The research of B. Helber is supported by a fellowship of the Agency for Innovation by Science and Technology (IWT, dossier #111529) in Flanders, and research of T.E. Magin by the European Research Council Starting Grant #259354. We acknowledge Mr. P. Collin for his valuable help as Plasmatron operator. We gratefully acknowledge George Law and Stephen Ellacott for providing the test material and for informative support.

1. Facility Preparation
<ol>
	<li>Define probe and sample-holder assignment based on availability and facility specifications (3 probe holders in this work) to obtain best views on test sample from outside the facility for optical measurements during the experiment.</li>
	<li>If a pyrolyzing material is used, place the test sample in a cooled environment (T &#60; 200 &#176;C) prior to test start to prevent early degradation and outgassing.</li>
	<li>Use available probe holders for heat flux measurements and pressure measurements of the plasma flow, details about heat flux and Pitot pressure measurements in the Plasmatron facility can be found in reference 24.</li>
</ol>
2. Measurement Techniques Setup
<ol>
	<li>Emission spectrometer setup &#38; alignment
	<ol>
		<li>Identify the desired spectrometer depending on the test objectives and the available apparatus: Possible setups consist of several small, but broad spectral-range spectrometers for point measurements, or high-resolution spectrographs connected to a 2D CCD array allowing for spatially resolved measurements (for instance along the centerline or the radius of the plasma jet in front of the test samples).</li>
		<li>Depending on the chosen spectrometer configuration, determine the magnification that will be required and choose the appropriate lens as outlined below:
		<ol>
			<li>Observe three locations within 4 mm (expected boundary layer thickness) in front of the test sample by the spectrometers, hence, 2 mm increments. This results in a magnification of m = 3 for the optical system due to the minimal distance between each of the fibers being limited to 6 mm by the fiber cladding (4 mm onto 12 mm yielding m = 3).</li>
			<li>Determine the required lens focal length by the magnification and thin lens equation: 
			m = si/so, with si and so being the distances from the lens to the image and to the object, respectively; 1/so + 1/si = 1/f, with f being the focal length of the lens. 
			Note: In this protocol: si = m x so = 3 x 1,000 mm = 3,000 mm, resulting in f = 750 mm.</li>
			<li>Use mirrors if the distance between lens and object is impractically large (here 3,000 mm).</li>
		</ol>
		</li>
		<li>Remove jacketing of the optical fibers in order to bring them as close together as possible and design a convenient mounting system. For example, use a simple press fit assembly with the fibers lying beside each other.</li>
		<li>Align the optical system (consisting of lens, mirrors, optical fiber ends) using a vertical and horizontal line laser: Bring all components to the same height (as the test sample) and align lens perpendicular to the sample&#39;s stagnation line (region in front of the sample&#39;s nose on the axis of the sample).</li>
		<li>Focus the optical path by placing the lens at distance so from the test sample and the optical fiber ends at distance si from the lens. Illuminate the sample stagnation point with a lamp and position the fiber ends at the location of the best focused image. 
		Note: Creating the image of a pencil style Mercury calibration lamp positioned in front of the test sample can help: connect one spectrometer to an optical fiber and place the moveable fiber end where the strongest mercury emission occurs.</li>
		<li>Once the lens-fiber system is aligned, send a laser point through the fiber ends (spectrometer side) and observe the focused laser on the sample side with a white paper sheet to confirm correct position and focusing in front of the test sample (prior to each test run).</li>
		<li>Prevent any emission except that from the focal point from entering the optical fiber ends by enclosing the optical path with black cardboard. Crosscheck with a laser beam that no light except that focused by the lens and reflected by the mirrors reaches the fiber ends within the enclosed system. To do so, send a laser beam through the optical fibers (spectrometer side) and check that no light emitted by the fiber end is able to reach the lens directly.</li>
	</ol>
	</li>
	<li>High-Speed Camera (HSC)
	<ol>
		<li>Use a high-speed camera for surface observation if available to allow for short exposure times for un-saturated images of the hot, ablating surface.</li>
		<li>Observe the test sample with the HSC perpendicular to the sample&#39;s surface. Use the sample - lens system axis for horizontal and vertical alignment of the camera optics. Make sure the center of field of view of the HSC coincides with the center of the lens and the sample stagnation point.</li>
		<li>Synchronize HSC and emission spectrometers with a Digital Delay Generator (DDG). Trigger the HSC recording with a single voltage peak from the DDG and trigger each spectrum recording with the desired frequency (2Hz) during the experiments (section 3).</li>
	</ol>
	</li>
	<li>Radiometry
	<ol>
		<li>Use a two-color pyrometer for observation of the surface temperature in combination with a quartz window at the test chamber. 
		Note: If very high target temperatures are expected, exceeding the measurement range of the device, consider decreasing the measureable radiance with an appropriate filter or window of lower transmittance.</li>
	</ol>
	</li>
</ol>
3. Experimental Testing
<ol>
	<li>Take photographs with a conventional DSLR camera, measure dimensions (using a caliber rule) and weight of the virgin test sample before installation in the test chamber.</li>
	<li>Setup HSC software:
	<ol>
		<li>Set high exposure time (90 msec) to align and focus the HSC prior to the experiment with the test sample in place and take a pre-test image (post-trigger = 1).</li>
		<li>Change exposure time for experiment (2-10 &#181;sec), and set post-trigger to maximum (to store all frames), set correct recording rate (fps) to cover the full experiment (here 30-90 sec at 100 fps).</li>
		<li>Set initial f-number to f/16.</li>
	</ol>
	</li>
	<li>Set the DDG to the desired repetition rate at which spectra shall be recorded by the spectrometers (here: 2 Hz). The first trigger pulse will start the HSC acquisition.</li>
	<li>Set up the spectrometer acquisition software (integration time &#964;exp: depending on emission intensity, here: 20-150 msec, adapt during the experiment if necessary, average = 1).
	<ol>
		<li>Make sure the optical system is still positioned correctly prior to the experiment with the sample in place (see step 2.1.6).</li>
		<li>Take background image Sbg with each spectrometer and save it.</li>
		<li>Change the trigger to &#39;external software&#39;, depending on the software (e.g., SpectraSuite) (other options are: &#39;external&#39;, and &#39;synchronize&#39;, with different purposes).</li>
		<li>Save each spectrum when receiving a trigger pulse.</li>
	</ol>
	</li>
	<li>Install a high definition (HD) camera at any optical access if desired.</li>
	<li>Place the test sample in the protection system and vacuum the test chamber using a group of three rotary-vane vacuum pumps and a roots pump.</li>
	<li>Start the plasma facility and bring it to the desired test condition in terms of heat flux and pressure by adjusting the electric power input and the vacuum pumps. Use heat flux probe and the pitot probe (step 1.3) to observe the achieved conditions (1 MW/m2 and 3 MW/m2 at 15 hPa and 200 hPa).</li>
	<li>Start recording of HD-camera and pyrometers.</li>
	<li>Take a free-stream spectrum with all spectrometers available (for calibration comparison) then lower integration time to prevent saturation (from 200 msec to 50 msec).</li>
	<li>Trigger HSC and spectrometers via DDG (see step 3.2 for setup) by pressing &#39;trig&#39; and setting the mode from &#39;external&#39; to &#39;internal&#39;.</li>
	<li>Inject the test sample into the plasma flow. Here, a pneumatic mechanism is used to inject the sample.</li>
	<li>Adjust integration time of spectrometers if necessary to avoid saturation (ideally, any change of setup configuration should now be avoided).</li>
