Fast discharge and high energy density of nanocomposite capacitors using Ba0.6Sr0.4TiO3 nanofibers

Nanocomposites combining high breakdown strength (BDS) polymer and high dielectric permittivity ceramic fillers have shown great potential for pulsed power application. Here a new composite material based on surface-functionalized Ba_0.6Sr_0.4TiO₃ nanofibers/poly(vinylidene fluoride) (BST NF/PVDF) has been prepared by solution casting. The nanocomposites containing 2.5 vol% isopropyl dioleic(dioctylphosphate) titanate (NDZ 101)-functionalized BST NF (N-h-BST NF) have large energy density of 6.95 J cm⁻³ at 380 MV m⁻¹, which is 1.85 times larger than that of the pure PVDF at the same electric field. Also, the discharge speed of the nanocomposites containing 7.5 vol% N-h-BST NF is approximately 0.11 μs. The good properties, together with the large energy density and fast discharge speed, make this material a promising candidate for pulsed power capacitor.     

Investigation of bismuth doped bioglass/graphene oxide nanocomposites for bone tissue engineering

In this study, bismuth doped 45S5 nanobioactive bioglass (nBG) and graphene oxide (GO) nanocomposites were developed and characterized in terms of microstructural, mechanical, bioactivity and biological properties. Bismuth (Bi) - doped nBG was synthesized by sol-gel method and sintered at 600 °C for 2 h. Nanosized GO was homogeneously mixed with Bi doped bioglass at various ratios to prepare nanocomposites. Addition of Bi increased the density of nBG samples while a considerable decrease in density was observed for nanocomposites with GO incorporation. Bi improved the diametral tensile strength of nBG and addition of 2.5% GO to the composite also increased the diametral tensile strength of the nanocomposites. However, addition of more than 2.5% GO had negative effect on the diametral tensile strength of the composites. Bi doping to bioglass and its composite with GO increased the biocompatibility of 45S5 nBG in which 96.5BG1Bi2.5GO (containing 96.5% BG 1% Bi 2.5% GO in weight ratio) showed highest cell viability. Overall, it can be concluded that composites of Bi doped 45S5 nBG with GO hold promise as biomaterial for biomedical applications.     

Fabrication and characterization of bioactive glass (45S5)/titania biocomposites

Bioactive glass (BG) (45S5) has been used successfully as bone-filling material in orthopedic and dental surgery but its lean mechanical strength limits its applications in load-bearing positions. Approaches to strengthen these materials decreased their bioactivity. In order to realize the optimal matching between mechanical and bioactivity properties, bioactive glass (45S5) was reinforced by introducing titania (TiO₂) in anatase form and treated at 1000 °C to form new bioactive glass/titania biocomposites. The prepared biocomposites were assessed by XRD, FT-IR, mechanical properties and SEM. The results verified that the increase of titania percentage to BG powder enhanced gradually the mechanical data of the prepared biocomposites. SEM and FT-IRRS confirmed the presence of a rich bone-like apatite layer post-immersion on the composite surface. It has been found that the new BG/titania biocomposite materials especially those containing high content of titania have high bioactivity properties and compressive strength values comparable to cortical bone. Therefore, these biocomposite materials are promising for medical applications such as bone substitutes especially in load-bearing sites.     

Synthesis and in vitro bioactivity assessment of injectable bioglass−organic pastes for bone tissue repair

The aim of this work was to study the bioactivity of systems based on a clinically tested bioactive glass (BG) particulates (mol%: 4.33 Na₂O−30.30 CaO−12.99 MgO−45.45 SiO₂−2.60 P₂O₅−4.33 CaF₂) and organic carriers. The cohesiveness of injectable bone graft products is of high relevance when filling complex volumetric bone defects. With this motivation behind, BG particulates with mean sizes within 11−14 μm were mixed in different proportions with glycerol (G) and polyethylene glycol (PEG) as organic carriers and the mixtures were fully injectable exhibiting Newtonian flow behaviors. The apatite forming ability was investigated using X-ray diffraction and field emission scanning electron microscopy under secondary electron mode after immersion of samples in simulated body fluid (SBF) for time durations varying between 12 h and 7 days. The results obtained revealed that in spite of the good adhesion of glycerol and PEG carriers to glass particles during preparation stage, they did not hinder the exposure of bioactive glass particulates to the direct contact with SBF solution. The results confirmed the excellent bioactivity in vitro for all compositions expressed by high biomineralization rates with the formation of crystalline hydroxyapatite being identified by XRD after 12 h of immersion in SBF solution.     

