The authors gratefully acknowledge continued funding and support for the project from the Atomic Weapons Establishment, AWE Plc. (UK) and Imperial College London.

1. Target Fabrication and Assembly
<ol>
	<li>Machine target cylinder to desired dimensions from solid stock.</li>
	<li>Prepare the cylinder surface by removing machining marks. A uniform diffuse surface is preferable for PDV reflection. Good results have been obtained with a light wet sanding with &#62;1,200 grit.</li>
	<li>Characterize the target constituents, i.e., measure the following: 
	Cylinder length, diameter and wall thickness (at multiple locations) 
	Projectile length, diameter 
	Ogive length, diameter 
	Mass of all the above</li>
	<li>Assemble the cylinder mounting ring and PDV arm.</li>
	<li>Mount the PDV probes in the kinematic mounts and onto the PDV arm.</li>
	<li>Insert the ogive in the target cylinder so that the rear of the ogive is flush with the rear of the cylinder (this should be done on a workshop flat). The three M3 screws are designed to hold the ogive in place while allowing the cylinder to &#8216;peel away&#8217; during the expansion.</li>
	<li>Place the target cylinder in the mounting hardware so that the entrance of the cylinder is flush with the leading face of the mounting ring. Secure the cylinder in place with 6 M4 grub screws.</li>
	<li>Install heating/cooling apparatus and bond thermocouples along the length of the cylinder outer wall.</li>
	<li>Clean the FC/APC (ferrule connector, angled physical contact) connectors on the end of the PDV probe fibers with fiber cleaning cloth and check with a fiber scope. This is important to reduce back-reflection.</li>
	<li>Using a visible (660 nm) Class 3R laser roughly align the probes so that they are normal to the cylinder (i.e., the reflected light falls back on the probe).</li>
	<li>Assemble a basic reflectivity circuit using a circulator. Connect the Class 1 1,550 nm laser to input 1, the PDV probe to input 2 and a power meter to input 3. Align the PDV probes in turn so that the power returned is maximized.</li>
</ol>
2. Gas Gun Preparation
<ol>
	<li>Using the barrel plug and the depth micrometer align the target ring to the end of the barrel to minimize impact tilt.</li>
	<li>Install the fragment mitigation system and the door protection.</li>
	<li>Place the target alignment plug in the barrel.</li>
	<li>Install the target assembly and align to the plug.</li>
	<li>Install the trigger make pair on the end of the barrel and connect to the timing hardware and diagnostics. Measure the distance from contact with the trigger to impact of the projectile on the ogive.</li>
	<li>Install the turning mirrors for high speed photography.</li>
	<li>Align the mirrors to give an orthogonal view of the cylinder through the target tank ports and lock in place.</li>
	<li>Align the high speed cameras and flash lamps outside the target tank. Looking down the barrel, place the high speed camera and one flash lamp at 3 o&#8217;clock relative to the cylinder. Place the IVV camera at 9 o&#8217;clock and another flash lamp at 12 o&#8217;clock. In this configuration the high speed camera will be front-lit for crack tracking and the IVV will provide silhouetted images for edge detection.</li>
	<li>Connect heating/cooling equipment to target and vacuum feed throughs.</li>
	<li>CAUTION: With the appropriate eyewear and other precautions turn on the Class IV lasers, oscilloscopes and PDV systems.</li>
	<li>Check the power levels being sent to the PDV probes. With the PDV system, typically use around 5 mW to each probe with 1 mW per channel for the reference.</li>
	<li>Check the alignment of the PDV probes with a power meter. Once satisfied with the alignment use IR card to measure where the PDV probes are looking on the cylinder surface.</li>
	<li>Turn on the reference laser and check the quality of the beat signals given by each probe. Adjust the wavelength of the laser(s) to set the desired zero velocity beat frequency (set this around 5 GHz).</li>
	<li>Once satisfied with the target alignment, trigger location, camera and mirror alignment, PDV probe alignment and location and the mitigation frame close the target tank.</li>
	<li>Remove the alignment plug; install the projectile.</li>
	<li>Setup cameras and lighting (frame rate, exposure, timings) and perform test imaging. Typical frame rates are around 250,000 frames/sec for both cameras, with an exposure of around 0.5 &#181;sec. The first image is normally timed to coincide with the moment of impact.</li>
</ol>
3. Firing Preparation
<ol>
	<li>Install the breech diaphragms that are applicable to the firing pressure needed.</li>
	<li>Close the breech and begin evacuation of the target tanks. Aim for a vacuum level in the region of 50 mTorr.</li>
	<li>Perform final setup of all diagnostics (oscilloscope delays, triggers, camera settings etc.). Set oscilloscopes for PDV at 50 &#181;sec per division, 25 psec per point and a pretrigger of 20% to give a 500 &#181;sec window. Trigger the oscilloscopes and cameras such that zero time coincides with the time of impact.</li>
	<li>Final trigger test; check timings are accurate.</li>
	<li>Turn on lasers; arm cameras.</li>
	<li>Close room; ensuring laser and high pressure interlocks are in the correct position.</li>
	<li>Begin heating / cooling as required using the LabVIEW software.</li>
	<li>Charge the gun to the required firing pressure.</li>
	<li>When at pressure, do a final check that all diagnostic systems are armed.</li>
	<li>Isolate the heating or cooling apparatus.</li>
	<li>Countdown &#8220;3, 2, 1 FIRE.&#8221;</li>
	<li>Vent the target and capture tanks.</li>
	<li>Save all oscilloscope and camera data.</li>
</ol>
4. Post Shot
<ol>
	<li>Shut down lasers and wait for the gun to fully equalize at atmosphere.</li>
	<li>Open the target tank, collect all metal fragments and sort out the Ti-6Al-4V.</li>
</ol>
5. Data Analysis
<ol>
	<li>Perform STFT analysis on the PDV oscilloscope data to reduce the velocity history as per the analysis of Ao and Dolan 12.</li>
	<li>Process high speed imaging data with software such as mentioned in the equipment table. The high speed camera footage will provide time and strain at failure and enable analysis of crack formation and growth. The silhouetted images from the IVV provide a clear edge to examine the full deformation profile of the cylinder.</li>
	<li>Measure and weigh recovered fragments. Select fragments with interesting features such as arrested fractures and prepare them for microscopy.
	<ol>
		<li>Section, mount, and polish the fragments; then analyze in the electron microscope. Electron backscatter diffraction provides information on texture and microstructure alongside secondary electron imaging to probe the fracture surfaces and identify the failure mode.</li>
	</ol>
	</li>
</ol>

