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Commercially pure titanium (c.p. Ti) and Ti6Al4V alloys are the most widely used metallic biomaterials in the biomedical sector. However, their high rigidity and the controversial toxicity of their alloying elements often compromise their clinical success. The use of porous β-Titanium alloys is proposed as a solution to these issues. In this regard, it is necessary to implement economic, repetitive, and non-destructive measurement techniques that allow for the semi-quantitative evaluation of the chemical nature of the implant, its microstructural characteristics, and/or surface changes. This study proposes the use of simple measurement protocols based on electrical impedance measurements, correlating them with the porosity inherent to processing conditions (pressure and temperature), as well as the chemical composition of the implant. Results revealed a clear direct relationship between porosity and electrical impedance. The percentage and/or size of the porosity decrease with an increase in compaction pressure and temperature. Moreover, there is a notable influence of the frequency used in the measurements obtained. Additionally, the sensitivity of this measurement technique has enabled the evaluation of differences in chemical composition and the detection of intermetallics in the implants. For the first time in the literature, this research establishes relationships between stiffness and electrical impedance, using approximations and models for the observed trends. All the results obtained corroborate the appropriateness of the technique to achieve the real-time characterization of Titanium implants, in an efficient and non-invasive way., (© 2024 The Author(s). Journal of Biomedical Materials Research Part A published by Wiley Periodicals LLC.)

Stress shielding and osseointegration are two main challenges in bone regeneration, which have been targeted successfully by chemical and physical surface modification methods. Direct irradiation synthesis (DIS) is an energetic ion irradiation method that generates self-organized nanopatterns conformal to the surface of materials with complex geometries (e.g., pores on a material surface). This work exposes porous titanium samples to energetic argon ions generating nanopatterning between and inside pores. The unique porous architected titanium (Ti) structure is achieved by mixing Ti powder with given amounts of spacer NaCl particles (vol % equal to 30%, 40%, 50%, 60%, and 70%), compacted and sintered, and combined with DIS to generate a porous Ti with bone-like mechanical properties and hierarchical topography to enhance Ti osseointegration. The porosity percentages range between 25% and 30% using 30 vol % NaCl space-holder (SH) volume percentages to porosity rates of 63%-68% with SH volume of 70 vol % NaCl. Stable and reproducible nanopatterning on the flat surface between pores, inside pits, and along the internal pore walls are achieved, for the first time on any porous biomaterial. Nanoscale features were observed in the form of nanowalls and nanopeaks of lengths between 100 and 500 nm, thicknesses of 35-nm and heights between 100 and 200 nm on average. Bulk mechanical properties that mimic bone-like structures were observed along with increased wettability (by reducing contact values). Nano features were cell biocompatible and enhanced in vitro pre-osteoblast differentiation and mineralization. Higher alkaline phosphatase levels and increased calcium deposits were observed on irradiated 50 vol % NaCl samples at 7 and 14 days. After 24 h, nanopatterned porous samples decreased the number of attached macrophages and the formation of foreign body giant cells, confirming nanoscale tunability of M1-M2 immuno-activation with enhanced osseointegration., (© 2023 The Authors. Journal of Biomedical Materials Research Part A published by Wiley Periodicals LLC.)

This research work proposes a synergistic approach to improve implants' performance through the use of porous Ti substrates to reduce the mismatch between Young's modulus of Ti (around 110 GPa) and the cortical bone (20-25 GPa), and the application of a biodegradable, acrylic acid-based polymeric coating to reduce bacterial adhesion and proliferation, and to enhance osseointegration. First, porous commercially pure Ti substrates with different porosities and pore size distributions were fabricated by using space-holder techniques to obtain substrates with improved tribomechanical behavior. On the other hand, a new diacrylate cross-linker containing a reduction-sensitive disulfide bond was synthesized to prepare biodegradable poly(acrylic acid)-based hydrogels with 1, 2, and 4% cross-linker. Finally, after the required characterization, both strategies were implemented, and the combination of 4% cross-linked poly(acrylic acid)-based hydrogel infiltrated in 30 vol % porosity, 100-200 μm average pore size, was revealed as an outstanding choice for enhancing implant performance.

In this research work, the fabrication of biphasic composite implants has been investigated. Porous, commercially available pure Ti (50 vol % porosity and pore distributions of 100-200, 250-355, and 355-500 μm) has been used as a cortical bone replacement, while different composites based on a polymer blend (gelatin and alginate) and bioactive glass (BG) 45S5 have been applied as a soft layer for cartilage tissues. The microstructure, degradation rates, biofunctionality, and wear behavior of the different composites were analyzed to find the best possible coating. Experiments demonstrated the best micromechanical balance for the substrate containing 200-355 μm size range distribution. In addition, although the coating prepared from alginate presented a lower mass loss, the composite containing 50% alginate and 50% gelatin showed a higher elastic recovery, which entails that this type of coating could replicate the functions of the soft tissue in areas of the joints. Therefore, results revealed that the combinations of porous commercially pure Ti and composites prepared from alginate/gelatin/45S5 BG are candidates for the fabrication of biphasic implants not only for the treatment of osteochondral defects but also potentially for any other diseases affecting simultaneously hard and soft tissues.

