Impact of Water Solubility on Chemical Composition and Surface Structure of Two Generations of Bioceramic Root Canal Sealers

Aimed to evaluate the effect of water solubility on chemical properties and surface structure of bioceramic-based (BC-HiFlow and BC-EndoSeqence) compared with resin-based (Adseal) root canal sealers. Fresh mix was inserted into polyethylene mold (n = 10) and subjected to Vicat needle to evaluate the setting time. The set discs were analyzed by Fourier transform infrared (FTIR) spectroscopy then immersed in deionized water for 1, 7, 14 and 28 days. The solubility%, pH changes, released calcium (Ca2+), phosphate (PO43−) and silicon (Si4+) ions were evaluated after each immersion period. The discs were analyzed by scanning electron microscopy/Energy dispersed X-ray (SEM/EDX) before and after solubility test. Although FTIR detected similar composition of both bioceramic-sealers, BC-EndoSequence determined the prolonged setting times. At the end of solubility test, both bioceramic-sealers exhibited significant greater solubility (>3%), alkaline pH (>11) at p < 0.001. Adseal displayed the significant greatest Ca2+ and PO43− released, while BC-HiFlow displayed the significant greatest Si4+ release (p < 0.001). SEM revealed voids and pores on the surface of all tested sealers with the greatest value on Adseal surface. In conclusion, although both bioceramic-sealers had high solubility, BC-Hiflow complied the ISO standard regarding setting time and least surface micropores better than that of BC-EndoSequence.

Characterization of Novel Cement-Based Carboxymethyl Chitosan/Amorphous Calcium Phosphate

Objective This study aimed to analyze, evaluate, and characterize novel cement-based carboxymethyl chitosan/amorphous calcium phosphate (CMC/ACP). Materials and Methods The three cement groups studied were gypsum (Gyp), and CMC/ACP—gypsum cement-based 5% (5% CAG) and 10% (10% CAG). The groups were characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), setting time, and scanning electron microscopy (SEM) data. The characterization results were analyzed qualitatively, but the data for setting time were analyzed using SPSS (p < 0.05). Statistical Analysis Data were statistically analyzed. One-way analysis of variance was used to compare numerical (parametric) data between more than two separate groups followed by post hoc Tukey. Results FTIR showed phosphate groups indicate the presence of calcium phosphate in the form of amorphous (ACP) in the CMC/ACP, CMC/ACP post-milled powder, and CMC/ACP cement-based (5% CAG and 10% CAG). XRD showed no difference in the diffraction spectra among the Gyp, 5% CAG, and 10% CAG groups. SEM images revealed that the CMC/ACP cement-based groups (5% CAG and 10% CAG) showed CMC/ACP cluster filled with hollow spaces between the gypsum crystals and aggregations surrounding the gypsum crystals. The CMC/ACP showed envelopes and attached to the crystalline structures of the gypsum. Setting times of 5% CAG and 10% CAG showed significant differences compared with Gyp (p < 0.05). Conclusion The result of our study showed that CMC/ACP cement-based (5% CAG and 10% CAG) demonstrated amorphous characteristic, which can stabilize calcium ions and phosphate group (ACP). In addition, the modification of gypsum using CMC/ACP as cement-based extended the time of setting.

Self-Desiccation of a Vernacular CSA Binder

The fast precipitation of ettringite in conventional Calcium Sulfo Aluminate (CSA) cement causes rapid stiffening of the cement paste and is directly associated with short setting times and self-desiccation. To extend the time during which those types of cement remain workable, retarding admixtures can be used. However, retarders may affect the amounts and types of hydration products formed and as a consequence the ability of hydrated cement to chemically bind water. This work investigates the influence of two natural-based admixtures on the self-desiccation ability of a vernacular CSA ternary binder used as earth stabilization. Vicat measurements were used to study the efficiency of citric acid and sucrose as retarding admixtures on the setting time of stabilized earth. A quantitative study of the self-desiccation ability of the binder was performed on dried binder pastes using thermogravimetric analysis (TGA). Results show that both admixtures have a significant impact on the setting time of the binder. Furthermore, TGA showed that the self-desiccation ability of this vernacular CSA binder is significantly reduced when citric acid at high dosages is used, both at early hydration and after 14 days. On the contrary, the use of sucrose does not affect the water chemically bound at an early age but can maximize bound water after 14 days of hydration.

