The authors would like to acknowledge the support of the DFG priority program 1599 &#34;Caloric effects in ferroic materials: New concepts for cooling&#34;&#160;(Projects: EG101/23-1, SCHU2217/2-1, SE704/2-1, EG101/29-2, SCH2217/3-2, SE704/2-2).&#160;

1. Sample Preparation

<ol>
	<li>Measure the SMA ribbon with calipers and determine the&#160;cross section of the sample.</li>
	<li>Prepare the sample for IR measurements by coating the ribbon with a thin layer of high emissivity (&#949;=0.96) paint. 
	Caution: The paint is classified as an irritant. Gloves, safety glasses and mouth protection must be worn during the processing of the paint.</li>
</ol>
2. Material Stabilization (Training)
Note: Initial mechanical cycling leads to a mechanical and thermal material stabilization. The investigation of the stabilization effect, and the training procedure itself, requires the use of the actuator and the sensors mounted in the upper level of the test rig as well as the IR camera.
<ol>
	<li>Start motor controller program and check the loaded settings. Change the settings to position mode and command mode. Verify the motor is in active mode.</li>
	<li>Set the target position in the motor controller program to 0 &#181;m and click on the &#34;operation enable&#34; button &#8212; at this position the distance between the clamps is 90 mm.</li>
	<li>Place the sample between clamps of the experimental setup and use a special designed alignment tool to align the sample.</li>
	<li>Tighten clamps using a mounting aid in order to avoid bending load on load cell and sample. Use a torque wrench for tightening the screws to ensure a reproducible clamping force (tightening torque: 20 Nm).</li>
	<li>Check current motor position and make sure that the motor is at start position (0 &#181;m).</li>
	<li>Start the IR camera software and load the calibration for a 50 mm lens combined with a close-up lens. Choose an image size of 1,280 x 100 pixels and a temperature range of -20 &#176;C to 50 &#176;C. Position the camera by using the motor focus unit and confirm the whole sample is in the field of view of the camera. 
	Note: The IR camera, in combination with the chosen lens system, has a focal length (f) of 50 mm, an aperture of f/2 and a minimum pixel size of 60 &#181;m at a working distance of 200 mm.</li>
	<li>Open the control program for training and material characterization and set the control parameters (displacement, velocity, holding time, maximum and minimum force, number of cycles and camera frame rate).
	<ol>
		<li>Set the start position (0 &#181;m) and choose the target position (4,500 &#181;m) so that the material undergoes a complete phase transformation.</li>
		<li>Set the linear direct drive velocity (velocity loading/ unloading) to meet the desired strain rate. Select a strain rate of 5 x 10-4 sec-1 (actuator velocity of 45 &#181;m/sec) for cooling process related training.
		<ol>
			<li>Determine the linear direct drive velocity (v) based on the chosen strain rate (<img alt="epsilon" src="/files/ftp_upload/53626/epsilon.jpg" />) and the initial sample length (l0) of 90 mm (v = <img alt="epsilon" src="/files/ftp_upload/53626/epsilon.jpg" />&#8729;l0)</li>
		</ol>
		</li>
		<li>Set the holding time to 0 sec.</li>
		<li>Set the number of cycles to 1 for the first cycle with a new sample.</li>
		<li>Set the sample-specific minimum and maximum force level to avoid compressive load and tensile overload (minimum load 1 MPa, maximum load 800 MPa).</li>
		<li>Choose an IR camera acquisition rate of 50&#160;msec/frame (20&#160;frames per second).</li>
		<li>Click on the start button to load the settings.</li>
	</ol>
	</li>
	<li>Open the IR camera software, choose a file name and allocate 5,000&#160;frames.
	<ol>
		<li>Switch from internal to external trigger source and start the data acquisition mode.</li>
	</ol>
	</li>
	<li>Open the control program and press the start experiment button.</li>
	<li>Data visualization
	<ol>
		<li>Once the experiment is finished, load the data into the data processing software and visualize it in terms of force/displacement, stress/strain, force/time and position/time diagrams.</li>
		<li>Load the IR data into the IR camera software and evaluate the time resolved temperature profiles. Define a measurement area which covers the surface of the SMA ribbon and plot the mean maximum and minimum temperature of the sample vs. time.</li>
	</ol>
	</li>
	<li>Repeat steps 2.6 to 2.9 until the material shows stable mechanical behavior and adapt the start position to compensate for residual strains.
	<ol>
		<li>After the first 10 cycles, increase the number of cycles per experiment to 10 and proceed with the experiments until stable material behavior is reached.</li>
	</ol>
	</li>
</ol>
3. Material Characterization
Note: The material characterization requires the use of the actuator and the sensors mounted in the upper level of the test rig as well as the IR camera. During the characterization procedure the sample is loaded and unloaded at different rates while performing a holding period after loading and unloading.
<ol>
	<li>If the SMA ribbon has been unclamped and the control system of the test rig has been switched off after the training, repeat steps 2.1 to 2.6 and clamp the sample again. If this was not the case, proceed as follows.</li>
	<li>Open the control program for training and material characterization and set the control parameters (displacement, velocity, holding time, number of cycles and camera frame rate).
