极紫外与软X射线用非晶碳膜全反射镜的研究

用高真空磁控溅射设备分别在工作气压为0.40Pa和0.67Pa下制备了非晶碳膜全反射镜样品,利用X射线掠入射反射测量了膜层厚度、粗糙度和膜层密度,用原子力显微镜测量了样品的表面粗糙度,用同步辐射测量了不同工作气压下制备的非晶碳膜全反射镜的反射率,并对测量结果进行了分析讨论.测试结果表明:在0.40Pa工作气压下制备的非晶碳膜反射镜的性能优于在0.67Pa工作气压下制备的反射镜的性能,在掠入射角小于4.5°时,非晶碳膜全反射镜在5nm以上波段有比较平坦的高反射率,在波长小于5nm波段,反射率急剧下降.     

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%。     

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%。     

磁控溅射法制备极紫外6.8～11.0nm波段Mo/B_4C横向梯度多层膜（英文）

用直流磁控溅射法结合掩模板控制膜厚的方法在Si衬底上制备了工作于6.8～11.0nm波段的[Mo/B_4C]60横向梯度多层膜。利用X射线掠入射反射测试以及同步辐射反射率测试对梯度多层膜的结构及性能进行了测试。X射线掠入射反射测试结果表明,多层膜周期厚度沿着长轴方向从4.39nm逐渐增加到7.82nm,周期厚度平均梯度为0.054nm/mm。对横向梯度多层膜沿长轴方向每隔5mm进行了一次同步辐射反射率测试,结果显示,横向梯度多层膜在45°入射角下的反射率约为10%,反射峰的半高全宽介于0.13nm到0.31nm之间。     

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.     

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。     

23.4nm软X射线多层膜反射镜研制

为了满足类氖-锗X射线激光研究的需要,设计制备了23.4 nm软X射线多层膜反射镜.依据多层膜选材原则并考虑材料的物理化学特性选择新的材料Ti与Si组成材料对.设计优化材料多层膜的周期厚度(d),材料比例(Γ),周期数(N),计算出Ti/Si反射率曲线.通过实验优化各种镀膜工艺参数,制备出了23.4 nm的Ti/Si多...     

30.4 nm波长处Mg基多层膜反射镜

太阳光谱中重要的He-Ⅱ谱线(波长30.4 nm)的观测对于研究太阳活动和日地空间环境具有重要意义,实现空间极紫外太阳观测需要采用多层膜作为反射元件.研究了工作在30.4 nm的Mg基多层膜.以反射率最高为评价函数设计了多层膜,采用直流磁控溅射技术制备了SiC/Mg,B4C/Mg和C/Mg多层膜,用X射线衍射仪测量了多层膜的结构.研究表明虽然B4C/Mg多层膜理论反射率最高,但实际制备结果显示,SiC/Mg多层膜的成膜质量最好,反射率最高.同步辐射反射率测量表明:在入射角10°时实测的SiC/Mg多层膜反射率为44.6%.     

磁控溅射法制备极紫外6.8~11.0 nm波段Mo/B4C横向梯度多层膜

用直流磁控溅射法结合掩模板控制膜厚的方法在Si衬底上制备了工作于6.8~11.0 nm波段的[Mo/B₄C]₆₀横向梯度多层膜。利用X射线掠入射反射测试以及同步辐射反射率测试对梯度多层膜的结构及性能进行了测试。X射线掠入射反射测试结果表明,多层膜周期厚度沿着长轴方向从4.39 nm逐渐增加到7.82 nm,周期厚度平均梯度为0.054 nm/mm。对横向梯度多层膜沿长轴方向每隔5 mm进行了一次同步辐射反射率测试,结果显示,横向梯度多层膜在45°入射角下的反射率约为10%,反射峰的半高全宽介于0.13 nm到0.31 nm之间。     

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。     

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。     

软X射线Mo/Si多层膜反射率拟合分析

由于多层膜的表界面粗糙度和材料之间的相互扩散等因素，导致多层膜的实际反射率小于理论计算的反射率，因此，多层膜结构参量的确定对镀膜工艺参量的标定具有重要意义。由于描述单个非理想粗糙界面散射的Stearns法适用于软X射线短波段区域，采用它的数学模型来描述软X射线多层膜的粗糙度，利用最小二乘法曲线拟合法对同步辐射测得的Mo／Si多层膜的反射率曲线进行拟合，得到了非常好的拟合结果，从而确定了多层膜结构参量，同时分析了多层膜周期厚度，厚度比率，界面宽度以及仪器光谱分辨率对多层膜反射特性的影响，这些工作都为镀膜工艺改进提供了一定的理论依据。     

Thin multilayers characterization by grazing X-ray reflectometry and use of Fourier transform

