Name: simulation of the planetary interior differentiation processes in the laboratory
Uploaded: 2013-11-15T17:30:00
Description: Watch this Scientific Journal Video about Simulation of the Planetary Interior Differentiation Processes in the Laboratory at JoVE.com

This work was supported by NASA grant NNX11AC68G and the Carnegie Institution of Washington. I thank Chi Zhang for his assistance with data collection. I also thank Anat Shahar and Valerie Hillgren for helpful reviews of this manuscript.

1. Prepare Starting Materials and Sample Chambers
<ol>
	<li>Prepare two types of starting materials, (1) a mixture of natural silicate olivine and metallic iron powder with 10 wt% sulfur (metal/silicate ratios ranging from 4 to 30 wt%) for simulating percolation of liquid iron alloy in a solid silicate matrix during the initial core formation of a small planetary body, and (2) a homogeneous mixture of finely-grounded pure iron and iron sulfide for determining the planetary inner core crystallization.</li>
	<li>Grind th...

<ol>
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J., Williams, Q., Lognonn&#233;, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Seismic+detection+of+the+Lunar+core.">Seismic detection of the Lunar core.</a> Science. 331, 309-312 (2011).</li><li>Li, J., Fei, Y., Carlson, R. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Experimental+constraints+on+core+composition.">Experimental constraints on core composition.</a> Geochemistry of the Mantle and Core. , 521-546 (2007).</li><li>Bertka, C. M., Fei, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mineralogy+of+the+Martian+interior+up+to+core-mantle+boundary+pressures.">Mineralogy of the Martian interior up to core-mantle boundary pressures.</a> Journal of Geophysical Research. 102, 5251-5264 (1997).</li><li>Tateno, S., Hirose, K., Ohishi, Y., Tatsumi, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+structure+of+iron+in+Earth's+inner+core.">The structure of iron in Earth's inner core.</a> Science. 330, 359-361 (2010).</li><li>Prakapenka, V. B., Kubo, A., 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=Advanced+flat+top+laser+heating+system+for+high+pressure+research+at+GSECARS:+application+to+the+melting+behavior+of+germanium.">Advanced flat top laser heating system for high pressure research at GSECARS: application to the melting behavior of germanium.</a> High Pressure Research. 28, 225-235 (2008).</li><li>Minarik, W. G., Ryerson, F. J., Watson, E. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Textural+entrapment+of+core-forming+melts.">Textural entrapment of core-forming melts.</a> Science. 272, 530-533 (1996).</li><li>Terasaki, H., Frost, D. J., Rubie, D. 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The techniques for the multi-anvil experiments are well established, generating stable pressure and temperature for an extended period of run time and producing relatively large sample volume. It is a powerful tool to simulate the interior processes of planets, especially for experiments, such as melt percolation, that require certain sample volume. The limitation is the maximum achievable pressure, up to 27 GPa with tungsten carbide (WC) anvils, reaching the core pressures of Mars and Mercury, but far too low pressure t...

