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We developed and demonstrate an analysis method in which we calibrate the intensity scale of cross-sectional transmission electron microscopy (TEM) using Cu Kα reflectometry. This results in quantitative in-depth density profiles of multilayer structures. Only three free parameters are needed to obtain the calibrated profiles, corresponding to three TEM image intensity levels. Additionally, the optical indices of the two multilayer materials used and the assumption that the layers are laterally homogeneous are used in the model. The power and the general usefulness of the method is demonstrated using experimental data of W/Si and Mo/Si multilayer systems with sharp interfaces as well as multilayers of which the interfaces were deliberately intermixed. [ABSTRACT FROM AUTHOR]

In this study, we combine low-energy ion scattering (LEIS) static and sputter depth profiles for characterization of the oxidation kinetics on Zr, Mo, Ru, and Ta films of various thicknesses, followed by exposure to atomic oxygen at room temperature (∼20 °C). A method for nondestructive determination of the oxide growth rate via LEIS static depth profiling (static DP) is presented in detail. This method shows high sensitivity to the oxide thickness formed, and the results are in agreement with those obtained by X-ray reflectometry and sputter depth profiling (sputter DP). Sequential exposures of oxygen isotopes in combination with LEIS sputter DP are applied to elucidate the growth mechanism of the oxide films. The results indicate that the oxidation kinetics at the applied experimental conditions is directly influenced by the metal work function, characterizing a Cabrera-Mott growth type. The maximum thickness of the formed oxide and oxide growth rate are in the order Zr ≈ Ta > Mo > Ru. The combining of analysis by LEIS static DP and isotope tracing sputter DP is decisive in the characterization of oxidation kinetics in the room temperature regime. [ABSTRACT FROM AUTHOR]

An experimental study of oxide reduction at the surface of ruthenium layers on top of multilayer mirrors and thin Ru/Si films is presented. Oxidation and reduction processes were observed under conditions close to those relevant for extreme ultraviolet lithography. The oxidized ruthenium surface was exposed to a low-temperature hydrogen plasma, similar to the plasma induced by extreme ultraviolet radiation. The experiments show that hydrogen ions are the main reducing agent. Furthermore, the addition of hydrogen radicals increases the reduction rate beyond that expected from simple flux calculations. We show that low-temperature hydrogen plasmas can be effective for reducing oxidized top surfaces. Our proof-of-concept experiments show that an in situ, EUV-generated plasma cleaning technology is feasible. [ABSTRACT FROM AUTHOR]

We have studied the effect of photoelectrons on defect formation in graphene during extreme ultraviolet (EUV) irradiation. Assuming the major role of these low energy electrons, we have mimicked the process by using low energy primary electrons. Graphene is irradiated by an electron beam with energy lower than 80 eV. After e-beam irradiation, it is found that the D peak, I(D), appears in the Raman spectrum, indicating defect formation in graphene. The evolution of I(D)/I(G) follows the amorphization trajectory with increasing irradiation dose, indicating that graphene goes through a transformation from microcrystalline to nanocrystalline and then further to amorphous carbon. Further, irradiation of graphene with increased water partial pressure does not significantly change the Raman spectra, which suggests that, in the extremely low energy range, e-beam induced chemical reactions between residual water and graphene are not the dominant mechanism driving defect formation in graphene. Single layer graphene, partially suspended over holes was irradiated with EUV radiation. By comparing with the Raman results from e-beam irradiation, it is concluded that the photoelectrons, especially those from the valence band, contribute to defect formation in graphene during irradiation. [ABSTRACT FROM AUTHOR]

We report on the influence of sample temperature on the development of hydrogen-induced blisters in Mo/Si thin-film multilayers. In general, the areal number density of blisters decreases with increasing exposure temperature, whereas individual blister size increases with exposure temperatures up to ~200 °C but decreases thereafter. Comparison as a function of sample temperature is made between exposures to a flux containing both hydrogen ions and neutrals and one containing only neutrals. In the case of the neutral-only flux, blistering is observed for exposure temperatures ~90 °C. The inclusion of ions promotes blister formation at <90 °C, while retarding their growth at higher temperatures. In general, ion-induced effects become less evident with increasing exposure temperature. At 200 °C, the main effect discernable is reduced blister size as compared with the equivalent neutral-only exposure. The temperature during exposure is a much stronger determinant of the blistering outcome than either pre- or post-annealing of the sample. The trends observed for neutral-only exposures are attributed to competing effects of defect density thermal equilibration and H-atom induced modification of the Si layers. Energetic ions modify the blistering via (temperature dependent) enhancement of H-mobility and re-crystallization of amorphous Si. [ABSTRACT FROM AUTHOR]

