Caution: Consult all relevant material safety data sheets. Chemicals used for the tests are toxic and carcinogenic. Use personal protective equipment (safety glasses, gloves, lab coat, full-length pants, and closed-toe shoes).
1. Setup for Tests
<ol>
	<li>Preparation of samples
	<ol>
		<li>Cut strips of fabric along the direction perpendicular to the fibers (in order to test wicking in the fiber direction). 
		NOTE: The lengths of the strips are calculated in order to obtain a defined fiber volume ratio. For carbon fabrics, to obtain Vf = 40%, the length of the strips was 150 mm. For untreated and treated flax, to achieve the same Vf, the length was 365 mm. The width of each strip will be equal to the height of sample holder, which is 20 mm (Figure 1).</li>
		<li>Roll the strips tightly to allow their insertion into the cylindrical sample holder of R = 6 mm.</li>
		<li>Add a thin paper filter between the sample holder and the sample reinforcements (in order to suppress the effect of the sample holder on the wicking). The maximum thickness of the paper filter should be 0.1 mm.</li>
		<li>Insert the sample into the cylinder and screw the drilled cap at the bottom and the piston at the top in order to ensure compaction.</li>
		<li>Clamp the sample holder with the fabric to the tensiometer.</li>
	</ol>
	</li>
	<li>Preparation of liquids
	<ol>
		<li>Fill a vessel with the liquid test and place it into the specific receptacle of the tensiometer. Use vessels made of borosilicate glass and with a diameter of 70 mm.</li>
		<li>For the first test (step 2.1), use n-hexane. For the second test (step 2.3), use water. Ensure that the liquid in the vessel reaches a height of at least 12 mm.</li>
	</ol>
	</li>
	<li>Experimental parameters
	<ol>
		<li>Set the surface detection threshold to 8 mg and the translation speed of the liquid vessel at 0.5 mm/s for detection of the liquid.</li>
	</ol>
	</li>
</ol>
2. Wicking tests
NOTE: After the preparation of samples and the setup of the tensiometer parameters, the wicking tests can start. The liquid vessel moves up until the liquid is in contact with the sample holder. Then, liquid rises into the sample holder, and the tensiometer measures the squared liquid mass gain over time. Data are recorded by the software provided with the tensiometer. One curve of mass against time is then visualized for each wicking test.
<ol>
	<li>Initial test for determining the geometric factor:
	<ol>
		<li>Use a totally-wetting liquid (for which the contact angle is 0&#176;), such as n-hexane.</li>
		<li>Stop the wicking test when the visualized curve achieves a constant value. This indicates that the liquid has reached the top of the sample holder and thus that the wicking is complete.</li>
		<li>Fit the linear trend of the wicking curve (m2(t)) with the Washburn equation: 
		<img alt="Equation 3" src="/files/ftp_upload/55059/image003.jpg" />&#160;&#160;&#160;&#160;&#160;&#160;&#160;&#160;(3) 
		Since the advancing contact angle is supposed 0&#176; with n-hexane, from the slope of linear fit, determine the geometric constant, C (mm5). 
		NOTE: All tests were carried out under standard conditions at 20 &#176;C. A change in temperature will modify the liquid surface tension and the results.</li>
	</ol>
	</li>
	<li>Cleaning of sample holder for the following tests 
	NOTE: After removing the wet fabric, the sample holder has to be cleaned perfectly to prevent errors in the following measurements.
	<ol>
		<li>Immerse the sample holder in a vessel with sulfochromic acid (50% of a saturated solution of potassium dichromate and 50% of concentrated sulfuric acid) for 30 sec.</li>
		<li>Rinse it with distilled water and then dry it.</li>
	</ol>
	</li>
	<li>Second test for determining the apparent advancing contact angle
	<ol>
		<li>Use the liquid for which the advancing contact angle has to be measured with a new, identical, and dry fabric sample. 
		NOTE: Water was used in order to validate the method.</li>
		<li>Stop the wicking test when the visualized curve achieves a constant value. This indicates that the liquid has reached the top of the sample holder and that the capillary rise is complete.</li>
		<li>Fit the linear part of the wicking curve (m2(t)) with the Washburn equation (Equation 3), since the constant, C, is already known due to the first test (step 2.1), with the slope of linear fit determining the advancing contact angle, &#952;a (&#176;). 
		NOTE: All tests were carried out under standard conditions at 20 &#176;C. A change in temperature will modify the liquid surface tension and the results.</li>
	</ol>
	</li>
	<li>Evaluation of the liquid weight contribution due to the sample holder 
	NOTE: The tensiometer, as a microbalance, measures the total mass of liquid, including both the liquid ascending in the fabric and the contribution of the external meniscus on the sample holder and the wicking in the filter. Those contributions must be isolated.
	<ol>
		<li>Put the same amount of filter paper as used in step 1.1.3 into the sample holder and repeat steps 2.1.1-2.1.2.</li>
		<li>Subtract the constant value obtained (m2) from the data recorded in step 2.1.3 and shift the curve to assess the correct evaluation of the geometric constant, C.</li>
		<li>Fill the sample holder with only the filter paper and repeat steps 2.3.1-2.3.2.</li>
		<li>Subtract the constant value obtained (m2) from the data recorded in step 2.3.3 and shift the curve to assess the correct evaluation of the advancing contact angle, &#952;a.</li>
	</ol>
	</li>
</ol>

