This research was supported by the European Union's Seventh Framework Programme (FP7/2007-2013) under grant agreement No. 604240, project title "An industrial system enabling the use of a patented, lab-proven materials processing technology for Low Cost forming of Lightweight structures for transportation industries (LoCoLite)."

1. Preparation of Specimens
<ol>
	<li>Machine flat dog-bone and cruciform specimens from commercial material aluminum alloy 6082 (AA6082) using a laser cutter and a computer numerical control (CNC) milling machine (for formability tests at different strain paths including uniaxial, plane strain, and equi-biaxial straining states).</li>
	<li>Measure the thickness of each cruciform specimen and each dog-bone specimen with a vernier caliper three times in the central gauge region and calculate the average values. Ensure that the thickness of the gauge section in a cruciform specimen is 0.7 &#177; 0.05 mm and that the thickness of the uniaxial specimen is 1.5 &#177; 0.1 mm.</li>
	<li>Spray-paint the entire top surface of a cruciform specimen by using a flame-resistant, black spray paint (capable of withstanding temperatures up to 1,093 &#176;C). Wait until the paint dries and then spray flame-resistant, white paint dots from arm&#39;s length to create a stochastic spraying pattern to be recognized by the DIC system (see the example in Figure 1).</li>
	<li>Weld a pair of thermocouples to the center of the back surface (opposite to the painted surface) of the specimen. Connect the other end of the thermocouple to the feedback temperature control system of the uniaxial testing machine to monitor and control the temperature change history.</li>
</ol>
2. Assembly of the Biaxial Testing Apparatus
<ol>
	<li>Assemble all parts of the biaxial testing apparatus, including a base plate, a central shaft, input and output rotatable plates, carriages, a clamp, guide rails, and rigid connecting rods (the assembled apparatus is shown in Figure 2).
	<ol>
		<li>Using a connecting rod, couple the input rotatable plate directly to the movable jaw of a resistance heating uniaxial tensile test machine, which provides the uniaxial tensile force. Couple the input rotatable plate to the central drive shaft and couple this central drive shaft to the output rotatable plate.</li>
		<li>Ensure that the rotation of the input rotatable plate around the axis of rotation rotates the drive shaft, thereby rotating the output rotatable plate to which it is coupled around the axis of rotation.</li>
		<li>At one end, couple each of the rigid connecting rods to one of the connection points on the output rotatable plate. Couple the other end to one of the carriages. 
		NOTE: This will cause the carriages with specimen holders to slide back and forth along the guide rails with low friction, which can apply a biaxial force to the cruciform specimen.</li>
		<li>Using screw bolts, clamp each arm of the cruciform specimen to a carriage with a specimen holder and a top plate.</li>
	</ol>
	</li>
	<li>Set up grips in the chamber of the uniaxial tensile test machine, as shown in Figure 3 (a). Attach four welding cables to each pair of grips, which are made of stainless steel and copper, respectively, and thus connect the welding cables to the electrical power supply. 
	NOTE: The conductor area of the welding cables is 50 mm2 and the current rating is 345 A.
	<ol>
		<li>Put the grips and the clamp of the biaxial testing apparatus into the two jaws of the uniaxial tensile test machine and tighten them inside (Figure 3 (a)).</li>
	</ol>
	</li>
	<li>Set up the biaxial testing apparatus in the chamber of the uniaxial tensile test machine, as shown in Figure 3 (b).
	<ol>
		<li>Use two frames and screw bolts on the top and the bottom sides of the base plate to fix the apparatus in the chamber of the uniaxial tensile test machine.</li>
		<li>Put the specimen into the specimen holder on top of the biaxial testing apparatus.</li>
		<li>Connect each terminal of the welding cables to each clamping region of the specimen.</li>
	</ol>
	</li>
</ol>
3. Setup of the Heating and Quenching System
<ol>
	<li>Tightly connect each clamping region of the specimen to the stainless steel top plate, which serves as the electrode for resistance heating.</li>
	<li>Tighten the welding cables with crimp ring terminals to the top plate of each clamping region.</li>
	<li>Connect flared nozzles with hoses to the high flow quench system with regulated air supply at 8,000 kg/m2 pressure for cooling.</li>
	<li>Use four nozzles to blow air from the arms of the specimen to the central region of the specimen. 
	NOTE: The nozzles are not directed onto the gauge section for cooling to avoid blocking the central zone from the camera&#39;s view.</li>
</ol>
4. Setup of the DIC System
<ol>
	<li>Connect the high-speed camera of the DIC system with a micro lens to a computer. Adjust the frame rates of the camera to 25 fps, 50 fps, and 500 fps from the menu of frame rates (for the tests at the stretching strain rates of 0.01/s, 0.1/s and 1/s, respectively). Set the resolutions of all images to 1,280&#215;1,024 pixels. 
	NOTE: The frame rates depend on the number of data points to be collected; at least 200 data points can be collected using the above settings.</li>
	<li>Use an additional spotlight with a power of 300 W for tests at high strain rates. Point the spotlight directly at the chamber of the uniaxial tensile test machine.</li>
	<li>Adjust the camera lens so that it is parallel to the top surface of the specimen in the chamber and focus the camera on the gauge section.</li>
</ol>
5. Experimental Program
<ol>
	<li>Run the resistance heating uniaxial tensile test machine by clicking the triangular run button in the control software. 
	NOTE: Electricity runs through the AA6082 material and heats it to the solution heat treatment temperature of 535 &#176;C14 at a heating rate of 30 &#176;C/s. The material is soaked at 535 &#176;C for 1 min, which is sufficient for the full resolution of precipitates. Air blowing from the quench system is used to quench the material at a cooling rate of 100 &#176;C/s15 to one of 3 designated elevated temperatures in the range of 370-510 &#176;C.</li>
	<li>Stretch the specimen with the biaxial testing apparatus at a constant strain rate in the range of 0.01-1/s and record the deformation history by manually pressing the trigger button connected to the high-speed camera. 
	NOTE: The input displacement from the uniaxial testing machine to the biaxial testing apparatus was controlled by the built-in software of the uniaxial testing machine.</li>
	<li>Perform the tests at different strain paths consisting of uniaxial, plane strain, and biaxial straining states3 by adjusting the configuration of the biaxial testing apparatus.
	<ol>
		<li>Disconnect two opposed connecting rods for uniaxial tests. Clamp a dog-bone specimen on the biaxial testing apparatus and connect it to welding cables, as in steps 3.1-3.4. Repeat steps 5.1-5.2.</li>
		<li>Fix two opposed carriages to the base plate with screw bolts to restrict the deformation on the corresponding direction for testing under plane strain state. Clamp a cruciform specimen on the biaxial testing apparatus and connect it to welding cables, as in steps 3.1-3.4. Repeat steps 5.1-5.2.</li>
	</ol>
	</li>
	<li>Repeat steps 5.3.1-5.3.2 for each test condition three times, using new dog-bone and cruciform specimens.</li>
</ol>
6. Data Processing
<ol>
	<li>Import all images recorded by the high-speed camera into the post-processing software and follow standard steps for data analysis according to the software manual.</li>
	<li>Use the ISO standard3 to determine the forming limits by clicking the FLC Mode button in the software. 
	NOTE: This method has already been integrated into the image correlation processing software.</li>
	<li>Mark each result of the forming limits at various temperatures, strain rates, and strain paths in a diagram.</li>
	<li>Plot the forming limit curves at all test conditions to obtain an FLD of an alloy under hot stamping conditions.</li>
</ol>

