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Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS are classified, relevant control parameters are identified, and their material-specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS are classified, relevant control parameters are identified, and their material-specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
Single Femtosecond Laser-Pulse-Induced Superficial Amorphization and Re-Crystallization of Silicon
(2021)
Superficial amorphization and re-crystallization of silicon in <111> and <100> orientation after irradiation by femtosecond laser pulses (790 nm, 30 fs) are studied using optical imaging and transmission electron microscopy. Spectroscopic imaging ellipsometry (SIE) allows fast data acquisition at multiple wavelengths and provides experimental data for calculating nanometric amorphous layer thickness profiles with micrometric lateral resolution based on a thin-film layer model. For a radially Gaussian laser beam and at moderate peak fluences above the melting and below the ablation thresholds, laterally parabolic amorphous layer profiles with maximum thicknesses of several tens of nanometers were quantitatively attained. The accuracy of the calculations is verified experimentally by high-resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray spectroscopy (STEM-EDX). Along with topographic information obtained by atomic force microscopy (AFM), a comprehensive picture of the superficial re-solidification of silicon after local melting by femtosecond laser pulses is drawn.
Laser-induced periodic surface structures (LIPSS) are a universal phenomenon and can be generated on almost any material by irradiation with linearly polarized radiation. This chapter reviews the current state in the field of LIPSS, which are formed in a “self-ordered” way and are often accompanying materials processing applications. LIPSS can be produced in a single-stage process and enable surface nanostructuring and, in turn, adaption of optical, mechanical, and chemical surface properties. Typically, they feature a structural size ranging from several micrometers down to less than 100 nm and show a clear correlation with the polarization direction of the light used for their generation. Various types of LIPSS are classified, relevant control parameters are identified, and their material-specific formation mechanisms are analyzed for different types of inorganic solids, i.e., metals, semiconductors, and dielectrics. Finally, technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed.
The influence of processing parameters on X‑ray emission during ultra‑short pulse laser machining
(2019)
During ultra-short laser material processing at high laser pulse repetition rates unwanted X-ray radiation can be generated in a quantity that may constitute a potential risk for health. An adequate X-ray radiation protection requires a thoroughly understanding of the influence of the laser processing parameters on the generation of X-ray radiation. In the present work, the generated X-ray dose during laser machining was investigated in air for varying beam scanning conditions at a pulse duration of 925 fs, a center wavelength of 1030 nm and a laser peak intensity of 2.6 × 10^14 W/cm^2. The X-ray radiation dose and the corresponding spectral X-ray emission were investigated in dependence on the laser’s pulse repetition rate and on the beam scanning speed. The results show a strong dependence of the X-ray emission on these laser processing parameters.
A laser-based bottom-up technique for the fabrication of Cu(In,Ga)Se2 (CIGSe) micro solar cells is presented.
We use femtosecond laser-induced forward transfer (LIFT) to transport a metallic precursor composed of copper, indium, and gallium onto a molybdenum back contact layer on a glass substrate. A CIGSe absorber forms by subsequent selenization. An array of micro absorbers with defined spacing is fabricated to solar cells and characterized under concentrated light illumination. The solar cell array exhibited a conversion efficiency of 1.4‰ at 1 sun as well as a significant efficiency enhancement of 68% rel. under 20-fold concentration. This work demonstrates the possibility of directly grown micrometer-sized solar cells based on chalcogenide absorber layers, enabling effective material usage.
In laser machining with ultrashort laser pulses unwanted X-ray radiation in the keV range can be generated when a critical laser intensity is exceeded. Even if the emitted X-ray dose per pulse is low, high laser repetition rates can lead to an accumulation of X-ray doses beyond exposure safety limits. For 925 fs pulse duration at a center wavelength of 1030 nm, the X-ray emission was investigated up to an intensity of 2.6 × 10^14 W/cm2. The experiments were performed in air with a thin disk laser at a repetition rate of 400 kHz. X-ray spectra and doses were measured for various planar target materials covering a wide range of the periodic table from aluminum to tungsten. Without radiation shielding, the measured radiation doses at this high repetition rate clearly exceed the regulatory limits. Estimations for an adequate radiation shielding are provided.
