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  • Biomimetic treatment on dental implants for short-term bone regeneration

     Gil Mur, Francisco Javier; Manzanares, Norberto; Badet de Mena, Armando; Aparicio, Conrado; Ginebra Molins, Maria Pau
    Clinical oral investigations
    Date of publication: 2014-01-01
    Journal article

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    Objectives: The main purpose of this work was to assess the short-term bone regenerative potential of new osteoconductive implants. The novelty of the study lies in the analysis of the effectiveness of a novel two-step treatment which combines shot-blasting with a thermo-chemical treatment, at very short times after implant placement in a minipig model. Materials and methods: Three hundred twenty implants with four different surface treatments, namely bioactivated surfaces, micro-rough grit-blasted, micro-rough acid-etched and smooth as-machined titanium implants were placed into the bone of 20 minipigs. The percent of bone-to-implant contact was determined 3 days, 1, 2, 3 and 10 weeks after implant placement by histomorphometric analysis. Surface composition, topography and wettability of the implant specimens were analysed. Results: The combination of shot-blasting and thermo-chemical treatment accelerated bone regeneration at early stages in comparison with all other treatments between day 3 and week 3 (p < 0.05). The value of osseointegration attained at week 2 was maintained until the end of the experiment without any significant changes (percent direct contact ¿ 85 %). This was mostly attributed to the ability of these implants to form in vivo a layer of apatitic mineral that coated the implant and could rapidly stimulate bone nucleation and growth from the implant surface. Conclusions: The surface quality resulting from this treatment on cpTi provided dental implants with a unique ability of rapid bone regeneration and osseointegration. Clinical relevance: This treatment represents a step forward in the direction of reducing the time prior to implant loading. © 2013 Springer-Verlag Berlin Heidelberg.

  • New Ni-free superelastic alloy for orthodontic applications

     Arciniegas, Milena; Manero Planella, Jose M.; Espinar Escalona, Eduardo; Llamas Carreras, Jose Maria; Barrera Mora, Jose Maria; Gil Mur, Francisco Javier
    Materials science and engineering C. Biomimetic and supramolecular systems
    Date of publication: 2013-08-01
    Journal article

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    A potential new Ni-free Ti alloy for biomedical applications was assessed in order to investigate the superelastic behavior, corrosion resistance and the biocompatibility. The alloy studied was Ti19.1Nb8.8Zr. The chemical composition was determined by X-ray microanalysis, the thermoelastic martensitic transformation was characterized by high sensitivity calorimeter. The critical stresses were determined by electromechanical testing machine and the corrosion behavior was analyzed by potentiostatic equipment in artificial saliva immersion at 37 °C. The results were compared with six different NiTi orthodontic archwire brands. The biocompatibility was studied by means of cultures of MG63 cells. Ni-free Ti alloy exhibits thermoelastic martensitic transformation with Ms = 45 °C. The phase present at 37 °C was austenite which under stress can induce martensite. The stress¿strain curves show a superelastic effect with physiological critical stress (low and continuous) and a minimal lost of the recovery around 150 mechanical cycles. The corrosion resistance improves the values obtained by different NiTi alloys avoiding the problem of the Ni adverse reactions caused by Ni ion release. Cell culture results showed that adhered cell number in new substrate was comparable to that obtained in a commercially pure Ti grade II or beta-titanium alloy evaluated in the same conditions. Consequently, the new alloy presents an excellent in-vitro response.

  • Influence of acid-etching after grit-blasted on osseointegration of titanium dental implants: in vitro and in vivo studies

     Herrero Climent, Mariano; Lázaro, Pedro; Rios Santos, Jose Vicente; Lluch Margarit, Sara; Marques Calvo, Maria Soledad; Guillem Marti, Jordi; Gil Mur, Francisco Javier
    Journal of materials science. Materials in electronics
    Date of publication: 2013-04
    Journal article

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  • In vitro response of preosteoblastic MG63 cells on Ni-free Ti shape memory substrates

     Arciniegas, Milena; Peña Andres, Francisco Javier; Gil Mur, Francisco Javier; Manero Planella, Jose M.
    Journal of biomedical materials research. Part B, Applied biomaterials
    Date of publication: 2013-07
    Journal article

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    Ni-free Ti alloys are a potential strategy to overcome the risk of Ni-adverse reactions and rigidity mismatch for implant materials. Here, we report the biological behavior induced for two promising candidate alloysTi19.1Nb8.8Zr (MS temperature of 46 degrees C and elastic modulus of 74 GPa) and Ti41.2Nb6.1Zr (elastic modulus of 67 GPa)on cultured MG63 cells, as well as their physical and chemical properties. Contact angle results revealed the hydrophobic character of the former alloy (59.02 degrees +/- 2.35 degrees) attributed to the presence of the martensitic phase, while the latter one presented a hydrophilic response (67.77 degrees +/- 2.78 degrees). Results showed also that the cell adhesion response (after 4 and 8 h of incubation) in both substrates was not statistically different to that obtained in the cp Ti as control material. These surfaces induced well spread cell morphology with cytoplasmic extension like filopodia of up to 100 m even at short culture times and presented an uninterrupted proliferation after longer incubation times (9 days). A decrement in the proliferation rate was appreciated from the Ti19.1Nb8.8Zr surface at that time, which was attributed to an earlier activation of the cell differentiation stage, as confirmed by the twofold increment of alkaline phosphatase activity. The results also evidenced that the presence of a 2 nm thick layer of amorphous Nb2O5, which was detected on both alloys, has a significant effect on cell behavior favoring the cell adhesion and morphology response of the new alloys studied.

