| Cite this article as: |
Kunlan Diao, Yuhuan Xu, Jingyu Du, Teng Zhou, Xiao Zhan, Daohai Zhang, Xiaosi Qi, and Shuhao Qin, High toughness and strong electromagnetic shielding properties of PAM/PEG dual network hydrogels, Int. J. Miner. Metall. Mater., 32(2025), No. 3, pp.747-755. https://dx.doi.org/10.1007/s12613-024-3012-7
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With the wide application of electromagnetic wave, a high performance electromagnetic shielding material is urgently needed to solve the harm caused by electromagnetic wave. Complete cross-linking strategy is adopted in this paper. Polyacrylamide (PAM) was synthesized by in-situ polymerization of acrylamide (AM) monomer. The obtained PAM was blended with polyethylene glycol (PEG) to prepare PAM/PEG hydrogels and form rigid support structures. Subsequently, the modified carbon nanotubes (S-CNTs) were incorporated into sodium alginate (SA) and PAM/PEG. Finally, Na+ was used to trigger SA self-assembly, which significantly improved the mechanical properties and electrical conductivity of the hydrogels, and prepared PAM/PEG/SA/S-CNTs-Na hydrogels with high toughness and strong electromagnetic interference (EMI) shielding efficiency (SE). The results showed that the compressive strength of PAM/PEG/SA/S-CNTs-Na hydrogel was 19.05 MPa, which was 7.69% higher than that of PAM/PEG hydrogel (17.69 MPa). More encouraging, the average EMI SE of PAM/PEG/SA/S-CNTs-Na hydrogels at a thickness of only 3 mm and a CNTs content of 16.53wt% was 32.92 dB, which is 113.21% higher than that of PAM/PEG hydrogels (15.44 dB).
With the wide use of communication technology such as computer and mobile phone, people’s daily life and electromagnetic wave have been inseparable. Electromagnetic wave can quickly transmit information and energy, so it is widely used in electronic and electrical engineering, radio communication, medicine, military, and other fields [1–5]. However, electromagnetic wave brings convenience to our life but also brings a lot of harm. For example, the interweaving of different electromagnetic (EM) signals can cause signal distortion [6–7]. If the body absorbs harmful electromagnetic radiation, it will lead to cancer, mental disorders, fetal abnormalities, cardiovascular diseases, and other diseases [8–9]. Various EM radiation sources will cause environmental pollution. Therefore, the harm caused by electromagnetic radiation must be solved immediately, and the use of electromagnetic protective materials (including electromagnetic shielding materials and absorbing materials) to “cut off” the transmission path of electromagnetic waves can effectively protect sensitive objects from the impact of electromagnetic radiation, which is the main way to solve electromagnetic hazards.
Traditional metal materials (such as silver, copper, iron, nickel, and their alloys) are usually used as equipment shielding shells. However, metal-based materials have disadvantages such as poor thermal stability, high density, and high mechanical stress, which limit their application in electromagnetic shielding field [10–13]. Therefore, it is urgent to develop an advanced electromagnetic shielding material with easy machining, high mechanical flexibility, and high controllable electromagnetic shielding efficiency. Studies have found that hydrogel materials have arbitrary shape adaptability and self-healing ability [14–15]. Their internal contains rich water groups, can absorb electromagnetic waves, in addition, hydrogels are easy to fill other functional fillers for modification. Therefore, hydrogel materials have great application prospects in wearable electronic products, aerospace fields, and electromagnetic shielding fields. Polyacrylamide (PAM) is a kind of hydrophilic polymer that has been widely studied. Its internal crosslinking network contains reactive groups such as amide bonds, which is conducive to the formation of hydrogen bonds and the chemical modifications with various types [16–17]. However, PAM hydrogel itself lacks conductive and sufficient electromagnetic shielding properties. Therefore, it is necessary to incorporate relevant functional fillers to impart conductive and electromagnetic shielding ability. Yang et al. [18] incorporated multi-walled carbon nanotubes (MWCNT) into hydrophobic association PAM hydrogels, and cellulose nanofibers (CNF) were used as dispersants. The optimal tensile strength and conductivity of PAM/CNF/MWCNT composite hydrogels were 0.24 MPa and 0.85 