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Article

Influence of Preparation Methods on the Physicochemical and Functional Properties of NiO-CeO2/Al2O3 Catalysts

by
Laura Myltykbayeva
1,
Manshuk Mambetova
1,2,*,
Moldir Anissova
1,
Nursaya Makayeva
1,2,
Kusman Dossumov
1 and
Gaukhar Yergaziyeva
1,2,*
1
Center of Physical Chemical Methods of Research and Analysis, Al-Farabi Kazakh National University, Tole Bi Str. 96A, Almaty 050012, Kazakhstan
2
The Laboratory of Catalytic Processes, Institute of Combustion Problems, Bogenbay Batyr Str. 172, Almaty 050012, Kazakhstan
*
Authors to whom correspondence should be addressed.
J. Compos. Sci. 2025, 9(8), 446; https://doi.org/10.3390/jcs9080446
Submission received: 25 July 2025 / Revised: 13 August 2025 / Accepted: 15 August 2025 / Published: 18 August 2025
(This article belongs to the Section Composites Manufacturing and Processing)
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Abstract

This study presents a comparative investigation of 3Ni2Ce/Al catalysts synthesized via different methods dry impregnation (DI), capillary impregnation (CI), and solution combustion synthesis (SC) for the complete oxidation of methane. The aim was to elucidate the influence of the preparation method on the catalytic activity and reduction behavior of the catalysts. Among the samples tested, the catalyst prepared by the solution combustion method exhibited the highest activity: at 500 °C, the methane conversion reached 82%, compared to 43% and 41% for the 3Ni2Ce/Al (CI) and 3Ni2Ce/Al (DI) prepared catalysts, respectively. At 550 °C, the 3Ni2Ce/Al (SC) catalyst achieved 99% conversion, surpassing the 3Ni2Ce/Al (CI) (72.5%) and 3Ni2Ce/Al (DI) (95%) analogs. Hydrogen temperature-programmed reduction (H2-TPR) analysis revealed that the 3Ni2Ce/Al (SC) catalyst exhibited enhanced hydrogen uptake in the range of 450–850 °C, indicating the presence of more easily reducible NiO species interacting with CeO2 and the alumina support. Scanning electron microscopy (SEM) further confirmed a more uniform distribution of the active phase on the surface of the 3Ni2Ce/Al (SC) catalyst in comparison to the impregnated samples. Overall, the findings demonstrate that the preparation method has a significant impact on the development of a redox-active catalyst structure. The superior performance of the SC-derived catalyst in methane oxidation is attributed to its improved reducibility and homogenous morphology, making it a promising candidate for high-temperature catalytic applications.

1. Introduction

Total oxidation of methane is one of the most relevant and important processes in the field of waste gas purification and reduction in emissions of greenhouse gas. Methane, the main component of natural gas, is one of the most potentially harmful greenhouse gases, strongly influencing Earth’s climate change. Flameless catalytic combustion of methane in special burners to CO2 and H2O (1) with heat release is the most rapidly developing area of modern fundamental and applied catalysis [1].
CH4 + 2O2 → CO2 + 2H2O + 890.31 kJ/mol
The methane total oxidation process is very important in industry as it is used to purify burning gases produced by industries, vehicles and catalytic heat generators. Methane is the most difficult compound to oxidize among lower hydrocarbons, so its oxidation requires catalysts. Catalysts have an important role in the total oxidation of methane, as they activate the methane oxidation reaction at lower temperatures and increase the efficiency of the process. They also promote selective methane oxidation, minimizing the formation of non-thermodynamically stable products such as methanol and formaldehyde.
Catalysts for total oxidation processes must provide selective formation of CO2 and prevent the appearance of harmful components (NOx, CO, etc.) in concentrations above sanitary standards
Currently, precious metals such as Pt [2,3], Pd [4,5,6,7,8] or their combinations are employed as the catalysts of methane total oxidation [9]. Practically, precious metals are the only type of catalysts that are often used in real processes. However, the use of catalysts based on precious metals is relatively expensive and is not promising for industrial applications. So in recent years, the focus has been on catalysts based on variable-valence metal oxides [10,11,12,13,14,15] and rare earth elements (REEs) [16,17,18], supported on various caries.
An analysis of the literature has shown [19,20,21,22,23,24,25] that the main components of oxide catalysts are oxides of nickel, cobalt, copper, etc. Nickel-based catalysts are not inferior in activity in the total methane oxidation to catalysts based on precious metals; however, they are less stable.
It is known [26] that the catalyst’s efficiency in the total oxidation of methane is determined based on a number of factors, such as the active phase, the nature of the support, the method of catalyst synthesis and the conditions used during catalyst pretreatment.
Catalyst synthesis methods lead to changes in the physical and chemical characteristics of the catalysts [27]. So, studying the influence of the preparation methods of modified catalysts on their physical and chemical characteristics and properties of catalytic will allow the development of methods for optimal synthesis and effective catalyst composition in methane total oxidation.
Thereby, the aim of the given paper is to comparatively study low-efficiency preparation methods (deep impregnation, capillary impregnation and solution combustion) on the performance of a Ni-Ce/γ-Al2O3 bimetallic catalyst in the total oxidation of methane. The physical and chemical characteristics of catalysts that affect their activity in the reaction have been studied.

