层状双金属氢氧化物(LDH)基光催化剂在太阳能燃料生产领域的研究进展

doi:10.1016/S1872-2067(21)63861-5

摘要/Abstract

摘要：

半导体光催化剂吸收太阳光分解水制氢或还原CO₂, 实现了太阳能燃料生产, 不仅可获取清洁、可再生、高热值的太阳能燃料, 还能有效减少CO₂的排放. 层状双金属氢氧化物(LDHs)是一类基于水镁石结构的二维阴离子黏土矿物材料, 具有独特的层状结构、主体层金属阳离子可调性、客体阴离子可交换、多维结构和可分层等优势, 在CO₂还原、光电催化水产氧及光解水制氢等领域研究广泛, 有望成为新型半导体光催化材料. 但单纯LDHs载流子迁移率低和电子空穴复合率高, 在太阳辐射下的量子效率非常低. 因此, 研究人员采用缺陷控制、设计多维结构或偶联不同类型半导体构建异质结等方法, 获得高能量转换效率的LDH基光催化剂.
本文首先总结了传统光催化剂的优缺点及其能带分布, 阐述了LDHs的六个主要方面特性, 包括主体层板金属阳离子可调性、客体阴离子插层、热分解、记忆效应、多维结构特征及分层, 进而提出LDH基光催化材料在增强反应物吸附活化、扩宽吸光范围、抑制光生载流子与空穴复合三个方面的改性策略. 然后, 分析了LDH光催化剂的光催化水解产氢反应机理, 并从材料结构与性能的关联, 概述LDH基复合光催化剂(金属硫化物LDH复合材料、金属氧化物LDH复合材料、石墨相氮化碳LDH复合材料)、三元LDH基光催化剂及混合金属氧化物光催化剂在水分解制氢领域的研究进展. 最后, 分析了LDH光催化还原CO₂反应机理, 归纳石墨相氮化碳复合LDH材料、MgAl-LDH基复合光催化剂、CuZn-LDH光催化剂及其它半导体系列LDH的结构特点和在还原CO₂领域的研究进展.
尽管LDH基光催化剂研究取得了一定的进展, 但是对LDH的结构调控及其光催化机理仍需进一步探索, 光催化活性位点、不同组分之间的协同作用和界面反应机理还有待进一步研究. 未来LDH在光催化领域的应用可以微观尺度调控和宏观性能为导向设计, 进一步研究不同组分的协同效应、界面反应及材料组成对物理化学性质的影响, 不断完善LDH基光催化剂的理论系统和开发其应用潜能.

关键词: 层状双金属氢氧化物, 水滑石, 产氢, 二氧化碳还原, 光催化, 太阳能燃料生产

Abstract:

Splitting water or reducing CO₂ via semiconductor photocatalysis to produce H₂or hydrocarbon fuels through the direct utilization of solar energy is a promising approach to mitigating the current fossil fuel energy crisis and environmental challenges. It enables not only the realization of clean, renewable, and high-heating-value solar fuels, but also the reduction of CO₂ emissions. Layered double hydroxides (LDHs) are a type of two-dimensional anionic clay with a brucite-like structure, and are characterized by a unique, delaminable, multidimensional, layered structure; tunable intralayer metal cations; and exchangeable interlayer guest anions. Therefore, it has been widely investigated in the fields of CO₂ reduction, photoelectrocatalytic water oxidation, and water photolysis to produce H₂. However, the low carrier mobility and poor quantum efficiency of pure LDH limit its application. An increasing number of scholars are exploring methods to obtain LDH-based photocatalysts with high energy conversion efficiency, such as assembling photoactive components into LDH laminates, designing multidimensional structures, or coupling different types of semiconductors to construct heterojunctions. This review first summarizes the main characteristics of LDH, i.e., metal-cation tunability, intercalated guest-anion substitutability, thermal decomposability, memory effect, multidimensionality, and delaminability. Second, LDHs, LDH-based composites (metal sulfide-LDH composites, metal oxide-LDH composites, graphite phase carbon nitride-LDH composites), ternary LDH-based composites, and mixed-metal oxides for splitting water to produce H₂ are reviewed. Third, graphite phase carbon nitride-LDH composites, MgAl-LDH composites, CuZn-LDH composites, and other semiconductor-LDH composites for CO₂ reduction are introduced. Although the field of LDH-based photocatalysts has advanced considerably, the photocatalytic mechanism of LDHs has not been thoroughly elucidated; moreover, the photocatalytic active sites, the synergy between different components, and the interfacial reaction mechanism of LDH-based photocatalysts require further investigation. Therefore, LDH composite materials for photocatalysis could be developed through structural regulation and function-oriented design to investigate the effects of different components and interface reactions, the influence of photogenerated carriers, and the impact of material composition on the physical and chemical properties of the LDH-based photocatalyst.

