Name: visually based characterization of the incipient particle motion in regular substrates: from laminar to turbulent conditions
Uploaded: 2018-02-22T15:00:00
Description: Watch this Scientific Journal Video about Visually Based Characterization of the Incipient Particle Motion in Regular Substrates: From Laminar to Turbulent Conditions at JoVE.com

The authors are thankful to unknown referees for valuable advice and to Sukyung Choi, Byeongwoo Ko and Baekkyoung Shin for the collaboration in setting up the experiments. This work was supported by the Brain Busan 21 Project in 2017.

1. Incipient Particle Motion in the Creeping Flow Limit.
NOTE: The measurements are conducted in a rotational rheometer that has been modified for this specific application.
<ol>
	<li>Preparing the Rheometer.
	<ol>
		<li>Connect the air supply to the rheometer in order to avoid damaging the air bearings. Open the valve besides the air filters until a pressure of approximately 5 bars in the system is achieved.</li>
		<li>Connect the fluid circulator to the measuring plate. En...

We present two different experimental methods for characterizing the incipient particle motion as a function of the sediment bed geometry. For that purpose, we use a monolayer of spheres regularly arranged according to a triangular or quadratic symmetry in such a way that the geometrical parameter simplifies to a single geometry. In the creeping flow limit, we describe the experimental method using a rotational rotameter to induce the laminar shear flow as in previous studies39,<sup cla...

