• No results found

Characterization of Cu and Cu/CNT composite powder

In document PDF gyan.iitg.ernet.in (Page 70-78)

Results and Discussion


Results and Discussion

500 1000 1500 2000 2500 3000 3500

1wt.% Cu/CNT Cu-O stretch

535 1385 1625 1745 2925



Wave Number (cm-1)

Treated CNT raw CNT

1wt.% CuO/CNT

Figure 4.1 a) FTIR transmittance spectra of CNT before and after the functionalization process, CuO- 1wt.% CNT powder and Cu- 1wt.% CNT powder and b) Schematic

diagram of Cu ion attachment over the CNT functional groups attached over it a)



Cu ion Functional


Results and Discussion

4.2.2 Structural characterisation of Cu/CNT composite powder

Figure 4.2 XRD pattern of CNT, CuO, Cu, CuO/CNT, and Cu/CNT composites having Diffraction angle (2(𝞱))°

Results and Discussion The X-ray diffractograms of CuO- 1wt.% CNT powder obtained from all types of CNT are shown in Figure 4.2. The peaks observed for CuO/CNT at (111) and (111) crystallographic plane correspond to tenorite phase (CuO) and cuprite phase (Cu2O), respectively, and these patterns are in consistent with their corresponding JCPDS PDF 5- 0661 and JCPDS PDF 5-0667 data. The same peaks are also noticed in copper powder synthesised through MLM technique without adding any CNT. The XRD patterns of unreinforced Cu and Cu/CNT composite powder having 1wt.% of 10-20 nm, 20-40 nm and 40-60 nm diameter CNT are also shown in Figure 4.2. It is observed that the XRD patterns obtained for both unreinforced Cu and Cu/CNT composite powder are found to be very similar irrespective of CNT diameter at 1wt.% of its concentration. The peaks identified at (111), (002), and (022) crystallographic planes are confirmed to follow JCPDS PDF 85-1326 and FCC structure. The major peak corresponding to CNT as per JCPDS PDF 26-1076 is also not observed at 26° in all composite powder and thus, it could be inferred that a thorough encapsulation on CNT is done by copper and there are no prominent structural changes in the Cu/CNT composite powder due to the incorporation of CNT.

Strain on the Cu and Cu/CNT composite powder due to synthesis process Figure 4.3 shows the XRD pattern of copper and Cu- 1wt.% CNT composite powder having all types of CNT diameter at (111) plane. It is observed that the presence of strain in the composite powder is noted to be 2.17 × 10-3, 2.16 × 10-3 and 3.24 × 10-3 for 10-20 nm, 20-40 nm and 40-60 nm diameter CNT reinforced Cu/CNT composite powder, respectively, whereas it is noticed to be 1.98 × 10-3 for pure Cu. In case of 40-60 nm diameter CNT composites, the presence of lattice strain in the composites is found to be about 1.5 times more in comparison to that of 10-20 nm and 20-40 nm diameter CNT composites. In addition, the Cu/CNT composite powder peak is observed to be similar to that of pure copper.

Results and Discussion

35 40 45 50 55 60 65

(0 0 2)

Intensity (A. U)

Diffraction angle (2()) (1 1 1)

40-60 nm

20-40 nm

10-20 nm

Pure Cu

Figure 4.3 XRD pattern of Cu and Cu- 1wt.% CNT composite powder having 10–20 nm, 20–40 nm and 40–60 nm diameter CNT in the focussed region

4.2.3 Morphology of Cu and Cu/CNT composite powder

Figure 4.4 shows the FESEM images of synthesized pure copper and Cu- 1wt.%

CNT composite powder having different CNT diameter in order to study the distribution pattern of CNT in the matrix, and entanglement and defects of CNT. Figures 4.4a-b show the morphology of copper particles obtained immediately after the reduction process, where the copper particles are observed to be glued together due to their low temperature solid- state sintering behaviour. It is noted from Guiderdoni et al. [2011] that the solid-state sintering of copper is observed at ~ 230C and the same is also observed in our present study.