Grazing X-ray reflectometry is used in order to characterize thin layer stacks, in particular periodic multilayers. The specular reflectivity depends on the thickness, the complex refractive index of each layer and on the roughness of the interfaces. By a trial and error method, the experimental reflectivity curve can be fitted with a theoretical one, and so, the parameters of the stack can be obtained. This numerical method needs usually initial guess of the kind of results.Fourier transform method allows to obtain directly the values of distances between interfaces, with a good approximation depending on the maximum angular scan of the measure. It can also reveal some particularity of the multilayer, i.e. periodic multilayered structures with more than two layers per period. As an illustration of this characterization method, some examples in XUV optical domain will be shown. This method can also be used for the characterization of many kinds of multilayer stacks, in particular semi-conductor heterostructures ones, under the condition that adjacent layers have sufficient contrast index at the wavelength of the X-ray source.     

X-ray standing waves in a multi-trilayer system with linearly varying period

Generation of X-ray standing waves in a multi-trilayer system with a varying periodicity along its depth is described. Microstructures of a synthetic 15-period Pt/Ni/C multilayer, which has such a varying periodicity, are investigated using X-ray reflectivity (XRR) and X-ray standing wave (XSW) analysis. Microstructural parameters, e.g., thicknesses and electron densities of individual layers, interface roughnesses, varying periodicity along the depth, etc. are precisely determined by the XRR technique. The variation of period is essentially introduced in multilayer fabrication by varying the thickness of the C-layer as a function of depth. The linear increase in C-layer thickness from the bottom of the multilayer towards the surface of the multilayer structure is found by simulating the XRR data with a depth-graded multilayer model. Intensity of the XSW field is computed as a function of depth over the first order Bragg peak. Integrated intensities over the Pt- and the Ni-layers are computed and compared with the measured fluorescence yield from Pt and Ni. Sensitivity for the detection of inter-atomic diffusion across the interfaces in comparison to multi-bilayer systems, such as Pt/C multilayer, is discussed.     

Interface roughness, surface roughness and soft X-ray reflectivity of Mo/Si multilayers with different layer number

A series of Mo/Si multilayers with the same periodic length and different periodic number were prepared by magnetron sputtering, whose top layers were respectively Mo layer and Si layer. Periodic length and interface roughness of Mo/Si multilayers were determined by small angle X-ray diffraction (SAXRD).Surface roughness change curve of Mo/Si multilayer with increasing layer number was studied by atomic force microscope (AFM). Soft X-ray reflectivity of Mo/Si multilayers was measured in National Synchrotron Radiation Laboratory (NSRL). Theoretical and experimental results show that the soft X-ray reflectivity of Mo/Si multilayer is mainly determined by periodic number and interface roughness, surface roughness has little effect on reflectivity.     

同步辐射掠出射X射线荧光分析薄膜膜厚

掠射X射线荧光分析为薄层和多层膜特性分析提供了潜在的可能. 尤其是可以探测膜层厚度、界面形貌和组成. 以北京同步辐射光源作激发光源, 采用掠出射方法测试了Si基片上不同厚度的单层Cr膜样品, 测试结果与理论计算基本符合. 同时观察到一定厚度的薄膜样品产生的掠出射X射线荧光的干涉现象.     

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.     

14.5% near-normal incidence reflectance of Cr/Sc x-ray multilayer mirrors for the water window

Cr/Sc multilayer mirrors, synthesized by ion-assisted magnetron sputter deposition, are proved to have a high near-normal reflectivity of R = 14.5% at a grazing angle of 87.5 degrees measured at the wavelength lambda = 3.11 nm, which is an improvement of more than 31% compared with previously published results. Elastic recoil detection analyses show that the mirrors contained as much as 15 at. % of N and traces of C and O. Soft x-ray reflectivity simulations reveal interface widths of sigma = 0.34 nm and an exceptionally small layer thickness drift of approximately 1.6 x 10(-5) nm/multilayer period throughout the stack. Simulations show that a reflectivity of R = 25.6% is attainable if impurities and layer thickness drift can be eliminated. The abrupt interfaces are achieved with ion assistance with a low ion energy of 24 eV and high ion-to-metal flux ratios of 7.1 and 23.1 during Cr and Sc sputter deposition, respectively. In addition, a near-normal incidence reflectivity of 5.5% for the C VI emission line (lambda = 3.374 nm) from a laser plasma source was verified.     

周期性梯度折射率多层膜的软X射线反射率

由于界面互扩散的存在，实际的超薄多层膜很难具有清晰的界面结构.假设超薄多层膜为具有周期性梯度折射率的多层膜结构，用直线模型和余弦模型模拟了周期性梯度折射率多层膜的软X射线反射率.结果证明，折射率余弦渐变的多层膜虽然不具有清晰的界面，但它同样具有很高的反射率.