Role of alkali cation in compressive strength of metakaolin based geopolymers

In this work, we carried out comprehensive studies on the role of alkali cations in the geopolymerization reaction and the subsequent network formation which affected the compressive strength of metakaolin (MK) based geopolymers. Rheological studies were used to provide real-time information for the geopolymerization from the initial stage. It was found that the difference in dissolution tendency between Na⁺ and K⁺ resulted in different morphologies, which affected the compressive strength. The compressive strength of the systems using Na⁺ was found to be higher than those using K⁺ under the same Si/Al ratio and alkali cation concentration. The highest compressive strength (~40.1 MPa) was obtained from a system using 12 M of Na⁺ with Si/Al ratio of 1.9:1 where a continuous monolithic microstructure was observed. Pycnometer was employed for the first time to gain an insight into the factors responsible for the compressive strength when similar morphologies were observed. The observation obtained from pycnometer compensates for the lack of visual evidence seen from similar morphologies and can serve as additional evidence for the different compressive strengths of MK based geopolymers.     

Sodalite zeolite as an alternative all-ceramic infiltrating material for alumina and zirconia toughened alumina frameworks

The purpose of this study was to determine the effects of synthesized sodalite zeolite infiltration achieved by a direct in-situ hydrothermal reaction followed by sintering process on the flexural strength and hardness of alumina and zirconia-toughened alumina (ZTA) frameworks. Ceramic core materials were prepared as disk-shaped specimens with 16 mm diameter and 1.2±0.2 mm thickness. The case-study group was synthesized sodalite zeolite-infiltrated alumina (IA-SOD) and synthesized sodalite zeolite-infiltrated ZTA (IZ-SOD); and the control group was glass-infiltrated alumina (IA-glass) and glass-infiltrated ZTA (IZ-glass). The biaxial flexural strength (piston-on-three-balls test) and Vickers microhardness were compared among groups (n=10 specimens in each group). Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) were used to investigate the structural characteristics of specimens at the fracture and cross-sectional surfaces. For both IA-SOD and IZ-SOD, the biaxial flexural strength exceeded the required value of 100–150 MPa as specified by ISO 6872(2015), indicating their potential as all-ceramic core materials. The flexural strengths and Vickers microhardness of IZ-SOD were respectively 324.7 MPa and 1162 VHN, while these values were measured 233.6 MPa and 1013 VHN for IA-SOD. The mechanical properties and microstructure of core materials have been advocated as crucial to the clinical performance of all-ceramic dental restorations. This investigation provides data regarding the flexural strength, hardness and microstructure of partially sintered alumina and ZTA frameworks with synthesized sodalite zeolite infiltration.     

Enhancement mechanical properties of in-situ preparated B4C-based composites with small amount of (Ti3SiC2+Si)

B₄C-based composites were synthesized by spark plasma sintering using B₄C、Ti₃SiC₂、Si as starting materials. The effects of sintering temperature and second phase content on mechanical performance and microstructure of composites were studied. Full dense B₄C-based composites were obtained at a low sintering temperature of 1800 °C. The B₄C-based composite with 10 wt% (TiB₂+SiC) shows excellent mechanical properties: the Vickers hardness, fracture toughness, and flexural strength are 33 GPa, 8 MPa m^1/2, 569 MPa, respectively. High hardness and flexural strength were attributed to the high relative density and grain refinement, the high fracture toughness was owing to the crack deflection and uniform distribution of the second phase.     

Preceramic paper-derived Ti3Al(Si)C2-based composites obtained by spark plasma sintering

The paper describes the structure and properties of preceramic paper-derived Ti₃Al(Si)C₂-based composites fabricated by spark plasma sintering. The effect of sintering temperature and pressure on microstructure and mechanical properties of the composites was studied. The microstructure and phase composition were analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. It was found that at 1150 °C the sintering of materials with the MAX-phase content above 84 vol% leads to nearly dense composites. The partial decomposition of the Ti₃Al(Si)C₂ phase becomes stronger with the temperature increase from 1150 to 1350 °C. In this case, composite materials with more than 20 vol% of TiC were obtained. The paper-derived Ti₃Al(Si)C₂-based composites with the flexural strength > 900 MPa and fracture toughness of >5 MPa m^1/2 were sintered at 1150 °C. The high values of flexural strength were attributed to fine microstructure and strengthening effect by secondary TiC and Al₂O₃ phases. The flexural strength and fracture toughness decrease with increase of the sintering temperature that is caused by phase composition and porosity of the composites. The hardness of composites increases from ~9.7 GPa (at 1150 °C) to ~11.2 GPa (at 1350 °C) due to higher content of TiC and Al₂O₃ phases.     