Key words: Layered double hydroxides, Hydrotalcite, H₂ production, CO₂ reduction, Photocatalysis, Solar fuel production

汪凯林, 王天琦, Quazi Arif Islam, 吴艳. 层状双金属氢氧化物(LDH)基光催化剂在太阳能燃料生产领域的研究进展[J]. 催化学报, 2021, 42(11): 1944-1975.

Kailin Wang, Tianqi Wang, Quazi Arif Islam, Yan Wu. Layered double hydroxide photocatalysts for solar fuel production[J]. Chinese Journal of Catalysis, 2021, 42(11): 1944-1975.

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图/表 42

Fig. 1. Traditional semiconductor photocatalysts for solar fuel production.

Fig. 2. Band positions of semiconductor photocatalysts at pH = 7 in aqueous solution.

Table 1 Characteristics of major semiconductor photocatalysts.

Photocatalyst	CB/VB level (V, vs. NHE (pH = 7))	Bandgap (eV)	Advantages	Disadvantages	Ref.
TiO₂	-0.2/3.0	3.2	resistant to chemical corrosion and photocorrosion; low cost	wide band gap; responds to ultraviolet (UV) light only; easy recombination of photoinduced carriers	[20]
Cu₂O	-0.28/1.92	2.2	CB matching	photocorrosion; poor stability; easy recombination of photoinduced carriers	[33,34]
CdS	-0.52/1.88	2.4	energy band matching	aggregation; poor cycle stability; easy recombination of photoinduced carriers	[36,94,95]
CdZnS	—	2.32-3.73	adjustable bandgap; high photocatalytic activity	aggregation; photocorrosion	[37-39]
g-C₃N₄	-0.65/2.05	2.7	nontoxic; low cost; resistant to photocorrosion; Narrow bandgap; Overall water splitting capacity	easy recombination of photoinduced carriers	[36,40]
BiOCl BiOBr BiOI	—	3.40 2.77 1.86	adjustable bandgap; highly anisotropic, layered structure	poor thermal stability; lattice transformation	[42-44]
CoO	-0.87/1.88	2.75	relatively narrow bandgap; good optical response to visible light; high electron mobility	particles are prone to aggregation; photocatalyst easily deactivates after short reaction time	[60-62]
ZnO	-0.3/2.9	3.2	low cost; high redox potential; innocuous and environmentally friendly	relatively wide bandgap; low utilization of sunlight	[48-53]
MoS₂	0.23/1.4	1.17	narrow bandgap; good light absorption ability; high carrier mobility	poor electrical conductivity	[63-65]
CuFeS₂	0.3/0.9	0.6	narrow bandgap; high electrical conductivity	photogenerated electrons easily recombine with holes	[66,67]
In₂S₃	-0.8/1.2	2	high thermal stability (750 °C); high photosensitivity; relatively narrow bandgap	rapid photogenerated electron-hole recombination; poor quantum yield	[68,69]
WO₃	0.74/3.44	2.7	excitable under 480 nm light (visible light); high VB potential (3.2 V); strong oxidation catalyst	electrons generated by light cannot react effectively with electron-acceptor molecules	[96-98]
ZnS	-1.04/2.56	3.6	high carrier mobility (reduced carrier scattering and recombination); good thermal stability; high electron mobility	relatively wide bandgap; only absorbs UV light	[57-59]
SrTiO₃	-1.26/2.14	3.4	photochemical corrosion resistance; good thermal stability; good heat resistance	relatively wide bandgap; mainly absorbs UV light; low utilization of sunlight	[54,55]
NiS	0.53/0.93	0.4	inexpensive; nontoxic; narrow bandgap; multiple active centers	rapid recombination of charge carriers; poor adsorption capacity	[99,100]
ZnIn₂S₄	-0.9/1.9	2.8	low cost; high photostability; low toxicity	relatively wide bandgap; slow charge transfer	[56,99]

Table 1 Characteristics of major semiconductor photocatalysts.

