Characteristics of quadruplet Ti–Mo–TiB2–TiC composites prepared by spark plasma sintering

The spark plasma sintering process was implemented to produce four different composites, namely Ti-10 wt% Mo-(0.5, 1, 2, and 4) wt% (TiB₂ + TiC). All samples were sintered at 1300 °C for 5 min under 50 MPa. A full study was carried out on the mechanical properties and the relative density of these SPSed composite samples. The best relative density of around 98.7% was related to the sample with 1 wt% (TiB₂ + TiC). The role of relative density was so predominant that the best values for all mechanical properties, i.e., bending strength, hardness, elongation, and ultimate tensile strength (UTS), were achieved for those with the highest relative density values. The formation of the in-situ TiB phase was proved by the XRD analysis. Besides, microscopical investigations (optical and SEM) showed that adding more ceramic additives led to an increased amount of porosity while Mo solubility decreased in the titanium matrix. Finally, different fracture modes on the surfaces of composite samples were studied using SEM images.     

Investigating the effect of porosity level and pore former type on the mechanical and corrosion resistance properties of agro-waste shaped porous alumina ceramics

The strength integrity and chemical stability of porous alumina ceramics operating under extreme service conditions are of major importance in understanding their service behavior if they are to stand the test of time. In the present study, the effect of porosity and different pore former type on the mechanical strength and corrosion resistance properties of porous alumina ceramics have been studied. Given the potential of agricultural wastes as pore-forming agents (PFAs), a series of porous alumina ceramics (Al₂O₃-xPFA; x=5, 10, 15 and 20 wt%) were successfully prepared from rice husk (RH) and sugarcane bagasse (SCB) through the powder metallurgy technique. Experimental results showed that the porosity (44–67%) and the pore size (70–178 µm) of porous alumina samples maintained a linear relationship with the PFA loading. Comprehensive mechanical strength characterization of the porous alumina samples was conducted not just as a function of porosity but also as a function of the different PFA type used. Overall, the mechanical properties showed an inverse relationship with the porosity as the developed porous alumina samples exhibited tensile and compressive strengths of 20.4–1.5 MPa and 179.5–10.9 MPa respectively. Moreover, higher strengths were observed in the SCB shaped samples up to the 15 wt% PFA mark, while beyond this point, the silica peak observed in the XRD pattern of the RH shaped samples favored their relatively high strength. The corrosion resistance characterization of the porous alumina samples in hot 10 wt% NaOH and 20 wt% H₂SO₄ solutions was also investigated by considering sample formulations with 5–15 wt% PFA addition. With increasing porosity, the mass loss range in RH and SCB shaped samples after corrosion in NaOH solution for 8 h were 1.25–3.6% and 0.44–2.9% respectively; on the other hand, after corrosion in H₂SO₄ solution for 8 h, the mass loss range in RH and SCB shaped samples were 0.62–1.5% and 0.68–3.3% respectively.     

Triplet carbide composites of TiC,WC, and SiC

In this study, the influence of adding 0, 10, 20, and 30 vol% SiC_w on the microstructure and physical-mechanical properties (relative density (RD), flexural strength, and Vickers hardness) of TiC-3 wt% WC_n was investigated. All designed samples were spark plasma sintered under the same conditions: sintering temperature of 1900 °C, external pressure of 40 MPa, and dwell time of 7 min. Microstructural evaluation and relative density calculation revealed that the additives were dispersed homogeneously in the TiC matrix. Based on the Archimedes principles, RD values of >100% were measured for the composite samples with 20 and 30 vol% SiC_w, due to not accounting the formation of non-stoichiometric TiC and (Ti,W)C phases in the calculations. On the contrary, the lowest RD was related to the sample with 10 vol% SiC_w. On the other hand, the most significant values of Vickers hardness (28.6 GPa) and flexural strength (694 MPa) were obtained for TiC-3 wt% WC_n and TiC-3 wt% WC_n-20 vol% SiC_w composite samples, respectively.     

