Name: experimental implementation of a new composite fabrication method: exposing bare fibers on the composite surface by the soft layer method
Uploaded: 2017-10-06T12:30:00
Description: Watch this Scientific Journal Video about Experimental Implementation of a New Composite Fabrication Method: Exposing Bare Fibers on the Composite Surface by the Soft Layer Method at JoVE.com

This research was supported by the Climate Change Research Hub of KAIST (grant No. N11160012), the Leading Foreign Research Institute Recruitment Program through the National Research Foundation of Korea funded by the Ministry of Science, ICT and Future Planning (grant No. 2011-0030065), the Leading Human Resource Training Program of Regional Neo Industry through the National Research Foundation of Korea (NRF) funded by the Ministry of Science, ICT and Future Planning (grant no. NRF-2016H1D5A1910603). Their support is greatly appreciated.

1. Material Preparation
<ol>
	<li>Preparation of the composite material 
	NOTE: CAUTION, Please consult all relevant material safety data sheets (MSDS) before use. Several of the chemicals used in these methods may be toxic and carcinogenic. Nanomaterials may have additional hazards compared to their bulk counterparts. Please use all appropriate safety practices when performing an experiment, including the use of engineering controls (fume hood, glove box) and personal protective equipment (safety...

<ol>
	<li>Hwang, I. U., 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=Bipolar+plate+made+of+carbon+fiber+epoxy+composite+for+polymer+electrolyte+membrane+fuel+cells.">Bipolar plate made of carbon fiber epoxy composite for polymer electrolyte membrane fuel cells.</a> J Power Sources. 184 (1), 90-94 (2008).</li><li>Avasarala, B., Haldar, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+surface+roughness+of+composite+bipolar+plates+on+the+contact+resistance+of+a+proton+exchange+membrane+fuel+cell.">Effect of surface roughness of composite bipolar plates on the contact resistance of a proton exchange membrane fuel cell.</a> J Power Sources. 188 (1), 225-229 (2009).</li><li>Yu, H. N., Lim, J. W., Kim, M. K., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Plasma+treatment+of+the+carbon+fiber+bipolar+plate+for+PEM+fuel+cell.">Plasma treatment of the carbon fiber bipolar plate for PEM fuel cell.</a> Compos Struct. 94 (5), 1911-1918 (2012).</li><li>Lim, J. W., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+composite-metal+hybrid+bipolar+plates+for+PEM+fuel+cells.">Development of composite-metal hybrid bipolar plates for PEM fuel cells.</a> Int J Hydrogen Energy. 37 (17), (2012).</li><li>Kim, B. G., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electromagnetic-carbon+surface+treatment+of+composite+bipolar+plate+for+high-efficiency+polymer+electrolyte+membrane+fuel+cells.">Electromagnetic-carbon surface treatment of composite bipolar plate for high-efficiency polymer electrolyte membrane fuel cells.</a> J Power Sources. 195 (6), 1577-1582 (2010).</li><li>Kim, B. G., Lim, J. W., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+single-type+aluminum/composite+hybrid+bipolar+plate+with+surface+modification+for+high+efficiency+PEMFC.">A single-type aluminum/composite hybrid bipolar plate with surface modification for high efficiency PEMFC.</a> Int J Hydrogen Energy. 36 (4), 3087-3095 (2011).</li><li>Yu, H. N., Lim, J. W., Suh, J. D., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+graphite-coated+carbon+fiber+epoxy+composite+bipolar+plate+for+polymer+electrolyte+membrane+fuel+cell.">A graphite-coated carbon fiber epoxy composite bipolar plate for polymer electrolyte membrane fuel cell.</a> J Power Sources. 196 (23), 9868-9875 (2011).</li><li>Kim, K. H., Kim, B. G., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+carbon+composite+bipolar+plate+(BP)+for+vanadium+redox+flow+battery+(VRFB).">Development of carbon composite bipolar plate (BP) for vanadium redox flow battery (VRFB).</a> Compos Struct. 109, 253-259 (2014).</li><li>Lee, D., Lim, J. W., Nam, S., Choi, I., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gasket-integrated+carbon/silicone+elastomer+composite+bipolar+plate+for+high-temperature+PEMFC.">Gasket-integrated carbon/silicone elastomer composite bipolar plate for high-temperature PEMFC.</a> Compos Struct. 128, 284-290 (2015).</li><li>Lee, D., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electro-mechanical+properties+of+the+carbon+fabric+composites+with+fibers+exposed+on+the+surface.">Electro-mechanical properties of the carbon fabric composites with fibers exposed on the surface.</a> Compos Struct. 140, 77-83 (2016).</li><li>Lee, D., Lim, J. W., Nam, S., Choi, I., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Method+for+exposing+carbon+fibers+on+composite+bipolar+plates.">Method for exposing carbon fibers on composite bipolar plates.</a> Compos Struct. 134, 1-9 (2015).</li><li>Lee, D., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+composite+bipolar+plate+for+high-temperature+proton+exchange+membrane+fuel+cells+(HT-PEMFCs).">Carbon composite bipolar plate for high-temperature proton exchange membrane fuel cells (HT-PEMFCs).</a> J Power Sources. 327, 119-126 (2016).</li><li>Lee, D., Choe, J., Nam, S., Lim, J. W., Choi, I., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Development+of+non-woven+carbon+felt+composite+bipolar+plates+using+the+soft+layer+method.">Development of non-woven carbon felt composite bipolar plates using the soft layer method.</a> Compos struct. 160, 976-982 (2016).</li><li>Lee, D., Lim, J. W., Lee, D. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode/anode+integrated+composite+bipolar+plate+for+high-temperature+PEMFC.">Cathode/anode integrated composite bipolar plate for high-temperature PEMFC.</a> Compos Struct. 167, 144-151 (2017).</li><li>Lee, D., Oh, Y., Nam, S., Choe, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Adhesion+Characteristics+of+Fiber-exposed+Glass+Composites.">Adhesion Characteristics of Fiber-exposed Glass Composites.</a> Compos Struct. 165, 9-14 (2017).</li></ol>