s/m, respectively. The electromagnetic interference (EMI) shielding efficiency (SE) is 28.5 dB. On this basis, Lu et al. [19] used a simple strategy to prepare polypyrrole nanotube–polyethylene glycol–polyvinyl alcohol hydrogel (PPPg). When the prepared hydrogel was in the X-band and the thickness was 2 mm, the EMI SE could reach 21 dB. In addition, this film has excellent flexibility, with an elastic deformation of 100.9% at 2.28 MPa. In addition, Zhou et al. [20] prepared Fe3O4@RGO/PAM conductive hydrogel by using the hydrothermal synthesis method Fe3O4@RGO as the precursor. The conductivity of the hydrogel reaches 16.2 s/m at 3 mm thickness, and the maximum EMI SE is 27.1 dB. It has been found that although carbon nanotubes (CNTs) have been widely used because of their mechanical and electrical properties such as high specific structure, durability, and high electrical conductivity. Unfortunately, the accumulation of hydrophobic carbon nanotubes weakens the mechanical and electrical properties of hydrogels [21–22]. It is worth mentioning that the abundant oxygen functional groups (=O, −OH, and −COO−) in sodium alginate (SA) easily form hydrogen bond interactions with termination groups on the surface of CNTs, thus improving the interface mechanical properties between CNTs and SA [23–24]. In addition, it can bind to metal cations and induce SA self-assembly, resulting in greater internal density, which is conducive to the free movement of electrons. Therefore, it is often used as a biological material with a promising function or other materials doping.
In this paper, PAM/PEG/SA/S-CNTs-Na hydrogels with high toughness and strong EMI SE were prepared by a clever strategy of complete cross-linking. Firstly, acrylamide (AM) monomer was thermally induced free radical in situ polymerization to produce PAM, which was then mixed with polyethylene glycol (PEG) to form rigid PAM/PEG support structure. Secondly, the dispersion of CNTs was promoted after the functionalization of SA and hydroxyl (–OH) groups by non-covalent grafting. Then, anionic surfactant sodium dodecyl benzene sulfonate (SDBS) was used as modifier to inhibit the agglomeration of CNTs. Finally, the mechanical properties, conductance, and electromagnetic shielding properties of the hydrogel were significantly improved by SA self-assembly induced by Na+ immersion method.
As shown in Fig. 1, hydrogels of PAM/PEG, PAM/PEG/SA, PAM/PEG/SA/CNTs, and PAM/PEG/SA/S-CNTs were prepared by thermal initiated in-situ polymerization. Taking PAM/PEG/SA/S-CNTs hydrogel as an example, AM, SA, and PEG were first dissolved in deionized water to form a homogeneous solution, and then SDBS modified CNTs were added. After magnetic stirring for 1 h, CNTs were poured into a silica gel. PAM/PEG/SA/S-CNTs hydrogel was obtained after thermal polymerization at 70°C for 5 h. Then PAM/PEG/SA, PAM/PEG/SA/CNTs, and PAM/PEG/SA/S-CNTs hydrogels were immersed in saturated NaCl solution for 120 min, respectively. Na+-rich PAM/PEG/SA-Na, PAM/PEG/SA/CNTs-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels were obtained (see the Supplementary Information experiment section for details). For convenience, in some illustrations, samples are abbreviated as PAM/PEG (PPM), PAM/PEG/SA (PPS), PAM/PEG/SA/CNTsC(PPSC), PAM/PEG/SA/S-CNTs (PPSC-S), and PAM/PEG/SA-Na (PPS-Na), PAM/PEG/SA/CNTs-Na (PPSC-S-Na), and PAM/PEG/SA/S-CNTs-Na (PPSC-S-Na).
In order to study the microstructure of the prepared hydrogel, the morphology of the hydrogel after drying was observed by scanning electron microscope (SEM), as shown in Fig. 2(a)–(f). Compared with PAM/PEG/SA hydrogels (Fig. 2(a)), PAM/PEG/SA/CNTs hydrogels (Fig. 2(b)) have obvious pore structure and more obvious lamellar structure, but their material orientation is disorderly. On the contrary, when CNTs were modified by SDBS, the resulting hydrogels of PAM/PEG/SA/S-CNTs grew toward the lower right, and their structures were arranged in a regular manner (Fig. 2(c)). In addition, by soaking the hydrogel in 10wt% NaCl solution (Fig. 2(d)–(f)), the pore size of PAM/PEG/SA-Na hydrogel increased (Fig. 2(d)), which is due to the excessive Na+ inhalation, which expands the hydrogel and increases its pore size [25]. In Fig. 2(e) and (f), the PAM/PEG/SA/CNTs-Na and PAM/PEG/SA/S-CNTs-Na hydrogels has an obvious massive structure, and its morphology is like a coral reef. In addition, the element mapping image of PAM/PEG/SA/S-CNTs-Na hydrogel (Fig. 2(g)) shows a uniform distribution of C, N, O, and Na.
