Thermal stability of Mo/Si multilayer soft-X-ray mirrors fabricated by electron-beam evaporation

Mo/Si multilayers are fabricated by electron-beam evaporation in UHV at different temperatures (30° C, 150° C, 200° C) during deposition. After completion their thermal stability is tested by baking them at temperatures (T _bak) between 200° C and 800° C in steps of 50° C or 100° C. After each baking step the multilayers are characterized by small angle Cu_K-X-ray diffraction. Additionally, the normal incidence soft-X-ray reflectivity for wavelengths between 11 nm and 19 nm is determined after baking at 500° C. Furthermore, the layer structure of the multilayers is investigated by means of Rutherford Backscattering Spectroscopy (RBS) and sputter/Auger Electron Spectroscopy (AES) technique. While the reflectivity turns out to be highest for a deposition temperature of 150° C, the thermal stability of the multilayer increases with deposition temperature. The multilayer deposited at 200° C stands even a 20 min 500° C baking without considerable changes in the reflectivity behaviour.     

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.     

TiCN/TiNbCN multilayer coatings with enhanced mechanical properties

Enhancement of mechanical properties by using a TiCN/TiNbCN multilayered system with different bilayer periods (Λ) and bilayer numbers (n) via magnetron sputtering technique was studied in this work. The coatings were characterized in terms of structural, chemical, morphological and mechanical properties by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nanoindentation. Results of the X-ray analysis showed reflections associated to FCC (1 1 1) crystal structure for TiCN/TiNbCN films. AFM analysis revealed a reduction of grain size and roughness when the bilayer number is increased and the bilayer period is decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 15 nm (n = 200), yielding the highest hardness (42 GPa) and elastic modulus (408 GPa). The values for the hardness and elastic modulus are 1.6 and 1.3 times greater than the coating with n = 1, respectively. The enhancement effects in multilayer coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain the increase in hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayers taking into account the thickness reduction at individual single layers that make the multilayered system. The Hall-Petch model based on dislocation motion within layers and across layer interfaces, has been successfully applied to multilayers to explain this hardness enhancement.     

Growth and characterization of Cd1−xZnxTe thin films prepared from elemental multilayer deposition

Cd_1−xZn_xTe is a key material for fabrication of high-energy radiation detectors and optical devices. Conventionally it is fabricated using single crystal growth techniques. The method adopted here is the deposition of elemental multilayer followed by thermal annealing in vacuum. The multilayer structure was annealed at different temperatures using one to five repetitions of Cd-Zn-Te sequence. X-ray diffraction pattern for the multilayer with five repetitions revealed that annealing at 475 °C yielded single-phase material compared to other annealing conditions. EDX spectroscopy was carried out to study the corresponding compositions. Photoluminescence properties and change of resistance of the multilayer under illumination were also studied. The resistivity of the best sample was found to be a few hundreds of Ω cm.     

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayers

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayer (ML) up to 600 °C have been studied and reported in this paper. Ti/Ni multilayer samples having constant layer thicknesses of 50 Å each are deposited on float glass and Si(1 1 1) substrates using electron-beam evaporation technique under ultra-high vacuum (UHV) conditions at room temperatures. The micro-structural parameters and their evolution with temperature for as-deposited as well as annealed multilayer samples up to 600 °C in a step of 100 °C for 1 h are determined by using X-ray diffraction (XRD) and grazing incidence X-ray reflectivity techniques. The X-ray diffraction pattern recorded at 300 °C annealed multilayer sample shows interesting structural transformation (from crystalline to amorphous) because of the solid-state reaction (SSR) and subsequent re-crystallization at higher temperatures of annealing, particularly at ≥400 °C due to the formation of TiNi₃ and Ti₂Ni alloy phases. Sample quality and surface morphology are examined by using atomic force microscopy (AFM) technique for both as-deposited as well as annealed multilayer samples. In addition to this, a temperature dependent dc resistivity measurement is also used to study the structural transformation and subsequent alloy phase formation due to annealing treatment. The corresponding magnetization behavior of multilayer samples after each stage of annealing has been investigated by using Magneto-Optical Kerr Effect (MOKE) technique and results are interpreted in terms of observed micro-structural changes.     

