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1.
Dent Mater ; 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38755041

RESUMO

Development of restorative materials capable of mimicking optical and mechanical performance of natural teeth is a quest in aesthetic density. Yttria-Stabilized Zirconia (YSZ) ceramics represent one of the most popular choices for dental restorations, owing to their biocompatibility, white colour, and the possibility to use CAD-CAM technologies. In particular, YSZ doped with 3 mol. % yttria (3YSZ) is popular because it presents high strength. Nonetheless, the limited light transmission of commercially available high strength 3YSZ does not meet the requirements of highly aesthetic cases. On the other side, YSZ presenting a larger portion of yttria are more translucent but exhibit modest strength. Here, we report on fabrication of dense zirconia nanostructures in bulk form via conventional pressure-less sintering at temperatures down to 1100-1200 °C, achieving highly translucent and strong 3YSZ with significant opalescent behaviour. Both Hall-Petch and inverse Hall-Petch relationship were observed in 3YSZ samples with average grain size in the range of 250 nm and 55 nm, demonstrating the importance of grain size control to enhance both optical and mechanical properties of zirconia ceramics, simultaneously. Maximum biaxial strength of 1980 ± 260 MPa, in-line light transmission of 38% in the visible spectrum and opalescence approaching that of enamel were obtained at optimum grain size of 80 ± 5 nm. The notable optical properties are linked to the miniaturization of the residual pores and refinement of grain size towards the nanoscale while the superior mechanical strength is justified by the activation of different energy dissipation processes at nano and macroscale.

2.
Mol Ecol Resour ; 22(6): 2158-2170, 2022 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-35218316

RESUMO

The study of environmental DNA (eDNA) released by aquatic organisms in their habitat offers a fast, noninvasive and sensitive approach to monitor their presence. Common eDNA sampling methods such as water filtration and DNA precipitation are time-consuming, require difficult-to-handle equipment and partially integrate eDNA signals. To overcome these limitations, we created the first proof of concept of a passive, 3D-printed and easy-to-use eDNA sampler. We designed the samplers from hydroxyapatite (HAp samplers), a natural mineral with a high DNA adsorption capacity. The porous structure and shape of the samplers were designed to optimize DNA adsorption and facilitate their handling in the laboratory and in the field. Here we show that HAp samplers can efficiently collect genomic DNA in controlled set-ups, but can also collect animal eDNA under controlled and natural conditions with yields similar to conventional methods. However, we also observed large variations in the amount of DNA collected even under controlled conditions. A better understanding of the DNA-hydroxyapatite interactions on the surface of the samplers is now necessary to optimize eDNA adsorption and to allow the development of a reliable, easy-to-use and reusable eDNA sampling tool.


Assuntos
DNA Ambiental , Animais , DNA/genética , Durapatita , Monitoramento Ambiental/métodos , Impressão Tridimensional
3.
Nat Commun ; 12(1): 4695, 2021 08 04.
Artigo em Inglês | MEDLINE | ID: mdl-34349114

RESUMO

Hyperpolarization by dissolution dynamic nuclear polarization (dDNP) has enabled promising applications in spectroscopy and imaging, but remains poorly widespread due to experimental complexity. Broad democratization of dDNP could be realized by remote preparation and distribution of hyperpolarized samples from dedicated facilities. Here we show the synthesis of hyperpolarizing polymers (HYPOPs) that can generate radical- and contaminant-free hyperpolarized samples within minutes with lifetimes exceeding hours in the solid state. HYPOPs feature tunable macroporous porosity, with porous volumes up to 80% and concentration of nitroxide radicals grafted in the bulk matrix up to 285 µmol g-1. Analytes can be efficiently impregnated as aqueous/alcoholic solutions and hyperpolarized up to P(13C) = 25% within 8 min, through the combination of 1H spin diffusion and 1H → 13C cross polarization. Solutions of 13C-analytes of biological interest hyperpolarized in HYPOPs display a very long solid-state 13C relaxation times of 5.7 h at 3.8 K, thus prefiguring transportation over long distances.

