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In construction and demolition waste (CDW) recycling, the preference to date has been to apply simple but proven techniques to sort and process large quantities of construction rubble in a short time. This contrasts with the increasingly complex composite materials and structures in the mineral building materials industry. An automated, sensor-based sorting of these building materials could complement or replace the practice of manual sorting to improve processing speed, recycling rates, sorting quality, and prevailing health conditions for the executing staff.
A joint project of partners from industry and research institutions approaches this task by investigating and testing the combination of laser-induced breakdown spectroscopy (LIBS) with near-infrared (NIR) spectroscopy and visual imaging. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of CDW, and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.)
We present current advances and results about the methodological development combining LIBS with NIR spectroscopy and visual imaging. Here, applying data fusion proves itself beneficial to improve recognition rates. In the future, a laboratory prototype will serve as a fully automated measurement setup to allow real-time classification of CDW on a conveyor belt.
Various industrial applications require the joining of DSS components. Tungsten Inert Gas (TIG) welding is particularly well-suited for this purpose due to the ability to achieve highly reproducible automated welds. However, during solidification of the weld pool, critical phase ratios of ferrite (α) and austenite (γ) may occur, leading to solidification cracking, increased corrosion susceptibility, lower ductility and critical strength values. Hence, in order to achieve the desired material characteristics, it is crucial to accurately predict the α/γ phase ratio within the weld. Conventionally, the WRC-1992 diagram is employed for this purpose. In our study, we used Laser-Induced Breakdown Spectroscopy (LIBS) to track alterations in the chemical composition of the weld metal on the surface throughout the welding process. One significant benefit of this method is its capability to provide precise and real-time measurements of chemical compositions during welding, both temporally and spatially. In previous investigations, we could develop routines to quantify the measurement of chemical compositions within the weld metal and the Heat-Affected Zone (HAZ). The conducted research focuses on examining the alterations in chemical concentrations of specific alloying elements, namely Cu and Mn as γ-forming elements, and Nb and Cr as α-forming elements, during welding. These changes are measured in real-time using Laser-Induced Breakdown Spectroscopy (LIBS). To achieve this, both the ferrite number, determined through magnetic-inductive techniques, and the weld microstructure are analyzed. Through image-analytical methods, a correlation is established between the microstructure and the LIBS data obtained.
LIBS ConSort: Development of a sensor-based sorting method for constuction and demolition waste
(2023)
Closed material cycles and unmixed material fractions are required to achieve high recovery and recycling rates in the building industry. In construction and demolition waste (CDW) recycling, the preference to date has been to apply simple but proven techniques to process large quantities of construction rubble in a short time. This is in contrast to the increasingly complex composite materials and structures in the mineral building materials industry. Manual sorting involves many risks and dangers for the executing staff and is merely based on obvious, visually detectable differences for separation. An automated, sensor-based sorting of these building materials could complement or replace this practice to improve processing speed, recycling rates, sorting quality, and prevailing health conditions. A joint project of partners from industry and research institutions approaches this task by investigating and testing the combination of laser-induced breakdown spectroscopy (LIBS) with near-infrared (NIR) spectroscopy and visual imaging. Joint processing of information (data fusion) is expected to significantly improve the sorting quality of various materials like concrete, main masonry building materials, organic components, etc., and may enable the detection and separation of impurities such as SO3-cotaining building materials (gypsum, aerated concrete, etc.) Focusing on Berlin as an example, the entire value chain will be analyzed to minimize economic / technological barriers and obstacles at the cluster level and to sustainably increase recovery and recycling rates. We present current advances and results about the test stand development combining LIBS with NIR spectroscopy and visual imaging. In the future, this laboratory prototype will serve as a fully automated measurement setup to allow real-time classification of CDW on a conveyor belt.
The high corrosion resistance and good mechanical properties of duplex stainless steel (DSS) are due to its special chemical composition, which is a balanced phase ratio of ferrite (α) and austenite (γ). Many industrial applications require the integration of DSS components. For this, tungsten inert gas welding (TIG) is an excellent choice, as it allows an automated operation with high reproducibility. However, when the weld pool solidifies, critical ratios of α- and γ- phases can occur, which leads to solidification cracking, increased susceptibility to corrosion, and a decrease in ductility and critical strength. Previous studies have shown that these defects can be caused by the accumulation of manganese and chromium in the heat affected zone (HAZ), and this accumulation can be detected using LIBS.