Sintering and microstructural study of mullite prepared from kaolinite and reactive alumina: Effect of MgO and TiO2

Mullite ceramic was prepared using kaolinite and synthesized alumina (combustion route) by solid-state interaction process. The influence of TiO₂ and MgO additives in phase formation, microstructural evolution, densification, and mechanical strengthening was evaluated in this work. TiO₂ and MgO were used as sintering additives. According to the stoichiometric composition of mullite (3Al₂O₃·2SiO₂), the raw materials, ie kaolinite, synthesized alumina, and different wt% of additives were wet mixed, dried, and uniaxially pressed followed by sintering at different temperature. 1600°C sintered samples from each batch exhibit enhanced properties. The 1 wt% TiO₂ addition shows bulk density up to 2.96 g/cm³ with a maximum strength of 156.3 MPa. The addition of MgO up to 1 wt% favored the growth of mullite by obtaining a density and strength matching with the batch containing 1 wt% TiO₂. These additives have shown a positive effect on mullite phase formation by reducing the temperature for complete mullitization by 100°C. Both additives promote sintering by liquid phase formation. However, the grain growth, compact microstructure, and larger elongated mullite crystals in MgO containing batch enhance its hardness properties.     

Thermodynamical evaluation,microstructural characterization and mechanical properties of B4C–TiB2 nanocomposite produced by in-situ reaction of Nano-TiO2

This work discusses the pressureless sintering of a boron carbide-titanium diboride (B₄C– TiB₂) nanocomposite via in-situ reaction of the boron carbide/titanium dioxide/carbon system. Attempting to sinter pure boron carbide leads to poor mechanical properties. In this work, the effect of adding TiO₂ to B₄C on mechanical properties of the boron carbide was investigated. Thermodynamic simulations were performed with HSC chemistry software to determine the phases which were most likely to form during the sintering process. The reaction thermodynamics suggested that during the sintering process, formation of TiB₂ occurs preferentially over formation of TiC. For examination of the microstructural evolution of the samples, Scanning Electron Microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) were utilized. The density, porosity, Young's modulus, microhardness and fracture toughness of the specimens were compared. Optimum properties were achieved by adding 10 wt% TiO₂. In the sample possessing 10 wt% TiO₂, the relative density, Young's modulus, hardness and fracture toughness were 94.26%, 428 GPa, 23.04 GPa and 5.19 MPa m^0.5, respectively, and the porosity was decreased to 5.73%. Furthermore, phase analysis via XRD confirmed that the final product was free of unreacted TiO₂ or carbon.     

Properties of phyllosilicate-based porous ceramics shaped by conventional tape casting and freeze tape casting

Silicate ceramics were shaped using tape casting (TC) and freeze tape casting (FTC) processes from three clays labeled HCR, KORS, and KCR. These clays exhibited mass content of 77% halloysite–10 Å, 29% kaolinite, and 98% kaolinite minerals, respectively. After casting the slurries, the dried tapes were sintered at 1200°C. The microstructure changes were characterized before and after sintering using scanning electron microscopy. The apparent porosity of TC samples was lower (36–47 vol.%) compared to values obtained with FTC samples (67–79 vol.%). The latter samples exhibited a highly textured porosity, with micron-sized pores aligned perpendicular to the tape surfaces. Upon sintering, the porosity of TC samples tended to decrease conversely to the case of FTC samples. Such behavior seemed related to the simultaneous effect of organic additives and ice templating. Consequently, the FTC samples showed a relatively low mechanical strength of 3–7 MPa and thermal conductivity of .14– .22 W m⁻¹ K⁻¹. After sintering, the mullite crystallization contributed to strengthen the bulk materials, helping to compensate for the detrimental effect of porosity on the stress to rupture and on thermal conductivity values.     

Investigation of microstructure and mechanical properties of Cu/Ti–B–SiCp hybrid composites

In this study, Cu/Ti–B-SiC_p hybrid composite materials were produced by powder metallurgy method using three different sintering temperatures (950, 1000, 1050 °C). The optimum sintering temperature of Cu main matrix composites reinforced with Ti–B-SiC_p reinforcement materials at 2-4-6-8 wt.% were determined and their microstructure and mechanical properties were investigated. As a result of microstructure studies, it was determined that reinforcement elements have a homogeneous interface in the main matrix. The hardness of the produced composites was determined by the Brinell hardness method. The highest hardness value (77.74 HB) was determined in the sample with 6 wt% reinforcement ratio. In the tensile and three point bending tests, maximum strength values (112.96 MPa, 37.76 MPa) were found in samples with a reinforcement ratio of 4 wt%. It was determined that increasing reinforcement ratios and sintering temperature made a positive contribution to the hybrid composite materials produced.     

