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Temporary pavement marking (TPM) tape adhesion with roadway surfaces is critical for tape performance. The two main TPM performance issues both stem from the adhesive strength. Weak adhesion results in premature detachment and excessive adhesion requires extensive removal processes that often leave ghost markings, both of which can cause dangerous confusion in road construction zones. Tape adhesion is directly related to the elastic modulus [Formula: see text] of TPM tapes. Thus, accurate characterization of [Formula: see text] before tape installation is essential to fully understand and predict the adhesion performance and ultimately the durability of TPMs. To determine the most appropriate [Formula: see text] characterization technique for three different commercial TPM tape brands, two commonly used techniques—tensile and three-point bend testing—were compared with a less common technique, the Peirce cantilever testing or “Tape Drape Test” (ASTM D1388-18). The Tape Drape Test was the only method that accurately characterized [Formula: see text] of tapes with raised surface features. Measured [Formula: see text] values from tensile and three-point bend testing showed significant variation caused by the structural features of the tapes. The Tape Drape Test, which can be implemented quickly in the field before tape installation with little equipment, effectively characterized [Formula: see text] for all the tapes to inform tape adhesion performances and installation procedures.

The ability to control adhesion is critical in various technologies including wearable electronics, pressure sensitive adhesives, and robotic systems. Biomimetic fibrillar structures, random surface roughness, and chemical surface treatments have been employed to modify the adhesion energy of materials used in these applications. However, polymer thin film dewetting has not been investigated as a surface modification tool to control adhesion. In this work, polystyrene thin films are thermally annealed on a polydimethylsiloxane substrate, causing them to dewet and form stiff, microscopic asperities on the soft substrate. The size of the asperities increases with increasing pre-annealing film thickness. Adhesion is quantified by flat-punch normal indentation testing. The largest asperities exhibited a decrease in adhesion to below the sensitivity of the instrument. More interestingly, the surfaces covered with the smallest asperities displayed a pressure-dependent adhesive response. By increasing the normal compressive stress applied prior to separation, the total debonding energy increased monotonically on the smallest asperity-covered surfaces.

Mechanophores (MPs) are a class of stimuli-responsive materials that are of increasing interest to engineers due to their potential applications as stress sensors. These mechanically responsive molecules change color or become fluorescent upon application of a mechanical stimulus as they undergo a chemical reaction when a load is applied. By incorporating MPs such as spirolactam, spiropyran, or dianthracene into a material system, the real-time stress distribution of the matrix can be directly observed through a visual response, ideal for damage and failure sensing applications. A wide array of applications that require continuous structural health monitoring could benefit from MPs including flexible electronics, protective coatings, and polymer matrix composites. However, there are significant technical challenges preventing MP implementation in industry. Effective strategies to quantitatively calibrate the photo response of the MP with applied stress magnitudes must be developed. Additionally, environmental conditions, including temperature, humidity, and ultraviolet light exposure can potentially impact the performance of MPs. By addressing these limitations, engineers can work to move MPs from the synthetic chemistry bench to the field. This review aims to highlight recent progress in MP research, discuss barriers to implementation, and provide an outlook on the future of MPs, specifically focused on polymeric material systems. Although the focus is on engineering MPs for bulk materials, a brief overview of mechanochemistry will be discussed followed by methods for activation and quantification of MP photo response (concentrating specifically on fluorescently active species). Finally, current challenges and future directions in MP research will be addressed.

Edges of two-dimensional (2D) halide perovskites are found to exhibit unusual properties such as enhanced photoluminescence lifetime and reduced photoluminescence emission energy. Here, we report the formation mechanism and the dynamic nature of edge states on exfoliated 2D halide perovskite thin crystals. In contrast to other 2D materials, the edge states in 2D perovskites are extrinsic and can be triggered by moisture with a concentration as low as ∼0.5 ppm. High-resolution atomic force microscopy and transmission electron microscopy characterizations reveal the width of the low-energy states is ∼40 nm wide. A temperature-dependent photoluminescence study suggests the edge states are a combination of several lower-energy states. Importantly, we demonstrate that the charge carriers on the dynamically formed edge states are not only long-lived but also highly mobile and can be conducted along the edges effectively with high mobilities of 5.4-7.0 cm2 V-1 s-1. This work provides significant insights on the origin of the edge states in 2D perovskites and provides routes to manipulate their optical and electrical properties through controlling their edges.