<ol>
	<li>Jones, D. R., Chapman, D. J., Eakins, D. 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+gas+gun+based+technique+for+studying+the+role+of+temperature+in+dynamic+fracture+and+fragmentation.">A gas gun based technique for studying the role of temperature in dynamic fracture and fragmentation.</a> J. Appl. Phys. 114, 173508 (2013).</li><li>Liao, S. C., Duffy, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adiabatic+shear+bands+in+a+Ti-6Al-4V+titanium+alloy.">Adiabatic shear bands in a Ti-6Al-4V titanium alloy.</a> J. Mech. Phys. Solids. 46 (11), 2201-2231 (1998).</li><li>Mott, N. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fragmentation+of+shell+cases.">Fragmentation of shell cases.</a> Proc. R. Soc. Lond. A. 189 (1018), 300-308 (1947).</li><li>Hoggatt, C. R., Recht, R. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fracture+behavior+of+tubular+bombs.">Fracture behavior of tubular bombs.</a> J. Appl. Phys. 39 (3), 1856-1862 (1968).</li><li>Banks, E. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+fragmentation+behavior+of+thin-walled+metal+cylinders.">The fragmentation behavior of thin-walled metal cylinders.</a> J. Appl. Phys. 40 (1), 437-438 (1969).</li><li>Warnes, R. H., Duffey, T. A., Karpp, R. R., Carden, 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=Improved+technique+for+determining+dynamic+metal+properties+using+the+expanding+ring.">Improved technique for determining dynamic metal properties using the expanding ring.</a> Los Alamos Scientific Laboratory Report. , (1980).</li><li>Niordson, F. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+unit+for+testing+materials+at+high+strain+rates.">A unit for testing materials at high strain rates.</a> Exp. Mech. 5 (1), 29-32 (1965).</li><li>Grady, D. E., Benson, D. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Fragmentation+of+metal+rings+by+electromagnetic+loading.">Fragmentation of metal rings by electromagnetic loading.</a> Exp. Mech. 23 (4), 393-400 (1983).</li><li>Winter, R. E., Prestidge, H. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+technique+for+the+measurement+of+the+high+strain+rate+ductility+of+metals.">A technique for the measurement of the high strain rate ductility of metals.</a> J. Mat. Sci. 13 (8), 1835-1837 (1978).</li><li>Vogler, T. J., 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=Fragmentation+of+materials+in+expanding+tube+experiments.">Fragmentation of materials in expanding tube experiments.</a> Int. J. Imp. Eng. 29, 735-746 (2003).</li><li>Strand, O. T., Goosman, D. R., Martinez, C., Whitworth, T. L., Kuhlow, W. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Compact+system+for+high-speed+velocimetry+using+heterodyne+techniques.">Compact system for high-speed velocimetry using heterodyne techniques.</a> Rev. Sci. Inst. 77, 083108 (2006).</li><li>Ao, T., Dolan, D. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=SIRHEN:+A+data+reduction+program+for+photonic+Doppler+velocimetry+measurements.">SIRHEN: A data reduction program for photonic Doppler velocimetry measurements.</a> Sandia National Laboratories Report. , (2010).</li></ol>

The authors have nothing to disclose.

