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Nickel-Based Catalysts for Dry Reforming of Methane： Synthesis Methods and Performance Modulation

Yi Wang , Xinjie Du , Zhe Chen

Progress in Chemistry ›› 2026, Vol. 38 ›› Issue (9) : 1650 -1663.

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Progress in Chemistry ›› 2026, Vol. 38 ›› Issue (9) : 1650-1663 DOI: 10.7536/PC20260219
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Nickel-Based Catalysts for Dry Reforming of Methane： Synthesis Methods and Performance Modulation
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Abstract

Dry reforming of methane（DRM）can simultaneously convert two greenhouse gases， methane and carbon dioxide， into valuable syngas， demonstrating significant application potential in the fields of energy conversion and environmental governance. Ni-based catalysts have been extensively studied and applied due to their low cost and excellent catalytic activity. This review focuses on the synthesis methods of nickel-based catalysts for dry reforming of methane， aiming to enhance the activity and stability of the reaction by modifying the synthesis approaches. The article provides a detailed introduction to the preparation principles， process characteristics， and catalytic performance of materials synthesized via different methods（impregnation， sol-gel， evaporation-induced self-assembly， templating， etc.）. Additionally， strategies for improving catalyst synthesis methods are discussed， including regulating oxygen vacancy concentration， active metal atomic size， and metal-support interactions. Optimizing the adsorption-dissociation processes of CH4 and CO2 on the catalyst， tuning the electronic states of metal sites， lowering reaction energy barriers， and suppressing particle sintering and carbon deposition can significantly improve reaction activity and stability. This review aims to provide insights for the development of next-generation nickel-based dry reforming catalysts and promote the advancement of DRM technology toward greater feasibility and sustainability.

Contents

1 Introduction

2 Reaction conditions， reaction mechanism， and deactivation mechanism of Ni-based catalysts for dry reforming

2.1 Reaction conditions

2.2 Dry reforming reaction mechanism

2.3 Nickel-based catalysts deactivation mechanism

3 Different synthesis methods of Ni-based catalysts

3.1 Impregnation method

3.2 Sol-gel method

3.3 Evaporation-induced self-assembly method

3.4 Template method

4 Strategies for enhancing the activity and stability of nickel-based catalysts

4.1 Oxygen vacancy

4.2 Size of metallic nickel nanoparticles and single-atom nickel

4.3 Metal-support interaction

5 Conclusions

Graphical abstract

Keywords

CO2 catalytic conversion / dry reforming of methane / nickel-based catalysts / synthesis methods / regulation strategies

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Yi Wang, Xinjie Du, Zhe Chen. Nickel-Based Catalysts for Dry Reforming of Methane： Synthesis Methods and Performance Modulation. Progress in Chemistry, 2026, 38(9): 1650-1663 DOI:10.7536/PC20260219

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1 Introduction

The rapid development of human society has led to a significant increase in fossil fuel consumption, with excessive carbon dioxide emissions exceeding 41 billion tons annually, triggering a series of environmental problems[1], including rising global temperatures, frequent extreme weather events, accelerated sea-level rise, and damage to ecosystems and biodiversity. Reducing greenhouse gas emissions can avoid more severe consequences of climate change and promote the development of a low-carbon, adaptive economy.
Converting carbon dioxide into high-value chemicals through chemical transformations, such as dry reforming of methane, water-gas shift, hydrogenation methanation, and hydrogenation to methanol, holds significant scientific and economic value[2]. The dry reforming of methane (DRM) reaction can convert CH4 and CO2 into synthesis gas composed of H2 and CO, consuming two greenhouse gases simultaneously, providing an efficient pathway for addressing the conversion of CO2. Meanwhile, the product synthesis gas is an important raw material gas for the chemical industry and can be further converted into various fuels and high-value chemicals[3]. Due to its significant carbon reduction effects and high product added value, dry reforming technology is increasingly gaining attention from all sectors[4].
CO2and CH4have very low Gibbs free energy, approximately -394 kJ/mol and -50.7 kJ/mol respectively. These two gases are very stable; activating CO2and CH4requires high temperatures and highly active metal catalysts[5]. However, under high-temperature conditions, metal catalysts are prone to sintering and coking, leading to loss of activity, reaction interruption, and in severe cases, pipeline blockage. Therefore, DRM catalysts must possess not only high activity but also high stability against coking and selectivity[6]. In the dry reforming process oriented toward industrial application, developing catalytic systems that combine economic viability, high activity, and excellent stability is crucial. Among numerous highly active metal catalysts, nickel-based catalysts demonstrate promising application prospects due to their cost advantages and high activity[5], becoming the preferred catalyst for the industrialization of the DRM reaction. However, they are prone to sintering and carbon deposition during high-temperature reactions, leading to catalyst deactivation, which severely limits their industrial progression. Optimizing preparation methods to achieve precise structural design and regulation of active sites can enhance catalyst activity and resolve stability issues. During synthesis, nickel-based catalysts can not only alter the particle size distribution, crystal plane structure, and dispersion state of metallic nickel but also precisely regulate metal-support interactions, reducing sintering and coking of active components during the reaction. This paper reviews and discusses the catalytic performance and structure-activity relationships of nickel-based catalysts prepared by different methods, starting from the thermodynamic and kinetic characteristics of dry reforming catalysis and the structure and preparation methods of nickel-based catalysts, expecting to provide references for the development of nickel-based dry reforming catalysts in the field of CO2catalytic conversion.

