Synthesis and mechanical properties of mullite ceramics with coal gangue and wastes refractory as raw materials

With coal gangue and high alumina refractory solid wastes as raw materials, needle-like mullite powder, with an average diameter of about 1 μm, was synthesized at 1300°C by using the conventional solid-state reaction method. Mullite ceramics were derived from the inexpensive needle-like powder. Phase composition was examined by using X-ray diffraction (XRD), while morphologies of the ceramics were observed by using scanning electron microscopy. The content and distribution of elements in the sintered samples were characterized with energy dispersive spectrometer and X-ray fluorescence spectroscopy. Mechanical properties of the mullite ceramics were studied by using the three-point bending method. The aspect ratio of the needle-like mullite particles was up to 6. The mullite sample sintered at 1500°C for 3 hours had a density of 2.515 g·cm⁻³, which was slightly lower than the theoretical density. Maximum fracture toughness and bending strength of the mullite ceramics were 1.82 MPa·m^1/2 and 71.76 MPa, respectively. This study realizes the resource utilization of gangue and high alumina refractory solid wastes, and the prepared mullite ceramics have good application prospect.     

Low-temperature synthesis of mullite-based ceramics from Moroccan naturally occurring andalusite and marble waste

The present work aims to prepare mullite-based ceramics at low temperature mainly from andalusite and marble byproduct by a solid-state interaction method. Marble powder byproduct was used, in the prospect of waste management, as a sintering aid. The influence of marble powder byproduct (5 wt.%) on the phase formation, microstructure-temperature evolution, densification, and mechanical strength was evaluated by means of XRD, TGA-DTA, and SEM. The results revealed that the andalusite remained present with mullite up to 1400°C, while the addition of 5 wt.% of marble byproduct involved its complete transformation into mullite and a trace of anorthite. The transformation of andalusite into mullite upon the heating in the range 1300–1400°C involved the densification of the matrix body and a significant increase in mechanical strength from 60 to 170 MPa, which promoted its application for refractory materials.     

Phase formation,microstructure development,and mechanical properties of kaolin-based mullite ceramics added with Fe2O3

The effects of Fe₂O₃ on phase evolution, density, microstructural development, and mechanical properties of mullite ceramics from kaolin and alumina were systematically studied. X-ray diffraction results suggested that the ceramics consisted of mullite, sillimanite, and corundum, in the sintering range of 1450°C–1580°C. However, as the sintering was raised to 1580°C, mullite is the main phase with a content of 94%, and the corundum phase content is 5.9%. Simultaneously, high-temperature sintering had a positive effect on the densification of the mullite ceramics, where both the bulk density and flexural strength could be optimized by adjusting the content of Fe₂O₃. It was found that 6 wt% Fe₂O₃ was optimal for the formation of rod-shaped mullite after sintering at 1550°C for 3 h. The sample's maximum bulk density was 2.84 g/cm³, with a flexural strength of 112 MPa. Meanwhile, rod-shaped mullite grains with an aspect ratio of ~9 were formed. As a result, a dense network structure was developed, thus leading to mullite ceramics with excellent mechanical properties. The effect of Fe₂O₃ on the properties might be attributed to the fact that Al³⁺ ions in the [AlO₆] octahedron were replaced by Fe³⁺ ions, resulting in lattice distortion.     

Mechanical properties of zirconia composite ceramics

Composite materials based on 8 wt% yttria partially stabilized zirconia, with additions of gadolinium zirconate, lanthanum lithium hexaaluminate, yttrium aluminum garnet and strontium zirconate were characterized. Samples were fabricated by hot-press sintering at 1550 °C. The effect of the secondary phase content on the mechanical properties of the composites was evaluated. Hardness, elastic modulus and fracture toughness of the fabricated composites were determined by means of depth-sensitive indentation testing. The fracture toughness of the samples as determined by the indentation method was found to increase with increasing YSZ content, reaching 3 MPa·m^0.5 for samples with 80 wt% YSZ. The fracture toughness appeared to be affected by thermal expansion coefficient mismatch, crack bridging and crack deflection.     

