Grazing Incidence X-ray Diffraction Measurements Research Articles

Towards wake-up free ferroelectrics and scaling: Al-doped HZO and its crystallographic texture

Ferroelectric (FE) hafnium zirconium oxide (HZO) is an excellent candidate for data storage applications. However, it has some reliability limitations such as imprint and retention. Herein, we explore Al doping of HZO to overcome these limitations. FE behavior is tuned by the aluminum (Al) concentrations in the films and by annealing temperature. A correlation is done between electrical behavior, crystallographic texture, and FE phases determined by grazing-incidence X-ray diffraction (GIXRD) measurements. Reduced coercive field (2Ec) values and wake-up free HZO-based ferroelectrics are explored. We show the tunability of remanent polarization (2Pr) and 2Ec with respect to Al-doping concentration and anneal temperature, hence crystallographic texture.

Enhancement of remnant polarization in ferroelectric HfO2 thin films induced by mechanical uniaxial tensile strain after the crystallization process

The effect of strain on the ferroelectricity of HfO2 thin films after crystallization was investigated by applying uniaxial mechanical strains to Au/HfO2/TiN metal–ferroelectric–metal (MFM) capacitors. The remnant polarization (2P r) of MFM capacitors increased when tensile strain was applied during polarization switching. This phenomenon should not be attributed to phase transformation from the non-ferroelectric to the ferroelectric phase, taking account of the fast relaxation of 2P r after removal of the mechanical strain and the fact that the crystal structure of HfO2 thin films evaluated by grazing incidence X-ray diffraction measurement was not changed by the tensile strain.

Aggregation induced strong photoluminescence at room temperature in large-area C8BTBT thin films

Study of optical properties of 2,7-dioctyl[1]benzothieno[2,3-b]benzothiophene (C8BTBT) is promising for applications in low-cost and flexible optoelectronic devices. Here, we systematically investigated the thickness dependent structural and photophysical properties of large-area C8BTBT films. The large-area C8BTBT thin films of different thickness below 80 nm were prepared by off-centre spin coating method. Grazing incidence X-ray diffraction measurements confirm the highly crystalline nature of the thin films and reveal that crystal coherence length increases with increase of film thickness. The film morphology and its thickness were studied using atomic force microscopy. Further, optical absorption and emission behaviors of the thin films were analyzed. The results show strong ultraviolet (UV) emissions at room temperature. The photoluminescence behaviour of higher-thickness films differs from that of lower-thickness films. The thickness dependent UV emission spectra are explained in terms of defects and aggregation behavior of C8BTBT thin films. We determine the impact of thickness and aggregation (J- and H-type) on emission behaviors of the C8BTBT thin films. Our findings open a new avenue for the future optimization and prospective applications in photonics based on two-dimensional organic semiconductors.

Icephobic Gradient Polymer Coatings Deposited via iCVD: A Novel Approach for Icing Control and Mitigation.

Materials against ice formation and accretion are highly desirable for different industrial applications and daily activities affected by icing. Although several concepts have been proposed, no material has so far shown wide-ranging icephobic features, enabling durability and manufacturing on large scales. Herein, we present gradient polymers made of 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane (V4D4) and 1H,1H,2H,2H-perfluorodecyl acrylate (PFDA) deposited in one step via initiated chemical vapor deposition (iCVD) as an effective coating to mitigate ice accretion and reduce ice adhesion. The gradient structures easily overcome adhesion, stability, and durability issues of traditional fluorinated coatings. The coatings show promising icephobic performance by reducing ice adhesion, depressing the freezing point, delaying drop freezing, and inhibiting ice nucleation and frost propagation. Icephobicity correlates with surface energy discontinuities at the surface plane resulting from the random orientation of the fluorinated groups of PFDA, as confirmed by grazing-incidence X-ray diffraction measurements. The icephobicity could be further improved by tuning the surface crystallinity rather than surface wetting, as samples with random crystal orientation show the lowest ice adhesion despite high contact angle hysteresis. The iCVD-manufactured coatings show promising results, indicating the potential for ice control on larger scales and various applications.

Reaction Layer Formation on MgO in the Presence of Humidity.

