Calcium phosphate substrates with emulsion-derived roughness: Processing,characterisation and interaction with human mesenchymal stem cells

Calcium phosphates (CaP) have been the subject of several studies that often lack a systematic approach to understanding how their properties affect biological response. CaP particles functionalised with a pH-responsive polymer (BCS) were used to prepare microporous substrates (porosity between 70 and 75% and pore sizes of 5–20 μm) through the aggregation of oil-in-water emulsions by controlling solid loading, emulsification energy, pH, drying and sintering conditions. The combined effect of surface roughness (roughness amplitude, R_a between 0.9–1.7 μm) and chemistry (varying Hydroxyapatite/β-Tricalcium phosphate ratio) on human mesenchymal stem cells was evaluated. HA substrates stimulated higher cell adhesion and proliferation (especially with lower R_a), but cell area increased with β-TCP content. The effect of surface roughness depended of chemistry: HA promoted higher mineralising activity when R_a ～ 1.5 μm, whereas β-TCP substrates stimulated a more osteogenic profile when R_a ～ 1.7 μm. A novel templating method to fabricate microporous CaP substrates was developed, opening possibilities for bone substitutes with controlled features.     

3D printed polylactide-based zirconia-toughened alumina composites: fabrication,mechanical, and in vitro evaluation

Fused deposition modeling (FDM) has been a commonly used technique in the fabrication of geometrically complex biodegradable scaffolds for bone tissue engineering. Generally, either individual polylactide (PLA) or its combination with calcium phosphates or bioglass has been employed to design scaffolds through the principles of FDM. In this study, FDM protocol has been employed to design 3D printed PLA/zirconia-toughened alumina (ZTA). A series of PLA/ZTA combinations have been attempted to determine the feasibility of the resultant in filament extrusion and their subsequent capacity to obtain a stable 3D printed component. A maximum of 80 wt.% PLA and 20 wt.% ZTA has been determined as an optimum combination to yield a stable 3D structure beyond which an enhanced ZTA content in the PLA matrix yielded a fragile filament that lacked effectiveness in 3D printing. 5 and 10 wt.% of ZTA addition in the PLA matrix produced a better 3D design that reasonably displayed good mechanical properties. Depending on the ceramic content, a homogeneous dispersion of the constituent elements representative of ZTA has been determined throughout the PLA matrix. Simulation studies through finite element analysis (FEA) exhibited good corroboration with the test results obtained from the mechanical studies.     

Effects of sintering curves on microstructure,physical and mechanical properties and on low temperature degradation of zirconia-toughened alumina

The objective of this work was to study two-step sintering as a means of controlling the microstructure of coarse Al₂O₃ matrix composites containing submicrometric and nanometric inclusions of ZrO₂ ranging from 0–30 wt. % by weight based on commercially available powders and evaluate its hydrothermal degradation as function of a water vapour pressure and its mechanical properties. The results showed that two-step sintering allowed a more efficient microstructural control than single-step sintering, resulting in good mechanical properties. The highest flexural strength was achieved for ZTA samples sintered in two-stage sintering conditions TSS2 with T1 = 1560 °C for 3 h, T2 = 1460 °C for 8 h. The studied composites showed good resistance to hydrothermal degradation compared to composites sintered in single step sintering conditions.     

Preparation and characterisation of mesoporous silica–alumina and silica–titania with a narrow pore size distribution

Amorphous mesoporous materials with a different degree of order in the arrangement of pores are outlined. Particularly, the synthesis of a class of mesoporous silica–alumina (MSA) materials with narrow pore size distribution and a disordered arrangement of pores is reported and discussed. Likewise, the preparation of titanium-containing ordered mesoporous silicates (Ti-MCM-41) and disordered mesoporous silica–titania (MST) are also described in detail. The structural properties of the solids are compared by means of X-ray diffraction and UV-Vis diffuse reflectance spectroscopy. The nitrogen adsorption–desorption measurements were performed and the textural properties are evaluated by the BET, DFT, BJH and t-plot methods.