Porous titanium is a metallic biomaterial with good properties for the clinical repair of cortical bone tissue, although the presence of pores can compromise its mechanical behavior and clinical use. It is therefore necessary to characterize the implant pore size and distribution in a suitable way. In this work, we explore the new use of electrical impedance spectroscopy for the characterization and monitoring of titanium bone implants. Electrical impedance spectroscopy has been used as a non-invasive route to characterize the volumetric porosity percentage (30%, 40%, 50% and 60%) and the range of pore size (100-200 and 355-500 mm) of porous titanium samples obtained with the space-holder technique. Impedance spectroscopy is proved to be an appropriate technique to characterize the level of porosity of the titanium samples and pore size, in an affordable and non-invasive way. The technique could also be used in smart implants to detect changes in the service life of the material, such as the appearance of fractures, the adhesion of osteoblasts and bacteria, or the formation of bone tissue.

The porous substrates of commercially pure titanium have been coated with a novel bilayer of bioactive glasses (BGs), 45S5 and 1393, to improve the osseointegration and solve the stress-shielding phenomenon of titanium partial implants. The porosity of the substrates and the scratch resistance and bioactivity of the coating have been evaluated. Results are discussed in terms of stiffness and yield strength of the substrates, as well as the chemical composition, thickness, and design of the bioglass coating (monolithic vs bilayer). The role of the pores was a crucial issue in the anchoring of the coating, both in porosity percentage (30 and 60 vol %) and in pore range size (100-200 and 355-500 μm). The study was focused on the adhesion and infiltration of a 1393 bioglass layer (in contact with a porous titanium substrate), in combination with the biofunctionality of the 45S5 bioglass layer (surrounded by the host bone tissue), as 1393 bioglass enhances the adherence, while 45S5 bioglass promotes higher bioactivity. This bioactivity of the raw powder was initially estimated by nuclear magnetic resonance, through the evaluation of the chemical environments, and confirmed by the formation of hydroxyapatite when immersed in a simulated body fluid. The results revealed that the substrate with 30 vol % of porosity and a range of 355-500 μm pore size, coated with this novel BG bilayer, presented the best combination in terms of mechanical and biofunctional properties.

Despite the well-known advantages of the titanium-based implant systems, they still lack an optimal balance between biofunctionality and mechanical strength, especially regarding the modulation of cellular response and a desired implant osseointegration. In this work, we fabricated a nanocomposite based on porous commercially pure grade 4 titanium (c.p. Ti) reinforced with carbon nanotubes (CNT) at 5% and 10% w/w, with the aim of obtaining a nanocomposite with lower stiffness compared to traditional titanium-based implants and with the mechanical strength and bioactivity owed by the CNT. Results obtained by scanning electron microscopy, X-ray photoelectron spectroscopy, and atomic force microscopy characterization showed that the CNT dispersed and incorporated into the porous c.p. Ti matrix. Interestingly, CNT were associated with a higher twining within neighbor Ti grains, which was indeed consistent with an increased in nano-hardness. Biological evaluation by MTT and Comet assay revealed that the nanocomposites did not induce genotoxicity and cytotoxicity on two different cells lines despite the presence of nickel at the surface. Accordingly, a purification step would be required before these CNT can be used for biomedical applications. Our results indicate that incorporation of CNT into porous c.p. Ti is a promising avenue to achieve an adequate balance between biofunctionality and mechanical strength in Ti-based scaffolds for tissue replacement. © 2018 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 107A: 719-731, 2019., (© 2018 Wiley Periodicals, Inc.)

One of the most important concerns in long-term prostheses is bone resorption as a result of the stress shielding due to stiffness mismatch between bone and implant. The aim of this study was to obtain porous titanium with stiffness values similar to that exhibited by cortical bone. Porous samples of commercial pure titanium grade-4 were obtained by following both loose-sintering processing and space-holder technique with NaCl between 40 and 70% in volume fraction. Both mechanical properties and porosity morphology were assessed. Young's modulus was measured using uniaxial compression testing, as well as ultrasound methodology. Complete characterization and mechanical testing results allowed us to determine some important findings: (i) optimal parameters for both processing routes; (ii) better mechanical response was obtained by using space-holder technique; (iii) pore geometry of loose sintering samples becomes more regular with increasing sintering temperature; in the case of the space-holder technique that trend was observed for decreasing volume fraction; (iv) most reliable Young's modulus measurements were achieved by ultrasound technique., (Copyright © 2013 Elsevier B.V. All rights reserved.)