<ol>
	<li>Lawrence, J. M., Neacsu, V., Advani, S. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modeling+the+impact+of+capillary+pressure+and+air+entrapment+on+fiber+tow+saturation+during+resin+infusion+in+lcm.">Modeling the impact of capillary pressure and air entrapment on fiber tow saturation during resin infusion in lcm.</a> Compos Part A: Appl Sci Manuf. 40 (8), 1053-1064 (2009).</li><li>Ravey, C., Ruiz, E., Trochu, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+the+optimal+impregnation+velocity+in+resin+transfer+molding+by+capillary+rise+experiments+and+infrared+thermography.">Determination of the optimal impregnation velocity in resin transfer molding by capillary rise experiments and infrared thermography.</a> Compos Sci Technol. 99, 96-102 (2014).</li><li>Verrey, J., Michaud, V., M&#229;nson, J. -. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Dynamic+capillary+effects+in+liquid+composite+moulding+with+non-crimp+fabrics.">Dynamic capillary effects in liquid composite moulding with non-crimp fabrics.</a> Compos Part A: Appl Sci Manuf. 37 (1), 92-102 (2006).</li><li>Abouorm, L., Moulin, N., Bruchon, J., Drapier, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Monolithic+approach+of+Stokes-+Darcy+coupling+for+LCM+process+modelling.">Monolithic approach of Stokes- Darcy coupling for LCM process modelling.</a> Key Eng Mater. 554, 447-455 (2013).</li><li>Washburn, E. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Note+on+a+method+of+determining+the+distribution+of+pore+sizes+in+a+porous+material.">Note on a method of determining the distribution of pore sizes in a porous material.</a> Proc Natl Acad Sci USA. , 115-116 (1921).</li><li>Pucci, M. F., Liotier, P. -. J., Drapier, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Capillary+effects+on+flax+fibers-modification+and+characterization+of+the+wetting+dynamics.">Capillary effects on flax fibers-modification and characterization of the wetting dynamics.</a> Compos Part A: Appl Sci Manuf. 77, 257-265 (2015).</li><li>Darcy, H., Dalmont, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Les fontaines publiques de la ville de Dijon: exposition et application. , (1856).</li><li>Pucci, M. F., Liotier, P. -. J., Drapier, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Capillary+wicking+in+a+fibrous+reinforcement-orthotropic+issues+to+determine+the+capillary+pressure+components.">Capillary wicking in a fibrous reinforcement-orthotropic issues to determine the capillary pressure components.</a> Compos Part A: Appl Sci Manuf. 77, 133-141 (2015).</li><li>Pucci, M. F., Liotier, P. -. J., Drapier, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Capillary+wicking+in+flax+fabrics+-+effects+of+swelling+in+water.">Capillary wicking in flax fabrics - effects of swelling in water.</a> Colloids Surf A: Physicochem Eng Aspects. 498, 176-184 (2016).</li><li>Nguyen, V. H., Lagard&#232;re, M., Park, C. H., Panier, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Permeability+of+natural+fiber+reinforcement+for+liquid+composite+molding+processes.">Permeability of natural fiber reinforcement for liquid composite molding processes.</a> J Mater Sci. 49 (18), 6449-6458 (2014).</li><li>Stuart, T., McCall, R., Sharma, H., Lyons, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Modelling+of+wicking+and+moisture+interactions+of+flax+and+viscose+fibres.">Modelling of wicking and moisture interactions of flax and viscose fibres.</a> Carbohydr Polym. 123, 359-368 (2015).</li></ol>