	<ol>
		<li>Set the start position so that the sample is under zero load and set the target position equivalent to the target position of the training (4,500 &#181;m).</li>
		<li>Set the linear direct drive velocity (velocity loading/unloading) to meet the desired strain rate. Choose a strain rate of 1 x 10-1 sec-1 (actuator velocity of 9,000 &#181;m/sec) which leads to an adiabatic phase transformation for samples with a cross section of 0.75 mm x 1.4 mm or larger.</li>
		<li>Set the holding time to 180 sec, which is sufficient for the sample to reach the initial temperature level. 
		Note: The holding time has to be verified after the experiment by calculating a thermal equilibration time constant (&#964;) and a holding time smaller than 4 x &#964; has to be increased before the next characterization experiment starts.</li>
		<li>Set the number of cycles to 1.</li>
		<li>Set the sample-specific minimum and maximum force level to avoid compressive load and tensile overload (minimum load 1 MPa, maximum load 800 MPa).</li>
		<li>Choose an IR camera acquisition rate of 5&#160;msec/frame (200 frames per second).</li>
		<li>Click on the start button to load the settings.</li>
	</ol>
	</li>
	<li>Open the IR camera software, choose a file name and allocate 80,000 frames.
	<ol>
		<li>Switch from internal to external trigger source and start the data acquisition mode.</li>
	</ol>
	</li>
	<li>Open the control program and press the start experiment button.</li>
	<li>Load the IR data into the IR camera software. Plot mean maximum and minimum sample temperatures vs. time. Export the data and calculate the thermal equilibration time constant with the data processing software 10,11.</li>
	<li>Adapt the holding time, if necessary, based on the calculated thermal equilibration time constant.</li>
	<li>Repeat steps 3.2 to 3.5 and vary the strain rate from 5 x 10-5 sec-1 to 1 x 10-1 sec-1, as well as the strain from 2% to a maximum strain of 5% (maximum strain is equivalent to the maximum strain during training).</li>
	<li>Investigation of local temperature peaks: 
	Note: The material shows a rate-dependent localization effect of the elastocaloric effect. Careful study of these effects requires a high special resolution of the SMA temperature profile. For this purpose, the lens of the IR Camera has to be replaced by a microscope lens. The microscope lens has an aperture of 3.0, a magnification of 1X and a pixel size of 15 &#181;m at a working distance of 195 mm.
	<ol>
		<li>Switch the light off, remove all heat sources from the field of view of the IR camera and change the lens.</li>
		<li>Change the camera calibration settings and load a microscope lens calibration within the temperature range of 20 &#176;C to 50 &#176;C and an image size of 500 x 250 pixels. Use the motor focus unit to focus the sample.</li>
		<li>Perform a tensile test at a strain rate of 1&#160;x 10-1&#160;sec-1 (9,000&#160;&#956;m/sec), follow the steps described in section 2: Material stabilization.</li>
	</ol>
	</li>
	<li>Data Visualization
	<ol>
		<li>Load the mechanical data into the data processing software and visualize it in terms of force/displacement, stress/strain, force/time and position/time diagrams.</li>
		<li>Load the IR data into the IR camera software and evaluate the time resolved temperature profiles. Define a measurement area which covers the surface of the SMA ribbon and plot the mean maximum and minimum temperature of the sample vs. time.</li>
	</ol>
	</li>
</ol>
4. Elastocaloric Cooling Process
Note: The investigation of elastocaloric cooling processes requires the use of actuators and sensors in the upper and lower level of the setup as well as the IR camera. These experiments include a variation of the control parameters in order to optimize the process performance.
<ol>
	<li>If the SMA ribbon has been unclamped and the test rig has been switched off after the material characterization, repeat steps 2.1 to 2.5 and clamp the sample again. If this was not the case, proceed as follows.</li>
	<li>Start the IR camera software and load the calibration for the 50 mm lens with close-up lens. Choose an image size of 1,280 x 1,024 pixels and a temperature range of -20 &#176;C to 50 &#176;C. Position the camera by using the motor focus unit and make sure that the entire sample is in the field of view of the camera. 
	Note: The IR camera in combination with the chosen lens system has a focal length (f) of 50 mm, an aperture of f/2 and a minimum pixel size of 60 &#181;m at a working distance of 200 mm.</li>
	<li>Open the control program for elastocaloric cooling processes and set the control parameters (displacement of linear direct drive one (upper level), velocity of linear direct drive one and two, contact time, maximum and minimum force, contact phase, number of cycles and camera frame rate).
	<ol>
		<li>Set the start position of the linear direct drive for SMA loading and unloading, so that the sample is under zero load and set the target position equivalent to the target position of the training (4,500 &#181;m).</li>
		<li>Set the velocity (velocity loading/unloading) of the linear direct drive for loading and unloading of the SMA to meet a strain rate of 1 x 10-1 sec-1 (9,000 &#181;m/sec). Set the velocity of the linear direct drive in the lower level of the setup to 100 mm/sec.</li>
		<li>Set the contact time to 6 sec. 
		Note: The contact time determines the duration of the heat transfer and can be set to any value above 10 msec.</li>
