The authors thank Destiny Garcia, Serena Ferraro, Erik Quiroz and Steven Kern (Advanced Composites Research, Engineering and Science laboratory) for their help in designing and manufacturing the test setup. Shawn Malone, Michael Akahori, David Kehlet (Engineering Fabrication Lab) are acknowledged for their suggestions and assistance in the machining process. The support of the National Science Foundation (collaborative grant CMMI-1265691 and its REU supplement) and the Office of Naval Research (N00014-13-1-0604 to A. Muliana, Texas &#38;M University (Principal Investigator), and V. La Saponara, managed by program director Yapa Rajapakse) are gratefully appreciated.

1. Loading the Specimens
<ol>
	<li>Raise the lid of the tank and rest it upon the side supports (Figure 4).</li>
	<li>Place the specimen in the U-bolt, and ensure that the cross bar is making contact at the center of the specimen.</li>
	<li>Rest the ends of the specimen on the aluminum supports hanging from the lid. The ends of the specimens should have 5-10 mm of overhang.</li>
	<li>Repeat steps 1.2-1.4 for all of the specimens that will be tested.</li>
	<li>Remove the lid supports, lower lid, and make sure that the lid is seated on the lip of the tank.</li>
	<li>Apply the desired force by adding weights to the steel rod next to the outer pulley.</li>
</ol>
2. Measuring Displacement
<ol>
	<li>Ensure that the string potentiometer line is pulled taut.</li>
	<li>Using a digital multimeter, measure the resistance across the outer pins of the potentiometer (Figure 3), with black to Pin 1 and red to Pin 3, and record the reading.</li>
	<li>Convert the resistance reading into a displacement reading by computing the calibration factor (in this case, 1 k&#8486; corresponds to a 64.895 mm displacement).</li>
	<li>Repeat steps 2.1-2.3 for each specimen.</li>
</ol>
3. Weighing the Specimens
<ol>
	<li>Before beginning the weighing procedure, record the displacement data and prepare an interim holding chamber filled with the testing fluid at RT, as per ASTM D522931, or the appropriate testing standard.</li>
	<li>Remove the slotted weights from the ends of the steel cables.</li>
	<li>Raise the lid of the tank and rest it upon the side supports.</li>
	<li>Remove the specimen and place it into the prepared interim holding chamber. Repeat this step for all of the specimens.</li>
	<li>Remove the specimens and dry them individually using a microfiber cloth in order to remove excess fluid.</li>
	<li>Place the specimen on a high-precision scale and record the data reading.</li>
	<li>Repeat steps 3.5-3.6 for all specimens and then follow Protocol Step 1.</li>
</ol>

<ol>
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S., Dulieu-Barton, J. M., Shenoi, R. A. <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+hygrothermal+ageing+effects+in+sandwich+construction+joints+using+thermoelastic+stress+analysis.">Determination of hygrothermal ageing effects in sandwich construction joints using thermoelastic stress analysis.</a> Compos Sci Technol. 63, 211-223 (2003).</li><li>Jeon, J., Muliana, A., La Saponara, V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+stress+and+deformation+analyses+in+fiber+reinforced+polymer+composites+undergoing+heat+conduction+and+mechanical+loading.">Thermal stress and deformation analyses in fiber reinforced polymer composites undergoing heat conduction and mechanical loading.</a> Compos. Struct. 111, 31-44 (2014).</li><li>Muliana, A. H., Rajagopal, K. 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The authors have nothing to disclose.

From the acquired data, it can be seen that the concurrent testing scenario did affect the durability of the closed-cell polyurethane foam specimens. This can be seen by comparing the significantly different displacements (Figure 5) and residual loads to failure (Figure 6) of dry and wet specimens. Figure 7 shows pictures of the specimens after the residual strength tests. It should also be observed that, while the displacement of the dry specimens reached steady state w...