Incipient particle motion is encountered in a wide range of industrial and natural processes. Environmental examples include the initial process of sediment transport in river and oceans, bed erosion or dune formation among others 1,2,3. Pneumatic conveying4, removal of pollutants or cleaning of surfaces5,6 are typical industrial applications involving the onset of particle motion.
Due to the broad range of applications, the onset of particle motion has been extensively studied over a century, mostly under turbulent conditions7,8,9,10,11,12,13,14,15. Many experimental approaches have been applied to determine the threshold for the onset of motion. The studies include parameters such as the particle Reynolds number13,16,17,18,19,20, the relative flow submergence21,22,23,24 or geometrical factors as the angle of repose16,18,25, exposure to the flow26,27,28,29, relative grain protrusion29 or streamwise bed slope30.
The current data for the threshold including turbulent conditions are broadly scattered12,31 and the results often seem inconsistent24. This is mostly due to the inherent complexity of controlling or determining flow parameters under turbulent conditions13,14. Besides, the threshold for sediment motion strongly depends on the mode of motion, i.e. sliding, rolling or lifting17 and the criterion to characterize the incipient motion31. The latter may be ambiguous in an erodible sediment bed.
During the last decade, experimental researchers have studied incipient particle motion in laminar flows32,33,34,35,36,37,38,39,40,41,42,43,44, where the wide spectrum of length scales interacting with the bed is avoided45. In many practical scenarios implying sedimentation, the particles are quite small and the particle Reynolds number remains lower than about 546. On the other hand, laminar flows are able to generate geometric patterns as ripples and dunes as turbulent flows do42,47. Similitudes in both regimens have been shown to reflect analogies in the underlying physics47 so important insight for the particle transport can be obtained from a better controlled experimental system48.
In laminar flow, Charru et al. noticed that the local rearrangement of a granular bed of uniformly sized beads, so-called bed armouring, resulted in a progressive increase of the threshold for the onset of motion until saturated conditions were achieved32. Literature, however, reveals different thresholds for saturated conditions in irregularly arranged sediment beds depending on the experimental set-up36,44. This scattering may be due to the difficulty of controlling particle parameters such as orientation, protrusion level and compactness of the sediments.
The main goal of this manuscript is to describe in detail how to characterize the incipient motion of single spheres as a function of geometrical properties of the horizontal sediment bed. For that purpose, we use regular geometries, consisting of monolayers of fixed beads regularly arranged according to triangular or quadratic configurations. Regular substrates similar to that we use are found in applications such as for the template-assembly of particles in microfluidic assays49, self-assembly of microdevices in confined structured geometries50 or intrinsic particle-induced transport in microchannels51. More importantly, using regular substrates allows us to highlight the impact of local geometry and orientation and to avoid any dubiety about the role of the neighborhood.
In laminar flow, we observed that the critical Shields number increased by 50% only depending on the spacing between the substrate spheres and thus on the exposure of the bead to the flow38. Similarly, we found that the critical Shields number changed by up to a factor of two depending on the orientation of the substrate to the flow direction38. We noticed that immobile neighbors only affect the onset of the mobile bead if they were closer than about three particle diameters41. Triggered by the experiment findings, we have recently presented a rigorous analytical model that predicts the critical Shields number in the creeping flow limit40. The model covers the onset of motion from highly exposed to hidden beads.
The first part of this manuscript deals with the description of the experimental procedure used in previous studies at shear Reynolds number, Re*, lower than 1. The laminar flow is induced with a rotational rheometer with a parallel configuration. In this low Reynolds number limit, the particle is not supposed to experience any velocity fluctuation20 and the system matches the so-called hydraulically smooth flow where the particle is submerged within the viscous sublayer.
Once incipient motion at laminar flow is established, the role of turbulence can become clearer. Motivated by this idea, we introduce a novel experimental procedure in the second part of the protocol. Using a G&#246;ttingen low-speed wind tunnel with open jet test section, the critical Shields number can be determined in a wide range of Re* including the hydraulically transitional flow and the turbulent regime. The experimental results can provide important insight about how forces and torques act on a particle due to the turbulent flow depending on the substrate geometry. Besides, these results can be used as a benchmark for more sophisticated models at high Re* in a similar way that past work in laminar flow has been used to feed semi probabilistic models52 or to validate recent numerical models53. We present some representative examples of applications at Re* ranging from 40 to 150.
The incipient criterion is established as the motion of the single particle from its initial equilibrium position to the next one. Image processing is used to determine the mode of onset of motion, i.e. rolling, sliding, lifting39,41. For that purpose, the angle of rotation of mobile spheres that were manually marked is detected. The algorithm tracks the position of the marks and compares it with the center of the sphere. A preliminary set of experiments was conducted in both experimental set-ups to clarify that the critical Shields number remains independent of finite size effects of the set-up and relative flow submergence. The experimental methods are thus designed to exclude any other parameter dependent on the critical Shields number beyond Re* and geometrical properties of the sediment bed. The Re* is varied using different fluid-particle combinations. The critical Shields number is characterized as a function of the burial degree, <img alt="Equation 01" src="/files/ftp_upload/57238/57238eq001.jpg" />, defined by Martino et al.37 as <img alt="Equation 02" src="/files/ftp_upload/57238/57238eq002.jpg" /> where <img alt="Equation 03" src="/files/ftp_upload/57238/57238eq003.jpg" /> is the angle of repose, i.e. the critical angle at which motion occurs54, and <img alt="Equation 04" src="/files/ftp_upload/57238/57238eq004.jpg" /> is the exposure degree, defined as the ratio between the cross-sectional area effectively exposed to the flow to the total cross-sectional area of the mobile bead.

