Study on Nitrile Oxide for Low-Temperature Curing of Liquid Polybutadiene

As a significant component of composite solid propellants, the cross-link alkenyl polymers need to cure at high temperatures and the current isocyanate curing systems are highly humidity sensitive. This paper presented a low-temperature curing method for a cross-linked polymer (polybutadiene) with stable wettability by using cycloaddition of the nitrile oxide of tetramethyl-terephthalobisnitrile oxide (TTNO) and the C=C group of liquid polybutadiene (PB). The TTNO was synthesized in four steps from 1,2,4,5-tetramethylbenzene and evaluated as a low-temperature hardener for curing liquid PB. To characterize the reaction ability of TTNO at 25 °C, the cross-linked rubber materials of various contents (8%, 10%, 12%, 14%, 16%) of curing agent TTNO were prepared. The feasibility of the curing method can be proved by the disappearance of the absorption peak of the nitrile oxide group (2300 cm⁻¹) by FT-IR analysis. Contact angle, TG-DTA and tensile-test experiments were conducted to characterize the wettability, thermo-stability and mechanical properties of the obtained cross-linked rubber materials, respectively. The results showed that the curing agent TTNO could cure PB at room temperature. With the growing content of the curing agent TTNO, the tensile strength of the obtained cross-linked rubber material increased by 260% and the contact angle increased from 75.29° to 89.44°. Moreover, the thermo-stability performances of the cross-linked rubber materials have proved to be very stable, even at a temperature of 300 °C, by TGA analysis.     

Influence of Curing on the Strength Development of Calcium-Containing Geopolymer Mortar

This paper investigated the curing effects on the mechanical properties of calcium-containing geopolymer mortar. Three precursors are used: Class C fly ash, Class F fly ash plus calcium hydroxide and Class F fly ash plus slag. Curing conditions included: (1) standard curing at 20 ± 3 °C and RH 95% (C); (2) steam curing at 60 °C for 24 h (S); (3) steam curing at 60 °C for 6 h (S6); and (4) oven curing at 60 °C for 24 h (O), then the latter three followed by the standard curing. Under the standard conditions, the flexural strength and compressive strength of Class C fly ash geopolymer mortars developed quickly until the age of 7 days, followed by a gradual increase. Specimens with Class F fly ash plus Ca(OH)₂ showed slow increase till the age of 28 days. Under these non-standard conditions (2–4), all specimens showed higher 3-day strength, while later strengths were either higher or lower than those in standard conditions, depending on the type of the precursor.     

Accelerated Curing for Glass-Based Mortars Using Water at 80 °C

The substitution of river sand with glass aggregate (GA) and cement with glass powder (GP) is a mainstream method to recycle waste glass. Traditionally, standard curing was widely used for glass-based mortars. However, it is time-consuming and cannot address low mechanical strengths of the early-age mortars. Therefore, the effect of water curing at 80 °C on the properties of GA mortars is investigated. Furthermore, the effect of the GP size is also considered. Results show that compared with the expansion of alkali-silica reaction (ASR), water curing at 80 °C has a negligible effect on the volume change. Moreover, the compressive strength of GA mortars under 1-day water curing at 80 °C is comparable with that under 28-day water curing at 20 °C. Therefore, the 1-day water curing at 80 °C is proposed as an accelerated curing method for GA mortars. On the other hand, the addition of GP with the mean size of 28.3 and 47.9 μm can effectively mitigate the ASR expansion of GA mortars. Compared with the size of 28.3 μm, GA mortars containing GP (47.9 μm) always obtain higher compressive strength. In particular, when applying the 1-day water curing at 80 °C, GA mortars containing GP (47.9 μm) can even gain higher strength than those containing fly ash.     

