Home Effect of different proportions of CNTs/Fe3O4 hybrid filler on the morphological, electrical and electromagnetic interference shielding properties of poly(lactic acid) nanocomposites
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Effect of different proportions of CNTs/Fe3O4 hybrid filler on the morphological, electrical and electromagnetic interference shielding properties of poly(lactic acid) nanocomposites

  • Bozhen Wu , Honghao Zhu , Yuhao Yang , Jiang Huang , Tong Liu , Tairong Kuang EMAIL logo , Shaohua Jiang EMAIL logo , Aleksander Hejna and Kunming Liu
Published/Copyright: April 1, 2023
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e-Polymers
From the journal e-Polymers Volume 23 Issue 1

Abstract

Due to the shortage of petroleum resources, poly(lactic acid) (PLA), a biodegradable polymer, has been widely considered as a replacement for traditional petroleum-based polymers. Therefore, multifunctional PLA composites have become increasingly popular. In this study, conductive carbon nanotubes (CNTs) and magnetic nano-Fe3O4 fillers were melt-blended with PLA. The impact of CNTs and nano-Fe3O4 composition on the electrical and electromagnetic interference (EMI) shielding properties of PLA nanocomposites was investigated in detail by adjusting the CNTs-to-nano-Fe3O4 ratio. When the hybrid filler content was fixed at 10 wt%, the electrical conductivity results indicated that the addition of single CNTs could effectively improve the conductivity of the nanocomposites, while nano-Fe3O4 contribution was hardly noted. A suitable ratio of electromagnetic hybrid fillers can yield excellent synergistic effects in EMI shielding properties. The nanocomposites containing CNTs and nano-Fe3O4 in a 50:50 ratio exhibited excellent electrical conductivity (90.6 S·m−1) and EMI shielding effectiveness (EMI SE ∼ 40.5 dB). This is primarily because CNTs provide good electrical conductivity, but the addition of magnetic nano-Fe3O4 provides additional interfacial polarization and eddy current losses caused by its dielectric and magnetic properties. These properties synergistically result in an impedance mismatch, dielectric loss, and polarization relaxation of the composite materials, improving the shielding properties against electromagnetic waves. Further, it was found that changing the ratio of electromagnetic hybrid fillers also affected electromagnetic wave absorption. When the ratio of CNT-to-nano-Fe3O4 was 25:75, the nanocomposites had an EMI SE of 24.6 dB, and the absorptivity could reach the maximum (40.3%). Thus, this study provides a valuable reference for preparing multifunctional polymer nanocomposites by constructing electromagnetic hybrid filler networks.

Keywords: multifunctional PLA nanocomposites; CNTs/Fe3O4 hybrid filler; electrical conductivity; EMI shielding

1 Introduction

Globally, energy and environmental issues have become a significant focus of attention. Due to the intensification of the energy crisis and environmental pollution, biodegradable polymers are considered vital to solving white pollution and conserving fossil fuels (1,2,3,4). As a biodegradable polymer with the fastest industrialization process, poly(lactic acid) (PLA) has excellent mechanical and processing properties, biodegradability, and biocompatibility. It is produced from renewable resources such as corn, potatoes, and crop straw, making it a promising alternative to petroleum-based polymers (5,6,7,8,9,10). Nevertheless, PLA has inherent defects, such as high brittleness, a slow crystallization rate, and a lack of functionality, which make it incompatible with electronic devices (11,12,13,14). Due to these factors, multifunctional PLA materials have attracted considerable interest from researchers who aim to improve their performance and broaden their application range.

Adding functionalized nano-fillers to PLA is the most common method of imparting multifunctionality to PLA. Multiple literature works have reported melt blending (1,15,16,17), solution blending (18,19,20), mechanical mixing (21,22), in situ polymerization (23,24), 3D printing (25,26,27), and other methods to introduce functional fillers into PLA to enhance the conductive and electromagnetic interference (EMI) shielding properties of the composites (5,28,29,30,31). Melt blending, among these methods, is more prevalent among researchers due to its easy mass production, simple process, and environmental benefits. Researchers initially used single-functional fillers to improve the properties of PLA composites (32). For example, Gupta et al. prepared PLA/graphene nanoplatelets (GNP) composites using melt blending and found that when filled with only 3 wt% GNP, the conductivity of the composites significantly improved by nine orders of magnitude, while filling with 15 wt% GNP could result in EMI shielding effectiveness (SE) values of up to 15.5 dB in the X-band frequency range (33).

Nevertheless, adding higher quantities of conductive filler to the composite is often necessary to achieve high EMI SE and conductivity, which leads to a significant reduction in other composite properties and a high cost (34,35,36). Introducing a second conductive filler is an efficient way to improve PLA composites’ conductive and EMI shielding properties by building a richer and more complete conductive network (25,37,38). For example, Ivanov et al. prepared PLA/GNP/multi-walled carbon nanotubes (MWCNT) hybrid composites by melt blending and found a synergistic effect between GNP and MWCNTs when they added the same amount of hybrid fillers with a higher electrical conductivity than either single filler alone (25). The synergistic effect of the hybrid fillers resulted in high EMI SE values (K-Band (18–26.5 GHz), 30 dB) for the composites (38). Despite the benefits of increasing the electrical conductivity and EMI shielding performance of the composites by introducing a large amount of hybrid conductive fillers, this may also result in a significant impedance mismatch between the material interface and air, resulting in a more significant amount of reflected electromagnetic waves and secondary pollution (32,35,39). To address this issue, it has been proven that compounding magnetic, semiconductor, and conductive fillers has successfully improved the EMI shielding performance and absorption loss of PLA composites (36,40,41,42,43). Adding magnetic fillers would increase the interfacial polarization between the magnetic and conductive fillers, resulting in increased magnetic and dielectric losses and, ultimately, enhancing electromagnetic absorption (40,44). Liu et al. used the solution blending method to obtain PLA/CNTs/Fe3O4 composite films and investigated the effect of the ratio of electromagnetic hybrid fillers on the EMI shielding of the composite films in greater detail (40). The composite films exhibited good EMI SE values (22 dB) when the CNT-to-Fe3O4 ratio was 3:1, but there was no reported improvement in their absorption losses. Although it has been shown that electromagnetic hybrid fillers have excellent synergistic effects, to our knowledge, melt blending methods have not yet been used to investigate the effects of different CNTs and nano-Fe3O4 ratios on the structure and properties of PLA composites.

