Porous Titanium for Biomedical Applications: Evaluation of the Conventional Powder Metallurgy Frontier and Space-Holder Technique

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.Ministry of Economy and Competitiveness of Spain Grant MAT2015-71284-PJunta de Andalucía Grant P12-TEP-1401Comisión Nacional de Investigación, Científica y Tecnológica (CONICYT) of the Chilean government project FONDECYT 1116086

Titanium scaffolds with multi-scale porosity obtained by controlled chemical and electrochemical treatments of porous solids from PM space holder technique

Junta de Andalucía (Spain) / FEDER (EU), through the project Ref. P12-TEP-140

Influence of the Compaction Pressure and Sintering Temperature on the Mechanical Properties of Porous Titanium for Biomedical Applications

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.Ministry of Economy and Competitiveness of the State General Administration of Spain grant MAT2015-71284-

Characterization and Monitoring of Titanium Bone Implants with Impedance Spectroscopy

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

Fatigue limit estimation for WC-Co cemented carbides on the basis of linear elastic fracture mechanics

En este trabajo se investiga el comportamiento a fractura y fatiga de dos grados de carburos cementados WC-Co con distintos contenidos de fase ligante y tamaño de carburo medio. La caracterización mecánica incluye la evaluación de la resistencia a flexión, la tenacidad de fractura, el límite de fatiga y la cinética de propagación de grietas grandes por fatiga (PGGF) para relaciones de carga diferentes. Se propone un enfoque basado en la mecánica de la fractura elástica lineal con el objetivo de evaluar la relación existente entre la vida a fatiga y la PGGF. El análisis se concentra en la correlación límite de fatiga–umbral de propagación de grietas para condiciones de vida a fatiga infinita. Así, se estima el límite de fatiga asociado con defectos naturales a partir del umbral de propagación experimentalmente determinado para grietas grandes, asumiendo que: (1) existe similitud en el comportamiento a fatiga de fisuras grandes y pequeñas, y (2) los defectos críticos bajo cargas monotónicas y cíclicas son los mismos. La fiabilidad de este enfoque para evaluar condiciones límites bajo solicitaciones cíclicas se sustenta en la concordancia satisfactoria observada para los valores del límite de fatiga estimados y los experimentalmente determinados para las distintas razones de carga investigadas.The fracture and fatigue behavior of two microstructurally different hardmetals (WC-Co cemented carbides) is investigated. Mechanical characterization includes flexural strength and fracture toughness as well as fatigue limit and fatigue crack growth (FCG) behavior under monotonic and cyclic loads respectively. Considering that fatigue lifetime of cemented carbides is given by subcritical crack growth of preexisting defects, a linear elastic fracture mechanics approach is attempted to assess fatigue life - FCG relationships for these materials. It concentrates on addressing the fatigue limit - FCG threshold correlation under infinite fatigue life conditions. Thus, the fatigue limit associated with natural flaws is estimated from FCG threshold experimentally determined for large cracks under the assumptions that (1) similitude on the FCG behavior of small and large cracks applies for cemented carbides, and (2) critical flaws are the same, in terms of nature, geometry and size, under monotonic and cyclic loading. The reliability of this fatigue mechanics approach is sustained through the satisfactory agreement observed between estimated and experimentally determined values for the fatigue limit under the different load ratios investigated.Comisión Interministerial de Ciencia y Tecnología (CICYT) proyecto No MAT2000-1014-C02-0

Fracture toughness of cemented carbides obtained by electrical resistance sintering

The unique combination of hardness, toughness and wear resistance exhibited by WC-Co cemented carbides (hardmetals) has made them a preeminent material choice for extremely demanding applications, such as metal cutting/forming tools or mining bits, in which improved and consistent performance together with high reliability are required. The high fracture toughness values exhibited by hardmetals are mainly due to ductile ligament bridging and crack deflection (intrinsic to carbides). In this work two WC-Co grades obtained by using the electric resistance sintering technique are studied. The relationships between the process parameters (cobalt volume fraction, sintering current and time, die materials, etc.), the microstructural characteristics (porosity, cobalt volume fraction, carbide grain size, binder thickness and carbide contiguity) and mechanical properties (Vickers hardness and fracture toughness) are established and discussed. Also the presence of microstructural anisotropy and residual stresses is studied. The sintering process at 7 kA, 600 ms and 100 MPa, in an alumina die, followed by a treatment of residual stress relief (800 °C, 2 h in high vacuum), allows to obtain WC-Co pellets with the best balance between an homogeneous microstructure and mechanical behaviour.EU for funding this research with in the framework of the EU 7th Framework FoF.NMP.2013-10 608729 EFFIPRO Projec