2. Experimental Section

2.1. Materials

The following materials were used in this study: γ-Al2O3 (Shanghai Jiuzhou Chemicals Co., Ltd., Shanghai, China)(surface area ≈180 m2/g, particle size ≈3 mm; Shanghai Jiuzhou Chemicals Co., China), nickel(II) nitrate hexahydrate (Ni(NO3)2·6H2O, GOST 4055-70) (Altey group, Almaty, Kazakhstan), cerium(III) nitrate hexahydrate (Ce(NO3)3·6H2O, TU 6-09-4081-84) (Altey group, Almaty, Kazakhstan),, methane (CH4, purity 99.9999%) and oxygen (O2, purity 99.9999%).

2.2. Preparation of Catalysts

The catalyst xNi/Al (CI) was prepared via the incipient wetness impregnation method using an aqueous solution of Ni(NO3)2·6H2O, applied to γ-Al2O3 support based on its pore volume capacity. Similarly, the xCe/Al (CI) catalyst was synthesized by impregnating the γ-Al2O3 support with an aqueous solution of Ce(NO3)3·6H2O following the same approach.
The xNiyCe/Al (CI) catalysts with varying cerium content were also prepared via incipient wetness impregnation using aqueous solutions of Ni(NO3)2·6H2O and Ce(NO3)3·6H2O. This method involves impregnating the support with metal nitrate solutions in volumes corresponding to its pore volume, resulting in the uniform distribution of the active components on the external surface in the form of a “shell”.
The xNiyCe/Al (DI) catalyst was prepared by the wet impregnation method, wherein the support was immersed in an excess amount of aqueous solutions of Ni(NO3)2·6H2O and Ce(NO3)3·6H2O, completely covering the support.
The xNiyCe/Al (SC) catalyst was synthesized via the solution combustion method. Initially, the γ-Al2O3 support was impregnated with an aqueous solution of a dispersing agent and dried at room temperature. Subsequently, aqueous solutions of Ni(NO3)2·6H2O and Ce(NO3)3·6H2O were simultaneously added to the sample. Urea was used as the fuel and dispersing agent. All samples were subjected to identical thermal treatment: drying at 300 °C for 2 h followed by calcination at 500 °C for 3 h.
The nickel content in all catalysts was fixed at 3 wt.%, while the cerium content varied from 1 to 5 wt.%. In the catalyst designations xNi/Al and xNiyCe/Al, the values x and y indicate the weight percentage of the respective metal oxides in the catalyst.

2.3. Catalytic Tests

The catalytic performance of the synthesized samples in the deep oxidation of methane was evaluated using a laboratory-scale fixed-bed flow reactor setup (Figure 1). The reactor was made of quartz glass with a height of 125 mm and an inner diameter of 11.0 mm. During the experiments, the reactor was positioned vertically. A mixed gas stream (CH4:O2:N2) was introduced from the top into the catalytic zone and, after passing through the catalyst bed, was directed to a gas chromatograph for product analysis. The temperature inside the reactor was monitored using a chromel–alumel thermocouple placed inside a quartz sheath and controlled by a Varta-720 temperature controller (No. 9) with an accuracy of ±1%. Gas analysis was performed using a “Chromos GC-1000” gas chromatograph equipped with thermal conductivity detectors (TCDs).
The chromatographic separation was carried out using packed columns (length: 2 m, inner diameter: 3 mm) filled with NaX (2 columns) and Porapak N (1 column) sorbents. Helium and argon were used as carrier gases. Quantitative analysis was conducted by absolute calibration with reference gases (methane, carbon dioxide, and oxygen), followed by the construction of calibration curves. The reaction monitoring, including gas feed rates and chromatographic data, was carried out in real time using a personal computer.
The process conditions were as follows: atmospheric pressure, temperature was set in the range of 350–600 °C, the ratio was N2:CH4:O2 = 78:2.5:19.5%, and the catalyst volume in the reactor was 2 mL. Conversion was calculated by the following equation:
X C H 4 = [ C H 4 ] i n − [ C H 4 ] o u t [ C H 4 ] o u t

