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Time-dependent in situ measurement of atmospheric corrosion rates of duplex stainless steel wires
(2018)
Corrosion rates of strained grade UNS S32202 (2202) and UNS S32205 (2205) duplex stainless steel wires have been measured, in situ, using time-lapse X-ray computed tomography. Exposures to chloride-containing (MgCl2) atmospheric environments at 50 °C (12–15 M Cl− and pH ~5) with different mechanical elastic and elastic/plastic loads were carried out over a period of 21 months. The corrosion rates for grade 2202 increased over time, showing selective dissolution with shallow corrosion sites, coalescing along the surface of the wire. Corrosion rates of grade 2205 decreased over time, showing both selective and pitting corrosion with more localised attack, growing preferentially in depth. The nucleation of stress corrosion cracking was observed in both wires.
Industrial Radiology is used for volumetric inspection of industrial objects. By penetration of these objects (typically weldments, pipes or castings) with X-ray or Gamma radiation the 3D-volume is projected onto a 2D image detector. The X-ray film is the oldest radiographic image detector and still in wide use in industry. The industrial X-ray film systems used today differ from these used in medicine. Medical film systems are described well in the literature, but industrial film systems not. So we start with a description of the properties and standards for industrial film systems. The requirements on image quality are defined by several standards and can be verified with different image quality indicators (IQIs). They describe the ability of the human being to detect small and low contrast indications in a noisy image background. The essential parameters for digital industrial radiology are described.
Since about 30 years electronic image detectors are gradually replacing the industrial film. These detectors are based on storage phosphor imaging plates in combination with Laser scanners (“Computed Radiography”, CR) or a variety of different digital detector arrays (DDA). Typical applications of CR and DDAs are discussed as well as new possibilities by digital image processing, which is enabled by the computer based image handling, processing and analysis.
The transition from X-ray film to digital detectors in radiography is accompanied by an increase of unsharpness due to the larger inherent digital detector unsharpness in comparison to film. The basic spatial resolution of digital detectors (see EN ISO 17636-2) is used today to describe this unsharpness. The geometrical unsharpness of the radiographic projection of object structures onto the detector plane is determined by the focal spot size of the X-ray tube and the magnification. The focal spot size is measured today (see ASTM E 1165) from pin hole camera exposures or edge unsharpness (see ASTM E 2903). The final image unsharpness is a result of a convolution of the geometrical and inherent detector unsharpness function, divided by the magnification factor of the object onto the detector plane. Different approximations of this convolution result in ASTM E 1000 and ISO 17636-2 in different optimum values for the magnification factor for a given focal spot size of a X—ray tube and the basic spatial resolution of the detector. The higher contrast sensitivity, an advantage of digital radiography, compared to film radiography is furthermore improved when using higher X-ray voltages as used with film and smaller focal spots of the X-ray tubes. This allows a higher distance between object and detector resulting in reduced object scatter in the image. The interactions between all these parameters will be discussed and simple rules for practitioners will be derived in this contribution.
Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering.
Die vorliegende Arbeit beschäftigt sich mit der experimentellen Validierung eingebetteter Sensorik zur pH-Wert Bestimmung basierend auf Fluoreszenspektroskopie.
Bisherige Karbonatisierungsmessungen basieren auf zerstörenden Methoden. Durch das Einbetonieren von immer erreichbaren pH-Sonden wird die Überprüfung zerstörungsfrei.
Um ein fehlerfreies, reproduzierbares Ergebnis zu gewährleisten, mussten diese pH-Sonden zunächst getestet und eine ausreichend präzise Methode zur Messung entwickelt werden.
Durch das Vorgeben unterschiedlicher pH-Milieus und dem Testen verschiedener Messmethoden und Versuchsaufbauten werden Situationen im Beton simuliert.
Hierzu werden die pH-Sonden mit unterschiedlich starken basischen und neutralen Lösungen in Kontakt gebracht, wodurch der in den Sonden befindliche Indikator je nach pH-Wert eine blaue oder orange Färbung annimmt. In den Sonden befindliche Quantenpunkte werden durch einen Laser angeregt. Diese Quantenpunkte fluoreszieren aufgrund der Anregung im blauen und orangen Spektrum. Mithilfe der Fluoreszenzspektroskopie wird die durch den Indikator gefilterte Fluoreszenz in Reflexion und Transmission gemessen. Die Ergebnisse werden genutzt, um ein Verhältnis zwischen den zwei Wellenlängen zu berechnen, anhand dessen zu erkennen ist, welche Farbe der Indikator in den Sonden angenommen hat. Die experimentelle Validierung dient der Optimierung der Methodik, des Versuchsaufbaus und der Zusammensetzung der Sonden. Nach eine Reihe unterschiedlicher Versuche, werden Bedingungen geschaffen, welche zu den gewünschten Ergebnissen führen. Das in Reflexion gemessene Licht kann Aussage darüber geben, welche Farbe der Indikator annimmt und das Verhältnis zwischen dem blauen und dem orangen Spektrum gibt die erwarteten Werte zurück. Die Ergebnisse dieser Arbeit sollen in Betonprobekörpern angewandt werden, um die hier erprüfte Methode in Realbedingungen zu testen.