The authors have nothing to disclose.

The critical steps in the protocol relate to the preparation of the samples. Firstly, the rolled sampled have to be tight in order to make the assumption of a homogeneous fiber volume ratio. If there is a tightness gradient in the sample, the Washburn equation5,6 cannot be used to fit the wicking curves. In addition, the boundary conditions between the fabric and the sample holder are difficult to control. Thus, the filter paper (1.1.3) must also be carefully ins...

During impregnation of fibrous reinforcements in liquid composite molding (LSM) processes, the resin flow is driven by a pressure gradient. Capillary effects have an additional effect that can compete with the pressure gradient, depending on the process parameters. Their influence on the process thus has to be evaluated1,2. This can be done by defining an apparent capillary pressure, Pcap, modifying the initial pressure gradient3. This parameter may subsequently be inserted into numerical models in order to simulate flows during processes and to accurately predict void formation4.
The spontaneous impregnation of a fabric by a liquid (wicking) can be described by the Washburn equation5. Originally, the Washburn equation described the capillary rise of a liquid in a tube. This equation was then extended for porous structures, such as fibrous reinforcements, that can be approximated to a capillary tube network. Considering a cylindrical sample holder with a radius, R, filled with a porous medium, the Washburn equation was modified in the form of squared mass gain (m&#178;(t)) over time, as follows6:
<img alt="Equation 1" src="/files/ftp_upload/55059/image001.jpg" />&#160;&#160;&#160;&#160;&#160;&#160;&#160;&#160;(1)
where c is a parameter that accounts for tortuosity, &#7773; is the mean pore radius, and &#949; = 1-Vf is the porosity (Vf being the fiber volume ratio). All parameters in the square brackets concern the morphology and configuration of the porous medium, and they can be consolidated into a constant, C, referred to as the &#34;geometric porous medium factor.&#34; The other parameters express the dependence of wicking on the interactions between the medium and the liquid (through &#961;, &#951;, and &#947;L, which are, respectively, the density, viscosity, and surface tension of the liquid, and through &#952;a, an apparent advancing contact angle).
In parallel, the flow through a porous medium is usually modelled with the well-known Darcy law7, which relates an equivalent fluid velocity, vD, to the pressure drop through the permeability of the medium, K, and the liquid viscosity, &#951;. This equation also allows for the expression of the mass gain over a square root of time and thus for the consideration of the equivalence between the two equations. From this equivalence between the Washburn equation and the Darcy law, the capillary pressure was then defined as follows8:
<img alt="Equation 2" src="/files/ftp_upload/55059/image002.jpg" />&#160;&#160;&#160;&#160;&#160;&#160;&#160;&#160;(2)
Here, the main focus is to describe the experimental procedure to measure the geometric factors and the apparent advancing contact angles for unidirectional fabrics, with the aim of determining the capillary pressure. This method relies on using a tensiometer to perform wicking tests (Figure 1). A tensiometer is a microbalance with a resolution of 10 &#181;g that measures the liquid mass either forming a meniscus around a solid or ascending a fibrous medium. Wicking tests were carried out considering a one-dimensional characterization (direction along the fibers)8,9. Quasi-unidirectional fabrics used to validate the procedure were carbon uni-directional (UD) fabrics at a Vf = 40%. Once the method was validated, flax fabrics were submitted to a thermal treatment that modifies the wetting behavior of fibers6, and wicking tests were performed with different fiber volume ratios (from 30% to 40%) for both untreated and treated flax fabrics. To determine morphological and wetting parameters, at least two wicking tests are mandatory: the first one with a totally-wetting liquid, like n-hexane, to determine C (Equation 1), and the second one with the liquid of interest, to determine the apparent advancing contact angle once C is known. In the first approach, water was used to evaluate the procedure.
This method can be applied to different fabrics and liquids, allowing for the evaluation of the influence of material geometry (morphology of fabrics), porosity (different fiber volume ratios), and viscosity and surface tension of liquid on the capillary impregnation phenomena. It is obvious that the procedure according to the Washburn theory (Equation 1) can be adopted only if wicking curves (m&#178;(t)) recorded by the tensiometer have a linear trend. This means that the parameters in Equation 1 must remain constant during the entire wicking process. If this is not the case, as for flax reinforcements in water, because fibers undergo swelling10,11, the Washburn equation should be modified to include the effect of swelling in order to describe the tests properly9. Treated fabrics were found to be less sensitive to water sorption9. Geometric factors and wetting parameters can be measured from linear fits, allowing for the calculation of the capillary pressure, Pcap.

