Mechanical reinforcement in nylon 6 nanocomposite fiber incorporated with dopamine reduced graphene oxide

doi:10.21203/rs.3.rs-1551072/v1

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Research Article

Mechanical reinforcement in nylon 6 nanocomposite fiber incorporated with dopamine reduced graphene oxide

https://doi.org/10.21203/rs.3.rs-1551072/v1

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posted 18 Apr, 2022

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The emergence of the graphene-based polymer composite fibers provides a new opportunity to study the high-performance and functional chemical fibers. In this work, we have developed an efficient and convenient method with polydopamine (PDA) to functionalize and reduce graphene oxide (GO) simultaneously, and the modified graphene nanosheets can obtain uniform dispersion and strong interfacial bonding in nylon 6(PA6). Furthermore, the reinforced PA6 composite fibers were prepared through mixing PDA-rGO into the PA6 polymer matrix and then melt spinning. The functional modification was characterized by surface analysis and structural testing including SEM, TEM, FTIR and Raman. When the addition amount of the modified GO was 0.15wt%, the tensile strength and Young's modulus of the composite fiber reached 310.4 MPa and 462.3MPa, respectively. The results showed a meaningful reinforcement with effect compared to the pure nylon 6 fiber. Moreover, the composite fiber also exhibited an improved crystallinity and thermal stability as measured by DSC and TGA.

graphene oxide

polydopamine

PA6

composite fiber

reinforce

Young's modulus

It is an efficient and simple route to prepare reinforced polymer nanocomposites by adding nanofillers. Extensive research work has reported that nanomaterials were used as reinforcing fillers such as SiO₂, MMT and CNTs, which obtained ideal results in the application of polymer reinforcement [1–3]. Graphene and its derivatives, as a new type of nanofillers, are two-dimensional materials composed of sp²-hybridized carbon atoms arranged in a honeycomb shape [4–5]. Its two-dimensional sheet-like wrinkled structure provides an ultra-high specific surface area, and the studies have confirmed that it became a promising new generation of nanofillers due to outstanding mechanical properties and chemical stability [6]. Compared with traditional zero and one-dimensional fillers, graphene nanosheets exhibit significant advantages among the reinforcing fillers. It has been found that graphene and its derivatives can endow the polymer good reinforcing effect at a lower loading content [7–9]. This greatly expands the application prospects of graphene in the reinforcement of polymer composites.

Graphene nanosheets are prone to agglomeration in the polymer matrix because of the existence of van der Waals force [7, 10]. Additionally, the poor interfacial characteristic between the graphene nanosheets and the polymer also leads to its restacking in the polymer matrix [11]. The main challenge is to achieve the effective dispersion and strong interface bonding of graphene nanosheet in polymer reinforced composites. In spite of that nevertheless, the surface of graphene nanosheets is smooth without reactive functional groups. As one of the representative graphene derivatives, the surface of GO owns carboxyl, epoxy and other active reaction functional groups onto the surface [4, 6]. Surface modification of GO can effectively solve the dispersibility of graphene and its derivatives in polymers and the interfacial compatibility with polymers. Various surface modified ways of GO have been used in graphene/polymer composites through covalent bonds and non-covalent bonds [12–14].

In recent years, dopamine (DA) has received much attention because it can occur self-polymerization to generate polydopamine (PDA) [15, 16]. The strong interfacial adhesion property was demonstrated between the PDA layer and the matrix, including many substrates with low surface energy such as glass, ceramics, teflon, etc, which was attributed to the presence of reactive functional groups onto its surface [17–18]. The PDA surface formed possesses highly reactive functional groups, and it can be used to enhance the compatibility of nanofillers and polymers. Thus, DA has emerged as a functional modifier of nanofillers in the field of polymer reinforced nanocomposites [19–22]. Y.L. Lu et.al incorporated PDA modified multi-walled carbon nanotubes (MWCNTs) into natural rubber (NR) via latex compounding. The modified carbon nanotubes showed excellent dispersion in the matrix, increasing the tensile strength of the composite by 42% [20]. Y. Fang et.al prepared polyimide (PI) with polydopamine functionalization boron nitride nanosheets composite fiber by in situ polymerization, and the results indicated that the tensile strength and modulus of the composite fiber were significantly improvement with the addition of modified boron nitride nanosheets (0.5wt% content) [21]. K.P. Chen et.al prepared TPU/PDA-GNP nanocomposite by in situ polymerization and discovered the strong interfacial interaction between PDA and TPU via covalent bonding, which leaded to remarkable enhancement of the mechanical properties of the nanocomposite [22].