Photocatalyst	CB/VB level (V, vs. NHE (pH = 7))	Bandgap (eV)	Advantages	Disadvantages	Ref.
TiO₂	-0.2/3.0	3.2	resistant to chemical corrosion and photocorrosion; low cost	wide band gap; responds to ultraviolet (UV) light only; easy recombination of photoinduced carriers	[20]
Cu₂O	-0.28/1.92	2.2	CB matching	photocorrosion; poor stability; easy recombination of photoinduced carriers	[33,34]
CdS	-0.52/1.88	2.4	energy band matching	aggregation; poor cycle stability; easy recombination of photoinduced carriers	[36,94,95]
CdZnS	—	2.32-3.73	adjustable bandgap; high photocatalytic activity	aggregation; photocorrosion	[37-39]
g-C₃N₄	-0.65/2.05	2.7	nontoxic; low cost; resistant to photocorrosion; Narrow bandgap; Overall water splitting capacity	easy recombination of photoinduced carriers	[36,40]
BiOCl BiOBr BiOI	—	3.40 2.77 1.86	adjustable bandgap; highly anisotropic, layered structure	poor thermal stability; lattice transformation	[42-44]
CoO	-0.87/1.88	2.75	relatively narrow bandgap; good optical response to visible light; high electron mobility	particles are prone to aggregation; photocatalyst easily deactivates after short reaction time	[60-62]
ZnO	-0.3/2.9	3.2	low cost; high redox potential; innocuous and environmentally friendly	relatively wide bandgap; low utilization of sunlight	[48-53]
MoS₂	0.23/1.4	1.17	narrow bandgap; good light absorption ability; high carrier mobility	poor electrical conductivity	[63-65]
CuFeS₂	0.3/0.9	0.6	narrow bandgap; high electrical conductivity	photogenerated electrons easily recombine with holes	[66,67]
In₂S₃	-0.8/1.2	2	high thermal stability (750 °C); high photosensitivity; relatively narrow bandgap	rapid photogenerated electron-hole recombination; poor quantum yield	[68,69]
WO₃	0.74/3.44	2.7	excitable under 480 nm light (visible light); high VB potential (3.2 V); strong oxidation catalyst	electrons generated by light cannot react effectively with electron-acceptor molecules	[96-98]
ZnS	-1.04/2.56	3.6	high carrier mobility (reduced carrier scattering and recombination); good thermal stability; high electron mobility	relatively wide bandgap; only absorbs UV light	[57-59]
SrTiO₃	-1.26/2.14	3.4	photochemical corrosion resistance; good thermal stability; good heat resistance	relatively wide bandgap; mainly absorbs UV light; low utilization of sunlight	[54,55]
NiS	0.53/0.93	0.4	inexpensive; nontoxic; narrow bandgap; multiple active centers	rapid recombination of charge carriers; poor adsorption capacity	[99,100]
ZnIn₂S₄	-0.9/1.9	2.8	low cost; high photostability; low toxicity	relatively wide bandgap; slow charge transfer	[56,99]

Fig. 3. The structure of carbonate-intercalated LDH.

Fig. 4. (a) Diagram of the photocatalytic mechanism of O2 production over LDH. Adapted with permission from Ref. [110]. Copyright 2009, American Chemical Society. (b) CuCoCr-LDH structural model. Adapted with permission from Ref. [111]. Copyright 2012, American Chemical Society. (c) Photoreduction schemes of different ZnM-LDH photocatalysts. Adapted with permission from Ref. [87]. Copyright 2020, Science China Press. Published by Elsevier B.V. and Science China Press.

Fig. 5. (a) Schematic diagram of intercalation of a series of boric acid anions between layers of LDH. Adapted with permission from Ref. [112]. Copyright 2010, Elsevier B.V. (b) Schematic diagram of ion exchange scheme and adsorption reaction principle of MoS4-LDH. Adapted with permission from Ref. [117]. Copyright 2016, American Chemical Society. (c) Schematic diagram of the anion-intercalated crystal structure of PAAS-LDH and its adsorption reaction principle. Adapted with permission from Ref. [118]. Copyright 2021, Elsevier B.V.