<table border="0" cellpadding="0" cellspacing="0" width="700">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Carbon UD fabrics</td>
			<td style="width:167px;">Hexcel&#160;</td>
			<td style="width:151px;">48580</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Flax UD fabrics</td>
			<td style="width:167px;">Libeco</td>
			<td style="width:151px;">FLAXDRY UD 180</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">n-Hexane</td>
			<td style="width:167px;">Sigma Aldrich</td>
			<td style="width:151px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Sulfochromic acid</td>
			<td style="width:167px;">home made</td>
			<td style="width:151px;"></td>
			<td>toxic and corrosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Filter paper</td>
			<td style="width:167px;">Dataphysic</td>
			<td style="width:151px;">FP11</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Tensiometer</td>
			<td style="width:167px;">Dataphysic</td>
			<td style="width:151px;">DCAT11</td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

Curves of mass gain during wicking obtained with the tensiometer for carbon and untreated and treated flax fabrics are shown in Figures 2 and 3. All curves are shown after the subtraction of both weights of the external meniscus due to the sample holder and filter paper and are shifted to zero.
It is possible to observe from the plots in Figure 2 that, with both n-hexane and wat...

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

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 ...

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8.7K Views.  Mines Saint-Étienne. 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.

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

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.

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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 ...

Fabrication and Visualization of Capillary Bridges in Slit Pore Geometry

A procedure for creating and imaging capillary bridges in slit-pore geometry is presented. High aspect ratio hydrophobic pillars are fabricated and functionalized to render their top surfaces hydrophilic. The combination of a physical feature (the pillar) with a chemical boundary (the hydrophilic film on the top of the pillar) provides both a physical and chemical heterogeneity that pins the triple contact line, a necessary feature to create stable long but narrow capillary bridges. The substrates with the pillars are attached to glass slides and secured into custom holders. The holders are then mounted onto four axis microstages and positioned such that the pillars are parallel and facing each other. The capillary bridges are formed by introducing a fluid in the gap between the two substrates once the separation between the facing pillars has been reduced to a few hundred micrometers. The custom microstage is then employed to vary the height of the capillary bridge. A CCD camera is positioned to image either the length or the width of the capillary bridge to characterize the morphology of the fluid interface. Pillars with widths down to 250 &#181;m and lengths up to 70 mm were fabricated with this method, leading to capillary bridges with aspect ratios (length/width) of over 1001.

A procedure for creating and imaging capillary bridges in slit-pore geometry is presented. The creation of capillary bridges relies on the formation of pillars to provide a directional physical and chemical heterogeneity to pin the fluid. Capillary bridges are formed and manipulated using microstages and visualized using a CCD camera.