2.4. Catalyst Characterization

SEM analysis was carried out on a JEOL JSM-6390 LA device with a JED 2300 energy-dispersive X-ray detector. An image of the surface of the coatings is obtained using a secondary electron detector, which has the highest lateral resolution (up to 3.5 nm). Images are taken in high and low vacuum modes. In the low vacuum mode, the microscope chamber is blown with water vapor so that the working pressure in the chamber is 100–120 Pa. This ensures a good outflow of excess negative charge from the sample. The calculation of the content of elements in the material being studied is carried out using the program supplied with the scanning electron microscope.
The textural properties of the developed catalysts (specific surface area (Ssp), pore volume and pore size distribution) were determined by low-temperature nitrogen adsorption at 77 K using a BEL Japan Inc. automatic setup, and thermal argon desorption was determined using a BELSORP-mini II device. Up to three samples can be analyzed independently of each other on the device. The experimental time is 3 h. Saturated steam pressure is 102.19 kPa., and Vm = 30.563 cm3(STP) g−1. The samples were decontaminated under a vacuum (1.33 × 10−2 Pa) at 200 °C before analysis. Surface area is calculated according to the BET equation.
XRD patterns of the catalyst were carried out on MiniFlex 600 with CuKa radiation diffractometers, K-beta(x2) filter. The diffractogram filming conditions were as follows: U = 40 kV; I = 15 mA; shooting θ-2θ; and detector 10 °C/min. XRD patterns on a semi-quantitative basis were analyzed using diffractograms of powder samples using the technique of equal portions and synthetic mixtures. The numerical ratios of the crystal phases were established. The interpretations of the diffractogram were carried out using data from the PDXL 2 card file: PDF 2 powder diffractometric database (Powder Diffraction File).
Temperature-programmed reduction (TPR-H2) was carried out on the laboratory installation Universal Sorption Gas Analyzer (USGA-101), which includes a gas treatment system, a reactor (inner diameter 4 mm) with a tubular oven and a thermal conductivity detector. The sample (106 mg, fraction 0.125 mm) was pre-blown with Ar at 480 °C for 40 min, following cooling to 50 °C, and then heated at a rate of 100 °C/min from 50 to 950 °C in a mixture flow of 15 vol.% H2 in Ar at a feed rate of 30 cm3/min. The variation in the hydrogen concentration in the flow was controlled using a thermal conductivity detector. Quantitative determination of absorbed hydrogen was carried out using a calibration based on the recovery of precise amounts of metal oxide.

