Internal Microstructure Research Articles

Density Modifications Toward High Mechanical Performance Nanocellulose Aerogels

ABSTRACTMechanical properties are crucial for the application of nanocellulose aerogels. In this work, a series of nanocellulose aerogels with solid content concentration gradient (0.5, 1.0, 1.5, 2.0 wt%) of precursor dispersion are prepared by freeze‐drying method, and the effect of nanocellulose solid content on the mechanical properties of nanocellulose aerogels was investigated. As the solid content concentration increased, the internal microstructure of the aerogel underwent a transition from a sparse reticular structure to a tightly arranged lamellar structure. This transition led to a substantial improvement in the mechanical properties of the aerogel. At 50% strain, the compressive strength of the aerogel increased from 8.4 to 37.56 kPa with the increase of nanofibrillar cellulose solid content. Furthermore, the specific strength, specific modulus, and compressive modulus also increased, while maintaining a low density (20.02 mg/cm3) and high porosity (98.63%). This work confirms the feasibility of structural strengthening and mechanical property enhancement of nanocellulose aerogels by density modification, which provides a guidance for the design of durability enhancement of nanocellulose aerogels for broadening their application fields.

Investigation of formation, microstructure and hardness of Ti-6Al-4V single tracks via Joule-fused filament additive manufacturing

Purpose This paper aims to investigate a novel additive manufacturing (AM) method for titanium alloy using Joule heat as the single heat source to melt TC4 wire, which intends to provide a new low-power, low-cost solution for the processing of titanium alloys. Design/methodology/approach When current flows through the wire and the substrate, Joule heat will be generated to melt the wire and join the wire with the substrate. By stacking the wire layer by layer, finally a part can be formed. The cross-sectional morphology, microstructure and hardness of TC4 single track deposits formed by Joule heat melting wire AM were investigated by various characterization methods. Findings The melting width and melting penetration decreased with the increase of printing speeds. There is no obvious change in single track morphology with the change of printing pressures. The melting width and melting penetration increased with the increase of printing currents. The observation of the internal microstructure of a single track reveals a decrease in grain size as printing speeds increase. The average hardness of the single track was about 363 HV, which is comparable to the hardness of the parts fabricated by selective laser melting process. The printing power is less than 300 W, which is lower than other AM processes. Originality/value This paper provides a novel solution for the processing of titanium alloy parts. Compared with other expensive energy sources, this work only uses an ordinary DC power supply as the energy source. The printing process is simple and the cost is low. The power is much lower than other AM processes.

Sintering Behavior of Molybdenite Concentrate During Oxidation Roasting Process in Air Atmosphere: Influences of Roasting Temperature and K Content

Sintering is a common phenomenon, which often takes place during the oxidation roasting process of molybdenite concentrate in multiple-hearth furnaces. The occurrence of sintering phenomena has detrimental effects on the product quality and the service life of the furnace. In this work, the influence of two key factors (roasting temperature and K content) on the sintering behavior is investigated using molybdenite concentrate as the raw material. Different technologies such as XRD, FESEM-EDS, and phase diagrams are adopted to analyze the experimental data. The results show that the higher the roasting temperature is, the greater the mass loss and the more serious the sintering degree will be. The results also show that with the increase in K content, the mass loss of the raw material is first increased and then decreased, while its sintering degree is still gradually increased. The sintering products obtained during the oxidation roasting process are often tightly combined with the bottom of the used crucible with a smooth and dense surface structure, while their internal microstructures are very complicated, which not only includes numerous MoO3 species, but also unoxidized MoS2, Mo sub-oxide, SiO2, and a variety of molybdates. Among them, both MoO3 and molybdates can be easily dissolved into the ammonia solution, leading to a residue mainly composed of SiO2 and CaMoO4. This study also finds that the sintering phenomenon is caused by the increase in local temperature and the formation of various low-melting-point eutectics. It is suggested that decreasing the roasting temperature and K content, especially the K content, are effective methods for reducing the sintering degree of molybdenite concentrate during the oxidation roasting process.

