Surface properties of a new lithium disilicate glass-ceramic after grinding.

This study aimed to evaluate the effect of grinding on some surface properties of two lithium disilicate-based glass-ceramics, one experimental new product denominated LaMaV Press (UFSCar-Brazil) and another commercial known as IPS e-max Press (Ivoclar), in the context of simulated clinical adjustment. Discs (N = 24, 12 mm in diameter) were separated into four groups: LaMaV Press with no grinding (E), LaMaV Press after grinding (EG), IPS e-max Press with no grinding (C), and IPS e-max Press after grinding (CG). A 0.1-mm deep grinding was carried out on EG and CG samples (final thickness of 1.4 mm) using a diamond stone in a low-speed device. The E and C samples had the same thickness. The effect of grinding on the sample surfaces was evaluated by X-ray diffraction, mechanical and optical profilometry, scanning electron microscopy, goniometry, and Vickers hardness. The mean roughness (Ra) was evaluated by Kruskal-Wallis and Student-Newman-Keuls statistics. The surface energy (SE) by the sessile drop method and Vickers hardness (VH) were analyzed using two-way ANOVA. The Ra medians were E = 1.69 µm, EG = 1.57 µm, C = 1.45 µm, and CG = 1.13 µm with p = 0.0284. The SE and VH were similar for all materials and treatments. Grinding smoothed the surfaces and did not significantly alter the hardness and surface energy of both LaMaV Press and IPS e-max Press. These glass-ceramics presented similar surface properties, and clinical adjustments can be implemented without loss of performance of both materials. A grinding standardization device developed that allowed to control the amount of grinding, the speed of rotation speed and the force exerted on the samples.

Enhanced model protein adsorption of nanoparticulate hydroxyapatite thin films on silk sericin and fibroin surfaces.

Hydroxyapatite coated metallic implants favorably combine the required biocompatibility with the mechanical properties. As an alternative to the industrial coating method of plasma spraying with inherently potential deleterious effects, sol-gel methods have attracted much attention. In this study, the effects of intermediate silk fibroin and silk sericin layers on the protein adsorption capacity of hydroxyapatite films formed by a particulate sol-gel method were determined experimentally. The preparation of the layered silk protein/hydroxyapatite structures on glass substrates, and the effects of the underlying silk proteins on the topography of the hydroxyapatite coatings were described. The topography of the hydroxyapatite layer fabricated on the silk sericin was such that the hydroxyapatite particles were oriented forming an oriented crystalline surface. The model protein (bovine serum albumin) adsorption increased to 2.62 µg/cm2 on the latter surface as compared to 1.37 µg/cm2 of hydroxyapatite on glass without an intermediate silk sericin layer. The BSA adsorption on glass (blank), glass/c-HAp, glass/m-HAp, glass/sericin/c-HAp, and glass/sericin/m-HAp substrates, reported as decrease in BSA concentration versus contact time.

In-vitro bioactivity of silicate-phosphate glasses using agriculture biomass silica.

In the present work, silica extracted from the agricultural waste material; rice husk (RH) was utilized for the synthesis of biocompatible glass of general composition SiO2-P2O5-CaO-MgO-MoO3. In the synthesized glasses P2O5 (5%) and CaO (25%) was kept constant whereas MgO and MoO3 was varied from 10% to 20% and 0% to 5% respectively. The structural, morphological, elemental and functional properties of silica as well as the derived glasses were analyzed by X-Ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Energy Dispersive X-ray spectroscopy (EDX) and Fourier Transform Infrared (FTIR) spectroscopy techniques. The effect of MoO3 on the structural and thermal properties of silicate phosphate glasses has been studied in details. The bioactivity of as-synthesized glass samples were further evaluated after immersion in Simulated Body Fluid (SBF) solution which shows bioactive properties thus enabling them to be used as scaffolds in implant materials.

3D printing of an integrated triphasic MBG-alginate scaffold with enhanced interface bonding for hard tissue applications.

Osteochondral defects affect both of cartilage and subchondral areas, thus it poses a significant challenge to simultaneously regenerate two parts in orthopedics. Tissue engineering strategy is currently regarded as the most promising way to repair osteochondral defects. This study focuses on developing a multilayered scaffold with enhanced interface bonding through 3D printing. One-shot printing process enables control over material composition, pore structure, and size in each region of the scaffold, while realizes seamlessly integrated construct as well. The scaffold was designed to be triphasic: a porous bone layer composed of alginate sodium (SA) and mesoporous bioactive glasses (MBG), an intermediate dense layer also composed of SA and MBG and a cartilaginous layer composed of SA. The mechanical strength including the interface adhesion strength between layers were characterized. The results indicated that SA crosslinking after 3D printing anchored different materials together and integrated all regions. Additional scaffold soaking in simulated body fluid (SBF) and cell culture medium induced apatite deposition and had weakened the compressive and tensile strengths, while no layer dislocation or delamination occurred.