3. Results and Discussion

The morphology of the catalysts was investigated using scanning electron microscopy (Figure 2). The results indicate that the catalyst synthesized by the solution combustion method contains smaller particles compared to those prepared via incipient wetness and wet impregnation methods. This, in turn, leads to a larger particle surface area, which is consistent with the BET surface area measurements.
The specific surface areas of the samples are as follows: 3Ni2Ce/Al (DI) = 102.12 m2/g, 3Ni2Ce/Al (CI) = 116.86 m2/g and 3Ni2Ce/Al (SC) = 124.83 m2/g.
X-ray diffraction (XRD) analysis was performed to compare the phase compositions of the samples Al2O3, 3Ni/Al (CI), 3Ni2Ce/Al (CI), 3Ni2Ce/Al (SC) and 3Ni2Ce/Al (DI) (Figure 3).
The XRD patterns of all samples clearly exhibit diffraction peaks corresponding to γ-Al2O3 (2θ ≈ 19.4°, 37.5°, 45.6° and 67.0°), indicating the preservation of the crystalline structure of the support after the deposition of active components. In the 3Ni/Al (CI) catalyst, reflections attributed to NiO (2θ ≈ 36.7°, 43.3° and 62.9°) are observed, along with weak peaks of the spinel phase NiAl2O4 (2θ ≈ 31.4°, 37.2°, 45.5° and 65.2°), suggesting partial interaction between nickel and the alumina support during thermal treatment [28,29].
The introduction of CeO2 (samples 3Ni2Ce/Al) results in additional reflections at 2θ ≈ 28.5°, 33.1° and 47.3°, characteristic of the fluorite-type structure of CeO2 [30]. At the same time, the intensity of NiO peaks significantly decreases in all Ce-containing catalysts, particularly in those synthesized by the SC and DI methods. This may indicate either higher dispersion of nickel or its partial incorporation into the CeO2 lattice, consistent with the formation of defective oxide structures of the NiCeOx type, as reported in the literature [31,32,33].
In the 3Ni2Ce/Al (CI) sample, weak reflections of NiAl2O4 are still observed, although their intensity is lower than in 3Ni/Al. The most intense CeO2 peaks and the suppression of NiAl2O4 signals are observed in the catalyst synthesized by the SC method, indicating minimal interaction between nickel and γ-Al2O3 and the probable formation of a Ni–Ce–O phase [32,34].
To investigate the reduction characteristics of the catalysts, H2 temperature-programmed reduction (H2-TPR) analysis was performed. Figure 4 presents the H2-TPR profiles of 3Ni/Al, 2Ce/Al, and 3Ni2Ce/Al catalysts prepared by the capillary impregnation method.
The 2Ce/Al catalyst exhibits reduction peaks at 192, 430, 558–640 and 804 °C. The low-temperature peak at 192 °C is attributed to the reduction of surface Ce4+ species, while the peaks at 430 °C and 558–640 °C correspond to the reduction of dispersed and bulk CeO2 particles. The high-temperature peak at 804 °C is associated with the reduction of thermally stable Ce–O–Al phases formed due to strong cerium–alumina interactions, consistent with literature data [29].
The 3Ni/Al catalyst shows four main peaks at 455, 545, 664 and 815 °C, corresponding to the reduction of free NiO, NiO weakly and strongly interacting with the support and the spinel phase NiAl2O4, respectively [35,36,37,38].
After modification of 3Ni/Al with CeO2 (3Ni2Ce/Al), the reduction temperature of surface CeO2 shifts to lower values, as indicated by the decrease in peak temperature from 192 °C to 164 °C [39,40]. A new peak at 286 °C appears, which can be attributed to the reduction of Ni2+ species interacting with CeO2 [31]. Additional peaks at 640 °C and 675 °C are related to the reduction of nickel and cerium oxides strongly interacting with the support.
The effect of the synthesis method on the reducibility of 3Ni2Ce/Al catalysts is presented in Figure 5 and Table 1. All TPR profiles exhibit characteristic peaks within the ranges of 165–223 °C, 290–450 °C, 658–675 °C and 786–787 °C. According to the literature [41,42], the low-temperature region (165–223 °C) corresponds to the reduction of free or weakly bound NiO particles on the Al2O3 surface. The mid-temperature region (290–450 °C) is attributed to the reduction of finely dispersed NiO species interacting with CeO2. Peaks in the 658–675 °C range are associated with the reduction of NiO, strongly interacting with both CeO2 and the support. The high-temperature peak at 786–787 °C is linked to the reduction of nickel aluminate phases.
The most significant differences between the catalysts were observed in the high-temperature region (450–850 °C). The catalyst synthesized via the solution combustion method exhibited the highest hydrogen consumption within the ranges of 450–750 °C and 750–850 °C, compared to those prepared by capillary and incipient wetness impregnation methods. This behavior may indicate the presence of a substantial number of oxygen vacancies capable of participating in redox cycles [41,42].
The effect of CeO2 content on methane conversion and specific surface area of 3Ni/Al catalysts prepared via capillary impregnation was studied in the deep methane oxidation reaction at 400 °C. The ceria content was varied in the range of 1–5 wt.% (Figure 6).
