Analytische Chemie
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Defect recognition in CFRP components using various NDT methods within a smart manufacturing process
(2018)
The manufacturing process of carbon fiber reinforced polymer (CFRP) components is gaining a more and more significant role when looking at the increasing amount of CFRPs used in industries today. The monitoring of the manufacturing process and hence the reliability of the manufactured products, is one of the major challenges we need to face in the near future. Common defects which arise during manufacturing process are e.g. porosity and voids which may lead to delaminations during operation and under load. To find irregularities and classify them as possible defects in an early stage of the manufacturing process is of high importance for the safety and reliability of the finished products, as well as of significant impact from an economical point of view. In this study we compare various NDT methods which were applied to similar CFRP laminate samples in order to detect and characterize regions of defective volume. Besides ultrasound, thermography and eddy current, different X-ray methods like radiography, laminography and computed tomography are used to investigate the samples. These methods are compared with the intention to evaluate their capability to reliably detect and characterize defective volume. Beyond the detection and evaluation of defects, we also investigate possibilities to combine various NDT methods within a smart manufacturing process in which the decision which method shall be applied is inherent within the process. Is it possible to design an in-line or at-line testing process which can recognize defects reliably and reduce testing time and costs? This study aims to show up opportunities of designing a smart NDT process synchronized to the production based on the concepts of smart production (Industry 4.0). A set of defective CFRP laminate samples and different NDT methods were used to demonstrate how effective defects are recognized and how communication between interconnected NDT sensors and the manufacturing process could be organized.
Analog zu Blitz und Donner können elektrische Entladungen innerhalb eines Gasvolumens als akustische Quellen agieren und haben daher eine starke Verbreitung als diagnostische Methode (bspw. in der Raumakustik und bei der Ortung von Teilentladungen). Diese auf dem Prinzip der Thermoakustik beruhende Möglichkeit der Schallerzeugung und die damit verbundenen physikalischen Wechselwirkungen machen die Notwendigkeit einer mechanisch ausgelenkten Membran überflüssig. Dabei wird dem hochfrequenten Träger das Nutzsignal aufgeprägt, welches eine Volumenänderung des umliegenden Gases um seinen Ruhezustand verursacht. Durch die somit hervorgerufene zyklische thermische Wechselwirkung mit dem umliegenden Gasgemisch bedarf es daher ebenfalls keiner akustischen Anpassung. In den vorgestellten Ergebnissen wurde das Übertragungsverhalten eines Oberflächenplasmas (SDBD, surface dielectric barrier discharge) untersucht. Als Maß für den Wirkungsgrad und das Übertragungsverhalten des Aktuators wurden Klirrfaktor- und THD- Messungen und unter Variation der Eingangsleistungen durchgeführt. Durch die positiven akustischen Eigenschaften eröffnen sich neue Applikationen für den Einsatz von Plasmahochtönern wie bspw. zerstörungsfreie Werkstoffprüfung von Verbundsystemen und Klebeverbindungen im Automobilsektor oder im Bauwesen.
In Glasfasern eingeschriebene Bragg-Gitter (FBG: fibre-based Bragg gratings) sind über die Verschiebung der Bragg-Wellenlänge in der Lage, Stauchungen und Dehnungen von Glasfasern hochgenau zu erfassen. In Kompositwerkstoffe eingebettete faseroptische Sensoren können Bauteile bezüglich ihrer mechanischen Integrität überwachen und früh-zeitig Informationen über Materialveränderungen gewinnen.
Um die Zuverlässigkeit eines solchen Sensors zu gewährleisten, ist es wichtig, die korrekte Funktion des Sensors im Verbund mit der Werkstoff-Matrix on-line und in-situ sicherzu-stellen. Im Rahmen des DFG-Projekts FAMOS² (FAser-basierter Magneto-Optischer SchichtSensor) wurde ein selbstdiagnosefähiger Schichtsensor entwickelt, der mit Hilfe von magnetostriktiven Aktorschichten aus Nickel bzw. Eisen-Nickel validiert werden kann.