Effects of oxide addition on structure and properties of WC–10Co cemented carbide obtained by in situ synthesized powder

Combining spray drying and in situ synthesized technology, WC–10Co cemented carbide with uniform composition was prepared by vacuum sintering. The effects of Al₂O₃ and additions of different rare-earth oxides (La₂O₃, Y₂O₃ and CeO₂) on the microstructure and mechanical properties of WC–10Co were investigated. As the Al₂O₃ content increased from .5 to 2 wt%, the hardness of the sintered sample increased, whereas the relative density and fracture toughness decreased. Compared with the addition of .5 wt% Al₂O₃, the WC–10Co alloy with .5 wt% rare-earth oxides had higher hardness. In addition, compared with the alloy without an inhibitor (.80 μm), after adding .5 wt% Al₂O₃, La₂O₃, Y₂O₃ and CeO₂, the WC grain sizes were reduced to .73, .65, .71 and .62 μm, respectively, which indicated that the addition of Al₂O₃ and rare-earth oxides could refine WC grain during sintering. Among these additives, CeO₂ had the best effect. With the addition of .5 wt% CeO₂, the hardness and the fracture toughness increased from 1299 to 1710 HV₃₀ and from 16.18 to 18.90 MPa m^1/2, respectively.     

The effect of alumina-based sintering aid on the microstructure,selected mechanical properties,and coefficient of friction of Cf/SiC composite prepared via spark plasma sintering (SPS) method

C_f-SiC air brake discs are being developed due to their high-temperature oxidation resistance compared to conventional C_f/C discs. The C_f-SiC air brake discs should have a coefficient of friction (COF) close to 0.4, a low wear rate, a density higher than 95% of the theoretical density, and flexural strength of more than 200 MPa. To reach the properties of C_f-SiC composite to the required characteristics of the air brake disc, different amounts of alumina-based sintering aid were used. For this purpose, first silicon carbide nanoparticles, sintering aids Al₂O₃–MgO, MgAl₂O₄, Al₂O₃–Y₂O₃, Al₂O₃–SiO₂–MgO, and carbon fiber (20 wt%) with a 5-mm length were prepared. Next, the final composite bulk was created via the SPS method at 1900 °C under a pressure of 50 MPa. The density of the sample sintered with the Al₂O₃–SiO₂–MgO sintering aid was higher than that of other sintering aids. The density value was obtained at 98% and 100% at 8 wt% and 4 wt% respectively. It was also found that the use of 4 wt% of Al₂O₃–SiO₂–MgO offered better mechanical properties compared to 8 wt%, due to the absence of Al₈Si₄O₂₀ phase at 4 wt%. The examination of mechanical properties showed that the hardness (3564 Vickers) and flexural strength (479 MPa) of the sample with the Al₂O₃–SiO₂–MgO sintering aid were higher than those of other sintering aids. The samples with the Al₂O₃–SiO₂–MgO sintering aid with 4 wt% revealed a COF of 0.41, showing the closest feature to the desired indices of aircraft brake discs.     

Effect of Li2CO3–Bi2O3 doping on the low-temperature sintering,structure, and dielectric and mechanical properties of MgO–TiO2(w) ceramics

Dense MgO–12% TiO₂(w) ceramics containing 12 wt% TiO₂, which were doped with Li₂CO₃–Bi₂O₃ composite sintering aids, were prepared at a low sintering temperature of 950 °C in this study. The effects of sintering additives on the sintering characteristics, phase composition, microstructure, and dielectric and mechanical properties of the ceramic samples were systematically investigated, and the influences of their phase composition and microstructure on the dielectric and mechanical properties were examined. The introduction of sintering aids produced a new Bi₄Ti₃O₁₂ phase in the sample structure, while the residual Bi₂O₃ mixed with the newly formed Mg₂TiO₄ and Bi₄Ti₃O₁₂ phases distributed at MgO grain boundaries formed a structure surrounding MgO grains. This structure filled the pores in the ceramic sample, which increased its density and enhanced the mechanical properties. At a Li₂CO₃–Bi₂O₃ content of 15 wt%, the density, flexural strength, and Vickers hardness of the ceramic samples reached their maximum values of 3.4 g/cm³, 218.9 MPa, and 778.7 HV, respectively. However, the further increase in the Li₂CO₃–Bi₂O₃ content deteriorated their dielectric properties although the dielectric constant and dielectric loss remained below 13.4 and 2.1 × 10⁻³, respectively. The findings of this work indicate that Li₂CO₃–Bi₂O₃ sintering aids can significantly lower the sintering temperature of MgO–12% TiO₂(w) ceramics and control their dielectric and mechanical properties through microstructural changes.     