	<li>Adjust aperture of HSC if necessary to prevent sensor saturation.</li>
	<li>Remove test sample after desired test time (30 sec or 90 sec) into the sample protection system and shut down plasma flow.</li>
	<li>Stop DDG and spectrometer acquisition, save HSC images, and stop pyrometer acquisition. 
	Note: Leave pyrometer running if a material with high thermal capacity is tested to monitor cool-off phase (not necessary for CBCF preform).</li>
	<li>Send laser point through optical fiber ends (spectrometer side) and observe laser focus with HSC, save this image to mark position of the spectrometer. Repeat this step with each spectrometer / optical fiber. 
	ATTENTION: Make sure laser is not too strong to damage the CCD array of the camera. A discharging device is preferred. Alternatively, an image of the laser pointing on a paper sheet in front of the tested sample can be taken.</li>
	<li>Place a chessboard at the position of the test sample and record image with HSC for calibration.</li>
	<li>Remove test sample (e.g., by hydraulic ejection), take weight, take photographs, and store in sample storage to protect the brittle char layer composed of oxidized fibers (do not touch the frontal sample surface).</li>
</ol>
4. Spectrometer Calibration
<ol>
	<li>Spectral calibration
	<ol>
		<li>Place a spectral calibration lamp in the focal point of the lens (e.g., a pencil style Mercury lamp) to determine the wavelength calibration and the full-width-half-maximum (FWHM) of the optical system, details on those steps can be found in the literature29.</li>
	</ol>
	</li>
	<li>Intensity calibration
	<ol>
		<li>Perform an intensity calibration of each optical system consisting of the light collection mechanism (lens) and spectrometer efficiencies in W/(m2&#183;sr&#183;nm) between 350 nm and 900 nm. Do this by placing a tungsten-ribbon lamp (OSRAM WI 17G) in the focus of each collection optic inside the test chamber. Record the calibration lamp&#39;s spectrum Scal, exp and obtain the calibration factor C by: 
		C = Scal, th / (Scal, exp-Sbg, cal) x &#964;cal, 
		with the theoretical spectral response of the calibration lamp (provided by manufacturer) Scal, th, the measured signal of the calibration lamp Scal, exp, the background Sbg, cal, and the integration time during the calibration measurement &#964;cal.</li>
	</ol>
	</li>
</ol>
5. Data Processing
<ol>
	<li>Surface recession rate and spectrometer probing location(s):
	<ol>
		<li>Observe sample injection and ejection times on the HSC video file for correct test time estimation.</li>
		<li>Observe pixel location of the test sample stagnation point at injection from the HSC video file.</li>
		<li>Calibrate HSC magnification by exporting image taken in step 3.17 (for instance, .tiff format) and counting the pixels in the measurement region spanning multiple chessboard squares. Compute the correlation pixels:mm (obtain a more detailed characterization of the intrinsic and extrinsic camera parameters using the camera calibration toolbox in MATLAB if desired).</li>
		<li>Export the image(s) taken in step 3.16 (for instance, .tiff format) and find the pixels of the spectrometer probing location(s) as bright spots on the image, indicating x- and y-position.</li>
		<li>Export HSC images (e.g., Multitiff-format) and perform edge detection (e.g., using Matlab build-in function &#39;edge&#39;) to define the stagnation point location at each time step i (xi and yi).</li>
		<li>Subtract the position of the surface (step 5.1.5) from the position of the spectrometer probing location(s) (step 5.1.4) for each time step to obtain their distances d(t) from the surface.</li>
	</ol>
	</li>
	<li>Emission spectra processing (all post-processing can for instance be performed within Matlab).
	<ol>
		<li>Export all recorded spectrum files (wavelength vs. intensity) and calibrate the intensity response of each recorded spectrum by: 
		Sexp,cal = (Sexp-Sbg) / &#964;exp x C, 
		with the experimentally obtained spectrum Sexp, the background file Sbg (step 3.4.2), the experimental integration time &#964;exp and the calibration factor C determined during step 4.2.1.</li>
		<li>If several spectrometers are used, assess the validity of the calibration coefficient C using the freestream spectra taken during step 3.9. Plot all calibrated free-stream spectra together; their responses should be nearly identical because the spectrometer collection volumes in the plasma flow are very close to each other.</li>
		<li>Open the file containing the wavelength vector of the calibrated spectra (e.g., double-click the .mat file in MATLAB) and identify the row indices corresponding to wavelengths &#955;1 = 370 nm and &#955;2 = 390 nm (alternatively, use the &#34;find&#34; command in Matlab). 
		Note: For pyrolyzing ablators phenol originated species are also available, such as C2, CH, H, NH, OH.</li>
		<li>Integrate the emission signal of interest (here CN violet emission, 370-390 nm) between the two indices (&#955;1 and &#955;2) from step 5.2.3 for each time step (I&#955;1-&#955;2(t)).</li>
		<li>Plot with software of choice the spectrally integrated emission (I&#955;1-&#955;2(t)) of each spectrometer (step 5.2.4) as a function of the spectrometer distances from the surface (step 5.1.6) (Figure 2) (For example, plot(d(:,1:3),I(:,1:3),&#39;x&#39;) ).</li>
		<li>For better interpretation of the results, perform a polynomial fit of the data and plot the results (e.g., using MATLAB&#39;s polyfit command: 
		[p,ErrorEst] = polyfit(d(:,1:3),I(:,1:3,9); 
		[fit,delta] = polyval(p,d(:,1:3),ErrorEst); plot(d,fit) ) 
		Note: Depending on the location and resolution of the recorded spectra, the excited states temperature of molecules can be determined. Use a radiation simulation tool to fit numerical spectra to experimental spectra of the CN violet and C2 swan systems. Several online tools include spectral fitting tools to obtain translational, rotational, vibrational, and electronic temperatures30.</li>
	</ol>
	</li>
</ol>
6. Post-test Sample Inspection
<ol>
	<li>Scanning Electron Microscopy (SEM) to study the carbon fibers &#38; char layer degradation 
	Note: Due to their high electrical conductivity, no further treatment is necessary in the case of fully charred carbon samples. Charging and distortion of the images will occur if virgin phenolic resin is present within the test sample.
	<ol>
		<li>If possible, place the full test sample in the vacuum chamber of the SEM device to examine the char layer avoiding any destruction of the surface. 
		Note: A detailed description of SEM and X-Ray Microanalysis applied to composite materials is given in literature31 and not included in this protocol.</li>
		<li>Use a virgin (not tested) material sample as reference to study the carbon fiber dimensions:
		<ol>
			<li>Select one single, well observable fiber with the SEM system.</li>
			<li>Estimate the virgin carbon fiber thickness and fiber length with the tools provided by the SEM system software according to manufacturer&#39;s instructions. For example, search in the toolbar for &#34;Measurement&#34; and select &#34;Ruler&#34;, then tap the beginning and end points of the target object (e.g., the start and end points of a single fiber). 
			Note: This produces a connecting line segment and the distance is displayed. Successively conduct this operation as necessary.</li>
		</ol>
		</li>
		<li>Identify the fiber degradation mechanisms on the tested sample, for instance a needle shape, suggests an oxygen diffusion-limited ablation regime28, whereas pitting of the fibers and local attacks might be due to a reaction controlled regime and/or local active sites due to impurities of the material.</li>
		<li>Cut the brittle material using a scalpel. Investigate the in-depth degradation and estimate the depth in which the fibers are thinned by comparing the thickness of ablated fibers to the virgin fiber thickness (step 6.1.2.2).</li>
		<li>Detect possible soot formation and carbon deposition at the surface on pyrolyzing ablators, this can be enhanced if the sample was tested in an oxygen-poor atmosphere (e.g., nitrogen or argon).</li>
		<li>Use Energy-dispersive X-ray analysis (EDX)31 along with the SEM to detect and identify impurities of the material that may lead to increased reactivity (e.g., calcium and potassium).</li>
	</ol>
	</li>
</ol>

