N-G/ZIF-8-Based/Derived Materials as Battery Electrodes

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This entry is adapted from the peer-reviewed paper 10.3390/batteries10020047

As electrodes for batteries, N-G/MOF(ZIF-8) materials can mitigate issues like an electrode volume expansion for Li-ion batteries and the ‘shuttle effect’ for Li-S batteries. As electrodes for electrochemical capacitors, these materials can considerably improve the ion transfer rate and electronic conductivity, thereby enhancing the specific capacitance while maintaining the structural stability. Batteries are widely recognized as the most convenient electrochemical energy storage systems, and considerable efforts have been dedicated to their development and enhancement. Despite these endeavors, various challenges persist, including sluggish reaction rates, irreversible electrochemical reactions, the formation of a solid electrolyte interface (SEI), and electrode volume expansion.

N-doped graphene zeolitic imidazolate framework-8 (ZIF-8) battery electrode

1. Synthesis Trends and Characteristics of N-G/ZIF-8-Based/Derived Battery Electrodes

One of the first attempts at preparing anodes for lithium-ion storage from ZIF-8-derived N-doped graphene materials was reported by Zheng et al. in 2014 ^[1]. Aiming to achieve a higher nitrogen doping level compared to the contemporary attempts (~10 wt% of N doping), they opted to leverage the ZIF-8′s elemental composition’s (C₈H₁₀N₄Zn) aspect of having a high nitrogen content of around 30 at% (excluding the hydrogen content) to form an N-doped graphene material. They first synthesized ZIF-8 through a room-temperature chemical process. Then, the ZIF-8 was subjected to thermal annealing in a nitrogen atmosphere at different elevated temperatures (500 to 900 °C) for 8 h applying a 5 °C/min heating rate. The final product maintained the framework structure and contained 17.72 wt% of nitrogen. Through characterizations by XRD and Raman spectroscopy, the presence of a zeolitic structure and graphitic characteristics was confirmed for the material. As an anode, this material generated a high reversible specific capacity of 2037 mAh·g⁻¹ with a coulombic efficiency of around 58.4%. The high specific capacity of the materials was attributed to the high nitrogen contact.

Martín-Jimeno et al. introduced a novel approach called ‘nanopore lithography’ to achieve the uniform porosity of ZIF-8, with the intention of using it as an electrode material in energy storage systems ^[2]. They emphasized that the lack of a considerable proportion of mesopores hindered the performance of such materials in electrochemical applications. To address this, they devised a chemical process to coat the ZIF-8 with GO (graphene oxide) sheets. This ZIF-8/GO hybrid was then subjected to pyrolysis in an inert environment at various temperatures ranging from 700 to 1000 °C. Subsequently, the material underwent activation using a specific KOH solution.

During the carbonization process, incipient pores were generated on the GO cover through the thermal etching of the highly oxidized regions of the GO, while the inner ZIF-8 core remained unaffected. The activation process using KOH resulted in the formation of uniform micropores in the composite, following the incipient pores on the GO sheet. Consequently, the composite sample exhibited a more uniform microporosity compared to the precursors. The material’s nitrogen doping content was confirmed, and four nitrogen functional groups were identified: pyridinic-N, pyrrolic-N, graphitic-N, and pyridinic-N-oxide.

As a sulfur host material in Li-S batteries, Ding et al. developed a 3D porous carbon framework (referred to as PCF) with a unique structure comprising polyhedral-shaped hollow carbon coated with reduced graphene oxide (rGO) ^[3]. The main goal for creating this material was to address the challenge of the spontaneous dissolution and diffusion of soluble lithium polysulfide intermediates in Li-S batteries, a phenomenon known as the shuttle effect, which negatively impacts a battery’s performance. To achieve this, they initially mixed ZIF-8 and GO suspensions in a specific ratio (2:15 mass ratio) through stirring. The charge differences between the ZIF-8 and GO (expressed as zeta potentials) led to the formation of a ZIF-8/GO composite through an electrostatic self-assembly process. This composite was then subjected to pyrolysis at 900 °C in a nitrogen atmosphere, transforming it into the desired structure of rGO-covered hetero-structured porous carbon with polyhedral-shaped hollow carbon. The resulting composite exhibited the expected morphological structure, as anticipated by the researchers. XPS analyses confirmed nitrogen doping in the material, with the dominant nitrogen contents identified as pyridinic-N and graphitic-N functional groups. These functional groups were considered as the potential active sites in the material.

