Metal–organic frameworks for organic transformations by photocatalysis and photothermal catalysis

Hong-Guang Jin *^a, Peng-Cheng Zhao^a, Yunyang Qian^c, Juan-Ding Xiao *^b, Zi-Sheng Chao^a and Hai-Long Jiang *^c
aSchool of Materials Science and Engineering, Changsha University of Science & Technology, Changsha, 410114, China. E-mail: jesonjin08@csust.edu.cn
^bInstitutes of Physical Science and Information Technology, Anhui University, Hefei, Anhui 230601, P. R. China. E-mail: jdxiao@ahu.edu.cn
^cHefei National Research Center for Physical Sciences at the Microscale, Department of Chemistry, University of Science and Technology of China, Hefei, Anhui 230026, China. E-mail: jianglab@ustc.edu.cn

First published on 20th August 2024

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Hong-Guang Jin

Hong-Guang Jin received his PhD (2016) from Aix-Marseille Université. He subsequently worked at Hunan University as a postdoc fellow (2017–2019). He is currently working at Changsha University of Science and Technology (CSUST). His research focuses on the synthesis and photocatalytic application of MOF-based materials.

Juan-Ding Xiao

Juan-Ding Xiao received her PhD (2017) from the University of Science and Technology of China (USTC), supervised by Prof. Hai-Long Jiang. She subsequently worked at Chinese Academy of Sciences (CAS) as an assistant researcher and postdoc fellow in 2017–2021. She is currently an associate professor in Anhui University. Her research interest is the synthesis and photocatalysis of MOF-based materials.

Hai-Long Jiang

Hai-Long Jiang earned his PhD (2008) from Fujian Institute of Research on the Structure of Matter, CAS. He subsequently worked at the National Institute of Advanced Industrial Science and Technology (AIST, Japan), first as an AIST Fellow and later as a JSPS Fellow during 2008-2011. After a postdoctoral stint at Texas A&M University (USA), he joined USTC as a full professor in 2013, and was appointed as a chair professor in 2022. He is a Fellow of both the Chinese Chemical Society (FCCS) and Royal Society of Chemistry (FRSC) and has been annually named as a highly cited researcher by Clarivate Analytics since 2017. His research group (http://mof.ustc.edu.cn) engages in microenvironment modulation (MEM) of catalytic centers based on reticular materials.

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1. Introduction

As one of the most crucial disciplines in the field of chemistry, organic synthetic chemistry, which can create a rich variety of functional molecules, plays a crucial role in improving human life and social civilization.¹ Conventional organic synthesis often involves complicated reaction steps with harsh reaction conditions, resulting in high energy consumption and aggravated environmental problems.² Solar energy is becoming one of the most appealing and achievable energy sources due to its magnitude, wide availability, versatility, and clean nature. Commonly, solar energy conversion can be achieved by converting photons into electricity, fuel and heat.³ Amongst, photo-assisted catalysis, which mainly includes two directly relevant applications involving the use of electrons and heat, photocatalysis and photothermal catalysis, is attractive for organic transformations.^4–8 Nevertheless, it is still challenging to develop a cheap and stable photocatalytic system with high organic transformation efficiency. Several strategies have been adopted to meet this challenge, focusing on the intrinsic structural optimization of photocatalysts to improve the key processes in solar energy utilization: (1) solar light absorption, (2) charge separation and transfer, (3) surface redox reactions, and (4) photothermal effect.

As for organic transformation by photocatalysis, the conversion efficiency depends mainly on light harvesting, charge separation, and redox reactions. While for organic transformation by photothermal catalysis, the conversion efficiency is highly dependent on the resulting photothermal effect. Photocatalytic organic transformation was first demonstrated in homogeneous systems by using transition metal complexes, precious metal complexes, and organic dyes as photosensitizers and/or photoactive sites.^9–13 These homogeneous photocatalysts exhibit excellent catalytic performance in various chemical reactions but suffer from drawbacks in terms of high cost and low recyclability for separation from reaction mixtures. In this case, heterogeneous photocatalysts, mainly including semiconductors (e.g., oxides, sulfides, and nitrides) and conjugated organic polymers,^14–18 can be alternatives due to their long lifetime and reusability. Although optimizing the band structures of semiconductors or synthesizing composites (commonly to construct heterojunctions) can ensure the activity and selectivity in photocatalytic organic transformations, the development of photocatalysts with well-defined structures is still particularly desirable because this route can provide in-depth studies on structure–activity relationships and guide the further design of photocatalysts with improved performance.

Metal–organic frameworks (MOFs) assembled from metal ions/clusters with organic linkers have received growing attention in the field of photo(thermal) catalysis.^19–23 MOFs feature defined crystalline structures, intrinsically high porosity, tunable chemical compositions, and abundant active sites, making them ideal platforms for studying key photocatalytic processes and structure–activity relationships in organic transformations. The structures of MOFs can be simply designed to enhance their catalytic properties and deepen the understanding of catalytic mechanisms. The main strategies for structural designation include: (1) modifying the organic ligands and/or metal nodes to optimize light absorption, (2) regulating the crystal surface and constructing heterojunctions to promote the migration and separation of photogenerated electron–hole (e⁻–h⁺) pairs, (3) increasing the number of active sites or creating defect sites to promote surface reactions, and (4) integrating plasmonic units to enhance catalysis via photothermal effects.

To date, several reviews have focused on organic transformations using MOF-based heterogeneous catalysts by photocatalysis or photothermal catalysis,^24–30 however, an overview of MOFs for organic transformations by photo(thermal) catalysis is still lacking. Herein, we summarize recent progress in organic transformations by photo(thermal) catalysis over MOF-based catalysts and pay special attention to the general mechanisms and unique advantages of MOF-based photocatalysts (Scheme 1). Given that photo(thermal) catalysis involves several key processes, namely, light absorption, e⁻–h⁺ separation, surface redox reactions, and photothermal effects, strategies for optimizing these processes and promoting the performance of MOF-based photocatalysts are presented. Subsequently, various organic transformations, including oxidation, reduction, coupling, tandem, synergistic redox, and CO₂ addition reactions over MOF-based photo(thermal) catalysts are introduced. It should be noted that, as a sort of oxidation reactions, the organic dyes photodegradation will not be discussed here due to its nature of mineralized reactions. Furthermore, representative advanced characterization techniques that can reveal the charge reaction kinetics and reaction intermediates during these organic transformation processes are described. Eventually, current challenges and perspectives in this area are briefly discussed.

2. General mechanism

2.1. Key processes in photocatalysis

A thorough understanding of the photocatalytic mechanism in MOF-based photocatalytic systems will contribute to the development of efficient photocatalysts. Typically, there are three key photophysical/photochemical processes involved in a photocatalysis reaction:^31–33 (i) light absorption by the light-harvesting antenna in MOFs to generate e⁻ at the lowest unoccupied molecular orbital (LUMO) and h⁺ at the highest occupied molecular orbital (HOMO), (ii) separation of e⁻ and h⁺ and migration to the catalyst surface, and (iii) e⁻ and h⁺-engaged surface redox reactions.

Optimization of the photocatalytic performance can be started from the perspective of promoting the above three key processes. For instance, to promote the efficiency of process (i), various methodologies have been adopted to expand the light harvesting of a photocatalytic system toward the visible region, such as the introduction of organic chromophores with large π-conjugated systems or the combination of two or more photocatalysts with different light responsive ranges.³⁴ Strategies including postmodification and construction of heterojunctions have been commonly utilized to create new electron transport channels that facilitate the process (ii) for efficient charge separation.³⁵ Surface reactions in process (iii) mainly consist of electron-engaged reduction reactions and hole-engaged oxidation reactions; the former are represented by photocatalytic hydrogen (H₂) production,³⁶ carbon dioxide (CO₂) reduction,³⁷ and nitrogen (N₂) fixation,³⁸ while the latter are known to involve photocatalytic water oxidation,³⁹ pollution degradation,⁴⁰ and organic oxidation reactions.⁴¹ All of these reactions can be promoted by introducing more active sites within a photocatalytic system.