Complex validation of novel mullite-based ceramic filters for microfiltration purposes

The goal of this paper is to investigate a complex validation, developed by Rauschert in Poland, of casted ceramic filters for microfiltration. For disc manufacturing, a self-developed material RaFo-MF-401e with a filtration membrane was used. The presented experiment was conducted on component, subsystem, and system levels. Component level analysis consisted of the investigation of mechanical strength, hardness, rough lifetime, and resistance against acids and alkalis. Annealing at high temperature and humidity was used to test the subsystem. The final system test was executed on the real filtration system. The final aim of the tests was to verify the filtration efficiency of a complete module (core and membrane) in a real filtration device. The filtration quality of the whole setup was very good and the particles in the permeate (filtrated solution) were smaller than 10 μm (defined as D99). Thus, the developed discs provide the expected filtration quality in the range of microfiltration.     

Mechanical properties of nylon-6 after treatment with metal halides

Conditioning of nylon-6 by immersion in metal chloride solutions modifies the mode of deformation under an applied tensile stress. Infra-red spectroscopy of salt-treated films shows significant modification of the spectrum, indicating changes in the intermolecular bonding. Modulus measurements support the hypothesis that modification of the intermolecular bonding in nylon results in some chain stiffening. This stiffening of the network of chains reduces the mobility that is required for shear deformation. This in turn leads to the onset of scission crazing. NaCl, however, spectroscopically shows no evidence for nylon-salt interactions having occurred. The deformation behaviour of both thin-film and bulk samples of NaCl-treated nylon-6 reflect the absence of any salt-amide interaction.     

Effects of sintering aids on microstructure,mechanical, and optical properties of AlON ceramics synthesized by SPS

Aluminum oxynitride (AlON) ceramics doped with different sintering aids were synthesized by spark plasma sintering process. The microstructures, mechanical, and optical properties of the ceramics were investigated. The results indicate that the optimal amount of sintering aids is 0.06 wt% La₂O₃ + 0.16 wt% Y₂O₃ + 0.30 wt% MgO. The addition of La³⁺ and Mg²⁺ decreases the rate of grain boundary migration in ceramics, promotes pore elimination, and inhibits grain growth. The addition of Y³⁺ facilitates liquid-phase sintering of AlON ceramics. Moreover, the addition of Mg²⁺ effectively promotes twin formation in the ceramics, which hinders crack propagation and dislocation motion when the ceramics are loaded. Hence, the AlON ceramic doped with 0.06 wt% La₂O₃ + 0.16 wt% Y₂O₃ + 0.30 wt% MgO exhibits a relative density of 99.95%, an average grain size of 9.42 μm, and a twin boundary content of 10.3%, which contributes to its excellent mechanical and optical properties.     

Microstructures,magnetic, and dielectric properties of Ba-doped BiFeO3 nanoparticles synthesized via molten salt route

As the paradigm of magnetoelectric multiferroic materials, BiFeO₃ (BFO) has potential applications in spintronics, memory devices, sensors, and actuators. However, its large leakage current and small magnetism at room temperature restrict its practical applications. It is demonstrated that the substitutions of Bi by alkali earth elements at A-site of BFO can significantly reduce the leakage current and enhance the remanent magnetization of BFO. In this work, Ba-doped BFO nanoparticles Bi_1-xBa_xFeO₃ (x = 0, 0.05, 0.10, 0.15 and 0.20) were synthesized via molten salt route. X-ray diffraction patterns revealed that with increasing the Ba-doped content the formation of the impurity phase was depressed and the rhombohedral distortions of these nanoparticles were suppressed, as confirmed by Raman spectra. X-ray photoelectron spectroscopy measurements reveal that the Fe element in the nanoparticles exists in the dual valence states of Fe³⁺ and Fe²⁺, and two kinds of oxygen atoms (lattice oxygen atoms and the adsorbed oxygen atoms) exist in the nanoparticles. With increasing the Ba-doped content, the content ratios of Fe³⁺ to Fe²⁺ ions were generally increased, whereas the oxygen vacancy concentrations were decreased. The average particle sizes of the Ba-doped BFO nanoparticles were decreased as compared with that of nondoped BFO nanoparticles. In contrast, the room temperature magnetization of the Ba-doped BFO nanoparticles was greatly enhanced by Ba-substitution, as confirmed by the M-H loops. At room temperature, the remanent magnetization and coercive field of the Bi_0.8Ba_0.2FeO₃ nanoparticles were 0.51 emu/g and 1130 Oe, respectively. Furthermore, the leakage current density was reduced by one order of magnitude at x = 0.2 and the dielectric properties are also improved by Ba-substitution. The improvements on the remanent magnetization, leakage current density as well as dielectric properties of the Ba-doped BFO nanoparticles make them promising candidates for spintronics and dielectric energy storages.     