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		<tr height="21">
			<td height="21" style="height:21px;width:368px;">MCR 302 Rotational Rheometer</td>
			<td style="width:255px;">Antoon Par</td>
			<td style="width:471px;">Induction of shear laminar flow</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Measuring Plate PP25</td>
			<td style="width:255px;">Antoon Par</td>
			<td>Induction of shear laminar flow</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Peltier System P-PTD 200</td>
			<td style="width:255px;">Antoon Par</td>
			<td>Keep temperature of silicon oils constant in the system at laminar flow</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">Silicone oils with viscosities of approx. 10 and 100 mPas</td>
			<td style="width:255px;">Basildon Chemicals</td>
			<td>Fluid used to induced the shear in the particles</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Soda-lime glass beads of (405.9 &#177; 8.7) &#956;m</td>
			<td style="width:255px;">The Technical Glass Company</td>
			<td>Construction of the regular substrates for laminar flow conditions</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">Opto Zoom 70 Module 0.3x-2.2x</td>
			<td style="width:255px;">WEISS IMAGING AND SOLUTIONS GmbH</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">2 x TV-Tube 1.0x, D=35 mm, L=146.5 mm</td>
			<td style="width:255px;">WEISS IMAGING AND SOLUTIONS GmbH</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">UI-1220SE CMOS Camera</td>
			<td style="width:255px;">IDS Imaging Development Systems GmbH</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">UI-3590CP CMOS Camera</td>
			<td style="width:255px;">IDS Imaging Development Systems GmbH</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
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			<td height="21" style="height:21px;width:368px;">Volpi IntraLED 3 - LED light source&#160;</td>
			<td style="width:255px;">Volpi USA</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Active light guide diameter 5mm</td>
			<td style="width:255px;">Volpi USA</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">300 Watt Xenon Arc Lamp</td>
			<td style="width:255px;">Newport Corporation</td>
			<td>Imaging system for recording the bead motion in the rheometer</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">Wind-tunnel with open jet test section, G&#246;ttingen type&#160;</td>
			<td style="width:255px;">Tintschl BioEnergie und Str&#246;mungstechnik AG</td>
			<td>Induction of turbulent flow</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Glass spheres of (2.00 &#177; 0.10) mm</td>
			<td style="width:255px;">Gloches South Korea</td>
			<td>Construction of the regular substrates for turbulent flow conditions</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Alumina spheres of (5.00 &#177; 0.25) mm</td>
			<td style="width:255px;">Gloches South Korea</td>
			<td>Targeted bead for experiments</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">CTA Anemometer DISA 55M01</td>
			<td style="width:255px;">Disa Elektronik A/S&#160;</td>
			<td>Measurement of&#160; flow velocity in the wind tunnel</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Miniaure Wire Probe Type 55P15</td>
			<td style="width:255px;">Dantec Dynamics</td>
			<td>Measurement of&#160; flow velocity in the wind tunnel</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:368px;">HMO2022 Digital Oscilloscope, 2 Analogue. Ch., 200MHz</td>
			<td style="width:255px;">Rohde &#38; Schwarz</td>
			<td>Measurement of&#160; flow velocity in the wind tunnel</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Phantom Miro eX1 High-speed Camera</td>
			<td style="width:255px;">Vision Research IncVis</td>
			<td>Imaging system for recording the bead motion in the wind-tunnel</td>
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		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Canon ef 180mm f/3.5 l usm macro lens</td>
			<td style="width:255px;">Canon</td>
			<td>Imaging system for recording the bead motion in the wind-tunnel</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:368px;">Table LED Lamp</td>
			<td style="width:255px;">Gloches South Korea</td>
			<td>Imaging system for recording the bead motion in the wind-tunnel</td>
		</tr>
	</tbody>
</table>

visually based characterization of the incipient particle motion in regular substrates: from laminar to turbulent conditions

Two different experimental methods for determining the threshold of particle motion as a function of geometrical properties of the bed from laminar to turbulent flow conditions are presented. For that purpose, the incipient motion of a single bead is studied on regular substrates that consist of a monolayer of fixed spheres of uniform size that are regularly arranged in triangular and quadratic symmetries. The threshold is characterized by the critical Shields number. The criterion for the onset of motion is defined as the displacement from the original equilibrium position to the neighboring one. The displacement and the mode of motion are identified with an imaging system. The laminar flow is induced using a rotational rheometer with a parallel disk configuration. The shear Reynolds number remains below 1. The turbulent flow is induced in a low-speed wind tunnel with open jet test section. The air velocity is regulated with a frequency converter on the blower fan. The velocity profile is measured with a hot wire probe connected to a hot film anemometer. The shear Reynolds number ranges between 40 and 150. The logarithmic velocity law and the modified wall law presented by Rotta are used to infer the shear velocity from the experimental data. The latter is of special interest when the mobile bead is partially exposed to the turbulent flow in the so-called hydraulically transitional flow regime. The shear stress is estimated at onset of motion. Some illustrative results showing the strong impact of the angle of repose, and the exposure of the bead to shear flow are represented in both regimes.