Polymer and fiber-reinforced polymer (FRP) composites have been adopted in a variety of engineering structures, ranging from aircraft and spacecraft, naval vessels, civil infrastructure, (see for examples reviews of Katnam et al.1, Hollaway2, Mouritz et al.3), cars and trains, wind turbine blades, to prosthetics and biomaterials for sutures and implants. These materials&#8217; durability is affected by complex service scenarios, which may include a combination of a) thermo-mechanical loading, e.g., freeze-thaw cycles in civil infrastructure4, subsonic/supersonic flight profiles5, wear in metal-backed polyethylene6); b) degradation due to environmental and chemical agents, e.g., sea water, de-icing, hydraulic fluid for aerospace and naval structures7-10, degradation of polymethylmethacrylate dental composites due to saliva11; c) complex interactions of materials in fastened or bonded joints, e.g., galvanic corrosion and debonding between dissimilar materials, whether in a carbon/fiber patch repair on an aircraft aluminum skin, or a carbon/PEEK bone plate fastened by stainless steel12.
There is unfortunately limited knowledge of the impact of concurrent in-service stimuli on the long-term durability of these materials. Most polymers may be categorized as viscoelastic materials. Mechanical loadings and environmental conditions significantly influence the viscoelastic response of polymers. Hence, reliable models for these materials&#8217; long-term behavior should be able to incorporate time-dependent responses to coupled hygrothermal, mechanical, chemical stimuli. This in turn will improve design predictions, safety and condition-based maintenance/replacement protocols.
There is a large literature body on experimental testing on hygrothermal effects, for example hygrothermal diffusion tests: if the scale of the samples allows it, the material samples may be positioned in a chamber at desired humidity and temperature levels. The samples are removed periodically to measure their mass and/or volume changes for a given amount of time, from weeks to years10,13-17. The hygrothermal test may be followed by mechanical testing, i.e., residual static/fatigue strength/fracture mechanics testing17-19, which only gives information on the effect of hygrothermal stimulus on the mechanical responses of materials. Test data may be fitted to diffusion models of varying complexity, from simple Fickian diffusion to models that include dependency on concentration, stress, temperature, reversible physical aging/plasticization and irreversible chemical reactions. This experimental output may be further incorporated in structural analyses.
Few authors have addressed the impact of simultaneous hygrothermal and mechanical stimuli. Among those researching FRP composites, Neumann and Garom20 immersed stressed and unstressed specimens in distilled water. Stress was applied by positioning the specimens inside compressed stainless steel springs, tuning the load by using different spring stiffnesses and compressive loads. A similar procedure is reported by Wan et al.21. Helbling and Karbhari22 employed a bending fixture inside an environmental chamber for different relative humidity percentages (RH%) and temperature levels. The pre-conditioned specimens were subjected to a given bending strain level, corresponding to a percentage of the static ultimate tensile strain for that composite. Kasturiarachchi and Pritchard23 prepared a stainless steel 4-point bending jig (one per specimen) that was positioned on a shelf in a large glass desiccator. The desiccator was partially filled with distilled water, had small leaks to prevent the buildup of pressure, and was placed in a humidity chamber at 95% RH. Gellert and Turley7 investigated marine-grade FRP composite specimens for their durability under combined creep loading and 100% RH. Their samples were loaded in 4-point bending at a constant load equal to 20% of the failure static flexure load, while fully immersed in sea water. The creep deflection was acquired periodically by using a thickness gauge between the outer surface of the beam in the central cross-section, and a glass plate (it is inferred that such measurement was performed outside the chamber). Abdel-Magid et al.24 placed samples of glass/epoxy in an Invar environmental fixture which was provided by NASA Langley, as the specimens were loaded in tension along the fiber direction, at 20% of the ultimate axial load. Ellyin and Rohrbarcher25 ran hygrothermal tests for up to 140 days, and then tested the specimens in fatigue on a hydraulic testing machine. The specimens were wrapped in a wet cheese cloth connected to a tube and a water supply. Earl et al.26 positioned their loading fixture and the specimens in a large environmental chamber (5.5 m3).