Considering the advantageous presence of nitrogen and carbon atoms in the ZIF-8, Tai et al. produced N-doped ZIF-8-derived carbon by calcinating the material at different temperatures in the range of 600–900 °C ^[4]. The process involved synthesizing the ZIF-8 by a solvothermal method first, then calcinating dried ZIF-8 powder at different elevated temperatures in a nitrogen atmosphere for 2 h at a heating rate of 5 °C/min. Depending on the calcination temperatures, the samples were denoted as NC-600, NC-700, NC-800, and NC-900. An acid (diluted HCl) wash and subsequent drying were carried out for the NC-800sample.

The Raman spectroscopy analysis of the samples showed that the I_D/I_G ratios were in the range of 0.92–1.33, indicating the graphitization of the material with a considerable presence of defects. Through the BET surface area analysis, it was shown that the specific surface area of the materials increased proportionally with the calcination temperature. The continuous removal of the zinc atoms at higher temperatures was justified by such an observation. This zinc removal process was also claimed to produce a higher porosity in this 3D framework structure. The elemental-level analysis of the samples by XPS suggested the presence of different C-N bons, such as pyridinic-N and pyrrolic-N, in the material.

Wang et al. addressed the challenge of addressing weak interactions between ZIF-8 and rGO when preparing composites for use as sulfur hosts in Li-S batteries to prevent the ‘shuttle effect’ ^[5]. They observed that a simple mixture of ZIF-8 and rGO resulted in a low capacity and limited coulombic efficiency, as the ZIF-8 particles tended to detach from the rGO surface due to weak bonding. Additionally, the ZIF-8 particles tended to agglomerate because of the surface tension of rGO. To overcome these issues, the researchers adopted a different approach by creating a ZIF-8@rGO composite through the facile hydrothermal conversion process of a Zn₅(OH)₆(CO₃)₂@rGO precursor with 2-methylimidazole. They avoided using high-temperature carbonization. Finally, they prepared a ZIF-8@rGO/S composite to evaluate its performance in preventing the ‘shuttle effect’ during Li-S battery operations. By deconvoluting the XPS S 2p narrow-scan spectra of the material, the researchers confirmed the existence of the Zn-S bond in the ZIF-8@rGO/S composite, demonstrating that ZIF-8 could effectively interact with the sulfur atoms of polysulfides, immobilizing them at the Zn sites.

Zhang et al. investigated the challenges faced by conventional anodes in potassium-ion batteries (PIBs) due to the large radius of potassium ions (K⁺), leading to significant volume changes and slow reaction kinetics ^[6]. Such an issue ultimately leads to an inferior structural stability and weak electrochemical activity for the PIB anodes. To address these issues and enhance the performance of PIB anodes, they introduced a novel zinc–cobalt bimetallic selenide material (ZnSe/Co_0.85Se@NC@C@rGO) and evaluated its synthesis, characterization, and performance in PIBs. They employed a multilevel space confinement process to create this material, involving the carbonization and subsequent salinization of a 2D graphene-encapsulated and resorcinol–formaldehyde (RF)-coated ZIF-8/ZIF-67 composite. It was presented that this ZIF-8/ZIF-67-derived highly porous carbon could provide a certain space margin to accommodate the volume stress arising from the repeated insertion and extraction of K⁺ ions. The material’s porosity offered ample channels for efficient ion and electron transfers, facilitating electrolyte transport, and exposing active sites to reactant species. The material was found to contain elements such as N, O, Zn, Co, and Se embedded in a carbon matrix. The presence of pyridinic-N, pyrrolic-N, and graphitic-N functional groups was confirmed, suggesting their potential roles in facilitating ion transport and enhancing the electron-donating capabilities of the material.

