Effect of post thermal annealing on the structural and optical properties of ZnO thin films prepared from polymer precursor

ZnO thin films were synthesised by a new method which uses polyvinyl alcohol (PVA) as polymer precursor. The films are annealed at different temperatures and for different annealing times. The structural parameters, like grain size, lattice constants, optical band gap, and Urbach energy, depend on the annealing temperature and annealing time. All the films possess tensile strain which relaxes as the annealing temperature and the annealing time increases. The photoluminescence (PL) spectra contain only ultraviolet (UV) peaks at low temperature, but as the annealing temperature and time increase we observe peaks at blue and green regions with variation of the intensities of these peaks with annealing temperature and annealing time.     

退火温度对低温生长MgxZn1－xO薄膜光学性质的影响

用射频磁控溅射法在80℃衬底温度下制备出Mg_xZn_1-xO(x=0.16)薄膜，用X射线衍射(XRD)、光致发光(PL)和透射谱研究了退火温度对Mg_xZn_1-xO薄膜结构和光学性质的影响.测量结果显示，Mg_xZn_1-xO薄膜为单相六角纤锌矿结构，并且具有沿c轴的择优取向；随着退火温度的升高，(002)XRD峰强度、平均晶粒尺寸和紫外PL峰强度增大，(002)XRD峰半高宽(F 关键词： xZn_1-xO薄膜')" href="#">Mg_xZn_1-xO薄膜 射频磁控溅射 退火     

Research on double resonance peaks and abnormal frequency shift in permeability spectra of annealed FeCoB films

A FeCoB magnetic film was prepared by a magnetron sputtering method and then was divided into several small pieces for vacuum annealing at different temperatures. The dependence of the coercivity along the hard axis on the annealing temperature reveals a degeneration of softness with the growth of grain size when the annealing temperature is above 350 °C. In permeability spectra measurements, double resonance peaks and an abnormal positive shift in the resonance peak at higher frequency with the increase in annealing temperature are observed. The existence of two peaks is attributed to the double magnetic phases (Fe and FeCo) in the films. The positive shift in the resonance peak at higher frequency has been analyzed and ascribed to the enhanced internal stray fields with the annealing temperature. This phenomenon of positive frequency-shift is very fascinating and novel, which makes the ferromagnetic films more efficient for the applications in the noise absorbing area.     

退火对ZnO薄膜光学特性的影响

用射频磁控溅射法在蓝宝石衬底上制备出ZnO薄膜,通过X射线衍射(XRD)、扫描电镜(SEM)和光致发光(PL)谱等研究了退火温度对ZnO薄膜结构和光学性质的影响。测量结果显示,所制备的ZnO薄膜为六角纤锌矿结构,具有沿c轴的择优取向;随着退火温度的升高,(002)XRD峰强度和平均晶粒尺寸增大,(002)XRD峰半高宽(FWHM)减小,光致发光紫外峰强度增强。结果证明,用射频磁控溅射法通过适当控制退火温度可得到高质量ZnO薄膜。     

Temperature dependent surface and spectral modifications of nano V<Subscript>2</Subscript>O<Subscript>5</Subscript> films

Nanocrystalline V₂O₅ films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO₂ (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.     

热处理温度对ZnO∶Al薄膜性能的影响

利用溶胶-凝胶技术在玻璃衬底上制备了ZnO∶Al薄膜,表征了薄膜的结构、光透过和光致发光特性,探讨了热处理温度对薄膜晶体结构和光学性质的影响.结果表明,在热分解温度400 ℃和退火温度600 ℃时,ZnO∶Al薄膜的C轴择优取向明显,透过率较高.在热处理温度400 ℃情况下,激发波长340 nm的光致发光谱中有三个发光中心,紫外发光强度随退火温度的升高先升高后下降,500 ℃时发光强度最强.其它两个发光峰的强度随退火温度的升高而降低甚至消失.激发波长不同,ZnO∶Al薄膜的发光中心和强度均发生变化.     

Si基CeO_2薄膜的发光特性

利用电子束蒸发技术在p型硅衬底上沉积了200 nm厚的CeO2薄膜样品,将样品置于弱还原气氛中高温退火后,观察到薄膜在385,418 nm以及445 nm左右出现三个明显的发光峰。结合激发光谱、吸收光谱以及XRD分析表明:CeO2薄膜在高温下容易发生失氧反应,出现Ce4+→Ce3+离子转变,Ce3+离子在紫外光的激发下,电子由O2p跃迁到5d能级,再由5d能级向4f能级跃迁,从而产生强烈的蓝紫外发射,而445 nm左右的发光峰则来自于SiO2薄膜的缺陷发光。样品选择900~1 200℃不同温度退火,并且在1 200℃下进行了不同时间的退火。研究结果显示:在1 200℃下进行2 h的退火,薄膜发光强度达到最大。     

