Biomorphic Silicon Carbide Research Articles

Advanced Hierarchical Biomorphous Silicon Carbide Monoliths

Porous silicon carbide (SiC) has attracted considerable attention in the field of cellular ceramics for a variety of applications such as catalyst supports, filters, or in the biomedical field due to its excellent structural properties, mechanical strength, and chemical stability. However, SiC has certain limitations due to high‐temperature profiles and costly manufacturing methods. Therefore, it is investigated that porous biomorphic silicon carbide monoliths using a powder blend of paper‐derived carbon fibers, phenolic resin, and silicon, resulting in comparatively low sintering temperatures (T = 1300 to 1550 °C) and good mechanical strength. This near‐net‐shape process uses low‐cost raw materials and enables the production of silicon carbides with high open porosity (P = 51.48% to 68.28%) and low shrinkage. The influence of different amounts of carbon sources (Cfibers and Cresin) on the mechanical (4‐point bending) and thermal properties (laser flash method) is investigated. In addition, to improve the pressure gradients, macrochannels with multiple layers of sacrificial polymer lattices are incorporated, resulting in hierarchical structures with high permeability. Thus, this advanced biomimetic approach offers great potential for structured cellular ceramics with tailored properties for biomedical, catalyst support, or nuclear fuel cladding materials.

Advanced Arc Plasma Synthesis of Biomorphic Silicon Carbide Using Charcoal and Silicon Dioxide in Air

This work presents the results revealing the possibility of obtaining a cubic phase of silicon carbide with features of a biomorphic structure. Renewable plant raw materials were used as a source of carbon, in particular, pyrolyzed sawdust, which is a waste of a timber enterprise. Silicon dioxide powder was used as a source of silicon. The synthesis was realized using DC arc discharge plasma initiated in an open air. In this case, the oxidation of the synthesis products was prevented due to the effect of the reaction volume self-shielding from atmospheric oxygen. It was possible due to the generation of protective gaseous medium predominantly consisting of carbon dioxide and monoxide. The dependences of the product phase composition on the supplied energy and composition of initial components were established. The synthesis product was characterized by a significant excess of carbon, which was a caused by the erosion of the electrodes. After removal of chemically unbound carbon from synthesis product by annealing in an atmospheric furnace at 850 °C, obtained powder was sintered by the spark plasma sintering method. In the result, a bulk ceramic sample was obtained in which the only one crystalline phase of silicon carbide with a lattice parameter of 4.359 Å was identified.

Ceria-based catalytic coatings on biomorphic silicon carbide: A system for soot oxidation with enhanced properties

In order to be efficient, catalysts require an adequate substrate with tailored porosity, specific surface area and pore size distribution. This work reports on the use of biomorphic silicon carbide, a wood-derived ceramic material, to fabricate a wall-flow filter onto which ceria-based catalytic coatings are synthesised in-situ with two different morphologies. Based on laboratory tests performed emulating realistic conditions, it is shown that the deposition of a ceria washcoat on the substrate reduces the temperature needed to regenerate the filter by 14 °C to 110 °C. The use of a ceria morphology that enhances the soot/catalyst contact conditions strengthens this effect. The influence of the substrate arrangement on the regeneration performance and the oxidative capacity of the catalytic coating is analysed. These results extend the possibilities of further reducing the soot oxidation temperature by combining the synergistic effects of an engineered ceria morphology and an optimum substrate arrangement.

Biomorphic SiC: porous SiC and ultrafine SiC powder formation through biomimicking route

ABSTRACT Natural wood is a ready-to-use template for making porous silicon carbide (SiC) body. Biomorphic β-SiC was synthesised from wood of a mango (Mangifera Indica) tree. Carbon template was made by carbonising this wood at 1000°C in argon gas atmosphere. Thus formed template was repeatedly infiltrated with a mixture of tetraethyl-orthosilicate (TEOS) (in alcohol) and oxalic acid solution (aqueous). Heat treatment at 1600°C for 1 h in vacuum converted the infiltrated template to β-SiC with a complex hierarchical cellular structure- a mimic of the plant structure. To produce phase pure SiC, unreacted carbon (C) and silica (SiO2) (if any) were removed by burning in air followed by treating with hydrofluoric acid. Mono dispersed SiC powder having particle size of ∼225 nm has been obtained by crushing, grinding and milling of thus formed biomorphic SiC body. A grinding limit is reported for the first time in SiC system.

