| Cite this article as: |
Zhaolin Li, Yaozong Yang, Jie Wang, Zhao Yang, and Hailei Zhao, Sandwich-like structure C/SiOx@graphene anode material with high electrochemical performance for lithium ion batteries, Int. J. Miner. Metall. Mater., 29(2022), No. 11, pp.1947-1953. https://dx.doi.org/10.1007/s12613-022-2526-0
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Silicon suboxide (SiOx, 0 < x < 2) is considered as one of the most attractive anode materials for high-energy-density lithium ion batteries (LIBs) because of its ultrahigh theoretical specific capacity (about 2600 mAh/g), low operating voltage (about 0.4 V vs. Li/Li+), rich natural resource, and environmental benignity [1–3]. However, its huge volume variation upon lithium uptake and release (about 160vol%) easily leads to particle fractures, resulting in continual structural deformation and eventually capacity loss of SiOx-based electrodes. In addition, the low intrinsic electric conductivity of Si seriously slows the electrode reaction kinetics and thereby reduces the capacity utilization. The two abovementioned drawbacks of SiOx severely hinder its further practical application in next-generation high energy density LIBs.
Tremendous efforts have been devoted to improving the structural stability and cyclic performance of SiOx-based materials. Nano-SiOx and SiOx–C materials are regarded as the most effective strategies to improve the electrochemical performance of SiOx according to the previous reports [4–9]. Nanosized particle can efficaciously release the structural stress induced during lithiation/delithiation process, resulting in the good structure durability of SiOx materials. However, the complex preparation and high manufacture cost of well-dispersed SiOx nanoparticles hinder the practical applications. Similar to other high-capacity electrode materials [10–12], compositing SiOx with carbonaceous materials is an effective and economic approach to improve the electrochemical performance of SiOx materials owing to the high electronic conductivity and relatively low-cost of carbon. Nevertheless, the continuous structure deterioration of SiOx causes the departure between SiOx and carbon, resulting in the loss of electric contact and thus fast capacity degradation of SiOx. In this case, the electrochemical performance of SiOx–C composite materials is still not satisfied to the commercial application in LIBs. Therefore, it is of great urgency to develop an effective approach to achieve a high-performance SiOx–C anode material so as to further boost the practical use of SiOx-based anode materials in high-energy-density LIBs.
Herein, we successfully prepared a C/SiOx@graphene material with a sandwich-like structure of C–SiOx–graphene via a facile and effective alcoholysis process at ambient temperature. Nanosized SiOx particles conformally distribute on graphene sheets, which is uniformly coated by amorphous carbon layers. Graphene sheets and amorphous carbon layer together construct a three-dimension (3D) electron transport network around SiOx, which homogenizes the local current density and ensures the uniform occurrence of electrode reactions on SiOx, thus resulting in the homogeneous volume variation and excellent structure stability of C/SiOx@graphene material. Moreover, Si–O–C bonds between SiOx and graphene guarantee the strong adhesion of SiOx particles on graphene sheets, which prevents the peeling and loss of electric contact of SiOx particles, thus ensuring the excellent structural durability of C/SiOx@graphene material during cycling. Owing to the structural advantages, the C/SiOx@graphene material presents an excellent cyclic performance (890 mAh/g after 100 cycles at current density of 0.1 C with capacity retention of 73.7%) and superior rate capability (~400 mAh/g at 5 C rate). This work provides a valuable exploration for development of high-energy-density lithium-ion batteries.
Graphene oxide (GO) was prepared by a modified Hummer’s method using natural graphite flasks (Alfa Aesar, Britain) as raw material. GO powder was calcinated at 700°C under Ar atmosphere to get reduced graphene oxide (rGO) without any oxygen-contained functional groups (Fig. S1). SiO2@rGO material was synthesized via a facile alcoholysis approach at ambient temperature. Typically, 300 mg GO powder was dissolved into 15 mL ethylene glycol (EG, Eg(OH)2 in Fig. 1(a)) with stirred for 2 h. Then, 5 mL silicon tetrachloride (SiCl4) was dropwise added into the GO solution under continuous stirring followed by 4 h stirring at room temperature. The obtained brown paste was put into oven to remove solvent at the temperature of 120°C, which was then calcinated at 500°C under flowing Ar atmosphere to obtain SiO2@rGO precursor material. Simultaneously, SiO2–rGO material was prepared with rGO powder instead of GO via the same approach.