  • Influence of Soft Drinks with Low pH on Different Ni-Ti Orthodontic Archwire Surface Patterns

     Ábalos, C.; Paúl, A.; Mendoza, A.; Solano, E.; Palazon, C.; Gil Mur, Francisco Javier
    Journal of materials engineering and performance
    Date of publication: 2013-03
    Journal article

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    The aim of this study was to determine the influence of soft drinks on the surface of Ni-Ti archwires and their corrosion behavior. Archwires with different patterns (smooth, scratch, dimple, and crack) were selected and characterized by scanning electron microscopy and laser confocal microscopy. Immersion tests were performed in artificial saliva (pH 6.7) with a soft drink with a pH of 2.5 for 28 days. The results showed an increase in the surface defects and/or roughness of the dimple, crack and scratch patterns with the immersion times, and a decrease in corrosion resistance. A relationship between the surface pattern and the extent of the corrosion in Ni-Ti archwires with soft drinks at low pH has been demonstrated. Pattern should be taken into account in future studies, and manufacturing processes that produce surface defects (especially cracks) should be avoided

  • Influence of the microstructure on electrochemical corrosion and nickel release in NiTi orthodontic archwires

     Briceño, J.; Romeu, A.; Espinar Escalona, Eduardo; Llamas Carreras, Jose Maria; Gil Mur, Francisco Javier
    Materials science and engineering C. Biomimetic and supramolecular systems
    Date of publication: 2013
    Journal article

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    The aim of this work was to determine the influence of the present phases and the chemical composition on the corrosion behavior and the nickel ion release of the NiTi orthodontic archwires. Eight Ni¿Ti archwires from six commercial brands, in the as-received condition, were studied. The chemical composition, roughness, microstructure and the proportion of the phases as well as the corrosion behavior were analyzed for each archwire. The nickel ion release was characterized in artificial saliva immersion settings ranging up to 4 weeks. The results show that the presence of the martensitic phase improves corrosion resistance and significantly decreases Ni release into exterior medium in comparison with the austenitic specimens. In spite of the partial loss of superelasticity produced in the martensitic phase, it could be of great interest for biomedical applications, as it could minimize sensitization and allergies and improve biocompatibility and corrosion resistance of NiTi shape memory alloys.

    The aim of this work was to determine the influence of the present phases and the chemical composition on the corrosion behavior and the nickel ion release of the NiTi orthodontic archwires. Eight Ni–Ti archwires from six commercial brands, in the as-received condition, were studied. The chemical composition, roughness, microstructure and the proportion of the phases as well as the corrosion behavior were analyzed for each archwire. The nickel ion release was characterized in artificial saliva immersion settings ranging up to 4 weeks. The results show that the presence of the martensitic phase improves corrosion resistance and significantly decreases Ni release into exterior medium in comparison with the austenitic specimens. In spite of the partial loss of superelasticity produced in the martensitic phase, it could be of great interest for biomedical applications, as it could minimize sensitization and allergies and improve biocompatibility and corrosion resistance of NiTi shape memory alloys.

  • Obtención y caracterización de un recubrimiento de quitosano con nanopartículas de plata sobre titanio

     Rodriguez Rius, Daniel; Mancino, Andrea Gennaro; Avilès, Marc; Godoy Gallardo, Maria; Gil Mur, Francisco Javier
    Congreso de la Sociedad Ibérica de Biomecánica y Biomateriales
    Presentation's date: 2013-10-26
    Presentation of work at congresses

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    Se ha desarrollado un recubrimiento de quitosano dopado con nanopartículas de plata sobre la superficie de titanio comercialmente puro de grado 2 para conferir a la superficie propiedades antibacterianas. Se ha escogido como método de inmovilización la deposición de la capa de quitosano mediante dip-coating, que es un método rápido y fiable de formación de capas de recubrimiento. El proceso estudiado consta de dos etapas: la formación de las nanopartículas de plata y la formación del film de quitosano. Dichas etapas han sido estudiadas con tal de optimizar la estabilidad de la capa y la respuesta antibacteriana in vitro.

  • Obtención y caracterización de un recubrimiento de poli(etilenglicol) sobre titanio por polimerización por plasma

     Buxadera Palomero, Judit; Gil Mur, Francisco Javier; Canal Barnils, Cristina; Rodriguez Rius, Daniel
    Congreso de la Sociedad Ibérica de Biomecánica y Biomateriales
    Presentation's date: 2013-10-26
    Presentation of work at congresses

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    En este trabajo se ha estudiado la formación de un recubrimiento de poli(etilenglicol) (PEG) sobre la superficie de titanio comercialmente puro de grado 2 para conferir a la superficie carácter antifouling con respecto a la adsorción de proteínas y a la adhesión bacteriana. Se ha escogido como método de inmovilización la polimerización por plasma, que es un método rápido que permite enlazar el polímero con la superficie. Este proceso consta de dos etapas: la activación superficial y la polimerización. Dichas etapas han sido estudiadas con tal de conseguir la mayor activación y el recubrimiento con mejores propiedades antifouling respecto a las proteínas y a las bacterias.

  • Microstructural characterization of a potential superelastic nickel-free titanium alloy

     Herranz, Carolina; Schaffer, Jeremy; Todorov Trifonov, Trifon; Gil Mur, Francisco Javier; Manero Planella, Jose M.
    Microscopy at the Frontiers of Science
    Presentation's date: 2013-09
    Presentation of work at congresses

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  • Bonlike apatite formation on the surface of chemically treated tantalum susbtrates

     Foixench, M.T.; Caparros Vazquez, Cristina Maria; Rodriguez Contreras, Alejandra Maria; Rupérez De Gracia, Elisa; Manero Planella, Jose M.; Gil Mur, Francisco Javier
    Microscopy at the Frontiers of Science
    Presentation's date: 2013-09-17
    Presentation of work at congresses

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  • Obtention and characterization of new superelastic polymer for biomedical applications. Comparison with NiTi and NiTiCu alloys

     Varela, J.C.; Velo, M.; Espinar Escalona, Eduardo; Llamas, Jose Maria; Gil Mur, Francisco Javier
    Materials letters
    Date of publication: 2013
    Journal article

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  • Friction coefficients and wear rates of different orthodontic archwires in artificial saliva

     Alfonso, M.V.; Espinar, E.; Llamas, J.M.; Rupérez De Gracia, Elisa; Manero Planella, Jose M.; Barrera, J.M; Solano, E.; Gil Mur, Francisco Javier
    Journal of materials science. Materials in medicine
    Date of publication: 2013-05
    Journal article

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    The aim of this paper is to analyze the influence of the nature of the orthodontic archwires on the friction coefficient and wear rate against materials used commonly as brackets (Ti–6Al–4V and 316L Stainless Steel). The mate- rials selected as orthodontic archwires were ASI304 stainless steel, NiTi, Ti, TiMo and NiTiCu. The array archwire’s materials selected presented very similar roughness but different hardness. Materials were chosen from lower and higher hardness degrees than that of the brackets. Wear tests were carried out at in artificial saliva at 37 C. Results show a linear relationship between the hardness of the materials and the friction coefficients. The material that showed lower wear rate was the ASI304 stainless steel. To prevent wear, the wire and the brackets have high hardness values and in the same order of magnitude.