As discussed in many experimental studies, the environmental conditions affect the polymers&#8217; mechanical properties and responses. Some limited experiments also show that the existence of mechanical stress/strain influences the diffusion process in the polymers. Hence, to enhance understanding on the overall performance of polymer-based materials under both mechanical and non-mechanical effects, there is a need for concurrent testing.
There were several objectives behind the design of the testing platform discussed in this paper. First, the platform is part of the experimental setup in a multi-year investigation on the hygrothermo-mechanical behavior of different types of FRP sandwich composites for wind turbine and naval engineering applications. The test data are used to calibrate the parameters in the viscoelastic constitutive equations for the polymeric composites. The constitutive models are based on the work developed over the years by Muliana and collaborators27-30. The second objective was to have a low-cost and user-friendly testing platform, for example one that could be easily relocated in a laboratory (e.g., to a scale for mass measurements, or to the source of the fluid, e.g., one coming from a faucet, a fumehood or a flammable cabinet). The third goal was to create a testing platform that is resistant to a number of chemicals commonly used in service (particularly hydraulic fluid, de-icing, cleaning solvents for aerospace applications8-10), thus specimens could be immersed in such chemicals, and their durability could be assessed.
The chamber (Figure 1) was constructed with high-density polyethylene, which has high chemical resistance. As mentioned above, it is expected that future work will include hygrothermo-mechanical investigation of composites immersed in hydraulic fluid, de-icing, cleaning solvents. Since thermal regulation is an integral aspect of testing, expanded polystyrene foam was fit around the sides of the tank and secured in place by tape and the steel frame itself, to prevent heat exchange with the environment.
The lid of the chamber (Figure 2) was manufactured from transparent, 9.525 mm-thick polycarbonate, allowing the users to observe the specimens during testing without disturbing the test. The lid is secured in place by aluminum T-bars, which were machined to slide under overhanging brackets on the sides of the tank.
Bending in the specimens is enacted by three aluminum blocks, which hang down from the lid, and are fastened through slots in the lid. The three blocks allow up to four specimens to be tested at one time, while the lid slots allow the block spacing to be adjusted depending on the length of the specimens. Each block is rounded at the contact edge to a 12.7 mm diameter, in adherence to ASTM standard D790-10. The specimens are positioned beneath two of the three blocks, with an upward force applied at its center to induce bending (Figures 1-2).
The apparatus was designed with maximum versatility and ease-of-use in mind. Casters with 41.275 mm diameter are fastened beneath the chamber for mobility purposes. Above them, the tank is supported by a welded steel frame with a wire mesh bottom and cross beams for support. Angle stock spacers for the outside tank corners were manufactured to keep the insulation from being crushed by the overhead weight and displacement gauges (string pot apparatus, discussed later). Around the top, angle stock was used again for framing. Pulley and string potentiometer systems to measure mid-span deflection are mounted on four steel, square-tubing arches (Figure 3). The center two arches out of these four carry the string potentiometers and are adjustable to account for specimen versatility. The string potentiometers were constructed using a torsional spring (as can be found in retractable key lanyards) and potentiometers with three-pronged electronic outputs. The pulleys are aligned and mounted for use with a steel cable running from a rigid connection by the specimen to a hanging rod over the side of the chamber for adjustable weight application.
The load is applied to the specimen using a series of cables, pulleys, linkages and bolts. First, the specimen is placed into the U-bolt so that the 10 mm cross bar is contacting the middle of the span. A 9.525 mm diameter steel rod with eye bolts at each end is then connected to the U-bolt. This steel connection passes through the lid of the chamber. A steel cable and Kevlar thread are attached to the eyebolt opposite the U-bolt. This allows the Kevlar thread from the string potentiometer to read data from a rigid point. The steel cable continues upwards and passes over two pulleys that allow the load to be applied at the periphery of the tank. The cable is then attached to a 9.525 mm diameter steel rod that serves as a slotted weight hanger. This hanger provides a place where the slotted weights can be set in order to apply the desired load.