Terrestrial planets such as the Earth, Venus, Mars, and Mercury are differentiated planetary bodies consisting of a silicate mantle and a metallic core. The modern planet formation model suggests that the terrestrial planets were formed from collisions of Moon-to-Mars-sized planetary embryos grown from km-sized or larger planetesimals through gravitational interactions1-2. The planetesimals were likely differentiated already once the metallic iron alloys reached melting temperature due to heating from sources such as radioactive decay of short-lived isotopes such as 26Al and 60Fe, impact, and release of potential energy3. It is important to understand how the liquid metal percolated through a silicate matrix during the early differentiation.
Planet differentiation could proceed through efficient liquid-liquid separation or by percolation of liquid metal in a solid silicate matrix, depending on the size and interior temperature of the planetary bodies. The percolation of liquid metal in the solid silicate matrix is likely a dominant process in the initial differentiation when the temperature is not high enough to melt the entire planetary body. The efficiency of percolation depends on the dihedral angle, determined by the interfacial energies of the solid-solid and solid-liquid interfaces. We can simulate this process in the laboratory by conducting high-pressure and high-temperature experiments on a mixture of iron alloy and silicate. Recent studies4-7&#160;have investigated the wetting ability of liquid iron alloys in a solid silicate matrix at high pressure and temperature. They used a conventional method to measure the relative frequency distributions of apparent dihedral angles between the quenched liquid metal and silicate grains on the polished cross-sections for determination of the true dihedral angle. The conventional method yields relatively large uncertainties in the measured dihedral angle and possible bias depending on the sampling statistics. Here we present a new imaging technique to visualize the distribution of liquid metal in the silicate matrix in three dimensions (3D) by combination of FIB milling and high-resolution field-emission SEM imaging. The new imaging technique provides precise determination of the dihedral angle and quantitative measure of the volume fraction and connectivity of the liquid phase.
The Earth&#39;s core was formed in a relatively short time (&#60;100 million years)8, presumably in a liquid state at its early history. Mars and Mercury also have liquid cores based on solar tidal deformation from the Mars Global Surveyor radio tracking data9&#160;and radar speckle patterns tied to the planetary rotation10, respectively. Thermal evolution models and high-pressure melting experiments on core materials further support a liquid Martian core11-12. Recent Messenger spacecraft data provide additional evidence for a liquid core of Mercury13. Even the small Moon likely has a small liquid core based on recent reanalysis of Appollo lunar seismograms14. Liquid planetary cores are consistent with high accretion energy at the early stage of planet formation. Subsequent cooling may lead to formation of solid inner core for some planets. Seismic data have revealed that the Earth consists of a liquid outer core and a solid inner core. The formation of the inner core has important implications for the dynamics of the core driven by thermal and compositional convections and the generation of the magnetic field of the planet.
Solidification of the inner core is controlled by the melting temperature of core materials and the thermal evolution of the core. Core formation of terrestrial planets shared similar accretion paths and the chemical composition of the cores is considered to be dominated by iron with about 10 weight % light elements such as sulfur (S), silicon (Si), oxygen (O), carbon (C), and hydrogen (H)15. It is essential to have knowledge of the melting relations in the systems relevant to the core, such as Fe-FeS, Fe-C, Fe-FeO, Fe-FeH, and Fe-FeSiat high pressure, in order to understand the composition of the planetary cores. In this study, we will demonstrate experiments conducted in the multi-anvil device and diamond-anvil cell, mimicking the conditions of the planetary cores. The experiments provide information on the crystallization sequence and element partitioning between solid and liquid metal, leading to a better understanding for the requirements of the inner core crystallization and the distribution of light elements between the crystalline inner core and liquid out core. To extend the melting relationships to very high pressures, we have developed new techniques to analyze the quenched samples recovered from laser-heated diamond-anvil cell experiments. With precision FIB milling of the laser-heating spot, we determine melting using quenching texture criteria imaged with high-resolution SEM and quantitative chemical analysis with a silicon drift detector at submicron spatial resolution.
Here we outline two sets of experiments to mimic planetary core formation by percolation of metallic melt in silicate matrix during early accretion and inner core crystallization by subsequent cooling. The simulation is aimed to understand the two important processes during the evolution of planetary core.