The role that energetic (>800 eV) hydrogen ions play in inducing and modifying the formation of blisters in nanoscale Mo/Si multilayer samples is investigated. Such samples are confirmed to be susceptible to blistering by two separate mechanisms. The first is attributed to the segregation of H atoms to voids and vacancies associated with the outermost Mo layer, driving blister formation in the form of H2 filled bubbles. This process can occur in the absence of ions. A second blister distribution emerges when energetic ions are present in the irradiating flux. This is attributed to an ion-induced vacancy clustering mechanism that produces void blisters. The defects and strained states associated with the Mo-on-Si interfaces provide the preferred nucleation points for blistering in both cases. The effects of ions are ascribed to promotion of hydrogen uptake and mobility, in particular through the Si layers; to the generation of additional mobile species in the Si and Mo layers; and to the creation of new blister nucleation points. In addition to directly stimulating blistering via vacancy clustering, ions modify the development of H2-filled blisters. This is most evident in the formation of multi-component structures due to overlapping delaminations at different layer interfaces. This affect is attributed to the introduction of active transport of hydrogen from the H2 filled blisters across the outermost Mo-on-Si interface to the underlying layers. Ion-induced variations in hydrogen uptake and distribution and in the rates of blister nucleation and growth produce lateral differences in blister size and areal number density that create a macroscopic concentric pattern across the surface. [ABSTRACT FROM AUTHOR]

Presents an x-ray absorption measurements on silicon clusters and silicon plasmas produced by pulsed laser irradiation of bulk silicon. Comparison of the results with earlier time-resolved x-ray absorption measurements on amorphous silicon foils under pulsed laser irradiation. Formation of clusters; Detection of a removed silicon layer.

Describes a time-resolved x-ray absorption measurements on pulsed laser irradiated silicon. Categories of the absorption spectra recorded at a delay time of 12 nanoseconds; Information on several time-resolved techniques; Steps in obtaining the irradiation beam; Analysis of the behavior at optical wavelengths.

Presents a study which examined some of the properties of laser-generated plasma emission in the soft x-ray region. Experimental details; Information on spectral distributions; Conclusions.

Investigates the process of ion bombardment for the fabrication of Mo/Si multilayer x-ray mirrors using e-beam evaporation. Application of the ion treatment after deposition of each of the Si layers; Analysis of multilayer structures; Determination of interface roughness.

A fully self-contained in-vacuum device for measuring thin film stress in situ is presented. The stress was measured by measuring the curvature of a cantilever on which the thin film was deposited. For this, a dual beam laser deflectometer was used. All optics and electronics needed to perform the measurement are placed inside a vacuum-compatible vessel with the form factor of the substrate holders of the deposition system used. The stand-alone nature of the setup allows the vessel to be moved inside a deposition system independently of optical or electronic feedthroughs while measuring continuously. A Mo/Si multilayer structure was analyzed to evaluate the performance of the setup. A radius of curvature resolution of 270 km was achieved. This allows small details of the stress development to be resolved, such as the interlayer formation between the layers and the amorphous-to-crystalline transition of the molybdenum which occurs at around 2 nm. The setup communicates with an external computer via a Wi-Fi connection. This wireless connection allows remote control over the acquisition and the live feedback of the measured stress. In principle, the vessel can act as a general metrology platform and add measurement capabilities to deposition setups with no modification to the deposition system. [ABSTRACT FROM AUTHOR]

The structural changes in Ru-coated Y films during hydrogenation were studied in this work. In situ XRD data were used to show that the Y to YH2 transition requires significant hydrogen loading of the Y lattice. By comparing the XRD data with the in situ spectroscopic ellipsometry data, an effective medium model for the transition was obtained. This model describes the Y to YH2 transition well. The YH2 to YH3 transition is also described by an effective medium model, however, with reduced accuracy around the midpoint of the transition. By comparing the YH2 and YH3 crystal sizes, we show that these deviations may be due to a surface plasmon resonance. The improved understanding of the ellipsometry measurements is important for optical hydrogen sensing applications. [ABSTRACT FROM AUTHOR]

The growth development of nanometer thick Mo and Si layers was studied using in situ laser deflection and Low Energy Ion Scattering (LEIS). The growth stress obtained from changes in wafer curvature during growth is correlated to changes in the surface stochiometry monitored by LEIS. For Si on Mo, the compressive-tensile-compressive stress development could be explained by the formation of interfacial silicide compounds and the transition between these and the bulk growth of Si. For Mo on Si, a strong initial tensile stress due to silicide formation saturates upon reduced availability of free Si at the growing Mo surface, followed by a near instantaneous tensile increase in stress related to the amorphous-to-crystalline phase transition, which coincides with the end of the compound formation, as determined with LEIS. [ABSTRACT FROM AUTHOR]

The effect of ion polishing in sputter deposited W/Si multilayer mirrors with a d-spacing of 2.5 nm was studied. 0.1 to 0.5 nm of Si were etched with 100 eV Ar+ ions. This process resulted in a pronounced reduction in diffused scattering, measured at wavelengths about 0.1 nm. However, CuKa X-ray specular reflectivity and AFM showed only a marginal reduction of the roughness amplitude in the systems. Furthermore, the soft X-ray reflectivity at 0.84 and 2.4 nm did not show any changes after the ion polishing as compared to the nonpolished structures. Grazing incidence X-ray reflectivity (GIXR) analysis revealed that there was no pure W present in the deposited multilayers, with WSi2 being formed instead. As a result, it was concluded that the initial roughness in W/Si multilayers grown by magnetron sputtering is not the major factor in the reflectivity deviation from the calculated value for an ideal system. Nevertheless, the grazing incidence small-angle X-ray scattering (GISAXS) analysis revealed that ion polishing reduces the vertical propagation of roughness from layer to layer by a factor of two, as well as favorably affecting the lateral correlation length and Hurst parameter. These improvements explain the reduction of diffused X-ray scattering at 0.1 nm by more than an order of magnitude, which is relevant for applications like high resolution XRD analysis. [ABSTRACT FROM AUTHOR]