Macroporous titanium structures are of interest in bone reconstruction because of their reduced modulus of elasticity (compared to bulk titanium), possibility of being colonized by cells, and biocompatibility. However, they are not bioactive and are not able to actively facilitate bone ingrowth or reduce bacterial adhesion. In the present research, work porous titanium scaffolds with different features (porosity 30–60 vol% and pore size 100–200 or 355–500 μm) are obtained by the space holder technique. Samples are characterized using optical microscopy, computed tomography, scanning electron microscopy (SEM), and X‐ray diffraction. Moreover, the theoretical elastic modulus and yield strength are calculated. A patented chemical treatment, able to produce a bioactive nanotextured oxide layer, has been optimized and successfully applied, for the first time, to structures with 50 vol% porosity and 100–200 μm pore size (as the most promising for bone substitution due to the biomechanical and biofunctional balance). Bare and modified samples are characterized using field emission SEM, zeta potential measurements, and in vitro bioactivity tests (soaking in simulated body solution) to evaluate the effectiveness of the surface chemical treatment. [ABSTRACT FROM AUTHOR]

In this work, the fatigue and cellular performance of novel superficially treated porous titanium dental implants made up using conventional powder metallurgy and space-holder techniques (30 vol.% and 50 vol.%, both with a spacer size range of 100–200 µm) are evaluated. Before the sintering stage, a specific stage of CNC milling of the screw thread of the implant is used. After the consolidation processing, different surface modifications are performed: chemical etching and bioactive coatings (BG 45S5 and BG 1393). The results are discussed in terms of the effect of the porosity, as well as the surface roughness, chemical composition, and adherence of the coatings on the fatigue resistance and the osteoblast cells' behavior for the proposed implants. Macro-pores are preferential sites of the nucleation of cracks and bone cell adhesion, and they increase the cellular activity of the implants, but decrease the fatigue life. In conclusion, SH 30 vol.% dental implant chemical etching presents the best bio-functional (in vitro osseointegration) and bio-mechanical (stiffness, yield strength and fatigue life) balance, which could ensure the required characteristics of cortical bone tissue. [ABSTRACT FROM AUTHOR]

Despite the increasing progress achieved in the last 20 years in both the fabrication of porous dental implants and the development of new biopolymers for targeting drug therapy, there are important issues such as bone resorption, poor osseointegration, and bacterial infections that remain as critical challenges to avoid clinical failure problems. In this work, we present a novel microtechnology based on polycaprolactone microspheres that can adhere to porous titanium implant models obtained by the spacer holder technique to allow a custom biomechanical and biofunctional balance. For this purpose, a double emulsion solvent evaporation technique was successfully employed for the fabrication of the microparticles properly loaded with the antibacterial therapeutic agent, rose bengal. The resulting microspheres were infiltrated into porous titanium substrate and sintered at 60 °C for 1 h, obtaining a convenient prophylactic network. In fact, the sintered polymeric microparticles were demonstrated to be key to controlling the drug dissolution rate and favoring the early healing process as consequence of a better wettability of the porous titanium substrate to promote calcium phosphate nucleation. Thus, this joint technology proposes a suitable prophylactic tool to prevent both early-stage infection and late-stage osseointegration problems. [ABSTRACT FROM AUTHOR]

Bone resorption and inadequate osseointegration are considered the main problems of titanium implants. In this investigation, the texture and surface roughness of porous titanium samples obtained by the space holder technique were modified with a femtosecond Yb-doped fiber laser. Different percentages of porosity (30, 40, 50, and 60 vol.%) and particle range size (100–200 and 355–500 μm) were compared with fully-dense samples obtained by conventional powder metallurgy. After femtosecond laser treatment the formation of a rough surface with micro-columns and micro-holes occurred for all the studied substrates. The surface was covered by ripples over the micro-metric structures. This work evaluates both the influence of the macro-pores inherent to the spacer particles, as well as the micro-columns and the texture generated with the laser, on the wettability of the surface, the cell behavior (adhesion and proliferation of osteoblasts), micro-hardness (instrumented micro-indentation test, P–h curves) and scratch resistance. The titanium sample with 30 vol.% and a pore range size of 100–200 μm was the best candidate for the replacement of small damaged cortical bone tissues, based on its better biomechanical (stiffness and yield strength) and biofunctional balance (bone in-growth and in vitro osseointegration). [ABSTRACT FROM AUTHOR]

