Metal oxide mesocrystals and mesoporous single crystals: synthesis, properties and applications in solar energy conversion

doi:10.1016/j.jmst.2020.09.025

Abstract

Abstract:

Metal oxide mesocrystals (MCs) and mesoporous single crystals (MSCs) exhibit superior carrier transport ability, high specific surface area, shortened photo-carrier diffusion lengths to interfaces and enhanced absorbance of the incident sunlight. These advanced features make metal oxide MCs and MSCs be a promising candidate material in photocatalysis, photoelectrocatalysis, dye sensitized solar cells (DSSCs) and perovskite solar cells (PSCs). Recently, remarkable advances of applying metal oxide MCs and MSCs in these areas have been achieved. Therefore, it is extremely important to deeply understand the influence of the unique properties of metal oxide MCs and MSCs on solar energy conversion systems. Herein, we presented a brief introduction on the synthesis and carrier transfer behavior of metal oxide MCs and MSCs. Then, the rational structure design and modification of metal oxide MCs and MSCs for photocatalysis, photoelectrocatalysis, DSSCs and PSCs are systematically discussed. Finally, the perspectives on extending the application of metal oxide MCs and MSCs are addressed.

Key words: Metal oxide mesocrystals, Mesoporous single crystals, Photocatalysis, Photoelectrocatalysis, Dye sensitized solar cells, Perovskite solar cells

Tingting Wu, Guoqiang Deng, Chao Zhen. Metal oxide mesocrystals and mesoporous single crystals: synthesis, properties and applications in solar energy conversion[J]. J. Mater. Sci. Technol., 2021, 73: 9-22.

Figures/Tables 14

Fig. 1. Basic principles of (a) DSSCs and PSCs, (b) photocatalysis and (c) PEC cells.

Fig. 2. The classical crystallization (blue route) via ion-by-ion addition versus single-crystal formation (red route) by a mesocrystal intermediate made of nanoparticles. (a-d) Illustrative diagrams of the four principal possibilities that could explain the 3D oriented alignment of nanoparticles, a) by an oriented organic matrix, b) by physical fields or mutual alignment of identical crystal faces, c) by epitaxial growth of a nanoparticle employing a mineral bridge connecting the two nanoparticles, and d) by spatial constraints [34].

Fig. 3. (a) SEM and (b) HRTEM images of nanoporous anatase TiO2 mesocrystals. The inset in (b) shows the SAED pattern related to the whole particle; (c) Schematic illustration of a tentative mechanism for the formation of nanoporous anatase TiO2 mesocrystals without additives [51].

Fig. 4. Illustration of the oriented transformation of NH4TiOF3 mesocrystal to TiO2 (anatase) mesocrystal [60].

Fig. 5. (a) Schematic of MSC nucleation and growth within a mesoporous template. (b) Template-nucleated variant of the solid crystals, grown from a seed at or near the external template surface such that a non-porous volume coexists with a mesoporous region within a single faceted microcrystal. (c) Fully mesoporous TiO2 crystals grown by seeded nucleation in the bulk of the silica template. (d) Schematic of the synthesis procedures of the films of nonporous single-crystal rod arrays (the top panel) and mesoporous single‐crystal rod arrays (the bottom panel) of rutile TiO2 supported on fluorine-doped tin oxide (FTO) glass substrates. (e) Top-view SEM images of mesoporous rutile TiO2 rod array films supported on FTO substrates [28,70].

Fig. 6. Nanostructure evolution mechanism. SEM images of (a) K-titanate, (b) H-titanate, and (c) porous single-crystalline TiO2, respectively. (d) Schematic illustration of converting K-titanate to porous single-crystalline TiO2 via ion exchange followed by calcination. (e) Atomic crystal model of crystal structure changes during ion-exchange and calcination processes [80].

Fig. 7. (a) Porous Meso-TiO2 consists of orderly aligned anatase nanocrystals with dominant {001} facets, leading to high efficiency of charge separation under UV light irradiation. (b) Response voltages achieving a current of 0.5 nA, plotted against UV intensity. The inset shows typical current-voltage curves measured for Meso-TiO2-500 (red) and Nano-TiO2 (blue) at constant UV intensity (9.1 mW/cm2). (c) Mobility dependence on photoinduced charge density for MSC and nanoparticle films measured via transient mobility spectroscopy [28,35].