Preparation,mechanical properties,and toughening mechanisms of SiCw/SiCp-reinforced zirconia-toughened alumina ceramics

Zirconia-toughened alumina (ZTA) ceramics with high mechanical properties were sintered by hot-pressing method using SiC particles (SiCp) and SiC whiskers (SiCw) as the reinforcing agents simultaneously. The influences of sintering temperature, SiCp, and SiCw contents on the microstructure and mechanical properties of ZTA ceramics were investigated. It was found that both SiCp and SiCw could contribute to grain refinement significantly and promote the mechanical properties of the ceramics. However, the excess addition of SiCp or SiCw led to the formation of pores with large sizes and degraded the mechanical properties instead. When 13 wt% SiCp was introduced, the maximum flexural strength of 1180.0 MPa and fracture toughness of 15.9 MPa·m^1/2 were obtained, whereas the maximum flexural strength of 1314.0 MPa and fracture toughness of 14.7 MPa·m^1/2 were achieved at 20 wt% SiCw. Interestingly, the simultaneous addition of SiCp and SiCw could further improve the mechanical properties, and the highest flexural strength of 1334.0 MPa and fracture toughness of 16.0 MPa·m^1/2 were achieved at a SiCw/SiCp ratio of 16/4. The reinforcement mechanisms in the ceramics mainly included the phase transformation toughening of ZrO₂, the crack deflection and bridging of SiCp and SiCw, and the pull-out of SiCw.     

Relative importance of Al(V) and reinforcement to the flexural strength of geopolymer composites

We prepared 1 cm × 1 cm × 10 cm geopolymer bars from sodium silicate and six commercial metakaolins, both unreinforced and reinforced with 20 wt% of 55-μm wollastonite (CaO·SiO₂) needles, to evaluate the relative contributions of five-coordinated aluminum in the metakaolin and the presence of a reinforcing phase to the flexural strength of geopolymers. Two metakaolins, with about 20 at% and lower of five-coordinated aluminum content, did not react sufficiently with our processing method and could not be tested. The flexural strengths of the other four geopolymers were similar at about 11–14 MPa unreinforced and 22–29 MPa reinforced. The effect of reinforcement on flexure strength is more significant than the choice of metakaolin provided that the metakaolin is reactive. The geopolymerization reaction depends on the amount of five-coordinated aluminum present in the metakaolin and is the primary difference between the samples that reacted and those that did not react.     

Synthesis of Si3N4/SiC reaction-bonded SiC refractories: The effects of Si/C molar ratio on microstructure and properties

Si₃N₄/SiC reaction-bonded SiC refractories have been fabricated on the basis of the microstructure design concept by introducing a binary-phases binding system. The influence of Si/C molar ratio on phase transformation, microstructure and mechanical properties was studied systematically. Thermodynamic analysis result proved the microstructure design was feasible under 0.03 MPa pressure of N₂ and the selected sintering temperature. In-situ grown SiC nano-whiskers/granule and lamellar Si₃N₄ were both observed in the matrix. The specimen with 2:1 Si/C molar ratio possessed highest cold modulus of rupture (28.27 MPa) but showed low toughness. The strength and toughness of such materials were controlled by two main factors, such as SiC grain boundary binding morphology and in situ grown of SiC in the matrix. The different mechanisms occurred predominantly to meet diverse practical cases and caused to various mechanical properties of final products. The corresponding strengthening and toughening mechanisms were explained in this paper.     

Low-temperature diffusion bonding of Ti3Si(Al)C2 ceramic with Au interlayer

Herein, a reliable diffusion bonding of Ti₃Si(Al)C₂ ceramic is achieved by applying Au foil as an interlayer at 650 °C for 30 min with an axial pressure of 20 MPa. This novel method significantly decreases the bonding temperature, which is about 150 °C lower than the lowest bonding temperature from current research to the best of our knowledge. Maximum shear strength of 58 MPa is achieved at 650 °C among the bonding temperature range of 600 °C~800 °C. The microstructure evolution mechanism and the relationship between microstructure and mechanical property are discussed. The facile mutual diffusion of Au with de-intercalated Al and Si from Ti₃Si(Al)C₂ is considered critical in achieving sound interfacial bonding.     