Effect of ethanol/TEOS ratios and amount of ammonia on the properties of copper-doped calcium silicate nanoceramics.

Calcium magnesium silicate glasses could be suggested for the synthesis of scaffolds for hard tissue regeneration, as they present a high residual glassy phase, high hardness values and hydroxyapatite-forming ability. The use of trace elements in the human body, such as Cu, could improve the biological performance of such glasses, as Cu is known to play a significant role in angiogenesis. Nano-bioceramics are preferable compared to their micro-scale counterparts, because of their increased surface area, which improves both mechanical properties and apatite-forming ability due to the increased nucleation sites provided, their high diffusion rates, reduced sintering time or temperature, and high mechanical properties. The aim of the present work was the evaluation of the effect of different ratios of Ethanol/TEOS and total amount of the inserted ammonia to the particle size, morphology and bioactive, hemolytic and antibacterial behavior of nanoparticles in the quaternary system SiO2-CaO-MgO-CuO. Different ratios of Ethanol/TEOS and ammonia amount affected the size and morphology of bioactive nanopowders. The optimum materials were synthesized with the highest ethanol/TEOS ratio and ammonia amount as verified by the enhanced apatite-forming ability and antibacterial and non-hemolytic properties.

Hydrated Zinc Borates and Their Industrial Use.

Zinc borates are important chemical products having industrial applications as functional additives in polymers, bio-composites, paints and ceramics. Of the thirteen well documented hydrated binary zinc borates, Zn[B3O4(OH)3] (2ZnO∙3B2O3∙3H2O) is manufactured in the largest quantity and is known as an article of commerce as 2ZnO∙3B2O3∙3.5H2O. Other hydrated zinc borates in commercial use include 4ZnO∙B2O3∙H2O, 3ZnO∙3B2O3∙5H2O and 2ZnO∙3B2O3∙7H2O. The history, chemistry, and applications of these and other hydrated zinc borate phases are briefly reviewed, and outstanding problems in the field are highlighted.

Ferrocene-Based Hyperbranched Polytriazoles: Synthesis by Click Polymerization and Application as Precursors to Nanostructured Magnetoceramics.

Ferrocene-based polymers have drawn much attention in the past decades due to their unique properties and promising applications. However, the synthesis of hyperbranched polymers is still a great challenge. Here, two ferrocene-based hyperbranched polytriazoles with high molecular weights are facilely prepared by the click polymerization reactions of ferrocene-containing diazides (1) and tris(4-ethynylphenyl)amine (2) using Cu(PPh3 )3 Br as catalyst in dimethylformamide at 60 °C for 5 and 9 h in satisfactory yields of 54.0% and 52.3%. The resulting polytriazoles are soluble in common organic solvents and thermally stable, with 5% weight loss temperatures up to 307 °C. They can be used as precursors to produce nanostructured ceramics with good magnetizability by pyrolysis at elevated temperature.

Synthesis of ß-tricalcium phosphate.

Ceramics play a key role in several biomedical applications. One of them is bone grafting, which is used for treating bone defects caused by injuries or osteoporosis. Calcium-phosphate based ceramic are preferred as bone graft biomaterials in hard tissue surgery because their chemical composition is close to the composition of human bone. They also have a marked bioresorbability and bioactivity. In this work, we have developed methods for synthesis of ß-tricalcium phosphate apatite (ß-TCP). These products were characterized by different techniques such as X-ray diffraction, infrared spectroscopy, scanning electron microscopy and chemical analysis.

Bone neoformation of a novel porous resorbable Si-Ca-P-based ceramic with osteoconductive properties: physical and mechanical characterization, histological and histomorphometric study.