Mechanical properties of borothermally synthesized zirconium diboride at elevated temperatures

The mechanical properties of a nominally phase pure ZrB₂ ceramic were measured up to 2300°C in an argon atmosphere. ZrB₂ was hot pressed at 2000°C utilizing borothermally synthesized powder from high purity ZrO₂ and B raw materials. The relative density of the ceramics was about 95% with an average ZrB₂ grain size of 8.8 µm. The room temperature flexural strength was 447 MPa, with strength decreasing to 196 MPa at 1800°C, and then increasing to 360 MPa at 2300°C. The strength up to 1800°C was likely controlled by a combination of effects: surface damage from oxidation of the specimens, stress relaxation, and decreases in the elastic modulus. The strength above 1800°C was controlled by flaws in the range consistent with sizes of the maximum ZrB₂ grain size and the largest pores. Fracture toughness was 2.3 MPa·m^1/2 at room temperature, increasing to 3.1 MPa·m^1/2 at 2200°C. The use of higher purity starting materials improved the mechanical behavior in the ultra-high temperature regime compared to previous studies.     

Microwave dielectric properties and crystal structures of Mg0.7Al2.2O4 and Mg0.4Al2.4O4 ceramics with defect structures

Mg_0.7Al_2.2O₄ and Mg_0.4Al_2.4O₄ ceramics with cation vacancies were synthesized using the molten salt method, and the relationships between the microwave dielectric properties and crystal structures of these materials were investigated. The ²⁷Al NMR spectra of these ceramics indicate that the preferential occupation of tetrahedral sites by Al³⁺ cations was enhanced by the introduction of cation vacancies. The λ values of Mg_0.7Al_2.2O₄ and Mg_0.4Al_2.4O₄ ceramics fired at 1600°C, which correspond to the fraction of Al³⁺ cations in tetrahedral sites, were 0.37 and 0.60, respectively. Crystal structure refinements using the Rietveld method suggest that cation vacancies are preferentially located at octahedral sites in both ceramics. The ε_r and Q·f values of a Mg_0.7Al_2.2O₄ ceramic fired at 1600°C were 7.7 and 201 111 GHz, respectively, while those of a Mg_0.4Al_2.4O₄ ceramic fired at 1600°C were 7.5 and 232 301 GHz, respectively. These data demonstrate that the preferential occupation of tetrahedral sites by Al³⁺ cations following the introduction of cation vacancies enhances the Q·f value.     

Comparison of a laboratorial scale synthesized and a commercial yttria-tetragonal zirconia polycrystals ceramics submitted to microwave sintering

Conventional sintering techniques of yttria-tetragonal zirconia polycrystals (Y-TZP) ceramics have presented limitations regarding the sintering time and temperature, increasing the cost of the final dental and biomedical products. Herein, microwave sintering comes to be an interesting alternative by providing fast heating, high densification, and grain-size control. The aim of this study was to compare the effect of microwave sintering of Y-TZP dental ceramics prepared from a pre-sintered commercial block and produced from powders synthesized in a laboratorial scale by the precipitation route. The synthetized and commercial discs were submitted to microwave sintering at 1450°C and 1350°C for 15, 30, and 60 minutes. Densification, fracture toughness, grain size, and crystalline phase quantification of the sintered groups were evaluated. Both synthetized and commercial groups sintered at 1450°C for 15 and 30 minutes showed the higher densification results (98% TD). XRD quantitative phase analysis indicates that samples present 89% tetragonal and 11% cubic phases, except for the group prepared from coprecipitated powders sintered at 1450°C for 30 minutes, that presented 79% and 21% of tetragonal and cubic phases. The microwave sintering at 1450°C allows hardness and fracture toughness values comparable to conventional sintering.     