A procedure for creating and imaging capillary bridges in slit-pore geometry is presented. High aspect ratio hydrophobic pillars are fabricated and ...

Single Plane Illumination Module and Micro-capillary Approach for a Wide-field Microscope

A module for light sheet or single plane illumination microscopy (SPIM) is described which is easily adapted to an inverted wide-field microscope and optimized for 3-dimensional cell cultures, e.g., multi-cellular tumor spheroids (MCTS). The SPIM excitation module shapes and deflects the light such that the sample is illuminated by a light sheet perpendicular to the detection path of the microscope. The system is characterized by use of a rectangular capillary for holding (and in an advanced version also by a micro-capillary approach for rotating) the samples, by synchronous adjustment of the illuminating light sheet and the objective lens used for fluorescence detection as well as by adaptation of a microfluidic system for application of fluorescent dyes, pharmaceutical agents or drugs in small quantities. A protocol for working with this system is given, and some technical details are reported. Representative results include (1) measurements of the uptake of a cytostatic drug (doxorubicin) and its partial conversion to a degradation product, (2) redox measurements by use of a genetically encoded glutathione sensor upon addition of an oxidizing agent, and (3) initiation and labeling of cell necrosis upon inhibition of the mitochondrial respiratory chain. Differences and advantages of the present SPIM module in comparison with existing systems are discussed.

A module for single plane illumination microscopy (SPIM) is described which is easily adapted to an inverted wide-field microscope and optimized for 3-dimensional cell cultures. The sample is located within a rectangular capillary, and via a microfluidic system fluorescent dyes, pharmaceutical agents or drugs can be applied in small quantities.

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Capillary-based Centrifugal Microfluidic Device for Size-controllable Formation of Monodisperse Microdroplets

Here, we demonstrate a simple method for the rapid production of size-controllable, monodisperse, W/O microdroplets using a capillary-based centrifugal microfluidic device. W/O microdroplets have recently been used in powerful methods that enable miniaturized chemical experiments. Therefore, developing a versatile method to yield monodisperse W/O microdroplets is needed. We have developed a method for generating monodisperse W/O microdroplets based on a capillary-based centrifugal axisymmetric co-flowing microfluidic device. We succeeded in controlling the size of microdroplets by adjusting the capillary orifice. Our method requires equipment that is easier-to-use than with other microfluidic techniques, requires only a small volume (0.1-1 &#181;l) of sample solution for encapsulation, and enables the production of hundreds of thousands number of W/O microdroplets per second. We expect this method will assist biological studies that require precious biological samples by conserving the volume of the samples for rapid quantitative analysis biochemical and biological studies.

Here, we demonstrate a simple production method for size-controllable, monodisperse, water-in-oil (W/O) microdroplets using a capillary-based centrifugal microfluidic device. This method requires only a small sample volume and enables high-yield production. We expect this method will be useful for rapid biochemical and cellular analyses.

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Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

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

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

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

Magnet Assisted Composite Manufacturing: A Flexible New Technique for Achieving High Consolidation Pressure in Vacuum Bag/Lay-Up Processes

This work demonstrates a protocol to improve the quality of composite laminates fabricated by wet lay-up vacuum bag processes using the recently developed magnet assisted composite manufacturing (MACM) technique. In this technique, permanent magnets are utilized to apply a sufficiently high consolidation pressure during the curing stage. To enhance the intensity of the magnetic field, and thus, to increase the magnetic compaction pressure, the magnets are placed on a magnetic top plate. First, the entire procedure of preparing the composite lay-up on a magnetic bottom steel plate using the conventional wet lay-up vacuum bag process is described. Second, placement of a set of Neodymium-Iron-Boron permanent magnets, arranged in alternating polarity, on the vacuum bag is illustrated. Next, the experimental procedures to measure the magnetic compaction pressure and volume fractions of the composite constituents are presented. Finally, methods used to characterize microstructure and mechanical properties of composite laminates are discussed in detail. The results prove the effectiveness of the MACM method in improving the quality of wet lay-up vacuum bag laminates. This method does not require large capital investment for tooling or equipment and can also be used to consolidate geometrically complex composite parts by placing the magnets on a matching top mold positioned on the vacuum bag.