Effect of manganese addition on sintering behavior and mechanical properties of alumina toughened zirconia

The effect of MnO₂ additives on the sintering behavior and mechanical properties of alumina-toughened zirconia (ATZ, with 10 vol% alumina) composites was investigated by incorporating different amounts of MnO₂ (0, 0.5, 1.0, and 1.5 wt%) and sintering at various temperatures ranging from 1300 to 1450 °C. The addition of MnO₂ up to 1.0 wt% improved the sintered density, hardness, flexural strength, and fracture toughness of the composite. However, the addition of 1.5 wt% MnO₂ degraded the relative density, hardness, and flexural strength of the composite due to the transformation of the ZrO₂ phase from tetragonal to monoclinic and grain coarsening. Optimal results were obtained with 1.0 wt% MnO₂ and sintering at 1450 °C, which improved the mechanical properties (hardness: 13.5 GPa, flexural strength: 1.2 GPa, fracture toughness: 8.5 MPa m^1/2) and lowered the sintering temperature compared to the conventional sintering temperature of ATZ composites (1550 °C). Thus, the ATZ composite doped with MnO₂ is a promising material for structural engineering ceramics owing to its improved mechanical properties and lower sintering temperature.     

Mechanical and dielectric properties of reduced graphene oxide nanosheets/alumina composite ceramics

Reduced graphene oxide (rGO) nanosheets/alumina (Al₂O₃) composite ceramics were fabricated by hot-pressing sintering. The density, porosity, microhardness, flexural strength and complex permittivity were investigated to study their mechanical and dielectric properties. The results revealed that the rGO nanosheets were uniformly distributed in the Al₂O₃ matrix and that the composite ceramics were highly dense at 3.67–3.99 g/cm³. Due to low rGO hardness and elevated porosity, the microhardness exhibits a decreasing trend as the rGO content increases. The flexural strength first increased and then decreased with the escalation of rGO content, and the highest strength of 313.75 MPa was obtained at 3 wt%, increasing by 37.61% relative to that of the hot-pressing sintered Al₂O₃ ceramic. Owing to the enhanced interfacial polarization, dipole polarization, polarization relaxation loss and conductance loss, the real part and imaginary part of complex permittivity increase from 10.40 to 52.73 and from 0.08 to 28.86 as the rGO content rose from 0 wt% to 4 wt%, respectively.     

The influence of silica nanoparticles addition on the physical,mechanical, thermo-mechanical as well as microstructure of Mag-Dol refractory composites

The high hydration potential of CaO and MgO phases restricted the application of Mag-Dol refractory composites. In this study, the impact of nano-silica (SiO₂) addition on the physical, mechanical, thermo-mechanical as well as microstructure of Mag-Dol refractory composites is investigated. Mag-Dol compositions were prepared by using calcined dolomite and magnesite particles (micron, 0–1, 1–3, 3–5, and 5–8 mm), liquid resin, and 0, 0.5, 1, 1.5, 2, and 2.5 wt% nano SiO₂ as additives. Specimens were heated up to 1650 °C for the 3 h soaking period. Fired specimens were characterized by physical (apparent porosity, bulk density, and hydration resistance), mechanical (cold crushing strength), and thermo-mechanical (flexural strength at 1200 °C) measurements. XRD and SEM/EDS analysis were done to study phases and microstructure analysis of the fired samples, respectively. Results showed that by adding up to 2.5 wt% nano-SiO₂, due to the formation of CaO·MgO·2SiO₂ (Diopside), 2CaO·MgO·2SiO₂ (Akermanite), and CaO·MgO·SiO₂ (Monticellite) phases, physical and mechanical properties were enhanced. But the highest flexural strength value is achieved for 1 wt% nano-SiO₂ containing sample.     