In this work, we prepared PLA/electromagnetic hybrid filler nanocomposites by direct melt blending, using CNTs for the conductive filler and nano-Fe3O4 for the magnetic filler with a 10% content of hybrid filler. The study’s main objective was to investigate the synergistic effects of different ratios of CNTs/Fe3O4 hybrid filler systems by melt blending on the electrical conductivity and EMI shielding performance of PLA nanocomposites and explained the mechanism. The results indicated that when the conductive filler and magnetic filler were 1:1 (the total hybrid filler content was 10 wt%), the nanocomposites had the highest EMI SE, which is significantly higher than the composites prepared by solution blending in previous literature (40). In addition, the effects of different proportions of hybrid fillers on the mechanical properties and thermal stability of PLA nanocomposites were investigated. X-Ray diffraction (XRD) and scanning electron microscopy (SEM) analysis were used to measure the dispersion of electromagnetic hybrid fillers in PLA nanocomposites.

2 Materials and methods

2.1 Materials

Poly(l-lactide) (PLA, 4032D) was supplied by Nature Works LLC, with an MFR of 7 g‧10 min−1 (210°C, 2.16 kg) and a density of 1.24 g‧cm−3. Multiwalled carbon nanotubes (CNTs, Nanocyl 7000) were provided by Nanocyl S.A. (Belgium) with an average length of 1.5 μm and an average diameter of 9.5 nm. Nano-Fe3O4 particles with an average size of 20 nm were obtained from Shanghai Macklin Biochemical Co., Ltd. (China). All materials were used without further purification.

2.2 Preparation of PLA/CNTs/Fe3O4 nanocomposites

Before melt blending, PLA, CNTs, and nano-Fe3O4 were dried at 80°C for 12 h to prevent hydrolytic degradation. Using an internal mixer (Haake Rheomix OS R600, Germany), hybrid fillers (CNTs/Fe3O4) were incorporated into PLA at a fixed content of 10 wt%. The mixing temperature was 180°C with roller rotors operating at 60 rpm for a mixing time of 10 min. PLA/CNTs/Fe3O4 nanocomposites were prepared with different ratios of hybrid fillers, and the nanocomposites were then compression molded at 190°C under 10 MPa for 5 min. For convenience, various nanocomposites with a CNTs/Fe3O4 mass ratio of 0/10, 2.5/7.5, 5/5, 7.5/2.5, and 10/0 were designated by the codes of 0C100F, 25C75F, 50C50F, 75C25F, and 100C0F. Figure 1 illustrates the schematic diagram for preparing the PLA/CNTs/Fe3O4 composite.

Figure 1 Schematic diagram illustrating the preparation process of PLA/CNTs/Fe3O4 nanocomposites.
Figure 1

Schematic diagram illustrating the preparation process of PLA/CNTs/Fe3O4 nanocomposites.

2.3 Characterization

2.3.1 Morphology analysis

The fracture surfaces of PLA/CNTs/Fe3O4 nanocomposites were observed using a scanning electron microscope (SEM, Tescan VEGA3 SBH, Czech Republic). The accelerated voltage of 5 kV was used for samples with a low content of CNTs, and 10 kV for samples with a CNTs content exceeding 5 wt%. A thin layer of gold was deposited on the fractured surfaces of the samples before observation. XRD determined the nanocomposites’ phase compositions (UltimaIV, Japan). XRD analysis with Cu Ka (λ = 1.5418 Å) radiation was performed in the scanning range of 10–80° at 2°‧s−1.

2.3.2 Mechanical properties

A universal testing instrument (Instron 5966, USA) was employed to conduct static mechanical tests at room temperature for both tensile and flexural tests. Samples were tested at a tensile rate of 2 mm‧min−1 during the tensile test with the dimension of 20 mm × 4 mm × 2 mm. Flexural tests were conducted using a three-point bending test at a strain rate of 2 mm·min−1 with the dimension of the specimen being 80 mm × 10 mm × 4 mm. The impact test was carried out using a Ray-Ran Izod impact tester (XC-22, Shandong Drick Instruments Co., Ltd., China). The samples were 80 mm × 10 mm × 4 mm with a 2 mm notch. For each mechanical test, the average value of 5 samples was taken as the result.

2.3.3 Dynamic mechanical analysis (DMA)

The DMA was performed in a tensile resonant mode at a heating rate of 3°C‧min−1 from 30°C to 100°C (Q800, TA Instruments, USA). The nanocomposites’ storage modulus (E′) and loss factor (tan δ) were determined. The dimension of the specimen was 30 × 10 mm2 with a thickness of 2 mm.

2.3.4 Thermogravimetric analysis (TGA)

TA model Q500IR thermogravimetric analyzer (New Castle, Delaware, USA) was used to analyze the thermal degradation properties of the nanocomposites. Under a nitrogen atmosphere, 12 mg samples were added to alumina crucibles and heated from 25°C to 750°C at a rate of 10°C‧min−1.

2.3.5 Electrical properties

For high conductivities (>1 × 10−6 S‧m−1), samples were measured with a four-point probe resistivity meter (RTS-8, Four Probes Tech., Guangzhou, China). The specimen dimension was 25 mm in diameter with a thickness of 2 mm. For low conductivities (≤1 × 10−6 S‧m−1), a high resistance insulation instrument (ZC36, Shanghai Anbiao Electronics Co., Ltd.) was employed for the test. The dimension of the specimen was 80 mm × 80 mm × 2 mm. Each group of specimen was tested five times and averaged.

