Cite this article as: |
Bo-yu Ju, Wen-shu Yang, Qiang Zhang, Murid Hussain, Zi-yang Xiu, Jing Qiao, and Gao-hui Wu, Research progress on the characterization and repair of graphene defects, Int. J. Miner. Metall. Mater., 27(2020), No. 9, pp. 1179-1190. https://doi.org/10.1007/s12613-020-2031-2 |
Wen-shu Yang E-mail: yws001003@163.com
Gao-hui Wu E-mail: wugh@hit.edu.cn
Graphene has excellent theoretical properties and a wide range of applications in metal-based composites. However, because of defects on the graphene surface, the actual performance of the material is far below theoretical expectations. In addition, graphene containing defects could easily react with a matrix alloy, such as Al, to generate brittle and hydrolyzed phases that could further reduce the performance of the resulting composite. Therefore, defect repair is an important area of graphene research. The repair methods reported in the present paper include chemical vapor deposition, doping, liquid-phase repair, external energy graphitization, and alloying. Detailed analyses and comparisons of these methods are carried out, and the characterization methods of graphene are introduced. The mechanism, research value, and future outlook of graphene repair are also discussed at length. Graphene defect repair mainly relies on the spontaneous movement of C atoms or heteroatoms to the pore defects under the condition of applied energy. The repair degree and mechanism of graphene repair are also different according to different preparations. The current research on graphene defect repair is still in its infancy, and it is believed that the problem of defect evolution will be explained in more depth in the future.
Graphene is a unique 2D carbon material with a honeycomb-like lattice structure and delocalized electrons. In its ideal state, the material is highly valued by scientific researchers because of its extremely high strength [1], electrical conductivity [2], and thermal conductivity [3]. Because of its high performance, graphene could be added to a number of composites, especially metal matrix composites, to enhance their properties.
Graphene is widely used in Al matrix composites. Bastwros et al. [4] reported that compositing graphene with Al results in a maximum enhancement of 47% in flexural strength when compared with the reference Al6061. Zhang et al. [5] revealed that enhancements of 15.4% in thermal conductivity, 9.1% in specific heat capacity, 21.1% in hardness, and 25.6% in compressive strength could be achieved by adding 0.3wt% graphene to pure Al. The group’s experimental results further showed that graphene could greatly improve the overall performance of Al matrix composites. However, the properties of graphene-reinforced Al matrix composites were also directly related to the defects of graphene. Specifically, as the content of graphene defects increased, the load transfer enhancement effect of the material deteriorated and the performance of the composite materials decreased [6]. Al4C3 is a harmful phase for graphene-reinforced Al matrix composites. Xin et al. [7] and Liu et al. [8] reported that generation of Al4C3 could disrupt the interfacial bonding of C–Al, resulting in degradation of composite properties. Ci et al. [9] and Zhou et al. [10] found that Al4C3 is preferentially generated in defects of the graphene structure.
These previous findings indicate that developing methods to improve the load transfer ability and structural integrity of graphene and reduce the generation of Al4C3 is an important research direction.
Graphene defects are mainly divided into functional group defects and lattice defects. Functional group defects refer to flaws related to the oxygen-containing functional groups attached to the graphene surface; these functional groups include hydroxyl, carbonyl, and carboxyl groups, which are widely present in graphene oxide. The distribution of functional groups in graphene is unevenly island-like. Erickson et al. [11] observed that the isolated and complete sp2 structure of graphene is surrounded by a large number of sp3 regions disrupted by oxygen-containing functional groups. The presence of oxygen-containing functional groups could greatly reduce the conductivity of graphene, increase the thickness of single-layer graphene, change the interfacial structure of the material, and enhance its hydrophilicity.
Lattice defects are mainly manifested as hole and edge flaws in the graphene plane. The carbon atom in these defects is mainly sp3 carbon, which destroys the delocalized electronic distribution of the material and leads to the degradation of graphene performance.
Macroscopic characterization of graphene defects is mainly achieved through Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), infrared (IR) spectrometry, and conductivity performance testing. Microscopic characterization is mainly achieved through scanning tunneling microscopy (STM), atomic force microscopy (AFM), and transmission electron microscopy (TEM).
