退火温度对Ta_2O_5/SiO_2多层反射膜结构和应力特性的影响

介质膜反射镜是星载激光测高仪系统中不可缺少的薄膜元件,其面形质量直接影响探测系统测距的分辨率和精度.本文采用离子束辅助电子束蒸发工艺在石英基底上沉积Ta_2O_5/SiO_2多层反射膜,并在200—600℃的空气中做退火处理.通过X射线衍射、原子力显微镜、分光光度计及激光干涉仪等测试手段,系统研究了退火温度对Ta_2O_5/SiO_2多层反射膜结构、光学性能以及应力特性的影响.结果表明:Ta_2O_5/SiO_2多层反射膜退火后,膜层结构保持稳定,膜层表面粗糙度得到有效改善;反射膜在500—600℃退火后,残余应力由压应力向张应力转变;采用合适的退火温度可以有效释放Ta_2O_5/SiO_2薄膜的残余应力,使薄膜与基底构成的介质膜反射镜具有较好的面形精度.本文的实验结果对退火工艺在介质膜反射镜面形控制技术方面的应用具有重要意义.     

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。     

用不同的Mo靶溅射功率制备Mo/Si多层膜

 用磁控溅射法制备了周期厚度和周期数均相同的Mo/Si多层膜，用原子力显微镜和小角X射线衍射分别研究了Mo靶溅射功率不相同时，Mo/Si多层膜表面形貌和晶相的变化。随后在国家同步辐射实验室测量了Mo/Si多层膜的软X射线反射率。研究发现，随着Mo靶溅射功率的增大，Mo/Si多层膜的表面粗糙度增加，Mo的特征X射线衍射峰也增强，Mo/Si多层膜的软X射线峰值反射率先增大后减小。     

溅射气压对X射线多层膜反射率的影响

本文在不同的溅射气压的情况下制备了具有相同结构参量的Mo/Si多层膜,测出了其对应的小角度X衍射曲线,在北京同步辐射实验室测量了多层膜的软X射线反射率.小角X射线衍射谱表明:随着溅射气压升高,多层膜的小角X射线衍射曲线的高次峰的峰高急剧变小,半峰宽变大.反射率测量结果也表明:多层膜的X射线反射率随溅射气压的升高而急剧降低.     

研究扩散屏障层对Mo/Si多层膜软X射线反射率影响的模拟

在特定波长下,用四层结构模型模拟了Mo/Si多层膜的软X射线反射率.研究了扩散屏障层dMo-on-Si和dSi-on-Mo对Mo/Si多层膜软X射线反射率的影响.研究发现,扩散屏障层并不总是损害Mo/Si多层膜的光学性能,通过合理设计dMo-on-Si和dSi-on-Mo厚度,增加dMo-on-Si与dSi-on-Mo的比值,也能提高多层膜的软X射线反射率.     

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%。     

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     

中心波长为28.5nm多层膜镜反射率测量

在“星光-Ⅱ”装置上以类Ne铬x射线激光作为标定源，以平场光栅谱仪为分光元件进行了285nm的Mo/Si多层膜反射镜效率测量.介绍了实验方法，给出了实验结果，本次研制的两块多层膜镜反射率分别为31%和9.6%. 关键词： x射线多层膜反射镜 反射率测量 x射线激光     

50～11O 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.     

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.     

Characterization of ion beam sputter deposited W and Si films and W/Si interfaces by grazing incidence X-ray reflectivity, atomic force microscopy and spectroscopic ellipsometry

An ion beam sputtering system, which uses a commercial ECR microwave based plasma ion source, has been designed and fabricated in-house for deposition of soft X-ray multilayer mirrors. To begin with, in the ion beam sputtering system W, Si thin films, W/Si bi-layer and W/Si/W tri-layer samples have been deposited on c-Si substrates as precursors to W/Si multilayer stack. The samples have been characterized by grazing incidence X-ray reflectivity (GIXR), atomic force microscopy (AFM) and spectroscopic ellipsometry (SE) techniques. By analyzing the results, density, thickness, surface roughness of the single layer samples and interface width of the bi-layer and tri-layer samples have been estimated.     

