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  1. Abstract

    We investigate the fracture response of metakaolin‐based geopolymer reinforced with 0.1 wt%, 0.2 wt%, and 0.5 wt% carbon nanofibers. We measure the elastoplastic response using microindentation tests. We note an increase in indentation modulus of 5%, 13%, and 21%, and an increase in indentation hardness of 9%, 18%, and 25%, respectively. We measure the fracture energy using cutting‐edge microscopic fracture tests. In our tests, a sphero‐conical diamond indenter pushes across the specimen's surface under a prescribed vertical force. We analyze the recorded penetration depth and horizontal force using nonlinear fracture mechanics and extract the fracture parameters. We find that carbon nanofibers enhance fracture resistance. The fracture toughness increases by, respectively, 38%, 40%, and 45%; meanwhile, the fracture energy increases by, respectively, 83%, 72%, and 74%. We find that carbon nanofibers lead to a densification of the microstructure. Moreover, we observe crack‐bridging mechanisms in geopolymer nanocomposites. This study is important to pave the way for novel enhanced‐performance and multifunctional structural materials.

     
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  2. Electrospinning is a versatile approach to generate nanofibers in situ. Yet, recently, wet electrospinning has been introduced as a more efficient way to deposit isolated fibers inside bulk materials. In wet electrospinning, a liquid bath is adopted, instead of a solid collector, for fiber collection. However, despite several studies focused on wet electrospinning to yield polymer composites, few studies have investigated wet electrospinning to yield ceramic composites. In this paper, we propose a novel in-situ fabrication approach for nanofiber-reinforced ceramic composites based on an enhanced wet-electrospinning method. Our method uses electrospinning to draw polymer nanofibers directly into a reactive pre-ceramic gel, which is later activated to yield advanced nanofiber-reinforced ceramic composites. We demonstrate our method by investigating wet electrospun Polyacrylonitrile and Poly(ethylene oxide) fiber-reinforced geopolymer composites, with fiber weight fractions in the range 0.1–1.0 wt%. Wet electrospinning preserves the amorphous structure of geopolymer while changing the molecular arrangement. Wet electrospinning leads to an increase in both the fraction of mesopores and the overall porosity of geopolymer composites. The indentation modulus is in the range 6.76–8.90 GPa and the fracture toughness is in the range 0.49–0.76 MPam with a clear stiffening and toughening effect observed for Poly(ethylene oxide)-reinforced geopolymer composites. This work demonstrates the viability of wet electrospinning to fabricate multifunctional nanofiber-reinforced composites. 
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    Cement is the most widely consumed material globally, with the cement industry accounting for 8% of human-caused greenhouse gas emissions. Aiming for cement composites with a reduced carbon footprint, this study investigates the potential of nanomaterials to improve mechanical characteristics. An important question is to increase the fraction of carbon-based nanomaterials within cement matrices while controlling the microstructure and enhancing the mechanical performance. Specifically, this study investigates the fracture response of Portland cement reinforced with 1D and 2D carbon-based nanomaterials, such as carbon nanofibers, multiwalled carbon nanotubes, helical carbon nanotubes, and graphene oxide nanoplatelets. Novel processing routes are shown to incorporate 0.1–0.5 wt% of nanomaterials into cement using a quadratic distribution of ultrasonic energy. Scratch testing is used to probe the fracture response by pushing a sphero-conical probe against the surface of the material under a linearly increasing vertical force. Fracture toughness is then computed using a nonlinear fracture mechanics model. Nanomaterials are shown to bridge nanoscale air voids, leading to pore refinement, and a decrease in the porosity and the water absorption. An improvement in fracture toughness is observed in cement nanocomposites, with a positive correlation between the fracture toughness and the mass fraction of nanofiller for graphene-reinforced cement. Moreover, for graphene-reinforced cement, the fracture toughness values are in the range of 0.701 to 0.717 MPa.sqrt(m). Thus, this study illustrates the potential of nanomaterials to toughen cement while improving the microstructure and water resistance properties. 
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  5. null (Ed.)
