A review on graphene and graphene composites for application in electromagnetic shielding

Vol.:(0123456789) 1 3 Graphene and 2D Materials (2023) 8:59–80 https://doi.org/10.1007/s41127-023-00065-3 REVIEW ARTICLE A review ongraphene andgraphene composites forapplication inelectromagnetic shielding SvetlanaJovanović1· MiroslavHuskić2· DejanKepić1· MuhammadYasir3· KamelHaddadi4 Received: 7 September 2023 / Revised: 30 September 2023 / Accepted: 4 October 2023 / Published online: 18 October 2023 © The Author(s) 2023 Abstract As wireless solutions for communication, information, and sensing in modern society, electromagnetic waves (EMWs) have contributed considerably to the increase in the quality of people’s everyday lives. At the same time, EMWs produce electromagnetic pollution, issues with electromagnetic interference (EMI), and radio frequency (RF) signal leakage. These circumstances lead to high demand for efficient EMI shielding materials. To design an EMI shielding product, a compromise must be achieved between the electromagnetic shielding efficiency, the thickness of shielding materials, durability, mechanical strength, reduced volume and weight, and elasticity. Due to its ability to block EMWs, flexibility, lightweight, and chemical resistivity, graphene has been identified as a promising candidate material for efficient EMI shielding. Herein, we reviewed the studies that investigated various graphene-based composites as potential EMI shielding materials, with a focus on the composites based on graphene and silver nanowires due to their high EMI shielding efficiency, low production price, and favorable mechanical properties. Keywords Graphene· Graphene oxide· Silver nanowires· Composites· Electromagnetic interference shielding 1 Introduction The rapid development of technology led to a large number of electronic devices used in everyday life and professionally. Smartphones and various smart gadgets became inevitable parts of modern life. These changes make our life more comfortable. All these electronic devices emit electromagnetic waves (EWs) and lead to a new form of modern contamination, named electromagnetic pollution. EWs can cause serious issues as a result of electromagnetic wave pollution leading to electromagnetic interference (EMI), and information leakage. Devices that generate EMI are those that transmit, distribute, or use electric energy. When EWs penetrate between equipment joints, they can affect the performance of different devices, lead to damage to instrument components, and eventually reduce the device’s lifetime. EMI could also be dangerous for people with pacemakers and implantable cardioverter–defibrillators (ICDs) [1–3]. Particularly important is professional exposure to radiofrequency (RF) electromagnetic fields. Power plant workers, those operating on medical instruments, workers in the metal industry, on welding machines, and in telecommunication are exposed to this type of electromagnetic field. Extremely low-frequency electromagnetic fields (ELF EMFs frequency < 300Hz) are ubiquitous. Surprisingly, their effects on living organisms are poorly understood and subjected to debate. Several studies linked the risk of childhood cancer, particularly leukemia, to ELF EMF exposure [4–7] and brain cancers such as glioma [4]. Chronic exposure leads to changes in neuronal activity, affects long-term potentiation in hippocampal CA1 region, and shows an inhibitory effect on the amplitude of long-term potentiation [5]. These changes indicated that ELF EMF affects learning and memory. Other studies associate ELF EMF with sleep quality, * Svetlana Jovanović svetlanajovano[email protected] 1 Vinča Institute ofNuclear Sciences-National Institute oftheRepublic ofSerbia, University ofBelgrade, P.O. Box522, 11000Belgrade, Serbia 2 Faculty ofPolymer Technology, Ozare 19, 2380SlovenjGradec, Slovenia 3 Carl Von Ossietzky Universität Oldenburg, 26111Oldenburg, Germany 4 CNRS, Centrale Lille, Univ. Polytechnique Hauts-de-France, UMR 8520 - IEMN - Institut d’Electronique de Microélectronique et de Nanotechnologie – Lille, Univ. Lille, 59650Villeneuve-d’Ascq, France 60 Graphene and 2D Materials (2023) 8:59–80 1 3 anxiety, and depression [6]. The study where 66 scientific publications were analyzed using a meta-analysis of observational studies in epidemiology (MOOSE) concluded that chronic exposure to EMFs elevated the risk for neurodegenerative diseases (amyotrophic lateral sclerosis and Alzheimer’s disease) by 10% [7]. Other studies showed that ELF EMFs induce stress reactions, causing morphological as well as physiological alterations in subjected organisms [8]. Occupational exposure to ELF EMFs was not connected to an increased risk of malignant lymphoma [9]. Jalilian etal. analyzed the cases of different lymphoma registered between 1961 and 2005 in Finland, Iceland, Norway, and