This method enables investigation of materials at high rates of tensile loading over a wide range of temperatures, from cryogenic to ~1,000 K, unique to this design. However, this adds certain challenges to the experimental setup and execution. Firstly, to optimize the temperature control the ogive insert needs to be machined from a suitable material. 4340 steel is used here, although any high-temperature high-hardness steel should suffice. Likewise, as the entire expansion drive is now originating from the polymer proje...

The dynamic failure of a material is an important aspect of its overall mechanical behavior, and has relevance to numerous industries including automotive, aerospace, and military to name a few. While failure at low strain-rates is typically studied through conventional tension tests, in which a long thin sample is loaded in tension from the ends, at high strain rates such a geometry/configuration requires a sample to be very small in order to maintain a pseudo-mechanical equilibrium throughout the test. At the appearance of a single crack, the surrounding material will be relaxed, effectively arresting the development of any adjacent failure sites. This limits the number of fractures that can be simultaneously observed in any one experiment, and prevents important information regarding the statistics of failure to be determined.
The expanding cylinder test is a well-established technique for characterizing the manner in which materials fail and fragment under high speed loading. In the test, a cylinder made of the material of interest is uniformly loaded along its inner circumference, launching a stress wave through the wall and causing the cylinder to expand. Soon this radial wave dissipates and a uniform tensile hoop stress around the circumference dominates. As the stress and strain rate is the same around the cylinder the fracture and fragmentation behavior is governed solely by the material&#8217;s properties. The test alleviates the aforementioned problem as the typically large sample circumferences promote initiation of multiple failure sites under uniform stress 1.
The main aim in developing this experimental technique was to enable the study of the role of temperature in the fracture and fragmentation behavior of an expanding cylinder. The control of the sample temperature will allow for investigation of how the dynamic tensile strength, fracture mechanism, and fragmentation behavior of the material is affected. For example in metals, an increase in temperature can cause a shift from brittle to ductile fracture, accommodating more plastic work before ultimately failing. Some materials such as Ti-6Al-4V can also exhibit adiabatic shear localization 2. While the sample deforms, the plastic work generates heat. If the rate of softening as a result of this temperature increase is greater than the rate of work hardening from the deformation, an instability can form where a large amount of plastic deformation occurs in a very localized band (adiabatic shear band). This response is promoted in Ti-6Al-4V due to its poor thermal conductivity, and can potentially limit its effectiveness for applications such as lightweight armor.
This new testing approach must satisfy two main criteria. Firstly, the method must produce a radial strain rate on the order of 104 sec-1, typically seen in ballistic and impact events, to allow comparison to previous studies employing more traditional loading schemes. Secondly, the drive mechanism needs to be unaffected by the sample temperature to ensure consistency between experiments. Initial cylinder expansion mechanisms used explosive charges, either simply filling the sample cylinder 3-5 directly or using an intermediate driver. In the latter case a buffer is used 6, where the sample is placed over a steel cylinder that in turn contains an explosive charge. The obvious limitation is that as the sample cylinder contains the drive material (in the form of the explosive) heating the cylinder will also heat the charge. While this may not directly cause initiation of the charge many types of explosive contain a polymeric binder material that will melt out from the sample cylinder. Likewise, some explosives become highly sensitive when cooled. This means that explosive drives are not suitable for temperature study. An alternative method uses the Lorentz force for expansion &#8212; the sample is placed over a driver coil 7, 8. A high current is injected into this driver coil (typically heavy gauge copper wire), inducing an opposite current in the sample. These opposing currents have associated magnetic fields which act against each other, the magnetic pressure driving the sample outwards from the inner face. Again, heating the material will adversely affect the copper drive coil inside the sample. Gas guns have been used for cylinder expansion since the late 1970s 9. In these experiments the material used for the insert in the cylinder is a polymer, the drive coming as a result of both the projectile and insert deforming at impact. This insert is typically a rubber or plastic 10, the strength and ductility of which will be severely affected by temperature. Heating will make the insert too soft, and cooling will make it behave in a brittle manner so it fails prematurely.
Unlike previous cylinder expansion techniques, the method described here is the first to provide a repeatable loading drive over a wide range of temperatures (100-1,000 K). Our technique is unique in the fact that the material used for driving the expansion (in our case the projectile) is separate from the cylinder until the point of impact. Consequently, it is unaffected by the initial temperature of the sample cylinder and provides a repeatable load.
The experimental geometry consists of a steel ogive mounted inside the target cylinder, with the tip located about halfway along the length of the cylinder. A single stage light gas gun is then used to launch a polycarbonate projectile with a concave face into the cylinder at velocities up to 1,000 m/sec-1. The axis of the target is cylinder is carefully aligned to the axis of the gas-gun barrel to facilitate a repeatable and uniform load. The impact and subsequent flow of the polycarbonate projectile around the pseudo-rigid steel ogive, drives the cylinder into expansion from the inside wall. The geometry of the ogive insert and the concave face of the projectile were carefully optimized using hydro-code computer simulations to generate the desired expansion of the cylinder. Using 4340 alloy steel for the ogive enables experimentation with the cylinder at temperature as its strength is much higher than the polycarbonate projectile over the temperature range of interest, ensuring the drive mechanism remains consistent. Ogives recovered from heated and cooled experiments only exhibit minimal deformation as a result of the impact.
The heating and cooling of the sample cylinder is accomplished by the installation of temperature control hardware into a machined recess in the rear of the ogive insert. For cooling the sample to cryogenic temperatures (~100 K), the recess in the ogive is sealed with an aluminum cap and liquid nitrogen is flowed through the cavity. As the target cylinder has a large contact area with the ogive the sample is cooled through conduction. To heat the target cylinder to temperatures approaching 1,000 K, a ceramic and NiChrome resistive heater is placed in the ogive recess. A high current power supply provides up to 1 kW, heating the ogive and cylinder. The cylinder and ogive are thermally isolated from the target mount in the single stage gas-gun through the use of MACOR ceramic spacers. The tank is also held under moderate vacuum (&#60;0.5 Torr) during the experiment which aids thermal manipulation.
In order to diagnose the fragmentation process of the cylinder, the experimental design includes multiple channels of frequency-conversion PDV, to measure the expansion velocity at points along the cylinder. PDV is a relatively new 11, optical fiber based interferometry technique which enables the measurement of surface velocities during highly dynamic events. During a PDV measurement, Doppler shifted light reflected from a moving surface of interest using a fiber-optic probe is combined with un-shifted light, creating a beat frequency that is directly proportional to the velocity of the moving surface. Essentially, a PDV system is a fast Michelson interferometer using advances in near-infrared (1,550 nm) communications technology to record beat frequencies in the GHz range. The mounting system for the 100 mm focal length PDV probes used in the current study ensures that they are isolated from the temperature of the cylinder and provides easy alignment. An additional advantage of using the 100 mm focal length probes is that they provide sufficient optical access to enable high speed photography to measure the expansion profile of the whole cylinder. The arrangement and location of the four probes, A-D, along the cylinder is shown in Figure 1. Two high speed cameras are employed here; a high speed video camera Phantom V16.10 operating at 250,000 fps and an IVV UHSi 12/24 framing camera, capturing 24 images. The IVV camera is backlit such that the cylinder is illuminated in silhouette enabling the radially expanding edge of the cylinder to be accurately tracked. The Phantom camera is front illuminated imaging the failure initiation and fragmentation process. The high speed photography can then be correlated with the velocimetry to give strain and strain rate along the full sample. The high speed imaging also allows for an accurate measure of failure strain and the fracture patterns along the surface.
The experimental technique presented in the following protocol section provides a means of controlling the sample temperature in an expanding cylinder experiment, through which different fracture mechanisms may be activated or suppressed. This technique will lead to a more comprehensive understanding of the role of temperature in dynamic loading scenarios.

