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。     

Pd2Si的生成对Pd/Si多层膜衍射性能的影响

本文研究了Pd₂Si的生成对周期性Pd/Si多层膜X射线衍射性能的影响。X射线衍射强度的测量数据表明Pd₂Si的生成对长周期多层膜的衍射强度影响不大,但对短周期多层膜衍射强度的影响较大。在引入折射率修正后,我们不仅用单个峰的位置计算了多层膜的周期,而且还用了以两个峰的位置联立消去折射率修正的方法计算了多层膜的周期,前者的误差大于后者。模拟计算的结果说明:均匀Pd₂Si层的生成不足以解释Pd/Si多层膜衍射强度随退火温度的变化,界面的平整化或粗糙化是影响衍射强度的另一个要素。 关键词：     

Pd_2Si的生成对Pd/Si多层膜衍射性能的影响

本文研究了Pd_2Si的生成对周期性Pd/Si多层膜X射线衍射性能的影响。X射线衍射强度的测量数据表明Pd_2Si的生成对长周期多层膜的衍射强度影响不大,但对短周期多层膜衍射强度的影响较大。在引入折射率修正后,我们不仅用单个峰的位置计算了多层膜的周期,而且还用了以两个峰的位置联立消去折射率修正的方法计算了多层膜的周期,前者的误差大于后者。模拟计算的结果说明:均匀Pd_2Si层的生成不足以解释Pd/Si多层膜衍射强度随退火温度的变化,界面的平整化或粗糙化是影响衍射强度的另一个要素。     

界面对ZrN/TaN纳米多层膜固氦性能的影响

采用射频磁控溅射方法, 在混合气氛下制备了ZrN/TaN多层膜. 利用X射线衍射、慢正电子束分析、增强质子背散射、扫描电子显微镜, 分别对ZrN/TaN多层膜中相结构、氦相关缺陷、氦含量、截面形貌等进行了分析. 结果表明, 调制周期为30 nm的ZrN/TaN多层膜在600℃退火后, 氦的保持率仍能达到45.6%. 在适当的调制周期下, ZrN/TaN多层膜能够耐氦损伤并且其界面具有一定的固氦性能. 关键词： ZrN/TaN 纳米多层膜 界面 固氦     

非晶态多层膜和单层膜的低角X射线衍射研究

本文对a-Si:H/(a-SiN_x:H)非晶态周期多层膜和单层膜进行了低角X射线衍射研究。在周期数较少的多层膜衍射的布喇格衍射峰的低角侧发现了一系列次级衍射峰;在单层膜样品的低角衍射中也发现了一系列小峰。对此,我们提出了一个用于计算非晶多层膜和单层膜衍射强度的简单公式,使实验结果得到解释,并提出了一种测量膜厚的方法。 关键词：     

薄膜结构分析中的低角X射线衍射方法

利用带折射修正的布喇格衍射定律和薄膜光学理论分析了低角Ｘ射线衍射谱中出现的一系列现象，导出了多层膜周期厚度和周期中不同材料间的配比率的计算公式，对多层膜的低角射线衍射谱中主峰间的次峰现象作出了解释，并对低角Ｘ射线衍射测量单层膜厚度进行了分析，给出了精确的测厚公式。     

真空退火对Ni80Fe20/Cu多层膜微结构的影响

用直流磁控溅射法在Si(001)衬底上制备了以Ta为缓冲层、含有15周期的Ni₈₀Fe₂₀（4nm)/Cu(6nm)多层膜.样品分别在150,250,350℃进行了真空退火处理.用低角和高角X射线衍射法研究了多层膜的微结构.结果表明,所有样品均有较好的[111] 取向,而且随退火温度或时间的增加,[111]取向程度变得更高.超晶格周期、平均面间距在退火后略有减小,表明多层膜结构在退火后变得更为致密.多层膜界面粗糙度随退火温度或时间的增加而增大,平均相关长度随退火温度或时间的增加而减小,分析认为这是由于Ni₈₀Fe₂₀/Cu界面存在严重的互扩散所导致的.模拟Ni₈₀Fe₂₀/Cu多层膜高角X射线衍射谱,发现在Ni₈₀Fe₂₀/Cu蜀面有非常厚的混合层存在,而且混合层厚度随退火温度或时间的增加而增大.模拟结果还表明,随退火温度或时间的增加,Ni₈₀Fe₂₀层面间距几乎保持不变,Cu层面间距则随退火温度的增加而略有减小. 关键词：     