Fig. 8. (a) Schematic illustration of charge transfer and photocatalytic H2 production in reduced TiO2 mesocrystals (R-TMC). (b)Photocatalytic hydrogen evolution of TMC and R-TMC (loaded with 1 wt % Pt) as a function of time under the solar light irradiation [93].

Fig. 9. SEM images of solid rutile TiO2 single crystals exposing (a) more (110) facets than (111) facets, (b) equivalent (110) facets to (111) facets and (c) total (111) facets. SEM images of mesoporous rutile TiO2 single crystals exposing (d) more (110) facets than (111) facets, (e) equivalent (110) facets to (111) facets and (f) total (111) facets. (g) Comparison of photocatalytic hydrogen generation after 5 h UV-vis irradiation over mesoporous and solid rutile TiO2 single crystals with different percentages of exposed {111} facets loaded with 1 wt% Pt in the presence of methanol as electron donor [70,76].

Fig. 10. (a) Schematic illustration of the growth of TiO2 mesocrystals on a g-C3N4 NS. (b) Photodegradation of MO (c) Photoreduction of Cr6+ over DTMCs, g-C3N4 NSs, 33.3 % g-C3N 4/DTMCs, and the corresponding mechanical mixture. (d) Proposed photocatalytic mechanism for photoinduced charge-carrier transfer within the DTMC/g-C3N4 NS heterostructure [112].

Fig. 11. (a) Preparation scheme for Au NRs/TMC. (b) UV-visible diffuse reflectance spectra of TMC and Au NRs/TMC with different aspect ratios. (c) Time courses of H2 production from water in the presence of methanol (20 vol%) using TMC, different Au NRs/TMC, or Au NRs/P25 as a photocatalyst under visible-NIR light irradiation (λ > 420 nm, 200 mW/cm2). (d) Extinction spectrum and action spectrum of AQE for the photocatalytic H2 production using Au NRs/TMC-780 [125].

Fig. 12. (a) Schematic illustration of the composites photoanode composed of rutile TiO2 mesocrystalline and nanoparticles. (b) A schematic diagram of the bi-layer photoanode with MCs scattering layer on top of the nanocrystalline underlayer [126,127].

Fig. 13. Cross-sectional FESEM image of device based on M-TiO2 (left) and P25 (right) ETM (scale bar 2 mm) [143].

Table 1 Summary of performance based on metal oxide MCs and MSCs.

Photoanode (DSSCs)	η (%)	Voc (V)	Js (mA/cm²)	FF	Ref.
Composite electrode with rutile TiO₂ MCs and P25 particles	7.3	0.68	15.21	0.7	[126]
Ellipsoidal TiO₂ MCs (scattering layer)	7.16	0.689	15	0.69	[127]
Spherical TiO₂ MCs (scattering layer)	8.10	0.748	16.6	0.652	[128]
TiO₂ MCs with 100 % exposed (101) facets (scattering layer)	7.23	0.73	14.35	0.69	[130]
Mesoporous TiO₂ microspheres with single-crystal-like anatase walls	12.1	0.75	22.91	0.71	[129]
TiO2 MCs with exposed (111) facets (scattering layer)	9.6	0.76	19.07	0.6621	[131]
Mesocrystalline TiO₂ nanosheet arrays with exposed (001) facets	8.85	0.826	16.86	0.634	[64]
Oliver-shaped mesoporous TiO₂ MCs	11.6	0.713	21.8	0.748	[135]
Oliver-shaped TiO₂ MSCs	11.3	0.727	21.4	0.731	[135]
Anatase TiO₂ MSCs with (001) and (101) facets	3.11	0.76	6.47	0.63	[28]
MSC TiO₂ Polyhedron-Constructed Core-Shell Microspheres	6.6	0.7	14.9	0.62	[137]
Ellipsoidal TiO₂ MSCs with polyhedral pores	8.3	0.855	14.5	0.67	[84]
In situ grown MSC TiO₂ nanosheets	5.83	0.704	12.86	0.64	[138]
MSC ZnO platelets with smaller size	5.63	0.774	12.42	0.59	[139]
Photoanode (PSCs)
Anatase TiO₂ MSCs with (001) and (101) facets	7.29	0.79	0.79	0.7	[28]
SnO₂ MSCs	3.76	0.546	0.546	0.633	[142]
SnO₂ MSCs coated with TiO₂	8.54	0.802	0.802	0.621	[142]
Anatase TiO₂ MSCs	12.96±0.26	0.859±0.011	0.859±0.011	0.66±0.01	[143]

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