Der FAMOS²-Schichtsensor wird durch ein PVD (physical vapour deposition)/ECD (electro-chemical deposition) Hybridschichtsystem realisiert, das auf dem Fasermantel im Bereich des FBG haftfest, homogen und langzeitfunktional abzuscheiden ist. Dabei wird in einem ersten Schritt ein etwa 100 Nanometer dünnes PVD-Schichtsystem aus Chrom und Kupfer als Haftvermittler auf der Glasfaser bzw. als leitfähige Startschicht für den nachfolgenden ECD-Prozess abgeschieden. Um eine rotationssymmetrische Schich-tabscheidung zu gewährleisten, erfolgt während der PVD-Beschichtung eine Rotation der Glasfasern. In einem zweiten Schritt wird dann unter Verwendung eines klassischen Watts-Elektrolyten in einer speziell entwickelten ebenfalls rotationssymmetrisch aufgebau-ten ECD-Durchströmungszelle dann die etwa 30 Mikrometer dicke, magnetostriktive Ak-torschicht auf dem PVD-Schichtsystem abgeschieden, im Vergleich sowohl reine Nickel-Schichten als auch Nickel-Eisen-Schichten.
Ein äußeres Magnetfeld dehnt die magnetostriktive Aktorschicht und damit auch die Faser reversibel. Diese Dehnung führt zu einer Verschiebung der Bragg-Wellenlänge, welche direkt mit der Stärke eines zu messenden oder zu Validierungszwecken vorgegebenen Magnetfeldes korreliert. Die Anpassung der Beschichtungsverfahren an die Fasergeome-trie und die mechanischen Eigenschaften der Hybridschichten werden hinsichtlich der me-chanischen Integrität des faseroptischen Sensors diskutiert und der Nachweis der Selbst-diagnosefähigkeit erbracht.
Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering (LS) as well as of acrylnitril-butadien-styrol (ABS) by Fused Layer Modeling (FLM), were tested with active thermography. For this, two different excitation methods (flash and impulse excitation) were used and compared, regarding the suitability for the detection of constructed and imprinted defects. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier-Transformation were applied. Furthermore, the long-term stability of the probes towards environmental stress, like UV-radiation, heat, water contact and frost is being investigated in the presented project with artificial weathering tests.
Es wird ein vereinfachtes Verfahren für die Bestimmung und Implementierung der Maschinennachgiebigkeit bei der Verwendung eines sphärischen Indenters dargestellt. Die Maschinennachgiebigkeit wird bei deutlicher Kraftabhängigkeit als Funktion der Kraft in die Auswertung implementiert. Als sensitiver Kennwert dient der aus der instrumentierten Eindringprüfung an Härtevergleichsplatten ermittelte Eindringmodul.
Minimally invasive injection of calcium phosphate cement into bone defects in aged sheep vertebrae has been used as a model for the treatment of osteoporotic vertebral fractures. One of the therapeutic criteria is a compression test of non-treated or treated vertebral bodies. In the present study, an in situ compression test with a stepwise load increase was performed with small spongiosa cylinders from the vertebrae under continuous monitoring by μCT. This allows localization of bone cracks and the visualization of correct placement and form of the bone cylinder. In addition, the effects of an uneven load distribution on the sample due to an irregular shape and a subsequent underperformance of the test sample can be excluded by controlling its shape under increasing load. There was a good agreement between the measured data and those obtained by simulated load-dependent transformation on the basis of a digital volume correlation between consecutive compression tests on the bone surface under the assumption of homogeneous bone material. Mechanic simulation was executed by directly using structural voxel data, resulting in maps of Von Mise stresses and predicted displacements.
Ionische Flüssigkeiten als neuartige Sensorbeschichtung für coulometrische Spurenfeuchtesensoren
(2018)
Die Arbeit präsentiert erste Messungen mit coulometrischen Sensoren, die mit einer ionischen Flüssigkeit beschichtet sind. Diese Sensoren werden in der Industrie verwendet, um die Spurenfeuchte in unterschiedlichen Gasen zu messen. Normalerweise erfolgt eine Beschichtung der Sensoren mit Phosphorpentoxid und dessen Hydrolyseprodukte. In dieser Arbeit wurde stattdessen eine hygroskopische ionische Flüssigkeit benutzt. Die generierte Gasfeuchte für die Untersuchungen betrug bezogen auf die Frostpunkttemperatur -80 °C bis -30 °C, was gleichbedeutend mit einem Wasserdampf-Stoffmengenanteil von 0,5 μmol·mol-1 bis 376 μmol·mol-1 ist. Zusätzlich zu der Messung mit coulometrischen Sensoren erfolgte eine Referenzmessung der Gasfeuchte mittels eines Taupunkthygrometers. Erste Ergebnisse haben gezeigt, dass es möglich ist mit dieser Art der Beschichtung unterschiedliche Gasfeuchten zu messen. Aber es ergaben sich trotz gleicher Feuchte unterschiedliche Signalintensitäten bei den benutzen Sensoren und es zeigte sich eine Drift des Sensorsignales.