Although silicon has the potential to be a high-capacity anode material in lithium-ion batteries (LiBs) due to its ultra-high theoretical capacitance, its practical application is hindered by challenges, such as lower conductivity, volume expansion during electrochemical processes, and the formation of a solid electrolyte interface (SEI). To address these issues, metal silicate-based materials have shown promise as electrode materials for LiBs. In this context, Guo et al. synthesized a composite material consisting of cobalt silicate (CSO) integrated with rGO and ZIF-8, denoted as CSO/rGO/ZIFC ^[7]. The synthesis involved a series of solvothermal processes to create a Co₂SiO₄/GO/ZIF composite, followed by calcination at 800 °C to obtain the final product. The resulting material exhibited a 3D porous morphology with a carbon network structure. A ZIF-8 layer was formed over the CSO/rGO/ZIFC surface, and upon calcination, the evaporation of Zn created a highly po

Chen et al. prepared an N-doped nanoporous carbon matrix by carbonizing ZIF-8 and then integrated it with sulfur producing a cZIF-8/S composite to apply as a cathode material for sodium–sulfur (Na-S) batteries ^[8]. Their synthesis process involved the chemical synthesis of ZIF-8 and carbonizing it to 800 °C for 2 h with a 2 °C/min heating rate. Then, the carbonized ZIF-8 or carbon matrix was impregnated with sulfur to produce the cZIF-8 composite. Through XRD and XPS analyses, the formation of a disordered graphene structure (ID/IG ratio of 1.11) and the presence of different nitrogen functional groups (pyridinic-N, pyrrolic-N, and quaternary/graphitic-N) were confirmed. The cZIF-8 exhibited a BET surface area of approximately 627 m²/g.

For anode materials of LiBs, employing a pyrolysis process, Liu et al. synthesized N-doped porous carbon-coated graphene (rGO) sheets (NPCGSs) with an in situ-grown ZIF-8 on a GO precursor ^[9]. The ZIF-8 particles were grown on GO sheets through a chemical process. Then, they was heated to 800 °C for 5 h at a 3 °C/min heating rate. A final acid (33 wt% HCl) wash was provided to the material to remove excess Zn and other impurities. The materials exhibited both graphene-like and ZIF-8-like morphological features. The presence of different nitrogen functional groups, such as pyridinic N, pyrrolic N, and graphitic N, was confirmed in the materials by the XPS study. The material had a BET-specific surface area of 781.3 m²/g and the pore sizes were concentrated around 0.55 and 1.5 nm.

2. Performance and Functionalities of N-G/ZIF-8-Based/Derived Battery Electrodes

This subsection is dedicated to thoroughly reviewing the electrochemical performance of the above-discussed N-G/ZIF-8-based/derived composites as electrodes of different battery systems. Also, a careful observation was performed to understand how the materials’ electrochemical functionalities were justified conforming to their structural and chemical properties. In general, these materials were observed to aid in managing different concurrent battery-electrode-related issues, such as volume expansion and irreversible ion dissolution. The key discussions in this section begin at this point.

According to the electrochemical performance data presented by Martín-Jimeno et al., the sample that underwent carbonization at 800 °C followed by activation with a specific amount of KOH (KOH/precursor weight ratio of 1) showed the highest capacitive storage and well-defined redox activity ^[2]. This particular sample was labeled as ZIF-8/GO (1|800).

The authors analyzed the SWV data to attribute the voltage-specific current flows observed for the sample electrodes to various probable faradic phenomena (provided in the Supporting Information of Martín-Jimeno et al. ^[2]). Nonetheless, in this study, the comparison of electrode performance was limited to different composite samples prepared with varied carbonization temperatures and individual precursors (GO and ZIF-8). Nevertheless, the study showcased a well-defined technique that could be employed to optimize the pore structures of graphene/ZIF-8-based materials and achieve improved electrode properties.