2 Dry reforming reaction conditions, mechanisms, and carbon deposition issues

2.1 Reaction conditions

CH4and CO2are both symmetric molecules with stable structures. Among them, CH4has a tetrahedral structure with a bond energy of 439 kJ/mol[7]; CO2is a linear molecule containing two C＝O double bonds within the molecule, with a bond energy as high as 804 kJ/mol[8]. To achieve the activation of CH4and CO2and overcome the reaction energy barrier, a large amount of energy input is required, which also determines that the DRM reaction is a strongly endothermic reaction. However, due to the presence of side reactions, the products H2and CO are mostly below a 1:1 ratio in most DRM reactions, reducing the yield of syngas. Asshown in Figure 1by the Gibbs free energy model, the occurrence of DRM and various side reactions exhibits significant temperature dependence. Among them, the Boudouard reaction (2CO → CO2 + C) is one of the typical carbon deposition pathways in the DRM reaction, with its thermodynamic spontaneous tendency mainly concentrated in the medium-to-low temperature range below 700 ℃. In contrast, the reverse water-gas shift reaction (RWGS reaction, CO2 + H2 → CO + H2O) occurs more readily under high-temperature conditions above 800 ℃[9], and its reaction spontaneity increases with rising temperature. To suppress the occurrence of these two major side reactions while balancing the thermodynamic conversion efficiency of the main reaction, most experiments control the reaction temperature at 700~800 ℃. The methane decomposition reaction (CH4 → C(s) + 2H2) is another core challenge in the DRM system[10]; this reaction is a side reaction that is thermodynamically relatively easy to occur spontaneously, and the generation of its product, deposited carbon, causes severe catalyst deactivation. Therefore, improving stability and mitigating carbon deposition are the core objectives of DRM catalyst design[11].
DRM catalysts are typically composed of two components[13](Figure 2). The first component is the active metal species (Ni, Co, Fe, Rh, Ru), among which Ni metal is widely used due to its high activity and low cost, while noble metals possess higher resistance to coking. Active metal species achieve the dissociative activation of C—H bonds in CH4 and the adsorptive activation of CO2 through interaction with reactant molecules, providing necessary active sites for the reaction. The second core component is a relatively inert metal oxide support (SiO2[14], Al2O3[15], MgO[16], TiO2[17]), which plays a decisive regulatory role in the overall performance of the catalyst. Active sites on the support surface anchor metal particles and can disperse active metal species. Strong metal-support interactions can control the size of metal particles/clusters and inhibit sintering, while providing mechanical strength and thermal stability under high-temperature reaction conditions. In addition, using reducible metal oxides (such as TiO2, CeO2) as support materials can increase the concentration of oxygen vacancies, promote oxygen migration to the active metal surface, thereby further reducing coke formation. Other promoters, such as alkali metals (Na, K, Ca) and rare earth metal oxides (La2O3[18]), can reduce catalyst coking and enhance stability by regulating the acidity and alkalinity of the catalyst surface. The composition, preparation parameters, reaction conditions, and activity of common DRM catalysts are shown inTable 1.

2.2 Dry reforming reaction mechanism

The DRM reaction mechanism primarily follows a bifunctional pathway, where methane undergoes stepwise dehydrogenation at metal sites, and carbon dioxide is adsorbed and activated at support or support-metal interface sites, with slight variations depending on the catalyst composition and performance. Asshown in Figure 3, the reaction mechanism mainly includes four types: (1) dissociative adsorption of methane at nickel sites and its subsequent dehydrogenation to generate hydrogen and carbonate species CHx(0 < x < 4); since the dissociation of C—H bonds is relatively difficult, this step is generally considered the rate-limiting step; (2) dissociative adsorption of carbon dioxide at nickel sites or on the surface of basic supports to form CO* and O* (partially combining with H to form OH*); (3) reaction of surface O* and OH* groups with adsorbed CHxintermediate species to form formate intermediates (CHxO); (4) decomposition of formate intermediates (CHxO) to form carbon monoxide, while simultaneously surface-adsorbed H* combines to form hydrogen[30].

2.3 Deactivation mechanisms of nickel-based catalysts

Dry reforming of methane is a typical heterogeneous catalytic reaction characterized by a complex reaction system and harsh conditions, which easily lead to catalyst deactivation. Common causes include sintering of active metals, carbon deposition, oxidation of metal active sites, and sulfur poisoning, among which metal sintering and carbon deposition are the primary deactivation mechanisms.

2.3.1 Metal sintering

Metal sintering is a thermally induced irreversible phenomenon that often occurs at high temperatures (≥700 °C)[32]. Sintering mainly involves two mechanisms: (1) Particle migration and coalescence, where particles move on the support surface in a manner similar to Brownian motion, colliding and coalescing into larger particles; this mechanism primarily applies to the sintering of small nanoparticles. (2) Ostwald ripening, where particle migration is driven by a reduction in chemical potential; atoms are released from individual particles, disperse across the support, and attach to adjacent particles, ultimately forming larger particles. The agglomeration of catalysts into larger sizes leads to a reduction in internal cavities or pores, blocking active sites, thereby decreasing the overall catalytically active surface area and eventually resulting in deactivation.[33]. The fundamental mechanism of sintering is the mutual contact of metal particles within the diffusion distance. Therefore, promoting the high dispersion of active metal sites and using confinement materials to increase the spacing between metal particles to achieve uniform distribution can slow down the sintering process, thereby enhancing the stability of catalytic materials. Zhang et al.[34]found that the Ni/BN-c catalyst deactivated rapidly under DRM reaction conditions at 700 °C. Using the Scherrer equation to calculate particle sizes from XRD patterns before and after the reaction, it was observed that the particle size of the Ni/BN-c catalyst increased by 13.8 nm after the reaction (46.3 nm) compared to before the reaction (32.5 nm). The rapid agglomeration and sintering of metallic Ni, along with the collapse of the pore network, reduced its surface area, leading to rapid catalyst deactivation within 5 hours. Other studies[35]prepared Ni/S-1 catalysts via dissolution-recrystallization and conventional impregnation methods. After operating at 800 °C for 150 hours, the material prepared by the recrystallization method exhibited good Ni dispersion, whereas the material prepared by the impregnation method suffered severe sintering under the same conditions and deactivated rapidly within a short time. HAADF-TEM analysis indicated that the dissolution-recrystallization method anchored Ni nanoparticles within the S-1 zeolite matrix through the spatial confinement effect of the zeolite channels, increasing the dispersion of Ni metal particles while suppressing particle migration and agglomeration.