The authors have nothing to disclose.

This protocol describes procedures for the material characterization of reacting thermal protection materials in high enthalpy flows and presents sample results obtained on a non-pyrolyzing, ablating carbon-bonded carbon fiber (CBCF) precursor. The CBCF material is very similar to the rigid precursor for low-density carbon-phenolic ablators such as PICA and Asterm, which are the ultimate targets of the presented techniques. The main advantages of the CBCF material are its low price and open availability, since it is not restricted to export control licenses. It was chosen for presentation of the authors&#39; approach as other research institutions can easily obtain raw CBCF material. With this publication, the authors envisage the definition of a relatively straightforward standard procedure, facilitating comparison with other laboratories.
The core techniques are a non-intrusive method to track the material recession and probing of the chemistry in the reactive boundary layer by emission spectroscopy. Application of high-speed imaging is a straightforward technique but care has to be taken with alignment of the camera system and the expected surface radiance. A short exposure time in the order of few microseconds helps to avoid saturation of the camera sensor.
A few photogrammetric techniques for ablator recession are reported in the literature, for example by L&#246;hle et al.34. They are superior to our technique due to imaging of the whole ablator surface at higher resolution. The authors state a resolution of 21 &#181;m, which is almost one order of magnitude higher than that of the technique presented in our work. However, installation of the photogrammetric setup, calibration, and post-processing are time consuming (the authors report 1 day/test), and two optical ports are required if two independent cameras have to be used. Test campaigns that require a high number of test samples make this application very costly. The technique presented in this protocol is easily set up and post-processing can be done with existing numerical tools. Our technique met the target objective of following the surface recession in situ. The accuracy of our technique could be further increased with a higher camera resolution or higher focal length of the optical system. However, if the material analysis requires high spatial resolution of surface details, we suggest the employment of photogrammetric techniques.
Care has to be taken with the alignment and calibration of the optical system for optical emission spectroscopy (OES). This technique is limited to line-of-sight measurements and the probing is constrained to electronically excited atoms and molecules. But its simplicity and high return on investment still governs over more elaborate techniques such as for example laser-induced fluorescence (LIF) spectroscopy, which is difficult to carry out near the surface during ablation analysis. Although LIF spectroscopy has successfully been applied to the investigation of ground state species populations in the plasma freestream39,40, LIF measurements in the boundary layer are relatively rare. Measurements of SiO in front of a hot SiC sample are reported by Feigl41 but have not been performed yet for ablating surfaces. The receding surface of the ablator prohibits long measurement times in the boundary layer. Apart from this are LIF systems very expensive due to the high number of specific components.
The spatial and temporal evolution of ablation products is of interest for this publication, which can be relatively simply carried out by emission spectroscopy. Three low resolution, broad range spectrometers served to detect multiple atoms and molecules present during ablation testing. The optical diagnostic bench consisted of a light collecting lens, two mirrors, and one optical fiber for each of the three spectrometers. It was important for the optical setup that no light, except that focused by the lens, reached the optical fibers.
If a pyrolyzing material is being studied, numerous hydrocarbons are ejected by the material, which are omnipresent in combustion flames, such as for example Hydrogen (Balmer series, H&#945; and H&#946;), C2 (Swan system), CH, OH, NH42. These can be detected with this setup. Several research groups are recently applying emission spectroscopy to analyze the reactive boundary layer forming around ablative heat shield materials19,22,43,44. MacDonald et al.22 preformed ablation tests in an inductively coupled plasma. The setup consisted of a similar low-resolution spectrometer with a spectral resolution of 1.16 nm, which is lower than the resolution provided by the spectrometer used for our setup. Their initial test sample shape was a cylinder, experiencing strong edge ablation, as demonstrated by the rising surface temperature during the test. Hence, the boundary layer thermochemical condition probably changed during the experiment, complicating a time-averaged analysis. The hemispherical test sample used for our analysis did not experience edge ablation and maintained its shape during the 30 - 90 sec test time45.
Hermann et al.44 provide first results on radiation-ablation coupling in a magnetoplasmadynamic arcjet facility applying emission spectroscopy. This is of high interest for the scientific community as there has not been much investigation in long-duration ground-test facilities on this topic. Unfortunately, no temporal behavior of the emission in front of the pyrolyzing material is reported. Their spectra in the range 300-800 nm were concatenated to a full spectrum during post-processing from 120 nm wavelength segments, by changing the center-wavelength of the used spectrograph. Hence, several spectra were taken over time to cover the full spectral range. If the ablative material, CBCF preform and Asterm in their case, experienced a strong temporal behavior caused by both transient pyrolysis gas ejection and surface ablation, this may falsify the temporally averaged spectrum.
One advantage of the spectrograph presented in our work is thus the wide spectral range (200-900 nm) compared to slit spectrographs, which usually result in a maximum range of 120 nm at lowest resolution. The wide spectral range observed with one single acquisition allows observation of various species in the boundary layer, resulting from the ablation and pyrolysis processes, such as hydrogen containing species (OH, NH, CH, H), carbon contributors (C, CN, C2), and contaminants (Na, Ca, K). However, if only a single species transition is of interest, a high-resolution slit-spectrograph may be applied, which further allows scanning of the full radial emission profile as was performed by Hermann et al.44
Applications of the experimental data are, for instance, validation of coupled CFD and material response codes. A stagnation-line code with ablative boundary condition has recently been developed at the VKI for reproduction of the flow field along the stagnation-line of spherical bodies in the VKI Plasmatron46. A preliminary comparison of the experimental boundary layer emission with simulated profiles was presented elsewhere45.
The microscale analysis of tested samples was indicative of different degradation phenomena of the carbon fibers in air and nitrogen plasma. The observed icicle morphology of ablated fibers further supported the assumption of diffusion-controlled ablation, as was suggested by the nearly identical recession rates at low pressure (15 hPa). Furthermore, the absence of internal material oxidation argues against the inflow or diffusion of hot boundary layer gases into the porous test sample. Such internal oxidation, as studied numerically by Weng et al. for PICA47, could lead to a weaker fiber structure, causing mechanical failure of the material, for example, in the form of spallation48,49. Therefore, we highly suggest a general microscale analysis along with high-enthalpy testing of porous carbon-composite materials for heat shield applications. The ultimate goal of a microscale analysis would be the identification of the carbon fiber intrinsic reactivities. Spatially resolved images could advance such analysis, for instance, by micro-tomography as carried out by Panerai et al.50. A material code was developed at the VKI using discontinuous Galerkin discretization to simulate the complex in-depth thermal response of ablative composite materials51.This code makes use of the new thorough physico-chemical library Mutation++, providing the thermal and transport properties of gas mixtures, including the calculation of both finite-rate gas-phase chemistry and homogeneous/heterogeneous gas/gas-solid equilibrium chemistry52. We envisage comparison of our experimental data to the material response code, which is able to represent the microscale state of the porous medium.

