Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
- nein (22)
Die Probenpräparation ist ein Teil im Prozess der Baustoffuntersuchung und muss dementsprechend sorgfältig geplant werden. Die Probenpräparation ist letztendlich der Grundstein für alle folgenden Untersuchungen, somit wirken sich alle hier getroffenen Entscheidungen direkt auf die Qualität der Ergebnisse aus.
For concrete production aggregates, cement and water are mixed together and after 28 days of hydration a porous and multiphase material is formed. To consider the heterogeneity of concrete a 2D scanning system is used. The coarse aggregates (limit > 2 X d ) can be excluded. laser spot The remaining content is a mixture of flour grains and cement particles (micro heterogeneity). Harmful species like chlorides may penetrate together with water through the capillary pore space. A quantification of Cl regarding to the cement content only (European standard EN 206) is necessary for the damage assessment. A LIBS system operating with a NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and two Czerny-Turner spectrometer (UV and NIR range) have been used.
Concrete is a multiphase material made of cement, aggregates and water. The heterogeneity of concrete is a result of mixing aggregates (grain size between 0.125 mm to 32 mm) and cement (grain size < 0.04 mm) together. There are always aggregates with a grain size below 0.125 mm (flour grains) therefore the cement matrix is always a mixture of these small particles. Different grain size distributions by making concrete are important to ensure the needed density and com-pressive strength. In order to estimate the remaining lifetime of concrete structures the quantification of element concentra-tions of alkali and chlorides regarding to the cement matrix only (1/3 of the total mass), is a major concern in civil engineer-ing. Due to two-dimensional scanning with LIBS the coarse aggregates can be evaluated and excluded from the analysis. In the case of particles (flour grains and cement) smaller than the laser spot size, the microscopic hetero-geneity influences the laser-plasma interaction and has therefore an impact on the results. In this study the influence of the micro-heterogeneity and the impact on the laser-material interaction is examined. The effect of changing ratios between cement particles and aggregate particles in the laser-induced plasma has been analyzed (see figure 1, right). Therefore, different samples with defined grain sizes are prepared and the obtained distributions were analyzed with x-ray diffraction (XRD). For the LIBS measurements, an automated system that operates with a low energy NdCr:YAG laser (pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns, a repetition rate of 100 Hz) and a NIR Czerny-Turner spectrometer has been used.
2D evaluation of spectral LIBS data derived from heterogeneous materials using cluster algorithm
(2017)
Laser-induced Breakdown Spectroscopy (LIBS) is capable of providing spatially resolved element maps in regard to the chemical composition of the sample. The evaluation of heterogeneous materials is often a challenging task, especially in the case of phase boundaries. In order to determine information about a certain phase of a material, the need for a method that offers an objective evaluation is necessary. This paper will introduce a cluster algorithm in the case of heterogeneous building materials (concrete) to separate the spectral information of non-relevant aggregates and cement matrix. In civil engineering, the information about the quantitative ingress of harmful species like Cl−, Na+ and SO2−4 is of great interest in the evaluation of the remaining lifetime of structures (Millar et al., 2015; Wilsch et al., 2005). These species trigger different damage processes such as the alkali-silica reaction (ASR) or the chloride-induced corrosion of the reinforcement. Therefore, a discrimination between the different phases, mainly cement matrix and aggregates, is highly important (Weritz et al., 2006). For the 2D evaluation, the expectation-maximizationalgorithm (EM algorithm; Ester and Sander, 2000) has been tested for the application presented in this work. The method has been introduced and different figures of merit have been presented according to recommendations given in Haddad et al. (2014). Advantages of this method will be highlighted. After phase separation, non-relevant information can be excluded and only the wanted phase displayed. Using a set of samples with known and unknown composition, the EM-clustering method has been validated regarding to Gustavo González and Ángeles Herrador (2007).
For the damage assessment of reinforced concrete structures the quantified ingress profiles of harmful species like chlorides, sulfates and alkali need to be determined. In order to provide on-site analysis of concrete a fast and reliable method is necessary. Low transition probabilities as well as the high ionization energies for chlorine and sulfur in the near-infrared range makes the detection of Cl I and S I in low concentrations a difficult task. For the on-site analysis a mobile LIBS-system (k = 1064 nm, Epulse ≤ 3 mJ, t = 1.5 ns) with an automated scanner has been developed at BAM. Weak chlorine and sulfur signal intensities do not allow classical univariate analysis for process data derived from the mobile system. In order to improve the analytical performance multivariate analysis like PLS-R will be presented in this work. A comparison to standard univariate analysis will be carried out and results covering important parameters like detection and quantification limits (LOD, LOQ) as well as processing variances will be discussed (Allegrini and Olivieri, 2014 [1]; Ostra et al., 2008 [2]). It will be shown that for the first time a low cost mobile system is capable of providing reproducible chlorine and sulfur analysis on concrete by using a low sensitive system in combination with multivariate evaluation.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). The aim of the work is to quantitatively measure the chemical composition in the weld seam of various DSS and to identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material. Spectra were recorded every 1.3 s at a spacing of approximately 2 mm. During the cooling process the location of the measurement was not changed. The LIBS method is proofed to be suitable for the quantitative representation of the chemical compositions during the welding process.