<table><tbody><tr><td>1,550 nm CW Laser</td><td>NKT Photonics</td><td>Koheras Adjustik</td><td>x 2</td></tr><tr><td>1,550 nm Power Amplifier</td><td>NKT Photonics</td><td>Koheras Boostik HPA</td><td></td></tr><tr><td>Delay Generators</td><td>Quantum Composers</td><td>9500+ Digital Delay Pulse Generator</td><td>8 output version</td></tr><tr><td>Stanford Research Systems</td><td>DG535 Digital Delay Generator</td><td></td><td></td></tr><tr><td>16 Channel Digitiser</td><td>Agilent Technologies</td><td>U1056B Chassis + 4 X U1063A Digitiser</td><td></td></tr><tr><td>High Bandwidth Oscilloscopes</td><td>Teledyne LeCroy</td><td>WaveMaster 816Zi-A</td><td>Expansion Velocity, Gen 3 PDV</td></tr><tr><td>Tektronix</td><td>DPO71604C</td><td>Projectile Velocity, Gen 1 PDV</td><td></td></tr><tr><td>High Speed Imaging Systems</td><td>Vision Research</td><td>Phantom v16.10</td><td></td></tr><tr><td>Invisible Vision</td><td>IVV UHSi-24</td><td></td><td></td></tr><tr><td>Zeiss Optics</td><td>Planar T* 1,4/85</td><td>85 mm Prime Lens</td><td></td></tr><tr><td>Nikon</td><td>AF-S Nikkor 70-200 mm f/2.8 ED VR II</td><td>70-200 mm Telephoto Lens</td><td></td></tr><tr><td>Flash Lamp</td><td>Bowens</td><td>Gemini Pro 1500 W</td><td>x 2</td></tr><tr><td>PDV Probe</td><td>Laser 2000</td><td>LPF-04-1550-9/125-S-21.5-100-4.5AS-60-3A-3-3</td><td>x 4 (Custom order)</td></tr><tr><td>PDV System</td><td>Built in-house by the Institute of Shock Physics</td><td>Custom Build</td><td>3&lt;sup&gt;rd&lt;/sup&gt; Generation (Upshifted) 8 Channel Portable PDV System</td></tr><tr><td>Control Software</td><td>National Instruments</td><td>LabVIEW 2013</td><td></td></tr><tr><td>Control Hardware for heating</td><td>National Instruments</td><td>NI-DAQ 6009 USB</td><td></td></tr><tr><td>Heating Power Supply</td><td>BK Precision</td><td>BK1900</td><td></td></tr><tr><td>Thermocouple Logger</td><td>Pico Technology</td><td>TC-08</td><td></td></tr><tr><td>100 mm Single Stage Light Gas Gun</td><td>Physics Applications, Inc. (PAI)</td><td>Custom Build</td><td>Capable of at least 1,000 m/sec with ~2 kg projectile</td></tr><tr><td>Image analysis software</td><td>National Institutes of Health</td><td>ImageJ</td><td>Open source, free</td></tr><tr><td>Image analysis software</td><td>Mathworks</td><td>MATLAB r2014a</td><td>With image processing toolboxes</td></tr><tr><td>Material sectioning saw</td><td>Struers</td><td>Accutom-50</td><td></td></tr><tr><td>Electron Microscope</td><td>Zeiss</td><td>Auriga</td><td></td></tr><tr><td>Electron Backscatter Diffraction</td><td>Bruker</td><td>e-Flash 1000</td><td></td></tr><tr><td>EBSD software</td><td>Bruker</td><td>eSprit</td><td></td></tr></tbody></table>