Kinetics and thermodynamic equilibrium of these three distinct processes determine the eventual performance of the photocatalysts. Therefore, it is of paramount importance to characterize and understand these processes objectively and theoretically. If the maximum capacity of one individual stage of these processes can be determined and utilized as a reference to identify the limiting step, the photocatalytic system can be optimized to boost the performance. Considering that the photocatalytic process is essentially an electron transfer process, the characterization of electron transfer involved in process (ii) is the most direct approach to understanding photocatalytic systems. Conventional techniques, mainly including electrochemical impedance spectroscopy, photocurrent and photovoltage spectroscopy, and open-circuit voltage decay techniques, have difficulty in quantitatively characterizing the electron transfer process inside photocatalysts.^42,43 Nevertheless, there are emerged time- and space-resolved advanced techniques, such as transient absorption (TA) spectroscopy,⁴⁴ time-resolved photoluminescence (TRPL) spectroscopy,⁴⁵ X-ray absorption spectroscopy (XAS),⁴⁶ and electron paramagnetic resonance (EPR) spectroscopy,⁴⁷ have been adopted to determine the electron transfer kinetics in photocatalysis, contributing to the further design and advancement of high-efficiency photocatalysts in the future.

2.2. Charge/energy transfer mechanism

MOF-based photocatalyst-driven organic transformations follow either charge transfer (CT, direct pathway) or energy transfer (EnT, mediated pathway) mechanism (Fig. 1), commonly assisted by generated reactive species, such as e⁻, h⁺, superoxide radical anion (O₂˙⁻), singlet oxygen (¹O₂), hydrogen peroxide (H₂O₂), and hydroxyl radical (˙OH).^{24–28,48,49} In photocatalytic organic transformations mediated by the CT mechanism, MOF-based photocatalysts are first light-excited to produce e⁻–h⁺ pairs (excitons or carriers). After efficient separation, the h⁺ at HOMO and the e⁻ at LUMO can interact with the organic substrates and/or sacrificial agents to initiate redox reactions. While in photocatalytic organic transformations driven by the EnT mechanism, the excited states of MOFs are first generated through the absorption of photons with sufficient energy. Then, an EnT process occurs from the excited-state MOF to a substrate molecule, resulting in the formation of more reactive species, which can react with a second substrate to form the final product.

Charge and energy transfer processes have their own advantages in photocatalysis.^50,51 The CT route can realize various advanced oxidation processes through the generation of reactive oxygen species (ROS) over the photocatalytic process, such as O₂˙⁻, ˙OH, and H₂O₂.^52,53 In contrast, the EnT route can allow oxidation reactions to occur via the generation of ROS ¹O₂.^54–56 There is one obvious advantage for the EnT route: it allows some reactions with high potentials, which are almost impossible to achieve via the CT route. For instance, the sensitization of conjugated olefins into their excited sates, which is very challenging in the CT route, can be carried out effectively following the EnT route.⁵⁷

The MOF-based photocatalytic organic transformations can be mediated by either CT or EnT alone or by the combination of these two pathways. For example, very recently, Zhang et al. synthesized a phosphonate-based Fe-MOF via an amorphization strategy, resulting in excellent photocatalytic activity for the selective oxidation of toluene. A mechanistic study revealed that the effective CT facilitated by the distortion of Fe-oxo clusters in the framework can support the abundant generation of O₂˙⁻, which is a crucial factor for the efficient oxidation reaction (Fig. 2a).⁵⁸ By using the representative pyrene-based MOF NU-1000 as the photocatalyst, Zhang et al. realized iodoperfluoroalkylation of olefins via the EnT-mediated atom-transfer radical addition (ATRA) route (Fig. 2b).⁵⁹ Taking C_nF_2n+1I as an example, the homolytic cleavage of the carbon–iodine bond triggered by EnT from photoexcited NU-1000 to C_nF_2n+1I can produce perfluoroalkyl and iodine radicals, resulting in the addition of the α- and β-positions of olefin, respectively, to complete the ATRA reaction (Pathway A). When the substrate is an aromatic alkene, the ATRA product undergoes base-assisted elimination of HI to form (E)/(Z)-isomeric mixtures, which are then enriched to the (Z)-isomer by imposing another EnT from the triplet excited state of NU-1000 (Pathway B). Additionally, Wang et al. demonstrated that a novel Zn-MOF based on porphyrin- and carbazole-based organic ligands was a remarkable photocatalyst for the oxidation of amines.⁶⁰ The synergistic CT and EnT processes upon light irradiation, accounting for the generation of O₂˙⁻ and ¹O₂, respectively, contributed to the high photocatalytic activity (Fig. 2c).

2.3. Photothermal effect

The photothermal effect refers to the property of a material that converts absorbed light to heat. The materials with photothermal effects that have been reported to date can be commonly divided into four categories, namely, precious metal nanoparticles (NPs),⁶¹ inorganic semiconductors,⁶² carbon-based materials,⁶³ and polymers.⁶⁴ A systematic elaboration of the photothermal effect from the perspective of the physiochemical mechanism is necessary for the further development of novel excellent photothermal materials and to apply in diverse fields, including photothermal catalysis.⁶⁵ The mechanism for light-to-heat conversion is dependent on the nature of the catalysts and generally involves the following three mechanisms (Fig. 3): (i) the light-induced localized surface plasmon resonance (LSPR) can convert light energy into the kinetic energies of electrons and holes, which dissipate nonradiatively to cause a temperature increase in the surrounding medium; (ii) the transition of electrons by photoexcitation can release heat in the nonradiative relaxation process to return to the ground state; and (iii) the molecular vibrations initiated by the light absorption can generate heat to increase the temperature.

Organic transformations over MOF-based photocatalysts by photothermal catalysis can utilize the individual photothermal effect of MOF itself, the incorporated plasmonic NPs supported by MOFs, or the combined photothermal effects of MOFs and NPs.^29,30,66,67 Taking the photothermal effect of MOFs without integrated plasmonic NPs as an example, Zhang et al. prepared FeTPyP with a two-dimensional (2D) layered structure, which exhibited excellent photothermal catalytic activity for the synthesis of styrene carbonate via the CO₂ cycloaddition reaction.⁶⁸ The results show that the crucial ring opening process can be accelerated by the holes generated from the photoexcited FeTPyP, and the promoted charge transfer and separation benefit from the increased temperature of the catalytic system owing to the photothermal effect of 5,10,15,20-tetra(4-pyridyl)porphyrin (H₂TPyP) at the FeTPyP framework (Fig. 4). The photothermal effect of MOFs can also contribute to organic transformations by activating the catalytic centers, as shown by Sharma and coworkers.⁶⁹ In their work, a novel Mn(II)-porphyrin MOF was successfully prepared, wherein the porphyrin ligands can absorb and convert light into heat to remove the coordinated water molecules around the Mn nodes. The catalytic Mn centers with Lewis acidity were thus activated, which improved their adsorption to the substrates and accelerated the synthesis of cyclic carbonates.

3. Unique advantages of MOFs in photo(thermal) catalysis

3.1. Modulated microenvironment

A microenvironment with unique structural and electronic characteristics around catalytic sites has an important effect on the catalytic behaviors of enzymes and homogeneous catalysis.⁷⁰ However, it remains a major challenge to discover the microenvironment modulation of active sites in heterogeneous catalysis because of their vague structure and/or low modifiability.⁷¹ As a class of emerging porous crystalline materials, MOFs with atomically precise and highly tunable structures are ideal candidates as heterogeneous catalysts for regulating the surrounding microenvironment to affect the catalytic performance.^30,72–77 There are many strategies, such as grafting extrinsic organic/inorganic units onto unsaturated metal nodes, functionalization of organic ligands, encapsulation of guests, control of pore/channel size and shape, and alteration of the spatial location of the catalytic sites, to modulate the microenvironment in MOFs to understand the intrinsic structure–activity relationship and further optimize the catalytic performance.^72,78

First, the coordination modulation of a single atom can be realized in MOF-based photocatalysis.^79,80 Zr-based MOFs are intensively utilized for the construction of single-atom catalysts (SACs) due to the presence of neighboring surface-O/OH_x sites at Zr₆-oxo clusters, allowing the anchoring of extraneous metal species.^81,82 With the help of microwave, Ma et al. developed a simple and general method to immobilize various single atoms, such as Ni(II), Co(II)²⁺, and Cu(II)²⁺, onto the Zr₆-oxo clusters of different Zr-MOFs.⁷⁴ Interestingly, following hydroxylation, sulfonation, or further oxidation, the coordination environments of these single-atom metals were flexibly modulated (Fig. 5a), affording representative Ni₁-X/UiO-66-NH₂ (X = S, O, S_ox; ox, oxidation) photocatalysts. The results show that Ni₁–S/UiO-66-NH₂ possessing a reductive oxidation state has a lowest proton activation barrier, leading to the highest photocatalytic activity for H₂ production, which is 270 times that of the pristine MOF.

