Influence of the Processes Parameters on the Properties of The ...

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Chapter 5. Characterization <strong>of</strong> Scaffolds for Connective Tissue Engineering pore size, PLGA 50:50 must be used instead <strong>of</strong> PLGA 85:15 . These results are in conformation with <strong>the</strong> observations <strong>of</strong> Tai et al. [2007b]. These authors found that when greater depressurization times are applied (actually very low, approximately 1 to 2 hours), <strong>the</strong> pore size is increasing with increasing LA composition <strong>of</strong> <strong>the</strong> PLGA co-polymer. Table 5.14: Coefficients <strong>of</strong> <strong>the</strong> 2 4 model for <strong>the</strong> PLGA 85:15 and <strong>the</strong> PLGA 50:50. â 50-50 â 85-15 a 0 83.4 111.1 a 1 -55.3 3.0 a 2 -117.1 -46.5 a 3 -1.2 -31.8 a 12 4.4 12.9 a 13 -48.3 28.4 a 23 -60.2 36.4 Average Pore Diameter (m) 500 Psat = 100 PLGA bars 50:50 + PLGA 85:15 Blend T 400 sat = 36.5 °C t sat = 20 min dP/dt = 25 bar/s 300 200 100 0 0 20 40 60 80 100 PLGA50:50 Fraction (%) Figure 5.13: Average pore diameter as a function <strong>of</strong> PLGA 50:50 ratio in <strong>the</strong> PLGA 50:50 /PLGA 85:15 blends. The comparison between <strong>the</strong> first order model <strong>the</strong>ory and experimental data has been realized and <strong>the</strong> Fisher-Snedecor test has been applied. The critical value with <strong>the</strong> error probability alpha <strong>of</strong> 5% and one degree <strong>of</strong> liberty at both <strong>the</strong> numerator and <strong>the</strong> denominator variance give F c = 161.4. The average pore value is equal, in <strong>the</strong> PLGA 50:50 model to 222.4 and <strong>the</strong> PLGA 85: 15 model to 1.1. This first order model is not statistically well suited in <strong>the</strong> PLGA 50:50 model. As various process parameters are correlated, it is necessary to control <strong>the</strong>ir effects by using a multifactor design. 3.2.2 Model with a Taguchi’ Design for PLGA 50:50 Foaming Taguchi’ design is a screening plan which helps at <strong>the</strong> determination <strong>of</strong> <strong>the</strong> more influent parameters for <strong>the</strong> experimental plan. We have chosen a L 9 table and decided to continue only with <strong>the</strong> PLGA 50:50 . Thus, it has left us 4 process parameters to optimize: <strong>the</strong> pressure, <strong>the</strong> temperature, <strong>the</strong> time <strong>of</strong> saturation and <strong>the</strong> rate <strong>of</strong> depressurization. The domain <strong>of</strong> definition <strong>of</strong> this Taguchi design is presented in Table 5.15. Table 5.15: Domain <strong>of</strong> definition for <strong>the</strong> Taguchi’ design. Factors T sat (°C) P sat (bar) t sat (min) dP/dt (bar/s) Level 1 36.5 120 20 3 Level 2 45 150 45 5 Level 3 60 200 90 10 Figure 5.15 represents <strong>the</strong> variation <strong>of</strong> <strong>the</strong> effects <strong>of</strong> <strong>the</strong> four process factors on <strong>the</strong> corresponding pore diameter. The pore diameter at a given level is estimated by taking <strong>the</strong> average <strong>of</strong> <strong>the</strong> average pore - 128 -
Chapter 5. Characterization <strong>of</strong> Scaffolds for Connective Tissue Engineering diameters. Except for <strong>the</strong> experiment P9, all produced foams have porosity higher than 75%, <strong>the</strong> maximum being reached for conditions P4 and P6. (cf. Figure 5.14). On <strong>the</strong> Table 5.16, A, B and C represent <strong>the</strong> position <strong>of</strong> polymer pellet in <strong>the</strong> chamber, top, centre and bottom position respectively (cf. Figure 4.12-a, Filling <strong>the</strong> chamber with Teflon). The effects shown in Table 5.17 have global meanings in two ways. The effects <strong>of</strong> a level are calculated by taking <strong>the</strong> difference <strong>of</strong> pore diameter and <strong>the</strong> global average pore diameter <strong>of</strong> all experiments. Firstly, if <strong>the</strong> effect is negative (positive respectively), that means that this factor has a negative (positive) effect and resulting pore diameter will be smaller (bigger). Second, <strong>the</strong> value is indicative <strong>of</strong> <strong>the</strong> importance <strong>of</strong> <strong>the</strong> effect. Table 5.16: Experiments with <strong>the</strong> Taguchi design and <strong>the</strong> average diameter <strong>of</strong> pores for PLGA 50:50 . Experiment T sat P sat t sat dP/dt Average Pore Diameter Average* Nr. (°C) (bar) (min) (bar/s) A B C (μm) P1 36.5 120 20 3 549.88 535.02 268.32* 542.45 P2 36.5 150 45 5 9.66 12.54* 9.19 9.42 P3 36.5 200 90 10 4.31 3.66* 4.29 4.30 P4 45 120 45 10 18.82 152.68* 18.25 18.53 P5 45 150 90 3 19.08 11.96* 21.66 20.37 P6 45 200 20 5 9.98 13.19 7.62 10.26 P7 60 120 90 5 127.83 87.50* 101.56 114.70 P8 60 150 20 10 113.23 105.81 80.66* 109.52 P9 60 200 45 3 10.72* 14.15 13.94 14.05 * values eliminated in <strong>the</strong> calculation <strong>of</strong> <strong>the</strong> average because varying more than 10% Table 5.17: Average diameter <strong>of</strong> pores for all factors and <strong>the</strong>ir effects. Factor Variation
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