Effect of ultrasound on HDPE/clay nanocomposites: Rheology,structure and properties

High density polyethylene (HDPE)/organoclay nanocomposites of varying concentrations of clay were prepared by a single screw compounding extruder with the attached ultrasound die operating at various amplitudes. The die pressure and power consumption due to ultrasound were measured at different feed rates of nanocomposites of various clay concentrations. The structure and morphology of nanocomposites were studied by X-ray diffraction (XRD), transmission electron microscopy (TEM) and infrared spectroscopy. It was found that ultrasonic treatment enhanced the intercalation of HDPE into lattice layers of clay by increasing d-spacing up to 50%. Mechanical and rheological properties of these nanocomposites were investigated as a function of clay concentration and ultrasonic amplitude. Complex viscosity, storage and loss moduli of nanocomposites were increased after ultrasonic treatment. Mechanical properties such as the elongation at break, yield stress, toughness and impact strength of ultrasonically treated nanocomposites increased in comparison with the untreated nanocomposites. A reduction in oxygen permeability of nanocomposites was observed after ultrasonic treatment at an amplitude of 10 μm with the highest reduction by 20% at 2.5% clay concentration and a residence time of 21 s. This reduction in permeability was achieved even though results indicate that the crystallinity of ultrasonically treated nanocomposites was reduced.     

Development and characterization of niobium-releasing silicate bioactive glasses for tissue engineering applications

Novel niobium-containing bioactive glass formulations (Nb-BGs) were designed, produced and used to fabricate sintered glass-ceramic granules to examine their in vitro bioactivity and angiogenic potential. Nb-BGs were prepared by melting and quenching. Afterwards, the glasses were crushed and milled into fine powders. These powders were used to make aqueous slurries which were poured into molds, dried and sintered to produce pellets, from which granules of 0.5–0.85 mm in size were obtained. In vitro bioactivity was tested by immersing the granules in simulated body fluid for up to 14 days. Cell biology tests were carried out by indirect culture of bone marrow stromal cells (ST-2) with supernatants resulting from incubation of BG granules in cell culture medium. The effect of dissolution products from Nb-BGs on the secretion of vascular endothelial growth factor (VEGF) was assessed to characterize the angiogenic potential of the new Nb-containing BG compositions.     

Microstructure development,hardness, toughness and creep behaviour of pressureless sintered alumina/SiC micro–nanocomposites obtained by slip-casting

Al₂O₃–SiC micro–nanocomposites are much more resistant materials than monolithic alumina regarding some mechanical properties. In order to study the possibility of obtaining creep resistant alumina/SiC micro–nanocomposites using inexpensive forming methods, alumina 1 and 5 vol% SiC materials were produced by slip-casting and pressureless sintering. Well-densified alumina–SiC pressureless sintered materials were obtained at 1700 °C for 2 h and attained 97–99% of the theoretical density. The microstructure, hardness and toughness were examined and 4-point flexure creep tests were performed at 1200 °C and 100 MPa in air. Compared with pure alumina materials, the creep resistance, toughness and hardness were enhanced drastically in materials containing 5 vol% of SiC.     

