Transactions of Materials Processing (소성∙가공)

The Korean Society for Technology of Plasticity and materials processing (한국소성∙가공학회)
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Optimization of MIL-53 Metal-organic Framework Coatings for Enhanced Durability in Carbon Dioxide Capture

이산화탄소 포집 성능 향상을 위한 MIL-53 금속-유기 골격체 코팅의 최적화

  • Received : 2024.07.15
  • Accepted : 2024.07.17
  • Published : 2024.08.01
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Abstract

This study aimed to optimize the MIL-53 metal-organic framework coatings for enhanced durability in carbon dioxide capture applications. We synthesized MIL-53 powders using a hydrothermal method and deposited them on stainless-steel substrates by spin coating at various speeds, ranging from 300 to 2,000 rpm. The microstructure, surface properties, and tribological characteristics of the coatings were analyzed systematically. The results indicated that the spin speed significantly impacted the coating uniformity and defect formation. Coatings prepared at moderate speeds of 500 to 1,000 rpm exhibited optimal thickness and density, resulting in superior wear resistance. The tribological tests revealed that the coatings prepared at 700 to 1000 rpm had the lowest wear rates. These findings offer valuable insights for the development of durable MOF-based coatings for carbon dioxide capture and other applications requiring long-term stability under mechanical stress.

Keywords

1. Introduction

Greenhouse gas-induced global warming is emerging as a severe problem worldwide, leading to increased interest in Carbon Capture and Storage (CCS) technology[1, 2]. Among CCS technologies, the capture process using carbon dioxide adsorbents has attracted significant attention owing to its high selectivity and energy efficiency[3, 4]. However, in actual carbon dioxide capture processes, performance degradation issues frequently occur because of friction between adsorbent particles and wear with the inner wall of the adsorption tower. In particular, the repetitive friction and wear that occur during the continuous adsorption/desorption process deteriorates the mechanical strength of the adsorbent, causing problems such as decreased adsorption capacity and increased pressure loss. Therefore, systematic research on friction and wear characteristics is essential to ensure the long-term stability and durability of carbon dioxide adsorbents.

In the carbon dioxide adsorption process, porous materials are used as adsorbents to selectively separate carbon dioxide from gas mixtures[5]. Inorganic-based materials such as zeolites and activated carbon have been primarily used as commercial adsorbents, but recently, Metal-Organic Frameworks (MOFs) have attracted attention as next-generation carbon dioxide adsorbents[6-8]. MOFs are porous crystalline materials formed through coordination bonds between metal ions or clusters and organic ligands, possessing high specific surface areas and regular pore structures, which are highly advantageous for carbon dioxide adsorption. In fact, many MOF materials have been reported to exhibit carbon dioxide adsorption capacities and selectivities that surpass those of existing adsorbents[9, 10]. However, MOF particles generally have high brittleness and low mechanical strength, making it difficult to ensure long-term stability during the carbon dioxide capture process. To overcome this, methods such as complexing MOF particles with polymer binders or coating them through chemical interactions have been proposed[11]. Zhang et al. studied the friction and wear characteristics of Cu-BTC MOF-impregnated epoxy coatings[12]. Although the wear resistance of the coatings improved slightly with the addition of MOFs, the problem of increased delamination was confirmed under high loading conditions. This is considered to be related to the interfacial strength between the MOF particles and polymer matrix, as mentioned earlier. Yang et al. investigated the tribological behavior of MIL-88 MOF particle coatings impregnated with oleylamine[13]. The ultralow friction characteristics of the coatings were manifested by the chemical action of oleylamine, and a self-lubricating mechanism utilizing the porosity of MOFs was proposed. The coating method is gaining attention as an effective way to enhance the mechanical durability while maintaining the physicochemical properties of the MOF particles. However, research on the friction and wear behavior of MOF coatings is still in its early stages, and there is a lack of systematic understanding of the changes in tribological characteristics according to the coating conditions. In the carbon dioxide capture process, the adsorbent coatings inside the adsorption tower are exposed to repetitive friction and deformation caused by fluid flow and thermal expansion. Therefore, the wear resistance of MOF coatings is considered to be a key factor for ensuring long-term stability.