4.
Materials (Basel) ; 14(11)2021 Jun 05.
Artigo em Inglês | MEDLINE | ID: mdl-34198831

RESUMO

Due to growing demand for metal-free dental restorations, dental ceramics, especially dental zirconia, represent an increasing share of the dental implants market. They may offer mechanical performances of the same range as titanium ones. However, their use is still restricted by a lack of confidence in their durability and, in particular, in their ability to resist hydrothermal ageing. In the present study, the ageing kinetics of commercial zirconia dental implants are characterized by X-ray diffraction after accelerated ageing in an autoclave at different temperatures, enabling their extrapolation to body temperature. Measurements of the fracture loads show no effect of hydrothermal ageing even after ageing treatments simulated a 90-year implantation.

5.
Acta Biomater ; 123: 123-153, 2021 03 15.
Artigo em Inglês | MEDLINE | ID: mdl-33359868

RESUMO

The field of bone tissue engineering (BTE) focuses on the repair of bone defects that are too large to be restored by the natural healing process. To that purpose, synthetic materials mimicking the natural bone extracellular matrix (ECM) are widely studied and many combinations of compositions and architectures are possible. In particular, the electrospinning process can reproduce the fibrillar structure of bone ECM by stretching a viscoelastic solution under an electrical field. With this method, nano/micrometer-sized fibres can be produced, with an adjustable chemical composition. Therefore, by shaping bioactive ceramics such as silica, bioactive glasses and calcium phosphates through electrospinning, promising properties for their use in BTE can be obtained. This review focuses on the in situ synthesis and simultaneous electrospinning of bioceramic-based fibres while the reasons for using each material are correlated with its bioactivity. Theoretical and practical considerations for the synthesis and electrospinning of these materials are developed. Finally, investigations into the in vitro and in vivo bioactivity of different systems using such inorganic fibres are exposed.


Assuntos
Dióxido de Silício , Engenharia Tecidual , Osso e Ossos , Fosfatos de Cálcio , Cerâmica
6.
J Mech Behav Biomed Mater ; 98: 40-47, 2019 10.
Artigo em Inglês | MEDLINE | ID: mdl-31185443

RESUMO

Ceramic-on-ceramic bearings in total hip replacement have shown the potential to provide low wear solutions in hip replacement. Assessing the tribological performance of these materials is important to predict their long-term performance in patients. In this study, a methodology was devised to assess the tribological in vitro behaviour of composite ceramics under combined adverse edge loading conditions and accelerated ageing. Two commercial ceramic composites were considered, namely Alumina-Toughened Zirconia (ATZ, ceramys®) and Zirconia-Toughened Alumina (ZTA, symarec®). The bearing couples were studied using the Leeds Mark II hip joint simulator for a total of eight million cycles, the first two million under normal gait (no edge loading) and the following six million cycles with the addition of edge loading conditions driven by medial-lateral separation. The bearing couples underwent hydrothermal ageing using an accelerated protocol in autoclave every million cycles. The influence of edge loading combined with ageing was significant for ATZ bearings, resulting in a slower overall ageing kinetics over the wear stripe than on the control heads. During the autoclave ageing steps, the monoclinic fraction increased more over the wear stripe area than over the unworn area. Both results thus indicated that the monoclinic phase was removed during shocks induced by edge loading. The wear performance of the two materials were similar exhibiting relatively low wear rates and low level of microstructural damage for these clinically relevant adverse conditions.