Si3N4/graphene nanocomposites for tribological application in aqueous environments prepared by attritor milling and hot pressing

Advanced ceramic materials have proved their superior wear resistance as well as mechanical and chemical properties in a wide range of industrial applications. Today there are standard materials for components and tools that are exposed to severe tribological, thermal or corrosive conditions. The main aim of this work is to develop novel, highly efficient tribological systems on the basis of ceramic/graphene nanocomposites as well as to prove their superior quality and to demonstrate their suitability for technical applications e.g. for slide bearings and face seals in aqueous media. Current research in the field of ceramic nanocomposites shows that is possible to make ceramic materials with improved mechanical and tribological properties by incorporating graphene into the Si₃N₄ structure. Multilayered graphene (MLG) was prepared by attritor milling at 10 h intensive milling of few micrometer sized graphite powders. The large quantity, very cheap and quick preparation process are a main strengths of our MLG. Si₃N₄/MLG nanocomposites were prepared by attritor milling and sintered by hot pressing (HP). The Si₃N₄ ceramics were produced with 1 wt%, 3 wt%, 5 wt% and 10 wt% content of MLG. Their structure was examined by transmission electron microscopy (TEM). The tribological behavior of composites in aqueous environment was investigated and showed the decreasing character of wear at increased MLG content. This new approach is very promising, since ceramic microstructures can be designed with high toughness and provide improved wear resistance at low friction.     

Microstructure,mechanical properties and machining performance of spark plasma sintered Al2O3–ZrO2–TiCN nanocomposites

The effect of addition of nanocrystalline ZrO₂ and TiCN to ultrafine Al₂O₃ on mechanical properties and microstructure of the composites developed by spark plasma sintering (SPS) was investigated. The distribution of the nanoparticles was dependent on their overall concentration. Maximum hardness (21 GPa) and indentation toughness (5.5 MPa m^1/2) was obtained with 23 vol% nanoparticles, which was considered as the optimum composition. The Zener pinning criteria were also satisfied at this composition with grain size of the restraining nanoparticles ～63–65 nm. Hardness of the composites follows the rule of mixtures; crack deflection and crack arrest by nanoparticles at grain boundaries along with mixed fracture mode led to high toughness in the nanocomposites. Cutting tool inserts were developed by SPS with the optimized composition and their machining performance was compared with commercial alumina based inserts. Increased toughness in the nanocomposite inserts reflects in the machining performance as the tool life improves drastically compared to that of the commercial inserts at high cutting speeds ≥500 m min^?1. This was attributed to differences in their failure modes; the commercial inserts fail catastrophically by fracture due to their low toughness whereas the nanocomposite inserts reach the tool failure criteria by crater wear at all machining conditions.     

Microstructure and mechanical properties of Ti (C,N) based cermets reinforced with different ceramic particles processed by spark plasma sintering

The addition effect of different ceramic particles such as TiB₂, TiN and nano-Si₃N₄ on the microstructure and mechanical properties of TiCN-WC-Co-Cr₃C₂ based cermets, which are prepared by spark plasma sintering, was studied. Microstructural characterization of the cermets was done by scanning electron microscope. X-ray diffraction was performed to study the crystal structures. Mechanical properties such as hardness and fracture toughness were measured for the different developed cermets. The hardness and fracture toughness of the TiCN-WC-Co-Cr₃C₂ cermets without TiN, TiB₂, and nano-Si₃N₄ were 8.4 GPa and 3.4 MPa m^1/2, respectively. It was found that 5 wt% TiB₂ addition alone improved the corresponding hardness and fracture toughness to 19.2 GPa and 6.9 MPa m^1/2, respectively. The addition of 5 wt% TiN, improved the hardness and fracture toughness to 16.7 GPa and 6.9 MPa m^1/2, respectively. With the combination of 5 wt% TiN and 5 wt% TiB₂, the hardness and fracture toughness were improved to 15.5 GPa and 6.6 MPa m^1/2, respectively. But, the addition of 5 wt% Si₃N₄ showed a balanced improvement in both hardness (17.6 GPa) and toughness (6.9 MPa m^1/2). Fracture toughness did not change much for all the above cermets with different ceramic inclusions.     