簿膜结构分析中的低角X射线衍射方法

利用带折射修正的布喇格衍射定律和薄膜光学理论分析了低角Ｘ射线衍射谱中出现的一系列现象，导出了多层膜周期厚度和周期中不同材料间的配比率的计算公式，对多层膜的低角Ｘ射线衍射谱中主峰间的次峰现象作出了解释，并对低角Ｘ射线衍射测量单层膜厚度进行分析，给出了精确的测厚公式。     

非晶调制多层膜Nb/Si中的互扩散研究

利用原位Ｘ射线衍射技术得到非晶调制多层膜Ｎｂ／Ｓｉ中的互扩散系数与退火温度的关系，调制周期Ｌ＝３.２ｎｍ的非晶调制多层膜是用粒子溅射方法制备的．温度范围为４２３—５２３Ｋ的有效互扩散系数通过原位测量多层膜的一级调制峰强度与退火温度之间的关系而得到．利用缺陷陷阱延迟扩散机制解释了所得到的扩散系数与退火温度的关系．建立了可以解释较小前置系数的模型 关键词：     

8.0 nm反射式偏振膜的设计和制备

讨论了软X射线反射式偏振膜的设计原理和方法,利用设计软件模拟设计了8.0 nm处的Mo/B4C偏振膜.对影响多层膜性能的参量进行了详细的误差分析.利用磁控溅射镀膜机进行了偏振膜的制备研究,X射线小角衍射测量了多层膜的周期厚度,测量数据的拟合结果与设计值吻合很好.     

Structural stability of heat-treated CoN/CN soft X-ray multilayers fabricated by dual-facing-target sputtering

286 , 176 (1996)]. (1) The interdiffusion critical wavelengths were calculated as 2.00–2.04 nm at temperatures ranging from 473 to 523 K, which is equal to those of Co/C multilayers within the experimental error, indicating that the interdiffusion behaviours in the CoN/CN multilayers are still decided by the thermodynamic properties of the Co-C system. (2) The effective interdiffusivities and macroscopic diffusion coefficients are smaller. (3) The activation energy for diffusion is larger. The features imply that it is possible to improve the thermal stability of Co/C multilayers by doping with N atoms. The high-temperature annealing results imply that the destructive threshold of the CoN/CN multilayers is 100–200 °C higher than that of Co/C multilayers. The small-angle X-ray diffraction of CoN/CN soft X-ray multilayers indicates that the period expansion of the multilayers is only 4% at 400 °C, and the interface pattern still exists even if they were annealed at 700 °C. The large-angle X-ray diffraction and transmission electron microscopy analysis reveal that the crystalline process is significantly retarded if doped with N atoms, leading to a smaller grain size at higher annealing temperatures. The significant improvement of the thermal stability can be interpreted with Raman spectroscopy and X-ray photoelectron spectroscopy analysis. The Raman spectra give the evidence that the formation of the sp³ bonding in the CN sublayers can be suppressed effectively by doping with N atoms, and thus the period expansion resulting from the changes in the density of CN layers can be decreased considerably. The X-ray photoelectron spectra give information about existence of the strong covalent bonding between N atoms and the ionic bonding between Co and N atoms, which can slow down the tendency of the structural relaxation. The interstitial N atoms decrease the mobility of Co atoms, and thus the fcc Co and hcp Co coexist even though the annealing temperature is much higher than the phase transformation temperature of 420 °C, leading to the suppression of the grain growth. Received: 29 May 1997/Accepted: 8 September 1997     

Dual-facing-target-sputtered amorphous CoMoN/CN compound soft-X-ray multilayers: structures and thermal stability

