低温退火的X射线W/Si多层膜应力和结构性能

W/Si多层膜反射镜在硬X射线天文望远镜中有重要应用. 为减小其应力对反射镜面形和望远镜分辨率的影响, 同时保证较高的反射率, 采用150, 175和200 ℃ 的低温退火工艺对采用磁控溅射镀制的W/Si周期多层膜进行后处理. 利用掠入射X射线反射测试和样品表面面形测试对退火前后W/Si多层膜的应力和结构进行表征. 结果表明, 在150 ℃ 退火3 h 后, 多层膜1级峰反射率和膜层结构几乎没有发生变化, 应力减少约27%; 在175 ℃ 退火3 h后, 多层膜膜层结构开始发生变化, 应力减少约50%; 在200 ℃退火3 h 后, 多层膜应力减小超过60%, 但1级布拉格峰反射率相对下降17%, 且膜层结构发生了较大变化. W, Si界面层的增大和相互扩散加剧是应力和反射率下降的主要原因.     

AIN/Si3N4 纳米多层膜的外延生长与力学性能

采用射频磁控溅射方法制备单层AlN,Si3N4薄膜和不同调制周期的AlN/S3N4纳米多层膜.采用X射线衍射仪、高分辨透射电子显微镜和纳米压痕仪对薄膜进行表征.结果发现,多层膜中Si3N4层的晶体结构和多层膜的硬度依赖于Si3N4层的厚度.当AlN层厚度为4.0 nm、Si3N4层厚度为0.4nm时,AlN和Si3N4层共格外延生长,多层膜形成穿过若干个调制周期的柱状晶结构,产生硬度升高的超硬效应.随着Si3N4层厚的增加,Si3N4层逐步形成非晶并阻断了多层膜的共格外延生长,多层膜的硬度迅速降低,超硬效应消失.采用材料热力学和弹性力学计算了Si3N4层由晶态向非晶转变的临界厚度.探讨了AlN/Si3N4纳米多层膜出现超硬效应的机理.     

Mo/Si多层膜表面保护层设计

为提高Mo/Si多层膜的稳定性与使用寿命,通过分析多层膜驻波电场的分布,对表面保护层及多层膜最上层材料的厚度进行优化设计,使优化后的反射率最高.计算表明,一定厚度的表面保护层总对应一个最优的最上层材料厚度.在13.36 nm波长,膜对数为50的Mo/Si多层膜10度入射的理论反射率为74.47%;当添加厚度为2.3 nm的Ru作为表面保护层,对应多层膜最上层Si的优化厚度为3.93 nm,其理论反射率为75.20％.设计结果表明,通过优化设计表面保护层,可以提高多层膜稳定性,改善多层膜性能.     

磁控溅射制备极紫外高反射率多层膜应力研究

为制备硼边附近6.7 nm波长的极紫外高反射率多层膜反射镜,研究了Mo_2C/B_4C,Mo/B_4C周期多层膜,重点解决薄膜应力难题。采用直流磁控溅射技术制备了膜层厚度为30 nm的Mo,Mo_2C,B_4C,单层膜,周期厚度为3.5 nm,30对的Mo_2C/B_4C,Mo/B_4C周期多层膜。利用台阶仪测试了镀膜前后基底面形,计算并比较了不同薄膜样品的应力值。结果表明Mo_2C/B_4C多层膜压应力要远小于Mo/B_4C多层膜,且成膜质量与Mo/B_4C相当。因此Mo_2C/B_4C是应用于6.7 nm反射镜较好的多层膜材料组合。     

磁控溅射方法制备直径120mm高均匀性Mo/Si多层膜

为满足极紫外、软X射线和X射线大口径多层膜反射镜的需求,采用基板扫掠过矩形靶材表面的镀膜方法,在直径120 mm的平面基板上镀制了Mo/Si周期多层膜。通过调整基板扫掠过矩形靶材表面的速率修正了薄膜的沉积速率,极大地提高了薄膜厚度的均匀性。采用X射线衍射仪对反射镜不同位置多层膜周期厚度进行了测量,结果表明,在直径120 mm范围内,Mo/Si多层膜周期厚度的均匀性达到了0.26%。同步辐射测量多层膜样品不同位置处的反射率,结果表明,在直径120 mm范围内,多层膜的膜层厚度均匀,在入射角10°时13.75 nm波长处平均反射率为66.82%。     