Mineralization by MgO is an attractive potential strategy for direct air capture (DAC) of CO2 due to its tendency to form carbonate phases upon exposure to water and CO2. Hydration of MgO during this process is typically assumed to not be rate limiting, even at ambient temperatures. However, surface passivation by hydrated phases likely reduces the CO2 capture capacity. Here, we examine the initial hydration reactions that occur on MgO(100) surfaces to determine whether they could potentially impact CO2 uptake. We first used atomic force microscopy (AFM) to explore changes in reaction layers in water (pH = 6 and 12) and MgO-saturated solution (pH = 11) and found the reaction layers on MgO are heterogeneous and nonuniform. To determine how relative humidity (R.H.) affects reactivity, we reacted samples at room temperature in nominally dry N2 (∼11-12% R.H.) for up to 12 h, in humid (>95% R.H.) N2 for 5, 10, and 15 min, and in air at 33 and 75% R.H. for 8 days. X-ray reflectivity and electron microscopy analysis of the samples reveal that hydrated phases form rapidly upon exposure to humid air, but the growth of the hydrated reaction layer slows after its initial formation. Reaction layer thickness is strongly correlated with R.H., with denser reaction layers forming in 75% R.H. compared with 33% R.H. or nominally dry N2. The reaction layers are likely amorphous or poorly crystalline based on grazing incidence X-ray diffraction measurements. After exposure to 75% R.H. in air for 8 days, the reaction layer increases in density as compared to the sample reacted in humid N2 for 5-15 min. This may represent an initial step toward the crystallization of the reaction layer. Overall, high R.H. favors the formation of a hydrated, disordered layer on MgO. Based on our results, DAC in a location with a higher R.H. will be favorable, but growth may slow significantly from initial rates even on short timescales, presumably due to surface passivation.

Simultaneous Growth Strategy of High-Optical-Efficiency GaN NWs on a Wide Range of Substrates by Pulsed Laser Deposition.

Here, we explore a catalyst-free single-step growth strategy that results in high-quality self-assembled single-crystal vertical GaN nanowires (NWs) grown on a wide range of common and novel substrates (including GaN, Ga2O3, and monolayer two-dimensional (2D) transition-metal dichalcogenide (TMD)) within the same chamber and thus under identical conditions by pulsed laser deposition. High-resolution transmission electron microscopy and scanning transmission electron microscopy (HR-STEM) and grazing incidence X-ray diffraction measurements confirm the single-crystalline nature of the obtained NWs, whereas advanced optical and cathodoluminescence measurements provide evidence of their high optical quality. Further analyses reveal that the growth is initiated by an in situ polycrystalline layer formed between the NWs and substrates during growth, while as its thickness increases, the growth mode transforms into single-crystalline NW nucleation. HR-STEM and corresponding energy-dispersive X-ray compositional analyses indicate possible growth mechanisms. All samples exhibit strong band edge UV emission (with a negligible defect band) dominated by radiative recombination with a high optical efficiency (∼65%). As all NWs have similar structural and optical qualities irrespective of the substrate used, this strategy will open new horizons for developing III-nitride-based devices.

Structure of graphene oxide-phospholipid monolayers: A grazing incidence X-ray diffraction and neutron and X-ray reflectivity study

HypothesisGraphene oxide-based nanotechnology has aroused a great interest due to its applications in the biomedical and optoelectronic fields. The wide use of these materials makes it necessary to study its potential toxicity associated with the inhalation of Graphene Oxide (GO) nanoparticles and its interaction with the lung surfactant. Langmuir monolayers have proven to be an excellent tool for studying the properties of the lung surfactant and the effect of intercalation of nanoparticles on its structure and properties. Therefore, to know the origin of the phospholipids/GO interaction and the structure of the lipid layer with GO, in this work we study the effect of the insertion of GO sheets on a Langmuir film of 1,2-Dipalmitoyl-sn-glycerol-3-phosphocholine (DPPC). ExperimentsSurface pressure-area isotherms, Neutron (NR) and X-ray Reflectivity (XRR) and Grazing Incidence X-ray Diffraction (GIXD) measurements of hydrogenated and deuterated DPPC monolayers with and without GO have been carried out. FindingsThe results outline a strong interaction between the GO and the zwitterionic form of DPPC and prove that GO is in three regions of the DPPC monolayer, the aliphatic chains of DPPC, the head groups and water in the subphase. Comparison between results obtained with hydrogenated and deuterated DPPC allows concluding that both, electrostatic attractions, and dispersion forces are responsible of the interaction GO/DPPC. Results also demonstrated that the insertion of GO into the DPPC aliphatic chains does not induce significant changes on unit cell of DPPC.