Low-temperature phase transformation of CZTS thin films

The low temperature phase transformation in the Cu_2ZnSnS_4(CZTS) films was investigated by laser annealing and low temperature thermal annealing.The Raman measurements show that a-high-power laser annealing could cause a red shift of the Raman scattering peaks of the kesterite(KS) structure and promotes the formation of the partially disordered kesterite(PD-KS) structure in the CZTS films,and the low-temperature thermal annealing only shifts the Raman scattering peak of KS phase by several wavenumber to low frequency and the broads Raman peaks in the low frequency region.Moreover,the above two processes were reversible.The Raman analyses of the CZTS samples prepared under different process show that the PD-KS structure tends to be found at low temperatures and low sulfur vapor pressures.Our results reveal that the control of the phase structure in CZTS films is feasible by adjusting the preparation process of the films.     

不同退火条件对纳米多孔氧化铝薄膜光致发光的影响

以草酸为电解液,采用二次阳极氧化法制备出了纳米多孔氧化铝薄膜,经不同退火温度和退火气氛处理氧化铝薄膜后,通过分析其光致发光光谱得出：相同的退火气氛中, 退火温度T≤600 ℃ 时,T=500 ℃具有最大的光致发光强度;退火温度T≥700 ℃时,随着退火温度的升高,样品的发光强度增大。在不同的退火气氛中,多孔氧化铝薄膜随着退火温度的升高,发光峰位改变不同,即在空气中退火处理后,随着退火温度的升高,发光峰位蓝移,而在真空中退火处理后,发光峰位并不随退火温度的升高而变化;通过对1 100 ℃高温退火处理后的氧化铝薄膜的光致发光曲线的高斯拟合,可以看出,经退火处理后的多孔氧化铝,主要存在三个发光中心,发光曲线在350～600 nm范围内对应三个发射峰, 发射波长分别为387,410,439 nm。相同的退火温度下,空气中退火得到的氧化铝薄膜的光致发光强度大于真空中退火处理后的氧化铝薄膜。基于实验结果,结合X射线色散能谱(EDS)、红外反射光谱等表征手段,探讨了多孔氧化铝薄膜的发光机制,并对经过不同退火条件得到的多孔氧化铝薄膜的光致发光特性的改变做出了合理的解释。     

The preparation and refractive index of BST thin films

Radio-frequency magnetron sputtering technique is used to deposit Ba_0.65Sr_0.35TiO₃ (BST) thin films on fused quartz substrates. In order to prepare the high-quality BST thin films, the crystallization and microstructure of the films were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and atomic force microscopy (AFM). More intense characteristic diffraction peaks and better crystallization can be observed in BST thin films deposited at 600 °C and subsequently annealed at 700 °C. The refractive index of the films is determined from the measured transmission spectra. The dependences of the refractive index on the deposition parameters of BST thin films are different. The refractive index of the films increases with the substrate temperature. At lower sputtering pressure, the refractive index increases from 1.797 to 2.197 with pressure increase. However, when the pressure increases up to 3.9 Pa, the refractive index reduces to 1.86. The oxygen to argon ratio also plays an important effect on the refractive index of the films. It has been found that the refractive index increases with increase in the ratio of oxygen to argon. The refractive index of BST thin films is strongly dependent on the annealing temperature, which also increases as the annealing temperature ascends. In a word, the refractive index of BST thin films is finally affected by the films’ microstructure and texture.     

Temperature-dependent luminescence dynamics for ZnO thin films

The paper presents the photoluminescence investigation of zinc oxide thin films. A high quality ZnO films fabricated by dip-coating (sol–gel) method were grown on quartz wafers. The films with different thickness (number of layers) were annealed at different temperatures after the preparation process. It was found that high quality, transparent ZnO thin films could be produced on quartz substrates at relatively low annealing temperature (450–550  $^{\circ }\mathrm{C}$ ). The dependence of the ZnO thin film quality was studied by X-ray diffraction and atomic force microscopy techniques. Optical properties were investigated by classic and time-resolved photoluminescence (TRPL) measurements. Photoluminescence spectra allowed us to estimate energy of the free excitons, bond excitons and their longitudinal optical (LO) phonon replicas as a function of the annealing temperature. An innovative TRPL technique let us precisely measure the decay time of the free- and bond excitons’ in the real time. TRPL measurements as a function of temperature reveal a biexponential decay behavior with typical free/bound exciton decay constants of 970/5310 ps for the as-grown sample and 1380/5980 ps after annealing process. Presented spectra confirm high structural and optical quality of investigated films. We proved that the thermal treatment improve both optical and structural quality and extend the photoluminescence’s lifetimes. The obtained experimental results are important for identification of exciton’s peaks and their LO phonon replicas for the investigated ZnO films.     