SiO2@rGO precursor powder was mixed with NaCl and Mg under the mass ratio of 1:10:0.9 by hand-grinding in agate mortar. Then the solid mixture was loaded into SS 316 Swagelok-type reactors in an argon-filled glovebox (<0.1 ppm H2O, <0.1 ppm O2), followed by heating in a tube furnace at 650°C for 4 h under an Ar atmosphere. After cooling down to ambient temperature, the obtained powder was successively washed with 1 M HCl solution and deionic water and then vacuum-dried at 80°C to get SiOx@rGO precursor material. Meanwhile, SiOx–rGO material was prepared via the same magnesiothermic reduction process.
Sandwich-like structure C/SiOx@rGO material was synthesized by a chemical vapor deposition method. First, 1 g of SiOx@rGO powder was placed in a tube furnace, which was heated to 700°C at a temperature ramping rate of 5°C/min under an Ar gas flow. Then the gas flow was switched to acetylene/Ar mixture gas (10vol% diluted in Ar) for 30 min, when the temperature reached 700°C. Finally, the C/SiOx@rGO was collected after the furnace cooling down.
The particle morphology was observed by the field emission scanning electron microscopy (FESEM, Tecnai, SUPRA55, Germany) and transmission electron microscopy (TEM, FEI Tecnai, F20, USA). Phase structure was detected by the Raman spectroscopy (HORIBA Scientific LabRAM HR Evolution, Japan) and the X-ray diffraction (XRD, RIGAKU, Japan, D/max-A, Cu Kα, λ = 0.15406 nm). Fourier transform infrared spectroscopy (FTIR, Thermo Scientific Nicolet iS20, USA) was conducted to analyze the bond structures. X-ray photoelectron spectroscopy (XPS, PerkinElmer PHI 5000C ESCA system, USA) using the Mg Kα radiation was performed to characterize the electron binding energies.
The working electrodes were prepared with an active materials/carboxymethylcellulose (CMC)/acetylene mass ratio of 70:15:15. The prepared electrodes were assembled in 2032-type coin cells with lithium foil as counter electrode, porous polypropylene film (Celgard 2400) as separator, and 1 M LiPF6 in the mixture of ethylene carbonate (EC), diethyl carbonate (DEC), and dimethyl carbonate (DMC) with the volume ratio of 1:1:1 as electrolyte. The mass loading of the prepared electrodes was 1.5 mg/cm2. Galvanostatic discharge–charge tests were conducted on LAND CT2001A system (Wuhan, China) within the voltage range of 0.01–1.5 V vs. Li/Li+.
The schematic illustration in preparation process of SiOx
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SiCl4+3HOCH2−CH2OH→Si(OH)4+2ClCH2−CH2OH(l)+ClCH2−CH2Cl(g) |
(1) |
After 4 h stirring, the in-situ formed Si(OH)4 combined with GO sheets via hydrogen bonds, forming the Si(OH)4@GO composite. Meanwhile, with the proceeding of alcoholysis reaction, the terreous solution turned to a dark-brown paste as shown in the inset Fig. 1(a). Subsequently, the Si(OH)4@GO paste successively underwent a drying and calcination process, during which the dehydration reaction took place with the generation of Si–O–C bonds between SiO2 and GO sheets. The FESEM image of prepared SiO2@rGO shows that SiO2 nanoparticles (NPs) conformally distribute on graphene sheets (Fig. 1(b)), which is attributed to the bi-functional EG. On one hand, the EG serves as a reactant in alcoholysis reaction (Eq. (1)) with SiCl4 to form SiO2 NPs. On the other hand, the GO-anchored EG molecules act as templates to induce the formation of conformally-coating SiO2 NPs on GO sheets. On the contrary, the SiO2–rGO material synthesized with rGO sheets without any functional groups exhibits obvious particle aggregations with severely stacked graphene sheets and aggregated SiO2 NPs (Fig. 1(c)). Notably, the stacked graphene sheets are bared without any loaded SiO2 NPs, indicating the critical role of bi-functional EG on uniform distribution of SiO2 NPs on graphene sheets.