Fig. 6. (a) Hydrogenation mechanism of a ZnFeAl-LDH photocatalyst under thermal decomposition. Adapted with permission from Ref. [123]. Copyright 2018, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. (b) Selectivity of CO hydrogenation after thermal decomposition of LDH nanosheets. Adapted with permission from Ref. [124]. Copyright 2019, Elsevier B.V.

Fig. 7. (a) Structural diagram and photocatalytic mechanism of TiO2/CuMgAl-RLDH. Adapted with permission from Ref. [130]. Copyright 2011, Elsevier B.V. (b) CuZnAl-LDH memory effect and structural transformation. Adapted with permission from Ref. [127]. Copyright 2013, Elsevier B.V.

Fig. 8. (a) Cross-sectional HRTEM image of a ZCT-1 nanohybrid (left) and its enlarged view and structural model (right). Adapted with permission from Ref. [139]. Copyright 2011, American Chemical Society. (b) Synthesis of TiO2@CoAl-LDH core-shell nanospheres for O2 production. Adapted with permission from Ref. [140]. Copyright 2015, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fig. 9. (a) Schematic diagram of the preparation of LDH single layers based on “top-down” and “bottom-up” approaches. Adapted with permission from Ref. [141]. Copyright 2012, American Chemical Society. (b) Schematic diagram of VO, VCo, and catalytic mechanism of composites. Adapted with permission from Ref. [154]. Copyright 2018, American Chemical Society. (c) Unsaturated coordination of nanocomposites and charge transfer and separation process of CO2 photoreduction. Adapted with permission from Ref. [155]. Copyright 2020, Elsevier B.V.

Fig. 10. Three strategies for the modification of LDH-based photocatalysts.

Fig. 11. Schematic diagram of the mechanism of H2 and O2 production over LDH-based photocatalysts.

Fig. 12. (a) Scheme of photoexcitation of electrons from Cr-3d t2g to Cr-3d eg in a CrO6 octahedron by irradiation with visible light. (b) Proposed mechanism of H2 production through water decomposition over a Zn/Cr-CO3 photocatalyst. (a) and (b) Adapted with permission from Ref. [184]. Copyright 2012, Royal Society of Chemistry. (c) Mechanism of H2 production through water decomposition over a Ni + Zn/Cr LDH photocatalyst under visible-light irradiation. Adapted with permission from Ref. [186]. Copyright 2013, Royal Society of Chemistry. (d) Comparison of the H2 evolution rate of different Mg/Al + Fe-CO3 LDHs under irradiation. Adapted with permission from Ref. [187]. Copyright 2012, Royal Society of Chemistry.

Fig. 14. (a) Schematic model of the linker-mediated self-assembly of ZnCr-LDH-CdS nanohybrids. Adapted with permission from Ref. [193]. Copyright 2014, Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. (b) The preparation of hierarchical flower-like CdZnS@LDH and its application in photocatalytic H2 production. Adapted with permission from Ref. [197]. Copyright 2015, Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. (c) Schematic model of photocatalysis of NiCo-LDH/P-CdS composites. Adapted with permission from Ref. [198]. Copyright 2019, Elsevier B.V.

Fig. 15. (a) Flow chart of the preparation of electrostatic MoS2/NiFe-LDH. (b) Diagrams of two charge-transfer mechanisms for MoS2/NiFe-LDH (double charge (left), direct Z-scheme mechanism (right)). (a) and (b) adapted with permission from Ref. [202]. Copyright 2019, American Chemical Society. (c) Schematic diagram of the synthesis of MgAl-LDH/NiS hybrids. Adapted with permission from Ref. [206]. Copyright 2019, Elsevier B.V.

Fig. 19. (a) Photocatalytic mechanism of CeO2/MgAl-LDH. Adapted with permission from Ref. [217]. Copyright 2016, Hydrogen Energy Publications LLC. (b) Schematic diagram of the photoexcited carrier separation/transport in a Cu2O@ZnCr-LDH photocatalyst. Adapted with permission from Ref. [218]. Copyright 2018, Royal Society of Chemistry.