退火处理对SnO2薄膜光致发光性质的影响

实验研究表明,SnO2薄膜经过退火处理后其光致发光谱有明显的变化。在氧和氮两种不同气氛中进行热处理,其变化也有差异。这种变化主要是由于SnO2膜中氧空位和自由载流于浓度变化所致。     

纳米BST薄膜的制备及其折射率特性.

" 采用射频磁控溅射法在石英衬底上沉积了纳米BST(Ba0:65Sr0:35TiO3)薄膜．为了制备优质的BST薄膜,借助X射线衍射仪、场发射扫描电镜和原子力显微镜研究了BST薄膜的晶化行为和显微结构．结果显示在衬底温度600 ℃下制备的BST薄膜经700 ℃退火处理后,具有较强的特征衍射峰和极好的晶化．同时还研究了纳米BST薄膜的制备参数和特性,BST薄膜的折射率是由测量的透射谱中获得的．实验结果表明：纳米BST薄膜的沉积参数对其折射率特性的影响是不尽相同的．折射率随着衬底温度的上升而增加;在较低的溅射     

Kr离子注入SiC的拉曼光谱研究

应用拉曼光谱研究了5 MeV Kr离子（注量分别为5×1013,2×1014,1×1015 ions/cm2）室温注入6H SiC单晶及其高温退火处理后结构的变化。 研究表明, 注入样品的拉曼光谱中不仅出现了Si—C振动的散射峰, 还产生了同核Si—Si键和C—C键散射峰。 Si—C散射峰强度随退火温度升高而增强, 当退火温度高达1000 ℃时, 已接近未辐照SiC的散射峰强度。晶体Si—Si键散射峰强度随退火温度变化不大, 而非晶Si—Si键散射峰强度随退火温度的增加逐渐消失。相对拉曼强度（Relative Raman Intensity, 简称RRI）随注量的增加逐渐减小并趋于饱和, 且不同退火温度样品的饱和注量不相同; RRI随退火温度的增加逐渐升高, 这在低注量样品中表现得尤为明显。 低、中、高3种注量样品的RRI随退火温度的增加从重合逐渐分离, 并且退火温度越高, 分离越大。 Raman spectroscopy was used to study the structure changes of 6H SiC single crystal implanted with 5 MeV Kr (Krypton) at room temperature and subsequently annealed at high temperature. The Raman spectrum of the implanted SiC displays not only Si—C bonds vibration peaks, but also homonuclear Si—Si and C—C bond vibration peaks. Si—C bond vibration peaks gradually strengthen with increasing temperature. When annealing at 1000 ℃, the peak intensity of Raman spectrum is close to that of virgin specimen. It is found that crystal Si—Si bond vibration peaks do not change when annealing, but amorphous Si—Si bond vibration peaks disappear with increasing annealing temperature. The Relative Raman Intensity (RRI) values decrease with increasing fluence and tend to saturate, but the saturation fluences is different for various anneal temperature. The RRI values increases with raising annealing temperature, which is more obvious in low implanted specimens. At the same time, the RRI values separate gradually with increasing temperature and this phenomenon is strengthened by annealing temperature.     

Factors affecting the electro-optical and structural characteristics of nano crystalline Cu doped (Cd–Zn)S films

This work investigates the effects of the temperature, deposition time and annealing ambient on the electro-optical and structural properties of nano crystalline (Cd–Zn)S films prepared by chemical bath deposition (CBD). The deposited films being uniform and adherent to the glass substrates are amorphous in nature and the crystallinity as well as the grain size is found to increase on post-deposition annealing. The obtained specimens are thoroughly characterized before and after annealing paying particular attention to their structure, composition and morphology. Annealing in air reduces the extent of disorder in grain boundaries and energy band-gap. A correlation between the structural and optical properties is investigated in detail. The surface morphology and structural properties of the as-deposited and annealed (Cd–Zn)S thin films are studied using X-ray diffraction (XRD), scanning electron microscope (SEM) and optical transmission spectra. The optical transmission spectra are recorded within the range of 300–800 nm and 300–900 nm. The electroluminescent (EL) intensity is found to be maximum at a particular temperature, which decreases with further increase in temperature and peaks of photoluminescent (PL) and EL spectra are centered at 546 nm and 592 nm. The emission intensity also increases with increasing thickness of the film.     