<table border="0" cellpadding="0" cellspacing="0" width="581">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:127px;">Name of Material/</td>
			<td rowspan="2" style="width:140px;">Company</td>
			<td rowspan="2" style="width:129px;">Catalog Number</td>
			<td rowspan="2" style="width:185px;">Comments/Description</td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:127px;">Equipment</td>
		</tr>
		<tr height="64">
			<td height="64" style="height:64px;width:127px;">Aluminum 6061 rectangular bars</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">8975K268, 1668T72, 7062T17,&#160;</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Aluminum 6061 90 deg. angles</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">8982K91, 8982K14&#160;</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">440C stainless steel</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">6253K52</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">High-density polyethylene sheets</td>
			<td rowspan="2" style="width:140px;">Tap Plastics, USA</td>
			<td rowspan="2" style="width:129px;">N/A (0.236 in. thick x 10.75 in. wide x 16.75 in. long)</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">High-density polyethylene sheets</td>
			<td rowspan="2" style="width:140px;">Tap Plastics, USA</td>
			<td rowspan="2" style="width:129px;">N/A (0.354 in. thick x 6 in. wide x 10 in. long)</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">High-density polyethylene sheets</td>
			<td rowspan="2" style="width:140px;">Tap Plastics, USA</td>
			<td rowspan="2" style="width:129px;">N/A (0.354 in. thick x 6 in. wide x 16.75 in. long)</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">Polycarbonate sheets</td>
			<td rowspan="2" style="width:140px;">Tap Plastics, USA</td>
			<td rowspan="2" style="width:129px;">N/A (0.375 in thick, 11.5 in. wide, 17.5 in long)</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">Expanded polystyrene foam</td>
			<td rowspan="2" style="width:140px;">Home Depot</td>
			<td rowspan="2" style="width:129px;">Model # 310880 Internet # 202532855</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Galvanized steel rope</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">3498T63</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Steel eye bolt</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">3013T341</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">Low-carbon steel 90 deg. angle</td>
			<td rowspan="2" style="width:140px;">McMaster-Carr, USA</td>
			<td rowspan="2" style="width:129px;">9017K444&#160;</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="78">
			<td height="100" rowspan="2" style="height:101px;width:127px;">Low-carbon steel rods</td>
			<td rowspan="2" style="width:140px;">McMaster-Carr, USA</td>
			<td rowspan="2" style="width:129px;">8920K84, 8920K75, 8920K231, 8920K135, 8920K84&#160;&#160;&#160;</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="58">
			<td height="80" rowspan="2" style="height:81px;width:127px;">Low-carbon steel tubes</td>
			<td rowspan="2" style="width:140px;">McMaster-Carr, USA</td>
			<td rowspan="2" style="width:129px;">6527K314, 8910K394, 8910K395, 8920K94&#160;&#160;</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">304 stainless steel U-bolt</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">8896T104</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Steel pulley</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">3099T34</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">1008 carbon steel sheets</td>
			<td style="width:140px;">McMaster-Carr, USA</td>
			<td style="width:129px;">9302T113</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Light duty swivel casters</td>
			<td style="width:140px;">Harbor Freight, USA</td>
			<td style="width:129px;">41519</td>
			<td style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="21">
			<td height="43" rowspan="2" style="height:43px;width:127px;">100-lbf Vinyl Weight Set</td>
			<td rowspan="2" style="width:140px;">Overstock.com</td>
			<td rowspan="2" style="width:129px;">11767059</td>
			<td rowspan="2" style="width:185px;">Part of testing platform</td>
		</tr>
		<tr height="22">
		</tr>
		<tr height="64">
			<td height="64" style="height:64px;width:127px;">Closed-cell polyurethane foam</td>
			<td style="width:140px;">General Plastics, USA</td>
			<td style="width:129px;">FR-3704</td>
			<td style="width:185px;">Testing samples</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Deionized water</td>
			<td style="width:140px;">Faucet, PurLab filtering system</td>
			<td style="width:129px;">N/A</td>
			<td style="width:185px;">Conditioning fluid of tank</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Torsional spring</td>
			<td style="width:140px;">Retractable Key Clip, Ebay, USA</td>
			<td style="width:129px;">Lot 10</td>
			<td style="width:185px;">Used to build string potentiometer</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">Kevlar thread</td>
			<td style="width:140px;">Cabela&#8217;s</td>
			<td style="width:129px;">IK-321909</td>
			<td style="width:185px;">Used to build string potentiometer</td>
		</tr>
		<tr height="43">
			<td height="43" style="height:43px;width:127px;">10 kOhm potentiometer</td>
			<td style="width:140px;">Ebay, USA</td>
			<td style="width:129px;">3590S-2-103L</td>
			<td style="width:185px;">Used to build string potentiometer</td>
		</tr>
		<tr height="64">
			<td height="64" style="height:64px;width:127px;">Digital multimeter</td>
			<td style="width:140px;">Harbor Freight, USA</td>
			<td style="width:129px;">98674</td>
			<td style="width:185px;">Used to take resistance measurements of string potentiometer</td>
		</tr>
	</tbody>
</table>