XPS study of annealing induced effects on surface and interface electronic properties of Si/Ge nanostructures

The present study is focused on the influence of vacuum thermal treatment on surface/interface electronic properties of Si/Ge multilayer structures (MLS) characterized using X-ray photoelectron spectroscopy (XPS) technique. Desired [Si(5 nm)/Ge(5 nm)]_×10 MLS were prepared using electron beam evaporation technique under ultra high vacuum (UHV) conditions. The core-level XPS spectra of as-deposited as well as multilayer samples annealed at different temperatures such as 100 °C, 150 °C and 200 °C for 1 h show substantial reduction in Ge 2p peak integrated intensity, whereas peak intensity of Si 2p remains almost constant. The complete interdiffusion took place after annealing the sample at 200 °C for 5 h as confirmed from depth profiling of annealed MLS. The asymmetric behaviour in intensity patterns of Si and Ge with annealing was attributed to faster interdiffusion of Si into Ge layer. However, another set of experiments on these MLS annealed at 500 °C suggests that interdiffusion can also be studied by annealing the system at higher temperature for relatively shorter time duration.     

Figure Error Correction by Reflection Wavefront Control of Cu K<Subscript>α</Subscript> Grazing Incidence Multilayer Mirrors

Reflection phase and amplitude of grazing incidence multilayer mirrors for CuK_α radiation have been studied theoretically to evaluate phase correction effects of multilayer surface milling, which revealed good possibilities of correcting mirror substrate figure errors for focusing and imaging application. The mirror multilayers composed of base materials of Cu and Ni were studied in combination with Al, Be, C, Mg and Si for high reflectivity at a grazing angle of 3° incidence. The theoretical surface milling of Cu/Al multilayers of a period thickness of 1.478 nm provides phase correction of 1.7° per period, which corresponds to an accurate correction of substrate figure errors at a rate of 0.007 nm per period. Thus, the milling after the multilayer fabrication, compared to the milling before the multilayer fabrication, enables far more accurate phase correction with 200 times finer control.     

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.     

Structural investigation of n-hexadecanoic acid multilayers on mica surface: Atomic force microscopy study

The structure of n-hexadecanoic acid (HA) multilayers formed by spreading an ethanol solution containing this molecule onto a freshly cleaved mica surface has been studied by atomic force microscopy (AFM). AFM images of multilayers obtained with different coating time showed that HA molecules first formed some sporadic domains on mica surface. With the proceeding of the coating process, these domains gradually enlarged and coalesced, until formed a continuous film finally. It was observed that HA molecules were always adsorbed on mica surface with tilted even-numbered layers structure. The height of the repeated tilted bilayer film was measured to be approximately 3.8 ± 0.2 nm, which implied a ∼60° tilt molecular conformation of the HA bilayers on mica surface. Phase image confirmed that the HA multilayers terminated with the hydrophilic carboxylic acid groups. The formation mechanism of the HA multilayers was discussed in detail. Thus, resulted hydrophilic surfaces are of special interest for further study in biological or man-made member systems.     

Gold and platinum diffusion: The key to the understanding of intrinsic point defect behavior in silicon

The study of gold and platinum diffusion is found to allow the separate observation of the intrinsic point defects, i.e., of silicon self-interstitials and of vacancies. The diffusion of gold in float zone (FZ) silicon is found to be dominated by the kick-out mechanism for temperatures of 800° C and higher. The diffusion of platinum in FZ silicon is described by the kick-out mechanism for temperatures above approximately 900° C, whereas for temperatures below approximately 850° C the dissociative mechanism governs platinum diffusion. As a result of numerical simulations, we suggest a complete and consistent set of parameters which describes the diffusion of platinum in silicon in the temperature range from 700° C to 950° C and the diffusion of gold in the temperature range from 800° C to 1100° C. The generation or recombination of self-interstitials and vacancies is found to be ineffective at least below 850° C. The concentration of substitutional platinum is determined by the initial concentration of vacancies at diffusion temperatures below 850° C. Platinum diffusion below 850°C can be used to measure vacancy distributions in silicon quantitatively.     