The FTIR spectral image of the hydrogel (Fig. 2(h) and (i)) shows that the prepared hydrogel has a C–C stretching band at about 1082 cm−1, and the characteristic peak formed is C–C stretching vibration in PAM. A characteristic peak was observed at around 1648 cm−1, which is due to the stretching vibration of C=O [26]. The tensile vibration of C–H is about 2881 cm−1. In addition, the tensile vibration peak of –OH is found at 3342–3394 cm−1 [27]. Among them, compared with PAM/PEG hydrogels, with the addition and modification of different substances, the absorption peaks of C–C and C–H bonds have different degrees of blue shift, and the absorption strength decreases, and the absorption peaks of O–H bonds have different degrees of red shift, and the absorption strength increases. However, the main components of the hydrogel cross-linked with Na+ did not form new absorption peaks, so no new substances were formed. However, the introduction of Na+ induced the self-assembly effect of sodium alginate, promoted the densification of the internal structure of the hydrogel, and caused certain changes in its structure, resulting in varying degrees of changes in the intensity of the absorption peaks (Fig. 2(i)).
XRD provides strong evidence for the existence of physical cross-linking in microregions. It can be seen from Fig. 2(j) that with the addition of SA, CNTs, and S-CNTs, the characteristic peaks of PAM/PEG at 36.34° gradually become smooth, and the strength of the characteristic peaks at 20.61° increase. Large characteristic peaks of PAM/PEG at about 22° can be clearly seen, and their peaks were 21.65°, 22.43°, and 22.43°, respectively. The results show that the introduction of SA, CNTs, and S-CNTs has significant effects on the crystallinity of PAM/PEG hydrogels, in which the introduction of SA has the greatest effect on the crystallinity of PAM/PEG hydrogels. Surprisingly, the introduction of Na+ resulted in many sharp characteristic peaks in PAM/PEG/SA-Na, PAM/PEG/SA/CNTs-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels (Fig. 2(k)), all of which crystallized similar to the XRD of NaCl (PDF #05-0628).
In order to further investigate the mechanical properties of hydrogels, the mechanical properties of PAM/PEG, PAM/PEG/SA, PAM/PEG/SA/CNTs, and PAM/PEG/SA/S-CNTs hydrogels were studied, and compression tests were carried out on the samples. As shown in Fig. 3(a)–(d), the compressive stress and ultimate strain of the hydrogels incorporated with SA, CNTs, and SDBS is significantly improved compared with that of PAM/PEG hydrogels. First, the presence of CNTs and S-CNTs causes entanglement and electrostatic attraction within the hydrogel [28–30]. Secondly, the self-assembly of SA induced by the introduction of Na+ improves the crystallinity of PAM/PEG/SA-Na, PAM/PEG/SA/CNTs-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels and densifies their internal structures [31]. These effects work together to provide a highly malleable support structure for hydrogels.
The PAM/PEG/SA/CNTs hydrogel had the highest compressive stress and ultimate strain and were 18.70 MPa and 48.86%, respectively, which is 5.6% and 21.8% higher than PAM/PEG hydrogel (Fig. 3(a) and (c)). As expected, the stress–strain of the hydrogels soaked in Na+ solution was improved (Fig. 3(b) and (d)), and the compressive stresses of PAM/PEG/SA/CNT-Na and PAM/PEG/SA/S-CNT-Na hydrogels increased to 19.18 MPa and 19.05 MPa, respectively. Compared with before Na+ immersion, the increase was 2.57% and 3.03%, respectively. Furthermore, it can be seen from Fig. 3(e)–(i) that PAM/PEG/SA/S-CNTs-Na hydrogels have good resilient deformation and recovery rate.