极紫外多层膜残余应力初步研究

 针对极紫外多层膜在激光等离子体诊断、极紫外光刻等方面的应用，进行了Mo/Si多层膜残余应力的实验研究，讨论了多层膜残余应力的成因。实验结果表明：Mo单层膜表现为张应力， Si单层膜表现为压应力；通过传统方法制备的13.0 nm处高反射率的40对Mo/Si多层膜会产生-500 MPa左右的压应力，其压应力主要是由膜层之间的贯穿扩散引起的；通过改变膜层比率可以在一定程度上补偿因贯穿扩散产生的压应力，但是以牺牲多层膜反射率为代价。     

大尺寸高性能X射线双通道多层膜反射镜研制

为满足同步辐射装置中X射线单色器的需求,在直线式磁控溅射设备上制备了W/Si和Ru/C双通道多层膜反射镜。制备的W/Si多层膜和Ru/C多层膜的周期厚度均为3 nm,平均界面宽度分别为0.30 nm和0.32 nm。在320 mm长度范围和20 mm宽度范围内,W/Si多层膜膜厚误差的均方根值分别为0.30%和0.19%,Ru/C多层膜膜厚误差的均方根值分别为0.39%和0.20%。对制备的样品进行了表面形貌测试和非镜面散射测试,对比了W/Si多层膜和Ru/C多层膜的表面和界面粗糙度大小。硬X射线反射率测试结果表明,W/Si多层膜和Ru/C多层膜在8.04 keV能量点处的一级布拉格峰测试反射率分别为63%和62%,角分辨率均为2.6%。基于以上研究,在尺寸为350 mm×60 mm的高精度Si平面镜表面镀制了W/Si和Ru/C双通道多层膜,并且其被成功应用于上海同步辐射光源线站中。     

磁控溅射制备横向梯度分布的Mo/Si周期多层膜

 采用磁控溅射方法在Si基板上镀制了横向梯度分布的Mo/Si周期多层膜。以X射线掠入射反射测量了横向梯度多层膜的膜系结构,在基板65 mm长度范围内,多层膜周期从8.21 nm线性减小到6.57 nm,周期梯度为0.03 nm/mm。国家同步辐射实验室反射率计的反射率测试结果表明：该横向梯度分布周期多层膜上不同位置,能反射在13.3~15.9 nm波段范围内不同波长的极紫外光,反射率为60%~65%。     

Si/SiO2多层膜的Ⅰ-Ⅴ特性研究

用射频磁控溅射法制备了Si/SiO2多层膜,并对多层膜的Ⅰ-Ⅴ特性实验结果进行了拟合.分析表明,Si/SiO2多层膜的Ⅰ-Ⅴ特性由多种因素决定,单一的电流输运模型不能控制Si/SiO2多层膜的Ⅰ-Ⅴ特性,多层膜结构及氧化硅层的厚度是影响薄膜Ⅰ-Ⅴ特性的主要因素.     

Mo/Si多层膜小角X射线衍射结构表征

为了实现对Mo/Si多层膜的结构表征,测量了多层膜样品的小角X射线衍射谱。介绍了小角X射线衍射谱的分析方法,包括Bragg峰值拟合法,傅里叶变换法,反射谱拟合法。Bragg峰值拟合法和反射谱拟合法得到多层膜的周期厚度为7.09nm,两种模型的反射谱拟合法得到界面的粗糙度(扩散长度)为0.40～0.41nm(Si在Mo上),0.52～0.70nm(Mo在Si上),前者要比后者小,这与透射电镜法(TEM)得到的结果0.40nm(Si在Mo上),0.6～0.65nm(Mo在Si上)是一致的。通过基于扩散模型的反射谱拟合法得到的折射率剖面也与由高倍率透射电镜(HRTEM)积分得到的灰度值剖面在趋势上是一致的。通过X射线衍射谱和TEM图像对Mo/Si多层膜进行综合表征,得到了多层膜的精细结构信息,这对多层膜制备工艺的优化具有十分重要的意义。     