Experimental Study of Slag Changes during the Very Early Stages of Its Alkaline Activation

The very early stages of alkaline activation of slag control its rheology and setting, but also affect its hydration, which occurs later. Simultaneously, these parameters are dictated by the nature and dose of the alkaline activator. Therefore, we investigated and compared the changes in slag particles (SEM, BET, laser diffraction), as well as in the pore solution composition (ICP–OES), pH, and conductivity, of alkali-activated slag (AAS) pastes containing the three most common sodium activators (waterglass, hydroxide, and carbonate) and water during the first 24 h of its activation. To ensure the best possible comparability of the pastes, a fairly nontraditional mixture design was adopted, based on the same concentration of Na+ (4 mol/dm3) and the same volume fraction of slag in the paste (0.50). The results were correlated with the pastes’ hydration kinetics (isothermal calorimetry), structural build-up (oscillatory rheology), and setting times (Vicat). Great differences were observed in most of these properties, in the formation of hydration products, and in the composition of the pore solution for each activator. The results emphasize the role of the anionic groups in the activators and of the pH, which help predict the sample’s behavior based on its calorimetric curve, and offer data for further comparisons and for the modelling of AAS hydration for specific activators.

Effect of Nitrate/Bromide on the Hydration Process of Cement Paste Mixed with Alkali Free Liquid Accelerator at Low Temperature

The effects of different inorganic salt accelerators (CaBr2, NaBr, Ca(NO3)2, NaNO3) and an alkali-free liquid accelerator were researched at a low temperature of 10 °C. The results showed the effects of 1.5% NaBr and 1.5% NaNO3 inorganic accelerator were pronounced. The 1-d compressive strengths of the mortar with these two inorganic salts were increased by 185.8% and 184.2%, respectively, and the final setting times were shortened from 7.74 to 6.08 min and 6.12 min, respectively. The hydration temperatures at 10 °C were measured, and the promotion effects of the inorganic accelerators were calculated: the relationship between the hydration degree was αAS + NN > αAS + NB > αAS + CB > αAS + CN > αAS. In addition, the reaction of C3A with NaBr and NaNO3 was used to analyze the products in an ettringite phase, i.e., Ca4Al2O6Br210·H2O, 3CaOAl2O3Ca(NO3)2X·H2O. The formation of these phases was detected in the hydration products of the cement paste hydration for 12 h, 24 h, and 28 d. Combined with the mass loss of the ettringite phase at 90–120 °C, determined using TG/DTG, the synergetic acceleration mechanism of the inorganic accelerators was comprehensively inferred.

Effect of Tantalum Pentoxide Addition on the Radiopacity Performance of Bi2O3/Ta2O5 Composite Powders Prepared by Mechanical Milling

Among the various phases of bismuth oxide, the high temperature metastable face-centered cubic δ phase attracts great attention due to its unique properties. It can be used as an ionic conductor or an endodontic radiopacifying material. However, no reports concerning tantalum and bismuth binary oxide prepared by high energy ball milling and serving as a dental radiopacifier can be found. In the present study, Ta2O5-added Bi2O3 composite powders were mechanically milled to investigate the formation of these metastable phases. The as-milled powders were examined by X-ray diffraction and scanning electron microscopy to reveal the structural evolution. The as-milled composite powders then served as the radiopacifier within mineral trioxide aggregates (i.e., MTA). Radiopacity performance, diametral tensile strength, setting times, and biocompatibility of MTA-like cements solidified by deionized water, saline, or 10% calcium chloride solution were investigated. The experimental results showed that subsequent formation of high temperature metastable β-Bi7.8Ta0.2O12.2, δ-Bi2O3, and δ-Bi3TaO7 phases can be observed after mechanical milling of (Bi2O3)95(Ta2O5)5 or (Bi2O3)80(Ta2O5)20 powder mixtures. Compared to its pristine Bi2O3 counterpart with a radiopacity of 4.42 mmAl, long setting times (60 and 120 min for initial and final setting times) and 84% MG-63 cell viability, MTA-like cement prepared from (Bi2O3)95(Ta2O5)5 powder exhibited superior performance with a radiopacity of 5.92 mmAl (the highest in the present work), accelerated setting times (the initial and final setting time can be shortened to 25 and 40 min, respectively), and biocompatibility (94% cell viability).

IMPLEMENTATION OF FELDSPAR AS PARTIALLY REPLACEMENT MATERIAL IN CEMENT MORTAR (EXPLORATION AND APPLICATION)

This paper aims to explore and evaluate the use of Jordanian Feldspar as a natural resource partially replacement material for each of cement and sand in cement mortar. First, Al-Jaishia area was explored through a global positioning system (GPS) navigation to gather site samples of Feldspar raw material. Afterward, cement and sand were partially replaced by Feldspar with substitution ratios of 5%, 10%, 15%, 20%, and 25% for each. The study included the effect of cement replacement on normal consistency and setting time for cement paste. The water content along with initial and final setting times increased via the increment of cement replacement ratio. Moreover, mechanical properties (compressive, flexural, and residual compressive strengths) of cement mortar due to both cement and sand replacement were evaluated. The compressive and flexural strengths after 3, 7, and 28 days of curing were examined for both cement and sand replacement. While, residual compressive strength for cement replacement after 28 days was measured at elevated temperatures of 400°C, 600°C, and 800°C. The compressive and flexural strengths decreased by increasing the Feldspar replacement ratio for both cement and sand at all specimen ages. Whereas, heat resistance properties were improved by cement/Feldspar replacement. The best result for residual compressive strength was obtained at 15% replacement ratio and 400°C temperature.