2.3.2 Carbon deposition

Carbon deposition on the catalyst surface is another important factor contributing to catalyst deactivation in the dry reforming of methane. Carbon deposits are mainly classified into three types: (1) adsorbed atomic carbon (Cα), also known as amorphous carbon, which is a highly reactive reaction intermediate and usually does not cause catalyst deactivation; most of it can react with CO2or undergo further gasification; (2) filamentous carbon (Cβ), a low-activity carbon derived from Cαthat reacts with water, carbon dioxide, and hydrogen, and can be slowly gasified by CO2or surface oxygen at high temperatures; (3) graphitic carbon (Cγ), which has a stable and dense structure approaching ideal graphite, is difficult to react with CO2or oxygen, and represents the most stubborn form of carbon deposition[36]. Carbon deposition mainly originates fromTable 2several side reactions. The research results of Bian et al.[37]indicate that the source of carbon deposition in dry reforming of methane is primarily dominated by the thermal decomposition of CH4. During the high-temperature syngas production process, elevated temperatures promote methane dehydrogenation at nickel metal sites to form C* species. These C* species further diffuse and accumulate along the metal surface, eventually forming various types of carbon deposits that encapsulate the active metal surface. This leads to complete coverage of active metal sites or pore blockage, hindering contact between active sites and reactant gases, thereby causing catalyst deactivation[38].

3 Different synthesis methods for nickel-based catalysts

The preparation method is one of the key factors affecting the catalyst's structure, composition, crystallite size, and dispersion, thereby influencing its catalytic activity, stability, and coking resistance. This section focuses on summarizing several common preparation methods.

3.1 Impregnation method

The impregnation method is the simplest and most commonly used method for preparing DRM catalysts to date, suitable for industrial production. The impregnation process involves contacting a solution containing active metal precursors with the support, followed by drying to obtain the catalyst.[39]. Depending on the amount of solution used, the impregnation method is mainly divided into two types: (1) Wet impregnation refers to using an excess of solution, removing the support from the solution after a predetermined time, and removing the excess solvent through drying.[40]; (2) Incipient wetness impregnation refers to adding a precursor solution with a volume equal to or slightly less than the pore volume of the support into the support, so that the solution is just absorbed by the support without forming a distinct free liquid phase. Because the interaction between nickel particles and the support in catalysts synthesized by traditional impregnation methods is weak, and they often grow in the outer pores, sintering and coking phenomena are highly prone to occur.[41]. To address this issue, researchers have found that using complexing agents such as glycine and citric acid to assist impregnation can significantly improve nickel dispersion, reduce nickel particle size, and enhance performance and stability. Zhang et al.[42]prepared a series of Ni/MSS catalysts using four different methods, including conventional impregnation, ethylene glycol-assisted impregnation (replacing water solvent with ethylene glycol), glycine-assisted impregnation (adding small amounts of C2H5NO2and ammonium nitrate), and ammonia evaporation (adding partial ammonia water). Compared with the conventional impregnation method, the other three methods reduced the Ni particle size, improved the interaction between the support and the metal, and lowered the apparent activation energy for CH4and CO2cracking, enabling the catalysts to maintain long-term activity and stability.

3.2 Sol-gel method

The sol-gel method can effectively prepare nickel-based catalysts with uniform structure and composition. Its core process involves a liquid precursor first transforming into a sol, which is a colloidal suspension system obtained through the hydrolysis and condensation of metal alkoxide precursors.[43], further reacting to form a gel with a three-dimensional network structure. Depending on the type of solvent, it can be classified into aqueous sol-gels and non-aqueous sol-gels. The aqueous sol-gel method uses water as the solvent in the reaction; its advantage lies in the fact that most precursors used have good hydrophilicity. However, the three core reactions of hydrolysis, condensation, and drying occur simultaneously, making it difficult to precisely control the morphology of material particles and resulting in poor reproducibility.[44]. Non-aqueous gels refer to those using organic solvents or where the metal precursors themselves provide the medium; this method utilizes organic solvents to supply oxygen sources, thereby allowing fine-tuning of the material's morphology, particle size, and composition.
In the application of the sol-gel preparation method, Wu et al.[45]used a multiple gel-sol method to prepare a tunable nano core-shell structured composite catalyst La2Ni1.6Fe0.4O6@CeO2. First, metal precursors were dissolved in water to form a mixed solution. A complexing agent (CA, EDTA) was added, and the temperature was raised to 80 °C with stirring to form a gel, which was then dried and calcined to form the core phase La2Ni2-xFexO6. Subsequently, a secondary gel synthesis was performed. The La2Ni2-xFexO6 core phase powder was dispersed in an ethanol solution, and evaporation yielded a concentrated suspension. The cerium precursor was dissolved in water and mixed with the suspension. After adding the complexing agent, the mixture was heated and stirred to form a gel, which was dried and calcined to form the core-shell structured composite catalyst (Figure 4).