    We elucidate the mechanisms by which multi-walled carbon nanotubes (MWCNTs) influence the microstructure, fracture behavior, and hydration of cement paste. We disperse MWCNTs using a multi-step approach that involves high-energy pre-dispersion using ultrasonic energy followed by low-energy dispersion using un-hydrated cement particles. In turn, the low-energy dispersion step involves high-shear mixing and mechanical stirring. High-resolution environmental scanning electron microscopy of cement+0.2 wt% MWCNT, cement+0.5 wt% MWNCT, and of cement+1 wt% MWCNT show that MWCNTs bridge air voids, thereby refining the pore size and strengthening the C-S-H matrix. The fracture toughness increased by 9.38% with the addition of 0.2 wt% multi-walled carbon nanotubes, and by 14.06% with the addition of 0.5 wt% multi-walled carbon nanotubes and ligament bridging was the dominant toughening mechanism. Moreover, for all reinforcement levels, MWCNTs induced a conversion of low-density C-S-H into high-density C-S-H along with a drastic drop in the capillary porosity: adding 0.1–0.5 wt% MWCNT resulted in a 200% increase in the volume fraction of high-density C-S-H. Thus, our experiments show that MWCNT enhances the mechanical properties and transport properties by: (i) promoting high-density C-S-H formation, (ii) promoting calcium hydroxide formation, (iii) filling microscopic air voids, (iv) reducing the capillary porosity, (v) increasing the fraction of small gel pores (1.2–2 nm in size), and (vi) by bridging microcracks. 
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  6. In recent years, carbon nanofibers have been investigated as a suitable reinforcement for cementitious composites to yield novel multifunctional materials with improved mechanical, electrical, magnetic, and self-sensing behavior. Despite several studies, the interactions between carbon nanofibers and Portland cement hydration products are not fully understood, with significant implications for the mechanical response and the durability at the macroscopic lengthscale. Thus, the research objective is to investigate the influence of carbon nanofibers on the nanostructure and on the distribution of hydration products within Portland cement paste. Portland cement w/c = 0.44 specimens reinforced with 0.0 wt%, 0.1 wt%, and 0.5 wt% CNF by mass fraction of cement are cast using a novel synthesis procedure. A uniform dispersion of carbon nanofibers (CNF) via a multi-step approach: after pre-dispersing carbon nanofibers using ultrasonic energy, the carbon nanofibers are further dispersed using un-hydrated cement particles in high shear mixing and mechanical stirring steps. High-resolution scanning electron microscopy analysis shows that carbon nanofibers fill nanopores and connect calcium–silicate hydrates (C–S–H) grains. Grid nano-indentation testing shows that Carbon nanofibers influence the probability distribution function of the local packing density by inducing a shift towards higher values, η = 0.76–0.93. Statistical deconvolution analysis shows that carbon nanofibers result in an increase in the fraction of high-density C–S–H by 6.7% from plain cement to cement + 0.1 wt% CNF and by 10.7% from plain cement to cement + 0.5 wt% CNF. Moreover, CNF lead to an increase in the C–S–H gel porosity and a decrease in both the capillary porosity and the total porosity. Based on scratch testing, adding 0.1 wt% CNF yields a 4.5% increase in fracture toughness and adding 0.5 wt% CNF yields a 7.6% increase in fracture toughness. Finally, micromechanical modelling predicts an increase of respectively 5.97% and 21.78% in the average Young’s modulus following CNF modification at 0.1 wt% CNF and 0.5 wt% CNF levels. 
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  7. We investigate the mechanisms by which titanium dioxide nano-particles (nano-TiO2) interact with cement hydration products. To this end, we synthesize nanomodified cement samples with 1 wt% and 5 wt% of TiO2. We investigate the physical properties using depth-sensing based methods such as statistical nano-indentation and microscopic scratch testing. Fourier transform infrared spectroscopy yields the chemistry, whereas micromechanics modeling provides insights into the nanostructure. The macroscopic plane strain modulus increases by 16% and 83%, respectively, and the macroscopic indentation hardness increases by 37% and 40%, respectively. The fracture toughness rises by 3% and 11%, respectively. Environmental scanning electron microscopy reveals a 30% reduction in crack width for TiO2 cement nanocomposites compared to plain cement. Meanwhile, Fourier transform infrared spectroscopy and statistical deconvolution show an increase in the fraction of high-density calcium silicate hydrates (by 22% and 12% respectively), and in the fraction of calcium hydroxide (by 101% and 251% respectively). Within the framework of the colloidal and granular models of C-S-H, the increase in stiffness and strength after nano-TiO2 modification of cement paste is due to the closely-packed structure and the high atomic coordination number of high-density C-S-H. Similarly, due to the high dimensional stability of high-density C-S-H and calcium hydroxide, our results explain the reported improvements in drying shrinkage and creep properties following cement modification with nano-TiO2. 
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