Assuntos
Artroplastia de Quadril , Cerâmica , Óxido de Alumínio/química , Cerâmica/química , Marcha , Estresse Mecânico , Fatores de Tempo , Suporte de Carga , Zircônio/química
7.
Acta Biomater ; 89: 391-402, 2019 04 15.
Artigo em Inglês | MEDLINE | ID: mdl-30831328

RESUMO

The efficiency of calcium phosphate (CaP) bone substitutes can be improved by tuning their resorption rate. The influence of both crystal orientation and ion doping on resorption is here investigated for beta-tricalcium phosphate (ß-TCP). Non-doped and Mg-doped (1 and 6 mol%) sintered ß-TCP samples were immersed in acidic solution (pH 4.4) to mimic the environmental conditions found underneath active osteoclasts. The surfaces of ß-TCP samples were observed after acid-etching and compared to surfaces after osteoclastic resorption assays. ß-TCP grains exhibited similar patterns with characteristic intra-crystalline pillars after acid-etching and after cell-mediated resorption. Electron BackScatter Diffraction analyses, coupled with Scanning Electron Microscopy, Inductively Coupled Plasma-Mass Spectrometry and X-Ray Diffraction, demonstrated the influence of both grain orientation and doping on the process and kinetics of resorption. Grains with c-axis nearly perpendicular to the surface were preferentially etched in non-doped ß-TCP samples, whereas all grains with simple axis (a, b or c) nearly normal to the surface were etched in 6 mol% Mg-doped samples. In addition, both the dissolution rate and the percentage of etched surface were lower in Mg-doped specimens. Finally, the alignment direction of the intra-crystalline pillars was correlated with the preferential direction for dissolution. STATEMENT OF SIGNIFICANCE: The present work focuses on the resorption behavior of calcium phosphate bioceramics. A simple and cost-effective alternative to osteoclast culture was implemented to identify which material features drive resorption. For the first time, it was demonstrated that crystal orientation, measured by Electron Backscatter Diffraction, is the discriminating factor between grains, which resorbed first, and grains, which resorbed slower. It also elucidated how resorption kinetics can be tuned by doping ß-tricalcium phosphate with ions of interest. Doping with magnesium impacted lattice parameters. Therefore, the crystal orientations, which preferentially resorbed, changed, explaining the solubility decrease. These important findings pave the way for the design of optimized bone graft substitutes with tailored resorption kinetics.


Assuntos
Reabsorção Óssea/metabolismo , Fosfatos de Cálcio , Osteoclastos/metabolismo , Animais , Reabsorção Óssea/patologia , Fosfatos de Cálcio/química , Fosfatos de Cálcio/farmacocinética , Fosfatos de Cálcio/farmacologia , Magnésio/química , Magnésio/farmacocinética , Magnésio/farmacologia , Espectrometria de Massas , Camundongos , Microscopia Eletrônica de Varredura , Osteoclastos/ultraestrutura , Difração de Raios X
8.
J Mater Sci Mater Med ; 30(1): 6, 2018 Dec 29.
Artigo em Inglês | MEDLINE | ID: mdl-30594987

RESUMO

Bone substitute fabrication is of interest to meet the worldwide incidence of bone disorders. Physical chitosan hydrogels with intertwined apatite particles were chosen to meet the bio-physical and mechanical properties required by a potential bone substitute. A set up for 3-D printing by robocasting was found adequate to fabricate scaffolds. Inks consisted of suspensions of calcium phosphate particles in chitosan acidic aqueous solution. The inks are shear-thinning and consist of a suspension of dispersed platelet aggregates of dicalcium phosphate dihydrate in a continuous chitosan phase. The rheological properties of the inks were studied, including their shear-thinning characteristics and yield stress. Scaffolds were printed in basic water/ethanol baths to induce transformation of chitosan-calcium phosphates suspension into physical hydrogel of chitosan mineralized with apatite. Scaffolds consisted of a chitosan polymeric matrix intertwined with poorly crystalline apatite particles. Results indicate that ink rheological properties could be tuned by controlling ink composition: in particular, more printable inks are obtained with higher chitosan concentration (0.19 mol·L-1).


