Investigation in the interface roughness of DC-sputtered Mo/B4C multilayer mirrors with variable layer pairs for 7-nm soft X-ray polarizers

The surface and interface roughness of Mo/B₄C multilayer mirrors for 7-nm soft X-ray polarizer with variable layer pairs (N = 50, 70, 90 and 110), fabricated by DC sputtering technique is investigated by atomic force microscopy and X-ray scattering and reflecting. The experimental results present that the surface and interface roughness of Mo/B₄C multilayer mirrors increase layer by layer from its substrate as its Mo layer thickness greater than 2 nm, and the roughness grown tendency could be characterized by a quadratic function.     

Determination of Tungsten Layer Profiles in Bilayer Structures Using X-Ray Reflectivity Method

An effectual method is presented to determine the profiles of a tungsten （W） layer, such as the density, the thickness and the roughness in the multilayer structures, using the x-ray reflectivity technique. To avoid oxidation effects of tungsten, a B4 C capping layer is deposited onto to the W layer. To observe the profiles of the tungsten layer with different thicknesses, three groups of W/B4 C bilayers with different thicknesses are prepared by using ultra high vacuum dc magnetron sputtering and measured by an x-ray diffractometer. A type of genetic algorithm called the differential evolution is used to simulate the measurement data so as to obtain the parameters of bilayers. According to the simulation, it is shown that the W layer density varies from 95.26% to 97.51% compared to the bulk. In our experiment, the deposition rate is 0.044 nm/s, and the thickness is varied in the range of 9.8-19.4 nm.     

X-ray properties and interface study of B4C/Mo and B4C/Mo2C periodic multilayers

We present a comparative study of B₄C/Mo and B₄C/Mo₂C periodic multilayer structures deposited by magnetron sputtering. The characterization was performed by grazing incidence X-ray reflectometry at two different energies and high resolution transmission electron microscopy. The experimental results indicate the existence of an interdiffusion layer at the B₄C-on-Mo interface in the B₄C/Mo system. Thus, the B₄C/Mo multilayers were modeled by an asymmetric structure with three layers in each period. The thickness of B₄C-on-Mo interfacial layer was estimated about 1.1 nm. The B₄C/Mo₂C multilayers present less interdiffusion and are well modeled by a symmetric structure without interfacial layers. This study shows that B₄C/Mo₂C structure is an interesting alternative to B₄C/Mo multilayer for X-ray optic applications.     

Structural and magnetic study of swift heavy ion irradiated W/Fe multilayer structure

The present study reports the effect of swift heavy ion irradiation on structural and magnetic properties of sputtered W/Fe multilayer structure (MLS) having bilayer compositions of [W(10 Å)/Fe(20 Å)]_10BL. The MLS is irradiated by 120 MeV Au⁹⁺ ions of fluences 1×10¹³ and 4×10¹³ ions/cm². Techniques like X-ray reflectivity (XRR), cross-sectional transmission electron microscopy (X-TEM) and DC magnetization with a vibrating sample magnetometer (VSM) are used for structural and magnetic characterization of pristine and irradiated MLS. Analysis of XRR data using Parratt’s formalism shows a significant increase in W/Fe layer roughness. X-TEM studies reveal that intra-layer microstructure of Fe layers in MLS becomes nano-crystalline on irradiation. DC magnetization study shows that with spacer layer thickness interlayer coupling changes between ferromagnetic to antiferromagnetic.     

Thickness dependence of microstructure and magnetic properties in FePt/B<Subscript>4</Subscript>C multilayer thin films

FePt/B₄C multilayer films with different single FePt layer thickness were prepared by magnetron sputtering and subsequently annealing in vacuum. Influence of single FePt layer thickness on microstructure and magnetic property of FePt/B₄C films is investigated. Experimental results suggest that the Fe and Pt rich regions will appear in the interior of single FePt layer. The increasing of FePt layer thickness leads to the increase of grain size and volume fraction of order phase f ₀, which eventually induce satisfied coercivity (5.8 kOe).     