Titanium and its alloys are reference materials in biomedical applications because of their desirable properties. However, one of the most important concerns in long-term prostheses is bone resorption as a result of the stress-shielding phenomena. Development of porous titanium for implants with a low Young's modulus has accomplished increasing scientific and technological attention. The aim of this study is to evaluate the viability, industrial implementation and potential technology transfer of different powder-metallurgy techniques to obtain porous titanium with stiffness values similar to that exhibited by cortical bone. Porous samples of commercial pure titanium grade-4 were obtained by following both conventional powder metallurgy (PM) and space-holder technique. The conventional PM frontier (Loose-Sintering) was evaluated. Additionally, the technical feasibility of two different space holders (NH4HCO3 and NaCl) was investigated. The microstructural and mechanical properties were assessed. Furthermore, the mechanical properties of titanium porous structures with porosities of 40% were studied by Finite Element Method (FEM) and compared with the experimental results. Some important findings are: (i) the optimal parameters for processing routes used to obtain low Young's modulus values, retaining suitable mechanical strength; (ii) better mechanical response was obtained by using NH4HCO3 as space holder; and (iii) Ti matrix hardening when the interconnected porosity was 36–45% of total porosity. Finally, the advantages and limitations of the PM techniques employed, towards an industrial implementation, were discussed. [ABSTRACT FROM AUTHOR]

Bone resorption and further failure of titanium implants are often associated to stress-shielding phenomenon. This problem of mechanical incompatibility is even worst due to anisotropy of bone tissue to be replaced. In this work, different samples with gradient longitudinal porosity by using space-holder technique were fabricated and characterized. Main results of this work indicated that: 1) Experimental procedure for space-holder elimination was effective, feasible and reproducible, with better results for a compaction pressure of 800 MPa, and for highest salt contents; 2) 3-D images by micro-CT and images analysis of optical micrographs showed that initial designs were reasonably repeatable; this was observed in terms of both porosity and interfaces quality; and 3) Designs of 30/40/50 and 30/50/30, allowed to solve stress shielding without any important effect on mechanical strength, from the cortical bone point of view. [ABSTRACT FROM AUTHOR]

The use of porous titanium samples fabricated by space-holder powder metallurgy with bioactive coatings has already been reported to prevent resorption of the bone surrounding the implant and improve osseointegration, respectively. However, the presence of pores as well as the poor adherence and the brittle behavior inherent to glassy coatings affect the service behavior of implants fabricated from these samples. Therefore, they need to be optimized. In this work, 50 vol.% of porosity titanium substrates were manufactured with different pore range size (100–200 and 355–500 µm) spacer particles and coated with a bilayer of bioactive glasses (45S5/1393). The effect of the pores on the tribomechanical properties and infiltration of the bioactive glass 1393 along with the bioactivity of the bioactive glass 45S5 were evaluated by instrumented micro-indentation and scratch tests and the formation of hydroxyapatite in simulated body fluid. The results obtained were very promising as potential implants for the replacement of small tumors in cortical bone tissues, mainly due to the smaller pores that present an improved biomechanical and biofunctional balance. [ABSTRACT FROM AUTHOR]

The chemical composition and surface topography of titanium implants are essential to improve implant osseointegration. The present work studies a non-invasive alternative of electrical impedance spectroscopy for the characterization of the macroporosity inherent to the manufacturing process and the effect of the surface treatment with femtosecond laser of titanium discs. Osteoblasts cell culture growths on the titanium surfaces of the laser-treated discs were also studied with this method. The measurements obtained showed that the femtosecond laser treatment of the samples and cell culture produced a significant increase (around 50%) in the absolute value of the electrical impedance module, which could be characterized in a wide range of frequencies (being more relevant at 500 MHz). Results have revealed the potential of this measurement technique, in terms of advantages, in comparison to tiresome and expensive techniques, allowing semi-quantitatively relating impedance measurements to porosity content, as well as detecting the effect of surface modification, generated by laser treatment and cell culture. [ABSTRACT FROM AUTHOR]

Commercially pure (c.p.) titanium grade IV with a bimodal microstructure is a promising material for biomedical implants. The influence of the processing parameters on the physical, microstructural, and mechanical properties was investigated. The bimodal microstructure was achieved from the blends of powder particles with different sizes, while the porous structure was obtained using the space-holder technique (50 vol.% of ammonium bicarbonate). Mechanically milled powders (10 and 20 h) were mixed in 50 wt.% or 75 wt.% with c.p. titanium. Four different mixtures of powders were precompacted via uniaxial cold pressing at 400 MPa. Then, the specimens were sintered at 750 °C via hot pressing in an argon gas atmosphere. The presence of a bimodal microstructure, comprised of small-grain regions separated by coarse-grain ones, was confirmed by optical and scanning electron microscopies. The samples with a bimodal microstructure exhibited an increase in the porosity compared with the commercially available pure Ti. In addition, the hardness was increased while the Young's modulus was decreased in the specimens with 75 wt.% of the milled powders (20 h). [ABSTRACT FROM AUTHOR]