We attempted to modify the GO by dopamine self-polymerization on its surface, and GO can be reduced to PDA-rGO at the same time. Furthermore, the reinforced PA6 composite fibers were prepared by simple melt mixing and spinning. It is a simple, efficient and low-cost method for the industrial production of polymer nanocomposite fibers. Herein, PA6 was selected as the polymer matrix of the fiber, while PA6 fiber was generally used for weaving various kinds of clothing materials and knitting, owing to excellent wear resistance and good resilience. As one of the widely used chemical fibers, it is also widely used in industrial textiles such as tire cords, fishing nets and parachutes, which require high physical and mechanical properties [23–24]. Therefore, the PDA-rGO reinforced PA6 composite fiber provides a new path for its application in the field of high-performance industrial textile materials.

Materials

PA6 slices were supplied by Yiwu Huading Nylon Co., Ltd.（China）; Graphite powder with particle size less than 20 μm was purchased from Doucheng chemical products trading Co., Ltd（China）; 98%Sulfuric acid (H₂SO₄), 37%Hydrochloric acid (HCl, L-Ascorbic acid (AR,99%), Dopamine (DA) and Tris-HCl were provided from Aladdin Reagent Co., Ltd.; Sodium hydroxide（NaOH）, 20%Hydrogen peroxide (H₂O₂) and 37%Hydrochloric acid (HCl)were purchased from Jiuding Reagent Co., Ltd.

Synthesis of Functionalized GO, rGO and PDA-rGO

Graphene oxide was prepared using a modified hummers method, as reported in our previous work [25]. The preparation of rGO was followed by previous studies. The reduction reaction of GO was performed for 24h at 80 ℃, using L-ascorbic acid as the reducing agent. The process of synthesizing PDA-rGO was shown in Fig. 1. First, 0.5g GO was added to 500ml deionized water and sonicated for half an hour to obtain a GO dispersion. Then, 0.64g Tris-HCl was added to the GO dispersion and adjust the PH of solution to 8.5. Next, 20ml (0.5mg/ml)DA was added dropwise and reacted at 50℃ for 24h. Finally, the resulting reactants were dialyzed and freeze-dried to obtain the powders of GO and PDA-rGO, respectively.

Preparation of PA6/-rGO and PA6/ PDA-rGO composite fibers

PA6 slices were dried in a vacuum oven at 100℃ for 24 hours. The preparation process of the composite fibers was depicted in Figure2. PA6 composite fiber containing 0.05wt%, 0.15 wt%, 0.3wt% PDA-rGO was prepared using the twin screw extruder (MinLab) via melt blending method as shown in Fig. 1and Fig. 2. The temperature of twin screw extrusion was 250℃，and the speed was 50rpm. The prepared primary fibers were then thermal drawn at 120 ℃ with a drawing rate of 3.5 times. As a comparison sample, the composite fiber incorporated with 0.15wt% unmodified rGO/PA6was prepared under the same processing conditions.

Characterization

The morphologies of GO, PDA-rGO and PA6 composite fibers were observed using field emission scanning electron microscopy (SEM, vltra55). Transmission electron microscopy (TEM, JEM-2100) was used to record the microstructure of GO and PDA-rGO. In transmission mode, Fourier transform infrared spectroscopy (FTIR, Nicolet 5700) of GO, rGO and PDA-rGO were tested with the scanning frequency 500~4000 cm^-1. Raman spectroscopy (Raman, ThinVia) was used to evaluate structural changes before and after GO modification. The sedimentation experiments were made a qualitative characterization of the dispersion properties. 1mg/ml nano-powder aqueous dispersion was prepared, and the settlement of the solution was observed after standing for 72 h. Thermal stability of GO, rGO, PDA-rGO and the composite fibers were conducted on thermogravimetric analyzer (TGA, TG209F3). The heating rate of TGA test was 5℃/min under nitrogen atmosphere. Mechanical properties of composite fibers were measured by a universal material stretching machine（6639, INSTRON）, and the composite fibers(length, 25 mm) were measured at a tensile rate of 20mm/min. Differential Scanning Calorimeter (DSC, Emerkin8000) was used to analyze the crystallization behavior of composite fibers. The heating and cooling rates were both 10℃/min under nitrogen atmosphere.