<table border="0" cellpadding="0" cellspacing="0" width="352">
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	<tbody> 
		<tr height="43" style="height:32.25pt">
			<td class="xl63" height="43" style="height:32.25pt;width:66pt" width="88">Multi-anvil apparatus</td>
			<td class="xl63" style="border-left:none;width:66pt" width="88">Geophysical Lab</td>
			<td class="xl63" style="border-left:none;width:66pt" width="88">Home Builder</td>
			<td class="xl63" style="border-left:none;width:66pt" width="88"> </td>
		</tr>
		<tr height="43" style="height:32.25pt">
			<td class="xl63" height="43" style="height:32.25pt;border-top:none;
 width:66pt" width="88">Diamond-anvil cell</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Geophysical Lab</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Home Builder</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88"> </td>
		</tr>
		<tr height="64" style="height:48.0pt">
			<td class="xl63" height="64" style="height:48.0pt;border-top:none;
 width:66pt" width="88">Laser-heating system</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">APS GSECARS</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Designed by beamline staff</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88"> Public beamline</td>
		</tr>
		<tr height="43" style="height:32.25pt">
			<td class="xl63" height="43" style="height:32.25pt;border-top:none;
 width:66pt" width="88">FIB/SEM Crossbeam</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Carl Zeiss Ltd.</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Auriga</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88"> </td>
		</tr>
		<tr height="64" style="height:48.0pt">
			<td class="xl63" height="64" style="height:48.0pt;border-top:none;
 width:66pt" width="88">Avizo 3D software</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">VSG</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88">Fire for materials science</td>
			<td class="xl63" style="border-top:none;border-left:none;width:66pt" width="88"> </td>
		</tr>
	</tbody>
</table>

simulation of the planetary interior differentiation processes in the laboratory

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to that layered structure, (1) percolation of liquid metal in a solid silicate matrix by planet differentiation, and (2) inner core crystallization by subsequent planet cooling. We conduct high-pressure and high-temperature experiments to simulate both processes in the laboratory. Formation of percolative planetary core depends on the efficiency of melt percolation, which is controlled by the dihedral (wetting) angle. The percolation simulation includes heating the sample at high pressure to a target temperature at which iron-sulfur alloy is molten while the silicate remains solid, and then determining the true dihedral angle to evaluate the style of liquid migration in a crystalline matrix by 3D visualization. The 3D volume rendering is achieved by slicing the recovered sample with a focused ion beam (FIB) and taking SEM image of each slice with a FIB/SEM crossbeam instrument. The second set of experiments is designed to understand the inner core crystallization and element distribution between the liquid outer core and solid inner core by determining the melting temperature and element partitioning at high pressure. The melting experiments are conducted in the multi-anvil apparatus up to 27 GPa and extended to higher pressure in the diamond-anvil cell with laser-heating. We have developed techniques to recover small heated samples by precision FIB milling and obtain high-resolution images of the laser-heated spot that show melting texture at high pressure. By analyzing the chemical compositions of the coexisting liquid and solid phases, we precisely determine the liquidus curve, providing necessary data to understand the inner core crystallization process.

We have conducted a series of experiments using mixtures of San Carlos olivine and Fe-FeS metal alloy with different metal-silicate ratios, as the starting materials. The S content of the metal is 10 weight % S. Here we show some representative results from high-pressure experiments performed at 6 GPa and 1,800 &#176;C, using well-calibrated multi-anvil assemblies15. Under the experimental conditions, the Fe-FeS metal alloy is completely molten and the silicate (San Carlos olivine) remains crystalline. The pur...

Watch this Scientific Journal Video about Simulation of the Planetary Interior Differentiation Processes in the Laboratory at JoVE.com

Simulation of the Planetary Interior Differentiation Processes in the Laboratory

The high-pressure and high-temperature experiments described here mimic planet interior differentiation processes. The processes are visualized and better understood by high-resolution 3D imaging and quantitative chemical analysis.

A planetary interior is under high-pressure and high-temperature conditions and it has a layered structure. There are two important processes that led to ...

simulation-planetary-interior-differentiation-processes

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Revealing Dynamic Processes of Materials in Liquids Using Liquid Cell Transmission Electron Microscopy