In addition, the modulation on the second coordination sphere interactions to improve the catalytic efficiency mimicking the supramolecular systems has been fulfilled in MOF-based photocatalysis.⁷⁶ It is known that interactions extending beyond the primary coordination sphere can contribute to the enhancement of the catalytic activity and/or selectivity.⁸⁴ Rayder et al. prepared a host–guest composite via the noncovalent encapsulation of a ruthenium complex into the pores of various functionalized UiO-66-X (X = CH₃, F, Br, NO₂, NH₂, NH₃⁺, 4F) hosts to study the influence of the outer sphere on the catalytic activity induced by the modulated host–guest interactions.⁷⁶ UiO-66-NH₃⁺ was found to possess the highest efficiency in CO₂ hydrogenation to methanol, benefiting from the ammonium functional group in close proximity to the encapsulated catalyst.

Moreover, by simply changing the –X groups on UiO-X shell of the sandwich-structured MOF@Pt@MOF, microenvironments of the UiO-66-NH₂ photosensitizer and Pt cocatalyst were simultaneously modulated.⁸³ A mechanistic study revealed that with the gradual increase in the electron-withdrawing capacity of the –X group (–OCH₃ < –NA < –H < –Br < –Cl < –NO₂), the charge separation efficiency (η₂) of the UiO-66-NH₂ core, as evaluated by the exciton binding energy (E_b), increased; while the intrinsic reduction efficiency (η₃) of Pt, as indicated by the electrochemical H₂ evolution reaction (HER), decreased (Fig. 5b). The relationship between the H₂ production activity and the electron-withdrawing/donating ability of the –X groups is nonlinear. Furthermore, Xu et al. encapsulated three different Pt cocatalysts into UiO-66-NH₂, with the microenvironment modulated by capping or partially removing polyvinylpyrrolidone (PVP or rPVP).⁸⁵ The presence of PVP decreased the electrical conductivity and hampered the electron transfer between MOF and Pt, resulting in greater photocatalytic H₂ activity of Pt@UiO-66-NH₂ than that of Pt_PVP@UiO-66-NH₂ and Pt_rPVP@UiO-66-NH₂.

3.2. Multivariability

The prerequisite for developing bi- or multifunctional catalysis is the incorporation of different catalytic centers into a single catalyst, which can cooperatively catalyze sequential, stepwise, tandem, etc., reactions.⁸⁶ Due to their structural designability, chemical variety, and inherent rigidity, MOFs are very promising catalysts for multivariate catalysis, including photo(thermal) catalysis, via synergistic effects. The synthesis of multivariate (MTV)-MOFs by mixing ligands was first reported by Yaghi and coworkers, wherein up to eight functionalities can be successfully integrated into MOF-5.⁸⁷ Since then, the introduction of multiple functionalities into MOFs to realize the potential of MOFs for multivariate catalysis has attracted increasing attention.^88–90 For instance, by combining the dynamic spacer installation approach with metal chelation and covalent postmodification processes, Cao et al. installed ligands with different lengths into the robust prototype MOF LIFM-28 for the construction of MTV MOFs.⁹¹ These MTV MOFs show activity in different catalytic reactions as well as in multivariate catalysis of sequential or stepwise reactions.

Based on reticular chemistry, MTV MOFs can be synthesized by using a mixture of ligands that have the same geometry and metrics but distinct lengths and degrees of functionalization.⁹² This is vital in MOF-based photocatalysis because it allows bandgap modulation to influence key photocatalytic processes and pore size modulation to modify the substrate diffusion. Bryant et al. presented a MTV library of Ti-MOFs (Fig. 6a and b), in which eleven isoreticular hex rod-packed MOFs named UCFMTV-n and UCFMTV-n-x% with the formula Ti₆O₉[links]₃ were successfully prepared (n is the number of p-arylene rings in the linear oligo-p-arylene dicarboxylates, and x% is the percentage of multivariate links with electron-donating groups).⁹³ Benefiting from the varied linker sizes and amine electron-donating group functionalization, the pore sizes and energy gaps of these MTV MOFs are well regulated, and their effects on the photooxidation of benzyl alcohol were studied in detail (Fig. 6c). As a result, UCFMTV-4–30%, which has the longest pore size and an appropriate content of electron-donating groups, exhibited the highest turnover rate, which is approximately 18-fold faster than that of the representative Ti-MOF photocatalyst MIL-125 (Fig. 6d).

To realize synergistic light harvesting, charge carrier separation and transfer processes, Zhang et al. organized photosensitive and photothermal units uniformly into a single MOF.⁹⁴ The solvothermal reactions of HoCl₃·6H₂O, Cd(OAc)₂·4H₂O, and different ratios of NiCl₂·6H₂O with the organic ligand 3-fluoropyridine-4-carboxylic acid (HFNA) afforded a stable 3D framework, named Ho₆–Cd_xNi_1−x–N₄, with a (4,12)-connected ftw topology (Fig. 7a and b). After simple sulfurization at 120 °C by using different amounts of thioacetamide, Ho₆–Cd_xNi_1−x–NS integrated with well-dispersed photosensitive Cd–NS and photothermal Ni–NS single sites was obtained (Fig. 7c). Upon light absorption of the connected FNA⁻ ligands, abundant photoelectrons generated around the photosensitive Cd–NS sites first transferred to the Ho₆ clusters and then to adjacent photothermal Ni–NS sites (Fig. 7d). Benefiting from the ultrashort molecule-scale electron transfer path, the suppressed recombination of the photoinduced charge carriers and the facilitated reaction rate by the presented photothermal effect, Ho₆–Cd_0.76Ni_0.24–NS exhibited a boosted H₂ production rate of 40.06 mmol g⁻¹ h⁻¹.

3.3. Steric effects

Steric effects are often invoked as a feature of nanoporous materials that can affect the catalytic activity and selectivity.⁹⁵ In contrast to traditional porous materials, such as zeolite anmesoporous silica, one unparalleled advantage of MOFs for catalysis is their highly adjustable physical/chemical environments (organic ligands, metal centers, pore sizes or pore shapes), which are promising platforms for regulating steric effects to realize target catalysis.^96–99 It is acknowledged that the aperture and shape of MOFs play complementary roles in controlling steric effects.¹⁰⁰

For instance, Wei et al. realized precision syntheses by utilizing the pore confinement effect of MIL-88B, a Fe(III) dicarboxylate framework wherein a regular triangle is defined by every three adjacent Fe(III) ions located on the same channel.⁹⁶ The highly oriented coordination bond arrangement of the octahedral Fe(III) ions can contribute to the fixation of three molecules for the [2+2+2] coordination-templated cyclotrimerization reaction. Bing et al. anchored single-site Cu^I active metal centers and alkali metal Cs⁺ onto the deprotonated [Zr₁₂O₈(μ₃-O-)₈(μ₂-O-)₆(carboxylate)₁₈]¹⁴⁻ secondary building units (SBUs) of a Zr₁₂-MOF.⁹⁷ In this Cu- and Cs-integrated MOF, the spatially proximate bimetallic Cu^I₂ centers can prompt the activation of H₂ via bimetallic oxidative addition as well as the direct C–C coupling of methanol and formyl species. Yang et al. prepared a Pd nanocube (NC)@ZIF-8 composite with a core–shell structure and demonstrated that it was an efficient photothermal catalyst for the hydrogenation of olefins upon light irradiation because of the excellent photothermal effects of Pd NCs.⁹⁸ Furthermore, because the ZIF-8 shell has a well-defined pore structure that can function as a molecular sieve, selective hydrogenation of olefins with specific sizes on the Pd NC@ZIF-8 composite can be realized (Fig. 8). These examples offer the opportunity to enhance the activity and selectivity of MOF-based photo(thermal) catalysis by rationally employing steric effects.