Processing of W/Si and Si/W bilayers and multilayers with single and multiple excimer-laser pulses

Interdiffusion phenomena, thermal damage and ablation of W/Si and Si/W bilayers and multilayers under XeCl-excimer laser (=308 nm) irradiation at fluences of 0.15, 0.3 and 0.6 J/cm² were studied. Samples were prepared by UHV e-beam evaporation onto oxidized Si. The thickness of W and Si layers and the total thickness of the structures were 1–20 nm and 40–100 nm, respectively. 1 to 300 laser pulses were directed to the same irradiation site. At 0.6 J/cm² the samples were damaged even by a single laser pulse. At 0.3 J/cm² WSi₂ silicide formation, surface roughening and ablation were observed. The threshold for significant changes depends on the number of pulses: it was between 3–10 pulses and 10–30 pulses for bilayers with W and Si surfaces, respectively, and more than 100 pulses for multilayers with the same total thickness of tungsten. At 0.15 J/cm² the periodicity of the multilayers was preserved. Temperature profiles in layered structures were obtained by numerical simulations. The observed differences of the resistance of various bilayers and multilayers against UV irradiation are discussed.     

Pd2Si的生成对Pd/Si多层膜衍射性能的影响

本文研究了Pd₂Si的生成对周期性Pd/Si多层膜X射线衍射性能的影响。X射线衍射强度的测量数据表明Pd₂Si的生成对长周期多层膜的衍射强度影响不大,但对短周期多层膜衍射强度的影响较大。在引入折射率修正后,我们不仅用单个峰的位置计算了多层膜的周期,而且还用了以两个峰的位置联立消去折射率修正的方法计算了多层膜的周期,前者的误差大于后者。模拟计算的结果说明:均匀Pd₂Si层的生成不足以解释Pd/Si多层膜衍射强度随退火温度的变化,界面的平整化或粗糙化是影响衍射强度的另一个要素。 关键词：     

Core-level study of WSi2 (110)

Angle resolved core level studies of the Si 2p and W 4f levels have been carried out on the (110) surface of a WSi₂ single crystal using synchrotron radiation. Surface shifted components have been revealed both in the Si 2p and W 4f spectra. Investigations were carried out at two different annealing temperatures. The results indicate Si enrichment at the surface, and a larger enrichment after the higher temperature anneals. The reactivity upon initial oxygen exposure was investigated. Strong Si oxidation was observed but chemically shifted W 4f components could also be detected.     

Direct nano‐scale patterning of Ag films using hard X‐ray induced oxidation

The morphological change of silver nano‐particles (AgNPs) exposed to an intense synchrotron X‐ray beam was investigated for the purpose of direct nano‐scale patterning of metal thin films. AgNPs irradiated by hard X‐rays in oxygen ambient were oxidized and migrated out of the illuminated region. The observed X‐ray induced oxidation was utilized to fabricate nano‐scale metal line patterns using sectioned WSi₂/Si multilayers as masks. Lines with a width as small as 21 nm were successfully fabricated on Ag films on silicon nitride. Au/Ag nano‐lines were also fabricated using the proposed method.     

Microstructure and dielectric properties of pulsed-laser-deposited CaCu 3 Ti 4 O 12 thin films on LaNiO 3 buffered Pt/Ti/SiO 2 /Si substrates

CaCu₃Ti₄O₁₂ (CCTO) thin films have been prepared by a pulsed-laser-deposition method on LaNiO₃ buffered Pt/Ti/SiO₂/Si substrates, and their microstructure and dielectric properties have been compared with those of the films deposited directly on Pt/Ti/SiO₂/Si substrates. The crystalline structure and the surface morphology of the CCTO thin films were markedly affected by the bottom electrodes. Both the films show temperature-independent dielectric properties in a wide temperature range, which is similar to those properties obtained in single-crystal or epitaxial thin films, while the room-temperature dielectric constant of the 350-nm-thick CCTO films on LaNiO₃/Pt/Ti/SiO₂/Si substrates at 100 kHz was found to be 2300, which was increased significantly compared with that obtained in the films on Pt/Ti/SiO₂/Si substrates. Using the impedance spectroscopy technique, it has been suggested that the high dielectric constant response of the CCTO thin films originates from the grain boundary layer mechanism as found in internal barrier layer capacitors. PACS 77.55.+f; 81.15.Fg; 68.55.-a     