Assuntos
Fosfatos de Cálcio/química , Quitosana/química , Impressão Tridimensional , Alicerces Teciduais/química , Materiais Biocompatíveis , Reologia
9.
Materials (Basel) ; 10(6)2017 May 24.
Artigo em Inglês | MEDLINE | ID: mdl-28772930

RESUMO

The surface morphologies and microstructures of Zirconia Toughened Alumina (ZTA) femoral heads were analyzed following in vitro tests aiming to simulate in vivo degradation. Three phenomena potentially leading to degradation were investigated: shocks, friction and hydrothermal ageing. Shocks due to micro-separation created the main damage with the formation of wear stripes on the femoral head surfaces. Atomic Force Microscopy (AFM) images suggested the release of wear debris of various shapes and sizes through inter- and intra-granular cracks; some debris may have a size lower than 100 nm. A decrease in hardness and Young's modulus was measured within the wear stripes by nanoindentation technique and was attributed to the presence of surface and sub-surface micro-cracks. Such micro-cracks mechanically triggered the zirconia phase transformation in those worn areas, which in return presumably reduced further crack propagation. In comparison with shocks, friction caused little wear degradation as observed from AFM images by scarce pullout of grains. The long-term resistance of the ZTA composite material against hydrothermal ageing is confirmed by the present observations.

10.
Acta Biomater ; 53: 515-525, 2017 04 15.
Artigo em Inglês | MEDLINE | ID: mdl-28232255

RESUMO

The mechanisms by which calcium phosphate bone substitutes evolve and are resorbed in vivo are not yet fully known. In particular, the formation of intermediate phases during resorption and evolution of the mechanical properties may be of crucial interest for their clinical efficiency. The in vitro tests proposed here are the first steps toward understanding these phenomena. Microporous Dicalcium Phosphate Dihydrate (DCPD) samples were immersed in tris(hydroxymethyl)aminomethane (TRIS) and Phosphate Buffered Saline (PBS) solutions, with or without daily refresh of the medium, for time-points up to 14days. Before and after immersion, samples were extensively characterised in terms of morphology, chemistry (XRD coupled with Rietveld analysis), microstructure (X-ray tomography, SEM observations) and local mechanical properties (instrumented micro-indentation). The composition of the immersion solutions was monitored in parallel (pH, elemental analysis). The results show the influence and importance of the experimental set-up and protocol on the formation of apatite and octacalcium phosphate concurrently to DCPD dissolution; moreover, strong inter-correlations between physico-chemistry, microstructure and mechanics are demonstrated. STATEMENT OF SIGNIFICANCE: Ideally, the resorption kinetics of biodegradable bone substitutes should be controlled to favor the healing processes of bone. Although biodegradable bone grafts are already used in surgeries, their resorption process is still partially unknown. The present work studies these resorption phenomena, their kinetics and mechanisms and their consequences on the properties of a calcium phosphate resorbable material. The original in vitro approach developed in this work couples for the first time physico-chemical, micro-structural and mechanical assessments. The dissolution of the CaP phase in body fluids and the reprecipitation of more stable phases are studied on a local scale, which has permitted to evidence and monitor the development of a gradient of properties between the surface and the core of the samples.


Assuntos
Líquidos Corporais/química , Cimentos Ósseos/química , Substitutos Ósseos/química , Fosfatos de Cálcio/química , Teste de Materiais/métodos , Absorção Fisico-Química , Adesividade , Força Compressiva , Módulo de Elasticidade , Tamanho da Partícula
11.
J Mech Behav Biomed Mater ; 65: 600-608, 2017 01.
Artigo em Inglês | MEDLINE | ID: mdl-27736716

RESUMO

Ceramics are materials of choice for hip joint implants because of their excellent biocompatibility and mechanical properties. Wear of the bearing couple (femoral head and cup) remains one of the main concerns of hip implants. Although ceramics are known for their good tribological properties, shocks due to micro-separation, friction and hydrothermal ageing in physiological environment remain the three main sources of wear. It has been recently suggested that shock effects dominate but the three degradation mechanisms were so far simulated separately. We developed a procedure that combines sequences of shocks, hydrothermal ageing in an autoclave and friction on hip-walking simulator to investigate their combined effects on Zirconia Toughened Alumina (ZTA) implants. Our results confirm that shocks can be considered as the key phenomenon causing wear, and that their effect is independent of friction and hydrothermal degradation. The analysis of retrieved femoral heads reveals wear features comparable to the ones created experimentally by shocks. Standards (ASTM or ISO) could be improved by including shock tests, which are more relevant than wear tests currently performed on hip simulators at least for Ceramic-on- Ceramic couplings.


