软X射线Mo/B4C多层膜应力和热稳定性研究

为了实现7 nm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3.58 nm、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。     

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Mo2C/B4C,Mo/B4C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,Mo2C,B4C单层膜,周期厚度为3.5 nm,30对的Mo2C/B4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Mo2C/B4C多层膜压应力要远小于Mo/B4C多层膜,且成膜质量与Mo/B4C相当。因此Mo2C/B4C是应用于6.7 nm反射镜较好的多层膜材料组合。C,Mo/B4C     

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。     

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。     

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。     

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。     

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.     

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。     

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。     

Mo/B4C软X射线多层膜结构特性研究

在6.7<λ<10.0nm波段选择Mo/B₄C作为多层膜材料,并采用磁控溅射法制备出多层膜样品.这些多层膜样品的周期结构为3.35nm～5.52nm.采用X射线衍射仪和透射电镜(TEM)对样品的微观结构进行研究.结构表明,这些多层膜样品的结构质量很高,并有很好的热稳定性.     

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.     

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.     

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.     

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.     

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.