退火对磁控溅射HfSi_xO_y薄膜光学性质的影响

采用射频反应磁控溅射方法在硅衬底制备了HfSixOy薄膜,用X射线光电子能谱(XPS)分析了HfSixOy薄膜的成分,用X射线衍射(XRD)检测了薄膜的结构,并用椭圆偏振光谱仪研究了退火处理对薄膜光学性质的影响。XRD谱显示,HfSixOy薄膜经700℃高温退火处理后仍为非晶态,而在900℃高温退火处理后出现晶化。采用Tauc-Lorentz(TL)色散模型对测试得到的曲线进行拟合并分析得出薄膜的光学常数,结果表明,薄膜的折射率随退火温度的升高而增加,而消光系数随退火温度的升高呈降低趋势。薄膜的光学带隙随着退火温度的升高增加,采用外推法得到薄膜沉积态和经500℃,700℃,900℃退火后的带隙分别为5.62,5.65,5.68,5.98eV。     

Effect of N2 ambient annealing on the field emission properties of HfNxOy thin films

HfN_xO_y thin films were deposited on Si substrates by direct-current sputtering. The influence of N₂ ambient annealing on the morphology, structure and field emission properties of the HfN_xO_y thin films was studied systematically. Scanning electron microscopy indicates that both the as-deposited and the annealed films are composed of nanoparticles, and the particle sizes of these films do not change much before and after annealing. Atomic force microscopy shows that the surface of the as-deposited films is smooth while that of the annealed films becomes rough, with many protrusions. X-ray diffraction patterns demonstrate that the as-deposited films are amorphous while the samples annealed at over 500 °C are polycrystalline. It is found that the field electron emission properties of the annealed films are better than those of the as-deposited films. The film annealed at 800 °C shows the best field emission properties. The mechanism for the improvement of the field electron emission property of the annealed thin films is also discussed. PACS 73.61.-r; 79.70.+q; 81.05.-t     

Annealing effect on microstructure and mechanical properties of amorphous Al-C-N films

Al-C-N thin films with different Al contents were deposited on Si (1 0 0) substrates by closed-field unbalanced reactive magnetron sputtering in the mixture of argon and nitrogen gases. These films were subsequently vacuum-annealed at 700 °C and 1000 °C, respectively. The microstructures of as-deposited and annealed films were characterized by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM); while the hardness and elastic modulus values were measured by nano-indention method. The results indicated that the microstructure of both as-deposited and annealed Al-C-N films strongly depended on Al content. For thin films at low Al content, film delamination rather than crystallization occurred after the sample was annealed at 1000 °C. For thin films at high Al content, annealing led to the formation of AlN nanocrystallites, which produced nanocomposites of AlN embedded into amorphous matrices. Both the density and size of AlN nanocrystallites were found to decrease with increasing depth from the film surface. With increasing of annealing temperature, both hardness and elastic modulus values were decreased; this trend was decreased at high Al content. Annealing did not change elastic recovery property of Al-C-N thin films.     

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     

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.     

Structure and magnetic properties of magnetron-sputtered [(Fe/Pt/Fe)/Au]n multilayer films

Using dc magnetron sputtering, Fe/Pt/Au multilayer films were prepared, and the effects of Au layer thickness and annealing temperature on structure and magnetic properties of the Fe/Pt/Au multilayer films were investigated. The as-deposited Fe/Pt/Au multilayer films have good periodic structure with composition modulation along the growth direction. The stress stored in the as-deposited films promoted the ordering of the films annealed at 400 °C. When the films were annealed at 500 °C, the thicker Au layer could restrain the order-disorder transformation region volume and lead to the decrease of the ordered volume fraction with Au layer thickness increasing.     

退火及超声处理对ZnO薄膜结构和发光特性的影响

 利用对向靶射频磁控溅射系统在Si（100）衬底上制备了ZnO薄膜,并对其进行了退火和超声处理。采用XRD,AFM和光致发光谱对其结构、表面形貌和性能进行了分析。结果表明：沉积态ZnO薄膜（002）择优取向稍差,尺寸较小,表面粗糙度较大。随退火温度的升高,颗粒粒径增大,样品的取向性和结晶度都明显变好,应力状态由压应力转变为张应力,粗糙度降低。超声处理缓解了薄膜中的张应力,晶粒尺寸更趋增大;用波长为280 nm的激发光激发薄膜时,沉积态薄膜无发光峰存在;随着退火温度升高,出现了一个378 nm的紫外峰和一个398 nm的紫峰;紫外峰峰值强度随退火温度升高不断增强,而紫峰的峰位随退火温度升高基本不发生变化,峰值强度增强;700 ℃退火后的薄膜经超声处理后,发光谱中出现了峰值波长为519 nm的绿色发光带。     