In this study, MIL-53, a representative MOF material, was selected as the coating material, and MIL-53 coatings were fabricated on stainless-steel substrates using the spin-coating method. To improve the uniformity and adhesion of the coatings, coatings were prepared under various spin-coating speeds, and the resulting changes in the microstructure and properties were analyzed. The friction and wear behavior of the fabricated MIL-53 coatings were evaluated through friction tests using the ball-on-reciprocating method, with the aim of assessing the long-term durability and applicability of MIL-53 coatings to the carbon dioxide capture process. The optimized fabrication conditions and tribological characterization results of the MIL-53 coatings derived from this study are expected to serve as important fundamental data for the commercialization of MOF-based carbon dioxide adsorbents.

2. Materials and methods

In this study, hydrothermal synthesis was prepared MIL-53 powder. Fig. 1 illustrates the synthesis process of the MIL-53 powder. The metal salt Al(NO3)3·9H2O and the organic linker terephthalic acid (TPA) were mixed in a weight ratio of 6:4 and completely dissolved in a mixed solvent of 100 mL N,N-Dimethylformamide (DMF) and 2 mL deionized water. During this process, coordination bonds are formed between Al3+ ions and TPA molecules. The homogeneous solution was transferred to an autoclave and subjected to hydrothermal reaction for 28 h in a vacuum oven at 150 °C. The synthesized solution was centrifuged at 2000 rpm for 30 min, washed three times with DMF, and dried to obtain a pure MIL-53 powder.

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Fig. 1 Schematic illustration of the hydrothermal synthesis of MIL-53 powders

MIL-53 coatings were fabricated on SUS 304 substrates using a spin-coating method. Fig. 2 shows a schematic of the spin coating process. The coating solution was prepared by dispersing 0.3 wt.% MIL-53 powder in DMF. The coating solution was dropped onto a cleaned SUS 304 substrate and spin coating was performed for 60 s at rotational speeds of 300, 500, 700, 1000, 1500, and 2000 rpm. During the spin-coating process, the coating solution spreads uniformly on the substrate surface owing to centrifugal force, and simultaneously, the solvent evaporates, forming a thin film coating layer with MIL-53 particles evenly distributed on the substrate. The rotational speed of the spin coating is a major process variable that determines the final thickness and microstructure of the coating layer. The coated samples were dried in a vacuum oven at 70 °C for 1 h to remove residual solvent. The MIL-53 coatings were designated as M-300 (300 rpm), M-500 (500 rpm), M-700 (700 rpm), M-1000 (1,000 rpm), M-1500 (1,500 rpm), and M-2000 (2,000 rpm) according to the speed conditions.

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Fig. 2 Schematic of the spin-coating process for fabricating MIL-53 coatings on SUS 304 substrates

The surface morphology of the fabricated MIL-53 coatings was observed using an optical microscope and the surface roughness was measured using a stylus profilometer. Surface wettability was evaluated by measuring the static contact angle of the water droplets using a contact-angle goniometer. Furthermore, friction tests using the ball-on-reciprocating method were performed to evaluate the tribological characteristics of the MIL-53 coatings. An SUS 304 ball with a diameter of 1 mm was used as the counter tip, and the reciprocating motion was repeated for 100 cycles with a reciprocating speed of 4 mm/s and a stroke of 2 mm under a normal load of 20 mN. After the tests, the morphology and depth of the wear tracks were analyzed using an optical microscope and a 2D profilometer, and the wear rate was calculated by dividing the wear volume by the normal load and total sliding distance[14, 15]. All experiments were repeated at least three times to ensure reliability, and the average values were used for the analysis.

3. Results and discussion

Fig. 3 shows the optical microscope observations of the morphology of the Al(NO3)3·9H2O powder and the hydrothermally synthesized MIL-53 powder. The starting material, Al(NO3)3·9H2O, exhibited a transparent crystalline particle form, while MIL-53 was obtained as a fine white powder. This suggests that the unique porous crystal structure of MIL-53 was successfully formed through coordination bonds between Al3+ ions and TPA molecules during the hydrothermal synthesis process[16]. Hydrothermal synthesis is one of the widely used representative methods for MOF synthesis, following the principle of forming porous structures through the self-assembly of metal ions and organic linkers under high-temperature and high-pressure conditions[17]. In this study, MIL-53 crystal nuclei were formed through coordination bonds between Al3+ ions and TPA molecules, and a stable crystalline phase was obtained through their continuous bonding and growth. The synthesized MIL-53 powder was expected to exhibit unique physicochemical properties, such as specific surface area, pore characteristics, and adsorption performance.