Sweden, and the prevalence was similar to the population that was not exposed to ELF EMFs. While short-term exposure does not affect cortisol levels in humans [10, 11], its secretion pattern is changing and it is related to the field intensity in the case of long-term exposure [12]. As a major glucocorticoid hormone, cortisol level was followed in the blood of workers occupationally exposed for 1–20years. This study revealed a change in the cortisol secretory pattern. The suppressive effect of ELF EMFs on the levels of chromogranin A, a marker of neuroendocrine tumors and stress, was also reported [13]. Scientists are disagreeing regarding the effects on human health, due to a lack of clear cause–effect connection. But ELF EMF certainly contributes to ROS production and oxidative stress and many other diseases [14]. Thus, the need for materials that can protect people but also instruments from both EWs and interference is increasing along with technological development. Material with EMI shielding efficiency (EMI SE) of 20dB is appropriate for commercial applications. Thick and dense conductive materials are efficient in EMI shielding. A highly effective EMI shielding material is metal. But, metals in the form of foil or fibers are rigid, with poor elasticity, they are not transparent, not good for wearable applications, and they reflect EWs leading to further secondary EWs pollution. Another material is conductive polymer composites (CPCs), which are lightweight, have good sealability, are easy to mold, are relatively low cost, and have no magnetic interference [15–17]. Silicone rubber also showed a good EMI performance due to excellent highand low-temperature stability, weather, and chemical resistance [18, 19]. For the use in EMI shielding, the new material should be lightweight, thin, elastic, durable, flexible, chemically stable, economically acceptable, produced by eco-friendly procedure, and resistive to moisture, in order to be applicable in the space and aircraft industry, motor vehicles, portable and wearable electronic devices. One of the promising materials for EMI shielding is graphene, its derivates, and composites. Due to its flexibility, lightweight, electrical conductivity, and chemical resistivity, graphene attracted large attention as a shielding material [20]. Graphene was discovered by Geim and Novocelov using adhesive tape to mechanically exfoliate graphite and isolated graphene for the first time in 2004 and won a Nobel prize in 2010 for this discovery [21]. From high-quality graphene produced by chemical vapor deposition (CVD), electrochemically exfoliated graphite, to more defective graphene with poorer electrical conductivity produced by the reduction of graphene oxide, graphene showed different properties as well as cost. In this review, we will analyze graphene produced using different methods, and its composites for application in EMI shielding addressing the most promising approaches to achieve desired shielding efficiency (SE), considering both economic and ecological aspects of production. Due to the volume of the work published in the field of electromagnetic shielding, we restricted our study to graphene, considering the rising interest in this material in EMW shielding. This field has evolved drastically in the last decade, which creates a need for comprehensive but clear studies understandable for researchers across different fields. A large number of review papers are analyzing MXene, conductive polymers, and graphene-based composites, while only a few review papers explore graphene as EMI shielding material [22–24]. In contrast, this review paper focuses on the EMI shielding of graphene and connects its structural characteristics with measured SE, and to composites with silver nanowires which greatly contribute to the efficiency of graphene sheet to block EMWs. 2 EMI shielding EM shielding is based on reflection, absorption, and multiple reflections [25, 26]. Shielding efficiency describes how well materials block EMWs and it is expressed in decibels—dB. Higher values of dB mean that material is more efficient in EMI shielding. The commercial application requires a minimum SE of 20dB, which is equivalent to the blocking of 99% of incident EMWs. The total shielding efficiency (SET) of a material is the sum of reflection (SER), adsorption (SEA), and multiple reflections (SEMR) shielding. EMWs are characterized by power (P), electric (E), and magnetic field (H) intensities. Thus, SET is defined as the logarithmic ratio of the incident (Pi) to transmitted power (PT) of electromagnetic radiation according to the following relations (1) and (2): where I—indicated incident, R—reflected, and T—transmitted component of EWs [27]. The interaction of the EM waves in the collision with different EMI shielding materials (1) SE T=10 log P I PT =20 log E I ET =20 log H I HT (2) SET=SEA+SER+SEMR 61Graphene and 2D Materials (2023) 8:59–80 1 3 is described in Fig.1, where reflection, absorption, and multiple reflections are presented. Electrically conductive materials such as metals are mainly reflecting EWs when they hit the surface rich in electrons and the SER is related to the ratio between the conductivity (σ) and permeability (μ) of the material, according to Eq.3. While reflection is primary, the absorption of EMWs is a secondary mechanism of EM shielding. Materials with magnetic or electrical dipoles are candidates for absorption shielding which is related to the following equation: where d is the thickness, and α is the attenuation constant of the slab, respectively. For magnetic conductive materials, absorption is the dominant shielding mechanism and it is directly proportional to the permittivity of the materials [27]. The multiple reflection is the process during which EW undergoes multiple internal reflections due to inhomogeneity and occurs between the interface layers [28, 29]. This type of shielding is characteristic of thin materials and happens when EWs are trapped inside the boundaries of materials, where they have reflected again from one to another boundary. The SEMR can be calculated using the following expression: where d is the sample thickness and δ is the penetration depth. This type of shielding is observed in porous structures, where hollows in the internal structures become active (3) SE R=39.5 +10 log 𝜎 2f𝜋𝜇 ∝𝜎∕ 𝜇 (4) SE A=20 log d e 𝜎 =8.7d √ f𝜋𝜎 ∝d𝜎𝜇 ∝𝛼d (5) SE MR =20 log ( 1−e −2 d 𝛿 ) spots for the scattering of EMWs and make SEMR similar to the absorption of EMWs. The schematic presentation is shown in Fig.1b. The most desirable shielding mechanism is absorption, considering that EMWs in that case were not emitted back into the environment. The higher the dB level of EMI shielding effectiveness, the less energy is transmitted through the shielding material. In EMI shielding theory, when an EM wave impinges on a shielding material, the incident power is divided into reflected, absorbed, and transmitted power and the corresponding power coefficients of absorbance (A), reflectance (R), and transmittance (T) are such that R + T + A = 1. The fraction of the absorbed EMWs is calculated from the previous equation, A = 1 − R − T. In a vector network analyzer (VNA), scattering parameters S11 (or S22) and S21 (or S12) are measured to calculate the reflectance and transmittance power coefficients, R = S112 and T = S122, and the absorbance is indirectly derived from A = 1 − R − T. Apart from these coefficients, to evaluate the efficiency of EMI shielding materials, the values of two more parameters were considered: specific EMI shielding effectiveness (SSE) and absolute effectiveness (SSE/thickness of material). In the recent past, graphene has become an interesting shielding material due to its electrical properties such as high electrical conductivity, and saturation velocity, good mechanical properties such as flexibility and strength, but also resistivity to corrosion and chemical reagents. Thus, in only the last 5years the interest in graphene as EMI shielding materials largely increased (Fig.2). Results of searching the Scopus database using keywords “electromagnetic interference shielding” and “graphene” showed that in 2022 was 262, while just 10years ago, the number of papers published with the same keywords was only 11. Fig. 1 Interaction of EMWs with materials, absorption, transmission, and multiple reflections (a). EW inside of lamellar materials (b), porous (c, d), and compact materials (e) 62 Graphene and 2D Materials (2023) 8:59–80 1 3 Composites based on graphene oxide and silver nanowires (AgNWs) were not explored widely as electromagnetic shielding material although they seem like a very efficient shielding material with good mechanical properties and chemical inertness. Table1 summarizes the morphology of graphene and AgNWs, electrical conductivity and sheet resistance, and EMI SE values for different composites. Results indicated that GO alone as well as in composite with AgNWs produces a good shielding barrier. In the further part, we are exploring structural properties as well as the mechanism behind the shielding effects of these nanomaterials. 