3.4. Defect and facet engineering

Traditionally, perfect MOFs, in which the metal motifs and organic ligands are perfectly coordinated, are highly pursued to fully exploit their potential for multifunctional applications. Nevertheless, defective MOFs have been demonstrated to be prevalently formed in general synthetic processes due to the uncoordinated metal and ligands or vacancies in the framework. Unexpectedly, defective MOFs frequently exhibit superior activity in contrast to their perfect counterparts in various fields because of their increased porosity and abundant active sites.^101–105 Thus, the defects of MOFs can also be utilized as an additional dimensionality to tailor the MOF photo(thermal)catalytic performance.^106–111 For instance, Wang et al. optimized the CO₂ photoreduction performance of UiO-66-NH₂ by tailoring its defect type and ligand vacancy degree. In their work, by simply regulating the molar ratio of the defect modulator (formic acid, FA) to the carboxylate ligand, UiO-66-NH₂ with different defect types and varied degrees of ligand vacancies can be obtained.¹⁰⁷ With increasing FA molar equivalent, the defect type changed from missing-linker (ML) to missing-cluster (MC), and the ligand vacancy degree also increased after thermal treatment of the samples to remove the thermolabile modulator FA. It was found that the ML defect decreased the Zr atom-dominated LUMO energy, while the MC defect increased the absorption energy. As a result, ML UiO-66-NH₂-ML-100 with a ligand vacancy exhibited the best activity toward CO₂ photoreduction.

Very recently, by using different powers of Ar radio frequency plasma, Wang et al. prepared Fe-based MOF catalysts with regulated defects of terminal inorganic ligands (OH⁻ and H₂O) and/or bridging organic ligands, which can result in the generation of different coordinatively unsaturated Fe centers (Fig. 9a).¹¹¹ Compared to the pristine MIL-100(Fe) with a nonporous compact surface, the MIL-100(Fe) samples, which were treated by plasma at powers of 50, 100, 200, and 300 W for 10 min, became highly porous. The different thermal behaviors of MIL-100(Fe) and MIL-100(Fe)-200 W (Fig. 9b) indicated that the defects of the former are only terminal inorganic ligands, while those of the latter are dominated by both terminal inorganic ligands and bridging organic ligands. The NH₃ synthesis activity of these plasma-treated photocatalysts from N₂-saturated water was proven to be dependent on the defect type and degree in the catalysts (Fig. 9c). The best activity of MIL-100(Fe)-100 W is due to the abundant exposed coordinatively unsaturated Fe sites induced by the dual defects, which possess different local electron structures to reduce the energy barrier of the rate-limiting step of N₂ reduction.

Facet engineering is an efficient approach for exposing various atomic arrangements on the surface of metal and metal oxide catalysts to modulate the kinetics and activity of catalytic reactions.^112–115 With regard to photocatalysis, through facet engineering, the light harvesting, surface electronic structure, and transport efficiency of surface electrons, which are vital for determining the photocatalytic performance, can be regulated.^116–118 Due to their crystalline structures and diverse active sites on different facets, MOFs have the potential to expose specific facets with more reactive sites for specific reactions through facet engineering. To date, facet engineering via simply controlling the morphology of MOFs, such as ZIF-8, MOF-5, and HKUST-1, has been realized.^119–123 For example, by using a crystal engineering method, Yang et al. prepared a bulky Ni-MOF and two nickel metal–organic layers (Ni-MOLs) with different exposed crystal facets, named Ni-MOL-100 and Ni-MOL-010 with abundant exposed (100) and (010) facets, respectively.¹¹⁹ When used as photocatalysts for CO₂ photoreduction, Ni-MOL-100 exhibited an obvious increased catalytic activity for converting CO₂ to CO compared with that of Ni-MOL-010 and bulky Ni-MOF (Fig. 10a). Results show that the excellent performance of Ni-MOL-100 is due to the synergistic catalysis provided by the two coordinatively unsaturated and close (3.50 Å) nickel sites on the surface of the (100) facet (Fig. 10b).

4. Strategies for improving MOF-based photo(thermal) catalytic performance

Because MOFs are assembled by metal nodes with organic linkers, the photocatalytic activity of MOFs can come from either the metal nodes and/or the organic ligands. For example, pristine zirconium, titanium, iron, or cerium oxo cluster-based robust MOFs have been intensively utilized as photocatalysts because of the intrinsic photoactivity of these types of clusters, which can evoke the formation of ROS and trigger electron transfer reactions.^124–126 Meanwhile, when photoactive molecules, such as porphyrin, pyrene, and anthracene, are adopted as organic linkers, the prepared pristine MOFs also show catalytic activity for various photochemical reactions.^127–129 Although the direct use of pristine MOFs as photocatalysts is very promising because of their facile synthetic processes and they can also provide good platforms for studying structure–activity relationships, their application in photocatalysis is still restricted for their limited light harvesting, charge generation and separation, and reaction activities. To further optimize the photocatalytic activity and widen the application field of pristine MOF photocatalysts, various modification/composite strategies are commonly introduced.^35,130–132 According to the general photo(thermal) catalytic mechanism and unique advantages of MOF-based photo(thermal) catalysts,^24–28 herein, several representative strategies from the perspectives of structural functionalization of MOFs and the fabrication of MOF-based composites with the aim of improving three intrinsic key photocatalytic processes and photothermal effect to enhance the photo(thermal) catalytic performance are listed.

4.1. Structural functionalization of MOFs

4.2. MOF-based composites

5. Organic transformations over MOF-based photocatalysis

Benefiting from the unique photophysical characteristics, for instance, effective charge separation and high charge carrier mobility, MOFs have been considered as promising photocatalysts for diverse types of organic transformations, such as oxidation, reduction, coupling, tandem, and synergistic redox reactions (Fig. 17). The representative organic transformation reactions using MOF-based photocatalysts are summarized in Table 1.

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5.1. Oxidation reactions

To date, photocatalytic organic oxidations with different reaction types have been developed, including selective oxidation of aromatic alcohols, oxidation coupling of amines, selective sulfoxidation reactions, and C–H oxidation.^41,271,272 There is often more than one ROS evolved in a photocatalytic system, which results in different distributions of products. For example, during the oxidation of benzyl alcohol, the existence of ROS ˙OH could lead to the overoxidation byproduct of benzyl acid, which can be suppressed by utilizing mild ROS, such as O₂˙⁻ or ¹O₂. Due to their unique excitation and CT/EnT mechanism, MOFs are often used as photocatalysts for various oxidation reactions.^28,273

5.2. Reduction reactions

Compared to photocatalytic oxidation reactions, photocatalytic reduction reactions, such as CO₂ reduction, N₂ reduction, and H₂ production, can provide more valuable chemicals from common materials.^344–355 To date, MOF-based photocatalysts have been widely applied in the photocatalytic oxidation based organic transformations and photoreduction reactions mentioned above; however, there are few reports on the use of MOF-based photocatalysts in photoreduction reactions of organic transformation.^253–255

Recently, Chen et al. prepared a novel 3D Zn-MOF based on a photoactive organic linker and used it for the photoreduction of aromatic nitro compounds.²⁵³ Upon direct interaction of the photoexcited Zn-MOF with nitrobenzene, no product was observed, possibly because no protons were present during the reaction. However, after the introduction of hydrazine hydrate (N₂H₄·H₂O), which can reduce oxidative holes and produce the protons needed for the photoreduction reaction with clean N₂ as the only byproduct, aniline (AN) can be obtained. As a result, in the presence of N₂H₄·H₂O, various nitroaromatics were selectively reduced to ANs with the use of the Zn-MOF photocatalyst.

The traditional synthesis of N-formylated products through the formylation of ANs is limited by the usage of toxic formylating sources and the generation of wastes.^356,357 Thus, it is necessary to develop sustainable approaches for synthesizing N-formylated compounds from nitroaromatics. Kar et al. constructed a photocatalyst, Pd-decorated Ti-MOF, which can be successfully applied in one-pot reductive N-formylation of nitroarenes with HCOOH as both the H₂ and formylating source.²⁵⁴ A detailed mechanistic study indicated that the photogenerated charge carriers, which contributed to the generation of CO₂ and H₂ via the photodecomposition of HCOOH, accounted for the N-formylation. The resulting dissociative H₂ was adsorbed at the Pd active sites, reducing nitroarene to AN and converting it to N-formyl AN through the adsorbed HCOOH or CO₂ and H₂.