3.3 Evaporation-induced self-assembly method

The evaporation-induced assembly method uses amphiphilic molecules as templating agents to regulate the sol-gel assembly process and can be employed to synthesize mesoporous metal oxide materials.[46]Its core mechanism involves surfactant molecules spontaneously arranging into specific ordered structures through the synergistic effects of electrostatic interactions, van der Waals forces, hydrogen bonds, and π bonds.[47]The preparation process of this material, as shown in Figure 5, primarily includes three steps: solvent evaporation triggering the self-assembly process, the system's solvent reaching equilibrium with the external environment, and the formation of organic-inorganic mesostructures, while inorganic precursors construct the mesoporous network via condensation reactions.
In the evaporation-induced self-assembly method[49]in practical applications, it can undergo various pathways. One approach is to first prepare a support material with an ordered mesoporous structure, followed by introducing the active material. For example: Ma et al.[49]research indicates that a bimodal meso-macroporous alumina support was prepared via the evaporation-induced self-assembly method, after which metallic nickel was loaded using the impregnation method. Deng et al.[50]used this method to first synthesize an ordered mesoporous MgAl2O4support, followed by loading active mesoporous Ni-Co oxides. Owing to their large surface area, uniform pore distribution, and tunable surface chemical properties, such supports enable highly dispersed loading of nickel-based active components. Another approach is the in-situ confined loading of active components to prepare an integrated catalyst in one step, by introducing Ni metal precursors during the self-assembly process. Ma et al.[51]prepared a mesoporous Ni-Al2O3catalyst via a one-step evaporation-induced self-assembly method, which exhibited superior activity and stability compared to catalysts prepared by conventional impregnation methods. Since the nickel particles are in-situ anchored within the carrier pores or on the pore walls, the particle size is controllable and the dispersion is extremely high. The active sites of such integrated catalysts are fully exposed, and their bonding with the support is stronger, resulting in superior performance.

3.4 Template method

The template method is a synthesis approach that precisely controls the pore structure and active component dispersion of catalysts through a "template-precursor assembly-template removal" process, primarily categorized into soft template and hard template methods.

3.4.1 Hard Template

The hard template method can utilize etchable templates (such as silica or combustible carbon) to design pore channels and core-shell structures. For example, using reducing agents (such as NaBH4and N2H4) to synthesize metal nanoparticles, coating the metal nanoparticles with template material, and then depositing oxide materials (such as CeO2, TiO2or ZrO2) on their surface, and finally removing the template material via chemical etching with concentrated NaOH solution to form hollow yolk-shell structured catalysts[52].
El Samrout et al.[53]CaO supports were prepared using the hard template method: SBA-15 was dispersed in an organic solution, calcium nitrate was added dropwise with multiple impregnations, followed by drying and calcination. The silica template SBA-15 was then removed with sodium hydroxide, and after washing, CaO with ordered mesopores was obtained. Li et al.[54]also synthesized mesoporous CeO2catalyst supports using SBA-15 as a hard template. After impregnating the template with metal, it was calcined and dried, then the template was removed with an alkaline solution, followed by loading with nickel metal (Figure 6). Catalysts prepared via the hard template method precisely replicate the pore structure of the template, achieving directed construction of mesoporous, macroporous, and hierarchical pore structures, which enhances mass transfer efficiency and reduces carbon deposition blockage. Meanwhile, the prepared supports exhibit high mechanical strength and can withstand the high-temperature conditions of DRM reactions.

3.4.2 Soft template

The template materials used in the soft template method include surfactants and droplets, which are easier to remove[55]. However, soft template materials suffer from the defect of being prone to deformation, making it still challenging to synthesize highly dispersed catalysts via the soft template method. Zhang et al.[56]employed a hydrothermal-assisted soft template method to synthesize CoCexcomposite catalysts; by adding the surfactant CTAB to a uniformly mixed metal precursor solution and then adjusting the pH for a hydrothermal reaction, catalysts with unique channel structures were formed. Kamieniak et al.[57]prepared nickel-based apatite catalysts using the soft template method; they uniformly mixed the metal precursors, adjusted the pH value with concentrated nitric acid, added polysorbate 60 (polyoxyethylene sorbitan monostearate) with heating and stirring, and after cooling to room temperature, added ammonia water to precipitate HAP, yielding catalysts with a larger specific surface area.

4 Strategies for improving the activity and stability of nickel-based catalysts

By precisely regulating the catalyst structure and preparation process, strategies such as adjusting the oxygen vacancy concentration of the catalyst, reducing the size of active metals, and tuning metal-support interactions to improve catalyst synthesis can achieve comprehensive enhancement of catalytic performance.

