50~110 nm波段高反射率多层膜的设计与制备

阐述了50~110 nm强吸收波段亚四分之一波长多层膜的设计方法.这种膜系是由强吸收材料叠加而成，每层膜光学厚度小于四分之一个波长.与常规周期多层膜相比，这种膜系更适用于提高强吸收波段的反射率.利用该方法设计了50 nm处高反射多层膜，并以此为初始条件通过Levenberg-Marquart优化方法完成了50~110 nm强吸收波段宽带高反射率Si/W/Co多层膜的设计，其平均反射率达到45%.采用直流磁控溅射方法制备了Si/W/Co多层膜,用X射线衍射仪(XRD)对膜层结构进行了测试，测试结果表明制作出的多层膜结构与设计结构基本相符.     

Terbium-based extreme ultraviolet multilayers

We have fabricated periodic multilayers that comprise either Si/Tb or SiC/Tb bilayers, designed to operate as narrowband reflective coatings near 60 nm wavelength in the extreme ultraviolet (EUV). We find peak reflectance values in excess of 20% near normal incidence. The spectral bandpass of the best Si/Tb multilayer was measured to be 6.5 nm full width at half-maximum (FWHM), while SiC/Tb multilayers have a more broad response, of order 9.4 nm FWHM. Transmission electron microscopy analysis of Si/Tb multilayers reveals polycrystalline Tb layers, amorphous Si layers, and relatively large asymmetric amorphous interlayers. Thermal annealing experiments indicate excellent stability to 100 degrees C (1 h) for Si/Tb. These new multilayer coatings have the potential for use in normal incidence instrumentation in a region of the EUV where efficient narrowband multilayers have not been available until now. In particular, reflective Si/Tb multilayers can be used for solar physics applications where the coatings can be tuned to important emission lines such as O V near 63.0 nm and Mg X near 61.0 nm.     

月基极紫外相机多层膜反射镜

月基极紫外相机用于月球表面对地球等离子体层辐射出的30.4 nm谱线进行成像观测,多层膜反射镜是月基极紫外相机的重要光学元件。根据月基极紫外相机技术参数,选择了B₄C/Mg,B₄C/Mg₂Si,B₄C/Al,B₄C/Si,Mo/Si等材料,对其周期厚度、材料比例、周期数等参数进行优化。计算了以上材料组合在30.4 nm的反射率曲线。考虑到月球环境的特殊性和材料的物理化学性质,从中选择出Mo/Si和B₄C/Si两种组合,利用磁控溅射进行镀制。Mo/Si和B₄C/Si多层膜在30.4 nm反射率分别达到15.3%和22.8%。     

Co/C and W/Si multilayers deposited by ion-beam sputtering for the soft X-ray range

We deposited Co/C multilayer mirrors for a wavelength of 4.77 nm and W/Si multilayer mirrors for a wavelength of 1.77 nm by use of ion-beam sputtering. The small-angle diffraction spectrum was used to analyze the structure of the multilayers. With a combination of the experimental diffraction spectra and Apeles’ theory for calculation of the interfacial roughnesses of the multilayers, the interfacial roughnesses of Co/C and W/Si are 0.80 nm and 0.60 nm, respectively, which are lower than that of the substrate. The reflectivity of the Co/C multilayer is measured to be about 20% and that of the W/Si multilayer about 1% at the grazing incidence angle of about 12°. Received: 30 May 2000 / Accepted: 1 August 2000 / Published online: 11 February 2002     

软X射线Mo/B_4C多层膜应力和热稳定性研究

为了实现7nm波段Mo/B4C多层膜反射镜元件的制备,研究了不同退火方式对Mo/B4C多层膜应力和热稳定性的影响。首先,采用直流磁控溅射方法分别基于石英和硅基板制作Mo/B4C多层膜样品,设计周期为3.58nm、周期数为60,Mo膜层厚度与周期的比值为0.4。其次,采用不同的退火方式对所制作的样品进行退火实验,最高退火温度500℃。最后,分别采用X射线掠入射反射、X射线散射和光学干涉仪的方法对退火前后的Mo/B4C多层膜的周期、界面粗糙度和应力进行测试。测试结果表明采用真空退火方式能够有效降低Mo/B4C多层膜的应力,且退火前后Mo/B4C多层膜的周期和界面粗糙度无明显变化,证明Mo/B4C多层膜在500℃以内具有很好的热稳定性。     

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.     