2.3.6 EMI shielding properties

EMI shielding performances of nanocomposites were measured using a Ceyear 3672C-S vector network analyzer (VNA) across the frequency range of 8.2–12.4 GHz (X-band). The measured samples were shaped into rectangular sheets to fit the sample holder. The dimensions of the measured samples were 22.86 mm × 10.16 mm × 4.00 mm. Three samples were prepared for testing in each group, and the average value was recorded.

VNA measurements are used to evaluate the EMI shielding performance by measuring the EM parameters S11 and S21. The SE of absorption (SEA), reflection (SER), and total (SET) were determined from the absorbance (A), reflectance (R), and transmittance (T) based on the equations given in Eqs. 1–6:

(1) R = | S 11 | 2

(2) T = | S 21 | 2

(3) A = 1 − R − T

(4) SE R = − 10 log ( 1 − R )

(5) SE A = − 10 log T 1 − R

(6) SE T = − 10 log T = SE A + SE R

3 Results and discussion

XRD was used to characterize the structure of pure PLA and PLA nanocomposites, and the result is shown in Figure 2. The XRD pattern of pure PLA shows only a broad peak at 16.5°, which corresponds to the (110)/(200) planes, indicating mainly an amorphous structure (45,46). A peak at 2θ = 26.0° is evident in the XRD pattern of PLA/CNTs/Fe3O4 nanocomposites exhibited by reflections of the CNTs (47). The diffraction peaks of nano-Fe3O4 can also be observed at 30.4°, 35.5°, 43.5°, 53.7°, 57.4°, and 62.8°, respectively. The nanocomposites’ peak positions and relative intensities were in good agreement with those obtained from the standard card (JCPDS no. 19-0629) (48,49). The 0C100F nanocomposites’ (002) peak disappeared due to the absence of CNTs in the matrix. Moreover, at low CNT content, the (002) peaks of the composites become insignificant, and similar results have been reported in the previous literature (50). It may be caused by the fact that CNTs with low content are dispersed more uniformly during the melt blending process.

Figure 2 XRD Spectra of PLA nanocomposites with different CNTs/Fe3O4 filler content ratios.
Figure 2

XRD Spectra of PLA nanocomposites with different CNTs/Fe3O4 filler content ratios.

SEM was used to analyze the distribution of single fillers (CNTs or nano-Fe3O4) and hybrid fillers (CNTs/Fe3O4) in PLA nanocomposites. A further investigation of the element distribution and content was conducted using EDS mapping. As shown in Figure 3, PLA/CNTs/Fe3O4 nanocomposites with different proportions of hybrid fillers exhibit different fracture morphologies as well as Fe element distributions. Compared to pure PLA (Figure 3a), the morphology of nanocomposites containing only nano-Fe3O4 (Figure 3c) is mainly flat with a small number of agglomerates. When the content of the CNTs network is low, as shown in Figure 3b, the network is relatively sparse. Conversely, the high CNTs content in the composites results in the CNTs being tightly entangled, resulting in a conductive network (Figure 3c–e). Thus, by increasing the content of CNTs, the matrix’s conductive network becomes denser and more perfect. Nevertheless, as CNT content increases, defects of composites also increase. According to Figure 3a′–f′, with a decrease in nano-Fe3O4 content, the Fe element distribution gradually becomes sparse, indicating a decrease in total Fe element content. Considering the Fe element distribution shown in Figure 3a′ and f′, pure PLA and 100C0F did not contain nano-Fe3O4 particles. As depicted in the figure, the points representing Fe should represent noise generated in the process of analyzing the element. As the nano-Fe3O4 content increases, the figure shows significant aggregation of elements, which can cause defects in the polymer matrix and adversely affect the polymer’s thermal stability.

Figure 3 SEM images of (a) pure PLA, (b) 0C100F, (c) 25C75F, (d) 50C50F, (e) 75C25F, and (f) 100C0F; EDS mapping results of Fe element: (a′) pure PLA, (b′) 0C100F, (c′) 25C75F, (d′) 50C50F, (e′) 75C25F, and (f′) 100C0F.
Figure 3

SEM images of (a) pure PLA, (b) 0C100F, (c) 25C75F, (d) 50C50F, (e) 75C25F, and (f) 100C0F; EDS mapping results of Fe element: (a′) pure PLA, (b′) 0C100F, (c′) 25C75F, (d′) 50C50F, (e′) 75C25F, and (f′) 100C0F.

It was also investigated whether different ratios of electromagnetic hybrid fillers would affect the mechanical properties of PLA nanocomposites. Compared with pure PLA, all composites showed a slight decrease in mechanical properties by adding single and hybrid fillers (Figure 4). Figure 4a illustrates the effect of different proportions CNTs/Fe3O4 hybrid fillers on the tensile properties of the nanocomposites. In pure PLA, the tensile strength reached 58.8 MPa. However, the strength of nanocomposites decreased continuously as the proportion of CNTs in the CNTs/Fe3O4 hybrid filler increased but still maintained about 80% of the strength of pure PLA. The lowest tensile strength of the 100C0F composite was 46.7 MPa, whereas the highest tensile strength of the 0C100F composite was 56.6 MPa. The flexural strength of the composites was strongly affected by the filler, especially at high proportions of CNTs (Figure 4b). Adding filler had the most negligible impact on impact toughness compared to other properties (Figure 4c). 100C0F, for example, showed an impact toughness of 2.37 kJ‧m−2, which was lower than 2.75 kJ‧m−2 for PLA. These phenomena are primarily related to the filler’s disruption of polymer molecular chain entanglement, which weakens their interaction. External forces may cause the gap between polymer molecular chain segments to become larger and cause cracks when they separate and slip from the filler particles. Meanwhile, due to the high content of CNTs, various defects are detected in the matrix, which negatively impacts its mechanical properties. However, due to the relatively low content of the fixed filler in this work, the defects and agglomeration in the composite are less, which makes the mechanical properties not decrease significantly (51). Additionally, the introduction of nano-Fe3O4 also adversely affects the mechanical properties of the composites, although not to the same extent as CNTs. This is because nano-Fe3O4 is smaller than CNTs, it is easier to disperse during blending, and it is less likely to cause cracks or defects when external forces are applied.