The morphology, composition and thermal properties of PDA- rGO

SEM and TEM images of the the surface morphology and microstructure of GO and PDA-rGO are presented in Fig. 3. GO has quite a multilayer sheet-like structure with a smooth surface and wrinkled edges, as shown in Fig. 3 (a) and (a'). However, the surface of PDA-rGO is covered with a thin film and the roughness of its surface is significantly increased after modification as presented in Fig. 3 (b) and (b'). This is the in-situ polymerization of DA on the surface of GO under alkaline environment, resulting in the formation of a uniformly wrapped PDA layer on the surface of GO [26]. It can also be seen that the PDA only wraps around the GO surface and does not change the multilayer sheet-like structure of GO.

Figure 4 shows the FTIR spectra of GO, rGO and PDA-rGO. The C = O stretching vibration peak at 1725cm^− 1, the C-O stretching vibration peak of the hydroxyl group at 1056 cm^− 1, the C = C vibration peak of the aromatic ring at 1625 cm^− 1, and the stretching vibration peak of hydroxyl group O-H at 3420cm^− 1 are the characteristic peaks of GO [19, 25, 27]. The C = O stretching vibration peaks of rGO and PDA-rGO at 1725 cm^− 1 decreased greatly, indicating that the carboxyl groups were mainly involved in the self-polymerization of dopamine onto the surface of GO. The newly generated peak at 1577 cm^− 1 is attributed to the N-H vibrational of PDA-rGO. The peaks of 2926 cm^− 1 and 2853 cm^− 1 can be ascribed to the symmetric stretching vibration and asymmetric stretching vibration of -CH₂ in the molecular of PDA, respectively [22]. It can be confirmed that PDA wase effectively coated onto the surface of GO through self-polymerization.

The structures of GO, rGO and PDA-rGO were further investigated using Raman spectra. As shown in Fig. 5, all samples revealed two distinct absorption peaks around 1350cm^− 1 and 1580cm^− 1, namely the D band peak formed by the vibration of SP³ carbon atoms and the G band peak generated from the sp² carbon atoms [27–28]. In most cases, the intensity ratio of the peaks (I_D/I_G, D band to G band) may be utilized to determine the degree of defects in the graphene structure [19, 29]. The I_D/I_G ratio of PDA-rGO was raised to 1.12 as compared to that of GO of 0.89. It demonstrated that PDA grafted on the surface of GO through the covalent bond and thus its intensity ratio was higher than that of GO [27].

The dispersion of carbon nanomaterials in aqueous solution can be investigated by sedimentation experiments. Figure 6 showed the optical photos of 1 mg/ml GO, rGO, and PDA-rGO after standing in aqueous solution for 72h. GO exhibited good hydrophilicity due to the abundant oxygen-containing functional groups on the surface, so it can be uniformly dispersed in aqueous solution for a long time. The rGO produced a sedimentation phenomenon in the solution, while the PDA-rGO could still be stably dispersed in the aqueous solution because of the hydrophilic functional groups such as hydroxyl groups on its surface. In addition, the color of the aqueous solution in the Fig. 6 changed from brown to black, which was attributed to the removal of oxygen-containing functional groups and the recovery of aromatic ring π-π bonds [26]. It was further confirmed that graphene oxide was reduced by ascorbic acid and PDA.

