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Herein, the synthesis of MoTe2 nanosheets by means of Atomic Layer Deposition (ALD) is demonstrated for the first time. ALD enables tight control over the thickness and the composition of the deposited material, which are highly appealing features for the nanostructure fabrication. The growth of ALD MoTe2 was studied on substrates of different nature, including TiO2 nanotube (TNT) layers used as active supporting material for fabricating hierarchical nanotubular MoTe2/TNT heterostructure. The combination of newly synthesized Te precursor with commercial Mo precursor rendered the growth of 2D flaky MoTe2 nanosheets mostly out-of-plane oriented. The as-deposited MoTe2 was extensively characterized by different techniques which confirmed its chemical composition and revealed 2D flaky nano-crystalline structures. In parallel, MoTe2/TNT layers were employed to explore and exploit both photoand electrocatalytic properties. The synergy stemming from the out-of-plane MoTe2 nanosheet orientation, with an optimized amount of catalytic active edges, and the fast electron transfer through 1D TiO2 nanotubes triggered the catalytic properties for both, organic pollutant degradation and hydrogen evolution reaction (HER) applications. Remarkably, the application of a cathodic potential originated a gradual HER electrochemical activation over time driving to a higher current density and an overpotential drop. (c) 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license ( http://creativecommons.org/licenses/by-nc-nd/4.0/ )

Herein, the synthesis of MoTe2 nanosheets by means of Atomic Layer Deposition (ALD) is demonstrated for the first time. ALD enables tight control over the thickness and the composition of the deposited material, which are highly appealing features for the nanostructure fabrication. The growth of ALD MoTe2 was studied on substrates of different nature, including TiO2 nanotube (TNT) layers used as active supporting material for fabricating hierarchical nanotubular MoTe2/TNT heterostructure. The combination of newly synthesized Te precursor with commercial Mo precursor rendered the growth of 2D flaky MoTe2 nanosheets mostly out-of-plane oriented. The as-deposited MoTe2 was extensively characterized by different techniques which confirmed its chemical composition and revealed 2D flaky nano-crystalline structures. In parallel, MoTe2/TNT layers were employed to explore and exploit both photoand electrocatalytic properties. The synergy stemming from the out-of-plane MoTe2 nanosheet orientation, with an optimized amount of catalytic active edges, and the fast electron transfer through 1D TiO2 nanotubes triggered the catalytic properties for both, organic pollutant degradation and hydrogen evolution reaction (HER) applications. Remarkably, the application of a cathodic potential originated a gradual HER electrochemical activation over time driving to a higher current density and an overpotential drop. (c) 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license ( http://creativecommons.org/licenses/by-nc-nd/4.0/ )

A reconstruction process of TiO2 nanotube (TNT) layers towards their superior photoelectrochemical performance and photocatalytic activity is presented. At first, TNT layers (similar to 5 mu m thick, similar to 250 nm in diameter) were prepared via electrochemical anodization to obtain double-wall (DW) TNT layers. Second, a selective chemical treatment was conducted to etch the inner wall, yielding single-wall (SW) TNT layers. Third, TNT layers were coated by an additional approx. 5.5 nm, 11 nm, and 16 nm thick TiO2 coatings, respectively, using Atomic Layer Deposition (ALD). A pronounced increase in the incident photon-to-electron conversion efficiency (reaching similar to 85% at lambda - 350 nm) was achieved on SW TNT layers coated with 11 nm thick ALD coatings compared to SW without coating (similar to 35% at lambda = 350 nm). This is due to the optimal thickness of the ALD TiO2 coating that passivates surface states and improves the separation of the photogenerated charge carriers. Photocatalytic performance of SW TNT layers with 11 nm thick ALD coatings (rate constant; k = 0.1156 min(-1)) was increased by approx. 10-times compared to that of the nowadays most reported blank DW TNT layers (rate constant; k = 0.0119 min(-1)).