  • Preventive midline laparotomy closure with a new bioabsorbable mesh: An experimental study

     López Cano, Manuel; Armengol Carrasco, Manuel; Quiles Pérez, María Teresa; Biel Arrufat, Alejandro; Velasco, Janice; Huguet, Pere; Mestre Vinardell, Aleix; Delgado Garoña, Luis María; Gil Mur, Francisco Javier; Arbós Vilà, Maria Antonia
    Journal of surgical research
    Date of publication: 2013-05
    Journal article

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  • Effect of temperature on the orthodontic clinical applications of NiTi closed-coil springs

     Espinar Escalona, Eduardo; Llamas Carreras, Jose Maria; Barrera Mora, Jose Maria; Ábalos, C.; Gil Mur, Francisco Javier
    Medicina oral, patología oral y cirugia bucal
    Date of publication: 2013-07-01
    Journal article

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    NiTi spring coils were used to obtain large deformation under a constant force. The device consists on a NiTi coil spring, superelastic at body temperature, in order to have a stress plateau during the austenitic retransformation during the unloading. The temperature variations induced changes in the spring force. Objectives: The aim of this study is to investigate the effect of the temperature variations in the spring forces and corrosion behaviour simulating the ingestion hot/cold drinks and food. Study Design: The springs were subjected to a tensile force using universal testing machine MTS-Adamel (100 N load cell). All tests were performed in artificial saliva maintained at different temperatures. The corrosion tests were performed according to the ISO-standard 10993-15:2000. Results: The increase in temperature of 18°C induced an increase in the spring force of 30%. However, when the temperature returns to 37°C the distraction force recovers near the initial level. After cooling down the spring to 15oC, the force decreased by 46%. This investigation show as the temperature increase, the corrosion potential shifts towards negative values and the corrosion density is rising. Conclusions: The changes of the temperatures do not modify the superelastic behaviour of the NiTi closed-coil springs. The corrosion potential of NiTi in artificial saliva is decreasing by the rise of the temperatures.

  • Surface functionalization of metallic biomaterials with antibacterial compounds

     Rodriguez Rius, Daniel; Gil Mur, Francisco Javier
    European cells and materials
    Date of publication: 2013-10-01
    Journal article

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  • A bioactive elastin-like recombinamer reduces unspecific protein adsorption and enhances cell response on titanium surfaces.

     Salvagni, Emiliano; Berguig, Geoffrey Yehuda; Engel Lopez, Elisabet; Rodriguez Cabello, Jose Carlos; Coullerez, Geraldine; Textor, Marcus; Planell Estany, Josep Antón; Gil Mur, Francisco Javier; Aparicio, Conrado
    Colloids and Surfaces B. Biointerfaces
    Date of publication: 2013-10-17
    Journal article

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    We present the immobilization on synthetic substrates of elastin-like recombinamers (ELR) that combine a bioactive motif for cell adhesion with protein antifouling properties. Physical adsorption of the recombinamers and covalent-grafting through organosilane chemistry were investigated. The biochemically-modified surfaces were thoroughly characterized and tested for protein absorption in serum by fluorescence-labelling, XPS, Ellipsometry, and OWLS. The ELR were successfully grafted and stable, even upon mechanical stresses; being the covalent bonding favourable over physical adsorption. The coated metal surfaces exhibited excellent reduction of serum protein adsorption (9 ng/cm2) compared to the bare metal surface (310 ng/cm2). Non-specific protein adsorption may mask the introduced bioactive motifs; therefore, the bioactivated surfaces should display serum-protein antifouling properties. Finally, improved hMSCs response was assessed on the bioactivated substrates. In summary, the coatings simultaneously displayed anti-fouling and bioactive properties. These studies investigated key factors to enhance tissue material interactions fundamental for the design of bioactive devices and future biomedical applications

  • In-vitro response of pre-osteoblastic MG63 cells on Ni-free Ti shape memory substrates

     Arciniegas, Milena; Peña Andrés, Javier; Gil Mur, Francisco Javier; Manero Planella, Jose M.
    Journal of biomedical materials research. Part B, Applied biomaterials
    Date of publication: 2013
    Journal article

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    Ni-free Ti alloys are a potential strategy to overcome the risk of Ni-adverse reactions and rigidity mismatch for implant materials. Here, we report the biological behavior induced for two promising candidate alloys¿Ti19.1Nb8.8Zr (MS temperature of 46°C and elastic modulus of 74 GPa) and Ti41.2Nb6.1Zr (elastic modulus of 67 GPa)¿on cultured MG63 cells, as well as their physical and chemical properties. Contact angle results revealed the hydrophobic character of the former alloy (59.02° ± 2.35°) attributed to the presence of the martensitic phase, while the latter one presented a hydrophilic response (67.77° ± 2.78°). Results showed also that the cell adhesion response (after 4 and 8 h of incubation) in both substrates was not statistically different to that obtained in the cp Ti as control material. These surfaces induced well spread cell morphology with cytoplasmic extension like filopodia of up to 100 µm even at short culture times and presented an uninterrupted proliferation after longer incubation times (9 days). A decrement in the proliferation rate was appreciated from the Ti19.1Nb8.8Zr surface at that time, which was attributed to an earlier activation of the cell differentiation stage, as confirmed by the twofold increment of alkaline phosphatase activity. The results also evidenced that the presence of a 2 nm thick layer of amorphous Nb2O5, which was detected on both alloys, has a significant effect on cell behavior favoring the cell adhesion and morphology response of the new alloys studied

  • S. sanguinis adhesion on rough titanium surfaces: Effect of culture media

     Rodríguez Hernández, Ana Guadalupe; Godoy Gallardo, Maria; Gil Mur, Francisco Javier; Juarez, Antonio; Muñoz Tabares, Jose Alejandro
    Materials science and engineering C. Biomimetic and supramolecular systems
    Date of publication: 2013-03-01
    Journal article

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    Bacterial colonization plays a key role in dental implant failure, because they attach directly on implant surface upon implantation. Between different types of bacteria associated with the oral environment, Streptococcus sanguinis is essential in this process since it is an early colonizer. In this work the relationship between titanium surfaces modified by shot blasting treatment and S. sanguinis adhesion; have been studied in approached human mouth environment. Bacteria pre-inoculated with routinary solution were put in contact with titanium samples, shot-blasted with alumina and silicon carbide, and adhesion results were compared with those obtained when bacteria were pre-inoculated with modified artificial saliva medium and on saliva pre-coated titanium samples. Our results showed that bacterial adhesion on titanium samples was influenced by culture conditions. When S. sanguinis was inoculated in routinary culture media, colonies forming unities per square millimeter presented an increment correlated with roughness and surface energy, but separated by the type of particle used during shot-blasting treatment; whereas in modified artificial saliva only a relationship between bacteria adhered and the increment in both roughness and surface energy were observed, regardless of the particle type. Finally, on human saliva pre-coated samples no significant differences were observed among roughness, surface energy or particle.