The soft layer method provides significant advantages compared with the conventional methods, and with a lower manufacturing cost. All three types of composites manufactured by the soft layer method show unique characteristics in terms of the electrical properties, mechanical properties, gas permeability, and adhesion properties.
For the measurement of the electrical property, a four-point probe method was used. ASR was measured 5 times and the average value was taken as a representative value...

The bipolar plate is a multi-functional key component of energy conversion systems and energy storage systems such as fuel cells and batteries. The key functional requirements of the bipolar plate are as follows: high electrical conductivity in the through-thickness direction to reduce ohmic-loss, high mechanical properties to withstand high compaction pressure and external impacts, and high productivity for mass production.
Compared with the graphite and metals that were conventionally adopted as materials for the bipolar plate, carbon fiber/epoxy composites have a higher specific strength and stiffness, which indicates that the weight of the system can be greatly reduced by replacing the conventional bipolar plate materials with composites1. However, conventional carbon/epoxy composites have poor electrical conductivity in the through-thickness direction, which results in a large areal specific resistance (ASR), due to the resin-rich layer that is formed on the composite surface. The insulating resin-rich layer prevents direct contact between the conductive carbon fibers and adjacent components, such as another bipolar plate, gas diffusion layer (GDL), and carbon felt electrode (CFE). 
Many studies were conducted to resolve the high ASR due to the resin-rich layer. The first approach was surface treatment methods to selectively remove the resin-rich layer. For example, mechanical abrasion was attempted to remove the resin on the surface2. However, the carbon fibers were also damaged, which resulted in a poor ASR. Plasma treatment3,4 and microwave treatment methods5,6 were also developed to avoid fiber damage, but they resulted in low productivity and uniformity. The second approach, conductive layer coating methods, includes expanded graphite coating7,8. This method successfully reduced the ASR and has been regarded as a standard method to manufacture a composite bipolar plate. However, it is costly and has durability and delamination issues due to the low mechanical strength.
In this study, the "soft layer method", a novel manufacturing method that can expose carbon fibers on the composite bipolar plate surface, is demonstrated. The main purpose of this method is to obtain a low ASR with a low manufacturing cost. The soft layer method adopts a thin soft layer such as a polymer release film between the compression mold and bipolar plate. After curing in the compression mold and the detaching of the soft layer, the fabricated bipolar plate displays carbon fibers exposed on the surface without any post-surface treatment. This method not only decreased the ASR but also significantly increased the mechanical properties and solved the gas permeability issue. This method can be applied for many other purposes: the development of an electrically conductive plate, the manufacture of a thin composite, and the fabrication of an adhesive joint without surface treatment.