Figure 1(a) represents a sketch of the experimental set-up used to characterize the critical Shields number in the creeping flow limit, Section 1 of the protocol. The measurements are conducted in a rotational rheometer that was modified for this specific application. A transparent Plexiglas plate of 70 mm in diameter was carefully fixed to a parallel plate of 25 mm in diameter. The inertia of the measuring system was therefore readjusted bef...

Watch this Scientific Journal Video about Visually Based Characterization of the Incipient Particle Motion in Regular Substrates: From Laminar to Turbulent Conditions at JoVE.com

Visually Based Characterization of the Incipient Particle Motion in Regular Substrates: From Laminar to Turbulent Conditions

Two different methods for characterizing the incipient particle motion of a single bead as a function of the sediment bed geometry from laminar to turbulent flow are presented.

Two different experimental methods for determining the threshold of particle motion as a function of geometrical properties of the bed from laminar to ...

The goal of this experimental procedure is to quantify the impact of sediment bed geometry on incipient particle motion by using regular substrates that consist of monolayers of fixed beads regularly arranged according to triangular or quadratic configurations. Incipient particle motion is found in a wide range of industrial applications such as cleaner surfaces, removal of pollutants, filtration processes, or microfluidics, including template assembly of microparticles. The main advantage of using regular substrates is that we can analyze the impact of a local sediment bed geometry orientation, avoiding any dubiety about the role of the neighborhood.We propose two different methods to cover a broad range of particle Reynolds number, from the creeping flow limit, to the hydraulically rough flow. The results of this method can also help us understand the impact of the local bed geometry in nature processes, such as sediment transport, or grain bed erosion. Visual demonstration of this method is important since the use of a rotational rheometer, for instance, may not be common for particle hydrodynamic applications.Demonstrating the method with the wind tunnel will be Jiwon Han, a graduate student from our lab that just finished her master thesis on this topic. These measurements take place in a rotational rheometer. The rheometer is modified to include a customized circular transparent container.There is an embedded microscope slide to improve imaging. The bottom of the container has a regular substrate, examples of which are in this schematic, which provides an overview of the setup, including its two digital cameras, and two light sources. Have the rheometer ready for normal operation.Then place a customized adapter on the rheometer plate, also mount the container with substrate on top of the plate. Ensure the microscope slide faces the camera. Start the rheometer and its software, initialize it, and set its temperature.Next, get the customized rotating disk. This is the 70 millimeter diameter transparent acrylic glass plate fixed to a 25 millimeter diameter plate. Mount this and set its height reference point.Then lift the rotating disk and remove it. Complete preparation by filling the container with silicon oil. Begin to work with the imaging system.This includes a CMOS camera and objective lens with an overhead view into the container. A second high speed camera has a side-view into the container. The view is through the microscope slide.Turn on and adjust the Xenon lamp and the LED to illuminate the container. Use imaging software in the CMOS camera to visualize the substrate. Adjust the vertical stage to bring it into focus.After focusing, identify the center of the substrate. Place a carefully marked soda-lined glass sphere at the position. Continue by remounting the rotating disk on the rheometer two millimeters above the height reference point.Finally, make any adjustments to the side-view camera. Enter the rotational speed range, program a linear increase in rotational speed, and start the measurements. Start recording a video sequence from both cameras, and observe the live video from one of them.When the bead displaces from its equilibrium position, stop the measurement and note the rotational speed, which is the critical rotating speed. Then, stop recording the videos. During data analysis, load recorded videos into a custom image processing routine to help determine the mode of incipient motion.Perform turbulent regime measurements in a customized low-speed wind tunnel. It has an open-jet test section with a regular substrate centered