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ABSTRACT: Surface modification of biomaterials has been shown to improve the biological response to dental implants. The ability to create a controlled micro-texture on the implant via additive surface modification techniques with bioactive nanohydroxyapatite (nanoHA) may positively influence guided tissue regeneration.
The main goal of this study was to produce micro-fabricated SiO(2) surfaces modified with nanohydroxyapatite particles and to characterize their influence on the biological response of Human Dental-Pulp Mesenchymal Stem Cells (hDP-MSCs) and Streptococcus mutans.
A combined methodology of sol-gel and soft-lithography was used to produce micropatterned SiO(2) thin films with different percentages of nanoHA micro-aggregates. The surfaces were characterized by SEM/EDS, FT-IR/ATR, AFM, XPS quantitative elemental percentage and contact angle measurements. Biological characterization was performed using hDP-MSCs cultures, while Streptococcus mutans was the selected microorganism to evaluate the bacterial adhesion on the thin films.
Micropatterned SiO(2) surfaces with 0%, 1% and 5% of nanoHA micro-aggregates were successfully produced using a combination of sol-gel and soft-lithography. These surfaces controlled the biological response, triggering alignment and oriented proliferation of hDP-MSCs and significant differences in the adhesion of S. mutans to the different surfaces.
The micropatterned surfaces exhibited biocompatible behavior that induced an oriented adhesion and proliferation of hDP-MSCs while SiO(2) presented low bacterial adhesion. These results show that the combination of sol-gel with soft-lithography is a good approach to create micropatterned surfaces with bioactive nanoparticles for guided tissue regeneration.
Dental materials: official publication of the Academy of Dental Materials 09/2012; 28(12):1250-60. · 2.88 Impact Factor
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ABSTRACT: Taking into account the phase equilibrium relationships within the Ca3(PO4)2-CaSiO3-CaMg(SiO3)2 ternary system, three bioactive glasses with a eutectic composition and analogous amounts of Ca3(PO4)2 (∼40 wt.%) have been prepared. The structure of the glasses was investigated by 31P and 29Si magic angle spinning nuclear magnetic resonance (MAS-NMR) spectroscopy. The glasses exhibited thermal expansion coefficients (50-600 °C) of 11.8-13.3×10(-6) °C(-1), a glass transition temperature of 790-720 °C and a softening temperature of 811-750 °C. The mechanical properties of the glasses were as follows: bending strength ∼100 MPa, Young's modulus 94-83 GPa, Vickers microhardness 7.1-4.1 GPa and toughness 0.8 MPa m1/2. The bioactive properties were discussed in terms of their structure deduced by MAS-NMR spectroscopy and the field strength of the network modifiers (Mg2+ and Ca2+). A knowledge of the glass structure was important in predicting its bioactivity.
Acta biomaterialia 02/2012; 8(2):820-9. · 3.98 Impact Factor
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ABSTRACT: Titanium implants are the gold standard in dentistry; however, problems such as gingival tarnishing and peri-implantitis have been reported. For zirconia to become a competitive alternative dental implant material, surface modification techniques that induce guided tissue growth must be developed.
To develop alternative surface modification techniques to promote guided tissue regeneration on zirconia materials, for applications in dental implantology.
A methodology that combined soft lithography and sol-gel chemistry was used to obtain isotropic micropatterned silica coatings on yttria-stabilized zirconia substrates. The materials were characterized via chemical, structural, surface morphology approaches. In vitro biological behavior was evaluated in terms of early adhesion and viability/metabolic activity of human osteoblast-like cells. Statistical analysis was conducted using one-way ANOVA/Tukey HSD post hoc test.
Isotropic micropatterned silica coatings on yttria-stabilized zirconia substrates were obtained using a combined approach based on sol-gel technology and soft lithography. Micropatterned silica surfaces exhibited a biocompatible behavior, and modulated cell responses (i.e. inducing early alignment of osteoblast-like cells). After 7d of culture, the cells fully covered the top surfaces of pillar microstructured silica films.