Porous titanium implants can be a good solution to solve the stress shielding phenomenon. However, the presence of pores compromises mechanical and corrosion resistance. In this work, porous titanium samples obtained using a space-holder technique are coated with Chitosan, Chitosan/AgNPs and Chitosan/Hydroxyapatite using only one step and an economic electrodeposition method. The coatings' topography, homogeneity and chemical composition were analyzed. A study of the effect of the porosity and type of coating on corrosion resistance and cellular behavior was carried out. The electrochemical studies reveal that porous samples show high current densities and an unstable oxide film; therefore, there is a need for surface treatments to improve corrosion resistance. The Chitosan coatings provide a significant improvement in the corrosion resistance, but the Chitosan/AgNPs and Chitosan/HA coatings showed the highest protection efficiency, especially for the more porous samples. Furthermore, these coatings have better adherence than the chitosan coatings, and the higher surface roughness obtained favors cell adhesion and proliferation. Finally, a combination of coating and porous substrate material with the best biomechanical balance and biofunctional behavior is proposed as a potential candidate for the replacement of small, damaged bone tissues. [ABSTRACT FROM AUTHOR]

The use of titanium implants with adequate porosity (content, size and morphology) could solve the stress shielding limitations that occur in conventional titanium implants. Experiments to assess the cellular response (adhesion, proliferation and differentiation of osteoblasts) on implants are expensive, time-consuming and delicate. In this work, we propose the use of impedance spectroscopy to evaluate the growth of osteoblasts on porous titanium implants. Osteoblasts cells were cultured on fully-dense and 40 vol.% porous discs with two ranges of pore size (100–200 μm and 355–500 μm) to study cell viability, proliferation, differentiation (Alkaline phosphatase activity) and cell morphology. The porous substrates 40 vol.% (100–200 µm) showed improved osseointegration response as achieved more than 80% of cell viability and higher levels of Cell Differentiation by Alkaline Phosphatase (ALP) at 21 days. This cell behavior was further evaluated observing an increase in the impedance modulus for all study conditions when cells were attached. However, impedance levels were higher on fully-dense due to its surface properties (flat surface) than porous substrates (flat and pore walls). Surface parameters play an important role on the global measured impedance. Impedance is useful for characterizing cell cultures in different sample types. [ABSTRACT FROM AUTHOR]

The failure of titanium implants is associated with two main problems that include the bone resorption and fracture of the surrounding bone tissue (stiffness incompatibility) and implant loosening (poor osseointegration). The development of porous titanium implants with low Young modulus solve the stress shielding phenomenon, while the modification of the implant surface must be implemented to promote a fast bond between the implant and bone. In this work, femtosecond laser micromachining was applied to modify the topography of the surface of Ti porous samples obtained by a space-holder technique to obtain hierarchical structures (micro and nano roughness patterns) to enhance osseointegration. Scanning electron microscopy, confocal laser microscopy, and image analysis were used for characterization of the surface morphology, roughness, and porosity before and after performing the laser treatment. Based on these results, the effect of the treatment on the mechanical behavior of the samples was estimated. In addition, a preliminary in-vitro test was performed to verify the adhesion of osteoblasts (filopodia presence) on modified titanium surface. Results revealed that laser texturing generated clusters of micro-holes and micro-columns both on the flat surface of the samples and inside the macro-pores, and periodic nanometric structures across the entire surface. The porous substrate offers suitable biomechanics (stiffness and yield strength) and bio-functional behavior (bone ingrowth and osseointegration), which improves the clinic success of titanium implants. [ABSTRACT FROM AUTHOR]

A great variety of powder metallurgy techniques can produce biomimetic porous titanium structures with similar mechanical properties to host bone tissue. In this work, loose sintering and space holder techniques, two frequently used metallurgical techniques, are compared to evaluate the influences of porosity (content, size, morphology and wall roughness), mechanical properties (stiffness and yield strength) and in-vitro cellular responses (adhesion and proliferation of myoblasts and osteoblasts). These comparisons are made to achieve the best balance between biomechanical and bifunctional behavior of a partial porous implant for cortical bone replacement. Cell adhesion (filopodia presence) and spreading were promoted on both porous surfaces and fully dense substrates (non-porous control surfaces). Porous scaffold samples designed using 50 vol.% NaCl space holder technique had an improved bioactive response over those obtained with the loose sintering technique due to higher roughness and scaffold pore diameter. However, the presence of large and heterogeneous pores compromises the mechanical reliability of the implant. Considering both scenarios, the substrates obtained with 40 vol.% NH4HCO3 and pore size ranges between 100 and 200 μm provide a balanced optimization of size and strength to promote in-vitro osseointegration. [ABSTRACT FROM AUTHOR]