Mechanical and Microstructural Characteristics of Calcium Sulfoaluminate Cement Exposed to Early-Age Carbonation Curing

The early-age carbonation curing technique is an effective way to improve the performance of cement-based materials and reduce their carbon footprint. This work investigates the early mechanical properties and microstructure of calcium sulfoaluminate (CSA) cement specimens under early-age carbonation curing, considering five factors: briquetting pressure, water–binder (w/b) ratio, starting point of carbonation curing, carbonation curing time, and carbonation curing pressure. The carbonization process and performance enhancement mechanism of CSA cement are analyzed by mercury intrusion porosimetry (MIP), thermogravimetry and derivative thermogravimetry (TG-DTG) analysis, X-ray diffraction (XRD), and scanning electron microscope (SEM). The results show that early-age carbonation curing can accelerate the hardening speed of CSA cement paste, reduce the cumulative porosity of the cement paste, refine the pore diameter distribution, and make the pore diameter distribution more uniform, thus greatly improving the early compressive strength of the paste. The most favorable w/b ratio for the carbonization reaction of CSA cement paste is between 0.15 and 0.2; the most suitable carbonation curing starting time point is 4 h after initial hydration; the carbonation curing pressure should be between 3 and 4 bar; and the most appropriate time for carbonation curing is between 6 and 12 h.     

The Curing Kinetics of E-Glass Fiber/Epoxy Resin Prepreg and the Bending Properties of Its Products

The curing kinetics can influence the final macroscopic properties, particularly the three-point bending of the fiber-reinforced composite materials. In this research, the curing kinetics of commercially available glass fiber/epoxy resin prepregs were studied by non-isothermal differential scanning calorimetry (DSC). The curing kinetic parameters were obtained by fitting and the apparent activation energy E_a of the prepreg, the pre-exponent factor, and the reaction order value obtained. A phenomenological nth-order curing reaction kinetic model was established according to Kissinger equation and Crane equation. Furthermore, the optimal curing temperature of the prepregs was obtained by the T-β extrapolation method. A vacuum hot pressing technique was applied to prepare composite laminates. The pre-curing, curing, and post-curing temperatures were 116, 130, and 153 °C respectively. In addition, three-point bending was used to test the specimens’ fracture behavior, and the surface morphology was analyzed. The results show that the differences in the mechanical properties of the samples are relatively small, indicating that the process settings are reasonable.     

Comparative Analysis of Strength and Deformation Behavior of Cemented Tailings Backfill under Curing Temperature Effect

Mineral resources are increasingly being developed in cold and permafrost regions. However, the mechanical and physical properties of cemented tailings backfill (CTB) cured at normal temperature are no longer applicable. To clarify the reasons for this variability, a series of tests were performed. The mechanical properties of CTB with different cement–tailings ratios (CTR, 1:4, 1:8, 1:12, 1:16, and 1:20) were tested at different curing ages (3, 7 and 28 days) and curing temperatures (20 °C, 5 °C, −5 °C, and −20 °C). The differences of CTB in mechanical and physical properties under positive- and negative-temperature curing conditions were analyzed, and the microscopic failure process of CTB under negative-temperature curing conditions was discussed. The results revealed that the mechanical properties and deformation behavior of CTB under positive- and negative-temperature curing conditions were different. The frozen CTB had higher early strength than the standard-temperature curing condition (20 °C), and the lower the temperature, the higher the early strength. The low-temperature curing condition, on the other hand, was not beneficial to CTB’s long-term strength. The low-temperature curing condition was not conducive to the long-term strength of CTB. After yielding, strain hardening and strain softening appeared in the deformation behavior of frozen backfill, indicating ductility. In contrast to the typical-temperature curing condition, the frozen CTB showed a new failure pattern that has little relation to curing time or CTR. Furthermore, the failure process of frozen backfill was reviewed and studied, which was separated into four stages, and altered as the curing time increased. The results of this study can act as a guide for filling mines in permafrost and cold climates.     

Effect of Sulphur-Containing Tailings Content and Curing Temperature on the Properties of M32.5 Cement Mortar

The effect of the dosage of sulphur-containing tailings (STs) and curing temperature on the properties of M32.5 cement mortar was studied in this work. An experimental study was conducted to evaluate the effects of STs with different substitution ratios (0, 10%, 20%, 30%, 40%) on the compressive strength experiment, fluidity, expansion ratio, and pore structure of M32.5 cement mortar. The results showed that the addition of STs reduced the fluidity of mortar, and the fluidity decreased with the increase of the STs dosage. The compressive strength of mortars increased at a lower substitution rate (0~20%) but decreased at a higher substitution rate (>20%). Ettringite peaks and new sulfate peaks were found by X-ray diffraction (XRD) analysis. Scanning electron microscope (SEM) observation of the microstructure showed that a large number of hydrated products, such as ettringite, formed and filled in the interstitial space, which was conducive to the development of strength. The optimal STs replacement ratio of river sand was 10%. Then, the performance of mortar at curing temperatures of 23 ± 1, 40, 60, and 80 °C was further investigated under the optimal STs replacement ratio. Under high-temperature curing conditions, the early strength of M32.5 cement mortar with STs increased greatly, but the late strength decreased gradually with the increase in curing temperature. The early strength development of the mortar mainly depended on the high speed of hydration reaction, and the late strength variation was mainly affected by hydration products and the pore size distribution. After comprehensive consideration, the optimal curing temperature of M32.5 cement mortar with STs was 40 °C.     

