Sanosh Kunjalukkal Padmanabhan

Micro-indentation fracture behavior of human enamel

OBJECTIVE The purpose of this study was to determine the crack resistance behavior (K(R)) of human enamel in relation to its microstructure. METHODS Human molar teeth were precision cut, polished and tested using Vickers micro-indentation at different loads ranging from 0.98 to 9.8 N. Five indentation load levels were considered, 20 indentation cracks for each load level were introduced on the surface of the test specimen (10 indentations per tooth) and their variability was evaluated using Weibull statistics and an empirical model. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used to analyze the crack morphology and propagation mechanisms involved. RESULTS The results showed that enamel exhibited increasing cracking resistance (K(R)) with increasing load. It was found that the crack propagation mainly depended on the location and the microstructure it encountered. SEM showed the formation of crack bridges and crack deflection near the indentation crack tip. The crack mode was of Palmqvist type even at larger loads of 9.8 N. This was mainly attributed to the large process zone created by the interwoven lamellar rod like microstructure exhibited by the enamel surface. SIGNIFICANCE This study shows that there are still considerable prospects for improving dental ceramics and for mimicking the enamel structure developed by nature.

Scaffolds for bone regeneration made of hydroxyapatite microspheres in a collagen matrix.

Biomimetic scaffolds with a structural and chemical composition similar to native bone tissue may be promising for bone tissue regeneration. In the present work hydroxyapatite mesoporous microspheres (mHA) were incorporated into collagen scaffolds containing an ordered interconnected macroporosity. The mHA were obtained by spray drying of a nano hydroxyapatite slurry prepared by the precipitation technique. X-ray diffraction (XRD) analysis revealed that the microspheres were composed only of hydroxyapatite (HA) phase, and energy-dispersive x-ray spectroscopy (EDS) analysis revealed the Ca/P ratio to be 1.69 which is near the value for pure HA. The obtained microspheres had an average diameter of 6 μm, a specific surface area of 40 m(2)/g as measured by Brunauer-Emmett-Teller (BET) analysis, and Barrett-Joyner-Halenda (BJH) analysis showed a mesoporous structure with an average pore diameter of 16 nm. Collagen/HA-microsphere (Col/mHA) composite scaffolds were prepared by freeze-drying followed by dehydrothermal crosslinking. SEM observations of Col/mHA scaffolds revealed HA microspheres embedded within a porous collagen matrix with a pore size ranging from a few microns up to 200 μm, which was also confirmed by histological staining of sections of paraffin embedded scaffolds. The compressive modulus of the composite scaffold at low and high strain values was 1.7 and 2.8 times, respectively, that of pure collagen scaffolds. Cell proliferation measured by the MTT assay showed more than a 3-fold increase in cell number within the scaffolds after 15 days of culture for both pure collagen scaffolds and Col/mHA composite scaffolds. Attractive properties of this composite scaffold include the potential to load the microspheres for drug delivery and the controllability of the pore structure at various length scales.

Development and Mechanical Characterization of a Collagen/Hydroxyapatite Bilayered Scaffold for Ostechondral Defect Replacement

In this work a novel three-dimensional ostechondral substitute is proposed that is made of an inorganic/organic hybrid material, namely collagen/hydroxyapatite. The two components of the substitute have been characterized separately. The inorganic part, a hydroxyapatite scaffold, was fabricated by a polymer sponge templating method using a reactive sub-micron powder synthesized in our laboratory by hydroxide precipitation sol-gel route. The organic part, a collagen scaffold, was fabricated by a freeze-dying technique varying design parameters. Both the parts were analysed by scanning electron microscopy and their mechanical properties assessed by compression tests. The hydroxyapatite scaffold showed a high and highly interconnected porosity and a mechanical strength equal to 0.55 MPa, higher than those reported in literature. The collagen scaffolds were seeded by chondrocytes, processed for histology analysis and tested in compression. The biological tests proved the ability of the scaffolds to be positively populated by chondrocytes and the mechanical analysis showed that the mechanical strength of the scaffolds significantly increased after 3 weeks of culture.