Figure 7 presents the TGA plots of GO, rGO and PDA-rGO. The weight loss of GO are substantially greater than that of rGO and PDA-rGO below 120 ℃, owing to the water and oxygen-containing groups on the surface of GO[30–31]. A major loss platform appears at around 200°C ~ 350°C, and the weight loss rate of rGO and PDA-rGO is far less than that of GO. This result was attributed to the restore of the carbon skeleton structure of rGO and PDA-rGO resulting in the improved thermal stability [19]. The weight loss of GO, rGO and PDA-rGO is 59.6%, 15.2% and 40.2%, respectively, when the temperature reaches 600℃. After GO was modified by PDA through covalent bond, the organic groups on the surface of PDA-rGO affected its thermal stability. In comparison with GO, the thermal stability of PDA-rGO was still effectively improved because the oxygen-containing functional groups on its surface are almost removed as a result of modification and reduction by PDA [22, 26].

The Morphology of composite fibers

Figure 8 depicts the surface and cross-section morphology of the pure PA6 fiber and composite fibers. The surface of the pure PA6 fiber is relatively smooth and fiber diameter is quite uniform with an average value of 20 µm. The surface roughness of the composite fiber increases with the addition of PDA- rGO (Fig. 8c), but the surface remains smooth and free of cracks and defects, demonstrating that the PDA-rGO / PA6 composite fiber can be spun and hot drawn continuously. The cross-sectional morphologies of the pure PA6 fiber and the 0.15wt%rGO/PA6 composite fibers are shown in Fig. 8 (a) and (b), respectively. It can be seen from Fig. 8 (b) that the unmodified rGO aggregates obviously in PA6 matrix because of the poor compatibility. PDA-rGO, on the other hand, is nicely embedded and uniformly dispersed in the PA6 matrix as shown in Fig. 8(d). Furthermore, neither holes or cracks are observed in the cross-section of the composite fiber, implying that the PDA-rGO and PA6 matrix has a robust interface interaction [32–33].

The mechanical properties of composite fibers

The mechanical characteristics of the pure PA6 fiber, the PA6 composite fiber with 0.15% unmodified rGO, and PDA-rGO/PA6 composite fibers with 0.05wt%, 0.15wt% ,0.3wt% PDA-rGO loading content are exhibited in Fig. 9 and Table 1. The tensile strength and Young's modulus (E) of 0.15wt% rGO/PA6 composite fiber increases slightly compared with that of pure PA6 fiber. The mechanical performance of the composite fiber is found to be significantly improved once PDA-rGO is added. The tensile strength and Young's modulus of the PDA-rGO/PA6 composite fiber reaches a maximum value at 310.4 MPa and 462.3MPa, respectively, when the PDA-rGO loading content is raised to 0.15wt%. However, as the loading content further increase, the composite fiber's tensile strength and Young's modulus begin to decline owing to the excessive addition of PDA-rGO, which resulted in the production of flaws and weak joints on the composite fiber [32]. Comparing PDA-rGO/PA6 and rGO/PA6 composite fibers, it is found that the mechanical strength of PDA-rGO/PA6 composite fiber increased by 45% over rGO/PA6 composite fiber when the content is the same at 0.15wt%.

Table 1

Tensile properties of PA6 fiber,0.15rGO/PA6 composite fiber and composite fibers containing different PDA-rGO content.
Loading content (wt%)	Tensile Strength (MPa)	Elongation at break (%)	Young's modulus (MPa)
0	204.3	75.2	386.4
0.05 PDA-rGO	247.8	67.3	412.3
0.15 PDA-rGO	310.4	58.4	462.3
0.3 PDA-rGO	229.1	54.1	405.8
0.15 rGO	213.5	46.5	394.6

The Halpin-Tsai model is one of the widely used polymer reinforcement mechanism models [19, 34, 35]. Herein, it is conducted to explore the reinforcement mechanism of PDA-rGO/PA6 composite fibers. In general, PDA-rGO may present ether an oriented or a random distribution state in the composite fibers. The theoretical Young's modulus of the composite fibers is calculated by the following modified Halpin-Tsai equations:

$${E}_{r}\left(random\right)={E}_{N}·\left[\frac{3}{8}\left(\frac{1+{\eta }_{L}·\xi ·{\nu }_{G}}{1-{\eta }_{L}·{\upsilon }_{G}}\right)+\frac{5}{8}\left(\frac{1+2{\eta }_{T}·{\upsilon }_{G}}{1-{\eta }_{T}·{\nu }_{G}}\right)\right] \left(1\right)$$