a method for studying the temperature dependence of dynamic fracture and fragmentation

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform stress and strain rate. This can be produced by evenly loading the inner surface of a cylinder. Due to the axial symmetry, as the cylinder expands the wall is placed into a tensile hoop stress that is uniform around the circumference. While there are various techniques to generate this expansion such as explosives, electromagnetic drive, and existing gas gun techniques they are all limited in the fact that the sample cylinder must be at room temperature. We present a new method using a gas gun that facilitates experiments on cylinders from 150 K to 800 K with a consistent, repeatable loading. These highly diagnosed experiments are used to examine the effect of temperature on the fracture mechanisms responsible for failure, and their resulting influence on fragmentation statistics. The experimental geometry employs a steel ogive located inside the target cylinder, with the tip located about halfway in. A single stage light gas gun is then used to launch a polycarbonate projectile into the cylinder at 1,000 m/sec-1. The projectile impacts and flows around the rigid ogive, driving the sample cylinder from the inside. The use of a non-deforming ogive insert allows us to install temperature control hardware inside the rear of the cylinder. Liquid nitrogen (LN2) is used for cooling and a resistive high current load for heating. Multiple channels of upshifted photon Doppler velocimetry (PDV) track the expansion velocity along the cylinder enabling direct comparison to computer simulations, while High speed imaging is used to measure the strain to failure. The recovered cylinder fragments are also subject to optical and electron microscopy to ascertain the failure mechanism.

The quality of the data will firstly depend on the experimental timing. If the delays from trigger to impact are correct then the flash lamps will be producing enough light when the target cylinder begins to deform, enabling the high speed cameras to produce clear images. In this case the images from the framing camera will have a clear silhouetted edge that can be used to track the deformation of the whole cylinder. Software such as ImageJ can be used to extract lineout data for each frame, producing an image as in <str...

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A Method for Studying the Temperature Dependence of Dynamic Fracture and Fragmentation

Fracture and fragmentation are late stage phenomena in dynamic loading scenarios and are typically studied using explosives. We present a technique for driving expansion using a gas gun which uniquely enables control of both loading rate and sample temperature.

The dynamic fracture of a body is a late-stage phenomenon typically studied under simplified conditions, in which a sample is deformed under uniform ...

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8.5K Views.  Imperial College London. Fracture and fragmentation are late stage phenomena in dynamic loading scenarios and are typically studied using explosives. We present a technique for driving expansion using a gas gun which uniquely enables control of both loading rate and sample temperature.

Video: A Method for Studying the Temperature Dependence of Dynamic Fracture and Fragmentation

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

High-pressure, High-temperature Deformation Experiment Using the New Generation Griggs-type Apparatus

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature (&#62; 300 &#176;C). However, because of the low stress resolution of current solid-pressure-medium apparatuses, high-resolution measurements are today restricted to low-pressure deformation experiments in the gas-pressure-medium apparatus. A new generation of solid-medium piston-cylinder (&#34;Griggs-type&#34;) apparatus is here described. Able to perform high-pressure deformation experiments up to 5 GPa and designed to adapt an internal load cell, such a new apparatus offers the potential to establish a technological basis for high-pressure rheology. This paper provides video-based detailed documentation of the procedure (using the &#34;conventional&#34; solid-salt assembly) to perform high-pressure, high-temperature experiments with the newly designed Griggs-type apparatus. A representative result of a Carrara marble sample deformed at 700 &#176;C, 1.5 GPa and 10-5 s-1 with the new press is also given. The related stress-time curve illustrates all steps of a Griggs-type experiment, from increasing pressure and temperature to sample quenching when deformation is stopped. Together with future developments, the critical steps and limitations of the Griggs apparatus are then discussed.

