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An ambient pressure cell is described for conducting synchrotron-based x-ray photoelectron spectroscopy (XPS) measurements during atomic layer deposition (ALD) processes. The instrument is capable of true in situ and operando experiments in which it is possible to directly obtain elemental and chemical information from the sample surface using XPS as the deposition process is ongoing. The setup is based on the ambient pressure XPS technique, in which sample environments with high pressure (several mbar) can be created without compromising the ultrahigh vacuum requirements needed for the operation of the spectrometer and the synchrotron beamline. The setup is intended for chemical characterization of the surface intermediates during the initial stages of the deposition processes. The SPECIES beamline and the ALD cell provide a unique experimental platform for obtaining new information on the surface chemistry during ALD half-cycles at high temporal resolution. Such information is valuable for understanding the ALD reaction mechanisms and crucial in further developing and improving ALD processes. We demonstrate the capabilities of the setup by studying the deposition of TiO2 on a SiO2 surface by using titanium(IV) tetraisopropoxide and water as precursors. Multiple core levels and the valence band of the substrate surface were followed during the film deposition using ambient pressure XPS.
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An amendment to this paper has been published and can be accessed via a link at the top of the paper.
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In this study, slot waveguide ring resonators patterned on a silicon-on-insulator (SOI) wafer and coated with an atomic layer deposited nanolaminate consisting of alternating layers of tantalum pentoxide and polyimide were fabricated and characterized. To the best of our knowledge, this is the first demonstration of atomic layer deposition (ALD) of organic materials in waveguiding applications. In our nanolaminate ring resonators, the optical power is not only confined in the narrow central air slot but also in several parallel sub-10 nm wide vertical polyimide slots. This indicates that the mode profiles in the silicon slot waveguide can be accurately tuned by the ALD method. Our results show that ALD of organic and inorganic materials can be combined with conventional silicon waveguide fabrication techniques to create slot waveguide ring resonators with varying mode profiles. This can potentially open new possibilities for various photonic applications, such as optical sensing and all-optical signal processing.
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X-ray Free Electron Lasers (FELs) can produce extremely intense and very short pulses, down to below 10 femtoseconds (fs). Among the key applications are ultrafast time-resolved studies of dynamics of matter by observing responses to fast excitation pulses in a pump-probe manner. Detectors with sufficient time resolution for observing these processes are not available. Therefore, such experiments typically measure a sample's full dynamics by repeating multiple pump-probe cycles at different delay times. This conventional method assumes that the sample returns to an identical or very similar state after each cycle. Here we describe a novel approach that can provide a time trace of responses following a single excitation pulse, jitter-free, with fs timing precision. We demonstrate, in an X-ray diffraction experiment, how it can be applied to the investigation of ultrafast irreversible processes.
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A growing number of X-ray sources based on the free-electron laser (XFEL) principle are presently under construction or have recently started operation. The intense, ultrashort pulses of these sources will enable new insights in many different fields of science. A key problem is to provide x-ray optical elements capable of collecting the largest possible fraction of the radiation and to focus into the smallest possible focus. As a key step towards this goal, we demonstrate here the first nanofocusing of hard XFEL pulses. We developed diamond based Fresnel zone plates capable of withstanding the full beam of the world's most powerful x-ray laser. Using an imprint technique, we measured the focal spot size, which was limited to 320 nm FWHM by the spectral band width of the source. A peak power density in the focal spot of 4×10(17)W/cm(2) was obtained at 70 fs pulse length.
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The issue of beam-induced damage on diffractive hard X-ray optics is addressed. For this purpose a systematic study on the radiation damage induced by a high-power X-ray beam is carried out in both ambient and inert atmospheres. Diffraction gratings fabricated by three different techniques are considered: electroplated Au gratings both with and without the polymer mold, and Ir-coated Si gratings. The beam-induced damage is monitored by X-ray diffraction and evaluated using scanning electron microscopy.
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A method for the fabrication of ultrahigh-resolution Fresnel zone plate lenses for x-ray microscopy is demonstrated. It is based on the deposition of a zone plate material (Ir) onto the sidewalls of a prepatterned template structure (Si) using an atomic layer deposition technique. This results in a doubling of the effective zone density, thus improving the achievable resolution of x-ray microscopes. Test structures with lines and spaces down to 15 nm were resolved in a scanning transmission x-ray microscope at 1 keV photon energy.
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A chemical approach to atomic layer deposition (ALD) of oxide thin films is reported here. Instead of using water or other compounds for an oxygen source, oxygen is obtained from a metal alkoxide, which serves as both an oxygen and a metal source when it reacts with another metal compound such as a metal chloride or a metal alkyl. These reactions generally enable deposition of oxides of many metals. With this approach, an alumina film has been deposited on silicon without creating an interfacial silicon oxide layer that otherwise forms easily. This finding adds to the other benefits of the ALD method, especially the atomic-level thickness control and excellent uniformity, and takes a major step toward the scientifically challenging and technologically important task of replacing silica as the gate dielectric in the future generations of metal oxide semiconductor field effect transistors.
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Different sol-gel-derived titania and titania-silica films were prepared and their properties related to in vitro bioactivity. The films were prepared by depositing the sols on the substrate surface using a dip-coating method. The sols were monitored carefully as a function of time, using rheological techniques and dynamic light scattering. The topography of the films was characterized using atomic force microscopy, and thicknesses and refractive indexes of the films were evaluated by fitting transmittance spectra measured in a wave length region of 370-1100 nm with a spectrophotometer. The in vitro bioactivity tests were performed in simulated body fluid. Surface topography was found to be of great importance with respect to the bioactivity of the studied films.