This paper demonstrates, for the first time, synthesis of uniform and crystalline WO3 mesopomus fibers with a diameter of approximate to 1 mu m via centrifugal spinning. This was achieved by using a stable aqueous precursor solution based on ammonium metatungstate (AMT, (NH4)6H(2)W(12)O(40)center dot xH(2)O)) and polyvinyl pyrrolidone (PVP, (C6H9NO)(n)). Annealing at 300 degrees C for 1 h followed by an additional annealing at 500 degrees C for 6 h was conducted to obtain crystalline WO3 fibers. The resulting centrifugally spun WO3 fibers possess approx. 1.4-4 times enhancement in photocatalytic activity under UV (k = 0.0205 min(-1)) and VIS (k = 0.0109 min(-1)) light irradiation compared to that of electrospun WO3 fibers and commercially available WO3 nanoparticles. This is due to the increased specific surface area of the centrifugally spun WO3 fibers (S-BET = 22.3 m(2)/g) compared to electrospun WO3 fibers (S-BET = 7.4 m(2)/g) and WO3 nanoparticles (S-BET = 6.4 m(2)/g). On the other hand, optical properties of all tested materials (including optical band gap) were nearly the same.

Herein, the synthesis of MoTe2 nanosheets by means of Atomic Layer Deposition (ALD) is demonstrated for the first time. ALD enables tight control over the thickness and the composition of the deposited material, which are highly appealing features for the nanostructure fabrication. The growth of ALD MoTe2 was studied on substrates of different nature, including TiO2 nanotube (TNT) layers used as active supporting material for fabricating hierarchical nanotubular MoTe2/TNT heterostructure. The combination of newly synthesized Te precursor with commercial Mo precursor rendered the growth of 2D flaky MoTe2 nanosheets mostly out-of-plane oriented. The as-deposited MoTe2 was extensively characterized by different techniques which confirmed its chemical composition and revealed 2D flaky nano-crystalline structures. In parallel, MoTe2/TNT layers were employed to explore and exploit both photoand electrocatalytic properties. The synergy stemming from the out-of-plane MoTe2 nanosheet orientation, with an optimized amount of catalytic active edges, and the fast electron transfer through 1D TiO2 nanotubes triggered the catalytic properties for both, organic pollutant degradation and hydrogen evolution reaction (HER) applications. Remarkably, the application of a cathodic potential originated a gradual HER electrochemical activation over time driving to a higher current density and an overpotential drop. (c) 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license ( http://creativecommons.org/licenses/by-nc-nd/4.0/ )

Herein, the synthesis of MoTe2 nanosheets by means of Atomic Layer Deposition (ALD) is demonstrated for the first time. ALD enables tight control over the thickness and the composition of the deposited material, which are highly appealing features for the nanostructure fabrication. The growth of ALD MoTe2 was studied on substrates of different nature, including TiO2 nanotube (TNT) layers used as active supporting material for fabricating hierarchical nanotubular MoTe2/TNT heterostructure. The combination of newly synthesized Te precursor with commercial Mo precursor rendered the growth of 2D flaky MoTe2 nanosheets mostly out-of-plane oriented. The as-deposited MoTe2 was extensively characterized by different techniques which confirmed its chemical composition and revealed 2D flaky nano-crystalline structures. In parallel, MoTe2/TNT layers were employed to explore and exploit both photoand electrocatalytic properties. The synergy stemming from the out-of-plane MoTe2 nanosheet orientation, with an optimized amount of catalytic active edges, and the fast electron transfer through 1D TiO2 nanotubes triggered the catalytic properties for both, organic pollutant degradation and hydrogen evolution reaction (HER) applications. Remarkably, the application of a cathodic potential originated a gradual HER electrochemical activation over time driving to a higher current density and an overpotential drop. (c) 2021 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license ( http://creativecommons.org/licenses/by-nc-nd/4.0/ )