Tensile stress regulated microstructures and ferroelectric properties of Hf0.5Zr0.5O2 films

The discovery of ferroelectricity in HfO2 based materials reactivated the research on ferroelectric memory. However, the complete mechanism underlying its ferroelectricity remains to be fully elucidated. In this study, we conducted a systematic study on the microstructures and ferroelectric properties of Hf0.5Zr0.5O2 (HZO) thin films with various annealing rates in the rapid thermal annealing. It was observed that the HZO thin films with higher annealing rates demonstrate smaller grain size, reduced surface roughness and a higher portion of orthorhombic phase. Moreover, these films exhibited enhanced polarization values and better fatigue cycles compared to those treated with lower annealing rates. The grazing incidence x-ray diffraction measurements revealed the existence of tension stress in the HZO thin films, which was weakened with decreasing annealing rate. Our findings revealed that this internal stress, along with the stress originating from the top/bottom electrode, plays a crucial role in modulating the microstructure and ferroelectric properties of the HZO thin films. By carefully controlling the annealing rate, we could effectively regulate the tension stress within HZO thin films, thus achieving precise control over their ferroelectric properties. This work established a valuable pathway for tailoring the performance of HZO thin films for various applications.

The Effect of Acyl Chain Position on the 2D Monolayer Formation of Monoacyl-sn-Glycerol at the Air/Water Interface: Quantum Chemical Modeling

This paper deals with the results of quantum chemical modeling of the monoacyl-sn-glycerol 2D cluster formation at the air/water interface using a semi-empirical PM3 method. The impact of the 2 or 3 positions of the acyl substituent on the thermodynamics of the monolayer formation is assessed for surfactants with an acyl substituent CnH2n+1COO chain length of n = 6–17 carbon atoms. The calculation shows a significant change in the spontaneous clusterization threshold for isomeric compounds, which differs only in the position of the acyl substituent with respect to the glycerol backbone. This change is almost equal to substituent shortening by approximately two methylene fragments. At the same time, the geometric parameters of the unit cell for resulting monolayers are not affected so drastically. The 2D films in question possess an oblique or orthorhombic unit cell with parameters for 2 and 3-monoacyl-sn-glycerol monolayers, as follows: a = 4.91 Å and 4.82 Å and b = 5.00 Å and 4.92 Å, with hydrocarbon chains tilted at t = 23.0° and 23.5°. The calculated results are in accordance with existing experimental data obtained using grazing incidence X-ray diffraction measurements and the π-A isotherm technique.

Ion irradiation induced modification in the electrical properties and the electronic structures of vanadium dioxide thin films

Ion irradiation modifies the physical properties of oxide materials. The present study focuses on the effect of 150 keV Fe and Ni ion irradiations in VO2 thin films. These films were deposited by pulsed laser on an r-cut sapphire substrate (1 1‾ 02). The range of ion fluences was from 1 × 1014 to 1 × 1016 ions/cm2 and these samples were characterized by using grazing incidence X-ray diffraction (GIXRD), Raman spectroscopy, Temperature-dependent resistivity measurements (R-T), and Hall effect measurement. While the presence of monoclinic phases is confirmed by GIXRD and Raman measurements, the ion irradiation on VO2 modifies the metal to insulator transition temperature (MIT). The R-T measurement with supporting analysis of carrier concentration authenticates a decrease in transition temperature and an increase in conductivity with an increment of ion-fluences. Synchrotron-based X-ray photoemission spectroscopy (XPS), and X-ray absorption spectroscopy (XAS) revealed that Vanadium ions are in mixed oxidation states of 4+ and 5+ after ion irradiation. Further, the Photo-Electron Spectroscopy (PES) measurement indicates the metallization of VO2 after ion irradiation consistent with R-T measurements.

