Microstructure and properties of porous anorthite/mullite whiskers ceramics with high porosity

Porous anorthite/mullite whiskers ceramics with high porosity (>91%) and high strength (>0.45 MPa) have been successfully prepared by foam gel-casting method. Effects of extra mullite whiskers on properties including thermal conductivity and compressive strength at different temperatures were investigated and discussed in terms of microstructure observed through SEM and TEM. The results showed that the addition of extra mullite whiskers in certain content could effectively reduce thermal conductivity, improve the compressive strength both at room and high temperature at same time. When the mullite whiskers content was 20 mol%, the porosity was as high as 91.6 ± 0.19%, the thermal conductivity was low to 0.034 ± 0.003 W/(m·K), and the compressive strength at 1000°C was high to 0.64 ± 0.11 MPa three times to the pure one. Small pores, small grains, and more phase interface or grain boundary caused by the addition of extra mullite whiskers were the main factors for low thermal conductivity. Meanwhile, small pores, closely bonded small grains, and the stable three-dimension network formed by mullite whiskers helped to improve strength.     

Preparation and characterization of porous anorthite ceramics from red mud and fly ash

The porous anorthite ceramics with high porosity, good mechanical strength and low heat conductivity were prepared using red mud and fly ash as raw materials via the pore forming method. The effects of sintering temperature and fly ash on phase evolution, densification, compressive strength, thermal conductivity and microstructure of the ceramic materials were investigated. The results showed that the compressive strength of the porous ceramics had an obvious improvement with the increase in fly ash, and the densification and heat conductivity decreased firstly and then increased. In particular, specimen S2 containing 30 wt% red mud and 40 wt% fly ash sintered at 1150°C had the better performances. It had the water absorption of 18.18%, open porosity of 38.52%, bulk density of 1.29 g/cm³, compressive strength of 42.46 MPa, and heat conductivity of 1.24 W/m·K. X-ray diffraction analysis indicated that mullite, anorthite, α-quartz, and diopside ferrian were the dominant phases in the specimens. Scanning electron microscopy micrographs illustrated that plenty of open pores with strip shape and closed pores with axiolitic shape existed in the specimens. Furthermore, the existence of mullite could prevent crack propagation to enhance the energy of inter-granular fracture. It endowed the porous anorthite ceramics with high porosity, good compressive strength, and low heat conductivity.     

Preparation and thermal shock resistance of anorthite solar thermal energy storage ceramics from magnesium slag

Anorthite solar thermal energy storage ceramics were fabricated from magnesium slag solid waste by pressureless sintering. The effects of CaO/SiO₂ ratio and sintering temperature on the physical, chemical, and thermophysical properties of ceramics were explored. X-ray diffraction results demonstrated that thermal shock process contributed to the formation of anorthite, and increasing CaO/SiO₂ ratio promoted the transformation of anorthite (CAS₂) into melilite (C₂AS). Some micro-cracks were found according to SEM analysis, forming by the mismatch of thermal expansion coefficients among phases. The combined effects of the low thermal expansion coefficient of anorthite and micro-crack toughing endowed the ceramic with good thermal shock resistance. Optimum comprehensive performances were observed in the sample with a CaO/SiO₂ ratio of 0.58 sintered at 1160°C, of which the specific thermal storage capacity was 0.63 J·g^-1·°C^-1(room temperature). The bending strength increased by 0.22% after 30 thermal shock times (room temperature-800°C, wind cooling). Therefore, the anorthite ceramics exhibited great potential for solar thermal energy storage.     

Effect of CaO/SiO2 ratio on phase transformation and properties of anorthite-based ceramics from coal fly ash and steel slag

Anorthite-based ceramics were produced entirely from coal fly ash and steel slag. The effect of the CaO/SiO₂ ratio (0.12–0.8) on the phase transitions was examined by adding steel slag to coal fly ash in the range of 10–50 wt%, and a temperature range of 900–1200 °C. The influence of CaO/SiO₂ and sintering temperatures on the technological properties were assessed by response surface methodology (RSM) and correlated with the phase changes. The results revealed that anorthite was the main phase for the CaO/SiO₂ ratio ranging from 0.12 to 0.56, while at 1200 °C, a ratio of 0.8 involved a high content of gehlenite. RSM showed that the CaO/SiO₂ ratio was the main influencing factor on the density, while the variation of apparent porosity and compressive strength were more affected by sintering temperature. The crystallisation of the anorthite phase significantly enhanced the properties of the obtained ceramics, whereas the appearance of gehlenite reduced the mechanical strength. The optimum conditions to fabricate anorthite-based ceramics with suitable properties were found to be a CaO/SiO₂ ratio of 0.46 and a temperature of 1188 °C. The optimised anorthite-based ceramic exhibited a low thermal conductivity (0.39 W/m.K) and a dielectric constant of 6.03 at 1 MHz, along with a compressive strength of 41 MPa, which makes this sample a potential candidate for insulator applications.     

