Si/SiO2 multilayers: synthesis by reactive magnetron sputtering and photoluminescence emission

This paper relates a complete study of Si/SiO₂ multilayer (ML) structures. First, we suggest an original way of synthesis based on reactive magnetron sputtering of a pure silica target. The photoluminescence spectra of these MLs consist of two Gaussian bands in the visible-near infrared spectral region. The stronger one (I band) is fixed at about 780 nm and probably due to interface states. The weaker one (Q band) is tuneable with the Si sublayer thickness and originates from a radiative recombination within the nanosized Si layers. For this latter band the peak position is a function of the Si sublayer thickness and shows a discontinuity at 30 Å. This corresponds to an Si phase change. For thicknesses above 30 Å, the sublayers are composed of nanocrystalline silicon whereas below 30 Å the sublayers are made of amorphous silicon. We develop a model based on a quantum well to which we have added an interfacial region between Si and SiO₂. It is characterised by an interfacial potential of 0.3 eV. This model depicts the simultaneous behaviour of Q and I bands for an Si sublayer thickness below 30 Å.     

Aperiodic multilayer mirrors for efficient broadband reflection in the extreme ultraviolet

Recent extreme ultraviolet sources using high-harmonic generation in a rare gas make new optics developments necessary. We report on the study and development of multilayer structures with efficient reflectivity in the 35–75 eV energy range. We have optimized, deposited and characterized two aperiodic broadband mirrors consisting of a Mo, Si and B₄C thin-film stack. We used the needle procedure in order to optimize mirror reflectivity. The magnetron sputter deposited multilayers have been calibrated and characterized using Cu K _α grazing incidence X-ray reflectometry. Reflectivity measured at near-normal incidence on a synchrotron radiation source reaches 12% with a full width at half maximum of nearly 40 eV. Experimental results are compared with theoretical simulation using available optical constants for Mo, Si and B₄C in this spectral range.     

单发实验测量软X射线多层膜反射镜反射特性

 提出了一种单发实验测量软X射线波段多层膜反射镜反射特性的简易方法。实验采用激光等离子体软X射线源作为光源,用平焦场光栅谱仪分光,在光路中引入掠入射镜以消除高级次谱的影响,用软X光CCD记录,在一发激光打靶实验中,测量了设计中心波长为13.9 nm的Mo/Si多层膜反射镜的反射特性。     

High-pressure polymorphic transformation of rutile to alpha-PbO2-type TiO2 at {011}R twin boundaries

The presence of nano-scale lamellae of the α-PbO₂-type polymorph of TiO₂ sandwiched between twinned rutile inclusions in jadeite has been confirmed by electron diffraction and high-resolution transmission electron microscopy, backed up by image simulation techniques, from ultrahigh-pressure jadeite quartzite at Shuanghe in the Dabie Mountains, China. The crystal structure is orthorhombic with lattice parameters a = 4.58 Å, b = 5.42 Å, c = 5.02 Å and space group Pbcn. A three-dimensional structural model has been constructed for the rutile to α-PbO₂-type TiO₂ phase transformation based on high-resolution electron microscopic images. Computer image simulation and structural model analysis reveal that rutile {0 1 1}_R twin interface is a basic structural unit of α-PbO₂-type TiO₂. Nucleation of α-PbO₂-type TiO₂ lamellae 1–2 nm thick is caused by the displacement of one half of the titanium cations within the {0 1 1}_R twin slab. This displacement reduces the Ti–O–Ti distance and is favored by high pressure.     

The corrosion behavior of intermetallic compounds Ni3(Si,Ti) and Ni3(Si,Ti) + 2Mo in acidic solutions

The corrosion behavior of the intermetallic compounds homogenized, Ni₃(Si,Ti) (L1₂: single phase) and Ni₃(Si,Ti) + 2Mo (L1₂ and (L1₂ + Ni_ss) mixture region), has been investigated using an immersion test, electrochemical method and surface analytical method (SEM; scanning electron microscope and EPMA: electron probe microanalysis) in 0.5 kmol/m³ H₂SO₄ and 0.5 kmol/m³ HCl solutions at 303 K. In addition, the corrosion behavior of a solution annealed austenitic stainless steel type 304 was studied under the same experimental conditions as a reference. It was found that the intergranular attack was observed for Ni₃(Si,Ti) at an initial stage of the immersion test, but not Ni₃(Si,Ti) + 2Mo, while Ni₃(Si,Ti) + 2Mo had the preferential dissolution of L1₂ with a lower Mo concentration compared to (L1₂ + Ni_ss) mixture region. From the immersion test and polarization curves, Ni₃(Si,Ti) + 2Mo showed the lowest corrosion resistance in both solutions and Ni₃(Si,Ti) had the highest corrosion resistance in the HCl solution, but not in the H₂SO₄ solution. For instance, it was found that unlike type 304 stainless steel, these intermetallic compounds were difficult to form a stable passive film in the H₂SO₄ solution. The results obtained were explained in terms of boron segregation at grain boundaries, Mo enrichment and film stability (or strength).     