The mechanical properties of cellulose nanocrystal (CNC) films critically depend on many microstructural parameters such as fiber length distribution (FLD), fiber orientation distribution (FOD), and the strength of the interactions between the fibers. In this paper, we use our coarse-grained molecular model of CNC to study the effect of length and orientation distribution and attractions between CNCs on the mechanical properties of neat CNCs. The effect of misalignment of a 2D staggered structure of CNC with respect to the loading direction was studied with simulations and analytical solutions and then verified with experiments. To understand the effect of FLD and FOD on the mechanical performance, various 3D microstructures representing different case studies such as highly aligned, randomly distributed, short length CNCs and long length CNCs were generated and simulated. According to the misalignment study, three different failure modes: sliding mode, mixed mode, and normal mode were defined. Also, comparing the effects of FOD, FLD, and CNC interaction strength, shows that the adhesion strength is the only parameter that can significantly improve the mechanical properties, regardless of loading direction or FOD of CNCs.

Compressing a thin, stiff film attached to a thick, compliant substrate can lead to a number of different modes of mechanical deformation depending upon the material properties of the system. In this article we explore direct transitions from surface wrinkling to buckle delamination, and provide a theoretical framework for understanding the conditions under which such transitions take place, as well as the resulting dimensions of the wrinkling-induced delamination. A key conclusion of this work is that the width of the delamination blister formed from a wrinkled film is relatively strain-independent, suggesting that delaminations can be used in such systems to measure the adhesion energy at the film-substrate interface. In addition, we demonstrate how the length and width of delaminations can be tailored through straightforward control of the substrate and film properties in the system, illustrating how wrinkling delaminations can be used for both thin film metrology and patterning applications.

Understanding the adhesion of rigid thin films to compliant substrates is critical for the development and implementation of flexible electronic devices and wearable sensor technologies. Quantifying the strength of a film-substrate interface can be challenging due to the brittleness of glassy films which can greatly complicate sample preparation, handling, and testing. Here, a method for measuring the adhesion of glassy thin films to soft elastomeric substrates is explored that exploits an understanding of surface buckling instabilities, specifically the transition from wrinkling to delamination. The adhesion (given by the critical strain energy release rate (Gc)) for two model materials' interfaces is quantified by determining the critical delamination strain for thin glassy polymer films (polystyrene (PS) and poly(methyl methacrylate) (PMMA)) from an elastomeric substrate (poly(dimethyl siloxane) (PDMS)). By accounting for edge defects that greatly reduce the critical strain for delamination, reasonable adjusted Gc values of 21.0 ± 5.1 mJ m-2 and 32.2 ± 4.9 mJ m-2 are found for PS-PDMS and PMMA-PDMS interfaces, respectively. The utilization of this method to characterize film modulus and adhesion could be used as a facile measurement technique for more applied polymer thin film systems.

Substantial research efforts are under way to optimize the production of composites enhanced by the incorporation of nanomaterial fillers such as multiwall carbon nanotubes (MWCNTs). It is therefore critical to develop robust methods to detect and characterize MWCNTs in nanocomposites to measure product performance and potential risks from release of the MWCNTs. In this study, the effectiveness of X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and scanning electron microscopy (SEM) methods is assessed on a series of MWCNT-epoxy nanocomposites samples. A general trend of positive correlation between signal intensity and MWCNT mass loading was observed by both Raman spectroscopy and XPS. Raman spectroscopy was capable of detecting MWCNTs at the lowest nominal concentration tested (0.01%), while for XPS, MWCNTs were detected down to a threshold of approximately 0.5%. Analysis of the same locations of two nanocomposite samples with nominal MWCNT mass fractions of 0.3% and 1% using Raman chemical imaging and SEM revealed a similar detectability of MWCNT clusters and with the higher mass loading sample having a greater number of MWCNT-rich domains. Overall, these results show a good comparability among the different techniques and therefore provide comprehensive, nondestructive microscopy methods to characterize nanocomposites.

