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Abstract Controlling the self-assembly of carbon nanotube (CNT) forests is important for tailoring their ensemble properties for specific applications. In this study, real-time electrical resistance measurements of in-situ CNT forest syntheses was established as a method to interrogate the evolution of CNT forest morphology. The method employs in-situ scanning electron microscopy (SEM) synthesis techniques to correlate observed morphological changes to electrical resistance. A finite-element simulation was used to simulate CNT forest synthesis and the evolution of electrical resistance in a configuration like that used experimentally. The simulation considers the contribution of CNT electrical resistance, CNT-CNT junction resistance, and CNT-electrode contact resistance. Simulation results indicate that an increased number of CNT-CNT junctions with time have a diminishing effect on increasing electrical conductance. Experimentally observed increases in electrical resistance are attributed to increasing CNT delamination from the electrical contacts. 

The piezoresistance of carbon nanotube (CNT)-coated microfibers is examined using diametric compression. Diverse CNT forest morphologies were studied by changing the CNT length, diameter, and areal density via synthesis time and fiber surface treatment prior to CNT synthesis. Large-diameter (30–60 nm) and relatively low-density CNTs were synthesized on as-received glass fibers. Small-diameter (5–30 nm) and-high density CNTs were synthesized on glass fibers coated with 10 nm of alumina. The CNT length was controlled by adjusting synthesis time. Electromechanical compression was performed by measuring the electrical resistance in the axial direction during diametric compression. Gauge factors exceeding three were measured for small-diameter (<25 μm) coated fibers, corresponding to as much as 35% resistance change per micrometer of compression. The gauge factor for high-density, small-diameter CNT forests was generally greater than those for low-density, large-diameter forests. A finite element simulation shows that the piezoresistive response originates from both the contact resistance and intrinsic resistance of the forest itself. The change in contact and intrinsic resistance are balanced for relatively short CNT forests, while the response is dominated by CNT electrode contact resistance for taller CNT forests. These results are expected to guide the design of piezoresistive flow and tactile sensors. 

Electron microscopy images of carbon nanotube (CNT) forests are difficult to segment due to the long and thin nature of the CNTs; density of the CNT forests resulting in CNTs touching, crossing, and occluding each other; and low signal-to-noise ratio electron microscopy imagery. In addition, due to image complexity, it is not feasible to prepare training segmentation masks. In this paper, we propose CNTSegNet, a dual loss, orientation-guided, self-supervised, deep learning network for CNT forest segmentation in scanning electron microscopy (SEM) images. Our training labels consist of weak segmentation labels produced by intensity thresholding of the raw SEM images and self labels produced by estimating orientation distribution of CNTs in these raw images. The proposed network extends a U-net-like encoder-decoder architecture with a novel two-component loss function. The first component is dice loss computed between the predicted segmentation maps and the weak segmentation labels. The second component is mean squared error (MSE) loss measuring the difference between the orientation histogram of the predicted segmentation map and the original raw image. Weighted sum of these two loss functions is used to train the proposed CNTSegNet network. The dice loss forces the network to perform background-foreground segmentation using local intensity features. The MSE loss guides the network with global orientation features and leads to refined segmentation results. The proposed system needs only a few-shot dataset for training. Thanks to it’s self-supervised nature, it can easily be adapted to new datasets. 

Carbon nanotube (CNT) forests are imaged using scanning electron microscopes (SEMs) that project their multilayered 3D structure into a single 2D image. Image analytics, particularly instance segmentation is needed to quantify structural characteristics and to predict correlations between structural morphology and physical properties. The inherent complexity of individual CNT structures is further increased in CNT forests due to density of CNTs, interactions between CNTs, occlusions, and lack of 3D information to resolve correspondences when multiple CNTs from different depths appear to cross in 2D. In this paper, we propose CNT-NeRF, a generative adversarial network (GAN) for simultaneous depth layer decomposition and segmentation of CNT forests in SEM images. The proposed network is trained using a multi-layer, photo-realistic synthetic dataset obtained by transferring the style of real CNT images to physics-based simulation data. Experiments show promising depth layer decomposition and accurate CNT segmentation results not only for the front layer but also for the partially occluded middle and back layers. This achievement is a significant step towards automated, image-based CNT forest structure characterization and physical property prediction. 

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