Assessment of dwell-fatigue properties of nickel-based superalloy coated with a multi-layered thermal and environmental barrier coating

A three-layered experimental thermal and environmental barrier coating (TEBC) was deposited using air plasma spraying technology on cylindrical specimens of nickel-based superalloy MAR-M247. TEBC consists of mullite (Al6Si2O13) and hexacelsian (BaAl2Si2O8) upper layer, Y2O3 stabilised ZrO2 interlayer and CoNiCrAlY bond coat deposited on the grit-blasted surface of MAR-M247. The cyclic plastic response and damage mechanisms in uncoated and TEBC-coated MAR-M247 have been studied in isothermal dwell-fatigue tests conducted under strain control with constant strain amplitude at 900 °C. In each cycle, 5-minute dwells were introduced in both tensile and compression peaks of the hysteresis loop. Fatigue hardening/softening curves, stress relaxation curves, cyclic stress-strain curves and fatigue life curves are reported. Ceaseless mild softening has been found in both uncoated and TEBC-coated MAR-M247. TEBC-coated MAR-M247 showed an improved lifetime in the whole range of tested strain amplitudes. Data obtained from stress relaxation curves were used to assess the fraction of creep damage. The generalised damage accumulation rule was used to evaluate damage due to fatigue-creep-environment interaction. A study of the surface relief and internal microstructure using SEM and TEM helped to interpret the specifics of fatigue behaviour of uncoated and TEBC-coated material. The effectiveness of this newly developed TEBC, together with the dwell sensitivity of MAR-M247, were discussed from the perspective relevant to dwell-fatigue cyclic straining.

Potential skincare benefits and self-healing properties of Lignosus rhinocerotis polysaccharides as affected by ultrasound-assisted H2O2/Vc treatment

Natural polysaccharides have been recognized as major bioactive components in skincare and wound care products. In this study, the skincare benefits and self-healing properties of Lignosus rhinocerotis polysaccharides (LRP) and its degraded products (DLRP-1, DLRP-2 and DLRP-3) by ultrasound assisted H2O2/Vc treatment (U-H/V) at different ultrasonic intensity (28.14, 70.35, and 112.56 W/cm2) were investigated. U-H/V altered the internal crystalline structure and microstructure of LRP, and enhanced the thermal stability. Due to the breakage of molecular chains after U-H/V, the moisture absorption of LRP was enhanced but the moisturizing property showed a different degree of reduction. U-H/V significantly improved the antioxidant, anti-tyrosinase and anti-inflammatory activities of LRP. Furthermore, the results of enzyme kinetic studies showed a mixed competitive-noncompetitive inhibition of tyrosinase activity by DLRP-3 and the inhibition constant of DLRP-3 on tyrosinase was 2.97 mg/mL. The apparent viscosity of LRP dispersions showed a first increasing followed by decreasing trend as ultrasonic intensity rose. U-H/V enhanced the viscoelastic properties of LRP gels without destroying their self-healing properties. This findings reveal that U-H/V is beneficial for improving the skincare efficacy of LRP, providing a theoretical foundation for the applicability of LRP in wound dressings.

Nano ZnO modified amorphous carbon materials enabling long-cycle performance and high-capacity for lithium/sodium-ion batteries

Zinc-modified carbon materials exhibit high specific capacity, good safety, and low self-discharge, making them promising anode materials for lithium-ion and sodium-ion batteries. However, the high cost of raw materials, complex fabrication processes, and limited cycle life remain significant challenges to their further development. In this study, we elucidated a two-step process, simple in technique and suitable for large-scale production, for in-situ zinc modification of amorphous carbon. The synthesized carbon material exhibited superior reversible specific capacity (maintaining 780.27 mAh·g−1 capacity after 80 cycles at 50 mA·g−1 current density), high cycling stability (maintaining Coulombic efficiency at 100.06 % after 15,000 cycles at 10 A·g−1 current density), and good application value (achieving a capacity of 89.67 mAh·g−1 after 1000 cycles at 200 mA·g−1 current density for the assembled MFAC-Zn||NVP full cell). Through our investigation, we discovered that Nano ZnO not only directly participate in electrochemical reactions but also effectively improve the microstructure of amorphous carbon, increasing its three-dimensional axial stacking and providing more reaction sites. The enrichment of open pores significantly enhances the diffusion efficiency of ions within the carbon-based matrix. The superior diffusion ability of alkali metal-ion in the electrode is the reason for the excellent electrochemical performance of Zinc-modified amorphous carbon. Moreover, the incorporation of Nano ZnO aids in the formation of a robust and thin SEI layer. This significantly enhances the stability of the electrode materials during cycling and improves charge transfer efficiency during the charge-discharge process. Our study provides a new strategy for adjusting the internal microstructure of amorphous carbon materials to achieve high-performance lithium/sodium storage.