New biomorphic filters to face upcoming particulate emissions policies: A review of the FIL-BIO-DIESEL project

With a high number of diesel vehicles worldwide, particulate emission control is an urgent issue with a global impact, from the health of citizens to commercial future of this technology in some transport segments. Particulate filters are widely used in automotive engines to comply emissions regulations, but current technologies have room for improvement as they add additional backpressure in the exhaust system, and efficient on-board regeneration process is challenging.The Fil-Bio-Diesel Project is a R&D initiative to improve current particle filtration systems, based on the development of novel biomorphic substrates. By replicating the biologic tissue of a wood precursor, a biomorphic silicon carbide with hierarchic orthotropic microstructure can be produced. The porosity, the pore size, and pore orientation of this bioceramic material can be tailored through the selection of a suitable precursor, widening the initially narrow relationship between filtration efficiency and pressure drop that characterizes granular ceramic materials. In this paper the methodology and main results of the Fil-Bio-Diesel Project are presented. This work shows the peculiar advantages of biomorphic silicon carbide through several experimental studies. The results show the potential of this novel filter substrate to be used in future particulate abatement systems.

Numerical Simulation of a Wall-Flow Particulate Filter Made of Biomorphic Silicon Carbide Able to Fit Different Fuel/Biofuel Inputs

To meet the increasingly strict emission limits imposed by regulations, internal combustion engines for transport applications require the urgent development of novel emission abatement systems. The introduction of biodiesel or other biofuels in the engine operation is considered to reduce greenhouse gas emissions. However, these alternative fuels can affect the performance of the post-combustion systems due to the variability they introduce in the exhaust particle distribution and their particular physical properties. Bioceramic materials made from vegetal waste are characterized by having an orthotropic hierarchical microstructure, which can be tailored in some way to optimize the filtration mechanisms as a function of the particle distribution of the combustion gases. Consequently, they can be good candidates to cope with the variability that new biofuel blends introduce in the engine operation. The objective of this work is to predict the filtration performance of a wall-flow particulate filter (DPF) made of biomorphic silicon carbide (bioSiC) with a systematic procedure that allows to eventually fit different fuel inputs. For this purpose; a well-validated DPF model available as commercial software has been chosen and adapted to the specific microstructural features of bioSiC. Fitting the specific filtration and permeability parameters of this biomaterial into the model; the filtration efficiency and pressure drop of the filter are predicted with sufficient accuracy during the loading test. The results obtained through this study show the potential of this novel DPF substrate; the material/microstructural design of which can be adapted through the selection of an optimum precursor.

Fabrication of Macroporous Biomorphic SiC from Cellulose Nanofibers Aerogel.

The biomorphic Silicon Carbide (BioSiC) ceramic with highly interconnected porous three-dimensional (3D) structure was fabricated by utilizing balsa wood cellulose nanofibers aerogel as the biotemplate and polycarbosilane (PCS) as the preceramic precursor. Evolution of morphology, composition, and pore properties from untreated wood to porous BioSiC was investigated systemically. The shrinkage and weight gain during pyrolysis was discussed. It was found that the structure of as-synthesized BioSiC was related to the microstructure of wood aerogel template and the concentration of PCS precursor. The proper microstructure of cellulose skeleton which was essential for the infiltration process could obtained by removing lignin and hemicellulose appropriately. The optimum PCS content was 40 wt. % for easy infiltration and proper SiC content. The results revealed that the dredged skeleton of cellulose was reproduced perfectly by PCS ceramization. The obtained BioSiC presented high porosity (61.03%) and low density (0.86 g/cm3) with good Darcy permeability (19.22 mD).