<table width="891">
	<tbody>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Unidirectional carbon/epoxy prepreg</td>
			<td class="xl63" style="width:72pt" width="96">SK Chemicals</td>
			<td class="xl63" style="width:110pt" width="146">USN020</td>
			<td class="xl66" style="width:264pt" width="352">Used to fabricate unidirectional carbon composite</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Plain weave carbon fabric/epoxy prepreg</td>
			<td class="xl63" style="width:72pt" width="96">SK Chemicals</td>
			<td class="xl63" style="width:110pt" width="146">WSN 1k</td>
			<td class="xl66">Used to fabricate fabric carbon composite</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Plain weave carbon fabric</td>
			<td class="xl63" style="width:72pt" width="96">SK Chemicals</td>
			<td class="xl63" style="width:110pt" width="146">C-112</td>
			<td class="xl66">Used to fabricate fabric carbon composite</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Non-woven carbon felt</td>
			<td class="xl63" style="width:72pt" width="96">Newell</td>
			<td class="xl63" style="width:110pt" width="146">Graphite felt 3 mm</td>
			<td class="xl66">Used to fabricated felt carbon composite</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Film type epoxy resin</td>
			<td class="xl63" style="width:72pt" width="96">SK Chemicals</td>
			<td class="xl63" style="width:110pt" width="146">K51</td>
			<td class="xl66">Used as a matrix of the composite</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Acetone 99.5%</td>
			<td class="xl63" style="width:72pt" width="96">Samchun</td>
			<td class="xl63" style="width:110pt" width="146">67-64-1</td>
			<td class="xl66">Used to cleanse the carbon fiber and the soft layers</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Mold release</td>
			<td class="xl63" style="width:72pt" width="96">ShinEtsu</td>
			<td class="xl63" style="width:110pt" width="146">KF-96</td>
			<td class="xl66">Used to coat the mold</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Release film</td>
			<td class="xl63" style="width:72pt" width="96">Airtech</td>
			<td class="xl63" style="width:110pt" width="146">A4000V</td>
			<td class="xl66">Used as a soft layer</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Compression mold</td>
			<td class="xl63" style="width:72pt" width="96">N/A</td>
			<td class="xl63" style="width:110pt" width="146">N/A</td>
			<td class="xl66">Machined in lab. Material: NAK80</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Hot press</td>
			<td class="xl63" style="width:72pt" width="96">Hydrotek 100</td>
			<td class="xl63" style="width:110pt" width="146">N/A</td>
			<td class="xl66">Used to apply pressure and heat</td>
		</tr>
		<tr height="21" style="height:15.75pt">
			<td class="xl63" height="21" style="width:223pt;height:15.75pt" width="297">Scanning electron microscope</td>
			<td class="xl63" style="width:72pt" width="96">FEI Compnay</td>
			<td class="xl63" style="width:110pt" width="146">Magellan 400</td>
			<td class="xl66">Used to investigate the surface of the composite</td>
		</tr>
	</tbody>
</table>

experimental implementation of a new composite fabrication method: exposing bare fibers on the composite surface by the soft layer method

The bipolar plate is a key component in proton exchange membrane fuel cells (PEMFCs) and vanadium redox flow batteries (VRFBs). It is a multi-functional component that should have high electrical conductivity, high mechanical properties, and high productivity.
In this regard, a carbon fiber/epoxy resin composite can be an ideal material to replace the conventional graphite bipolar plate, which often leads to the catastrophic failure of the entire system because of its inherent brittleness. Though the carbon/epoxy composite has high mechanical properties and is easy to manufacture, the electrical conductivity in the through-thickness direction is poor because of the resin-rich layer that forms on its surface. Therefore, an expanded graphite coating was adopted to solve the electrical conductivity issue. However, the expanded graphite coating not only increases the manufacturing costs but also has poor mechanical properties.
In this study, a method to expose fibers on the composite surface is demonstrated. There are currently many methods that can expose fibers by surface treatment after the fabrication of the composite. This new method, however, does not require surface treatment because the fibers are exposed during the manufacture of the composite. By exposing bare carbon fibers on the surface, the electrical conductivity and mechanical strength of the composite are increased drastically.