Comparative Analysis of Mechanical Characteristics: Ultrasonically Compacted vs. Conventionally Additive Manufactured Polymeric Samples

This scientific paper presents a comparative analysis of the mechanical characteristics of PLA samples fabricated through conventional AM methods and AM then ultrasonically compacted. The study aims to assess the potential advantages and limitations of ultrasonic compaction of PLA AM samples, as a reinforcing manufacturing technique. The methodology involves the fabrication of PLA samples using AM processes, then ultrasonically compact part of them to make a comparative study on their mechanical characteristics, including tensile strength. Additionally, the surface morphology and internal microstructure of the samples are analysed using microscopy techniques. The results of the study provide insights into the mechanical performance and structural integrity of the ultrasonically compacted samples compared to the conventionally PLA AM samples. The findings highlight any potential improvements or limitations in terms of mechanical properties, such as strength, durability, and overall performance.

Multiscale image-based modeling for failure prediction of sheet molding compound composite under uniaxial tension

Carbon fiber reinforced polymer (CFRP) composites are extensively utilized as primary load-bearing components in various engineering applications due to their superior strength-to-weight ratio and excellent mechanical properties. However, their intricate microstructural interactions within composite present a significant challenge for failure analysis of CFRP. Although finite element (FE) simulations have been proven feasible to conduct the failure analysis, the classical FE models are developed based on homogeneous fiber characteristics, ignoring the influence of internal structures on the damage evolution process. This paper presents a multiscale image-based modeling approach to predict the tensile failure procedure of chopped carbon fiber sheet molding compound (SMC) composite. To accurately reconstruct the representative volume element (RVE) model of the SMC composite, synchrotron micro-X-ray computed tomography (μXCT) was adapted to explore the SMC internal microstructure. Then microscale RVE models with different fiber volume fractions were constructed to predict the corresponding microcosmic mechanical properties, which were used as the inputs for mesoscale RVE models to determine the constitutive parameters of fiber chips having varied fiber volume and orientations. Finally, the YOLOv5_Seg algorithm was employed to extract the geometric feature parameters of the fiber chips for mesoscale RVE modeling and then the failure location and sequence under uniaxial tension were predicted. It is found that the final simulated failure behaviors were consistent with the experimental observations, confirming the feasibility of this approach for understanding the failure mechanisms of CFRP composites. Thus, once the internal microstructure is determined using experimental techniques or predicted by simulating the composite manufacturing process, this approach can also be utilized for design optimization and performance evaluation for CFRP composites.

In-situ experimental characterization and numerical investigation of the crack initiation of SMC composite under uniaxial tension

This paper explored the crack initiation of sheet molding compound (SMC) composite under uniaxial tensile loads by integrating in-situ experimental characterization and subsequent numerical analysis. Firstly, a synchrotron micro-X-ray computed tomography was utilized to character the morphology and evolution of the microstructure and fracture features of the SMC sample with different loading conditions. Meanwhile, the digital volume correlation technology was employed to determine the internal three-dimensional deformation. Then, a numerical analysis was conducted to describe the relationships among the microstructure, deformation distribution, and position of the crack initiation. Finally, a predictive model was developed based on the internal microstructure and the deformation distribution and then utilized to predict the location and sequence of crack initiation. The good agreement between the predicted results with the experimental ones reveals the feasibility of the proposed model in exploring the fracture behaviors of carbon fiber reinforced polymer composites with complex internal microstructure.