a testing platform for durability studies of polymers and fiber-reinforced polymer composites under concurrent hygrothermo-mechanical stimuli

The durability of polymers and fiber-reinforced polymer composites under service condition is a critical aspect to be addressed for their robust designs and condition-based maintenance. These materials are adopted in a wide range of engineering applications, from aircraft and ship structures, to bridges, wind turbine blades, biomaterials and biomedical implants. Polymers are viscoelastic materials, and their response may be highly nonlinear and thus make it challenging to predict and monitor their in-service performance. The laboratory-scale testing platform presented herein assists the investigation of the influence of concurrent mechanical loadings and environmental conditions on these materials. The platform was designed to be low-cost and user-friendly. Its chemically resistant materials make the platform adaptable to studies of chemical degradation due to in-service exposure to fluids. An example of experiment was conducted at RT on closed-cell polyurethane foam samples loaded with a weight corresponding to ~50% of their ultimate static and dry load. Results show that the testing apparatus is appropriate for these studies. Results also highlight the larger vulnerability of the polymer under concurrent loading, based on the higher mid-point displacements and lower residual failure loads. Recommendations are made for additional improvements to the testing apparatus.

The testing apparatus has successfully held specimens immersed in a fluid under three-point bending. With reasonable precisions, specimens can be loaded and tested with accurate readouts from the potentiometers for mid-point deflection changes. The change in electrical resistance can be recorded to 4 significant figures, resulting in a displacement resolution of the order of 0.1 &#181;m.
Hygrothermo-mechanical tests were conducted at RT on two groups of four specimens of closed-cell polyuretha...

Watch this Scientific Journal Video about A Testing Platform for Durability Studies of Polymers and Fiber-reinforced Polymer Composites under Concurrent Hygrothermo-mechanical Stimuli at JoVE.com

A Testing Platform for Durability Studies of Polymers and Fiber-reinforced Polymer Composites under Concurrent Hygrothermo-mechanical Stimuli

The durability of polymers and fiber-reinforced polymer composites in service is a critical aspect for their designs and condition-based maintenance. We present a novel low-cost laboratory testing platform for the investigation of the influence of concurrent mechanical and environmental loadings, and may help design more efficient yet safer composite structures.

The durability of polymers and fiber-reinforced polymer composites under service condition is a critical aspect to be addressed for their robust designs ...

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13.7K Views.  University of California, Davis. The durability of polymers and fiber-reinforced polymer composites in service is a critical aspect for their designs and condition-based maintenance. We present a novel low-cost laboratory testing platform for the investigation of the influence of concurrent mechanical and environmental loadings, and may help design more efficient yet safer composite structures.

Video: A Testing Platform for Durability Studies of Polymers and Fiber-reinforced Polymer Composites under Concurrent Hygrothermo-mechanical Stimuli