Carbothermal reduction synthesis of high porosity and low thermal conductivity ZrC-SiC ceramics via an one-step sintering technique

In this work, porous ZrC-SiC ceramics with high porosity and low thermal conductivity were successfully prepared using zircon (ZrSiO₄) and carbon black as material precursors via a facile one-step sintering approach combining in-situ carbothermal reduction reaction (at 1600 °C for 2 h) and partial hot-pressing sintering technique (at 1900 °C for 1 h). Carbon black not only served as a reducing agent, but also performed as a pore-foaming agent for synthesizing porous ZrC-SiC ceramics. The prepared porous ZrC-SiC ceramics with homogeneous microstructure (with grain size in the 50–1000 nm range and pore size in the 0.2–4 µm range) possessed high porosity of 61.37–70.78%, relatively high compressive strength of 1.31–7.48 MPa, and low room temperature thermal conductivity of 1.48–4.90 W·m^?1K^?1. The fabricated porous ZrC-SiC ceramics with higher strength and lower thermal conductivity can be used as a promising light-weight thermal insulation material.     

Processing and properties of silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity

Silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity were prepared by sintering nano-SiC powder-carbon black template compacts at 600–1200 °C for 2 h in air. The microstructure of the silica-bonded porous nano-SiC ceramics consisted of SiC core/silica shell particles, a silica bonding phase, and hierarchical (meso/macro) pores. The porosity and thermal conductivity of the silica-bonded porous nano-SiC ceramics can be controlled in the ranges of 8.5–70.2 % and 0.057–2.575 Wm⁻¹ K⁻¹, respectively, by adjusting both, the sintering temperature and template content. Silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity (0.057 Wm⁻¹ K⁻¹) were developed at a very low processing temperature (600 °C). The typical porosity, average pore size, compressive strength, and specific compressive strength of the porous nano-SiC ceramics were ∼70 %, 50 nm, 2.5 MPa, and 2.7 MPa·cm³/g, respectively. The silica-bonded porous nano-SiC ceramics were thermally stable up to 1000 °C in both air and argon atmospheres.     

Investigation of the thermal shrink mechanism,thermal conductivity and compressive resistance of TaTiP3O12 ceramics

Dense TaTiP₃O₁₂ ceramics were synthesized by the solid-state method and spark plasma sintering (SPS) with 6 wt% V₂O₅ as a sintering aid, and their phase, microstructure, thermal conductivity, hardness, compressive strength, and expansion property and mechanism were investigated. Results show that the pure phase can be achieved by the two methods. In particular, the sample prepared by SPS possesses a relative density of 97.62% and a porosity of 3.07%, and has better properties than that prepared by the solid-state method. The SPS sample has a thermal conductivity at room temperature of 2.03 w/(m· °C), a Vickers hardness of 4.34 GPa and a compressive strength of 175.98 MPa, which are 0.95, 1.49 and 1.59 times greater than those of the sample prepared by the solid-state method, respectively. In addition, the TaTiP₃O₁₂ ceramic prepared by SPS exhibits a linear ultralow negative thermal expansion property with a coefficient of thermal expansion of ?0.74 × 10^?6 °C ^?1 (-100–400 °C). The negative thermal expansion in TaTiP₃O₁₂ is induced by the coupling effect of [Ta(Ti)O₆] octahedron and [PO₄] tetrahedron caused by the transverse vibration of bridging oxygen atoms.     

Thermal shock behavior of co-continuous TiCx-Cu cermets in air and anaerobic environment

The present work investigated the microstructure and mechanical properties of TiC_x-Cu cermets before and after thermal shock tests. Thermal shock temperature was from 800 °C to 1200 °C and number of cycles was from 1 to 20. The results indicated that TiC_x-Cu cermets with co-continuous structure exhibited a stable and excellent thermal shock resistance. When quenched at 1000 °C for 1 cycle, the residual flexural strength of the cermet increased to 882 MPa, which was 10.1% higher than that without thermal shock. After 20 cycles of thermal shock, the residual flexural strength still maintain 760 MPa. When quenched at 800 °C and 1200 °C, the strengths of cermet decreased correspondingly, which were caused by the thermal mismatch between metal and ceramics and effusion of Cu or collapses of oxide layer, respectively. Herein, the recrystallization and refinement of metal phase grains caused during the thermal shock process, resulting in the superior thermal shock performance of cermet.     