The SiOx@rGO was prepared via a modified magnesiothermic reduction process according to the Eq. (2).
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SiO2+(2−x)Mg→SiOx+(2−x)MgO |
(2) |
The FESEM image of SiOx@rGO material shows that it still maintains the laminar structure even after the exothermal magnesiothermic reduction (Fig. 2(a)). Moreover, the magnified image clearly presents the conformal distribution of SiOx NPs on graphene sheets (Fig. 2(b)), which is similar to that of SiO2@rGO (Fig. 1(b)). The excellent structural stability is attributed to the Si–O–C bonds existing between SiOx and rGO, resulting in the strong adhesion of SiOx particles on graphene sheets. After the carbon coating, the laminar structure in C/SiOx@rGO material is still preserved (Fig. 2(c)), which is in favor of the electrolyte penetration and rate capability. The larger particle size further indicates the carbon coating layer on SiOx particles (Fig. 2(d)). Moreover, the TEM image of C/SiOx@rGO material shows that SiOx nanoparticles with particle diameter of ~50 nm uniformly distribute on rGO sheets (Fig. 2(e)), which is agreed to the FESEM results. The high-resolution TEM image clearly presents a single SiOx particle with an outer amorphous carbon coating layer (thickness of ~2 nm) on surface, suggesting the C–SiOx–rGO sandwich-like structure (Fig. 2(f)).
In order to elucidate the chemical structures, Raman, FTIR, and XPS measurements were conducted and the related results are presented in Fig. 3. The Raman peaks of both SiOx–rGO and SiOx@rGO composites located at ~490 and 908 cm−1 are in excellent accordance with Si band (Fig. 3(a)) [13], which is agreed with the XRD results (Fig. S2). In addition, the peak centered at 417 cm−1 is assigned to the O–Si–O linkage, while the peaks situated at ~585, 685, and 785 cm−1 are associated with the Si–O–Si bonds [14–16]. More importantly, a significant blue-shifting Si–Si bond in the Raman spectrum of SiOx@rGO can be clearly observed, revealing the stronger Si–Si backbone due to the lower oxygen content in SiOx. Meanwhile, the lower peak intensity of O–Si–O and Si–O–Si bonds further demonstrate the lower oxygen content in SiOx of SiOx@rGO, which is attributed to a more sufficient magnesiothermic reduction arising from the full contact between Mg vapor and conformally-distributed SiO2 NPs on graphene sheets. The three bands at 1105, 883, and 471 cm−1 in the FTIR spectrum of SiOx@rGO material are assignable to Si–O–Si asymmetric stretching, symmetric stretching, and bending vibrations, respectively (Fig. 3(b)) [17]. It is noteworthy that the absorption peak centered at 1070 cm−1 is related to Si–O–C bond [18], which is in accordance with the alcoholysis reaction mechanism proposed in Fig. 1(a).