Structure and magnetic properties of annealed metastable FeAg/Pt films

FeAg and FeAg/Pt films were prepared by dc magnetron sputtering at room temperature. The effects of Ag volume fraction in FeAg films and postannealing temperature and time on structure and magnetic properties of FeAg and FeAg/Pt films have been investigated. The results show that the as-deposited FeAg films are metastable. After annealing at 300°C, the phase separation of metastable FeAg films happened and the highest coercivity is obtained in Fe₅₀Ag₅₀/Pt film. With increasing annealing temperature, the ordering and the magnetic properties of the Fe₅₀Ag₅₀/Pt films were improved. When the Fe₅₀Ag₅₀/Pt films are annealed at 600°C for different annealing times, a long annealing time enhances the ordering of the metastable Fe₅₀Ag₅₀/Pt films and affects the orientation development. When the films are annealed for a long time, the grain size and the magnetic domain size also increase, which lead to an increase of correlation length due to the growth of FePt grains.     

A Spectroscopic Ellipsometry Study of TiO2 Thin Films Prepared by dc Reactive Magnetron Sputtering： Annealing Temperature Effect

TiO2 thin films are obtained by dc reactive magnetron sputtering. A target of titanium （99.995%） and a mixture of argon and oxygen gases are used to deposit TiO2 films on to silicon wafers （100）. The crystalline structure of deposited and annealed film are deduced by variable-angle spectroscopic ellipsometry （VASE） and supported by x-ray diffractometry. The optical properties of the films are examined by VASE. Measurements of ellipsometry are performed in the spectral range O. 72-3.55 e V at incident angle 75^o. Several SE models, categorized by physical and optical models, are proposed based on the ＇simpler better＇ rule and curve-fits, which are generated and compared to the experimental data using the regression analysis. It has been found that the triple-layer physical model together with the Cody-Lorentz dispersion model offer the most convincing result. The as-deposited films are found to be inhomogeneous and amorphous, whereas the annealed films present the phase transition to anatase and rutile structures. The refractive index of TiO2 thin films increases with annealing temperature. A more detailed analysis further reveals that thickness of the top sub-layer increases, whereas the region of the bottom amorphous sub-layer shrinks when the films are annealed at 300℃.     

Influence of films thickness and structure on the photo-response of ZnO films

ZnO thin films were grown using Successive Ionic Layer Adsorption and Reaction (SILAR) method on glass substrates at room temperature. Annealing temperatures and film thickness effect on the structural, morphological, optical and electrical properties of the films were studied. For this as-deposited films were annealed at 200, 300, 400 and 500 °C for 30 min in oxygen atmosphere. The X-ray diffraction (XRD) and scanning electron microscopy (SEM) studies showed that the films are covered well with glass substrates and have good polycrystalline structure and crystalline levels. The film thickness effect on band gap values was investigated and band gap values were found to be within the range of 3.49-3.19 eV. The annealing temperature and light effect on electrical properties of the films were investigated and it was found that the current increased with increasing light intensity. The resistivity values were found as 10⁵ Ω-cm for as-deposited films from electrical measurements. The resistivity decreased decuple with annealing temperature and decreased centuple with light emission for annealed films.     

The effects of post-thermal annealing on the optical parameters of indium-doped ZnO thin films

Indium-doped ZnO thin films are deposited on quartz glass slides by RF magnetron sputtering at ambient temper- ature. The as-deposited films are annealed at different temperatures from 400 C to 800 C in air for 1 h. Transmittance spectra are used to determine the optical parameters and the thicknesses of the films before and after annealing using a nonlinear programming method, and the effects of the annealing temperatures on the optical parameters and the thickness are investigated. The optical band gap is determined from the absorption coefficient. The calculated results show that the film thickness and optical parameters both increase first and then decrease with increasing annealing temperature from 400 C to 800 C. The band gap of the as-deposited ZnO:In thin film is 3.28 eV, and it decreases to 3.17 eV after annealing at 400 C. Then the band gap increases from 3.17 eV to 3.23 eV with increasing annealing temperature from 400 C to 800 C.     

Effects of oxygen partial pressure on optical properties of NiOX films deposited by reactive DC-magnetron sputtering

The influence of oxygen partial pressure on the optical properties of NiOX thin films deposited by reactive DC-magnetron sputtering from a nickel metal target in a mixture gas of oxygen and argon was presented.With the oxygen ratio increasing, the reflectivity of the as-deposited films decreased, and optical band gap increased. Thermogravimetric analysis (TGA) showed that the decompose temperature of the films was above 250 ℃. After annealed at 400 ℃, only films deposited at 5% O2/Ar ratio showed high opticalcontrast which was about 52%. Scanning electron microscope (SEM) results revealed that the changes ofsurface morphology were responsible for the optical property variations of the films after annealing. Itsthermal stability and high optical contrast before and after annealing made it a good potential write-onceoptical recording medium.     