Commercial grade-1 titanium samples (Ti, 99.6%) were treated using three alternative methods, (i) femtosecond laser processing, (ii) thermal heat treatment, and (iii) electrochemical anodization, respectively, resulting in the formation of differently conditioned superficial titanium oxide layers. The laser processing (i) was carried out by a Ti:sapphire laser (pulse duration 30 fs, central wavelength 790 nm, pulse repetition rate 1 kHz) in a regime of generating laser-induced periodic surface structures (LIPSS). The experimental conditions (laser fluence, spatial spot overlap) were optimized in a sample-scanning setup for the processing of several square-millimeters large surface areas covered homogeneously by these nanostructures. The differently oxidized titanium surfaces were characterized by optical microscopy, micro Raman spectroscopy, variable angle spectroscopic ellipsometry, and instrumented indentation testing. The tribological performance was characterized in the regime of mixed friction by reciprocating sliding tests against a sphere of hardened steel in fully formulated engine oil as lubricant. The specific tribological performance of the differently treated surfaces is discussed with respect to possible physical and chemical mechanisms.
Many wooden artworks are contaminated by DDT (dichlorodiphenyltrichloroethane) as a result of a surface treatment by means of the liquid preservative Hylotox-59©. It was used until the end of the 1980s. DDT crystal structures are formed on the wood surfaces by the "blooming" of chlorine compounds. In addition to an aesthetic disturbance, it is assumed that DDT represents a health risk. Even decades after applying, the toxins in the wood preservatives are still detectable because they are of low volatility in many wood samples. Contaminated waste wood with natural biocide ageing, gilded and wood carved elements of an old picture frame and wooden samples with paint layers were provided by the Schlossmuseum Sondershausen. Non-contact procedures using laser and plasma appear reasonable to remove the DDT crystals. During the experiments, health and safety issues for the operator have to be taken into account.
The removal of DDT was evaluated employing femtosecond and nanosecond laser radiation and cold atmospheric plasma techniques with different working gases (air, nitrogen, and argon). Before laser application, a chlorine measurement representing the DDT density on the wooden surface is done by X-ray fluorescence (XRF) analysis as reference. After laser processing, the XRF analysis is used again at the same surface position to determine the depletion rate. Additionally, a documentation and characterization of the sample surface is performed before and after laser and plasma treatment using optical microscopy (OM). For plasma processing with various systems a chlorine measurement is done by gas chromatographic-mass spectrometry (GCMS) analysis.
A bottom-up approach to produce arrays of indium islands on a molybdenum layer on glass using 30-fs laser pulses at 790 nm wavelength is presented. These islands can serve as micro-sized precursors for indium compounds such as copper-indium-gallium-diselenide (CIGSe) used in photovoltaics. Molybdenum is the standard back contact material of CIGSe solar cells. Femtosecond laser ablation of glass and a subsequent deposition of a molybdenum film or direct laser processing of the molybdenum film both allow the preferential nucleation and growth of indium islands at the predefined locations in a following indium-based physical vapor deposition (PVD) process. A proper choice of laser and deposition parameters ensures the controlled growth of indium islands exclusively at the laser ablated spots. Based on a statistical analysis, these results are compared to the non-structured molybdenum surface, leading to randomly grown indium islands after PVD.
A promising technology in photovoltaics is based on micro-concentrator solar cells, where the photovoltaic active area is realized as an array of sub-millimeter sized cells onto which the incident light is focused via microlenses. This approach allows to increase the cell efficiency and to realize much more compact modules compared to macroscopic concentrator devices. At the same time, expensive raw materials can be saved, which is of interest, for example, with respect to indium in the case of copper-indium-gallium-diselenide (CIGSe) thin film solar cells. Two methods to produce micro-sized precursors of CIGSe absorbers on molybdenum are presented using 30-fs laser pulses at 790 nm wavelength. On the one hand, a multi pulse surface structuring of the molybdenum film or the underlying glass substrate and a subsequent physical vapor deposition were used for a site-selective aggregation of indium droplets. On the other hand, a single pulse laser-induced forward transfer was utilized to selectively deposit combined copper-indium precursor pixels on the molybdenum back contact of the solar cell. Post-processing (selenization, isolation, contacting) of the laser-generated micro-sized precursors results in functional CIGSe solar cells.