$${E}_{P}\left(parallel\right)={E}_{N}·\left(\frac{1+{\eta }_{L}·\xi ·{\upsilon }_{G}}{1-{\eta }_{L}·{\upsilon }_{G}}\right) \left(2\right)$$

$${\eta }_{L}=\frac{{E}_{G}/{E}_{N}-1}{{E}_{G}/{E}_{N}+\xi } \left(3\right)$$

$${\eta }_{G}=\frac{{E}_{G}/{E}_{N}-1}{{E}_{G}/{E}_{N}+2} \left(4\right)$$

$$\xi =\frac{l+\omega }{d} \left(5\right)$$

Where E_r and E_p denote Young's modulus of PDA-rGO/PA6 composite fibers with random and parallel oriented PDA-rGO nanosheets. E_N represents the Young's modulus of pure PA6 fiber (386.4 MPa), while E_G refers to the modulus of PDA-rGO (250 GPa) [19, 34]; In this model, the modified graphene nanosheets are regarded as strip solid fibers, with l, ω, and d representing the length, width and thickness of PDA-rGO (l = 3µm, ω = d 2µm, d = 2.4nm), respectively[35]. The mass fraction of PDA-rGO used in experimental section is converted into volume fraction V_G (%) from the following equations:

$${V}_{G}\left(\%\right)=\frac{{W}_{G}/{\rho }_{G}}{{W}_{G}/{\rho }_{G}+\left(1-{W}_{G}\right)/{\rho }_{N}} \left(6\right)$$

Where W_G is the mass fraction of PDA-rGO in the PA 6 matrix, ρ_G(1.8g/cm³) and ρ_N (1.13g/cm³) denote the density of PDA-rGO and pure PA6 fiber, respectively [19, 35].

Figure 10 shows the experimental modulus and the Halpin-Tsai theoretical modulus of PDA-rGO/PA6 composite fiber. When the volume fraction of PDA-rGO is less than 0.1%, the experimentally measured Young's modulus data is pretty much close to theoretical calculated value by the random distribution model of PDA-rGO in PA6 matrix, and they both show an upward trend with the increase of filler content. This indicates on the one hand that PDA-rGO is randomly distributed in the matrix, and on the other hand that at low contents, the experimental and theoretical values basically coincide because PDA-rGO can be uniformly dispersed in the matrix without causing stress concentration due to agglomeration in the matrix. Similar findings were reported by Liu Haihui, Jia Hongbing, etc[19, 35, 38]. When the volume fraction of PDA-rGO exceeds 0.09%, however, the experimental modulus deviates from the value of theoretical model and shows a downward trend. This is primarily due to the agglomerates of PDA-rGO in the matrix, which may introduce defects and thus become a mechanical weak point.

At this point, we can rule out the contribution of PDA-rGO orientation to the mechanical properties, and the reason directed at the non-orientation is probably related to the fact that the tensile stress field applied by our processing equipment is not that strong. The following aspects are accountable for the substantial improvement in the mechanical properties : (i) The PDA modified graphene nanosheets can be uniformly dispersed in the PA6 matrix, which not only greatly avoids the stress concentration caused by agglomeration, but also brings out the laminar fold structure of rGO as much as possible, playing a much better role in stress dispersion and transfer [37]; (ii) there is a good interfacial compatibility and strong interfacial bonding between the PDA-rGO and PA6 matrix, which on the one hand can prevent the slip of the matrix molecular chain on the PDA-rGO surface, and can also make the stress effectively transferred to the PDA-rGO; (iii) The molecules onto the surface of PDA-rGO and the PA6 macromolecular chain formed a three-dimensional network structure through hydrogen bond interactions chain and entanglement during during melt mixing and spinning, which restricted the movement of the macromolecular chains and thus it also explained the gradual decrease in the elongation at break of the composite fibers [11, 32].