Effect of coarse aggregates on contact explosion resistance of concrete—A mesoscopic investigation

The intricate relationship between the mechanical properties of concrete and its internal microstructure underscores the importance of comprehending explosion performance and damage mechanisms at a mesoscopic level to effectively enhance blast resistance. This study employed three-dimensional (3D) mesoscale models to numerically investigate the dynamic behavior of concrete mixed with coarse aggregates under contact explosion. Rigorous validation of numerical models and simulation techniques was untaken through the contact explosion tests. The study explored mesoscopic damage mechanisms in heterogeneous concrete targets with randomly distributed coarse aggregates, drawing comparisons with a homogeneous concrete target. Critical mesoscopic parameters influencing the contact explosion resistance of concrete were thoroughly examined. Structural effects of coarse aggregates emerge as pivotal, shifting the damage mode from overall failure with spalling-dominated damage in homogeneous concrete to localized failure in mesoscopic concrete. The mesoscopic concrete experienced a distinct four-stage damage evolution—cratering, crack initiation, perforation, and dynamic fragmentation—diverging from homogeneous concrete with multi-layer spalling originating from the boundaries. The exponential attenuation of shock waves observed in homogeneous concrete was locally disrupted by coarse aggregates in mesoscopic concrete, attributed to wave impedance mismatch and aggregate extrusion effects. Mortar strength primarily contributed to concrete cracking, with minimal impact on damage modes. Failure modes were predominantly influenced by the content and particle size of coarse aggregates. Higher volumetric fractions significantly reduced concrete spalling, while increased coarse aggregate size exacerbated perforation failure. This comprehensive study advances our understanding of blast-resistant concrete design at a mesoscopic level, providing valuable insights for strategies aimed at enhancing structural resilience.

Bloating zone of artificial lightweight aggregates in triaxial whiteware compositions using ME-DOE

This study examines the characteristics of manufactured aggregates by designing an experiment using Mixture Experiments Design of Experiments (ME-DOE) for triaxial whiteware compositions and proposes the optimal mixture for manufacturing artificial lightweight aggregates. The optimal mixture designed using ME-DOE was manufactured in a pilot-scale rotary kiln. The density and water absorption rate of the manufactured aggregates were measured, and the cross-section was observed. Additionally, Mercury Intrusion Porosimetry (MIP) and 3D-CT observation were conducted to observe the pores. The samples designed using the ME-DOE were classified into five types based on the internal microstructure, which had a high correlation with the physical properties of the aggregates. The matrix composition, excluding Fe2O3 and carbon in the area where the black core was created and bloated, was formed in the area of a typical triaxial whiteware mixture. Lightweight aggregates were manufactured at the Pilot Rotary Kiln using a 50:50 mixture of feldspar and ball clay, and the manufactured lightweight aggregates met ASTM C330 standards.

Enhancing high-temperature wear resistance of cladded Inconel 718 through hybrid of directed energy deposition with ultrasonic nano-crystal surface modification

We present an innovative method for achieving highly durable and finely controllable internal microstructures within cladded 718 layers utilizing a hybrid cladding approach. This process alternates between two methods: laser directed energy deposition in which four layers of Inconel 718 built up using a laser power of 350 W and a scanning speed of 800 mm/min, and ultrasonic nanocrystal surface modification (UNSM), applied to every fourth deposited surface at elevated temperatures of 300 and 600 °C, with a frequency of 20 kHz and an interval of 0.05 mm, respectively. Electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) are used to analyze the effect of grain refinement and concentrated dislocation distribution induced by the hybrid cladding. Through the employment of high temperature UNSM treatment between the cladded Inconel 718 layers, profound grain refinement and dislocation enhancement occur, significantly bolstering the wear resistance of the intermediate layer under high temperature conditions. We conducted thorough analyses, employing finite element analysis and experiments, to investigate the diverse temperature conditions of UNSM treatment and their impact on increasing the affected depth of UNSM treatment. Furthermore, we closely examined the changes in microstructure and mechanical properties within the remelted and UNSM-treated zone of the internal layers. Our study confirms that the high temperature hybrid cladding process, operating below 600 °C, resulted in a 27 % reduction in overall material wear-loss compared to conventional cladding methods. Notably, even in high temperature wear tests ranging from 200 to 800 °C, the proposed method significantly mitigated wear amounts in each case, indicating its potential to enhance the mechanical integrity of various components operating under elevated temperature conditions.