  • Alumina shot-blasted particles on commercially pure titanium surfaces prevent bacterial attachment

     Rodríguez Hernández, Ana Guadalupe; Espinar Escalona, Eduardo; Llamas, Jose Maria; Barrera, J.; Gil Mur, Francisco Javier
    Materials letters
    Date of publication: 2013-02-01
    Journal article

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  • NiTi superelastic orthodontic wires with variable stress obtained by ageing treatments

     Gil Mur, Francisco Javier; Cenizo, M.; Espinar Escalona, Eduardo; Rodriguez Contreras, Alejandra Maria; Rupérez De Gracia, Elisa; Manero Planella, Jose M.
    Materials letters
    Date of publication: 2013-08
    Journal article

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    A new strategy to obtain NiTi orthodontic archwires with variable correcting stresses in different segments is presented. Different heat treatments are applied in selected segments, which produce variations in the superelastic properties. These allow to modulate the correcting stresses to the requirements of the specific teeth. This method avoids laser welding, which is associated with corrosion and brittleness problems. The aim of this study is to analyze the effect of the heat treatment by zones on transformation temperatures, and stresses in NiTi orthodontic archwires with identical chemical composition. A reduction of the Ti content is observed, in the matrix of the posterior segment, due to the formation of Ti2Ni precipitates. This produces a decrease of the transformation temperatures and consequently an increase of correction stresses. The changes are smaller in the lateral segment due to the lower temperature reached. No changes are observed in the anterior segment in relation to the original archwire. The titanium-rich precipitates undergo observation and characterization by Transmission Electron Microscopy (TEM) and electron diffraction.

  • A Constitutive Model of Human Esophagus Tissue with Application for the Treatment of Stenosis  Open access

     Sanchez Molina, David
    Defense's date: 2013-11-07
    Universitat Politècnica de Catalunya
    Theses

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    This dissertation is a research about the mechanical behavior of the human esophagus. This work is intended to be applied in the treatment of stenosis and other esophageal diseases that frequently require a procedure of forced dilation, that involves high pressures on the esophagus wall. This study proposes a constitutive model to simulate forced dilatations. This study includes the experimental characterization of the mechanical behavior of human esophagus. In addition, some theoretical questions and experimental issues were addressed and solved. This dissertation summarizes the previous work on esophageal tissues by other authors. Additionally, a short explanation about the microcontinuum theory developed in the last decades is given, as well as a summary of the general theory of nonlinear hyperelastic constitutive models (with large deformation). This study required extensive testing of esophageal tissue in order to characterize the in vitro mechanical behavior. The testing included mainly tensile tests and complementary inflation tests. Optical motion track analysis was used for accurate computation of the strains in the tissue. The results of the tests were used for adjusting the mechanical properties that characterize the mechanical behavior of esophagus in the proposed models of the literature. The statistical analysis of the data revealed, some significant correlations between anthropometric factors, such as the body mass index, and some mechanical properties were found in the analysis of the data. The typical values of the mechanical properties were used to perform some numerical finite element simulations based on the proposed models. In addition, a number of theoretical results were obtained concerning the residual stress and the predictions of statistical mechanics for a system of collagenous fibers inside a soft tissue. The main result is a constitutive non-linear microstretch anisotropic hyperelastic constitutive model with large deformations (and with residual stresses) to characterize the multi-layered tissue of human esophagus. This model is suitable for numerical simulation.

    Esta tesis es una investigación sobre el comportamiento mecánico del esófago humano. Este trabajo se pensó para ser aplicado al tratamiento de la estenosis y otras afecciones esofágicas que, con frecuencia, requieren dilatación forzada, lo que supone altas presiones sobre la pared esofágica. Este estudio propone un modelo constitutivo para simular estas dilataciones forzadas. Este estudio incluye la caracterización experimental del comportamiento mecánico del esófago. Además, se han planteado algunas cuestiones teóricas y experimentales que han sido resueltas. Esta tesis resume el trabajo previo sobre tejido esofágico de otros investigadores. Además, se da una pequeña explicación sobre la teoría del medio microntinuo desarrollada en las últimas décadas y un breve resumen de la teoría general de modelos constitutivos hiperelásticos no-lineales (con grandes deformaciones). El estudio requirió experimentación de tejido para caracterizar el comportamiento in vitro. Los test incluyeron test de tracción y test de inflado. Se empleó rastreo óptico para un cálculo adecuado de la deformación. Los resultados de los test permitieron encontrar las propiedades mecánicas según dos modelos de esófago de la literatura. El análisis de los datos rebeló, algunas correlaciones significativas entre factores como el índice de masa corporal y algunas propiedades mecánicas. Los valores típicos de las propiedades fueron usados para algunas simulaciones numéricas basadas en los modelos propuestos. Además se han obtenido algunos resultados teóricos sobre la tensión residual y las predicciones de la mecánica estadística para un sistema de fibras de colágeno del tejido. El principal resultado es un modelo constitutivo de microestiramiento anisótropo no-lineal e hiperelástico para caracterizar el esófago Este modelo es adecuado para la computación numérica.