The electrical conductivity of PAM/PEG/SA and PAM/PEG/SA/S-CNTs hydrogels was characterized by light-emitting diode (LED)-assisted characterization techniques (Fig. 4(a)–(d). The incorporation of SA helps to improve the conductivity of hydrogel, which increases from 0.179 to 0.197 s/m (Fig. 4(e)). As expected, CNTs wound around each other to form a tightly connected conductive network, thereby increasing the conductivity to 0.204 s/m (Fig. 4(e)). Finally, PAM/PEG/SA/CNTs hydrogel were modified with SDBS to enhance their electrical conductivity up to 0.377 s/m (Fig. 4(f)).This is because the porous structure inside the PAM/PEG/SA/CNTs hydrogel was filled with a large amount of water, and the close packing of S-CNTs in the pore wall would bring about the volume exclusion effect, forming a better conductive path [30]. Surprisingly, with the introduction of Na+, PAM/PEG/SA-Na, PAM/PEG/SA/CNT-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels allow ions to move freely in their internal networks, moving in a directional manner in response to electric field forces, thus providing high electrical conductivity [32–33], and a brighter LED light is produced (Fig. S1, see the Supplementary Information). Their conductivities increased to 6.949, 6.988, and 7.794 s/m (Fig. 4(f)), which were 3427.411%, 3325.490%, and 1967.374% higher than that of hydrogels without Na+ solution, respectively.
Water content and swelling rate of hydrogels were calculated by Eqs. (S1) and (S2), and the results are shown in Fig. 4(g) and (h). The water content and swelling rate of PAM/PEG hydrogels (69.91wt% and 469.24wt%) were higher than those of PAM/PEG/SA, PAM/PEG/SA/CNTs, and PAM/PEG/SA/S-CNTs, which are 61.99wt% and 456.66%, 62.01wt% and 458.84%, 60.58wt% and 423.80%, respectively. The lowest water content was found in the modified PAM/PEG/SA/S-CNTs hydrogels, which is due to the agglomeration of S-CNTs, the decrease of hydrophilicity of S-CNTs, the cross-linking of hydrogels, and the entanglement and collapsing of their pores on the penetration of water molecules [34–35], which leads to the decrease of their water content and solubility, but they were all greater than 60wt% (Fig. 4(g)). Surprisingly, Na+ migration increased the water content and swelling rate of PAM/PEG/SA-Na, PAM/PEG/SA/CNTs-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels with 66.45wt% and 229.56%, 68.33wt% and 261.59%, 63.70wt% and 113.10%, respectively (Fig. 4(h)). However, the water content of the PAM/PEG/SA/CNTs-Na hydrogel with the highest water content in Na+ solution-soaked hydrogels (68.33wt%) is also lower than that of PAM/PEG hydrogel (69.91wt%).
Fig. 4(i) shows that although the PAM/PEG/SA/S-CNTs hydrogel has the smallest water content, its apparent density is the largest, and the water content of hydrogel is inversely proportional to its apparent density. Besides, comparing Fig. 4(i) and (j), it can be seen that the apparent densities of hydrogels were reduced to different degrees after under Na+ solution soak. This is because Na+ can better fill the void of the material, resulting in larger expansion of the hydrogel and lower density when Na+ solution is sucked into the solid hydrogel material [35]. Fig. 4(k) and (l) is the swelling curve of each hydrogel. It can be seen that each hydrogel absorbs water rapidly and expands in volume before 6 h of immersion. After 6 h, the swelling efficiency reaches saturation and the swelling curve tends to be flat. The swelling rate was obtained by calculating the mass of each hydrogel after 24 h.
On the basis of studying the conductivity of hydrogel, the electromagnetic shielding performance of hydrogel was further characterized. The EMI SE of hydrogels is shown in Fig. 5(a)–(f), and its change rule is consistent with that of electrical conductivity. The average total EMI SE (ηSE,T) of PAM/PEG hydrogel in the X-band (8.2–12.4Hz) was 15.44 dB (Fig. 5(e)), and the EMI SE of hydrogels mixed with SA, CNTs, and SDBS was improved Fig. 5(a) and (e). Among them, the average ηSE,T was increased to 16.79, 23.01, and 25.26 dB, respectively, as shown in Fig. 5(e), which basically meets the commercial requirements of 20 dB and achieves moderate electromagnetic interference [36]. As expected, with the introduction of Na+, the EMI SE of the prepared hydrogels was significantly improved (Fig. 5(b)), with the mean ηSE,T increasing to 23.80 dB, 28.89 dB, and 32.92 dB (Fig. 5(f)), respectively, 41.75%, 25.55%, and 30.32% higher than that of the hydrogels without Na+ solution. In order to clarify the electromagnetic shielding mechanism of hydrogel, the reflected EMI SE (ηSE,R), and absorbed EMI SE (ηSE,A) values of hydrogel materials are also given in Fig. 5(c) and (d). As can be seen from Fig. 5(c) and (d), ηSE,R remained relatively constant, but ηSE,A gradually increased with the incorporation of SA, CNTs, and SDBS. Moreover, with the introduction of Na+. This trend is also evident in Fig. 5(e) and (f). Fig. 5(g) and (h) shows that the absorption coefficient (A) is always high, while the reflection coefficient (R) is always low and decreasing, indicating that the main EMI mechanism of the prepared hydrogel is absorption rather than reflection (Fig. 5(i)).