Assuntos
Óxido de Alumínio/análise , Prótese de Quadril , Teste de Materiais , Falha de Prótese , Zircônio/análise , Cerâmica , Fricção , Propriedades de Superfície
12.
Mater Sci Eng C Mater Biol Appl ; 72: 268-277, 2017 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-28024586

RESUMO

Drug release from tissue scaffolds is commonly controlled by using coatings and carriers, as well as by varying the binding affinity of molecules being released. This paper considers modulating synthetic peptide incorporation and release through the use of interconnected microporosity in biphasic calcium phosphate (BCP) and identifies the microstructural characteristics important to the release using experiments and a model of relative diffusivity. First, the release of three modular peptides designed to include an osteocalcin-inspired binding sequence based on bone morphogenic protein-2 (BMP-2) was compared and one was selected for further study. Next, the incorporation and release of the peptide from four types of substrates were compared: non-microporous (NMP) substrates had no microporosity; microporous (MP) substrates were either 50% microporous with 5µm pores (50/5), 60% microporous with 5µm pores (60/5), or 50% microporous with 50µm pores (50/50). Results showed that MP substrates incorporated significantly more peptide than NMP ones, but that the three different microporous substrates all incorporated the same total amount of peptide. NMP had a markedly lower release rate compared to each of three of the MP samples, though the initial burst release was the highest. The initial release and the release rate for the 60/5 samples were different from the 50/50, though they were not statistically different from the 50/5. The model indicated that the pore interconnection to pore size ratio, affecting the constriction between pores, had the greatest influence on the calculated relative diffusivity. While the model was consistent with the trends observed experimentally, the quantitative experimental results suggested that to attain an appreciable difference in release characteristics, both pore size and pore fraction should be changed for this system. These results contribute to rational scaffold design by showing that microstructure, specifically microporosity, can be used to modulate drug release.


Assuntos
Fosfatos de Cálcio/química , Peptídeos/metabolismo , Sequência de Aminoácidos , Proteína Morfogenética Óssea 2/química , Proteína Morfogenética Óssea 2/metabolismo , Fosfatos de Cálcio/metabolismo , Portadores de Fármacos/química , Microscopia Eletrônica de Varredura , Dados de Sequência Molecular , Peptídeos/química , Porosidade , Ligação Proteica
13.
Acta Biomater ; 46: 323-335, 2016 12.
Artigo em Inglês | MEDLINE | ID: mdl-27686041

RESUMO

High-performance bioinert ceramics such as zirconia have been used for biomedical devices since the early seventies. In order to promote osseointegration, the historical solution has been to increase the specific surface of the implant through roughness. Nevertheless these treatments on ceramics may create defects at the surface, exposing the material to higher chances of early failure. In zirconia, such treatments may also affect the stability of the surface. More recently, the interest of improving osseointegration of implants has moved the research focus towards the actual chemistry of the surface. Inspired by this, we have adapted the current knowledge and techniques of silica functionalization and applied it to successfully introduce 3-aminopropyldimethylethoxy silane (APDMES) directly on the surface of zirconia (3Y-TZP). We used plasma of oxygen to clean the surface and promote hydroxylation of the surface to increase silane density. The samples were extensively characterized by means of X-ray photoelectron spectroscopy (XPS) and contact angle, mechanically tested and its cytotoxicity was evaluated through cell adhesion and proliferation tests. Additionally, aging was studied to discard negative effects of the treatment on the stability of the tetragonal phase. No adverse effect was found on the mechanical response of treated samples. In addition, plasma-treated samples exhibited an unexpectedly higher resistance to aging. Finally, silane density was 35% lower than the one reported in literature for silica. However cells displayed a qualitatively higher spreading in opposition to the rounder appearance of cells on untreated zirconia. These results lay the foundations for the next generation of zirconia implants with biologically friendlier surfaces. STATEMENT OF SIGNIFICANCE: The use of zirconia-based ceramics in biomedical devices is broad and well accepted, especially in dental implants. However, they do not bond naturally to bone, therefore to ensure fixation surgeons typically rely on roughness at different scales, or on cements. Alternatively in this work we present a new perspective of surface modification through chemistry to enhance the interaction between surface and biological environment, without the downsides of roughness. This surface treatment is proposed for zirconia, which allowed a direct silanization of its surface and a higher cell attachment. The results of this research may open the possibility for the next generation of bioinert ceramic implants with more advanced tailored surfaces for increased osseointegration.