Temperature characteristics of a piezoresistive accelerometer for high impact shock application
(2018)
This study presents the characterization of a piezoresistive accelerometer damped with silicon oil for the application in drop tests carried out at BAM. Experiments were performed with the Hopkinson Bar method in close correlation to the real-world application conditions. The results point out certain limitations regarding the temperature influence and the frequency response. Additional experiments were performed with a gas damped type of piezoresistive accelerometer, which has superior specifications, particularly for low temperatures. The results allow for a comparison.
In order to test their suitability different non-destructive methods were performed to inspect a GFRP plate with artificial defects. These defects were manufactured by means of thin PTFE sheets inserted between two plies in three different depth. The inspection methods were microwave reflection, flash thermography and phased array ultrasonics, all applied to the same specimen. Selected results are shown for all methods demonstrating opportunities and limits of the particular inspection methods. The achieved detection limits and further application aspects are compared directly to provide a useful information for the planning of inspection tasks.
Systematic errors in the evaluation of uncorrected data from thermographic lock-in measurements
(2018)
Lock-in thermography (LT) is based on the correct evaluation of phase differences between the temperature oscillations at different surface regions of the object under test during periodic heating. Since the usual heating procedures contain a DC component, the actual heating pattern achieved is not harmonic. This causes systematic deviations when phase differences are determined by means of harmonic analysis, e.g. with FFT analysis. The resulting errors depend clearly on the ratio between DC and AC amplitude, which is demonstrated at simulated and experimentally recorded temperature transients. Further experimental LT data obtained by different oscillating energy inputs showed a variety of possible shapes of transients with different DC components.
Um den sicheren Betrieb von Windkraftanlagen zu gewährleisten, werden Rotorblätter nach der Fertigung und nach Reparatur mit verschiedenen zerstörungsfreien Verfahren auf Schaden untersucht. Bei der Fertigung von Blattschalen, die in einer Sandwich-Schalenbauweise gefertigt werden, entstehen Imperfektionen, die unter Belastung zu großen Rissen führen können. Zur Prüfung von Blattschalen wird unter anderem Ultraschallprüfung in Kontakttechnik eingesetzt. Um den Wartungsaufwand von Ultraschallanlagen zu reduzieren und um manche Kompositstrukturen vor Koppelmittel zu schützen, wird die Anwendung von Luftultraschall erforscht. Insbesondere große Fortschritte gibt es im Bereich der Entwicklung neuer Wandler.
In diesem Beitrag berichten wir über die Luftultraschallprüfung von Schalen für Rotorblätter. Es wurden typische Sandwichschalenstrukturen hergestellt und mit einem eigenentwickelten Schalenprüfstand unter simulierter Betriebsbeanspruchung belastet. Die in den Schalenprüfkörpern entstandenen Schäden wurden außerhalb des Prüfstandes mit Luftultraschall in Durchschallung untersucht. Es wurden fokussierende Wandler auf Basis von Ferroelektreten entwickelt und für diese Prüfungen eingesetzt. Mit zusätzlicher elektrischer Vorspannung konnte die Empfindlichkeit der Empfänger deutlich erhöht werden. Die nach dem Lastwechsel entstandenen Schäden in den Rotorblattschalen waren eindeutig zu detektieren.
Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing.
Air-coupled ultrasound (ACU) is increasingly used for automated and contactless inspection of large-scale composite structures as well as for non-destructive testing (NDT) of water-sensitive or porous materials. The major challenge to overcome using ACU in NDT is the enormous loss of ultrasonic energy at each solid-air interface caused by the high acoustic impedance mismatch. Resonant low-frequency piezoceramic transducers are specially designed to achieve high sound pressure levels. For an expanded use of this technique, however, the spatial resolution needs to be increased.
Recent studies of our collaborative research group demonstrated the successful application of a resonance-free, highly sensitive receiver that uses a Fabry-Pérot etalon instead of piezoceramic materials or membranes. However, to reach the full potential of this broadband small-aperture optical microphone, novel transmitter concepts have to be developed and evaluated for advanced NDT applications.