On 6 August 2012, NASA&#39;s Mars Science Laboratory (MSL) mission successfully landed a rover on the Martian surface. This rover already includes an automated sample collection system for chemistry and mineralogy analysis. Not long after, on 12 November 2014, the robotic European Space Agency lander Philae achieved the first soft landing on a comet. These examples indicate that the next steps will be to identify, develop, and qualify required technologies for returning Martian or asteroid samples safely to Earth. Currently, ablative materials are the only option for the Thermal Protection System (TPS) of such sample return missions, which shields the spacecraft from the severe heating during hypervelocity entry. Chemical and physical decomposition of ablators transform the thermal energy into mass loss and recession, whilst the remaining solid material insulates the vehicle substructure1,2. With the methods presented throughout this protocol, we want to contribute with new experimental data to the ongoing efforts of improving the heat shield reliability by reducing design uncertainties and developing new thermo-chemical ablation models.
To achieve high performance characteristics of the ablative Thermal Protection Material (TPM) engineers of planetary probes and space vehicles make use of a wide range of composites3,4. TPMs are generally composed of a rigid precursor and a filling matrix, to serve as a pyrolyzing, ablating, and insulating material at low weight with reasonable mechanical properties. Current examples of a new family of porous lightweight ablators for high-speed entry missions, made of a carbon fiber preform impregnated with phenolic resin, are PICA (phenolic impregnated carbon ablator) developed by NASA5,6, and the European ablator Asterm7. In addition to the space agencies in collaboration with industry, several research groups started on an academic level to manufacture and characterize new lightweight ablators, see for example references 2,8-12.
During atmospheric entry, part of the heat flux coming from the shock heated gas is transferred inside the heat shield and the virgin material is transformed following two mechanisms: Pyrolysis progressively carbonizes the phenolic resin into a low density, porous char, losing around 50% of its mass producing pyrolysis gases by vaporization. The pyrolysis gases are transported out of the material by diffusion and the pressure increase caused by their decomposition. They exhaust into the boundary layer, providing a further barrier for the heat exchange by blowing and undergo additional chemical reactions. The usage of polymers such as phenolic resins for the matrix takes advantage of their endothermic degradation nature, thereby absorbing energy, and serving as a binder for the other components. The second transformation phenomenon is the ablation of the char layer, composed of the carbonized resin and the remaining carbon fibers. This is promoted by heterogeneous chemical reactions, phase change and mechanical erosion, such as spallation, altogether leading to recession of the material.
Despite available flight data on the material performance during past missions, and efforts in material modeling13,14, prediction of the heat flux to the spacecraft remains a critical problem. Ground testing in plasma wind-tunnels is currently the only affordable option for qualification of the thermal protection material. Additionally, new multi-scale material response models are proposed in order to take into account the porous micro-structure of the new class of materials15,16. Those models require extensive experimental data for their development and validation.
The facilities in use for material characterization are most commonly arc-heated17-20 or induction coupled21,22 torches, which provide high gas enthalpies with air as test gas, ideal for the simulation of atmospheric reentry. The subsonic 1.2MW Inductively Coupled Plasma (ICP) torch of the Plasmatron facility at the von Karman Institute (VKI) is able to reproduce the aerothermodynamic environment of atmospheric entry in the stagnation point boundary layer of a test object for a wide range of pressures and heat fluxes23-25. An extensive numerical rebuilding procedure offers a detailed characterization of the boundary layer and extrapolation of ground-test data to real re-entry flight conditions based on the Local Heat Transfer Simulation (LHTS) concept26,27.
We present a procedure for material characterization on a porous carbon-fiber precursor in a well-characterized plasma gas environment representative of re-entry flight. The plasma freestream characterization is not part of this protocol but can be found elsewhere28. A comprehensive experimental setup of intrusive and non-intrusive techniques was integrated for in-situ analysis of the material exposed to the hot plasma flow. The results of those ablation experiments were already presented and widely discussed in another reference28. This protocol is meant to provide detailed information on the experimental techniques, their installation at the facility, and the procedures for data analysis. Target audiences of this publication are manifold: on the one hand, this publication is meant to provide a better insight into the experimental methods and procedures to improve the understanding of the facility&#39;s characteristics for material code developers and engineers of thermal protection materials. On the other hand, experimentalists of laboratories with similar facilities are addressed for data reproduction and comparison, and to extend the database of ablative material response to a wider heat-flux and pressure range.