Fig. 21. (a) Schematic of the band structure and charge transfer process in NiAl-LDH/g-C3N4. Adapted with permission from Ref. [222]. Copyright 2017, Hydrogen Energy Publications LLC. (b) Schematic of the charge separation and transfer mechanism in a CNLDH composite material. Adapted with permission from Ref. [220]. Copyright 2015, Royal Society of Chemistry. (c) Schematic of the synthesis of a ZnCr-LDH-g-C3N4 nanohybrid. Adapted with permission from Ref. [223]. Copyright 2018, Royal Society of Chemistry.

Fig. 23. (a) Photocatalytic performance of Au/LDH and Au/LDH750 photocatalysts; (◆) Au/ZnCeAlLDH; (△) Au/ZnAl-LDH; (○) Au/ZnAl-LDH750; (◇) Au/ZnCeAl-LDH750. (b) Mechanism of H2 generation from water-methanol mixtures on Au/LDH. (a) and (b) Adapted with permission from Ref. [224]. Copyright 2013, the Royal Society of Chemistry. (c) Schematic illustration of H2 production over an LDHLFO nanocomposite under visible-light irradiation. (d) Schematic illustration of photocatalytic decolorization of rhodamine B under solar-light irradiation. (c) and (d) Adapted with permission from Ref. [226]. Copyright 2017, Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim. (e) Mechanism of the charge separation process and photocatalytic H2 and O2 evolution over Co(OH)2/ZnCr-LDH. Adapted with permission from Ref. [227]. Copyright 2018, American Chemical Society.

Fig. 24. (a) Illustration of the photocatalytic mechanism of H2 production over ZnS-ZnO/ZnAl-LDH. Adapted with permission from Ref. [231]. Copyright 2019, Elsevier B.V. (b) Proposed mechanism of charge separation and transfer kinetics in rGO/LTO/NiFe-LDH composite photocatalysts. Adapted with permission from Ref. [232]. Copyright 2018, Elsevier B.V. (c) Synthesis of a CNNG-X-LDH heterostructure. (d) (i) Rhodamine B degraded, (ii) phenol treated, and (iii) H2 and O2 evolved in five consecutive photocatalytic cycles of 120 mins each over CNNG-3-LDH. (c) and (d) Adapted with permission from Ref. [233]. Copyright 2019, Susanginee Nayak.

Fig. 25. (a) The energy band arrangement of LDH and CFO (i) before and (ii) after contact between LDH and CFO, and (iii) after loading gold (iii). Adapted with permission from Ref. [234]. Copyright 2019, Partner Organizations. (b) Proposed photocatalytic mechanisms of the (left) Ag/WO3-X/LDH heterostructure and (right) WO3-X/Ag/LDH-based reaction systems for TC degradation and H2 evolution. Adapted with permission from Ref. [235]. Copyright 2019, American Chemical Society.

Fig. 26. The band structures (a) and the proposed photocatalytic water splitting mechanism (b) over NiAl-LDH/g-C3N4/Ag3PO4. Adapted with permission from Ref. [236]. Copyright2021, Royal Society of Chemistry.

Fig. 27. (a) Synthesis of a porous MgO/MgCr2O4(x) nanocomposite. Adapted with permission from Ref. [241]. Copyright 2018, American Chemical Society. (b) Schematic of the mechanism of photocatalytic H2 production over CN/MgFe-X. Adapted with permission from Ref. [242]. Copyright 2018, Elsevier B.V. (c) Proposed mechanism describing the role of Zn6Al2O9 in the photoactivity of the material calcined at 600 °C (ZnAl 600). Adapted with permission from Ref. [243]. Copyright 2018, Elsevier B.V.

Table 2 Summary of LDH-based photocatalysts for H2 evolution.