Bamboo fiber-enhanced UHPC: Early hydration and microstructural/mesoscale analysis

This study investigates the impact of incorporating bamboo fibers, a natural and renewable material, into ultra-high performance concrete (UHPC) on its early hydration, mechanical properties, internal relative humidity, autogenous shrinkage, and microstructure. The results show that adding bamboo fibers significantly improves various UHPC properties. Bamboo fibers regulate hydration and prolong the hydration process through their water absorption and retention abilities. With a fiber content of 1.0 vol percent (vol%), the compressive strength increases by 10.2 %, reaching 97.1 MPa, and at 2.0 vol%, flexural strength and toughness increase by 37.9 % and 739.5 %, respectively. Additionally, bamboo fibers help maintain internal relative humidity above 98 % during the first 7 days of curing and reduce autogenous shrinkage by up to 55.9 %. The fibers also optimize the microstructure by minimizing voids, with a 1.0 % fiber content reducing the void ratio to 1.64 %. This reduces large voids and improves the material's density. Overall, bamboo fibers show great promise in enhancing UHPC's structural performance and environmental adaptability while being a sustainable and cost-effective material.

Heat treatment effects on the shear performance and microstructure evolution of W-core SiC fibers

SiC fiber reinforced titanium alloy matrix composites employed in elevated temperature aeroengine components are subjected to complex loading conditions. Investigating the shear performance of SiC fibers after heat treatment can help ensure the load-carrying capability of composites at service temperatures. This study presents a novel double shear testing method for W-core SiC fibers. The shear strength and stiffness of the SiC fibers in as-received and heat-treated conditions were measured. The morphologies of SiC fibers’ shear fracture surfaces and C coatings were thoroughly analyzed. The evolution of the internal microstructure and the composition of reaction layers after heat treatments were investigated. The shear strength of W-core SiC fibers at 95% survival probability reached 588.64MPa after 200 h of heat treatment at 600°Celsius, representing a 55% improvement over both the as-received and 1100°Celsius heat-treated conditions. After heat treatment at 1100°Celsius, the reaction layer between the W core and the SiC sheath thickened exponentially due to extensive elemental diffusion, resulting in the formation of numerous Kirkendall voids. The voids facilitated crack initiation and propagation, leading to a deterioration in fiber shear performance. The insights gained in this study regarding the shear properties of SiC fibers can provide support for predicting the mechanical performance of composites under complex loading conditions.

Influence of water scouring on chloride ion diffusion in rice husk ash recycled aggregates concrete

This study investigates the chloride ion diffusion behavior in concrete incorporating rice husk ash (RHA) and recycled aggregates (RA) under water scouring conditions. The research results indicate that both free and total chloride ion concentrations in recycled aggregate concrete (RAC) exhibit an initial increase, followed by a subsequent decrease, as the distance from the concrete surface increases. The incorporation of RHA reduces both free and total chloride ion concentrations while increasing bound chloride ion content. However, an excessive amount of RHA can weaken the resistance of RAC to chloride ion penetration. Water erosion deteriorates the internal microstructure of RAC, accelerating the transport of free and total chloride ions. However, it does not compromise the chloride ion binding mechanism conferred by RHA. The fine particulate of RHA provides additional nucleation sites for cement hydration, while the reservoir effect ensures a steady supply of free water to these sites. This synergistic interaction enhances the pozzolanic reaction between cement hydration products and RHA, resulting in reduced Ca(OH)₂ content and increased formation of C-S-H gel.