Effect of zirconia content and particle size on the properties of 3D-printed alumina-based ceramic cores

Alumina-based ceramic cores are used to manufacture the internal structures of hollow alloy blades, requiring both high precision and moderate properties. In this work, zirconia is regarded as a promoter to improve the mechanical properties of sintered ceramic. The effect of zirconia content and particle size on the microstructure and mechanical properties of ceramics was evaluated. The results indicate that the flexural strength of sintered ceramics reached the maximum of 14.5 ± 0.5 MPa when 20 wt% micron-sized (10 μm) zirconia (agglomerate size, consistent with the alumina particle size) was added, and 26.5±2.5 MPa when 15 wt% 0.3 μm zirconia was added. Zirconia with submicron-sized (0.3 μm) particles effectively filled the pores between alumina particles, thus leading to the maximum flexural strength with a relatively low content. The corresponding sintered ceramics had a bulk density of 2.0 g/cm³ and open porosity of 59.6%.     

High temperature strength of silicon carbide sintered with 1 wt.% aluminum nitride and lutetium oxide

A heat-resistant SiC ceramic was developed from submicron β-SiC powders using a small amount (1 wt.%) of AlN–Lu₂O₃ additives at a molar ratio of 60:40. Observation of the ceramic using high-resolution transmission electron microscopy (HRTEM) showed a lack of amorphous films in both homophase (SiC–SiC) boundaries and junction areas. The junction phase consisted of Lu–Si–O elements, and the homophase boundaries contained Lu, Al, O, and N atoms as segregates. The ceramic maintained its room temperature (RT) strength up to 1600 °C. The flexural strength of the ceramic was 630 MPa and 633 MPa at RT and 1600 °C, respectively.     

Thin fly ash/ ladle furnace slag geopolymer: Effect of elevated temperature exposure on flexural properties and morphological characteristics

The flexural properties and thermal performance of 10 mm-thin geopolymers made from fly ash and ladle furnace slag were evaluated before and after exposure to elevated temperatures (300 °C, 600 °C, 900 °C, 1100 °C and 1150 °C). Class F fly ash was mixed with liquid sodium silicate (Na₂SiO₃) and 12 M sodium hydroxide (NaOH) solution using aluminosilicate/activator ratio of 1:2.5 and Na₂SiO₃/NaOH ratio of 1:4 to synthesise thin fly ash (FA) geopolymers. 40 wt% of ladle furnace slag was partially replacing fly ash to produce fly ash/slag-based (FAS) geopolymers. Thermal treatment enhanced the flexural strength of thin geopolymers. In comparison to the unexposed specimen, the flexural strength of FA geopolymers at 1150 °C and FAS geopolymers 1100 °C was increased by 161.3% to 16.2 MPa and 208.9% to 24.1 MPa, respectively. A more uniform heating was achieved in thin geopolymers which favoured the phase transformation at high temperatures and contributed to the substantial increase in flexural strength. The joint effect of elevated temperature exposure and the incorporation of ladle furnace slag further improved the flexural strength of thin geopolymers. The calcium-rich slag refined the pore structure and increased the crystallinity of thin geopolymers which aided in high strength development.     

High-strength Ti2AlN ceramics prepared by pulse electric current sintering based on powders synthesized by molten salt method

Ti₂AlN powders were synthesized through molten salt method and re-calcination process using TiH₂, Al and TiN powders as raw materials at 1100 ℃. The composition of final composite was directly influenced by the initial Al and TiH₂ content in the starting mixture. The purity of the synthesized Ti₂AlN powder could reach 97.1 wt% when the Al molar ratio was 1.05. Then high strength Ti₂AlN ceramics were successfully prepared in different modes, including two forms of pulse electric current sintering (PECS/SPS) and hot-pressing sintering (HP). A record-high flexural strength of 719 MPa was obtained for the PECS/SPS with an electrical insulating die (PECS/SPS II) sintered sample, based on the synthesized powder in which the initial molar ratio of Al was 1.1. The sintering behaviors in various modes were analyzed, confirming the shrinkage of particles starting at lower temperature in PECS/SPS II. The density, microstructure, Vickers hardness and elastic modulus of sintered ceramics were also investigated. Therefore, the present work provided the new methods about powder preparation and ceramic sintering of Ti₂AlN, making it possible to be used as high strength structural ceramics.     