Evaluating the role of uniformity on the properties of B4C–SiC composites

Fully dense boron carbide-silicon carbide composites were successfully produced by spark plasma sintering method at 1950 °C under 50 MPa applied pressure. The effect of dry and wet mixing methods on uniformity was observed. Density, elastic modulus, microstructure, Vickers hardness and fracture toughness were evaluated. The results showed that dry mixing did not provide uniformity on composites properties. On the other hand wet mixing provided uniformity in microstructure and consistency in material properties. The hardness of the sample containing 50 wt% B₄C was measured to be 30.34 GPa hardness value was found at 50 wt% B₄C content sample. The increase in the B₄C content of the composites decreased the Young's modulus, shear modulus, bulk modulus and fracture toughness. The highest values were found at 10 wt% B₄C sample which were 415 GPa (E), 177 GPa (G), 209 GPa (K), and 2.89 MPa m^1/2 fracture toughness (K_Ic).     

High thermal conductivity silicon nitride ceramics prepared by pressureless sintering with ternary sintering additives

Silicon nitride ceramics were pressureless sintered at low temperature using ternary sintering additives (TiO₂, MgO and Y₂O₃), and the effects of sintering aids on thermal conductivity and mechanical properties were studied. TiO₂–Y₂O₃–MgO sintering additives will react with the surface silica present on the silicon nitride particles to form a low melting temperature liquid phase which allows liquid phase sintering to occur and densification of the Si₃N₄. The highest flexural strength was 791(±20) MPa with 12 wt% additives sintered at 1780°C for 2 hours, comparable to the samples prepared by gas pressure sintering. Fracture toughness of all the specimens was higher than 7.2 MPa·m^1/2 as the sintering temperature was increased to 1810°C. Thermal conductivity was improved by prolonging the dwelling time and adopting the annealing process. The highest thermal conductivity of 74 W/(m∙K) was achieved with 9 wt% sintering additives sintered at 1810°C with 4 hours holding followed by postannealing.     

Preparation,microstructure and mechanical properties of ZrB2–ZrO2 ceramics

ZrB₂–ZrO₂ ceramics with ZrO₂ content varied from 15 to 30 vol.% were prepared by hot pressing. The content of ZrO₂ was found to have an evident effect on the preparation, phase constitution, microstructure as well as the mechanical properties of ZrB₂–ZrO₂ ceramics. ZrB₂–30 vol.% ZrO₂ provided the optimal combination of dense microstructure (2.6 μm, as the average grain size) and excellent properties, including the flexural strength of 803 MPa, and the hardness of 22.7 GPa tested under 9.8 N. The highest t-ZrO₂ transformability of 35.2 vol.% during fracture for ZrB₂–30 vol.% ZrO₂ brought the best toughness of 6.5 MPa m^1/2 compared with any other ceramic. In addition, the dependence of toughness on the test method as well as the hardness on the indentation load was also investigated.     

Fabrication and characterization of porous mullite ceramics with ultra-low shrinkage and high porosity via sol-gel and solid state reaction methods

Porous mullite ceramics with ultra-low shrinkage and high porosity were prepared by solid state reaction between MoO₃ and mullite precursor powders which were synthesized from tetraethylorthosilicate and aluminium nitrate nonahydrate via sol-gel methods. The synthetic process of mullite precursor powder and effects of MoO₃ amount on the phase composition, microstructure, physical properties such as firing shrinkage, open porosity, bending strength, water absorption and bulk density of porous mullite ceramics were investigated. The results indicated that the addition of MoO₃ not only lowered the mullite forming temperature from 985.4 to 853.3 °C, but also restrained densification behavior of samples due to the formation of mullite and Al₂O₃–MoO₃ solid solution, besides, MoO₃ also improves the formability, open porosity and bending strength of samples. The optimal amounts of MoO₃ is 8 wt%, and the resultant samples exhibit outstanding properties, including a low shrinkage rate of 1.86 ± 0.07%, an open porosity of 61.91 ± 0.16% and a bending strength of 9.35 ± 1.11 MPa.     