The activation of inert bonds, such as the reductive cleavage of aryl halide bonds through the SET pathway, is a cornerstone of synthetic chemistry.³⁵⁸ Recently, Zeng et al. constructed a MOF, named Cd-SNDI, in which the NDI dye was decorated with S-bearing branches, and S⋯S-bridged nonaromatic NDI stacking was obtained (Fig. 23a and b).²⁵⁵ The separation of the NDI cores by interdye aromatic stacking was inhibited by coordination-oriented structural coercions, promoting the linking of neighboring NDI units via S-mediated noncovalent interactions (Fig. 23c). Benefiting from the interligand S⋯S contacts, which bridged the CT throughout the nonaromatic stacked NDI string in a long-range order way (Fig. 23d–f), the redox potential of a single excited-state NDI/NDI˙⁻ unit can be maintained. Moreover, since S-branches with electron-donating ability are prone to connect with electron-deficient inert substrates, the probability of contact between the generated excited states and the substrates improved (Fig. 23g). As a result, high-efficiency photoreduction of aryl halides as well as the successive formation of C_Ar–C/S/P/B bonds based on Cd-NDI were realized.

5.3. Coupling reactions

Benefiting from their wide application in modern synthetic organic chemistry, catalyzed homo- and cross-coupling reactions have received much attention since the realization of the Grignard reagent-assisted Ni-catalyzed coupling of aryl and alkenyl halides in 1972.³⁵⁹ In contrast to the traditional thermal catalytic systems used for coupling reactions that require high temperature, photocatalytic coupling reactions under mild conditions have attracted increasing research attention.^{156,256,258,259,360–366} Nevertheless, because it is difficult to understand and design suitable catalytic systems, the development of coupling reactions by photocatalysis is still in its infancy.

The C–H arylation reaction and decarboxylation cross-coupling reaction are two art methods for C–C bond formation.^367,368 Cheng et al. modulated the microenvironment of Pd NPs by using Fe-MOFs with different framework structures.²⁵⁶ The photocatalytic tests of thiazole C–H arylation and cinnamic acid decarboxylation cross-coupling were conducted. Results showed that the Pd/MIL-101(Fe) photocatalyst possessed the highest activity for both types of reactions due to its most effective electron migration from Fe–O clusters to Pd NPs. It was proposed that the C–H arylation was realized following a three-step procedure, namely, (i) activation of the C–halogen bond by Pd NPs, (ii) aryl radical generation, and (iii) subsequent radical addition. However, the decarboxylation cross-coupling was carried out mainly follows the procedure (i), during which the selectivity of the products depended on the base additives.

The development of efficient and green approaches for C–S bond formation has attracted increasing interest due to the universality of C–S bonds in the fields of chemistry and medicine.^369,370 Zhu et al. utilized a robust and porous Zr₁₂ MOF, named Zr₁₂–Ir–Ni, combined an Ir(III) photoredox catalyst with a Ni(II) cross-coupling catalyst for the formation of C–S bonds between aryl iodides and thiols (Fig. 24).²⁵⁷ Benefiting from well-isolated Ni catalysts, the space confinement of Ir catalysts, as well as the close proximity (ca. 0.6 nm) between them, the transfer of electrons and thiophenol radicals from Ir to Ni(II) centers accelerated the catalytic cycle, and Zr₁₂–Ir–Ni exhibited a turnover number of up to 38500.

The coupling reactions that form disulfide bonds (–S–S–) are at the center of attention in synthetic organic chemistry due to their critical role in the biochemistry of life and unique application in the industry of –S–S– bonds.³⁷¹ Razavi et al. constructed a mixed-ligand Zn-MOF, TMU-34(-2H), using 4,4′-oxybis(benzoic acid) (H₂OBA) as the carboxylic linker and tetrazine-functionalized 3,6-di(pyridin-4-yl)-1,2,4,5-tetrazine (DPT) as the pillar.²⁵⁸ Upon visible-light irradiation, the excited neutral tetrazine sites within the DPT pillars with photogenerated redox activity accept one electron from the reactants to generate tetrazine radical anions as electron mediator sites, which can then be transferred to other substrates in the reaction system to complete the synthesis of disulfides in an efficient way.

5.4. Tandem reactions

In contrast to traditional one-catalyst/one-reaction systems, tandem reactions are highly desirable for further catalysis because they can realize one-pot multiple organic transformations without separation or purification of the intermediates.^372–376 Despite their enormous advantages in terms of atom and step economy, tandem reactions are still in their infancy because of the great challenge in designing and synthesizing efficient catalysts with multifunctional active sites that can work synergistically to conduct multiple organic transformations in one pot. As one class of excellent solid supports, MOFs can be hierarchically immobilized with different catalysts in an ordered fashion to overcome the above challenge and are promising heterogeneous photocatalysts for tandem reactions.^{260–262,377–383}

Artemisinin is currently the most efficient drug for treating malaria, however, its traditional synthetic approaches are still accompanied by complicated reaction and treatment steps as well as high cost.³⁸⁴ Feng et al. prepared a series of porphyrinic MOF-based tandem photocatalysts, PCN-22X-SO₄ (X = 2, 3, 4), through postsynthetic treatment of acid-stable PCN-22X with dilute sulfuric acid.²⁶⁰ A stability screening experiment supported that PCN-222-SO₄ is a potentially excellent photocatalyst for the tandem synthesis of artemisinin. As expected, under the conditions of visible light and O₂, PCN-222-SO₄ exhibited the best efficiency for the synthesis of artemisinin among reported photocatalysts, although with a selectivity between 50–60% resulting from byproducts that were unavoidably formed during the ¹O₂ ene step. The excellent performance of this tandem photocatalytic process was benefited from the synergistic effect of the photosensitivity and abundant acid sites of PCN-222-SO₄.

The synthesis of quinazolinones has attracted much attention because their derivatives commonly have outstanding pharmacological and biological properties, such as antibacterial, anti-inflammatory and anticancer activities.³⁸⁵ Ghaleno et al. developed a simple one-step strategy to decorate the nodes of PCN-222(Fe) with Fe(III), wherein the metal precursor Fe(III) chloride can remove the benzoic acids through the in situ generated HCl and metalation of the Zr₆-nodes.²⁶¹ The resulting bioinspired MOF, Fe@PCN-222(Fe), was successfully applied as a photocatalyst to prepare quinazolin-4(3H)-ones via a one-pot three-step tandem reaction process (oxidation-cyclization-oxidation) from alcohols and 2-amonibenzamide (Fig. 25a). The excellent performance was contributed from the bifunctional characteristic of Fe@PCN-222(Fe), which can function as a photoredox as well as Lewis acid catalyst.

The development of efficient catalysts for synthesizing primary alcohols with terminal alkenes and alkynes as hydrocarbon feedstocks is particularly urgent due to their intensive application in chemical and pharmaceutical industries.^386,387 Via the Schiff-base condensation reaction between Cu(I) unit (Cu-CTU) and boron dipyrro–methene (Bodipy) ligand, Lin et al. have prepared a new 2D MOF, denoted as JNM-20 (Fig. 25b).²⁶² Benefiting from the good light-harvesting capacity of Bodipy and the large π-conjugated structure, JNM-20 possesses high charge separation efficiency. JNM-20 can catalyze the one-pot tandem synthesis of primary alcohols from terminal alkenes and alkynes with remarkable regioselectivity, high yields, and broad substrate compatibility. The detailed mechanism study indicated that the outstanding performance was derived from the synergistic effect of the Cu-catalyzed hydroboration and the photocatalyzed aerobic oxidation, which were provided by Cu-CTU and Bodipy ligands, respectively.