		<li>Choose the contact after loading/unloading mode. 
		Note: The contact phase influences whether the loading and unloading is adiabatic (contact after loading/unloading) or combined with a heat transfer to the heat sink/source (contact during loading/unloading).</li>
		<li>Set the number of cycles to 40.</li>
		<li>Set the sample-specific minimum and maximum force level to avoid compressive load and tensile overload (minimum load 1 MPa, maximum load 800 MPa).</li>
		<li>Choose an IR camera acquisition rate of 20 msec/frame (50 frames per second). Click on the start button to load the settings.</li>
	</ol>
	</li>
	<li>Open the IR camera software, choose a file name and allocate 50000 frames. Switch from internal to external trigger source and start the data acquisition mode.</li>
	<li>Open the control program and press the start experiment button.</li>
	<li>Data visualization
	<ol>
		<li>Once the experiment is finished load the data into the data processing software and visualize the following data: force/displacement, stress/strain, temperature/time (temperature of the heat sink/source), force/time, contact force/ time and position of the linear actuators/time.</li>
		<li>Load the IR data into the IR camera software and evaluate the time resolved temperature profiles. Define three measurement areas which cover the surface of the SMA sample as well as the surface of the heat sink and the heat source. Export the time resolved mean, maximum and minimum temperature data of the defined measurement areas and load them into the data processing software.</li>
		<li>Visualize the IR data in a temperature/time diagram.</li>
	</ol>
	</li>
	<li>Repeat the experiment under variation of the parameters: strain, contact time and contact phase.</li>
</ol>
5. Model Validation
Note: The validation of thermo-mechanically coupled material models requires experiments adhering to material stabilization or material characterization. Use a Ni-Ti wire with a cross section of 0.6 mm to perform the experimental investigations.
<ol>
	<li>Perform an isothermal tensile test at a strain rate of 5 x 10-5 sec-1 and a strain of 5%, proceed by performing the steps described in Section 2.</li>
	<li>Once the experiment is finished, load the data into the data processing software and visualize the stress/strain measurement. Calculate the elastic modulus of the austenite and the martensite phase, the transformation strain as well as the width of the hysteresis. The aforementioned data function as mechanical input data for the model 7.</li>
	<li>Perform further tensile tests at strain rates of 1 x 10-4 sec-1, 5 x 10-4 sec-1, 1 x 10-3 sec-1, 5 x 10-3 sec-1, 1 x 10-2 sec-1, 5 x 10-2 sec-1, 1 x 10-1 sec-1 to generate validation data for the model.</li>
	<li>If the experiments are completed take the sample out of the test system and perform a differential scanning calorimetric measurement (DSC) 18 to determine the caloric material properties (latent heats of the phase transformation and specific heat capacity of the material) of the stabilized material. 
	Note: The DSC measurements provide caloric input data for the thermo-mechanically coupled model.</li>
	<li>Start the simulation of the tensile tests described in step 5.3.
	<ol>
		<li>Implement custom model for shape memory alloys into commercially available finite element software:
		<ol>
			<li>Select Geometry node and choose Interval to draw 1D wire geometry.</li>
			<li>Select Parameters node to define model parameters identified from mechanical tests in step 5.2.</li>
			<li>Right-click Definitions node and select Variables to create a Variables node. Select Variables node and define algorithm for determining the transition probabilities derived from statistical thermodynamics 19.</li>
			<li>Select Add Physics and add Coefficient Form PDE or General Form PDE to define set of one-dimensional partial differential equations describing the behavior of superelastic Shape Memory Alloy, consisting of the stationary momentum balance, the balance of internal energy and kinetic equations of phase transformation 20.</li>
		</ol>
		</li>
		<li>Select Initial Values sub-node to set the initial temperature of the wire to the environment temperature.
		<ol>
			<li>Select Dirichlet Boundary Condition to prescribe mechanical boundary conditions for applying a strain following the experimental procedure described in section 2, for the strain-rates in step 5.3, constraining the displacement of one end of the wire and prescribing the displacement of the other end.</li>
			<li>Select Dirichlet Boundary Condition to set thermal boundary conditions to constant temperature because of the massive clamps compared to the thin wire. 
			Note: Standard settings of the finite element software do not lead to a converging solution.</li>
			<li>Select sub-nodes of Solver Configuration to modify standard settings (e.g., absolute and relative tolerances and damping coefficient of the nonlinear, iterative Newton-Raphson solver) and click &#34;Compute&#34; to run solver.</li>
		</ol>
		</li>
	</ol>
	</li>
	<li>Data Analysis
	<ol>
		<li>Load the experimental and simulation results into the data analysis software and visualize the mechanical and thermal data.</li>
		<li>Compare the experimental and simulation results, respective mechanical (stress/strain response) and thermal (special resolved temperature evolution of the sample) material behavior.</li>
	</ol>
	</li>
</ol>