Tailored pore structures and mechanical properties of porous alumina ceramics prepared with corn cob pore-forming agent

In this work, the effects of porosity and different particle sizes of pore-forming agent on the mechanical properties of porous alumina ceramics have been reported. Different grades of porous alumina ceramics were developed using corn cob (CC) of different weight contents (5, 10, 15, and 20 wt%) and particle sizes (<63 µm, 63-125 µm and 125-250 µm) as the pore-forming agent. Experimental results showed that total porosity and pore cavity size of the porous alumina ceramics increased with rising addition of CC pore former. Total porosity increased with increasing particle size of CC with the Al₂O₃-^<63CC₅ sample exhibiting the lowest total porosity of 41.3 vol% while the highest total porosity of 68.1 vol% was exhibited by the Al₂O₃-^125-250CC₂₀. The particle size effect of CC on the mechanical properties revealed that diametral tensile strength and hardness of the porous alumina ceramics deteriorated with increasing particle size of CC pore former. The Al₂O₃-^<63CC₅ sample exhibited the highest diametral tensile strength and hardness of 25.1 MPa and 768.2 HV, respectively, while Al₂O₃-^125-250CC₂₀ exhibited the lowest values of 1.1 MPa and 35.9 HV. Overall, porous alumina ceramics with the smallest pore sizes under each particle size category exhibited superior mechanical properties in their respective categories.     

Mechanical,tribological and electrical properties of ZrB2 reinforced Cu processed via milling and high-pressure hot pressing

The present work investigates the effect of (0–10 wt%) ZrB₂ reinforcement on densification, mechanical, tribological and electrical properties of Cu. The consolidation of Cu–ZrB₂ samples was carried out using a hot press (temperature: 500 °C, pressure: 500 MPa, time: 30 min, vacuum pressure: 1.3 × 10^-2 mbar). The bulk density of the hot-pressed Cu composites decreased from 8.84 g/cc to 8.16 g/cc and the relative density of samples lowered from 98.6% to 92.1% with the addition of ZrB₂. The incorporation of hard ZrB₂ (up to 10 wt%) improved the hardness of Cu (1.32–2.55 GPa). However, the yield strength and compressive strength of Cu composites increased up to 5 wt% ZrB₂, and further addition of ZrB₂ lowered its strength. The yield strength of Cu samples varied from 602 to 672 MPa and the compressive strength between ~834 and 971 MPa. On the other hand, the coefficient of friction (COF) (from 0.49 to 0.18) and wear rate (from 49.3 × 10^-3 mm³/Nm to 9.1 × 10^-3 mm³/Nm) of Cu–ZrB₂ samples considerably decreased with the addition of ZrB₂. Significantly low wear was observed with Cu-10 wt% ZrB₂ (Cu-10Z) samples, which is 5.41 times less than pure Cu. As far as the wear mechanisms are concerned, in pure Cu, continuous chips (wear debris) were formed during sliding wear by plowing. Whereas the major amount of material loss was occurred due to the plowing mechanism with discontinuous and short chip formation for Cu–ZrB₂ composites. The electrical conductivity of Cu–ZrB₂ samples decreased from 75.7% IACS to 44.1% IACS. In particular, Cu with ZrB₂ (up to 3 wt%) could retain the conductivity of 66.8% IACS. This study reveals that the addition of ZrB₂ (up to 3 wt%) is advantageous to have a good combination of properties for Cu.     

Densification,microstructure and mechanical properties of ZrB2–SiCw ceramic composites

ZrB₂–SiCw composites were prepared through hot-pressing at a low temperature of 1800 °C, and Al₂O₃ plus Y₂O₃ were added as sintering aids. Analysis revealed that additives may react with impurities (i.e. surface oxygen impurities and residual metallic impurities) to form a transient liquid phase, thus promote the sintering and densification of ZrB₂–SiCw composites. The content of additives was found to have a significant influence on the sinterability, microstructure and mechanical properties of ZrB₂–SiCw composites. ZrB₂–SiCw composite prepared with a small amount of additives (3 vol.%) provided the optimal combination of microstructure (relative density of 98.3%) and excellent properties, including flexural strength of 783 MPa and fracture toughness of 6.7 MPa m^1/2. With further addition of additives, SiC whiskers were inclined to gather together and be enveloped by excessive liquids to form core-rim-like structures, which lead to little decrease in mechanical properties.