Figure 4 Mechanical properties of pure PLA and PLA nanocomposites: (a) tensile strength, (b) flexural strength, and (c) impact strength.
Figure 4

Mechanical properties of pure PLA and PLA nanocomposites: (a) tensile strength, (b) flexural strength, and (c) impact strength.

Figure 5 illustrates the tensile and flexural moduli of PLA composites with different proportions of CNT and nano-Fe3O4. It indicates that the modulus of composites increases to a certain extent with the addition of filler. With the increase of CNT content, the tensile and bending moduli of composites also increase. Figure 5a illustrates that different proportions of CNT and ferric oxide compounds have little influence on the modulus of the composite, but both have great improvement compared with pure PLA. The tensile modulus of pure CNT is higher, indicating that compared with nano-Fe3O4, CNT has more obvious rigidity enhancement for the composite. Figure 5b shows a similar result, but the flexural modulus change is more dependent on the CNT content change. Combined with Figure 4, it can be found that the modulus is usually negatively correlated with strength, which means that increasing the modulus of the filling material usually results in a decrease of strength. This is consistent with previous literature reports (51).

Figure 5 (a) Tensile modulus and (b) flexural modulus of pure PLA and PLA nanocomposites.
Figure 5

(a) Tensile modulus and (b) flexural modulus of pure PLA and PLA nanocomposites.

Viscoelasticity can not only provide information on the processing and mechanical properties of polymers but can also provide information on the structure and motion of molecules. Hence, DMA was used to examine the effect of hybrid filler on the viscoelastic properties of the nanocomposites, including storage and loss moduli, as well as loss tangent (tan δ). Values of storage and loss moduli quantify the portion of elastic and viscous components in the analyzed material. In contrast, loss tangent defines the phase lag of strain with respect to applied stress. According to Figure 6a and b, the storage and loss modulus of nanocomposites containing varying proportions of hybrid fillers varied significantly between 60°C and 80°C, attributed to the glass transition (52). For various nanocomposite samples, the values of glass transition temperature (T g), determined as the temperature position of tan δ peak (Figure 6c), were in the range of 70.4–71.9°C, which is typical for PLA materials. Therefore, changes in T g can be considered negligible. By adding fillers, the storage modulus and loss modulus of nanocomposites increased. The storage modulus enhancement is attributed to the stiffening of the composites’ structure due to the reduced mobility of PLA macromolecular chains around the filler nanoparticles. The loss tangent peak of the composites decreased significantly, confirming the inhibition of the movement of molecular chain segments due to the rigid nature of both CNTs and nano-Fe3O4 (53,54). The volume of constrained polymer chains (C v) can be calculated from the DMA results, particularly from the tan δ peak values. According to Bindu and Thomas (55), C v can be calculated using Eq. 7:

(7) C v = 1 − ( 1 − C 0 ) · W W 0

where C 0 is the volume of constrained polymer chains with unfilled fillers, and W is the energy loss fraction determined by the Eq. 8:

(8) W = π · tan δ π · tan δ + 1

Figure 6 DMA results of pure PLA and PLA nanocomposites: (a) storage modulus, (b) loss modulus, and (c) tan δ.
Figure 6

DMA results of pure PLA and PLA nanocomposites: (a) storage modulus, (b) loss modulus, and (c) tan δ.

Values of C v calculated for prepared nanocomposites are presented in Table 1. It can be seen that these values are increasing proportionally to the share of CNTs in filler compositions. It suggests the significantly higher ability to immobilize PLA macromolecular chains of CNTs compared to nano-Fe3O4 particles. Moreover, the decrease of the tan δ peak magnitude indicates that CNTs and nano-Fe3O4 improve the crystallization ability of PLA.

Table 1

Values of constrained chain volume and composite performance factor of PLA/CNTs/Fe3O4 nanocomposites with different proportions

Samples C v (vol%) C Factor Samples C v (vol%)
Pure PLA 0 — Pure PLA 0
0C100F 1.15 1.04 0C100F 1.15
25C75F 5.40 0.62 25C75F 5.40
50C50F 10.68 0.25 50C50F 10.68
75C25F 12.10 0.21 75C25F 12.10
100C0F 18.51 0.09 100C0F 18.51

The composite performance factor may also quantify the impact of applied fillers on the composites’ stiffening (C factor) (56), expressed by the following Eq. 9:

(9) C = ( E g ′ / E r ′ ) composite ( E g ′ / E r ′ ) matrix

where E′ is the storage modulus tested by DMA analysis, and subscripts g and r related to the glassy and rubbery state, respectively.

The decreasing values of the C factor indicate increased efficiency of introduced fillers in stiffening polymer matrix. Clearly, the values are significantly decreasing with the CNTs content and the increasing volume of constrained polymer chains. Such an effect is related to the significantly higher E′ values over T g for higher shares of CNTs, even despite the higher storage modulus with higher nano-Fe3O4 proportions in CNTs/Fe3O4 hybrid fillers below the glass transition temperature.

We also examined the effects of different ratios of electromagnetic hybrid fillers on the nanocomposites’ electrical conductivity and electromagnetic shielding properties. It is widely known that the electrical conductivity of materials is one of the most critical factors affecting EMI shielding performance (57,58). The high electrical conductivity of the material allows the incident electromagnetic waves to interact with moving carriers when they enter the surface and interior of the material, causing them to reflect and dissipate. As shown in Figure 6, the electrical conductivity of nanocomposites is primarily determined by the content of CNTs. When 10 wt% nano-Fe3O4 is added, the nanocomposite conductivity reaches 1.33 × 10−13 S‧m−1, which is two orders of magnitude higher than that of pure PLA; when 10 wt% CNTs is added, the conductivity of the composite is increased from 1.88 × 10−15 S‧m−1 of pure PLA to 286.67 S‧m−1, which is a substantial performance improvement of 17 orders of magnitude. A slight decrease in conductivity was observed between PLA/CNTs/Fe3O4 nanocomposites (Figure 7a) and PLA/CNTs composites (Figure 7b) with the exact content of CNTs. This was mainly the consequence of Fe3O4’s small particle size compared to pure CNTs (40), and its difficulty forming conductive pathways when combined with CNTs and PLA due to its dispersion as nanoparticles in the matrix. In this regard, it can be concluded that nano-Fe3O4 is unlikely to contribute to the perfection of conductive networks. Based on the EDS mapping results, the agglomeration of nano-Fe3O4 inhibits the formation of CNT conductive networks. Other literature has reported similar results (59,60).