Assuntos
Osseointegração/efeitos dos fármacos , Silanos/química , Zircônio/farmacologia , Linhagem Celular , Proliferação de Células/efeitos dos fármacos , Humanos , Cinética , Espectroscopia Fotoeletrônica , Propriedades de Superfície
14.
Acta Biomater ; 46: 308-322, 2016 12.
Artigo em Inglês | MEDLINE | ID: mdl-27639312

RESUMO

Due to their outstanding mechanical properties and excellent biocompatibility, zirconia-toughened alumina (ZTA) ceramics have become the gold standard in orthopedics for the fabrication of ceramic bearing components over the last decade. However, ZTA is bioinert, which hampers its implantation in direct contact with bone. Furthermore, periprosthetic joint infections are now the leading cause of failure for joint arthroplasty prostheses. To address both issues, an improved surface design is required: a controlled micro- and nano-roughness can promote osseointegration and limit bacterial adhesion whereas surface porosity allows loading and delivery of antibacterial compounds. In this work, we developed an integrated strategy aiming to provide both osseointegrative and antibacterial properties to ZTA surfaces. The micro-topography was controlled by injection molding. Meanwhile a novel process involving the selective dissolution of zirconia (selective etching) was used to produce nano-roughness and interconnected nanoporosity. Potential utilization of the porosity for loading and delivery of antibiotic molecules was demonstrated, and the impact of selective etching on mechanical properties and hydrothermal stability was shown to be limited. The combination of injection molding and selective etching thus appears promising for fabricating a new generation of ZTA components implantable in direct contact with bone. STATEMENT OF SIGNIFICANCE: Zirconia-toughened alumina (ZTA) is the current gold standard for the fabrication of orthopedic ceramic components. In the present work, we propose an innovative strategy to provide both osseointegrative and antibacterial properties to ZTA surfaces: we demonstrate that injection molding allows a flexible design of surface micro-topography and can be combined with selective etching, a novel process that induces nano-roughness and surface interconnected porosity without the need for coating, avoiding reliability issues. These surface modifications have the potential to improve osseointegration. Furthermore, our results show that the porosity can be used for drug delivery and suggest that the etched surface could reduce bacterial adhesion.


Assuntos
Óxido de Alumínio/química , Antibacterianos/farmacologia , Cerâmica/farmacologia , Implantes Experimentais , Osseointegração , Zircônio/química , Sistemas de Liberação de Medicamentos , Liberação Controlada de Fármacos , Escherichia coli/efeitos dos fármacos , Análise de Elementos Finitos , Injeções , Interferometria , Cinética , Testes de Sensibilidade Microbiana , Microscopia de Força Atômica , Osseointegração/efeitos dos fármacos , Espectroscopia Fotoeletrônica , Porosidade , Propriedades de Superfície
15.
Dent Mater ; 31(1): 15-25, 2015 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-25262212