Preparation of Porous Mullite Ceramics Using Fly Ash Cenosphere as a Pore‐Forming Agent by Gelcasting Process

Porous mullite ceramics were fabricated from an industrial grade mullite powder by gelcasting process using fly ash cenospheres (FAC) as a pore‐forming agent. The influence of content of FAC and sintering temperature on the density and strength was evaluated. The microstructure showed that FAC can act as a sintering aid and a pore‐forming agent. When the sintering temperature at 1200°C, porous mullite ceramics with a relatively high porosity (48.1–72.2%), low density (0.84–1.64 g/cm³), low thermal conductivity (0.16–0.22 W/m · K), and high compressive strength (6.21–14.70 MPa) have been obtained.     

Experimental study on foam glass prepared by hydrothermal hot pressing-calcination technique using waste glass and fly ash

Foam glass is a lightweight and high-strength building and decoration material with superior performance in heat insulation, sound absorption, moisture resistance and fire protection. The use of waste glass powder and fly ash to prepare foam glass is one of the most important ways to utilize solid waste as a resource. In this study, waste glass powder and fly ash were used as raw materials to prepare foam glass by a hydrothermal hot pressing–calcination method. The effects of fly ash content (0 wt%, 10 wt%, 20 wt%, 30 wt%), heating rate (1 °C/min, 3 °C/min, 5 °C/min, 8 °C/min, 10 °C/min) and calcination temperature (600 °C, 700 °C, 750 °C, 800 °C, 850 °C, 900 °C) on the microscopic morphology, density, compressive strength, porosity and other properties of the foam glass samples were studied. Their microstructure and morphology were analyzed by thermogravimetric analysis–mass spectrometry, X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. At a fly ash content of 10 wt%, the heating rate was 5 °C/min, the calcination temperature was 800 °C, the foam glass density was 0.3 g/cm³, the compressive strength was 1.65 MPa, the total porosity was 75.5%, and the effective thermal conductivity was 0.206 W/m·K. The effective thermal conductivity models of the composite materials were used to verify the experimental data. The relationship between the thermal conductivity of foam glass materials and the related influencing factors was investigated.     

Novel SiC/C composite targets for the production of radioisotopes for nuclear applications

A partially porous SiC ceramic, reinforced with 30 vol% short carbon fibers, was hot pressed and characterized as potential ISOL target for nuclear applications. Powder milling and hot pressing were effective for the realization of a ceramic with about 40% interconnected porosity in the 0.6–0.8 µm size range. A fiber-free porous SiC material was also synthesized for the sake of comparison. Compression strength of the fiber-rich SiC passed from about 200 MPa at room temperature to about 120 MPa upon testing at 1200 °C. The thermal conductivity was higher than the fiber-free SiC and other state-of-art ISOL target materials and was 48 W/m·K at 600 °C and decreased to 17 W/m·K at 1400 °C, owing to the porosity. Remarkably, this fiber-rich ceramic in form of thin disk, possessed suitable thermo-mechanical behavior to successfully withstand a 350 °C thermal gradient without failure.     

Carbon nanotube/graphene oxide‐added CaO‐B2O3‐SiO2 glass/Al2O3 composite as substrate for chip‐type supercapacitor

A CaO‐B₂O₃‐SiO₂ (CBS) glass/40 wt% Al₂O₃ composite sintered at 900°C exhibited a dense microstructure with a low porosity of 0.21%. This composite contained Al₂O₃ and anorthite phases, but pure glass sintered at 900°C has small quantities of wollastonite and diopside phases. This composite was measured to have a high bending strength of 323 MPa and thermal conductivity of 3.75 W/(mK). The thermal conductivity increased when the composite was annealed at 850°C after sintering at 900°C, because of the increase in the amount of the anorthite phase. 0.25 wt% graphene oxide and 0.75 wt% multi‐wall carbon nanotubes were added to the CBS/40 wt% Al₂O₃ composite to further enhance the thermal conductivity and bending strength. The specimen sintered at 900°C and subsequently annealed at 850°C exhibited a large bending strength of 420 MPa and thermal conductivity of 5.51 W/(mK), indicating that it would be a highly effective substrate for a chip‐type supercapacitor.     