Effects of YH2 addition on pressureless sintered AlN ceramics

A new type of non-oxide sintering additive of YH₂ was introduced for the fabrication of AlN ceramics with high thermal conductivity and flexural strength. The effects of YH₂ addition (0–5 wt%) on the phase composition, densification, microstructure, thermal conductivity and flexural strength of pressureless sintered AlN ceramics were investigated and compared with those Y₂O₃-added samples (1–5 wt%). The addition of 1 wt% YH₂ led to an in-situ reduction reaction with oxygen impurities, the formation of Y₂O₃ and finally the formation of yttrium aluminate, which in turn improved densification and microstructure. A high flexural strength (408.69 ± 28.23 MPa) was achieved. The addition of 3 wt% YH₂ increased the average grain size and purified the lattice. All these effects are believed to help achieve a high thermal conductivity of 184.82 ± 1.75 W·m^?1·K^?1. Although the thermal conductivity was close to the value of 3 wt% Y₂O₃-added sample, its strength was much increased to 381.53 ± 43.41 MPa. Meanwhile, it demonstrated a good combination of the thermal conductivity and flexural strength than the values reported in some literature. However, further increasing the YH₂ addition to 5 wt% resulted in a high N/O ratio that inhibited the densification behavior of AlN ceramics. The current study showed that AlN ceramics with excellent thermal and mechanical properties could be obtained by the introduction of a suitable YH₂ additive.     

High-temperature resistant ambient pressure-dried aluminum doped silica aerogel from inorganic silicon and aluminum sources

Aluminum doped silica aerogel (ASA) exhibiting improved high-temperature resistance is usually prepared via supercritical drying from organic silicon and/or aluminum precursors, which propels the production cost significantly. Herein we demonstrate a simple and effective method to prepare highly thermal resistant ASA via the sol-gel and ambient pressure drying route by using water glass and aluminum chloride as precursors. Effects of the Al/Si molar ratio in precursor, the calcination temperature and the modifier type on the crystallinity, morphology, pore structure of ASA are investigated. Results show that the Al/Si molar ratio and the calcination temperature have significant effects on the structure and heat resistance performance of ASA at temperature of 600–1000 °C. The sample with Al/Si molar ratio of 0.15 shows the highest specific surface area of 805.9 m²/g and pore volume of 5.038 cm³/g after heated to 600 °C, and retains 179.5 m²/g and 1.295 cm³/g respectively after heated to 1000 °C. Mechanism analysis indicates that, though the actual aluminum content is extremely low (0.18%, wt%), the high-temperature resistance of ASA is greatly improved owing to the effective doping of aluminum in the lattice of SiO₂ and the corresponding electrostatic repulsion between neighboring nanoparticles induced by the replacement of Si⁴⁺ by Al³⁺ ions.     

Preparation and characterization of tungsten tailing-based geopolymers

Using tailings to prepare constructive materials is of great significance for sustainable development of mineral processing industry. In this study, the possibility of preparing tungsten tailing-based geopolymers was explored in detail. XRD, FTIR, PLM, SEM and XPS analyses were carried out to characterize the phase composition, chemical bonding, microstructure, chemical state, and interface properties of tungsten tailing-based geopolymers. Results showed tungsten tailings presented little activity using NaOH as activator, while geopolymers with 60% non-pretreatment tungsten tailing and 40% metakaolin presented a 3-day compressive strength of 8.4 MPa and 28-day compressive strength of 9.1 MPa. The geopolymerization products of tungsten tailing-based geopolymers were N-A-S-H gels and aluminosilicate zeolite crystals, while tungsten tailings were wrapped by metakaolin-derived geopolymerization phases as aggregates with interfaces containing Si–O–Si bonding between quartz in tungsten tailings and zeolite and/or gel phase in metakaolin-derived geopolymer in the geopolymerization process. Besides, the leaching test results indicated that the immobilization efficiency of T6M4 geopolymers for Mn and Pb derived from tungsten tailings reached up to 97.28% and 99.95%, respectively. This research results provide a new idea for utilization of tungsten tailings on a large scale.     

Effect of TiO2 addition on the properties of Ti3Si(Al)C2 based ceramics fabricated by reactive melt infiltration

In this paper, Ti₃Si(Al)C₂ based ceramics were fabricated by reactive melt infiltration (RMI) of TiC/TiO₂ preforms with liquid silicon. The microstructure, phase composition, and mechanical properties of the Ti₃Si(Al)C₂ based ceramics have been investigated to understand the effect of phase composition of the preforms on the formation mechanisms of Ti₃Si(Al)C₂. The preforms with different content of TiO₂ infiltrated at 1500 °C with liquid silicon for 1 h were composed of Ti₃Si(Al)C₂, Al₂O₃, TiC, TiSi_xAl_y and residual Al. The prior generated Al₂O₃ phases inhibited the dispersion of Ti₃Si(Al)C₂ phases, resulting in the drastically grain growth of Ti₃Si(Al)C₂. Subsequently, the microstructure with gradually increasing Ti₃Si(Al)C₂ grain size resulted in the decrease of the bending strength and fracture toughness of samples. When the content of TiO₂ reached 20 wt%, the bending strength reached the maximum, 326.6 MPa. The fracture toughness attained the maximum, 4.3 MPa m^1/2, when the content of TiO₂ was 10 wt%.     

