NITRILE RUBBER (NBR) NANOCOMPOSITES BASED ON DIFFERENT FILLER GEOMETRIES (Nanocalcium carbonate, Carbon nanotube and Nanoclay)

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1 CHAPTER 5 NITRILE RUBBER (NBR) NANOCOMPOSITES BASED ON DIFFERENT FILLER GEOMETRIES (Nanocalcium carbonate, Carbon nanotube and Nanoclay) 5.1 Introduction Nanocalcium carbonate (NCC) is a particulate nanofiller that has advantages in terms of cost and commercial availability compared to nanoclay or nano-fibres. NCC has low aspect ratio and large surface area [30]. There are reinforcing effect of nanometric calcium carbonate in thermoplastic polymers has been demonstrated in various studies [ , ]. In recent years, similar studies have been done on thermosets filled with NCC [ ]. Though the volume of literature on NCC filled thermoplastics and thermosets is relatively large, there are only few reported studies on nanometric calcium carbonate filled elastomers. It has been reported that incorporation of NCC increased the mechanical and thermal properties in natural rubber [292, 293], butadiene rubber [295], styrene butadiene rubber [199] and EPDM rubber [215]. While several researchers reported tremendous property improvement in NBR nanoclay composites [26-32], there are very few studies on nanometric CaCO 3 filled nitrile rubber (NBR) composites. As discussed earlier, NCC gave remarkable improvements in rubbers like natural rubber, SBR, EPDM and butadiene rubber. In this chapter, the effect of NCC on mechanical, thermal and transport properties of nitrile rubber were studied and the properties have been compared with those of NBR precipitated CaCO 3 vulcanizates. The morphological studies on the NBR nanocomposites were carried out using transmission electron microscopy. The mechanical properties of polymer composites are affected by particle size, particle content and particle/matrix interfacial adhesion [26]. The enhancement in properties of polymer nanocomposites is attributed to the large interfacial area between the polymer and the nanofiller. The surface area per unit volume of the nanofiller depends on its geometry. For particles and fibres, the surface area per unit volume is inversely proportional to the diameter of the particle [10]. To evaluate the effect of geometry on the properties, NBR nanocomposites were prepared using three different nanofillers, viz. 99

2 nanoclay (layered structure 1D), carbon nanotube (2D) and nanocalcium carbonate (particulate 3D). The aspect ratio of the fillers followed the order nanoclay > carbon nanotube > nanocalcium carbonate. The differences in the properties of nanocomposites were attributed to the differences in structure and aspect ratio of the fillers. 5.2 Nitrile rubber (NBR) nanocalcium carbonate (NCC) composites Cure characteristics The curing behaviour of the NBR NCC nanocomposites was analyzed at 150 C on a TechPro Rheotech oscillating disc cure meter. The cure characteristics of NBR nanocomposites are summarized in Table 5.1. Table 5.1 Cure characteristics of NBR NCC composites at 150 C Name NCC content (phr) Scorch time (min) Cure time (min) τ min (Nm) τ max (Nm) Δτ (Nm) Cure rate index (min -1 ) NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC It was observed that addition of nanocalcium carbonate decreased the scorch time (t s2 ) of the NBR NCC composites. The cure time (t 90 ) of the compounds showed a decrease on incorporation of NCC up to 5 phr and thereafter increased at higher NCC content. It may be inferred that the NCC activated the cure reaction up to 5 phr. At higher nanofiller content, the activation may be lesser due to agglomeration of the particles as evident from morphological studies. Cure rate index (CRI), a direct measure of the fast curing nature of the rubber compounds, was calculated using equation (4.1). For the NBR NCC composites, CRI increased with addition of NCC and it facilitated the activation of cure reaction up to 5 phr. On further increase in the filler content, cure time increased while CRI decreased, but was higher than unfilled NBR. At higher loading the t 90 values increased indicating deactivation of the cure process which was due to 100