The fabricated specimens are observed using scanning electron microscopy (SEM) (Figure 1). Because the resin-rich layer that covers the top of the fibers is only a few micrometers thick, an optical microscopic image observed at the top of the specimen is not appropriate. A SEM image observed by tilting the specimen by 5&#176; provides a more representative image. Compared to the composites fabricated by conventional compression molding, which has its surface ...

Watch this Scientific Journal Video about Experimental Implementation of a New Composite Fabrication Method: Exposing Bare Fibers on the Composite Surface by the Soft Layer Method at JoVE.com

Experimental Implementation of a New Composite Fabrication Method: Exposing Bare Fibers on the Composite Surface by the Soft Layer Method

A protocol to expose bare fibers on the composite surface by eliminating resin rich area is presented. The fibers are exposed during fabrication of the composites, not by the post surface treatment. The exposed carbon composites exhibit high electrical conductivity in the through-thickness direction and high mechanical property.

The bipolar plate is a key component in proton exchange membrane fuel cells (PEMFCs) and vanadium redox flow batteries (VRFBs). It is a multi-functional ...

The overall goal of this procedure is to fabricate a fiber-reinforced composite with bare fibers exposed on the surface without any surface treatment. This technique can expose bare fibers on a composite surface without the use of expensive and inefficient surface treatments. The main advantage of this technique is that it improves the electrical conductivity and mechanical strengths of the composite.This technique also has high productivity. To prepare unidirectional carbon fiber fabric, pre-impregnated with epoxy, stack squares of prepreg with a fiber volume fraction of 50 to 60%in a sequence including zero degree and 90 degree orientations to avoid splitting of the laminate. To prepare each square of prepreg plain-weave carbon fiber fabric, first cleanse the fabric with acetone or ethanol.Place the fabric on a clean surface or on a lint-free laboratory wipe, and allow the acetone to evaporate under ambient conditions. Peel off one backing of a sheet of film-type epoxy resin with a curing temperature of 125 degrees Celsius. Apply a single sheet of epoxy resin film to the clean carbon fabric.Place the fabric epoxy side down on a hot plate at 70 degrees Celsius. Heat the fabric for 10 seconds to pre-impregnate the fabric with epoxy. Allow the prepreg fabric to cool under ambient conditions for 10 minutes.Then, remove the remaining backing sheet from the epoxy-coated side. Stack the plain-weave prepreg fabric in the desired stacking sequence to form the plain-weave carbon fiber fabric laminate. To prepare non-woven carbon fiber felt laminate, apply triple-layered epoxy sheet to each side of a piece of clean, dry carbon felt.Heat the epoxy-coated sides of the felt at 70 degrees Celsius for 10 seconds each with mass applied on the top. Allow the prepreg felt to cool for 10 minutes, and then peel off the remaining backing sheets. Next, wash sheets of 25 micrometer thick, non-perforated, fluorinated ethylene propylene release film with ethanol or acetone.Carefully dry the FEP sheets with lint-free wipes without causing wrinkles or pinholes. Ensure that the sheets are free of contaminants and particulate matter. Then, place each clean, dry sheet between lint-free wipes, and store the sheets in a dust-free, clean, plastic case.To begin the composite fabrication, apply silicone mold release to the compression mold. Wipe the mold with lint-free wipes to leave only a thin layer of mold release. Then, trim a piece of prepared carbon fiber laminate to be slightly smaller than the mold cavity.Place a sheet of 25 micrometer thick clean FEP film on the lower mold. Place the laminate on the mold, and cover it with 25 or 100 micrometer thick FEP film, depending on the fiber type. Carefully smooth out the film so that no air bubbles remain between the soft layer and the laminate.Then, close the compression mold. Heat a hot press to 150 degrees Celsius, and place the compression mold in the press. For unidirectional fiber composite, constantly apply 20 megapascals for 30 minutes.For a woven composite, apply 20 megapascals for four minutes, release the pressure, and immediately reapply 20 megapascals. Purge the material in this way until the viscosity of the resin begins increasing. Then, hold the pressure at 20 megapascals until the composite has cured for 30 minutes in total.For a felt composite, slowly increase the pressure to three megapascals, being careful not to overshoot. Cure the material at three megapascals for 30 minutes. Once the sample is cured, without releasing the pressure, cool the compression mold to below 120 degrees Celsius.Then, release the pressure, remove the mold, and de-mold the fabricated specimen. Scanning electron microscopy images acquired at a five-degree tilt showed that fibers were visible in greater detail in composites fabricated with the soft-layer method than with conventional compression molding. This was attributed to the elimination of the resin-rich layer on top of the composite.Despite the elimination of the epoxy resin layer, the fibers did not show visible defects. The through-thickness electrical conductivity was greater in composites fabricated with the soft-layer method, with a corresponding decrease in area-specific resistance to below 20 milliohms per square centimeter at a compaction pressure of 1.38 megapascals. The measured tensile strengths of soft-layer composites were comparable to those fabricated by the conventional compression method.The woven fabric and felt composites showed increases of 22%and 15%respectively. These increases were attributed to the soft layer applying a uniform pressure across the composite surface. By following this procedure, you will be able to fabricate a fiber-exposed composite without difficulty.The mechanism is simple. And with a good understand of your material, the implementation is even simpler. While attempting this procedure, remember to fine tune it to fit your specific application.Consider the curing condition of the composite and the thermal properties of the soft layer, and adjust the procedure accordingly to obtain the desired results.

