退火温度对TiO2薄膜结构、组分和光学性能的影响

利用射频磁控溅射,在硅和石英基底上制备了厚度为150 nm的TiO2薄膜.利用X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)、紫外可见分光光度计(UV-vis)和光致发光谱(PL)等多种测试分析技术,研究退火温度对TiO2薄膜结构、组分及光学性能的影响.研究结果表明,未退火薄膜为无定型结构;随着退火温度的升高薄膜的金红石相含量逐渐增加,并沿(110)晶面择优取向.能隙也由退火前的3.03 eV逐渐增加到900℃退火后的3.18eV.对于TiO2薄膜催化活性最优的退火温度应为800℃.     

CuAlSe2光伏吸收层薄膜的制备

用同族元素Al和Fe取代CulnGaSe2薄膜中的In和Ga元素.采用粉末冶金工艺制备CuAlSe2和CuAlSe2∶Fe光伏吸收层薄膜.依次对薄膜样品进行了表面形貌、化学成分、薄膜厚度、晶体结构和光学特性测试分析.结果表明,退火温度为450℃、500℃、550℃时薄膜的生长特性较好,薄膜较为致密,结晶度较高.薄膜主要为黄铜矿结构,并沿(112)晶相择优生长.CuAlSe2薄膜和CuAlSe2∶Fe薄膜样品的光学吸收系数达到105 cm-1,且随着掺Fe比例增加而增加.未掺杂的薄膜的光学带隙约为1.6 eV,掺Fe薄膜的禁带宽度接近1.8 eV.     

原子层沉积与磁控溅射法制备TiO2薄膜性能对比研究

分别采用原子层沉积(ALD)和磁控溅射法(MS)在Si和石英衬底上制备TiO2薄膜,并进行退火处理.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、原子力显微镜(AFM)和紫外分光光度计对这两种方法制备薄膜的晶型结构、表面形貌和光学特性进行分析对比.结果显示,对于沉积态TiO2薄膜,ALD-TiO2和MS-TiO2未能检测到TiO2衍射峰.ALD-TiO2为颗粒膜,其表面粗糙,颗粒尺寸大;MS-TiO2薄膜表面平整.经退火后,两种方法制备的TiO2薄膜能检测到锐钛矿A(101)衍射峰,但结晶质量不高.受薄膜表面形貌和晶型结构等因素影响,退火前后ALD-TiO2透过率与MS-TiO2透过率变化不一致.对于沉积态和退火态薄膜的禁带宽度,ALD-TiO2分别为3.8eV和3.7 eV,吸收边带发生红移,MS-TiO2分别为3.74 eV和3.84 eV,吸收边带发生蓝移.     

镓掺杂对二氧化钛薄膜光吸收性能的影响

通过向TiO2粉体中加入质量分数为1;～15;的Ga2O3粉末,制备了Ga掺杂的TiO2陶瓷靶,并采用脉冲激光沉积法(PLD)用陶瓷靶制备出TiO2薄膜,将薄膜于800～1000℃下退火.对薄膜结构和光学性质的研究表明1000℃退火条件下浓度为1; Ga2O3掺杂能有效将金红石相TiO2的禁带宽度减小至2.62 eV,使其吸收边红移动至470 nm.     

硅薄膜晶化机制的光学分析

采用拉曼光谱和分光光度计等测试手段,对快速光热过程(RTP)和常规炉过程(CFP)退火后的硅薄膜结构性能和光学性能进行了研究。用Avrami-Mehl-Johnson和Monte Carlo晶体生长模型和黑体辐射理论分析得出,RTP法退火温度低、速度快的原因,是RTP中不仅存在“光量子效应”,而且还存在“光热相长效应”。由光学带隙的计算得知,RTP退火法可使带隙约为1.7eV的非晶硅薄膜变为带隙约为1.28eV的微晶硅薄膜,说明RTP退火达到了较好的结晶效果。     