Structural and phase transformations in C/Si multilayers during annealing

The structural evolution of a C/Si periodical multilayers is studied by small-angle X-ray diffraction and cross-section transmission electron microscopy. Mixed zones 0.6–0.65 nm thick with different densities are detected at the C/Si and Si/C interfaces in the initial state. The effect of annealing on the thickness, the density, and the phase composition of the layers and the mixed zones is investigated in the temperature range 300–1050°C. Two stages of changing the multilayer composition period upon heating are found. The period increases as the temperature increases up to 700°C and then decreases. The fracture of the composition begins in the silicon layers, where pores and cubic 3C-SiC nanocrystals form at 900°C. The fracture of the layered structure of the composition is completed at T > 1000°C.     

Multilayer x-ray mirrors based on W/B 4 C with ultrashort (d = 0.7–1.5 nm) periods

A method using resonance diffuse x-ray scattering has been developed to investigate the properties of multilayer structures composed of ultrathin films. Multilayer structures W/B ₄ C with ultra-short periods (d=0.7–1.5 nm) have been studied using specular and diffuse x-ray scattering. The contributions of the interface roughness and the mixing of the layer materials to the total width of the transition region between the layers have been separated for these structures. Quasi-Bragg peaks in the diffuse scattering spectra have been observed experimentally, and their analysis has shown that the interface roughnesses in multilayer W/B ₄ C structures are correlated well.     

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.     

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.     

Effect of interfacial diffusion on microstructure and properties of FePt/B4C multifunctional multilayer composite films

FePt/B₄C multilayer composite films were prepared by magnetron sputtering and subsequent annealing in vacuum. By changing Fe layer thickness of [Fe/Pt]₆/B₄C films, optimal magnetic property (8.8 kOe and remanence squareness is about 1.0) is got in [Fe(5.25 nm)/Pt(3.75 nm)]₆/B₄C sample whose composition is Fe rich and near stoichiometric ratio. The characterizations of microstructure demonstrate that the diffusion of B and C atoms into FePt layer depends strongly on B₄C interlayer thickness. When B₄C interlayer thickness of [Fe(2.625 nm)/Pt(3.75 nm)/Fe(2.625 nm)/B₄C]₆ films is bigger than 3 nm, stable value of grain size (6-6.5 nm), coercivity (6-7 kOe) and hardness (16-20 GPa) is observed. Finally, the multifunctional single FePt/B₄C composite film may find its way to substitute traditional three-layer structure commonly used in present data storage technology.     

Nanolayered multilayer coatings of CrN/CrAlN prepared by reactive DC magnetron sputtering

Single-phase CrN and CrAlN coatings were deposited on silicon and mild steel substrates using a reactive DC magnetron sputtering system. The structural characterization of the coatings was done using X-ray diffraction (XRD). The XRD data showed that both the CrN and CrAlN coatings exhibited B1 NaCl structure with a prominent reflection along (2 0 0) plane. The bonding structure of the coatings was characterized by X-ray photoelectron spectroscopy and the surface morphology of the coatings was studied using atomic force microscopy. Subsequently, nanolayered CrN/CrAlN multilayer coatings with a total thickness of approximately 1 μm were deposited on silicon substrates at different modulation wavelengths (Λ). The XRD data showed that all the multilayer coatings were textured along {2 0 0}. The CrN/CrAlN multilayer coatings exhibited a maximum nanoindentation hardness of 3125 kg/mm² at a modulation wavelength of 72 Å, whereas single layer CrN and CrAlN deposited under similar conditions exhibited hardness values of 2375 and 2800 kg/mm², respectively. Structural changes as a result of heating of the multilayer coatings in air (400-800 °C) were characterized using XRD and micro-Raman spectroscopy. The XRD data showed that the multilayer coatings were stable up to a temperature of 650 °C and peaks pertaining to Cr₂O₃ started appearing at 700 °C. These results were confirmed by micro-Raman spectroscopy. Nanoindentation measurements performed on the heat-treated coatings revealed that the multilayer coatings retained hardness as high as 2250 kg/mm² after annealing up to a temperature of 600 °C.     