Effect of Ni content and its particle size on electrical resistivity and flexural strength of porous SiC ceramic sintered at low-temperature using clay additive

A low-temperature sintered porous SiC-based clay-Ni system with controlled electrical resistivity (2.54 × 10¹⁰ Ω cm to 2 Ω cm), and thermal conductivity (3.5 W/m. K to 12.6 W/m. K) was successfully designed. Clay (20 wt% kaolin) was used as a sintering additive in all the compositions. The electrical resistivity, and thermal conductivity was controlled by varying the Ni content (0–25 wt%) in the samples. The electrical resistivity was recorded as low as 2 Ω cm with 25 wt% Ni that was sintered at 1400 °C in argon. The interface reaction between Ni and SiC formed conductive nickel silicide (Ni₂Si), while the transformation of kaolin to mullite strengthened the mechanical properties. Submicron-sized Ni (0.3 μm) was more effective than micron-sized Ni (3.5 μm) in reducing the electrical resistivity, and increasing the thermal conductivity along with flexural strength. A comparative study of sintering temperatures showed that 1400 °C resulted in the lowest electrical resistivity (2 Ω cm) and the highest thermal conductivity of 12.6 W/m. K with flexural strength of 54 MPa at 32% porosity in the SiC-kaolin-Ni system.     

Microstructure and mechanical properties of SiC-SiC joints joined by spark plasma sintering

The development of reliable joining technology is of great importance for the full use of SiC. Ti₃SiC₂, which is used as a filler material for SiC joining, can meet the demands of neutron environment applications and can alleviate residual stress during the joining process. In this work, SiC was joined using different powders (Ti₃SiC₂ and 3Ti/1.2Si/2C/0.2Al) as filler materials and spark plasma sintering (SPS). The influence of the joining temperature on the flexural strength of the SiC joints at room temperature and at high temperatures was investigated. Based on X-ray diffraction and scanning electron microscopy analyses, SiC joints with 3Ti/1.2Si/2C/0.2Al powder as the filler material possess high flexural strengths of 133 MPa and 119 MPa at room temperature and at 1200 °C, respectively. The superior flexural strength of the SiC joint at 1200 °C is attributed to the phase transformation of TiO₂ from anatase to rutile.     

Low thermal expansion porous SiC–WC composite ceramics

Low thermal expansion porous SiC–WC composite ceramics were prepared by solid state reaction of Si and WC at 1560 °C, with NH₄HCO₃ as a pore generating agent. Phase composition, thermal expansion, flexural strength, and microstructure of the carbide ceramics were examined. Presence of the SiC, WC and WC_1−X phases were detected in the carbide ceramics. As Si content increased from 2 to 14 wt%, the coefficient of thermal expansion first decreased and then increased, with a minimum of 4.11 × 10⁻⁶ °C at 8 wt% Si, whereas the flexural strength decreased gradually, from 143.9 to 82.7 MPa. Pores of SiC–WC ceramics were less than 2 μm in diameter, because of the stacking interstice of carbide particles and volatilization of silicon. However in the presence of NH₄HCO₃, pores of SiC–WC ceramics were bimodally distributed, the stacking interstice of carbide particles loosened from 1 to 4 μm and pores larger than 5 μm were also formed.     

Ti3Si(Al)C2-based ceramics fabricated by reactive melt infiltration with Al70Si30 alloy

Dense Ti₃Si(Al)C₂-based ceramics were synthesized using reactive melt infiltration (RMI) of Al₇₀Si₃₀ alloy into the porous TiC preforms. The effects of the infiltration temperature on the microstructure and mechanical properties of the synthesized composites were investigated. All the composites infiltrated at different temperatures were composed of Ti₃Si(Al)C₂, TiC, SiC, Ti(Al, Si)₃ and Al. With the increase of infiltration temperature from 1050 °C to 1500 °C, the Ti₃Si(Al)C₂ content increased to 52 vol.% and the TiC content decreased to 15 vol.%, and the Vickers hardness, flexural strength and fracture toughness of Ti₃Si(Al)C₂-based composite reached to 9.95 GPa, 328 MPa and 4.8 MPa m^1/2, respectively.