Si/Ti原子比对TiO2-SiO2复合薄膜亲水性能与摩擦磨损性能的影响

采用直流(DC)反应磁控溅射法在玻璃上制备了不同Si/Ti原子比的TiO2-SiO2复合薄膜.使用X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)、X射线光电子能谱仪(XPS)、紫外可见分光光度计、CA-XP150型接触角仪、UMT-2型多功能微摩擦仪,研究了不同Si/Ti原子比的TiO2-SiO2复合薄膜微观结构、表面形貌、亲水性能和摩擦磨损性能.结果表明,所制备的纯TiO2薄膜具有锐钛矿结构,其平均晶粒尺寸为11 nm,TiO2-SiO2复合薄膜呈现非晶结构,其粒子尺寸相对减小;随着Si/Ti原子比的增大,薄膜在可见光区的平均透过率从76.6; 增加到84.3;.当复合薄膜中Si/Ti原子比为1:2时,薄膜的摩擦系数为0.11,薄膜具有最佳的亲水性能;在紫外光照射2 h后水接触角降到3.0°;在黑暗中放置30 h后水接触角略增加到7.7°.     

单晶硅外延生长晶化硅薄膜的研究

采用P型单晶硅片为衬底,并经混合酸溶液腐蚀抛光、清洗后,利用射频磁控溅射镀膜系统在其表面制备非晶硅薄膜;再结合快速光热退火工艺,于N2气氛下480℃退火30 min,得到晶化硅薄膜;利用光学金相显微镜、XRD衍射仪和拉曼散射光谱(Raman)仪对单晶硅衬底和晶化硅薄膜进行结构和性能表征.研究了混合酸溶液对单晶硅表面腐蚀效果、籽晶诱导外延生长晶化硅薄膜的物相结构和薄膜带隙.结果表明:采用混合酸溶液腐蚀后得到表面平整、光滑的单晶硅衬底;非晶硅薄膜经过快速退火后受籽晶诱导生成晶化硅薄膜,其晶相沿单晶硅衬底取向择优生长;随着非晶硅薄膜厚度从80 nm增加到280 nm,晶化后硅薄膜的表面粗糙度逐渐减小,晶化率从90.0;逐渐降低到37.0;;晶粒尺寸从6.65 nm逐渐减小到1.71 nm;带隙从1.18 eV逐渐升高到1.52 eV.     

脉冲偏压及退火处理对电弧离子镀N掺杂TiO_2薄膜结构和性能的影响

本文利用电弧离子镀技术,施加不同脉冲偏压,在玻璃基体上沉积了N掺杂TiO2薄膜。研究了基体偏压和热处理对薄膜结构、光吸收性能及光催化降解甲基橙的反应活性。结果表明:随脉冲偏压的提高,薄膜相结构先由锐钛矿向非晶转变然后向锐钛矿和金红石的混合相转变,吸收边先红移后蓝移,透明度先下降后升高。400℃下退火4 h,薄膜结晶形貌更加明显,吸收边进一步红移,透明度提高。原始薄膜和退火后的薄膜都具有高的紫外光催化活性。可见光下经过退火的-300V偏压下制备的薄膜具有最好的光催化活性。     

溶胶-凝胶法制备高Mg含量Zn1-x MgxO薄膜

采用溶胶-凝胶法在石英玻璃基板上制备了ZB1-xMgxO薄膜,研究退火温度对高Mg含量Zn0.5Mg0.5O薄膜的相组成、相偏析及紫外-可见透过光谱中吸收边移动的影响,当退火温度≤500℃时,Zn0.5Mg0.5O薄膜未发生相偏析现象,且400℃退火处理制备的Zn0.5Mg0.5O薄膜的紫外-可见透过光谱中吸收边蓝移最大.因此,对于高Mg含量Zn0.5Mg0.5O薄膜,退火温度是影响Mg2+在ZnO中固溶度的关键因素,且400℃是其理想的退火温度.在此条件下研究了不同Mg含量对Zn1-xMgO(x=0～0.8)薄膜带隙调节的影响,随着Mg含量的增加,其紫外-可见透过光谱中紫外光区吸收边呈现规律性蓝移,光学带隙值Eg从纯ZnO的3.3 eV调节至4.2 eV.     