  • Study for Poly[(R)-3-Hydroxybutyrate] production by bacterial strains and its modification for drug delivery systems.  Open access

     Rodriguez Contreras, Alejandra Maria
    Defense's date: 2013-06-06
    Universitat Politècnica de Catalunya
    Theses

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    Nowadays biopolymers are a good alternative to petrochemical polymers. One of these biopolymers is Poly[(R)-3- Hydroxybutyrate] (PHB) which is produced from renewable resources by various microorganisms and, after its use it can be composted. It has different applications as bulk material in packing films, containers or paper coatings. Due to its excellent biocompatibility and biodegradability, PHB is a potential material for applications in drug delivery. It is therefore important to continue investigating the different strategies to ensure the competitiveness between these biopolymers and petroleumbased polymers. The first part of the thesis is mainly focused on finding a new PHB-producing bacterium capable of developing and producing a significant concentration of biopolymer using one of the conventional medium for PHB industrial production. Therefore, four water and mud samples were taken from four Bolivian salty lakes and the microorganisms were isolated in order to detect the best PHB-producing bacterial strain. A bacterium identified as a new strain of the genus Bacillus was selected for polymer production studies. This microorganism was tested under fed-batch fermentations. The results showed a high specific growth rate, and a percentage of 70% PHB in cell dry mass , with limitation in nitrogen source. The strain not only grew properly in the industrial condition proposed, but it also produced and accumulated a larger content of PHB than ever reached before for its genus. The strain was deposited in the Spanish Type Culture Collection (CECT), as Bacillus megaterium uyuni S29. The characterization of the resultant biopolymers concluded that the strain synthesized PHB homopolymer with two main molecular masses around 600 and 125 kDa with polydispersity index of 1.2 and 1.5 respectively. Moreover, the thermal analyses of the biomaterial showed different properties compared to the ones of common PHB, enlarging the application possibilities to this biopolyester. After obtaining the polymer from the bacteria, the second part was focused on its transformation. A sustainable degradation process set out for an easy industrial scale application was proposed in the second part of this thesis. A copolymer from PHA family, poly[3-hydroxybutyrate-co-4-hydroxybutyrate] , was used to carry out an enzymatic degradation of the material. Two commercially available lipases were used to decrease the polymer molecular mass to oligomers between 5 and 1 kDa. It was the first time that these triglyceride lipases were used for this type of application and due to the positive results one of them was used for degradation of PHB. The results confirmed the enzymatic reaction of the used lipase with PHB and showed a controlled decrease of the molecular mass from 300 kDa to 4 kDa. In the third part of the study, the application of the PHB as a drug delivery system was analyzed. Doxycycline is a well known broad-spectrum antibiotic but there are some concerns over its possible side effects. In order to avoid this problem and reach the infection with an effective drug concentration, protection and controlled delivery of doxycycline are desirable. Thus, different drug-entrapment and emulsification methods were studied in order to obtain optimal doxycycline -loaded PHB micro- and nano-particles. The results showed that the combination of ultrasounds with high speed stirring in the preparation of double emulsion is highly effective in obtaining doxycycline -loaded PHB particles with high drug loading and entrapment efficiency, and with great method efficiency. Furthermore, the qualitative antibacterial activity found in different formulations show that these particles are good candidates for drug delivery systems. These best methods were used with the PHAs produced throughout the thesis in order to confirm their suitability for different PHAs and to study the possibility of improving the results of drug entrapment and method efficiency.

    Actualmente, los biopolímeros son una buena alternativa a los polímeros derivados del petróleo. Uno de estos biopolímeros es el poli[(R)-3-hidroxibutirato] (PHB) producido a partir de recursos renovables por diversos microorganismos. Tiene diferentes aplicaciones como material a granel para films de embalaje, recipientes o revestimientos de papel. Debido a su excelente biocompatibilidad y biodegradabilidad, el PHB es un material con gran potencial para ser aplicado como vehículo para administración de fármacos. La primera parte de la tesis se centra en la búsqueda de una nueva bacteria productora de PHB capaz de desarrollar y producir una concentración significativa de biopolímero usando un medio convencional de forma industrial. Se partió de cuatro muestras de agua y barro tomadas de cuatro lagos salados de Bolivia. Los microorganismos se aislaron con el fin de detectar las mejores cepas bacterianas productoras de PHB. Para los estudios de producción de polímeros, se seleccionó una nueva cepa del género Bacillus, identificada como Bacillus megaterium uyuni S29. Se utilizó este microorganismo en diferentes fermentaciones fed-batch. Los resultados mostraron una alta tasa de crecimiento específico y se llegó a un porcentaje final de PHB de 70% en masa celular, llegando a limitar la fuente de nitrógeno. La cepa no sólo creció adecuadamente en las condiciones industriales propuestas, sino que también produjo y acumuló un gran contenido de PHB que no se había logrado antes con este género. La caracterización de los biopolímeros resultantes concluyó que Bacillus megaterium uyuni S29 sintetiza PHB homopolímero con dos masas moleculares principales de alrededor de 600 y 125 kDa con índices de polidispersidad de 1,2 y 1,5 respectivamente. Además, los análisis térmicos mostraron propiedades diferentes a las del PHB común, ampliando las posibilidades de aplicación de este biopoliéster. Después de obtener el polímero, la segunda parte de la tesis se centró en el estudio de su transformación. Por lo tanto, se estudió una propuesta de proceso sostenible de degradación de PHAs pensada para una posterior aplicación a escala industrial. Se utilizó un copolímero de la familia de los PHAs, el poli(3-hidroxibutirato-co-4- hidroxibutirato), para llevar a cabo su degradación enzimática. Se emplearon dos lipasas comerciales para disminuir la masa molecular del polímero y obtener oligómeros con masa molecular entre 5 y 1 kDa. Fue la primera vez que dichas lipasas de triglicéridos han sido utilizadas con este copolímero. Por consiguiente, se empleó una de ellas para la degradación de PHB. Se confirmó que la reacción enzimática de esta lipasa con el PHB produjo una disminución controlada de la masa molecular de 300 kDa a 4 kDa. En la tercera parte de la tesis se analizó la aplicación del PHB como sistema de liberación de fármaco. Doxiciclina es un conocido antibiótico de amplio espectro. Con el fin de evitar efectos secundarios y llegar a la infección con una concentración de fármaco eficaz, se requiere una protección y administración controlada de doxiciclina . Así que se estudiaron diferentes métodos de atrapamiento molecular y de preparación de emulsificaciones con el fin de obtener micro- y nano-partículas de PHB cargadas con doxiciclina . Los resultados mostraron que la combinación de ultrasonidos con agitación a alta velocidad en la preparación de emulsión doble es muy eficaz para la obtención de estas partículas. Además, los resultados de actividad antibacteriana llevados a cabo con estas partículas mostraron que son buenas candidatas para la liberación doxiciclina . Los mejores métodos encontrados para la formación de partículas de PHB se utilizaron con los PHAs producidos a lo largo de la tesis para confirmar su idoneidad con otros PHAs.