<table border="0" cellpadding="0" cellspacing="0" width="765">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">Carbon-bonded carbon fiber</td>
			<td style="width:167px;"></td>
			<td style="width:175px;"></td>
			<td style="width:211px;">sample shape was a hemisphere of 25mm&#160;</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">&#160;preform</td>
			<td style="width:167px;">MERSEN (CALCARB)</td>
			<td style="width:175px;">CBCF 18-2000</td>
			<td>radius attached to a 25mm cylinder</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">UV-VIS-NIR Spectrometer</td>
			<td style="width:167px;">Ocean Optics&#160;</td>
			<td style="width:175px;">HR4000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">Optical fiber</td>
			<td style="width:167px;">Ocean Optics&#160;</td>
			<td style="width:175px;">&#160;QP600-2-SR/BX,</td>
			<td>modified fiber cladding for fixation</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">SpectraSuite</td>
			<td style="width:167px;">Ocean Optics&#160;</td>
			<td style="width:175px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">Lens, plano-convex</td>
			<td style="width:167px;">Ocean Optics&#160;</td>
			<td>LA4745, 750mm focal length</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:212px;">Two-color pyrometer</td>
			<td style="width:167px;">Raytek</td>
			<td>Marathon Series MR1SC</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:212px;">Digital Delay Generator</td>
			<td style="width:167px;">Stanford Research Systems</td>
			<td style="width:175px;">DG535</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:212px;">High-speed camera&#160;</td>
			<td style="width:167px;">Vision Research&#160;</td>
			<td style="width:175px;">Vision Research Phantom 7.1</td>
			<td></td>
		</tr>
	</tbody>
</table>

emission spectroscopic boundary layer investigation during ablative material testing in plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