The Effects of Temperature Curing on the Strength Development,Transport Properties,and Freeze-Thaw Resistance of Blast Furnace Slag Cement Mortars Modified with Nanosilica

This investigation studies the effects of hot water and hot air curing on the strength development, transport properties, and freeze-thaw resistance of mortars incorporating low-heat blast furnace slag cement and nanosilica (NS). Mortar samples were prepared and stored in ambient conditions for 24 h. After demolding, mortar samples were subjected to two different hot curing methods: Hot water and hot air curing (40 °C and 60 °C) for 24 h. For comparison purposes, mortar reference mixes were prepared and cured in water and air at ambient conditions. Strength development (from 1 to 180 days), capillary water porosity, water sorptivity, and freeze-thaw resistance were tested after 180 days of curing. The experimental results showed that both curing regimes accelerate the strength development of mortars, especially in the first seven days of hydration. The highest early strengths were reported for mortars subjected to a temperature of 60 °C, followed by those cured at 40 °C. The hot water curing regime was found to be more suitable, as a result of more stable strength development. Similar findings were observed in regard to durability-related properties. It is worth noting that thermal curing can more efficiently increase strength in the presence of nanosilica, suggesting that NS is more effective in enhancing strength under thermal curing.     

Effect of Early Curing Temperature on the Tunnel Fire Resistance of Self-Compacting Concrete Coated with Aerogel Cement Paste

In this paper, the effect of early curing temperature on the tunnel fire resistance of self-compacting concrete (SCC) coated with aerogel cement paste (ACP) was studied. The physical properties in terms of the compressive strength, flexural strength, and thermal conductivity of ACP were tested under different early curing temperatures. The tunnel fire resistance of ACP and SCC coated with ACP was determined, and the microstructure of ACP and SCC after a tunnel fire were characterized by scanning electron microscopy. The results show that the strength of ACP initially increased (by 10–40 °C) and then later decreased (by 40–60 °C) with the increase in early curing temperature. ACP under 40 °C early curing exhibited the minimum number of cracks and mass loss after the tunnel fire. Too high or too low early curing temperature reduced the thermal conductivity of ACP but accelerated the formation and expansion of microcracks during the tunnel fire. The residual compressive strength of SCC coated with ACP under 40 °C early curing after the tunnel fire was the highest, demonstrating the best tunnel fire resistance.     

Preparation of Low-Cost Magnesium Oxychloride Cement Using Magnesium Residue Byproducts from the Production of Lithium Carbonate from Salt Lakes

Magnesium oxychloride cement (abbreviated as MOC) was prepared using magnesium residue obtained from Li₂CO₃ extraction from salt lakes as raw material instead of light magnesium oxide. The properties of magnesium residue calcined at different temperatures were researched by XRD, SEM, LSPA, and SNAA. The preparation of MOC specimens with magnesium residue at different calcination temperatures (from 500 °C to 800 °C) and magnesium chloride solutions with different Baume degrees (24 Baume and 28 Baume) were studied. Compression strength tests were conducted at different curing ages from 3 d to 28 d. The hydration products, microstructure, and porosity of the specimens were analyzed by XRD, SEM, and MIP, respectively. The experimental results showed that magnesium residue’s properties, the BET surface gradually decreased and the crystal size increased with increasing calcination temperature, resulting in a longer setting time of MOC cement. Additionally, the experiment also indicated that magnesium chloride solution with a high Baume makes the MOC cement have higher strength. The MOC specimens prepared by magnesium residue at 800 °C and magnesium chloride solution Baume 28 exhibited a compressive of 123.3 MPa at 28 d, which met the mechanical property requirement of MOC materials. At the same time, magnesium oxychloride cement can be an effective alternative to Portland cement-based materials. In addition, it can reduce environmental pollution and improve the environmental impact of the construction industry, which is of great significance for sustainable development.     