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	<li>Karbasian, H., Tekkaya, A. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+review+on+hot+stamping.">A review on hot stamping.</a> J. of Mater. Process. Tech. 210 (15), 2103-2118 (2010).</li><li>Miller, W. S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Recent+development+in+aluminium+alloys+for+the+automotive+industry.">Recent development in aluminium alloys for the automotive industry.</a> Mater. Sci. and Eng. 280 (1), 37-49 (2000).</li><li>Shao, Z., Li, N., Lin, J., Dean, T. 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A. 10 (1), 41-46 (1979).</li><li>Shao, Z., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Experimental+investigation+of+forming+limit+curves+and+deformation+features+in+warm+forming+of+an+aluminium+alloy.">Experimental investigation of forming limit curves and deformation features in warm forming of an aluminium alloy.</a> P. I. Mech. Eng. B-J. Eng. , (2016).</li><li>Marciniak, Z., Kuczynski, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Limit+strains+in+the+processes+of+stretch-forming+sheet+metal.">Limit strains in the processes of stretch-forming sheet metal.</a> Int. J. Mech. Sci. 9 (9), 609-620 (1967).</li><li>Li, D., Ghosh, A. K., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Biaxial+warm+forming+behavior+of+aluminum+sheet+alloys.">Biaxial warm forming behavior of aluminum sheet alloys.</a> J. of Mater. Process. Tech. 145 (3), 281-293 (2004).</li><li>Palumbo, G., Sorgente, D., Tricarico, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+design+of+a+formability+test+in+warm+conditions+for+an+AZ31+magnesium+alloy+avoiding+friction+and+strain+rate+effects.">The design of a formability test in warm conditions for an AZ31 magnesium alloy avoiding friction and strain rate effects.</a> Int. J. Mach. Tool. Manu. 48 (14), 1535-1545 (2008).</li><li>Raghavan, K. 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The authors have nothing to disclose.