The openly available bulk material was a highly porous carbon-bonded carbon fiber preform (CBCF), consisting of a short fiber insulation originating from rayon (cellulose fiber made from purified cellulose). The chopped, discontinuous virgin carbon fibers are interconnected in a matrix produced by the carbonization of phenolic resin. During this process the fibers become oriented and the microstructure and properties are anisotropic. The material is then vacuum-treated at temperatures above 2,300 K to ensure its temperature stability and the absence of outgassing. The material was machined in-house to hemispherical (HS) test samples of radius 25 mm with 50 mm in length. The samples have an initial density of about 180 kg/m3 with an initial porosity of 90%.
The VKI Plasmatron facility has been used for all the experiments for the reproduction of the aero-thermodynamic environment of re-entry plasma flows, creating a high-enthalpy, highly dissociated subsonic gas flow. The gas is heated by induction through a coil, creating a high purity plasma flow. An overview of the test chamber and a schematic of the experimental instrumentation for in-situ ablation measurements can be found in Fig. 1(a) and 1(b). Experimental test conditions and overall results, such as averaged recession rate obtained from HSC imaging and mass loss are listed in Table 1. We used a two-color pyrometer, employing a wide (0.75-1.1 &#181;m) and narrow (0.95-1.1 &#181;m) spectral band for the temperature determination at 1 Hz acquisition rate (1,300-3,300 K). Using two narrow wavelength bands and under the assumption of an emissivity being independent of the wavelength, the surface temperature can be estimated without knowledge of its emissivity. The pyrometer was pointed and focused in the stagnation area of the sample through a 1 cm thick quartz window, at an angle of 35&#176; with respect to the stagnation line. The instrument was calibrated up to 3,300 K by a black body source.
The surface recession was measured by the HSC with a resolution of 0.2 mm. It is evident that caliper rule recession measurements generally resulted in larger values than those performed by HSC imaging, with a difference in total recession between the two methods ranging from 0.45 to 0.9 mm. The highest uncertainty for this measurement was introduced by compressing the brittle char layer with the caliper rule. Recession rates in air varied between 44.6 and 58.4 &#181;m/sec. It is furthermore apparent that HSC-determined recession rates in air plasma did not differ much, probably due to a diffusion-controlled ablation regime. In this regime, the surface temperature is high enough to cause complete consumption of the available oxygen at the surface, and consequently, ablation is restricted by the diffusion of oxygen through the boundary layer32,33. Conversely, in an oxidation reaction controlled environment, oxygen diffuses faster through a boundary layer than it is consumed at the surface and ablation increases with surface temperature. Recession rates of the CBCF material in high-enthalpy environments are also reported by MacDonald et al. (56 &#181;m/sec)22 and L&#246;hle et al. (50 &#181;m/sec)34. Those values lie between our measurements, although MacDonald et al. used a cylindrical test sample shape and L&#246;hle et al. a test sample embedded in a water-cooled probe.
Three low-resolution spectrometers were used for observation of the gas-phase. Advantage of this instrument is a fast scanning of a wide spectral range (200 - 1,000 nm) that allows for detection of multiple molecules and atoms, present in ablation analysis.
Integrated CN emission intensities, plotted over distance from the ablating surface show very good agreement with respect to each other (Fig. 2). The data are labeled according to their respective positions from the sample surface with &#39;close&#39;, &#39;middle&#39;, and &#39;far&#39;. The three spectrometers measured the same CN violet emission intensity once the fixed optical path collected light from the same distance in front of the surface. The integrated intensities of all three spectrometers almost coincide 3.4 mm before the ablating surface. Both cases show that the recorded CN violet emission peaked just in front of the test sample, before decreasing through the boundary layer. From those results we deduce that the material burn-off in air during the whole test time was very stable, and that the recorded emission signal dropped about 90% within 5 mm frontal of the surface. CN violet experimental spectra were then used for comparison to simulated spectra in order to obtain gas temperatures. The synthetic spectra were obtained using SPECAIR 2.2, assuming a Boltzmann distribution of excited levels and a least-squares fitting procedure was applied to estimate translational-rotational temperatures Trot and vibrational-electronic temperatures Tvib (Fig. 3). Two conditions, at low (a) and high (b) pressure are presented, with the spectra taken close to the wall in the boundary layer. The estimated temperatures yielded a high deviation from thermal equilibrium at low pressure (Fig. 3(a)). The same analysis was performed for several distances from the surface, better illustrating the deviation from thermal equilibrium close to the wall at low pressure (Fig. 4(a), 15 hPa), equilibrating through the boundary layer. The retrieved temperatures were in the order of 8,200 K for Trot and 21,000 K for Tvib close to the wall, with Tvib decreasing towards 8,200 K through the boundary layer. This is in contrast to the equilibrium condition throughout the boundary layer at higher pressure (Fig. 4(b), 200 hPa). The temperature bounds were based on an uncertainty of 10% on the spectrometer emission intensity, allowing a theoretical spectrum variation within those limits for the fitting procedure.
At low pressure, excitation transfer between molecules is reduced due to fewer collisions, which may explain the equilibrating effect towards the boundary layer edge. We assume a strong influence of molecular nitrogen at low plasma enthalpies on CN production, followed by vibrational excitation of CN. Dissociative adsorption of highly vibrationally excited nitrogen is assumed to create reactive sites at the surface that lead to CN production. Boubert and Vervisch describe this process in a nitrogen/carbon-dioxide plasma at low pressure35. This process may create a pool of nitrogen atoms at the surface, with exothermic reactions leading to excess energy being converted into rotational and vibrational excitation of CN.
Micrographs proved that carbon oxidation in air plasma led to an icicle shape of the ablated fibers with an oxidation depth of around 0.2 mm (Fig. 5(a)). This kind of icicle shaping due to ablation is widely reported in literature for carbon-carbon composite materials36-38. The icicle shape (opening angle) depends on the reaction-diffusion competition at the surface of the porous material, and hence, varies with oxygen diffusion. This length is assumed to correspond to the average depth of oxygen diffusion. The icicle shape additionally confirms diffusion-controlled ablation. In contrast, reaction limited ablation would allow oxygen to float into the deeper fiber structure, producing local pitting of the carbon fibers.
Bright sparking was observed during some ablation tests (Fig. 5(b)), which might be caused by hot fiber clusters detaching from the surface. Ablation in nitrogen plasma led to highly degraded fibers along their surface, which led to a slow recession of the material by nitridation (Fig. 5(c)). As the reactivity of carbon to nitrogen is much lower than that to oxygen, nitrogen is able to diffuse deeper into the material, leading to degradation along the whole fiber.
<img alt="Figure 1" src="/files/ftp_upload/53742/53742fig1.jpg" /> 
Figure 1. Plasmatron and experimental setup overview. (a) VKI Plasmatron test chamber overview indicating test sample outside the retention system, heat flux and pressure probes, and optical accesses for radiometers, HSC, and spectrometer optics. (b) Schematic of the experimental setup. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53742/53742fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Table1" src="/files/ftp_upload/53742/53742table1.jpg" /> 
Table 1. Plasmatron test conditions and experimental results of carbon preform samples. Test case reference, test gas, static pressure ps, dynamic pressure pd, generator power P, mean cold wall heat flux qcw, test sample exposure time &#964;, mean surface temperature Ts, recession rate r/&#964;, and mass loss rate m/&#964;.
<img alt="Figure 2" src="/files/ftp_upload/53742/53742fig2.jpg" /> 
Figure 2. Spatial CN violet emission in boundary layer. Emission profiles recorded by three adjacent spectrometers during preform ablation in air coincide well when the fixed optical paths were collecting light from the same distance in front of the ablating surface: stable material burn-off, and reactive boundary layer size ~5 mm frontal of the surface (condition A1a). <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53742/53742fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 3" src="/files/ftp_upload/53742/53742fig3.jpg" /> 
Figure 3. CN violet temperatures estimated from spectral fitting method. Least-squares method for best fitting of CN violet spectra computed with SPECAIR 2.2 provided translational-rotational and vibrational-electronic temperatures Trot and Tvib: (a) Condition A1a: Trot = 8,240 K &#177; 400 K, Tvib = 21,600 K &#177; 1,700 K, TLTE = 12,600 K &#177; 500 K (equilibrium simulation TLTE indicated for comparison); (b) Condition A1a: Trot = 6,880 K &#177; 200 K, Tvib = 7,120 K &#177; 180 K. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53742/53742fig3large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 4" src="/files/ftp_upload/53742/53742fig4.jpg" /> 
Figure 4. CN violet temperature profiles in boundary layer. Translational-rotational and vibrational-electronic temperatures Trot and Tvib from simulated, fitted CN violet spectra computed with a radiation simulation tool at four distances from the ablating surface suggest deviation from a thermal equilibrium condition close to the wall at a low pressure of 15 hPa (a) but present equilibrium throughout the boundary layer at 200 hPa (b). The temperature bounds [K] were based on an uncertainty of 10% on the spectrometer emission intensity, allowing a theoretical spectrum variation within those limits for the fitting procedure. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53742/53742fig4large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<img alt="Figure 5" src="/files/ftp_upload/53742/53742fig5.jpg" /> 
Figure 5. Scanning Electron Micrographs after air ablation (a), including in-situ photograph (b) and micrographs after nitrogen ablation (c). (a) Post air-ablation micrographs taken at frontal surface close to stagnation point present thinning of carbon fibers due to oxidation from fiber tip, leading to icicle shape, the depth of oxygen diffusion is close to 200 &#181;m (diffusion limited ablation); (b) Photograph taken during ablation test of a cylindrical test sample (exposure time: 1/200 sec) illustrates bright sparking; (c) Strong corrosion was observed in nitrogen along whole fiber length. <a href="https://www-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/53742/53742fig5large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>

Watch this Scientific Journal Video about Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron at JoVE.com

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

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12.3K Views.  von Karman Institute for Fluid Dynamics. Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Video: Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Characterization of Full Set Material Constants and Their Temperature Dependence for Piezoelectric Materials Using Resonant Ultrasound Spectroscopy