Thermophysical and Mechanical Properties of Hardened Cement Paste with Microencapsulated Phase Change Materials for Energy Storage

In this research, structural-functional integrated cement-based materials were prepared by employing cement paste and a microencapsulated phase change material (MPCM) manufactured using urea-formaldehyde resin as the shell and paraffin as the core material. The encapsulation ratio of the MPCM could reach up to 91.21 wt%. Thermal energy storage cement pastes (TESCPs) incorporated with different MPCM contents (5%, 10%, 15%, 20% and 25% by weight of cement) were developed, and their thermal and mechanical properties were studied. The results showed that the total energy storage capacity of the hardened cement specimens with MPCM increased by up to 3.9-times compared with that of the control cement paste. The thermal conductivity at different temperature levels (35–36 °C, 55–56 °C and 72–74 °C) decreased with the increase of MPCM content, and the decrease was the highest when the temperature level was 55–56 °C. Moreover, the compressive strength, flexural strength and density of hardened cement paste decreased with the increase in MPCM content linearly. Among the evaluated properties, the compressive strength of TESCPs had a larger and faster degradation with the increase of MPCM content.     

Multiphase Model for Predicting the Thermal Conductivity of Cement Paste and Its Applications

Thermal conductivity plays a significant role in controlling thermal cracking of cement-based materials. In this study, the thermal conductivity of cement paste at an early age was measured by the hot plate method. The test results showed that the thermal conductivity of cement paste decreased with the increase of water/cement ratio and curing age. Meanwhile, a multiphase model for the thermal conductivity of cement paste was proposed and used to study the influence of saturation and curing temperature on the thermal conductivity of cement paste. To determine the parameters involved in this model, the thermal conductivity of each phase in cement paste was calculated by the molecular dynamic simulation method, and the hydration of cement was simulated by the Virtual Cement and Concrete Testing Laboratory. The inversion results showed that the relative error between experimental and simulation results lay between 1.1% and 6.5%. The thermal conductivity of paste in the saturated condition was 14.9–32.3% higher than that in the dry state. With the curing temperature increasing from 10 °C to 60 °C, the thermal conductivity of cement paste decreased by 3.9–4.9% depending on the water/cement ratio.     

Properties of Blended Cement Containing Iron Tailing Powder at Different Curing Temperatures

The properties of blended cement containing 0%, 20%, and 50% iron tailing powder (ITP) at 20 °C and 60 °C were investigated by determining the hydration heat, microstructure, and compressive strength. The addition of ITP decreases the exothermic rate and cumulative hydration heat of blended cement at 20 °C. The high temperature increases the hydration rate and leads to the hydration heat of blended cement containing 20% ITP higher than that of Portland cement. Increasing the amount of ITP decreases the non-evaporable water content and Ca(OH)₂ content as well as compressive strength at both of the two studied temperatures. The addition of ITP coarsens the early-age pore structure but improves the later-age pore structure at 20 °C. The high temperature significantly improves the early-age properties of blended cement containing ITP, but it is detrimental to the later-age properties development. The reaction of ITP is limited even at high temperature. The large ITP particles bond poorly with surrounding hydration products under early high-temperature curing condition. The properties of blended cement containing a large amount of ITP are much poorer at high temperature.     

Mechanical Properties and Microstructure of Calcium Sulfate Whisker-Reinforced Cement-Based Composites

This study aims to investigate the effect of calcium sulfate whisker (CSW) on the properties and microstructure of cement-based composites. Further, nanosilica (NS) was used as a comparison. The results show that the compressive strength and fracture toughness of cement-based composites increased by 10.3% and 10.2%, respectively, with 2% CSW. The flexural strength, splitting tensile strength, and fracture energy increased by 79.7, 34.8 and 28.7%, respectively, with 1% CSW. With the addition of CSW, shrinkage deformation was aggravated, and the capillary water absorption coefficients were clearly reduced. Compared with NS, CSW-reinforced cement-based composites show better tensile, flexural, and fracture properties and smaller shrinkage deformations and capillary water absorption coefficients. The residual mechanical properties of all groups improve when the treating temperature is lower than 400 °C and decline rapidly when the temperature goes over 600 °C. When treated at 900 °C, the residual mechanical properties are 40% less than those at ambient temperature, with the NS group showing the best performance, followed by the control group and the CSW group. X-ray diffraction (XRD) and scanning electron microscopy (SEM) tests show that the addition of CSW improves the microstructure of the matrix. CSW can reinforce and toughen composites by generating ettringite and whisker pullout, whisker breakage, crack bridging, and crack deflection at the microstructure level.     