Characterization of electrochemical deposition of copper and copper(I) oxide on the carbon nanotubes coated stainless steel substrates

The nanocomposite coatings composed of carbon nanotubes and various forms of copper were prepared in the two-step process. Firstly, carbon nanotubes were coated on stainless steel substrate using electrophoretic deposition at constant current. Then, the process of electrochemical deposition using copper(II) sulphate solutions was performed under high overpotential conditions. The modification of the copper(II) cations concentration in the solution and the deposition time provided the formation of various forms of crystals. The samples and their cross-sections were observed and examined using scanning electron microscope equipped with electron dispersive spectroscopy system. The analysis of chemical composition revealed that in addition to the pure copper crystals, the crystals characterized by the presence of copper and oxygen were formed. Therefore, Raman spectroscopy was applied to determine the unknown stoichiometry of this copper oxide. The point and in-depth analysis identified copper(I) oxide in the form of different size crystals depending on the concentration of the copper(II) sulphate solution. To confirm these findings, grazing incidence X-ray diffraction measurements were also performed. the combination of the applied methods has provided the detailed description of the preparation of the nanocomposite coatings with the proposed mechanism of copper(I) oxide formation.

Study of Nitridation Effect on Structural, Morphological, and Optical Properties of GaAs Film Growth on Silicon Substrates via Close Space Vapor Transport Technique

In this work, Gallium Arsenide (GaAs) films growth via Close Space Vapor Transport (CSVT) technique on n-type Silicon (Si) substrates (100) and its nitridation effect in the ammonia (NH3) environment is reported. The GaAs films were grown at 800, 900, and 1000 ∘C, and the nitridation process was carried out at 900 ∘C with an NH3:H2 gasses ratio. The GaAs films with and without nitridation process were analyzed using X-ray diffraction (XRD), Raman spectroscopy, Diffuse Reflectance Spectroscopy, and Scanning Electron Microscopy with Energy Dispersive X-ray analysis (SEM-EDX). Grazing incidence X-ray diffraction measurements of GaAs films nitrided confirm a polycrystalline GaN wurtzite structure with preferential orientation along (002), and additionality, a crystallographic plane (310) of low intensity is observed in 2θ=52.18∘ corresponding to Ga2O3. The average quantification results in weight (Wt. %) of GaAs films nitrided was determined by EDS; Ga∼79, N∼17.1, O∼2 and As∼1.8 Wt. %. The presence of GaN, GaxOy, Si, and GaAs modes were found by Raman measurements, demonstrating a partial nitriding. The band gap estimation by diffuse reflectance was between 3.2 and 3.38 eV such values are close to that reported for bulk GaN (3.4 eV). The presence of oxygen in the structure could be related to substrates or the GaAs source.

Mechanisms of Silicon Surface Passivation by Negatively Charged Hafnium Oxide Thin Films

We have studied the mechanisms underpinning effective surface passivation of silicon with hafnium oxide (HfO <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> ) thin films grown <italic xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">via</i> atomic layer deposition (ALD). Plasma-enhanced ALD with O <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> plasma and a tetrakis(dimethylamido)hafnium precursor was used to deposit 12 nm thick HfO <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> films at 200 °C on high-lifetime 5 Ωcm <italic xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">n</i> -type Czochralski silicon wafers. The passivation was activated by postdeposition annealing, with 30 min in air at 475 °C found to be the most effective. High-resolution grazing incidence X-ray diffraction measurements revealed the film crystallized between 325 and 375 °C, and this coincided with the onset of good passivation. Once crystallized, the level of passivation continued to increase with higher annealing temperatures, exhibiting a peak at 475 °C and yielding surface recombination velocities of <5 cm s <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">−1</sup> at 5 × 10 <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">14</sup> cm <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">−3</sup> injection. A steady decrease in effective lifetime was then observed for activation temperatures >475 °C. By superacid repassivation, we demonstrated this reduction in lifetime was not because of a decrease in the bulk lifetime, but rather because of changes in the passivating films themselves. Kelvin probe measurements showed the films are negatively charged. Corona charging experiments showed the charge magnitude is of order 10 <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">12</sup> qcm <sup xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">−2</sup> and that the reduced passivation above 475 °C was mainly because of a loss of chemical passivation. Our study, therefore, demonstrates the development of highly charged HfO <sub xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink">2</sub> films and quantifies their benefits as a standalone passivating film for silicon-based solar cells.