Raman spectroscopy is a reliable means of reflecting graphene defects. Raman spectra show four main peaks of graphene, namely, D, G, D + G, and 2D peaks; 2D peaks are also written as G′ peaks. The D peak appearing at approximately 1400 cm–1 reflects asymmetric lattice vibrations, while the G peak appearing at approximately 1500 cm–1 reflects symmetrical lattice vibrations; these peaks could be considered the characteristic peaks of sp3 and sp2 C, respectively. Many researchers use the intensity ratio of D peak and G peak (ID/IG ratio) to reflect the defect content of graphene. As the number of graphene layers increases, the position of the G peak redshifts [12‒13]. 2D peaks appearing at approximately 2700 cm–1 are related to the number of graphene layers, and the shape variety of the 2D peaks of graphene can be used to judge the number of layers (less than 5 layers). Wu et al. [14] systematically summarized the characteristics and physical significance of Raman peaks. Detection of the second-order Raman peak (2D peak) with a single Lorentz peak is a simple and effective method for determining single-layer graphene; multi-layer graphene has a 2D peak with multiple Lorentz peaks because of the splitting of the electronic band structure [15]. Because 2D peaks are redshifted when electrons are doped and blueshifted when holes are doped, Raman spectroscopy could be used to determine the doping type and concentration of graphene [16‒17]. Previous research used ID/IG and the intensity ratio of 2D peak and G peak (I2D/IG ratio) to reflect changes in defects, and the surface distribution of defects could be directly reflected by surface scanning [18], as shown in Fig. 1. The D + G peak at approximately 2960 cm–1 is related to the defect density and could reflect the defect content of graphene. In the Raman characterization of defective graphene, a unique D′ peak appears near 1620 cm–1. Eckmann et al. [19] found that this D′ peak is related to the defect type. For defects generated by sp3 C, the intensity ratio of D and D′ peaks (ID/ID′) is the highest at approximately 13. For gap-type defects, this ratio is approximately 7. Finally, for graphene edge-type defects, this ratio is the lowest at approximately 3.5.
Raman data could help estimate the defect distance (LD) [20‒21], defect density (nD) [22], and crystal size (La) [13‒23], all of which are useful to characterize the distribution of defects quantitatively. Raman spectroscopy could reflect the two states of the graphene defect distribution. When the average defect distance LD > 3 nm, sp2 C is the main form of C atoms and ID/IG increases as the defect density increases. When LD < 3 nm, a large number of defect structures are distributed on the surface of graphene and ID/IG decreases with increasing defect density.
XPS is a common surface analysis method that could accurately calibrate the valence and content of atoms by determining chemical shifts. It is often used in the field of graphene research to characterize the carbon/oxygen (C/O) ratio and carbon atom hybrid state of various materials, as shown in Fig. 2. Daukiya et al. [24], Hafiz et al. [25], Lesiak et al. [26], Dwivedi et al. [27], and Xie et al. [28] studied the binding energy of different carbon structures and concluded that the binding energy of sp2 C is approximately (284.4 ± 0.3) eV while the binding energy of sp3 C is approximately (285.2 ± 0.3) eV. Oxygen-containing functional groups could also be characterized by XPS. The binding energies of –OH, –C–C=O, and C=O are approximately 285.7, 287.5, and 288.7 eV, respectively [25]. IR spectroscopy is another method that can help characterize functional groups; it is widely used in graphene oxide reduction characterization [29].
STM and AFM are excellent means of characterizing the number of graphene layers. The thickness of graphene could reflect the number of graphene layers and surface functional groups. Generally speaking, the thickness of graphene is approximately 1 nm when single-layer graphene bears oxygen-containing functional groups on its surface. When no functional group is present on the surface of single-layer graphene, the thickness of the layer is close to the theoretical value of 0.34 nm. The thickness of single-layer graphene could be used to judge the effect of functional group defect repair. Rozada et al. [30] found that STM is appropriate for analyzing the defect repair mechanism of graphene. Because STM is highly sensitive to electrons, some structural defects not detected by AFM could be observed by atomic STM. TEM is also a useful tool to determine the structure of graphene [31]. Direct analysis of the number of graphene layers in composites through STM and AFM is difficult to achieve because the material of interest is dispersed in a matrix. TEM allows the direct observation of the structure of graphene in this case [29]. STM is more advantageous in analyzing the types of graphene defects. Rozada et al. [30] observed and analyzed hole defects on the surface of graphene by STM in Fig. 3.
The repair of functional group defects, especially oxygen-containing functional group defects, has been extensively studied. Several reducing agents, such as hydrazine hydrate [32], alcohols [33], and sodium borohydride [34], are used for thermal reduction. This reduction method has been widely used in the large-scale preparation of reduced graphene and could achieve the stable dispersion and surface modification of graphene sheets while eliminating oxygen-containing functional groups. However, the reducing agent cannot improve the integrity of the graphene skeleton structure, and new defects may be introduced during the reduction process. Therefore, further lattice defect repair is needed to obtain higher quality graphene.
