Effect of LiAlSiO4 particle size on the properties of LAS/SiC porous ceramics with near zero thermal expansion

Near zero thermal expansion porous ceramics were fabricated by using SiC and LiAlSiO₄ as positive and negative thermal expansion materials, respectively, bonded by glassy material. The microstructure, mechanical properties, and thermal expansion behavior of LAS/SiC porous ceramics with different particle sizes of LiAlSiO₄ were investigated. The results indicated that the coefficient of thermal expansion of the LAS/SiC porous ceramics decreased from 0.5206×10⁻⁶ to −1.1053×10⁻⁶ K⁻¹ with increasing the LiAlSiO₄ particle size from ~45 µm to ~125 μm. It was attributed to the reduction in the reaction between LiAlSiO₄ and SiO₂ as the particle size of LiAlSiO₄ increased. Young’s modulus increased from 36 MPa to 54 MPa as the sintering temperature increased from 850 °C to 950 °C because of the good bonding between the SiC grains and the glass materials.     

Biomorphic silicon/silicon carbide ceramics from birch powder

A novel process has been developed for the fabrication of biomorphic silicon/silicon carbide (Si/SiC) ceramics from birch powder. Fine birch powder was hot-pressed to obtain pre-templates, which were subsequently carbonized to acquire carbon templates, and these were then converted into biomorphic Si/SiC ceramics by liquid silicon infiltration at 1550 °C. The prepared ceramics are characterized by homogeneous microstructure, high density, and superior mechanical properties compared to biomorphic Si/SiC ceramics from birch blocks. Their maximum density has been measured as 3.01 g/cm³. The microstructure is similar to that of conventional reaction-bonded silicon carbide. The Vicker's hardness, flexural strength, elastic modulus, and fracture toughness of the biomorphic Si/SiC were 19.6 ± 2.2 GPa, 388 ± 36 MPa, 364 ± 22 GPa, and 3.5 ± 0.3 MPa m^1/2, respectively. The outstanding mechanical properties of the biomorphic Si/SiC ceramics are assessed to derive from the improved uniform microstructure of the pre-templates made from birch powder.     

Effects of the initial α-SiC content on the microstructure, mechanical properties, and permeability of macroporous silicon carbide ceramics

By using α- and/or β-SiC staring powders, the effects of the initial α-phase content on the microstructure, mechanical properties, and permeability of macroporous SiC ceramics were investigated. When β-SiC powder or a mixture of α/β powders containing a small amount (≤10%) of α-SiC powder was used, the microstructure consisted of large platelet grains. In contrast, when using α-SiC powder or α/β powders containing a large amount (>10%) of α powders, the microstructure consisted of small equiaxed grains. The development of large α-SiC platelet grains in the microstructure did not result in any improvement of the flexural strength of the macroporous SiC ceramics because of the accompanying pore growth and grain growth. The growth of the platelet-SiC grains was beneficial in increasing the gas permeability of the macroporous SiC ceramics from 4.12 × 10⁻¹³ m² for macroporous SiC with an equiaxed microstructure to 1.89 × 10⁻¹² m² for macroporous SiC ceramics with large platelet grains.     

Preparation of SiC nanowires-filled cellular SiCO ceramics from polymeric precursor

SiC nanowires-filled cellular SiCO ceramics were prepared using polyurethane sponge as a porous template infiltrated with silicone resin by pyrolysis at 1400 °C under Ar atmosphere. The pyrolysis temperature was an important parameter affecting the formation of SiC nanowires. The as-prepared sample obtained at 1000 °C was composed of SiCO glasses and turbostratic carbon. The SiCO ceramic was further converted into SiO₂ crystals and amorphous carbon by pyrolysis at 1200 °C. With the increasing pyrolysis temperature, SiC nanocrystals embedded in the non-crystalline SiCO matrix were observed. Furthermore, the SiC nanowires were formed in the pores of the SiCO ceramic. The diameters of the SiC nanowires are in the range 80–150 nm and the lengths are up to several tens of micrometers. The growth mechanism of the nanowires was supported by the vapor-solid mechanism.     