Integration of Zr0.52Ti0.48O3 (PZT) films on glass substrates is of high importance for device applications. However, to make use of the superior ferro- and piezoelectric properties of PZT, well-oriented crystalline or epitaxial growth with control of the crystal orientation is a prerequisite. In this article, we report on epitaxial growth of PZT films with (100)- and (110)-orientation achieved by utilizing Ca2Nb3Oi0 (CNO) and Ti0 87O2 (TO) nanosheets as crystalline buffer layers. Fatigue measurements demonstrated stable ferroelectric properties of these films up to 5 x 109 cycles. (100)-oriented PZT films on CNO nanosheets show a large remnant polarization of 21 iC/cm2 that is the highest remnant polarization value compared to (110)-oriented and polycrystalline films reported in this work. A piezoelectric response of 98pm/V is observed for (100)-oriented PZT film which is higher than the values reported in the literature on Si substrates. [ABSTRACT FROM AUTHOR]

We have investigated the thermal stability of La/B-based (LaN/La/B) multilayer structures with partial-layer nitridation of La, a method shown earlier to result in enhanced reflectivity. The structures were annealed in the temperature range 100–500 °C for 70 h. They showed period drifts by 0.005 nm at 100 °C to 0.06 nm at 500 °C. A reflectivity loss of more than 2% was only observed after annealing above 300 °C. The study included separate investigation of B-on-LaN and LaN-on-La-on-B interfaces. [ABSTRACT FROM AUTHOR]

The initial growth of DC sputtered ZrO2 on top of a-Si, SiN, and SiO2 layers has been studied by in vacuo high-sensitivity low energy ion scattering for two gas deposition conditions with different oxygen contents (high-O and low-O conditions). This unique surface sensitive technique allowed the determination of surface composition and thicknesses required to close the ZrO2 layer on all three substrates for both conditions. The ZrO2 layer closes similarly on all substrates due to more favorable enthalpies of formation for ZrO2 and ZrSiO4, resulting in passivation of the Si from the substrate. However, this layer closes at about half of the thickness (~1.7 nm) for low-O conditions due to less oxidative conditions and less energetic particles arriving at the sample, which leads to less intermixing via silicate formation. In contrast, for high-O conditions, there is more ZrSiO4 and/or SiOx formation, giving more intermixing (~3.4 nm). In vacuo X-ray photoelectron spectroscopy (XPS) measurements revealed similar stoichiometric ZrO2 layers deposited by both conditions and a higher interaction of the ZrO2 layer with the underlying a-Si for high-O conditions. In addition, oxygen diffusion through low-O ZrO2 films on a-Si has been investigated by ex situ angular-resolved XPS of samples annealed in atmospheric oxygen. For temperatures below 400 °C, no additional oxidation of the underlying a-Si was observed. This, together with the amorphous nature and smoothness of these samples, makes ZrO2 a good candidate as an oxidation protective layer on top of a-Si. [ABSTRACT FROM AUTHOR]

Highlights: [•] In vacuum study of nanometers thick molybdenum silicon layers and multilayers under growth conditions used for typical Mo/Si multilayer optics. [•] Scanning tunneling microscopy of these layers allows detailed morphology characterization up to lateral dimensions of 1nm at any time during multilayer growth. [•] Both silicon and molybdenum layers contribute to an equal amount to the surface morphology of Mo/Si multilayers. [ABSTRACT FROM AUTHOR]

Abstract: We report on the uptake of deuterium by thin-film Mo/Si multilayer samples as a result of exposure to fluxes of predominantly thermal atomic and molecular species, but also containing a small fraction of energetic (800–1000eV) ions. These exposures result in blister formation characterized by layer detachment occurring exclusively in the vicinity of the Mo-on-Si interfaces. This localization is attributed to strained centers introduced within the interfacial region during silicide formation and subsequent Mo crystallization. The correlation between D-content and blistering was studied. After an initial uptake period the D-content stabilized at ~1.3×1016 at./cm2. Blister development is not simply a function of the content. Different blistering processes are simultaneously operative, with three distinct distributions being observed. The areal number densities of the initial two blister distributions to appear are established before the content stabilizes, while the multilayer is susceptible to successive stages of blistering associated with the effects of energetic ions. H-atom depth profiling of hydrogen-exposed samples by resonant nuclear reaction analysis shows preferential accumulation in the Mo layers. A distinct local maximum with a remarkably high hydrogen concentration (~19at.%) develops in the outermost Mo layer. This is attributed to enhanced accommodation of hydrogen in voids and vacancies within the layer as a consequence of its polycrystalline structure and its highly-constrained state. [Copyright &y& Elsevier]