RESUMO

OBJECTIVES: Based on the current lack of standards concerning zirconia dental implants, we aim at developing a protocol to validate their functionality and safety prior their clinical use. The protocol is designed to account for the specific brittle nature of ceramics and the specific behavior of zirconia in terms of phase transformation. METHODS: Several types of zirconia dental implants with different surface textures (porous, alveolar, rough) were assessed. The implants were first characterized in their as-received state by Scanning Electron Microscopy (SEM), Focused Ion Beam (FIB), X-Ray Diffraction (XRD). Fracture tests following a method adapted from ISO 14801 were conducted to evaluate their initial mechanical properties. Accelerated aging was performed on the implants, and XRD monoclinic content measured directly at their surface instead of using polished samples as in ISO 13356. The implants were then characterized again after aging. RESULTS: Implants with an alveolar surface presented large defects. The protocol shows that such defects compromise the long-term mechanical properties. Implants with a porous surface exhibited sufficient strength but a significant sensitivity to aging. Even if associated to micro cracking clearly observed by FIB, aging did not decrease mechanical strength of the implants. SIGNIFICANCE: As each dental implant company has its own process, all zirconia implants may behave differently, even if the starting powder is the same. Especially, surface modifications have a large influence on strength and aging resistance, which is not taken into account by the current standards. Protocols adapted from this work could be useful.


Assuntos
Implantes Dentários , Zircônio/química , Planejamento de Prótese Dentária , Falha de Restauração Dentária , Análise do Estresse Dentário , Teste de Materiais , Microscopia Eletrônica de Varredura , Propriedades de Superfície , Difração de Raios X
16.
Acta Biomater ; 9(6): 6992-7004, 2013 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-23518476

RESUMO

This paper presents a new aqueous precipitation method to prepare silicon-substituted hydroxyapatites Ca10(PO4)6-y(SiO4)y(OH)2-y(VOH)y (SiHAs) and details the characterization of powders with varying Si content up to y=1.25molmolSiHA(-1). X-ray diffraction, transmission electron microscopy, solid-state nuclear magnetic resonance and Fourier transform infrared spectroscopy were used to accurately characterize samples calcined at 400°C for 2h and 1000°C for 15h. This method allows the synthesis of monophasic SiHAs with controlled stoichiometry. The theoretical maximum limit of incorporation of Si into the hexagonal apatitic structure is y<1.5. This limit depends on the OH content in the channel, which is a function of the Si content, temperature and atmosphere of calcination. These results, particularly those from infrared spectroscopy, raise serious reservations about the phase purity of previously prepared and biologically evaluated SiHA powders, pellets and scaffolds in the literature.


Assuntos
Substitutos Ósseos/análise , Substitutos Ósseos/síntese química , Durapatita/análise , Durapatita/química , Precipitação Fracionada/métodos , Silício/análise , Silício/química , Contaminação de Medicamentos/prevenção & controle , Teste de Materiais/métodos , Pós , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
17.
Dent Mater ; 29(2): 157-65, 2013 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-23228334

RESUMO

OBJECTIVES: The phenomena occurring during zirconia frameworks veneering process are not yet fully understood. In particular the study of zirconia behavior at the interface with the veneer remains a challenge. However this interface has been reported to act on residual stress in the veneering ceramic, which plays a significant role in clinical failures such as chipping. The objective of this study was thus to investigate the veneer-zirconia interface using a recent 3D-analysis tool and to confront these observations to residual stress measurements in the veneering ceramic. METHODS: Two cross-sectioned bilayered disc samples (veneer on zirconia), exhibiting different residual stress profiles in the veneering ceramic, were investigated using 2D and 3D imaging (respectively Scanning Electron Microscopy (SEM) and Focused Ion Beam nanotomography (FIB-nt), associated with chemical analysis by Energy Dispersive X-ray Spectroscopy (EDS). RESULTS: The observations did not reveal any structural change in the bulk of zirconia layer of both samples. However the presence of structural alterations and sub-surface microcracks were highlighted in the first micrometer of zirconia surface, exclusively for the sample exhibiting interior tensile stress in the veneering ceramic. No interdiffusion phenomena were observed. SIGNIFICANCE: FIB nanotomography was proven to be a powerful technique to study the veneer-zirconia interface. The determination of the origin and the nature of zirconia alterations need to be further studied. The results of the present study support the hypothesis that zirconia surface property changes could be involved in the development of tensile stress in the veneering ceramic, increasing the risk of chipping.