Amorphous CoMoN/CN compound soft-X-ray multilayers were fabricated by dual-facing-target sputtering. Their structural thermal stability has been investigated by monitoring the structural evolutions of CN and CoMoN sublayers at annealing temperatures up to 800 °C using complementary measurement techniques, and measuring the coefficient of interfacial diffusion at annealing temperatures below 300 °C. The period expansion at annealing temperatures below 600 °C, which is usually observed in annealed metal/carbon soft-X-ray multilayers, is only 5%. The enhanced sp² to sp³ bond ratio caused by the incorporation annealing effect of nitrogen [1] is thought to be responsible for the improved thermal stability of CN sublayers. Mo addition greatly suppresses the structural thermal evolution of CoMoN sublayers. XPS and TEM analyses indicate that the strong chemical bonding between N and Co atoms and Mo nitride aggregation in the grain boundary of cobalt are the main mechanisms for the high thermal stability of CoMoN sublayers. The layered structure of the CoMoN/CN multilayers still exists at the annealing temperature of 800 °C, while Co/C and CoN/CN multilayers have already been destroyed at this temperature. Compared with Co/C and CoN/CN multilayers, the smaller negative interdiffusivity measured by X-ray diffraction reveals the stable interfaces of CoMoN/CN multilayers. These results illustrate that refractory metal incorporation and strong chemical bond establishment are quite effective in obtaining thermally highly stable compound soft-X-ray optical multilayers . PACS 68.65+g; 68.55.Ln; 68.35.Fx; 68.60.Dv     

Structural stability of heat-treated Co/C soft X-ray multilayers fabricated by dual-facing-target sputtering

Thermal stability of Co/C multilayers prepared by a dual-facing-target sputtering system was studied. A picture of the thermally induced changes in the microstructure was obtained using complementary measurement techniques including low-angle and high-angle X-ray diffraction, transmission electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. It was found that the period expansion, reflectivity change and compound formation, that were observed after annealing are caused by structural changes both in the sublayers and at the interfaces. Below 400°C, the period expansion is mainly caused by the graphitization of the amorphous carbon layers, and a significant increase in the reflectivity at grazing incidence was observed. By 500°C, the crystallization and agglomeration of Co layers induce an enormous period expansion and a serious decrease in reflectivity. A small amount of carbide is found to form at this temperature. Our results imply that new multilayer structures, e.g., compound multilayers will have to be developed for use at high temperatures or under high X-ray incident flux.     

Superconductivity of MgB 2 Thin Films Prepared By CoEvaporation and Magnetism of MgB 2 /Fe Multilayers Studied By Mössbauer Spectroscopy

MgB 2 thin films and MgB 2 /Fe multilayers have been prepared by vapor deposition of the elements in vacuum. X-ray diffraction studies of the MgB 2 samples show preferred c -axis growth along the film normal direction. Superconducting transition temperatures of 18 K and 22 K have been measured before and after annealing, respectively, of an MgB 2 film of 1575 Å thickness. Atomic force microscope images show island growth of the films leading to a rough surface. Mössbauer spectroscopy on MgB 2 /Fe/MgB 2 multilayers of various Fe layer thicknesses indicates superparamagnetic behavior. Evidence is provided for the formation of interfacial amorphous (a-) Fe 3 B. The magnetic ordering of Fe and a-Fe 3 B and the size effect in MgB 2 are assumed to be the cause for the destruction of the superconductivity in the as-grown multilayers.     

Characterization of heat-treated CN films fabricated by dual-facing-target sputtering for soft X-ray multilayer mirrors

The structural characterization of heat-treated CN films fabricated by dual-facing-target sputtering for soft X-ray multilayer mirrors was performed by means of X-ray diffraction (XRD), Raman spectroscopy (RS) and X-ray photoelectron spectroscopy (XPS). The XRD analyses indicate a graphization process in the CN films during thermal annealing. The Raman analyses imply that the primary bonding in the CN films is sp². In other words, the formation of the sp³ bonding in the CN films can be suppressed effectively by doping with N atoms, and thus the thickness expansion resulting from the changes in the density of CN films during annealing can be decreased considerably. This result is also clarified by the increased conductivity measured. The XPS results give the information of the existence of the strong covalent bonding between N and C atoms, which can slow down the tendency of the structural relaxation during annealing. These results suggest that CN films suitable for soft X-ray multilayers used at high-temperature environments can be obtained by reactive dual-facing-target sputtering. With the low-angle X-ray diffraction measurements, we do observe the enhanced thermal stability of CoN/CN multilayers. Received: 2 October 1998 / Accepted: 21 April 1999 / Published online: 23 September 1999     

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.