可见光响应(001)晶面纳米TiO2光催化剂的制备及性能研究

以钛酸丁酯为钛源,氢氟酸为形貌控制剂,采用水热法合成了具有高表面能(001)晶面的锐钛矿相TiO2纳米材料.利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)及紫外-可见漫反射光谱分析(UV-vis)对样品的形貌、结构和谱学性能进行表征,并以甲基橙溶液为目标污染物,研究其光催化性能和最佳制备条件.结果表明,以氢氟酸为形貌控制剂时,可制备锐钛矿相(001)晶面纳米TiO2纳米材料,能拓宽TiO2体系光响应范围,并具有较高的光催化性能;当反应温度为180.℃、时间为24 h、F/Ti摩尔比为1.5时,样品对甲基橙溶液光催化降解率最高,在紫外光照射条件下1h内降解率可达99.08;,其可见光降解率为66.79;.     

Effect of annealing on the properties of chemical bath deposited nanorods of CdSe thin films

Cadmium selenide (CdSe) thin films have been deposited by chemical bath deposition (CBD) on a glass substrate and they are annealed at 450 °C for 1 h. Scanning electron microscopic (SEM) image of as‐deposited CdSe shows the spherical shaped grains distributed over entire glass substrate. When it is annealed at 450 °C, clusters of nano‐rods with star shaped grains are formed. The X‐ray diffraction (XRD) study of the as‐deposited films exhibits a polycrystalline nature and it undergoes a structural phase transition from the metastable cubic to the stable hexagonal phase when annealed at 450 °C. Optical band gap of as‐deposited films (2.0 eV) has a blue shift with respect to the bulk value (1.7 eV) due to quantum confinement. The band gap energies of the films are decreased from 2.0 eV to 1.9 eV due to annealing at the temperature of 450 °C. The electrical resistivity, Hall mobility and carrier concentration of as‐deposited and annealed films are determined.     

Role of annealing environment and partial pressure on structure and optical performance of TiO2 thin films fabricated by rf sputter method

Influences of the different annealing ambient (in air, 1 bar, 2 bar, 3 bar and 4 bar oxygen partial pressure) on the titanium dioxide (TiO₂) thin films deposited on soda lime glass by standard radio frequency (rf) magnetron reactive sputtering method at 100 watt were investigated by means of X–ray diffractometer (XRD), ultra violet spectrometer (UV–vis), and Scanning Electron Microscopy (SEM). It was found that either optical properties or energy band gaps of the films enhanced with increase in the oxygen partial pressure up to 3 bar. The energy band gaps of the films (except for the film annealed in 4 bar oxygen partial pressure) became larger than the film annealed in atmospheric pressure. The best transmission was observed for the thin film annealed in 3 bar oxygen partial pressure. Moreover, not only was grain–like structure found to be more dominant than dot–like structure but also growth of anatase phase was observed instead of that of the rutile phase with increasing oxygen partial pressure up to 3 bar. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

衬底温度对磁控溅射法制备掺Ta氧化锌薄膜性能的影响

采用射频磁控溅射法,在不同的衬底温度下制备了钽(Ta)掺杂的氧化锌(ZnO)薄膜,采用X射线能谱(EDS)、X射线衍射(XRD)、扫描电镜(SEM)、紫外-可见分光光度计和光致发光(PL)光谱研究了衬底温度对制备的Ta掺杂ZnO薄膜的组分、微观结构、形貌和光学特性的影响.EDS的检测结果表明,Ta元素成功掺入到了ZnO薄膜;XRD图谱表明,掺入的Ta杂质是替代式杂质,没有破坏ZnO的六方晶格结构,随着衬底温度的升高,(002)衍射峰的强度先增大后降低,在400℃时达到最大;SEM测试表明当衬底温度较高时(400℃和500℃),Ta掺杂ZnO薄膜的晶粒明显变大;紫外-可见透过光谱显示,在可见光范围,Ta掺杂ZnO薄膜的平均透光率均高于80;,衬底不加热时制备的Ta掺杂ZnO的透光率最高;制备的Ta掺杂ZnO薄膜的禁带宽度范围为3.34~3.37eV,衬底温度为500℃时制备的Ta掺杂ZnO薄膜的禁带宽度最小,为3.34eV.PL光谱表明衬底温度为500℃时制备的Ta掺杂ZnO薄膜中缺陷较多,这也是造成薄膜禁带宽度变小的原因.     