Controlling the Size, Shape and Stability of Supramolecular Polymers in Water

For aqueous based supramolecular polymers, the simultaneous control over shape, size and stability is very difficult1. At the same time, the ability to do so is highly important in view of a number of applications in functional soft matter including electronics, biomedical engineering, and sensors. In the past, successful strategies to control the size and shape of supramolecular polymers typically focused on the use of templates2,3, end cappers4 or selective solvent techniques5. 
Here we disclose a strategy based on self-assembling discotic amphiphiles that leads to the control over stack length and shape of ordered, chiral columnar aggregates. By balancing electrostatic repulsive interactions on the hydrophilic rim and attractive non-covalent forces within the hydrophobic core of the polymerizing building block, we manage to create small and discrete spherical objects6,7. Increasing the salt concentration to screen the charges induces a sphere-to-rod transition. Intriguingly, this transition is expressed in an increase of cooperativity in the temperature-dependent self-assembly mechanism, and more stable aggregates are obtained. 
For our study we select a benzene-1,3,5-tricarboxamide (BTA) core connected to a hydrophilic metal chelate via a hydrophobic, fluorinated L-phenylalanine based spacer (Scheme 1). The metal chelate selected is a Gd(III)-DTPA complex that contains two overall remaining charges per complex and necessarily two counter ions. The one-dimensional growth of the aggregate is directed by &pi;-&pi; stacking and intermolecular hydrogen bonding. However, the electrostatic, repulsive forces that arise from the charges on the Gd(III)-DTPA complex start limiting the one-dimensional growth of the BTA-based discotic once a certain size is reached. At millimolar concentrations the formed aggregate has a spherical shape and a diameter of around 5 nm as inferred from 1H-NMR spectroscopy, small angle X-ray scattering, and cryogenic transmission electron microscopy (cryo-TEM). The strength of the electrostatic repulsive interactions between molecules can be reduced by increasing the salt concentration of the buffered solutions. This screening of the charges induces a transition from spherical aggregates into elongated rods with a length &gt; 25 nm. Cryo-TEM allows to visualise the changes in shape and size. In addition, CD spectroscopy permits to derive the mechanistic details of the self-assembly processes before and after the addition of salt. Importantly, the cooperativity -a key feature that dictates the physical properties of the produced supramolecular polymers- increases dramatically upon screening the electrostatic interactions. This increase in cooperativity results in a significant increase in the molecular weight of the formed supramolecular polymers in water.

The goal of this experiment is to determine and control the size, shape and stability of self-assembled discotic amphiphiles in water. For aqueous based supramolecular polymers such level of control is very difficult. We apply a strategy using both repulsive and attractive interactions. The experimental techniques applied to characterize this system are broadly applicable.

For aqueous based supramolecular polymers, the simultaneous control over shape, size and stability is very difficult1. At the same time, the ability to do ...

Concurrent Quantitative Conductivity and Mechanical Properties Measurements of Organic Photovoltaic Materials using AFM

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. Thus, understanding of spatial variations in composition as well as electrical properties of OPV materials is of paramount importance for moving PV technology forward.1,2 In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution. Currently, materials properties measurements performed using commercially available AFM-based techniques (PeakForce, conductive AFM) generally provide only qualitative information. The values for resistance as well as Young's modulus measured using our method on the prototypical ITO/PEDOT:PSS/P3HT:PC61BM system correspond well with literature data. The P3HT:PC61BM blend separates onto PC61BM-rich and P3HT-rich domains. Mechanical properties of PC61BM-rich and P3HT-rich domains are different, which allows for domain attribution on the surface of the film. Importantly, combining mechanical and electrical data allows for correlation of the domain structure on the surface of the film with electrical properties variation measured through the thickness of the film.

Organic photovoltaic (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale inhomogeneity of OPV materials affects performance of photovoltaic devices. In this paper, we describe a protocol for quantitative measurements of electrical and mechanical properties of OPV materials with sub-100 nm resolution.

Organic photovoltaic  (OPV) materials are inherently inhomogeneous at the nanometer scale. Nanoscale  inhomogeneity of OPV materials affects performance ...

Ultrasonic Welding of Thermoplastic Composite Coupons for Mechanical Characterization of Welded Joints through Single Lap Shear Testing

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ultrasonic welding process described in this paper is based on three main pillars. Firstly, flat energy directors are used for preferential heat generation at the joining interface during the welding process. A flat energy director is a neat thermoplastic resin film that is placed between the parts to be joined prior to the welding process and heats up preferentially owing to its lower compressive stiffness relative to the composite substrates. Consequently, flat energy directors provide a simple solution that does not require molding of resin protrusions on the surfaces of the composite substrates, as opposed to ultrasonic welding of unreinforced plastics. Secondly, the process data provided by the ultrasonic welder is used to rapidly define the optimum welding parameters for any thermoplastic composite material combination. Thirdly, displacement control is used in the welding process to ensure consistent quality of the welded joints. According to this method, thermoplastic-composite flat coupons are individually welded in a single lap configuration. Mechanical testing of the welded coupons allows determining the apparent lap shear strength of the joints, which is one of the properties most commonly used to quantify the strength of thermoplastic composite welded joints.