Understanding the relationship between composition and rheology in alkali-activated binders

Based on the knowledge that exists today, it is generally accepted that there are basic parameters and characteristics to obtain effective mixtures for their use in 3D printing. Rheological behavior and setting time (initial and final) are those characteristics that determine workability, as well as the speed and nature of hardening of the molded pastes and, as a result, the final framework and the integrity of the resulted structure. Among the promising options for 3D printing, the literature often contains information on alkali-activated binders. In this work, an alkali-activated binding system based on electrometallurgical slag, as well as citrogypsum, a waste of the industrial production of citric acid, was studied. Some rheological characteristics of experimental binders were considered: the nature of the mixture flow under the action of torsional loads and their initial and final setting times. It was found that the joined use of both components in the experimental system “slag - water”: an alkaline activator and citrogypsum, promotes the transition of the character of the system from thixotropic to mixed: dilatant-thixotropic (for the Na2SiO3 activator) and dilatant (for the NaOH activator). It was found that the addition of alkaline activators and citrogypsum to the binding system separately in both cases helps to reduce the initial and final setting times from 18 and 22 hours to 1 hour and 1.5 hours. Also, experimental results have shown that the jointed action of both components: an alkaline activator and cytogypsum, has a synergistic effect on the setting time.

Metakaolin Addition to Improve Geopolymerization Process and Properties of Waste Clay-Based Materials

The exploitation of different kind of clayey waste (halloysitic, smectitic/illitic, kaolinitic) for the production of geopolymers in the view of a circular economy of mines is the main goal of this study. In particular, the addition of low percentages of metakaolin (5-15%) was evaluated to improve the chemical-physical properties and the consolidation degree of geopolymeric formulations produced with clays classified as mine’s by-products. In fact, these secondary raw materials are often not sufficient alone to obtain chemically stable formulations with acceptable mechanical properties but require the addition of reactive fillers. All samples contained thermally treated clays (600°C-700°C) and metakaolin as aluminosilicate precursors, alkaline solution of NaOH and Na2SiO3, and were cured at room temperature. The influence on the final products with MK addition was monitored with the evaluation of the chemical stability in water (pH and ionic conductivity measures), the comparison of setting times (Vicat needle) and mechanical performance.

Investigation on the Compressive Strength and Time of Setting of Low-Calcium Fly Ash Geopolymer Paste Using Response Surface Methodology

Approximately 2.78 Mt of coal fly ash is produced in the Philippines, with a low utilization rate. Using fly ash-based geopolymer for construction will lessen the load sent to landfills and will result in lower GHG emissions compared to OPC. It is necessary to characterize the fly ash and optimize the geopolymer components to determine if it can replace OPC for in situ applications. The activator-to-precursor ratio, the water-to-solids ratio, and the sodium hydroxide-to-sodium silicate ratio were optimized using a randomized I-optimal design from the experimental results of 21 runs with five replicates, for a total of 105 specimens of 50 mm × 50 mm × 50 mm paste cubes. The engineering properties chosen as the optimization responses were the unconfined compressive strength (UCS), the initial setting time, and the final setting time. The samples were also ambient-cured with the outdoor temperature ranging from 30 °C to 35 °C and relative humidity of 50% ± 10% to simulate the on-site environment. Runs with high unconfined compressive strength (UCS) and short setting times were observed to have a low water-to-solids (W/S) ratio. All runs with a UCS greater than 20 MPa had a W/S ratio of 0.2, and the runs with the lowest UCS had a W/S of 0.4. The initial setting time for design mixes with a W/S ratio of 0.2 ranged from 8 to 105 min. Meanwhile, five out of seven design mixes with a W/S ratio of 0.4 took longer than 1440 min to set. Specimens with an alkali activator ratio (NaOH/WG) of 0.5 (1:2) and 0.4 (1:2.5) also had significantly lower setting times than those with an alkali activator ratio of 1. The RSM model was verified through confirmatory tests. The results of the confirmatory tests are agreeable, with deviations from the expected UCS ranging from 0 to 38.12%. The generated model is a reliable reference to estimate the UCS and setting time of low-calcium FA geopolymer paste for in situ applications.