4.1 oxygen vacancies

Oxygen vacancies (Ov), also known as oxygen-deficient sites, refer to the absence of oxygen ions (O2-) at specific lattice sites in materials. They can be formed through various mechanisms such as heat treatment, improved preparation methods, and dopant introduction, playing a critical role in DRM reactions within certain catalytic systems. Kumar et al.[58]used isotopic gas mixtures to investigate the catalytic process of dry reforming reactions, finding that creating oxygen vacancies promotes the migration of lattice oxygen ions, reduces carbon deposition during the reaction, and facilitates oxygen exchange between lattice oxygen and adsorbed carbon dioxide, significantly enhancing the reaction rate. It has also been reported that using SBA-15 as a hard template, followed by repeated impregnation and calcination, and then etching away the template with NaOH, yields ordered mesoporous CeO2supported nickel atoms. Compared to traditional impregnation methods, catalysts synthesized via the template method exhibit numerous oxygen vacancies and active sites, which help activate CO2and generate active oxygen to remove carbon deposits, thereby enhancing catalyst stability and demonstrating superior performance over long cycling periods[54].
Huang et al.[59]found that Ni/CeO2 catalysts with different morphologies (octahedral, rod-like, cubic) (Fig. 7a~c) exhibit different dominant crystal facets and oxygen vacancy concentrations. The three catalysts Ni/CeO2(111), Ni/CeO2(110), and Ni/CeO2(100) have CeO2 crystal facet structures that can regulate the Ni-CeO2 interaction strength and oxygen vacancy concentration, thereby affecting the catalytic active sites for reactants and their activation capability. XPS results (Fig. 7h~i) indicate that the oxygen vacancy concentrations of the three catalysts are Ni/CeO2 (110) (0.49) > Ni/CeO2(100) (0.17) > Ni/CeO2 (111) (0.07). In long-term cycling performance experiments (Fig. 7d~f), Ni/CeO2(110), leveraging its high oxygen vacancy-mediated dual-site (metal + interface) synergistic activation capability, maintained a CH4 conversion rate of 80% and a CO2 conversion rate of 90% at 750 °C (Fig. 7d~f), maintaining high activity and stability over 100 h of reaction. In Ni/CeO2(111), the metallic Ni sites, and in Ni/CeO2(100), the oxygen vacancies, present greater difficulty for CO2 adsorption, thereby hindering CO2 activation and leading to performance degradation. In contrast, the abundant oxygen vacancies at the interface of Ni/CeO2(110) provide sufficient active sites for CO2 adsorption and activation; the generated reactive oxygen species can rapidly oxidize CH4 dissociation-derived CHₓ intermediates and carbon precursor deposits, achieving a dynamic balance between reactant activation and coke elimination (Fig. 7g). Constructing a catalytic system with high oxygen vacancy concentration through crystal facet regulation achieves synergistic enhancement of catalytic activity and stability, providing important support for the industrial application of DRM[60-61].
Dendritic mesoporous silica was prepared via surface confinement technology; the unique dendritic pore structure and ZrO2doping generated abundant oxygen vacancies, significantly enhancing the catalyst's reaction rate and reducing carbon deposition[62]. In situ characterization and theoretical calculations revealed an L-H pathway, wherein the oxygen vacancy-rich support promoted CO₂ adsorption and activation, thereby facilitating the oxidation of C* species and suppressing coke formation. Designing nanosheet-like, hierarchically porous special morphologies to increase the support's specific surface area and interfacial defects could provide more sites for oxygen vacancy formation, ultimately achieving a synergistic enhancement of catalytic activity and stability.