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The authors have nothing to disclose.

The presented scientific test rig enables comprehensive investigation of elastocaloric materials and cooling processes by performing the experiments described in the protocol section. Precise alignment of the sample before clamping is crucial for all the experiments. Bad alignment can potentially lead to early material failure. Furthermore, the maximum applied strain has significant influence on the material lifetime, whereas the required strain to reach a complete phase transformation depends on the alloy composition. T...

Solid state cooling processes based on ferroic materials have potential to be environmentally friendly alternatives to the conventional vapor compression based process. Ferroic materials may exhibit magnetocaloric, electrocaloric and elastocaloric effects 1,2, as well as combinations of these effects, which are described as multicaloric material behavior 3. The different caloric effects in ferroic materials are currently being investigated as part of the German Science Foundation (DFG) Priority program SPP 1599 &#34;Caloric Effects in Ferroic Materials: New Concepts for Cooling&#34; 4. Shape Memory Alloys (SMA) which are investigated within this program show large elastocaloric effects, in particular Ni-Ti based alloys due to their large latent heats 5. The strain-induced phase transformation at high strain rates leads to significant temperature changes of the SMA, as shown in Figure 1. The adiabatic, exothermic phase transformation from austenite to martensite increases the SMA temperature. The endothermic transformation from martensite to austenite leads to a significant temperature decrease. These elastocaloric material properties can be used for solid-state cooling processes by applying a suitable mechanical loading and unloading cycle. Figure 2 shows a typical elastocaloric cooling cycle, following the Brayton cycle. The heat transfer between the heat source and the cold, unloaded SMA take place at low temperature levels. In the next phase, the SMA is in a contact-free state and the fast, adiabatic loading leads to a significant temperature increase of the SMA. The subsequent heat transfer between the hot SMA and the heat sink take place at constant strain of the SMA. Upon completion of the heat transfer, fast, adiabatic unloading leads to a significant temperature drop of the SMA below the temperature of the heat source, whereupon the next cooling cycle and the heat transfer with the heat source can start. The efficiency of the elastocaloric cooling process depends on the required mechanical work and the absorbed heat.
First, experiments monitoring the temperature field during tensile tests were performed by Shaw et al. 6,7, with the objective to investigate the formation of local temperature peaks during tensile tests of SMA strips and wires at different rates. The applied experimental method combined the measurement of the mechanical parameters (stress, strain and strain rate) with simultaneous acquisition of temperature fields by means of thermographic measurements. During loading and unloading of a SMA specimen with a tensile testing machine, an infrared (IR) camera was used to acquire IR images of the SMA sample. This technique enables the investigation of the strain rate dependent formation of temperature peaks. The measurement of the temperature distribution on the sample is very important for the investigation of the elastocaloric effects and the determination of the cooling properties of the material. A local temperature measurement &#8212; by applying a contacting temperature measurement &#8212; is not sufficient in order to characterize the cooling properties of the material. A measurement of the temperature field was also used by Cui et al. 8 for the study of elastocaloric effects in Ni-Ti wires. Furthermore, Ossmer et al. 9,10 showed that thermographic temperature measurements are also suitable for the investigation of elastocaloric effects in Ni-Ti based thin films, which required high frame rates of the IR camera for the investigation of adiabatic phase transformations at high strain rates. This technique allows for the investigation of elastocaloric quantities and the homogeneity of the temperature profile, which has a significant influence on the solid-state based heat transfer and the efficiency of elastocaloric processes.
The cooling efficiency of the material can be determined by calculating the required work based on the stress/strain measurements as well as the heat (which can be determined taking into account the temperature change and the heat capacity of the material). However, the experimental method does not enable the investigation of the elastocaloric material under process condition. This includes a heat transfer between the SMA and a heat source, which has a significant influence on the efficiency of the cooling effect.
The material characterization of cooling process conditions and the investigation of elastocaloric cooling processes require a test rig enabling solid-state based heat transfer, which cannot be investigated by any existing commercial system. To this end, a novel testing platform has been developed. The test rig is set up in two levels as shown in Figure 3. The upper level allows for basic elastocaloric material characterization and initial training procedures, similar to the previously described method (see Figure 4). The setup is equipped with a linear direct drive capable of loading and unloading the SMA at strain rates up to 1 sec-1 (see Figure 5). The linear direct drive enables the investigation of samples with a cross section of up to 1.8 mm2, while the typical sample length is 90 mm. The advantage of a linear direct drive is the high velocity and the high acceleration &#8212; in contrast to ball screw drives which are typically used for tensile tests. Furthermore, a load cell, as well as the integrated position measurement system of the linear drive, provides mechanical measurement data. A high-resolution IR camera (1,280 x 1,024 pixels) is used to measure the temperature profile of the SMA with up to 400 Hz (in the required temperature range). The use of a microscope lens with a resolution of 15 &#181;m/pixel enables the investigation of local temperature effects. The lower level of the test rig contains a mechanism that allows for alternating conductive heat transfer between the SMA and the heat source/heat sink (see Figures 6 and 7). The linear direct drive in the lower level switches between the heat source to the SMA and from the SMA to the heat sink, whereas a pneumatic cylinder lifts and lowers the heat source/sink (see Figure 8). Each actuator can be controlled independently allowing for investigation of different cooling process variations. The comprehensive measurement system enables measurements of mechanical parameters: actuator position, actuator velocity, SMA loading force, contact force between SMA and heat source/sink during heat transfer as well as thermal parameters (i.e., temperatures inside the heat source/sink, temperature distribution on the surface of the SMA and the heat source/sink). A more detailed description of the scientific testing platform is given in Schmidt et al. 11.
