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。     

一种软X射线多层膜界面粗糙度的计算方法

提出一个利用多层膜小角X射线衍射谱衍射峰积分强度计算多层膜界面粗糙度的公式。用磁控溅射技术制备Mo／Si多层膜，用波长为0．154nm的硬X射线测量样品在小掠入射角区的衍射曲线，分别用本文公式和反射率曲线拟合方法计算了样品的界面粗糙度。实验结果表明：由本文公式获得的界面粗糙度近似于拟合方法获得的界面粗糙度，它们略等于多层膜界面实际粗糙度。     

4.48 nm正入射软X射线激光用Cr/C多层膜高反射镜的研制

针对4.48nm类镍钽软X射线激光及其应用实验,设计制备了工作于这一波长的近正入射多层膜高反射镜。选择Cr/C为制备4.48nm高反射多层膜的材料对,通过优化设计,确定了多层膜的周期、周期数以及两种材料的厚度比。模拟了多层膜非理想界面对高反射多层膜性能的影响。采用直流磁控溅射方法在超光滑硅基片上实现了200周期Cr/C多层膜高反射镜的制备。利用X射线衍射仪测量了多层膜结构,在德国BessyⅡ同步辐射上测量了在工作波长处多层膜反射率,测量的峰值反射率达7.5%。对衍射仪测量的掠入射反射曲线和同步辐射测量的反射率曲线分别进行拟合,得到的粗糙度和厚度比的结果相近。测试结果表明,所制备的Cr/C多层膜样品结构良好,在指定工作波长处有较高的反射峰,达到了设计要求。     

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.     

水窗波段反射式偏振光学元件的设计和制作

水窗波段是软X射线进行生物活细胞显微成像的最佳波段,因此对于水窗波段偏振光学元件的研究有着非常重要的意义。用菲涅耳公式计算出在水窗波段内不同材料组合对应不同波长的最大反射率,模拟分析了多层膜周期和表界面粗糙度对多层膜偏振光学元件性能的影响。用超高真空磁控溅射镀膜设备,制作出2．40nm、3．00nm和4．30nm波长处W／B4C多层膜偏振元件,并用X射线衍射仪对元件的周期厚度进行了测量,得到的测量结果与设计值偏差很小,可以进行实际应用。为水窗波段反射式偏振光学元件的研究提供了理论依据,同时也为相应偏振光学元件的制备确定了合适的工艺参量。     

小波变换表征多层膜氧化层、界面层和膜厚漂移

用小波变换的方法分析了纳米多层膜的X射线掠入射反射率测试曲线.从小波变换的自相关函数峰位和峰强度信息中得到了常规曲线拟合方法难以表征的含有氧化层、界面层或厚度漂移的多层膜结构,利用其作为多层膜的初始结构再进行常规的曲线拟合,可实现多层膜结构精确表征的目的.研究成功地鉴别出钒单层膜的表面存在约3 nm厚的氧化层,分析得到Mo/Si多层膜的界面纯粗糙度约0.42 nm,表明在Ni/C多层膜中接近表面和基底的膜层存在大于5%的厚度漂移.     

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。     

入射光单色性与界面粗糙度对多层膜反射性能的不同影响

多层膜界面粗糙度、入射光单色性对软X射线多层膜实际反射率均有影响。利用数学卷积积分,理论上推导出一个在入射光不同单色性下精确计算多层膜反射率的公式。利用给出的理论计算公式,简要分析了入射光不同单色性、不同界面粗糙度对Mo/Si多层膜反射率的影响。理论分析发现这两种因素对Mo/Si多层膜反射率影响完全不同:入射光低的单色性不但极大降低Mo/Si多层膜峰值反射率,而且使反射曲线的半峰全宽增加;而界面粗糙度是降低Mo/Si多层膜反射曲线上各点对应值,基本不改变Mo/Si反射曲线的半峰全宽,不改变反射曲线的形状。说明这两个因素在软X射线的长波段对多层膜反射性能的影响不同。     

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...     

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%。     

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。     

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.     

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.     

The effect of capping layers on low-angle Bragg peaks from copper-cobalt multilayers

Using simulations based on the Parratt theory for grazing incidence X-ray specular reflectivity, we show that small variations in the thickness of the gold cap used to prevent oxidation in Co/Cu multilayers can have a dramatic effect on the height and position of the low-order Bragg peaks from these multilayers. The height of the specular Bragg peak cannot be used as a measured of interface roughness nor its position used to determine multilayer period unless the cap thickness is known or determined precisely by simulation.     

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.     

ZnO thin film characterization by X-ray reflectivity optimization using genetic algorithm and Fourier transformation

Zinc oxide (ZnO) thin film was fabricated by sol-gel spin coating method on glass substrate. X-ray reflectivity (XRR) and its optimization have been used for characterization and extracting physical parameters of the film. Genetic algorithm (GA) has been applied for this optimization process. The model independent information was needed to establish data analyzing process for X-ray reflectivity before optimization process. Independent information was exploited from Fourier transform of Fresnel reflectivity normalized X-ray reflectivity. This Fourier transformation (Auto Correlation Function) yields thickness of each coated layer on substrate. This information is a keynote for constructing optimization process. Specular X-ray reflectivity optimization yields structural parameters such as thickness, roughness of surface and interface and electron density profile of the film. Acceptable agreement exists between results obtained from Fourier transformation and X-ray reflectivity fitting.     

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。     

Analysis of periodic Mo/Si multilayers: Influence of the Mo thickness

A set of Mo/Si periodic multilayers is studied by non-destructive analysis methods. The thickness of the Si layers is 5 nm while the thickness of the Mo layers changes from one multilayer to another, from 2 to 4 nm. This enables us to probe the effect of the transition between the amorphous and crystalline state of the Mo layers near the interfaces with Si on the optical performances of the multilayers. This transition results in the variation of the refractive index (density variation) of the Mo layers, as observed by X-ray reflectivity (XRR) at a wavelength of 0.154 nm. Combining X-ray emission spectroscopy (XES) and XRR, the parameters (composition, thickness and roughness) of the interfacial layers formed by the interaction between the Mo and Si layers are determined. However, these parameters do not evolve significantly as a function of the Mo thickness. It is observed by diffuse scattering at 1.33 nm that the lateral correlation length of the roughness strongly decreases when the Mo thickness goes from 2 to 3 nm. This is due to the development of Mo crystallites parallel to the multilayer surface.