Effect of γ-ray irradiation on structure formation and optical constants of thermally evaporated rhodamine B thin films

Rhodamine B (RhB) is polycrystalline in powder form; it becomes nanocrystalline in thermally evaporated films. Gamma-rays induce nanocrystalline to amorphous transformation of RhB films. The optical constants are independent of film thickness. The type of electronic transition for as-deposited and gamma-ray irradiated RhB film is indirect allowed one. The onset and optical energy gap for as-deposited films are 2 and 3.45 eV, respectively. Exposure to different γ-ray doses did not change the transmittance and reflectance behavior of RhB films. γ-ray irradiation decreases onset and optical energy gap, refractive index and dispersion parameters and increase extinction coefficient, oscillator and electric dipole strengths.     

Influence of annealing on the physical properties of filtered vacuum arc deposited tin oxide thin films

Tin oxide (SnO₂) thin films were deposited on UV fused silica (UVFS) substrates using filtered vacuum arc deposition (FVAD). During deposition, the substrates were at room temperature (RT). As-deposited films were annealed at 400 and 600 °C in Ar for 30 min. The film structure, composition, and surface morphology were determined as function of the annealing temperature using X-ray diffraction (XRD), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS). The XRD patterns of the SnO₂ thin films deposited on substrates at RT indicated that the films were amorphous, however, after the annealing the film structure became polycrystalline. The grain size of the annealed films, obtained from the XRD analysis, increased with the annealing temperature, and it was in the range 8-34 nm. The AFM analysis of the surface revealed an increase in the film surface average grain size from 15 nm to 46 nm, and the surface roughness from 0.2 to 1.8 nm, as function of the annealing temperature. The average optical transmission of the films in the visible spectrum was >80%, and increased by the annealing ∼10%. The films’ optical constants in the 250-989 nm wavelength range were determined by variable angle spectroscopic ellipsometry (VASE). The refractive indexes of as-deposited and annealed films were in the range 1.83-2.23 and 1.85-2.3, respectively. The extinction coefficients, k(λ), of as-deposited and annealed films were in the range same range ∼0-0.5. The optical energy band gap (E_g), as determined by the dependence of the absorption coefficient on the photon energy at short wavelengths, increased with the annealing temperature from 3.90 to 4.35 eV. The lowest electrical resistivity of the as-deposited tin oxide films was 7.8 × 10⁻³ Ω cm, however, film annealing resulted in highly resistive films.     

Substrate effect on microstructure and optical performance of sputter‐deposited TiO2 thin films

This study deals with the role of the different substrates on the microstructural, optical and electronical properties of TiO₂ thin films produced by conventional direct current (DC) magnetron sputtering in a mixture of pure argon and oxygen using a Ti metal target with the aid of X–ray diffractometer (XRD), ultra violet spectrometer (UV–vis) and atomic force microscopy (AFM) measurements. Transparent TiO₂ thin films are deposited on Soda lime glass, MgO(100), quartz and sitall substrates. Phase purity, surface morphology, optical and photocatalytic properties of the films are compared with each other. It is found that the amplitude of interference oscillation of the films is in a range of 77‐89%. The transmittance of the film deposited on Soda lime glass is the smallest while the film produced on MgO(100) substrate obtains the maximum transmittance value. The refractive index and optical band gap of the TiO₂ thin films are also inferred from the transmittance spectra. The results show that the film deposited on Soda lime glass has the better optical property while the film produced on MgO(100) substrate exhibits much better photoactivity than the other films because of the large optical energy band gap. As for the XRD results, the film prepared on MgO(100) substrate contains the anatase phase only; on the other hand, the other films contain both anatase and rutile phases. Furthermore, AFM images show that the regular structures are observed on the surface of all the films studied. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Annealing temperatures induced optical constant variations of methyl violet 2B thin films manufactured by the spin coating technique