质子辐照下Mo/Si多层膜反射镜的微观结构状态

利用透射电子显微镜对质子辐照前后空间太阳望远镜Mo/Si多层膜的微观结构进行了表征, 并对其辐照前后反射率的变化进行了测量.研究表明, Mo/Si多层膜经质子辐照后形成了一些缺陷结构,局部区域Mo/Si的周期性遭到破坏, Mo层与Si层的宽度发生了变化,多层膜层与层之间的界面也比辐照前更为粗糙,部分层状结构由于质子辐照发生了明显的扭曲和折断等现象;此外,质子辐照导致了Mo/Si多层膜反射率的下降,这些微观缺陷的形成是光学性能降低的直接诱因. 关键词： 空间太阳望远镜 Mo/Si多层膜 微观结构 反射率     

13 nm窄带Si/Mo/C多层膜反射镜

基于多层膜准单色覆盖50~1500 eV能谱的多能点发射光谱测量系统可获得聚龙一号装置Z-pinch等离子体X射线源的能谱结构和总能量等信息。考虑装置的条件,在13 nm处的多层膜需要工作在掠入射角60。常规的Mo/Si多层膜尽管反射率最高,但其带宽较大,不能满足多层膜准单色的要求。因此提出将Mo和C共同作为多层膜的吸收层材料与Si组成Si/Mo/C多层膜,可使反射率降低较小而带宽明显减小。采用磁控溅射方法制备了Si/Mo/C多层膜,其掠入射X射线反射测量表面多层膜的结构清晰完整,同步辐射工作条件下反射率测量,得到Si/Mo/C多层膜在13 nm处和掠入射角60时的反射率为56.5%,带宽为0.49 nm（3.7 eV）。     

Ion beam sputter deposited W/Si multilayers: Influence of re-sputtering on the interface structure and structure modification at ultra short periods

X-ray multilayer mirrors of period ranging from 9.6 to 1.7 nm, deposited using ion beam sputtering, have been examined using grazing incidence X-ray reflectivity (GIXRR) and grazing incidence X-ray diffraction. Detailed analysis of GIXRR data revealed that significant amount of re-sputtering of Si layer takes place while W deposition is underway. Re-sputtering is mainly due to bombardment of high-energy neutrals getting reflected from the W target. Due to re-sputtering interface of the multilayer becomes asymmetric. This puts a major hindrance in avoiding the intermixing and achieving sharp interfaces at shorter periods. Maximum thickness of Si which gets lost due to re-sputtering during deposition is ∼0.8 nm. The shortest period multilayer estimated, that could be deposited without intermixing, was 2.7 nm. These results are of significance for developing low period W/Si multilayers.     

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。     

Design and performance of two-channel EUV multilayer mirrors with enhanced spectral selectivity

In this paper, we present a study on two-channel multilayer mirrors which can operate at two wavelengths in Extreme Ultraviolet (EUV) spectral range. We propose a new method to design two-channel EUV multilayer mirrors with enhanced spectral selectivity. The mirror structure is a stack of two periodic multilayers separated by a buffer layer. We have defined the main parameters which allow adjustment of the distance between different order Bragg’s peak and of wavelength positions of reflectivity minima. Two mirrors have been designed and deposited for solar EUV telescope applications by using this method. The first mirror reflects Fe IX–X line (17.1 nm) and Fe XVI (33.5 nm) lines with attenuation of the He II line (30.4 nm). The second mirror reflects Fe IX–X and He II lines with attenuation of Fe XV (28.4 nm) and Fe XVI lines. Measurements with synchrotron radiation source confirm that, in both cases, for these mirrors, we are able to adjust reflectivity maxima (Bragg peak position) and minima. Such multilayers offer new possibilities for compact design of multi-wavelength EUV telescopes and/or for high spectral selectivity.     

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.     

Mo/Si软X射线多层膜的界面粗糙度研究

 用磁控溅射法分别制备了以Mo膜层和Si膜层为顶层的Mo/Si多层膜系列, 利用小角X射线衍射确定了各多层膜的周期厚度。以不同周期数的Mo/Si多层膜的新鲜表面近似等同于同一多层膜的内界面，通过原子力显微镜研究了多层膜界面粗糙度随膜层数的变化规律。并在国家同步辐射实验室测量了各多层膜的软X射线反射率。研究表明：随着膜层数的增加，Mo膜层和Si膜层的界面粗糙度先减小后增加然后再减小，多层膜的峰值反射率先增加后减小。     

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.     

30.4 nm波长SiC/Mg多层膜反射镜

波长30.4 nm的He-II谱线是极紫外天文观测中最重要的谱线之一,空间极紫外太阳观测光学系统需要采用多层膜作为反射元件。为此研究了SiC/Mg、B4C/Mg、C/Mg、C/Al、Mo/Si、B4C/Si、SiC/Si、C/Si、Sc/Si等材料组合的多层膜在该波长处的反射性能。基于反射率最大与多层膜带宽最小的设计优化原则,选取了SiC/Mg作为膜系材料。采用直流磁控溅射技术制备了SiC/Mg多层膜,用X射线衍射仪测量了多层膜的周期厚度,用国家同步辐射计量站的反射率计测量了多层膜的反射率,在入射角12°时,实测30.4 nm处的反射率为38.0%。