Conventional formability test methods used to determine forming limits are usually applicable only at room temperature. The presented technique can be used to evaluate the formability of metals for hot sheet stamping applications by introducing a novel biaxial testing apparatus to a resistance heating uniaxial testing machine. This cannot be performed using conventional methods for hot stamping applications. The setup of heating and cooling systems and the DIC system is critical to controlling the uniformity of temperatu...

The automotive industry is facing a huge global challenge of reducing fuel consumption and minimizing environmental pollution from vehicle emissions. Weight reduction is beneficial to improving the performance of automobiles and can directly reduce energy consumption1. Due to the low formability of sheet metals at room temperature, hot stamping and cold die quenching processes (referred to as hot stamping)2 are used to improve the formability of alloys and thus to obtain complex shaped components in automotive applications.
A forming limit diagram (FLD) is a useful tool to evaluate the formability of an alloy3. Out-of-plane tests, such as the Nakazima test4,5, and in-plane tests, such as the Marciniak test6,7,8, are conventional experimental methods to obtain the FLDs of sheet metals under various conditions9,10,11. A servo-hydraulic biaxial testing machine has also been used to investigate the formability of alloys at room temperature12,13.
However, none of the methods above are applicable to formability tests under hot stamping conditions, since a cooling process prior to forming is required along with control of the heating and cooling rates. The deformation temperature and strain rate are difficult to obtain accurately. Therefore, a novel formability testing system is proposed in this study to experimentally determine the forming limits of sheet metals under hot stamping conditions.

