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

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3.3 Contact Angle Measurement ............................................................................................................................... 101 4 Protocols for Porosity and Pore Size Measurement ................................................................................... 102 4.1 Average Geometric Porosity ................................................................................................................................ 102 4.2 2D Image Analysis .............................................................................................................................................. 103 4.2.1 Sputter Coater ........................................................................................................................................... 103 4.2.2 SCION Image Analysis .......................................................................................................................... 104 4.3 3D Hg Intrusion Porosity ..................................................................................................................................... 107 4.4 3D Micro Computer Tomography ....................................................................................................................... 108 4.4.1 Acquisition ................................................................................................................................................ 109 4.4.2 Corrections ................................................................................................................................................ 109 4.4.3 Reconstruction .......................................................................................................................................... 109 4.4.4 Viewing Results ........................................................................................................................................ 109 4.4.5 Wide Variety <strong>of</strong> Post Processing ............................................................................................................... 109 5 Mechanical Tests on Foams ....................................................................................................................... 110 5.1 Experimental Conditions <strong>of</strong> Test ......................................................................................................................... 110 5.2 Principle <strong>of</strong> Curve Analysis ................................................................................................................................. 110 6 Conclusion .................................................................................................................................................. 111 Chapter 5 ...................................................................................................................................................... 112 1 Characterization <strong>of</strong> Biomaterials ................................................................................................................ 113 1.1 Characterization <strong>of</strong> Polylactide Powders ............................................................................................................. 113 1.1.1 Experiments on Polylactide Powders by Viscosimetry. ............................................................................ 115 1.1.2 Discussion on <strong>the</strong> Molecular Mass ........................................................................................................... 116 1.1.3 Characterization <strong>of</strong> Polylactide Powders by DSC ..................................................................................... 116 1.1.4 Discussion on <strong>the</strong> Transitions ................................................................................................................... 118 1.1.4.1 Effect <strong>of</strong> L and DL Ratio on Thermal Property <strong>of</strong> Polylactide Acid .............................................. 118 1.1.4.2 Effect <strong>of</strong> LA/GA Ratio on T g <strong>of</strong> Polylactides ................................................................................. 119 1.2 Characterization <strong>of</strong> Biomaterials Pellets .............................................................................................................. 119 1.2.1 Mechanical Experiments ........................................................................................................................... 119 1.2.2 Discussion on Mechanical Modulus ......................................................................................................... 119 2 Kinematics and Thermodynamics Experiments ......................................................................................... 120 2.1 Sorption-Diffusion Kinetics ................................................................................................................................. 120 2.2 Desorption-Diffusion Kinetics ............................................................................................................................. 121 2.3 The Sorption Iso<strong>the</strong>rm ......................................................................................................................................... 123 3.1.2 Discussion on <strong>the</strong> Blends <strong>of</strong> P L,DL LA and PLGA 50:50 ................................................................................ 125 3.1.3 P L,DL LA and PLGA 85:15 Blend ................................................................................................................... 125 3.1.4 Discussion on <strong>the</strong> Blends <strong>of</strong> P L,DL LA and PLGA 85:15 ................................................................................ 126 3.2 <strong>Influence</strong> <strong>of</strong> <strong>the</strong> <strong>Parameters</strong> <strong>of</strong> <strong>the</strong> scCO 2 Process ............................................................................................... 126 3.2.1 Model with a 2 4 Complete Design ............................................................................................................. 126 3.2.2 Model with a Taguchi’ Design for PLGA 50:50 Foaming ............................................................................ 128 3.2.3 Model with a Doehlert’ Design for PLGA 50:50 Foaming ........................................................................... 130 3.2.3.1 Experiments with a Doehlert’ Design ............................................................................................ 130 3.2.3.2 Discussion on <strong>the</strong> Effect <strong>of</strong> <strong>the</strong> Various CO 2 Process <strong>Parameters</strong> .................................................. 132 4 Factors Affecting on Pores Size and Porosity ............................................................................................ 135 - xv -
4.1 Effect <strong>of</strong> <strong>the</strong> Polymer Composition ..................................................................................................................... 135 4.2 Effect <strong>of</strong> Depressurization Rates ......................................................................................................................... 135 4.3 Effect <strong>of</strong> Saturation Pressure (P sat ) ...................................................................................................................... 137 4.4 Effect <strong>of</strong> Saturation Temperature (T sat ) ............................................................................................................... 138 4.5 Effect <strong>of</strong> Saturation Time (t sat ) ............................................................................................................................. 139 4.6 Effect <strong>of</strong> <strong>the</strong> dP/dt and dT/dt ............................................................................................................................... 139 4.7 Effect <strong>of</strong> <strong>the</strong> Geometry <strong>of</strong> <strong>the</strong> Pressure Chamber ................................................................................................ 140 4.8 Interconnectivity and Coalescence Behaviour <strong>of</strong> <strong>the</strong> Scaffolds........................................................................... 141 4.9 <strong>Influence</strong> <strong>of</strong> Pellet Thickness on Foaming .......................................................................................................... 142 4.9.1 Porosity and Cell Density ......................................................................................................................... 142 4.9.2 Pores Size Distribution ............................................................................................................................. 143 4.9.3 Correlation Between Effects <strong>of</strong> Pellet Thickness and Process <strong>Parameters</strong> ............................................... 143 4.10 Discussion on Foam Morphology ........................................................................................................................ 144 5 Conclusion .................................................................................................................................................. 146 Chapter 6 ...................................................................................................................................................... 147 1 Optimization <strong>of</strong> PLA’s Foams Processed by Wet and Dry Methods ......................................................... 147 1.1 Experimental Procedure ...................................................................................................................................... 147 1.1.1 Preparation <strong>of</strong> Pellets by Wet and Dry Methods ....................................................................................... 147 1.1.2 Taguchi’ Design for Foaming ................................................................................................................... 148 1.2 P L,D LA Foams Processed by Wet and Dry Methods: Initial Taguchi Plan .......................................................... 148 1.2.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent Pore Diameter (d e ) .............................................................. 150 1.2.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 150 1.3 P L,D LA Foams Processed by Wet and Dry Methods: Complementary Taguchi’ Plan ......................................... 151 1.3.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent Pore Diameter (d e ) .............................................................. 153 1.3.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 153 1.4 P L,DL LA Foams Processed by Wet and Dry Methods: Initial Taguchi Plan ......................................................... 154 1.4.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent Pore Diameter (d e ) .............................................................. 155 1.4.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 156 1.5 P L,DL LA Foams Processed by Wet and Dry Methods: Complementary Taguchi’ Plan ....................................... 156 1.5.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent pore diameter (d e ) ................................................................ 158 1.5.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 158 1.6 Comparison Between Both PLAs ........................................................................................................................ 159 2 Optimization <strong>of</strong> PLGA’s Foams by Wet and Dry Method. ........................................................................ 161 2.1 PLGA 50:50 Foams Processed by Wet and Dry Methods ....................................................................................... 161 2.1.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent Pore Diameter (d e ) .............................................................. 162 2.1.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 163 2.2 PLGA 50:50 Foams by Wet and Dry Methods by Complementary Taguchi’ Plan ................................................. 163 2.2.1 Effect <strong>of</strong> Process <strong>Parameters</strong> on Equivalent Pore Diameter (d e ) .............................................................. 165 2.2.2 Effect <strong>of</strong> Process <strong>Parameters</strong> on Geometric Porosity ............................................................................... 165 - xvi -
Page 1 and 2: Institut National Polytechnique de
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