2.1 Graphene andgraphene oxide, fromstructure andproperties toapplication inEMI shielding 2.1.1 Graphene analysis Graphene is a 2D nanomaterial composed only of C atoms that are sp2 hybridized. C atoms are organized in the 6-membered so-called benzene ring. Each atom is covalently bonded to three neighboring carbons, which leaves one unpaired electron per each C. Orbitals of these unpaired ones are overlapping creating a π-cloud above and over each ring, while in graphene, these clouds from each benzene ring create a unique cloud where electrons traveling freely. This structure makes graphene a unique material considering its electrical, mechanical, thermal, and chemical properties [46]. To study these mostly sp2 structures and their derivates such as graphene oxide, the most important techniques are Raman, Fourier Transform infrared, X-ray photoelectron spectroscopy, X-ray diffraction, and others [47–56]. Typical Raman, XPS, FTIR, and XRD spectra of graphene and its oxidized derivate, GO are presented in Fig.3. In the Raman spectrum of graphene (Fig.3a), the most intense band is the so-called graphitic or G band which stems from in-plane starching of sp2 bonded C atoms, it is located usually around 1585 cm−1 [57, 58], while the 2D band is the second-order overtone of the G band and its intensity and shape are related to the number of the graphene layers, as presented in the left part of Fig.3a showing deconvolution of 2D band and estimation of layers numbers [47]. In the Raman spectra of GO, an additional band around 1380 cm−1 is present (defect or D-band) and its intensity is correlated with defects in graphene structure such as edges, heteroatoms, vacancies, and Stone-Wale [59–62]. The ratio between the intensity of D and G bands (ID/IG) is proportional to the level of structural disorder and it is 0 for defect-free graphene and from 0 to above 2 for highly defective structures such as GO [62]. The shoulder bands in the Raman spectra of the GO locates around D and G bands can be identified by spectral deconvolution [50], and their position is dependent on the oxygen content in GO or reduced GOs, as presented in Fig.3b. Typical wide-scan XPS spectra of graphene oxide show peaks from C and O 1s [64–66], while analysis of those reveals the at% of each functional group in materials [48]. In Fig.3b, the removal of oxygen-containing function groups at different temperatures can be observed as an increase in at% of sp2 C atoms, and lowering of C–OH, C–O–C, C=O/ HO–C=O, and C=O, as well as the enhancement in the C/O ratio presented in the upper right corner. FTIR spectra are often used to identify the presence of functional groups, but it does not give quantitative data about their content [67, 68]. Band assign to carboxyl (–COOH) is usually around 1020 cm−1, epoxy (C–O–C) at 1243 cm−1, aromatic sp2 (C=C) at 1544 cm−1, 1627 cm−1 from carbonyl (C=O), and from hydroxyl (–OH) groups band is located at 3420 cm−1 [68]. XRD is a valuable tool to investigate graphene-like structures and one example is presented in Fig.3e. Graphite shows only one sharp peak at 2θ = 26.4° which corresponds to the (002) diffraction plane [69–71] and the lattice distance of 0.34nm. Oxidation leads to an increase in the interlayer distance due to layers exfoliation, water intercalation, and incorporation of functional groups on the basal plane of graphene sheets and this could be observed by shifting the peak to a lower angle, to 10.9° which corresponds to layer distance of 0.81nm [49]. When GO is reduced, the peak 2θ is shifting to higher angles, while declining in the interlayer distance could be used to follow the process of reduction as well. This can be seen in Fig.3e, where GO loses functional groups over time of the hydrothermal reduction treatment and the graphene structure has been partially restored. The morphology of the graphene and graphene oxide is usually studied using atomic force microscopy (AFM) which gives information about surface roughness, sheets size, sheets height, and profiles (Fig.4a–h) [72, 73]. By measuring the height of the sheet using AFM, the number Fig. 2 Results of the Scopus database on 1st February 2023, using TITLE-ABS-KEY “electromagnetic interference shielding” AND “graphene” 63Graphene and 2D Materials (2023) 8:59–80 1 3 of graphene layers could be estimated (Fig.4b, d) or it can show the surface roughness of the sheet which is usually related to functional groups (Fig.4g, h). Scanning electron microscopy (SEM) is used for the investigation of the cross section morphology of the standing films and the film thickness (Fig.4i, j) [74–76] but also for analysis of sheet morphology (Fig.4k, l) [77–79]. Transmission electron microscopy (TEM) is an inevitable tool for the analysis of sheets size, and layers numbers (Fig.4m, n, o) [80]. It even offers the possibility to investigate graphene structure at the atomic level and contributes to the estimation of the presence of defects such as vacancies (Fig.4n) or to study edges (Fig.4o). Apart from microscopic techniques, methods such as dynamic light scattering (DLS) [81] and zeta sizer are Table 1 Summarized results of various graphene-based nanomaterials, and their electrical (sheet resistance, R and electrical conductivity, σ), structural properties, and EMI SE a D is diameter, L is length Material Graphene or GO AgNWsaR or σStructure EMI SE Graphene oxide (GO) films [30]Hummer’s ≈ 1.1nm thick 1.2μm – 1000 S/cm XPS C/O 73.1; XRD: 