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Fig. 3 Optical microscopy images of (a) Al(NO3)3·9H2O precursor; (b) as-synthesized MIL-53 powders

Fig. 4 shows the optical microscope images of the surface morphology of the MIL-53 coatings fabricated under different spin-coating conditions. In all conditions, it was confirmed that MIL-53 particles were coated on the SUS 304 substrate, but the uniformity of the coating layer and the nature of the defects varied depending on the spin-coating speed. In the case of the low-speed sample M-300, a coating layer with MIL-53 particles non-uniformly agglomerated was observed. This is interpreted as a result of the low flowability of the coating solution at a low speed of 300 rpm, which prevents complete spreading and leads to the formation of a nonuniform liquid film. In contrast, relatively uniform coating layers were obtained in the medium-speed samples M-500 and M-700. This is attributed to the formation of a uniform liquid film due to the appropriate flowability and spreadability of the coating solution in the spin-coating speed range of 500-700 rpm. On the other hand, in the high-speed samples M-1000, M-1500, and M-2000, uniform coating layers were formed throughout the samples, but localized coating defects were observed as the rotational speed increased. In particular, a relatively large number of defects were distributed in the M-2000 sample fabricated at the highest rotational speed of 2,000 rpm. The reason for the increased occurrence of defects under high-speed conditions is interpreted as the weakening of the cohesion between MIL-53 particles within the coating layer due to the excessively high centrifugal force, and simultaneously, the formation of defects such as microcracks within the coating layer due to rapid solvent evaporation. Therefore, medium-speed conditions in the range of 500-1,000 rpm are considered suitable for achieving uniform and defect-free MIL-53 coating layers.

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Fig. 4 Optical microscope images of MIL-53 coatings fabricated at different spin-coating speeds: (a) M-300; (b) M-500; (c) M-700; (d) M-1000; (e) M-1500; (f) M-2000

Fig. 5 shows the variation in the surface roughness (Ra) of the MIL-53 coatings with the spin coating speed. The surface roughness was highest at 1.63 μm in the low-speed coating condition sample M-300 and gradually decreased with increasing coating speed, reaching the lowest value of 0.57 μm in the medium-speed coating condition sample M-700. Thereafter, the surface roughness showed a slight increasing trend with increasing speed, and the Ra values of the M-500, M-1000, M-1500, and M-2000 samples were 0.95, 0.61, 0.72, and 0.66 μm, respectively. These changes in the surface roughness are closely related to the uniformity and defect occurrence tendency of the coating layer according to the spin-coating speed[18]. Under low-speed conditions, a rough surface is formed owing to the non-uniform spreading of the coating solution, whereas under medium-speed conditions, a smooth surface is obtained owing to the formation of a uniform and dense coating layer. However, under high-speed conditions, it is considered that the surface roughness increases again owing to the occurrence of coating layer defects caused by excessive centrifugal force. This suggests that the selection of an appropriate spin-coating speed is important for controlling the uniformity and defects of MIL-53 coating layers.

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Fig. 5 Surface roughness (Ra) of MIL-53 coatings as a function of spin-coating speed

Fig. 6 shows the water droplet contact angle results measured to evaluate the surface wettability of MIL-53 coatings. The contact angle was the highest at 121.19° in the low-speed coating condition sample M-300 and gradually decreased with increasing coating speed, reaching the lowest value of 110.61° in the high-speed coating condition sample M-2000. The measured contact angles of the M-500, M-700, M-1000, and M-1500 samples were 117.38°, 116.46°, 115.22°, and 114.03°, respectively. These changes in the contact angle are attributed to the differences in surface roughness observed earlier[19]. In the case of low-speed coating samples with rough surfaces, the contact area with water droplets decreases, resulting in high hydrophobicity, whereas medium-speed and high-speed coating samples with smooth surfaces exhibit relatively low hydrophobicity. However, in the case of the M-2000 sample with the thinnest coating layer, the inherent hydrophobicity of the MIL-53 material and the influence of the substrate act together, resulting in a significant decrease in the contact angle.

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Fig. 6 Water contact angles of MIL-53 coatings fabricated at different spin-coating speeds