This paper demonstrates, for the first time, synthesis of uniform and crystalline WO3 mesopomus fibers with a diameter of approximate to 1 mu m via centrifugal spinning. This was achieved by using a stable aqueous precursor solution based on ammonium metatungstate (AMT, (NH4)6H(2)W(12)O(40)center dot xH(2)O)) and polyvinyl pyrrolidone (PVP, (C6H9NO)(n)). Annealing at 300 degrees C for 1 h followed by an additional annealing at 500 degrees C for 6 h was conducted to obtain crystalline WO3 fibers. The resulting centrifugally spun WO3 fibers possess approx. 1.4-4 times enhancement in photocatalytic activity under UV (k = 0.0205 min(-1)) and VIS (k = 0.0109 min(-1)) light irradiation compared to that of electrospun WO3 fibers and commercially available WO3 nanoparticles. This is due to the increased specific surface area of the centrifugally spun WO3 fibers (S-BET = 22.3 m(2)/g) compared to electrospun WO3 fibers (S-BET = 7.4 m(2)/g) and WO3 nanoparticles (S-BET = 6.4 m(2)/g). On the other hand, optical properties of all tested materials (including optical band gap) were nearly the same.

In this work, the anodization of Ti spheres using bipolar electrochemistry is reported for the first time. TiO2 nanotubes were found over the entire surface area of the Ti spheres when a square-wave potential was employed. The TiO2 nanotubes were similar to 77 nm in inner diameter and had a thickness of similar to 2 mu m on the extremities of the Ti spheres. Due to their increased surface area, the Ti spheres covered with TiO2 nanotubes had a rate constant for the photocatalytic degradation of methylene blue which was approximately 2.15 times higher than that of non-anodized Ti spheres with a thin thermal oxide layer.

In this work, the anodization of Ti spheres using bipolar electrochemistry is reported for the first time. TiO2 nanotubes were found over the entire surface area of the Ti spheres when a square-wave potential was employed. The TiO2 nanotubes were similar to 77 nm in inner diameter and had a thickness of similar to 2 mu m on the extremities of the Ti spheres. Due to their increased surface area, the Ti spheres covered with TiO2 nanotubes had a rate constant for the photocatalytic degradation of methylene blue which was approximately 2.15 times higher than that of non-anodized Ti spheres with a thin thermal oxide layer.

Ti films electrodeposited on Ni foils from molten salts were anodized towards TiO2 nanotube formation for the first time. The resulting TiO2 nanotube (TNT) layers were compared with TNT layers prepared under identical conditions on Ti foils by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) measurements, X-ray photoelectron spectroscopy (XPS), and photocurrent measurements. No significant differences were found between the TNT layers prepared on the two different substrates. Electrodeposited Ti films prepared in this way could thus be a viable option for anodization purposes.

TiO2 nanotube layers of different thicknesses and tube wall morphologies exploited. Single-wall nanotubes were obtained by chemical etching of double-wall ones. Photocurrents, structure, optical and electronic properties of tubes were compared.

TiO2 nanotube layers of different thicknesses and tube wall morphologies exploited. Single-wall nanotubes were obtained by chemical etching of double-wall ones. Photocurrents, structure, optical and electronic properties of tubes were compared.

Ti films electrodeposited on Ni foils from molten salts were anodized towards TiO2 nanotube formation for the first time. The resulting TiO2 nanotube (TNT) layers were compared with TNT layers prepared under identical conditions on Ti foils by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) measurements, X-ray photoelectron spectroscopy (XPS), and photocurrent measurements. No significant differences were found between the TNT layers prepared on the two different substrates. Electrodeposited Ti films prepared in this way could thus be a viable option for anodization purposes.

In this work, the anodization of Ti spheres using bipolar electrochemistry is reported for the first time. TiO2 nanotubes were found over the entire surface area of the Ti spheres when a square-wave potential was employed. The TiO2 nanotubes were ∼77 nm in inner diameter and had a thickness of ∼2 µm on the extremities of the Ti spheres. Due to their increased surface area, the Ti spheres covered with TiO2 nanotubes had a rate constant for the photocatalytic degradation of methylene blue which was approximately 2.15 times higher than that of non-anodized Ti spheres with a thin thermal oxide layer.