26° (002), ID/IG 0.14 20dB Graphene oxide [31] Hummer’s Small SGO 1 μm2 Large LGO 23 μm2 –152 ± 7.5 S/cm XPS: C/O 1.79 (rSGO) to 6.75 (rLGO); ID/IG 0.9–1.4 XRD: (002) AgNW/cellulose papers [32]– Polyol D 19nm L 18μm 67.51 S/cm XRD: (101), (002), (111), (200), (220), (311) 48.6dB at 1GHz GO/AgNWs/GO films [33] Hummer’s D 15–35nm L 15–25μm 6.5 × 104 S/m XPS C/O: 9 Raman ID/IG 1.4 38dB at 8.4–12GHz PET/AgNWs/Graphene [34]CVD graphene D 90nm L 40μm 199.75 to 152.33 Ω/sq – – rGO/AgNWs composites on glass, textile fabric, and PET [35] High shear speed of expanded graphite 3–15 layers 10 to 30μm Polyol D 30–50nm L 30–50μm 6–24 Ω/sq XRD: (002), (111), (200), (004), (220) XPS O/C 0.041 contact angle: 129 – PET/AgNWs/GO/acrylic NP [36]0.5–5μm D 35–45nm L 5–15μm 34.8 Ω/sq Contact angle 86.3° 20dB (0.5–3GHz) GO/AgNWs composite [37]40μm D ~ 37nm L < 10μm 2.9 × 106 S/m density 2.9g/cm392dB for 2.9g/cm3, 32dB for 18μm on cotton G/GQDs/AgNP in PVDF [38]Improved Hummers XRD: (111), (200), (220), (311) 43dB at 8GHz GO/AgNWs/PDMS aerogel [39]Hummer’s Polyol 12.1 S/cm 34.1dB Polyurethane/GO/AgNW [40]D 20–25nm L 25–30μm 20dB PET/GO/AgNWs/Ag grids/PET [41]Polyol 1.6 Ω/sq Transparency 74.4% 42.9dB at 1.8GHz rGO/AgNWs aerogels [39] 5–8μm D 60nm L 20–30μm XPS C/O 6.6, ID/IG 1.6, XRD: (002), (111), (200), (220), (311) 45.2dB PMMA/graphene/metal mesh hybrid [42]5.53 Ω/sq 28.9dB at 12–18GHz AgNWs/GO [43] XRD: (002) GO, (111), (200), (100) 40.1dB AgNWs/GO [44]ID/IG: 1.1–0.7, XPS: O groups, XRD: 25–46nm 35.5dB Free-standing GO–AgNW composite [45]0.5–2μm size D 40nm L 20–45μm 1144.32 to 2255.8 S/cm Charge of GO: − 47.4, Ag NWs: + 16.2mV XRD: (001), (111), (200), (220), XPS C/O 0.33–0.37 55.16dB 66 779.66dB cm−1 64 Graphene and 2D Materials (2023) 8:59–80 1 3 particularly useful for investigating the average sheets size and charge of the GO in solution, respectively [82]. With numerous astonishing structural, chemical, physical, and mechanical properties, graphene attracted attention across various scientific fields [84–88]. Recently, the interest in its potential application in EMI shielding is growing. First, we will summarize the results regarding graphene, graphene oxide, and doped graphene, and after we will deal with composites with graphene and silver nanowires. 2.1.2 EMI shielding withgraphene‑based materials One of the first studies reporting the ability of the graphenebased composite to block EMW was published in 2009 [89]. Liang etal. produced a composite based on GO and epoxy polymer using an insitu polymerization. GO was produced using the modified Hummer’s method, followed by chemical reduction with hydrazine leading to the production of rGO. Then, the epoxy polymer was obtained directly on the Fig. 3 Raman spectra of graphene (a), reprinted with permission from Raman Studies of Monolayer Graphene: The Substrate Effect, by Yingying Wang, Zhen Hua Ni, Ting Yu, et al., The Journal of Physical Chemistry C, 112, 29, 10,637–10640. Copyright 2008 American Chemical Society [47], and graphene oxide (b) reprinted with permission from The Importance of Interbands on the Interpretation of the Raman Spectrum of Graphene Oxide by Sergi Claramunt, Aïda Varea, David López-Díaz, et al., 2015, 119, 18, 10,123–10129, Copyright 2015 American Chemical Society [51], XPS from (c and d) reprinted with permission from Probing the Thermal Deoxygenation of Graphene Oxide Using High-Resolution InSitu X-ray-Based Spectroscopies by Abhijit Ganguly, Surbhi Sharma, Pagona Papakonstantinou, etal., 2011, 115, 34, 17,009–17019, Copyright 2011 American Chemical Society [48], FTIR spectra of rGO and GO reprinted with permission from Controlled synthesis, characterization and reduction of graphene oxide: A convenient method for large-scale production by Tarko Fentaw Emiru, Delele Worku Ayele Egyptian Journal of Basic and Applied Sciences 4, 1, 2017, 74–79, Copyright Creative Commons Attribution-NonCommercial-NoDerivatives License (e) [50], and XRD spectra of graphite, GO and reduced GO at different condistion, reprinted from Structural Evolution of Hydrothermally Derived Reduced Graphene Oxide, Hsin-Hui Huang, K. Kanishka H. De Silva, G. R. A. Kumara, Masamichi Yoshimura, Scientific Reports, 8, Article, 6849 (2018) a under a Creative Commons Attribution 4.0 International License (f) [49] 65Graphene and 2D Materials (2023) 8:59–80 1 3 graphene surface and cured. rGO/polymer composite with 15 wt% of rGO had SE of 21dB in the frequency range between 8.2 and 12.4GHz (X-band). Another study proved the EMI shielding efficiency of graphene, where SE was 35dB in the frequency range of 0.1–15GHz [90]. They showed that the electrical conductivity of graphene could be tuned by electrostatic or magnetostatic bias revealing its potential application in EMI SE. The graphene monolayer produced using the CVD method showed a rather low EMI SE of 2.27dB, and the