Laser-induced breakdown spectroscopy (LIBS) is a rapidly developing technique for chemical materials analysis. LIBS is applied for fundamental investigations, e.g., the laser plasma matter interaction, for element, molecule, and isotope analysis, and for various technical applications, e.g., minimal destructive materials inspection, the monitoring of production processes, and remote analysis of materials in hostile environment. In this review, we focus on the element analysis of industrial materials and the in-line chemical sensing in industrial production. After a brief introduction we discuss the optical emission of chemical elements in laser-induced plasma and the capability of LIBS for multi-element detection. An overview of the various classes of industrial materials analyzed by LIBS is given. This includes so-called Technology materials that are essential for the functionality of modern high-tech devices (smartphones, computers, cars, etc.). The LIBS technique enables unique applications for rapid element analysis under harsh conditions where other techniques are not available. We present several examples of LIBS-based sensors that are applied in-line and at-line of industrial production processes.
Femtosecond laser-induced breakdown spectroscopy (fs-LIBS) is employed to detect tiny amounts of mass ablated from macroscopic specimens and to measure chemical images of microstructured samples with high spatial resolution. Frequency-doubled fs-pulses (length 400 fs, wavelength 520 nm) are tightly focused with a Schwarzschild microscope objective to ablate the sample surface. The optical emission of laser-induced plasma (LIP) is collected by the objective and measured with an echelle spectrometer equipped with an intensified charge-coupled device camera. A second fs-laser pulse (1040 nm) in orthogonal beam arrangement is reheating the LIP. The optimization of the experimental setup and measurement parameters enables us to record single-pulse fs-LIBS spectra of 5 nm thin metal layers with an ablated mass per pulse of 100 femtogram (fg) for Cu and 370 fg for Ag films. The orthogonal double-pulse fs-LIBS enhances the recorded emission line intensities (two to three times) and improves the contrast of chemical images in comparison to single-pulse measurements. The size of ablation craters (diameters as small as 1.5 µm) is not increased by the second laser pulse. The combination of minimally invasive sampling by a tightly focused low-energy fs-pulse and of strong enhancement of plasma emission by an orthogonal high-energy fs-pulse appears promising for future LIBS chemical imaging with high spatial resolution and with high spectrochemical sensitivity.
The properties of natural and synthetic rubber critically depend on the concentration of the vulcanizing system, among others. Sulfur and zinc oxide are typically used as cross-linking and activating agents for the vulcanization reaction (0−3 wt %). We present an advanced spectroscopic method to chemically analyze the vulcanizing system in rubber under ambient conditions, and we demonstrate a novel application to measure the elements in-line of industrial rubber production. The laser-induced breakdown spectroscopy (LIBS) technique is optimized to ablate material from the surface of produced rubber sheets and to measure the optical emission of S and Zn from the rubber plasma in air. The sulfur lines in the near-infrared range are masked by molecular emission bands of the C−N radical and spectrally interfered by atomic lines of O. Plasma excitation in collinear doublepulse geometry and detection of plasma emission with time-gated detectors suppresses the spectroscopic overlays and enables to resolve the sulfur lines. For the determination of ZnO the weak Zn lines in the ultraviolet range are measured due to their superior intensity stability compared to the much stronger lines in the deeper UV. S and ZnO are quantified in three different rubber materials prepared from the most important polymers used in rubber production. The mean error of prediction of concentrations RMSEP is ≤0.07 wt % for S and ≤0.33 wt % for ZnO for all polymer types. Our results demonstrate that the vulcanizing system of rubber can be quantified under ambient conditions with LIBS. Other chemical elements could be analyzed also and the rubber production could be controlled employing this multielement detection technique as process analytical sensor.
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