<table border="0" cellpadding="0" cellspacing="0" width="923">
	<colgroup>
		<col />
		<col />
		<col />
		<col />
	</colgroup>
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Aluminium Alloy&#160;</td>
			<td style="width:152px;">Smiths Metal</td>
			<td style="width:121px;">6082</td>
			<td style="width:421px;">Specimens machining</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Laser cutter</td>
			<td style="width:152px;">LVD Ltd</td>
			<td style="width:121px;">HELIUS 25/13</td>
			<td>Laser cutting specimens</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">CNC machine</td>
			<td style="width:152px;">HAAS Automation</td>
			<td style="width:121px;">TM-2CE</td>
			<td>Machine specimens by milling</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Vernier caliper</td>
			<td style="width:152px;">Mitutoyo</td>
			<td style="width:121px;">575-481</td>
			<td>Thickness measurement</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:229px;">Resistance heating uniaxial testing machine</td>
			<td style="width:152px;">Dynamic System Inc</td>
			<td style="width:121px;">Gleeble 3800</td>
			<td>Thermo-mechanical materials simulator</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">High flow quench system</td>
			<td style="width:152px;">Dynamic System Inc</td>
			<td style="width:121px;">38510</td>
			<td>For air cooling</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Thermocouples</td>
			<td style="width:152px;">Dynamic System Inc</td>
			<td style="width:121px;">K type</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Nozzles</td>
			<td style="width:152px;">Indexa</td>
			<td style="width:121px;"></td>
			<td>Nozzle flared 1/4 inch bore</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Welding cables</td>
			<td style="width:152px;">LAPP Group</td>
			<td style="width:121px;">H01N2-D</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">High-speed camera</td>
			<td style="width:152px;">Photron</td>
			<td style="width:121px;">UX50</td>
			<td>For DIC testing</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Camera lens</td>
			<td style="width:152px;">Nikon</td>
			<td style="width:121px;">Micro 200mm</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Lamp</td>
			<td style="width:152px;">Liliput</td>
			<td style="width:121px;">150ce</td>
			<td>300W</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Laptop</td>
			<td style="width:152px;">HP</td>
			<td style="width:121px;">Campaq 2530p</td>
			<td>For images recording</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:229px;">Biaxial testing apparatus</td>
			<td style="width:152px;">Manufactured independently</td>
			<td style="width:121px;"></td>
			<td style="width:421px;">All parts were designed and machinced by authors for biaxial testing</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:229px;">Steel&#160;</td>
			<td style="width:152px;">West Yorkshire Steel</td>
			<td style="width:121px;">H13</td>
			<td style="width:421px;">Mateials of the biaxial testing apparatus</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:229px;">Image correlation processing software</td>
			<td style="width:152px;">GOM</td>
			<td style="width:121px;">ARAMIS</td>
			<td>Non-contact measuring system and data post-pocessing</td>
		</tr>
	</tbody>
</table>

a novel biaxial testing apparatus for the determination of forming limit under hot stamping conditions

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional experimental approaches, such as out-of-plane and in-plane tests, are not applicable to the determination of forming limits when heating and rapid cooling processes are introduced prior to forming for tests conducted under hot stamping conditions. A novel in-plane biaxial testing system was designed and used for the determination of forming limits of sheet metals at various strain paths, temperatures, and strain rates after heating and cooling processes in a resistance heating uniaxial testing machine. The core part of the biaxial testing system is a biaxial apparatus, which transfers a uniaxial force provided by the uniaxial testing machine to a biaxial force. One type of cruciform specimen was designed and verified for the formability test of aluminum alloy 6082 using the proposed biaxial testing system. The digital image correlation (DIC) system with a high-speed camera was used for taking strain measurements of a specimen during a deformation. The aim of proposing this biaxial testing system is to enable the forming limits of an alloy to be determined at various temperatures and strain rates under hot stamping conditions.

Since FLDs are highly strain path-dependent, the linearity of the strain path for each test condition was verified by analyzing the DIC results; the strain paths are proportional throughout deformation for each test condition. The range of the minor-to-major strain ratio is approximately -0.37 (uniaxial condition) to 0.26 (near biaxial condition). By processing data for different AA6082 conditions, forming limit data for different strain paths were determined and hence, the FLDs for AA608...

Watch this Scientific Journal Video about A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions at JoVE.com

A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional ...

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7.5K Views.  Imperial College London. This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

Video: A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

Fabrication of VB2/Air Cells for Electrochemical Testing

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for synthesizing nanoscopic VB2 is presented as well as step-by-step procedure for applying a zirconium oxide coating to the VB2 particles for stabilization upon discharge. The process for disassembling existing zinc/air cells is shown, in addition construction of the new working electrode to replace the conventional zinc/air cell anode with a the nanoscopic VB2 anode. Finally, discharge of the completed VB2/air battery is reported. We show that using the zinc/air cell as a test bed is useful to provide a consistent configuration to study the performance of the high-energy high capacity nanoscopic VB2 anode.