OBJECTIVE: The aims of the present work were to study a new porous Nurse's A ceramic (Si-Ca-P-based material) bone substitute and examine its mechanical properties in vitro and the biocompatibility, osteoconductivity and resorption process in vivo. MATERIALS AND METHOD: Porous ceramic scaffolds were prepared by solid-state reaction and implanted in critical-sized defect created in 15 NZ rabbits. Strength values were determined by the diametrical compression of disk test. Weibull analyses were performed following the European Standard for technical ceramics EN-843-5: 1996, considering 90% of confidence intervals. Results were correlated with scanning microscope observations of fracture surfaces. Implanted scaffolds were characterized by histological and histomorphometric point of view. RESULTS: The parameters of the Weibull distribution of strength, determined by diametrical compression of disks, were modulus m = 13, and characteristic strength σ0  = 0.60 MPa (90% confidence limit: m = 7.2-17.6, σ0  = 0.570-0.578). Porous calcium silicophosphate scaffolds showed significantly more bone formation in the pores and in the periphery of the implant than the control group. Histomorphometric analysis revealed that the ceramic scaffold (62.23 ± 0.34*) produced higher values of bone-to-implant contact (BIC) percentages (higher quality, closer contact); moreover, defect closure was significative in relation with control group. CONCLUSIONS: The porous calcium silicophosphate ceramic is biocompatible, partially resorbable and osteoinductive material. This rabbit study provides radiological and histological evidences confirming the suitablity of this new material for bone tissue regeneration on critical defects.

Effects of Fuel to Synthesis of CaTiO3 by Solution Combustion Synthesis for High-Level Nuclear Waste Ceramics.

A solution combustion process for the synthesis of perovskite (CaTiO3) powders is described. Perovskite is one of the crystalline host matrics for the disposal of high-level radioactive wastes (HLW) because it immobilizes Sr and Lns elements by forming solid solutions. Solution combustion synthesis, which is a self-sustaining oxi-reduction reaction between nitrate and organic fuel, the exothermic reaction, and the heat evolved convert the precursors into their corresponding oxide products above 1100 degrees C in air. To investigate the effects of amino acid on the combustion reaction, various types of fuels were used; a glycine, amine and carboxylic ligand mixture. Sr, La and Gd-nitrate with equivalent amounts of up to 20% of CaTiO3 were mixed with Ca and Ti nitrate and amino acid. X-ray diffraction analysis, SEM and TEM were conducted to confirm the formed phases and morphologies. While powders with an uncontrolled shape are obtained through a general oxide-route process, Ca(Sr, Lns)TiO3 powders with micro-sized soft agglomerates consisting of nano-sized primary particles can be prepared using this method.

Synthesis and Characterization of a Novel Borazine-Type UV Photo-Induced Polymerization of Ceramic Precursors.

A preceramic polymer of B,B',B''-(dimethyl)ethyl-acrylate-silyloxyethyl-borazine was synthesized by three steps from a molecular single-source precursor and characterized by Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) spectrometry. Six-member borazine rings and acrylate groups were effectively introduced into the preceramic polymer to activate UV photo-induced polymerization. Photo-Differential Scanning Calorimetry (Photo-DSC) and real-time FTIR techniques were adapted to investigate the photo-polymerization process. The results revealed that the borazine derivative exhibited dramatic activity by UV polymerization, the double-bond conversion of which reached a maximum in 40 s. Furthermore, the properties of the pyrogenetic products were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD), which proved the ceramic annealed at 1100 °C retained the amorphous phase.

Smart soft-templating synthesis of hollow mesoporous bioactive glass spheres.

Hollow bioactive glass spheres with mesoporous shells were prepared by using dual soft templates, a diblock co-polymer poly(styrene-b-acrylic acid) (PS-b-PAA) and a cationic surfactant cetyltrimethylammonium bromide (CTAB). Hollow mesoporous bioactive glass (HMBG) spheres comprise the large hollow interior with vertical mesochannels in shell, which realize large uptake of drugs and their sustained release. The formation of hydroxyapatite layer on the surface of HMBG particles shows the clear evidence for promising application in bone regeneration.

Surface-initiated anionic polymerization of [1]silaferrocenophanes for the preparation of colloidal preceramic materials.

A novel strategy for the preparation of poly(ferrocenylsilane) (PFS) immobilized on the surface of cross-linked polystyrene (PS) nanoparticles is reported. The ferrocene-containing core/shell architectures are shown to be excellent candidates as preceramic polymers yielding spherical ceramic materials consisting of iron silicide (Fe3 Si) and metallic iron after thermal treatment. For this purpose, dimethyl- and hydromethyl[1]silaferrocenophane monomers are polymerized by surface-initiated ring-opening polymerization upon taking advantage of residual vinylic moieties at the PS particle surface. A strategy for selective chain growth from the particle surface is developed without the formation of free PFS homopolymer in solution. The grafted particles are characterized using transmission electron microscopy (TEM) and dynamic light scattering (DLS). These particles are excellent precursors for ceramics as studied by thermogravimetric analysis (TGA). The composition of the ceramics is studied using X-ray diffraction (XRD) measurements, while the morphology is probed by scanning electron microscopy (SEM) revealing the original spherical shape of the precursor particles. Obtained ceramic materials- predominantly based on iron silicides-show ferromagnetic behavior as investigated by superconducting quantum interference device (SQUID) magnetization measurements at different temperatures.