A straightforward procedure for ultrasonic welding of thermoplastic composite coupons for basic mechanical testing is described. Key characteristics of this ultrasonic welding process are the use of flat energy directors for simplified process preparation and the use of process data for the fast definition of optimum processing conditions.

This paper presents a novel straightforward method for ultrasonic welding of thermoplastic-composite coupons in optimum processing conditions. The ...

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

Nanostructured Ag-zeolite Composites as Luminescence-based Humidity Sensors

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high external quantum efficiencies (EQE) and spans the whole visible spectrum. It has been recently reported that the UV excited luminescence of partially Li-exchanged sodium Linde type A zeolites [LTA(Na)] containing luminescent silver clusters can be controlled by adjusting the water content of the zeolite. These samples showed a dynamic change in their emission color from blue to green and yellow upon an increase of the hydration level of the zeolite, showing the great potential that these materials can have as luminescence-based humidity sensors at the macro and micro scale. Here, we describe the detailed procedure to fabricate a humidity sensor prototype using silver-exchanged zeolite composites. The sensor is produced by suspending the luminescent Ag-zeolites in an aqueous solution of polyethylenimine (PEI) to subsequently deposit a film of the material onto a quartz plate. The coated plate is subjected to several hydration/dehydration cycles to show the functionality of the sensing film.

A protocol for the synthesis of moisture-responsive luminescent Ag-zeolite composites is described in this report.

Small silver clusters confined inside zeolite matrices have recently emerged as a novel type of highly luminescent materials. Their emission has high ...

A Novel Biaxial Testing Apparatus for the Determination of Forming Limit under Hot Stamping Conditions

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional experimental approaches, such as out-of-plane and in-plane tests, are not applicable to the determination of forming limits when heating and rapid cooling processes are introduced prior to forming for tests conducted under hot stamping conditions. A novel in-plane biaxial testing system was designed and used for the determination of forming limits of sheet metals at various strain paths, temperatures, and strain rates after heating and cooling processes in a resistance heating uniaxial testing machine. The core part of the biaxial testing system is a biaxial apparatus, which transfers a uniaxial force provided by the uniaxial testing machine to a biaxial force. One type of cruciform specimen was designed and verified for the formability test of aluminum alloy 6082 using the proposed biaxial testing system. The digital image correlation (DIC) system with a high-speed camera was used for taking strain measurements of a specimen during a deformation. The aim of proposing this biaxial testing system is to enable the forming limits of an alloy to be determined at various temperatures and strain rates under hot stamping conditions.

This protocol proposes a novel biaxial testing system used on a resistance heating uniaxial tensile test machine in order to determine the forming limit diagram (FLD) of sheet metals under hot stamping conditions.

The hot stamping and cold die quenching process is increasingly used to form complex shaped structural components of sheet metals. Conventional ...

Preparation of Aligned Steel Fiber Reinforced Cementitious Composite and Its Flexural Behavior

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the Earth&#39;s magnetic field, for manufacturing a cementitious composite reinforced with aligned steel fibers. Aligned steel fiber reinforced cementitious composites (ASFRC) were prepared by applying a uniform electromagnetic field to fresh mortar containing short steel fibers, whereby the short steel fibers were driven to rotate in alignment with the magnetic field. The degree of alignment of steel fibers in hardened ASFRC was assessed both by counting steel fibers in fractured cross-sections and by X-ray computed tomography analysis. The results from the two methods show that the steel fibers in ASFRC were highly aligned while the steel fibers in non-magnetically treated composites were randomly distributed. The aligned steel fibers had a much higher reinforcing efficiency, and the composites, therefore, exhibited significantly enhanced flexural strength and toughness. The ASFRC is thus superior to SFRC in that it can withstand greater tensile stress and more effectively resist cracking.

This protocol describes an approach for manufacturing aligned steel fiber reinforced cementitious composite by applying a uniform electromagnetic field. Aligned steel fiber reinforced cementitious composite exhibits superior mechanical properties to ordinary fiber reinforced concrete.