Results and Discussion

Pure Cu40-60 nm20-40 nm10-20 nm

Figure 4.4 Morphology of Cu and Cu- 1 wt.% CNT composite powder a-b) Synthesized Cu powder, c-d) 40–60 nm CNT in Cu matrix, e-f) 20–40 nm CNT in Cu matrix, and g-h)

10–20 nm CNT in Cu matrix

Figures 4.4c - d, 4.4e - f and 4.4g - h show the microstructure of Cu- 1wt.% CNT composite powder having 40-60 nm (l/d = 200), 20-40 nm (l/d = 333) and 10-20 nm (l/d =

a) b)

c) d)


e) f)

Non-straightness g)

Non-straightness h)


Results and Discussion 666) diameter CNT, respectively, where the non-straightness effect of CNT is observed to be increased with its aspect ratio (l/d). It is also observed that the CNT is distributed homogeneously and it is embedded with copper with the help of different chemical groups generated over it during the chemical treatment, which is expected to increase the rigidity of final composites. Though different kinds of defects are observed in CNT in the composite powder irrespective of its diameter, aspect ratio, chemical treatment and processing technique followed to prepare the composite powder, only bending defects are noticed significantly throughout the composite powder. As there is chemical bonding between the matrix and reinforcement, which is confirmed through FTIR studies, it is expected to improve the load bearing characteristics of the composites. It is also noted from Figure 4.4g - h that the 10-20 nm CNT composite powder has significant level of entanglement in comparison to that of 20-40 nm and 40-60 nm diameter CNT composite powder.

4.2.4 Studies on different defects of CNT in the composite powder

Figure 4.5 Different types of defects observed in 1wt.% 10–20 nm CNT- Cu composite powder

Kinks a)

Knot b)

Structural Defect c)


Cu d)

Results and Discussion Figures 4.5a-d show the TEM images of different types of defects noted from 1wt.%

10-20 nm CNT- Cu composite powder, where bending of the tubes, defects/damages on the outer and inner wall of CNT, kinks, knots, and entanglement of CNT are observed. In addition, filling of copper ions inside the CNT is also noticed. Chu et al. [2010a] reported that the above noticed defects are expected to increase the chemical affinity towards the matrix leading to enhance the bonding strength between the matrix and reinforcement. In addition, these defects may restrict the filling pattern of composite powder in the cavity during the compaction process leading to decrease the relative density of sintered composites. These defects may also act as barriers for electron and phonon conduction leading to reduce their corresponding electrical and thermal conductivity of the composites.

4.2.5 Thermal stability of Cu and Cu/CNT composite powder

Figure 4.6 shows the thermal stability of commercially available spheroidal copper powder (Sigma-Aldrich, 10 micron), synthesized Cu powder and Cu- 1wt.% CNT composite powder, which are studied to understand their individual oxidation behaviour up to 800 °C.

It is observed that the thermal stability of commercially available and synthesized copper powder is observed to follow the same trend upto 800 °C. A gradual increase in weight gain of pure Cu is noticed from 250 °C onwards irrespective of source of pure copper powder.

The oxidation behaviour of Cu and Cu/CNT is observed to be saturated at 725 °C and 550

°C, respectively. The oxidation process of Cu/CNT composite powder is found to be saturated about 175 °C lower than that of respective temperature of pure copper. Due to the presence of chemical bonding between CNT and copper and the copper coating over the CNT, the oxidation process of Cu/CNT composite powder is limited to 550 °C and its thermal stability is retained from 550 °C onwards. However, the rate of oxidation of Cu/CNT composite powder is observed to be about 45 % higher that of than the synthesized copper powder, though both are observed to be saturated after attaining about 25% of weight gain.

It is inferred that the oxidation temperature of composite powder is reduced to the range of 550 to 250 °C in comparison to the range of 725 to 250 °C in case of pure copper powder.

Thus, the product developed using composite powder might be having less oxidation products in comparison to that of pure copper sample.

Results and Discussion

100 200 300 400 500 600 700 800

100 105 110 115 120 125 130

Synthesised Cu Cu 10 micron

Relative weight of the sample (%)

Temperature (C)


Figure 4.6 Thermal stability analysis of synthesized Cu, commercially available copper, Cu- 1wt.% CNT composite powder under Argon environment

In document PDF gyan.iitg.ernet.in (Page 70-78)