Fabrication of VB2/Air Cells for Electrochemical Testing

A protocol is presented to study multi-electron metal/air battery systems by using previous technology developed for the zinc/air cell. Electrochemical testing is then performed on fabricated batteries to evaluate performance.

A technique to investigate the properties and performance of new multi-electron metal/air battery systems is proposed and presented. A method for ...

High-Sensitivity Nuclear Magnetic Resonance at Giga-Pascal Pressures: A New Tool for Probing Electronic and Chemical Properties of Condensed Matter under Extreme Conditions

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their electronic properties. The application of high pressure enables one to synthesize new materials, but the response of known materials to high pressure is a very useful tool for studying their electronic structure and developing theories. For example, high-pressure synthesis might be at the origin of life; and understanding the behavior of small molecules under extreme pressure will tell us more about fundamental processes in our universe. It is no wonder that there has always been great interest in having NMR available at high pressures. Unfortunately, the desired pressures are often well into the Giga-Pascal (GPa) range and require special anvil cell devices where only very small, secluded volumes are available. This has restricted the use of NMR almost entirely in the past, and only recently, a new approach to high-sensitivity GPa NMR, which has a resonating micro-coil inside the sample chamber, was put forward. This approach enables us to achieve high sensitivity with experiments that bring the power of NMR to Giga-Pascal pressure condensed matter research. First applications, the detection of a topological electronic transition in ordinary aluminum metal and the closing of the pseudo-gap in high-temperature superconductivity, show the power of such an approach. Meanwhile, the range of achievable pressures was increased tremendously with a new generation of anvil cells (up to 10.1 GPa), that fit standard-bore NMR magnets. This approach might become a new, important tool for the investigation of many condensed matter systems, in chemistry, geochemistry, and in physics, since we can now watch structural changes with the eyes of a very versatile probe.

Nuclear magnetic resonance is one of the most important spectroscopic tools. Here, the development of a new approach under high pressure, currently up to 10.1 GPa, is presented. This opens a new window into condensed matter physics and chemistry, where high-pressure research is of great importance.

Nuclear Magnetic Resonance (NMR) is one of the most important techniques for the study of condensed matter systems, their chemical structure, and their ...

A Testing Platform for Durability Studies of Polymers and Fiber-reinforced Polymer Composites under Concurrent Hygrothermo-mechanical Stimuli

The durability of polymers and fiber-reinforced polymer composites under service condition is a critical aspect to be addressed for their robust designs and condition-based maintenance. These materials are adopted in a wide range of engineering applications, from aircraft and ship structures, to bridges, wind turbine blades, biomaterials and biomedical implants. Polymers are viscoelastic materials, and their response may be highly nonlinear and thus make it challenging to predict and monitor their in-service performance. The laboratory-scale testing platform presented herein assists the investigation of the influence of concurrent mechanical loadings and environmental conditions on these materials. The platform was designed to be low-cost and user-friendly. Its chemically resistant materials make the platform adaptable to studies of chemical degradation due to in-service exposure to fluids. An example of experiment was conducted at RT on closed-cell polyurethane foam samples loaded with a weight corresponding to ~50% of their ultimate static and dry load. Results show that the testing apparatus is appropriate for these studies. Results also highlight the larger vulnerability of the polymer under concurrent loading, based on the higher mid-point displacements and lower residual failure loads. Recommendations are made for additional improvements to the testing apparatus.

The durability of polymers and fiber-reinforced polymer composites in service is a critical aspect for their designs and condition-based maintenance. We present a novel low-cost laboratory testing platform for the investigation of the influence of concurrent mechanical and environmental loadings, and may help design more efficient yet safer composite structures.

The durability of polymers and fiber-reinforced polymer composites under service condition is a critical aspect to be addressed for their robust designs ...