4.2 Size of metallic nickel nanoparticles and single-atom nickel

The number of atoms in the active component directly affects its surface energy, coordination environment, and electronic structure, thereby influencing the intrinsic activity and stability of catalytic active sites. With the development of nanomaterial preparation technologies, the particle size of active components can be controlled down to the nanoscale or even single-atom level; active components of different sizes exhibit significantly different catalytic performances in DRM reactions. Extensive research has been conducted on the relationship between Ni particle size and catalytic activity as well as carbon resistance. When the Ni particle diameter exceeds a critical value, the particle size shows a positive correlation with the carbon deposition rate; larger Ni particles are more prone to inducing carbon deposition.[63]. Dai et al.[64]research indicates that when the Ni particle size is controlled around 6.0 nm, good structural stability can be maintained without additional anti-sintering aids, effectively inhibiting sintering. Meanwhile, the size of Ni particles has a significant impact on the activation of CO2and CO formation. DFT studies[65]show that changes in Ni particle size directly lead to variations in the CO2activation pathway. On the catalyst with the smallest particle size, Ni13/MgO, CO2tends to dissociate directly, whereas on the catalyst with larger particle size, Ni25/MgO, the activation mechanism of CO2shifts to a hydrogen-assisted dissociation pathway with a lower energy barrier, which is kinetically more favorable. This suggests that by precisely controlling Ni particles to specific nanosizes, reactant activation pathways can be effectively optimized and reaction energy barriers significantly reduced. Chen et al.[66]conducted a comparative study using DFT calculations on the CH4activation and carbon growth mechanisms of Ni active metal clusters of different sizes. The calculations indicate that the adsorption energy barrier of intermediates (CH4) produced by stepwise dehydrogenation is influenced by the size of the metal cluster. Among them, the medium-sized Ni cluster Nixexhibits the lowest reaction energy barrier for the four-step dehydrogenation. Smaller Ni25clusters have limited active sites and geometric structures, while larger Ni13clusters show an enhanced tendency for carbon deposition. This study demonstrates that regulating the size of Ni metal particles can reduce carbon deposition generation.37
The size regulation effect is not only reflected in reactant activation and coke reduction processes but also directly influences the distribution status of active sites on the catalyst surface and reaction performance. Appropriately reducing the Ni particle size helps improve the dispersion of active sites while enhancing their reducibility, providing more effective sites for methane activation. Therefore, due to the uniform dispersion and strong reducibility of active sites in nanoscale Ni, higher methane conversion rates are demonstrated.[63]. Studies have shown that ultra-small nanoparticles (3–4 nm) of Ni/SBA-15 prepared by the solid impregnation method exhibit excellent stability, maintaining stable DRM catalytic activity during a 48-hour long-term experiment, whereas Ni/SBA-15 synthesized by the wet impregnation method shows a significant decline in activity within just 2 hours.[67], because smaller nanoparticles improve the availability of surface nickel active sites for the DRM reaction and enhance coking resistance. Min et al.[68]designed an innovative synthesis method (Figure 8a), employing a one-pot approach combined with sol-gel technology and a reprecipitation process. Without adding any metal promoters, they successfully prepared a catalyst (NiES) featuring nickel nanoclusters (particle size approximately 2 nm) embedded in a silica support. The particle sizes of catalysts prepared by traditional impregnation methods and simplified one-pot methods are both larger than those of the NiES catalyst (Figure 8b). The NiES catalyst exhibited superior performance and long-term stability during a 500-hour DRM cycling reaction at 800 °C, with reactant conversion rates remaining close to 100% and no obvious deactivation observed (Figure 8c). TEM results indicate that during prolonged reactions, the nickel nanoclusters maintained their particle size. In contrast, the average size of Ni particles prepared by the traditional impregnation method increased from 68 nm to 78 nm, forming encapsulated carbon after 31 hours of operation. The average size of Ni particles prepared by the one-pot method increased from 4.2 nm to 9 nm, forming whisker-like carbon structures and deactivating within 60 hours. Characterization revealed that smaller Ni particles promote methane decomposition, while hydroxylated Ni—O—Si species facilitate the surface oxidation of carbon species by enhancing carbon dioxide adsorption, thereby preventing coke formation. Research[69]indicates that modifying with nitrogen radio-frequency discharge plasma combined with a surfactant (cetyltrimethylammonium bromide, CTAB) enables the preparation of Ni crystallite sizes (4.9 nm) significantly smaller than those synthesized by the impregnation method (NM-C, 18 nm), maintaining stability after 20 hours of reaction. This provides new insights for reducing Ni crystallite size and increasing Ni particle dispersion to enhance material performance through CTAB plasma treatment assistance.
Single-atom catalysts (SACs) consist of isolated metal atoms dispersed on a support[70]. Compared with traditional catalysts, their highly dispersed active sites fully expose metal atoms, achieving an atomic utilization rate close to 100%. Although single-atom structures are generally considered thermodynamically unstable, research[71]indicates that some atomically dispersed metals exhibit better stability and activity than their nanoparticle catalyst systems. Rational design of stable Ni-based single-atom catalysts represents a key future direction for DRM reactions. Akri et al.[72]constructed an atomically dispersed nickel single-atom catalyst (2Ni1/HAP-Ce,Figure 9a) on a hydroxyapatite (HAP) support via strong electrostatic adsorption combined with co-precipitation and Ce doping modification. The 2Ni1/HAP-Ce catalyst demonstrated excellent catalytic performance and stability over a long reaction period of 100 h at 750 °C, maintaining a CO2conversion rate around 95%, with carbon balance approaching 100%, no coke formation, and no significant deactivation (Figure 9d). After prolonged cycling, the catalyst remained predominantly in single-atom form, with only minor clusters <1.5 nm formed. In contrast, catalytic materials dominated by Ni nanoparticles and Ni nanoclusters (Figure 9b) rapidly deactivated due to coking within 15 h (Figure 9c). The authors revealed the intrinsic mechanism behind its superior anti-coking capability through theoretical calculations and experimental characterization. The energy barrier for the initial dehydrogenation of CH4to generate CH3is only 0.63 eV, whereas the barrier for further dehydrogenation of CH3reaches as high as 1.54 eV. Consequently, further dissociation of CH3is strongly suppressed on the Ni1/CeO2surface, kinetically reducing coke formation (Figure 9e), blocking the pathway for deep decomposition of CH4into C*, resulting in no significant deposition of carbon species on the catalyst surface after long-term reaction. This unique mechanism breaks through the bottleneck of rapid deactivation due to coking in traditional Ni-based catalysts. Secondly, the strong Ni–Ce interaction constructed by Ce doping not only anchors Ni single atoms to prevent sintering but also provides active O species through the Ce3+/Ce4+redox cycle, promoting the oxidation conversion of CH3* intermediates into CO. Meanwhile, the electronic interaction between Ni2+active sites and the support optimizes the adsorption and activation efficiency of reactants, fundamentally avoiding coke formation.
Based on a special activation pathway, nickel single-atom catalysts exhibit significant advantages in coking resistance. Jiang et al.[73]successfully prepared single-atom nickel catalysts (Niₛₐ/DMS) and nickel nanoparticle catalysts (Ninₚ/DMS) by adjusting the loading amount via impregnation and combining it with the spatial confinement effect of dendritic mesoporous silica. Niₛₐ/DMS demonstrated excellent low-temperature activity during a long-cycle oxygen-assisted dry reforming of methane (ODRM) reaction at 550 °C for 110 h, maintaining stable performance throughout without significant decay, whereas Ninₚ/DMS rapidly deactivated due to coking during the reaction. Characterization and DFT calculations revealed that the unique Ni—O—Si coordination structure of the single-atom catalyst suppressed the competitive adsorption and oxidation of O2, preferentially activating CO2, thereby exhibiting superior oxygen tolerance while inhibiting deep dehydrogenation of CH4to prevent coke formation. Although nickel nanoparticles can rapidly and efficiently dissociate CH4, they are highly susceptible to oxidation by O2, leading to poor stability in long-term reactions due to coking and loss of active species. The authors also found that optimizing the coordination environment and dispersion of Ni sites through methods such as plasma treatment and atmosphere regulation can further enhance the oxygen tolerance and coking resistance of Ni-based catalysts, providing a new pathway for designing low-temperature DRM catalysts.