The discrepancy between the stiffness of commercially pure titanium and cortical bone tissue compromises its success as a biomaterial. The use of porous titanium has been widely studied, however, it is still challenging to obtain materials able to replicate the porous structure of the bones (content, size, morphology and distribution). In this work, the freeze-casting technique is used to manufacture cylinders with elongated porosity, using a home-made and economical device. The relationship between the processing parameters (diameter and material of the mold, temperature gradient), microstructural features and mechanical properties is established and discussed, in terms of ensuring biomechanical and biofunctional balance. The cylinders have a gradient porosity suitable for use in dentistry, presenting higher Young's modulus at the bottom, near the cold spot and, therefore better mechanical resistance (it would be in contact with a prosthetic crown), while the opposite side, the hot spot, has bigger, elongated pores and walls. [ABSTRACT FROM AUTHOR]

For the design of smart titanium implants, it is essential to balance the surface properties without any detrimental effect on the bulk properties of the material. Therefore, in this study, an irradiation-driven surface modification called directed irradiation synthesis (DIS) has been developed to nanopattern porous and "as-received" c.p. Ti surfaces with the aim of improving cellular viability. Nanofeatures were developed using singly-charged argon ions at 0.5 and 1.0 keV energies, incident angles from 0° to 75° degrees, and fluences up to 5.0 × 1017 cm−2. Irradiated surfaces were evaluated by scanning electron microscopy, atomic force microscopy and contact angle, observing an increased hydrophilicity (a contact angle reduction of 73.4% and 49.3%) and a higher roughness on both surfaces except for higher incident angles, which showed the smoothest surface. In-vitro studies demonstrated the biocompatibility of directed irradiation synthesis (DIS) reaching 84% and 87% cell viability levels at 1 and 7 days respectively, and a lower percentage of damaged DNA in tail compared to the control c.p. Ti. All these results confirm the potential of the DIS technique to modify complex surfaces at the nanoscale level promoting their biological performance. [ABSTRACT FROM AUTHOR]

In the present work, the use of porous titanium is proposed as a solution to the difference in stiffness between the implant and bone tissue, avoiding the bone resorption. Conventional powder metallurgical technique is an industrially established route for fabrication of this type of material. The results are discussed in terms of the influence of compaction pressure and sintering temperature on the porosity (volumetric fraction, size, and morphology) and the quality of the sintering necks. A very good agreement between the predicted values obtained using a simple 2D finite element model, the experimental uniaxial compression behavior, and the analytical model proposed by Nielsen, has been found for both the Young's modulus and the yield strength. The porous samples obtained by the loose sintering technique and using temperatures between 1000 °C −1100 °C (about 40% of total porosity) are recommended for achieving a suitable biomechanical behavior for cortical bone partial replacement. [ABSTRACT FROM AUTHOR]

Two main problems limit the success of titanium implants: bacterial infection, which restricts their osseointegration capacity; and the stiffness mismatch between the implant and the host cortical bone, which promotes bone resorption and risk of fracture. Porosity incorporation may reduce this difference in stiffness but compromise biomechanical behavior. In this work, the relationship between the microstructure (content, size, and shape of pores) and the antibacterial and cellular behavior of samples fabricated by the space-holder technique (50 vol % NH4HCO3 and three ranges of particle sizes) is established. Results are discussed in terms of the best biomechanical properties and biofunctional activity balance (cell biocompatibility and antibacterial behavior). All substrates achieved suitable cell biocompatibility of premioblast and osteoblast in adhesion and proliferation processes. It is worth to highlighting that samples fabricated with the 100–200 μm space-holder present better mechanical behavior—in terms of stiffness, microhardness, and yield strength—which make them a very suitable material to replace cortical bone tissues. Those results exposed the relationship between the surface properties and the race of bacteria and mammalian cells for the surface with the aim to promote cellular growth over bacteria. [ABSTRACT FROM AUTHOR]

Here, titanium porous substrates were fabricated by a space holder technique. The relationship between microstructural characteristics (pore equivalent diameter, mean free-path between pores, roughness and contact surface), mechanical properties (Young's modulus, yield strength and dynamic micro-hardness) and bacterial behavior are discussed. The bacterial strains evaluated are often found on dental implants: Methicillin-resistant Staphylococcus aureus (MRSA) and Pseudomonas aeruginosa. The colony-forming units increased with the size of the spacer for both types of studied strains. An antibiofouling synthetic coating based on a sulfonated polyetheretherketone polymer revealed an effective chemical surface modification for inhibiting MRSA adhesion and growth. These findings collectively suggest that porous titanium implants designed with a pore size of 100–200 µm can be considered most suitable, assuring the best biomechanical and bifunctional anti-bacterial properties. [ABSTRACT FROM AUTHOR]