Flame retardancy and thermal stability of ethylene-vinyl acetate copolymer nanocomposites with alumina trihydrate and montmorillonite

The development of fire retardant for wire and cable sheathing materials has oriented toward low smoke and halogen-free flame retardant technology to achieve better safety for electrical equipment and devices and to satisfy standards. However, many polymer flame resistance materials require a very high proportion of metal hydrate filler within the polymer matrix (60 wt%) to achieve a suitable level of flame resistance, which may lead to inflexibility, poor mechanical properties and problems during compounding and processing. In this study, the alumina trihydrate (ATH) was added to montmorillonite (MMT) as the halogen-free flame retardant of ethylene-vinyl acetate (EVA) copolymer, with various ratios of EVA/ATH/MMT. The prepared nanocomposites were characterized through various techniques of XRD, tensile test, DSC analysis, TGA, LOI evaluation, and FE-SEM to explore the effects of organic modified clay (OMMT) and the layer distance on the mechanical, thermal, and flame resistance properties. In the XRD examinations, the layer-distance of MMT increased from 1.27 to 1.96 nm when polymer was added to the octadecylamine modified MMT. The best tensile strength was obtained at 3 wt% MMT. In addition, the halogen-free flame resistance grade of EVA containing 3 wt% OMMT and 47 wt% ATH revealed the best elongation and fire resistance (LOI = 28). The tensile and flame resistance properties of the nanocomposites were also significantly improved.     

Can the regenerative potential of an alkali-free bioactive glass composition be enhanced when mixed with resorbable β-TCP?

The addition of resorbable β-tricalcium phosphate (β-TCP) to other bone substitute materials such as hydroxyapatite (HA) has been pointed out as a suitable strategy to enhance the regenerative potential of bone grafts made thereof. To check the generalization of this hypothesis, a new synthetic composite bone graft material consisting of a mixture of 30 vol% of pure β-TCP and 70 vol% of FastOs^®BG (an alkali-free bioactive glass - BG) was prepared and tested in vivo. The in vivo performance of the new synthetic bone graft (30β-TCP-70FastOs^®BG) was compared with those of FastOs^®BG alone and of adbone^®BCP, a biphasic calcium phosphate, consisting of 75% of HA and 25% of β-TCP. Two defects with 4 mm diameter were performed in Wistar rats calvaria and filled with the bone graft materials. The animals were sacrificed after 9 weeks of implantation and the calvaria was excised. Empty bone defects were used as negative control. The percentages of new bone formed (von Kossa staining) were always higher in the treated groups (FastOs^®BG, 30β-TCP-70FastOs^®BG and adbone^®BCP) than in empty group. There were differences with statistical significance between empty and FastOs^®BG groups and between empty and adbone^®BCP groups. But the differences observed between empty and 30β-TCP-70FastOs^®BG groups were less remarkable. The results demonstrated the superior bone regeneration ability of FastOs^®BG alone, which was not further enhanced by adding β-TCP in the composition, confirming its already proven regenerative potential.     

Reinforcement of precursor-derived Si–C–N ceramics with carbon nanotubes

Nanocomposites consisting of precursor-derived Si–C–N ceramics incorporated with carbon nanotubes (CNTs) were successfully prepared by casting of a mixture of CNTs and a liquid precursor polymer followed by cross-linking and thermolysis. The effect of CNTs on the fracture toughness of these nanocomposites was investigated by a thermal loading technique. The results reveal a dependence of the fracture toughness on the type of the CNTs. One type shows a significant increase of the fracture toughness at CNT contents of only 1–2 mass%, whereas the other one exhibits no effect. The microstructural effects of CNTs observed at the fracture surfaces of the nanocomposites by scanning electron microscope (SEM) and transmission electron microscope (TEM) can be correlated with the observed fracture toughness behavior.     