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Research

JoVE Journal

Engineering

Fabrication and Characterization of Disordered Polymer Optical Fibers for Transverse Anderson Localization of Light

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed polymer optical fiber is composed of 80,000 strands of poly (methyl methacrylate) (PMMA) and polystyrene (PS) that are randomly mixed and drawn into a square cross section optical fiber with a side width of 250 &mu;m. Initially, each strand is 200 &mu;m in diameter and 8-inches long. During the mixing process of the original fiber strands, the fibers cross over each other; however, a large draw ratio guarantees that the refractive index profile is invariant along the length of the fiber for several tens of centimeters. The large refractive index difference of 0.1 between the disordered sites results in a small localized beam radius that is comparable to the beam radius of conventional optical fibers. The input light is launched from a standard single mode optical fiber using the butt-coupling method and the near-field output beam from the disordered fiber is imaged using a 40X objective and a CCD camera. The output beam diameter agrees well with the expected results from the numerical simulations. The disordered optical fiber presented in this work is the first device-level implementation of 2D Anderson localization, and can potentially be used for image transport and short-haul optical communication systems.

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. This microstructured fiber can transport a small localized beam with a radius that is comparable to the beam radius of conventional optical fibers.

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed ...

Emission Spectroscopic Boundary Layer Investigation during Ablative Material Testing in Plasmatron

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution for future high-speed reentry missions. But despite the advancements made since Apollo, heat flux prediction remains an imperfect science and engineers resort to safety factors to determine the TPS thickness. This goes at the expense of embarked payload, hampering, for example, sample return missions. 
Ground testing in plasma wind-tunnels is currently the only affordable possibility for both material qualification and validation of material response codes. The subsonic 1.2MW Inductively Coupled Plasmatron facility at the von Karman Institute for Fluid Dynamics is able to reproduce a wide range of reentry environments. This protocol describes a procedure for the study of the gas/surface interaction on ablative materials in high enthalpy flows and presents sample results of a non-pyrolyzing, ablating carbon fiber precursor. With this publication, the authors envisage the definition of a standard procedure, facilitating comparison with other laboratories and contributing to ongoing efforts to improve heat shield reliability and reduce design uncertainties.
The described core techniques are non-intrusive methods to track the material recession with a high-speed camera along with the chemistry in the reactive boundary layer, probed by emission spectroscopy. Although optical emission spectroscopy is limited to line-of-sight measurements and is further constrained to electronically excited atoms and molecules, its simplicity and broad applicability still make it the technique of choice for analysis of the reactive boundary layer. Recession of the ablating sample further requires that the distance of the measurement location with respect to the surface is known at all times during the experiment. Calibration of the optical system of the applied three spectrometers allowed quantitative comparison. At the fiber scale, results from a post-test microscopy analysis are presented.

