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Nondestructive testing of defects in adhesive joints

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2.7. Fabrication <strong>of</strong> curcum<strong>in</strong> elut<strong>in</strong>g polymer films and its structure<br />

Curcum<strong>in</strong> load<strong>in</strong>g <strong>in</strong> EVA grades was achieved by prepar<strong>in</strong>g solutions <strong>of</strong> polymer and<br />

curcum<strong>in</strong> and cast on glass plates. Cast films were washed with de-ionized water and air-dried. FT-IR<br />

spectra <strong>of</strong> the curcum<strong>in</strong> loaded EVA grades were recorded on a Thermo Nicolet 5700 spectrometer<br />

(Thermo Scientific, Germany).<br />

2.8. Contact angle measurement<br />

Contact angle <strong>of</strong> the films are measured at room temperature (~23 o C) us<strong>in</strong>g the sessile drop<br />

method by a video based contact angle measur<strong>in</strong>g device (Data Physics OCA 15 plus, Germany) and<br />

imag<strong>in</strong>g s<strong>of</strong>tware (SCA 20). Five <strong>in</strong>dependent measurements were performed on different region <strong>of</strong><br />

the sample surface.<br />

2.9. Curcum<strong>in</strong> release pr<strong>of</strong>ile<br />

Samples <strong>of</strong> 1 cm 2 surface area were cut from the curcum<strong>in</strong> loaded polymer films and<br />

suspended <strong>in</strong> 5ml phosphate buffered sal<strong>in</strong>e (PBS) at 37 o C and placed <strong>in</strong> a shak<strong>in</strong>g water bath (Julabo,<br />

SW22, Germany) at 60rpm. At def<strong>in</strong>ite time <strong>in</strong>tervals whole quantity <strong>of</strong> PBS was withdrawn and fresh<br />

PBS was added. Elution k<strong>in</strong>etics was monitored us<strong>in</strong>g UV spectroscopy at a wavelength <strong>of</strong> 420nm for<br />

a period <strong>of</strong> 15 days.<br />

3. Results and discussion<br />

3.1. Physico-chemical characterization <strong>of</strong> Curcum<strong>in</strong>, EVA grades and Curcum<strong>in</strong> loaded<br />

EVA<br />

Solubility <strong>of</strong> EVA grades tends to <strong>in</strong>crease with <strong>in</strong>crease <strong>in</strong> v<strong>in</strong>yl acetate content <strong>in</strong> the<br />

polymer. EVA-40 was found to be soluble <strong>in</strong> a number <strong>of</strong> organic solvents such as tetrahydr<strong>of</strong>uran,<br />

toluene, dichloromethane, cyclohexane, etc. FTIR spectra <strong>of</strong> EVA, Curcum<strong>in</strong> and Curcum<strong>in</strong>-loaded<br />

EVA matrices are shown <strong>in</strong> the Figure 1. Spectra <strong>of</strong> EVA shows characteristic absorption peaks at<br />

1735.9 cm -1 due to the stretch<strong>in</strong>g vibrations <strong>of</strong> C = O. A peak <strong>in</strong> the region 2872 and 2956 cm -1<br />

corresponds to symmetric and asymmetric stretch<strong>in</strong>g vibration <strong>of</strong> C-H bond. A peak was observed <strong>in</strong><br />

the region 1143cm-1 correspond<strong>in</strong>g to C-O-C stretch. The spectrum <strong>of</strong> Curcum<strong>in</strong> shows characteristic<br />

aromatic absorption peaks <strong>in</strong> the range 1600.1 to 1504.9 cm -1 . A broad peak <strong>in</strong> the region from 3223.6<br />

to 3508.6 cm -1 <strong>in</strong>dicates the presence <strong>of</strong> OH. A feeble peak was observed at 1624.8cm -1 correspond<strong>in</strong>g<br />

to C=O, C-O-C peak was obta<strong>in</strong>ed at 1272.7 cm -1 , benzoate trans-CH <strong>in</strong> CH=CH obta<strong>in</strong>ed at 959.2<br />

cm -1 , cis CH <strong>in</strong> aromatic at 713 cm -1 . The spectra <strong>of</strong> polymer matrix <strong>in</strong>corporated with Curcum<strong>in</strong><br />

(10wt%) does not exhibit any shift <strong>in</strong> peaks with respect to the characteristic peaks discussed above.<br />

From these results it is clear that curcum<strong>in</strong> <strong>in</strong>corporated <strong>in</strong> the EVA matrix does not undergo any<br />

reaction or complexation with the matrix.<br />

The storage modulus and tan delta <strong>of</strong> EVA grades and curcum<strong>in</strong> loaded EVA are given as a<br />

function <strong>of</strong> temperature <strong>in</strong> figure 2. It may be seen that the two grades <strong>of</strong> EVA, i.e., EVA 12 and EVA<br />

18 have higher modulus compared to EVA 28 and EVA 40. All the EVA grades show glass transition<br />

<strong>in</strong> the range -15°C to -19°C. EVA 40 shows lower modulus because it has maximum v<strong>in</strong>yl acetate<br />

content which <strong>in</strong>creases the flexibility <strong>of</strong> the polymer and hence <strong>in</strong>creased the damp<strong>in</strong>g. Incorporation<br />

<strong>of</strong> Curcum<strong>in</strong> on to EVA matrices does not alter the characteristic glass transition temperature <strong>of</strong> the<br />

matrices. However, substantial <strong>in</strong>crease <strong>in</strong> storage modulus is evident.<br />

Mechanical properties <strong>of</strong> EVA grades are given <strong>in</strong> Table 1. Depend<strong>in</strong>g upon the v<strong>in</strong>yl acetate<br />

content and source <strong>of</strong> EVA grades properties tends to vary. Effect <strong>of</strong> addition <strong>of</strong> curcum<strong>in</strong> <strong>in</strong> EVA-40<br />

3

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