Effect of Curing Temperature on High-Strength Metakaolin-Based Geopolymer Composite (HMGC) with Quartz Powder and Steel Fibers

Geopolymer is a new type of synthesized aluminosilicate material. Compared with ordinary Portland cement, it has better fire resistance and durability, and is more environmentally friendly. In this paper, a high-strength metakaolin-based geopolymer composite (HMGC) has been developed by utilizing quartz powder and steel fibers. The optimization compositions and effect of curing temperatures (from ambient temperature to 90 °C) on the strength performance of the HMGC is studied. The optimized 1-day compressive strength of the HMGC can reach 80 MPa, and the 3-day compressive strength is close to 100 MPa (97.49 MPa). Combined with XRD, FTIR, SEM and MIP characterization, the mechanisms behind the strength development under different curing temperatures are analyzed. The results show that heat curing can significantly speed up the process of geopolymerization and increase the early strength of the HMGC. However, long-term heat curing under high temperature (such as 90 °C, 7 days) would reduce the mechanical strength of the HMGC. Prolonged high-temperature curing increases the pores and micro-defects in the gel phase of the HMGC, which may be attributed to chemical shrinkage. Thus, the curing temperature should be carefully controlled to make a HMGC with better performance.     

Synthesis of High Crystallinity 1.13 nm Tobermorite and Xonotlite from Natural Rocks,Their Properties and Application for Heat-Resistant Products

The main measure to reduce energy losses is the usage of insulating materials. When the temperature exceeds 500 °C, silicate and ceramic products are most commonly used. In this work, high-crystallinity 1.13 nm tobermorite and xonotlite were hydrothermally synthesized from lime and Ca–Si sedimentary rock, opoka. By XRD, DSC, TG and dilatometry methods, it has been shown that 1.13 nm tobermorite becomes the predominant compound in stirred suspensions at 200 °C after 4 h of synthesis in the mixture with a molar ratio CaO/SiO₂ = 0.83. It is suitable for the production of insulating products with good physical–mechanical properties (average density < 200 kg·m⁻¹, compressive strength ~0.9 MPa) but has a limited operating temperature (up to 700 °C). Sufficiently pure xonotlite should be used to obtain materials with a higher operating temperature. Even small amounts of semi-amorphous C–S–H(I) significantly increase its linear shrinkage during firing. It has also been observed that an increase in the strength values of the samples correlated well with the increase in the size of xonotlite crystallites. The optimal technological parameters are as follows: molar ratio of mixture CaO/SiO₂ = 1.2; water/solid ratio W/S = 20.0; duration of hydrothermal synthesis at 220 °C—8 h, duration of autoclaving at 220 °C—4 h. The average density of the samples was ~180 kg·m⁻¹, the operating temperature was at least 1000 °C, and the compressive strengths exceeded 1.5 MPa.     

Shrinkage Mitigation of an Ultra-High Performance Concrete Submitted to Various Mixing and Curing Conditions

Ultra-High Performance Concretes (UHPC) are cement-based materials with a very low water-to-binder ratio that present a very-high compressive strength, high tensile strength and ductility as well as excellent durability, making them very interesting for various civil engineering applications. However, one drawback of UHPC is their pretty high autogenous shrinkage stemming from their very low water-to-binder ratio. There are several options to reduce UHPC shrinkage, such as the use of fibers (steel fibers, polypropylene fibers, wollastonite microfibers), shrinkage-reducing admixtures (SRA), expansive admixtures (EA), saturated lightweight aggregates (SLWA) and superabsorbent polymers (SAP). Other factors related to curing conditions, such as humidity and temperature, also affect the shrinkage of UHPC. The aim of this paper is to investigate the impact of various SRA, different mixing and curing conditions (low to moderate mixing temperatures, moderate to high relative humidity and water immersion) as well as different curing starting times and durations on the shrinkage of UHPC. The major importance of the initial mixing and curing conditions has been clearly demonstrated. It was shown that the shrinkage of the UHPC was reduced by more than 20% at early-age and long-term when the fresh UHPC temperature was closer to 20 °C. In addition, curing by water immersion led to drastic reductions in shrinkage of up to 65% and 30% at early-age and long-term, respectively, in comparison to a 20% reduction for fog curing at early-age. Finally, utilization of a liquid polyol-based SRA allowed for reductions of 69% and 63% of early-age and long-term shrinkages, respectively, while a powder polyol-based SRA provided a decrease of 47% and 35%, respectively.     