  • Functionalization of titanium surfaces with TGF-beta inhibitor peptides  Open access

     Sevilla Sanchez, Pablo
    Defense's date: 2013-07-16
    Universitat Politècnica de Catalunya
    Theses

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    Esta tesis queda enmarcada en el ámbito de los biomateriales metálicos, concretamente en superficies de titanio desarrolladas para la regeneración ósea. Las aplicaciones más habituales del titanio como biomaterial son los implantes dentales y las prótesis de cadera y rodilla. Estos componentes requieren, en servicio, buena estabilidad y fijación al hueso a largo plazo. El titanio es un material idóneo para el cumplimiento de estos requisitos gracias a su alta resistencia mecánica, tenacidad, resistencia a la corrosión y, sobre todo, por su alta capacidad de osteointegración. En general, el titanio es un biomaterial bioinerte donde, una vez implantado, el tejido vivo genera una fina capa de tejido fibroso alrededor del implante la cual separa el hueso del implante. Un espesor excesivo de esta capa de tejido fibroso puede comprometer la estabilidad e integración del implante y conllevar el fracaso del tratamiento. El objetivo principal de esta tesis es el desarrollo de una nueva superficie de titanio que sea capaz de controlar e inhibir la generación de tejido fibroso en la superficie del implante. De esta manera, tratamos de mejorar la osteointegración de implantes y prótesis mediante la mejora de la respuesta celular sobre la superficie del implante. Para el control del crecimiento de tejido fibroso en la superficie se han desarrollado nuevas superficies de titanio donde se han inmovilizado dos tipos de péptidos cortos capaces de inhibir la interacción de la citoquina TGF-β, la cual incrementa la producción de este tipo de tejido por parte de las células fibroblásticas. Estos péptidos, llamados P17 y P144 han sido desarrollados por el equipo de nuestro colaborador el Dr. Francisco Borrás-Cuesta, en el Centro de Investigación Médica aplicada de la Universidad de Navarra. Esta tesis está dividida en 6 capítulos donde se describe el desarrollo y caracterización de las superficies de titanio funcionalizadas con péptidos inhibidores del TGF-β: • Capítulo 1: Introducción a los ámbitos y conceptos importantes de la tesis. • Capítulo 2: Diseño y desarrollo de un método de inmovilización covalente de péptidos cortos sobre superficies de titanio. • Capítulo 3: Estudio de los factores que intervienen en la inmovilización de péptidos cortos sobre las superficies de titanio. • Capítulo 4: Caracterización físico-química de las superficies de titanio funcionalizadas con el péptido P17. • Capítulo 5: Caracterización físico-química de las superficies de titanio funcionalizadas con el péptido P144. • Capítulo 6: Respuesta biológica in vitro de las superficies de titanio funcionalizadas con P17 y P144. Los resultados más relevantes en el desarrollo de esta tesis han sido: • El desarrollo de un nuevo método de inmovilización covalente de péptidos sobre superficies de titanio obteniendo una alta densidad de péptido en superficie con una buena estabilidad mecánica y termoquímica. • La consecución de superficies de titanio capaces de inhibir la acción del TGF-β. • Las nuevas superficies desarrolladas son capaces de incrementar la diferenciación osteoblástica y así, potencialmente mejorando la capacidad de osteointegración de implantes y prótesis de titanio. Este trabajo de investigación contribuye a aumentar el conocimiento sobre la inmovilización covalente y no covalente de péptidos cortos en superficies de titanio. También contribuye en aumentar el conocimiento de la acción e inhibición del TGF-β en células fibroblasticas y osteoblásticas, estas últimas sembradas sobre superficies de titanio. El material desarrollado es un excelente candidato para su aplicación en implantología y traumatología ósea.

    This thesis is framed in the field of metallic biomaterials, specifically on titanium surfaces developed for bone regeneration. The most common applications of titanium as a biomaterial are dental implants and hip and knee prostheses. These components clinically require good stability and fixation to the bone in the long term. Titanium is an ideal material for these applications as it has high mechanical strength, toughness, corrosion resistance and, above all, a high capacity for osseointegration. In general, titanium is a bioinert material where, once implanted, the living tissue generates a thin layer of fibrous tissue around the implant which separates the bone to the implant. An excessive thickness of this layer of fibrous tissue can compromise the stability and integration of the implant leading to the failure of the biomedical treatment. The main objective of this thesis is the development of a new titanium surface with control and inhibition of the generation of fibrous tissue on the surface of the implant. We aim improving the osseointegration of implants and prostheses by benefiting cellular responses on the surface of the implant. For the control of the formation of fibrous tissue on the surface we have developed new biofunctional titanium surfaces by covalently immobilizing two different short peptides on the metallic substrate. These two peptides are inhibitors of the effect of the cytokine TGF-β1, which increases the production of fibrous tissue by the activity of fibroblastic cells. These peptides, P17 and P144, have been developed by the team of our collaborators at the Dr. Francisco Borrás-Cuesta’s lab, in the Centro de Investigación Médica Aplicada of the Universidad de Navarra This thesis is divided into 6 chapters describing the development and characterization of titanium surfaces functionalized with TGF-β inhibitor peptides: * Chapter 1: Introduction to the areas and important concepts of the thesis. • Chapter 2: Design and development of a method of covalent immobilization of short peptides on titanium surfaces. • Chapter 3: Study of the factors involved in the immobilization of short peptides on the titanium surfaces. • Chapter 4: Physical-chemical characterization of titanium surfaces functionalized with the P17 peptide. • Chapter 5: Physical-chemical characterization of titanium surfaces functionalized with the P144 peptide. • Chapter 6: In vitro biological response of titanium surfaces functionalized with P17 and P144. The most relevant results in the development of this thesis are: • The development of a new method of covalent immobilization of peptides on titanium surfaces with a high density of peptide on the surface and with a good mechanical and thermal-chemical stability. • The development of titanium surfaces with inhibitory action of TGF-β activity. • The developed new surfaces are able to increase osteoblast differentiation, thereby potentially enhancing osseointegration of the biofunctionalized titanium implants and prostheses. This research work contributes to increase the knowledge on covalent and noncovalent immobilization of short peptides on titanium surfaces. It also helps in increasing the knowledge of the action and inhibition of TGF-β on fibroblastic and osteoblastic cells; the later seeded on titanium surfaces. The developed material is an excellent candidate for its application in implantology and orthopedics.