Fig. 3(c) and (d) presents the Si 2p XPS spectra of SiOx@rGO and SiOx–rGO materials, respectively. The two main broad peaks in the spectrum of SiOx@rGO composite can be fitted into four small peaks centered at 103.6, 102.3, 100.5, and 99.5 eV, which are associated with Si–O, Si–O–C, Si–C, and Si–Si bonds, respectively (Fig. 3(c)) [19–22]. With respect to the Si 2p spectrum of SiOx–rGO, it can be fitted into the small peaks of Si–O, Si–C, and Si–Si bonds (Fig. 3(d)). Intuitively, the peak intensity of Si–Si bond is much higher than that of Si–O bond in SiOx@rGO and the related average valence state of Si is estimated to be +2.6 (x = 1.3 in SiOx) based on the respective area of Si–Si and Si–O peaks. On the contrary, the peak intensity of Si–Si bond is much lower than that of Si–O bond in SiOx–rGO spectrum, corresponding to a higher average valence state of Si element (+3). The lower oxygen content is owing to the more sufficient magnesiothermic reduction of conformally-coating SiO2 NPs on graphene sheets in SiO2@rGO precursor, which is agreed with the blue shift in Raman result (Fig. 3(a)). Moreover, the Si–O–C peak centered at 102.2 eV in Si 2p spectrum (Fig. 3(c)), as well as the stronger peak of C–O/C–O–Si bonds centered at 532.8 eV in O 1s spectrum (Fig. 3(e)) [23], further indicates the existence of Si–O–C bridging bonds between SiOx NPs and graphene sheets in SiOx@rGO material. In addition, the peak situated at ~532 cm−1 is related to carbonyl groups originated from the residual oxygen-contained functional group on rGO [24]. Surprisingly, both the Si 2p XPS spectra of SiOx@rGO and SiOx–rGO show the weak peaks of Si–C bond at ~100.5 eV, which is associated with silicon carbide (SiC). This is consistent with the XRD result shown in the supplementary information (Fig. S2). The chemical reaction between ultrafine SiO2 particles and carbon carbonized from ethylene chlorohydrin (formed according to Eq. (1)) may be accounted for the formation of SiC.
The electrochemical measurements were performed based on a half-cell configuration using metallic lithium foils as counter electrodes. The galvanostatic charge/discharge profiles of SiOx@rGO electrode present an initial specific charge capacity of 1278 mAh/g and an initial Coulombic efficiency (ICE) of 74.8%, which are both higher than those of the SiOx–rGO electrode (1104 mAh/g and 67.9%). The higher electrochemical performance of SiOx@rGO electrode is beneficial from the more sufficient magnesiothermic reduction and therefore lower oxygen content in SiOx (Fig. 4(a)). With respect to the sandwich-like structure C/SiOx@rGO material, it delivers a reversible specific capacity of 890 mAh/g and an ICE of 47%. The relatively low ICE is ascribed to the amorphous carbon with pretty high irreversible capacity which can be evidenced by the much longer slope in the charge/discharge profiles of C/SiOx@rGO electrode. This low ICE can be addressed by employing prelithiation techniques in the future study [25–27]. Subsequently, the electrodes undergo a repeated galvanostatic cycling at the current density of 0.1 C within the voltage range of 0.01–1.5 V (Fig. 4(b)). Compared to SiOx–rGO, the SiOx@rGO electrode presents a relatively higher cyclic performance which is attributed to the Si–O–C bonds and thereby strong adhesion of SiOx NPs on graphene sheets. As for the C/SiOx@rGO, it delivered an excellent cyclic performance with a high capacity retention (73.7%) and Coulombic efficiencies in the repeated cycles, suggesting a physically and chemically stable solid electrolyte interface (SEI) film in C/SiOx@rGO electrode, which is owing to the well-designed sandwich-like C–SiOx–graphene structure.
Rate performance were tested at various current densities from 0.1 to 5 C (Fig. 4(c)). The C/SiOx@rGO electrode presents the reversible specific capacity of 946.7, 896.5, 830.1, 725.6, 596.8, 512.0, and 395.9 mAh/g at the current densities of 0.1, 0.2, 0.5, 1, 2, 3, and 5 C, respectively. With respect to the SiOx@rGO, it delivers a poor rate capability with a fast capacity decrease from 0.1 to 5 C due to the direct exposure of SiOx NPs to electrolyte. The related capacity retentions, calculated based on the capacity of the 3rd cycle at each current rate, are summarized in Fig. 4(d). Obviously, the C/SiOx@rGO electrode delivers a higher capacity retention than SiOx@rGO at each current rate, indicating a superior rate performance. In addition, the differential capacity versus potential (dQ/dV) curves at different current densities show that the anodic peaks of C/SiOx@rGO electrode present lower polarization than those of SiOx@rGO electrode with the increase of current rate (Fig. S3(a) and (b)). Moreover, the lithium ion diffusion coefficient is calculated to be 1.4 × 10−12 cm2/s according to the cyclic voltammetry (CV) curves at various scan rates (Fig. S3(c) and (d), detailed calculation seen in supplementary information) [28–29], which is much higher than that of pure SiOx (~10−14 cm2/s), suggesting a fast electrode reaction kinetics of C/SiOx@rGO material. When switching back to 0.1 from 5 C, the C/SiOx@rGO electrode presents a specific capacity of 886.3 mAh/g accompanying with a capacity recovery rate of 93.7%, and the capacity is well-maintained in the following cycles, revealing a robust structure of C/SiOx@rGO material even after ultra-fast charging/discharging process. The comparison of electrochemical properties suggests the high-level performance of C/SiOx@rGO material among the previously-reported SiOx–graphene composites (Table S1).