Abstract: The adsorption and reactions of ethanol on Ru(0001) were studied with temperature-programmed desorption (TPD) and reflection–absorption infrared spectroscopy (RAIRS). Ethanol was found to adsorb intact onto Ru(0001) below 100K. From 175K to 200K, ethanol is converted into ethoxy groups, which undergo further dehydrogenation, leading to the formation of hydrogen, CO and surface carbon. The absence of aldehydes and methane as desorbing product molecules, as well as the intermediate species observed in the RAIRS spectra, show that the reaction proceeds via β-hydrogen abstraction of the ethoxy groups, resulting in an oxametallacycle reaction intermediate that undergoes decarbonylation to CO, C and hydrogen. The surface carbon, formed by the reaction, decreases the reactivity of the surface in subsequent reaction cycles. The amount of CO produced from a full monolayer of ethanol is limited to about 0.1ML, because of the competition between ethanol dehydrogenation and desorption. [Copyright &y& Elsevier]

In vacuo high-sensitivity low energy ion scattering (HS-LEIS) has been used to investigate the initial growth stages of DC sputtered Ru on top of Si, SiN, and SiO2. The high surface sensitivity of this technique allowed an accurate determination of surface coverages and thicknesses required for closing the Ru layer on all three substrates. The Ru layer closes (100% Ru surface signal) at about 2.0, 3.2, and 4.7 nm on top of SiO2, SiN, and Si, respectively. In-depth Ru concentration profiles can be reconstructed from the Ru surface coverages when considering an error function like model. The large intermixing (4.7 nm) for the Ru-on-Si system is compared to the reverse system (Si-on-Ru), where only 0.9 nm intermixing occurs. The difference is predominantly explained by the strong Si surface segregation that is observed for Ru-on-Si. This surface segregation effect is also observed for Ru-on-SiN but is absent for Ru-on-SiO2. For this last system, in vacuo HS-LEIS analysis revealed surface oxygen directly after deposition, which suggests an oxygen surface segregation effect for Ru-on-SiO2. In vacuo XPS measurements confirmed this hypothesis based on the reaction of Ru with oxygen from the SiO2, followed by oxygen surface segregation. [ABSTRACT FROM AUTHOR]

Freestanding silicon nitride membranes with thicknesses down to a few tens of nanometers find use as TEM windows or soft X-ray spectral purity filters. As the thickness of a membrane decreases, emissivity vanishes, which limits radiative heat emission and resistance to heat loads. We show that thin metal layers with thicknesses in the order of 1 nm enhance the emissivity of thin membranes by two to three orders of magnitude close to the theoretical limit of 0.5. This considerably increases thermal load capacity of membranes in vacuum environments. Our experimental results are in line with classical theory in which we adapt thickness dependent scattering terms in the Drude and Lorentz oscillators. [ABSTRACT FROM AUTHOR]

This paper reports on the studies of anisotropic heat conduction phenomena in Mo/Si multilayers with individual layer thicknesses selected to be smaller than the mean free path of heat carriers. We applied the frequency-domain thermoreflectance technique to characterize the thermal conductivity tensor. While the mechanisms of the cross-plane heat conduction were studied in detail previously, here we focus on the in-plane heat conduction. To analyze the relative contribution of electron transport to the in-plane heat conduction, we applied sheet-resistance measurements. Results of Mo/Si multilayers with variable thickness of the Mo layers indicate that the net in-plane thermal conductivity depends on the microstructure of the Mo layers. [ABSTRACT FROM AUTHOR]

In situ X-ray reflectivity was used to reveal oxygen diffusion kinetics for thermal oxidation of polycrystalline ruthenium thin films and accurate determination of activation energies for this process. Diffusion rates in nanometer thin RuO2 films were found to show Arrhenius behaviour. However, a gradual decrease in diffusion rates was observed with oxide growth, with the activation energy increasing from about 2.1 to 2.4 eV. Further exploration of the Arrhenius pre-exponential factor for diffusion process revealed that oxidation of polycrystalline ruthenium joins the class of materials that obey the Meyer-Neldel rule. [ABSTRACT FROM AUTHOR]

We present a model independent approach for the analysis of X-ray fluorescence yield modulated by an X-ray standing wave (XSW), that allow a fast reconstruction of the atomic distribution function inside a sample without fitting procedure. The approach is based on the direct regularized solution of the system of linear equations that characterizes the fluorescence yield. The suggested technique was optimized for, but not limited to, the analysis of periodic layered structures where the XSW is formed under Bragg conditions. The developed approach was applied to the reconstruction of the atomic distribution function for LaN/BN multilayers with 50 periods of 43A ° thick layers. The object is especially difficult to analyze with traditional methods, as the estimated thickness of the interface region between the constituent materials is comparable to the individual layer thicknesses. However, using the suggested technique, it was possible to reconstruct width of the La atomic distribution showing that the La atoms stay localized within the LaN layers and interfaces and do not diffuse into the BN layer. The analysis of the reconstructed profiles showed that the positions of the center of the atomic distribution function can be estimated with an accuracy of 1A ° . VC 2014 AIP Publishing LLC. [ABSTRACT FROM AUTHOR]

An analysis procedure was developed that enables studying diffusion in ultrathin films by utilizing the depth-resolved information that is contained in the background of low energy ion scattering (LEIS) spectra. Using a high-sensitivity analyzer/detector combination allows for such a low ion dose that the ion-induced perturbation caused by this technique is negligible and not measurable with LEIS. The developed analysis procedure provides a unique opportunity to study diffusion processes in nanoscaled systems. It was applied to the Mo/Si system, a system that is relevant for extreme ultraviolet optics. [ABSTRACT FROM AUTHOR]