Mechanical and thermal enhancements of benzoxazine‐based GF composite laminated by in situ reaction with carboxyl functionalized CNTs

An easy and efficient approach by using carboxyl functionalized CNTs (CNT‐COOH) as nano reinforcement was reported to develop advanced thermosetting composite laminates. Benzoxazine containing cyano groups (BA‐ph) grafted with CNTs (CNT‐g‐BA‐ph), obtained from the in situ reaction of BA‐ph and CNT‐COOH, was used as polymer matrix and processed into glass fiber (GF)‐reinforced laminates through hot‐pressed technology. FTIR study confirmed that CNT‐COOH was bonded to BA‐ph matrices. The flexural strength and modulus increased from 450 MPa and 26.4 GPa in BA‐ph laminate to 650 MPa and 28.4 GPa in CNT‐g‐BA‐ph/GF composite, leading to 44 and 7.5% increase, respectively. The SEM image observation indicated that the CNT‐COOH was distributed homogeneously in the matrix, and thus significantly eliminated the resin‐rich regions and free volumes. Besides, the obtained composite laminates showed excellent thermal and thermal‐oxidative stabilities with the onset degradation temperature up to 624°C in N₂ and 522°C in air. This study demonstrated that CNT‐COOH grafted on thermosetting matrices through in situ reaction can lead to obvious mechanical and thermal increments, which provided a new and effective way to design and improve the properties of composite laminates. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Near-net-size preparation of porous mullite matrix ceramics with in situ formed 3D mullite whisker network

Porous mullite matrix ceramics have excellent thermal and mechanical properties suitable for applications such as in thermal insulation. However, their applications are limited by processing defects from nonuniform sintering shrinkage and the trade-off between high porosity (preferred for low thermal conductivity) and high mechanical strength. Herein, we seek to minimize the sintering shrinkage by near-net-size preparation and improve the strength by in situ formed whisker network structure. Gelcasting forming technology and pressureless sintering were used to prepare porous mullite matrix ceramics using kyanite and α-Al₂O₃ powders as the starting materials and using MoO₃ to promote the growth of mullite whiskers. The results showed that the sintering shrinkage could be compensated by the volume expansion from solid-state reaction during reaction sintering. The in situ formed three-dimensional (3D) whisker network further reduced sintering shrinkage and effectively improved the strength of the ceramics. An ultralow sintering shrinkage of .78% was achieved. The near-net-shape porous mullite matrix ceramics strengthened by 3D whisker network had a high porosity of 63.9%, a high compressive strength of 83.8 MPa and a high flexural strength of 53.5 MPa.     

Structure and properties of phenolic resin/nanoclay composites synthesized by in situ polymerization

An in situ semibatch polymerization process for making phenolic resin/montmorillonite clay nanocomposites is developed. It is found that auxiliary mixing in phenol allows intercalation of the monomer and polymer between montmorillonite clay layers. At 2.7% clay by mass the montmorillonite is predominantly exfoliated (fully dispersed). At higher clay loading, a substantial amount of the clay remains in aggregate or intercalated form. When the montmorillonite is exfoliated, the material is mechanically superior. The composite has a tensile modulus that is 21% higher than the neat resin and has 87% improved fracture strength, 100% larger fracture energy, and strain to failure 13% above the pure resin. Thermogravimetric analysis shows the montmorillonite system maintains its thermal stability up to 200°C. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 95: 1169–1174, 2005     

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.     

Properties and microstructural aspects of TiO2‐doped sintered Alumina‐Zirconia composite ceramics

The effect of titania content on the densification, the phase transformation, the microstructures, and mechanical properties of 50 wt% Al₂O₃‐50 wt% ZrO₂ (12 mol% CeO₂) was evaluated. Ceramic composites with different TiO₂ content (0.27, 5, 10 wt%) were prepared by pressureless sintering at low temperature (1400°C) for 2 hours in air. Dense ceramic was obtained by adding 5 wt% of TiO₂ loading to improved mechanical properties. The microstructure analysis provided lots of information about solid‐state reactivity in alumina‐zirconia‐titania ternary system. The content of TiO₂ strongly affected the phases evolution and the grain growth during sintering. Furthermore, a significant effect on mechanical properties and fracture behavior was also observed.     