Figure 7 Electrical conductivity of (a) PLA/CNT/Fe3O4 nanocomposites with different ratios of hybrid filler and (b) PLA/CNTs composites with various CNTs content.
Figure 7

Electrical conductivity of (a) PLA/CNT/Fe3O4 nanocomposites with different ratios of hybrid filler and (b) PLA/CNTs composites with various CNTs content.

Figure 8 shows the EMI shielding properties of nanocomposites at the X-band (8.2–12.4 GHz). In pure PLA, the EMI SE is only 1.8 dB, mainly because PLA is a poor conductor and cannot shield electromagnetic waves. The EMI SE of PLA nanocomposites (0C100F) does not significantly improve when a nano-Fe3O4 filler is added, as shown in Figure 8a. This is mainly because nano-Fe3O4 does not contribute enough to the composite conductivity to generate acceptable carriers for electromagnetic waves to reflect and dissipate. With a single CNTs filler, the EMI SE values of 100C0F composites reached 33.8 dB, primarily due to the good electrical conductivity of CNTs. The results of different ratios of CNTs/Fe3O4 hybrid fillers on the EMI shielding performance showed that the 50C50F sample showed the highest average EMI SE of 40.5 dB (Figure 8b), which is much higher than that of the PLA/MWCNTs/Fe3O4 composites prepared by solution blending (EMI SE∼18.5 dB) (36). Thus, the electromagnetic hybrid fillers have an excellent synergistic effect at an optimum ratio. Aside from this, with increasing nano-Fe3O4 content in the electromagnetic hybrid filler, the absorption coefficient of electromagnetic waves is also increasing, and the EMI SE for the 25C75F sample remains at 24.6 dB, and the absorption coefficient reaches 40.3% (Figure 8c). This can be attributed to the decrease in conductivity, which improves the impedance matching, and the addition of magnetic fillers, which enhances the absorption loss of electromagnetic waves by the composite. A comparison of EMI SET with other reports containing CNT or nano-Fe3O4 is shown in Figure 9, which indicates that EMI SE in this work is at a high level with low filler content. The mechanism of electromagnetic hybrid fillers’ effect on EMI shielding performance is also discussed (Figure 8d). In contrast to conductive fillers, magnetic nanofillers contribute to electromagnetic shielding differently. A single magnetic filler has an eddy current loss due to its magnetism and polarization loss and relaxation loss due to its own magnetism. Despite this, conductive fillers have a significantly higher shielding efficiency than magnetic fillers (68,69). Electromagnetic hybrid filler systems can shield electromagnetic waves by introducing magnetic fillers that synergize with conductive fillers. This is because the combination of conductive and magnetic fillers with compatible impedance matching characteristics and dissipation ability has better microwave response, and the small gap between permittivity and permeability of the magnetic material can lead to the introduction of more incident microwaves. The introduction of hybrid fillers in the system will make the composites have more defects, and the asymmetric charge distribution will lead to increased polarization and relaxation losses (70,71).

Figure 8 EMI SE of (a) 8.2–12.4 GHz, (b) SEA, SER and SET, (c) absorbance (A), reflectance (R) and transmittance (T), and (d) EMI shielding mechanism of PLA/CNTs/Fe3O4 composites with different ratios of hybrid filler.
Figure 8

EMI SE of (a) 8.2–12.4 GHz, (b) SEA, SER and SET, (c) absorbance (A), reflectance (R) and transmittance (T), and (d) EMI shielding mechanism of PLA/CNTs/Fe3O4 composites with different ratios of hybrid filler.

Figure 9 Comparison of EMI SET and content of filler for different polymer composites (61,62,63,64,65,66,67).
Figure 9

Comparison of EMI SET and content of filler for different polymer composites (61,62,63,64,65,66,67).

Different proportions of hybrid fillers were examined regarding their effects on the thermal stability of PLA/CNTs/Fe3O4 nanocomposites. The TGA curves are shown in Figure 10, and the corresponding data are summarized in Table 2. Compared to pure PLA, the thermal decomposition temperature of 100C0F decreased by 23.3°C. In general, CNT additions could significantly improve the thermal stability of polymer composites (72); however, excessive MWCNT agglomeration caused the composite to decompose more rapidly. Due to the high thermal conductivity of CNTs, on the one hand, heat could be conducted quickly to the interior of the composite, thereby reducing its thermal degradation temperature. On the other hand, the agglomeration of CNTs weakens the molecular chain interaction between fillers and PLA matrix and thus reduces the thermal stability of nanocomposites. A similar phenomenon has been observed in the previous literature (73,74). Moreover, the thermal decomposition temperature of 0C100F decreased after adding nano-Fe3O4 (by 7.27°C), which could be because the active sites on the surface of nano-Fe3O4 can act as depolymerization catalysts to accelerate PLA degradation (75). Furthermore, compared to 0C100F, the thermal decomposition temperature of nanocomposites containing electromagnetic hybrid fillers was lower but still higher than 100C0F. The results indicated that although the single fillers reduced the thermal stability of the composites, the hybrid fillers did not significantly affect the composites’ thermal stability. Furthermore, compared to nano-Fe3O4, the amount of CNTs in the polymer matrix plays a significant role in determining thermal stability since CNT content influences thermal decomposition temperature significantly.

Figure 10 TGA curves of PLA/CNTs/Fe3O4 nanocomposites with different proportions of CNTs/Fe3O4 filler.
Figure 10

TGA curves of PLA/CNTs/Fe3O4 nanocomposites with different proportions of CNTs/Fe3O4 filler.