The applicability of Ding et al.’s PCF composite as a sulfur host material for Li-S batteries was assessed by creating a PCF/sulfur composite electrode through a slurry coating process ^[3]. This composite electrode was then subjected to CV measurements in an electrochemical environment simulating the conditions of an Li-S battery. The CV curves exhibited well-defined peaks during both the cathodic and anodic processes, indicating a two-step reduction of elemental sulfur to Li₂S_n/Li₂S₂/Li₂S and the subsequent oxidation of Li₂S_n back to elemental sulfur, respectively. The CV curves maintained a consistent shape over four cycles, leading to the conclusion that the PCF composite effectively mitigated the shuttle effect, which is a desirable property for Li-S batteries. The data also indicate promising charging and discharging capacities for the PCF composite; an initial capacity of 1339 mAh/g at 0.1 C was generated. Also, the material retained a capacity of 1046 mAh/g (starting from 1335 mAh/g) at 0.5 C after 500 cycles, which was a capacitance retention of 79.7%. As shown in the XPS N 1s spectra, the PFC composite contains a higher ratio of pyridinic-N and graphitic-N, which are ascribed as the key active sites for the material.

However, the study did not explicitly explain the underlying mechanisms that contributed to the functionality of the composite, apart from identifying the presence of two critical nitrogen functional groups. Further research is needed to achieve a greater understanding of how the material’s chemical and structural features contribute to its ability to manage the shuttle effect effectively. Investigating these aspects will shed more light on the rationale behind the composite’s electrochemical performance in Li-S batteries.

The electrochemical performance of Tai et al.’s NC-800 samples (depicted as the best-performing one) was first evaluated by cyclic voltammetry (CV) tests within 0.01 to 3 V at a 0.1 mV/s scan rate ^[4]. Although a strong redox peak can be observed at 0.41 V in the first cycle indicating the formation of a solid electrolyte interface (SEI) layer, this peak is absent from the subsequent cycles, indicating fair reversibility in the charge–discharge process. The anode prepared for LIBs with this sample was tested by galvanostatic charge–discharge cycles in a voltage range of 0.01–3.0 V. Conforming to the CV results in the first cycle, a higher specific discharge capacity of 815.15 mAh/g was observed. In the two subsequent cycles, the capacities were 464.96 and 453.29 mAh∙g⁻¹, respectively. It can be assumed that the redox interaction contributes to a considerable portion of pseudocapacitance in the first cycle. The cyclic performance of the LIB anode with the samples was measured at 100 mA/g over 100 cycles. The NC-800 sample retained 94.7% of the initial capacity after 100 cycles and the coulombic efficiency was 56%.

Wang et al. reported that CV curves for the initial five cycles with the ZIF-8@rGO/S electrode showed that the electrochemical reaction in the Li-S battery was fairly reversible in the electrode, and the ZIF-8@rGO host effectively curbed the dissolution of polysulfides ^[5]. The coulombic efficiency during this test was measured at 98.6% with the ZIF-8@rGO/S cathode. Additionally, a persistent improvement in the cyclic performance of ZIF-8@rGO/S was observed for 300 charging and discharging cycles measured at 0.1 A/g. This study articulated that the presence of rGO in the ZIF-8@rGO/S cathode improved the electrical conductivity and helped suppress the volume change in sulfur during cycling, thereby enhancing the coulombic efficiency.

Zhang et al.’s zinc–cobalt bimetallic selenide material (ZnSe/Co_0.85Se@NC@C@rGO) exhibited an excellent capacitive behavior, attributed to its large surface area and abundance of active sites ^[6]. The low-charge-transfer resistance indicated the efficient transfer of K⁺ ions within the material. Through the ex situ XRD and XPS analyses conducted at different charging and discharging stages, the mechanisms of K⁺ ion storage and release in the material were proposed. According to their findings, the storage of K⁺ ions in the material involved conversion-alloy reactions. During the discharging process, ZnSe converts into Zn and K₂Se, and Zn also forms KZn₁₃, while Co_0.85Se transforms into Co and K₂Se. Conversely, during the charging process, K⁺ ions are released from the K₂Se components. These insertion and de-insertion reactions of K⁺ ions were observed to be highly reversible, indicating the material’s potential for stable and efficient cycling in PIBs. In a recent study, Deng et al. synthesized hierarchically porous nitrogen-doped carbon (HPNC) as a host for an Se cathode, aiming to enhance the performance of Li–Se batteries. The Se/HPNC cathode could attain a discharge capacity of 582 mAh/g at 0.2 C with a 90.5% capacity retention rate ^[10].