Different types of transmitter were tested in combination with the optical microphone acting as receiver and they were compared to conventional piezoceramic transducers in through-transmission mode. Monolithic carbon fiber-reinforced plastics (CFRP) and CFRP sandwich structures containing different defect types were inspected. Presented results are processed as C-scan images and further evaluated for spatial resolution, signal-to-noise ratio and sensitivity of each measurement setup. Novel transmitter concepts, such as ferroelectret and thermoacoustic emitters, show promising findings with a considerably improved time and spatial resolution for ACU-NDT.
Using an infrared camera for radiometric imaging allows the contactless temperature measurement of multiple surface pixels simultaneously. From the measured surface data, a sub-surface structure, embedded inside a sample or tissue, can be reconstructed and imaged when heated by an excitation light pulse. The main drawback in radiometric imaging is the degradation of the spatial resolution with increasing depth, which results in blurred images for deeper lying structures. We circumvent this degradation with blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. The ground-breaking concept of super-resolution can be transferred from optics to thermographic imaging.
Half-Cell-Potential Mapping (HP) is the most popular non-destructive testing (NDT) method for the detection of active corrosion in reinforced concrete. HP is influenced by parameters such as moisture and chloride gradients in the component. The sensitivity to the spatially small, but dangerous pitting is low. In this study we show how additional measurement information can be used with multi-sensor data fusion to improve the detection performance and to automate data evaluation. The fusion is based on supervised machine learning (SML). SML are methods that recognize relationships in (sensor) data based on given labels. We use SML to distinguish "defective" and "intact" labeled areas in our dataset. It consists of 18 measurement - each contains HP, ground radar, microwave moisture and Wenner resistance data. Exact labels for changing environmental conditions were available in a laboratory study on a reinforced concrete slab, which deteriorated controlled and accelerated. The deterioration progress was monitored continuously and corrosion was generated targeted at a predefined location. The detection results are quantified and statistically evaluated. The SML results shows a significant improvement over the best single method (HP).
Magneto resistance sensors like GMR (giant magneto resistance) or TMR (tunnel magneto resistance) are widely used in industrial applications, examples are position measurement and read heads of hard disk drives. However, in case of non-destructive testing (NDT) applications these sensors, although their properties are outstanding like high spatial resolution, high field sensitivity, low cost and low energy consumption, never reached a technical transfer to an application beyond sci-entific scope.
This paper deals with benefits of GMR/TMR sensors in terms of high spatial resolution testing for different NDT applica-tions. The first example demonstrates the preeminent advantages of MR-elements compared with conventional coils used in eddy current testing (ET). The probe comprises one-wire excitation with an array of MR elements. This led to a better spatial resolution in terms of neighboring defects.
The second section concentrates on MFL-testing (magnetic flux leakage) with active field excitation during and before test-ing. The latter illustrated the capability of highly resolved crack detection of a crossed notch. This example is best suited to show the ability of tiny magnetic field sensors for magnetic material characterization of a sample surface. Another example is based on characterization of samples after tensile test. Here, no external field is applied. The magnetization is only changed due to external load and magnetostriction leading to a field signature which GMR sensors can resolve. This gives access to internal changes of the magnetization state of the sample under test.
Nach 1850 wurde zur weiteren Herabsetzung der Einbrenntemperatur von Glasmalfarben Borax (Na2B4O7 · 10 H2O) zugesetzt. Das Verhältnis war nun 1 Teil SiO2, 3 Teile PbO und 0,5 Teile Borax. Der analytische Nachweis von Bor in eingebrannten Malschichten war bisher jedoch nicht möglich.Daher wurden in Laborversuchen Glasmalfarben mit unterschiedlichem Gehalt an Borax auf Modellgläser aufgetragen, eingebrannt und anschließend unter simulierten Umweltbedingungen zeitraffend im Klimaschrank bewittert.
Mit Hilfe von elektronenmikroskopischen Untersuchungen können Malschichten charakterisiert werden und somit Hinweise auf mögliche Schadensursachen liefern. Erste Versuche zum Nachweis von Bor erfolgten mit Hilfe von LIBS-Messungen (Laser Induced Breakdown Spectroscopy) an im Labor hergestellten Glasmalfarben mit unterschiedlichem Boraxgehalt.