Titanium implant failures are mainly related to stress shielding phenomenon and the poor cell interaction with host bone tissue. The development of bioactive and biomimetic Ti scaffolds for bone regeneration remains a challenge which needs the design of Ti implants with enhanced osseointegration. In this context, 4 types of titanium samples were fabricated using conventional powder metallurgy, fully dense, dense etched, porous Ti, and porous etched Ti. Porous samples were manufactured by space holder technique, using ammonium bicarbonate particles as spacer in three different ranges of particle size (100–200 μm, 250–355 μm and 355–500 μm). Substrates were chemically etched by immersion in fluorhydric acid at different times (125 and 625 s) and subsequently, were characterized from a micro-structural, topographical and mechanical point of view. Etched surfaces showed an additional roughness preferentially located inside pores. In vitro tests showed that all substrates were biocompatible (80% of cell viability), confirming cell adhesion of premioblastic cells. Similarly, osteoblast showed similar cell proliferation rates at 4 days, however, higher cell metabolic activity was observed in fully dense and dense etched surfaces at 7 days. In contrast, a significant increase of alkaline phosphatase enzyme expression was observed in porous and porous etched samples compared to control surfaces (dense and dense etched), noticing the suitable surface modification parameters (porosity and roughness) to improve cell differentiation. Furthermore, the presence of pores and rough surfaces of porous Ti substrates remarkably decreased macrophage activation reducing the M1 phenotype polarization as well M1 cell marker expression. Thus, a successful surface modification of porous Ti scaffolds has been performed towards a reduction on stress shielding phenomenon and enhancement of bone osseointegration, achieving a biomechanical and biofunctional equilibrium. Unlabelled Image • Porous Ti were developed with controlled pore size morphology and distribution by powder metallurgy and space particles. • Etching surface modification produced an increase kinetic roughness of Porous Ti with higher affinity for pores walls. • Porous and etched surfaces were cell biocompatible, promoting osteoblast adhesion and cell differentiation. • Etching modification showed a biomimetic treatment reducing the M1 macrophages phenotype. [ABSTRACT FROM AUTHOR]

Abstract In this work, bacterial behavior on dense and porous titanium substrates is discussed. Porous titanium was fabricated by a space holder technique (using 50 vol%, NH 4 HCO 3 with particle sizes between 250 and 355 μm). These substrates were coated by sulfonated PEEK (termed SPEEK). Characterization of the porous substrate was carried out using the Archimedes Method, Image Analysis, and three-dimensional X-ray Micro-Computed Tomography (including total and interconnected porosity, equivalent diameter, and pore shape factor), as well as mechanical characterization (specifically stiffness and yield strength). A detailed study was performed here to investigate the influence of substrate porosity on the adhesion and proliferation of E. coli , MRSA , and P. aeruginosa (common causes of orthopedic device-associated infections). Bacterial colonization was examined in terms of the initial bacterial concentration, as well as bacterial adherence to and growth on the surface and inside the pores. Results suggest that fully dense titanium supported the least bacterial colonization, while the porous titanium promoted bacterial growth in the medium and inside the cavities. Furthermore, the SPEEK coating deposited onto the samples inhibited bacteria growth inside the porous materials. In this manner, this study showed for the first time that SPEEK could have potential antibacterial properties to offset the increase in bacteria growth commonly observed in porous materials. Graphical abstract Unlabelled Image Highlights • Porous Ti substrates with enhanced biomechanical and biofunctional equilibrium • Simple, reliable and economical protocols to study bacterial behavior • Effect of pores' roughness and superficial area on the bacteria proliferation • Novel sulfonated PEEK polymer coating inhibits bacteria adhesion. [ABSTRACT FROM AUTHOR]

Commercial pure titanium is known as good substitute for cortical bone tissue. Nevertheless, stress-shielding and the lack of osseointegration are still some limitations to solve. In this study, porous titanium substrates were manufactured by space-holder technique (50 vol% of NH 4 HCO 3 with particle size between 250 and 355 μm). The obtained stiffness and yield strength of specimens were compatible with cortical bone tissue. The substrates were coated with three layers of Bioglass® 45S5 (BG) by dripping sedimentation, a new and economic technique. The porosity and surface characterization were performed by Archimedes' method, image analysis, X-ray micro computed tomography and confocal laser microscopy, while the mechanical behavior was analyzed by ultrasound technique, uniaxial compression and micro-mechanical testing. Homogeneity, infiltration efficiency and coating integrity were evaluated. The adhesion of the coating was better on porous titanium substrates than on full dense ones. Finally, the bioactivity of the BG coating was determined via immersion in Simulated Body Fluid. The formation and growth of hydroxyapatite on the substrate were studied by scanning electron microscopy and X-ray diffraction analysis. The results showed hydroxyapatite formation in both coated full dense and porous samples. These features indicate the improvement of osseointegration for this sort of load bearing Ti implants. [ABSTRACT FROM AUTHOR]