<img alt="Figure 5" src="/files/ftp_upload/53626/53626fig5.jpg" /> 
Figure 5. Scheme of the upper level of the test rig. A linear direct drive for loading and unloading of the SMA sample with integrated position measurement system; a load cell for measuring of tensile forces, as well as a high-resolution IR camera (1,280 x 1,024 pixels) for temperature profile acquisitions.
<img alt="Figure 7" src="/files/ftp_upload/53626/53626fig7.jpg" /> 
Figure 7. Scheme of the lower level of the test rig. A linear direct drive for switching between heat sink and heat source; a pneumatic cylinder to make contact between the SMA sample and the heat source/sink; temperature sensors have been integrated in the heat sink/source to measure the core temperature of the blocks. A compression load cell for measuring the contact force between the SMA and the heat source/sink is integrated in the heat transfer mechanism and not visible in this scheme.
The test rig allows for the investigation of different alloy compositions and sample sizes as well as geometries (ribbons, wires). Furthermore, the setup enables comprehensive investigations of elastocaloric materials and cooling processes. The previously described experiments can be performed and the execution will be described step-by-step in the protocol section of this manuscript.
Material stabilization:
Stable material behavior is important for the use of elastocaloric materials in cooling systems. To this end, a mechanical stabilization procedure is applied. During this procedure the material passes mechanical loading and unloading cycles and performs a phase transformation from austenite to martensite. The material stabilization shows a strong rate dependency. High loading rates lead to a temperature change of the material, which is caused by the latent heat of the phase transformation. This temperature change has a similar influence on the material stabilization, as do mechanical training cycles at various temperatures 12-15. In addition to the well-known mechanical 13 and caloric 16 stabilization, a thermal material stabilization can be observed with the designed setup by applying thermography 17.
Material characterization:
After an initial mechanical training procedure, the material shows stable mechanical, thermal and caloric behavior allowing the elastocaloric material properties to be characterized. Therefore, mechanical cycling at different rates is performed whereas, in contrast to the training procedure, the elastocaloric characterization includes a holding phase after loading and unloading. For the duration of the holding phase the SMA strain is kept constant until an ambient temperature level is reached again. This type of experiment is required in order to determine the lowest achievable temperature after unloading, starting from ambient temperature levels, as well as the material efficiency. Rate dependent formation of local temperature peaks can be observed, with higher rates leading to an increasingly homogeneous temperature distribution. Furthermore, by increasing the strain rate the temperature change equally increases until adiabatic conditions are achieved. The material efficiency can be determined by calculating the required mechanical work, based on a force-displacement diagram of an adiabatic experiment, as well as the absorbable heat, based on the mean temperature change of the material during unloading and the heat capacity of the sample.
Elastocaloric cooling process:
The investigation of the cooling efficiency of SMAs under process conditions requires the heat transfer between the SMA cooling medium and a heat source, as well as a heat sink. For this purpose, the SMA is in contact with a solid-state heat source (following adiabatic unloading) and a heat sink (following adiabatic loading). The efficiency of the process strongly depends on the process control and the thermal boundary conditions. The comprehensive investigation of the cooling process requires a variation of the control parameters in order to determine the most efficient process control. The individual influence of the parameters (contact time, SMA strain, SMA strain rate, contact phase (contact during the loading/unloading phase or following) and contact force) on the process performance has to be investigated. Furthermore, the influence of the changing thermal boundary condition by increasing number of cooling cycles has to be taken into account.
Model validation:
The development of a thermomechanically coupled material model, capable of reproducing the mechanical and thermal material behavior during cooling cycle, is crucial for the development of a novel cooling technology. The model allows for material and process optimization by reduced experimental and material development effort. The validation requires an initial isothermal tensile test of a stabilized material to generate the required mechanical material input data (elastic modulus of the austenite and the martensite phase, the width of the mechanical hysteresis as well as the transformation strain). The validation of the model takes place on the basis of tensile tests at different rates. The required caloric input data for the model can be determined by differential scanning calorimetry (DSC) following the mechanical experiments. The DSC measurements have to be performed after the mechanical test in order to measure the caloric material properties of a stabilized sample.