Table 2

TGA results of PLA/CNTs/Fe3O4 nanocomposites with different proportions of CNTs/Fe3O4 filler

Samples T 5 (°C) T 50 (°C) T 75 (°C) Char (%)
Pure PLA 336.2 367.7 376.4 1.1
0C100F 328.9 341.8 347.1 9.4
25C75F 322.8 342.5 349.1 10.2
50C50F 317.4 340.2 346.7 10.5
75C25F 313.4 342.1 349.7 10.3
100C0F 312.9 359.2 370.6 10.4

4 Conclusions

In summary, this study investigated the effects of electromagnetic hybrid fillers (CNTs/Fe3O4) on the morphological, thermal, mechanical, electrical, and EMI shielding properties of PLA nanocomposites. The XRD and SEM results indicated that the CNTs were well dispersed at low contents, and the random conductive networks formed by the CNTs were clearly visible. As revealed by TGA analysis, CNTs/Fe3O4 hybrid fillers adversely affected the thermal stability of PLA but did not affect conventional processing. According to DMA analysis, nano-Fe3O4 contributed most to the stiffness of the composites, and the addition of the hybrid filler promoted crystallization and resulted in a decrease and broadening of the internal friction peak. Furthermore, the addition of electromagnetic hybrid fillers reduced the mechanical properties of the composites but still maintained a high tensile strength. Finally, the composites’ electrical conductivity and EMI shielding performances demonstrate that the addition of CNTs can significantly improve their electrical conductivity, whereas nano-Fe3O4 has little effect on it. When the CNTs:Fe3O4 ratio is 50:50, nano-Fe3O4 has an excellent synergistic effect with the CNTs hybrid filler, and the EMI SE can be as high as 40.6 dB. Also, the ratio of electromagnetic hybrid filler was altered, and electromagnetic wave absorption was impacted by this change. At maximum absorption (40.3%), the SEtotal of the 25C75F composite remains 24.6 dB, which complies with commercial requirements. Therefore, the results of this study indicate that incorporating magnetic nanofillers and conductive fillers in PLA composites can significantly enhance their electromagnetic wave absorption capacities and EMI shielding properties without significantly affecting their mechanical properties and thermal properties stability.

  1. Funding information: This work was financially supported by the National Natural Science Foundation of China (52173086, 52173046, 51873193, and 51803062) and the Natural Science Foundation of Zhejiang Province (LZ21E030002).

  2. Author contributions: Bozhen Wu: formal analysis, funding acquisition, methodology, resources, and supervision; Honghao Zhu: data curation, formal analysis, investigation, and writing – original draft; Yuhao Yang: investigation; Jiang Huang: investigation; Tong Liu: formal analysis; Tairong Kuang: conceptualization, data curation, formal analysis, funding acquisition, investigation, supervision, writing – original draft, and writing – review and editing; Shaohua Jiang: supervision and writing – review and editing; Aleksander Hejna: formal analysis and writing – review and editing; Kunming Liu: formal analysis. All authors have read and agreed to the published version of the manuscript.

  3. Conflict of interest: One of the corresponding authors of this article (Shaohua Jiang) is an Associate Editor of e-Polymers.

  4. Data availability statement: Data are available from the authors on request.

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Received: 2023-01-28
Revised: 2023-02-21
Accepted: 2023-02-28
Published Online: 2023-04-01