Mechanical properties of an epoxy resin toughened by polyester

The epoxy resins were toughened by 4–24 phr polyester with average molecular weight 1.9×10⁴ g/mol in this investigation. The mechanical properties were examined and dynamic mechanics analyses were performed for the epoxy resins before and after the modification. The toughening mechanism of polyester to epoxy resin is discussed in light of the scanning electronic microscopy observation of the fracture surfaces. The results showed that the impact strength and tensile strength of the modified epoxy resin were remarkably greater than those of the unmodified cured epoxy resin. The most suitable composition for the modified epoxy resin was the addition of 16 phr polyester, which led to 138 and 46% increments in the impact strength and the tensile strength, respectively. And the mechanical properties depended greatly on the congregating state of polyester added. The polyester dispersing in the epoxy matrix was amorphous when its addition was less than or equal to 12 phr, and was sphere crystals when the addition was over 16 phr. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 90: 3384–3389, 2003     

Effects of holding time on structure and the properties of spodumene/mullite composite ceramics

In this paper, spodumene/mullite ceramics with good thermal shock resistance were prepared from spodumene, quartz, talc, and clay when the sintering temperature was 1270℃. In the sintering process, the effect of holding time on densification, mechanical properties, phase transformation, microstructure, and thermal shock resistance of the composite ceramics were investigated. The phase transition and microstructures of the ceramics were identified via X-ray diffraction (XRD) and scanning electron microscopy (SEM). The interaction between holding time and bulk density was studied by response surface methodology. The result show that an appropriate holding time can improve the mechanical properties of spodumene/mullite ceramics. When the holding time was kept 90 min, the spodumene/mullite ceramics with the apparent porosity was .47%, the bulk density was 2.28 g/cm³, and bending strength was 63.46 MPa. Furthermore, since no cracks formed after 20 thermal shock cycles for the composite ceramics with a bending strength decreasing rate of 12.66%, it is revealed that spodumene/mullite ceramics exhibit good thermal shock resistance. Therefore, this study can provide beneficial guidance for both industrial production and energy conservation.     

Mechanical properties of ZrB2 ceramics determined by two laboratories

The mechanical properties for zirconium diboride (ZrB₂) were measured at two laboratories and compared. Two billets of ZrB₂ were prepared by hot-pressing commercial powder. The relative densities of the billets were >99% and with an average grain size of 5.9 ± 4.5 µm. Both laboratories prepared American Society for Testing and Materials (ASTM) C1161 B-bars for strength and ASTM C1421 bars with notch configuration A for fracture toughness. Specimens were machined by diamond grinding at the Army Research Laboratory (ARL) and electrical discharge machining (EDM) at Missouri S&T. Strength bars tested at Missouri S&T were polished to a .25 μm finish while the bars were tested as-ground at ARL. Strengths were 473 ± 79 MPa for the Missouri S&T bars and 438 ± 68 for the ARL bars while the fracture toughness values were 3.9 ± .7 MPa•m^1/2 for the Missouri S&T bars and 4.4 ± .6 MPa•m^1/2 for the ARL bars. Vickers hardness was measured by both laboratories over a range of indentation loads. The resulting hardness values were on the low end of previously reported values and were quite different from each other especially at indentation loads ≤20N. The study demonstrated that the properties of materials tested to ASTM standards at different laboratories can be compared directly. In addition, strength and fracture toughness were nearly identical for bars prepared by conventional diamond grinding or EDM.     

Mechanical properties of 3D printed polycaprolactone honeycomb structure

Polycaprolactone is well known as a healing agent material in crack self-healing applications but not as a structural material. In this study, the focus is on the durability and energy absorption of honeycomb structure made from polycaprolactone through three-dimensional (3D) printing. The mechanical behavior of honeycomb structures was investigated through in-plane quasi-static compression tests at temperatures of 5 °C, room temperature (22 °C), and 40 °C. Energy absorption efficiency and energy absorption capability at different temperatures and in different loading directions was investigated according to the selected stepping upward stress. The “shape recovery” ratio after compression deformation was calculated. The results reveal that the polymeric honeycomb structure has exceptional repeatability under compressive loads. Specimens with relative density 0.20 showed high energy absorption capability, up to 0.988 J cm⁻³. After the removal of compression loads, specimens recovered up to 80% after the first deformation and up to 70% after the fifth deformation. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46018.