In this study, after the introduction of SA molecules, they will dissociate into negatively charged ions in water, which will subsequently bind to Na+, promoting the self-assembly of SA. With the migration of Na+, the crystallinity of PAM/PEG/SA-Na, PAM/PEG/SA/CNTs-Na, and PAM/PEG/SA/S-CNTs-Na hydrogels also increased, and the molecules in the crystals were arranged tightly and neatly, which was conducive to ion transfer. Therefore, enhances the characteristics of the conduction path through crosslinking, reduces the resistance of impedance adaptation, so as to achieve effective magnetic field reflection and dissipation, so that electromagnetic shielding has been greatly improved [37–39]. In addition, with the addition of CNTs, an increasingly rich and continuous network provides more electron transport channels. In addition, since the conductivity of SA, CNTs, and S-CNTs hydrogels is inconsistent with that of PAM/PEG hydrogels, polarization loss can also be effectively improved [40–41]. Therefore, total EMI SE and absorbed EMI SE increase significantly due to these dopants enhancing the conductivity and polarization loss of the hydrogel.
In short, there are a lot of interfaces inside PAM/PEG/SA/S-CNTs hydrogels, and electromagnetic energy loss and dielectric loss will be absorbed and attenuated through the interface structure inside the hydrogels [42]. In addition, with the introduction of Na+, the formation of ion transfer channels is promoted, thus achieving the ideal electromagnetic shielding efficiency. In summary, PAM/PEG/SA/S-CNTs-Na hydrogel is an electromagnetic shielding material with an EMI SE of up to 32.92 dB, which is an absorption-based electromagnetic shielding material.
In this study, PAM/PEG/SA/S-CNTs-Na hydrogels with well mechanical strength and electromagnetic shielding properties were prepared by a simple one-bath method. Firstly, AM monomer is thermally induced in situ polymerization of free radicals to form PAM, and the resulting PAM is blended with PEG to prepare PAM/PEG hydrogels to form rigid support structures. Subsequently, SDBS modified S-CNTs were incorporated into SA and PAM/PEG, and finally Na+ was used to trigger the self-assembly of SA, which significantly improved the mechanical properties and electrical conductivity of the hydrogel. The compressive strength of PAM/PEG/SA/S-CNTs-Na hydrogel prepared was 19.05 MPa, and the electromagnetic interference efficiency was as high as 32.92 dB when the thickness was only 3 mm and the CNTs content was 16.53wt%. This innovative inorganic nanocomposite hydrogel material is cheap to manufacture, does not pollute the environment, and is easy to biodegrade, which may be a feasible solution to the problem of harmful electromagnetic waves.
This work was financially supported by the National Natural Science Foundation of China (No. 52163001), the Guizhou Provincial Science and Technology Program Project Grant, China (Qiankehe Platform Talents-CXTD [2021]005, Qiankehe Platform Talents-GCC [2022]010-1, Qiankehe Fuqi [2023]001, Qiankehe Platform Talents-GCC [2023]035, and Qiankehe Platform Talents-CXTD [2023]003), the Guizhou Minzu University Research Platform Grant, China (No. GZMUGCZX [2021]01), the Central Guided Local Science and Technology Development Funds Project, China (Qiankehe Zhong Yindi [2023]035), the Green Chemistry and Resource Environment Innovation Team of Guizhou Higher Education Institutions, China (Guizhou Education and Technology [2022]No. 13), and the Doctor Startup Fund of Guizhou Minzu University, China (No. GZMUZK [2024]QD77).
The authors declare no conflict of interest.
The online version contains supplementary material available at https://doi.org/10.1007/s12613-024-3012-7.
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