3 formation of aggregates of NCC that resulted in poor interfacial interaction between rubber and NCC [291]. From the study on the effect of NCC content on rheometric torque of NBR nanocomposites, it was observed that the minimum torque (τ min ), an indirect measure of viscosity of the compound, decreased as NCC loading increased to 5 phr and thereafter showed an increase. However, no such trend was observed for the maximum torque (τ max ) of NCC filled NBR. The difference between maximum and minimum torques (Δτ), an indication of the extent of crosslinking, was found to increase for the nanocomposites up to 5 phr. [175, 275]. This may be due to the interaction between the NCC and the rubber matrix, the interaction being enhanced by the larger interfacial area between the nanofiller and the matrix. However at NCC content greater than 5 phr, Δτ decreased due to the reduction in interaction between the nanofiller and NBR which was attributed to agglomeration of NCC Morphology Figure 5.1 TEM micrographs of NBR- NCC composites (a) 0 phr (b) 2 phr (c) 5 phr and (d) 10 phr 101

4 Transmission electron microscopy was used to study the nanostructure of NBR NCC composites. The TEM micrographs of NBR nanocomposites containing 0, 2, 5 and 10 phr are shown in Figure 5.1(a), 5.1(b), 5.1(c) and 5.1(d) respectively. The NCC particles are indicated by the arrow in the figure. It was observed that NCC was finely and uniformly dispersed in composites containing 2 and 5 phr. However, as the filler content was increased to 10 phr, the NCC formed aggregates. From the TEM micrographs, it may be concluded that at higher NCC contents, strong particle-particle interaction caused the formation of agglomerates. In EPDM rubbers, the formation of agglomerates was attributed to the high surface energy of NCC [215] Mechanical properties The stress-strain characteristics of the NBR nanocomposites are shown in Figure 5.2. Figure 5.2 Stress strain characteristics of NBR NCC composites It was seen that the stress continuously increased with deformation of NBR; the stress strain behaviour was typical of synthetic elastomers. Incorporation of NCC increased the stress in the nanocomposites for the same strain level. The mechanical properties of NBR nanocomposites with different NCC contents are given in Table

5 Table 5.2 Mechanical properties of NBR NCC composites Name NCC content (phr) Pptd CaCO 3 content (phr) Tensile strength (MPa) Elongation at break (%) M100 (MPa) M300 (MPa) M 100f /M 100u NBRNCC ± ± ± ± NBRNCC ± ± ± ± NBRNCC ± ± ± ± NBRNCC ± ± ± ± NBRNCC ± ± ± ± NBRCC ± ± ± ± NBRCC ± ± ± ± NBRCC ± ± ± ± NBRCC ± ± ± ± It was observed that the tensile strength increased with the NCC content. The increase in the tensile strength was 24% and 42% for 5 and 10 phr of NCC respectively. This was equivalent to the increase in tensile strength from 10 phr and 20 phr respectively of commercial precipitated CaCO 3. To get an equivalent increase in tensile strength using commercial precipitated CaCO 3, the filler content should be two times that of NCC. The modulus at 100% elongation increased up to 7.5 phr and then decreased. It may be noted that by adding 5 phr of NCC, the modulus obtained was comparable to that obtained by adding 20 phr of precipitated CaCO 3. The reinforcing effect of the NCC was evident from the increase in the ratio of modulus of filled compounds (M 100f ) to that of unfilled NBR (M 100u ). The improvement in mechanical properties of the nanocomposites, which was greater than that produced by equivalent quantity of precipitated calcium carbonate, was due to the smaller size of the NCC, resulting in larger surface area of the filler and better interfacial bonding with the rubber matrix. This, along with good dispersion and homogeneity in bonding, improved the mechanical properties of the nanocomposites [200, 275]. In natural rubber, the reinforcing ability of the NCC was attributed to the smaller particle size, greater surface area and consequent increase in contact area between the filler and rubber particles. This inhibited the movement of polymer chains while increasing the ability to inhibit microcrack expansion [292]. But as the amount of the reinforcing filler exceeded a critical value, the contact between the rubber and filler got 103