main shielding mechanism was concluded to be absorption [91]. The high sheet resistance of 635Ω/sq indicated that monolayers had a defective structure and showed very poor SE, while those with 2 and 3 layers showed SE of 4.13 and 6.91dB, respectively, in the frequency range of 2.2–7GHz. With the increase in graphene layer number, the absorption component is lowering while the refection one is increasing, which is similar behavior that was observed in thin metal films, such as Au film. Defect-free graphene was proven to be better in EMI SE than those with defects, while SE increases with the number of graphene layers [92]. When few-layer graphene was produced using the same method, the thickness of the graphene sample was 4nm, EMI SE was 19.1dB (18–26.5GHz), Fig. 4 AFM images of the graphene deposited on SiO2 support before and after thermal reduction (a–d) adapted under the terms of the Creative Commons Attribution 3.0 license, by Lene Gammelgaard, José M Caridad, Alberto Cagliani, David M A Mackenzie, Dirch H Petersen, Timothy J Booth, Peter Bøggild Graphene transport properties upon exposure to PMMA processing and heat treatments, 2D Materials 1 (2014) 035005. https:// doi. org/ 10. 1088/ 20531583/1/ 3/ 035005 [73], AFM images of unreduced (e, g) and reduced GO (f, h), adapted with permission from Langmuir 2009, 25, 10, 5957–5968. Copyright 2009 American Chemical Society [72]; SEM images of air-dried rGO (i) and vacuum-annealed rGO (j), adapted with permission from ACS Nano 2010, 4(7), 3845–3852, Copyright 2010 American Chemical Society [74]; SEM image of graphite flakes (k) and exfoliated GO sheets (l) under the terms of the Creative Commons CC BY license, Copyright © 2018, Samar Azizighannad etal., Stepwise Reduction of Graphene Oxide (GO) and Its Effects on Chemical and Colloidal Properties, Scientific Reports, 2018, 8, 10,083 [83]; high resolution-TEM images of GO (m, n, and o) adapted from adapted with permission from Nano Letters 2010, 10, 4, 1144–1148 by Cristina Gómez-Navarro, Jannik C. Meyer, Ravi S. Sundaram, etal. Copyright 2010 American Chemical Society [80] 66 Graphene and 2D Materials (2023) 8:59–80 1 3 and transmittance was 80.5% [93]. With an increase in the electrical conductivity of graphene, i.e., multilayered graphene, a higher electrical conductivity was achieved as compared to monolayer graphene leading to higher reflection and vice versa. But, due to restrictions in the size of CVD-produced graphene, this method is inappropriate for transfer to large-scale, technically complicated, and uneconomical, thus other approaches must be considered. Graphene for application in EMI shielding is usually produced as a bulk material, using Hummer’s method in the form of graphene oxide followed by reduction. The schematic presentation of the single-layered graphene structure and EM shielding is presented in Fig.5. Due to the presence of the discontinuities in the π-cloud, EWs are able to pass through graphene, while a part of the waves is absorbed are absorbed and converted into heat. In the case of a few-layer graphene, better shielding efficiency could be explained by multiple absorptions of the transmitted waves, as presented in Fig.6. When GO films were fabricated by direct evaporation of GO suspension under mild heating, it was noticed that the material possess a high EMI SE [30]. Ultrathin GO films (8.4μm) were annealed at 2000°C and showed excellent EMI shielding effectiveness of 20dB and high in‐plane thermal conductivity of 1100W m−1 K‐1. The material had excellent mechanical flexibility and structural integrity during bending, indicating that the graphitization of GO film could be considered a new alternative way to produce excellent EMI shielding material. Chemically reduced graphene thin film had a similar EMI SE, of around 20dB [31]. GO flakes were obtained by Hummer’s method and separated into large (LGO, with a surface area of 23 μm2) and small GO flakes (SGO, area 1μm2) by centrifugation. Free-standing films were produced Fig. 5 Schematic presentation of single-layer graphene structure with indicated covenant bonds and π-cloud, and defect in graphene structure and the faith of EMW when they hit its surface, reflection, transmission, and absorption from top (left) and side view (right) Fig. 6 Schematic presentation of multilayer graphene the faith of EMW when they hit its surface, reflection, transmission, and absorption of EMWs 67Graphene and 2D Materials (2023) 8:59–80 1 3 by vacuum deposition, while film thickness was controlled by changing the volume of GO dispersion. Using HI vapor, the chemical reduction was achieved and rLGO and rSGO were produced. The film thickness was from 7.5 to 10μm. XPS analysis showed that the ratio C/O was 1.56 and 1.79 for SGO and LGO, and it increased to 5.25 and 6.75, respectively, after the reduction. Structural disorder of GO is