As shown in Figure 6, increasing the CeO2 content from 1 to 2 wt.% leads to a significant rise in methane conversion from 11% to 30%, which is accompanied by an increase in the specific surface area of the catalyst from 73 to 125 m2/g. Although the literature reports that specific surface area is not always the key factor in high-temperature reactions [43,44], in this case, the optimal CeO2 content appears to enhance NiO dispersion, strengthen Ce–Ni interactions, and increase the concentration of oxygen vacancies involved in methane activation [45].
Moreover, in the sample containing 2 wt.% CeO2, temperature-programmed reduction (TPR) results suggest the formation of additional active oxygen species, which may account for the high catalytic performance (see Figure 5). The decrease in both catalytic activity and specific surface area with a further increase in ceria content could be attributed to surface saturation with CeO2, which may reduce surface area and potentially inhibit adsorption of active oxygen species required for efficient total oxidation of methane. Similar limitations at high modifier loadings have been reported in the literature, where excess La2O3, for example, was shown to reduce the availability of oxygen centers [46].
The catalytic activity of 3Ni/Al, 2Ce/Al and 3Ni2Ce/Al catalysts in the deep oxidation of methane under atmospheric pressure in the temperature range of 300–600 °C is shown in Figure 7.
A comparative study of catalytic activity demonstrated that increasing the reaction temperature from 300 to 600 °C leads to a significant rise in methane conversion across all catalysts. For the 3Ni/Al and 2Ce/Al catalysts, methane conversion increased from 9% to 95% and from 6% to 93%, respectively. The incorporation of cerium oxide into the 3Ni/Al system resulted in a marked enhancement of catalytic performance: for the 3Ni2Ce/Al catalyst, conversion increased from 10% to 99% with rising temperature. The most pronounced improvement was observed in the temperature range of 350–550 °C. This enhancement is attributed to the formation of nanosized clusters with active catalytic components (Ni and NiO) and the role of CeO2 as an oxygen storage material, supplying active oxygen species required for deep methane oxidation [47].
The low activity observed at temperatures below 450 °C can be explained by the high activation energy (~104 kcal/mol) required to cleave the C–H bonds in methane molecules, and the need for in situ reduction of NiO to the active metallic phase, which typically occurs at elevated temperatures [39].
Subsequently, the influence of the preparation method on the catalytic activity of 3Ni2Ce/Al in the deep oxidation of methane was investigated (Figure 8).
The investigation of the effect of synthesis methods on the catalytic activity of the 3Ni2Ce/Al catalyst in the deep oxidation of methane at 500 °C demonstrated that the highest methane conversion (82%) was achieved with the catalyst synthesized via the solution combustion method. In contrast, the catalysts prepared by capillary impregnation (CI) and incipient wetness impregnation (DI) exhibited significantly lower methane conversions of 43% and 41%, respectively.
To explain the observed differences in catalytic activity, temperature-programmed reduction (H2-TPR) data were analyzed, and the fraction of reduced active nickel species within specific temperature ranges was calculated. For the catalyst obtained by the solution combustion method, the reduced fraction of active phase in the 400–850 °C range reached approximately 80%, notably higher than the corresponding values for the 3Ni2Ce/Al (CI) (60%) and 3Ni2Ce/Al (DI) (54%) samples (Table 1).
In contrast, within the low-temperature region (<400 °C), a larger fraction of nickel was reduced in the catalysts synthesized by 3Ni2Ce/Al (DI) and 3Ni2Ce/Al (CI) methods (40% and 33%, respectively), indicating weaker metal–support interactions and the presence of larger NiO particles [42].
The superior performance of the 3Ni2Ce/Al catalyst synthesized via solution combustion is directly correlated with a higher proportion of reducible Ni species at elevated temperatures. This is indicative of finely dispersed nickel particles strongly anchored to the Ce–Al matrix and a greater density of oxygen vacancies [48]. These structural features promote more efficient dissociative adsorption of methane and oxygen at active sites, thereby enhancing catalytic activity and resistance to sintering [49,50].
A comparison of the catalytic activity of the studied catalyst with that reported in the literature is presented in Table 2. Conversion rates in deep methane oxidation depend significantly on the gas hourly space velocity (GHSV). Increasing GHSV reduces the contact time of the reactants with the catalyst, increasing the effect of mass transfer limitations and reducing conversion at a given temperature [51]. In this work, GHSV = 2000 h−1 was chosen, which allows minimizing external diffusion limitations and correctly comparing the catalytic properties of samples obtained by different synthesis methods.