The thermal properties of composite fibers

The crystallization behavior of PA6 fiber and composite fibers can be measured by DSC. Here, T_m (the melting temperature) and T_c (the crystallization temperature) were tested as the peak points. $\text{X}\text{c}$(crystallinity) was measured by the following formula:

$${X}_{c}=\frac{{\Delta }{\text{H}}_{f}}{\left(1-\alpha \right){\Delta }{\text{H}}_{{f}^{*}}} \times 100\% \left(7\right)$$

where α represents the proportion of PDA-rGO filler in the PA6 matrix, ΔH_f refers to the melting enthalpy of the prepared composite fibers, and ΔH_f* is the melting enthalpy of 100% crystallization of PA6 corresponding to190 J/g.

T_m of the PDA-rRG/PA6 composite fibers does not change much with the incorporation of PDA-rGO, as shown in Fig. 11 and Table 2, while T_c moves toward higher temperature. In addition, the crystallinity increases slightly up to 33.4% when the PDA-rGO content is 0.15%. Because of its homogeneous dispersion in the PA6 matrix, PDA-rGO may act as a heterogeneous nucleating agent, promoting crystallization of PA6 [36]. The crystallinity of the composite fibers starts to decline inversely after the addition of 0.3% PDA-rGO. his is due to the reduced nucleation efficiency since that the excess graphene nanosheets may agglomerate and accumulate in PA6. As can be observed, the effect of PDA-rGO on the crystallization behavior of the composite fibers is not significant. This may be due to the thermal stretching field experienced in the fiber preparation, where the stresses ordered the PA6 molecular chains and promoted the crystallization, thus the effect of PDA-rGO on the crystallization of the matrix is weakened and not to be manifested [37]. It also suggests that crystallinity should have little to do with the above mechanical properties.

Table 2

DSC data of PA6 fiber and composite fibers containing different PDA-rGO content
Loading content (wt%)	T_m (℃)	ΔH_f (J/g)	T_c (℃)	X_c (%)
0	223.84	57.1	187.2	30.1
0.05 PDA-rGO	223.73	60.4	187.8	31.8
0.15 PDA-rGO	223.11	63.4	189.2	33.4
0.3 PDA-rGO	223.69	59.2	189.5	31.2

The TGA results of pure PA6 and composite fibers are shown in Fig. 12, meanwhile, the specific data of T₅ (the decomposition temperature at 5% weight loss) and T_max (the decomposition temperature at maximum weight loss) are listed in Table 3. Compared with pure PA6 fiber, T₅ of the composite fiber increases by 13℃ to 364.3℃ when the PDA-rGO loading content is 0.15wt%, and the T_max decomposition occurs at 445.7℃. The addition of PDA-rGO significantly improves the thermal stability of composite fibers. The improved thermal stability of the composite fiber is assisted by the uniform dispersion of modified graphite nanosheets in the matrix, which can form a three-dimensional network structure that will restrict the molecular movement of PA6 matrix as well as a certain physical barrier effect suppresses the thermal decomposition of the composite fibers [32, 39].

Table 3

TGA data of PA6 fiber and composite fibers containing different PDA-rGO content
Loading content(wt%)	T₅(℃)	T_max (℃)
0	351.3	440.5
0.05 PDA-rGO	355.8	443.8
0.15 PDA-rGO	364.3	445.7
0.3 PDA-rGO	363.9	442.1

In summary, the reinforced PDA-rGO/PA6 composite fibers with 3D network structure were prepared by simple melt mixing. PDA was successfully grafted on the surface of GO through covalent bond, and the modification and reduction of GO were completed simultaneously. At a loading content of 0.15wt% PDA-rGO, the PDA-rGO/PA6 composite fiber displayed significantly improved tensile strength (310.4MPa) and Young's modulus (462.3MPa). The DSC results revealed that the crystallinity increased from 30–33% due to the heterogeneous nucleation of PDA-rGO, and the thermal stability also showed meaningfully enhancement. The good dispersibility and enhanced interfacial interaction endowed the composite fibers with excellent comprehensive properties, especially the remarkable mechanical properties. Therefore, modified graphene composite fibers provide a new ideal way to prepare reinforcing fibers.

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posted 18 Apr, 2022

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Mechanical reinforcement in nylon 6 nanocomposite fiber incorporated with dopamine reduced graphene oxide

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Abstract

Figures

Introduction

Experiment

Results And Discussion

The morphology, composition and thermal properties of PDA- rGO

Conclusion

References

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