In this work, we present the influence of thermal annealing on morphological, structural, electrical, optical, and photoelectrochemical properties of double- (DW) and single-wall (SW) TiO2 nanotube (TNT) layers. High-aspect ratio TNT layers with a thickness of ~5 µm and ~20 µm with an average inner diameter of ~250 nm and ~130 nm, respectively, were prepared via electrochemical anodization of Ti foil in two different fluoride containing ethylene glycol-based electrolytes. The inner wall of the native DW TNT layers was quantitatively removed via a mild pre-annealing followed by a selective etching treatment in piranha solution, yielding SW TNT layers. The obtained SW TNT layers annealed at 300 – 500 °C possess enhanced conductivity by 1 – 2 orders compared to their DW counterparts. The photoelectrochemical properties of SW TNT layers are enhanced compared to their DW counterparts in the annealing temperature range 300 – 800 °C. In principle, the SW TNT layers could be potentially favored to the DW TNT layers in electrical and photoelectrochemical applications due to their more superior intrinsic properties.

Ti films, electrodeposited on Ni foils from molten salts, were anodized towards TiO2 nanotube formation for the first time. The resulting TiO2 nanotube (TNT) layers were compared with TNT layers prepared under identical conditions on Ti foils by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) measurements, X-ray photoelectron spectroscopy (XPS), and photocurrent measurements. No significant differences can be found for the TNT layers prepared on the two different substrates. As-electrodeposited Ti films could be a viable candidate for anodization purposes.

In this work, a two-step treatment of TiO2 nanotube (TNT) layers towards enhanced photocatalytic performance is presented. TNT layers with a thickness of ~7 µm and an average inner diameter of ~190 nm were prepared via electrochemical anodization of Ti foil in a fluoride containing ethylene glycol-based electrolyte. To improve the photocatalytic activity of the produced TNT layers a two-step post-treatment was conducted. First, the inner shell of the native double-wall TNT layers was removed via a mild pre-annealing followed by a selective etching treatment of the inner shell in piranha solution yielding single-wall TNT layers. Second, reduction via annealing in H2/Ar atmosphere was performed. The resulting Ti3+ doped single-wall TNT layers possess 100% enhancement of photocatalytic activity compared to their non-treated counterparts.

In this work, we show that sulfur treated 1D anodic TiO2 nanotube layers leads to improved photo-electrochemical and catalytic properties compared to the blank nanotube layers. This treatment was performed in the evacuated quartz ampoules in the temperature range from 250 to 450°C. Inspection of the sulfurized nanotube layers via scanning electron microscopy (SEM) and X-ray diffraction (XRD) has disclosed a gradual crystal growth within nanotube walls, represented by TiS2 or TiS3 phases. Optimally sulfurized TiO2 nanotube layers exhibit 3 times enhanced photocurrent in the UV spectral region, compared to the blank counterpart, with a shift of the light absorption up to the wavelength of 550 nm. In addition, the photocatalytic decomposition of a methylene blue aqueous solution using a wavelength of 365 nm is gradually improved with increasing sulfurization temperature. The highest photocatalytic decomposition rate is 2.3 times larger compared to the blank TiO2 nanotube layer. The application of sulfurized TiO2 nanotube layers for the electrocatalytic hydrogen evolution is also discussed.

In this work, the photoelectrochemical response of single-walled (SW) and double-walled (DW) TiO2 nanotube (TNT) layers is presented. TNT layers were grown on Ti substrates by anodization in two different ethylene glycol-based electrolytes to obtain ~5 and ~15 µm thick TNT layers. The inner shell of the TNT was quantitatively removed via a mild pre-annealing followed by a selective chemical etching treatment in piranha solution. All TNT layers were investigated for their photoelectrochemical response in the ultraviolet and near visible spectral range. Significantly enhanced photocurrent densities were revealed for the SW-TNT layers. This is ascribed to improved charge carrier separation along the tube walls due to the lack of the C- and F-rich inner shell removed by etching.