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

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Figure 6.36: Micrographs <strong>of</strong> particle before grinding. .................................................................................. 179 Figure 6.37: Evolution <strong>of</strong> <strong>the</strong> particle size distribution for PLGA+HA co-grinding. .................................... 180 Figure 6.38: Micrographs <strong>of</strong> blend PLGA+ HA after different co-grinding time. ........................................ 181 Figure 6.39: Surface evolution <strong>of</strong> blend PLGA 85:15 + 10% HA pellets with co-grinding time. ..................... 182 Figure 6.40: <strong>Influence</strong> <strong>of</strong> <strong>the</strong> co-grinding and <strong>the</strong> ratio <strong>of</strong> HA on <strong>the</strong> dispersive component <strong>of</strong> <strong>the</strong> blend surface energy.PLGA/HA. ......................................................................................................... 183 Figure 6.41: <strong>Influence</strong> <strong>of</strong> co-grinding time and <strong>the</strong> ratio <strong>of</strong> HA on <strong>the</strong> components Acid-Base <strong>of</strong> surface energy. ........................................................................................................................................ 184 Figure 6.42: <strong>Influence</strong> <strong>of</strong> co-grinding time and <strong>the</strong> ratio <strong>of</strong> HA on S nd and S ............................................. 184 Figure 6.43: Micrographs <strong>of</strong> PLGA 85:15 foams at P sat = 120 bars , t sat = 20 min and T sat = 35 o C, [50×]. ........ 185 Figure 6.44: Micrographs <strong>of</strong> blends PLGA 85:15 /HA 10% foams processed at P sat = 120 bars, t sat = 20 min, T sat = 35 o C, [100×]. .......................................................................................................................... 186 Figure 6.45: Micrographs <strong>of</strong> blend PLGA/HA 10% foams processed at P sat = 120 bars, t sat = 20 min and dP/dt = 3 bar/s. ........................................................................................................................... 187 Figure 7.1: IR absorption spectrum <strong>of</strong> amorphous tricalcium phosphate (ATCP) doped with 10% Sr. ....... 192 Figure 7.2: IR absorption spectrum <strong>of</strong> amorphous calcium phosphate (ACP) doped with 10% Sr after calcination 24 h. ......................................................................................................................... 192 Figure 7.3: IR absorption spectrum <strong>of</strong> tricalcium phosphate doped with 10% Sr after 2 hours <strong>of</strong> calcination. ................................................................................................................................................... 193 Figure 7.4: Particles size <strong>of</strong> two different tricalcium phosphates analyzed by granulometry. ...................... 194 Figure 7.5: Melting and crystallisation <strong>of</strong> <strong>the</strong> wax A (TERHELL-907). ...................................................... 194 Figure 7.6: TGA curve <strong>of</strong> <strong>the</strong> wax-A (907). .................................................................................................. 195 Figure 7.7: Micrographs <strong>of</strong> PLGA 85:15 (8523) + tricalcium phosphate processed at scCO 2 conditions- T sat 50°C, t sat 20 min, dP/dt 3bar/s and varying P sat. ................................................................. 196 Figure 7.8: Micrographs <strong>of</strong> P L,D LA + tricalcium phosphate processed at scCO 2 conditions- T sat 50°C, t sat 20 min, dP/dt 3bar/s and varying P sat. .................................................................................... 197 Figure 7.9: Micrographs <strong>of</strong> P L,DL LA foams at different process conditions. ................................................. 199 Figure 7.10: Micrographs <strong>of</strong> P L,DL LA +(10%) wax-A foams at different process conditions. ...................... 199 Figure 7.11: Micrographs <strong>of</strong> P L,DL LA +(20%) wax-A foams at different process conditions. ...................... 200 Figure 7.12: Micrographs <strong>of</strong> P L,DL LA +(30%) wax-A foams at different process conditions. ...................... 200 Figure 7.13: Average effect <strong>of</strong> wax-A on <strong>the</strong> equivalent pore diameter for polymer wax blends. ............... 202 Figure 7.14: Average effect <strong>of</strong> wax-A on <strong>the</strong> geometric porosity for polymer wax blends. ......................... 202 Figure 7.15: Micrographs <strong>of</strong> foams obtained by simple mixing <strong>of</strong> polymer and wax and processed - at [T sat 45°C, P sat 120 bars, t sat 20 min, dP/dt 3bar/s]. ................................................................. 204 Figure 7.16: Micrographs <strong>of</strong> foams obtained by simple mixing <strong>of</strong> polymer and wax and processed at [T sat 45°C, P sat 100 bars t sat 20 min, dP/dt 3bar/s]. .................................................................. 204 Figure 7.17: Micrographs <strong>of</strong> foams obtained by co-grinding polylactide and fillers processed at T sat 45°C, P sat 120 bars, t sat 20 min and dP/dt 3 bar/s. ........................................................................ 205 Figure 7.18: Micrographs <strong>of</strong> foams obtained by co-grinding polylactide and fillers processed at................ 206 Figure 7.19: Micrographs <strong>of</strong> foams containing different percentages <strong>of</strong> wax A. .......................................... 208 Figure 7.20: Effect <strong>of</strong> particle size <strong>of</strong> polymer and different % <strong>of</strong> wax on foam pore diameter and porosity. ................................................................................................................................................... 209 Figure 8.1: Micrographs <strong>of</strong> pure polymer and polymer with filler foams processed at scCO 2 condition T sat = 50 o C, P sat = 100 bars, t sat = 20 min, dP/dt = 3 bar/s. ................................................................... 