Development of new ablative materials and their numerical modeling requires extensive experimental investigation. This protocol describes procedures for material response characterization in plasma flows with the core techniques being non-intrusive methods to track the material recession along with the chemistry in the reactive boundary layer by emission spectroscopy.

Ablative Thermal Protection Systems (TPS) allowed the first humans to safely return to Earth from the moon and are still considered as the only solution ...

Strain Sensing Based on Multiscale Composite Materials Reinforced with Graphene Nanoplatelets

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are proposed to create the electrical network in this work: (a) the incorporation of the nanoplatelets into the epoxy matrix and (b) the coating of the glass fabric with a sizing filled with the same nanoplatelets. Both types of multiscale composite materials, with an in-plane electrical conductivity of ~10-3 S/m, showed an exponential growth of the electrical resistance as the strain increases due to distancing between adjacent functionalized graphene nanoplatelets and contact loss between overlying ones. The sensitivity of the materials analyzed during this research, using the described procedures, has been shown to be higher than commercially available strain gauges. The proposed procedures for self-sensing of the structural composite material would facilitate the structural health monitoring of components in difficult to access emplacements such as offshore wind power farms. Although the sensitivity of the multiscale composite materials was considerably higher than the sensitivity of metallic foils used as strain gauges, the value reached with NH2 functionalized graphene nanoplatelets coated fabrics was nearly an order of magnitude superior. This result elucidated their potential to be used as smart fabrics to monitor human movements such as bending of fingers or knees. By using the proposed method, the smart fabric could immediately detect the bending and recover instantly. This fact permits precise monitoring of the time of bending as well as the degree of bending.

The integration of conductive nanoparticles, such as graphene nanoplatelets, into glass fiber composite materials creates an intrinsic electrical network susceptible to strain. Here, different methods to obtain strain sensors based on the addition of graphene nanoplatelets into the epoxy matrix or as a coating on glass fabrics are proposed.

The electrical response of NH2-functionalized graphene nanoplatelets composite materials under strain was studied. Two different manufacturing methods are ...

Flow-assisted Dielectrophoresis: A Low Cost Method for the Fabrication of High Performance Solution-processable Nanowire Devices

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of nanowires. DEP is used for nanowire analysis, characterization, and for solution-based fabrication of semiconducting devices. The method works by applying an alternating electric field between metallic electrodes. The nanowire formulation is then dropped onto the electrodes which are on an inclined surface to create a flow of the formulation using gravity. The nanowires then align along the gradient of the electric field and in the direction of the liquid flow. The frequency of the field can be adjusted to select nanowires with superior conductivity and lower trap density. 
In this work, flow-assisted DEP is used to create nanowire field effect transistors. Flow-assisted DEP has several advantages: it allows selection of nanowire electrical properties; control of nanowire length; placement of nanowires in specific areas; control of orientation of nanowires; and control of nanowire density in the device. 
The technique can be expanded to many other applications such as gas sensors and microwave switches. The technique is efficient, quick, reproducible, and it uses a minimal amount of dilute solution making it ideal for the testing of novel nanomaterials. Wafer scale assembly of nanowire devices can also be achieved using this technique, allowing large numbers of samples for testing and large-area electronic applications.

In this paper, flow assisted dielectrophoresis is demonstrated for the self-assembly of nanowire devices. The fabrication of a silicon nanowire field effect transistor is shown as an example.

Flow-assisted dielectrophoresis (DEP) is an efficient self-assembly method for the controllable and reproducible positioning, alignment, and selection of ...