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted significant interests across the research fields of materials science, physics, chemistry and biology. The key enabling technology is a liquid cell. We fabricate liquid cells with thin viewing windows through a sequential microfabrication process, including silicon nitride membrane deposition, photolithographic patterning, wafer etching, cell bonding, etc. A liquid cell with the dimensions of a regular TEM grid can fit in any standard TEM sample holder. About 100 nanoliters reaction solution is loaded into the reservoirs and about 30 picoliters liquid is drawn into the viewing windows by capillary force. Subsequently, the cell is sealed and loaded into a microscope for in situ imaging. Inside the TEM, the electron beam goes through the thin liquid layer sandwiched between two silicon nitride membranes. Dynamic processes of nanoparticles in liquids, such as nucleation and growth of nanocrystals, diffusion and assembly of nanoparticles, etc., have been imaged in real time with sub-nanometer resolution. We have also applied this method to other research areas, e.g., imaging proteins in water. Liquid cell TEM is poised to play a major role in revealing dynamic processes of materials in their working environments. It may also bring high impact in the study of biological processes in their native environment.

We have developed a self-contained liquid cell, which allows imaging through liquids using a transmission electron microscope. Dynamic processes of nanoparticles in liquids can be revealed in real time with sub-nanometer resolution.

The recent development for in situ transmission electron microscopy, which allows imaging through liquids with high spatial resolution, has attracted ...

Flame Experiments at the Advanced Light Source: New Insights into Soot Formation Processes

The following experimental protocols and the accompanying video are concerned with the flame experiments that are performed at the Chemical Dynamics Beamline of the Advanced Light Source (ALS) of the Lawrence Berkeley National Laboratory1-4. This video demonstrates how the complex chemical structures of laboratory-based model flames are analyzed using flame-sampling mass spectrometry with tunable synchrotron-generated vacuum-ultraviolet (VUV) radiation. This experimental approach combines isomer-resolving capabilities with high sensitivity and a large dynamic range5,6. The first part of the video describes experiments involving burner-stabilized, reduced-pressure (20-80 mbar) laminar premixed flames. A small hydrocarbon fuel was used for the selected flame to demonstrate the general experimental approach. It is shown how species&#8217; profiles are acquired as a function of distance from the burner surface and how the tunability of the VUV photon energy is used advantageously to identify many combustion intermediates based on their ionization energies. For example, this technique has been used to study gas-phase aspects of the soot-formation processes, and the video shows how the resonance-stabilized radicals, such as C3H3, C3H5, and i-C4H5, are identified as important intermediates7. The work has been focused on soot formation processes, and, from the chemical point of view, this process is very intriguing because chemical structures containing millions of carbon atoms are assembled from a fuel molecule possessing only a few carbon atoms in just milliseconds. The second part of the video highlights a new experiment, in which an opposed-flow diffusion flame and synchrotron-based aerosol mass spectrometry are used to study the chemical composition of the combustion-generated soot particles4. The experimental results indicate that the widely accepted H-abstraction-C2H2-addition (HACA) mechanism is not the sole molecular growth process responsible for the formation of the observed large polycyclic aromatic hydrocarbons (PAHs).

Gas sampling from laboratory-scale flames with online analysis of all species by mass spectrometry is a powerful method to investigate the complex mixture of chemical compounds occurring during combustion processes. Coupled with tunable soft ionization via synchrotron-generated vacuum-ultraviolet radiation, this technique provides isomer-resolved information and potentially fragment-free mass spectra.

The following experimental protocols and the accompanying video are concerned with the flame experiments that are performed at the Chemical Dynamics ...

Laboratory Drop Towers for the Experimental Simulation of Dust-aggregate Collisions in the Early Solar System

For the purpose of investigating the evolution of dust aggregates in the early Solar System, we developed two vacuum drop towers in which fragile dust aggregates with sizes up to ~10 cm and porosities up to 70% can be collided. One of the drop towers is primarily used for very low impact speeds down to below 0.01 m/sec and makes use of a double release mechanism. Collisions are recorded in stereo-view by two high-speed cameras, which fall along the glass vacuum tube in the center-of-mass frame of the two dust aggregates. The other free-fall tower makes use of an electromagnetic accelerator that is capable of gently accelerating dust aggregates to up to 5 m/sec. In combination with the release of another dust aggregate to free fall, collision speeds up to ~10 m/sec can be achieved. Here, two fixed high-speed cameras record the collision events. In both drop towers, the dust aggregates are in free fall during the collision so that they are weightless and match the conditions in the early Solar System.