Rock deformation needs to be quantified at high pressure. A description of the procedure to perform deformation experiments in a newly designed solid-medium Griggs-type apparatus is here given. This provides technological basis for future rheological studies at pressures up to 5 GPa.

In order to address geological processes at great depths, rock deformation should ideally be tested at high pressure (&#62; 0.5 GPa) and high temperature ...

Environment

Stress Distribution During Cold Compression of Rocks and Mineral Aggregates Using Synchrotron-based X-Ray Diffraction

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) coupled with synchrotron X-radiation. A cube-shaped sample assembly is prepared and compressed, at room temperature, by a set of four X-ray transparent sintered diamond anvils and two tungsten carbide anvils, in the lateral and the vertical planes, respectively. All six anvils are housed within a 250-ton hydraulic press and driven inward simultaneously by two wedged guide blocks. A horizontal energy dispersive X-ray beam is projected through and diffracted by the sample assembly. The beam is commonly in the mode of either white or monochromatic X-ray. In the case of white X-ray, the diffracted X-rays are detected by a solid-state detector array that collects the resulting energy dispersive diffraction pattern. In the case of monochromatic X-ray, the diffracted pattern is recorded using a two-dimensional (2-D) detector, such as an imaging plate or a charge-coupled device (CCD) detector. The 2-D diffraction patterns are analyzed to derive lattice spacings. The elastic strains of the sample are derived from the atomic lattice spacing within grains. The stress is then calculated using the predetermined elastic modulus and the elastic strain. Furthermore, the stress distribution in two-dimensions allow for understanding how stress is distributed in different orientations. In addition, a scintillator in the X-ray path yields a visible light image of the sample environment, which allows for the precise measurement of sample length changes during the experiment, yielding a direct measurement of volume strain on the sample. This type of experiment can quantify the stress distribution within geomaterials, which can ultimately shed light on the mechanism responsible for compaction. Such knowledge has the potential to significantly improve our understanding of key processes in rock mechanics, geotechnical engineering, mineral physics, and material science applications where compactive processes are important.

We report detailed procedures for compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus coupled with synchrotron X-radiation. Such experiments allow quantification of the stress distribution within samples, that ultimately sheds light on compaction processes in geomaterials.

We report detailed procedures for performing compression experiments on rocks and mineral aggregates within a multi-anvil deformation apparatus (D-DIA) ...

Laser-heating and Radiance Spectrometry for the Study of Nuclear Materials in Conditions Simulating a Nuclear Power Plant Accident

Major and severe accidents have occurred three times in nuclear power plants (NPPs), at Three Mile Island (USA, 1979), Chernobyl (former USSR, 1986) and Fukushima (Japan, 2011). Research on the causes, dynamics, and consequences of these mishaps has been performed in a few laboratories worldwide in the last three decades. Common goals of such research activities are: the prevention of these kinds of accidents, both in existing and potential new nuclear power plants; the minimization of their eventual consequences; and ultimately, a full understanding of the real risks connected with NPPs. At the European Commission Joint Research Centre&#39;s Institute for Transuranium Elements, a laser-heating and fast radiance spectro-pyrometry facility is used for the laboratory simulation, on a small scale, of NPP core meltdown, the most common type of severe accident (SA) that can occur in a nuclear reactor as a consequence of a failure of the cooling system. This simulation tool permits fast and effective high-temperature measurements on real nuclear materials, such as plutonium and minor actinide-containing fission fuel samples. In this respect, and in its capability to produce large amount of data concerning materials under extreme conditions, the current experimental approach is certainly unique. For current and future concepts of NPP, example results are presented on the melting behavior of some different types of nuclear fuels: uranium-plutonium oxides, carbides, and nitrides. Results on the high-temperature interaction of oxide fuels with containment materials are also briefly shown.

We present experiments in which real nuclear fuel, cladding, and containment materials are laser heated to temperatures beyond 3,000 K while their behavior is studied by radiance spectroscopy and thermal analysis. These experiments simulate, on a laboratory scale, the formation of a lava-phase following a nuclear reactor core meltdown.

Major and severe accidents have occurred three times in nuclear power plants (NPPs), at Three Mile Island (USA, 1979), Chernobyl (former USSR, 1986) and ...