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%。     

质子辐照下Mo/Si多层膜反射镜的微观结构状态

利用透射电子显微镜对质子辐照前后空间太阳望远镜Mo/Si多层膜的微观结构进行了表征, 并对其辐照前后反射率的变化进行了测量.研究表明, Mo/Si多层膜经质子辐照后形成了一些缺陷结构,局部区域Mo/Si的周期性遭到破坏, Mo层与Si层的宽度发生了变化,多层膜层与层之间的界面也比辐照前更为粗糙,部分层状结构由于质子辐照发生了明显的扭曲和折断等现象;此外,质子辐照导致了Mo/Si多层膜反射率的下降,这些微观缺陷的形成是光学性能降低的直接诱因. 关键词： 空间太阳望远镜 Mo/Si多层膜 微观结构 反射率     

Analysis of lead molybdate and lead tungstate synthesized by a sonochemical method

Lead molybdate and lead tungstate nanoparticles were successfully synthesized by a sonochemical method for 1 h. XRD patterns showed the body-centered tetragonal structures of PbMoO₄ and PbWO₄, and were in accordance with those of the simulation and JCPDS software. Calculated lattice parameters are a = b = 5.4233 Å and c = 12.1253 Å for PbMoO₄, and 5.4570 Å and 12.0995 Å for PbWO₄. They are in accordance with those of the corresponding JCPDS software. TEM images show that the particles were 29.09 ± 5.22 nm and 21.05 ± 2.68 nm for PbMoO₄ and PbWO₄, respectively. Raman and FTIR vibrations were investigated to identify a definite existence of the structures.     

B4C/Mo/Si high reflectivity multilayer mirror at 30.4 nm

The B4C/Mo/Si high reflectivity multilayer mirror was designed for He-Ⅱ radiation (30.4 nm) using the layer-by-layer method. The theoretical peak reflectivity was up to 38.2% at the incident angle of 5°. The B4C/Mo/Si multilayer was fabricated by direct current magnetron sputtering and measured at the National Synchrotron Radiation Laboratory (NSRL) of China. The experimental reflectivity of the B4C/Mo/Si multilayer at 30.4 nm was about 32.5%. The promising performances of the B4C/Mo/Si multilayer mirror could be used for the construction of solar physics instrumentation.     

Optical and IR studies on r.f. magnetron sputtered ultra-thin MoO3 films

Ultra-thin MoO₃ films were deposited onto glass and Si substrates by r.f. magnetron sputtering. The optical and IR properties of the films were studied in the range of 250 to 1000 nm and 400 to 1500 cm⁻¹, respectively. The optical transmission spectra show a significant shift in absorption edge. The energy gap of the films deposited at 373 K and 0.1 mbar was found to be 3.93 eV, and it decreases with increasing substrate temperature and decreasing sputtering pressure. The IR transmittance spectra shows strong modes of vibrations of Mo=O and Mo–O–Mo units of MoO₃ molecule. A significant change in energy gap and a shift in frequency of IR modes were observed in ultra-thin MoO₃ films.     

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.     

Surface phenomena related to mirror degradation in extreme ultraviolet (EUV) lithography

One of the most promising methods for next generation device manufacturing is extreme ultraviolet (EUV) lithography, which uses 13.5 nm wavelength radiation generated from freestanding plasma-based sources. The short wavelength of the incident illumination allows for a considerable decrease in printed feature size, but also creates a range of technological challenges not present for traditional optical lithography. Contamination and oxidation form on multilayer reflecting optics surfaces that not only reduce system throughput because of the associated reduction in EUV reflectivity, but also introduce wavefront aberrations that compromise the ability to print uniform features. Capping layers of ruthenium, films ∼2 nm thick, are found to extend the lifetime of Mo/Si multilayer mirrors used in EUV lithography applications. However, reflectivities of even the Ru-coated mirrors degrade in time during exposure to EUV radiation. Ruthenium surfaces are chemically reactive and are very effective as heterogeneous catalysts. In the present paper we summarize the thermal and radiation-induced surface chemistry of bare Ru exposed to gases; the emphasis is on H₂O vapor, a dominant background gas in vacuum processing chambers. Our goal is to provide insights into the fundamental physical processes that affect the reflectivity of Ru-coated Mo/Si multilayer mirrors exposed to EUV radiation. Our ultimate goal is to identify and recommend practices or antidotes that may extend mirror lifetimes.     