Biomorphic Silicon Carbide from Malaysian Hardwood

Porous silicon carbide with mimicking the original microstructure of wood are prepared by pyrolysis and subsequently impregnated with silicon by silicon melt infiltration. The infiltration process was performed at 1500 °C for 3 hours holding times in inert atmosphere. Two types of wood were used as precursor which is Kapur and dark red Meranti.The morphology of resulting porous SiC have been investigated using scanning electron microscope (SEM/EDX) and X-ray diffraction (XRD) analysis. The density of the samples was characterized by Archimedes methods. The excess of silicon was removed by etching with the mixture of hydrofluoric and nitric acid. The flexural strength was tested by the three-point flexural method at room temperature.It has been shown that the final SiC for both precursors have similar density. The existence of SiC was proved by the XRD result, whereas EDX analysis of silicon content revealed that the formation of silicon carbide in dark red Meranti is higher than that of Kapur. The flexural strength and modulus of dark red Meranti samples were much higher than those of the kapur samples because of higher formation of silicon carbide in dark red Meranti.

Preliminary study on the performance of biomorphic silicon carbide as substrate for diesel particulate filters

This paper presents the results of a preliminary experimental study to assess the performance of biomorphic silicon carbide when used for the abatement of soot particles in the exhaust of Diesel engines. Given its optimal thermal and mechanical properties, silicon carbide is one of the most popular substrates in commercial diesel particulate filters. Biomorphic silicon carbide is known for having, be-sides, a hierarchical porous microstructure and the possibility of tailoring that microstructure through the selection of a suitable wood precursor. An experimental rig was designed and built to be integrated within an engine test bench that allowed to characterizing small lab-scale biomorphic silicon carbide filter samples. A particle counter was used to measure the particles distribution before and after the samples, while a differential pressure sensor was used to measure their pressure drop during the soot loading process. The experimental campaign yielded promising results: for the flow rate conditions that the measuring devices imposed (1 litre per minute; space velocity = 42,000 L/h), the samples showed initial efficiencies above 80%, pressure drops below 20 mbar, and a low increase in the pressure drop with the soot load which allows to reach almost 100% efficiency with an increase in pressure drop lower than 15%, when the soot load is still less than 0.01 g/L. It shows the potential of this material and the interest for advancing in more complex diesel particle filter designs based on the results of this work.

Experimental measurement of the filtration efficiency and pressure drop of wall-flow diesel particulate filters (DPF) made of biomorphic Silicon Carbide using laboratory generated particles

Biomorphic Silicon Carbide (bioSiC) has been recently introduced in the scope of porous ceramic substrates for hot gas filtration applications, where it has demonstrated to have good thermal and mechanical properties, and a high potential to meet the requirements for current Diesel Particulate Filters (DPF). In this experimental study, a small wall-flow bioSiC diesel filter was characterized using a soot generator, the particle size distribution of which being similar to the one generated by a diesel engine. The bioSiC samples were manufactured from Medium Density Fiberboard (MDF) following a general manufacturing procedure for bioSiC ceramics, but paying special attention in the mechanizing stage to the geometry and optimal design of the honeycomb structure required for diesel engine applications. The samples had a cell density of 57.59 cell/cm2 (371.6 cpsi), a square cross section of 9.2 × 9.2 mm, and a length of 31 mm. To generate the particle laden stream and perform the filtration tests, a synthetic Soot Generator (SG) was used. Tests were performed under controlled and reproducible conditions, with a fixed gas flow rate of 5 LPM and a soot mass flow rate of 4 mg/h. The filtration efficiency was determined with the aid of a Scanning Mobility Particle Sizer (SMPS) from the measurements of the particle concentration upstream and downstream the filter samples. During the soot loading process, the pressure drop was also monitored. The results show that, in the initial stage (clean filter), bioSiC wall-flow DPFs may have a filtration efficiency between 0.7 and 0.85 and a pressure drop of around 2 kPa for a normalized wall velocity of 0.01 m/s at ambient temperature. The filtration performance of wall-flow bioSiC particle filters showed in this work can help us to better understand their real potential for automotive applications.