Bi surfactant effects of Co/Cu multilayered films prepared by sputter deposition

The influence of a Bi surfactant layer on the structural and magnetic properties of Co/Cu multilayers grown onto Cu(1 1 0) buffer layer by RF magnetron sputtering has been studied. The results of X-ray diffraction revealed the initial deposition of a 2.0 Å-thick Bi layer onto the Cu buffer layer prior to the deposition of the Co/Cu multilayer yielded high-quality fcc-(1 1 0) oriented epitaxial films. The X-ray photoelectron spectra revealed that Bi was segregated at around the top of the surface. Therefore, Bi was concluded to be an effective surfactant to enhance the epitaxial growth of Co/Cu(1 1 0) multilayer. The maximum giant magnetoresistance and antiferromagnetic interlayer coupling ratios of the Co/Cu multilayers were increased by using the Bi surfactant layer.     

Ion beam sputter deposited W/Si multilayers: Influence of re-sputtering on the interface structure and structure modification at ultra short periods

X-ray multilayer mirrors of period ranging from 9.6 to 1.7 nm, deposited using ion beam sputtering, have been examined using grazing incidence X-ray reflectivity (GIXRR) and grazing incidence X-ray diffraction. Detailed analysis of GIXRR data revealed that significant amount of re-sputtering of Si layer takes place while W deposition is underway. Re-sputtering is mainly due to bombardment of high-energy neutrals getting reflected from the W target. Due to re-sputtering interface of the multilayer becomes asymmetric. This puts a major hindrance in avoiding the intermixing and achieving sharp interfaces at shorter periods. Maximum thickness of Si which gets lost due to re-sputtering during deposition is ∼0.8 nm. The shortest period multilayer estimated, that could be deposited without intermixing, was 2.7 nm. These results are of significance for developing low period W/Si multilayers.     

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。     

The effects of Si3N4 interlayer on the thermal stability and hardness of Ti/TiNx (x = 0.5-1) nanolayered coatings

The polycrystalline Ti/TiN_x multilayer films were deposited by magnetron sputtering, and the as-deposited multilayer coatings were annealed at 500-800 °C for 2-4 h in vacuum. We investigated the effects of annealing temperature and annealing time on the microstructural, interfacial, and mechanical properties of the polycrystalline Ti/TiN_x multilayer films. It was found that the hardness increased with annealing temperature. This hardness enhancement was probably caused by the preferred crystalline orientation TiN(1 1 1). The X-ray reflectivity measurements showed that the layer structure of the coatings could be maintained after annealing at 500 °C and the addition of the Si₃N₄ interlayer to Ti/TiN_x multilayer could improve the thermal stability to 800 °C.     

50~110 nm波段高反射率多层膜的设计与制备

阐述了50~110 nm强吸收波段亚四分之一波长多层膜的设计方法.这种膜系是由强吸收材料叠加而成，每层膜光学厚度小于四分之一个波长.与常规周期多层膜相比，这种膜系更适用于提高强吸收波段的反射率.利用该方法设计了50 nm处高反射多层膜，并以此为初始条件通过Levenberg-Marquart优化方法完成了50~110 nm强吸收波段宽带高反射率Si/W/Co多层膜的设计，其平均反射率达到45%.采用直流磁控溅射方法制备了Si/W/Co多层膜,用X射线衍射仪(XRD)对膜层结构进行了测试，测试结果表明制作出的多层膜结构与设计结构基本相符.     

Transitions of microstructure and photoluminescence properties of the Ge/ZnO multilayer films in certain annealing temperature region

The Ge/ZnO multilayer films have been prepared by rf magnetron sputtering. The effects of annealing on the microstructure and photoluminescence properties of the multilayers have been investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier-transform infrared (FTIR) spectrometry and photoluminescence (PL) spectrometry. The investigation of structural properties indicates that Zn₂GeO₄ has been formed with (2 2 0) texture and Zn deficiency from Ge/ZnO multilayer films in the process of annealing. However, lower Zn/Ge ratio can be improved by annealing. The annealed multilayers show three main emission bands at 532, 700, and 761 nm, which originate from the transition between oxygen vacancy () and Zn vacancies (V_Zn), the radiative recombination of quantum-confined excitons (QCE) in Ge nanocrystals, and the optical transition in the GeO color centers, respectively. Finally, the fabrication of thin film Zn₂GeO₄ from Ge/ZnO multilayer films by annealing at low temperature provides another approach to prepare the green-emitting oxide phosphor film:Zn₂GeO₄:Mn.     