Based on the above discussions, the remarkable electrochemical performance in terms of excellent cyclic performance and superior rate capability is attributed to the well-elaborated sandwich-like structure in C/SiOx@rGO material. A schematic illustration of the structural evolution during lithiation/delithiation process is presented in order to intuitively understand the critical role of sandwich-like structure on electrochemical performance (Fig. 5). The structural advantages in C/SiOx@rGO material can be summarized as the following three aspects. First, the ultrafine SiOx particles, achieved by a facile and controllable alcoholysis process, can effectively resist the inner structural stress induced by large volume variation of SiOx, thus well-maintaining the structural integrity during lithiation and delithiation processes. Second, graphene sheets and amorphous carbon layer together construct a 3D conductive network for fast electron movement around SiOx NPs, which effectively homogenizes local current density and electrode reactions on SiOx, resulting in uniform volume variation and excellent structural durability of SiOx during the repeated cycles. Third, Si–O–C bonds between SiOx NPs and graphene sheets can strengthen the particle adhesion on graphene matrix, which prevents the peeling of SiOx NPs from graphene sheets and therefore structural deterioration. Owing to the synergetic effects of structural merits, the sandwich-like C/SiOx@rGO material shows a remarkable electrochemical performance in terms of excellent cyclic performance and rate capability.
Herein, we successfully fabricated a sandwich-like structure C/SiOx@rGO material via a facile and controllable alcoholysis process. In this well-engineered structure, a 3D highly-conductive network constructed by graphene sheets and amorphous carbon layer not only improves the electrode reaction kinetics of SiOx, but also ensures the uniform local current density and electrode reactions on surface of SiOx. Moreover, Si–O–C bonds existing between SiOx and graphene strengthen the particle adhesion on graphene sheets, enabling the outstanding structural integrity during charge/discharge process. Benefiting from the above structural merits, the C/SiOx@rGO material exhibits a remarkable electrochemical performance in terms of excellent cyclic performance and superior rate capability. The C/SiOx@rGO electrode delivers a reversible specific capacity of 890 mAh/g and a high capacity retention of 73.7% after 100 cycles at the current density of 0.1 C. In addition, a capacity of ~400 mAh/g at 5 C, as well as a nearly full capacity recovery when switching back to 0.1 C is achieved. The elaborate structural design sheds light on the future improvement of high-capacity electrode materials for lithium/sodium ion batteries.
This work was financially supported by the National Natural Science Foundation of China (Nos. 52102205 and U1637202) and the Fundamental Research Funds for the Central Universities (No. FRF-TP-20-048A1).
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
The online version contains supplementary material available at https://doi.org/10.1007/s12613-022-2526-0.
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| 4. | Kangzhe Cao, Sitian Wang, Yanan He, et al. Constructing Al@C–Sn pellet anode without passivation layer for lithium-ion battery. International Journal of Minerals, Metallurgy and Materials, 2024, 31(3): 552. DOI:10.1007/s12613-023-2720-8 |
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| 6. | Yu Zhang, Sheng Tian, Yongkang Zhang. A New Equalization Method for Lithium-Ion Battery Packs Based on CUK Converter. Energy Engineering, 2024, 121(6): 1459. DOI:10.32604/ee.2024.047247 |
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