离子束增强沉积制备p型氧化锌薄膜及其机理研究

采用离子束增强沉积方法在Si和SiO₂/Si衬底上制备In-N共掺杂ZnO薄膜(INZO)，溅射靶是用ZnO和2 atm% In₂O₃粉体均匀混合并压制而成，在氩离子溅射ZnO靶的同时，氮、氩混合离子束垂直注入沉积的薄膜.实验结果显示INZO薄膜具有(002)的择优取向，并且为p型导电，电阻率最低为0.9Ωcm.薄膜在氮气、氧气气氛下退火，对薄膜的结构和电学特性与成膜和退火条件的关系进行了分析. 关键词： 氧化锌薄膜 p型掺杂 离子束增强沉积     

Nanostructure characterization of high k materials by spectroscopic ellipsometry

In this work, the optical and structural properties of high k materials such as tantalum oxide and titanium oxide were studied by spectroscopic ellipsometry, where a Tauc-Lorentz dispersion model based in one (amorphous films) or two oscillators (microcrystalline films) was used. The samples were deposited at room temperature by radio frequency magnetron sputtering and then annealed at temperatures from 100 to 500 °C. Concerning the tantalum oxide films, the increase of the annealing temperature, up to 500 °C does not change the amorphous nature of the films, increasing, however, their density. The same does not happen with the titanium oxide films that are microcrystalline, even when deposited at room temperature. Data concerning the use of a four-layer model based on one and two Tauc-Lorentz dispersions is also discussed, emphasizing its use for the detection of an amorphous incubation layer, normally present on microcrystalline films grown by sputtering.     

退火温度对a-Se0.70Ge0.15Sb0.15薄膜的结构和光学性质的影响

研究了退火温度对Se0.70Ge0.15Sb0.15薄膜的影响.通过热蒸发技术,在300K温度下将大块无定形Se0.70Ge0.15Sb0.1s沉积在石英和玻璃衬底上.研究发现,未经过退火处理的薄膜结构和在300K,1.33×10-5Pa下退火1小时后的薄膜结构都是无定形结构,而在同样气压470K温度下退火1小时的薄膜有结晶现象.通过在300 2 500nm范围内垂直入射光方向上透射率和反射率的测试,研究了薄膜的一些光学参数,如消光系数(k),折射系数(n)和吸收系数(a).研究发现,n和k同热处理温度有关.通过光学数据的分析,得到了不同条件下薄膜的间接带隙宽度(Enong),未经过热处理薄膜的Enong是1.715±0.021eV,300K下退火薄膜的Enong是1.643±0.021eV,470K下退火的Enong是1.527±0.021eV.退火温度降低了带隙宽度Enong,但增加了带尾eo这种效应可以根据Mott和Davis提出的多晶体系中态密度来解释.     

Effect of Co layer thickness on structural and magnetic properties of C/Co/C films

Granular C/Co/C films have been prepared by magnetron sputtering from C and Co onto glass substrates at room temperature and subsequent in situ annealing. It has been found that the structure and magnetic properties of the C/Co/C films depend strongly on the Co layer thickness. Vibrating sample magnetometer measurements indicate that the in-plane coercivities reach maximum in 20 nm Co thickness of both as-deposited and annealed films. The squareness ratio of annealed films was more than 0.8. X-ray diffraction shows that majority Co nanograins are formed as the hexagonal-close-packed (HCP) structure in 20 nm Co thickness with annealing at 400 °C. Scanning probe microscope was used to scan surface morphology and magnetic domain structures. The values of the surface roughness were lower than 0.6 nm in all annealed samples. The average magnetic cluster size was estimated to be about 10 nm in annealed 20 nm Co thickness films.     

Optical properties of ZnO thin films on SiO2 substrates deposited by radio frequency magnetron sputtering

The optical properties of both the annealed and as-deposited ZnO thin films by radio frequency (RF)magnetron sputtering on SiO2 substrates were studied. In the annealed films, two pronounced well defined exciton absorption peaks for the A and B excitons were obtained in the absorption spectra, a strong free exciton emission without deep-level emissions was observed in the photoluminescence (PL) spectra at room temperature. It was found that annealing the films in oxygen dramatically improved the optical properties and the quality of the films.     