Graphene lattice defects may be repaired in several ways. The major repair methods include chemical vapor deposition (CVD), doping, liquid-phase repair, external energy graphitization (such as high-temperature, microwave, and irradiation treatment), and alloying repair.
The CVD process mainly repairs holes through the decomposition of molecules in the gas or carbon source by plasma at high temperature. Because carbon atoms at the defect have higher activity than carbon atoms in other regions of graphene, the repair and growth of graphene holes and edges preferentially occurs [35]. The reaction temperature of CVD ranges from 500 to 1000°C, and the gas sources used mainly include methane [36‒37], hydrogen [18], ethylene [38], ethanol [39], and their plasma.
Zhu et al. [36] used H2 to assist CH4 in graphene repair and found that the latter could decompose at high temperatures to generate CHx (x = 1, 2, 3) plasma, which has high repair activity. Zhu et al. [36] used H2 to corrode the edges of graphene, promote the growth of new graphene, and inhibit the formation of sp3 C; the scholar observed excellent defect repair effects. Introduction of H2 could effectively reduce the temperature of the CVD process, reduce instrument requirements, and save experimental costs. Zhou et al. [40] explored whether CF4 could be connected with graphene-defective C atoms to form highly dispersive fluorinated GO (FGO) with a tunable atomic ratio of F/O (RF/O); the group discovered that RF/O could be readily manipulated by simply adjusting the reaction time.
López et al. [38] used conductivity and Raman experiments to characterize graphene defects and observed that the conductivity of graphene repaired by CVD is remarkably improved compared with the original material. This result confirms that the defects in graphene are carbon vacancies that could be filled by CVD. The ID/IG ratio determined by Raman spectroscopy was also greatly improved. It was due to the large mismatch between the lattice parameters of the newly grown CVD graphene and that of the original lattice structure. Lattice mismatches could cause defects leading to an increase of D peaks. Kim et al. [41] used CVD to grow graphene balls on a Ni surface and then applied graphene hollow spheres after Ni removal to repair defects, as shown in Fig. 4. The resulting material had an electrical conductivity of 18620 S/m and specific surface area of 527 m2/g.
During liquid-phase and doping repair, atoms are diffused into graphene defects in the liquid phase to achieve carbon atom-filled or heteroatom-doped graphene structures.
Cao et al. [42] intercalated ethanol molecules between graphene layers and performed heat treatment in a microwave environment. The authors found that the graphene layers separate during the decomposition of ethanol. The carbon atoms in ethanol were calibrated by means of isotope tracing. After treatment, the content of 13C atoms in the graphene structure remarkably increased, thereby proving that carbon atoms in ethanol enter the graphene lattice to repair its defects. The study also found that methanol does not repair the graphene via the same process. Under the experimental conditions, methanol could not be broken down similarly to ethanol to repair graphene defects. This work confirmed that the repair of graphene defects occurs on an atomic, rather than molecular, basis.
Tung et al. [43] used poly(1-vinyl-3-ethylimidazolium bromide) as a raw material to prepare an N-doped graphene structure. Subsequent TEM observation revealed that the repaired graphene has a large area and complete lattice structure. XPS confirmed N doping into the graphene lattice structure. Omidvar et al. [44] prepared GO/Pd, characterized the repair status of oxygen-containing functional groups by IR, and found that Pd doping redshifts the original functional groups. This result reflects an interaction between Pd atoms and graphene. A photoluminescence spectrum test revealed that the luminous intensity of GO/Pd is significantly higher than that of GO, which demonstrates an increase in the sp2 structure of the graphene and indirectly proves that Pd repaired the defects of the material.
The liquid-phase and doping repair processes have the advantages of simple equipment, high yield, and low cost. Because the process conditions of these methods are similar to those of the thermal repair process, they are often performed together in functional group repair. These methods are widely used in the large-scale reduction of graphene oxide. However, these two repair methods can only partially fill holes; they cannot achieve atomic diffusion and rearrangement in the defect area. Therefore, the theoretical strength of graphene repaired by these methods may be insufficient for some applications.
The high-temperature repair of graphene is a stable and reliable method for repairing lattice defects. The graphene structure could be graphitized through the self-diffusion of carbon atoms in a high-temperature (>2000°C) environment, and defects, such as holes, in the material could be repaired.