Chemistry

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and increasing the recovery of coalbed methane. A visualized and constant-volume gas-solid coupling system is introduced here to investigate the influence of CO2 sorption on the physical and mechanical properties of coal. Being able to keep a constant volume and monitor the sample using a camera, this system offers the potential to improve instrument accuracy and analyze fracture evolution with a fractal geometry method. This paper provides all steps to perform a uniaxial compression experiment with a briquette sample in different CO2 pressures with the gas-solid coupling test system. A briquette, cold-pressed by raw coal and sodium humate cement, is loaded in high-pressure CO2, and its surface is monitored in real-time using a camera. However, the similarity between the briquette and the raw coal still needs improvement, and a flammable gas such as methane (CH4) cannot be injected for the test. The results show that CO2 sorption leads to peak strength and elastic modulus reduction of the briquette, and the fracture evolution of the briquette in a failure state indicates fractal characteristics. The strength, elastic modulus, and fractal dimension are all correlated with CO2 pressure but not with a linear correlation. The visualized and constant-volume gas-solid coupling test system can serve as a platform for experimental research about rock mechanics considering the multifield coupling effect.

A Uniaxial Compression Experiment with CO2-Bearing Coal Using a Visualized and Constant-Volume Gas-Solid Coupling Test System

This protocol demonstrates how to prepare a briquette sample and conduct a uniaxial compression experiment with a briquette in different CO2 pressures using a visualized and constant-volume gas-solid coupling test system. It also aims to investigate changes in terms of coal&#8217;s physical and mechanical properties induced by CO2 adsorption.

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and ...

Conducting Elevated Temperature Normal and Combined Pressure-Shear Plate Impact Experiments Via a Breech-end Sabot Heater System

A novel approach for conducting normal and/or combined pressure-shear plate impact experiments at test temperatures up to 1000 &#176;C is presented. The method enables elevated temperature plate-impact experiments aimed towards probing dynamic behavior of materials under thermomechanical extremes, while mitigating several special experimental challenges faced while performing similar experiments using the conventional plate impact approach. Custom adaptations are made to the breech-end of a single-stage gas-gun at Case Western Reserve University; these adaptations include a precision-machined extension piece made from SAE 4340 steel, which is strategically designed to mate the existing gun-barrel while providing a high tolerance match to the bore and keyway. The extension piece contains a vertical cylindrical heater-well, which houses a heater assembly. A resistive coil heater-head, capable of reaching temperatures of up 1200 &#176;C, is attached to a vertical stem with axial/rotational degrees of freedoms; this enables thin metal specimens held at the front-end of a heat-resistant sabot to be heated uniformly across the diameter to the desired test temperatures. By heating the flyer plate (in this case, the sample) at the breech-end of the gun-barrel instead of at the target-end, several critical experimental challenges can be averted. These include: 1) severe changes in the alignment of the target plate during heating due to the thermal expansion of the several constituents of the target holder assembly; 2) challenges that arise due to the diagnostics elements, (i.e., polymer holographic gratings, and optical probes) being too close to the heated target assembly; 3) challenges that arise for target plates with an optical window, where crucial tolerances between the sample, bond layer, and window become increasingly difficult to maintain at high temperatures; 4) in the case of combined compression-shear plate impact experiments, the need for high-temperature resistant diffraction gratings for the measurement of transverse particle velocity at the free surface of the target; and 5) limitations imposed on the impact velocity necessary for unambiguous interpretation of the measured free surface velocity versus time profile due to thermal softening and possibly yielding of the bounding target plates.By utilizing the adaptations mentioned above, we present results from a series of reverse geometry normal plate impact experiments on commercial purity aluminum at a range of sample temperatures. These experiments show decreasing particle velocities in the impacted state, which are indicative of material softening (decrease in post-yield flow stress) with increasing sample temperatures.

Here, we present a detailed protocol of a new approach for conducting elevated temperature reverse normal plate impact, and combined pressure-and-shear plate impact. The approach involves the use of a breech-end resistive coil heater to heat a sample held at the front-end of a heat-resistant sabot to the desired temperature.

A novel approach for conducting normal and/or combined pressure-shear plate impact experiments at test temperatures up to 1000 &#176;C is presented. The ...

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic glasses (MGs). Despite their amorphous nature, the identification of hyperfine interactions unveils faint structural modifications. For this purpose, we have employed two techniques that utilize nuclear resonance among nuclear levels of a stable 57Fe isotope, namely M&#246;ssbauer spectrometry and nuclear forward scattering (NFS) of synchrotron radiation. The effects of heat treatment upon (Fe2.85Co1)77Mo8Cu1B14 MG are discussed using the results of ex situ and in situ experiments, respectively. As both methods are sensitive to hyperfine interactions, information on structural arrangement as well as on magnetic microstructure is readily available. M&#246;ssbauer spectrometry performed ex situ describes how the structural arrangement and magnetic microstructure appears at room temperature after the annealing under certain conditions (temperature, time), and thus this technique inspects steady states. On the other hand, NFS data are recorded in situ during dynamically changing temperature and NFS examines transient states. The use of both techniques provides complementary information. In general, they can be applied to any suitable system in which it is important to know its steady state but also transient states.

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Here, we present a protocol to describe ex situ and in situ investigations of structural transformations in metallic glasses. We employed nuclear-based analytical methods which inspect hyperfine interactions. We demonstrate the applicability of M&#246;ssbauer spectrometry and nuclear forward scattering of synchrotron radiation during temperature-driven experiments.