Spin coating technique has been successfully applied to deposit uniform methyl violet 2B (MV2B) thin films. X-ray diffraction and Fourier-transform infrared techniques were used to study the crystal and molecular structure of MV2B. The optical properties of the films have been studied by spectrophotometer measurements of transmittance and reflectance at normal incidence of light in the spectral range of 200–2500 nm. The absorption and refractive indices are independent of the film thickness. The absorption parameters such as molar extinction coefficient, oscillator strength and electric dipole strength have been reported before and after annealing. The type of electronic transition is indirect allowed transition with onset energy gap of 1.82 eV and optical energy gap of 3.65 eV. Annealing temperatures reduce structure disorder, remove trap level, increase values of the onset and optical energy gaps and decrease refractive index. The single oscillator model has been applied for calculating the dispersion parameters. The oscillator energy, the dispersion energy, the high frequency dielectric constant, the lattice dielectric constant and the ratio of free charge carriers' concentration to its effective mass were evaluated before and after annealing. The dielectric properties of the films were also determined.     

热蒸发制备CdSe薄膜及其光电特性研究

采用真空热蒸发法技术制备CdSe薄膜,通过XRD、SEM、Hall效应和分光光度计测试了薄膜的结构、表面形貌、I-V特性和光学透过率。结果表明:CdSe薄膜(100)晶面的面间距为0.369 nm,晶粒大小约为10.2 nm,薄膜表面晶粒分布较为均匀;CdSe薄膜与锡和银的肖特基势垒高度分别为0.76 V和0.69 V;CdSe薄膜的光透过率在远红外区较高,且呈上升趋势;折射率随波长增加按指数规律减小;根据Tauc关系和Urbach规则,获得能量带隙为1.79 eV和Urbach能量为0.217 eV。     

空气退火对ZnS薄膜结构和光学特性的影响

采用X射线衍射、扫描电子显微镜和光致发光等技术研究了空气退火对ZnS薄膜的结构和光学特性的影响.薄膜在500℃以下退火后结晶质量得到改善,仍呈ZnS立方相结构.退火温度达到550℃时,薄膜中出现ZnO六方相结构.薄膜退火后,大气中的氧掺入薄膜中,出现ZnS-ZnO复合层.随退火温度升高,薄膜晶粒尺寸增大,透过率增加,带隙逐渐接近ZnO带隙.薄膜光致发光结果表明,复合层内ZnS和ZnO绿色发光的叠加替代了来自ZnS缺陷能级间的绿色发光.     

Optical properties of thermally evaporated CdS thin films

CdS thin films of varying thicknesses were deposited on cleaned glass substrates at room temperature by thermal evaporation technique in a vacuum of about 2 x 10^‐5 torr. UV‐VIS spectra of the films were studied using the optical transmittance measurements which were taken in the spectral region from 300 nm to 1100 nm. The absorbance and reflectance spectra of the films in the UV‐VIS region were also studied. Optical constants such as optical band gap, extinction coefficient, refractive index, optical conductivity and complex dielectric constant were evaluated from these spectra. All the films were found to exhibit high transmittance (∼ 60 ‐ 93 %), low absorbance and low reflectance in the visible/near infrared region from ∼ 500 nm to 1100 nm. The optical band gap energy was found to be in the range 2.28 – 2.53 eV. All the films annealed at 300°C for 4 hours in vacuum (∼ 10^‐2 torr) showed a decrease in the optical transmittance with its absorption edge shifted towards the longer wavelength, leading to the result that the optical band gap decreases on annealing the films. Also, on annealing crystallinity of the films improves, resulting in decrease in the optical transmittance. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)