温度对AZO薄膜红外辐射性能的影响

随着全球资源的减少和环境的恶化,节能减排已成为人们关注的焦点,具有保温隔热功能的低辐射玻璃成为研究的热点。提高玻璃保温隔热性能最有效的方法就是在其表面涂覆低辐射率层。原材料丰富、导电性能好、可见光透过率高等优势使得Al掺杂ZnO (AZO)薄膜成为最具潜力的低辐射率层。系统研究了温度对AZO薄膜红外辐射性能的影响,分析了变化机理。首先研究了在一定的温度下持续一段时间后,AZO薄膜的红外比辐射率的变化情况。然后研究了在变温环境中红外比辐射率的变化情况。采用直流磁控溅射法在室温下玻璃基片上沉积500 nm厚的AZO薄膜,将薄膜放到马弗炉中进行热处理,在100～400 ℃空气气氛下保温1 h,随炉冷却。采用X射线衍射仪对AZO薄膜进行物相分析,采用扫描电子显微镜观察薄膜表面形貌变化。利用四探针测试法测量AZO薄膜的电阻率,采用红外比辐射率测试仪测试薄膜红外比辐射率, 可见分光光度计测量可见光谱。测试的结果表明,薄膜热处理前后均为六角纤锌矿结构,(002)择优取向。300 ℃及以下热处理1 h后,(002)衍射峰增强,半高宽变窄,晶粒尺寸长大。随着热处理温度的升高,薄膜的电阻率先减小后增大,200 ℃热处理后的薄膜具有最小的电阻率(0.9×10-3 Ω·cm)。热处理温度升高,晶粒长大使得薄膜电阻率降低。热处理温度过高,薄膜会从空气中吸收氧,电阻率下降。薄膜的红外比辐射率变化趋势和电阻率的一致,在200 ℃热处理后获得最小值(0.48)。自由电子对红外光子有较强的反射作用,当电阻率低,自由电子浓度高的时候,更多的红外光子被反射,红外辐射作用弱,红外比辐射率小。薄膜的可见光透过率随着热处理温度的升高先减小后增大,200 ℃热处理后的薄膜的可见光透过率最小,但仍高达82%。这种变化是由于自由电子浓度变化引起的,自由电子对可见光有很强的反射作用。选取未热处理和200 ℃热处理后的样品进行变温红外比辐射率的测量,将样品放在可加热的样品台上,位置固定,在室温到350 ℃的升温和降温过程中每隔25 ℃测量一次红外比辐射率,结果表明,在室温到350 ℃的温度范围内,AZO薄膜的红外比辐射率在升温过程中随着温度的上升而增大,在降温过程中减小,经过整个升、降温过程后,薄膜的红外比辐射率增大。     

Optical and electrical properties of plasma-oxidation derived HfO2 gate dielectric films

High-k gate dielectric HfO₂ thin films have been deposited on Si(1 0 0) by using plasma oxidation of sputtered metallic Hf thin films. The optical and electrical properties in relation to postdeposition annealing temperatures are investigated by spectroscopic ellipsometry (SE) and capacitance-voltage (C-V) characteristics in detail. X-ray diffraction (XRD) measurement shows that the as-deposited HfO₂ films are basically amorphous. Based on a parameterized Tauc-Lorentz dispersion mode, excellent agreement has been found between the experimental and the simulated spectra, and the optical constants of the as-deposited and annealed films related to the annealing temperature are systematically extracted. Increases in the refractive index n and extinction coefficient k, with increasing annealing temperature are observed due to the formation of more closely packed thin films and the enhancement of scattering effect in the targeted HfO₂ film. Change of the complex dielectric function and reduction of optical band gap with an increase in annealing temperature are discussed. The extracted direct band gap related to the structure varies from 5.77, 5.65, and 5.56 eV for the as-deposited and annealed thin films at 700 and 800 °C, respectively. It has been found from the C-V measurement the decrease of accumulation capacitance values upon annealing, which can be contributed to the growth of the interfacial layer with lower dielectric constant upon postannealing. The flat-band voltage shifts negatively due to positive charge generated during postannealing.     

Exchange coupling in CoO–Co bilayer

In this work, exchange bias and coercivity enhancement in ferromagnet (FM)–antiferromagnet (AFM) bilayer have been investigated. CoO film (50 nm) was deposited by sputtering with a relatively high oxygen partial pressure. The deposited films were subsequently annealed at varied temperature up to 973 K in the air atmosphere. The CoO film shows a disordered structure in the as-deposited state and an increase of crystallinity after annealing characterized by XRD and Raman spectra. A 40-nm Co film was deposited on the as-deposited CoO and annealed films. The Co–CoO bilayer shows a large exchange bias up to 1600 Oe and relatively high coercivity up to 3200 Oe (H_C−) at 5 K, which is much larger than that of crystalline Co–CoO bilayer films without any treatment. The spin glass behavior combined with increasing crystallinity, surface roughness of CoO after annealing may be attributed to the large exchange bias and high coercivity.