4. Conclusions

In summary, the synthesized low-percentage 3Ni2Ce/Al catalysts, prepared via incipient wetness impregnation (DI), capillary impregnation (CI), and solution combustion (SC), exhibit distinct catalytic performances in the deep oxidation of methane, depending on the preparation method. The catalyst synthesized by the solution combustion method demonstrated the highest efficiency: At 500 °C, it achieved 82% methane conversion, surpassing the 3Ni2Ce/Al (CI) and 3Ni2Ce/Al (DI) catalysts, which showed 43% and 41% conversion, respectively. Upon further temperature increase to 550 °C, the activity of the 3Ni2Ce/Al (SC) catalyst reached 99%, compared to 72.5% and 95% for the 3Ni2Ce/Al (CI) and 3Ni2Ce/Al (DI) catalysts, respectively.
X-ray diffraction analysis revealed weak signals of Ni and Ce oxides due to their low loading. However, in the 3Ni2Ce/Al (SC) sample, additional diffraction reflections were observed, which may indicate the formation of a solid solution between NiO and CeO2, in agreement with literature data. According to the H2-TPR results, the 3Ni2Ce/Al (SC) catalyst exhibited pronounced reduction peaks in the 450–850 °C range, suggesting the presence of NiO species strongly interacting with CeO2 and the support. This indicates the formation of thermally stable, redox-active nickel species.
Moreover, SEM analysis confirmed a more homogeneous dispersion of the active phase on the surface of the 3Ni2Ce/Al (SC) catalyst compared to the impregnated counterparts. Thus, the solution combustion method promotes the formation of a catalyst with enhanced reducibility and uniform morphology, ensuring its superior performance in the deep oxidation of methane.

Author Contributions

Conceptualization, L.M. and G.Y.; methodology, L.M., G.Y. and K.D.; validation, M.A.; formal analysis, N.M. and M.M.; investigation, L.M. and M.A.; resources, G.Y. and K.D.; data curation, L.M. and G.Y.; writing—original draft preparation, L.M. and G.Y.; writing—review and editing, G.Y., M.M. and L.M.; supervision, project administration, and funding acquisition, M.A. All authors have read and agreed to the published version of the manuscript.

Funding

This research has been funded by the Ministry of Science and Higher Education of the Republic of Kazakhstan (Grant No. AP19678248).