A promising technology in photovoltaics is based on micro-concentrator solar cells, where the photovoltaic active area is realized as an array of sub-millimeter sized thin-film solar cells. For copper-indium-gallium-diselenide (CIGSe), the solar cells can be arranged in the foci of a regular arrangement of micro-lenses to enhance their efficiency by light concentration, to allow a better heat dissipation and to save expensive raw material (indium). Different approaches to produce micro-sized precursors of CIGSe absorbers on molybdenum are presented using 30-fs laser pulses at 790 nm wavelength. On the one hand, a multi pulse surface structuring of the molybdenum or the underlying glass substrate and a subsequent physical vapor deposition (PVD) process were used for a site-selective aggregation of indium droplets. On the other hand, a single pulse laser-induced forward transfer (LIFT) was utilized to selectively deposit combined copper/indium/gallium precursor pixels on the molybdenum back contact of the solar cell. It was demonstrated that a postprocessing (selenization, isolation, contacting) of the laser-generated micro-sized precursors results in an array of working CIGSe solar cells with an efficiency of 2.8% for 1 sun illumination.
Decontamination of biocidal loaded wooden artworks
using femtosecond and nanosecond laser processing
(2017)
Until the end of the 1980s many wooden artworks underwent surface treatment by liquid preservatives, e.g. Hylotox-59. As a result, DDT (dichlorodiphenyltrichloroethane) crystal structures are formed on the wood surfaces by the "blooming" of chlorine compounds. In addition to an aesthetic disturbance, it is assumed that DDT represents a health risk. Even decades after applying, the toxins in the wood preservatives are still detectable. Contaminated waste wood with natural biocide ageing, gilded and wood carved elements of an old picture frame and wooden samples with paint layers were provided by the Schlossmuseum Sondershausen, Germany.
Laser cleaning of areas of some square millimeters on the surfaces of the objects was done by means of femtosecond and nanosecond laser pulses. For 30-fs laser pulses at 800 nm wavelength a line-wise meandering movement of the object under the focused beam was performed. 10-ns laser pulses at 1064 nm and 7-ns laser pulses at 532 nm wavelength were applied to the sample surface using a scanner. Before laser application, a chlorine measurement was done by X-ray fluorescence analysis (XRF) as reference. After laser processing, the XRF analysis was used again at the same surface position to determine chlorine depletion rates of up to 75% (30 fs, 800 nm), 70% (10 ns, 1064 nm), and 22% (7 ns, 532 nm). For the application of 30-fs laser pulses on waste wood, no crystalline DDT residues remain on the sample surface observed utilizing optical microscopy.
Biofilm formation poses high risks in multiple industrial and medical settings. However, the robust nature of biofilms makes them also attractive for industrial applications where cell biocatalysts are increasingly in use. Since tailoring material properties that affect bacterial growth or its inhibition is gaining attention, here we focus on the effects of femtosecond laser produced nanostructures on bacterial adhesion. Large area periodic surface structures were generated on steel surfaces using 30-fs laser pulses at 790 nm wavelength. Two types of steel exhibiting a different corrosion resistance were used, i.e., a plain structural steel (corrodible) and a stainless steel (resistant to corrosion). Homogeneous fields of laser-induced periodic surface structures (LIPSS) were realized utilizing laser fluences close to the ablation threshold while scanning the sample under the focused laser beam in a multi-pulse regime. The nanostructures were characterized with optical and scanning electron microscopy. For each type of steel, more than ten identical samples were laser-processed. Subsequently, the samples were subjected to microbial adhesion tests. Bacteria of different shape and adhesion behavior (Escherichia coli and Staphylococcus aureus) were exposed to laser structures and to polished reference surfaces. Our results indicate that E. coli preferentially avoids adhesion to the LIPSS-covered areas, whereas S. aureus favors these areas for colonization.
A bottom-up approach is presented for the production of arrays of indium islands on a molybdenum layer on glass using 30-fs laser pulses at 790 nm wavelength. The indium islands can serve as micro-sized precursors for indium compounds such as copper-indium-gallium-diselenide (CIGSe) used in photovoltaics. Molybdenum is the standard back contact material of CIGSe solar cells. Femtosecond laser ablation of glass and a subsequent deposition of a molybdenum film or direct laser processing of the molybdenum film both allow the preferential nucleation and growth of indium islands at the predefined locations in a following indium-based physical vapor deposition (PVD) process. A proper choice of laser and deposition parameters ensures the controlled growth of indium islands exclusively at the laser ablated spots. Based on a statistical analysis, these results are compared to the non-structured molybdenum surface, leading to randomly grown indium islands after PVD.
