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1. Influence of multi-walled carbon nanotubes on the hydration products of ordinary Portland cement paste

   https://doi.org/https://doi.org/10.1016/j.cemconres.2020.106197  

   Jiaxin Chen, Ange-Therese Akono (November 2020, Cement and concrete research)

   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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2. Multiwalled carbon nanotubes as hard templates to yield advanced geopolymer-based self-assembled nanostructured ceramics

   https://doi.org/10.1016/j.mechrescom.2023.104216  

   Xu, Yunzhi; Lee, Haklae; Buettner, Nathanial; Akono, Ange-Therese (December 2023, Mechanics Research Communications)

   Novel multifunctional construction materials are needed to promote resilient infrastructure in the face of climate change and extreme weather. Nanostructured materials such as geopolymer reinforced with carbon-based nanomaterials are a promising way to reach that goal. In recent years, several studies have investigated the influence of nanomaterials on the physical properties of geopolymer composites such as compressive strength and fracture toughness. Yet, a fundamental understanding of the influence of nanomaterials on the nanoscale and micron-scale structure has been elusive so far. Our research objective is to understand how multiwalled carbon nanotubes (MWCNT) can help tailor the microstructure of geopolymers to yield architected multifunctional nanocomposites. We synthesized geopolymer nanocomposites reinforced with 50-nm thick multiwalled carbon nanotubes with mass fractions in the range of 0.1 wt%, 0.2 wt%, and 0.5 wt%. Our major finding is that MWCNTs act as hard templates that promote geopolymer formation via self-assembly. Geopolymer nanoparticle growth is observed along the walls of MWCNTs. A refinement in grain size is observed: increasing the fraction of MWCNTs by 0.5 wt% leads to a reduction in grain size by 54%. Similarly, increasing the mass fraction of MWCNTs leads to a densification of the geopolymer matrix as demonstrated by the Fourier transform infrared spectroscopy results and the statistical deconvolution analysis. Mercury intrusion porosimetry shows a nanoscale tailoring of the pore size distribution: a 26% decrease in porosity is observed as the fraction of MWCNTs is increased to 0.5 wt%. As a result of these nanoscale structural changes, a greater resistance to long-term deformation is observed for MWCNT-reinforced geopolymers, as the creep modulus increases both locally and macroscopically. At the macroscopic level, a 42% increase in the macroscopic logarithmic creep modulus is observed as the fraction of MWCNTs is increased to 0.5 wt%. These findings and the supporting methodology are important to understand how to manipulate matter below 100 nm. This research also paves the way for the design of resilient infrastructure materials with tailored microstructure and mechanical properties. 

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3. Nanostructure and Fracture Behavior of Carbon Nanofiber-Reinforced Cement Using Nanoscale Depth-Sensing Methods

   https://doi.org/10.3390/ma13173837  

   Akono, Ange-Therese (September 2020, Materials)

   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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4. Thermoelectric, Magnetic, and Mechanical Characteristics of Antiferromagnetic Manganese Telluride Reinforced with Graphene Nanoplates

   https://doi.org/10.1002/adem.202000816  

   Hooshmand Zaferani, Sadeq; Ghomashchi, Reza; Vashaee, Daryoosh (October 2020, Advanced Engineering Materials)

   Mechanical and thermal stability are the two challenging aspects of thermoelectric compounds and modules. Microcrack formation during material synthesis and mechanical failure under thermo‐mechanical loading is commonly observed in thermoelectric materials made from brittle semiconductors. Herein, the results of graphene‐nanoplates (GNPs) reinforcement on the mechanical and thermoelectric properties of MnTe compound are reported. The binary antiferromagnetic MnTe shown promising thermoelectric characteristics due to the paramagnon–hole drag above the Néel temperature. In this study, different bulk MnTe samples are synthesized with the addition of GNPs in a small quantity (0.25–1 wt%) by powder metallurgy and spark plasma sintering. The thermoelectric factors, magnetic behavior, microstructure, and mechanical properties of the samples are evaluated and analyzed. Nearly 33% improvement is observed in the fracture toughness of MnTe reinforced with 0.25 wt% GNPs compared to the pristine structure. The Néel temperature remains approximately unaffected with the GNP inclusion; however, the low‐temperature ferromagnetic phase impurity is significantly suppressed. The thermal conductivity and power factor decrease almost equally by ≈34% at 600 K; hence, the thermoelectric figure‐of‐merit is not affected by GNP reinforcement in the optimized sample. 

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5. Fracture toughness and fatigue crack growth resistance of precipitate-free and precipitation hardened NiTiHf shape memory alloys

   https://doi.org/10.1016/j.msea.2024.146443  

   Young, Benjamin; Orrostieta, Roberto; Haghgouyan, Behrouz; Lagoudas, Dimitris C; Baxevanis, T; Karaman, Ibrahim (May 2024, Materials Science and Engineering: A)

   The present work investigates fracture toughness, and actuation and mechanical fatigue crack growth responses of Ni50.3Ti29.7Hf20 HTSMAs across martensitic transformation with two different microstructures, one with H-phase nanoprecipitates and one without. H-phase precipitation is known to stabilize the actuation cycling response of NiTiHf HTSMAs and notably impacts transformation-induced plasticity. The fracture toughness tests performed reveal that precipitate-free NiTiHf has a higher fracture toughness and undergoes significantly more inelastic deformation than the one with the precipitates resulting in toughness enhancement, i.e., stable crack advance during fracture toughness experiments, which is not observed in the precipitated NiTiHf for the crack configuration and loading conditions tested. Furthermore, the precipitate free NiTiHf has higher actuation and mechanical fatigue crack growth resistance than the precipitation-hardened microstructure. This is attributed to plasticity buildup, which exacerbates the manifestation of retained martensite upon repeated transformations. The fatigue crack growth rates obtained from both actuation and mechanical fatigue experiments align to a single Paris Law Curve for the precipitation-hardened NiTiHf. This work aims to determine if unified Paris Law curves can be generated from mechanical and actuation fatigue experiments, irrespective of composition and microstructure, to estimate actuation fatigue crack growth rates, laborious and challenging to measure, from easier to detect mechanical fatigue crack growth rates. 

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