  • Premi Henry Schein 2013

     Guillem Marti, Jordi; Delgado Garoña, Luis María; Godoy Gallardo, Maria; Pegueroles Neyra, Marta; Herrero, Mariano; Gil Mur, Francisco Javier
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  • Surface functionalization of metallic biomaterials with antibacterial compounds

     Rodriguez Rius, Daniel; Gil Mur, Francisco Javier
    International symposium on surface and interface of biomaterials
    Presentation's date: 2013-09-25
    Presentation of work at congresses

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  • NUEVOS BIOMATERIALES METALICOS BIOFUNCIONALIZADOS PARA APLICACIONES ORTOPEDICAS,

     Lluch Margarit, Sara; Gil Mur, Francisco Javier
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  • Comparative study on AISI 440 and AISI 420B stainless steel for dental drill performance

     Albertini, M.; Herrero Climent, Mariano; Lázaro, Pedro; Ríos, Jose Vicente; Gil Mur, Francisco Javier
    Materials letters
    Date of publication: 2012-07-15
    Journal article

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    One of the most usual causes of the failure in dental implant osseointegration is the increase of the temperature above 47 °C during the drilling of the bone because it produces irreversible osteonecrosis. The result is weakened contact of implants with bone and possible loss of rigid fixation. Many studies about the design of the drill bit, contact forces, drill speed, drill point angle and feed-rate have been made. However, in all studies a martensitic stainless steel (AISI 440) has been used. The aim of this study was to determine the behavior of AISI420B stainless steel with higher hardness, higher heat conductivity and lower wear than the conventional stainless steel used in oral implantology. This steel showed adequate temperature increases, with or without irrigation, and a decrease of the weight lost of the drills with use.

  • Fibroblast adhesion and activation onto micro-machined titanium surfaces

     Guillem Marti, Jordi; Delgado Garoña, Luis María; Godoy Gallardo, Maria; Pegueroles Neyra, Marta; Herrero, Mariano; Gil Mur, Francisco Javier
    Clinical oral implants research
    Date of publication: 2012-03-11
    Journal article

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    Objectives: Surface modifications performed at the neck of dental implants, in the manner of micro-grooved surfaces, can reduce fibrous tissue encapsulation and prevent bacterial colonization, thereby improving fibrointegration and the formation of a biological seal. However, the applied procedures are technically complex and/or time consuming methods. The aim of this study was to analyse the fibroblast behaviour on modified titanium surfaces obtained, applying a simple and low-cost method

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  • Corrosion and corrosion-fatigue behavior of cp-Ti and Ti-6Al-4V laser-marked biomaterials

     Gil Mur, Francisco Javier; Delgado, Luís María; Espinar Escalona, Eduardo; Llamas, Jose Maria
    Journal of materials science. Materials in medicine
    Date of publication: 2012-04
    Journal article

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  • Adsorption of fibronectin, fibrinogen and albumin on TiO2: A kinetics, structural changes, and competition study

     Pegueroles Neyra, Marta; Tonda Turo, Chiara; Planell Estany, Josep Antón; Gil Mur, Francisco Javier; Aparicio, Conrado
    Journal of the Royal Society Interface
    Date of publication: 2012-12
    Journal article

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  • Analysis of tantalum implants used for avascular necrosis of the femoral head: A review of five retrieved specimens

     Fernández-Fairén, Mariano; Murcia, A.; Iglesias, Roberto; Sevilla Sanchez, Pablo; Manero Planella, Jose M.; Gil Mur, Francisco Javier
    Journal of applied biomaterials and biomechanics
    Date of publication: 2012
    Journal article

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  • Caracterización y Optimización de Superfícies Biomimétricas pra Regeneración de Tejido Óseo  Open access

     Paredes Méndez, Virginia Nathaly
    Defense's date: 2012-10-26
    Department of Automatic Control, Universitat Politècnica de Catalunya
    Theses

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    Este proyecto se propone caracterizar y optimizar superficies biofuncionalizadas con diferentes secuencias peptídicas, para lograr la regeneración ósea (oseointegración) y por ende la disminución de los problemas de rechazo que ocurren al implantar materiales metálicos dentro del cuerpo humano. En base a lo descrito bibliográficamente, se utilizará una aleación de CoCr aprobada por las normas ASTM, para usos en dispositivos médicos y una aleación de Ti libre de Níquel desarrollada para tal fin por el grupo de biomateriales de la UPC. Para la caracterización y optimización del proceso de biofuncionalización los estudios se dividirán en tres etapas: Limpieza y Activación, Silanización e Inmovilización de biomoléculas. En cuanto a la limpieza y activación se realizará un estudio comparativo entre el plasma y diferentes tratamientos químicos (piraña en el caso de la aleación de Ti y ácido nítrico para la aleación de CoCr), para seleccionar el mejor en términos de introducción de grupos activos en superficie (grupos hidroxilos), grado de limpieza y composición química de la capa de óxidos superficial. La silanización es un proceso intermedio que enlaza un material inorgánico (metal) con un material orgánico (biomoléculas), en este proyecto se usarán 3 silanos: APTES+Maleimido, GPTES, CPTES sobre cada una de las superficies y se procederá a seleccionar aquel que presente el mejor enlace covalente con la superficie metálica y la mayor estabilidad térmica, química y mecánica. Una vez silanizadas las superficies se realizará la inmovilización de diversas secuencias peptídicas (RGD, PHSRN, FHRRIKA, RGD + FHRRIKA Y RGD + PHSRN), que forman parte de las proteínas presentes en el cuerpo humano y por ende podrán ser fácilmente reconocidas por las células; en esta fase se hará uno estudio comparativo de la cantidad de peptidos, así como se evaluará también la estabilidad de los mismos sobre las superficies. Durante el desarrollo de la biofuncionalización se hará énfasis en la optimización de los procedimientos y la caracterización superficial de cada etapa por medio de diversas técnicas, entre ellas: XPS, ángulo de contacto, ToF SIMS, Interferometría, espectrometría de luz UV, y técnicas de fluorescencia. Para finalizar se evaluará el proceso de optimización, estudiando la influencia de las secuencias pépticas cortas en la respuesta celular, en términos de adhesión y proliferación de células madres mesenquimales de ratas.