During the operation of high power electromechanical devices, a temperature rise is unavoidable due to mechanical and electrical losses, causing the degradation of device performance. In order to evaluate such degradations using computer simulations, full matrix material properties at elevated temperatures are needed as inputs. It is extremely difficult to measure such data for ferroelectric materials due to their strong anisotropic nature and property variation among samples of different geometries. Because the degree of depolarization is boundary condition dependent, data obtained by the IEEE (Institute of Electrical and Electronics Engineers) impedance resonance technique, which requires several samples with drastically different geometries, usually lack self-consistency. The resonant ultrasound spectroscopy (RUS) technique allows the full set material constants to be measured using only one sample, which can eliminate errors caused by sample to sample variation. A detailed RUS procedure is demonstrated here using a lead zirconate titanate (PZT-4) piezoceramic sample. In the example, the complete set of material constants was measured from room temperature to 120 &#176;C. Measured free dielectric constants <img alt="Equation 1" src="/files/ftp_upload/53461/image001.jpg" /> and&#160;<img alt="Equation 2" src="/files/ftp_upload/53461/image002.jpg" /> were compared with calculated ones based on the measured full set data, and piezoelectric constants d15 and d33 were also calculated using different formulas. Excellent agreement was found in the entire range of temperatures, which confirmed the self-consistency of the data set obtained by the RUS.

This protocol describes the procedure of measuring the temperature dependence of the full set material constants of piezoelectric materials using resonant ultrasound spectroscopy (RUS).

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Experimental Methods for Investigation of Shape Memory Based Elastocaloric Cooling Processes and Model Validation

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor compression based cooling process. Nickel-Titanium (Ni-Ti) based alloy systems, especially, show large elastocaloric effects. Furthermore, exhibit large latent heats which is a necessary material property for the development of an efficient solid-state based cooling process. A scientific test rig has been designed to investigate these processes and the elastocaloric effects in SMAs. The realized test rig enables independent control of an SMA&#39;s mechanical loading and unloading cycles, as well as conductive heat transfer between SMA cooling elements and a heat source/sink. The test rig is equipped with a comprehensive monitoring system capable of synchronized measurements of mechanical and thermal parameters. In addition to determining the process-dependent mechanical work, the system also enables measurement of thermal caloric aspects of the elastocaloric cooling effect through use of a high-performance infrared camera. This combination is of particular interest, because it allows illustrations of localization and rate effects &#8212; both important for efficient heat transfer from the medium to be cooled.
The work presented describes an experimental method to identify elastocaloric material properties in different materials and sample geometries. Furthermore, the test rig is used to investigate different cooling process variations. The introduced analysis methods enable a differentiated consideration of material, process and related boundary condition influences on the process efficiency. The comparison of the experimental data with the simulation results (of a thermomechanically coupled finite element model) allows for better understanding of the underlying physics of the elastocaloric effect. In addition, the experimental results, as well as the findings based on the simulation results, are used to improve the material properties.

Experimental methods for investigation of solid state cooling processes and characterization of elastocaloric material properties of Shape Memory Alloys (SMA) are presented. A custom-built test rig has been designed for controlling and comprehensive monitoring of elastocaloric cooling processes. Furthermore, it provides a validation platform for thermomechanically coupled modeling approaches.

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Experimental Methodology for Estimation of Local Heat Fluxes and Burning Rates in Steady Laminar Boundary Layer Diffusion Flames

Modeling the realistic burning behavior of condensed-phase fuels has remained out of reach, in part because of an inability to resolve the complex interactions occurring at the interface between gas-phase flames and condensed-phase fuels. The current research provides a technique to explore the dynamic relationship between a combustible condensed fuel surface and gas-phase flames in laminar boundary layers. Experiments have previously been conducted in both forced and free convective environments over both solid and liquid fuels. A unique methodology, based on the Reynolds Analogy, was used to estimate local mass burning rates and flame heat fluxes for these laminar boundary layer diffusion flames utilizing local temperature gradients at the fuel surface. Local mass burning rates and convective and radiative heat feedback from the flames were measured in both the pyrolysis and plume regions by using temperature gradients mapped near the wall by a two-axis traverse system. These experiments are time-consuming and can be challenging to design as the condensed fuel surface burns steadily for only a limited period of time following ignition. The temperature profiles near the fuel surface need to be mapped during steady burning of a condensed fuel surface at a very high spatial resolution in order to capture reasonable estimates of local temperature gradients. Careful corrections for radiative heat losses from the thermocouples are also essential for accurate measurements. For these reasons, the whole experimental setup needs to be automated with a computer-controlled traverse mechanism, eliminating most errors due to positioning of a micro-thermocouple. An outline of steps to reproducibly capture near-wall temperature gradients and use them to assess local burning rates and heat fluxes is provided.

We describe the use of micro-thermocouples to estimate local temperature gradients in steady laminar boundary layer diffusion flames. By extension of the Reynolds Analogy, local temperature gradients can be further used to estimate the local mass burning rates and heat fluxes in such flames with high accuracy.

Modeling the realistic burning behavior of condensed-phase fuels has remained out of reach, in part because of an inability to resolve the complex ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

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Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering thermal wave fields that are disturbed by the defect. This effect is measured and used to locate the defect. We form the destructively interfering wave fields by using a modified projector. The original light engine of the projector is replaced with a fiber-coupled high-power diode laser. Its beam is shaped and aligned to the projector&#39;s spatial light modulator and optimized for optimal optical throughput and homogeneous projection by first characterizing the beam profile, and, second, correcting it mechanically and numerically. A high-performance infrared (IR) camera is set up according to the tight geometrical situation (including corrections of the geometrical image distortions) and the requirement to detect weak temperature oscillations at the sample surface. Data acquisition can be performed once a synchronization between the individual thermal wave field sources, the scanning stage, and the IR camera is established by using a dedicated experimental setup which needs to be tuned to the specific material being investigated. During data post-processing, the relevant information on the presence of a defect below the surface of the sample is extracted. It is retrieved from the oscillating part of the acquired thermal radiation coming from the so-called depletion line of the sample surface. The exact location of the defect is deduced from the analysis of the spatial-temporal shape of these oscillations in a final step. The method is reference-free and very sensitive to changes within the thermal wave field. So far, the method has been tested with steel samples but is applicable to different materials as well, in particular to temperature sensitive materials.

