提高极紫外光谱纯度的多层膜设计及制备

极紫外光刻是实现22nm技术节点的候选技术。极紫外光刻使用的是波长为13.5nm的极紫外光,但在160～240nm波段,极紫外光刻中的激光等离子体光源光谱强度、光刻胶敏感度以及多层膜的反射率均比较高,光刻胶在此波段的曝光会降低光刻系统的光刻质量。从理论和实验两方面验证了在传统Mo/Si多层膜上镀制SiC单层膜可对极紫外光刻中的带外波段进行有效抑制。通过使用X射线衍射仪、椭偏仪以及真空紫外(VUV)分光光度计来确定薄膜厚度、薄膜的光学常数以及多层膜的反射率,设计并制备了[Mo/Si]40SiC多层膜。结果表明,在极紫外波段的反射率减少5%的前提下,带外波段的反射率减少到原来的1/5。     

Characterization of EUV periodic multilayers

Nanometric Co/Mg, Co/Mg/B₄C, Al/SiC and Al/Mo/SiC periodic multilayers deposited by magnetron sputtering are studied in order to correlate their optical performances in the extreme ultraviolet (EUV) range to their structural quality. To that purpose, our recently developed methodology based on high‐resolution X‐ray emission spectroscopy (XES) and X‐ray and EUV reflectometry is now extended to nuclear magnetic resonance (NMR) spectroscopy and time‐of‐flight secondary ions mass spectrometry (ToF‐SIMS). The analysis of the Co Lαβ and Mg Kβ emission spectra shows that the Co and Mg atoms within the multilayers are in a chemical state equivalent to that of the atoms in the pure Co and Mg references, respectively. But NMR spectra give evidence for a reaction between Co atoms and B and/or C atoms from B₄C. The Al and Si Kβ emission spectra do not reveal the formation of an interfacial compound in Al/SiC and Al/Mo/SiC. Only the roughness limits the optical quality of Al/SiC. The comparative analysis of the ToF‐SIMS spectra of Al/SiC and Al/Mo/SiC indicates that the structural quality is enhanced when Mo is introduced within the stack. Copyright © 2011 John Wiley & Sons, Ltd.     

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.     

低原子序数材料窄带多层膜的研制

为研制极紫外波段窄带多层膜反射镜,采用低原子序数材料组合设计了30.4 nm波长处Mg/SiC,Si/SiC,Si/B4C和Si/C多层膜反射镜,并与极紫外波段传统的Mo/Si多层膜反射镜进行对比。采用直流磁控溅射技术制备了这些多层膜,在国家同步辐射实验室辐射与计量光束线完成了多层膜反射率测量,测量结果表明:Mg/SiC多层膜的带宽最小,为1.44 nm,且反射率最高,为44%;而Mo/Si多层膜的反射率仅为24%,带宽为3.11 nm。实验结果证明了采用低原子序数材料组成的多层膜的带宽要比常规多层膜窄,该方法可以应用于极紫外波段高分辨研究。     

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。     

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%。     

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.     

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。     

The thermal stability of Al(1%wtSi)/Zr EUV mirrors

Six Al(1%wtSi)/Zr multilayers are deposited on Si substrates by using the direct-current magnetron sputtering system, and annealed from 100?°C to 500?°C temperature in a vacuum furnace for 1?h. To evaluate the thermal stability of Al(1%wtSi)/Zr multilayers, the multilayers were characterized by grazing incidence X-ray reflectance, X-ray diffraction, X-ray emission spectroscopy, and near-normal incident extreme ultraviolet (EUV) reflection. The symmetric and asymmetric interlayer models are used to present the interfacial structure before and after 300?°C. The Al(1%wtSi)/Zr multilayer annealed up to 200?°C maintains the initial symmetric multilayer structure, and keeps almost the similar EUV reflectivity as the nonannealed sample. From 300?°C, interdiffusion is much greater at the Zr/Al interface compared with the Al/Zr interface. And the interfacial phases of Al-Zr alloy transform from amorphous to polycrystalline, which induces the deterioration of multilayer structure and the decrease of EUV reflectivity. However, up to 500?°C, the polycrystalline Al-Zr compound does not destroy the multilayer completely.     