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	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:273px;">Linear direct drives</td>
			<td style="width:116px;">ESR-Pollmeier</td>
			<td style="width:179px;">ML 1418-U5-W1</td>
			<td style="width:567px;">SMA loading/unloading; heat transfer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Pneumatic cylinder&#160;</td>
			<td>Festo</td>
			<td>ADNGF-40 574031</td>
			<td>Contact between heat source/sink and SMA</td>
		</tr>
		<tr height="17">
			<td height="17" style="height:17px;">Inductive position measurement system&#160;</td>
			<td>AMO</td>
			<td>LMKA-1101.1NN-1.0-0</td>
			<td></td>
		</tr>
		<tr height="19">
			<td height="19" style="height:19px;width:273px;">Tension and compression load cell</td>
			<td style="width:116px;">Futek</td>
			<td>LCF451; FSH02241</td>
			<td>SMA force</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:273px;">Compression load cell</td>
			<td style="width:116px;">Futek</td>
			<td>LTH300; FSH00297</td>
			<td>Contact force</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:273px;">IR camera</td>
			<td style="width:116px;">Infra Tec</td>
			<td>Image IR 9360; M91129</td>
			<td>1280x1024 pixels; Maximum frame rate 3200 Hz&#160;</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:273px;">Real-Time Controller&#160;</td>
			<td style="width:116px;">National Instruments</td>
			<td style="width:179px;">NI CompactRIO-9074</td>
			<td>Data acquisiton and control system</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:273px;">Camera varnish</td>
			<td style="width:116px;">Tetenal</td>
			<td align="right" style="width:179px;">105202</td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

Material stabilization (Training):
Figure 9 shows a stress/strain diagram of 50 training cycles. The investigated sample is a Ni-Ti ribbon with a cross section of A = 1.45 mm2. The applied strain rate of 1 x 10-3 sec-1 leads to a mean temperature increase of &#916;T = 12.2 K. The temperature increase has a significant influence on the stabilization effect 12...

Watch this Scientific Journal Video about Experimental Methods for Investigation of Shape Memory Based Elastocaloric Cooling Processes and Model Validation at JoVE.com

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

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.

Shape Memory Alloys (SMA) using elastocaloric cooling processes have the potential to be an environmentally friendly alternative to the conventional vapor ...

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11.0K Views.  Saarland University. 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. 