We present a technique to achieve low-velocity to intermediate-velocity collisions between fragile dust aggregates in the laboratory. For this purpose, two vacuum drop-tower setups have been developed that allow collision velocities between &#60;0.01 and ~10 m/sec. The collision events are recorded by high-speed imaging.

For the purpose of investigating the evolution of dust aggregates in the early Solar System, we developed two vacuum drop towers in which fragile dust ...

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and non-destructively reveals the hydrogen density distribution at surfaces, at interfaces, and in the volume of solid materials with high depth resolution. The technique applies a 15N ion beam of 6.385 MeV provided by an electrostatic accelerator and specifically detects the 1H isotope in depths up to about 2 &#956;m from the target surface. Surface H coverages are measured with a sensitivity in the order of ~1013 cm-2 (~1% of a typical atomic monolayer density) and H volume concentrations with a detection limit of ~1018 cm-3 (~100 at. ppm). The near-surface depth resolution is 2-5 nm for surface-normal 15N ion incidence onto the target and can be enhanced to values below 1 nm for very flat targets by adopting a surface-grazing incidence geometry. The method is versatile and readily applied to any high vacuum compatible homogeneous material with a smooth surface (no pores). Electrically conductive targets usually tolerate the ion beam irradiation with negligible degradation. Hydrogen quantitation and correct depth analysis require knowledge of the elementary composition (besides hydrogen) and mass density of the target material. Especially in combination with ultra-high vacuum methods for in-situ target preparation and characterization, 1H(15N,&#945;&#947;)12C NRA is ideally suited for hydrogen analysis at atomically controlled surfaces and nanostructured interfaces. We exemplarily demonstrate here the application of 15N NRA at the MALT Tandem accelerator facility of the University of Tokyo to (1) quantitatively measure the surface coverage and the bulk concentration of hydrogen in the near-surface region of a H2 exposed Pd(110) single crystal, and (2) to determine the depth location and layer density of hydrogen near the interfaces of thin SiO2 films on Si(100).

We illustrate the application of 1H(15N,&#945;&#947;)12C resonant nuclear reaction analysis (NRA) to quantitatively evaluate the density of hydrogen atoms on the surface, in the volume, and at an interfacial layer of solid materials. The near-surface hydrogen depth profiling of a Pd(110) single crystal and of SiO2/Si(100) stacks is described.

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and ...

Simulation of Human-induced Vibrations Based on the Characterized In-field Pedestrian Behavior

For slender and lightweight structures, vibration serviceability is a matter of growing concern, often constituting the critical design requirement. With designs governed by the dynamic performance under human-induced loads, a strong demand exists for the verification and refinement of currently available load models. The present contribution uses a 3D inertial motion tracking technique for the characterization of the in-field pedestrian behavior. The technique is first tested in laboratory experiments with simultaneous registration of the corresponding ground reaction forces. The experiments include walking persons as well as rhythmical human activities such as jumping and bobbing. It is shown that the registered motion allows for the identification of the time variant pacing rate of the activity. Together with the weight of the person and the application of generalized force models available in literature, the identified time-variant pacing rate allows to characterize the human-induced loads. In addition, time synchronization among the wireless motion trackers allows identifying the synchronization rate among the participants. Subsequently, the technique is used on a real footbridge where both the motion of the persons and the induced structural vibrations are registered. It is shown how the characterized in-field pedestrian behavior can be applied to simulate the induced structural response. It is demonstrated that the in situ identified pacing rate and synchronization rate constitute an essential input for the simulation and verification of the human-induced loads. The main potential applications of the proposed methodology are the estimation of human-structure interaction phenomena and the development of suitable models for the correlation among pedestrians in real traffic conditions.

A protocol is presented for the characterization of the in-field pedestrian behavior and the simulation of the resulting structural response. Field-tests demonstrate that the in situ identified pacing rate and synchronization rate among the participants constitute an essential input for the simulation and verification of the human-induced loads.