within it. Linear, vertical, and horizontal stages support an anemometer and other instrumentation in the test section.The high-speed camera with macro lens is mounted at one side. This schematic provides an overview of the equipment. Note that the anemometer signal is input to an oscilloscope and computer.Locate where on the substrate to place a marked alumina bead. Identify the point along the substrate's central axis and 110 millimeters from the leading edge and place the bead there. Use the high-speed camera, and adjust an LED light-source to achieve a clear, focused image of the bead and its marks.Start the wind tunnel's fan well below the approximate critical fan speed. Monitor the bead and increase the fan speed four to six RPM every 10 seconds. Start recording with the imaging software when close to incipient conditions.Stop increasing the fan speed when incipient motion occurs, and note the critical speed value, and stop the video. Again, for data analysis, use custom software to analyze the recorded video, and determine the mode of incipient motion of the bead. Now, work with the anemometer with a miniature hot-wire probe.Switch its control function to stand-by and adjust the resistance for an overheat ratio of 65%Remove the marked bead from the substrate. Move the anemometer to place the hot-wire probe in its initial position. To calibrate the anemometer, the probe should be in the free stream zone.Here, the probe must be at least 10 millimeters above the substrate. Run the probe, and start the fan at a rotational speed of 200 RPM. Then employ an impeller anemometer in the air stream.Read and record the stream-wise velocity from the impeller anemometer. In addition, read and record the hot-wire probe voltage on the oscilloscope. Repeat recording the anemometer readings for increments of 50 RPM in the rotational speed up to 450 RPM.Use the data to establish a calibration curve. Monitor the probe with the camera, and lower it as close as possible to the substrate surface without touching it. Start the fan at the mean speed for incipient motion and begin collecting probe data.After each data set, increase the height of the probe, and repeat data collection. These top-view snapshots are of a marked bead on a quadratic surface during incipient motion in laminar flow. Software tracks features on the particle and the center of mass.The data allow determination of the angle of rotation as a function of the trajectory, and closely follow the expectations of pure rolling motions indicated by the dotted line. These are analogous side-view snapshots for a marked alumina bead on a quadratic surface in turbulent flow. In this case, the bead seems to carry out a pure rolling motion only early in its motion.A plot of the time averaged stream-wise velocity profile, the circles, is possible using data from the constant temperature anemometer. Here, the solid line is a fit using the logarithmic log law, and the blue Xs are for a fit using the modified wall law. The shear velocity needed to determine the critical shields number is inferred from the fits.Here, both wall laws suggest similar values for the shear velocity. Here is a plot of the root mean square stream-wise velocity profile within a small height range. The measured viscus sub-layer is about 1/4 of a millimeter, indicating that the mobile bead is mainly exposed to a turbulent flow.Each measurement in the rheometer doesn't take more than five minutes if it is performed properly. Experiments in the wind tunnel, however, may take about five hours, since the measurement of the boundary layer is a complex process. The proper setting of the gap in the rheometer is critical to avoid any systematic error when calculating the critical shear rate and the critical shields numbers.In the wind tunnel, the animal with the calibration wants to be carefully conduct to determine the shear velocity. It is recommended to perform a calibration before and after measurement, to ensure that no significant changes occurred in the course of the measurement. Following the procedure in the wind tunnel, other criteria beyond the classical shields one can be used to signify incipient motion.The inputs or energy criteria can be adopted since the duration of events can be measured by thermal anemometer. The results can provide important insight into how forces and torques act on a particular due to turbulent flow depending on the substrate geometry. The results can be used as a benchmark for more sophisticated models.After watching this video, you should have a good understanding of how we can systematically quantify the inference of sediment bed geometry on the incipient particle motion.