Screening of factors influencing the extraction of gelatin from the skin of cuttlefish using supersaturated design

Supersaturated design (SSD) was used for screening the key parameters influencing gelatin extraction yield from cuttlefish (Sepia officinalis) skin. Results indicated that among a list of 17 factors only five parameters, namely, alkali (NaOH) concentration, acid reagent (acetic acid), enzyme, thermal treatment temperature and centrifugation time, were factors influencing gelatin yield. The optimal conditions for gelatin extraction were found to be: pretreatment with NaOH 0.03 M for 1 h; treatment with pepsin for 24 h at 4 °C in acetic acid 100 mM; extraction for 14 h at 40 °C. The yield of gelatin extraction was 54.6%. Cuttlefish skin gelatin (CSG) contained protein as the major compound (90.95%) and low fat (0.3%) and ash (0.05%) contents. The physico-chemical properties of the CSG were characterized and compared with those of bovine gelatin (BG). The result of textural properties showed that hardness, elasticity and cohesiveness of CSG were lower than those of BG. Further, the gel strength of CSG (192.01 g) was lower than that of BG (259.65 g), possibly due to lower imino-acid content. The functional properties, including emulsion activity index and foam stability were similar to those of BG. The CSG showed stronger ability of apple juice clarification, than BG without affecting its nutritional values.     

Montmorillonite-carbon nanocomposites with nanosheet and nanotube structure: Preparation,characterization and structure evolution

In this study, the preparation of montmorillonite (Mt)-polyvinyl alcohol (PVA) nanocomposites (MtPVAN), and the formation of corresponding Mt carbon nanocomposites with nanosheet and nanotube structures were investigated. MtPVAN was prepared by solution intercalation combined with the dispersion method of ultrasonic radiation (UR) and mechanical stirring (MS). XRD analysis showed that the MtPVAN with d₀₀₁ at 2.16 nm were successfully obtained with optimum mass ratio of 1:1.5 (Mt:PVA) and solid content of 10%. Then, the Mt-carbon, nanocomposites (d₀₀₁ = 1.56 nm) with sandwich structure was prepared by carbonizing MtPVAN at 400 °C in nitrogen atmosphere for 3 h; and Mt-carbon nanosheets or nanotubes with carbon content of 5.10% was obtained by exfoliating the sandwich-like Mt-carbon nanocomposites with further airflow pulverization process. The average diameter and the thickness of the Mt-carbon nanosheets was about 2 μm and 10 nm, respectively; while the diameter of the nanotubes was 7–80 nm. The mechanism of the formation and the structure evolution of the Mt-carbon nanocomposites were also discussed.     

Microstructure and mechanical properties of alumina 5 vol% zirconia nanocomposites prepared by powder coating and powder mixing routes

Zirconia toughened alumina (ZTA) nanocomposites are attractive structural materials which combine the high hardness and Young's modulus of the alumina matrix with an additional toughening effect by the zirconia dispersion.In this study two approaches to prepare ZTA are compared. For the first approach, an ultrafine alumina powder was coated with 5 vol% zirconia by a wet chemical method. For the second one, the reference material was prepared by intensively mixing and milling the same alumina with nanoscale zirconia powder. Samples were consolidated at 1350–1600 °C by hot pressing and their mechanical properties, microstructure and transformation behavior were compared. Toughness increments derived from different toughening mechanisms are also briefly discussed. Besides better sinterability, the mixed material exhibited a finer grain size of both matrix and dispersion and thus higher hardness and strength. The alumina matrix was under compressive hydrostatic residual cooling stress, whereas zirconia was under tensile one. The coated material, however, showed higher transformability, deeper transformation zones and thus higher fracture toughness. In addition, it contained more monoclinic zirconia so the matrix was under tension.     

Microstructure and properties of B4C-SiC composites prepared by polycarbosilane-coating/B4C powder route

B₄C-SiC composites with fine grains were fabricated with hot-pressing pyrolyzed mixtures of polycarbosilane-coated B₄C powder without or with the addition of Si at 1950 °C for 1 h under the pressure of 30 MPa. SiC derived from PCS promoted the densification of B₄C effectively and enhanced the fracture toughness of the composites. The sinterability and mechanical properties of the composites could be further improved by the addition of Si due to the formation of liquid Si and the elimination of free carbon during sintering. The relative density, Vickers hardness and fracture toughness of the composites prepared with PCS and 8 wt% Si reached 99.1%, 33.5 GPa, and 5.57 MPa m^1/2, respectively. A number of layered structures and dislocations were observed in the B₄C-SiC composites. The complicated microstructure and crack bridging by homogeneously dispersed SiC grains as well as crack deflection by SiC nanoparticles may be responsible for the improvement in toughness.     