聚碳硅烷粘结法低温制备碳化硅多孔陶瓷

分别以平均粒径为10μm和20μm的两种规格碳化硅(SiC)粉末为原料、聚碳硅烷(PCS)为粘结剂,通过包混、过筛、模压成型、1000℃热解等工序制备了SiC多孔陶瓷,研究了PCS含量对SiC多孔陶瓷微观形貌、线收缩率、孔隙率与抗弯强度的影响,并对两种规格粉末制备的SiC多孔陶瓷性能进行了对比。结果表明:随着PCS含量的增加,两种规格粉末制备的SiC多孔陶瓷微观形貌都逐渐变得致密,当PCS含量为13%时,两种规格粉末制备的多孔陶瓷都出现了微观裂纹。随着PCS含量的增加,两种规格粉末制备的SiC多孔陶瓷孔隙率都逐渐降低,线收缩率都逐渐增大,抗弯强度先增大后降低,在PCS含量为10%时,平均粒径为10μm与20μm的SiC粉末制备的多孔陶瓷抗弯强度取得最大值,分别为31.6MPa与29.0MPa。     

Tough organogels based on polyisobutylene with aligned porous structures

Macroporous gels with aligned porous structures were prepared by solution crosslinking of butyl rubber (PIB) in cyclohexane at subzero temperatures. Sulfur monochloride was used as a crosslinker in the organogel preparation. The reactions were carried out at various temperatures between 20 and −22 °C as well as at various freezing rates. The structure of the gel networks formed at −2 °C consists of pores of about 100 μm in length and 50 μm in width, separated by polymer domains of 10-20 μm in thickness. The aligned porous structure of PIB gels indicates directional freezing of the solvent crystals in the direction of the temperature gradient. The size of the pores in the organogels could be regulated by changing the freezing rate of the reaction solution. The results suggest that frozen cyclohexane templates are responsible for the porosity formation in cyclohexane. In contrast to the regular morphology of the gels formed in cyclohexane, benzene as a crosslinking solvent produces irregular pores with a broad size distribution from micrometer to millimeter sizes due to the phase separation of PIB chains at low temperatures. Macroporous organogels prepared at subzero temperatures are very tough and can be compressed up to about 100% strain without any crack development. The gels also exhibit superfast swelling and deswelling properties as well as reversible swelling-deswelling cycles in toluene and methanol, respectively.     

Fabrication of CaSiO3 bioceramics with open and unidirectional macro-channels using an ice/fiber-templated method

Porous CaSiO₃ bioceramics with open and unidirectional macro-channels of pore size more than 200 μm are of particular interest for biomedical applications. An ice/fiber-templated method was employed for the fabrication of CaSiO₃ bioceramics with interconnected lamellar pores and macro-channels of pore size more than 200 μm. The pores formed by ice crystals transformed from cellular to lamellar, while the pores formed by fibers were aligned macro-channels, which were also in alignment with the lamellar pores. Keeping the initial slurry concentration constant and increasing the packing density of fibers, the volume fraction of macro-channels and open porosity increased, and the compressive strength decreased. Maintaining the packing density of fibers and increasing the initial slurry concentration, the pore sizes of lamellar pores and open porosity decreased, and the compressive strength increased. The results indicated that it was possible to manufacture porous CaSiO₃ bioceramics with the macro-channels of 250–350 μm, lamellae spacing of 50–100 μm, open porosity of 71.12–83.94% and compressive strength of 0.87–3.59 MPa, indicating the suitability for tissue engineering.     

Influence of β-Si3N4 particle size and heat treatment on microstructural evolution of α:β-SiAlON ceramics

In the present study, we report the effects of starting β-Si₃N₄ particle sizes and post-sintering heat treatment on microstructure evolution and mechanical properties of prepared α-β SiAlON ceramics. Three different β-Si₃N₄ starting powders, with particle sizes of 2, 1 and 0.5 μm were used to prepare α-β SiAlON ceramics by gas-pressure sintering. Elongated β-SiAlON grain morphology was identified in the samples prepared using 0.5 μm particle size β-Si₃N₄ powder. Low-aspect ratio grain morphology was observed in samples prepared from starting powders with coarse particles (2 μm and 1 μm). The sintered samples were further heat treated to develop desired microstructure with elongated grains. The hardness and indentation fracture toughness values of sintered and heat treated samples were found to lie in the range of 12.4-14.2 GPa and 5.1-6.4 MPa m^1/2 respectively. It was revealed that fracture toughness increases with decrease in particle size of starting β-Si₃N₄ powder.     

