycrystalline nature of ZnO film. Optical constants were determined through transmittance spectra using an envelope method. It was found that there was a significant effect of annealing temperature on the refractive index and extinction coefficient of deposited ZnO films. In this experiment, the optimum refractive index value of 1.97 was obtained at 350 °C annealing temperature at visible (vis) wavelength. The optical energy gap was found to be of ∼3.2 eV for all the samples. The top view of SEM showed the ZnO grain growth on the glass substrates.     

不锈钢丝网上薄膜TiO2光催化剂的Raman光谱研究

用Raman光谱方法来研究用Sol Gel法负载于金属丝网的薄膜TiO2 光催化剂的物相结构、厚度以及粒径大小。研究结果显示 ,薄膜达到一定厚度能够阻止基底Fe元素向薄膜表层的扩散 ;在 4 0 0℃下灼烧制得的薄膜TiO2 光催化剂具有锐钛矿晶型 ,而高于 4 0 0℃时 ,将出现金红石相TiO2 ;锐钛矿晶型TiO2 的Raman特征峰产生偏移 ,表明薄膜粒径的变化 ,通过计算表明 ,薄膜TiO2 的粒径为 10nm左右 ,TEM的分析结果也与之一致。     

退火对电子束热蒸发Al2O3薄膜性能影响的实验研究

用电子束热蒸发方法镀制了Al2O3材料的单层膜,对它们在空气中进行了250~400 ℃的高温退火。对样品的透射率光谱曲线进行了测量,计算了样品的消光系数、折射率和截止波长。通过X射线衍射仪（XRD）测量分析了薄膜的微观结构,采用表面轮廓仪测量了样品的表面均方根粗糙度。结果发现随着退火温度的提高光学损耗下降,薄膜结构在退火温度为400 ℃时仍然为无定形态,样品的表面粗糙度随退火温度的升高而增加。引起光学损耗下降起主导作用的是吸收而不是散射,吸收损耗的下降主要是由于退火使材料吸收空气中的氧而进一步氧化,从而使薄膜材料的非化学计量比趋于正常。     

Structural and optical properties of low temperature synthesized Nanostructured BiFeO3 thin films

Nanostructured bismuth ferrite (BiFeO₃) thin films were deposited on glass substrate by the sol-gel process. The as-fired film at 250 °C was found to be amorphous crystallizing to pure rhombohedral phase after annealing at 450 °C for 2 h in air. The XRD pattern shows that the sample is polycrystalline in nature. The average grain size of the film calculated from the XRD data was found to be 16 nm. The as-fired film show high transmittance that decreases after crystallization. The absorption edge of the films was found to be sharper and shifting towards the lower energy as the annealing temperature increases. The optical energy band gaps of the amorphous and crystalline films were found to be 2.63 and 2.31 eV, respectively. The refractive indices of the amorphous and crystalline films were 2.05 and 2.26, respectively.     

Anatase type titania nanotube arrays direct fabricated by anodization without annealing

In this paper, anatase type titania nanotube arrays were direct fabricated by anodization in dimethyl sulfoxide electrolyte containing 1 wt% HF solution at above 50 °C without subsequently annealing. The length of the nanotubes decreases with increasing anodization temperature from about approximately 15 μm at 40 °C to approximately 4.5 μm at 60 °C. High resolution transmission electron microscope images and selected area electron diffraction pattern confirm the polycrystalline anatase specimen consisting of many nanocrystals with a random orientation.     

Optical and electrical properties of BaSnO3 and In2O3 mixed transparent conductive films deposited by filtered cathodic vacuum arc technique at room temperature

For the crystalline temperature of BaSnO$_{3}$ (BTO) was above 650 ℃, the transparent conductive BTO-based films were always deposited above this temperature on epitaxy substrates by pulsed laser deposition or molecular beam epitaxy till now which limited there application in low temperature device process. In the article, the microstructure, optical and electrical of BTO and In$_{2}$O$_{3}$ mixed transparent conductive BaInSnO$_x$ (BITO) film deposited by filtered cathodic vacuum arc technique (FCVA) on glass substrate at room temperature were firstly reported. The BITO film with thickness of 300 nm had mainly In$_{2}$O$_{3}$ polycrystalline phase, and minor polycrystalline BTO phase with (001), (011), (111), (002), (222) crystal faces which were first deposited at room temperature on amorphous glass. The transmittance was 70%-80% in the visible light region with linear refractive index of 1.94 and extinction coefficient of 0.004 at 550-nm wavelength. The basic optical properties included the real and imaginary parts, high frequency dielectric constants, the absorption coefficient, the Urbach energy, the indirect and direct band gaps, the oscillator and dispersion energies, the static refractive index and dielectric constant, the average oscillator wavelength, oscillator length strength, the linear and the third-order nonlinear optical susceptibilities, and the nonlinear refractive index were all calculated. The film was the n-type conductor with sheet resistance of 704.7 $\Omega /\Box $, resistivity of 0.02 $\Omega \cdot$cm, mobility of 18.9 cm$^{2}$/V$\cdot$s, and carrier electron concentration of $1.6\times 10^{19}$ cm$^{-3}$ at room temperature. The results suggested that the BITO film deposited by FCVA had potential application in transparent conductive films-based low temperature device process.     

纳米TiO2薄膜的低温等离子体制备技术

以四氯化钛为源物质,氩气为载气,氧气为反应气体,利用低温等离子体增强化学气相沉积在硅基表面制备出了TiO2薄膜。使用场发射扫描电子显微镜、X射线衍射仪等检测分析表征TiO2薄膜的性能与性质,并探讨了工艺条件如基片材料、沉积时间和基片温度对薄膜性能的影响。结果表明：制备的薄膜表面光滑均匀,结构致密,最小晶粒尺寸约15 nm;薄膜的晶型主要依赖于沉积温度,低于300 ℃沉积的薄膜是无定形的,300 ℃之上沉积的薄膜是锐钛矿结构。     

Measurement of gold surface self-diffusion by scanning tunneling microscopy

Measurement of gold surface self-diffusion by the method of surface profile decay, using a scanning tunneling microscope (STM) have been done on a polycrystalline gold film deposited on a glass substrate. The peak-to-peak surface roughness was measured as a function of annealing time after annealing at 170 °C with a special pan-cake furnace in the STM. The gold surface diffusion coefficient at 170 °C can then be extracted from these measurements.     

纳米多孔SiO2薄膜的制备与红外光谱研究

以正硅酸乙酯为原料,采用溶胶-凝胶法,结合旋转涂胶、超临界干燥工艺在硅片上制备了纳米多孔SiO2薄膜。XRD表明薄膜为无定形态;SEM显示薄膜具有多孔网络结构,其SiO2粒子直径为10~20nm。利用FTIR研究了薄膜的结构,纳米多孔SiO2薄膜含有Si—O—Si与Si—OR结构,呈疏水性;该SiO2薄膜热处理后因含有Si—OH基团而呈吸水性;用三甲基氯硅烷对热处理SiO2薄膜进行修饰可使其呈疏水性,修饰后的薄膜在N2中温度不高于450℃可保持其疏水性与多孔结构。