Assuntos
Cerâmica/química , Facetas Dentárias , Imageamento Tridimensional/métodos , Zircônio/química , Análise do Estresse Dentário , Microscopia Eletrônica de Varredura/métodos , Espectrometria por Raios X/métodos , Propriedades de Superfície
18.
PLoS One ; 6(10): e26474, 2011.
Artigo em Inglês | MEDLINE | ID: mdl-22028886

RESUMO

The control of the growth morphologies of ice crystals is a critical issue in fields as diverse as biomineralization, medicine, biology, civil or food engineering. Such control can be achieved through the ice-shaping properties of specific compounds. The development of synthetic ice-shaping compounds is inspired by the natural occurrence of such properties exhibited by antifreeze proteins. We reveal how a particular zirconium acetate complex is exhibiting ice-shaping properties very similar to that of antifreeze proteins, albeit being a radically different compound. We use these properties as a bioinspired approach to template unique faceted pores in cellular materials. These results suggest that ice-structuring properties are not exclusive to long organic molecules and should broaden the field of investigations and applications of such substances.


Assuntos
Acetatos/química , Proteínas Anticongelantes/química , Materiais Biomiméticos/química , Complexos de Coordenação/química , Gelo , Zircônio/química , Cristalização , Suspensões
19.
Acta Biomater ; 7(7): 2986-93, 2011 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-21414426

RESUMO

Today there is growing interest in zirconia in the dental field, but its use is still recent. Dental zirconia is mainly found in the form of yttria-stabilized zirconia crowns, bridges and abutments, and several companies are developing zirconia implants as an alternative to the standard biomedical grade titanium. In order to favor bone in-growth and osseointegration of zirconia implants, several strategies are now being explored to process rough and/or porous surfaces. The aim of this paper was to evaluate the resistance to environmental degradation of yttria-stabilized zirconia coated with a porous layer. We show that specific conditions of processing to generate the porous layer at the surface can lead to an accelerated tetragonal-monoclinic transformation of the porous layer in the presence of water. The impact of the transformation was evaluated in terms of structural integrity. Bending strength was not affected but the cohesion of the porous coating and its adhesion with the dense part deteriorated. We show that other processing conditions insure much better stability. Low-temperature degradation resistance of such porous surfaces should therefore be carefully followed and controlled in order to avoid critical problems in the future.


Assuntos
Temperatura Baixa , Porosidade , Zircônio/química , Zircônio/metabolismo , Materiais Biocompatíveis/química , Materiais Biocompatíveis/metabolismo , Planejamento de Prótese Dentária , Teste de Materiais , Osseointegração , Estresse Mecânico , Propriedades de Superfície , Resistência à Tração , Difração de Raios X
20.
J Mech Behav Biomed Mater ; 4(3): 303-14, 2011 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-21316618

RESUMO

Alumina-zirconia nano-composites were recently developed as alternative bearing materials for orthopedics. Previous, preliminary reports show that such alumina-zirconia nanocomposites exhibit high crack resistance and low wear rate. In this paper, additional information is given in terms of wear, crack resistance and ageing behaviour: femoral heads are inspected after 7 million cycles of wear testing on a hip simulator, crack resistance is measured and compared to other ceramics used today in orthopedics, slow crack growth is reported under static and cyclic fatigue, and aging resistance is assessed. We also report on the load to failure of femoral heads prototypes during compression tests. This overall reliability assessment ensures a potential future development for these kinds of new nanocomposites in the orthopedic field.


Assuntos
Teste de Materiais/métodos , Nanocompostos , Ortopedia , Óxido de Alumínio/química , Cerâmica/química , Articulação do Quadril/cirurgia , Prótese de Quadril , Medições Luminescentes , Microscopia de Força Atômica , Microscopia Eletrônica de Varredura , Falha de Prótese , Estresse Mecânico , Fatores de Tempo , Zircônio/química
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