The micropatterned silica films on zirconia showed a biocompatible response, and were capable of inducing guided osteoblastic cell adhesion, spreading and propagation. The results herein presented suggest that surface-modified ceramic implants via soft lithography and sol-gel chemistry could potentially be used to guide periodontal tissue regeneration, thus promoting tight tissue apposition, and avoiding gingival retraction and peri-implantitis.
Dental materials: official publication of the Academy of Dental Materials 04/2011; 27(6):581-9. · 2.88 Impact Factor
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ABSTRACT: This research describes the preparation, characterisation and in vitro behavior of a bioactive glass ceramic containing 44.8 wt% apatite, 28.0 wt% wollastonite-2 M and 27.2 wt% of amorphous phase. The biomaterial was obtained by a specific thermal cycle process that caused the devitrification of the Ca 3 (PO 4) 2 –CaSiO 3 binary system's stoichiometric eutectic composition. Overall, the material combines the properties of a resorbable Si–Ca-rich glass, in addition to bioactive properties of wollastonite and apatite phases. The bioactivity of this material was studied by soaking the samples in a simulated body fluid (SFB) for 3, 7, 14 and 21 days at 36.5 • C. During the soaking, the amorphous phase and also wollastonite-2 M phase underwent steady dissolution by releasing Si and Ca ions into the SBF medium. After 7 days, a porous hydroxy-carbonate apatite (HCA) layer was formed at the SBF–glass ceramic interface. The micro-nanostructured apatite–wollastonite-2 M glass ceramics with improved mechanical properties, in comparison with the parent glass, could serve as a promising platform for hard tissue regeneration.
Journal of the European Ceramic Society 01/2011; 31:1549-1561. · 2.35 Impact Factor
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XI Congreso Nacional de Materiales, Zaragoza; 01/2010
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XI Congreso Nacional de Materiales, Zaragoza; 01/2010
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ABSTRACT: This article presents the results of a post-mortem study of various MgO-C and MgO-C-Al pieces that are used in the electric furnaces at the Acerinox factory in Cádiz. From the chemical, thermal, mineralogical and microstructural characterization of the materials prior to use and post-mortem it has been established that, in both types of refractories, the corrosion has lead to the formation of reaction layers with different chemical and mineralogical composition, as a function of temperature and oxygen partial pressure, ranging from the hot to the cold face and strongly depending on the zone of the electric furnace where the piece is situated. Changes in graphite content have been observed in both types of materials by X-ray diffraction. These changes have been quantified by Differential Thermal Analysis. In MgO-C-Al refractories it has been observed the formation of small amounts of C3Al4 inside the pieces and MgAl2O4 in the refractories’ hot face. Keeping in mind the obtained results and the phase equilibrium diagram of Mg-C-Al-O it has been established a corrosion mechanism for both types of materials. It cannot be established by the present results that additions of Al (≈ 2 % in weight) improve the performance of MgO-C materials.Se describen los resultados del estudio post-mortem de diversas piezas de MgO-C y MgO-C-Al utilizadas en los hornos eléctricos de la factoría de Acerinox en Cádiz. De la caracterización química, térmica, mineralógica y microestructural de los materiales sin usar y post-mortem se ha establecido que la corrosión ha dado lugar, en ambos tipos de refractarios, a la formación de capas de reacción con distinta composición química y mineralógica, en función de la temperatura y presión parcial de oxígeno en la pieza, que varían desde la cara caliente a la cara fría y dependen fuertemente de la zona del horno eléctrico en que está situada la pieza. En ambos tipos de materiales se han observado por difracción de rayos X cambios en el contenido de grafito con la distancia a la cara fría. Estos cambios se han cuantificado mediante análisis térmico diferencial. En los refractarios de MgO-C-Al se observa la formación de pequeñas cantidades de C3Al4 en el interior de las piezas y de MgAl2O4 en la cara caliente del refractario. Teniendo en cuenta los resultados obtenidos y los diagramas de equilibrio de fases Mg-C-Al-O se ha establecido el mecanismo de corrosión en ambos tipos de materiales. De los resultados obtenidos no se puede establecer que adiciones de Al (≈ 2% en peso) mejoren el comportamiento en servicio de los materiales de MgO-C.
