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W. Richard Bowen and Nidal Hilal 4

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(a)<br />

4 µm<br />

0<br />

(b)<br />

4 µm<br />

0<br />

6.2 THE AfM AS A fORCE MEASUREMENT TOOL IN PHARMACEUTICALS 181<br />

Force (nN)<br />

(e)<br />

8<br />

7<br />

6<br />

5<br />

4<br />

3<br />

2<br />

1<br />

0<br />

�1<br />

Retracting<br />

0 20 40 60<br />

Log E (Pa)<br />

Force (nN)<br />

The value of indentation can then be related to the combined elastic<br />

modulus of the tip <strong>and</strong> the sample (K) by:<br />

L<br />

K �<br />

( � R)<br />

10<br />

9<br />

8<br />

7<br />

6<br />

5<br />

4<br />

3<br />

2<br />

1<br />

3 2<br />

0 50 100 150<br />

Relative z (nm)<br />

200 250 300<br />

1<br />

1. Si Reference<br />

2. Crystalline<br />

3. Amorphous<br />

1.0 � 10 8<br />

1.0 � 10 7<br />

1.0 � 10 6<br />

1.0 � 10 5<br />

1.0 � 10 4<br />

2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0<br />

Load (nN)<br />

Extending<br />

80 100 120 140 160 180<br />

Relative z (nm)<br />

3 1/ 2<br />

8<br />

Crystalline<br />

Amorphous<br />

FIgure 6.4 (a) AFM images of unmodified sorbitol (topographic height <strong>and</strong> phase<br />

images), insert highlights b<strong>and</strong>ing pattern; (b) AFM images within a quench-cooled<br />

domain of sorbitol, which would be expected to have a more amorphous nature;<br />

(c) nanoindentation curves for the crystalline <strong>and</strong> amorphous domains; (d) load dependence<br />

on Young’s modulus <strong>and</strong> (e) force curve from the amorphous domain. Reproduced<br />

with permission [37].<br />

(6.1)<br />

where L is the load <strong>and</strong> R is the radius of the probe. Since the combined<br />

elastic modulus contains the elastic moduli for the tip <strong>and</strong> the sample,<br />

(c)<br />

(d)

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