Carbon nanotube (CNT) polymer nanocomposites are attractive multifunctional materials with a growing range of commercial applications. With the increasing demand for these materials, it is imperative to develop and validate methods for on-line quality control and process monitoring during production. In this work, a novel combination of characterization techniques is utilized, that facilitates the non-invasive assessment of CNT dispersion in epoxy produced by the scalable process of calendering. First, the structural parameters of these nanocomposites are evaluated across multiple length scales (10 −10 m to 10− 3 m) using scanning gallium-ion microscopy, transmission electron microscopy and small-angle neutron scattering. Then, a non-contact resonant microwave cavity perturbation (RCP) technique is employed to accurately measure the AC electrical conductivity of the nanocomposites. Quantitative correlations between the conductivity and structural parameters find the RCP measurements to be sensitive to CNT mass fraction, spatial organization and, therefore, the processing parameters. These results, and the non-contact nature and speed of RCP measurements identify this technique as being ideally suited for quality control of CNT nanocomposites in a nanomanufacturing environment. When validated by the multiscale characterization suite, RCP may be broadly applicable in the production of hybrid functional materials, such as graphene, gold nanorod, and carbon black nanocomposites.

Cellulose nanocrystals (CNCs) have great potential as sustainable reinforcing materials for polymers, but there are a number of obstacles to commercialization that must first be overcome. High levels of water absorption, low thermal stabilities, poor miscibility with nonpolar polymers, and irreversible aggregation of the dried CNCs are among the greatest challenges to producing cellulose nanocrystal–polymer nanocomposites. A simple, scalable technique to modify sulfated cellulose nanocrystals (Na-CNCs) has been developed to address all of these issues. By using an ion exchange process to replace Na+ with imidazolium or phosphonium cations, the surface energy is altered, the thermal stability is increased, and the miscibility of dried CNCs with a nonpolar polymer (epoxy and polystyrene) is enhanced. Characterization of the resulting ion exchanged CNCs (IE-CNCs) using potentiometry, inverse gas chromatography, dynamic vapor sorption, and laser scanning confocal microscopy reveals that the IE-CNCs have lower...

Carbon nanotube (CNT) nanocomposites are enticing materials that enable engineers to tailor structural and electrical properties for applications in the automotive and aerospace industries. CNT mass fraction and the matrix cure temperature are two ways to tune the direct and alternating current electrical properties of these nanocomposites; yet, how mass fraction and cure temperature affect electrical properties remains unclear. In many cases, nanofillers such as carbon nanotubes appear in concentrated domains within the nanocomposite. Recent insights into nanoparticle-rich domain formation and its influence on electrical properties raise questions about which processing variables might optimally tune a material's functionality. Utilizing recently developed, nondestructive measurement techniques such as scanning lithium ion microscopy and microwave cavity perturbation spectroscopy, new insights are presented into the role of mass fraction and cure temperature in multiwall carbon nanotube – bisphenol A diglycidyl ether epoxy composites. Here, it is found that both mass fraction and cure temperature affect the electrical properties. Specifically, beyond the electrical percolation threshold, the DC conductivity is an order of magnitude higher for composites prepared at elevated cure temperatures for a given CNT mass fraction. Direct observations of the microdomain morphology do not show substantial differences due to cure temperature. These findings suggest pathways to generate designer nanocomposites for advanced electrically-active applications.