Xin et al. [45] prepared graphene sheet fibers under high-temperature conditions. Performance testing of the obtained graphene revealed an increase in thermal conductivity from 400 to 1300 W/(m·K) after heating and an increase in electrical conductivity from 0.8 × 10–5 to 2.2 × 10–5 S/m. Moreover, the tensile strength and Young’s modulus of the sample were greatly improved. The D peak of the samples treated at 2850°C could not be observed by Raman characterization, which proved that the graphene defects were basically eliminated at high temperatures. Ruan et al. [46] carried out graphene thermal repair research using electrochemistry and found that samples repaired at high temperature show high cyclic stability and low alternating current impedance. Raman spectroscopy and XPS further demonstrated the disappearance of graphene defects (Fig. 5).
Rozada et al. [47] used two-step heat treatment to perform graphene repair and conducted a detailed study on the thermal defect repair mechanism of graphene. Increasing the heat treatment temperature remarkably decreased ID/IG and greatly increased Lc, which is the crystal size calculated by XRD, and La, which is the crystal size calculated by Raman spectroscopy. The performance of the graphene treated at the highest temperature (HG1500-2700) was close to that of highly oriented pyrolytic graphite, and nearly all defects were repaired. Obvious stacking structures were found under high-resolution STM characterization, and a 3° difference between the angle of the stacked graphene and the original region was observed. These results suggest that graphitization of the graphene structure occurs via continuous and layer-by-layer crystallization.
Sun et al. [48] carried out research on Ni etching-assisted graphene thermal repair and found that Ni atoms are adsorbed around the saturated hydrocarbon structure and destroy the C–H bond to act as a catalyst and promote growth of graphene.
Besides traditional heating, irradiation and microwave heating could also be used to provide energy for graphene repair. Chen et al. [49] found that the interlayer spacing of GO decreases while that of amorphous C–C increased after electron-beam irradiation. Shi et al. [50], Xu et al. [51], and Zhang et al. [52] reported that γ-rays could etch the edge defects of graphene and promote the combination of graphene with metals or polymers to control edge defects. Restoration of the sp2 structure could also be achieved by γ-rays. Shi et al. [53] prepared a graphene-reinforced PVA material and characterized its properties. As the radiation intensity increased from 0 to 100 kGy, the tensile properties of the material gradually improved; 2D peaks were also observed in graphene. This finding indicated the repair of the lattice structure of graphene. Xu et al. [54] found that irradiation could cause graphene ID/IG values to increase, which could be beneficial to the large-scale functionalization of graphene. However, inappropriate irradiation conditions could also cause graphene defects to increase [55]. Voiry et al. [56] used microwave heating to repair the defects of graphene oxide (Mw-rGO). The repair effect of Mw-rGO was significantly higher than that of ordinary chemically reduced graphene and slightly lower than that of CVD-grown graphene and highly oriented pyrolytic graphite. These results showed that the microwave repair method has excellent repair effects. The original graphene structure was irregular, and oxygen-containing functional groups and holes could be found on the graphene surface; these characteristics affected the comprehensive performance of graphene. The repaired graphene had a very ordered lattice structure, and functional group defects and lattice defects were minimized. This excellent repair effect was attributed to the rapid heating of GO, which decomposes functional groups and rearranges planar atoms, during the microwave process.
High-temperature graphitization repair is one of the most effective methods for minimizing graphene skeleton defects and is suitable for repairing most carbon material structures. However, high temperatures also mean high instrument requirements, which limits the large-scale application.
Alloying repair is a special repair method applied to composite materials. The interface of composites is one of the key factors determining their strength, and matrix alloying can achieve the segregation of elements at the interface. In this repair method, segregated elements are spontaneously adsorbed on the surface of graphene to fill graphene defects and improve the interfacial bonding of graphene to the matrix.
Shao et al. [57] found that Mg is spontaneously enriched at the interface of the graphene-reinforced 5083 Al matrix, as shown in Fig. 6, to form the Mg@GNP structure. After adsorption of Mg on the surface of graphene, the production of Al4C3 was greatly reduced and the tensile strength of the composite material was improved. Guan et al. [58] studied Ni@graphene reinforced Al and found remarkable improvements in the mechanical properties of the composite material. Growing graphene on a metal matrix by CVD could also form the metal@graphene structure. Liu et al. [59] and Wang et al. [60] respectively prepared Ni@GNS/Al and Cu@GNS/Al via CVD. TEM clearly showed that Ni and Cu combine well with graphene. The mechanical properties of the CVD-grown graphene composites were much higher than those of the graphene-added composites. Because the CVD-grown graphene was covered by Ni and Cu elements, its lattice structure had high integrity. Complete graphene has a stronger load transfer effect and higher enhancement efficiency than defective graphene.