6 saturated. Further increase in filler content caused the size of the agglomerates and the distance between rubber particles and agglomerates to increase, thus making the filler and rubber behave as different phases resulting in poorer reinforcing effect [292]. Thus, the slight reduction in mechanical properties at NCC content greater than 7.5 phr was due to the aggregation of the nanofiller. Similar improvement in tensile properties for NCC based composites of natural rubber [293], butadiene rubber [294], polybutadiene rubber [295] and NR and NR/NBR blends [296] was reported in literature Dynamic mechanical behaviour The dynamic elastic (storage) modulus E data for neat NBR and NBR-NCC composites are plotted as a function of temperature in Figure 5.3. Figure 5.3 Storage modulus (E ) as a function of temperature for NBR- NCC composites at 1 Hz Above T g, at all loadings of NCC, the nanocomposites showed clear increase in storage modulus. The effectiveness of the filler on the moduli of the composites may be represented by the coefficient C calculated using equation (4.5). The higher the value of the coefficient C the lower the effectiveness of the filler. The measured values of E at - 50 C and +50 C were used as E G and E R respectively. It was noted from the values of C, given in Table 5.3, that the effectiveness of the filler was optimum at 7.5 phr, 104

7 comparable to the effectiveness of double the concentration of precipitated CaCO 3. At this concentration, there was maximum stress transfer between the matrix and the filler. Table 5.3 Dynamic mechanical properties of NBR NCC composites Sample E tan δ max T g from tan δ T g from E max (MPa) ( C) ( C) C at 1 1 Hz 10 Hz 1 Hz 10 Hz 1 Hz 10 Hz 1 Hz 10 Hz Hz NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC NBRCC The effect of NCC content on loss factor (tan δ) as a function of temperature at a frequency of 1 Hz is shown in Figure It was observed that the effect of NCC content on the peak value of tan δ and T g values of the NBR-NCC composites was marginal. The area under the peak in tan δ vs temperature curve is a measure of energy dissipated. As observed from the figure, there was marginal narrowing of peaks and marginal reduction of damping properties. The effect of NCC content on values of tan δ max, E max and the T g values obtained for all the samples at 1Hz and 10 Hz are tabulated in Table 5.3. The maximum value of tan δ was greater than that of unfilled NBR at 2 and 7.5 phr, indicating better damping properties. But at other NCC contents it was lower than for unfilled NBR. The maximum value of loss modulus was observed to be at 7.5 phr of NCC. The dynamic mechanical properties of NBR-NCC composites at 7.5 phr may be different due to the increased NCC NBR interaction and interphase properties at this critical filler content. The storage modulus, loss modulus and damping peaks were analyzed at frequencies 1Hz and 10 Hz. The variation of E and tan δ with frequency for NBRNCC5 as a function of temperature is shown in Figure

8 Figure 5.4 Effect of NCC content on tanδ of NBR- NCC composites at 1 Hz Figure 5.5 Variation of storage modulus and tan δ with frequency for NBRNCC5 106

9 There was a slight increase in both modulus values and tan δ with frequency. For a viscoelastic material subjected to constant stress, the modulus decreases as time elapses due to molecular rearrangements that result in reduction of localized stresses. Hence modulus measurement at higher frequency (shorter time interval) will have higher values compared to those taken at lower frequency (long time period) [281]. The same trend was observed at all concentrations of NCC. The tan δ curve peak corresponding to the T g was shifted for NBR NCC composites at higher frequency. The maximum value of tan δ also increased. The tan δ curves were broadened, indicating restriction in segmental mobility at higher frequency. The effect of NCC content on values of tan δ max, E max and the T g values obtained for all the samples at frequencies 1 Hz and 10 Hz are given in Table 5.3. The Cole Cole plot of storage modulus E vs. loss modulus E was utilized to examine the homogeneity of NBR NCC composites (Figure 5.6). Homogenous polymeric systems exhibit a semicircle diagram in the Cole-Cole plot [282, 283]. Figure 5.6 Cole-Cole plot of storage modulus E vs. loss modulus E for NBR NCC composites at 1 Hz 107

10 The Cole- Cole plot of storage modulus (E ) vs. loss modulus (E ) of NBR NCC composites deviated from semicircular shape implying that the system was heterogeneous. It indicated structural changes on addition of nanoclay, the changes being more prominent above 5 phr NCC Thermal behaviour The thermal stabilities of NBR/nano-CaCO3 composites were studied by means of TGA in nitrogen atmosphere. The thermograms for the NBR nanocomposites at different NCC content are given in Figure 5.7. Figure 5.7 Thermograms of NBR- NCC composites The thermal stability factors, viz. initial decomposing temperature (IDT), temperature at the maximum rate of weight loss (T max ) and the char content at 500 C were calculated from the TGA thermograms and are listed in Table