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.     

Mechanical properties of sintered ZrB2-SiC ceramics

ZrB₂ ceramics containing 10-30 vol% SiC were pressurelessly sintered to near full density (relative density >97%). The effects of carbon content, SiC volume fraction and SiC starting particle size on the mechanical properties were evaluated. Microstructure analysis indicated that higher levels of carbon additions (10 wt% based on SiC content) resulted in excess carbon at the grain boundaries, which decreased flexure strength. Elastic modulus, hardness, flexure strength and fracture toughness values all increased with increasing SiC content for compositions with 5 wt% carbon. Reducing the size of the starting SiC particles decreased the ZrB₂ grain size and changed the morphology of the final SiC grains from equiaxed to whisker-like, also affecting the flexure strength. The ceramics prepared from middle starting powder with an equiaxed SiC grain morphology had the highest flexure strength (600 MPa) compared with ceramics prepared from finer or coarser SiC powders.     

Formation of porous glass via core/shell-structured poly(methyl methacrylate)/powder glass prepared by ultrasonic irradiation in liquid CO2

The formation of porous glass ceramic via core/shell-structured poly(methyl methacrylate)(PMMA)/powder glass was investigated. Core/shell structures were prepared via ultrasonic irradiation in high-pressure liquid carbon dioxide (CO₂) using PMMA microspheres as the core material and glass powder as the shell material. The mean particles sizes of PMMA template microspheres and glass powder were 9.8 μm and 0.9 μm, respectively. After removal of the PMMA template by calcination in air, porous glass was obtained. The products were characterized by scanning electronic microscopy (SEM) and thermogravimetric-differential thermal analysis (TG-DTA). The average pore diameter of porous glass was 4.3 μm. Compared with porous glass prepared by the other method, the porous glass prepared by ultrasonic irradiation of liquid CO₂ was achieved the narrow pore size distribution (CV = 35%) and the higher porosity (89%). The pores are not isolated and connected each other. Furthermore, the effects of experimental conditions, such as coating method, crosslink density of the template PMMA microspheres, ultrasonic intensity and calcination temperature, on the product morphology were investigated. The higher ultrasound intensity achieved the uniform coating of PMMA templates with powder glass. The calcination temperature and crosslinked density of PMMA template microspheres affect the pore structure.     

Fabrication of Sn doped Ba(Mg1/3Ta2/3)O3 transparent ceramics by a solid state reaction method

Transparent disordered BMT ceramics were obtained by solid state reaction. Sn⁴⁺ ions were incorporated to make the B site of the perovskite structure disordered. The stoichiometric powder mixture with and without Sn doping was calcinated at 1300 °C, respectively and they were both characterized. After dry pressing, the pellets with Sn doping were sintered at 1600 °C in oxygen atmosphere for 4 h. The grain size of the transparent ceramics is around 12 μm. No pores were detected in or among the grains. The inline transmittance of the material is 66% at 580 nm. The refractive index is 2.09 at 1600 nm.     

Erosion behavior of SiC–WC composites

Dense silicon carbide (SiC) ceramics were prepared with 0, 10, 30 or 50 wt% WC particles by hot pressing powder mixtures of SiC, WC and oxide additives at 1800 °C for 1 h under a pressure of 40 MPa in an Ar atmosphere. Effects of alumina or SiC erodent particles and the WC content on the erosion performance of sintered SiC–WC composites were assessed. Microstructures of the sintered composites consisted of WC particles distributed in the equi-axed grain structure of SiC. Fracture surfaces showed a mixed mode of fracture, with a large extent of transgranular fracture observed in SiC ceramics prepared with 30 wt% WC. Crack bridging by WC enhanced toughening of the SiC ceramics. A maximum fracture toughness of 6.7 MPa*m^1/2 was observed for the SiC ceramics with 50 wt% WC, whereas a high hardness of 26 GPa was obtained for the SiC ceramics with 30 wt% WC. When eroded at normal incidence, two orders of magnitude less erosion occurred when SiC–WC composites were eroded by alumina particles than that eroded by SiC particles. The erosion rate of the composites increased with increasing angle of SiC particle impingement from 30° to 90°, and decreased with WC reinforcement up to 30 wt%. A minimum erosion wear rate of 6.6 mm³/kg was obtained for SiC–30 wt% WC composites. Effects of mechanical properties and microstructure on erosion of the sintered SiC–WC composites are discussed, and the dominant wear mechanisms are also elucidated.     