4.3 Metal-support interaction

Metal-support interaction is a key factor influencing the structure and performance of supported catalysts. In DRM reactions, the interaction between the active metal and the support can regulate the electronic state, dispersion, particle size, and resistance to sintering and coking of the active components, achieving synergistic enhancement of catalyst stability and catalytic performance.[74], its mechanism of action is complex and diverse[75].
The selection, synthesis, and regulation of supports are key factors in modulating metal-support interactions[76]. The study synthesized several Al2O3-ZrO2-supported Ni catalysts using different synthesis methods, such as modified Pechini sol-gel, urea hydrolysis, and physical mixing[77]. Among these, the sol-gel method can form more uniform Zr-Al oxide supports, thereby influencing the interaction between Ni and the support as well as the stability against coke formation. The enhanced interaction between Ni and Al2O3-ZrO2promotes CO2 dissociation, maintaining a balance between the reaction of oxygen intermediates generated from deposited carbon and methane dehydrogenation and CO2 dissociation, thus exhibiting higher stability in the DRM reaction.
The study employed a sacrificial Zr-MOFs template strategy to design three differentiated synthesis routes: in-situ introduction of nickel source, post-impregnation of nickel source into Zr-MOFs, and post-impregnation of nickel source into ZrO2(Zr-MOFs calcined at high temperature). The timing of nickel source introduction directly led to differences in the catalyst's microstructure and phase characteristics[78]. In-situ introduction of the nickel source (Ni-ZrO2-A) resulted in reduced overall Ni particle size because Ni2+and Zr4+formed tight coordination connections through organic ligands; whereas post-impregnation of the nickel source into Zr-MOFs (Ni-ZrO2-B) achieved highly dispersed Ni particles by leveraging the large pore structure of Zr-MOFs, while its Zr-MOFs support exhibited the highest proportion of the tetragonal phase (t-ZrO2). However, for post-impregnation of the nickel source into ZrO2(Ni-ZrO2-C), Ni2+and Zr4+could not form effective coordination and bonding, resulting in severe aggregation of NiO particles, and the Zr support was dominated by the monoclinic phase (m-ZrO2). Ni-ZrO2-B, possessing specific structural and interfacial properties, demonstrated optimal catalyst performance in the DRM reaction, achieving not only the highest conversion rates for reactants CH4and CO2, but also an H2/CO ratio that better met industrial requirements, along with the best stability; the other two catalysts deactivated rapidly within 6 hours of reaction. This advantage stems from the dual regulation effect of strong metal-support interaction. On one hand, the Ni—Zr—O species formed by SMSI (Strong metal-support interaction) anchored Ni particles onto the Zr-MOFs support, effectively preventing sintering and migration of Ni particles at high temperatures, with almost no sintering observed after the reaction. On the other hand, the synergy between strong interactions and phase characteristics limited the carbon deposition of this catalyst to only 3.8%, while the high proportion of the tetragonal phase (t-ZrO2) provided abundant strong Lewis acid sites, significantly enhancing the adsorption and activation capability of CO2.
Multiple studies have shown that confining active metal particles within cavities or shell/tubular structures enhances metal-support interactions through confinement effects, effectively inhibiting the migration and aggregation of nickel particles, thereby improving the structural stability and catalytic activity of the catalyst. Recently, Yin et al.[79]synthesized a hollow tubular Ni/La2O3-ES catalyst via electrospinning. The unique structure of the hollow tubular nanofibers achieves strong interactions between the active metal and the support, uniform dispersion of active Ni species, and a confinement stabilization effect within the support, thereby effectively suppressing metal clustering during stability testing at 800 °C. In long-term reactions, it maintains superior activity and stability compared to traditional Ni/La2O3catalysts prepared by spinning, ball milling, and co-precipitation methods.
The pore channels of mesoporous materials can provide natural confinement spaces. There are reports using H2O2adsorption methods to perform hydroxylation modification on the SBA-15 support[80], finding that the mesoporous channels of SBA-15 can load highly dispersed ultra-small Ni nanoparticles (Figure 10a). During the reaction process, the nickel particle size on unhydroxylated Ni/S-SBA-15 increases with prolonged reaction time, whereas hydroxylated Ni/S-SBA-15-OH maintains an ideal ultrafine nanoparticle state (particle size less than 3.2 nm, Figure 10b), maintaining high activity and high stability during long-term cycling (Figure 10d). Calculations show that the nickel sintering rate for the DRM reaction at 750 °C (Figure 10c) is extremely low for Ni/S-SBA-15-OH, at only 0.7%/h. The excellent high-temperature anti-sintering performance and reaction stability of this material are mainly attributed to its dual-confinement microenvironment, which greatly strengthens metal-support interactions. The modification of the SBA-15 support by H2O2generated a large amount of Si—OH, achieving Ni–O–Si bonding coordination between Ni and the support via strong electrostatic adsorption. The ordered mesoporous space of the SBA-15 support restricts the structural evolution and agglomeration of Ni particles. Under this dual confinement, atomically dispersed low-valence Ni(I) was obtained. High-temperature reduction can convert it from an atomically dispersed state into ultra-small nanoparticles with a narrow particle size distribution and a metal dispersion of 42.61%. DFT results indicate that ultra-small Ni sites make CO2easier to directly dissociate into CO and O*(Figure 10e).Figure 10(f)comparison shows that on ultra-small sized Ni catalysts, the energy barrier for the non-deep dissociation pathway of CH*CHO as a reaction intermediate is lower than that for the CH4dehydrogenation to generate C4deep dissociation pathway energy barrier, indicating that the*CHO route is more likely to occur. PDOS analysis (*CHO route is more likely to occur. PDOS analysis (Figure 10g) reveals that at the CH + O → *CHO transition state, the d-band center of Ni is closer to the Fermi level, indicating that this pathway has more favorable electronic coupling and a lower energy barrier, thereby effectively reducing coke formation tendency, promoting CO generation, and enhancing catalyst activity and high-temperature stability.
The core-shell structure can create a confined space, exhibiting novel metal-support interactions. By confining active metal particles within the support shell, metal sites can be effectively fixed, suppressing the migration, sintering, and loss of metal particles. Meanwhile, the interfacial interaction between the shell material and the metal can also achieve electron transfer, lattice matching, and interfacial synergy. Kaviani et al.[81]employed an innovative ammonia vapor method to prepare Ni-SiO2@SiO2core-shell structured catalysts, constructing a chemical-physical dual confinement effect. The ammonia evaporation method induces Ni2+to form nickel phyllosilicate with the SiO2support; this phase anchors Ni atoms into the SiO2framework via Ni—O—Si chemical bonds, forming strong metal-support interactions. Meanwhile, the porous shell formed by secondary SiO2encapsulation constructs a physical barrier, which not only prevents the sintering and migration of Ni particles but also restricts the growth of filamentous carbon. The mesopore size ensures effective contact between reactants and active sites, avoiding mass transfer hindrance caused by encapsulation. This catalyst still exhibits high and stable catalytic activity under low-temperature conditions of 600 °C (CH4 = 52%, CO2 = 72%). The basicity of metal oxides is also crucial for the activation of CO2. Yang et al.[82]prepared Co/Ni supported on CeO2supports as core-shell type Ni@Coₓnanoparticles via colloidal synthesis. The oxygen vacancies of CeO2provide lattice oxygen and strengthen metal-support interactions; the introduction of Co enhances the surface basicity of the catalyst and its CO2adsorption and activation capability, directionally diffusing during the reaction process to form a uniform NiCo alloy. This catalyst achieves high conversion rates of CH4and CO2at 800 °C and operates stably for over 100 h.