11 Table 5.4 Thermal stability factors of NBR- NCC composites obtained from TGA Name NCC Content (phr) IDT ( C) T max ( C) Char (%) NBRNCC NBRNCC NBRNCC NBRNCC The thermal stability of the composites was enhanced on addition of NCC. In neat rubber, IDT was around 400 o C. On addition of NCC, the IDT increased by 6-11 C depending on the content of the filler. This increase in the IDT was also visible in the shoulder region of the derivative thermograms shown in Figure 5.8. Figure 5.8 Derivative thermograms for NBR- NCC composites Another notable feature from the derivative thermogram was that the maximum rate of decomposition of the nanocomposites decreased significantly on addition of NCC. This was clearly evident in the reduction in peak height of the derivative thermogram with increasing NCC content. However, NCC content had no significant effect on the 109

12 temperature at which maximum rate of decomposition occurs. Jin and Park [294] postulated that the increased area of contact of the nanometric CaCO 3 with the rubber matrix increases the absorption of heat energy during decomposition, resulting in higher IDT and lower decomposition rate for the nanocomposites. The char content of the nanocomposites at 500 C increased with NCC content Transport characteristics The effects of NCC concentration on the diffusion, sorption and permeation of toluene through NBR nanocomposites were studied. The transport behaviour through composites depends on filler type, matrix, temperature, reaction between solvent and the matrix, etc. Hence the study of the transport process through composites can be used as an effective tool to understand the interfacial interaction and morphology of the system. The swelling behavior of NBR - NCC composites was assessed by calculating swelling coefficient (β) using the equation 4.6. Table 5.5 shows that the swelling coefficient decreased with increase in NCC content. Figure 5.9 Sorption isotherms for NBR- NCC composites at 30 C 110

13 The sorption curves were plotted as Q t (moles of solvent sorbed per 100 g of rubber) against (time). Figure 5.9 shows the effect of NCC content on the toluene uptake with time. The sorption of the solvent was reduced for the nanofilled composites compared to unfilled rubber. The dispersion of NCC in the rubber matrix introduced a tortuous path for the transport of the solvent. The Q t vs. t curve showed two distinct regions - an initial steeper region with high sorption rate due to large concentration gradient and a second region exhibiting reduced sorption rate that ultimately reached equilibrium sorption. The sorption rate and equilibrium solvent uptake of NBR nanocomposites reduced with increasing NCC content. However, at 10 phr the sorption rate was reduced. Beyond 7.5 phr there was no appreciable change in equilibrium solvent uptake. This was due to the formation of agglomerates of NCC which was evident from the TEM micrographs. The crosslink density and the molecular weight of the polymer between the crosslinks (M c ) were calculated from the sorption data using equation The estimated values of M c for NBR - NCC composites are tabulated in Table 5. NCC filled systems exhibited lower M c values, i.e. lower molar mass between crosslinks than unfilled NBR and M c decreased with increasing NCC content. As the value of M c decreased the available volume between adjacent crosslinks decreased. The decrease in volume restricted the diffusion process. The slight increase in M c at 10 phr was due to the aggregation of the nanofiller as seen in the TEM micrographs. The calculated values of crosslink density supported this observation. The crosslink density of NBR NCC composites is tabulated in Table 5.5. As the nanofiller content in the composites increased, the crosslink density also increased. Table 5.5 Swelling coefficient and crosslink densities of NBR - NCC composites Sample Swelling coefficient (β) (cm 3 /g) Molar mass between crosslinks (M c ) (g/mol) Crosslink density x 10 4 (gmol/cm 3 ) NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC

14 The diffusivity (D), the sorption coefficient (S) and permeability (P) of NBR NCC composites were calculated using equations To study the effect of temperature on transport coefficients, the experiment was conducted at 30 C, 50 C and 75 C. The diffusion, sorption and permeability coefficients of NBR NCC composites at 30 C, 50 C and 75 C are given in Table 5.6. Table 5.6 Sample Transport coefficients of NBR- NCC composites Diffusion coefficient (Dx10 7 ) (m 2 /s) Sorption coefficient (S) (g/g) Permeability coefficient (P x10 7 ) (m 2 /s) 30 C 50 C 75 C 30 C 50 C 75 C 30 C 50 C 75 C NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC The diffusion of solvent through a composite depended on the geometry of the filler (size, shape, size distribution, concentration, and orientation), properties of the filler, properties of the matrix, and interaction between the matrix and the filler [287]. The diffusion and permeation coefficients of the nanofilled composites were considerably lower than the unfilled NBR. The diffusion of the penetrant solvent depended on the concentration of available space in the matrix that is large enough to accommodate the penetrant molecule [154]. The addition of NCC reduced the availability of these spaces and also restricted segmental mobility of the rubber matrix. However at 10 phr, there was an increase in diffusion and permeation coefficients. This increase was due to the aggregation of the nanofiller. Similar trends were observed for sorption studies conducted at 50 C and 75 C. As the temperature increased, the coefficient of diffusion also increased for all the samples. As temperature increased, the thermal energy increased and consequently molecular vibration of solvent molecules, the free volume in the polymer matrix and flexibility of the polymer chains increased [288]. As a result, the diffusion coefficients of the NBR composites increased with temperature. The transport coefficients at 50 C and 75 C are also tabulated in Table 5.6. Maiti et al had reported similar reduction in transport coefficients for fluoroelastomer-clay nanocomposites [287]. 112

15 The energy required for the diffusion or permeation of solvent molecules was computed using Arrhenius equations The activation energies for diffusion, sorption and permeation are listed in Table 5.7 Table 5.7 Thermodynamic parameters for transport of toluene through NBR- NCC composites Sample E D (kj/mol) E D (kj/mol) ΔH s (kj/mol) NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC The activation energy of diffusion of toluene through NBR NCC composites was found to be higher than that of unfilled NBR. The nanofillers have higher specific surface area resulting in greater rubber-filler interaction and enhanced reinforcement. As the nanofiller content increased, the activation energy needed for diffusion also increased. The activation energy for permeation (E P ), also evaluated using the Arrhenius equation, showed similar trend as E D. It is observed that the sorption is an exothermic process. The value of ΔH s increased with increasing nanofiller content. To evaluate the mechanism of sorption, the solvent uptake data of the nanocomposites were fitted to the equation 4.19 The values of n and k were determined by linear regression analysis are shown in Table 5.8. In the case of NBR-NCC the value of n at room temperature (30 C) was close to 0.5 and the diffusion was Fickian type, controlled by concentration dependent diffusion coefficient [290]. In rubbery polymers, well above their glass transition temperatures, the polymer chains adjusted quickly to the presence of penetrant molecules and hence they did not exhibit anomalous behaviour. It was observed that as the temperature increased, the values of n increased for NBR-NCC composites, implying that the diffusion tended to be of anomalous type. The constant k decreased with increasing temperature. 113

16 Table 5.8 Parameters for diffusion mechanism of toluene through NBR NCC composites 30 C 50 C 75 C SAMPLE n k (g/gmin 2 ) n k (g/gmin 2 ) n k (g/gmin 2 ) NBRNCC NBRNCC NBRNCC NBRNCC NBRNCC NBR nanocomposites with nanofillers of different geometries The nanofillers used in this study are (i) one dimensional layered silicate (nanoclay) having aspect ratio 1:100 (ii) two dimensional carbon nanotube (CNT) and (iii) three dimensional nanoparticle nanocalcium carbonate (NCC). For comparison of properties of NBR nanocomposites formed using the above nanofillers, were prepared as per the procedure described in 3.2. The nanofiller content in each case was 2 phr. The nanocomposites prepared using nanoclay, CNT and NCC were designated as NBRNCL2, NBRCNT2 and NBRNCC2 respectively. The unfilled NBR was designated as NBR Mechanical properties of NBR nanocomposites The mechanical properties of NBR nanocomposites with different fillers are tabulated in Table 5.9. Table 5.9 Mechanical properties of NBR nanocomposites Name Nanofiller content (phr) Tensile strength (MPa) Elongation at break (%) M300 (MPa) NBR ± ± ±0.06 M f /M u NBRNCL ± ± ± NBRCNT ± ± ± NBRNCC ± ± ±

