Jacobus Marinus Sturm

Imaging of oxide charges and contact potential difference fluctuations in atomic layer deposited Al2O3 on Si

Ultrathin 2.5 nm high-k aluminum oxide (Al2O3) films on p-type silicon (001) deposited by atomic layer deposition (ALD) were investigated with noncontact atomic force microscopy (NC-AFM) in ultrahigh vacuum, using a conductive tip. Constant force gradient images revealed the presence of oxide charges and experimental observations at different tip-sample potentials were compared with calculations of the electric force gradient based on a spherical tip model. This model could be substantially improved by the incorporation of the image of the tip in the semiconductor substrate. Based on the signals of different oxide charges observed, a homogenous depth distribution of those charges was derived. Application of a potential difference between sample and tip was found to result in a net electric force depending on the contact potential difference (CPD) and effective tip-sample capacitance, which depends on the depletion or accumulation layer that is induced by the bias voltage. CPD images could be constructed from height-voltage spectra with active feedback. Apart from oxide charges large-scale (150-300 nm lateral size) and small-scale (50-100 nm) CPD fluctuations were observed, the latter showing a high degree of correlation with topography features. This correlation might be a result from the surface-inhibited growth mode of the investigated layers.

Emissivity of freestanding membranes with thin metal coatings

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 Lorentzoscillators.

Highly efficient blazed grating with multilayer coating for tender X-ray energies

For photon energies of 1 - 5 keV, blazed gratings with multilayer coating are ideally suited for the suppression of stray and higher orders light in grating monochromators. We developed and characterized a blazed 2000 lines/mm grating coated with a 20 period Cr/C- multilayer. The multilayer d-spacing of 7.3 nm has been adapted to the line distance of 500 nm and the blaze angle of 0.84° in order to provide highest efficiency in the photon energy range between 1.5 keV and 3 keV. Efficiency of the multilayer grating as well as the reflectance of a witness multilayer which were coated simultaneously have been measured. An efficiency of 35% was measured at 2 keV while a maximum efficiency of 55% was achieved at 4 keV. In addition, a strong suppression of higher orders was observed which makes blazed multilayer gratings a favorable dispersing element also for the low X-ray energy range.

Adsorption and Dissociation of CO2 on Ru (0001)

The adsorption and dissociation of carbon dioxide on a Ru(0001) single crystal surface was investigated by reflection–absorption infrared spectroscopy (RAIRS) and temperature-programmed desorption (TPD) spectroscopy for CO2 adsorbed at 85 K. RAIRS spectroscopy shows that the adsorption of CO2 on a Ru(0001) single crystal is partially dissociative, resulting in CO2 and CO. The CO vibrational mode was also observed to split into two distinct modes, indicating two general populations of CO present at the surface. Furthermore, a time-dependent blue-shift is observed, which is characteristic of increasing CO surface coverage. TPD showed that coverages of up to 0.3 ML were obtained, and no evidence for chemisorption of oxygen on ruthenium was found.

Electronegativity-dependent tin etching from thin films

The influence of a thin film substrate material on the etching of a thin layer of deposited tin (Sn) by hydrogen radicals was studied. The amount of remaining Sn was quantified for materials that cover a range of electronegativities. We show that, for metals, etching depends on the relative electronegativity of the surface material and Sn. Tin is chemically etched from surfaces with an electronegativity smaller than Sn, while incomplete Sn etching is observed for materials with an electronegativity larger than Sn. Furthermore, the amount of remaining Sn increases as the electronegativity of the surface material increases. We speculate, that, due to Fermi level differences in the material’s electronic structure, the energy of the two conduction bands shift such that the availability of electrons for binding with hydrogen is significantly reduced.

Structure of high-reflectance La/B-based multilayer mirrors with partial La nitridation

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.

Mechanism of single-shot damage of Ru thin films irradiated by femtosecond extreme UV free-electron laser

Ruthenium is a perspective material to be used for XUV mirrors at free-electron laser facilities. Yet, it is still poorly studied in the context of ultrafast laser-matter interaction. In this work, we present single-shot damage studies of thin Ru films irradiated by femtosecond XUV free-electron laser pulses at FLASH. Ex-situ analysis of the damaged spots, performed by different types of microscopy, shows that the weakest detected damage is surface roughening. For higher fluences we observe ablation of Ru. Combined simulations using Monte-Carlo code XCASCADE(3D) and the two-temperature model reveal that the damage mechanism is photomechanical spallation, similar to the case of irradiating the target with optical lasers. The analogy with the optical damage studies enables us to explain the observed damage morphologies.

Nanoscale topography-capacitance correlation in high-K films : Interface heterogeneity related electrical properties

Kelvin probe force microscopy in ultrahigh vacuum was used to study inhomogeneities of the contact potential difference (CPD) and differential capacitance of thin atomic layer deposited Al2O3 films. CPD fluctuations correlate equally strongly with the surface topography for deposition on hydrogen-terminated Si and thermal SiO2. The correlation of the differential capacitance with the topography clearly distinguishes films based on the starting surface. The lateral electrical homogeneity of these thin oxides depends crucially on their initial nucleation.

Intermixing and thermal oxidation of ZrO2 thin films grown on a-Si, SiN, and SiO2 by metallic and oxidic mode magnetron sputtering

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.

Tin etching from metallic and oxidized scandium thin films

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.