Internal damage evolution of C/SiC composites in air at 1650 °C studied by in-situ synchrotron X-ray imaging

Carbon fibre reinforced silicon carbide (C/SiC) ceramic matrix composites have attracted considerable attention due to their exceptional properties and extensive potential applications as high-temperature structural materials. However, due to their complex structure and manufacturing defects, C/SiC composites exhibit intricate mechanical behaviour under thermal-mechanical-oxidative coupling environments. To date, systematic studies on the internal damage evolution and failure mechanisms of C/SiC composites under high-temperature oxidative environments are lacking. In this study, a combination of synchrotron X-ray micro-computed tomography (SR-μCT) and in-situ experiments under thermal-mechanical-oxidative coupling environments at room temperature and 1650 °C in air was used to characterize the internal microstructures and damage evolution processes of C/SiC composites at different loading levels. Additionally, the 3D strain fields during in-situ loading were quantitatively analysed using the Digital Volume Correlation (DVC) method. The findings underscore the substantial impact of oxidative damage on the mechanical response of C/SiC composites, particularly concerning tensile properties and fracture modes. At room temperature, severe delamination, fibre bundle pull-out and interfacial debonding occurred internally. Whereas, under high-temperature atmospheric conditions, severe fibre oxidation reactions occurred at the specimen edges, resulting in rapid porosity escalation. Crack initiation from surface defects followed by rapid inward propagation is observed. Moreover, while the strain distribution remains relatively uniform until fracture, a pronounced concentration of strain is evident near the fracture zones at room temperature, with an even greater concentration observed at 1650 °C. Notably, the region of concentrated strain within the 3D deformation field corresponds closely to the final fracture location, as revealed by quantitative DVC analysis.

Effect of ZrSiO4 as additive on the mechanical properties of DLP printing porous mullite ceramics

In order to satisfy the demand for mullite porous ceramics with complex geometries in the engineering field, the digital light processing (DLP) technology is employed to prepare mullite porous ceramics in this study. However, the poor mechanical properties of the mullite porous ceramics prepared using the DLP technology limits its further application in engineering field. In this work, the microstructure of mullite crystals was regulated by adding the sintering aid ZrSiO4 to enhance the mechanical properties of the mullite ceramics, and the effects of sintering aid ZrSiO4 content and sintering temperature on the internal microstructure evolutions of mullite porous ceramics were investigated. Results showed that the decomposition of ZrSiO4 promoted the generation of the silica-rich liquid phase at high temperatures, which effectively promoted the nucleation and growth of needle-like mullite crystals. When the sintering temperature was 1600 °C and the ZrSiO4 content was 10 wt%, the well-developed elongated crystals formed an interlocking nonwoven structure. The corresponding mullite porous ceramics exhibited a compressive strength of 2.52 MPa and a porosity of 74.51%. The strategy of this study can be a feasible route for preparing lightweight and high-strength mullite porous ceramics via digital light processing.

Coupled cellular automata-crystal plasticity modeling of microstructure-sensitive damage and fracture behaviors in deformation of α-titanium sheets affected by grain size