Smart scaffolds: the future of bioceramic.

The commercial offer for bioceramic bone substitutes is very large, however, the prerequisites for applications in bone reconstruction and tissue engineering, are most often absent. The main criteria being: on the one hand physico-chemical features providing surgeons with an injectable and/or shapeable biomaterial; on the second hand the multi-scale bioactivity leading to osteoconduction and osteoinduction properties. In order to obtain greater suitability according to the nature of the bone defect to be treated, new bone regeneration technologies, "smart scaffolds" must be developed and optimize to support suitable Ortho Biology.

Biomimetic apatite-based composite materials obtained by spark plasma sintering (SPS): physicochemical and mechanical characterizations.

Nanocrystalline calcium phosphate apatites are biomimetic compounds analogous to bone mineral and are at the origin of the bioactivity of most biomaterials used as bone substitutes. Their unique surface reactivity originates from the presence of a hydrated layer containing labile ions (mostly divalent ones). So the setup of 3D biocompatible apatite-based bioceramics exhibiting a high reactivity requests the development of «low¼ temperature consolidation processes such as spark plasma sintering (SPS), in order to preserve the characteristics of the hydrated nanocrystals. However, mechanical performances may still need to be improved for such nanocrystalline apatite bioceramics, especially in view of load-bearing applications. The reinforcement by association with biopolymers represents an appealing approach, while preserving the advantageous biological properties of biomimetic apatites. Herein, we report the preparation of composites based on biomimetic apatite associated with various quantities of microcrystalline cellulose (MCC, 1-20 wt%), a natural fibrous polymer. The SPS-consolidated composites were analyzed from both physicochemical (X-ray diffraction, Fourier transform infrared, solid state NMR) and mechanical (Brazilian test) viewpoints. The preservation of the physicochemical characteristics of apatite and cellulose in the final material was observed. Mechanical properties of the composite materials were found to be directly related to the polymer/apatite ratios and a maximum crushing strength was reached for 10 wt% of MCC.

Crown fracture: Failure load, stress distribution, and fractographic analysis.

STATEMENT OF PROBLEM: The outcomes from load-to-failure tests may not be applicable to clinical situations. PURPOSE: The purpose of this study was to critically evaluate the efficacy of load-to-failure tests in the investigation of the fracture load and pattern of metal-free crowns. MATERIAL AND METHODS: Four groups were formed from 128 bovine roots restored with metal posts, resin cores, and feldspathic, leucite, or lithium disilicate ceramic systems or polymer crowns. Each group was divided into 4 (n=8) according to the cement: zinc phosphate, self-adhesive resin, autopolymerizing resin, and glass ionomer. Mean fracture loads from compressive tests were submitted to ANOVA and Tukey HSD test. Finite element and fractographic analyses were performed and associated with the fracture load and pattern. RESULTS: Significantly higher fracture load values were obtained for the lithium disilicate ceramic, but finite element and fractographic analyses showed that the cement effect could not be determined. The finite element analysis showed the cement likely affected the fracture pattern, confirmed that stresses in the cements were little affected by the crown materials, and found that the stressed conditions were lowest in the lithium disilicate compared with other crowns for all cement combinations. The stressed conditions in the crowns depended more on the adhesive properties than on the elastic modulus of the cement materials. The level of the stressed condition in the crowns at the occlusal surface was about the same or higher than along their cement interface, consistent with the fractography, which indicated fractures starting at the load point. Higher stress levels in the crowns corresponded with a lower number of catastrophic fractures, and higher stresses in the cements seemed to reduce the number of catastrophic fracture patterns. The highest stressed conditions occurred along the occlusal surface for crown materials with a low elastic modulus or in combination with adhesive cements. CONCLUSIONS: The method used was not appropriate either for investigating the crowns' fracture load and pattern or for stating the role of the cements within the crown-cement-tooth interaction.