5.5. Synergistic redox reactions

Photocatalytic organic transformations to prepare useful molecules can provide a potential alternative for the synthesis of industrially relevant chemicals. However, to increase the reaction efficiency, in some cases, sacrificial reagents, including electron acceptors or donors, are added to photocatalytic organic reaction systems.³⁸⁸ Such additives increase the consumption of e⁻ or h⁺, limiting the practical application of photocatalytic organic transformation systems. Recently, the construction of dual-function photocatalytic systems, which can simultaneously utilize photogenerated h⁺ and e⁻ to realize the selective oxidation and reduction of value-added products, has been considered as an ingenious strategy to overcome this obstacle.^389–394 Herein, we introduce several representative MOF-based bifunctional photocatalysis systems for coupling selective organic transformations with H₂ production or CO₂ reduction.

6. Organic transformations over MOF-based photothermal catalysis

Upon light irradiation, in addition to e⁻- or h⁺-engaged surface redox reactions, thermal energy (heat) can also be generated to promote endothermic reactions in the presence of components with photothermal effect in photocatalysts. Currently, photothermal catalysis over MOF-based materials is in its infancy yet highly desirable for efficient solar energy conversion. For instance, benefiting from the large pore structures of MOFs allowing the deposition of NPs with photothermal effect and the excellent absorption capacity of MOFs for CO₂ gas, MOF-based materials exhibit great potential in the photothermal catalysis of CO₂ hydrogenation,⁴⁰⁴ which is a typical challenging reaction that requires high activation energy.⁴⁰⁵

The representative organic transformations over MOF-based photothermal catalysis are summarized in Fig. 30 and Table 2, mainly toward the different reaction types of oxidation, reduction, and CO₂ addition reactions. Given that the MOF itself and the NPs incorporated in MOF/NP composite photocatalysts can both display photothermal effect, the distinct reaction mechanisms of photothermal-mediated organic transformations will be strongly elucidated in this section.

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6.1. Oxidation reactions

The photothermal effect of the MOF itself is usually attributed to the organic antenna within the framework, which can absorb long wavelength light. Typically, porphyrinic MOFs, with porphyrin ligands as effective photosensitizers, have been considered as potential photothermal catalysts due to their strong light-harvesting capacity in the visible light range. Chen et al. reported the photothermal effect of a porphyrinic MOF, PCN-224(M) (M represents the central metal ion of the porphyrin ligand), and fabricated Pt/PCN-224(M) composite catalysts with the synergistic photothermal effects of Pt and MOF, by simple addition of presynthesized PCN-224(M) to a preparation system of Pt NCs (Fig. 31a and b).⁴⁰⁶ The synergistic photothermal conversion was fully demonstrated by the obvious differences in the aromatic alcohol oxidation yields when the reaction was carried out at 16 °C to eliminate the photoinduced heat, with heating instead of light irradiation, or without external disturbance (Fig. 31c). Furthermore, by simple changing the irradiation light intensity, the electron state of Pt can be regulated through competitive e⁻ transfer between Pt and PCN-224(Zn), influencing the eventual catalytic activity (Fig. 31d).

Advanced oxidation processes for the decomposition of wastewater pollutants, including antibiotics, pathogenic organisms, and pesticides, are highly desirable for freshwater production.⁴¹¹ As a typical antibiotic pollutant, the decomposition process of tetracycline (TC), which involves series of organic transformation reactions, requires an effective catalyst.⁴¹² Very recently, Bai et al. constructed a dual-functional Co-MOF/carbon nanotube (CNT) photocatalyst, in which the ligand H₂BDC used for MOF synthesis was prepared from the catalytic degradation of waste poly(ethylene terephthalate).⁴¹³ Benefiting from the synergistic effect of the localized solar heat derived from the outstanding photothermal effect of CNTs and the abundant open Lewis acid sites of Co-MOF in the composite photocatalyst, peroxymonosulfate can be efficiently activated to generate various ROS, including SO₄˙⁻, ˙OH, O₂˙⁻ and ¹O₂, contributing to the superb degradation performance of TC. This work provides a sustainable platform for developing MOF-based materials that combine photothermal and photocatalytic methods with advanced oxidation processes for wastewater purification.

6.2. Reduction reactions

The development of catalytic hydrogenation reduction reactions that can avoid the use of heat, high-pressure H₂, and hydride reagents to replace traditional ones is highly desirable.⁴¹⁴ High-efficiency conversion of sunlight to heat via the surface plasmonic properties of metal NPs for hydrogenation reactions is a promising alternative.⁴¹⁵

Selective semihydrogenation of alkynes to alkenes has received particular attention in both scientific and industrial fields but remains a major challenge.⁴¹⁶ Li et al. constructed a core–shell composite of CuPd@ZIF-8, wherein cubic Cu supported Pd were used as the core and porous ZIF-8 was used as the shell.⁴⁰⁷ Upon light irradiation, the CuPd@ZIF-8 composite was demonstrated to be an outstanding photocatalyst for alkyne semihydrogenation due to the photothermal effect of Cu NCs and the in situ formed active hydrogen species from NH₃BH₃ (Fig. 32a). The Cu–Pd interaction-mediated chemoselectivity is dominated by the steric hindrance effect of the ZIF-8 shell. The catalytic activity of CuPd@ZIF-8 was far exceeded those of other reported metal-based catalysts, with a high turnover frequency of 6799 min⁻¹; in addition, the chemoselectivity remained even upon an extended reaction time.

It is still tricky to realize selective hydrogenation of nitroaromatics in the presence of other reducible groups. Although Pd-based catalysts have been widely utilized in the hydrogenation of nitrocompounds, harsh reaction conditions, including high H₂ pressure and high temperature, are still needed.^417,418 By using Cu₂O as a sacrificial material, Li et al. successfully constructed yolk–shell structured PdAg@ZIF-8.⁴⁰⁸ In this composite, Ag NCs with excellent LSPR properties can generate heat upon light irradiation to improve the hydrogenation activity of Pd sites. Moreover, the aggregation of small Pd NPs can be avoided under the protection of the MOF shell, which also allows mass transport and the accessibility of Pd sites due to its porous nature. Furthermore, the hollow space between the PdAg core and the MOF shell can contribute to the enrichment of reactants and the preferential adsorption of –NO₂ groups. As a result, compared to the core–shell PdAg@ZIF or the PdAg NCs, the yolk–shell structured PdAg@ZIF-8 showed the efficient and selective hydrogenation of nitrostyrene to aminostyrene (Fig. 32b).

6.3. CO₂ addition reactions

CO₂ chemical fixation, which converts CO₂ into valuable chemicals under mild conditions, has attracted increasing amounts of attention because it follows the criteria of green chemistry.⁴¹⁹ However, highly efficient catalysts are still required due to the chemical inertness of CO₂. Ag NPs are active species for CO₂ conversion and are excellent photothermal materials due to their strong LSPR effect.⁴²⁰ Nevertheless, their catalytic performance is limited by their tendency to aggregate during catalysis. By using a simple solution impregnation-reduction method, Jing et al. successfully loaded Ag NPs into MIL-100(Fe) (Fig. 33).⁴¹⁰ The resulting Ag/MIL-100(Fe) composite could be utilized as a photothermal catalyst to efficiently promote the conversion of various aromatic alkynes to the corresponding carboxylic products due to the photothermal effects and catalytic capabilities of both Ag NPs and MIL-100(Fe). Notably, the catalytic performance of the composite under these mild conditions can be impaired by heating, indicating that the conventional heat source should be replaced by light to drive this reaction.

The cycloaddition of epoxides with CO₂ as the C1 source is considered as one of the most promising approaches for the chemical fixation of CO₂ because of the widespread application of the cyclic carbonate products.⁴²¹ However, most MOF-based CO₂ cycloaddition reactions have been conducted by direct heating.⁴²² Chen et al. constructed a superstructure MOF and used it for CO₂ cycloaddition via photothermal catalysis.⁴⁰⁹ A hierarchical tubular MOF-74 (Cu), named MOF-74-HT, was prepared by immersing a rod-like precursor MOF into a mixed solution of methanol and H₂O with the addition of sodium dodecyl benzene sulfonate as the modulator. The resulting MOF-74-HT with cavities in the core and well-aligned nanosheet arrays on the outer surface showed superior photothermal catalytic performance in the CO₂ cycloaddition with styrene oxide due to the combined photothermal conversion and catalytic capacities.