Photocatalyst	Synthetic method	Light source (λ > 420 nm)	Scavenger/ Cocatalyst	H₂ (μmol·h^-1·g^-1)	Ref.
Zn/Cr-CO₃^2- LDH	coprecipitation method	125 W Hg	CH₃OH	1732	[184]
Ni-Zn/Cr-CO₃^2- LDH	coprecipitation method	125 W Hg	CH₃OH	1915	[186]
Mg/Al/Fe-CO₃^2-LDH	coprecipitation method	125 W Hg	CH₃OH	493	[187]
CdS/ZnCr-LDH	exfoliation-restacking approach	300 W Xe	Na₂S + Na₂SO₃	374	[192]
CdS/ZnCr-LDH	electrostatic assembly	450 W Xe	Na₂S + Na₂SO₃/Pt	1560	[193]
CdZnS@ZnCr-LDH	one-pot hydrothermal method	300 W Xe	CH₃OH/ Pt	916.2	[197]
NiCo-LDH/p-CdS	P-doping and in-situ loading methods	300 W Xe	lactic acid	8665	[198]
MoS₂/NiFe-LDH	electrostatic self-assembly and in situ hydrothermal method	125 W Hg	CH₃OH	18363	[202]
CdS/NiFe-LDH	in situ growth method	300 W Xe	CH₃OH	469	[94]
MoS₂/CoAl-LDH	simple hydrothermal method	300 W Xe	CH₃OH	17.1	[208]
ZnS/ZnIn-LDH	in situ etching and growth process	300 W Xe	Na₂S + Na₂SO₄	154.8	[58]
MgAl-LDH/NiS	facile hydrothermal treatment and precipitation	300 W Xe	CH₃OH	895	[206]
CeO₂/MgAl-LDH	combination of coprecipitation and hydrothermal treatment	125 W Hg	CH₃OH	16500	[217]
CoO/NiCo-LDH	hydrothermal synthesis	100 W Xe	Na₂S + Na₂SO₃	1500	[62]
g-C₃N₄/NiFe-LDH	coprecipitation method	125 W Hg	CH₃OH	24800	[220]
ZnCr LDH/g-C₃N₄	electrostatic self-assembly	300 W Xe	TEOA/Pt	186.97	[222]
ZnCr LDH/g-C₃N₄	—	300 W Xe	TEOA	155.7	[223]
g-C₃N₄/CoAl-LDH	hydrothermal synthesis	300 W Xe	TEOA	680.13	[168]
CdSe/ZnCr-LDH	electrostatic self-assembly	300 W Xe	Na₂S + Na₂SO₃	2196	[225]
Co(OH)₂/ZnCr-LDH	homogeneous precipitation method	125 W Hg	CH₃OH	27875	[227]
NiFe-LDH/N-rGO/g-C₃N₄	calcination-electrostatic self-assembly and hydrothermal treatment	125 W Hg	CH₃OH	41800	[233]
Au/CaFe₂O₄/CoAl-LDH	Simple sol-gel method	150 W Xe	CH₃OH	18955	[234]
WO_3-_x/Ag/ZnCr-LDH	—	150 W Xe	CH₃OH	29375	[235]
NiAl-LDH/g-C₃N₄/Ag₃PO₄	—	150 W Xe	Na₂SO₄	268	[236]
MgO/MgCr₂O₄	coprecipitation and heat treatment	125 W Hg	CH₃OH	14000	[241]
g-C₃N₄/MgFe-MMO	coprecipitation and heat treatment	300 W Xe	TEOA/Pt	1260	[242]

Table 2 Summary of LDH-based photocatalysts for H2 evolution.