Both multilayer period thickness expansion and compaction were observed in Mo/B4C multilayers upon annealing, and the physical causes for this were explored in detail. Using in situ time-dependent grazing incidence X-ray reflectometry, period changes down to picometer-scale were resolved. It was shown that the changes depend on the thickness of the B4C layers, annealing temperature, and annealing time. Although strong stress relaxation during annealing was observed, it was excluded as a cause for period expansion. Auger electron spectroscopy and wide angle X-ray diffraction measurements revealed the growth of interlayers, with associated period changes influenced by the supply of B and C atoms to the growing compound interlayers. For multilayers with a Mo thickness of 3 nm, two regimes were recognized, depending on the deposited B4C thickness: in multilayers with B4C ≤ 1.5 nm, the supply of additional Mo into the already formed MoBxCy interlayer was dominant and led to densification, resulting in period compaction. For multilayers with B4C ≥ 2 nm, the B and C enrichment of interlayers formed low density compounds and yielded period expansion. [ABSTRACT FROM AUTHOR]

In this work, a technique for hydrogen diffusion measurements through thin films is proposed and demonstrated. A yttrium film, which changes its refractive index upon hydrogen absorption, is used as an optical sensor to detect hydrogen. The yttrium sensor is coated with a thin (up to 12 nm) layer of test material and exposed to atomic hydrogen. To ensure that the calculated diffusion constant is not artificially changed by surfaces processes, the test layer is coated with palladium. Hydrogen diffusion through test layers of Si, Al, Ag, Ru, Mo, Al2O3 and SiO2 were measured and compared with existing data. The hydrogenation time (time to form YH2) was found to exponentially scale with the enthalpy of hydrogen solution in the test material. Comparison between measured diffusion coefficients for different film thicknesses, as well as previously reported results, highlights the strong dependence of the diffusion constant on sample fabrication conditions, and hydrogen exposure conditions. It is concluded that diffusion through thin films can be reliably compared only when specimen form and exposure conditions are the same. The relevance of this study for applications is discussed. [ABSTRACT FROM AUTHOR]

In this paper, an experimental measurement of the diffusion constant of hydrogen in ruthenium is presented. By using a hydrogen indicative Y layer, placed under the Ru layer, the hydrogen flux through Ru was obtained by measuring the optical changes in the Y layer. We use optical transmission measurements to obtain the hydrogenation rate of Y in a temperature range from room temperature to 100 °C. We show that the measured hydrogenation rate is limited mainly by the hydrogen diffusion in Ru. These measurements were used to estimate the diffusion coefficient, D, and activation energy of hydrogen diffusion in Ru thin films to be D = 5.9 × 10−14 m2/s ∙ exp (-0.33 eV/ k B τ), with k B the Boltzmann constant and τ the temperature. Image 1 • Hydrogen diffusion through Ru films was studied. • Optical monitoring in transmission is used, with Y as H sensitive layer. • Pd capping layer ensures that H diffusion through Ru is limiting for H transport. • Diffusion constant and activation energy obtained in range 25–100 °C. [ABSTRACT FROM AUTHOR]

X-ray W/B multilayer mirrors with a period of 2.5 nm were deposited by dc magnetron sputtering and studied in comparison with W/Si multilayer systems of the same period. Transmission electron microscopy, grazing incidence X-Ray reflectivity, and x-ray photoelectron spectroscopy analysis revealed that the layer quality and interfaces of the W/B multilayers are not better than those of the W/Si multilayers. Strong intermixing between W and B is present, which leads to compound formation with little or no pure W left after the interaction: an optically unfavorable boride formation and an increased roughness result in a reduced reflectivity. The deposited W/B multilayer mirrors showed a reflectivity of 34.5% at 0.84 nm and angle of incidence 9.7°, compared to 40% obtained for W/Si multilayers. Ion polishing applied on the boron layers did not result in improvements of the reflectivity. [ABSTRACT FROM AUTHOR]

Following the recent demonstration of grazing‐incidence X‐ray fluorescence (GIXRF)‐based characterization of the 3D atomic distribution of different elements and dimensional parameters of periodic nanoscale structures, this work presents a new computational scheme for the simulation of the angular‐dependent fluorescence intensities from such periodic 2D and 3D nanoscale structures. The computational scheme is based on the dynamical diffraction theory in many‐beam approximation, which allows a semi‐analytical solution to the Sherman equation to be derived in a linear‐algebraic form. The computational scheme has been used to analyze recently published GIXRF data measured on 2D Si3N4 lamellar gratings, as well as on periodically structured 3D Cr nanopillars. Both the dimensional and structural parameters of these nanostructures have been reconstructed by fitting numerical simulations to the experimental GIXRF data. Obtained results show good agreement with nominal parameters used in the manufacturing of the structures, as well as with reconstructed parameters based on the previously published finite‐element‐method simulations, in the case of the Si3N4 grating. [ABSTRACT FROM AUTHOR]

