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

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List <strong>of</strong> Tables Table 1.1: Summary <strong>of</strong> mechanical properties <strong>of</strong> osteoporotic (OP) bone and normal bone. ........................... 9 Table 1.2: Main physical properties <strong>of</strong> different PLAs. .................................................................................. 15 Table 1.3: Main physical properties <strong>of</strong> PGA and several PLGAs. .................................................................. 17 Table 1.4: Degradation times <strong>of</strong> common polylactides. .................................................................................. 18 Table 1.5: Solubility products <strong>of</strong> TCP phases in water at 25°C. ..................................................................... 23 Table 2.1: Typical values <strong>of</strong> physical properties <strong>of</strong> gas, supercritical fluid and liquid. .................................. 43 Table 2.2: Critical conditions <strong>of</strong> several substances. ....................................................................................... 44 Table 2.3: SL-EOS characteristic parameters for CO 2 and PLGA 50:50 . ........................................................... 51 Table 2.4: <strong>Parameters</strong> used to calculate <strong>the</strong> depression <strong>of</strong> T g according to Chow’s model. ............................ 52 Table 4.1: Sieving mesh for different powder particles................................................................................... 89 Table 4.2: Dimensional data <strong>of</strong> PLGA 50:50 pellets and foams for geometric porosity. .................................. 102 Table 4.3: Example <strong>of</strong> data obtained from SCION® image analysis. ........................................................... 105 Table 4.4: Example <strong>of</strong> pore distribution data, pore morphology and final SCION ® image. ......................... 106 Table 5.1: Polylactide origin and physical state. ........................................................................................... 114 Table 5.2: Mean diameters <strong>of</strong> <strong>the</strong> polymers after knife mill grinding by granulometry. .............................. 115 Table 5.3: Viscosity values <strong>of</strong> PLGA 50:50. ...................................................................................................... 115 Table 5.4: Comparison between molecular weight <strong>of</strong> various polylactides. ................................................. 116 Table 5.5: Glass transitions parameters <strong>of</strong> <strong>the</strong> various polylactides. ............................................................. 118 Table 5.6: Mechanical Properties <strong>of</strong> <strong>the</strong> polymer used. ................................................................................ 119 Table 5.7: Desorption-diffusion coefficients and sorption <strong>of</strong> CO 2 after different saturation times at saturation pressure 125 bars and saturation temperature 36.5°C. ............................................................... 122 Table 5.8: Desorption-diffusion coefficients <strong>of</strong> CO 2 from PLGA 50:50 for plasticized and glassy states, after different saturation pressures at 36.5°C for 120 min. <strong>of</strong> saturation time. .................................. 122 Table 5.9: Sorption data for PLGA 50:50 at 36.5°C. ......................................................................................... 123 Table 5.10: Blends <strong>of</strong> PLGA 50:50 and P L,DL LA. .............................................................................................. 124 Table 5.11: Blends <strong>of</strong> PLGA 85:15 and P L,DL LA. .............................................................................................. 125 Table 5.12: Variation domain <strong>of</strong> <strong>the</strong> various factors. .................................................................................... 127 Table 5.13: 2 4 design <strong>of</strong> experiments: levels <strong>of</strong> factors and average size <strong>of</strong> pores. ....................................... 127 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. ............................................ 128 Table 5.15: Domain <strong>of</strong> definition for <strong>the</strong> Taguchi’ design. ........................................................................... 128 Table 5.16: Experiments with <strong>the</strong> Taguchi design and <strong>the</strong> average diameter <strong>of</strong> pores for PLGA 50:50 . .......... 129 Table 5.17: Average diameter <strong>of</strong> pores for all factors and <strong>the</strong>ir effects. ....................................................... 129 Table 5.18: Doehlert’ design and <strong>the</strong> results for <strong>the</strong> average diameter <strong>of</strong> pores. .......................................... 130 Table 5.19: Repetitions experiments <strong>of</strong> Doehlert’ design (P sat = 100 bars and dP/dt = 5 bar/s). ................... 131 Table 5.20: Variation in <strong>the</strong> average size <strong>of</strong> pores with different dP/dt values at P sat = 100 bars. ................ 132 Table 5.21: Complementary Doehlert’ design experiments. ......................................................................... 133 Table 5.22: Analysis <strong>of</strong> <strong>the</strong> Doehlert design: coefficients <strong>of</strong> <strong>the</strong> model. ....................................................... 133 Table 5.23: Analysis <strong>of</strong> <strong>the</strong> Doehlert design: research <strong>of</strong> <strong>the</strong> optimum <strong>of</strong> <strong>the</strong> pore dimension. .................... 134 Table 5.24: Hidebrand’ and Hansen’ parameters <strong>of</strong> <strong>the</strong> PLA and <strong>the</strong> PGA in (MPa) 1/2 . .............................. 135 Table 5.25: Pellets <strong>of</strong> variable thickness and <strong>the</strong>ir foam data. ...................................................................... 142 Table 5.26: ScCO 2 process conditions for foaming <strong>of</strong> PLGA 50:50. ................................................................. 144 - xxix -