In the field of optically excited thermography, flash lamps (impulse shaped planar heating) and halogen lamps (modulated planar heating) have become established for the specific regimes of impulse and lock-in thermography. Flying-spot laser thermography is implemented by means of a rasterized focused laser, e. g. for crack detection (continuous wave operation) and photothermal material characterization (high-frequency modulated). The availability of novel technologies, i. e. fast and high-resolution IR cameras, brilliant innovative light sources and high-performance data acquisition and processing technology will enable a paradigm shift from stand-alone photothermal and thermographic techniques to uniform quantitative measurement and testing technology that is faster and more precise. Similar to an LED array, but with irradiance two orders of magnitude higher, a new type of brilliant laser source, i. e. the VCSEL array (vertical-cavity surface-emitting laser), is now available. This novel optical energy source eliminates the strong limitation to the temporal dynamics of established light sources and at the same time is spectrally clearly separated from the detection wavelength. It combines the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination area of flash lamps. In addition, heating can also be carried out in a structured manner, because individual areas of the VCSEL array can be controlled independently of each other. This new degree of freedom enables the development of completely new thermographic NDT methods.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowattclass laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. We present current activities with kilowatt-class highpower laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.
Mit Laserlicht kann man eine Materialoberfläche berührungslos und schnell moduliert aufheizen. Dabei entsteht eine stark gedämpfte Wärmewelle, die tief ins Material eindringen kann. Erzeugt und überlagert man solche thermischen Wellen auf kohärente Weise, dann kann man damit versteckte Materialfehler zerstörungsfrei und sehr präzise aufspüren. Sogar eine bildgebende Tomografie ist denkbar.
Impact damages and delaminations in fibre-reinforced composites (FRC) might not be visible at the surface, but could have an influence on the resistance and on the long-term behaviour of the component. Therefore, and especially for safety relevant structures, non-destructive methods are required for the assessment of such damages.
Active thermography methods are suitable to characterize damages after loading using different kind of excitation techniques and various configurations of infrared (IR) camera and heating sources. Here, flash lamps, impulse excitation with infrared radiator and lock-in technique with halogen lamps or widened laser beams are suited. In addition, non-optical sources like sonotrodes (requiring direct contact to the structure) or induction generators (only suited for carbon fibre reinforced polymer (CFRP) structures) could be applied as well. For the investigation of the evolution of the damage during the impact, passive thermography can be applied in-situ. Elastic and plastic deformations alter the temperature of the structure and thus the temperature on the surface.
In this contribution, at first the general principles of quantitative defect characterisation in FRC using active thermography with flash, impulse and lock-in excitation are described. Optical and thermal properties of the FRC material and its anisotropy are considered. Results of phase differences obtained at flat bottom holes with flash and lock-in thermography are compared for qualifying both methods for quantitative defect characterization. Secondly, the damage evolution of CFRP and GFRP structures under impact load and static tensile loading is described. The spatial and temporal evolution of the surface temperature enables us to distinguish matrix cracks or fibre-matrix separation from delaminations between the layers. Afterwards, all results for loading defects, obtained by passive and active thermography, are compared with each other. Fig. 1 and 2 show the difference of passive and flash thermography obtained at impact and tensile loaded CFRP plates, respectively. As one purpose of these investigations is the development of standards within national (DIN) and European (CEN) standardisation bodies, new draft and final standards are presented and further needs are discussed at the end of the presentation.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration.
We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.
Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz, see Fig.1. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration.
Using the one-dimensional solution to the thermal heat diffusion equation together with the absorptance of the material which is illuminated with a harmonically modulated light source, we can calculate the temperature oscillation at the surface of a solid. As a second step, we calculate the corresponding oscillation of the total thermal emission using Stefan-Boltzmann law as a first order approximation and taking into account the emissivity of the material. Within this framework we can calculate the minimal irradiance of a light source necessary to provoke a measurable signal within a thermographic camera at a noise equivalent temperature difference (NETD) of 30 mK. In Fig. 2 this relationship is displayed for a wide spectrum of modulation frequencies and for a number of different light sources scaled to the same electrical input power and illumination area. Using this figure, it is now easily possible to analyze the range of materials to be tested using lock-in thermography, since only the materials (dotted lines) below the irradiance-vs-frequency curves (solid lines) are heated in excess of the camera’s NETD. This figure clearly shows that laser sources considerably increase the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in texting.
We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages.