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Porosity Study of Sintered Titanium Foams M.V. Oliveira 1, A.C. Moreira2, C.R. Appoloni,2, R.T. Lopes3, L.C. Pereira3, C.A.A. Cairo 4
1

Instituto Nacional de Tecnologia, INT/DPCM, Av. Venezuela 82/602, CEP 20081-312, Rio de Janeiro-RJ, Brasil, marizeva@int.gov.br 2 Universidade Estadual de Londrina, Departamento de Fsica, acamargo@uel.br, appoloni@uel.br 3 Universidade Federal do Rio de Janeiro, UFRJ/COPPE, lula@metalmat.ufrj.br, ricardo@lin.ufrj.br 4 Centro Tcnico Aeroespacial, CTA/IAE/AMR, ccairo@iae.cta.br

Keywords: Titanium foam, Porosity, Powder Metallurgy. Abstract: Titanium foams have been used for surgical implants and biomedical engineering because they exhibit inert behavior and good corrosion resistance. Substantial progress has been achieved for metallic foam fabrication techniques, however the porosity characterization methods available havent been studied sufficiently. A previous research has developed a powder metallurgy route to produce pure titanium foams attaining the porosity requisites for porous surfaced surgical implants. In this study, titanium foams porosity was evaluated employing different techniques: optical quantitative metallographic analysis with automatic image technique, gamma-ray transmission and x-ray microtomography. These techniques demonstrated to be appropriate for the analized titanium foams, though their results can not be simply compared, because they use quite different methodologies and take different measurement assumptions. Introduction Metallic foams are porous materials with specific properties like low stiffness and good acoustic, thermal, electric and mechanical properties. They are used in many fields such as construction, chemical and petroleum industries, and biomedical engineering. Their microstructure may exhibit closed or open (interconnected) porosity, with different ranges of pore size, volume fraction and morphology. Among the methods available to produce metallic foams, powder metallurgy is an advantageous process due to the low sintering temperature, specially for metals with extreme contamination susceptibility, like titanium. Another benefit is the possibility of obtaining high porosity and a good control of the porous structure, which is related with processing reproducibility [1,2]. Titanium and titanium alloys are widely used for surgical implants, due to their low density an excellent combination of mechanical properties, high chemical and corrosion resistance and excellent biocompatibility, when compared with other metallic biomaterials. Titanium foams also exhibit low stiffness witch is desirable to avoid bone resorption and the consequent loosening of implant [3,4]. Porosity characterization is considered essential for porous surfaced implants because the pore size and pore morphology influence cellular adhesion. An increase in the fraction of open porosity is required, because it improves implant to bone fixation by the growing of bone-forming tissues inside de pores [5].

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A previous research has developed a powder metallurgy processing route to produce pure titanium foams attaining the porosity requisites for porous surfaced surgical implants [6]. Although substantial progress has been achieved for metallic foams fabrication techniques, the porosity characterization methods available havent been studied sufficiently. [7]. In this study, it was evaluated the pore volume fraction, connectivity, morphology and pore size distribution of titanium foams employing different techniques. The optical quantitative metallographic analysis with automatic image technique is considered the conventional method that allows the measurement of pore size and volume fraction of pores. The gammarays transmission is a fast, accurate and non-destructive technique which permit the determination of the volume fraction of pores and the x-rays microtomography is a technique that permit the observation of the inside topology and geometry of the pores and image acquisition by sample irradiation [8,9,10]. Methodology Porous titanium cylindrical samples with density 4,5 g/cm3 were processed by a powder metallurgy route. Pure titanium powder grade 2 (Micron Metals-EUA) made by HDHhydrogenation-dehydrogenation process were used, presenting an acicular shape and a particle size range of 149-177 m. An organic additive (urea) was used for pore formation with a 250297 m particle size range. Titanium powders were mixed with the organic additive in the proportions of 10, 20 and 30%wt, designed after the foams processing as F1, F2 and F3, respectively. The powder mixture was encapsulated in flexible molds, compacted by of cold isostatic pressing at 300 MPa and treated at 200C for 2 hours in order to evaporate the organic additive. Compacted samples were sintered at 1200C in vacuum furnace (better than 10-6 Torr) for 1 hour. The sintered samples dimensions were: diameter varying from 7,44 to 7,96 mm, medium height of 5,00 mm (for optical metallography) and 10,00 mm (for gammarays transmission and x-ray microtomography). One transversal metallographic cut section along the longitudinal axis of the samples was prepared for optical microscopy, using the standard methodology. Porosity volume fraction evaluation was performed by quantitative metallographic analysis, using an Image Pro Plus version 4.0 software. In each sample, at least 20 images were taken in a random order at the same magnification along the transverse section. The gamma rays transmission technique consists in the attenuation that an incident radiation beam suffers when go across this material. The experimental setup is constituted by a micrometer automated table for the sample positioning, Am-241 radioactive source (59.53 keV, 100 mCi), 2 mm diameter Pb collimators, NaI(Tl) detector and appropriate nuclear electronics [8]. The transmission measurements were accomplished with the sample F2 (20%wt organic additive), taken 13 different positions along the longitudinal axis in a random order, with a measurement time of 240 s for position. The X-rays microtomography technique consists in the linear attenuation coefficient mapping of the sample crossed by the X-ray beam. Several projections of the material intern structure were realized, transversally of the sample longitudinal axis, originating image of the 3D volume of the whole sample and its 2D slices [9]. The images of the sample F2 were analyzed with Imago software which allows the determination of geometric parameters of the sample. The arrangement used is a system setup constituted by a microfocus X-ray tube operated at 55 kV and 0.24 mA, automated system of sample movement, image intensifier and a CCD

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camera. 508 images (slices) of the sample were obtained, with 18 m spatial resolution. 147 slices in 21 sequential images packages were selected for the image analysis. Results and Discussion The SEM topographic view of sample the F2 (fig. 1a and 1b) evidence that the porous microstructure is consists of micropores, mostly rounded and macropores. It can be observed that the macropore walls are rough due to the titanium powder nature, which is a desired feature for implant osseointegration [3]. Figures 2a and 2b show the optical micrographs of the samples F1 and F2, with 10% and 20% of additive, respectively, and figure 2c (central region) and 2d (outside region) show the micrograph of the sample F3 with 30% of additive. Pores are the dark regions in the micrographs. Sample F1 (fig. 2a) exhibit a closed porosity type with small micropores (< 30 m) and dispersed macropores (> 100 m). The porous structure of sample F2 (fig. 2b) exhibit an interconnected porosity type in most of the regions and some areas with closed pores. Sample F3 (fig. 2c and 2d) exhibit an interconnected porosity and close pores similary to sample F2. The central region of sample F3 (fig. 2c) presents a lower porosity than the outside region (fig. 2d). This kind of pore distribution was also observed occasionally in the samples F1 and F2, but it is more noticeably in sample F3. The measured volume fraction of pores (medium values) of the samples F1, F2 and F3 were respectively 48.59 5.52%, 64.29 6.00% and 70.73 6.82%. Porosity structure is quite different between the three samples, as expected, since porosity quantity and morphology depends on the powder sizes and their quantities in the mixture [1,4]. Compacting and sintering response of the different quantities of the powders in the mixture also affects the foam processing. All samples exhibited a high volume fraction of pores. In sample F1 (fig. 2a), probably the open channels already formed may be connected to other channels outside the plane of polished given a high real fraction of open porosity. The variation of the additive quantity affected significantly the volume fraction of pores. By increasing the quantity of additive from 10% to 20% (sample F1 to F2), the opening of porosity takes place with a 32.31% significant increase in the volume fraction of pores. From a 20% to 30% increase in organic additive quantity (sample F2 to F3) the pore connectivity is enlarged with a raise in volume fraction of pores in a lesser extent (10,02%).

Figure 1 SEM topographic views of sample F2 at different magnifications.

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(a)

(b)

(c)

(d)

Figure 2 Optical micrograph of metallographic sections taken from samples: F1 (a), F2 (b) F3 in the central region (c) in the outside region (d). Figure 3 shows the porosity variation measured by the gamma rays transmission technique, in relationship of the positions (P) analyzed on the sample F2. The position of smaller porosity was P-11 with = 59.1% and the greater one was P-9 with = 70.8%. The average total porosity for sample F3 was = 64.4 8.4 % (Student statistics, 95% of confidence level).

Figure 3 Porosity variation of the measured positions in sample F2.

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For the geometric characterization of the porous material by X-rays microtomography technique, the Imago software needs a pre-processing of the images. The images of sample F2 had a quadrilateral area selected which were converted in a binary mode, starting from a grays tones histogram. Figure 4 shows the selected area of slice the S-298 before (fig. 4a) and after (fig 4b) the conversion in the binary mode.

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Figure 4 Image area of the slice S-298 (a); the same image converted in the binary mode (b). The Imago software calculated the porosity of each slice (S) of the sample with the images in the binary mode. The slice that presented the smallest porosity was the S-311 one, with = 40.1% and the slice S-50 presented the biggest porosity = 67.1%. The average total porosity was = 51.7 14%. These results indicate the heterogeneity of the sample. Figure 5 shows the pore size distribution (frequency of pores x sample radius) of the sample F2 which indicates that approximately 64% of the material porous phase refers to pores with radius varying from 120 to 235 m. It also can be observed that pores with 18 m in radius (obtained spatial resolution) appear with approximately 4% of frequency, showing that measurements with smaller spatial resolution than that accomplished in these measurements would not modify substantially the data of the pore size distribution.

Figura 5 Pore size distribution of sample F2 (frequency of pores x sample radius).

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Conclusions The techniques used demonstrated the occurrence of pore distribution irregularities along the sample sections of the titanium foams. Pore volume fractions measured from the titanium foam with 20%wt of organic additive were 64.29 6.00%, 64.4 8.4 %, 51.7 14%, respectively, for the quantitative metallographic analyses, gamma-ray transmission and X-ray microtomography techniques. These results can not be simply compared as these techniques use quite different methodologies and take different measurement assumptions. Two-dimensional quantitative metallographic analysis and gamma-rays transmission techniques have been considered to be valuable techniques for determination of the titanium foam pore volume fraction, however they only allow a qualitative pore-size distribution and connectivity evaluation. The X-rays microtomography technique permitted a three-dimensional porosity assessment and the accurate measurement of the pore volume fraction and the pore-size distribution of the titanium foam. Both gamma-rays transmission and X-rays microtomography have the additional advantage of being non-destructive methodologies. Acknowledgements The authors wish to thank Prof. Wilson Roberto Dejato da Rocha (UEL) and Dr. Paulo Sergio Parreira (UEL) for the work assistance and Leonardo M. Reis (INT), Luciano A. de Lima (INT), Larcio R. Guzela (UFRJ), Jos Luiz de Oliveira (CTA) for valuable technical support. References [1] D.C. Dunand, Advanced Engineering Materials 6 (2004), p. 369-376. [2] N.G.D. Murray and D.C. Dunand, Composites Science and Technology 63 (2003), p. 2311-2316. [3] F.H. Jones, Surface Science Reports 42 (2001), p. 75. [4] C.E. Wen, M. Mabuchi, Y. Yamada, K. Shimojima, Y. Chino and T. Asahina, Scripta Materialia 45 (2001, p. 1147-1153. [5] C.A. Simmons, S.A. Meguid, R.M. Pilliar, Journal of Orthopedic Research, 19 (2002), p. 187-195. [6] M.V. Oliveira, L.M.R. Vasconcellos, Y.R. Carvalho, C.A.A. Cairo, L.C. Pereira, Proceedings of 7th World Biomaterials Congress, Sydney/Austrlia (2004). [7] H. Shen, S.M. Oppenheimer, D.C. Dunand and L.C. Brinson, Mechanical Materials, January (2005), p. 1-29. [8] C.R. Appoloni, W.E. Pottker, Applied Radiation and Isotopes 61 (2004), p. 1133-1138. [9] N. Gerward, K.B. Guilbert, Jensen and H. Levring, Radiation Phys. and Chem. 60 (2001), p. 23-24. [10] W.R.D. Rocha, Determinao de parmetros geomtricos estruturais de espumas cermicas industriais por transmisso de raios gama e microtomografia de raios X. Dissertao de Mestrado. Universidade Estadual de Londrina (2005).