Highly efficient broadband light management to enhance the light trapping inside active layer is critical for many energy conversion devices such as thin film solar cells and photoelectrochemical cells. In this work, we demonstrate highly transparent, mesoporous wood composite via fast extraction of lignin along naturally formed low tortuosity channels followed by fast filling of polymers. The transparent wood displays a high optical transmittance and at the same time a high haze in a broad wavelength range between 400 nm and 1100 nm. With such unique optical properties, the transparent wood composite with cellulose nanofibers can be utilized for a range of optoelectronics, especially for solar cells and wide-angle lighting where light management is crucial to enhance device operation efficiency. We demonstrate that the newly developed transparent wood composite can function as a broad range light management layer and substantially improve the overall energy conversion efficiency by as much as 18% when simply coated with a GaAs thin film solar cell. Our research on wood based light management material provides an attractive platform for future development embracing green, disposable optoelectronic devices with efficient light management.

Material extrusion (ME)2 is a layer-by-layer additive manufacturing process that is now used in personal and commercial production where prototyping and customization are required. However, parts produced from ME frequently exhibit poor mechanical performance relative to those from traditional means; moreover, fundamental knowledge of the factors leading to development of inter-layer strength in this highly non-isothermal process is limited. In this work, we seek to understand the development of inter-layer weld strength from the perspective of polymer interdiffusion under conditions of rapidly changing mobility. Our framework centers around three interrelated components: in-situ thermal measurements (via infrared imaging), temperature dependent molecular processes (via rheology), and mechanical testing (via mode III fracture). We develop the concept of an equivalent isothermal weld time and test its relationship to fracture energy. For the printing conditions studied the equivalent isothermal weld time for Tref = 230 °C ranged from 0.1 ms to 100 ms. The results of these analysis provide a basis for optimizing inter-layer strength, the limitations of the ME process, and guide development of new materials.

Polymer composite materials are found throughout the world both natural and artificial in origin. In the vast majority of applications in these arenas, composites serve as structural support or reinforcement. Demand for lightweight tough composites is growing in multiple application spaces such as aerospace, biomaterials, and infrastructure with physical properties as diverse as the applications. The unifying component in all composites is the presence of the interphase. Many measurement techniques and measurement tools have been developed for the study of this crucial region in composite materials. Many of these methods are great for the measurement and study of bulk properties or model systems. However, development of tools that permit the direct observation of interactions at the interphase during applied stress are needed. Here we employ fluorescence lifetime imaging and hyperspectral imaging to observe activation of a fluorogenic dye at the composite interface as a result of applied stress. The advantages of this system include commercial availability of the dye precursor, and simple one-pot functionalization. The attachment of the dye at the interface is easily monitored through emission wavelength shifts or fluorescence lifetime. Interfacial mechano-responsive dyes have potential for both fundamental studies as well as industrial use as a structural health monitoring tool.

International audience; The adhesive properties of a material can be greatly affected simply by wrinkling its surface. We show the importance of selecting the wrinkle feature sizes (amplitude, b; and wavelength, lambda) that complement the material-defined length scale related to the adhesion energy and modulus. A rigid circular cylindrical punch patterned with aligned wrinkles ranging in amplitude from 0.5 to 5.0 mu m with a fixed aspect ratio of 0.1 is used to characterize the adhesion of elastic films of smooth poly(dimethyl siloxane) (PDMS). The cross-linker concentration used to form the PDMS layers is varied to determine the impact of material properties on wrinkled surface adhesion. The elastic films have an average thickness of 240 mu m and the average probe radius is 1 mm, leading to a confined contact scenario. The separation stress and work of debonding are presented for each cross-linker concentration with testing rates ranging over 3 orders of magnitude. For stiffer films (10 wt % cross-linker, E' approximate to 3.00 MPa), small wrinkles (b approximate to 0.5 mu m) increase the separation stress by nearly 200% relative to a smooth interface whereas large wrinkles (b approximate to 5.0 mu m) are shown to reduce adhesion significantly. A substantial increase in the debonding energy is also observed for these small-amplitude wrinkles contacting stiff materials. No discernible impact of wrinkled surface topography on the adhesion of softer (2 and 4 wt % cross-linker, 0.05 MPa < E' < 0.30 MPa) films is measured.