Fig. 7 shows the variation in the friction coefficient of the MIL-53 coatings with the spin coating speed. During the 100-cycle reciprocating friction test, periodic fluctuations in the friction coefficient were observed in all samples; however, the magnitude of fluctuations and stability varied among the samples. In the case of the low-speed coating condition of sample M-300, the friction coefficient initially showed a level of 1.0, then increased to a level of 1.5 after 50 cycles, and then gradually decreased. In the medium-speed coating condition samples M-500 and M-700, the friction coefficient initially showed a level of 0.9-1.0, increased to a level of 1.3-1.5 in the 20-30 cycle range, and then stabilized at a level of 1.25-1.30 with somewhat unstable behavior. In contrast, in the case of the high-speed coating condition samples M-1000, M-1500, and M-2000, the initial friction coefficient of 1.0 rapidly increased in the 5-20 cycle range, reaching a maximum level of 1.75-2.0, and then maintained a high friction coefficient of 1.5-1.9 while repeating large fluctuations. These differences in friction behavior are attributed to differences in the thickness and durability of the MIL-53 coating layers[20]. In the case of low- and medium-speed coating samples with relatively thick coating layers, the friction coefficient is initially maintained low owing to the MIL-53 coating layer, but as the coating layer gradually wears out owing to repeated shear stress, the underlying SUS substrate is exposed, resulting in an increase in the friction coefficient. Thereafter, it can be interpreted that the wear particles acted as lubricants, maintaining a stable friction coefficient. On the other hand, in the case of high-speed coating samples, a thin and dense coating layer is formed that initially exhibits a low friction coefficient, but is easily destroyed by repeated stress, resulting in direct contact with the substrate and a rapid increase in the friction coefficient. In particular, the thinnest M-2000 coating layer was mostly delaminated within a few cycles, resulting in dominant direct friction with the substrate and leading to the highest and most unstable friction coefficient.

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Fig. 7 Friction coefficient history of MIL-53 coatings as a function of sliding cycles at different spin-coating speeds

Fig. 8 shows the average friction coefficient of each MIL-53 coating sample. The average friction coefficient showed a continuously increasing trend with increasing spin coating speed, measuring 1.30 in the low-speed coating condition sample M-300, 1.32 and 1.38 in the medium-speed coating condition samples M-500 and M-700, respectively, and 1.48, 1.58, and 1.86 in the high-speed coating condition samples M-1000, M-1500, and M-2000, respectively. These changes in the average friction coefficient are closely related to the wear resistance characteristics of the MIL-53 coating layers. The coating layers formed under low- and medium-speed coating conditions exhibit excellent wear resistance based on appropriate thickness and density, maintaining a low average friction coefficient, while the thin coating layers formed under high-speed coating conditions are easily destroyed and delaminated during the repeated friction process owing to low durability, which causes direct contact with the substrate, resulting in a high average friction coefficient.

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Fig. 8 Average friction coefficients of MIL-53 coatings fabricated at different spin-coating speeds

Fig. 9 shows a quantitative comparison of the widths and depths of the wear tracks formed after the friction tests. The wear width was smallest at 0.17 mm in the low-speed coating condition sample M-300, while the medium-speed and high-speed coating condition samples M-500, M-700, M-1000, and M-1500 showed similar values of 0.21 mm. In contrast, the widest wear width (0.27 mm was observed for the M-2000 sample, which had the highest coating speed. On the other hand, in the case of wear depth, the low-speed coating condition sample M-300 showed the highest value of 2.53 μm, while the medium-speed coating condition samples M-500, M-700, and M-1000 exhibited a gradual decreasing trend with increasing coating speed, measuring 1.53, 1.36, and 0.94 μm, respectively. The wear depths of the high-speed coating condition samples M-1500 and M-2000 were measured as 0.99 and 1.04 μm, respectively. These changes in the wear width and depth are considered to be due to the differences in the thickness and density of the MIL-53 coating layers. In the case of low-speed coating samples, the contact area between the ball and the coating layer decreases owing to the thick coating layer, resulting in a small wear width; however, the low coating layer hardness leads to localized plastic deformation and fatigue failure, significantly increasing the wear depth. In contrast, the medium-speed coating samples exhibited excellent wear resistance based on the optimized thickness and density of the coating layer, resulting in a significant decrease in wear depth. On the other hand, in the case of the high-speed coating samples, the load-bearing capacity was greatly reduced owing to the thin coating layer, leading to an increase in wear width owing to the increased contact area between the ball and the coating layer, and an increase in wear depth due to the exposure of the substrate.

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Fig. 9 Wear track width and depth of MIL-53 coatings fabricated at different spin-coating speeds: (a) wear width; (b) wear depth

Fig. 10 compares the wear rates of the MIL-53 coatings according to the spin-coating speed. The wear rate was lowest at 2.92 × 10-5 mm3/N·mm in the medium-speed coating condition sample M-1000 and highest at 5.38 × 10-5 mm3/N·mm in the low-speed coating condition sample M-300. The wear rates of M-500, M-700, M-1500, and M-2000 samples were measured as 4.06 × 10-5, 3.78 × 10-5, 3.42 × 10-5, and 4.75 × 10-5 mm3/N·mm, respectively. These changes in wear rate are consistent with the trends in wear width and depth explained earlier, indicating that the MIL-53 coating layer formed under medium-speed coating conditions exhibits excellent wear resistance. In contrast, under low-speed coating conditions, the wear rate significantly increased owing to the plastic deformation and fatigue failure caused by the low hardness of the coating layer. Under high-speed coating conditions, the wear rate was high because of the rapid destruction and delamination of the thin coating layer.