高反射率Mo/B4C多层膜设计及制备

 运用遗传算法优化设计了Mo/B₄C多层膜结构。入射光入射角度取10°时,设计的理想多层膜膜对数为150,周期为3.59 nm,Gamma值（Mo膜厚与周期的比值）为0.41,峰值反射率为33.29%。采用恒功率模式直流磁控溅射方法制作Mo/B₄C多层膜。通过在Mo/B4C多层膜与基底之间增加15 nm厚的Cr粘附层,提高多层膜与基底的粘附力。另外,还采用调整多层膜Gamma值的方法减小其内应力,调整后多层膜结构周期为3.59 nm, Mo膜厚1.97 nm, B4C膜厚1.62 nm,峰值反射率26.34％。制备了膜对数为150的Mo/B₄C膜并测量了其反射率,在波长7.03 nm处,Mo/B₄C多层膜的近正入射反射率为21.0％。最后对测量结果进行了拟合,拟合得到Mo/B₄C多层膜的周期为3.60 nm,Gamma值0.60,界面粗糙度为0.30 nm。     

Influence of interface roughness on reflectivity of tungsten/boron-carbide multilayers with variable bi-layer number by X-ray reflection and diffuse scattering

Infuence of interface roughness on the reflectivity of Tungsten/boron-carbide （W/B4C） multilayers varying with bi-layer number, N, is investigated. For W/B4C multilayers with the same design period thickness of 2.5 nm, a real-structure model is used to calculate the variation of reflectivities with N = 50, 100, 150, and 200, respectively. Then, these multilayers are fabricated by a direct current （DC） magnetron sputtering system. Their reflectivity and scattering intensity are measured by an X-ray diffractometer （XRD） working at Cu Kα line. The X-ray reflectivity measurement indicates that the reflectivity is a function of its bi-layer number. The X-ray scattering measured results show that the interface roughness of W/B4C multilayers increases slightly from layer to layer during multilayer growing. The variation of the reflectivity and interface roughness with bi-layer number is accurately explained by the presented realstructure model.     

Molybdenum-strontium multilayer mirrors for the 8-12-nm extreme-ultraviolet wavelength region

Mo-Sr multilayer mirrors were successfully deposited by dc-magnetron sputtering and characterized in situ with synchrotron radiation. Normal-incidence (3.6 degrees ) reflectance of 23.0% at 8.8 nm, 40.8% at 9.4 nm, and 48.3% at 10.5 nm were measured before the samples were exposed to air. After exposure, as a result of the reactivity of Sr with oxygen and water vapor, the reflectance of these multilayers decreased rapidly. Attempts to use thin layers of C to passivate the surface of these Mo-Sr multilayers were unsuccessful.     

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.     

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.     

X射线W/B4C宽带多层膜的优化设计和制备

介绍了X射线宽带多层膜材料W和B4C的选定方法,依据伯宁(BERNING)公式确定出了在0.154 nm处X射线宽带多层膜的最佳膜对数。引入适当的评价函数,利用具有全局寻优特性且效率较高的遗传算法,在波长0.154 nm处优化设计出了掠入射角(θ)0.5°~0.9°范围内反射率值达到40%的宽角度宽带多层膜。宽带多层膜反射镜采用磁控溅射方法制备,并用X射线衍射仪对样品进行了检测,结果表明在掠入射角(2θ)1.0°~1.8°之间的相对反射率光谱曲线比较平坦。     

同步辐射软X射线多层膜反射偏振元件研究

利用多靶磁控溅射方法分别镀制了W/C和Mo/Si两种周期性结构多层膜。通过对其相关参数周期数、厚度比以及周期厚度的调整,使薄膜的布拉格衍射峰出现在布儒斯特角附近,两种多层膜的应用能量范围分别落于C的近K边处和Si的L边前。在北京同步辐射装置3W1B光束线的软X射线光学实验站上进行了反射率的测量,得到W/C膜的反射率在214eV时达到4.18%;Mo/Si周期性多层膜的反射率在89eV处达到32.3%。根据测量结果,分析了在同步辐射装置作为偏振元件的可行性     

Interface characteristics of Mo/Si and B4C/Mo/Si multilayers using non-destructive X-ray techniques