Detection and Recovery of Palladium, Gold and Cobalt Metals from the Urban Mine Using Novel Sensors/Adsorbents Designated with Nanoscale Wagon-wheel-shaped Pores

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in industrialized countries. Here, the development of optical mesosensors/adsorbents (MSAs) for efficient recognition and selective recovery of Pd(II), Au(III), and Co(II) from urban mine was achieved. A simple, general method for preparing MSAs based on using high-order mesoporous monolithic scaffolds was described. Hierarchical cubic Ia3d wagon-wheel-shaped MSAs were fabricated by anchoring chelating agents (colorants) into three-dimensional pores and micrometric particle surfaces of the mesoporous monolithic scaffolds. Findings show, for the first time, evidence of controlled optical recognition of Pd(II), Au(III), and Co(II) ions and a highly selective system for recovery of Pd(II) ions (up to ~95%) in ores and industrial wastes. Furthermore, the controlled assessment processes described herein involve evaluation of intrinsic properties (e.g., visual signal change, long-term stability, adsorption efficiency, extraordinary sensitivity, selectivity, and reusability); thus, expensive, sophisticated instruments are not required. Results show evidence that MSAs will attract worldwide attention as a promising technological means of recovering and recycling palladium, gold and cobalt metals.

Because of the importance and extensive use of palladium, gold and cobalt metals in high-technology equipment, their recovery and recycling constitute an important industrial challenge. The metal recovery system described herein is a simple, low-cost means for the effective detection, removal, and recovery of these metals from the urban mine.

Developing low-cost, efficient processes for recovering and recycling palladium, gold and cobalt metals from urban mine remains a significant challenge in ...

Development of an Experimental Setup for the Measurement of the Coefficient of Restitution under Vacuum Conditions

The Discrete Element Method is used for the simulation of particulate systems to describe and analyze them, to predict and afterwards optimize their behavior for single stages of a process or even an entire process. For the simulation with occurring particle-particle and particle-wall contacts, the value of the coefficient of restitution is required. It can be determined experimentally. The coefficient of restitution depends on several parameters like the impact velocity. Especially for fine particles the impact velocity depends on the air pressure and under atmospheric pressure high impact velocities cannot be reached. For this, a new experimental setup for free-fall tests under vacuum conditions is developed. The coefficient of restitution is determined with the impact and rebound velocity which are detected by a high-speed camera. To not hinder the view, the vacuum chamber is made of glass. Also a new release mechanism to drop one single particle under vacuum conditions is constructed. Due to that, all properties of the particle can be characterized beforehand.

The coefficient of restitution is a parameter that describes the loss of kinetic energy during collision. Here, a free-fall setup under vacuum conditions is developed to be able to determine the coefficient of restitution parameter for particles in micrometer range with high impact velocities.

The Discrete Element Method is used for the simulation of particulate systems to describe and analyze them, to predict and afterwards optimize their ...

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 ...

Spark Plasma Sintering Apparatus Used for the Formation of Strontium Titanate Bicrystals

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with one twist grain boundary. This apparatus utilizes high uniaxial pressure and a pulsed direct current for rapid consolidation of material. Diffusion bonding of strontium titanate bicrystals without fracture, in a spark plasma sintering apparatus, is possible at high pressures due to the unusual temperature dependent plasticity behavior of strontium titanate. We demonstrate a method for the successful formation of bicrystals at accelerated time scales and lower temperatures in a spark plasma sintering apparatus compared to bicrystals formed by conventional diffusion bonding parameters. Bond quality was verified by scanning electron microscopy. A clean and atomically abrupt interface containing no secondary phases was observed using transmission electron microscopy techniques. Local changes in bonding across the boundary was characterized by simultaneous scanning transmission electron microscopy and spatially resolved electron energy-loss spectroscopy.

A viable technique for the formation of strontium titanate bicrystals at high pressure and fast heating rate via the spark plasma sintering apparatus is developed.

A spark plasma sintering apparatus was used as a novel method for diffusion bonding of two single crystals of strontium titanate to form bicrystals with ...

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 &#176;C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. 
Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

This article describes a setup and method for the in situ visualization of oil samples under a variety of temperature and pressure conditions that aim to emulate refining and upgrading processes. It is primarily used for studying isotropic and anisotropic media involved in the fouling behavior of petroleum feeds.

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method 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 ...

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.

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 ...