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

Controlling the Size, Shape and Stability of Supramolecular Polymers in Water

For aqueous based supramolecular polymers, the simultaneous control over shape, size and stability is very difficult1. At the same time, the ability to do so is highly important in view of a number of applications in functional soft matter including electronics, biomedical engineering, and sensors. In the past, successful strategies to control the size and shape of supramolecular polymers typically focused on the use of templates2,3, end cappers4 or selective solvent techniques5. 
Here we disclose a strategy based on self-assembling discotic amphiphiles that leads to the control over stack length and shape of ordered, chiral columnar aggregates. By balancing electrostatic repulsive interactions on the hydrophilic rim and attractive non-covalent forces within the hydrophobic core of the polymerizing building block, we manage to create small and discrete spherical objects6,7. Increasing the salt concentration to screen the charges induces a sphere-to-rod transition. Intriguingly, this transition is expressed in an increase of cooperativity in the temperature-dependent self-assembly mechanism, and more stable aggregates are obtained. 
For our study we select a benzene-1,3,5-tricarboxamide (BTA) core connected to a hydrophilic metal chelate via a hydrophobic, fluorinated L-phenylalanine based spacer (Scheme 1). The metal chelate selected is a Gd(III)-DTPA complex that contains two overall remaining charges per complex and necessarily two counter ions. The one-dimensional growth of the aggregate is directed by &pi;-&pi; stacking and intermolecular hydrogen bonding. However, the electrostatic, repulsive forces that arise from the charges on the Gd(III)-DTPA complex start limiting the one-dimensional growth of the BTA-based discotic once a certain size is reached. At millimolar concentrations the formed aggregate has a spherical shape and a diameter of around 5 nm as inferred from 1H-NMR spectroscopy, small angle X-ray scattering, and cryogenic transmission electron microscopy (cryo-TEM). The strength of the electrostatic repulsive interactions between molecules can be reduced by increasing the salt concentration of the buffered solutions. This screening of the charges induces a transition from spherical aggregates into elongated rods with a length &gt; 25 nm. Cryo-TEM allows to visualise the changes in shape and size. In addition, CD spectroscopy permits to derive the mechanistic details of the self-assembly processes before and after the addition of salt. Importantly, the cooperativity -a key feature that dictates the physical properties of the produced supramolecular polymers- increases dramatically upon screening the electrostatic interactions. This increase in cooperativity results in a significant increase in the molecular weight of the formed supramolecular polymers in water.

The goal of this experiment is to determine and control the size, shape and stability of self-assembled discotic amphiphiles in water. For aqueous based supramolecular polymers such level of control is very difficult. We apply a strategy using both repulsive and attractive interactions. The experimental techniques applied to characterize this system are broadly applicable.

For aqueous based supramolecular polymers, the simultaneous control over shape, size and stability is very difficult1. At the same time, the ability to do ...

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of ...

Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T.

We describe the methodology of mechanical exfoliation and deposition of flakes of novel materials with micron-sized dimensions onto substrate, fabrication of experimental device structures for transport experimentation, and the magnetotransport measurement in a dry helium close-cycle cryostat at temperatures down to 0.300 K and magnetic fields up to 12 T.

Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film ...

SSVEP-based Experimental Procedure for Brain-Robot Interaction with Humanoid Robots

Brain-Robot Interaction (BRI), which provides an innovative communication pathway between human and a robotic device via brain signals, is prospective in helping the disabled in their daily lives. The overall goal of our method is to establish an SSVEP-based experimental procedure by integrating multiple software programs, such as OpenViBE, Choregraph, and Central software as well as user developed programs written in C++ and MATLAB, to enable the study of brain-robot interaction with humanoid robots.
This is achieved by first placing EEG electrodes on a human subject to measure the brain responses through an EEG data acquisition system. A user interface is used to elicit SSVEP responses and to display video feedback in the closed-loop control experiments. The second step is to record the EEG signals of first-time subjects, to analyze their SSVEP features offline, and to train the classifier for each subject. Next, the Online Signal Processor and the Robot Controller are configured for the online control of a humanoid robot. As the final step, the subject completes three specific closed-loop control experiments within different environments to evaluate the brain-robot interaction performance.
The advantage of this approach is its reliability and flexibility because it is developed by integrating multiple software programs. The results show that using this approach, the subject is capable of interacting with the humanoid robot via brain signals. This allows the mind-controlled humanoid robot to perform typical tasks that are popular in robotic research and are helpful in assisting the disabled.

The overall goal of this method is to establish an SSVEP-based experimental procedure by integrating multiple software programs to enable the study of brain-robot interaction with humanoid robots, which is prospective in assisting the sick and elderly as well as performing unsanitary or dangerous jobs.

Brain-Robot Interaction (BRI), which provides an innovative communication pathway between human and a robotic device via brain signals, is prospective in ...

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.

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 ...