Fundamental differences may be observed between alloying repair and three other repair methods. Other repair methods mainly introduce foreign atoms or promote internal rearrangement of graphene to reduce defects and improve its integrity. However, alloying repair does not substantially reduce the number of graphene defects. Alloying repair is carried out by adsorption of alloying elements onto the graphene surface to fill defects and improve the integrity of the material as a whole. Thus, the performance of defective graphene repaired by alloying is close to that of complete graphene.
Defects have been reported to result in different behaviors at different temperatures. According to Bagri et al. [61] and Sun et al. [62], oxygen functional groups begin to decompose at low-temperature conditions (approximately 27–127°C), but some functional groups, such as carbonyl groups, could be converted into stable functional groups. Stable functional groups begin to decompose above 1300 K. When the functional groups on the graphene surface are thermally decomposed, the C atoms leave the graphene lattice in the form of CO and CO2, resulting in the generation of vacancies. C atom vacancies destroy the integrity of the graphene lattice, and generate graphene lattice defects.
The change process of graphene defects at high temperature is shown in Fig. 7. Rozada et al. [30] treated highly reduced, moderately reduced, and unreduced graphene at high temperature. The graphene structure of the non-reduced samples was greatly damaged after high-temperature treatment, and only small pieces of the original structure remained on the substrate. A large number of functional groups were present on the surface of unreduced graphene, and carbon atoms in the crystal lattice were eliminated during thermal decomposition; this modification caused great damage to the graphene structure. Moreover, the edges of the graphene sheet were smoother after heat treatment, which is the result of the high-temperature diffusion of carbon atoms. Two forms of hole defect movement occur during such diffusion, i.e., hole defects either merge together to form larger defects or move toward the edge and disappear.
Cao et al. [42] studied the graphene repair mechanism with a C source through 13C isotope tracer reaction. The repair process for hole defects is shown in Fig. 8. GO was rehabilitated with ethanol and methanol under a microwave environment. Ethanol and methanol were evaporated into a gas to reduce oxygen-containing functional groups on the surface and edges of GO. Ethanol was cracked into carbene radicals to heal the defects caused by radical–radical reaction with active carbon atoms from carbene. However, because methanol could not be cracked into carbene radicals and interact with the active carbon atoms at the edge of defect sites, some defects remained in the material. The results reveal that active atoms are a key factor in repairing the graphene lattice structure.
Given the rapid development of graphene-containing materials, interest in the effect of graphene defects on composite performance has steadily grown. The characterization and repair of defects has become a main focus of graphene research. Several approaches to repair graphene have been implemented, and graphene characterization technology is more and more advanced. However, two major problems in graphene research persist.
(1) Knowledge of the optimal process conditions for graphene repair is limited. Graphitization repair often requires extremely high temperatures. However, high temperatures exceeding 2000 K cannot be directly applied to composites and other fields because they could damage underlying structures. Although CVD repair and liquid phase repair require mild conditions, the process is complicated, and the repair effect is less than ideal. Alloying repair can be easily and directly applied to composite material systems, but the selection of elements has stringent requirements.
(2) Characterization of graphene in composite materials is difficult. Graphene added to composites cannot be characterized by AFM and STM. Although graphene could be removed by corrosion, the corrosion process could cause secondary damage to the material. Raman and XPS signals may be affected by the shielding and reflection effects of the base alloy in the matrix. Therefore, accurately characterizing the existence of graphene in a matrix is an important research direction.
High-quality few-layer graphene is expensive and obtained in low yields. If low-quality graphene could be repaired so that its performance resembles that of high-quality graphene, production costs would dramatically be reduced and the development of existing graphene products would be revolutionized. More research could result in effective methods for graphene repair and enhanced graphene performance.
This work was financially supported by the National Natural Science Foundation of China (Nos. 51871073, 51871072, 51771063, 61604086, and U1637201), China Postdoctoral Science Foundation (Nos. 2016M590280 and 2017T100240), Heilongjiang Postdoctoral Foundation (No. LBH-Z16075), and the Fundamental Research Funds for the Central Universities (Nos. HIT.NSRIF.20161 and HIT. MKSTISP. 201615).
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