    The aim of this project is to characterise and optimise biofunctionalised surfaces bearing different peptide sequences in order to achieve an improved bone regeneration (osteointegration) and to reduce rejection problems associated with metal implant materials in human body. On the basis of previous studies reported in the literature, a CoCr alloy approved by the American Society for Testing and Materials (ASTM) was chosen. This material has been widely used for biomedical devices. In addition, a nickel free Ti alloy, previously developed in the biomaterials group at the UPC, was also investigated for the same purpose. The biofunctionalised surface were achieved in three fundamental steps and characterised after each modification: 1) Cleaning and activation, 2) Silanization and 3) biomolecule immobilization. As for the cleaning and activation a comparative study between oxygen plasma and acidic treatment (piranha solution for Ti alloy and nitric acid for CrCo alloy) was performed with the aim to select the best method to oxidise the surface, introduce hydroxyl groups and simultaneously remove impurities. Silanization is an intermediary step that allows to bind an inorganic material (metal) to an organic material (biomolecule). The organosilanes employed on each metal surface for this purpose were three: 3-aminopropyltriethoxisilane (APTES) further derivitised with a Maleimide group for activation, 3-glycidoxypropyltriethoxisilane (GPTES), 3-chloropropyltriethoxisilane CPTES. Covalent binding and mechanical, chemical and thermical stability at the surface were the criteria followed to determine the best silanization method. The following step was the surface immobilization of different peptide sequences (RGD, PHSRN, FHRRIKA, RGD + FHRRIKA Y RGD + PHSRN), which are the ¿active part¿ of more complex proteins present in the human body that cells may easily recognise and bind. A comparative studies of amount of bound peptide was carried out along with stability studies at the surface. In order to develop and optimise the whole biofunctionalisation process each modification step was fully characterised by several analitical techniques, such as XPS, contact angle, Tof-SIMS, interferometry, UV ligt spectrometry and fluorescence techniques. Finally, to select the best biofunctionalised material samples were tested for mesenchymal rat stem cells (MRSCs) response in terms of number of cells adhered and proliferation at the surface. In conclusion, this study has proven that: for surface cleaning and activation, either acidic treatments or oxygen plasma demonstrated to be effective for removal of impurities, increase of hydrophilicty and higher surface energy. Moreoever, the optimization process led to the conclusion that for optimal surface activation a high ratio of OH-/O2- is necessary. For CoCr the most effective method for the introduction of hydroxyl groups density at the surface and therefore a higher OH -/O2- ratio was nitric acid, whereas for the Ti alloy was oxygen plasma.

  • Distinguished Professor in Biomaterials

     Gil Mur, Francisco Javier
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  • Desarrollo y funcionalización de espumas metálicas de titanio de alta porosidad interconectada y mínima rigidez para aplicaciones biomédicas. Proyecto ¿BioA+¿. AME12-C04

     Molmeneu Trias, Meritxell; Punset Fusté, Miquel; Caparros Vazquez, Cristina Maria; Gil Mur, Francisco Javier
    Date: 2012-12-12
    Report

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  • Estudio comparativo de la resistencia al desgaste de diferentes fresas quirúrgicas.

     Gil Mur, Francisco Javier; Punset Fusté, Miquel; Molmeneu Trias, Meritxell; Fernandez Yagüe, Marc-antoni; Ortiz Hernandez, Monica
    Date: 2012-12-10
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  • Access to the full text
  • Estudi preliminar cargol i clau Ball Head System: Avaluació de la resistència a torsió a 0º, 20º i 30º mitjançant torquímetre manual

     Gil Mur, Francisco Javier; Ortiz Hernandez, Monica; Buxadera Palomero, Judit; Delgado, Luís María
    Date: 2012-04-16
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  • Análisis de fallos de implantes fracturados

     Punset Fusté, Miquel; Gil Mur, Francisco Javier; Rodriguez Rius, Daniel
    Date: 2012-11-19
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  • Caracterización superficial de los implantes PHIBO TSH-S4

     Punset Fusté, Miquel; Gil Mur, Francisco Javier; Rodriguez Rius, Daniel
    Date: 2012-11-16
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  • Determinación del ángulo de contacto de 2 muestras

     Fernandez Yagüe, Marc-antoni; Gil Mur, Francisco Javier
    Date: 2012-06-19
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    Evaluación de implantes dentales de Ti c.p. grado 4 C  Open access

     Pegueroles Neyra, Marta; Gil Mur, Francisco Javier
    Date: 2012-07-23
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  • Implants dentals biofuncionalitats

     Gil Mur, Francisco Javier
    Participation in a competitive project

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    Evaluación de implantes dentales de Ti c.p. grado 4 A  Open access

     Pegueroles Neyra, Marta; Gil Mur, Francisco Javier
    Date: 2012-07-23
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    Evaluación de implantes dentales de Ti c.p. grado 4 B  Open access

     Pegueroles Neyra, Marta; Gil Mur, Francisco Javier
    Date: 2012-07-23
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  • Estudio estadistico de datos procedentes de análisis

     Molmeneu Trias, Meritxell; Gil Mur, Francisco Javier
    Date: 2012-06-15
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  • Desarrollo y funcionalización de espumas metálicas de titanio de alta porosidad interconectada y mínima rigidez para aplicaciones biomédicas. Proyecto ¿BioA+¿

     Molmeneu Trias, Meritxell; Gil Mur, Francisco Javier; Punset Fusté, Miquel; Caparros Vazquez, Cristina Maria
    Date: 2012-10-03
    Report

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    Determinación de la rugosidad superficial de una placa polimérica GRATEC y biocompatibilidad Cr, Mo y Zr.  Open access

     Punset Fusté, Miquel; Pegueroles Neyra, Marta; Gil Mur, Francisco Javier; Fernandez Yagüe, Marc-antoni
    Date: 2012-02-24
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