© 2023 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  51. Preparation and characterization of polymeric cross-linked hydrogel patch for topical delivery of gentamicin
  52. Mechanical properties of rCB-pigment masterbatch in rLDPE: The effect of processing aids and water absorption test
  53. Pineapple fruit residue-based nanofibre composites: Preparation and characterizations
  54. Effect of natural Indocalamus leaf addition on the mechanical properties of epoxy and epoxy-carbon fiber composites
  55. Utilization of biosilica for energy-saving tire compounds: Enhancing performance and efficiency
  56. Effect of capillary arrays on the profile of multi-layer micro-capillary films
  57. A numerical study on thermal bonding with preheating technique for polypropylene microfluidic device
  58. Development of modified h-BN/UPE resin for insulation varnish applications
  59. High strength, anti-static, thermal conductive glass fiber/epoxy composites for medical devices: A strategy of modifying fibers with functionalized carbon nanotubes
  60. Effects of mechanical recycling on the properties of glass fiber–reinforced polyamide 66 composites in automotive components
  61. Bentonite/hydroxyethylcellulose as eco-dielectrics with potential utilization in energy storage
  62. Study on wall-slipping mechanism of nano-injection polymer under the constant temperature fields
  63. Synthesis of low-VOC unsaturated polyester coatings for electrical insulation
  64. Enhanced apoptotic activity of Pluronic F127 polymer-encapsulated chlorogenic acid nanoparticles through the PI3K/Akt/mTOR signaling pathway in liver cancer cells and in vivo toxicity studies in zebrafish
  65. Preparation and performance of silicone-modified 3D printing photosensitive materials
  66. A novel fabrication method of slippery lubricant-infused porous surface by thiol-ene click chemistry reaction for anti-fouling and anti-corrosion applications
  67. Development of polymeric IPN hydrogels by free radical polymerization technique for extended release of letrozole: Characterization and toxicity evaluation
  68. Tribological characterization of sponge gourd outer skin fiber-reinforced epoxy composite with Tamarindus indica seed filler addition using the Box–Behnken method
  69. Stereocomplex PLLA–PBAT copolymer and its composites with multi-walled carbon nanotubes for electrostatic dissipative application
  70. Enhancing the therapeutic efficacy of Krestin–chitosan nanocomplex for cancer medication via activation of the mitochondrial intrinsic pathway
  71. Variation in tungsten(vi) oxide particle size for enhancing the radiation shielding ability of silicone rubber composites
  72. Damage accumulation and failure mechanism of glass/epoxy composite laminates subjected to repeated low velocity impacts
  73. Gamma-ray shielding analysis using the experimental measurements for copper(ii) sulfate-doped polyepoxide resins
  74. Numerical simulation into influence of airflow channel quantities on melt-blowing airflow field in processing of polymer fiber
  75. Cellulose acetate oleate-reinforced poly(butylene adipate-co-terephthalate) composite materials
  76. Radiation shielding capability and exposure buildup factor of cerium(iv) oxide-reinforced polyester resins
  77. Recyclable polytriazole resins with high performance based on Diels-Alder dynamic covalent crosslinking
  78. Adsorption and recovery of Cr(vi) from wastewater by Chitosan–Urushiol composite nanofiber membrane
  79. Comprehensive performance evaluation based on electromagnetic shielding properties of the weft-knitted fabrics made by stainless steel/cotton blended yarn
  80. Review Articles
  81. Preparation and application of natural protein polymer-based Pickering emulsions
  82. Wood-derived high-performance cellulose structural materials
  83. Flammability properties of polymers and polymer composites combined with ionic liquids
  84. Polymer-based nanocarriers for biomedical and environmental applications
  85. A review on semi-crystalline polymer bead foams from stirring autoclave: Processing and properties
  86. Rapid Communication
  87. Preparation and characterization of magnetic microgels with linear thermosensitivity over a wide temperature range
  88. Special Issue: Biodegradable and bio-based polymers: Green approaches (Guest Editors: Kumaran Subramanian, A. Wilson Santhosh Kumar, and Venkatajothi Ramarao)
  89. Synthesis and characterization of proton-conducting membranes based on bacterial cellulose and human nail keratin
  90. Fatigue behaviour of Kevlar/carbon/basalt fibre-reinforced SiC nanofiller particulate hybrid epoxy composite
  91. Effect of citric acid on thermal, phase morphological, and mechanical properties of poly(l-lactide)-b-poly(ethylene glycol)-b-poly(l-lactide)/thermoplastic starch blends
  92. Dose-dependent cytotoxicity against lung cancer cells via green synthesized ZnFe2O4/cellulose nanocomposites
https://doi.org/10.1515/epoly-2023-0006
Keywords for this article
multifunctional PLA nanocomposites; CNTs/Fe3O4 hybrid filler; electrical conductivity; EMI shielding
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BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Chitosan nanocomposite film incorporating Nigella sativa oil, Azadirachta indica leaves’ extract, and silver nanoparticles
  3. Effect of Zr-doped CaCu3Ti3.95Zr0.05O12 ceramic on the microstructure, dielectric properties, and electric field distribution of the LDPE composites
  4. Effects of dry heating, acetylation, and acid pre-treatments on modification of potato starch with octenyl succinic anhydride (OSA)
  5. Loading conditions impact on the compression fatigue behavior of filled styrene butadiene rubber
  6. Characterization and compatibility of bio-based PA56/PET
  7. Study on the aging of three typical rubber materials under high- and low-temperature cyclic environment
  8. Numerical simulation and experimental research of electrospun polyacrylonitrile Taylor cone based on multiphysics coupling
  9. Experimental investigation of properties and aging behavior of pineapple and sisal leaf hybrid fiber-reinforced polymer composites
  10. Influence of temperature distribution on the foaming quality of foamed polypropylene composites
  11. Enzyme-catalyzed synthesis of 4-methylcatechol oligomer and preliminary evaluations as stabilizing agent in polypropylene
  12. Molecular dynamics simulation of the effect of the thermal and mechanical properties of addition liquid silicone rubber modified by carbon nanotubes with different radii
  13. Incorporation of poly(3-acrylamidopropyl trimethylammonium chloride-co-acrylic acid) branches for good sizing properties and easy desizing from sized cotton warps
  14. Effect of matrix composition on properties of polyamide 66/polyamide 6I-6T composites with high content of continuous glass fiber for optimizing surface performance
  15. Preparation and properties of epoxy-modified thermosetting phenolic fiber
  16. Thermal decomposition reaction kinetics and storage life prediction of polyacrylate pressure-sensitive adhesive
  17. Effect of different proportions of CNTs/Fe3O4 hybrid filler on the morphological, electrical and electromagnetic interference shielding properties of poly(lactic acid) nanocomposites
  18. Doping silver nanoparticles into reverse osmosis membranes for antibacterial properties
  19. Melt-blended PLA/curcumin-cross-linked polyurethane film for enhanced UV-shielding ability
  20. The affinity of bentonite and WO3 nanoparticles toward epoxy resin polymer for radiation shielding
  21. Prolonged action fertilizer encapsulated by CMC/humic acid
  22. Preparation and experimental estimation of radiation shielding properties of novel epoxy reinforced with Sb2O3 and PbO
  23. Fabrication of polylactic acid nanofibrous yarns for piezoelectric fabrics
  24. Copper phenyl phosphonate for epoxy resin and cyanate ester copolymer with improved flame retardancy and thermal properties