Based on the electrochemical characterization data, the material also demonstrated a high Li-ion diffusion coefficient and a lower circuit resistance. The authors attributed the improved performance of the composite to several factors. The 2D rGO acted as a lamellar template and supporting substrate, enhancing the electrical conductivity of the material. The porous structure derived from ZIF-8 facilitated the diffusion of Li-ions, and it also helped in mitigating the volume expansion during the operation and promoted favorable electrochemical interface reactions.

The cZIF-8/S composite synthesized by Chen et al., as an Na-S battery cathode, generated specific capacities of 1000, 850, 650, 480, 220, and 850 mAh/g at the current densities of 0.1 C, 0.2 C, 0.5 C, 1.0 C, 2.0 C, and 0.1 C, respectively. The capacity retention was 60% when, for the first 5 cycles, the current density was kept at 0.1 C and then at 0.2 C for 250 cycles ^[8].

As an anode material of a LiB test system, Lui et al.’s NPCGS composite generated initial charge and discharge capacities of 873 and 1391 mAh/g, respectively, at 0.5 A/g current densities ^[9]. The initial coulombic efficiency (CE) was approximately 62.7%. This low initial value of CE indicated a possible formation of solid–electrolyte interphase (SEI) film. Nonetheless, the data show that the coulombic efficiency reaches 100% after 200 cycles. In the rate performance tests, the NPCGSs produced capacities of 936, 854, 806, 728, 652, 606, 546, and 459 mAh/g at current densities of 0.1 to 0.2, 0.4, 0.6, 0.8, 1, 2, and 4 A/g, respectively. When the current density returned to 0.1 A/g, the capacity returned to 930 mAh/g.

The capacitive performances of the above-discussed N-G/ZIF-8-based/derived materials developed as different battery electrodes are summarized in Table 1.

Table 1. Discharge capacitive performances of the N-G/ZIF-8-based/derived materials for different battery/energy storage systems.

Material	Discharge Capacitive Performance (of the Best Sample)
N-doped graphene analogousp articles (Anode materials for LIBs) (Zheng et al.—2014 ^[1])	Specific discharge capacity: 2037 mA·h/g at 100 mA/g. Capacity retention: 99.2% after 50 cycles at 100 mA/g. Coulombic efficiency: ~53.4% over 200 cycles at 500 mA/g.
Activated ZIF-8/GO (General energy storage materials) (Martín-Jimeno et al.—2017 ^[2])	Specific capacitance: 241 F/g calculated from CV measurement in 1 M of H₂SO₄ at a 2 mV/s scan rate. Capacitance retention: not specified.
Three-dimensional porous carbon framework (PCF) (Host material for Li−S batteries) (Ding et al.—2019 ^[3])	Specific capacitance: 1339 mAh/g at 0.1 C or a 167.5 mA/g current rate (1 C = 1675 mA/g). Capacitance retention: 79.7% after 500 cycles at 0.5 C. Coulombic efficiency: 100% over 650 cycles at 1 C.
N-doped ZIF-8-derived carbon (NC-ZIF) (Anode materials for LIBs) (Tai et al.—2019 ^[4])	Reversible specific capacity: ~453–465 mAh/g at 100 mA/g. Capacitance retention: ~94.7% after 100 cycles at 100 mA/g. Coulombic efficiency: ~56% over 100 cycles at 100 mA/g.
ZIF-8 nanocrystals attached to reduced graphene oxide/sulfur (ZIF-8@rGO/S) (Cathode material for Li-S batteries) (Wang et al.—2021 ^[5])	Specific capacitance: 1297 mAh/g at 100 mA/g. Capacitance retention: ~33.87% after 200 cycles at 200 mA/g. Coulombic efficiency: 98.6% over 100 cycles at 200 mA/g.
Zinc–cobalt bimetallic selenide (ZnSe/Co_0.85Se@NC@C@rGO) (Anode material for PIBs) (Zhang et al.—2023 ^[6])	Specific capacity: 422.2 mAh/g at 100 mA/g. Capacitance retention: ~83.2% after 2000 cycles at 2000 mA/g. Coulombic efficiency: 100% over 2000 cycles at 2000 mA/g.
Three-dimensional porous Co₂SiO₄/rGO/ZIFC conductive network (Anode materials for LIBs) (Guo et al.—2023 ^[7])	Specific capacitance: 1060 mAh/g at a 200 mA/g current density. Capacitance retention: not specified. Coulombic efficiency: 100% over 250 cycles.
N-doped nanoporous carbon matrix with sulfur (cZIF-8/S). (Cathode materials for Na-S batteries) (Chen et al.—2016 ^[8])	Specific capacitance: 1000 mAh/g at 0.1 C or ~167.5 mA/g current density. Capacitance retention: 60% after 250 cycles at 0.1 C for 5 cycles and then 0.2 C for 250 cycles.
N-doped porous carbon-coated graphene (rGO) sheets (NPCGSs). (Anode materials for LIBs) (Liu et al.—2016 ^[9])	Specific capacitance: 936 mAh/g at a 100 mA/g current density. Coulombic efficiency: 100% over 200 cycles.

