Andreas Hertwig

New Approach on Quantification of Porosity of Thin Films via Electron-Excited X-ray Spectra.

One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thin templated mesoporous TiO2 films, dip-coated on silicon wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films.

Results of a round-robin experiment in multiple-pulse LIDT measurement with ultrashort pulses

For the development of standard measurement procedures in optics characterization, comparative measurement campaigns (Round-robin experiments) are indispensable. Within the framework of the CHOCLAB project in the mid-90s, several international Round-robins were successfully performed qualifying procedures for e. g. 1 on 1-LIDT, laser-calorimetry and total scattering. During the recent years, the demand for single pulse damage investigations has been overtaken by the more practically relevant S on 1-LIDT. In contrast to the industrial needs, the comparability of the multiple-pulse LIDT has not been proven by Round-robin experiments up to now. As a consequence of the current research activities on the interaction of ultra-short pulses with matter as well as industrial applications, numerous fs-laser systems become available in universities and research institutes. Furthermore, special problems for damage testing may be expected because of the intrinsic effects connected with the interaction of ultrashort pulses with optical materials. Therefore, a Round-robin experiment on S on 1-damage testing utilizing fs-pulses was conducted within the framework of the EUREKA-project CHOCLAB II. For this experiment, seven parties investigated different types of mirrors and windows. Most of the partners were guided by the International Standard ISO 11254-2, but one partner employed his own damage testing technique. In this presentation, the results of this comparative experiment are compiled demonstrating the problems induced by special effects of damage testing in the ultra-short pulse regime.

Ultrafast lattice response of photoexcited thin films studied by X-ray diffraction

Using ultrafast X-ray diffraction, we study the coherent picosecond lattice dynamics of photoexcited thin films in the two limiting cases, where the photoinduced stress profile decays on a length scale larger and smaller than the film thickness. We solve a unifying analytical model of the strain propagation for acoustic impedance-matched opaque films on a semi-infinite transparent substrate, showing that the lattice dynamics essentially depend on two parameters: One for the spatial profile and one for the amplitude of the strain. We illustrate the results by comparison with high-quality ultrafast X-ray diffraction data of SrRuO3 films on SrTiO3 substrates.

Characterization of thin-film thickness

Analysis methods and instrumentation for obtaining optical parameters and thickness profiles of thin-film samples from spectrophotometric and ellipsometric measurements are presented. Measured samples include thermally grown and evaporated SiO2 on a silicon substrate and a polymer photoresist layer on silicon. Experimental results at multiple sample positions give the thickness uniformity and optical constants of thin films. The thickness results obtained with spectrophotometry and ellipsometry agree within 1 nm for the 300 nm thick layer of SiO2 on silicon. For the 1600 nm thick resist sample the agreement of the measurement methods is within 8 nm. For the sample with a nominally 6000 nm thick layer of SiO2 on silicon, there is a deviation of ~100 nm between the spectrophotometry and ellipsometry results. As an application, the optical parameters of a SiO2 layer on an induced junction silicon photodiode are determined by spectrophotometry and are used to confirm earlier values and uncertainties of the SiO2 refractive index and layer thickness non-uniformity.

Ultra-short pulse laser safety - a challenge to materials science

In this paper, safety-related experiments with ultra-short laser pulses (down to 30 fs) on various components (goggles, curtains) for laser protection are presented. The damage and failure behaviour of protective devices has been investigated dependent on practical conditions such as pulse duration, laser fluence, pulse number, and repetition rate. The effects of laser-irradiation on materials can be roughly divided into transient ones like laser-induced transmission (LIT) or short-lived colour centres and permanent damages like the stable colour centres and ablation. The former effects are particularly important for transparent devices like laser goggles. To obtain a complete overview on laser safety issues and the prevention of failure there are two important fields of investigation: 1. the effects of laser radiation on human eyes and skin, and 2. on the possible protection materials. Both fields have been addressed during the recently finished German project SAFEST (safety aspects in femtosecond technology). The amount of safety data available in the ultrashort pulse region has been increased remarkably. This allows for a re-evaluation of known laser protection materials for this region of pulse durations and for the evaluation of new designs that promise high protection levels while being light-weight and convenient to use.

Thin SnOx films for surface plasmon resonance enhanced ellipsometric gas sensing (SPREE)

Background: Gas sensors are very important in several fields like gas monitoring, safety and environmental applications. In this approach, a new gas sensing concept is investigated which combines the powerful adsorption probability of metal oxide conductive sensors (MOS) with an optical ellipsometric readout. This concept shows promising results to solve the problems of cross sensitivity of the MOS concept. Results: Undoped tin oxide (SnOx) and iron doped tin oxide (Fe:SnOx) thin add-on films were prepared by magnetron sputtering on the top of the actual surface plasmon resonance (SPR) sensing gold layer. The films were tested for their sensitivity to several gas species in the surface plasmon resonance enhanced (SPREE) gas measurement. It was found that the undoped tin oxide (SnOx) shows higher sensitivities to propane (C3H8) then to carbon monoxide (CO). By using Fe:SnOx, this relation is inverted. This behavior was explained by a change of the amount of binding sites for CO in the layer due to this iron doping. For hydrogen (H2) no such relation was found but the sensing ability was identical for both layer materials. This observation was related to a different sensing mechanism for H2 which is driven by the diffusion into the layer instead of adsorption on the surface. Conclusion: The gas sensing selectivity can be enhanced by tuning the properties of the thin film overcoating. A relation of the binding sites in the doped and undoped SnOx films and the gas sensing abilities for CO and C3H8 was found. This could open the path for optimized gas sensing devices with different coated SPREE sensors.

Spot size dependence of femtosecond laser ablation of dielectrics

In this paper, dependence of femtosecond laser ablation threshold on the beam radius for barium borosilicate glass (Corning 7059) at a repetition rate of 1 kHz (1000 pulses per spot, 800 nm wavelength) is observed.