The high specific surface area and pore volume, as well as the acidity, make MSA solids interesting catalysts in several petrochemical transformations, i.e. oligomerisation, alkylation, hydroisomerisation, rearrangement reactions. Besides, thanks to the width of the mesopores of such solids, the catalytic activity of titanium-containing silicates may have a potential application in the epoxidation of bulky unsaturated fine chemical substrates.     

有序介孔氧化铝的合成、结构表征及催化应用

综述了新型介孔材料———有序介孔氧化铝的各种合成方法、结构和性能的表征方法及在催化领域的应用前景。介孔氧化铝比表面可达500~700 m2/g,,平均孔径2~10 nm,孔径分布窄,具有分子筛性质,催化应用价值高。     

Biphasic calcium phosphate scaffolds fabricated by direct write assembly: Mechanical,anti-microbial and osteoblastic properties

The present work reports on the fabrication of 3-D porous calcium phosphate scaffolds by robocasting from biphasic (HA/β-TCP ≈ 1.5) powders, undoped and co-doped with Sr and Ag. Scaffolds with different pore sizes and rod diameter of 410 μm were fabricated and sintered at 1100 °C. The size and morphology of the powder particles, and the concentrations of the processing additives, were shown to play major roles in the robocasting process. For all pore sizes tested, the compressive strength of scaffolds was comparable to or even higher than that of cancellous bone, and mechanical data could be systematically correlated with the porosity fraction. Co-doping the starting powders with Sr and Ag enhanced the mechanical strength of scaffolds, conferred good antimicrobial activity against Staphylococcus aureus and Escherichia coli, and did not induce any cytotoxic effects on human MG-63 cells. Furthermore, the co-doped powder was more effective in inducing pre-osteoblastic proliferation.     

Permeability and corrosion resistance of the porous alumina doped by Y2O3 with monodispersed PMMA as pore former

Porous alumina, with monodispersed PMMA as pore former and Y₂O₃ as sintering additive, was prepared via a gel casting route with Isobam as a gelling agent. The effects of PMMA addition on its properties, including apparent porosity, bulk density, strength, permeability, and corrosion resistance to acid/alkali, were investigated. With PMMA addition increased, the apparent porosity and permeability were increased obviously, while strength and corrosion resistance to acid/alkali were deteriorated due to increased porosity. Higher firing temperature resulted in lower porosity, higher strength, lower permeability, and better corrosion resistance to acid/alkali. Coarser raw powders resulted in lower strength and higher permeability due to the coarser structure and larger pores of the fabricated samples. Because Y₂O₃ was used as a sintering additive, and no silica was introduced, the resulting samples possess better corrosion resistance to acid and alkali, especially much better corrosion resistance to alkali, than those reported with silica introduced.     

Morphological and structural features of individual and composite nanooxides with alumina, silica, and titania in powders and aqueous suspensions

Morphological, structural, and adsorptive characteristics of such fumed oxides as alumina, silica, composite silica/alumina and alumina/silica/titania were studied using a variety of experimental methods. Heating of nanooxides caused several processes resulting in the temperature dependent structural changes of the materials because of changes in the amounts of intact and dissociatively adsorbed water not only at the surface of the nanoparticles but also in their volume that lead to changes in the oxide matrix structure. These processes dependent on the composition of nanooxides are much stronger for nanosilica than for alumina or composite oxides. The morphology of primary nanoparticles is more stable on different treatments than the structure of secondary and ternary particles. The amounts of water adsorbed onto the nanooxides from air correspond to the amounts of water strongly bound (unfrozen at T < 273 K) to the oxide surfaces in aqueous suspensions.     

Fabrication and structural control of anodic alumina films with inverted cone porous structure using multi-step anodizing

Porous anodic alumina (PAA) film has recently attracted much attention as a key material for the fabrication of various nanostructures. In this study, a multi-step anodization and leaching process was employed to produce three-dimensional nanometer scale structured film. During the leaching process, the porous alumina film was dipped in phosphoric acid solution for pore widening. Each anodization process was followed by this leaching process. This method produced alumina film with multi-step structure. Meanwhile, with five-step film production, the structure showed inverted cone structure. We produced the low aspect ratio pores of this structure, which would be applicable for fabrications of nanomaterials. In addition, the aspect ratio was controlled by changing the anodization duration.     