Table 6.1: Initial Taguchi plans for scCO 2 foaming <strong>of</strong> pellets prepared by wet and dry method. ................. 148 Table 6.2: P L,D LA foams pore data <strong>of</strong> wet and dry method by initial Taguchi’ plan. .................................... 148 Table 6.3: Complementary Taguchi plans for scCO 2 foaming <strong>of</strong> pellets prepared by wet and dry method. . 151 Table 6.4: P L,D LA foams pore data <strong>of</strong> wet and dry method by complementary Taguchi plan. ..................... 151 Table 6.5: P L,DL LA foams pore data <strong>of</strong> wet and dry method by initial Taguchi’ plan. .................................. 155 Table 6.6: P L,DL LA foams pore data <strong>of</strong> wet and dry method by complementary Taguchi plan. .................... 156 Table 6.7: P L,D LA equivalent pore diameter and geometric porosity results for both methods and plans. .... 159 Table 6.8: P L,DL LA equivalent pore diameter and geometric porosity results for both methods and plans. .. 159 Table 6.9: PLGA 50:50 foams pore data <strong>of</strong> wet and dry method by initial Taguchi plan. ................................ 162 Table 6.10: PLGA 50:50 foams pore data <strong>of</strong> wet and dry method by complementary Taguchi plan. ............... 163 Table 6.11: PLGA 85:15 foams pore data <strong>of</strong> wet and dry method by initial Taguchi plan. .............................. 167 Table 6.12: PLGA 85:15 foams pore data <strong>of</strong> wet and dry method by complementary Taguchi plan. ............... 169 Table 6.13: PLGA 50:50 equivalent pore diameter and porosity results for both methods and plans. .............. 171 Table 6.14: PLGA 85:15 equivalent pore diameter and porosity results for both methods and plans ............... 172 Table 6.15: Comparison <strong>of</strong> foam porosities obtained by two different methods. .......................................... 177 Table 6.16: Compressive modulus and compressive strength <strong>of</strong> polymer foams by both methods. ............. 178 Table 6.17: Contact Angle between water and pellets constituted by HA, PLGA or HA-PLGA blends. ..... 181 Table 6.18: Angle measured by different liquids on PLGA pellet ................................................................ 182 Table 6.19: Comparison <strong>of</strong> energies by two different methods for PLGA and PLGA/HA blends ............... 183 Table 6.20: scCO 2 process conditions for PLGA/HA foams. ........................................................................ 185 Table 6.21: Pore analysis for PLGA 85:15 foams processed at P sat = 120 bars, t sat = 20 min and T sat = 35 o C. .. 186 Table 6.22: Pore analysis data for blends PLGA 85:15 /HA 10% foams. .......................................................... 186 Table 6.23: Blend PLGA 85:15 /HA 10% foams processed at P sat =120 bars, t sat =20 min. and dP/dt = 3 bar/s .. 188 Table 6.24: PLGA 85:15 /10%HA composite foams pore data process at P sat =120 bars and t sat =20 min. ......... 188 Table 7.1: Position <strong>of</strong> resulting bands in <strong>the</strong> FTIR analysis. ......................................................................... 191 Table 7.2: Position <strong>of</strong> bands in FTIR for amorphous calcium phosphate (ACP). ......................................... 192 Table 7.3: Position <strong>of</strong> bands in FTIR for o<strong>the</strong>r groups. ................................................................................. 193 Table 7.4: Position <strong>of</strong> bands in FTIR for pyrophosphate. .............................................................................. 193 Table 7.5: Thermodynamics transitions and <strong>the</strong>rmal properties <strong>of</strong> <strong>the</strong> waxes. .............................................. 195 Table 7.6: Levels selected for each parameter <strong>of</strong> <strong>the</strong> scaffold and foaming process with supercritical CO 2 at (T sat = 50°C, dP/dt = 3 bar/min and t sat = 20 min). ..................................................................... 196 Table 7.7: PLGA 85:15 and P L,D LA Foams pore data with different % <strong>of</strong> tricalcium phosphate. ..................... 197 Table 7.8: Mass ratio <strong>of</strong> polymer and different waxes and Taguchi’ plan (L 9 ) for polymer-wax blend foams. .................................................................................................................................................... 198 Table 7.9: Equivalent pore diameter <strong>of</strong> pure P L,DL LA and polymer-wax blend foams. ................................. 201 Table 7.10: Geometric porosity <strong>of</strong> pure P L,DL LA and polymer-wax blend foams. ........................................ 201 Table 7.11: Pure P L,DL LA and polymer-wax blend equivalent pore diameter and porosity results. .............. 202 Table 7.12: Equivalent pore diameter and geometric porosity <strong>of</strong> foams <strong>of</strong> composite plus wax by simple mixing processed at T sat 45°C, t sat 20 min, and dP/dt 3bar/s............................................... 204 Table 7.13: Equivalent pore diameter and geometric porosity <strong>of</strong> foams <strong>of</strong> composite plus wax by co-grinding processed at two saturation presures. ......................................................................................... 206 Table 7.14: Composition <strong>of</strong> pellets <strong>of</strong> different polymer particle size and with variable % <strong>of</strong> wax. ............ 207 Table 7.15: Pore diameter <strong>of</strong> foams with different particle size and with variable % <strong>of</strong> wax. ...................... 207 - xxx -
Page 1 and 2: Institut National Polytechnique de
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Chapter 2. Processes</stron
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Influence of the Processes Parameters on the Properties of The ...

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