Boletín de la Sociedad Española de Cerámica y Vidrio. 01/2010;
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ABSTRACT: This study concerns the preparation and in vitro characterization of an apatite-wollastonite-2M bioactive glass ceramic which is intended to be used for the regeneration of hard tissue (i.e. in dental and craniomaxillofacial surgery). This bioglass ceramic has been obtained by appropriate thermal treatment through the devitrification (crystallization) of a glass with a stoichiometric eutectic composition within the Ca(3)(PO(4))(2)-CaSiO(3) binary system. Crack-free specimens of the bioglass ceramic were immersed in human bone marrow cell cultures for 3, 7, 14 and 21days, in order to study biocompatibility. Cell morphology, proliferation and colonization were assessed by scanning electron microscopy and confocal laser scanning microscopy. A total protein content assay was used to evaluate the viability and proliferation of cultured bone marrow cells. The results showed that the cells were able to adhere and proliferate on the designed material due to the essentiality of silicon and calcium as accessory factors for cell activity stimulation.
Acta biomaterialia 12/2009; 6(6):2254-63. · 3.98 Impact Factor
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ABSTRACT: The present paper describes and discusses the devitrification and crystallization process of wollastonite-tricalcium phosphate (W-TCP) eutectic glass. This process was studied in situ from room temperature up to 1375 degrees C, by neutron diffractometry in vacuum. The data obtained were combined and compared with those performed in ambient atmosphere by differential thermal analysis and with those of samples fired in air at selected temperatures, and then cooled down and subsequently studied by laboratory XRD and field emission scanning electron microscopy fitted with energy X-ray dispersive spectroscopy. The experimental evidence indicates that the devitrification of W-TCP eutectic glass begins at approximately 870 degrees C with the crystallization of a Ca-deficient apatite phase, followed by wollastonite-2M (CaSiO(3)) crystallization at approximately 1006 degrees C. At 1375 degrees C, the bio-glass-ceramic is composed of quasi-rounded colonies formed by a homogeneous mixture of pseudowollastonite (CaSiO(3)) and alpha-tricalcium phosphate (Ca(3)(PO(4))(2)). This microstructure corresponds to irregular eutectic structures. It was also found that it is possible to obtain from the eutectic composition of the wollastonite-tricalcium phosphate binary system a wide range of bio-glass-ceramics, with different crystalline phases present, through appropriate design of thermal treatments.
Acta biomaterialia 06/2009; 5(8):3057-66. · 3.98 Impact Factor
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ABSTRACT: This document describes and discusses the non-isothermal devitrification process of the wollastonite-tricalcium phosphate (W-TCP) eutectic glass. This eutectic glass has been studied in situ, from room temperature up to 1375 ºC, by Neutron Diffractometry (ND) in vacuum. The data obtained were complemented and compared with those performed on ambient atmosphere by Differential Thermal Analysis (DTA) and with those of samples fired in air, at selected temperatures, and then cooled down and subsequently studied by laboratory X-ray Powder Diffraction (LXRD) and Field Emission Scanning Electron Microscopy (FE-SEM) fitted with Energy X-Ray Dispersive Spectroscopy (EDS). Selected samples have been investigated by quantitative full-phase analysis (including the amorphous content) using the Rietveld method. The experimental evidence indicates that the devitrification of W-TCP eutectic glass, begins at ~870ºC, with the crystallization of a Ca-deficient apatite phase (Ca9.92(P5.85O23.54)(OH)2.03 (H2O)2.194)
followed by wollastonite-2M (-CaSiO3) crystallization at 1006ºC. At 1375ºC the bio glassceramic
is comprised of quasi-rounded colonies formed by a homogeneous mixture of pseudowollastonite (-CaSiO3) and -tricalcium phosphate (-Ca3(PO4)2). This microstructure corresponds to irregular eutectic structures and is similar to that of Bioeutectic® W-TCP material obtained previously, via controlled slow solidification of the eutectic composition, by some of the present authors. It has also been found that from the eutectic composition of the wollastonite-tricalcium phosphate binary system is possible to obtain a wide range of bio glass-ceramics through appropriate design of thermal treatments.