Although titanium is widely used as biomaterial, the control of the interface properties between its surface and the surrounding physiological environment (like bone, other tissues or biofluids) results crucial to achieve a successful osseointegration and good biomechanical and functional performance. In this work, commercially pure titanium (Grade IV) discs obtained by conventional powder metallurgy were coated with 1–3 µm of Ti6Al4V (Grade V) alloy using DC-pulsed or high-power impulse magnetron sputtering (HiPIMS) technique with the aim of improving their biomedical performance. SEM, confocal microscopy, X-ray diffraction, nanoindentation and wetting measurements are used to evaluate the bio-interface role of the titanium-coated implants. Conformal Ti6Al4V coatings with controlled nano-roughness can be deposited with enhanced mechanical (H = 5–8 GPa; E = 140–160 GPa) and hydrophobic properties thanks to a dense columnar structure. The increased Ti-O bonding at the interface helps to prevent the corrosion due to the formation of a surface passivation layer. Particularly in the case of the HiPIMS process, the surface modification of titanium implants (chemistry, morphology and structure) appears as an effective strategy for satisfying the biomedical requirements and functionality, with enhanced mechanical properties and nanostructuration for prevention of bacteria colonization. [Display omitted] • The bio-interface of titanium specimens was tuned by pulsed magnetron sputtering. • Conformal adherent Ti6Al4V coatings with controlled nanoroughness values below 50 nm. • A surface TiO 2 layer ensures a good corrosion protection to biological media. • The mechanical properties were improved in the case of the novel HiPIMS technology. • Hydrophobic surfaces thanks to surface nanostructuring and chemical functionalization. [ABSTRACT FROM AUTHOR]

In this work, the surface of porous titanium samples obtained by the space-holder technique was treated with a femtosecond laser to improve their osseointegration. Instrumented micro-indentation and scratch test were implemented to evaluate the tribo-mechanical behavior of the surface of the modified samples. A detailed study of micro-hardness, stiffness, scratch resistance and elastic recovery was performed. Also, in vitro analysis was carried out to evaluate the cellular behavior. Modified samples showed less ALP activity, which could indicate a greater differentiation of the cells. The cell culture was similar in all cases although more differentiated morphology, good cell adherence and biological response were observed on treated samples. Finally, the discs with a pore size between 100–200 μm present being potential candidates for the replacement of small portions of damaged cortical bone tissues. [Display omitted] [ABSTRACT FROM AUTHOR]

Ti implants are highly biocompatible and allow orderly bone growth but, unfortunately, in the first five years after implantation, 5–10% of them fail due to poor osseointegration and to the presence of bacterial infections in prosthesis. Silver nanoparticles have been described to damage bacterial cell via prolonged release of Ag+ ions as a mode of action when immobilized on a surface. In this work, two routes to synthetize silver nanoparticles have been proposed including, on the one hand, a NaBH 4 -reduction and, on the other hand, a citrate-reduction combined with a stabilized biodegradable polymer. The deposition of these nanomaterials on porous Ti substrates previously fabricated using the space-holder technique (40 vol% and two size distributions, 100–200 and 355–500 μm) was investigated to aim for the best match. Before the deposition of nanoparticles accomplished by immersion, a silanization treatment of the substrate surface was carried out. After silver nanoparticles were deposited on the porous Ti substrates, microstructural characteristics and antibacterial behavior were evaluated against the proliferation of Staphylococcus aureus on the AgNPs functionalized substrates. Finally, the preliminary qualitative analysis showed the presence of inhibitory halos, being more relevant in the substrates with larger pores. • Synthesis of AgNPs via NaBH 4 -reduction • Synthesis of AgNP-polymer nanocomposite using citrate reduction • Deposition of AgNPs on the surface of titanium substrate after its silanization • The AgNP coating process induces potential antibacterial characteristics. • Larger pore sizes would allow a more efficient deposition of Ag-NPs. [ABSTRACT FROM AUTHOR]

• Dripping-sedimentation technique is suitable for depositing bilayer coating. • The pores of the titanium substrate favor infiltration and adhesion of the coating. • Micromechanical behavior evaluated by instrumented microindentation. • Biomechanical and biofuntional balance of substrates coated by BG 45S5 – BG 1393. Porous titanium substrates coated by dripping-sedimentation technique with a novel bilayer of (45S5 / 1393) bioactive glasses are proposed to overcome some limitations of the use of titanium for implants, such as the stress shielding and the poor osseointegration. Composition, thickness, roughness and micromechanical behavior (P-h curves) of the coating and the influence of the porous titanium substrates have been characterized. Best results were found for the substrate with 30 vol.% of porosity and a range size of 355 ‒ 500 μm, since it enhanced the mechanical and biofunctional behavior, due to the good adhesion of the 1393 bioglass to the substrate and the greater bioactivity of the 45S5 bioglass, which would be in contact with the bone. [ABSTRACT FROM AUTHOR]