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Equilibrium of a Particle

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Echo Particle Image Velocimetry

The transport of mass, momentum, and energy in fluid flows is ultimately determined by spatiotemporal distributions of the fluid velocity field.1 Consequently, a prerequisite for understanding, predicting, and controlling fluid flows is the capability to measure the velocity field with adequate spatial and temporal resolution.2 For velocity measurements in optically opaque fluids or through optically opaque geometries, echo particle image velocimetry (EPIV) is an attractive diagnostic technique to generate "instantaneous" two-dimensional fields of velocity.3,4,5,6 In this paper, the operating protocol for an EPIV system built by integrating a commercial medical ultrasound machine7 with a PC running commercial particle image velocimetry (PIV) software8 is described, and validation measurements in Hagen-Poiseuille (i.e., laminar pipe) flow are reported.
For the EPIV measurements, a phased array probe connected to the medical ultrasound machine is used to generate a two-dimensional ultrasound image by pulsing the piezoelectric probe elements at different times. Each probe element transmits an ultrasound pulse into the fluid, and tracer particles in the fluid (either naturally occurring or seeded) reflect ultrasound echoes back to the probe where they are recorded. The amplitude of the reflected ultrasound waves and their time delay relative to transmission are used to create what is known as B-mode (brightness mode) two-dimensional ultrasound images. Specifically, the time delay is used to determine the position of the scatterer in the fluid and the amplitude is used to assign intensity to the scatterer. The time required to obtain a single B-mode image, t, is determined by the time it take to pulse all the elements of the phased array probe. For acquiring multiple B-mode images, the frame rate of the system in frames per second (fps) = 1/&delta;t. (See 9 for a review of ultrasound imaging.)
For a typical EPIV experiment, the frame rate is between 20-60 fps, depending on flow conditions, and 100-1000 B-mode images of the spatial distribution of the tracer particles in the flow are acquired. Once acquired, the B-mode ultrasound images are transmitted via an ethernet connection to the PC running the PIV commercial software. Using the PIV software, tracer particle displacement fields, D(x,y)[pixels], (where x and y denote horizontal and vertical spatial position in the ultrasound image, respectively) are acquired by applying cross correlation algorithms to successive ultrasound B-mode images.10 The velocity fields, u(x,y)[m/s], are determined from the displacements fields, knowing the time step between image pairs, &Delta;T[s], and the image magnification, M[meter/pixel], i.e., u(x,y) = MD(x,y)/&Delta;T. The time step between images &Delta;T = 1/fps + D(x,y)/B, where B[pixels/s] is the time it takes for the ultrasound probe to sweep across the image width. In the present study, M = 77[&mu;m/pixel], fps = 49.5[1/s], and B = 25,047[pixels/s]. Once acquired, the velocity fields can be analyzed to compute flow quantities of interest.

An echo particle image velocimetry (EPIV) system capable of acquiring two-dimensional fields of velocity in optically opaque fluids or through optically opaque geometries is described, and validation measurements in pipe flow are reported.

The transport of mass, momentum, and energy in fluid flows is ultimately determined by spatiotemporal distributions of the fluid velocity field.1 ...

Patterning via Optical Saturable Transitions - Fabrication and Characterization

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical Saturable Transitions (POST). In this technique the chemical properties of organic photochromic molecules that undergo single-photon reactions are exploited, enabling rapid top-down nanopatterning over large areas at low light intensities, thereby, allowing for the circumvention of the far-field diffraction barrier.4 Simple, cost-effective, high throughput and resolution alternatives to nanopatterning are being explored, such as, two-photon polymerization5,6, beam pen lithography (BPL)7, scanning electron beam lithography (SEBL), and focused ion beam (FIB) patterning. However, multi-photon approaches require high light intensities, which limit their potential for high throughput and offer low image contrast. Although, electron and ion beam lithographic processes offer increased resolution, the serial nature of the process is limited to slow writing speeds, which also prevents patterning of features over large areas. Beam-pen lithography is an approach towards parallel near-field optical lithography. However, the gap between the source of the beam and the surface of the photoresist needs to be controlled extremely precisely for good pattern uniformity and this is very challenging to accomplish for large arrays of beams. Patterning via Optical Saturable Transitions (POST) is an alternative optical nanopatterning technique for patterning sub-wavelength features1-3. Since this technique uses single photons instead of electrons, it is extremely fast and does not require high light intensities1-3, opening the door to massive parallelization.