Finite Element Analysis Of Thermal Characteristics in Continuous Wave Long Wavelength Surface Emitting Lasers (I): Dielectric Cavity Structures

We numerically analyzed the thermal characteristic in continuous wave (cw) GalnAsP/InP surface emitting lasers with dielectric multilayer mirrors by using finite element method. From the simulation of temperature distribution in cw devices, we found that MgO/Si multilayer mirror which has a high thermal conductivity is effective for heat sinking; the thermal resistance of device using MgO/Si mirror is nearly half of that using SiO₂/Si one, almost independently of their thicknesses. It was also indicated that the optimum design for other structural parameters, especially the thickness of active region, is important to effectively suppress the temperature increase. The minimum threshold current was estimated to be 3 mA under cw condition for the active region diameter of 4 μm and thickness of 0.5 μm.     

Thickness dependence of superconductivity for In/Mo thin films

We report on the superconducting characteristics of the Indium thin films on molybdenum under-layer as a function of the In film thickness. Our molybdenum under-layer with thickness of 50 Å does not cause the occurrence of superconductivity until 1.5 K and the sheet resistance has logarithmic temperature dependence observed in the present investigation. As thickness of In increased, the oscillation phenomenon of T_C was observed at early stage of deposition and the value of T_C is higher than the that for bulk of In. Furthermore, it is found that with increase of the In thickness, there are large differences of the strengths of the upper critical magnetic field H_C2(T), resistivity and T_C between films with thickness below and above 100 Å. On the other hand, the T_C decreases monotonously as sheet resistance increases, when the T_C is plotted against sheet resistance. To clarify the relation of superconducting characteristics and the surface structure of the films with different thickness, we have performed surface observation by atomic force microscope. As a result, we have found that the surface changes from homogeneous structure to inhomogeneous (or percolative) structure, when the thickness of in films pass through about 100 Å. Superconductivity of In/Mo films with relatively thick-inhomogeneous films cannot be explained in terms of the simple percolation theory. Therefore, we analysis the experimental data of H_C2(T) near T_C, using a extended Landau–Ginzburg model. It is found out that our In/Mo films must consider some factors; such as, grain size, the distance of grain space, and the strength of couplings between grains.     

Phase-change behavior in Si/Sb80Te20 nanocomposite multilayer films

Phase-change behavior in Si/Sb₈₀Te₂₀ nanocomposite multilayer films were investigated by utilizing in situ resistance measurements. It was found that the crystallization temperature increased firstly with increasing Si layer thickness within the multilayer films, and then remained almost unchanged at 170°C. The multilayer films have the merits of both good thermal stability and fast phase-change speed. An increase in crystallization temperature by around 95°C was observed for the multilayer films when the Sb₈₀Te₂₀ layer thickness was reduced to 3 nm. Cross-sectional transmission electron microscopy (TEM) observations revealed that Si/Sb₈₀Te₂₀ nanocomposite multilayer films had layered structures with clear interfaces. The reversible phase change between set and reset states was verified in phase-change random access memory (PCRAM) cell based on [Si (1 nm)/Sb₈₀Te₂₀ (5 nm)]₁₇ multilayer film.     

Design of the chirped Mo/Si multilayer mirror with SiC capping layer in extreme ultraviolet region

The design procedures were discussed in detail for a normal incident chirped Mo/Si multilayer mirror with Group Delay Dispersion (GDD) of ?3600 as² in the wavelength region of 13–17 nm. The GDD was calculated using an analytical approach by fitting the optical constants of the coating materials in the wavelength range of 12.8–17.2 nm, respectively. The final structure of the chirped mirror was obtained by using the simplex algorithm from the initial structure obtained by the genetic algorithm based on structure generated by a random generator. After considering the interfacial roughness and layers thickness deviation, the effects on the reflectivity and the GDD were discussed. It was found that the average reflectivity decreases from 5.98% to 4.22% and the average GDD decreases from ?3561.86 as² to ?3462.03 as², the vibration of GDD were larger than that of the reflectivity. The reflectivity was affected greatly by the 9th layer and the GDD was affected greatly by the 25th layer when each layer thickness changes ±0.2 nm. Compared with the GDD, the reflectivity was affected greatly by the layer thickness error.     