Preparation and performance study of cordierite/mullite composite ceramics for solar thermal energy storage

The employment of solar energy in recent years has reached a remarkable edge. It has become even more popular as the cost of fossil fuel continues to rise. Energy storage system improves an adjustability and marketability of solar thermal and allowing it to produce electricity in demand. This study attempted to prepare cordierite/mullite composite ceramics used as solar thermal storage material from calcined bauxite, talcum, soda feldspar, potassium feldspar, quartz, and mullite. The thermal physical performances were evaluated and characterized by XRD, SEM, EPMA, and EDS. It was found that the optimum sintering temperature was 1280°C for preparing, and the corresponding water adsorption was 11.25%, apparent porosity was 23.59%, bulk density was 2.10 mg·cm^?3, bending strength was 88.52 MPa. The residual bending strength of specimen sintered at 1280°C after thermal shock of 30 times decreased to be 57 MPa that was 36% lower than that before. The thermal conductivity of samples sintered at 1280°C was tested to be 2.20 W·(m·K)^?1 (26°C), and after wrapped a PCM (phase change materials) of K₂SO₄, the thermal storage density was 933 kJ·kg^?1 with the temperature difference (ΔT) ranged in 0‐800°C. The prepared cordierite/mullite composite ceramic was proved to be a promising material for solar thermal energy storage.     

SiC junction enhanced carbon nanofiber aerogels with extremely high specific strength and ultra-low thermal conductivity

C/SiC aerogels with both ultra-low thermal conductivity and extremely high strength were fabricated by freeze casting. SiC junctions originated from pyrolysis of polycarbosilane (PCS) were formed between carbon nanofibers (C_f) to enhance the strength of aerogels. The effects of PCS content and total solid content on the phase composition, pore structure, thermal conductivity and compressive property were studied. The fabricated aerogels possess hierarchical pore structure. In the micro-scale, it contains circular pores with size of about 15 µm, while it is mesoporous and macroporous in the nano-scale. Both thermal conductivity and compressive strength increase with the increase in PCS content. Through tailoring PCS content and total solid content, C_f/SiC aerogels with porosity of 99.5%, thermal conductivity of 33 mW·m⁻¹·K⁻¹ and compressive strength of 7.14 MPa can be obtained. The specific strength of the fabricated C_f/SiC aerogels is up to 467.6 MPa/(g/cm³), which is the highest value for ceramic aerogels.     

Seed assisted in-situ synthesis of porous anorthite/mullite whisker ceramics by foam-freeze casting

Porous anorthite/mullite whisker ceramics with both high strength and low thermal conductivity have been successfully prepared by combining seed-assisted in situ synthesis and foam-freeze casting techniques. The addition of mullite seed was conducive to a reduction in the sintering shrinkage, pore size, and anorthite grain size. This increased the high aspect ratio of mullite whiskers, which enhanced the strength and diminished the thermal conductivity. Mullite whiskers overlapped to form a stable three-dimensional network structure similar to the bird's nest, which was also beneficial to heighten the mechanical properties of the prepared porous ceramics. Through this method, the prepared materials had a high apparent porosity of 87.7–90.2%, a low bulk density of 0.29–0.36 g/cm³, a high compressive strength of 0.65–3.31 MPa, and low thermal conductivity of 0.067–0.112 W/m·K. The results indicated that the method described here can fabricate porous ceramics with excellent properties for further thermal insulating applications.     

Microstructural evolution and sintering properties of palygorskite nanofibers

In this study, the morphological evolution and sintering properties of the palygorskite nanofibers were studied along with the increase of temperature, using raw palygorskite as materials. The palygorskite powder was calcined at different temperatures in the range of 100°C-1200°C, and the microstructural evolution of the palygorskite nanofibers was investigated by thermogravimetric and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscope (HRTEM). Furthermore, the palygorskite powder was shaped to bars by dry pressing and sintered from 700°C to 1200°C. The properties of the sintered palygorskite were characterized by bending strength, mercury intrusion porosimeter (MIP), and stepwise isothermal dilatometry (SID). The results showed that the morphology of palygorskite nanofibers maintained unchanged till 1000°C. The palygorskite nanofibers molted to bind each other and formed a solid interwoven network structure at 1100°C. Correspondingly, it was shown from the sharply decrease of the sintered palygorskite porosity from 45.46% at 1000°C to 1.82% at 1100°C that the dense sintering of palygorskite started at 1100°C. With the sintering proceeding, some closed micropores fused each other to form bigger opening pores, resulting in a slight increase of porosity at 1200°C. However, the pore size distribution got more uniform and the density of the sintered body increased. So the bending strength of the sintered body reached the maximum of 176.67 Mpa and finally the main crystalline phases of the sintered sample changed to quartz, enstatite, and kyanite. The sintering activation energy of the palygorskite was measured by means of SID with a value of 906.46 kJ·mol⁻¹.     