211 - 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Figure 8.2: Micrographs <strong>of</strong> PLGA 85:15 (RG 858 S) processed at P sat =100 bars, t sat =20 min and dP/dt =3 bar/s. .................................................................................................................................................... 213 Figure 8.3: Size distributions <strong>of</strong> <strong>the</strong> ground and sieved particles <strong>of</strong> PLGA 85:15 . ............................................ 213 Figure 8.4: Comparison <strong>of</strong> micrographs <strong>of</strong> foams with different polymer particle size range processed at scCO 2 condition T sat 48°C, t sat 20 min, dP/dt 3 bar/s, P sat 120 bars or P sat 100 bars. .... 214 Figure 8.5: Effect <strong>of</strong> particle size on equivalent pore size and geometric porosity <strong>of</strong> PLGA 85:15 foams processed at T sat 48°C, t sat 20 min and dP/dt 3bar/s ........................................................... 215 Figure 8.6: Size distribution <strong>of</strong> composite formulation at different co-grinding time. .................................. 216 Figure 8.7: Micrographs <strong>of</strong> PLGA 85:15 composites foams processed at T sat = 50 o C, P sat = 100 bars, t sat = 20 min, and dP/dt = 3 bar/s with different co-grinding times. ........................................................ 216 Figure 8.8: Micrographs <strong>of</strong> foams with different filler ratio processed at five different scCO 2 conditions. . 218 Figure 8.9: Micrographs <strong>of</strong> foams <strong>of</strong> polymer with different particle size range +5% βTCP (sr) + 5% ATCP (sr) processed at. T sat 45°C, P sat 100 bars, t sat 20 min and, dP/dt 3 bar/s. .............................. 219 Figure 8.10: Effect <strong>of</strong> particle size on Pore diameter and porosity <strong>of</strong> foams containing 90% PLGA 85:15 +5%βTCP (sr) and 5%ATCP (sr) processed at--[45 o C-100 bar-20 min-3 bar/s] ............................. 220 Figure 8.11: ScCO 2 Foaming installation with 3 perforated stailess steel plates stage. ................................ 220 Figure 8.12: Foams <strong>of</strong> polymer composite blend on 3 SS plates stage. ........................................................ 220 Figure 8.13: Micrographs <strong>of</strong> foams obtained from each plate processed at sc CO 2 process condition T sat 45°C, P sat 100 bars, t sat 20 min and dP/dt 3bar/s. ............................................................ 221 Figure 8.14: Equivalent pore size and geometric porosity <strong>of</strong> foams at different places in <strong>the</strong> chamber. ...... 221 Figure 8.15: Foams <strong>of</strong> pellets prepared in one batch. .................................................................................... 222 Figure 8.16: Pore equivalent size and geometric porosity <strong>of</strong> composite foam in <strong>the</strong> same batch. ................ 223 Figure 8.17: Percentage <strong>of</strong> pores in composite foams in <strong>the</strong> same batch. ..................................................... 223 Figure 8.18: Surface area <strong>of</strong> pores in composite foams in <strong>the</strong> same batch. ................................................... 223 Figure 8.19: 90% PLGA 85:15 +5%ATCP (sr) +5%βTCP (sr) foams randomly selected from different batches processed at - T sat 45°C, P sat 100 bar t sat 20 min and dual dP/dt 1 and 3bar/s. ............... 225 Figure 8.20: SEM micrographs <strong>of</strong> 90 % PLGA 85:15 + 5 % ATCP (sr) + 5 % βTCP (sr) foams sected from different batches and processed at: T sat 48°C, P sat 100 bars, t sat 20 min and dual dP/dt 1 and 3bar/s ................................................................................................................................... 226 Figure 8.21: Equivalent pore size and geometric porosity <strong>of</strong> 90% PLGA 85:15 + 5% ATCP (sr) + 5% βTCP (sr) foams from different batches. ..................................................................................................... 227 Figure 8.22: Pore frequency and cummulative total pore area as a function <strong>of</strong> average pore diameter for 90% PLGA 85:15 +5%ATCP (sr) +5%βTCP (sr) foams selected randomly from different runs. ................ 227 Figure 8.23: Equivalent pore diameter vs pore numbers for selected ............................................................ 228 Figure 8.24: Pore diameter and porosity <strong>of</strong> composite foams from different batches ................................... 228 Figure 8.25: Pore morphology <strong>of</strong> selected polymer composite foams. ......................................................... 229 Figure 8.26: Internal morphology <strong>of</strong> 90% PLGA 85:15 +5%ATCP (sr) +5%βTCP (sr) foams ............................... 229 Figure 8.27: Some typical stress–strain curves <strong>of</strong> PLGA 85:15 porous scaffolds with internal macropores at different porosities produced at different process conditions..................................................... 230 Figure 8.28: Compressive properties <strong>of</strong> pure PLGA 85:15 foams with different porosities. ............................ 231 Figure 8.29: Compressive properties <strong>of</strong> foams containing 90 % PLGA 85:15 + 5 % TCP (sr) + 5 % ATCP (sr) processed at T sat 48°C, P sat 100 bars, t sat 20 min, dual and dP/dt 1 bar/s and 3 bar/s. ..... 231 Figure 8.30: Compressive properties <strong>of</strong> foams containing 90 % PLGA 85:15 + 5 % TCP (sr) + 5 % ATCP (sr) obtained after co-grinding. ......................................................................................................... 232 Figure 8.31: Compressive properties <strong>of</strong> 90%PLGA 85:15 + 5%TCP (sr) +5%ATCP (sr) foams with different fillers ratios ........................................................................................................................................... 233 - xxvi -
Page 1 and 2: Institut National Polytechnique de
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Influence of the Processes Parameters on the Properties of The ...

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