Thermal cycles, interface chemistry and optical performance of Mg/SiC multilayers

The interplay between optical performance and the thermally activated interface chemistry of periodic Mg/SiC multilayers designed for application at 30.4 nm are investigated by optical (hard X-ray, soft X-ray and ultraviolet ranges, i.e. from 0.154 to 30.4 nm) reflectivity and X-ray emission spectroscopy. The multilayers are prepared by magnetron sputtering and then annealed up to a temperature of 500 °C. Two clear changes take place in the multilayer upon annealing. At first, between 200 and 300 °C a strong decrease of the reflectivity is observed, due to the development of interfacial roughness following the crystallization of the Mg layers. No interfacial compound is detected. Then, between 350 and 400 °C there is formation of the Mg₂Si magnesium silicide at the interfaces following the reaction between the Mg and SiC layers. This also leads to the almost total loss of reflectivity of the multilayer. Thus, this kind of multilayer is thermally stable only for application requiring no heating above 200 °C.     

An etched multilayer as a dispersive element in a curved‐crystal spectrometer: implementation and performance

Etched multilayers obtained by forming a laminar grating pattern within interferential multilayer mirrors are used in the soft X‐ray range to improve the spectral resolution of wavelength dispersive spectrometers equipped with periodic multilayers. We describe the fabrication process of such an etched multilayer dispersive element, its characterization through reflectivity measurement and simulations, and its implementation in a high‐resolution Johann‐type spectrometer. The specially designed patterning of a Mo/B₄C multilayer is found fruitful in the range of the C K emission as the diffraction pattern narrows by a factor 4 with respect to the non‐etched structure. This dispersive element with an improved spectral resolution was successfully implemented for electronic structure study with an improved spectral resolution by X‐ray emission spectroscopy. As first results, we present the distinction between the chemical states of carbon atoms in various compounds, such as graphite, SiC and B₄C, by the different shape of their C K emission band. Copyright © 2012 John Wiley & Sons, Ltd.     

Comparative study of multilayers used in monochromators for synchrotron‐based coherent hard X‐ray imaging

A systematic study is presented in which multilayers of different composition (W/Si, Mo/Si, Pd/B₄C), periodicity (from 2.5 to 5.5 nm) and number of layers have been characterized. In particular, the intrinsic quality (roughness and reflectivity) as well as the performance (homogeneity and coherence of the outgoing beam) as a monochromator for synchrotron radiation hard X‐ray micro‐imaging are investigated. The results indicate that the material composition is the dominating factor for the performance. By helping scientists and engineers specify the design parameters of multilayer monochromators, these results can contribute to a better exploitation of the advantages of multilayer monochromators over crystal‐based devices; i.e. larger spectral bandwidth and high photon flux density, which are particularly useful for synchrotron‐based micro‐radiography and ‐tomography.     

含n＝k超薄金属膜的周期对称膜系的性质及窄带高反膜设计

本文阐述了n≈k的超薄金属膜与介质膜组成周期对称膜系的光学特性,并结合Ag、Al等膜层的高反特性提出了可见光区诱导窄带高反膜系结构,推导出膜系的反射率、反射峰值、反射半波带宽等光谱反射特性的近似公式,实验证实了理论设计和分析.同时也提出了设计红外和紫外窄带高反滤光片的方法.     

19.5nm极紫外反射镜的研制

介绍了一种用于太阳观测19.5nm极紫外多层膜的研究工作。利用软件对规整的Mo/Si膜系结构进行了优化,拓宽了反射带宽,提高了积分反射率。采用双离子束溅射技术,时间控厚,成功制备了该反射镜。通过同步辐射反射率计测试表明,峰值反射率27.5%,均匀性在1%以内,已初步达到预设要求。     

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。     

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.     

Mo/Si多层膜表面保护层设计

为提高Mo/Si多层膜的稳定性与使用寿命,通过分析多层膜驻波电场的分布,对表面保护层及多层膜最上层材料的厚度进行优化设计,使优化后的反射率最高.计算表明,一定厚度的表面保护层总对应一个最优的最上层材料厚度.在13.36 nm波长,膜对数为50的Mo/Si多层膜10度入射的理论反射率为74.47%;当添加厚度为2.3 nm的Ru作为表面保护层,对应多层膜最上层Si的优化厚度为3.93 nm,其理论反射率为75.20％.设计结果表明,通过优化设计表面保护层,可以提高多层膜稳定性,改善多层膜性能.     

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 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.     

短波长软X射线多层膜高级次峰设计与制备

考虑了短波长软X射线多层膜的设计问题，比较了一、二、三级布喇格衍射峰设计的反射率结果，分析了反射率与周期厚度及金属层在周期中的比率的关系．本文认为，在存在不连续金属膜层的情况下，用布喇格衍射峰的二级次设计，有助于获得实测的反射率．给出了利用磁控溅射方法沉积的Mo/Si多层膜在4.47nm处同步辐射测量，在60°入射角下获得8.5%实测反射率的结果． 关键词：