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

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Chapter 2.<br />

<str<strong>on</strong>g>Processes</str<strong>on</strong>g> to Manufacture Foams and to Functi<strong>on</strong>alize <str<strong>on</strong>g>the</str<strong>on</strong>g> Surface<br />

(f)<br />

(g)<br />

And <str<strong>on</strong>g>the</str<strong>on</strong>g>n put into a freezer.<br />

<strong>The</strong> manufactured microspheres are freeze-dried under low temperature and pressure.<br />

(a) Dissolving (b) Dropping (c) Stirring (d) Centrifuging (e) Washing (f) Freezing (g) Freeze-Drying<br />

Figure 2.5: Schematic procedure <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> processing <str<strong>on</strong>g>of</str<strong>on</strong>g> PLGA microsphere scaffolds.<br />

[Ko et al., 2007]<br />

2.6 Particle-Aggregated Scaffolds Technique<br />

<strong>The</strong> particle aggregati<strong>on</strong> method described herein allows <strong>on</strong>e to obtain scaffolds with high<br />

mechanical properties (thus assuring scaffold stability) and full three-dimensi<strong>on</strong>al interc<strong>on</strong>nectivity, which is<br />

assured in a 3D perspective by <str<strong>on</strong>g>the</str<strong>on</strong>g> c<strong>on</strong>tact points between <str<strong>on</strong>g>the</str<strong>on</strong>g> particles. <strong>The</strong> described technique is based <strong>on</strong><br />

<str<strong>on</strong>g>the</str<strong>on</strong>g> random packing <str<strong>on</strong>g>of</str<strong>on</strong>g> prefabricated microspheres with fur<str<strong>on</strong>g>the</str<strong>on</strong>g>r aggregati<strong>on</strong> by physical or <str<strong>on</strong>g>the</str<strong>on</strong>g>rmal means to<br />

create a three-dimensi<strong>on</strong>al porous structure. <strong>The</strong> polymer (at desired c<strong>on</strong>centrati<strong>on</strong>) is dissolved in a good<br />

solvent. For <str<strong>on</strong>g>the</str<strong>on</strong>g> producti<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> composite particles, hydroxyapatite (HAp) is added at an adequate<br />

c<strong>on</strong>centrati<strong>on</strong> to <str<strong>on</strong>g>the</str<strong>on</strong>g> soluti<strong>on</strong> and dispersed homogeneously. <strong>The</strong> detailed procedure (cf. Figure 2.6) is <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

following:<br />

(a)<br />

(b)<br />

(c)<br />

(d)<br />

(e)<br />

<strong>The</strong> polymer or composite (polymer plus HAp) soluti<strong>on</strong> is left overnight to assure complete<br />

dissoluti<strong>on</strong> [Figure a]. <strong>The</strong> polymer/composite soluti<strong>on</strong> is filtered to eliminate any residual particles.<br />

<strong>The</strong> polymer/composite soluti<strong>on</strong> is extruded through a syringe in a dispenser (syringe pump) at a<br />

c<strong>on</strong>trolled and c<strong>on</strong>stant rate in order to shape <str<strong>on</strong>g>the</str<strong>on</strong>g> particles into a NaOH soluti<strong>on</strong> [Figure b]. <strong>The</strong><br />

particle size can be c<strong>on</strong>trolled by tailoring <str<strong>on</strong>g>the</str<strong>on</strong>g> polymer soluti<strong>on</strong> c<strong>on</strong>centrati<strong>on</strong>, needle diameter, and<br />

dispensing rate.<br />

<strong>The</strong> particles are <str<strong>on</strong>g>the</str<strong>on</strong>g>n exhaustively washed to remove all exceeding reagents, namely from <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

precipitati<strong>on</strong> bath [Figure c]. To produce composite particles, cross-linking can be used with<br />

appropriate polymer cross-linkers. <strong>The</strong> particles are immersed in <str<strong>on</strong>g>the</str<strong>on</strong>g> cross-linking soluti<strong>on</strong> for a<br />

determined short period and <str<strong>on</strong>g>the</str<strong>on</strong>g>n washed again.<br />

For producti<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> scaffolds, appropriate particles are press-fitted into a specific mould [Figure d].<br />

And left in <str<strong>on</strong>g>the</str<strong>on</strong>g> oven for a necessary time for aggregati<strong>on</strong> to take place [Figure e].<br />

(a) (b) (c) (d) (e)<br />

Figure 2.6: Schematic procedure for manufacturing <str<strong>on</strong>g>of</str<strong>on</strong>g> scaffolds with <str<strong>on</strong>g>the</str<strong>on</strong>g> particle-aggregated technique.<br />

[Malafaya and Reis, 2007]<br />

2.7 Freeze-Drying Method<br />

Porosity can be acquired in <str<strong>on</strong>g>the</str<strong>on</strong>g> first step <str<strong>on</strong>g>of</str<strong>on</strong>g> freeze-drying (lyophilising) <str<strong>on</strong>g>the</str<strong>on</strong>g> soluti<strong>on</strong> c<strong>on</strong>taining<br />

polymeric biomaterials, when <str<strong>on</strong>g>the</str<strong>on</strong>g> ice crystals <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> solvents are formed within <str<strong>on</strong>g>the</str<strong>on</strong>g> soluti<strong>on</strong>. <strong>The</strong> ice crystals<br />

serve as a porogen whose size can be easily c<strong>on</strong>trolled by adjusting <str<strong>on</strong>g>the</str<strong>on</strong>g> freezing temperature and <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

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