A Fabrication and Measurement Method for a Flexible Ferroelectric Element Based on Van Der Waals Heteroepitaxy

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on high-density data storage and low-power consumption capabilities. However, the high-quality oxide based nonvolatile memory on flexible substrates is often constrained by the material characteristics and the inevitable high-temperature fabrication process. In this paper, a protocol is proposed to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica. The versatile deposition technique and measurement method enable the fabrication of flexible yet single-crystalline non-volatile memory elements necessary for the next generation of smart devices.

In this paper, we present a protocol to directly grow an epitaxial yet flexible lead zirconium titanate memory element on muscovite mica.

Flexible non-volatile memories have received much attention as they are applicable for portable smart electronic device in the future, relying on ...

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 ...

Operation of the Collaborative Composite Manufacturing (CCM) System

The automated tape placement and the automated fiber placement (AFP) machines provide a safer working environment and reduce the labor intensity of workers than the traditional manual fiber placement does. Thus, the production accuracy, repeatability and efficiency of composite manufacturing are significantly improved. However, the current AFP systems can only produce the composite components with large open surface or simple revolution parts, which cannot meet the growing interest in small complex or closed structures from industry.
In this research, by employing a 1-degree of freedom (DoF) rotational stage, a 6-RSS parallel robot, and a 6-DoF serial robot, the dexterity of the AFP system can be significantly improved for manufacturing complex composite parts. The rotational stage mounted on the parallel robot is utilized to hold the mandrel and the serial robot carries the placement head to mimic two human hands that have enough dexterity to lay the fiber to the mandrel with complex contour.
Although the CCM system increases the flexibility of composite manufacturing, it is quite time-consuming or even impossible to generate the feasible off-line path, which ensures uniform lay-up of subsequent fibers considering the constraints like singularities, collisions between the fiber placement head and mandrel, smooth fiber direction change and keeping the fiber placement head along the norm of the part&#39;s surface, etc. Moreover, due to the existing positioning error of the robots, the on-line path correction is needed. Therefore, the on-line pose correction algorithm is proposed to correct the paths of both parallel and serial robots, and to keep the relative path between the two robots unchanged through the visual feedback when the constraint or singularity problems in the off-line path planning occur. The experimental results demonstrate the designed CCM system can fulfill the movement needed for manufacturing a composite structure with Y-shape.

Operation of the Collaborative Composite Manufacturing CCM System

A collaborative composite manufacturing system is developed for robotic lay-up of composite laminates using the prepreg tape. The proposed system allows the production of composite laminates with high levels of geometrical complexity. The issues in the path planning, coordination of the robots and control are addressed in the proposed method.

The automated tape placement and the automated fiber placement (AFP) machines provide a safer working environment and reduce the labor intensity of ...

Fabrication of Surface Acoustic Wave Devices on Lithium Niobate

Manipulation of fluids and particles by acoustic actuation at small scale is aiding the rapid growth of lab-on-a-chip applications. Megahertz-order surface acoustic wave (SAW) devices generate enormous accelerations on their surface, up to 108 m/s2, in turn responsible for many of the observed effects that have come to define acoustofluidics: acoustic streaming and acoustic radiation forces. These effects have been used for particle, cell, and fluid handling at the microscale&#8212;and even at the nanoscale. In this paper we explicitly demonstrate two major fabrication methods of SAW devices on lithium niobate: the details of lift-off and wet etching techniques are described step-by-step. Representative results for the electrode pattern deposited on the substrate as well as the performance of SAW generated on the surface are displayed in detail. Fabrication tricks and troubleshooting are covered as well. This procedure offers a practical protocol for high frequency SAW device fabrication and integration for future microfluidics applications.

Two fabrication techniques, lift-off and wet etching, are described in producing interdigital electrode transducers upon a piezoelectric substrate, lithium niobate, widely used to generate surface acoustic waves now finding broad utility in micro to nanoscale fluidics. The as-produced electrodes are shown to efficiently induce megahertz order Rayleigh surface acoustic waves.&#160;

Manipulation of fluids and particles by acoustic actuation at small scale is aiding the rapid growth of lab-on-a-chip applications. Megahertz-order ...

