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This PDF file contains the front matter associated with SPIE Proceedings Volume 7770, including the Title Page, Copyright information, Table of Contents, Introduction, and the Conference Committee listing.
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Porous films of TiO2 and TiO2/WO3 were deposited onto transparent electrodes from aqueous suspensions with
polyethylene glycol, TiO2 particles and different amounts of tungistic acid. After annealing, crystalline samples were
obtained. The band gap energy, approximately 3.1 eV for TiO2, decreased from 2.9 to 2.7 eV for varying W/Ti molar
ratios from 3 to 12 %. The electrochemical properties were investigated in Na2SO4 aqueous solution; for the TiO2
electrode, the open circuit potential changed from 0.18 V in the dark to -0.25 V under irradiation from a solar simulator.
For hybrid TiO2/WO3 electrodes, the VOC values were almost independent of the WO3 content and corresponded to 0.3 V
in the dark and -0.1 V under irradiation; however, photocurrent and interfacial capacitance increased with a higher WO3
concentration. The electrodes were then used as photocatalysts for 17-α-etinylestradiol removal from water, and the
mixed TiO2/WO3 exhibited better performance for photocatalytic oxidation of estradiol than TiO2. Adding WO3
enhances the visible light harvesting and minimizes the charge recombination resulting in higher efficiency for solar
energy conversion.
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We employ x-ray photoelectron spectroscopy (XPS), reflection high-energy electron diffraction
(RHEED) and nuclear reaction analysis (NRA) to characterize the concentration-dependent
structural properties of nitrogen doping into rutile TiO2. High quality N-doped TiO2 were
prepared on rutile single crystal TiO2(110) substrates using plasma-assisted molecular beam
epitaxy with an electron cyclotron resonance (ECR) plasma and Ti effusive sources. Films with
N dopant concentrations at or below 2 at.% exhibited predominately substitutional doping based
on NRA data, whereas films with concentrations above this limit resulted in little or no
substitutional N and surfaces rich in Ti3+ . The binding energy of the N 1s feature in XPS did not
readily distinguish between these two extremes in N-doping, rendering features within 0.4 eV of
each other and similar peak profiles. Although widely used to characterize the state of N in
anion-doped TiO2 materials, we find that XPS is unsuitable for this task.
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Bandgap Engineering and Modeling of Semiconductors and SEI
ZnO1-xSex films have been prepared through pulsed laser deposition as a step toward stable films with a band gap
appropriate for water splitting. The films show a clear red shift in absorption with increasing Se content and a shift
in the flat band voltage toward spontaneity. Due to the films' electron affinities, there exists a natural tunnel
junction between these n- ZnO1-xSex films when grown on the p-side of a Si diode. The overall performance,
emphasized by flat band potential measurements, can be improved by growing films on Si p-n diodes.
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We perform extensive density-functional theory total-energy calculations and ab-initio molecular dynamics simulations
to evaluate the stability and reactivity of surface oxides and hydroxides of InP(001) for photoelectrochemical
water cleavage. In order to achieve maximal accuracy, our simulations include the full interface between
the semiconductor surface and liquid water. Certain oxide contaminants are found to have a dramatic impact
on the surface reactivity, pointing to the importance of surface oxide and hydroxide intermediates in facilitating
the water-dissociation component of the hydrogen evolution process. Our results are used to relate the chemical
activity of the surface towards water dissociation to the oxygen bond topology. The importance of the
liquid hydrogen-bond network near the interface is discussed, particularly in relation to the generation of local
configurations favorable for dissociative water adsorption on InP(001).
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Efficient photo-electrochemical (PEC) splitting of water to hydrogen usually requires photoelectrodes to have certain
electronic properties. Unfortunately, at present available semiconductors do not meet all these criteria. So, a thorough
understanding of band-engineering for mixed alloys is necessary to successfully design these photoelectrodes. Among
the semiconductors, transition metal oxides are of particular interest due to their low cost and relatively high stability in
aqueous media. Here, we will present a theoretical study of delafossite-alloys for PEC photo-electrodes. Previous studies
have indicated that the group IIIA delafossite family (CuMO2, M = Al, Ga, In) do not exhibit direct band gaps. Their
fundamental band gaps are significantly smaller than their reported optical band gaps. On the other hand group IIIB
delafossite family (CuMO2, M = Sc, Y, La) in general show direct band gaps and, except for CuLaO2, band gaps are
above 3.00 eV. However, both of these two families exhibit p-type conductivity. We will show that by appropriate
alloying of these two delafossite-families we can tune their band gaps and other opto-electronic properties. These types
of alloying are desirable, as these introduce no localized impurity states in the band gap due to isovalent alloying. Also,
the electronic effective masses can be lowered by selective doping of main group elements. Finally, it will be discussed
that, lowering the symmetry constraints of these alloys would enhance their optical absorption properties. We'll also
discuss that alloying with other 3d metal elements may decrease the band gap, but would increase the effective masses of
the photo-electrons.
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Hematite is a promising material for solar energy conversion via photo-electrochemical water splitting. However, the
precise control of substitutional doping and nanometer feature size is important for high photon harvesting efficiency.