The recycling of incinerated sewage sludge ash as a raw material for CaO-Al2O3-SiO2-P2O5 glass-ceramic production.

In this paper, the recycling of incinerated sewage sludge ash (ISSA) into glass-ceramic materials by a two-stage sintering cycle of nucleation stage and crystallization stage without any pressure and binder is presented. The parent glasses were subjected to the following nucleation/crystallization temperature and time level: (A) 790°C, 1.0 h/870°C, 1.0-3.0 h; (B) 790°C, 1.0 h/945°C, 1.0-3.0 h and (C) 790°C, 1.0 h/1065°C, 1.0-3.0 h. X-ray power diffraction analysis results revealed that multiple crystalline phases coexisted in the glass-ceramic materials and the crystalline phase compositions were more affected by crystallization temperature than crystallization time. Scanning electron microscopy analysis showed an interlocking microstructure of glass phases and crystals with different sizes and spatial distribution. The glass-ceramics crystallized at 945°C for 2.0 h exhibited optimal properties of density of 2.88±0.08 g/cm3, compression strength of 247±12 MPa, bending strength of 118±14 MPa and water absorption of 0.42±0.04. The leaching concentrations of heavy metals were far lower than the limits required by the regulatory standard of EPA. This paper provides a feasible, low-cost and promising method to produce ISSA-based glass-ceramics and highlights the principal characteristics that must be taken into account to use ISSA correctly in glass-ceramics.

Contribution to the sustainable management of resources by novel combination of industrial solid residues into red ceramics.

Limited amounts of industrial residues are recycled while the remaining huge quantities are stockpiled or disposed of, thus frequently leading to soil contamination. The utilization of industrial residues as valuable secondary resources into ceramics can contribute to efficient waste management and substitution for massive amounts of natural resources (clayey minerals) demanded for ceramic production. The low cost of these residues and even possible energy savings during mixture firing may also be beneficial. In the present study, the innovative combination of lignite fly ash with steel-making dust into clay-based red ceramics is undertaken, to contribute both to sustainable use of resources and prevention of soil contamination. Brick specimens were shaped by extrusion and fired, their microstructure was examined and the effect of the mixture composition and firing temperature on physico-mechanical properties was determined. Ceramic microstructures were successfully obtained by a suitable combination of fly ash with steel dust (5 + 5 wt%) into clays. Properties can be predicted and tailored to meet the needs for specific applications by appropriately adjusting the mixture composition and sintering temperature.

Synthesis and characterization of visible-to-UVC upconversion antimicrobial ceramics.

The objective of this study was to develop visible-to-ultraviolet C (UVC) upconversion ceramic materials, which inactivate surface-borne microbes through frequency amplification of ambient visible light. Ceramics were formed by high-temperature sintering of compacted yttrium silicate powders doped with Pr(3+) and Li(+). In comparison to previously reported upconversion surface coatings, the ceramics were significantly more durable and had greater upconversion efficiency under both laser and low-power visible light excitation. The antimicrobial activity of the surfaces under diffuse fluorescent light was assessed by measuring the inactivation of Bacillus subtilis spores, the rate of which was nearly 4 times higher for ceramic materials compared to the previously reported films. Enhanced UVC emissions were attributed to increased material thickness as well as increased crystallite size in the ceramics. These results represent significant advancement of upconversion surfaces for sustainable, light-activated disinfection applications.

Osteopontin, osteocalcin and OB-cadherin expression in Synthetic nanohydroxyapatite vs bovine hydroxyapatite cultured Osteoblastic-like cells.

Calcium phosphate ceramics have been applied in bone replacement for several decades due to their excellent biocompatibility, bioactivity, osteo-conductivity and mechanical strength. Several studies have demonstrated that porous hydroxyapatite (HA) is an excellent scaffold for osteogenic proliferation and differentiation of the osteoprogenitor cells. However, different methods of synthesis and production of HA ceramic-based materials may have considerable effect on the physical and biological properties. In the present work, two hydroxyapatite-based materials, a natural hydroxyapatite ceramic of bovine origin and a synthetic nano-cristalline hydroxyapatite were tested in vitro with MG63 cell line. The results displayed that both the materials demonstrated a good biocompatibility. The immunocytochemical stain revealed a different positivity of the osteogenic markers between the cultures with the biomaterials, and the control culture. Western blot data confirmed the immunocytochemical stain. Both the materials tested in the present study demonstrated a good biocompatibility with the osteoblastic cells allowing, at the same time, the osteogenic differentiation, and they may be useful in clinical use.