Unlike conventional LIBS analyses, which requires reference samples to generate a calibration curve, calibration-free LIBS (CF-LIBS) can determine the chemical composition solely from the emission spectrum of the plasma. Numerous publications show that CF-LIBS is a fast and efficient analytical method for quantitative analysis of metal samples.
We present the results of in situ CF-LIBS analysis during TIG DSS welding. Using a new approach, it is possible to quantitatively determine the chemical composition of the weld metal directly in the welding process. The results of the CF-LIBS analysis are compared with the results of the calibration-based PLS analysis and reasonable agreement is found. Thus, the CF-LIBS method offers the significant advantage of quickly measuring in situ the concentrations of the main alloying elements that prevent the formation of welding defects, without the tedious calibration procedure.
The Boltzmann plot method is widely used to determine the temperature of laser induced plasma. It involves the use of individual lines that are not easy to find in complex spectra and/or in the spectral range available. If the number of such lines is not enough to build a reliable Boltzmann plot, overlapping lines are often used, which are separated by software. However, line separation is a rather imprecise procedure, which, in addition, requires significant computational costs. This study proposes an extension of the Boltzmann plot method that allows a specific group of unresolved lines to be included in a Boltzmann plot without the need to separate them. This group of lines are multiplets, lines of the same element with similar upper and lower transition states. The multiplet lines along with the individual lines are included in the algorithm, which also includes a correction for self-absorption and is used to determine the plasma temperature. The algorithm is tested on synthetic spectra which are consistent with the model of a homogeneous isothermal plasma in local thermodynamic equilibrium and is shown to be superior to the standard Boltzmann plot method both in more accurate determination of the plasma temperature and in a significant reduction in the computational time. The advantages and disadvantages of the method are discussed in the context of its applications in laser induced breakdown spectroscopy.
Measurement of hydrogen concentration in steel using Laser-induced Breakdown spectroscopy (LIBS)
(2023)
Currently, the ISO 3690 standard requires a thermal activation of the diffusible hydrogen in weld metal for the subsequent ex situ concentration measurement by TDS. Laser-induced breakdown spectroscopy (LIBS) would offer a time and spatially resolved, almost non-destructive, measurement of hydrogen at surfaces. We could already show that this analysis technique allows for highly accurate in situ measurements of chemical compositions of e.g. Mn, Cr and Ni during welding e.g. in the melt pool, the weld metal or the heat affected zone. For quantitative LIBS measurements of hydrogen in steel, certified reference materials with different hydrogen concentrations were used for calibration.
There is a significant problem in welding steels: A critical combination of diffusible hydrogen, hardness microstructure and weld residual stresses can cause cold cracks to form in the weld microstructure. We investigated hydrogen in steels, which was loaded either electrochemically or with high-pressure hydrogen gas. Subsequently, various experiments were conducted to verify the feasibility of hydrogen measurements with LIBS. For example, depth profiles of hydrogen distribution could be obtained. Furthermore, samples were water jet cut and a line scan was made over the cross section to obtain a spatially resolved representation of the hydrogen. Total hydrogen concentrations were determined using carrier gas hot extraction. Our results show that LIBS is a promising technique for time and spatially resolved measurement of hydrogen in steels.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic method for detecting the chemical composition of optically accessible surfaces. In principle, the measurement of all elements of the periodic table is possible. System calibrations allow the quantification of element concentrations. In combination with scanner systems, the two-dimensional element distribution can be determined. Even rough surfaces can be measured by online adjustment of the laser focus. To detect element ingress into the concrete, typically cores are taken, cut in half, and LIBS measurements are performed on the cross-section. The high spatial resolution as well as the simultaneous multi-element analysis enables a separate evaluation of the binder-matrix and aggregates. Therefore, the element concentrations can be determined directly related to the cement paste. LIBS measurements are applicable in the laboratory, on-site and also over a distance of several meters.