Foaming strategies for bioabsorbable polymers in supercritical fluid mixtures. Part II. Foaming of poly(?-caprolactone-co-lactide) in carbon dioxide and carbon dioxide + acetone fluid mixtures and formation of tubular foams via solution extrusion

This paper reports on the foaming of poly(?-caprolactone-co-lactide) in carbon dioxide and carbon dioxide + acetone mixtures. Experiments were carried out in specially designed molds with porous metal surfaces and fluid circulation features to generate foams with uniform dimensions at 60, 70 and 80 °C at pressures in the range 7-28 MPa. Depending upon the conditions, foams with pores in the range from 5 to 200 μm were generated. Adding acetone to carbon dioxide improved the uniformity of the pores compared to foams formed by carbon dioxide alone. In addition, a unique high-pressure solution extrusion system was designed and used to form porous tubular constructs by piston-extrusion of a solution from a high-pressure dissolution chamber through an annular die into a second chamber maintained at controlled pressure/temperature and fluid conditions. Long uniform porous tubular constructs with 6 mm ID and 1 mm wall thickness were generated with glassy polymers like poly(methyl methacrylate) by extruding solutions composed of 50 wt% polymer + 50 wt% acetone, or 25 wt% polymer + 10% acetone + 65% carbon dioxide at 70 °C and 28 MPa. Pores were in the 50 μm range. The feasibility of forming similar tubular constructs were demonstrated with poly(?-caprolactone-co-lactide) as well. Tubular foams of the copolymer with interconnected pores with pore sizes in the 50 μm range were generated by extrusion of the copolymer solution composed of 25 wt% polymer + 10 wt% acetone + 65 wt% carbon dioxide at 70 °C and 28 MPa. Reducing the acetone content in the solution led to a reduction of pore sizes. Comparisons with the foaming behavior of the homopolymer poly(?-caprolactone) that were carried out in the molds with porous metal plates show that the foaming behavior of the copolymer is more akin to the foaming behavior of the caprolactone homopolymer component.     

Dielectric properties of barium titanate ceramics with different materials powder size

The dielectric properties of barium titanium ceramics fabricated with nano-size fine powders (about 40 nm) are compared with that fabricated with micro-size coarse powders (about 2 μm). Three kinds of ceramics were fabricated; one using pure nano-size fine powders, the other using pure micro-size coarse powders, and the third using the combination of both. The sintering temperature of the ceramics with pure nano-size fine powders is 150 °C lower than that with pure micro-size coarse powders. For the same sintering conditions, the relative density of the ceramics is increases with the amount of nano-size fine powders. The grain size of the ceramics body with pure micro-size coarse powder is about 5 μm, but that of pure nano-size fine powder is about 1 μm. The room temperature dielectric constant of the ceramics increases with the increasing of the amount of nano-size fine powder. For pure nano-size fine powders, the room temperature dielectric constant is about 5000, and that of micro-size coarse powders is about 2200.     

Manufacture and characterization of ultra and microfiltration ceramic membranes by isostatic pressing

This paper describes the manufacture of tubular UF and MF porous and supported ceramic membranes to oil/water emulsions demulsification. For such a purpose, a rigorous control was realized over the distribution and size of pores. Suspensions at 30 vol.% of solids (zirconia or alumina powder and sucrose) and 70 vol.% of liquids (isopropyl alcohol and PVB) were prepared in a jar mill varying the milling time of the sucrose particles, according to the pores size expected. The membranes were prepared by isostatic pressing method and structurally characterized by SEM, porosimetry by mercury intrusion and measurements of weight by immersion. The morphological characterization of the membranes identified the formation of porous zirconia and alumina membranes and supported membranes. The results of porosimetry analysis by mercury intrusion presented an average pore size of 1.8 μm for the microfiltration porous membranes and for the ultrafiltration supported membranes, pores with average size of 0.01-0.03 μm in the top-layer and 1.8 μm in the support. By means of the manufacture method applied, it was possible to produce ultra and microfiltration membranes with high potential to be applied to the separation of oil/water emulsions.     