17 It was observed that among the three nanofillers, the highest tensile strength and modulus were obtained for NBR nanoclay composites while the lowest was for NBR NCC composites. This can be explained using the aspect ratio and the surface area per unit volume of the filler given in Table The higher tensile strength in nanoclay composite was an indication of good intercalation/exfoliation of nitrile rubber segments into the silicate layers as evident from the TEM micrographs and XRD diffraction pattern. Table 5.10 Comparison of surface area to volume ratio of nanofillers Nanofiller Surface area / Volume Surface area / Volume* Nanoclay t = 1 nm t l l = 100 nm 2.04 Carbon nanotube r = 10 nm r l l = 10 μm Nanocalcium carbonate 3 r r = 20 nm 0.15 * calculated using material data given in

18 In NBR NCC composites, the NCC particles were individual species having lesser interaction with the nitrile rubber segments due to the lower surface area per unit volume of the filler resulting in less reinforcement [179]. The overall tensile performance of different fillers in nitrile rubber was in the order of NBR nanoclay > NBR CNT > NBR NCC > unfilled NBR. The elongation at break for nanocomposites was lower than unfilled NBR except for NBR nanoclay composites. In NBR nanoclay composites, the alkylammonium ions that are located at the clay NBR interface imparted plasticizing effect thereby increasing the elongation at break [165]. For particles and fibres, the surface area per unit volume is inversely proportional to the diameter of the particle [10]. The improvement in mechanical properties of NBRnanoclay composites over NBR CNT and NBR NCC composites can be explained on the basis of the higher surface area to volume ratio of the nanoclay. The larger surface area to volume ratio of nanoclay resulted in larger interfacial area between the nanofiller and the rubber matrix. As mentioned earlier, Cloisite 20A is an organo-modified nanoclay. The organic modifier in the nanoclay reduces the surface energy of the nanoclay and improves the wetting characteristics of the polymer. As observed by Kim et al in their studies on NBR organoclay systems [181], it improves the strength of the interface between the inorganics and the polymer. Surface treatment of nanocalcium carbonate with lipophilic substances like stearic acid or calcium stearate is used to improve dispersability and surface interaction with the polymer [67]. In this study, the nanocalcium carbonate used was of uncoated grade and hence there was no surface interactions between the NBR matrix and the nanocalcium carbonate filler. Functionalization of the CNT surface leads to increased dispersability of the CNTs in polymers and also increases the strength of the interface between the CNT and the polymer matrix [52, 108, 139, 162]. As the CNT used in the study was non-functionalized, filler surface NBR matrix interactions were not prominent in the case of NBR-CNT composites. As the structural arrangements on the molecular scale and the efficient transfer of stress across the composite components depend on the interfacial region, nanoclay composites exhibited higher reinforcement than the CNT and NCC based composites [30]. 116

19 5.3.2 Dynamic mechanical properties of NBR nanocomposites The effect of temperature on the storage modulus of NBR nanocomposites are compared in Figure Above T g nanoclay the nanocomposites showed enhancement in storage modulus indicating the strong effect of nanoclay on the dynamic properties of NBR. The enhancement in E was due to the high aspect ratio of the nanoclay and the formation of exfoliated and intercalated structures [20]. However, for CNT and NCC composites, the enhancement in storage modulus was less than that of NBR nanoclay composites. This behaviour can also be attributed to the increased interfacial surface area of the NBR nanoclay composites. Below T g, the difference in the value of E was less significant. Figure 5.10 Storage modulus (E ) vs. temperature of NBR nanocomposites at 1 Hz 117

20 Table 5.11 Dynamic mechanical properties of NBR nanocomposites evaluated at 1 Hz Sample tan δ max E max (MPa) T g ( C) from tanδ E NBR NBRNCL NBRNCNT NBRNCC Similarly, the maximum value of loss modulus (E max ) was the highest for NBR - nanoclay composites. It was observed that the nanofillers had no significant effect on the glass transition temperature. The values of tan δ max, E max and T g for NBR nanocomposites evaluated at 1 Hz is tabulated in table Transport characteristics The effects of type of nanofiller on the diffusion, sorption and permeation of toluene through NBR nanocomposites were studied. The swelling behaviour of NBR - nanoclay composites was assessed by calculating swelling coefficient, β using equation (4.6). Table 5.12 shows that the swelling coefficient was lowest for NBR nanoclay composites and highest for NBR CNT composites. The sorption curves i.e., Q t (moles of solvent sorbed per 100 g of rubber) vs. t curves at 30 C for NBR nanocomposites are shown in Figure It was observed that the sorption of toluene was reduced for the nanofilled composites compared to unfilled rubber. It was the lowest for nanoclay composites. The sorption rate and equilibrium solvent uptake also were the lowest for NBR nanoclay composites. As evident from the TEM micrographs of NBR nanoclay composites (Figure 4.3), the dispersion of nanoclay forming exfoliated and intercalated structure in the rubber matrix created tortuous path for the transport of the solvent, resulting in lower sorption. 118