Preparation of mesoporous NiO with a bimodal pore size distribution and application in electrochemical capacitors

Mesoporous nickel oxide with a porous structure exhibiting a bimodal pore size distribution (2.6 and 30.3 nm diameter pores) has been synthesized in this paper. Firstly, a mesoporous precursor of coordination complex Ni₃(btc)₂·12H₂O (btc = 1,3,5-benzenrtricarboxylic acid) is synthesized based on the metal-organic coordination mechanism by a hydrothermal method. Then mesoporous NiO with a bimodal size distribution is obtained by calcining the precursor in the air, and characterized by transmission electron microscopy and N₂ adsorption measurements. Such unique multiple porous structure indicates a promising application of the obtained NiO as electrode materials for supercapacitors. The electrochemical behavior has been investigated by cyclic voltammogram, electrochemical impedance spectra and chronopotentiometry in 3 wt.% KOH aqueous electrolyte. The results reveal that the prepared NiO has high-capacitance retention at high scan rate and exhibits excellent cycle-life stability due to its special mesoporous character with bimodal size distribution.     

Tailored pore structures and mechanical properties of porous alumina ceramics prepared with corn cob pore-forming agent

In this work, the effects of porosity and different particle sizes of pore-forming agent on the mechanical properties of porous alumina ceramics have been reported. Different grades of porous alumina ceramics were developed using corn cob (CC) of different weight contents (5, 10, 15, and 20 wt%) and particle sizes (<63 µm, 63-125 µm and 125-250 µm) as the pore-forming agent. Experimental results showed that total porosity and pore cavity size of the porous alumina ceramics increased with rising addition of CC pore former. Total porosity increased with increasing particle size of CC with the Al₂O₃-^<63CC₅ sample exhibiting the lowest total porosity of 41.3 vol% while the highest total porosity of 68.1 vol% was exhibited by the Al₂O₃-^125-250CC₂₀. The particle size effect of CC on the mechanical properties revealed that diametral tensile strength and hardness of the porous alumina ceramics deteriorated with increasing particle size of CC pore former. The Al₂O₃-^<63CC₅ sample exhibited the highest diametral tensile strength and hardness of 25.1 MPa and 768.2 HV, respectively, while Al₂O₃-^125-250CC₂₀ exhibited the lowest values of 1.1 MPa and 35.9 HV. Overall, porous alumina ceramics with the smallest pore sizes under each particle size category exhibited superior mechanical properties in their respective categories.     

Processing and properties of low cost macroporous alumina ceramics with tailored porosity and pore size fabricated using rice husk and sucrose

The present study demonstrates a cost effective way to fabricate porous ceramics with tailored microstructures using rice husk (RH) of various range of particle sizes as a pore former and sucrose as a binder as well as a pore former. Sample microstructures reveal randomly oriented elongated coarse pores and fine pores (avg. size 4 μm) created due to burnout of RH and sucrose, respectively. Porous alumina ceramics with 20–66 vol% porosity and 50–516 μm avg. pore size (length), having isolated and/or interconnected pores, were fabricated using this process. Mechanical properties of the porous samples were determined as a function of porosity and pore microstructure. The obtained porous ceramics exhibited flexural strength of 207.6–22.3 MPa, compressive strength of 180–9.18 MPa, elastic modulus of 250–18 GPa and hardness of 149–18 HRD. Suggested application area includes thermal, filtration, gas purging etc.     

Mesoporous alumina (I): Comparison of synthesis schemes using anionic, cationic, and non-ionic surfactants

A series of mesoporous alumina was prepared using a selected group of anionic, non-ionic, and cationic surfactants with Al-tri-sec-butoxide or Al³⁺ in organic solvent with stoichiometric amount of water, and in aqueous solution with different hydrolyzing agents, or with complexing agent at room temperature to 100 °C. A comparison of the physicochemical properties of the materials prepared was made with respect to surface area, thermal stability, and porosity. Anionic surfactants in aqueous solution produced thermally unstable materials but in organic solvent resulted in a moderately stable alumina phase. Both cationic and non-ionic surfactants produced thermally stable mesoporous alumina after removal of the surfactant upon calcination at 500 °C when the materials were synthesized in organic solvents. Overall, mesoporous alumina prepared with cationic cetyltrimethylammonium bromide in sec-butanol in the optimized substrate composition of Al:surfactant:H₂O:solvent = 1.0:0.3:2.0:15 exhibited the best textural property among the various synthesis systems investigated.     