Photocatalyst	Synthetic method	Light source (λ > 420 nm)	Scavenger/ Cocatalyst	H₂ (μmol·h^-1·g^-1)	Ref.
Zn/Cr-CO₃^2- LDH	coprecipitation method	125 W Hg	CH₃OH	1732	[184]
Ni-Zn/Cr-CO₃^2- LDH	coprecipitation method	125 W Hg	CH₃OH	1915	[186]
Mg/Al/Fe-CO₃^2-LDH	coprecipitation method	125 W Hg	CH₃OH	493	[187]
CdS/ZnCr-LDH	exfoliation-restacking approach	300 W Xe	Na₂S + Na₂SO₃	374	[192]
CdS/ZnCr-LDH	electrostatic assembly	450 W Xe	Na₂S + Na₂SO₃/Pt	1560	[193]
CdZnS@ZnCr-LDH	one-pot hydrothermal method	300 W Xe	CH₃OH/ Pt	916.2	[197]
NiCo-LDH/p-CdS	P-doping and in-situ loading methods	300 W Xe	lactic acid	8665	[198]
MoS₂/NiFe-LDH	electrostatic self-assembly and in situ hydrothermal method	125 W Hg	CH₃OH	18363	[202]
CdS/NiFe-LDH	in situ growth method	300 W Xe	CH₃OH	469	[94]
MoS₂/CoAl-LDH	simple hydrothermal method	300 W Xe	CH₃OH	17.1	[208]
ZnS/ZnIn-LDH	in situ etching and growth process	300 W Xe	Na₂S + Na₂SO₄	154.8	[58]
MgAl-LDH/NiS	facile hydrothermal treatment and precipitation	300 W Xe	CH₃OH	895	[206]
CeO₂/MgAl-LDH	combination of coprecipitation and hydrothermal treatment	125 W Hg	CH₃OH	16500	[217]
CoO/NiCo-LDH	hydrothermal synthesis	100 W Xe	Na₂S + Na₂SO₃	1500	[62]
g-C₃N₄/NiFe-LDH	coprecipitation method	125 W Hg	CH₃OH	24800	[220]
ZnCr LDH/g-C₃N₄	electrostatic self-assembly	300 W Xe	TEOA/Pt	186.97	[222]
ZnCr LDH/g-C₃N₄	—	300 W Xe	TEOA	155.7	[223]
g-C₃N₄/CoAl-LDH	hydrothermal synthesis	300 W Xe	TEOA	680.13	[168]
CdSe/ZnCr-LDH	electrostatic self-assembly	300 W Xe	Na₂S + Na₂SO₃	2196	[225]
Co(OH)₂/ZnCr-LDH	homogeneous precipitation method	125 W Hg	CH₃OH	27875	[227]
NiFe-LDH/N-rGO/g-C₃N₄	calcination-electrostatic self-assembly and hydrothermal treatment	125 W Hg	CH₃OH	41800	[233]
Au/CaFe₂O₄/CoAl-LDH	Simple sol-gel method	150 W Xe	CH₃OH	18955	[234]
WO_3-_x/Ag/ZnCr-LDH	—	150 W Xe	CH₃OH	29375	[235]
NiAl-LDH/g-C₃N₄/Ag₃PO₄	—	150 W Xe	Na₂SO₄	268	[236]
MgO/MgCr₂O₄	coprecipitation and heat treatment	125 W Hg	CH₃OH	14000	[241]
g-C₃N₄/MgFe-MMO	coprecipitation and heat treatment	300 W Xe	TEOA/Pt	1260	[242]

Fig. 28. Schematic diagram of the reduction of CO2 over LDH-based photocatalysts.

Fig. 29. (a) Schematic illustration of the synthesis of g-C3N4/NiAl-LDH hybrid heterojunctions. (b) Schematic illustration of the proposed mechanism of CO2 photoreduction over g-C3N4/NiAl-LDH. (a) and (b) Adapted with permission from Ref. [289]. Copyright 2018, American Chemical Society. (c) Schematic illustration of the proposed mechanism for CO2 photoreduction over a NCD/LDH/CN hybrid photocatalyst. Adapted with permission from Ref. [290]. Copyright 2019, Elsevier B.V.

Fig. 30. (a) Scheme for synthesizing a sea urchin-like CoZnAl-LDH/RGO/g-C3N4 hybrid. (b) Schematic diagram of the possible photocatalytic mechanism of LDH/RGO/CN. Adapted with permission from Ref. [263]. Copyright 2019, Elsevier B.V.

Fig. 32. Atomic force microscopy images of MgAl-LDH (a), and Fe3O4/MgAl-LDH (b); (c) the mechanism for the photocatalytic reduction of CO2 over Fe3O4/MgAl-LDH and charge carrier transfer under UV-light irradiation. Adapted with permission from Ref. [299]. Copyright 2019, Elsevier B.V.

Fig. 33. (a,b,c) The performance of MgAl-LDO/TiO2-2 with a Pt cocatalyst in the photocatalytic reduction of CO2; (d) The mechanism of photocatalytic CO2 reduction over Pt/MgAl-LDO/TiO2 in the presence of H2O vapor. Adapted with permission from Ref. [305]. Copyright 2018, Elsevier B.V.