21 Figure 5.11 Sorption isotherms for NBR nanocomposites at 30 C The crosslink density (υ) and molecular weight of the polymer between the crosslinks (M c ) calculated from the sorption data using equation (4.9) and (4.10) respectively are tabulated in Table Table 5.12 Swelling coefficient and crosslink densities of NBR nanocomposites Sample Swelling coefficient (β) (cm 3 /g) Molar mass between crosslinks (M c ) (g/mol) Crosslink density x 10 4 (gmol/cm 3) NBR NBRNCL NBRCNT NBRNCC

22 The transport coefficients for sorption of toluene trough NBR nanocomposites were calculated using equations and are tabulated in Table Table 5.13 Transport coefficients of NBR nanocomposites at 30 C Sample Diffusion coefficient (Dx10 7 ) (m 2 /s) Sorption coefficient (S) (g/g) Permeability coefficient (P x10 7 ) (m 2 /s) NBR NBRNCL NBRCNT NBRNCC The diffusion of solvent through a composite depends on the geometry of the filler (size, shape, size distribution, concentration, and orientation), properties of the filler, properties of the matrix, and interaction between the matrix and the filler [287]. The transport coefficients for the nanocomposites were considerably lower than those of the unfilled NBR. The diffusion of the penetrant solvent depends on the concentration of free space available in the matrix to accommodate the penetrant molecule [154]. The addition of nanoclay reduced the availability of these free spaces, restricted segmental mobility of the rubber matrix and created tortuous path for transport of solvent molecules through the nanocomposites [40-44]. However, at nanoclay content greater than 5 phr, there was an increase in diffusion and permeation coefficients. In this case also the increase in transport coefficients can be attributed to the aggregation of the nanofiller. 5.4 Conclusion NBR nanocalcium carbonate (NCC) composites were prepared from a masterbatch of NBR and NCC in an internal mixer followed by mixing on a two-roll mill. The cure time of the compounds showed a decrease on incorporation of NCC upto 5 phr and thereafter increased at higher NCC content. The dispersion of NCC in NBR matrix was analyzed from transmission electron micrographs. The tensile strength and modulus increased with NCC content. The mechanical properties of NBR - NCC nanocomposites were found to be superior to those of NBR-CaCO3 microcomposites. Investigation of dynamic mechanical properties showed that addition of NCC increased and lowered the tan δ peak 120

23 value, without altering the T g of the nanocomposite. Addition of NCC to NBR resulted in enhanced thermal stability. The sorption of toluene through the nanocomposite decreased with increasing NCC content. The values of the transport coefficients were slightly higher at 10 phr NCC content than at 7.5 phr because of aggregation of the nanofiller. Activation energy for diffusion and permeation for the nanocomposites were higher than that forunfilled NBR. Diffusion of toluene through NBR-NCC composites was found to exhibit Fickian behavior. The properties of NBR nanocomposites prepared using three different nanofillers viz. nanoclay (layered structure 1D), carbon nanotube (2D) and nanocalcium carbonate (particulate 3D) were compared in this chapter. The aspect ratio and the surface area per unit volume of the fillers were in the order nanoclay > carbon nanotube > nanocalcium carbonate. The larger surface area to volume ratio of nanoclay resulted in larger interfacial area between the nanofiller and the rubber matrix and consequently nanoclay composites exhibited higher reinforcement than the CNT and NCC based composites. The equilibrium solvent uptake and transport coefficients for the diffusion of toluene through the NBR nanocomposites were lowest for NBR nanoclay composites. 121

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