Solution Blow Spinning of Polymeric Nano-Composite Fibers for Personal Protective Equipment

Light-weight, protective armor systems typically consist of high modulus (&#62;109 MPa) and high-strength polymeric fibers held in place with an elastic resin material (binder) to form a non-woven, unidirectional laminate. While significant efforts have focused on improving the mechanical properties of the high-strength fibers, little work has been undertaken to improve the properties of the binder materials. To improve the performance of these elastomeric polymer binders, a relatively new and simple fabrication process, known as solution blow spinning, was used. This technique is capable of producing sheets or webs of fibers with average diameters ranging from the nanoscale to the microscale. To achieve this, a solution blow spinning (SBS) apparatus has been designed and built in the laboratory to fabricate non-woven fiber mats from polymer elastomer solutions.
In this study, a commonly used binder material, a styrene-butadiene-styrene block-co-polymer dissolved in tetrahydrofuran, was used to produce nanocomposite fiber mats by adding metallic nanoparticles (NPs), such as iron oxide NPs, that were encapsulated with silicon oil and thus incorporated in the fibers formed via the SBS process. The protocol described in this work will discuss the effects of the various critical parameters involved in the SBS process, including the polymer molar mass, the selection of the thermodynamically appropriate solvent, the polymer concentration in solution, and the carrier gas pressure to assist others in performing similar experiments, as well as provide guidance to optimize the configuration of the experimental setup. The structural integrity and morphology of the resultant non-woven fiber mats were examined using scanning electron microscopy (SEM) and elemental X-ray analysis via energy-dispersive X-ray spectroscopy (EDS). The goal of this study is to evaluate the effects of the various experimental parameters and material selections to optimize the structure and morphology of the SBS fiber mats.

The primary goal of this study is to describe a protocol to prepare polymeric fiber mats with consistent morphology via solution blow spinning (SBS). We aim to use SBS to develop novel, tunable, flexible polymeric fiber nanocomposites for various applications, including protective materials, by incorporating nanoparticles in a polymer-elastomer matrix.

Light-weight, protective armor systems typically consist of high modulus (&#62;109 MPa) and high-strength polymeric fibers held in place with an elastic ...

Microfluidic Channel-Based Soft Electrodes for Capacitive Pressure Sensing

Microfluidic Channel-Based Soft Electrodes and Their Application in Capacitive Pressure Sensing

Flexible and stretchable electrodes are essential components in soft artificial sensory systems. Despite recent advances in flexible electronics, most electrodes are either restricted by the patterning resolution or the capability of inkjet printing with high-viscosity super-elastic materials. In this paper, we present a simple strategy to fabricate microchannel-based stretchable composite electrodes, which can be achieved by scraping elastic conductive polymer composites (ECPCs) into lithographically embossed microfluidic channels. The ECPCs were prepared by a volatile solvent evaporation method, which achieves a uniform dispersion of carbon nanotubes (CNTs) in a polydimethylsiloxane (PDMS) matrix. Compared to conventional fabrication methods, the proposed technique can facilitate the rapid fabrication of well-defined stretchable electrodes with high-viscosity slurry. Since the electrodes in this work were made up of all-elastomeric materials, strong interlinks can be formed between the ECPCs-based electrodes and the PDMS-based substrate at the interfaces of the microchannel walls, which allows the electrodes to exhibit mechanical robustness under high tensile strains. In addition, the mechanical-electric response of the electrodes was also systematically studied. Finally, a soft pressure sensor was developed by combining a dielectric silicone foam and an interdigitated electrodes (IDE) layer, and this demonstrated great potential for pressure sensors in soft robotic tactile sensing applications.

Author Spotlight: Microfluidic Channel-Based Soft Electrodes and Their Application in Capacitive Pressure Sensing  

Flexible electrodes have a wide range of applications in soft robotics and wearable electronics. The present protocol demonstrates a new strategy to fabricate highly stretchable electrodes with high resolution via lithographically defined microfluidic channels, which paves the way for future high-performance soft pressure sensors.

Flexible and stretchable electrodes are essential components in soft artificial sensory systems. Despite recent advances in flexible electronics, most ...