The aim of this work is to present an approach, inspired by the way in which a compass needle maintains a consistent orientation under the action of the ...

Installation Method to Enhance Quality Control for Fiber Reinforced Polymer Spike Anchors

Fiber reinforced polymer (FRP) anchors are a promising way to enhance the performance of externally-bonded FRPs applied to existing structures, as they can delay or even prevent debonding failure. However, a major concern faced by designers is the premature failure of the anchors due to stress concentration. Poor installation quality and preparation of the clearance holes can result in stress concentration that provokes this premature failure. This paper deals with an installation method that aims to reduce the impact of the stress concentration and to provide a proper quality control of the preparation of the drill hole. The method involves three parts: the drilling and cleaning of the holes, the smoothing of the hole edges with a customized drill bit, and the installation of the anchor itself, including the impregnation of the anchor dowel and its insertion. Anchor fans (the free length of the spikes) are then bonded to the external FRP reinforcement. For the end anchorage, and in the case of reinforcements with multiple plies, it is recommended that the anchor fan be inserted between two plies to assist the stress-transfer mechanism. 
The proposed procedure is complemented with a design approach for spike anchors, based on an extensive database. It is proposed that the design follow a number of steps, namely: selection of the anchor diameter and subsequent tensile strength of the connector (that is to say, the anchor before fanning out the free end), evaluation of the reduction in the tensile strength due to bending, provision of enough embedment to prevent slippage failure, and consideration of the number and spacing of anchors for a given reinforcement. In this sense, it should be noted that further research is needed in order to obtain a general expression for the contribution of spike anchors to overall bond strength of FRP reinforcements.

This manuscript presents a method for controlling the quality of installation for spike anchors designed to delay delamination of externally bonded fiber reinforced polymers. The protocol includes the preparation of the drill hole and the insertion process. The most influential parameters on the efficiency of the anchors are discussed.

Fiber reinforced polymer (FRP) anchors are a promising way to enhance the performance of externally-bonded FRPs applied to existing structures, as they ...

Applicability Analysis of Assessment Methods for Morphological Parameters of Corroded Steel Bars

The irregular and uneven residual sections along the length of a corroded steel bar substantially change its mechanical properties and significantly dominate the safety and performance of an existing concrete structure. As a result, it is important to measure the geometry and amount of corrosion of a steel bar in a structure properly to assess the residual bearing capacity and service life of the structure. This paper introduces and compares five different methods for measuring the geometry and amount of corrosion of a steel bar. A single 500 mm long and 14 mm diameter steel bar is the specimen that is subjected to accelerated corrosion in this protocol. Its morphology and the amount of corrosion were carefully measured before and after using mass loss measurements, a Vernier caliper, drainage measurements, 3D scanning, and X-ray micro-computed tomography (XCT). The applicability and suitability of these different methods were then evaluated. The results show that the Vernier caliper is the best choice for measuring the morphology of a non-corroded bar, while 3D scanning is the most suitable for quantifying the morphology of a corroded bar.

This paper measures the geometry and the amount of corrosion of a steel bar using different methods: mass loss, calipers, drainage measurements, 3D scanning, and X-ray micro-computed tomography (XCT).

The irregular and uneven residual sections along the length of a corroded steel bar substantially change its mechanical properties and significantly ...

Method Development for Contactless Resonant Cavity Dielectric Spectroscopic Studies of Cellulosic Paper

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of data that can be obtained from an individual sample and renders it difficult to produce statistically relevant data for unique and rare materials. Resonant cavity dielectric spectroscopy is a non-destructive, contactless technique which can simultaneously interrogate both sides of a sheeted material and provide measurements which are suitable for statistical interpretations. This offers analysts the ability to quickly discriminate between sheeted materials based on composition and storage history. In this methodology article, we demonstrate how contactless resonant cavity dielectric spectroscopy may be used to differentiate between paper analytes of varying fiber species compositions, to determine the relative age of the paper, and to detect and quantify the amount of post-consumer waste (PCW) recycled fiber content in manufactured office paper.

A protocol for the non-destructive analysis of the fiber content and relative age of paper.

The current analytical techniques for characterizing printing and graphic arts substrates are largely ex situ and destructive. This limits the amount of ...