usually estimated using Raman spectra analysis where the ratio between D and G bands is proportional to defects in graphene structure [61, 93]. In this case, the ID/IG peak intensity ratios were 0.93, 0.90, 1.40, and 1.35, corresponding to SGO, LGO, rSGO, and also rLGO films. These values are considered relatively high meaning that in the graphene structure defects are present. XRD showed a 2θ peak of graphite sharply appearing at 26.71°, indicating a d-spacing of 3.34Å, while the shift of 2θ peak from 10.39° (SGO) to 26.0° (rSGO) and from 10.7° (LGO) to 26.14° (rLGO) suggest the reduction. With the increase in GO sheets size, drastic enhancement in both electrical (243 ± 12 S cm−1) and thermal conductivity (1390 ± 65 W m−1 K−1) was detected. Total EMI shielding effectiveness of both rSGO and rLGO thin films in L and S bands (300MHz–4GHz) frequency range with various thicknesses: • 3μm shows EMI SET values of ∼ 4.5 and 6dB for rSGO and rLGO, • 7.5μm reaches up to ∼ 15dB for rLGO film and ∼ 12dB for rSGO film at 1GHz, • two films of 7.5μm thicknesses together (total thickness ∼ 15μm):∼ 20.2dB (rLGO) and ∼ 17dB (rSGO). EMI SE value increases with the film thickness. This indicates that not only electrical conductivity but also the thickness of the shielding materials plays a key role in EMI shielding efficiency. For rLGO of thickness ∼ 15μm, SET, SER, and SEA were measured to be ∼ 20.2, 5.55, and 14.65dB, respectively. A similar trend was found for rSGO with smaller sheets, where SET, SER, and SEA were ∼ 16.7, 5.42, and 11.28dB, respectively. These results suggest that graphene films have both reflective and absorptive characteristics to electromagnetic radiation; with absorption as the dominant shielding mechanism. But also, these results indicate that sheet size does not play a key factor in the EMI shielding of graphene. The graphene pellet was produced in the CVD procedure and analyzed as a free-standing film for EMI shielding [94]. The thickness of the film was 50μm, electrical conductivity was 1136 S/cm, and EMI shielding efficiency was 60dB. For graphene paper, EMI SE was between 53 and 55dB [95]. The material was obtained using five-stage process, from graphite thermal exfoliation at 1150°C, sonication, vacuum filtration, thermal annealing (up to 450°C), and mechanical compression (5MPa). The conductivity of 443 S/cm was achieved and reached 1435S/cm after compression. In another study, GO flakes in three different sizes (5–8μm, 20–30μm, and 40–50μm) were used to obtain GO free-standing films [96]. The reduction was achieved by thermal treatment at 2600°C, and samples were mechanically compressed at 300MPa maximal. The highest SE was measured for the film prepared from the largest GO flakes (73.7dB) and it was noticed that mechanical compression leads to lowering the EMI SE. This phenomenon was explained by pore crashing. Namely, in free-standing graphene films, insulated air pores and graphene walls are present. When the incident EMWs hit the interference between graphene and air pore, one portion of EMW is transmitted while the other is reflected, and multiple reflections and transmissions are repeated infinitely between graphene walls in the lamellar structure of free-standing films. But after compression, the distance between the wall in pores is lowered which leads to destructive interference of EMWs. One more study investigated free-standing graphene films [97]. Herein, GO was first obtained using chemical exfoliation of graphite using sodium perborate (BH8NaO7) and concentrated H2SO4. Vacuum filtration followed by mechanical compression (20MPa) was used to obtain graphene film. Graphene with low defect and low O content (1.8–2.6 at%) was produced. Very thin free-standing films of 1.6 and 3.2μm showed astonishing EMI SE of 33 and 68dB, respectively. This is a record shielding efficiency compared to the sample thickness. The main shieling mechanism was absorption. Figure7 presents the structure of GO with indicated defects such as wholes and O-functional groups, as well as the interaction with EMWs and absorption. With the doping of graphene sheets, the EMI SE was largely improved [98]. Herein, researchers selected large graphene sheets, doped them with iodine, and produced free-standing films with a remarkable EMI SE of 52.2dB, when the sample thickness was only 12.5μm. Using GO dispersion, free-standing films were obtained by vacuum filtration, and annealed at 1600°C in Ar atmosphere, followed by expositing to I2 vapor at 200°C to incorporate I atoms in the graphene structure. Apart from EMI shielding efficiently, the material showed astonishing electrical conductivity of 1.05 × 105S/cm. Also, when graphene was doped with only 1.95 at% of S atoms, produced free-standing films showed the EMI shielding efficiency of 38.6dB [99], and around 33.2dB for graphene doped with 5.6wt% of