Common applications include the investigation of material deterioration due to the ingress of harmful ions and their interaction in porous building materials. LIBS is able to provide precise input parameters for simulation and modelling of the remaining lifetime of a structure. Besides the identification of materials, also their composition can be determined on hardened concrete, such as the type of cement or type of aggregate. This also involves the identification of environmentally hazardous elements contained in concrete. Another possible application is the detection of the composition of material flows during dismantling. Non-contact NDT for “difficult to assess” structures as an example application through safety glass or in combination with robotics and automation are also possible.
This work presents the state of the art concerning LIBS investigations on concrete by showing exemplary laboratory and on-site applications.
Laser-induced breakdown spectroscopy (LIBS) is a spectroscopic method for the analysis of the chemical composition of sample materials. Generally, the measurement of all elements of the periodic table is possible. In particular, light elements such as H, Li, Be, S, C, O, N and halogens can be measured. Calibration with matrix-matching standards allows the quantification of element concentrations. In combination with scanner systems, the two-dimensional element distribution can be determined. Even rough surfaces can be measured by online adjustment of the laser focus. LIBS can also be used on-site with mobile systems. Hand-held systems are available for point measurements.
Common applications include the investigation of material deterioration due to the ingress of harmful ions and their interaction in porous building materials. Due to the high spatial resolution of LIBS and the consideration of the heterogeneity of concrete, the determination of precise input parameters for simulation and modelling of the remaining lifetime of a structure is possible. In addition to the identification of materials, it is also possible to assess the composition for example of hardened concrete, which involves the cement or aggregate type used. Other important fields of application are the detection of environmentally hazardous elements or the material classification for sorting heterogeneous material waste streams during dismantling. Non-contact NDT for “difficult to assess” structures as an example application through safety glass or in combination with robotics and automation are also possible.
In this work, an overview of LIBS investigations on concrete is given based on exemplary laboratory and on-site applications.
Concrete structures experience severe damage during service, for example due to pitting corrosion of rebars caused by the ingress of chlorine (Cl) into the porous concrete structure. The ingress can be monitored using laser-induced breakdown spectroscopy (LIBS), a recently introduced civil engineering technique used to detect Cl in concrete structures in addition to conventional wet chemistry methods. The key advantages of LIBS are high spatial resolution, which is important when analyzing heterogeneous concrete samples, as well as the almost complete absence of sample preparation. To assess LIBS as a reliable analytical method, its accuracy and robustness must be carefully tested. This paper presents the results of an interlaboratory comparison on the analysis of Cl in cement paste samples conducted by 12 laboratories in 10 countries. Two sets of samples were prepared with Cl content ranging from 0.06 to 1.95 wt% in the training set and 0.23–1.51 wt% in the test set, with additional variations in the type of cement and Cl source (salt type). The overall result shows that LIBS is suitable for the quantification of the studied samples: the average relative error was generally below 15%. The results demonstrate the true status quo of the LIBS method for this type of analysis, given that the laboratories were not instructed on how to perform the analysis or how to process the data.
The combination of high corrosion resistance and good mechanical properties of duplex steels (DSS) is due to their chemical composition and the balanced phase ratio of ferrite (α) and austenite (γ).
Many industrial applications require a material joint of DSS. Tungsten inert gas (TIG) welding is relatively easy to use, requires little space and allows automated welding, with very high reproducibility and is therefore excellent for welding DSS.
During solidification of these steels, critical phase ratios of α and γ can occur, leading to solidification cracking, susceptibility to corrosion, lower ductility, and critical strength values. Therefore, to obtain the desired material properties, the α/γ distribution must be reliably predicted. This is usually done using the WRC1992 diagram. However, the prediction accuracy of the ferrite content in this diagram is usually not accurate enough and must therefore be optimized. It is therefore necessary to monitor even the smallest changes in the chemical composition of the weld metal, ideally during welding. This is done in these experiments using Laser-induced Breakdown Spectroscopy (LIBS). A major advantage of this technique is the highly accurate time- and spatially-resolved measurement of chemical composition during welding. Previous work has quantified the chemical composition in the weld metal and heat affected zone. In the presented study, the influence of individual elements, such as Nb and Cu, on the resulting weld microstructure is investigated.