Zur Messung von Konzentrationen in Flüssigkeiten können akustische Sensoren genutzt werden. Ziel der vorliegend Arbeit ist es einen Sensor zu entwerfen der sehr hohe Messgenauigkeiten erzielen kann. Der Sensor besteht aus einem rechteckigen Rohr, welches auf einem Halbraum angebracht ist. Die Konzentrationsbestimmung erfolgt anhand des Resonanzverhaltens der Struktur, wodurch eine hohe Messgenauigkeit erreicht werden kann. Um den Sensors zu verwirklichen, muss eine Optimierung der Geometrie mit vielen Iterationsschritten durchlaufen werden. Da keine analytische Beschreibung des akustischen Verhaltens vorliegt, wird eine effiziente Simulationsmethode benötigt. Die Scaled Boundary Finite Element Method (SBFEM) für prismatische Strukturen erscheint für die Simulation geeignet, da Teile der Geometrie ohne neue Vernetzung geändert werden können. Für die Berechnung des Sensors wird ein Modell der akustischen Fluid-Struktur Interaktion benötigt, das bisher nicht vorhanden ist.
Die Präsentation behandelt die Implementierung des Fluidmodells in die SBFEM und deren Validierung. Für die Validierung werden die Ergebnisse mit analytischen Beispielen ohne Fluid-Struktur Kopplung und mit Comsol-Ergebnissen der Dispersionskurven mit Wasser gefüllter Rohre verglichen.
Schließlich wird das neuartige Verfahren für die Modellierung der Sensorgeometrie angewendet. An einer einfachen Geometrie wird das Sensorprinzip zur Bestimmung der Salzkonzentration demonstriert.
Austenitic stainless steel welds as well as dissimilar metal welds with nickel alloy filler material, used in safety relevant parts of nuclear power plants, still challenge the ultrasonic inspection. The weld material forms large oriented grains which lead on the one hand to high sound scattering and on the other hand – to inhomogeneity and to the acoustic anisotropy of the weld structure. The ultrasonic wave fronts propagate not linearly, as in ferritic weld joints, but along the curves, which depend on the specific grain structure of the weld. Due the influence of these phenomena, it is difficult to analyze the inspection results and to classify the ultrasonic indications, which could be both from the weld geometry and from the material defects. A correct flaw sizing is not possible.
In an ongoing research project, different techniques to improve the reliability of ultrasonic testing at these kinds of welds are investigated. In a first step (in the previous research project) two ultrasonic inspection techniques were developed and validated on plane test specimens with artificial and realistic flaws. In the ongoing project, these techniques are applied to circumferential pipe welds with longitudinal and transverse flaws.
The technique developed at the Federal Institute for Materials Research and Testing (BAM) in Germany uses a combination of ray tracing and synthetic aperture focusing technique (SAFT). To investigate the unknown grain structure, the velocity distribution of weld-transmitting ultrasound waves is measured and used to model the weld by ray tracing.
The second technique, developed at the Fraunhofer Institute for Nondestructive Testing (IZFP) in Germany, uses Sampling Phased Array (Full Matrix Capture) combined with the reverse phase matching (RPM) and the gradient elastic constant descent algorithm (GECDM). This inspection method is able to estimate the elastic constants of the columnar grains in the weld and offers an improvement of the reliability of ultrasonic testing through the correction of the sound field distortion. The unknown inhomogeneity and anisotropy are investigated using a reference indication and the special optimization algorithm.
Both reconstruction techniques give quantitative inspection results and allow the defect sizing. They have been compared to conventional ultrasonic testing with techniques, which are state of the art for components in nuclear power plants. The improvement will be quantified by the comparison of the probability of detection (POD) of each technique.
This work presents a first attempt to use ionic liquids as a new coating for planar coulometric sensors. These sensors are used for the measurement of trace humidity in various gases. Usually, the coating of the sensors is tetraphosphorus decaoxide and its hydrolysis products. Instead, a hygroscopic ionic liquid was used as sensor coating in this work. Generated frost point temperatures tf in the gas ranged from -80 °C to -30 °C, which is equivalent to vapour mole fractions xv from 0.5 μmol·mol-1 to 376 μmol·mol-1. In addition to the coulometric sensors, the generated humidity is determined by a precision dew point hygrometer as reference. First results show that it is possible to measure humidity with ionic liquid based coulometric sensors.