A methodology combining non-destructive X-ray techniques is proposed to study the interfacial zones of periodic multilayers. The used X-ray techniques are X-ray emission spectroscopy induced by electrons and X-ray reflectivity in the hard and soft X-ray ranges. The first technique evidences the presence of compounds at the interfaces and gives an estimation of the thickness of the interfacial zone. These informations are used to constrain the fit of the X-ray reflectivity curves that enables to determine the thickness and roughness of the various layers of the stacks. The results are validated in the soft X-ray range where the reflectivity curves are very sensitive to the chemical state of the elements present in the stack. The methodology is applied to characterize Mo/Si (1-4 nm/2 nm) and B₄C/Mo/Si (1 nm/2 nm/2 nm) multilayers. It is shown that the two interfacial zones of the Mo/Si multilayers are composed of the silicides MoSi₂ and Mo₅Si₃. It is found that the interface thickness is about to be 0.4-0.8 nm depending on the samples. The molybdenum silicides are also evidenced at the interfaces of the B₄C/Mo/Si multilayers. However, their interface thickness is 0.2 nm thinner than that of the same stack without the B₄C layers, these layers being at the Mo-on-Si side or at the Si-on-Mo side. Thus, the B₄C layers do not stop but only reduce the interdiffusion between the Mo and Si layers.     

B4C/Mo/Si high reflectivity multilayer mirror at 30.4 nm

The B4C/Mo/Si high reflectivity multilayer mirror was designed for He-Ⅱ radiation (30.4 nm) using the layer-by-layer method. The theoretical peak reflectivity was up to 38.2% at the incident angle of 5°. The B4C/Mo/Si multilayer was fabricated by direct current magnetron sputtering and measured at the National Synchrotron Radiation Laboratory (NSRL) of China. The experimental reflectivity of the B4C/Mo/Si multilayer at 30.4 nm was about 32.5%. The promising performances of the B4C/Mo/Si multilayer mirror could be used for the construction of solar physics instrumentation.     

Influence of working gas pressure on the performance of W/Si multilayers

The effect of Ar pressure on the performance of W/Si multilayers is investigated. W/Si multilayers were deposited by a high vacuum DC magnetron sputtering system. The Ar pressure was changed from 1.0 to 5.0 mTorr with an interval of 1.0 mTorr during the deposition process. Electron probe microanalysis and Rutherford backscattering are performed to determine the Ar content incorporated within these multilayers. The results demonstrate that less Ar is incorporated within the sample when more Ar is used in the plasma, which could be explained by the increase of the collision probability and the decrease in the kinetic energy of Ar ions arriving at the substrate when more Ar exists. The grazing incident X-ray reflectivity (GIXR) at 0.154 nm is used to determine the structural parameters of the layers. The results show that the structures of these multilayers prepared at different Ar pressure are very similar and that the interface roughness increases quickly when the Ar pressure is higher than 3.0 mTorr. The measurements of the extreme ultraviolet (EUV) reflectivity indicate that the reflectivity decreases when Ar pressure increases. The fitting results of GIXR and EUV reflectivity curves indicate that with an increase of Ar pressure, the density and decrement of the refractive index are increased for W and decreased for Si, which is mainly due to (1) the decrease in Ar content incorporated within these multilayers which affects their performance and (2) the increase of collision probability for sputtered W and Si, the decrease of their average kinetic energy arriving at the substrate, and thus the loosing of their layers.     

Normal-incidence reflectance of optimized W /B(4) C x-ray multilayers in the range 1.4 nm < l > 2.4 nm

We have fabricated W/B(4)C multilayers having periods in the range d = 0.8-1.2 nm and measured their soft-x-ray performance near normal incidence in the wavelength range 1.4相似文献   

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。     

Subnanometer-scale measurements of the interaction of ultrafast soft x-ray free-electron-laser pulses with matter

At the recently built FLASH x-ray free-electron laser, we studied the reflectivity of Si/C multilayers with fluxes up to 3 x 10(14) W/cm2. Even though the nanostructures were ultimately completely destroyed, we found that they maintained their integrity and reflectance characteristics during the 25-fs-long pulse, with no evidence for any structural changes over lengths greater than 3 A. This experiment demonstrates that with intense ultrafast pulses, structural damage does not occur during the pulse, giving credence to the concept of diffraction imaging of single macromolecules.     

北京同步辐射装置3W1B软X射线光束线偏振特性测量

应用自行研制的Mo/Si周期多层膜作为起偏器和检偏器的光学元件, 测量了北京同步辐射装置3W1B束线的偏振状态. 通过数据分析, 得到了3W1B软X射线的有关偏振参数, 在86—89eV能区经过起偏器后的偏振度超过98%, 圆偏振分量介于1%—3%之间.