Polyoxymethylene/polyurethane/alumina ternary composites: Structure,mechanical, thermal and dielectric properties

Ternary composites composed of polyoxymethylene (POM), polyurethane (PU), and boehmite alumina were produced by melt blending with and without latex precompounding. Latex precompounding served for the predispersion of the alumina particles. The related masterbatch (MB) was produced by mixing the PU latex with water‐dispersible boehmite alumina. The dispersion of the alumina was studied by transmission and scanning electron microscopy techniques (TEM and SEM, respectively) and discussed. The crystallization of POM was inspected by means of differential scanning calorimetry (DSC) and polarized optical microscopy (DSC and polarized light microscopy, respectively). The mechanical and thermomechanical properties of the composites were determined in uniaxial tensile, dynamic‐mechanical thermal analysis (DMTA), short‐time creep tests (performed at various temperatures), and thermogravimetric analysis (TGA). The melt flow of the composites was characterized in a plate/plate rheometer. In addition, the dielectric response of the nanocomposites was investigated by means of broadband dielectric spectroscopy at an ambient temperature. The composites produced by the MB technique outperformed the direct melt (DM) compounded composites in respect to the thermal and mechanical characteristics. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Electrochemical synthesis of nickel hexacyanoferrate nanoarrays with dots, rods and nanotubes morphology using a porous alumina template

Transition metal hexacyanoferrate (MeHCF) have attracted extensive attention because of their outstanding properties including, electrocatalysis, molecular magnetism, biosensing and ion-exchange. This paper describes an approach for fabrication of ordered nanoarrays of Ni hexacyanoferrate (NiHCF) structures with different morphologies such as dots, rods and tubes in order to advance their properties and applications. The method is based on the conversion of Ni into NiHCF nanostructures by electrochemical oxidation in the presence of hexacyanoferrate ions, using nanoporous anodic alumina oxide (AAO) as a template. The structure and morphology of formed Ni and NiHCF nanoarrays were confirmed by scanning electron microscopy (SEM), showing agreement with the pore structures of the AAO template. The electrocatalytic activity of NiHCF nanorod array electrodes showed high catalytic properties for the detection of hydrogen peroxide and the potential to be used as a platform for direct biosensing applications. The ion-exchange ability of fabricated NiHCF nanostructures (nanorods and nanotubes) toward alkali cations such as Na⁺ has been successfully confirmed.     

Mullite Alumina Particulate Composites by Infiltration Processing: II, Infiltration and Characterization

Mullite/alumina composites were fabricated by infiltrating porous alumina preforms with a hydrolyzed ethyl silicate sol. Evidence is presented which suggests that initial infiltration occurred without complete filling of the porosity by the sol. Multiple infiltrations were used to increase the amount of SiO₂ introduced but led to blockage of the pores in the surface of the preform. Sintered bodies had concentration gradients, SiO₂ decreasing from the surface inward. Although mullite limited grain growth in alumina, in partially modified bodies large grains (>1 mm) with a preferred orientation were observed at the interface between the two zones.     

Fibrous monolithic ceramic with a single alumina phase: Fracture and high-temperature tribological behaviors

Fabrication of fibrous monolithic ceramic with bamboo-like structures is a promising method to improve the mechanical properties of ceramics through extrinsic reinforcement. Nevertheless, heterogeneous boundaries are easily oxidized at high temperatures, which seriously limits the long-term use of these materials when employed in high-temperature and high/low-temperature alternating environments. In this study, a “plain” ceramic—a single-component and complex-structure Al₂O₃ ceramic—was successfully designed and prepared using nano-sized Al₂O₃ as polycrystalline fibers and micro-sized Al₂O₃ as boundaries to obtain a structure with a fibrous monolithic architecture. Self-toughening of Al₂O₃ ceramics can be achieved by introducing hierarchical architectures derived from the difference between grain sizes of fibers and boundaries, which gives the ceramics high fracture toughness and reliability. Moreover, the material demonstrated a low friction coefficient and high wear-resistance properties when coupled with C/C composites at room temperature, 800°C, and in the alternating temperature enviroment between room temperature and 800°C.     