Key engineering materials 01/2009; 396-398:127-130.
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ABSTRACT: The biological response following subcutaneous and bone implantation of β-wollastonite(β-W)-doped α-tricalcium phosphate bioceramics in rats was evaluated. Tested materials were: tricalcium phosphate (TCP), consisting of a mixture of α- and β-polymorphs; TCP doped with 5 wt. % of β-W (TCP5W), composed of α-TCP as only crystalline phase; and TCP doped with 15 wt. % of β-W (TCP15), containing crystalline α-TCP and β-W. Cylinders of 2x1 mm were implanted in tibiae and backs of adult male Rattus norvegicus, Holtzman rats. After 7, 30 and 120 days, animals were sacrificed and the tissue blocks containing the implants were excised, fixed and processed for histological examination. TCP, TCP5W and TCP15W implants were biocompatible but neither bioactive nor biodegradable in rat subcutaneous tissue. They were not osteoinductive in connective tissue either. However, in rat bone tissue β-W-doped α-TCP implants
(TCP5W and TCP15W) were bioactive, biodegradable and osteoconductive. The rates of biodegradation and new bone formation observed for TCP5W and TCP15W implants in rat bone tissue were greater than for non-doped TCP.
Key engineering materials 01/2009; 396-398:7-10.
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ABSTRACT: In this study a ceramic composite with nominal composition 40 wt% Ca3(PO4)2 – 60 wt% CaMg(SiO3)2 was obtained by solid state sintering of compacts of both synthetic fine powders. The ceramic composite showed a fine grained and homogeneous microstructure consisting of CaMg(SiO3)2 and b-Ca3(PO4)2 grains. The results of X-ray diffraction and scanning electron microscopy demonstrated that, during
soaking in SBF, the grains of β-Ca3(PO4)2 dissolved preferably than those of CaMg(SiO3)2, leaving
a porous surface layer rich in CaMg(SiO3)2. Subsequently, partial dissolution of the remaining CaMg(SiO3)2 occurred and the porous surface of the b-Ca3(PO4)2-CaMg(SiO3)2 ceramic became
coated by a bone-like apatite layer after 7 days in SBF.
Key engineering materials 01/2009; 396-398:103-106.
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21st International Symposium on Ceramics in Medicine (ISCM), Buzios; 01/2009
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21st International Symposium on Ceramics in Medicine (ISCM), Buzios; 01/2009
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21st International Symposium on Ceramics in Medicine (ISCM), Buzios; 01/2009
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Bioceramics 21: 21st International Symposium on Ceramics in Medicine (ISCM), Buzios; 01/2009
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ABSTRACT: In this work a new kind of CaSiO3-doped α-Ca3(PO4)2 ceramic materials, with compositions lying outside the field of the Ca3(PO4)2 solid solution in the system Ca3(PO4)2-CaSiO3, were obtained and some of their properties, relevant for bone repairing, were studied in vitro. Crystalline α-Ca3(PO4)2 solid solution and minor amounts of non-equilibrium residual glass were the only phases in the materials containing 2 and 5 wt% of CaSiO3. α-Ca3(PO4)2, crystalline eutectic-like phase and residual glass were observed for sample containing 15 and 20 wt% of CaSiO3. The mechanical strength improved for all the doped ceramics with regard to un-doped Ca3(PO4)2. The release of ionic Ca and Si in simulated physiological conditions increased with the content of CaSiO3 and favored α-Ca3(PO4)2 surface transformation. The soluble components extracted from the CaSiO3-doped α-Ca3(PO4)2 bioceramics were not cytotoxic to human fibroblast-like cells. Initial cell adhesion onto the surface of the materials seemed to be partially hindered by surface reactivity and remodeling, however those cells adhered to the experimental bioceramics were viable and proliferated normally.
Key engineering materials 01/2008; 361-363:237-240.