sulfur [100], and for ultrathin films with nitrogen (7.89at%) SE was 58.5dB [101]. This remarkable increase in the EMI SE was explained by the increase in the electron density in the graphene π-cloud, as can be observed in Fig.8, where S-, N-doped GO was presented. Although heteroatoms increase structural disorder, if they have higher electronegativity or are incorporated into the graphene structure 74 Graphene and 2D Materials (2023) 8:59–80 1 3 1. AgNWs colloid deposited on support followed by on-top synthesis of graphene using CVD [34], 2. AgNWs colloid and GO dispersion mixed in different volume/mass ratios [33, 35, 37], 3. wet-coating of AgNWs on PET support followed by a coating of GO dispersion [36], 4. aerogel of GO flakes and polyol-synthesized AgNWs backfilled with PDMS [39], 5. synthesis of AgNWs on supports by electroless depositing techniques followed by GO electrodeposition [44], 6. vacuum filtration to achieve layer-by-layer self-assembly of GO and AgNWs [45], 7. aerogel was obtained by GO water dispersion mixing with AgNWs followed by reduction [142], 8. in situ synthesis of AgNWs on GO flakes by hydrothermal route [144]. Due to simplicity, the quick establishing of the interactions between GO and AgNWs, the possibility to produce the composite at a large scale, processability, and the ease of control of the content of each component of the composite, the method listed under 2 is mostly used in AgNWs-GO preparation. Thanks to excellent flexibility, transparency, processability, and a high EMI SE, these films showed great promise in various applications, from instrument protection, car, and other vehicles industry, to the application textile industry. 3 Conclusion Graphene and its composites are being increasingly studied as EMI SE materials. With the development of synthetic methods and possibilities to modulate graphene structure, EMI shielding efficiency is getting higher. The mass-scale production of graphene requires it to be both cost-effective and ecologically friendly. Most of the recent studies performed in recent times considering graphene for shielding applications involve the production of graphene with either the Hummers method or the CVD method. It seems that the electrochemical exfoliation of graphite for graphene production has great potential and many advantages for example due to avoidance of chemical use, mild conditions, simplicity as well as the potential to be transferred to a large scale. Various possibilities to doped graphene structure from heteroatoms to functionalization with electron-donating functional groups lead to improvements in the electrical conductivity of this material as well as its EMI SE. In the future, the development of new, green approaches for graphene doping, such as hydrothermal approach, microwave or laser-induced doping, or gamma irradiation could highly improve graphene EMI shielding behavior. Due to their chemical properties, AgNWs create complex easily with GO and highly improve electrical conductivity and EMI SE. However, they are not stable in the environments. Combining graphene or GO with AgNWs with different polymers is a promising strategy to produce commercial proactive cover against EMWs that are Table 2 EMI SE, sample thickness, and transparency of the sample a GNR-g raphene nanor ibbons b TCP-transparent cellulose paper Material SET (dB) Thickness Transparency (%) CVD graphene [91] 2.27 0.4nm 98.3 PEI/RGO [162] 6.36 20nm 62 Graphene/PMMA [163] 48% 800nm 97.8 Graphene/PET [92] 19.14 4nm graphene 80.5 Metal mesh/graphene [164] 14.1 – 97.3 graphene/metallic mesh/transparentdielectric 67.9 – 85 Graphene/metal network [42] 20.67 320µm 94 Acrylic polymer-coated/rGO/AgNWs [92] 24 – 85 Ni mesh/GO [165] 12.1 20nm 83 PVA GNRa—Fe3O4 [166] 16.36 – 79.8 Ti3C2Tx MXene-PU-AgNWs [167] 27.8 – 86 Epoxy/carbon nanotube sandwich [168] 23.4 6mm 0 Graphene mesh [169] 3.86 3–5 95 PDMS/AgNWs/TCP [169] 39.1 – 86.8 PET/AgNWs/rGO [170] 33.6 – 82 75Graphene and 2D Materials (2023) 8:59–80 1 3 efficient shielding materials, transparent, durable, stable, lightweight, and thin. Acknowledgements This work was supported by the EU, Horizon Europe program, Coordination and Support Action, project Twinning for new graphene-based composites in electromagnetic interference shielding—GrInShield (No. 101079151), and by the Ministry of Science, Technological Development and Innovation of the Republic of Serbia [Grant Number 451-03-68/2023-14/200017]. Also, the authors thank Ph.D. student A. Misovic for preparing figure1. Author contributions SJ wrote the main manuscript text, MH prepared sect.2.2.2, DK worked on sect.2.1, MY prepared sect.2, introduction part, and KH worked on sect.2., sect.2.2.2. All authors reviewed the manuscript. Declarations Conflict of interest The authors declare no competing interests. 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