Data Availability Statement

Data are contained within the article.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. Scheme of the laboratory catalytic equipment.
Figure 1. Scheme of the laboratory catalytic equipment.
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Figure 2. Microphotographs of catalysts: (a) 3Ni2Ce/Al (DI); (b) 3Ni2Ce/Al (CI); (c) 3Ni2Ce/Al (SC).
Figure 2. Microphotographs of catalysts: (a) 3Ni2Ce/Al (DI); (b) 3Ni2Ce/Al (CI); (c) 3Ni2Ce/Al (SC).
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Figure 3. XRD patterns of fresh catalysts.
Figure 3. XRD patterns of fresh catalysts.
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Figure 4. H2-TPR profiles of catalysts.
Figure 4. H2-TPR profiles of catalysts.
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Figure 5. H2-TPR profile of catalysts: 1—3Ni2Ce/Al (DI); 2—3Ni2Ce/Al (CI); 3—3Ni2Ce/Al (SC).
Figure 5. H2-TPR profile of catalysts: 1—3Ni2Ce/Al (DI); 2—3Ni2Ce/Al (CI); 3—3Ni2Ce/Al (SC).
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Figure 6. Effect of ceria content on the catalytic activity and specific surface area of 3Ni/Al catalyst at 400 °C.
Figure 6. Effect of ceria content on the catalytic activity and specific surface area of 3Ni/Al catalyst at 400 °C.
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Figure 7. Effect of reaction temperature on the activity of 3Ni/Al, 2Ce/Al and 3Ni2Ce/Al catalysts in the deep oxidation of methane.
Figure 7. Effect of reaction temperature on the activity of 3Ni/Al, 2Ce/Al and 3Ni2Ce/Al catalysts in the deep oxidation of methane.
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Figure 8. Effect of synthesis method and reaction temperature on the activity of 3Ni2Ce/Al catalysts in the deep oxidation of methane.
Figure 8. Effect of synthesis method and reaction temperature on the activity of 3Ni2Ce/Al catalysts in the deep oxidation of methane.
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Table 1. Reduced fraction of the active phase of 3Ni2Ce/Al catalysts prepared by different synthesis methods in various temperature intervals (%).
Table 1. Reduced fraction of the active phase of 3Ni2Ce/Al catalysts prepared by different synthesis methods in various temperature intervals (%).
Samples<400 °C, %400–850 °C, %>850 °C, %
3Ni2Ce/Al (SC)15.080.05.0
3Ni2Ce/Al (CI)33.060.07.0
3Ni2Ce/Al (DI)40.054.06.0
Table 2. Comparison of catalytic activity of catalysts in the reaction of deep oxidation of methane.
Table 2. Comparison of catalytic activity of catalysts in the reaction of deep oxidation of methane.
YearSampleCalcination
Temperature and Time		Initial Gases Space Velocity, h−1Process
Temperature, °C		Conversion of CH4, %Preparation CatalystRef.
20253Ni2Ce/Al (SC)550 °C for 6 hN2:CH4:O2 = 78:2.5:19.52000500
600		82
100		capillary impregnationThis work
2009NiO/Ce0.75Zr0.25O2 He:CH4:O2 = 87.5:3.0:1039,00060060wetness impregnation[52]
2018Ce0.6Fe0.4O2-δ500 °C for 2 hN2:CH4:O2 = 89:1.0:2030,00050075wetness impregnation[53]
2019Co/CeO2-H500 °C for 5 hHe:CH4:O2 = 89.5:0.5:1025,00060090wetness impregnation[54]
2019Cu(15) CeMgAlO750 °C for 8 hCH4:Air = 1.0:99.016,00055090coprecipitation[55]
2019Pt/γ-Al2O3600 °C for 4 hN2:CH4:O2 = 89.8:0.2:1030,000550100impregnating[56]
2020Pd/Al2O3600 °C for 2 hAr:CH4:O2 = 97:1.0:2.0 45020incipient wetness impregnation[57]
2020CeO2-S500 °C for 4 hAr:CH4:O2 = 80:1.0:1920,00055097wet impregnation[58]
2020NiO/CeO2450 °C for 4 hAr:CH4:O2 = 95:1.0:4.015,000600100wetness impregnation[59]
2020Co/20Ce-Al600 °C for 4 hN2:CH4:O2 = 89:1.0:1015,00060095basic precipitation[60]
2020Ni9Mg550 °C for 6 hHe:CH4:O2 = 89:1.0:1010,00060094co-precipitation[61]
2021LaNi0.5Mn0.5O3800 °C for 4 hHe:CH4:O2 = 88:1.0:2145,00056050coprecipitation
and Pechini sol–gel		[62]
2023Pd-CeO2-cube catalyst-0.05% to 0.5% of CH4 leakage in marine natural gas36,000–120,000500100wet impregnation[63]
2024Cu/HAP-Ar:CH4:O2 = 95:1.0:4.039,000600100co-precipitation[64]
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Myltykbayeva, L.; Mambetova, M.; Anissova, M.; Makayeva, N.; Dossumov, K.; Yergaziyeva, G. Influence of Preparation Methods on the Physicochemical and Functional Properties of NiO-CeO2/Al2O3 Catalysts. J. Compos. Sci. 2025, 9, 446. https://doi.org/10.3390/jcs9080446

AMA Style

Myltykbayeva L, Mambetova M, Anissova M, Makayeva N, Dossumov K, Yergaziyeva G. Influence of Preparation Methods on the Physicochemical and Functional Properties of NiO-CeO2/Al2O3 Catalysts. Journal of Composites Science. 2025; 9(8):446. https://doi.org/10.3390/jcs9080446

Chicago/Turabian Style

Myltykbayeva, Laura, Manshuk Mambetova, Moldir Anissova, Nursaya Makayeva, Kusman Dossumov, and Gaukhar Yergaziyeva. 2025. "Influence of Preparation Methods on the Physicochemical and Functional Properties of NiO-CeO2/Al2O3 Catalysts" Journal of Composites Science 9, no. 8: 446. https://doi.org/10.3390/jcs9080446

APA Style

Myltykbayeva, L., Mambetova, M., Anissova, M., Makayeva, N., Dossumov, K., & Yergaziyeva, G. (2025). Influence of Preparation Methods on the Physicochemical and Functional Properties of NiO-CeO2/Al2O3 Catalysts. Journal of Composites Science, 9(8), 446. https://doi.org/10.3390/jcs9080446

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