7. Advanced characterization techniques

The conventional characterization techniques, such as mass spectroscopy, gas chromatograph mass spectroscopy, gas chromatograph, and nuclear magnetic resonance spectroscopy, are used to identify the reaction products and/or determine the yields of products. However, these techniques show limitation in characterizing the reaction intermediates. Thus advanced characterization techniques, which can unveil the key processes in photo(thermal) catalysis, are crucial for understanding the intrinsic mechanisms involved in photo(thermal) catalytic reactions. Benefiting from the atomically well-defined and adjustable structures of MOFs, the photo(thermal) catalytic mechanisms of MOFs in organic transformations can be discussed in depth with the help of advanced characterization techniques. In this section, representative characterization techniques for determining charge reaction kinetics, identifying photo(thermal) catalytic intermediates, and elucidating the related mechanisms are discussed.

7.1. Transient absorption spectroscopy

To determine the CT kinetics, conventional electrochemical characterization techniques, including electrochemical impedance spectroscopy, transient photocurrent spectroscopy, and time-resolved photoluminescence spectroscopy, are readily available. However, their wide application is limited by their low temporal resolution, ranging from microseconds to seconds. TA spectroscopy, which can probe both photogenerated e⁻ and h⁺ and boasts exceptional temporal resolution up to the femtosecond (fs) range, has become a powerful experimental technology for studying ultrafast electronic dynamics processes in MOF-based photo(thermal) catalytic systems for organic transformations.^255,423

The accessibility of (dye˙⁻)* to reaction substrates, which can alleviate the consumption of back-electron transfer, plays a crucial role in photocatalytic organic reduction reactions.⁴²⁴ As mentioned above, by regulating the aromatic stacking mode of dyes relative to the CT kinetics in MOFs, Zeng et al. realized the efficient photoreduction of inert aryl halides to form C_Ar–C/S/P/B bonds.²⁵⁵ To obtain a deeper understanding, the fs-TA spectra of the radical anionic samples of the organic ligand H₄SNDI and the MOF photocatalyst Cd-SNDI were recorded. After the radical anionic H₄SNDI and Cd-SNDI were irradiated with a laser at 630 nm for ca. 1 ps, an excited-state absorption band with a broad coverage band of 400–550 nm was obtained (Fig. 34a and c), providing a decay time (τ) of 93 ps (probed at 445 nm, Fig. 34b) and 164 ps (probed at 480 nm, Fig. 34d), respectively. The τ value of Cd-SNDI was comparable to that of reported (NDI˙⁻)*. Moreover, the excited-state absorption of H₄SNDI was blue-shifted and narrower. These results indicate that the prolonged excited-state lifetime of (NDI˙⁻)* in Cd-SNDI enhances the CT process by increasing the accessibility of (NDI˙⁻)* to the substrate to promote the photoreduction efficiency of aryl halides.

7.2. Time-resolved photoluminescence spectroscopy

TRPL spectroscopy can be utilized to decipher the electron dynamics in the photoinduced process by detecting the average lifetime. Furthermore, the reduced lifetime can also be used to study the simultaneous electron transfer from excited photoactive units to catalytic active sites or the EnT process in photocatalytic systems related to ROS generation, both of which are crucial in MOF-based photo(thermal) catalysis for organic transformations.^143,156,269

By using the mixed-ligand MOF NPF-500-H₂TCPP as a photocatalyst, Fiankor et al. realized the efficient photocatalytic oxidation of thioanisole benefiting from the EnT process from the N,N′-bicarbazole ligand H₄L to the porphyrin ligand H₂TCPP.¹⁴³ TRPL technology was used to verify the EnT process in NPF-500-H₂TCPP. The emission lifetime of H₄L in NPF-500-H₂TCPP collected at 440 nm upon excitation at 280 nm was much shorter than that in NPF-500 (Fig. 35), indicating that the integrated H₂TCPP can quench the emission of H₄L. In addition, by fitting the emission decay kinetics, the average emission lifetimes of L in NPF-500 and NPF-500-H₂TCPP were 2.34 and 0.73 ns, respectively. The reduced lifetime further confirmed the efficient EnT process in NPF-500-H₂TCPP, which can mediate the generation of ROS ¹O₂ for the oxidation of thioanisole.

7.3. X-ray absorption spectroscopy

Based on synchrotron radiation, XAS can probe the local coordination environment of an element by monitoring fluctuations in the absorption of an ejected photoelectron. Generally, XAS is divided into two forms, namely, X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy, which can be used to determine the valence states and the coordination structure information (coordination elements, bond lengths, and coordination numbers) of catalytically active metal sites within MOF-based photo(thermal) catalysts for organic transformations, respectively.^423,425

To address the Pd reoxidation problem and efficiently improve Pd catalyst turnover for oxidative transformations, Li et al. successfully synthesized MOF-based photocatalysts UiO-67-Ir-PdX₂ (X = OAc, TFA), wherein spatially proximate Ir(III) and Pd(II) catalysts were integrated (Fig. 36a).⁴²³ XAS was performed to reveal the oxidation states and coordination environments of Pd and Ir in UiO-67-Ir–PdX₂. Based on XANES results of various standard species (Fig. 36b and d), the oxidation states of Pd(II) and Ir(III) are similar to those of their homogeneous counterparts. Fitting of the EXAFS data for UiO-67-Ir–Pd(OAc)₂ at the Pd K-edge revealed that the coordination number of Pd was approximately 4, and the average bond length of Pd–O/N was 2.00 Å (Fig. 36c). The EXAFS characteristic of UiO-67-Ir–Pd(OAc)₂ at the Ir L3 edge suggested that the Ir center was six-coordinated, and the average bond lengths of Ir–N_ppy, Ir–C_ppy, and Ir–C_bpy were 2.05 Å, 1.97 Å, and 2.12 Å, respectively (Fig. 36d). These XAS results fully demonstrated that the fabricated Ir(III) and Pd(II) catalysts in the UiO-66 framework possess well-defined coordination geometries and can contribute to the high turnover numbers in various photocatalytic oxidative organic transformations.

7.4. In situ Fourier transform infrared spectroscopy

In situ Fourier transform infrared (FTIR) spectroscopy, which has high sensitivity and a fast characterization speed, is a powerful technique that can be adopted by organic chemists for structural analysis. The characteristic vibration frequencies attributed to specific functional groups in the FTIR spectrum can be utilized to identify the chemical structures of unknown reaction intermediates (a process that resembles “fingerprinting”) over MOF-based photo(thermal) catalysis for organic transformations, conducing related mechanism studies at the molecular scale.^175,298

To further reveal the influence of surface functional sites, including the fully exposed Ti sites and the abundant oxygen vacancy sites, in the NH₂-MIL-125(Ti) nanosheet (MTN) photocatalyst modified with surface Pd on the oxidation of BA, in situ FTIR was conducted.²⁹⁸ In contrast to that of free BA molecules (1300 cm⁻¹), the characteristic peak of C–N bonds in the BA molecules absorbed on the surface of the MTNs shifts to a lower wavenumber (1280 cm⁻¹, Fig. 37a), suggesting that the C–N bonds in BA can be polarized and activated by the low-coordinate Ti metal sites in the MTNs via strong chemical adsorption to form Ti–N coordination bonds to enhance BA transformation. Moreover, the adsorption behavior of MTNs for the target product N-BBA was also studied. The inappreciable signal of the peak attributed to the CN bond of the adsorbed product on the spectrum (Fig. 37b) indicates that the product would not be adsorbed on MTNs, supporting that overoxidation can be inhibited in this photocatalytic system.

7.5. Diffuse reflectance infrared Fourier transform spectroscopy

Diffuse reflectance infrared Fourier transform (DRIFTS) spectroscopy, which can collect diffuse scattered signals from infrared radiation on powder samples, is widely applied for probing the structural information of species involved in photocatalytic processes. With regard to organic transformations by MOF-based photo(thermal) catalysis, DRIFTS can be used to trace reaction intermediates, detect the structural information of products, and assess the electron states of catalytic sites.^{58,176,256,408}

DRIFTS was carried out to obtain direct evidence of the unique advantages of the hollow microenvironment in yolk–shell nanostructured PdAg@ZIF8 on the selective adsorption and enrichment of substrates, which play a crucial role in the photothermal-catalyzed hydrogenation of nitrostyrene to vinylaniline.⁴⁰⁸ Under light irradiation, signals belonging to the –NO₂ and –CC– groups appear simultaneously at 5 min for the core–shell counterpart (Fig. 38a), suggesting its weak substrate enrichment effect and the lack of selective adsorption on both substrates. In contrast, with regard to the yolk–shell nanostructure, the signal of the –NO₂ group emerges rapidly within 1 min, and no signal attributed to the –CC– group is observed (Fig. 38b), indicating that the yolk–shell nanostructure has an excellent capacity to enrich the substrate and selectively adsorbs the –NO₂ group. Based on these results, the differences in the activity and selectivity of these two photocatalysts can be well understood.