We report that the diffraction limit of conventional optical lithography can be overcome by exploiting the transitions of organic photochromic derivatives induced by their photoisomerization at low light intensities.1-3 This paper outlines our fabrication technique and two locking mechanisms, namely: dissolution of one photoisomer and electrochemical oxidation.

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical ...

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

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

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

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

Characterization of Nanocrystal Size Distribution using Raman Spectroscopy with a Multi-particle Phonon Confinement Model

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The common techniques used for the size analysis are transmission electron microscopy (TEM), X-ray diffraction (XRD) and photoluminescence spectroscopy (PL). These techniques, however, are not suitable for analyzing the nanocrystal size distribution in a fast, non-destructive and a reliable manner at the same time. Our aim in this work is to demonstrate that size distribution of semiconductor nanocrystals that are subject to size-dependent phonon confinement effects, can be quantitatively estimated in a non-destructive, fast and reliable manner using Raman spectroscopy. Moreover, mixed size distributions can be separately probed, and their respective volumetric ratios can be estimated using this technique. In order to analyze the size distribution, we have formulized an analytical expression of one-particle PCM and projected it onto a generic distribution function that will represent the size distribution of analyzed nanocrystal. As a model experiment, we have analyzed the size distribution of free-standing silicon nanocrystals (Si-NCs) with multi-modal size distributions. The estimated size distributions are in excellent agreement with TEM and PL results, revealing the reliability of our model.

We demonstrate how to determine the size distribution of semiconductor nanocrystals in a quantitative manner using Raman spectroscopy employing an analytically defined multi-particle phonon confinement model. Results obtained are in excellent agreement with the other size analysis techniques like transmission electron microscopy and photoluminescence spectroscopy.

Analysis of the size distribution of nanocrystals is a critical requirement for the processing and optimization of their size-dependent properties. The ...

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 ...

In Vitro Culture of Epicardial Cells From Mouse Embryonic Heart

During embryogenesis, the epicardial contribution to coronary vasculature development has been very well established. Cells derived from the epicardium differentiate into smooth muscle cells, fibroblasts and endothelial cells that contribute to the formation of coronary vessels. Here we have established an in vitro culture method for embryonic epicardial cells. Using genetic labelling, we have demonstrated that the majority of the migrating cells in our explant culture are of epicardial origin. Epicardial explant cells also retain the expression of epicardial markers (Wt1 and Tbx18). Furthermore, we provide evidence that epicardial explant cells undergo epithelial to mesenchymal transition (EMT), migrate and differentiate into smooth muscle cells after Transforming growth factor beta 1 (TGF-&#946;1) treatment in a manner indistinguishable from that of epicardial cells in vivo. In conclusion, we provide a novel method for the culture of embryonic epicardial cells, which will help to explore the role of specific genes in epicardial cell biology.

In Vitro Culture of Epicardial Cells From Mouse Embryonic Heart

The epicardium is an essential source of multipotent cardiovascular progenitor cells and paracrine factors that are required for cardiovascular development and regeneration. We describe here a method to culture mouse embryonic epicardial cells.

During embryogenesis, the epicardial contribution to coronary vasculature development has been very well established. Cells derived from the epicardium ...

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 ...