Reinforcement with reduced graphene oxide of bioactive glass scaffolds fabricated by robocasting

45S5 bioactive glass composite scaffolds reinforced with reduced graphene oxide (rGO) were fabricated for the first time by robocasting (direct-writing) technique. Composite scaffolds with 0–3 vol.% content of rGO platelets were printed, and then consolidated by pressureless sintering at 550 or 1000 °C in Ar atmosphere. It was found that the addition of rGO platelets up to 1.5 vol.% content enhanced the mechanical performance of the 45S5 bioactive glass scaffolds in terms of strength and toughness. Best performance was obtained for 1 vol.% rGO, which yielded an enhancement of the fracture toughness of ∼850 and 380% for sintering temperatures of 550 and 1000 °C, respectively, while the compressive strength increased by ∼290 and 75%. rGO addition thus emerges as a promising approach for the fabrication of novel bioglass scaffolds with improved mechanical performance without deterioration of their bioactivity, which may then find use in load-bearing bone tissue engineering applications.     

Influence of processing on fracture toughness of Si3N4 + graphene platelet composites

Silicon nitride + 1 wt% graphene platelet composites were prepared using various graphene platelets (GPL) and two processing routes; hot isostatic pressing (HIP) and gas pressure sintering (GPS). The influence of the processing route and graphene platelets’ addition on the fracture toughness has been investigated. The matrix of the composites prepared by GPS consists of Si₃N₄ grains with smaller diameter in comparison to the composites prepared by HIP. The indentation fracture toughness of the composites was in the range 6.1–9.9 MPa m^0.5, which is significantly higher compared to the monolithic silicon nitride 6.5 and 6.3 MPa m^0.5. The highest value of K_IC was 9.9 MPa m^0.5 in the case of composite reinforced by the smallest multilayer graphene nanosheets, prepared by HIP. The composites prepared by GPS exhibit lower fracture toughness, from 6.1 to 8.5 MPa m^0.5. The toughening mechanisms were similar in all composites in the form of crack deflection, crack branching and crack bridging.     

Fabrication and cytotoxicity assessment of novel polysiloxane/bioactive glass films for biomedical applications

This work evaluates for the first time the cyto-compatibility of silicone (polysiloxane)/bioactive glass composite films produced by dip coating on stainless steel substrates using osteoblast-like (MG-63) cells. With the aim of creating corrosion resistant coatings for biomedical applications, bioactive glass (BG) of 45S5 composition was used as a filler in conjunction with commercial silicones (MK and H62C). Bioactive glass has the property of forming a direct bond to living bone, and polysiloxane is an attractive candidate for protective coatings due to its resistance to oxidation and corrosion. Suspensions based on polysiloxanes (MK/H62C) and micro-sized BG fillers were used for dip coating stainless steel substrates at room temperature, followed by curing in oxidative atmosphere at 260 °C and 500 °C. Fourier transform infrared spectroscopy (FTIR) analysis revealed the presence of Si–O–Si, Si–OR, Si–CH₃ and Si–OH groups on the substrate. Field emission scanning electron microscopy showed that the coatings were homogeneous with no obvious cracks or pinholes at relatively high concentrations of both polysiloxane and BG. The cell biology experiments confirmed that the expressed cell-morphology, analyzed on chosen surfaces, was pheno-typical for MG-63 cells after 48 h of incubation. On the film containing the lower amount of polysiloxane/BG the most dense cell layer was formed. Our results indicated that polysiloxane/BG composite films exhibited good cyto-compatibility at 260 °C and 500 °C and showed no toxicity toward MG-63 cells suggesting the potential of this composite for applications in medical implants.