Concerning the micro-scale deformation of titanium metal sheets, the number of grains in the sheet thickness direction decreases, and their formability exhibits a strong grain size sensitivity. Meanwhile, the twinning-induced dynamic recrystallization (TDRX) associated with grain size significantly affects the fracture behavior in the microforming of titanium sheets. Therefore, an accurate prediction of formability to improve manufacturing reliability remains challenging in the microforming of miniaturized titanium components. To address this issue, an in-depth understanding of the grain size-dependent TDRX behavior and its role in damage and fracture development in the microforming of α-titanium sheets is critical, and a coupled cellular automata-crystal plasticity (CA-CP) modeling framework was thus developed as an approach providing efficient solutions and insightful comprehensions of the issue. For the proposed modeling framework, a kinematic model for TDRX was established and integrated into the CP model by the CA algorithm. As a result, the microstructure evolution caused by TDRX was regarded as an intrinsic part of the constitutive behavior to connect heterogeneous plastic deformation and damage evolution through data transmission between the CP model and the CA algorithm. Additionally, the coupled CA-CP modeling framework was validated with the internal defect morphologies and deformation microstructures characterized by X-ray computed tomography (X-CT) and electron backscattered diffraction (EBSD). Experiment and simulation results demonstrated that the fine recrystallized (DRXed) grains were generated after the twin fragmentation when the dislocation density at twin boundaries reached a threshold of 9.2 × 1013 /m2. After TDRX, the dislocation density and the stress concentration intensity in recrystallization regions were revealed to decrease, accounting for the ductility improvement. Nevertheless, the dislocation density at twin boundaries was determined to decrease with the increase of grain size, leading to less twin fragmentation and the absence of TDRX. The uncoordinated deformation between fine DRXed grains motivated defects to grow spherically into microvoids, thereby preventing premature intergranular cracks along twins/grain boundaries. Ultimately, the deformation microstructures resulting from TDRX with the decrease of grain size were confirmed to control the brittle to ductile fracture transition of α-titanium sheets. The presented modeling framework and simulation procedure were validated to be able to predict the material integrity affected by crystalline microstructure in the deformation of titanium metal sheets.

Study on the influence of early frost attack on the performance of cement mortar

The loss of strength and durability caused by early frost attack is the macro performance of internal microstructure deterioration. Understanding the influence mechanism of early frost attack at the micro level is necessary to avoid or minimize the early frost attack to macro performance. In this study, the influence of early frost attack on the strength, water sorptivity, chloride permeability, and microstructure of cement mortar was investigated. The fresh mortars were pre-cured for 10, 12, 14, and 16 h and then frozen at −10 °C for 7 days to simulate an early frost attack. After freezing, the standard curing (20 °C) was carried out until the testing. It is found that after standard curing of 28 days, the strength of early-frozen mortar can reach more than 95 % of the 28-day strength of unfrozen mortar. Interestingly, the sorptivity coefficient and total charge passed of early-frozen mortar are much higher than the level of unfrozen mortar, and the loss of resistance to water penetration and chloride ion penetration exceeds 20 %, indicating that early frost attack causes more severe damage to the durability than to the strength of mortar. Mercury intrusion porosimetry (MIP) results show that early frost attack can increase the pore volume of >50 nm and coarsen the pores within 10–50 nm. Correspondingly, key pore parameters (critical pore diameter, threshold pore diameter, and tortuosity) that affect the durability of mortar are also negatively affected. Energy dispersive spectroscopy (EDS) analysis also shows that after suffering early frost attack, the interfacial transition zone (ITZ) thickness of mortar is increased from 4 to 10 μm to 8–13 μm, and the probability of high Ca/Si ratios (4–10) in the ITZ is also increased. Finally, it is concluded that the coupling effect of pore structure coarsening and ITZ degradation leads to more severe durability loss.

Experimental analysis of a beam with a 2D triangular substructure

AbstractThe aim of this study is to determine experimentally the higher material parameter of a metamaterial with a triangular substructure and to verify a higher‐gradient elasticity model for beams with internal substructures or microstructures. The investigations of the higher‐gradient elasticity models of Bernoulli‐Euler and Timoshenko beams with a periodic triangular substructure in Khakalo et al. show that the bending stiffness strongly depends on the geometrical parameters of the lattice structure. To achieve this goal, beams with triangular substructures were additively manufactured using fused deposition modeling and stereolithography. They were experimentally investigated in tensile and bending tests. Three different types of beams with triangular substructures were produced, consisting of one, two and four layers of triangular beams, using two different materials: Polylactide and epoxy resin. The higher material parameter g was quantitatively determined based on the experimental results using inverse analysis. The results are valid for these specific variations of the substructure and can adequately represent the elastic size effects. In addition, this study investigates the relationship between the bending stiffness and the geometric parameters of the lattice structure as well as the influence of the curing time on the elastic properties of epoxy resin. The experiments involved testing the triangular beams under tensile and bending loads. The numerical and experimental results were compared using digital image correlation. Based on the experimental data, a higher gradient material parameter representing the geometric structure of the lattice was determined.