Effective Analysis of Human Exposure Conditions with Body-worn Dosimeters in the 2.4 GHz Band

A well-defined experimental procedure is put forward to evaluate maximum exposure conditions in a worst-case scenario whilst avoiding the uncertainties caused by the use of personal exposimeters (PEMs) as measuring devices: the body shadow effect (BSE), the limited sensitivity range, and the non-identification of the radiation source. An upper bound for exposure levels to EMF in several indoor enclosures has been measured and simulated. The frequency used for the study is 2.4 GHz, as it is the most commonly used band in indoor communications. Although recorded values are well below the International Commission for Non-Ionizing Radiation Protection (ICNIRP) reference levels, there is a particular need to provide reliable exposure levels within particularly sensitive environments. In terms of electromagnetic field (EMF) exposure, limits established in national and international standards for health protection have been set for unperturbed exposure conditions; that is, for real and objective exposure data that have not been altered in any way.

This study describes a protocol to measure exposure levels in the 2.4 GHz band, avoiding the uncertainties caused by the use of personal exposimeters as measuring devices. These alterations of the exposure levels should be taken into account, especially in compliance testing, where exposure limits are defined from non-perturbed data.

A well-defined experimental procedure is put forward to evaluate maximum exposure conditions in a worst-case scenario whilst avoiding the uncertainties ...

The Diffusion of Passive Tracers in Laminar Shear Flow

A simple method to experimentally observe and measure the dispersion of a passive tracer in a laminar fluid flow is described. The method consists of first injecting fluorescent dye directly into a pipe filled with distilled water and allowing it to diffuse across the cross-section of the pipe to obtain a uniformly distributed initial condition. Following this period, the laminar flow is activated with a programmable syringe pump to observe the competition of advection and diffusion of the tracer through the pipe. Asymmetries in the tracer distribution are studied and correlations between the pipe cross-section and the shape of the distribution is shown: thin channels (aspect ratio &#60;&#60; 1) produce tracers arriving with sharp fronts and tapering tails (front-loaded distributions), while thick channels (aspect ratio ~1) present the opposite behavior (back-loaded distributions). The experimental procedure is applied to capillary tubes of various geometries and is particularly relevant to microfluidic applications by dynamical similarity.

A protocol for the study of the diffusion of passive tracers in laminar pressure-driven flow is presented. The procedure is applicable to various capillary pipe geometries.

A simple method to experimentally observe and measure the dispersion of a passive tracer in a laminar fluid flow is described. The method consists of ...

Pore-scale Imaging and Characterization of Hydrocarbon Reservoir Rock Wettability at Subsurface Conditions Using X-ray Microtomography

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to characterize the complex wetting conditions of hydrocarbon reservoir rock using pore-scale three-dimensional X-ray imaging at subsurface conditions. In this work, heterogeneous carbonate reservoir rocks, extracted from a very large producing oil field, have been used to demonstrate the protocol. The rocks are saturated with brine and oil and aged over three weeks at subsurface conditions to replicate the wettability conditions that typically exist in hydrocarbon reservoirs (known as mixed-wettability). After the brine injection, high-resolution three-dimensional images (2 &#181;m/voxel) are acquired and then processed and segmented. To calculate the distribution of the contact angle, which defines the wettability, the following steps are performed. First, fluid-fluid and fluid-rock surfaces are meshed. The surfaces are smoothed to remove voxel artefacts, and in situ contact angles are measured at the three-phase contact line throughout the whole image. The main advantage of this method is its ability to characterize in situ wettability accounting for pore-scale rock properties, such as rock surface roughness, rock chemical composition, and pore size. The in situ wettability is determined rapidly at hundreds of thousands of points. 
The method is limited by the segmentation accuracy and X-ray image resolution. This protocol could be used to characterize the wettability of other complex rocks saturated with different fluids and at different conditions for a variety of applications. For example, it could help in determining the optimal wettability that could yield an extra oil recovery (i.e., designing brine salinity accordingly to obtain higher oil recovery) and to find the most efficient wetting conditions to trap more CO2 in subsurface formations.

This protocol is presented to characterize the complex wetting conditions of an opaque porous medium (hydrocarbon reservoir rock) using three-dimensional images obtained by X-ray microtomography at subsurface conditions.

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to ...