7.6. Electron paramagnetic resonance spectroscopy

EPR spectroscopy is an indispensable technique for monitoring unpaired electrons in materials. Under a static magnetic field, the resonance transitions between different electron spin levels highly depend on the geometric structure and chemical microenvironment of paramagnetic species, which provides accurate EPR signals. As far, EPR spectroscopy has been intensively utilized in MOF-based photo(thermal) catalytic systems to detect various paramagnetic species, including active radicals and transition metal ions involved in organic transformation reactions.^{142,155,237,238,248,266,360}

To elucidate the light-induced electron transfer mechanism during the photocatalytic toluene oxidation process by Fe-UiO-66, in situ EPR was carried out.¹⁵⁵ After light irradiation in air, an EPR peak at g = 2.02 attributed to O₂˙⁻ absorbed on the Zr-oxo clusters appears, while the peak at g = 4.10 assigned to high-spin Fe(III) decreases (Fig. 39a). In addition, with the use of methanol as a hole sacrificial agent and under light irradiation in a N₂ atmosphere, the signal at g = 2.00 ascribed to oxygen-centered active sites in Zr-oxo clusters can be observed upon accepting e⁻ from Fe(III) (Fig. 39b). However, this signal significantly decreased after the introduction of air, indicating e⁻ transfer from the Zr-oxo cluster to O₂ molecules. Based on these in situ EPR results, e⁻ transfer from Fe(III) to the Zr-oxo-cluster, namely, the MCCT process, which contributes to the generation of ROS O₂˙⁻, can be evidenced.

8. Summary and outlook

This review comprehensively summarizes recent outstanding progress in the field of MOF-based photo(thermal) catalysis for organic transformations. The main focused aspects include the general mechanisms, the unique advantages of MOFs in photo(thermal) catalysis, common strategies to improve the performance of MOF-based photo(thermal) catalysts, the application of MOF-based photo(thermal) catalysts in organic transformation reactions of oxidation, reduction, coupling, tandem, synergistic redox, and CO₂ addition, as well as advanced characterization techniques that can help researchers understand the mechanisms of MOF-based photo(thermal) catalytic organic transformations. Although MOF-based photo(thermal) catalysts have provided a new platform for organic transformation because of their diverse structures, high specific surface area, and adjustable photophysical properties, this research is still at an early stage. Therefore, herein, some personal insights for advancing the long-term and high-quality development of this research area have been proposed.

First, the types of MOFs used for organic transformation reactions by photo(thermal) catalysis are limited. Currently, mainly Zr-, Ti-, and Cr-based MOFs have been widely studied, while MOF skeletons with traditional transition metals and lanthanides as metal centers are relatively rare. Moreover, in most cases, precious metal complexes such as Ru, Pd, Rh, and Ir are incorporated into and/or supported on MOF skeletons to function as efficient photosensitizers or cocatalysts, which is not favorable from the principle of economy. Hence, synthesis of MOFs with desired metal ions as well as the development of cost-effective sensitizers or cocatalysts are desirable for the further exploration of MOF-based photo(thermal) catalysts for organic transformations.

Second, the scope and efficiency of organic transformation reactions employing MOF-based photo(thermal) catalysts is still limited. To address this issue, MOFs with new/specific structures should be considered: (i) for tandem reactions, heterometallic MOFs consisting of more than one type of metal elements can realize the synergistic catalysis of different metal ions/clusters are suitable;^426–429 (ii) for photocatalytic asymmetric catalysis, chiral MOFs integrated with photoactive ingredients are targeted;^430,431 (iii) for high reaction efficiency, hierarchically porous MOFs with hierarchical pores can promote reaction kinetics via facilitating the diffusion rate and mass transfer of substrates,^432,433 and low-dimensional MOFs with selectively increased active sites or facets,^434–437 are desirable; (iv) for improved reaction selectivity, MOFs with atomically dispersed metal sites can function as durable photocatalysts, are targeted.⁴³⁸

Third, although pristine MOFs have been demonstrated to be popular photocatalysts, their application in photo(thermal) catalytic organic transformations is still restricted by their limited active sites. Coupling MOFs with other photo(thermal) active materials (such as metal NPs, POMs, and semiconductors) to construct MOF composites is promising way to develop this field. In this regard, low-temperature synthetic approaches for MOFs,^439,440 which can be utilized to construct MOF composites based on fragile compounds, are highly desirable. In addition, the fabrication of MOF-based core–shell composites,^183,441 which possess more exposed active sites, suppressed aggregation behavior in the photo(thermal) process, as well as efficient interfacial charge transfer and separation facilitated by the tight interaction between the core and shell, is also one of the most promising approaches worthy of attention. Moreover, synergistic catalysis by integrating photocatalysis with photothermal catalysis is believed to be an ideal way to improve the photocatalytic performance toward organic transformations.^442–444

Fourth, there are still some vague points in the mechanistic study of MOF-based photo(thermal) catalytic organic transformations. More detailed and clearer interpretations of the structure–activity relationship, temporal evolution of the photoinduced electron transition, charge carrier dynamics, and interactions between the excited states and the substrates are still needed. In addition, in contrast to the well-understood CT process, there is still room to clarify and understand the EnT mechanism, as well as the emerged HAT mechanism which has been recently utilized for MOF-based photocatalytic organic transformations through bond energy and polar match effect between the substrate and the HAT catalyst.⁴⁴⁵ Therefore, coupling advanced in situ or operando characterization techniques with computational chemistry or physics, which has been introduced to study the photo(thermal) catalysis of MOFs but at its infancy, is especially desirable for the development of the next generation of efficient MOF-based photo(thermal) catalysts for organic transformation reactions.

Last but not least, to realize industrial practical applications, many important factors still need to be carefully considered: (i) the reaction/cyclic stability and activity due to the structure collapse and/or the mechanical damage of MOFs during the photo(thermal) catalytic process; MOF-derived nano-materials consisting of metals, oxides, chalcogenides, phosphides, or carbides embedded in porous carbon matrix, which possess enhanced stability and effective photocatalytic efficiency, could be considered as the extensibility of the MOF-based photo(thermal) catalysts for organic transformations;^446,447 (ii) the unsatisfactory selectivity to target products in most MOF-based photo(thermal) catalytic systems; (iii) the lack of a scientific and recognized measure of efficiency that allows to get an unequivocally evaluation on the catalytic performances of different photocatalytic systems; (iv) the relatively low cost/performance ratio resulting from the high cost of functional components in MOF-based photo(thermal) catalysts, likely precious metal complexes and porphyrin derivatives; and (v) the potential problems that emerges when large-scale reactions for industrial production are conducted.

In summary, organic transformations driven by MOF-based photo(thermal) catalysts are still in their infancy, and there are both promising opportunities and tricky challenges. If these challenges can be solved due to the ever-increasing progress in the synthesis of MOF-based materials and the in-depth study of the properties and catalytic mechanisms of MOF-based photo(thermal) catalysts, a bright future wherein MOF-based photocatalysts contribute to the mass production of high-value-added chemicals utilizing real-life solar fuel can be envisioned.

Data availability

No primary research results, software or code have been included and no new data were generated or analysed as part of this review.

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

This work is supported by the National Key Research and Development Program of China (2021YFA1500400), the NSFC (22331009, U22A20401, 22205005), the Natural Science Foundation of Hunan Province (2023JJ30010), the Natural Science Foundation Project of Changsha City (kq2208217), the Strategic Priority Research Program of the Chinese Academy of Sciences (XDB0450302 and XDB0540000), and Fundamental Research Funds for the Central Universities (WK9990000137).

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