5 Conclusion

The core of designing efficient catalysts lies in achieving deep synergy among synthesis methods, microstructures, and regulation mechanisms. The impregnation method, characterized by its simple process and low cost, facilitates the convenient loading of active components and is a traditional preparation technique commonly used in industry. The sol-gel method ensures good structural and compositional uniformity of the catalyst, enabling uniform dispersion of active components and providing a structural foundation for stable catalytic performance. Evaporation-induced self-assembly leverages solvent evaporation to drive the self-assembly process, achieving the synergistic construction of active components and supports; this not only simplifies the preparation workflow but also strengthens the interaction between the two. The template method, through the core process of "template guidance-precursor assembly-template removal," enables the precise construction of catalysts with specific pore structures.
By modifying the synthesis method to regulate oxygen vacancy content, active metal atom size, and metal-support interactions, the activity and stability of the catalyst can be improved. Oxygen vacancies serve as key sites for CO2adsorption and activation; their content and distribution directly affect CO2conversion efficiency and the ability to oxidize and remove carbon deposits. Precisely controlling the size of active metal atoms can enhance the exposed crystal facets of the active metal and suppress high-temperature sintering via size effects. Metal-support interaction is core to maintaining catalyst activity and long-term stability. Strengthening SMSI through methods such as in-situ assembly can effectively anchor active metal sites, inhibit particle agglomeration and carbon deposit formation, while simultaneously regulating the electronic state of the metal to optimize CH4and CO2adsorption-dissociation processes, thereby lowering the reaction energy barrier.
Based on existing research progress and the above discussion, this paper summarizes and prospects the development direction of future catalyst structure design, mainly in the following three aspects.
(1) Innovate the system of synthesis methods by coordinating multiple composite preparation techniques to regulate the dispersion of active metals and the key structure of catalysts, thereby solving the dilemma where single preparation methods struggle to balance precision and practicality in catalyst fabrication.
(2) Integrate theoretical simulations with density functional theory calculations or molecular dynamics simulations to reveal the dynamic characteristics of SMSI and the principles by which it regulates catalytic activity. Precisely analyze the formation energy, types, distribution characteristics, and evolution laws of oxygen vacancies from the perspective of electronic structure, clarify the electron transfer rules between them and metal active sites, and quantify the adsorption and dissociation of CH4, CO2 under the synergistic effect of oxygen vacancies and SMSI, as well as the oxidation reaction pathways of carbon deposition species, establishing the interrelationship between microscopic structure and catalytic performance.
(3) Focus on practical industrial applications to break through the limitations of traditional academic research that evaluates performance under ideal conditions. Instead, examine catalyst activity, stability, and resistance to deactivation under operating conditions closer to real industrial environments. For instance, simulate industrial feedstock gas conditions with low purity and multiple impurities, paying attention to the impact of sulfur- and nitrogen-containing impurities in the feedstock on catalyst structural evolution, active site poisoning, and coking behavior. Simultaneously, consider issues present in industrial processes such as temperature fluctuations, changes in space velocity, and imbalances in reactant ratios. Strengthen the connection between laboratory research and actual industrial application conditions to promote the transition of high-performance nickel-based catalysts from laboratory studies to industrial deployment.

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Funding

National Natural Science Foundation of China(52572101)

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