  25. Synergistic effect of thermal oxygen and UV aging on natural rubber
  26. Effect of zinc oxide suspension on the overall filler content of the PLA/ZnO composites and cPLA/ZnO composites
  27. The role of natural hybrid nanobentonite/nanocellulose in enhancing the water resistance properties of the biodegradable thermoplastic starch
  28. Performance optimization of geopolymer mortar blending in nano-SiO2 and PVA fiber based on set pair analysis
  29. Preparation of (La + Nb)-co-doped TiO2 and its polyvinylidene difluoride composites with high dielectric constants
  30. Effect of matrix composition on the performance of calcium carbonate filled poly(lactic acid)/poly(butylene adipate-co-terephthalate) composites
  31. Low-temperature self-healing polyurethane adhesives via dual synergetic crosslinking strategy
  32. Leucaena leucocephala oil-based poly malate-amide nanocomposite coating material for anticorrosive applications
  33. Preparation and properties of modified ammonium polyphosphate synergistic with tris(2-hydroxyethyl) isocynurate for flame-retardant LDPE
  34. Thermal response of double network hydrogels with varied composition
  35. The effect of coated calcium carbonate using stearic acid on the recovered carbon black masterbatch in low-density polyethylene composites
  36. Investigation of MXene-modified agar/polyurethane hydrogel elastomeric repair materials with tunable water absorption
  37. Damping performance analysis of carbon black/lead magnesium niobite/epoxy resin composites
  38. Molecular dynamics simulations of dihydroxylammonium 5,5′-bistetrazole-1,1′-diolate (TKX-50) and TKX-50-based PBXs with four energetic binders
  39. Preparation and characterization of sisal fibre reinforced sodium alginate gum composites for non-structural engineering applications
  40. Study on by-products synthesis of powder coating polyester resin catalyzed by organotin
  41. Ab initio molecular dynamics of insulating paper: Mechanism of insulating paper cellobiose cracking at transient high temperature
  42. Effect of different tin neodecanoate and calcium–zinc heat stabilizers on the thermal stability of PVC
  43. High-strength polyvinyl alcohol-based hydrogel by vermiculite and lignocellulosic nanofibrils for electronic sensing
  44. Impacts of micro-size PbO on the gamma-ray shielding performance of polyepoxide resin
  45. Influence of the molecular structure of phenylamine antioxidants on anti-migration and anti-aging behavior of high-performance nitrile rubber composites
  46. Fiber-reinforced polyvinyl alcohol hydrogel via in situ fiber formation
  47. Preparation and performance of homogenous braids-reinforced poly (p-phenylene terephthamide) hollow fiber membranes
  48. Synthesis of cadmium(ii) ion-imprinted composite membrane with a pyridine functional monomer and characterization of its adsorption performance
  49. Impact of WO3 and BaO nanoparticles on the radiation shielding characteristics of polydimethylsiloxane composites
  50. Comprehensive study of the radiation shielding feature of polyester polymers impregnated with iron filings
  51. Preparation and characterization of polymeric cross-linked hydrogel patch for topical delivery of gentamicin
  52. Mechanical properties of rCB-pigment masterbatch in rLDPE: The effect of processing aids and water absorption test
  53. Pineapple fruit residue-based nanofibre composites: Preparation and characterizations
  54. Effect of natural Indocalamus leaf addition on the mechanical properties of epoxy and epoxy-carbon fiber composites
  55. Utilization of biosilica for energy-saving tire compounds: Enhancing performance and efficiency
  56. Effect of capillary arrays on the profile of multi-layer micro-capillary films
  57. A numerical study on thermal bonding with preheating technique for polypropylene microfluidic device
  58. Development of modified h-BN/UPE resin for insulation varnish applications
  59. High strength, anti-static, thermal conductive glass fiber/epoxy composites for medical devices: A strategy of modifying fibers with functionalized carbon nanotubes
  60. Effects of mechanical recycling on the properties of glass fiber–reinforced polyamide 66 composites in automotive components
  61. Bentonite/hydroxyethylcellulose as eco-dielectrics with potential utilization in energy storage
  62. Study on wall-slipping mechanism of nano-injection polymer under the constant temperature fields
  63. Synthesis of low-VOC unsaturated polyester coatings for electrical insulation
  64. Enhanced apoptotic activity of Pluronic F127 polymer-encapsulated chlorogenic acid nanoparticles through the PI3K/Akt/mTOR signaling pathway in liver cancer cells and in vivo toxicity studies in zebrafish
  65. Preparation and performance of silicone-modified 3D printing photosensitive materials
  66. A novel fabrication method of slippery lubricant-infused porous surface by thiol-ene click chemistry reaction for anti-fouling and anti-corrosion applications
  67. Development of polymeric IPN hydrogels by free radical polymerization technique for extended release of letrozole: Characterization and toxicity evaluation
  68. Tribological characterization of sponge gourd outer skin fiber-reinforced epoxy composite with Tamarindus indica seed filler addition using the Box–Behnken method
  69. Stereocomplex PLLA–PBAT copolymer and its composites with multi-walled carbon nanotubes for electrostatic dissipative application
  70. Enhancing the therapeutic efficacy of Krestin–chitosan nanocomplex for cancer medication via activation of the mitochondrial intrinsic pathway
  71. Variation in tungsten(vi) oxide particle size for enhancing the radiation shielding ability of silicone rubber composites
  72. Damage accumulation and failure mechanism of glass/epoxy composite laminates subjected to repeated low velocity impacts
  73. Gamma-ray shielding analysis using the experimental measurements for copper(ii) sulfate-doped polyepoxide resins
  74. Numerical simulation into influence of airflow channel quantities on melt-blowing airflow field in processing of polymer fiber
  75. Cellulose acetate oleate-reinforced poly(butylene adipate-co-terephthalate) composite materials
  76. Radiation shielding capability and exposure buildup factor of cerium(iv) oxide-reinforced polyester resins
  77. Recyclable polytriazole resins with high performance based on Diels-Alder dynamic covalent crosslinking
  78. Adsorption and recovery of Cr(vi) from wastewater by Chitosan–Urushiol composite nanofiber membrane
  79. Comprehensive performance evaluation based on electromagnetic shielding properties of the weft-knitted fabrics made by stainless steel/cotton blended yarn
  80. Review Articles
  81. Preparation and application of natural protein polymer-based Pickering emulsions
  82. Wood-derived high-performance cellulose structural materials
  83. Flammability properties of polymers and polymer composites combined with ionic liquids
  84. Polymer-based nanocarriers for biomedical and environmental applications
  85. A review on semi-crystalline polymer bead foams from stirring autoclave: Processing and properties
  86. Rapid Communication
  87. Preparation and characterization of magnetic microgels with linear thermosensitivity over a wide temperature range
  88. Special Issue: Biodegradable and bio-based polymers: Green approaches (Guest Editors: Kumaran Subramanian, A. Wilson Santhosh Kumar, and Venkatajothi Ramarao)
  89. Synthesis and characterization of proton-conducting membranes based on bacterial cellulose and human nail keratin
  90. Fatigue behaviour of Kevlar/carbon/basalt fibre-reinforced SiC nanofiller particulate hybrid epoxy composite
  91. Effect of citric acid on thermal, phase morphological, and mechanical properties of poly(l-lactide)-b-poly(ethylene glycol)-b-poly(l-lactide)/thermoplastic starch blends
  92. Dose-dependent cytotoxicity against lung cancer cells via green synthesized ZnFe2O4/cellulose nanocomposites
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