Alumina/silicon carbide composites fabricated via in situ synthesis of nano-sized SiC particles

Alumina/silicon carbide composites have been fabricated by a new technique involving the in situ synthesis of nano-sized SiC particles. A mixture of alumina powder and silicon carbide precursors was prepared in an aqueous suspension. Green bodies were formed by cold isostatic pressing of granules obtained by freeze granulation, and pressureless sintered at 1750 °C for 4 h in an argon atmosphere. Mullite (10–20 vol%) formed in addition to SiC during sintering. The SiC particles were located predominantly to the interior of the mullite and alumina matrix grains.     

Preparation and properties of porous SiC–Al2O3 ceramics using coal ash

In this paper, we first reported that porous SiC–Al₂O₃ ceramics were prepared from solid waste coal ash, activated carbon, and commercial SiC powder by a carbothermal reduction reaction (CRR) method under Ar atmosphere. The effects of addition amounts of SiC (0, 10, 15, and 20 wt%) on the postsintering properties of as-prepared porous SiC–Al₂O₃ ceramics, such as phase composition, microstructure, apparent porosity, bulk density, pore size distribution, compressive strength, thermal shock resistance, and thermal diffusivity have been investigated. It was found that the final products are β-SiC and α-Al₂O₃. Meanwhile, the SEM shows the pores distribute uniformly and the body gradually contacts closely in the porous SiC–Al₂O₃ ceramics. The properties of as-prepared porous SiC–Al₂O₃ ceramics were found to be remarkably improved by adding proper amounts of SiC (10, 15, and 20 wt%). However, further increasing the amount of SiC leads to a decrease in thermal shock resistance and mechanical properties. Porous SiC–Al₂O₃ ceramics doped with 10 wt% SiC and sintered at 1600°C for 5 hours with the median pore diameter of 4.24 μm, room-temperature compressive strength of 21.70 MPa, apparent porosity of 48%, and thermal diffusivity of 0.0194 cm²/s were successfully obtained.     

Pressureless sintered Al2O3–SiC nanocomposites

Al₂O₃ + 5 vol% SiC composite ceramics were prepared via a conventional powder processing route followed by pressureless sintering. Commercially available Al₂O₃ and SiC powders were milled together in an aqueous suspension. The slurry was freeze granulated, and green bodies were obtained by cold isostatic pressing of the granules. Pressureless sintering was carried out in a nitrogen atmosphere at 1750 and 1780 °C. Near full density (>99%) was achieved at 1780 °C. Densification at the lower sintering temperature was promoted by smaller additions of MgO. Vickers hardness and indentation fracture toughness varied around 18 GPa and 2.3 MPa m^1/2 after sintering at 1780 °C. Transmission electron microscopy revealed that the SiC particles were located predominantly to the interior of the matrix grains and well distributed throughout the composite microstructures. The intragranular particles had sizes in the range 50–200 nm while the intergranular particles were larger, typically 200–500 nm in diameter.     

Spheroidization of SiC powders and their improvement on the properties of SiC porous ceramics

Spherical SiC powders were prepared at high temperature using commercial SiC powders (4.52 µm) with irregular morphology. The influence of spherical SiC powders on the properties of SiC porous ceramics was investigated. In comparison with the as-received powders, the spheroidized SiC powders exhibited a relatively narrow particle size distribution and better flowability. The spheroidization mechanism of irregular SiC powder is surface diffusion. SiC porous ceramics prepared from spheroidized SiC powders showed more uniform pore size distribution and higher bending strength than that from as-received SiC powders. The improvement in the performance of SiC porous ceramics from spheroidized powder was attributed to tighter stacking of spherical SiC particles. After sintering at 1800 °C, the open porosity, average pore diameter, and bending strength of SiC porous ceramics prepared from spheroidized SiC powder were 39%, 2803.4 nm, and 66.89 MPa, respectively. Hence, SiC porous ceramics prepared from spheroidized SiC powder could be used as membrane for micro-filtration or as support of membrane for ultra/nano-filtration.