In the electrochemical battery systems, as the energy is stored and released by means of different ion transfer processes to and from the electrodes and electrolytes, to study the electrode materials, the aspects of porosity are of significant interest. To this end, the porosity-related parameters of the N-G/ZIF-8-based/derived materials are meticulously compiled in Table 2. As the electrochemically assessable surface area is another crucial parameter that is also related to the pore structure of the materials, the BET surface areas of these materials are also carefully noted here.

Table 2. Collected data of the porosity parameters of the N-G/ZIF-8-based/derived materials for application in battery systems.

Material	Pore Diameter (nm)	Pore Volume (cm³/g)	BET Surface Area (m²/g)
N-doped graphene analogous particles (Zheng et al. ^[1])	2.02	0.32	634.6
Activated ZIF-8/GO (Martín-Jimeno et al. ^[2])	<1 to 4	1.219	1304
Three-dimensional porous carbon framework (PCF) (Ding et al. ^[3])	~0.6	0.35	643
N-doped ZIF-8-derived carbon (NC-ZIF) (Tai et al. ^[4])	~1.8 to 2.0<	~0.3	815.8
ZIF-8 nanocrystals attached to reduced graphene oxide/sulfur (ZIF-8@rGO/S) (Wang et al. ^[5])	3.4 to 15.5	0.329	905.6
Zinc–cobalt bimetallic selenide (ZnSe/Co0.85Se@NC@C@rGO) (Zhang et al. ^[6])	~4.0	~0.12	232.51
Three-dimensional porous Co₂SiO₄/rGO/ZIFC conductive network (Guo et al. ^[7])	Not specified	0.50	210
N-doped nanoporous carbon matrix with sulfur (cZIF-8/S) (Chen et al. ^[8])	~0.5	Not specified	627
N-doped porous carbon-coated graphene (rGO) sheets (NPCGSs) (Liu et al. ^[9])	0.55, 1.5	Not specified	781.3

It is generally understood that mesopores (2 to 50 nm diameters) in carbon-based materials are advantageous for electrochemical activities ^[11]^[12]^[13]. Mesopores allow the facile penetration of the ions of the electrolyte in the material, hence increasing the effective mass transport for the electrochemical reactions. Nonetheless, micropores (less than a 2 nm diameter) also hold some significance in maintaining the structural integrity of the materials. Most of the N-G/ZIF-8-based/derived materials were observed to have a combination of micropores and mesopores in various degrees, which apparently turned out to be advantageous for electrochemical activities.

References

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1. Synthesis Trends and Characteristics of N-G/ZIF-8-Based/Derived Battery Electrodes

2. Performance and Functionalities of N-G/ZIF-8-Based/Derived Battery Electrodes

References