Knowledge Based Cloud FE Simulation of Sheet Metal Forming Processes

The use of Finite Element (FE) simulation software to adequately predict the outcome of sheet metal forming processes is crucial to enhancing the efficiency and lowering the development time of such processes, whilst reducing costs involved in trial-and-error prototyping. Recent focus on the substitution of steel components with aluminum alloy alternatives in the automotive and aerospace sectors has increased the need to simulate the forming behavior of such alloys for ever more complex component geometries. However these alloys, and in particular their high strength variants, exhibit limited formability at room temperature, and high temperature manufacturing technologies have been developed to form them. Consequently, advanced constitutive models are required to reflect the associated temperature and strain rate effects. Simulating such behavior is computationally very expensive using conventional FE simulation techniques.
This paper presents a novel Knowledge Based Cloud FE (KBC-FE) simulation technique that combines advanced material and friction models with conventional FE simulations in an efficient manner thus enhancing the capability of commercial simulation software packages. The application of these methods is demonstrated through two example case studies, namely: the prediction of a material's forming limit under hot stamping conditions, and the tool life prediction under multi-cycle loading conditions.

The following paper presents a novel FE simulation technique (KBC-FE), which reduces computational cost by performing simulations on a cloud computing environment, through the application of individual modules. Moreover, it establishes a seamless collaborative network between world leading scientists, enabling the integration of cutting edge knowledge modules into FE simulations.

The use of Finite Element (FE) simulation software to adequately predict the outcome of sheet metal forming processes is crucial to enhancing the ...

Studying Dynamic Processes of Nano-sized Objects in Liquid using Scanning Transmission Electron Microscopy

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a microfluidic chamber assembled in the specimen holder for Transmission Electron Microscopy (TEM) and STEM. The microfluidic system consists of two silicon microchips supporting thin Silicon Nitride (SiN) membrane windows. This article describes the basic steps of sample loading and data acquisition. Most important of all is to ensure that the liquid compartment is correctly assembled, thus providing a thin liquid layer and a vacuum seal. This protocol also includes a number of tests necessary to perform during sample loading in order to ensure correct assembly. Once the sample is loaded in the electron microscope, the liquid thickness needs to be measured. Incorrect assembly may result in a too-thick liquid, while a too-thin liquid may indicate the absence of liquid, such as when a bubble is formed. Finally, the protocol explains how images are taken and how dynamic processes can be studied. A sample containing AuNPs is imaged both in pure water and in saline.

This protocol describes the operation of a liquid flow specimen holder for scanning transmission electron microscopy of AuNPs in water, as used for the observation of nanoscale dynamic processes.

Samples fully embedded in liquid can be studied at a nanoscale spatial resolution with Scanning Transmission Electron Microscopy (STEM) using a ...

Experimental Procedure for Warm Spinning of Cast Aluminum Components

High performance, cast aluminum automotive wheels are increasingly being incrementally formed via flow forming/metal spinning at elevated temperatures to improve material properties. With a wide array of processing parameters which can affect both the shape attained and resulting material properties, this type of processing is notoriously difficult to commission. A simplified, light-duty version of the process has been designed and implemented for full-size automotive wheels. The apparatus is intended to assist in understanding the deformation mechanisms and the material response to this type of processing. An experimental protocol has been developed to prepare for, and subsequently perform forming trials and is described for as-cast A356 wheel blanks. The thermal profile attained, along with instrumentation details are provided. Similitude with full-scale forming operations which impart significantly more deformation at faster rates is discussed.

An experimental protocol for instrumented warm rotary forming of cast aluminum alloys employing a bespoke industrially scaled apparatus is presented. Experimental considerations including thermal and mechanical effects are discussed, as well as similitude with full-scale processing of automotive wheels.

High performance, cast aluminum automotive wheels are increasingly being incrementally formed via flow forming/metal spinning at elevated temperatures to ...

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 ...

Experimental Methods for Trapping Ions Using Microfabricated Surface Ion Traps

Ions trapped in a quadrupole Paul trap have been considered one of the strong physical candidates to implement quantum information processing. This is due to their long coherence time and their capability to manipulate and detect individual quantum bits (qubits). In more recent years, microfabricated surface ion traps have received more attention for large-scale integrated qubit platforms. This paper presents a microfabrication methodology for ion traps using micro-electro-mechanical system (MEMS) technology, including the fabrication method for a 14 &#181;m-thick dielectric layer and metal overhang structures atop the dielectric layer. In addition, an experimental procedure for trapping ytterbium (Yb) ions of isotope 174 (174Yb+) using 369.5 nm, 399 nm, and 935 nm diode lasers is described. These methodologies and procedures involve many scientific and engineering disciplines, and this paper first presents the detailed experimental procedures. The methods discussed in this paper can easily be extended to the trapping of Yb ions of isotope 171 (171Yb+) and to the manipulation of qubits.

This paper presents a microfabrication methodology for surface ion traps, as well as a detailed experimental procedure for trapping ytterbium ions in a room-temperature environment.

Ions trapped in a quadrupole Paul trap have been considered one of the strong physical candidates to implement quantum information processing. This is due ...