Fig. 34. (a) Performance of MAl-LDH (M = Co2+, Ni2+, Zn2+, and Mg2+) photocatalysts; (b) bandgaps of different MAl-LDH photocatalysts; (c) scheme of the photocatalytic reduction of CO2 over CoAl-LDH. Adapted with permission from Ref. [306]. Copyright 2020, American Chemical Society.

Fig. 37. (a) The mechanism of CO2 photoreduction over a P25@CoAl-LDH nanocomposite. Adapted with permission from Ref. [178]. Copyright 2017, Elsevier B.V. (b) The mechanism of CO2 reduction over CoAl-LDH-DS@TiO2-NT. Adapted with permission from Ref. [321]. Copyright 2017, WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. (c) The mechanism of photocatalytic CO2 reduction over TiO2/LDH. Adapted with permission from Ref. [325]. Copyright 2020, Royal Society of Chemistry.

Table 3 Summary of LDH-based photocatalysts for CO2 reduction.

Photocatalyst	Synthetic method	Light source	Scavenger / Cocatalyst	Production/ Selectivity	Yield (μmol·h^-1·g^-1)	Ref.
g-C₃N₄/NiAl-LDH	electrostatic assembly	300 W Xe	ethanol/nafion	CO/—	8.2	[289]
NCD/LDH/CN	one-pot hydrothermal method	300 W Xe	—	CH₄/99%	25.69	[290]
CoZnAl-LDH/RGO/g-C₃N₄	hydrothermal synthesis	300 W Xe	deionized water	CO/—	10.11	[263]
g-C₃N₄/NiAl-LDH	self-sacrificing template	300 W Xe	deionized water	CO/—	27.02	[291]
Fe₃O₄/MgAl-LDH	coprecipitation method	8 W UV	ethanol and oleic acid	CO/68.9%	442.2	[299]
MgAl-LDO/TiO₂	hydrothermal and coprecipitation methods	450 W Xe	—	CO/—	4.3	[304]
CoAl-LDH	one-pot hydrothermal synthesis	300 W Xe	TEOA/CH₃CN	CO/—	43730	[306]
Pt/MgAl-LDO/TiO₂	in situ deposition	300 W Xe	CH₃OH	CH₄/—	4.6	[305]
ZnO@CuZnAl-LDH	interfacial deposition and precipitation	450 W Xe	—	CH₄/—	11.42	[315]
Cu-Zn(1-x) Ga(x)-O₃/LDH	aqueous miscible organic solvent treatment	Visible light	—	CH₃OH/97%	187.5	[316]
ZnCr-LDH/Cu₂O	in situ reduction	200 W Hg-Xe	Na₂SO₄/Na₂CO₃	CO/62.3%	26	[252]
CoAl-LDH@P25	one-pot hydrothermal synthesis	300 W Xe	—	CO/>90%	2.21	[178]
CoAl-LDH-DS @TiO₂	one-pot hydrothermal synthesis	300 W Xe	—	CO/—	4.57	[321]
TiO_2-_x/LDH	solvothermal, hydrogen treatment, and hydrothermal methods	300 W Xe	—	CH₃OH CH₄	251 63	[169]
TiO₂/NiAl-LDH	hydrothermal calcination	—	—	CH₄/78% CO	20.56 2.48	[325]
NiCoFe-LDH	coprecipitation method	300 W Xe	TEOA	CH₄/78.9%	—	[326]
Co-Co LDH/TNS	in situ MOF-derived strategy	5 W LED	TEOA	CO/63.9%	12500	[327]
β-In₂S₃/NiAl-LDH	simple one-step hydrothermal method	300 W Xe	—	CH₄/—	36.1	[68]

Fig. 38. (a) Schematic illustration of photocatalytic CO2 reduction to CH4 over CoFe-LDH and NiCoFe-LDH under λ > 500 nm in the presence of a Ru complex sensitizer. Adapted with permission from Ref. [326]. Copyright 2021, American Chemical Society. (b) Proposed photocatalytic CO2 reduction mechanism of Co-Co-LDH/TNS. Adapted with permission from Ref. [327]. Copyright 2019, Elsevier B.V.

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