Until the end of the 1980s many wooden artworks underwent surface treatment by liquid preservatives, e.g. Hylotox-59. DDT (dichlorodiphenyltrichloroethane) crystal structures are formed on the wooden surfaces by the "blooming" of chlorine compounds by time. In addition to an aesthetic disturbance, it is assumed that DDT represents a health risk. Therefore, the removal of DDT crystals from the surfaces is requested. Contaminated wood with natural biocide ageing, gilded and wood carved elements and wooden samples with paint layers were provided by the Schlossmuseum Sondershausen, Germany. Laser cleaning on selected surface areas on the objects was done by means of femtosecond and nanosecond laser pulses. For the same object, cleaning results using 30-fs laser pulses at 800 nm wavelength are compared to findings utilizing 10-ns laser pulses at 1064 nm wavelength. Before and after laser treatment, chlorine measurements at the same surface position were done by X-ray fluorescence analysis (XRF) as an indicator for the presence of DDT. In this way, pointwise chlorine depletion rates can be obtained for the different pulse duration regimes and wavelengths. Additionally, the object surfaces were examined using optical microscopy and multi spectral imaging analysis.
Miniaturized pacemakers with a surface consisting of a Ti alloy may have to be removed after several years from their implantation site in the heart and shall, therefore, not be completely overgrown by cells or tissue. A method to avoid this may be to create at the surface by laser-ablation self-organized sharp conical spikes, which provide too little surface for cells (i.e., fibroblasts) to grow on. For this purpose, Ti-alloy substrates were irradiated in the air by 790 nm Ti:sapphire femtosecond laser pulses at fluences above the ablation threshold. The laser irradiation resulted in pronounced microstructure formation with hierarchical surface morphologies. Murine fibroblasts were seeded onto the laser-patterned surface and the coverage by cells was evaluated after 3–21 days of cultivation by means of scanning electron microscopy. Compared to flat surfaces, the cell density on the microstructures was significantly lower, the coverage was incomplete, and the cells had a clearly different morphology. The best results regarding suppression of cell growth were obtained on spike structures which were additionally electrochemically oxidized under acidic conditions. Cell cultivation with additional shear stress could reduce further the number of adherent cells.
Single-pulse femtosecond laser-induced forward transfer (LIFT, 30 fs, 790 nm) is used to deposit micron-sized dots of copper and/or indium onto a molybdenum layer on glass. Such systems can serve as precursors for the bottom-up manufacturing of micro-concentrator solar cells based on copper-indium-gallium-diselenide. The influence of the thickness of the copper, indium and combined copper-indium donor layers on the quality of the transferred dots was qualified by scanning electron microscopy, energy-dispersive X-ray analysis, and optical microscopy. The potential for manufacturing of a spatial arrangement adapted to the geometry of micro-lens arrays needed for micro-concentrator solar cells is demonstrated.
The chemical characteristics of two different types of laser-induced periodic surface structures (LIPSS), so-called high and low spatial frequency LIPSS (HSFL and LSFL), formed upon irradiation of titanium surfaces by multiple femtosecond laser pulses in air (30 fs, 790 nm, 1 kHz), are analyzed by various optical and electron beam based surface analytical techniques, including micro-Raman spectroscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, and Auger electron spectroscopy. The latter method was employed in a high-resolution mode being capable of spatially resolving even the smallest HSFL structures featuring spatial periods below 100 nm. In combination with an ion sputtering technique, depths-resolved chemical information of superficial oxidation processes was obtained, revealing characteristic differences between the two different types of LIPSS. Our results indicate that a few tens of nanometer shallow HSFL are formed on top of a ∼150 nm thick graded superficial oxide layer without sharp interfaces, consisting of amorphous TiO2 and partially crystallized Ti2O3. The larger LSFL structures with periods close to the irradiation wavelength originate from the laser-interaction with metallic titanium. They are covered by a ∼200 nm thick amorphous oxide layer, which consists mainly of TiO2 (at the surface) and other titanium oxide species of lower oxidation states underneath.