Advanced titanium scaffolds obtained by directional freeze-drying: on the influence of processing conditions

Ministry of Science and Innovation of Spain under Grant No. MAT2010-20855Junta de Andalucía (Spain) / FEDER (EU), through the project Ref. P12-TEP-140

Influence of temperature on the biaxial strength of cemented carbides with different microstructures

The effect of the temperature on the mechanical strength of WC-Co cemented carbides with different microstructures (grain size and binder content) was evaluated. Biaxial flexural tests were performed on three cemented carbide grades at 600 °C using the ball-on-three-balls (B3B) method. Results were interpreted by Weibull statistics and compared to biaxial strength results at room temperature. A detailed fractographic analysis, supported by Linear Elastic Fracture Mechanics, was performed to differentiate the nature and size of critical defects and the mechanism responsible for the fracture. A significant decrease in the mechanical strength (around 30%) was observed at 600 °C for all grades of cemented carbides. This fact was ascribed to the change in the critical flaw population from sub-surface (at room temperature) to surface defects, associated with the selective oxidation of Co. Additionally, an estimation of the fracture toughness at 600 °C was attempted for the three cemented carbides, based upon the B3B strength results, the corresponding number of the tested specimens fragments and the macroscopic area of the B3B fracture surfaces. The fracture toughness was not affected by the temperature, at least up to 600 °C. In addition, the good agreement with the Single Edge Notch Beam toughness data suggests the possibility of employing this approach for fracture toughness evaluation of brittle materials under different testing conditions.Peer ReviewedPostprin

Designing, processing and characterisation of titanium cylinders with graded porosity: An alternative to stress-shielding solutions

Bone resorption events and consequent failure of titanium implants are frequently related to stress-shielding problems, due to stiffness mismatch with respect to bone. This is a mechanical incompatibility problem, which is difficult to resolve because of the challenge of replacing highly anisotropic biomechanical systems, as is the case of dental implants. This work describes the designing, processing and characterisation of cylindrical titanium samples with a longitudinally graded porosity obtained by conventional powder-metallurgy techniques. The design concept used was biomimetic, based on the stiffness properties of the tissues to be in contact with titanium dental implants. Processing conditions were optimised in terms of different parameters: structural integrity, porosity and mechanical properties. The influence of sintering temperature was evaluated in search of optimum results under the above criteria. The behaviour of longitudinal porosity and Young’s modulus were consistent with the preliminary design concept from the original biomechanical system. Mechanical strength results were reasonably suitable for dental applications and they were favourably sensitive to increasing sintering temperature, due to a stronger adhesion between initial green layers of cylindrical samples. Results showed that it is possible to obtain a desired longitudinal gradient in Young’s modulus, as well as suitable yield strength values. The optimised processing described suggests that it is a plausible candidate for manufacturing dental implants with a good balance between reduced stress shielding and suitable mechanical strength, which encourages us to undertake further work along the same lines.Ministerio de Economía y Competitividadt MAT2010- 2085

Influence of the Test Configuration and Temperature on the Mechanical Behaviour of WC-Co

In this work, the effect of the test configuration and temperature on the mechanical behaviour of cemented carbides (WC-Co) with different carbide grain sizes (dWC) and cobalt volume fractions (VCo), implying different binder mean free paths ( Co), was studied. The mechanical strength was measured at 600º C with bar-shaped specimens subjected to uniaxial four-point bending (4PB) tests and with disc specimens subjected to biaxial ball-on-three-balls (B3B) tests. The results were analysed within the frame of theWeibull theory and compared with strength measurements performed at room temperature under the same loading conditions. A mechanical degradation greater than 30% was observed when the samples were tested at 600ºC due to oxidation phenomena, but higherWeibull moduli were obtained as a result of narrower defect size distributions. A fractographic analysis was conducted with broken specimens from each test configuration. The number of fragments (Nf) and the macroscopic fracture surface were related to the flexural strength and fracture toughness of WC-Co. For a given number of fragments, higher mechanical strength values were always obtained for WC-Co grades with higher KIc. The observed differences were discussed based on a linear elastic fracture mechanics (LEFM) model, taking into account the effect of the temperature and microstructure of the cemented carbides on the mechanical strength.Junta de Andalucía P12-TEP-262