Low-temperature ordering and enhanced coercivity of L10-FePt thin films with Al underlayer

FePt multilayer films with and without Al underlayer were prepared by magnetron sputtering on SiO₂ substrate and subsequently annealed in vacuum. Experimental results suggest that the existence of Al underlayer can effectively reduce the ordering temperature and increase the coercivity of FePt films. Due to the slight larger lattice constant of Al underlayer than that of FePt films, [Fe (0.66 nm)/Pt (0.84 nm)]₃₀ films begin to order at 350 °C and the coercivity of them reach to 5.7 kOe after annealing at 400 °C for half an hour.     

Improvement of mechanical and tribological properties in steel surfaces by using titanium-aluminum/titanium-aluminum nitride multilayered system

Improvement of mechanical and tribological properties on AISI D3 steel surfaces coated with [Ti-Al/Ti-Al-N]_n multilayer systems deposited in various bilayer periods (Λ) via magnetron co-sputtering pulsed d.c. method, from a metallic binary target; has been studied in this work exhaustively. The multilayer coatings were characterized in terms of structural, chemical, morphological, mechanical and tribological properties by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), scanning electron microscopy, nanoindentation, pin-on-disc and scratch tests, respectively. The failure mode mechanisms were studied by optical microscopy. Results from X-ray diffraction analysis revealed that the crystal structure of TiAl/TiAlN multilayer coatings has a tetragonal and FCC NaCl-type lattice structures for Ti-Al and Ti-Al-N, respectively, i.e., it was found to be non-isostructural multilayers. An enhancement of both hardness and elastic modulus up to 29 GPa and 260 GPa, respectively, was observed as the bilayer periods (Λ) in the coatings were decreased. The sample with a bilayer period (Λ) of 25 nm and bilayer number n = 100 showed the lowest friction coefficient (∼0.28) and the highest critical load (45 N), corresponding to 2.7 and 1.5 times better than those values for the coating deposited with n = 1, respectively. These results indicate an enhancement of mechanical, tribological and adhesion properties, comparing to the [Ti-Al/Ti-Al-N]_n multilayer systems with 1 bilayer at 26%, 63% and 33%, respectively. This enhancement in hardness and toughness for multilayer coatings could be attributed to the different mechanisms for layer formation with nanometric thickness such as the novel Ti-Al/Ti-Al-N effect and the number of interfaces that act as obstacles for the crack deflection and dissipation of crack energy.     

Ultrathin Mo/MoN bilayer nanostructure for diffusion barrier application of advanced Cu metallization

Ultrathin Mo (5 nm)/MoN (5 nm) bilayer nanostructure has been studied as a diffusion barrier for Cu metallization. The Mo/MoN bilayer was prepared by magnetron sputtering and the thermal stability of this barrier is investigated after annealing the Cu/barrier/Si film stack at different temperatures in vacuum for 10 min. The failure of barrier structure is indicated by the abrupt increase in sheet resistance and the formation of Cu₃Si phase proved by X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS). High resolution transmission electron microscopy (HRTEM) examination suggested that the ultrathin Mo/MoN barrier is stable and can prevent the diffusion of Cu at least up to 600 °C.     

Structure of sputter-deposited Pt/Fe and Cr/Fe multilayers

Conversion electron Mössbauer spectroscopy (CEMS) and X-ray diffraction (XRD) have been used to investigate the structure of Pt/Fe and Cr/Fe multilayers deposited by magnetron sputtering. The Cr/Fe samples consisted of four samples prepared under Ar sputtering pressures of 1.3, 3.0, 5.0, and 10.0 mT, all with the same multilayer structure of 3.5 nm Cr/2.5 nm Fe, repeated 35 times onto c-Si wafer substrates. The quality of the interfaces between Cr and Fe is clearly degraded with increasing sputter pressure, as seen by changes in the relative intensities of four magnetic subspectra in the CEMS and the gradual appearance of a single-line resonance similar to Fe in solution in Cr. The low-angle XRD superlattice peaks also disappear with increasing sputter pressure, while the high-angle XRD shows a tendency for loss of the preferred (110) texture. Two films of Pt/Fe were deposited epitaxially onto MgO single crystals with bilayer periods of 1.3 nm and 2.6 nm and total thickness of 300 nm each. A transition from fcc-PtFe with near-perpendicular magnetic anisotropy to a bcc-Fe/fcc-PtFe mixture with in-plane magnetic texture is observed by CEMS for the factor of two increase in bilayer period.