Biomorphic Ceramics for Drug Delivery in Bone Tissue Regeneration.

Incorporating therapeutic molecules into biomorphic ceramics for in situ drug release can be used to generate novel systems for tissue regeneration. These systems couple the complex hierarchical porous structures of biomorphic ceramics with the therapeutic activity of drugs. There are a large number of natural precursors available to be used as templates to obtain biomorphic silicon carbide ceramics. Additionally, different drug loading techniques can be used for these systems. The high versatility in structures and drugs allows the selection of the right structure-drug fit in each case according to the tissue needs. This paper reviews the utility of biomorphic ceramics for tissue engineering as well as their use for local drug release.

Performance of biomorphic Silicon Carbide as particulate filter in diesel boilers

Biomorphic Silicon Carbide (bioSiC) is a novel porous ceramic material with excellent mechanical and thermal properties. Previous studies have demonstrated that it may be a good candidate for its use as particle filter media of exhaust gases at medium or high temperature. In order to determine the filtration efficiency of biomorphic Silicon Carbide, and its adequacy as substrate for diesel particulate filters, different bioSiC-samples have been tested in the flue gases of a diesel boiler. For this purpose, an experimental facility to extract a fraction of the boiler exhaust flow and filter it under controlled conditions has been designed and built. Several filter samples with different microstructures, obtained from different precursors, have been tested in this bench. The experimental campaign was focused on the measurement of the number and size of particles before and after placing the samples. Results show that the initial efficiency of filters made from natural precursors is severely determined by the cutting direction and associated microstructure. In biomorphic Silicon Carbide derived from radially cut wood, the initial efficiency of the filter is higher than 95%. Nevertheless, when the cut of the wood is axial, the efficiency depends on the pore size and the permeability, reaching in some cases values in the range 70–90%. In this case, the presence of macropores in some of the samples reduces their efficiency as particle traps. In continuous operation, the accumulation of particles within the porous media leads to the formation of a soot cake, which improves the efficiency except in the case when extra-large pores exist. For all the samples, after a few operation cycles, capture efficiency was higher than 95%. These experimental results show the potential for developing filters for diesel boilers based on biomorphic Silicon Carbide.

Fabrication of Biomorphic Silicon Carbide from Agriculture Waste Powders

Fabrication of Biomorphic Silicon Carbide from Agriculture Waste Powders

Characterisation of Silicon Carbide from Dark Red Meranti Wood

Porous biomorphic silicon carbide is a promising ceramic materials for used in wide variety of applications especially in filtration and separation. Wood derived silicon carbide retains the heterogeneous structure of initial wood. Silicon carbide ceramic was derived from Dark Red Meranti wood precursor in this study. The derivation process was prepared by reaction between liquid silicon and carbon preform. The carbon preform was obtained via pyrolysis process at 850 °C in Argon gas flow atmosphere. This process was followed by Si infiltration at 1500 °C for different holding hours. The density was determined using Archimedes method. SEM was performed to observe their microstructures while the compositions and phase analysis were analysed by EDX and XRD respectively. Thermogravimetric analysis showed that a major weight loss of about 60% of carbon perform due to the decomposition of cellulose and lignin.XRD results revealed the presence of SiC and excess of silicon. It was found that conversion efficiency of carbon into SiC has been improved when the holding time was increased.