Effect of Elevated Temperature on Rhyolitic Rocks’ Properties

The effect of high temperatures on rock’s thermophysical and mechanical properties is critical to the design of underground geotechnical applications. The current work investigates the impact of temperature on rhyolitic turf rock’s physical and mechanical properties. Intact cylindrical core rock samples were heated to different temperatures (200, 400, 600, and 800 °C). The uniaxial compressive strength (UCS) and elastic modulus of unheated and heated samples were determined as important mechanical properties. In addition, the effect of temperature on the physical properties of rhyolite rock (density, color, and absorption) was investigated in conjunction with its microstructural properties. The hardening of the rhyolitic rock samples was observed below 600 °C, at which point the UCS and elastic modulus decreased to 78.0% and 75.9%, respectively, at 800 °C. The results also show that heating does not significantly affect the density and volume of permeable pore space, but a color change can be observed at 400 °C and above. A microscopic analysis shows the change in microstructural properties of rhyolite rock after heating to 600 °C. Furthermore, the SEM observations of heated materials show structural particle displacements and microcracking, leading to apparent surface cracks.     

Supercritical CO2 Curing of Resource-Recycling Secondary Cement Products Containing Concrete Sludge Waste as Main Materials

This study aims to develop highly durable, mineral carbonation-based, resource-recycling, secondary cement products based on supercritical carbon dioxide (CO₂) curing as part of carbon capture utilization technology that permanently fixes captured CO₂. To investigate the basic characteristics of secondary cement products containing concrete sludge waste (CSW) as the main materials after supercritical CO₂ curing, the compressive strengths of the paste and mortar (fabricated by using CSW as the main binder), ordinary Portland cement, blast furnace slag powder, and fly ash as admixtures were evaluated to derive the optimal mixture for secondary products. The carbonation curing method that can promote the surface densification (intensive CaCO₃ formation) of the hardened body within a short period of time using supercritical CO₂ curing was defined as “Lean Carbonation”. The optimal curing conditions were derived by evaluating the compressive strength and durability improvement effects of applying Lean Carbonation to secondary product specimens. As a result of the experiment, for specimens subjected to Lean Carbonation, compressive strength increased by up to 12%, and the carbonation penetration resistance also increased by more than 50%. The optimal conditions for Lean Carbonation used to improve compressive strength and durability were found to be 35 °C, 80 bar, and 1 min.     

GTR/NBR/Silica Composites Performance Properties as a Function of Curing System: Sulfur versus Peroxides

In this work, conventional sulfur and two types of organic peroxides (dicumyl peroxide (DCP) and di-(2-tert-butyl-peroxyisopropyl)-benzene (BIB)) curing systems were used to investigate the possibility for tailoring of the performance properties of GTR/NBR blends reinforced with a variable content of highly dispersive silica (0–30 phr). The curing characteristics, static mechanical and acoustical properties, swelling behavior, thermal stability, and microstructure of the prepared composites were investigated. The results show that regardless of the curing system used, increasing the content of highly dispersive silica resulted in the improvement of the mechanical properties of the studied materials. It was observed that sulfur-based systems are the best choice in terms of cross-linking efficiency determined based on torque increment and cross-link density parameters. However, further analysis of the physico-mechanical properties indicated that the cross-linking efficiency does not match the performance of specimens, and the materials obtained using organic peroxides show higher tensile properties. This is due to the improved physical interactions between the GTR/NBR matrix and highly dispersive silica when using peroxide systems. It was confirmed using the analysis of the Wolff activity coefficient, indicating the enhanced synergy.