Cu interfaced Fe/Pt multilayer with improved (001) texture, enhanced L10 transformation kinetics and high magnetic anisotropy

In the present work, enhanced L10 ordering kinetics with improved crystallographic texturing in [001] direction and high magnetic coercivity of about 6 kOe is observed in L10 ordered Fe(1-x)CuxPt films, after successive isochronal vacuum annealing of multilayer structure [(Fe(1-x)/Cux)/Pt]x10. Synchrotron grazing incidence x-ray diffraction (GIXRD) measurements, performed using area detector confirms the onset of L10 ordering at 200 °C and presence of high degree of ordering at 300 °C. In-plane and out-of-plane GIXRD measurements validates texturing of magnetic easy axis [001] in out of film plane direction. Enormous increase in magnetic coercivity is observed from MOKE measurements in L10 ordered state. Lower ordering temperature with enhance (001) texturing and high magnetic coercivity is desirable for potential device applications of FePt. Effect of Cu and annealing temperature on structural and magnetic properties is investigated systematically in Fe(1-x)CuxPt films. Structural investigation discloses that lattice distortion in L10 ordered state caused by Cu addition and high interfacial energy associated with initial multilayer structure drives faster interdiffusion. Both of these aspects collectively work for FCC to FCT transformation, hence results in enhanced kinetics and texturing effects of L10 FePt.

A grazing incidence diffraction setup for Langmuir trough experiments at the high-resolution diffraction beamline P08 at PETRA III

The Langmuir Grazing Incidence Diffraction setup at the high-resolution diffraction beamline P08 of PETRA III is a dedicated setup for grazing incidence X-ray scattering measurements on Langmuir troughs. The instrument is optimized for low background grazing incidence X-ray diffraction measurements at vapour-water interfaces, while offering rapid layer structure assessment by grazing incidence X-ray off-specular scattering, and interfacial element analysis by total reflection X-ray fluorescence spectroscopy. Its control system is intuitive and standardized to provide easy access for non-expert users, and permits automated operation except for sample exchange.

Study of ruthenium film grown in oxygen environment for x-ray optics application

Ru shows high damage threshold as compared to other standard materials Au, Rh and Pt for high heat load applications in high brilliance synchrotron radiation source and x-ray free electron laser. It is also a promising candidate to be used as a protective capping layer in multilayers for increasing their life time. In the present study, Ru thin films of 500Å thickness were deposited in oxygen environment at different substrate temperatures varying from 70°C to 500°C. In reactive ion beam sputtering process, the flow of Ar and reactive O2 gas was maintained in 4:1 ratio keeping total flow 3 SCCM constant. The deposited films were characterized using grazing incidence x-ray reflectivity (GIXRR), grazing incidence x-ray diffraction (GIXRD) and secondary ion mass spectroscopy (SIMS) techniques. A significant change in GIXRR profile was observed in the sample grown at 100°C and 500°C whereas the GIXRD measurements indicated no significant formation of ruthenium oxide at different temperatures. However, a strong peak of Ru2Si3 (222) at 500°C was observed indicating a strong interfacial reaction at ruthenium/ substrate interface.The experimental data suggested a weak signature of RuO2 phase in the films deposited at RT, 70°C and 100°C and therefore the effect of ruthenium oxide with 10% composition in pure ruthenium was calculated on optical performance in extreme ultra violet region of photon energy (85-115 eV).

Residual strain engineering in seed layer assisted Kesterite Cu2ZnSnS4 absorber layer

Narrow-phase stability of CZTS often leads to the formation of secondary phases and defects that eventually results in disorder in the crystal structure. Moreover, lattice-mismatch and thermal stress at CZTS/Mo interface nourish strained growth, which adversely affects the Cu-Zn ordering in CZTS. Thus far, understanding and evolution of these residual strains and their influence on the optoelectronic properties of CZTS are lacking. Herein, we probed the residual strain along penetration depth and demonstrated a facile approach of tailoring lattice strain in CZTS. High quality CZTS films with seed layer (SL) growth are developed to investigate residual strain distribution using depth-dependent grazing incidence X-ray diffraction (GIXRD) measurements. A graded strain has been identified in SL films than uniformly strained no SL films. Besides improvement in Cu-Zn order, Photoluminescence (PL) signal in SL films was substantially quenched by 55.3%, which is ascribed to the charge transfer as a consequence of graded strain. Graded strain in SL films tends to form multi-homojunction, influencing charge carrier dynamics, resulting in a 36-fold increase in photocurrent and approximately 5 times faster response over No SL CZTS based device. • Seed layer influences the distribution of residual strain in CZTS absorber layer • Graded strain present in seed layer CZTS films relative to uniform strain in pristine • Structural ordering improved with seed layer growth • Charge transfer within the absorber layer leads to substantial PL quenching • Enhanced photocurrent and 5 times faster response recorded in SL-CZTS photodetector