Low energy ion polishing is attractive in thin films because of the small interaction zone with the treated material. In this context, various noble gases (Ne, Ar, Kr, and Xe) have been applied for low energy ion polishing of interfaces in nanoscale optical Mo/Si multilayers in order to mitigate the evolving roughness during the deposition process. The interface morphology has been studied by grazing incidence small angle x-ray scattering, the multilayer composition by x-ray photoelectron spectroscopy, and the general performance by extreme ultraviolet (EUV) reflectometry. Both the average roughness level and the vertical correlation length of the roughness can be reduced significantly by increasing the atomic mass of the ion species applied for polishing. Maximum EUV reflectance is observed for Kr+-polishing, while Xe+-polishing shows a superior structure. This apparent contradiction is explained by taking into account the optical absorption from noble gas residuals in the amorphous silicon layers. [ABSTRACT FROM AUTHOR]

B4C diffusion barrier layers are often introduced into Mo/Si multilayered films for enhancement of thermal stability. We observe that such multilayered films exhibit both period expansion and period compaction upon annealing at temperatures below 300 °C, depending on the annealing temperature and time. Using in-situ grazing incidence x-ray reflection measurements during sequential annealing, we resolved picometer periodicity changes in Mo/B4C/Si/B4C, Si/B4C, and Mo/B4C multilayer films, and show that the two opposite period-change effects are a result of interaction of Si with B4C layers, leading to expansion, and MoxSiy formation, leading to compaction. The study of Si/B and Si/C multilayer sub-systems suggests that the cause of expansion is the formation of relatively low density SixBy compounds at the Si-B4C interface. Although the Mo-B4C interface seems to be stable based on reflectometry data, other techniques such as depth profiling x-ray photoelectron spectroscopy and wide angle x-ray diffraction measurements show that Mo and B4C actually intermix. [ABSTRACT FROM AUTHOR]

We investigated the thermal stability of e-beam deposited Mo/B4C/Si/B4C layered systems, with and without ion assistance during the growth of the B4C diffusion barrier layers. The thermal stability was investigated by in situ thermal annealing during grazing incidence X-ray reflection. By studying partially treated B4C barrier layers, we found that the improvement in thermal stability is caused by an enhanced density of the B4C layer. [ABSTRACT FROM AUTHOR]

To enhance the thermal stability, B4C diffusion barrier layers are often added to Mo/Si multilayer structures for extreme ultraviolet optics. Knowledge about the chemical interaction between B4C and Mo or Si, however is largely lacking. Therefore, the chemical processes during annealing up to 600 °C of a Mo/B4C/Si layered structure have been investigated in situ with hard x-ray photoelectron spectroscopy and ex situ with depth profiling x-ray photoelectron spectroscopy. Mo/B/Si and Mo/C/Si structures have also been analyzed as reference systems. The chemical processes in these systems have been identified, with two stages being distinguished. In the first stage, B and C diffuse and react predominantly with Mo. MoSix forms in the second stage. If the diffusion barrier consists of C or B4C, a compound forms that is stable up to the maximum probed temperature and annealing time. We suggest that the diffusion barrier function of B4C interlayers as reported in literature can be caused by the stability of the formed compound, rather than by the stability of B4C itself. [ABSTRACT FROM AUTHOR]

The effect of an amorphous-to-nanocrystalline phase transition on the diffusion across an interface layer of subnanometer thickness has been investigated in real-time. The diffusion in the Mo/B4C/Si thin film structure studied was found to instantaneously enhance by an order of magnitude upon the formation of nanocrystals inducing the atomic-scale onset of grain boundary diffusion. [ABSTRACT FROM AUTHOR]

The formation and development of Mo-Si interfaces in Mo/Si multilayers upon thermal annealing, including a transition to h-MoSi2, have been investigated using high resolution transmission electron microscopy, x-ray reflectivity, and x-ray diffraction measurements. The silicide layers naturally formed at Mo-Si interfaces, i.e., just upon and after the deposition, are amorphous and have different thicknesses for as-deposited samples, with the Mo-on-Si interlayer being the largest. In addition, silicide growth at Mo-Si interfaces during annealing before the phase transformation predominantly takes place at the Mo-on-Si interface and a MoSi2 interface layer is formed. Diffusion continues until a thick MoSi2 layer is formed at the interface, at which point the interface crystallizes and diffusion speeds up, finally resulting in an abrupt intermixing and phase transition of the entire interface to h-MoSi2. This model predicts an onset of the phase transition which does not depend primarily on the annealing temperature but on a threshold thickness of the MoSi2 interface before crystallization takes place. This crystallization threshold is shown to exist not only in the Mo/Si system, but also occurs for Mo/Si multilayers where the natural interfaces are replaced by diffusion barriers. [ABSTRACT FROM AUTHOR]

We present a kinetic simulation of the plasma formed by photoionization in the intense flux of an extreme ultraviolet lithography (EUVL) light source. The model is based on the particle-in-cell plus Monte Carlo approach. The photoelectric effect and ionization by electron collisions are included. The time evolution of the low density argon plasma is simulated during and after the EUV pulse and the ion-induced sputtering of the coating material of a normal incidence collector mirror is computed. The relation between the time and position at which the ions are created and their final energy is studied, revealing how the evolution and the properties of the sheath influence the amount of sputtered material. The influence of the gas pressure and the source intensity is studied, evaluating the behavior of Ar+ and Ar2+ ions. A way to reduce the damage to the collector mirror is presented. [ABSTRACT FROM AUTHOR]