Electrical and mechanical properties of proton conducting SrCe0.95Yb0.05O3 − α

Yb³⁺-doped ceramic strontium cerate of exactly the composition SrCe_0.95Yb_0.05O_{3 − α} was prepared, having a relative density of 99.0 (± 0.3%). Great care was taken to obtain homogeneous, carbonate free material. Analysis are made of the X-ray powder diffraction pattern of the as-prepared dense ceramic, resulting in the orthorhombic unit cell parameters a = 6.997(2) Å, b = 12.296(3) Å, c = 8.588(2) Å, Z = 8 and d_x = 5.806(2) g cm⁻³. Bending strength values of the ceramic in non-proton and proton conducting state are found to be 177 and 194 MPa respectively. The ceramic kept under proton conducting conditions for 500 h at 300 °C to 800 °C in a N₂ flow containing 155 mbar water vapour and 245 mbar H₂, have shown to remain chemically and structurally stable. Impedance spectroscopy measurements of the bulk conductivity of the proton conducting ceramic revealed an activation energy of 53.2 kJ mol⁻¹ and a preexponential factor of 359.1 (Ω cm)⁻¹ K. In the non-proton conducting state the ceramic is mainly oxygen ion vacancy conducting, which indicates that charge compensation on substituting Yb⁺³ in SrCeO₃ takes place by oxygen ion vacancies.     

Componentry of reflection optics for application in the tesis X-ray astrophysics experiment

Reflection characteristics of multilayer structures for the CORONAS-FOTON optical schemes are described. Mo/Si, Al/Zr, Cr/Mg, Si/Mg, and Mg/B₄C material combinations were studied. Multilayer X-ray mirrors based on these combinations and used at wavelengths 13.2, 17.1, and 30.4 nm were designed.     

Thin film characterization by laser interferometry combined with SIMS

Thin film properties of technologically important materials (Si, GaAs, SiO₂, WSi_x) have been measured by using a novel technique that combines secondary ion mass spectrometry (SIMS) and laser interferometry.The simultaneous measurement of optical phase and reflectance as well as SIMS species during ion sputtering yielded optical constants, sputtering rates and composition of thin films with high depth resolution. A model based on the principle of multiple reflection within a multilayer structure, which considered also transformation of the film composition in depth and time during sputtering, was fitted to the reflectance and phase data. This model was applied to reveal the transformation of silicon by sputtering with O ₂ ⁺ ions. Special attention was paid to the preequilibrium phase of the sputter process (amorphization, oxidation, and volume expansion). To demonstrate the analytical potential of our method the multilayer system WSi_x/poly-Si/SiO₂/Si was investigated. The physical parameters and the stoichiometry of tungsten suicide were determined for annealed as well as deposited films. A highly sensitive technique that makes use of a Fabry-Perot etalon integrated with a Michelson type interferometer is proposed. This two-stage interferometer has the potential to profile a sample surface with subangstroem resolution.     

On the interplay of internal/external stress and thermal stability of Mo/Si multilayers

Mo/Si multilayer (ML) systems were deposited on Si(100) substrate by DC magnetron sputtering. The MLs were annealed at temperatures up to 440 °C under high-vacuum conditions, both with and without the influence of external mechanical stress, and characterized before and after thermal treatment by means of X-ray reflectometry, wide-angle X-ray scattering and optical microscopy. Two ML configurations were compared, one composed of pure Mo and Si layers and another with additional B₄C and C interlayers at the Mo/Si interfaces, respectively. The external mechanical stress applied caused bending of the substrate and adherent ML, with an accompanied internal stress of approximately 60 GPa. An important outcome of the investigation was that dedicated release bending of MLs can reduce/compensate the influences of the internal stressed states. Thermal stability could be increased for both ML systems during sample annealing. For ML samples with additional B₄C and C layers at the Mo/Si interfaces, the influence of external stress was more significant compared to that for pure Mo/Si MLs. This indicates that the additional layers mainly act as diffusion barriers and additionally as stress-relaxing buffers. PACS 68.60.Dv; 68.65.Ac; 42.79.Bh