Porous biomorphic silicon carbide ceramics coated with hydroxyapatite as prospective materials for bone implants

Porous and cytocompatible silicon carbide (SiC) ceramics derived from wood precursors and coated with bioactive hydroxyapatite (HA) and HA-zirconium dioxide (HA/ZrO2) composite are materials with promising application in engineering of bone implants due to their excellent mechanical and structural properties. Biomorphic SiC ceramics have been synthesized from wood (Hornbeam, Sapele, Tilia and Pear) using a forced impregnation method. The SiC ceramics have been coated with bioactive HA and HA/ZrO2 using effective gas detonation deposition approach (GDD). The surface morphology and cytotoxicity of SiC ceramics as well as phase composition and crystallinity of deposited coatings were analyzed. It has been shown that the porosity and pore size of SiC ceramics depend on initial wood source. The XRD and FTIR studies revealed the preservation of crystal structure and phase composition of in the HA coating, while addition of ZrO2 to the initial HA powder resulted in significant decomposition of the final HA/ZrO2 coating and formation of other calcium phosphate phases. In turn, NIH 3T3 cells cultured in medium exposed to coated and uncoated SiC ceramics showed high re-cultivation efficiency as well as metabolic activity. The recultivation efficiency of cells was the highest for HA-coated ceramics, whereas HA/ZrO2 coating improved the recultivation efficiency of cells as compared to uncoated SiC ceramics. The GDD method allowed generating homogeneous HA coatings with no change in calcium to phosphorus ratio. In summary, porous and cytocompatible bio-SiC ceramics with bioactive coatings show a great promise in construction of light, robust, inexpensive and patient-specific bone implants for clinical application.

SILICON CARBIDE FORMATION FROM NATURAL WOODS

Processing of cellular ceramics with anisotropic pore structure by using silicon infiltration into carbonized template was investigated. Biomorphic silicon carbide (bioSiC) was produced by using two different types of natural woods which are Kapur and Dark Red Meranti. Carbon template was produced from a pyrolysis process followed by an infiltration process of melting silicon to produce bioSiC. The samples were dried in an oven in order to remove the moisture of the samples. The pyrolysis was done in two stages at a temperature of 500°C followed by 850°C. This study was to investigate the effect of infiltration temperature in the formation of SiC composites. Two different infiltration temperatures of 1500°C and 1600°C were used with constant holding time of 1 hour. The characteristic of the biomorphic silicon carbide was analyzed using the TGA, FESEM and EDX analysis. A wide variety of microstructures, densities and porosities were found depending on the type of wood used. Instead of carbon, it was found that both woods also reacted with nitrogen gas, which reduced the formation of SiC. The density of samples was increased as the working temperature increased. Dark Red Meranti was found to be denser and exhibit higher porosity than Kapur due to the higher formation of SiC.

The synergistic effect of VEGF and biomorphic silicon carbides topography on in vivo angiogenesis and human bone marrow derived mesenchymal stem cell differentiation

Topographical features of biomaterials are able to modulate cell attachment, spreading and differentiation. The addition of growth factors to implantable biomaterials can modify these cellular responses, enhancing their therapeutic potential.The aim of this research is to establish the influence of biomorphic silicon carbide ceramics (bioSiCs) surface topography on the proliferation and osteoblastic differentiation of mesenchymal stem cells and the potential synergistic effect of the ceramic porous structure together with vascular endothelial growth factor loading (VEGF) on the surface mediated osteoblastic differentiation.Three porous bioSiCs with important differences in their microstructure were obtained from different natural precursors. Samples loaded with or without VEGF through ionic interactions were cultured with human umbilical vein endothelial cells (HUVEC) or bone marrow derived mesenchymal stem cells (hMSCs). Cell behaviour and protein activity with regard to bioSiC porous structure and surface properties were analysed. An in vivo model (Chick Chorioallantoic Membrane; CAM) was used to assess the capability of the VEGF loaded systems to promote angiogenesis.Experimental data show that loaded systems were able to control the release of VEGF for up to 15 d ensuring the activity of the protein, increasing the proliferation of HUVECs and the formation of new blood vessels in the CAM. It was found that the selection of bioSiCs with a higher pore size promoted a higher concentration of osteoblastic differentiation markers of MSCs cultured on the surface of bioSiCs. Furthermore, the addition of VEGF to the systems was able to promote a faster osteoblastic differentiation according to the qPCR results, suggesting a synergy between both the surface properties and the controlled release of the growth factor.The VEGF loaded sapelli bioSiC was found to be the most promising material for bone tissue engineering applications.