For slender and lightweight structures, vibration serviceability is a matter of growing concern, often constituting the critical design requirement. With ...

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 ...

Wicking Tests for Unidirectional Fabrics: Measurements of Capillary Parameters to Evaluate Capillary Pressure in Liquid Composite Molding Processes

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify their influence on void formation in composite parts. Wicking in a fibrous medium described by the Washburn equation was considered equivalent to a flow under the effect of capillary pressure according to the Darcy law. Experimental tests for the characterization of wicking were conducted with both carbon and flax fiber reinforcement. Quasi-unidirectional fabrics were then tested by means of a tensiometer to determine the morphological and wetting parameters along the fiber direction. The procedure was shown to be promising when the morphology of the fabric is unchanged during capillary wicking. In the case of carbon fabrics, the capillary pressure can be calculated. Flax fibers are sensitive to moisture sorption and swell in water. This phenomenon has to be taken into account to assess the wetting parameters. In order to make fibers less sensitive to water sorption, a thermal treatment was carried out on flax reinforcements. This treatment enhances fiber morphological stability and prevents swelling in water. It was shown that treated fabrics have a linear wicking trend similar to those found in carbon fabrics, allowing for the determination of capillary pressure.

An experimental method to measure geometrical parameters and the apparent advancing contact angles describing capillary wicking in unidirectional synthetic and natural fabrics is proposed. These parameters are mandatory for the determination of the capillary pressures that must be taken into account for liquid composite molding (LCM) applications.

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify ...

Characterization of Ultra-fine Grained and Nanocrystalline Materials Using Transmission Kikuchi Diffraction

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and nanocrystalline materials. The traditional techniques associated with scanning electron microscopy (SEM), such as electron backscatter diffraction (EBSD), do not possess the required spatial resolution due to the large interaction volume between the electrons from the beam and the atoms of the material. Transmission electron microscopy (TEM) has the required spatial resolution. However, due to a lack of automation in the analysis system, the rate of data acquisition is slow which limits the area of the specimen that can be characterized. This paper presents a new characterization technique, Transmission Kikuchi Diffraction (TKD), which enables the analysis of the microstructure of UFG and nanocrystalline materials using an SEM equipped with a standard EBSD system. The spatial resolution of this technique can reach 2 nm. This technique can be applied to a large range of materials that would be difficult to analyze using traditional EBSD. After presenting the experimental set up and describing the different steps necessary to realize a TKD analysis, examples of its use on metal alloys and minerals are shown to illustrate the resolution of the technique and its flexibility in term of material to be characterized.

This paper provides a detailed method to characterize the microstructure of ultra-fine grained and nanocrystalline materials using a scanning electron microscope equipped with a standard electron backscatter diffraction system. Metal alloys and minerals presenting refined microstructures are analyzed using this technique, showing the diversity of its possible applications.

One of the challenges in microstructure analysis nowadays resides in the reliable and accurate characterization of ultra-fine grained (UFG) and ...

Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued development of nanocrystalline metals. Despite these efforts, the transition of these materials from the lab bench to actual applications has been blocked by the inability to produce large scale parts that retain the desired nanocrystalline microstructures. Following the development of a method proven to stabilize the nanosized grain structure to temperatures approaching that of the melting point for the given metal, the US Army Research Laboratory (ARL) has progressed to the next stage in the development of these materials - namely the production of large scale parts suitable for testing and evaluation in a range of relevant test environments. This report provides a broad overview of the ongoing efforts in the processing, characterization, and consolidation of these materials at ARL. In particular, focus is placed on the methodology used for producing the nanocrystalline metal powders, in both small and large-scale amounts, that are at the center of ongoing research efforts.

This paper provides a brief overview of the ongoing efforts at the Army Research Laboratory on the processing of bulk nanocrystalline metals with an emphasis on the methodologies used for the production of the novel metal powders.

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued ...

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 ...