Structural and magnetic properties of RF sputtered FePt/Fe multilayers

Series of [FePt(4min)/Fe(t_Fe)]₁₀ multilayers have been prepared by RF magnetron sputtering and post-annealing in order to optimize their magnetic properties by structural designs. The structure, surface morphology, composition and magnetic properties of the deposited films have been characterized by X-ray diffractometer (XRD), Rutherford backscattering (RBS), scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDX) and vibrating sample magnetometer (VSM). It is found that after annealing at temperatures above 500 °C, FePt phase undergoes a phase transition from disordered FCC to ordered FCT structure, and becomes a hard magnetic phase. X-ray diffraction studies on the series of [FePt/Fe]_n multilayer with varying Fe layer thickness annealed at 500 and 600 °C show that lattice constants change with Fe layer thickness and annealing temperature. Both lattice constants a and c are smaller than those of standard ones, and lattice constant a decreases as Fe layer deposition time increases. Only a slight increase in grain size was observed as Fe layer decreased in samples annealed at 500 °C. However, the increase in grain size is large in samples annealed at 600 °C. The coercivities of [FePt/Fe]_n multilayers decrease with Fe layer deposition time, and the energy product (BH)_max reaches a maximum in the samples with Fe layer deposition time of 3 min. Comparison of magnetic properties with structure showed an almost linear relationship between the lattice constant a and the coercivities of the FePt phase.     

Grazing incidence diffraction of X-rays in semiconductor heterostructures: Application of the integral mode

The grazing incidence diffraction (GID) of X-rays enables to characterize thin subsurface layers in semiconductor heterostructures having a thickness smaller than 100 nm. The dynamical theory of X-ray diffraction is extended for the case of identical in plane lattice parameters at the heterointerface. Especially the variation in the specular diffracted (220) Bragg intensity measured with open detector (integral mode) is evaluated in dependence on the grazing angle Φ₀ of the primary beam with respect to the (001) surface. Using a parallel beam an oscillation behaviour occurs at the high angle side Θ _c < Φ₀≦0.5⁰(Θ _c is the angle of total external reflection) of the diffraction curveI(Φ₀) which can be related to the thickness of the perfect crystalline part of the epilayert _K . Having an incident beam divergence and a small difference in the effective refractive indices of the layer and the substrate the oscillations are almost leveled. They are further visible in case of a minute inclination of the (220) lattice plane with respect to the surface normal. In the interval 0 < Φ₀<Θ _c the slope of the integral curve depends on the thickness of the subsurface layert _A which does not contribute to the Bragg diffraction. The integral mode is sensitive for layers of about 0<t _A <15 nm and 15<t _K <80 nm. The proposed theory working principally for multilayer structures is presently suplicated to interpret GID curves ofA ^III B ^v heterostructures.     

Interface characterization of B4C‐based multilayers by X‐ray grazing‐incidence reflectivity and diffuse scattering

B₄C‐based multilayers have important applications for soft to hard X‐rays. In this paper, X‐ray grazing‐incidence reflectivity and diffuse scattering, combining various analysis methods, were used to characterize the structure of B₄C‐based multilayers including layer thickness, density, interfacial roughness, interdiffusion, correlation length, etc. Quantitative results for W/B₄C, Mo/B₄C and La/B₄C multilayers were compared. W/B₄C multilayers show the sharpest interfaces and most stable structures. The roughness replications of La/B₄C and Mo/B₄C multilayers are not strong, and oxidations and structure expansions are found in the aging process. This work provides guidance for future fabrication and characterization of B₄C‐based multilayers.     

Reflectivity modeling of Si-based amorphous superlattices

The structural properties of superlattices composed by hydrogenated amorphous silicon/silicon carbide (a-Si:H/a- Si_1 − xC_x:H) and silicon/germanium (a-Si:H/a-Ge:H), deposited by the plasma-enhanced chemical vapor deposition (PECVD) technique, were analyzed by means of small-angle X-ray diffraction. The relevant structural parameters, such as the multilayer period, the individual layer thickness, the width of the interface and the optical constants, were determined by modeling the experimental reflectivity. The model was based on the dynamical diffraction theory, including material mixing at the interface, interface roughness and random variation of component thickness. In addition, the effect of the direct beam and background on the measured intensities were considered.     

Si/Si<Subscript>1 − <Emphasis Type="Italic">x</Emphasis></Subscript>Ge<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>: Er/Si(100) heterostructures grown by sublimation of silicon in germane gas atmosphere

High-quality Si_{1 ? x} Ge _x :Er epitaxial layers have been grown on Si(100) substrates at a relatively low temperature (500°C) by sublimation of silicon in GeH₄ gas atmosphere. It has been established using capacitance-voltage measurements, X-ray diffraction, and secondary-ion mass spectrometry that the spread in the deposited layer thickness in the central part of the substrate (40 × 10 mm² in size) is 5%. High homogeneity of layer doping is obtained within the same area.     