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

The Role of Fabric in Frictional Properties of Phyllosilicate-Rich Tectonic Faults

Many rock deformation experiments used to characterize the frictional properties of tectonic faults are performed on powdered fault rocks or on bare rock surfaces. These experiments have been fundamental to document the frictional properties of granular mineral phases and provide evidence for crustal faults characterized by high friction. However, they cannot entirely capture the frictional properties of faults rich in phyllosilicates.
Numerous studies of natural faults have documented fluid-assisted reaction softening promoting the replacement of strong minerals with phyllosilicates that are distributed into continuous foliations. To study how these foliated fabrics influence the frictional properties of faults we have: 1) collected foliated phyllosilicate-rich rocks from natural faults; 2) cut the fault rock samples to obtain solid wafers 0.8-1.2 cm thick and 5 cm x 5 cm in area with the foliation parallel to the 5x5cm face of the wafer; 3) performed friction tests on both solid wafers sheared in their in situ geometry and powders, obtained by crushing and sieving and therefore disrupting the foliation of the same samples; 4) recovered the samples for microstructural studies from the post experiment rock samples; and 5) performed microstructural analyses via optical microscopy, scanning and transmission electron microscopy. 
Mechanical data show that the solid samples with well-developed foliation show significantly lower friction in comparison to their powdered equivalents. Micro- and nano-structural studies demonstrate that low friction results from sliding along the foliation surfaces composed of phyllosilicates. When the same rocks are powdered, frictional strength is high, because sliding is accommodated by fracturing, grain rotation, translation and associated dilation. Friction tests indicate that foliated fault rocks may have low friction even when phyllosilicates constitute only a small percentage of the total rock volume, implying that a significant number of crustal faults are weak.

Friction of phyllosilicates-rich faults sheared in their in situ geometry is significantly lower than friction of their powdered equivalents.

Many rock deformation experiments used to characterize the frictional properties of tectonic faults are performed on powdered fault rocks or on bare rock ...

Full-field Strain Measurements for Microstructurally Small Fatigue Crack Propagation Using Digital Image Correlation Method

A novel measurement approach is used to reveal the cumulative deformation field at a sub-grain level and to study the influence of microstructure on the growth of microstructurally small fatigue cracks. The proposed strain field analysis methodology is based on the use of a unique pattering technique with a characteristic speckle size of approximately 10 &#181;m. The developed methodology is applied to study the small fatigue crack behavior in body centered cubic (bcc) Fe-Cr ferritic stainless steel with a relatively large grain size allowing a high spatial measurement accuracy at the sub-grain level. This methodology allows the measurement of small fatigue crack growth retardation events and associated intermittent shear strain localization zones ahead of the crack tip. In addition, this can be correlated with the grain orientation and size. Thus, the developed methodology can provide a deeper fundamental understanding of the small fatigue crack growth behavior, required for the development of robust theoretical models for the small fatigue crack&#160;propagation in polycrystalline materials.

Microstructurally small fatigue crack growth behavior is investigated using a novel methodological approach combining crack growth rate measurement and strain-field analysis to reveal the cumulative deformation field at sub-grain level.

A novel measurement approach is used to reveal the cumulative deformation field at a sub-grain level and to study the influence of microstructure on the ...

Performing Microscope-Mounted Y-Shaped Cutting Tests

Y-shaped cutting has recently been shown to be a promising method by which to understand the threshold length scale and failure energy of a material, as well as its failure response in the presence of excess deformation energy. The experimental apparatus used in these studies was vertically oriented and required cumbersome steps to adjust the angle between the Y-shaped legs. The vertical orientation prohibits visualization in standard optical microscopes. This protocol presents a Y-shaped cutting apparatus that mounts horizontally over an existing inverted microscope stage, can be adjusted in three dimensions (X-Y-Z) to fall within the objective&#39;s field of view, and allows easy modification of the angle between the legs. The latter two features are new for this experimental technique. The presented apparatus measures the cutting force within 1 mN accuracy. When testing polydimethylsiloxane (PDMS), the reference material for this technique, a cutting energy of 132.96 J/m2 was measured (32&#176; leg angle, 75 g preload) and found to fall within the error of previous measurements taken with a vertical setup (132.9 J/m2 &#177; 3.4 J/m2). The approach applies to soft synthetic materials, tissues, or bio-membranes and may provide new insights into their behavior during failure. The list of parts, CAD files, and detailed instructions in this work provide a roadmap for the easy implementation of this powerful technique.

Y-shaped cutting measures fracture-relevant length scales and energies in soft materials. Previous apparatuses were designed for benchtop measurements. This protocol describes the fabrication and use of an apparatus that orients the setup horizontally and provides the fine positioning capabilities necessary for in situ viewing, plus failure quantification, via an optical microscope.

Y-shaped cutting has recently been shown to be a promising method by which to understand the threshold length scale and failure energy of a material, as ...

A Method for Studying the Temperature Dependence of Dynamic Fracture and Fragmentation

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