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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 />

(a)<br />

(b)<br />

(c)<br />

(d)<br />

(e)<br />

(f)<br />

(g)<br />

(h)<br />

(i)<br />

Salt particulates are prepared by sieving. <strong>The</strong> sizes <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> salt particulates are c<strong>on</strong>trolled by <str<strong>on</strong>g>the</str<strong>on</strong>g><br />

desirable sieving.<br />

Polymer soluti<strong>on</strong>s are prepared by dissolving different amounts and types <str<strong>on</strong>g>of</str<strong>on</strong>g> polymers in solvent<br />

(e.g. methylene chloride or chlor<str<strong>on</strong>g>of</str<strong>on</strong>g>orm).<br />

Sieved salt particulates are added to <str<strong>on</strong>g>the</str<strong>on</strong>g> polymer soluti<strong>on</strong>, and <str<strong>on</strong>g>the</str<strong>on</strong>g> dispersi<strong>on</strong> is gently vortexed.<br />

<strong>The</strong> soluti<strong>on</strong> is poured into <str<strong>on</strong>g>the</str<strong>on</strong>g> designed silic<strong>on</strong> mould.<br />

Subsequently, <str<strong>on</strong>g>the</str<strong>on</strong>g> mould with dispersi<strong>on</strong> is pressed (~ 6 MPa) by pressure apparatus.<br />

<strong>The</strong> formed samples are taken out <str<strong>on</strong>g>of</str<strong>on</strong>g> <str<strong>on</strong>g>the</str<strong>on</strong>g> mould.<br />

Samples are dissolved for a desirable time (48 h) in dei<strong>on</strong>ised water.<br />

Salt-removed samples are freeze-dried for a desirable time (about 48 h) at low temperature and<br />

reduced pressure (around 8 Pa,−55°C).<br />

<strong>The</strong> scaffolds are dried in a vacuum oven at 25°C for 1 week to remove <str<strong>on</strong>g>the</str<strong>on</strong>g> residual solvent.<br />

Scaffolds are kept under vacuum until use.<br />

(a) Salt<br />

(b) Preparing <str<strong>on</strong>g>of</str<strong>on</strong>g> polymer,<br />

solvent, salt<br />

(c) Mixing <str<strong>on</strong>g>of</str<strong>on</strong>g> polymer,<br />

solvent, salt<br />

(d) Moulding<br />

(e) Pressing<br />

(f) Removal from (g) Dissoluti<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> salt (h) Freezing & freeze<br />

drying<br />

(i) Removal <str<strong>on</strong>g>of</str<strong>on</strong>g> residual<br />

solvent and storage<br />

Figure 2.1: Procedure <str<strong>on</strong>g>of</str<strong>on</strong>g> solvent casting/particulate leaching.<br />

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

Porosity is independent <str<strong>on</strong>g>of</str<strong>on</strong>g> particle diameters, but increases with <str<strong>on</strong>g>the</str<strong>on</strong>g> quantity <str<strong>on</strong>g>of</str<strong>on</strong>g> salt. A minimum<br />

<str<strong>on</strong>g>of</str<strong>on</strong>g> 70% <str<strong>on</strong>g>of</str<strong>on</strong>g> salt particles is needed to create interc<strong>on</strong>nected pores [Mikos et al., 1994]. When particle diameter<br />

increases, pore size increases. Mechanical properties, such as compressive strength or modulus, are<br />

independent <str<strong>on</strong>g>of</str<strong>on</strong>g> pore size but decrease when porosity increases. Porosity up to 90-95%, with varying pore<br />

size, and a compressive modulus <str<strong>on</strong>g>of</str<strong>on</strong>g> 0.15 to 150 MPa, depending <strong>on</strong> porosity can be achieved. This method<br />

is <strong>on</strong>ly applicable to <str<strong>on</strong>g>the</str<strong>on</strong>g> preparati<strong>on</strong> <str<strong>on</strong>g>of</str<strong>on</strong>g> thin films since all <str<strong>on</strong>g>the</str<strong>on</strong>g> salt particles <strong>on</strong> <str<strong>on</strong>g>the</str<strong>on</strong>g> bulk must be leached out<br />

completely. To obtain thicker scaffolds <str<strong>on</strong>g>of</str<strong>on</strong>g> desired shape, an improved porogen salt-leaching technique has<br />

been proposed [Gross and Rodríguez-Lorenzo, 2004]. By adding small hydroxyapatite (HAp) fibres to a<br />

PLGA soluti<strong>on</strong>, it is possible to create composite foams with a c<strong>on</strong>trolled porosity [Hou et al., 2003; Chen et<br />

al., 2001b; Thoms<strong>on</strong> et al., 1998; Widmer et al., 1998].<br />

2.2 Ice Particle-Leaching<br />

Previous scaffold manufacturing usually involves (1) dissolving <str<strong>on</strong>g>the</str<strong>on</strong>g> polymer in organic solvent,<br />

(2) incorporating porogens, and (3) leaching porogens. Despite <str<strong>on</strong>g>the</str<strong>on</strong>g>se advantages, <str<strong>on</strong>g>the</str<strong>on</strong>g> problem <str<strong>on</strong>g>of</str<strong>on</strong>g> residual<br />

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