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Fig. 10 Wear rates of MIL-53 coatings fabricated at different spin-coating speeds

Fig. 11 shows the morphology of the wear tracks observed using optical microscopy after the friction tests. In all samples, wear tracks formed by ball-coating layer contact were clearly observed, and abraded wear particles were distributed inside the tracks. In the low-speed coating samples M-300 and M-500, deep and narrow wear tracks were observed, and a large amount of plastic deformation traces and delaminated coating layer fragments were identified inside the tracks. This is interpreted as a result of the rapid progression of plastic deformation and fatigue failure of the coating layer at the contact area where the load is concentrated owing to the low support of the thick coating layer. In contrast, relatively shallow and smooth wear tracks were observed in the medium-speed coating condition samples M-700 and M-1000, and the localized fatigue failure traces were significantly reduced. This is attributed to the suppression of localized failure as the load at the contact area is evenly distributed owing to the optimized thickness and density of the coating layer. On the other hand, in the high-speed coating condition samples M-1500 and M-2000, a large amount of brittle fracture traces, such as pull-out and cracks, were observed inside the wear tracks. Particularly, in the case of the M-2000 sample, severe fracture behavior was observed to the extent that the underlying substrate was mostly exposed, which is considered to be the result of the excessively thin coating layer failing to support the load and rapid fracturing, as explained earlier.

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Fig. 11 Optical microscope images of wear tracks formed on MIL-53 coatings fabricated at different spin-coating speeds: (a) M-300; (b) M-500; (c) M-700; (d) M-1000; (e) M-1500; (f) M-2000

Taken together, these results indicate that the tribological characteristics of MIL-53 coatings are highly dependent on the thickness and microstructure of the coating layer, according to the spin-coating speed. Under low-speed coating conditions (M-300, M-500), thick and rough coating layers were formed, exhibiting high contact angles and low average friction coefficients, but relatively high wear rates owing to localized plastic deformation and fatigue failure caused by low load-bearing capacity. In contrast, under medium-speed coating conditions (M-700, M-1000), smooth and dense coating layers with optimized thicknesses were formed, exhibiting excellent wear resistance along with low average friction coefficients and appropriate surface hydrophobicity. However, under high-speed coating conditions (M-1500, M-2000), rapid destruction and delamination occurred because of the excessively thin coating layer, resulting in direct contact with the substrate and the highest average friction coefficient and wear rate.

In conclusion, this study utilized the spin-coating method to apply MIL-53 powder as a coating material and investigated the changes in the microstructure and tribological characteristics of MIL-53 coatings according to coating speed. In terms of wear resistance, the M-1000 sample exhibited the lowest wear rate (2.92 × 10-5 mm3/N·mm) and was determined to be the optimal condition. These results suggest that controlling the thickness and density of the coating layer is essential for improving the tribological characteristics of MOF-based coating materials, and that optimization of the spin-coating speed is important for achieving this. The findings of this study are expected to provide useful guidelines for the development of multifunctional surface-coating materials utilizing MOFs, and further research on various applications and commercialization should be conducted in the future.

4. Conclusions

This research demonstrates the critical role of spin-coating speed in optimizing the tribological properties of MIL-53 coatings for carbon dioxide capture applications. Moderate spin speeds (700-1,000 rpm) produced coatings with an ideal balance between thickness and density, resulting in superior wear resistance and low friction coefficients. Specifically, the coatings prepared at 1000 rpm exhibited the lowest wear rate (2.92 × 10-5 mm3/N·mm). These results highlight the importance of precise control of the coating parameters to enhance the long-term durability of MOF-based materials for practical applications. Future work should focus on further optimizing the coating processes and exploring other MOF materials to develop highly efficient and durable carbon dioxide capture systems.

ACKNOWLEDGMENTS

This work was supported by the National Research Foundation of Korea(NRF) grant funded by the Korea government(MSIT) (No. RS-2023-00219369). This work was supported by the National Research Foundation of Korea(NRF) grant funded by the Korea government(MSIT) (RS-2024-00349019).

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