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ABSTRACT: Wollastonite bioceramics prepared from synthetic and natural precursors were implanted in rats in bone and subcutaneous tissues. The implant sites were excised after 7, 30 and 120 days, fixed, dehydrated, embedded in paraffin wax for serial cutting and examined under transmitted light microscope. It was found a very similar behavior for both wollastonite bioceramics. They were biocompatible, bioactive and biodegradable when implanted in rat bone. The synthetic ceramic was more reabsorbable than the one from natural powder. When implanted in subcutaneous rat tissue, both materials elicited a mild initial inflammatory reaction that practically disappeared after 120 days. Both materials were encapsulated with a very thin fibrous capsule and slightly reabsorbed at their surfaces. None of the materials induced ectopic osteogenesis. According to the results, the studied materials seem to be able for manufacturing reabsorbable bone implants.
Key engineering materials 01/2008; 361-363:1083-1086.
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ABSTRACT: Partially deuterated Ca3Al2(SiO4)y(OH)12−4y–Al(OH)3 mixtures, prepared by hydration of Ca3Al2O6 (C3A), Ca12Al14O33 (C12A7) and CaAl2O4 (CA) phases in the presence of silica fume, have been characterized by 29Si and 27Al magic-angle spinning–nuclear magnetic resonance (MAS–NMR) spectroscopies. NMR spectroscopy was used to characterize anhydrous and fully hydrated samples. In hydrated compounds, Ca3Al2(OH)12 and Al(OH)3 phases were detected. From the quantitative analysis of 27Al NMR signals, the Al(OH)3/Ca3Al2(OH)12 ratio was deduced. The incorporation of Si into the katoite structure, Ca3Al2(SiO4)3−x(OH)4x, was followed by 27Al and 29Si NMR spectroscopies. Si/OH ratios were determined from the quantitative analysis of 27Al MAS–NMR components associated with Al(OH)6 and Al(OSi)(OH)5 environments. The 29Si NMR spectroscopy was also used to quantify the unreacted silica and amorphous calcium aluminosilicate hydrates formed, C–S–H and C–A–S–H for short. From 29Si NMR spectra, the amount of Si incorporated into different phases was estimated. Si and Al concentrations, deduced by NMR, transmission electron microscopy, energy dispersive spectrometry, and Rietveld analysis of both X-ray and neutron data, indicate that only a part of available Si is incorporated in katoite structures.
Journal of Solid State Chemistry - J SOLID STATE CHEM. 01/2008; 181(8):1744-1752.
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ABSTRACT: Pseudowollastonite ceramics (beta-CaSiO3) from synthetic and natural sources were assessed with regard to their properties relevant to biomedical applications. Synthetic and natural CaSiO3 powders, with average particle size of 1.6 and 13.2 microm, respectively, were first employed. Powders were pressed and sintered at 1400 degrees C for 2 h. Pseudowollastonite was the only crystalline phase in sintered materials. Glassy phase, eight times more abundant in sintered natural wollastonite (SNW) than in the synthetic one (SSW), was observed in grain boundaries and in triple points. Larger grains and bigger and more abundant pores were present in SNW, resulting in lower diametral tensile strength (26 MPa), than in SSW (42 MPa). However, by milling the natural wollastonite starting powder to a particle size of 2.0 microm and sintering (SNW-M), the microstructure became finer and less porous, and diametral tensile strength increased (48 MPa). Weibull modulus of SNW and SNW-M samples was twice that of the SSW. All the samples released Si and Ca ions, and removed phosphate ions from simulated body fluid in similar amounts and were completely coated by apatite-like spherules after soaking in simulated body fluid for 3 wk. The aqueous extracts from all samples studied were not cytotoxic in a culture of human fibroblastic cells. No differences in fibroblast-like human cells adhesion and proliferation were observed between samples. According to the obtained results, properly processed pseudowollastonite bioceramics, obtained from the natural source, exhibit the same in vitro behavior and better performance in terms of strength and reliability than do the more expensive synthetic materials.
Journal of Biomedical Materials Research Part A 12/2007; 83(2):484-95. · 2.63 Impact Factor