Synthesis and Characterization of Mixed Iron-Manganese Oxide Nanoparticles and Their Application for Efficient Nickel Ion Removal from Aqueous Samples

Mixed iron-manganese oxide nanoparticles, synthesized by a simple procedure, were used to remove nickel ion from aqueous solutions. Nanostructures, prepared by using different weight percents of manganese, were characterized by transmission electron microscopy, selected area diffraction, X-ray diffraction, Raman spectroscopy, and vibrating sample magnetometry. Adsorption/desorption isotherm curves demonstrated that manganese inclusions enhance the specific surface area three times and the pores volume ten times. This feature was crucial to decontaminate both aqueous samples and food extracts from nickel ion. Efficient removal of Ni2+ was highlighted by the well-known dimethylglyoxime test and by ICP-MS analysis and the possibility of regenerating the nanostructure was obtained by a washing treatment in disodium ethylenediaminetetraacetate solution.

Mechanical Performance and In Vitro Studies of Hydroxyapatite/Wollastonite Scaffold for Bone Tissue Engineering

A highly porous (~90%) interconnected hydroxyapatite/wollastonite (HA/WS) scaffolds were prepared by polymeric sponge replica method using a slurry containing HA:Calcium silicate in the weight ratio of 50:50 and sintered at 1300 °C. The phase purity of the scaffolds were analyzed by using XRD. The pore size, pore structure, microstructure and elemental analysis of the scaffolds before and after SBF soaking were analyzed using SEM and EDS. In-vitro bioactivity and bioresorbability confirmed the feasibility of the developed scaffolds. The HA/WS scaffold shows two fold increase in the compressive strength compared to pure HA scaffold.

Strategies to Improve Bioactivity of Hydroxyapatite Bone Scaffolds

Two different approaches are proposed in this study to enhance the bioactivity of hydroxyapatite-based scaffolds for bone tissue regeneration. The first method consists in a structural modification of Hydroxyapatite (HA) through doping it with Magnesium (1,3% wt) while the second one in using HA in combination with a calcium silicate, i.e. Wollastonite (WS), to form a composite bioceramic. Scaffolds with high and strongly interconnected porosity (pores ranging from 300 to 800 µm) were produced throughout both procedures. Higher mechanical properties in compression were obtained when the composite Ws/HA bioceramic was adopted. That one showed a weight loss after 6 months in physiological solution seven times higher than doped HA. Preliminary in vitro tests highlighted that both kinds of scaffold allowed the adhesion of MG63, without significant differences in terms of vitality, indicating a good biocompatibility of both used biomaterials.

Influence of the Precipitation Temperature on Properties of Nanohydroxyapatite Powder for the Fabrication of Highly Porous Bone Scaffolds

The aim of the present work is to study the influence of the precipitation temperature in the synthesis of nanohydroxyapatite (n-HAp) on the properties of the resulting n-HAp powder for the fabrication of highly porous scaffolds for bone tissue engineering. The n-HAp powder was obtained by a wet precipitation technique starting from calcium nitrate tetrahydrate (Ca (NO3)2*4H2O) and phosphoric acid (H3PO4) at different temperatures: 10°C, 37°C and 50°C. Highly porous scaffolds were fabricated using the three different powders by the sponge replica method and sintering at 1300°C. Combined X-ray diffraction (XRD) and transmission electron microscopy (TEM) analyses on powders indicated that on increasing the precipitation temperature the formation of pure n-HAp is accelerated, without significant changes in particles morphology and size. Scaffolds characterized by high porosity (89%) and good compressive strength (0.53 MPa for n-HAp prepared at 37°C) were obtained. XRD analyses on sintered n-HAp confirmed the thermal stability of the material. Therefore, the as-synthesized n-HAp powder can be successfully used for the fabrication of highly porous scaffolds as bone substitutes.