Nichtrostende Duplexstähle (DSS) werden häufig verwendet, insbesondere bei Anwendungen, die eine hohe Festigkeit in Verbindung mit einer hohen Korrosionsbeständigkeit in aggressiven Medien erfordern. Beispiele hierfür sind Kraftwerkskomponenten und maritime Anwendungen. Beim Schweißen dieser Stähle kann es zu lokalen Schwankungen in der chemischen Zusammensetzung kommen. Dies führt zu einer Ferritisierung des Werkstoffs und beeinträchtigt die mechanischen Eigenschaften der Bauteile. In dieser Arbeit wurden Versuche zum Wolfram-Inertgas-Schweißen (WIG) mit DSS durchgeführt. Die Analyse der chemischen Zusammensetzung wurde in situ mit Hilfe der laserinduzierten Plasmaspektroskopie (LIBS) durchgeführt. Ziel der Arbeit ist es, die chemische Zusammensetzung in der Schweißnaht verschiedener DSS quantitativ zu messen und mögliche Einflüsse der Schweißparameter auf die Mikrostruktur des Werkstoffs zu ermitteln. Gemessen wurden die chemischen Konzentrationen der Hauptlegierungselemente Cr, Ni, Mn auf der Oberfläche der Probe während des Schweißprozesses und des Abkühlungsprozesses. Mn und Ni sind Austenitstabilisatoren, deren Gehalt beim Schweißen durch die Verwendung bestimmter hochlegierter Schweißzusatzwerkstoffe zunimmt. Die Spektren wurden alle 1,3 s in einem Abstand von etwa 2 mm aufgezeichnet. Während des Abkühlungsprozesses wurde der Ort der Messung nicht verändert. Die LIBS-Methode eignet sich nachweislich zur quantitativen Darstellung der chemischen Zusammensetzungen während des Schweißvorgangs.
Duplex stainless steels (DSS) are frequently used, especially in applications requiring high strength combined with high corrosion resistance in aggressive media. Examples include power plant components and maritime structures. During welding of these steels, local variations in chemical composition can occur. This results in ferritization of the material and negatively affects the mechanical properties of the components. In this work, tungsten inert gas (TIG) welding experiments were performed with DSS. Chemical composition analysis was realized in situ by using Laser Induced Breakdown Spectroscopy (LIBS). We could quantitatively measure the chemical composition in the weld seam of various DSS and identify possible influences of welding parameters on the microstructure of the material. The chemical concentrations of the main alloying elements Cr, Ni, Mn on the surface of the sample during the welding process and the cooling process were measured. Mn and Ni are austenite stabilizers and their content increases during welding by using certain high alloyed filler material.
Erstellung von Tiefenprofilen auf Schweißnähten mittels Laserinduzierter plasmaspektroskopie (LIPS)
(2021)
Duplexstähle sind hochlegierte, nichtrostende Stähle. Sie bieten aufgrund des ausgewogenen Phasenverhältnisses von Austenit und Ferrit einige physikalische Vorteile gegenüber anderen nichtrostenden Stählen. Beim Schweißen können sich durch die Kondensation von Schweißrauch und verdampftem Material verschiedene chemische Elemente auf der Oberfläche der erstarrten Schweißnaht anreichern. Dann ist die Bildung einer schützenden Chromoxidschicht nicht mehr gewährleistet und es kann an diesen Stellen zu Lochfraß kommen. Frühere Arbeiten haben gezeigt, dass die Anreicherung von Mangan und Chrom an der Oberfläche der Wärmeeinflusszone des geschweißten Edelstahls 304L mit LIBS gemessen werden kann. Wir stellen die Ergebnisse der Optimierung der LIBS-Parameter für präzise Dickenmessungen solcher dünnen Schichten und für Tiefenprofilmessungen vor. Dazu haben wir galvanisch beschichtete Kupferproben mit bekannten Schichtdicken verwendet. Die Mangankonzentration im Schweißgut ist reduziert. Dies hat einen großen Einfluss auf die metallografische Struktur des Materials.
Duplex steels are high-alloyed, stainless steels. They offer some physical advantages over other stainless steels due to the balanced phase ratio of austenite and ferrite. During welding processes, when welding fumes and vaporized material condensates, different chemical elements can accumulate on the surface of the solidified weld. Then, the formation of a protective chromium oxide layer is no longer guaranteed and pitting corrosion can occur at these places. Previous work has shown that the accumulation of manganese and chromium on the surface of the heat-affected zone of the welded high-grade steel 304L can be measured by LIBS.
We present the results of the optimization of LIBS parameters for precise thickness measurements of such thin films and for depth profile measurements Therefore, we used galvanically coated copper samples with known film thicknesses. The Concentration of manganese is reduced in the weld metal. This has a high impact on the metallografic structure of the material.