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

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Chapter 4.<br />

Experimental Procedures and Protocols for Analyses<br />

<str<strong>on</strong>g>of</str<strong>on</strong>g> pores in <str<strong>on</strong>g>the</str<strong>on</strong>g> foams are present in functi<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> nature <str<strong>on</strong>g>of</str<strong>on</strong>g> polymers (P L,D LA) under <str<strong>on</strong>g>the</str<strong>on</strong>g> same scCO 2<br />

c<strong>on</strong>diti<strong>on</strong>s T sat = 55°C, P sat = 80 bar, t sat = 30 min, dP/dt=4.5 bar/s (cf. Figure 4.26).<br />

Compairing all <str<strong>on</strong>g>the</str<strong>on</strong>g> graphs provide a clearer picture about <str<strong>on</strong>g>the</str<strong>on</strong>g> foam morphology SEM image is in<br />

2D and it is already supposed that <str<strong>on</strong>g>the</str<strong>on</strong>g> pore diameter obtained from SCION ® image analysis is <str<strong>on</strong>g>of</str<strong>on</strong>g> a circular<br />

pore, so if we c<strong>on</strong>sider pore volume <str<strong>on</strong>g>the</str<strong>on</strong>g> calculati<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> equivalent pore diameter, <str<strong>on</strong>g>the</str<strong>on</strong>g>re will be ano<str<strong>on</strong>g>the</str<strong>on</strong>g>r<br />

hypo<str<strong>on</strong>g>the</str<strong>on</strong>g>sis that <str<strong>on</strong>g>the</str<strong>on</strong>g> pores are sphere which is not possible. Hence to make <str<strong>on</strong>g>the</str<strong>on</strong>g> result more close to <str<strong>on</strong>g>the</str<strong>on</strong>g> real<br />

foam pore surface area is c<strong>on</strong>sidered for calculati<strong>on</strong>s. SCION ® image analysis also provide informati<strong>on</strong><br />

about <str<strong>on</strong>g>the</str<strong>on</strong>g> nature <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> pores ei<str<strong>on</strong>g>the</str<strong>on</strong>g>r <str<strong>on</strong>g>the</str<strong>on</strong>g>y are el<strong>on</strong>gated, regular or irregular. Figure 4.26 (A) presents <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

percentage <str<strong>on</strong>g>of</str<strong>on</strong>g> micro, meso and macro pores in a scaffold while Figure 4.26 (B) presents <str<strong>on</strong>g>the</str<strong>on</strong>g> percentage <str<strong>on</strong>g>of</str<strong>on</strong>g><br />

pore surface area. <strong>The</strong> number <str<strong>on</strong>g>of</str<strong>on</strong>g> macro pores are though in less percentage but <str<strong>on</strong>g>the</str<strong>on</strong>g> area <str<strong>on</strong>g>of</str<strong>on</strong>g> macro pores has<br />

highest value. Figure 4.26 (C) presents <str<strong>on</strong>g>the</str<strong>on</strong>g> volume <str<strong>on</strong>g>of</str<strong>on</strong>g> each poreand we can see that macro pores almost<br />

c<strong>on</strong>sist <str<strong>on</strong>g>of</str<strong>on</strong>g> 95% <str<strong>on</strong>g>of</str<strong>on</strong>g> total scaffold volume. <strong>The</strong> shape <str<strong>on</strong>g>of</str<strong>on</strong>g> pores is calculated by equati<strong>on</strong> 4.2 and for P L,D LA<br />

regular, irregular and el<strong>on</strong>gated pores are 68%, 23% and 9% as presented in Figure 4.26 (D).<br />

Micro<br />

Meso<br />

Macro<br />

Pie Graph 1<br />

Micro<br />

Meso<br />

Macro<br />

Pie Graph 1<br />

(A)-Percentage <str<strong>on</strong>g>of</str<strong>on</strong>g> pore quantitity.<br />

(B)-Percentage <str<strong>on</strong>g>of</str<strong>on</strong>g> pore surface area.<br />

Micro<br />

Meso<br />

Macro<br />

Pie Graph 1<br />

El<strong>on</strong>gated<br />

Irregular<br />

Regular<br />

Pie Graph 1<br />

(C)-Percentage <str<strong>on</strong>g>of</str<strong>on</strong>g> pore volume.<br />

(D)-Percentage <str<strong>on</strong>g>of</str<strong>on</strong>g> pore types.<br />

Figure 4.26: Pore distributi<strong>on</strong> comparis<strong>on</strong> in a foam with different aspects.<br />

4.3 3D Hg Intrusi<strong>on</strong> Porosity<br />

Porosity and pore diameter <str<strong>on</strong>g>of</str<strong>on</strong>g> randomly selected foams were determined by AutoPore IV 9500<br />

(cf. Figure 4.27) mercury porosimeter located at <str<strong>on</strong>g>the</str<strong>on</strong>g> CIRIMAT/UPS and analysis were performed by Sophie<br />

Cazalbou. Mercury intrusi<strong>on</strong> porosimeter (Pascal 140, <strong>The</strong>rmo- Quest) was used to study <str<strong>on</strong>g>the</str<strong>on</strong>g> pore structure<br />

<str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> PLGA scaffolds. For each different pore diameter scaffolds, three measurements were performed.<br />

Dimensi<strong>on</strong>s <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> porous scaffolds with mass approximately 0.1 g were first measured and placed in <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

ultramacropore dilatometer for out-gassing. <strong>The</strong> dilatometer was <str<strong>on</strong>g>the</str<strong>on</strong>g>n filled with mercury up to 1800 mm 3<br />

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