退火对非故意掺杂4H-SiC外延材料386 nm和388 nm发射峰的影响

10 K条件下,采用光致发光(PL)技术研究了不同退火处理后非故意掺杂4H-SiC外延材料的低温PL特性.结果发现,在370—400 nm范围内出现了三个发射峰,能量较高的峰约为3.26 eV,与4H-SiC材料的室温禁带宽度相当.波长约为386 nm和388 nm的两个发射峰分别位于~3.21 eV和~3.19 eV,与材料中的N杂质有关.当退火时间为30 min时,随退火温度的升高,386 nm和388 nm两个发射峰的PL强度先增加后减小,且退火温度为1573 K时,两个发射峰的PL强度均达到最大. 关键词： 光致发光 退火处理 能级 4H-SiC     

Investigations on vacuum-evaporated CSZ thin films for thermal barrier applications

Ceria-stabilized zirconia (CSZ) thin films have been developed over Ni-based alloy substrate by vacuum evaporation method using an electron beam. X-ray diffraction (XRD) analysis of the film heat treated at different temperatures reveals monoclinic phase stabilization. Transmission measurements of the films annealed at different temperatures, in the wavelength region 300–1,100 nm, indicate that the band gap energy of the films lies between 3.6 and 3.8 eV. Refractive index of the films was found to increase with the increase in the annealing temperature. Micro hardness of the films increases nonlinearly with the increase in annealing temperature, indicating an improvement in the hardness of the films. Thermal conductivity studies of the CSZ-coated substrate show a nonlinear decrease with the increase in annealing temperature. Surface investigations of the CSZ films confirm an increase in grain size and a decrease in surface roughness with the increase in annealing temperature of the films. Paper presented at the Third International Conference on Ionic Devices (ICID 2006), Chennai, Tamilnadu, India, Dec. 7–9, 2006.     

Studies on CdS nanoparticles dispersed in silica matrix prepared by sol-gel technique

SiO₂/CdS-nanoparticle composite films (SiO₂:CdS=85:15, 80:20, 75:25 and 70:30) were prepared by the sol-gel route. The films were characterized by studying microstructural (XRD and TEM) and optical (transmittance and photoluminescence) properties. Band gaps of these films annealed at different temperatures (373-473 K) for different times (10-120 min) indicated that the signature of nanocrystallinity is retained throughout the range of our experimental conditions. A thermal diffusion process controlled growth in the crystallite size with increasing annealing time and temperature. The average radii of the nanoparticles varied as the cube root of the annealing time but showed exponential dependence on the inverse of annealing temperature. Photoluminescence (PL) studies of the composite films indicated excitonic transitions. Theoretical analysis of the line shapes of the PL peaks recorded at 300 K and 80 K could be accounted for by the combined effects of size distribution and phonon broadening. It was observed that the deformation potential (E _d) effectively controlled the line shapes of the PL measurements. Received 24 May 2002 Published online 27 January 2003 RID="a" ID="a"e-mail: msakp@mahendra.iacs.res.in     

退火对ZnO:Al薄膜光致发光性能的影响

 采用溶胶-凝胶工艺在石英衬底上制备ZnO:Al（AZO）薄膜，通过不同温度的退火处理，研究了退火对AZO薄膜结构和光致发光特性的影响。XRD图谱表明：所制备的薄膜具有c轴高度择优取向，随着退火温度的升高，(002)峰的强度逐渐增强，同时(002)峰的半高宽逐渐减小,表明晶粒在不断增大。未退火样品的光致发光（PL）谱由361 nm附近的紫外带边发射峰和500 nm附近的深能级发射峰组成。样品经退火后，以500 nm为中心的绿带发射逐渐减弱，而带边发射强度有所增强,并且逐渐红移到366 nm附近，与吸收边移动的测试结果相吻合。对经过不同时间退火的样品分析表明，AZO薄膜的发光特性与退火时间也有很大关系，时间过短可见波段的发射较强，但时间过长会使晶粒发生团聚，导致紫外发射峰强度减弱。     

Initial study on the structure and photoluminescence properties of SiC films doped with Al

SiC films doped with aluminum (Al) were prepared by the rf-magnetron sputtering technique on p-Si substrates with a composite target of a single crystalline SiC containing several Al pieces on the surface. The as-deposited films were annealed in the temperature range of 400-800 °C under nitrogen ambient. The thin films have been characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The results show that the introduction of Al into films hinders crystalline formation process. And with the increase of annealing temperature, more Si particles are formed in the films, which strongly affect the optical absorption properties. The photoluminescence (PL) spectra of the samples show two peaks at 370 nm and 412 nm. The intensities of the PL peaks are evidently improved after Al doped. We attribute the origin of the two PL peaks to a kind of Si-related defect centres. The obtained results are expected to have important applications in modern optoelectronic devices.