Silica nanoboxes from alumina rich zeolites: thermal and chemical stability of the monomodal and bimodal materials

Silica nanoboxes synthesized from alumina-rich zeolites, showed two distinct categories of nano-structured materials. Entirely mesoporous nanoboxes (monomodal Al-nanoboxes) were highly thermally and chemically resistant even in the acidic form whereas calcination at high temperature of materials still containing some zeolite remnants (bimodal Al-nanoboxes), resulted in dramatic loss of surface area and pore volume. Pore closure by mobile and amorphous aluminic species was believed to occur. The high thermal and chemical stability of the monomodal Al-nanoboxes was found to be related to the highly siliceous character of the mesopore walls which contained isolated tetrahedral Al atoms linked to tetrahedral Si atoms. Treatment of the acid form of the bimodal nanoboxes with La or Ce containing solutions resulted in quite thermally stable materials owing to the reduction of the number of protonic sites by the rare-earth metal ions.     

Morphology of sodium salt of calf thymus DNA on mica,alumina, and silica surfaces: Effect of solvent and drying method

ABSTRACT

Investigation of morphology of deoxyribonucleotide triphosphate (DNA) dried on different surfaces by atomic force microscopy (AFM) is important in DNA research that is focused on subjects of condensation for gene therapy, sizing, DNA mapping, and cancer examination. The solvent, the surface type, and the method of drying effect the morphology of DNA on solid surfaces. Ethanol and water were used as solvents, flat mica, silica, and alumina surfaces were used as the substrates in the present study. Different methods such as ambient air-drying, N₂-forced flow regime drying, and freeze-drying have been applied to droplets of DNA solutions in water or ethanol on the substrates. Forced flow drying regime causes nonlinear DNA attachment on the surface and self-assembly. DNA vertical distance on mica surface was found to be 6 and 1.4?nm for DNA dried in ambient air from ethanol and water solutions, respectively. It was 1.6?nm for N₂ flow drying of aqueous DNA solution on mica surface. It was 4.6, 4.6, and 1.99?nm for ambient, N₂ flow, and freeze-dried aqueous DNA on alumina surfaces, respectively. Aqueous solution of DNA dried under N₂ flow on silica surface had 0.8?nm vertical distance. The smallest standard deviation of 0.05?nm was observed for DNA dried under N₂ flow on alumina surface.     

Dispersion characteristics of magnetic particles: Surface charge, surface adsorption and acid-base interaction behavior

Electrophoretic mobility (EM) of magnetic oxide particles has been measured in aqueous as well as organic solvent media using a zeta meter and a mass transporter analyzer. EM has also been measured for the magnetic particles after treatment with surface active compounds and/or in the presence of a surfactant. The results show that the sign and magnitude of the EM values change depending on the type and polarity of the surfactants or surface-treating compounds. The sign reversal of the EM values when the medium is changed from water to organic solvent can be understood on the basis of acid-base interaction. The potential energy between particles calculated using the maximum available EM value in an organic solvent is far below the value required for dispersion stability. These results along with the calculation o magnetic potential energy show that the stability of these dispersions cannot be maintained by electrostatic potential alone. Treatment of these oxide particles with surface active compounds provide stable dispersions by a ‘stearic stabilization’ mechanism. Adsorption of surfactants such as organic phosphate compounds and binder resins such as nitrocellulose or polyurcthanes on magnetic oxide particles is due to acid-base interfacial interaction between oxide particles, organic macromolecules, and solvents. Adsorption of these macromolecules in multilayers seems to be a major cause for high dispersion viscosity and the poor magnetic properties of these dispersions on tapes. These results indicate flocculation of the particles, possibly by a bridging mechanism. Thus, surface treatment of oxide particles with proper compounds inhibits adsorption of the binder resins in multilayers, promotes better rheological properties of the formulated grinds, and improves magnetic performance of tapes coated with these grinds.