Amorphous Si/insulator multilayers grown by vacuum deposition and electron cyclotron resonance plasma treatment

a-Si/insulator multilayers have been deposited on (0 0 1) Si by electron gun Si evaporation and periodic electron cyclotron resonance plasma oxidation or nitridation. Exposure to an O or N plasma resulted in the formation of a thin SiO₂ and SiN_x layer whose thickness was self-limited and controlled by process parameters. For thin-layer (2 nm) Si/SiO₂ and Si/SiN_x multilayers no visible photoluminescence (PL) was observed in most samples, although all exhibited weak “blue” PL. For the nitride multilayers, annealing at 750°C or 850°C induced visible PL that varied in peak energy with Si layer thickness. Depth profiling of a-Si caps on thin insulating layers revealed no detectable contamination for the SiN_x layers, but substantial O contamination for the SiO₂ films.     

Influence of annealing temperature on structural,electrical and optical properties of WSi2

WSi₂ polycrystalline films of different thicknesses were prepared by low pressure chemical vapor deposition on silicon wafers, and their crystallization properties were studied as a function of the annealing temperature. Structural measurements were performed by X-ray diffraction, detailing for the first time the phase transition from the amorphous to the hexagonal structure at an annealing temperature 380° C and from hexagonal to tetragonal above 700° C. The electrical sheet resistance showed the same transition temperatures.Optical characterization was performed by spectroscopic ellipsometry, and the real and imaginary part of the complex refractive index were obtained as a function of the annealing temperature in the 0.25–0.9 m wavelength range. A broad optical band was found for samples annealed up to 700° C, while for higher annealing temperatures a transparency region for wavelengths greater than 0.5 m and some significant structures appear. A corresponding behavior was observed in the infrared reflectance spectra. Furthermore, it was shown that the determination of the thickness of SiO₂ grown on WSi₂ requires a multilayer model, taking into account the transparency of tetragonal WSi₂.     

Optical and mechanical properties of AlF3 films produced by pulse magnetron sputtering of Al targets with CF4/O2 gas

In this study, AlF₃ thin films were deposited by pulse magnetron sputtering of Al targets with different ratios of CF₄/O₂ gas and at different sputtering powers. The optical and mechanical properties of the AlF₃ thin films were analyzed. The transmittance spectra showed no obvious negative inhomogeneous refractive indices. Denser films with a low optical absorption were obtained when high sputtering powers were used (larger than 30 W). The lowest extinction coefficient (7.3 × 10⁻⁴ at 193 nm) of the films can be reached with 12 sccm O₂ flow rate and at 160W sputtering power. All of the residual stresses were compressive and their trends were consistent with the refractive indices. The lowest compressive stress (0.068 GPa) was obtained when the AlF₃ films were prepared at 160W sputtering power.     

Thermal behaviour of Co/Si/W/Si multilayers under rapid thermal annealing

The e-beam deposited multilayers (MLS) were studied under rapid thermal annealing (RTA) between 250°C and 1000°C during 30 s. MLS with five Co/Si/W/Si periods, each 13.9 nm (MLS1) and 18 nm (MLS2) were deposited onto oxidized Si substrates. Samples were analyzed by X-ray diffraction, hard and soft X-ray reflectivity measurements and grazing incidence X-ray diffuse scattering. The MLS period, interface roughness and its lateral and vertical correlations were obtained by simulation of the hard X-ray reflectivity and diffuse scattering spectra. The MLS1 with thinner Co layers is more temperature resistant. However, its soft X-ray reflectivity is smaller. The results show that this is because of shorter lateral and vertical correlation lengths of the interface roughness which may considerably influence the X-ray reflectivity of multilayers.