Thickness dependence of spin Seebeck resistivity in polycrystalline YIG films grown by metal organic decomposition method

In this work, we investigated the dependence of spin Seebeck effect (SSE) voltages on the thickness of yttrium iron garnet (Y3Fe5O12-YIG) thin films grown on a silicon (Si) substrate fabricated by a metal-organic decomposition (MOD) method. The thickness of films was controlled by repeated spin coating and annealing cycles. Based on grazing incidence X-ray diffraction measurements, the YIG thin films displayed high crystallinity without secondary peaks, despite the increase in thickness. Scanning electron microscopy revealed uniform, highly dense films for samples having a thickness in the range of 37–260 nm. Magnetic hysteresis loops showed similar coercivities of <36 Oe for all samples, confirming the high quality of the YIG films, regardless of mismatch between the lattice constants of YIG and the substrate. Spin Seebeck resistivity results revealed a strong dependence on the thickness of the samples and the local maxima for 138-nm-thick YIG. This was attributed to the effect of the magnon energy relaxation length (ξL), which is shorter in comparison to that of a single-crystal YIG film grown on gadolinium gallium garnet. In this study, facile fabrication of hundreds of nanometers-thick YIG films on a Si substrate was achieved, for applications involving thermoelectric energy harvesting.

Evidence of rutile to anatase phase transition of TiO2 thin film electrode during 1st discharging cycle of Li ion batteries

TiO2 is a potential candidate for thin film electrode in Li ion batteries since it is abundant, cheap, has high theoretical specific capacity and can be produced in thin film form of desired crystallographic phase relatively easily by various physical vapor deposition techniques. Rutile phase TiO2 thin films have been prepared by radio frequency magnetron sputtering technique on stainless steel substrates at 450 °C substrate temperature, followed by post deposition annealing in air at 600 °C. These samples have been used as anode in Li ion batteries which are subjected to discharge/charge cycles. The electrodes have been extracted by de-crimping the batteries at various stages during the 1st discharge and 1st charge cycles and structural characterizations of these samples have been carried out by Grazing Incidence X-ray diffraction measurements with a laboratory X-ray source and Extended X-ray absorption fine structure measurements using synchrotron radiation. A clear signature of rutile to anatase phase transition has been observed in the samples during 1st discharge or Li ion insertion process, which is subsequently retained during the 1st charging cycle also. This is also verified by Raman spectroscopy measurements on few samples and is further corroborated by the constant voltage plateau observed in the galvanostatic cycle (potential versus capacitance plot) of the Li ion battery also during the 1st discharge cycle.

Investigation of long term stability of W/B4C multilayer structures

The long term stability of as-deposited, annealed, and synchrotron radiation exposed W/B4C multilayer structures was investigated. The multilayer structures were studied using hard X-ray reflectivity, grazing incidence X-ray diffraction (GIXRD), extended X-ray absorption fine structure (EXAFS), and atomic force microscopy (AFM). The structural degradation in annealed and synchrotron radiation exposed samples occurs at faster rate as compared to untreated samples. The structural degradation rate clearly depends on the thickness of B4C layer in multilayer structures. GIXRD measurements confirm the formation of tungsten carbide and boride phases. From EXAFS measurements at the W L3-edge, we find that the increase in the diffusion of oxygen is responsible for the observed structural degradation at faster rate in annealed samples consisting of thinner B4C layer. AFM images reveal that the surface modifications occur at slower rate in untreated samples as compared to annealed samples. Moreover, B4C proves to be an efficient cap layer to protect the as-deposited and annealed multilayer structures from oxidation.