A structural characterization of W/Si multilayers using X‐ray reflectivity (XRR), scanning transmission electron microscopy (STEM) and grazing‐incidence small‐angle X‐ray scattering (GISAXS) is presented. STEM images revealed lateral, periodic density fluctuations in the Si layers, which were further analysed using GISAXS. Characteristic parameters of the fluctuations such as average distance between neighbouring fluctuations, average size and lateral distribution of their position were obtained by fitting numerical simulations to the measured scattering images, and these parameters are in good agreement with the STEM observations. For the numerical simulations the density fluctuations were approximated as a set of spheroids distributed inside the Si layers as a 3D paracrystal (a lattice of spheroids with short‐range ordering but lacking any long‐range order). From GISAXS, the density of the material inside the density fluctuations is calculated to be 2.07 g cm−3 which is 89% of the bulk value of the deposited layer (2.33 g cm−3). An inhomogeneity of material in W/Si multilayer structures was studied with grazing‐incidence small‐angle X‐ray scattering. The experimental study revealed lateral density fluctuations in the Si spacer layers. [ABSTRACT FROM AUTHOR]

Presents a study to optimize the growth process of Mo/Si multilayers, while observing the effect of an elevated susbstrate temperature during deposition in a temperature range of 300 K and 550 K. Details on methodology used to conduct study; Results of study; Discussion on findings.

We discuss a new method to characterize multilayer structures with grazing-incidence reflectivity measurements using hard x-ray radiation, such as Cu-K[sub α] or Mo-K[sub α] radiation. The method is based on the analysis of the reverse Fourier transforms of the reflectivity at the Bragg peaks in q-space, the reflectivity data being obtained from an angular scan (θ−2θ). This method is faster than curve fitting of the reflectivity data, results in an accurate value of the density and thickness of both materials, and needs no pre-assumptions about the material composition and the parameters of the multilayer. The method makes a distinction between interface roughness and layer thickness errors, and is independent of measurement of the critical angle. A minor disadvantage is that only an average value of the layer thickness is determined, rather than the individual layer thicknesses. As an example our method is used to analyze small-angle reflectivity measurements of Mo/Si and Co/C multilayers. The parameters thus obtained are used to model a structure, which is subsequently used to predict the near-normal incidence reflectivity at soft x-ray wavelengths. The accuracy thus found corresponds to a relative error of 5%. The densities of a Mo/Si multilayer are determined independently with critical angle measurements to verify the values obtained from the grazing incidence reflectivity measurements. The results of the analysis of the Co/C multilayer are compared to values obtained using a conventional method based on the kinematical theory. However, the conventional method requires additional data of soft x-ray reflectivity measurements. The new method yields the same values for the multilayer parameters but does not require the extra soft x-ray measurements. [ABSTRACT FROM AUTHOR]

In this work, we study the reaction of the dissociation products of carbon dioxide on a Ru(0 0 0 1) surface under Extreme Ultraviolet (EUV) light with a partial pressure of hydrogen. Our results show that both amorphous carbon and H 2 O are the end products of the CO 2 dissociation at the Ru surface, and these are produced only in the presence EUV and H 2 . Partial dissociation of CO 2 on the Ru surface is an intermediate step in the overall reaction. Using Reflection Absorption Infrared spectroscopy (RAIRS) and Temperature Programmed Desorption (TPD), only water is detected as molecular reaction product. We further show that this reaction deactivates the Ru surface due to the formation of an amorphous carbon layer, thereby confirming the catalytic role of Ru in the total reaction. [ABSTRACT FROM AUTHOR]

Grazing‐incidence X‐ray diffraction (GID) is a well known technique for the characterization of crystal surfaces. A theoretical study has been performed of the sensitivity of GID to the structure of a crystal surface and distorted nanometre‐thin surface layers. To simulate GID from crystals that have a complex subsurface structure, a matrix formalism of the dynamical diffraction theory has been applied. It has been found that the azimuthal rocking curves of a crystal that has a distorted subsurface, measured over a wide angular range, show asymmetric thickness oscillations with two distinguishable sets of frequencies: one corresponding to the diffraction in the single‐crystal subsurface layer and the second corresponding to the diffraction in the single‐crystal substrate. Therefore, azimuthal rocking curves allow characterization of the subsurface structure of a single crystal. Furthermore, thickness oscillations induced by evanescent diffraction modulate the specular reflection intensity, showing high‐intensity modulations. This will potentially allow implementation of subsurface crystal characterization using, for instance, a laboratory‐scale X‐ray diffractometer. [ABSTRACT FROM AUTHOR]