Preparation of biomorphic silicon carbide–mullite ceramics using molten salt synthesis

Biomorphic silicon carbide–mullite ceramics were prepared from beech wood using liquid Si infiltration and molten salts synthesis. The resulting mullite whiskers coating, as well as the growth mechanism in molten Al2(SO4)3–Na2SO4 environment, have been investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) techniques. The biomorphic SiC ceramics derived from the beech wood template have coarse pore walls consisting of β-SiC grains with diameters ranging from 5 μm to 20 μm. After the molten salts reactions between biomorphic SiC substrate and mixture molten salts (Al2(SO4)3–Na2SO4), porous Silicon carbide–mullite ceramics with cilia-like microstructure were obtained. This unique structure has potential application in hot gases filters. An oxidation–dissolution cycle was proposed to explain the mullite whiskers growth in molten salts environment.

Key parameters in blood-surface interactions of 3D bioinspired ceramic materials

Direct contact of materials with blood components may trigger numerous processes which ultimately lead to hemolysis, clot formation and recruitment of inflammatory cells. In this study, the blood-surface interactions for two inert bioinspired ceramic scaffolds obtained from natural resources; biomorphic carbon and silicon carbides (bioSiC) from different origins have been studied. The response of the blood in contact with carbon is well known, however little has been identified on the influence of their 3D porous structure. Moreover, to our knowledge, there is no reference in the literature about the hemocompatibility of biomorphic silicon carbide as a porous scaffold. The experimental results showed the surface energy to be crucial to evaluate the hemocompatibility of a material however the surface topography and material porosity are also parameters to be considered. Surface roughness modifies clot formation whereas for protein adsorption total sample porosity seems to be the key parameter to be considered for hydrophilic materials (biomorphic silicon carbides), while the size of the pores determines the hemolytic response.

New Bio-ceramization process applied to vegetable hierarchical structures for bone regeneration: an experimental model in sheep.

Bone loss is still a major problem in orthopedics. The purpose of this experimental study is to evaluate the safety and regenerative potential of a new scaffold based on a bio-ceramization process for bone regeneration in long diaphyseal defects in a sheep model. The scaffold was obtained by transformation of wood pieces into porous biomorphic silicon carbide (BioSiC®). The process enabled the maintenance of the original wood microstructure, thus exhibiting hierarchically organized porosity and high mechanical strength. To improve cell adhesion and osseointegration, the external surface of the hollow cylinder was made more bioactive by electrodeposition of a uniform layer of collagen fibers that were mineralized with biomimetic hydroxyapatite, whereas the internal part was filled with a bio-hybrid HA/collagen composite. The final scaffold was then implanted in the metatarsus of 15 crossbred (Merinos-Sarda) adult sheep, divided into 3 groups: scaffold alone, scaffold with platelet-rich plasma (PRP) augmentation, and scaffold with bone marrow stromal cells (BMSCs) added during implantation. Radiological analysis was performed at 4, 8, 12 weeks, and 4 months, when animals were sacrificed for the final radiological, histological, and histomorphometric evaluation. In all tested treatments, these analyses highlighted the presence of newly formed bone at the bone scaffolds' interface. Although a lack of substantial effect of PRP was demonstrated, the scaffold+BMSC augmentation showed the highest value of bone-to-implant contact and new bone growth inside the scaffold. The findings of this study suggest the potential of bio-ceramization processes applied to vegetable hierarchical structures for the production of wood-derived bone scaffolds, and document a suitable augmentation procedure in enhancing bone regeneration, particularly when combined with BMSCs.