Effect of swift heavy ion irradiation in Fe/W multilayer structures

Present study reports effect of swift heavy ion irradiation on structural and magnetic properties of sputtered Fe/W multilayer structures (MLS) having bilayer compositions of [Fe(20 Å)/W(10 Å)]_5BL and [Fe(20 Å)/W(30 Å)]_5BL. These MLS are irradiated by 120 MeV Au⁹⁺ ions up to fluence of 4 × 10¹³ ions/cm². X-ray reflectivity (XRR), wide-angle X-ray diffraction (WAXD), cross-sectional transmission electron microscopy (X-TEM) and magneto optical Kerr effect (MOKE) techniques are used for structural and magnetic characterization of pristine and irradiated MLS. Analysis of XRR data using Parratt's formalism shows a significant increase in W/Fe interface roughness. WAXD and X-TEM studies reveals that intra-layer microstructure of Fe-layers in MLS becomes nano-crystalline on irradiation. MOKE study shows increase in coercivity at higher fluence, which may be due to increase in surface and interface roughness after recrystallization of Fe-layers.     

Cosegregation of tungsten and nitrogen on Fe-9%W-N(100)

Auger electron spectroscopy (AES) and low energy electron diffraction (LEED) have been used to study the cosegregation of tungsten and nitrogen on ferritic Fe-9%W-N(100) single crystals with nitrogen contents ranging from c_N = 11 to 51 wt-ppm. Cosegregation occurs at temperatures T≲600°C depending on the nitrogen content. The thickness of the cosegregated surface layer is estimated by means of Ar⁺ ion depth profiling as being less than two atomic layers. The LEED pattern of the tungsten and nitrogen covered Fe-9%W-51ppmN(100) substrate shows a sharp (1 × 1) structure at a low background intensity indicating epitaxial stabilization of the cosegregated tungsten nitride layer on the bcc (100) surface. The tungsten and nitrogen covered Fe-9%W-11ppmN(100) substrate exhibits a c(2 × 2) structure. On Fe-9%W-51ppmN(100) a temperature-driven phase transition between the cosegregated (1 × 1) and c(2 × 2) surface phases is observed.     

Structural evolution of nanocrystalline/amorphous Fe/Ni75B25 multilayers: temperature dependence of electrical resistivity

X-ray specular-reflectivity measurements have been carried out on nanocrystalline/amorphous Fe/Ni₇₅B₂₅ multilayer films which were sputter-deposited on Si substrates, to investigate the evolution of interface roughness and the correlation between structure and transport properties. A significant interface roughness correlation with increasing Fe/NiB layer repetition was observed. The investigated films indicated a temperature dependent high electrical resistivity—10⁴ μΩ-cm at 10 K and 10³ μΩ-cm at 300 K—with a semiconductor-metal transition like behavior. Selected area electron diffraction revealed the presence of crystalline bcc Fe phase and NiB in amorphous state. The structural and transport properties of the multilayers are discussed.     

Structural and magnetic properties of Li-Cu mixed spinel ferrites

Li_0.5−x/2Cu_xFe_2.5−x/2O₄ (where x=0.0-1.0) ferrites have been prepared by solid-state reaction. X-ray diffraction was used to study the structure of the above investigated ferrites at various sintering temperatures. Samples were sintered at 1000, 1100 and 1200 °C for 3 h in the atmosphere. For the sintering temperature of 1000 °C, Li_0.5−x/2Cu_xFe_2.5−x/2O₄ undergoes cubic to tetragonal transformation for higher Cu content. However, for the sintering temperature of 1100 and 1200 °C, X-ray diffraction patterns are mainly characterized by fcc structure, though presence of tetragonal distortion was found by other temperature dependence of initial permeability curves. The lattice parameter, X-ray density and bulk density were calculated for different compositions. Curie temperature was measured from the temperature dependence of initial permeability curves. Curie temperatures of Li-Cu mixed ferrites were found to decrease with the increase in Cu²⁺ content due to the reduction of A-B interaction. As mentioned earlier, temperature dependence of initial permeability curves was characterized by tetragonal deformation for the samples containing higher at% of Cu. The complex initial permeability has been studied for different samples. The B-H loops were measured at constant frequency, f=1200 Hz, at room temperature (298 K). Coercivity and hysteresis loss were estimated for different Cu contents.