A new technique for applying consolidation pressure on the vacuum bag lay-up to fabricate composite laminates is described. The goal of this protocol is to develop a simple, cost-effective technique to improve the quality of laminates fabricated by the wet lay-up vacuum bag method.

This work demonstrates a protocol to improve the quality of composite laminates fabricated by wet lay-up vacuum bag processes using the recently developed ...

Cutting Procedures, Tensile Testing, and Ageing of Flexible Unidirectional Composite Laminates

Many body armor designs incorporate unidirectional (UD) laminates. UD laminates are constructed of thin (&#60;0.05 mm) layers of high-performance yarns, where the yarns in each layer are oriented parallel to each other and held in place using binder resins and thin polymer films. The armor is constructed by stacking the unidirectional layers in different orientations. To date, only very preliminary work has been performed to characterize the ageing of the binder resins used in unidirectional laminates and the effects on their performance. For example, during the development of the conditioning protocol used in the National Institute of Justice Standard-0101.06, UD laminates showed visual signs of delamination and reductions in V50, which is the velocity at which half of the projectiles are expected to perforate the armor, after ageing. A better understanding of the material property changes in UD laminates is necessary to comprehend the long-term performance of armors constructed from these materials. There are no current standards recommended for mechanically interrogating unidirectional (UD) laminate materials. This study explores methods and best practices for accurately testing the mechanical properties of these materials and proposes a new test methodology for these materials. Best practices for ageing these materials are also described.

The goal of the study was to develop protocols to prepare consistent specimens for accurate mechanical testing of high-strength aramid or ultra-high-molar-mass polyethylene-based flexible unidirectional composite laminate materials and to describe protocols for performing artificial ageing on these materials.

Many body armor designs incorporate unidirectional (UD) laminates. UD laminates are constructed of thin (&#60;0.05 mm) layers of high-performance yarns, ...

Use of Capillary Aerosol Generator in Continuous Production of Controlled Aerosol for Non-Clinical Studies

The capillary aerosol generator (CAG) is operated with the principal of thermal liquid evaporation through heating of e-liquid in the initial phase, followed by nucleation and condensation regulated through a mixture of airflow to generate aerosols, such as in an electronic cigarette (EC). The CAG is particularly useful in generating aerosols of large volumes in a continuous manner, for instances such as in vivo inhalation toxicology studies, where usage of ECs is not feasible. The thermal effects of generating aerosol from the CAG are similar in terms of temperature applied in an EC, thus allowing investigators to assess the vapors of e-liquids at scale and reproducibility. As the operation of the CAG allows users to control critical parameters such as the flow rate of e-liquid, heating temperatures and dilution air flows, it allows investigators to test various e-liquid formulations in a well-controlled device. Properties, such as aerosol particle size, are demonstrated to be regulated with the air flow rate with respect to the e-liquid flow and e-liquid composition. The CAG, however, is limited in assessing common EC-related issues, such as overheating of its elements. We seek to demonstrate that the CAG can generate aerosol that is reproducible and continuous, by assessing the chemical and physical aerosol characteristics with a chosen e-liquid formulation. The protocol describes the operating parameters of liquid flow rate, dilution air-flow rates and operating procedures needing to optimize the aerosol concentration and particle size required for an in vivo toxicology study. Presenting the representative results from the protocol and discussing the challenges and applications of working with a CAG, we demonstrate that CAG can be used in a reproducible fashion. The technology and protocol, that has been developed from prior work, serve as a foundation for future innovations for laboratory-controlled aerosol generation investigations.

The protocol describes the settings and use of a capillary aerosol generator for continuous production of controlled aerosol from a multispecies liquid solution, suitable for steady large-volume aerosol delivery (e.g., in vivo inhalation studies).

The capillary aerosol generator (CAG) is operated with the principal of thermal liquid evaporation through heating of e-liquid in the initial phase, ...