Low sintering shrinkage porous mullite ceramics with high strength and low thermal conductivity via foam-gelcasting

Excessive sintering shrinkage leads to severe deformation and cracking, affecting the microstructure and properties of porous ceramics. Therefore, reducing sintering shrinkage and achieving near-net-size forming is one of the effective ways to prepare high-performance porous ceramics. Herein, low-shrinkage porous mullite ceramics were prepared by foam-gelcasting using kyanite as raw material and aluminum fluoride (AlF₃) as additive, through volume expansion from phase transition and gas generated from the reaction. The effects of AlF₃ content on the shrinkage, porosity, compressive strength, and thermal conductivity of mullite-based porous ceramics were investigated. The results showed that with the increase of content, the sintering shrinkage decreased, the porosity increased, and mullite whiskers were produced. Porous mullite ceramics with 30 wt% AlF₃ content exhibited a whisker structure with the lowest shrinkage of 3.5%, porosity of 85.2%, compressive strength of 3.06 ± 0.51 MPa, and thermal conductivity of 0.23 W/(m·K) at room temperature. The temperature difference between the front and back sides of the sample reached 710°C under high temperature fire resistance test. The low sintering shrinkage preparation process effectively reduces the subsequent processing cost, which is significant for the preparation of high-performance porous ceramics.     

Controllable preparation of porous ZrB2–SiC ceramics via using KCl space holders

In this work, a novel and facile technique based on using KCl as space holders, along with partial sintering (at 1900 °C for 30 min), was explored to prepare porous ZrB₂–SiC ceramics with controllable pore structure, tunable compressive strength and thermal conductivity. The as-prepared porous ZrB₂–SiC samples possess high porosity of 45–67%, low average pore size of 3–7 μm, high compressive strength of 32–106 MPa, and low room temperature thermal conductivity of 13–34 W m⁻¹ K⁻¹. The porosity, pore structure, compressive strength and thermal conductivity of porous ZrB₂–SiC ceramics can be tuned simply by changing KCl content and its particle size. The effect of porosity and pore structure on the thermal conductivity of as-prepared porous ZrB₂–SiC ceramics was examined and found to be consistent with the classical model for porous materials. The poring mechanism of porous ZrB₂–SiC samples via adding pore-forming agent combined with partial sintering was also preliminary illustrated.     

Fabrication and properties of porous anorthite/mullite ceramics with both high porosity and high strength

Porous anorthite/mullite ceramics with both high porosity and high strength have been successfully fabricated by foam-gelcasting and pressureless sintering technology, using α-Al₂O₃, SiO₂, and CaCO₃ as starting materials and MnO₂ as sintering aids. The porous mullite ceramics prepared in this study had 83.3% porosity and 0.3 W/m·K thermal conductivity, exhibited compressive strength value as high as 6.1 MPa. The samples fabricated with mullite content of 30 mol% possessed 79.4% porosity and 5.9 MPa compressive strength showed thermal conductivity as low as 0.19 W/m·K. With the addition of MnO₂, the properties of the prepared materials varied slightly when mullite content changed in a large scale. The results showed that the addition of MnO₂ promoted the reaction, affected sintering and grain growth, and contributed to high strength and low-thermal conductivity.     

Sintering behaviors and properties of porous ceramics derived from artificially cultured diatom frustules

Bimodal porous ceramics with high strength have been fabricated by conventional powder metallurgy utilizing artificially cultured diatom frustules (DFs). The effect of sintering temperature on thermal behaviors, phase transition, and pore structures features of DFs-based porous ceramics is investigated between 800 and 1200°C. The phase evolution of DFs powders is investigated with thermal analysis (DIL and DSC-TG). Phase transition behaviors analyzed with XRD, Raman, and FT-IR spectra confirm the transformation of quartz into cristobalite phases occurs under 1050°C. Sintering under 950°C could bind DFs powders tightly into high strength porous ceramics while maintain the multilayer pore structures simultaneously, having porosity of 56.4%, compressive strength of 15.0 MPa and surface area of 50.9 m²/g, respectively. Slit-shaped microstructures and mesopores (2-50 nm) are observed in DFs-based porous ceramics sintered under 1050°C. Collapse and blockage of pore structures as well as partial fusion of DFs particles happened at the temperature of 1100°C, indicating the presence of diminished multilayers and particle agglomeration.