In this paper we study the reaction of water and graphene under Extreme Ultraviolet (EUV) irradiation and in the presence of hydrogen. In this work, single layer graphene (SLG) on amorphous Si as an underlying substrate was dosed with water (0.75 mL) and exposed to EUV ( λ = 13.5 nm, 92 eV) with partial pressures of H 2 in the background. The results show that the aromatic structure of graphene, when exposed to EUV and H 2 , breaks down into aryl ketones and enols of 1,3 di-ketone. Infrared (IR) spectroscopy shows that SLG oxidizes, with increasing H 2 pressure leading to the grain boundary edges of graphene forming ketones and carboxylic acids. In situ and post exposure analyses also reveal that EUV exposure reduces the sp 2 content of the graphene layer, with the sp 3 content increasing, resulting in a more defective graphene layer. [ABSTRACT FROM AUTHOR]

The diffusion barrier properties of Sc2O3 against metal diffusion were studied. Tin and ruthenium were used as probe materials to study the barrier properties of Sc2O3 in thickness ranges that are of relevance for gate materials. Tin deposition and hydrogen radical etching from Sc2O3 layers of 0.5-1.5 nm thickness, deposited on Ru, show that these Sc2O3 layers effectively block the diffusion of Sn into Ru. We show that Sn adhesion and etching depends strongly on the thickness of the Sc2O3 film. The etch-rate is found to be inversely proportional to the Sc2O3 layer thickness, which we attribute to Sc2O3 becoming a more effective charge transfer barrier at larger thicknesses. [ABSTRACT FROM AUTHOR]

The role of oxide on Sn adhesion to Sc surfaces was studied with in-situ ellipsometry, X-ray photoelectron spectroscopy and secondary electron microscopy. Sn etching with hydrogen radicals was performed on metallic Sc, metallic Sc with a native oxide, and a fully oxidized Sc layer. The results show that Sn adsorbs rather weakly to a non-oxidized Sc surface, and is etched relatively easily by atomic hydrogen. In contrast, the presence of native oxide on Sc allows Sn to adsorb more strongly to the surface, slowing the etching. Furthermore, thinner layers of scandium oxide result in weaker Sn adsorption, indicating that the layer beneath the oxide plays a significant role in determining the adsorption strength. Unexpectedly, for Sn on Sc2O3, and, to a lesser extent, for Sn on Sc, the etch rate shows a variation over time, which is explained by surface restructuring, temperature change, and hydrogen adsorption saturation. [ABSTRACT FROM AUTHOR]

We have modified and stabilized the ruthenium surface by depositing a self-assembled monolayer (SAM) of 1-hexadecanethiol on a polycrystalline ruthenium thin film. The growth mechanism, dynamics, and stability of these monolayers were studied. SAMs, deposited under ambient conditions, on piranha-cleaned and piranha + H2SO4 cleaned substrates were compared to monolayers formed on H-radical-cleaned Ru surfaces. We found that alkanethiols on H-radical-cleaned Ru formed densely packed monolayers that remained stable when kept in a nitrogen atmosphere. X-ray photoelectron spectroscopy (XPS) shows a distinct sulfur peak (BE = 162.3 eV), corresponding to metal-sulfur bonding. When exposed to ambient conditions, the SAM decayed over a period of hours. [ABSTRACT FROM AUTHOR]

The icosahedral boride B12P2 has been reported to exhibit "self-healing" properties, after transmission electron microscopy recordings of sample surfaces, which were exposed to highly energetic particle beams, revealed little to no damage. In this work, employing calculations from first-principles within the density functional theory (DFT) framework, the structural characteristics of boron interstitial and vacancy defects in B12P2 are investigated. Using nudged elastic band simulations, the diffusion properties of interstitial and vacancy defects and their combination, in the form of Frenkel defect pairs, are studied. We find that boron icosahedra maintain their structural integrity even when in a degraded state in the presence of a vacancy or interstitial defect and that the diffusion activation energy for the recombination of an interstitial vacany pair can be as low as 3 meV, in line with the previously reported observation of "self-healing". [ABSTRACT FROM AUTHOR]

We investigate a hybrid thin film deposition procedure that significantly enhances reflectivity of La/B based nanoscale multilayer structures to be used as Extreme UV mirrors at 6.7 nm wavelength and beyond. We have analyzed the La-nitridation process in detail, and proposed a growth mechanism and deposition procedure for full, stoichiometric passivation of La, avoiding the formation of optically unfavorable BN formation at the LaN-on-B interface. A partial nitridation was applied and studied as a function of the nitridation delay. [ABSTRACT FROM AUTHOR]

The influence of a plasma density gradient on ions accelerated along the specular (back reflection) direction in the transparent Target Normal Sheath Acceleration regime is investigated. Enhanced acceleration of ions is experimentally observed in this regime using high-intensity and ultra-high contrast laser pulses and extremely thin foils of few nanometer thicknesses. The experimental trend for the maximum proton energy appeared quite different from the already published numerical results in this regime where an infinitely steep plasma gradient was assumed. We showed that for a realistic modelling, a finite density gradient has to be taken into account. By means of particle-incell (PIC) simulations, we studied for the first time the influence of the plasma density scale length on ion acceleration from these nanofoil targets. Through a qualitative agreement between our numerical particle-in-cell simulations and our experiments, the main conclusion with regard to the experimental requirements is that, in the transparent regime evidenced with nanofoils as compared to the opaque regime, the plasma expansion has to be taken into account and both the pulse contrast and the damage threshold of the material are essential parameters. [ABSTRACT FROM AUTHOR]