This method aims at locating vertical subsurface defects. Here, we couple a laser with a spatial light modulator and trigger its video input to heat a sample surface deterministically with two anti-phased modulated lines while acquiring highly resolved thermal images. The defect position is retrieved from evaluating thermal wave interference minima.

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering ...

Ultrasonic Fatigue Testing in the Tension-Compression Mode

Ultrasonic fatigue testing is one of a few methods which allow investigating fatigue properties in the ultra-high cycle region. The method is based on exposing the specimen to longitudinal vibrations on its resonance frequency close to 20 kHz. With use of this method, it is possible to significantly decrease the time required for the test, when compared to conventional testing devices usually working at frequencies under 200 Hz. It is also used to simulate loading of material during operation in high speed conditions, such as those experienced by components of jet engines or car turbo pumps. It is necessary to operate only in the high and ultra-high cycle region, due to the possibility of extremely high deformation rates, which can have a significant influence on the test results. Specimen shape and dimensions have to be carefully selected and calculated to fulfill the resonance condition of the ultrasonic system; thus, it is not possible to test the full components or specimens of arbitrary shape. Before each test, it is necessary to harmonize the specimen with the frequency of the ultrasonic system to compensate for deviations of the real shape from the ideal one. It is not possible to run a test until a total fracture of the specimen, since the test is automatically terminated after initiation and propagation of the crack to a certain length, when the stiffness of the system changes enough to shift the system out of the resonance frequency. This manuscript describes the process of evaluation of materials' fatigue properties at high-frequency ultrasonic fatigue loading with use of mechanical resonance at a frequency close to 20 kHz. The protocol includes a detailed description of all steps required for a correct test, including specimen design, stress calculation, harmonizing with the resonance frequency, performing the test, and final static fracture.

A protocol for ultrasonic fatigue testing in the high and ultra-high cycle region in axial tension-compression loading mode.

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Fabrication of an Optical Cell Dryer for the Spectroscopic Analysis Cells

Optical cells, which are experimental instruments, are small, square tubes sealed on one side. A sample is placed in this tube, and a measurement is performed with a spectroscope. The materials used for optical cells generally include quartz glass or plastic, but expensive quartz glass is reused by removing substances, other than liquids, to be analyzed that adhere to the interior of the container. In such a case, the optical cells are washed with water or ethanol and dried. Then, the next sample is added and measured. Optical cells are dried naturally or with a manual hairdryer. However, drying takes time, which makes it one of the factors that increase the experiment time. In this study, the objective is to drastically reduce the drying time with a dedicated automatic dryer that can dry multiple optical cells at once. To realize this, a circuit was designed for a microcomputer, and the hardware using it was independently designed and manufactured.

A protocol for fabricating a device for simultaneously drying multiple optical cells is presented.

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Cutting Procedures, Tensile Testing, and Ageing of Flexible Unidirectional Composite Laminates

Many body armor designs incorporate unidirectional (UD) laminates. UD laminates are constructed of thin (&#60;0.05 mm) layers of high-performance yarns, where the yarns in each layer are oriented parallel to each other and held in place using binder resins and thin polymer films. The armor is constructed by stacking the unidirectional layers in different orientations. To date, only very preliminary work has been performed to characterize the ageing of the binder resins used in unidirectional laminates and the effects on their performance. For example, during the development of the conditioning protocol used in the National Institute of Justice Standard-0101.06, UD laminates showed visual signs of delamination and reductions in V50, which is the velocity at which half of the projectiles are expected to perforate the armor, after ageing. A better understanding of the material property changes in UD laminates is necessary to comprehend the long-term performance of armors constructed from these materials. There are no current standards recommended for mechanically interrogating unidirectional (UD) laminate materials. This study explores methods and best practices for accurately testing the mechanical properties of these materials and proposes a new test methodology for these materials. Best practices for ageing these materials are also described.

The goal of the study was to develop protocols to prepare consistent specimens for accurate mechanical testing of high-strength aramid or ultra-high-molar-mass polyethylene-based flexible unidirectional composite laminate materials and to describe protocols for performing artificial ageing on these materials.

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Carrier Lifetime Measurements in Semiconductors through the Microwave Photoconductivity Decay Method

This work presents a protocol employing the microwave photoconductivity decay (&#956;-PCD) for measurement of the carrier lifetime in semiconductor materials, especially SiC. In principle, excess carriers in the semiconductor generated via excitation recombine with time and, subsequently, return to the equilibrium state. The time constant of this recombination is known as the carrier lifetime, an important parameter in semiconductor materials and devices that requires a noncontact and nondestructive measurement ideally achieved by the &#956;-PCD. During irradiation of a sample, a part of the microwave is reflected by the semiconductor sample. Microwave reflectance depends on the sample conductivity, which is attributed to the carriers. Therefore, the time decay of excess carriers can be observed through detection of the reflected microwave intensity, whose decay curve can be analyzed for estimation of the carrier lifetime. Results confirm the suitability of the &#956;-PCD protocol in measuring the carrier lifetime in semiconductor materials and devices.

As one of the important physical parameters in semiconductors, carrier lifetime is measured herein via a protocol employing the microwave photoconductivity decay method.

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Intermediate Strain Rate Material Characterization with Digital Image Correlation

The mechanical response of a material under dynamic load is typically different than its behavior under static conditions; therefore, the common quasistatic equipment and procedures used for material characterization are not applicable for materials under dynamic loads. The dynamic response of a material depends on its deformation rate and is broadly categorized into high (i.e., greater than 200/s), intermediate (i.e., 10&#8722;200/s) and low strain rate regimes (i.e., below 10/s). Each of these regimes calls for specific facilities and testing protocols to ensure the reliability of the acquired data. Due to the limited access to high-speed servo-hydraulic facilities and validated testing protocols, there is a noticeable gap in the results at the intermediate strain rate. The current manuscript presents a validated protocol for the characterization of different materials at these intermediate strain rates. Strain gauge instrumentation and digital image correlation protocols are also included as complimentary modules to extract the utmost level of detailed data from every single test. Examples of raw data, obtained from a variety of materials and test setups (e.g., tensile and shear) is presented and the analysis procedure used to process the output data is described. Finally, the challenges of dynamic characterization using the current protocol, along with the limitations of the facility and methods of overcoming potential problems are discussed.

Here we present a methodology for the dynamic characterization of tensile specimens at intermediate strain rates using a high-speed servo-hydraulic load frame. Procedures for strain gauge instrumentation and analysis, as well as for digital image correlation strain measurements on the specimens, are also defined.