Doped and nanostructured hematite electrodes can be prepared by a simple solution-based colloidal approach however, a
high temperature (800°C) annealing is required to activate the dopant atoms. This high temperature annealing step also
increases the particle size above the dimension necessary for high photon harvesting efficiencies. Here we investigate a
strategy to control the two kinetic processes occurring during sintering (particle size increase and dopant
diffusion/activation) by incorporating Ti dopant directly into the colloid solution and reducing the annealing time. We
find that this strategy leads to porous, high-surface area hematite electrodes giving a solar photocurrent density of 1.1
mA cm-2 at 1.23 V vs. the reversible hydrogen electrode (RHE) under standard testing conditions where only 0.56 mA
cm-2 was observed at 1.23 V vs. RHE with our previous work. In addition, scanning electron micrographs examining the
morphology of the electrodes suggests that our kinetic strategy is indeed effective and that further optimization may
result in higher photocurrents.
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As many water splitting photocatalysts only evolve hydrogen under irradiation due to complications with high energy water oxidation steps, a three component nano-catalyst was designed by combining sites for water reduction and oxidation with solar-charge-supplying semiconductor. The semiconductor framework was derived from K4Nb6O17, a known UV-light photocatalyst with a band gap of 3.5 eV. Following ion exchange and exfoliation with terabutyalammonium hydroxide, the layered material separates into nanosheets that coil into 1 ± 0.5 um long and 10 ± 5 nm wide nanoscrolls to redue surface energy. PT (reduction sites) and IrOx (oxidation sites) were photochecmically deposited on the surface of the nanoscrolls to produce two-and three-component nanostructures. Upon irradiation with UV-light, H2 was evolved from aqueous methanol and pure water, substoichiometric O2 from aqueous AgNo3. The band structures of each catalyst and reason for lack of O2 evolution from pure water was evaluated with cyclic voltammetry and photoelectrochemistry.
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We synthesized molybdenum disulfide (MoS2) nanostructures and investigated their electrochemical activity for driving
the hydrogen evolution activity as well as their photoelectrochemical activity for the water splitting reaction. MoS2
nanoparticles were made using a reverse micelle encapsulation method and exhibit quantum confinement of the indirect
band gap up to 1.8 eV. A MoS2 double-gyroid bi-continuous structure was made using an evaporation induced self
assembly method. Both nanostructures exhibit improved activity for the hydrogen evolution reaction versus bulk MoS2.
Photoelectrochemical activity was also observed in both nanostructures.
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This paper summarises some recent results of applying in-situ EPR spectroscopy at low temperature to observe directly
the creation and trapping of conduction band electrons in rutile, and indirectly in hematite thin films via observation of a
photo-induced superparamagnetic resonance signal.
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There is increasing interest in photochemical schemes for converting CO2 into a useful product as a means of mitigating
atmospheric levels of this gas. Although photoelectrochemical schemes have been considered for this application,
typically very high overpotentials are observed, and thus, semiconductor-electrolyte interfaces have not been observed to
actually convert light energy to chemical energy in the aqueous CO2 redox system. We report here on a catalytic system
that efficiently converts CO2 to methanol and other alcohols. The system couples a III-V p-type semiconductor electrode
with a pyridinium catalyst. The conversion of CO2 to alcohols can be driven solely with light to yield faradaic
efficiencies approaching 100% at potentials well below the thermodynamic potential. Mechanistic studies on the
formation of methanol indicate that the observed six-electron reduction occurs via a series of one electron reductions
mediated by pyridinium.
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The properties of thin film InVO4 photoanodes for water splitting have been studied. Compact films of InVO4 were
prepared by spray pyrolysis and are found to be stable between pH 3 - 11. Although the indirect bandgap is 3.2 eV, a
modest amount of visible light absorption is observed. The origin of this absorption is attributed to the presence of deep
donor states at ~0.7 eV below the conduction band. Shallow donors are absent in this material, in contrast to what is
normally observed for metal oxides. The deep donor model explains the much stronger visible light absorption of
powders compared to thin films, and is supported by photoluminescence data. The origin of the deep donors is attributed
to deviations in the In:V ratio, and the corresponding defect-chemical reactions will be discussed.
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For more than a decade, the Hawaii Natural Energy Institute has conducted research on photoelectrochemical (PEC)
technologies and achieved major milestones, including the fabrication of high-performance photoactive thin film
materials and the development of innovative device integrations (hybrid-photo-electrode). In this paper, we focus our
discussion on tungsten oxide-based materials, one of our two principal topics of research in this field. After a description
of pure WO3 physical, chemical and energetic properties we present our latest results on tungsten oxide PEC properties
improvement. In our general approach, each component of the PEC electrode is addressed, from the absorber (bulk) to
the surface energetics (near-surface) and catalysis (surface). Recently, progresses have been made on surface treatment
for catalytic purposes as well as on PEC materials integration. In the case of catalytic treatment, our studies show that
reactive sputtering technique is suitable to form high quality RuO2 thin films and nanoparticles. Tests conducted on
RuO2 thin films pointed out an oxygen evolution reaction potential as low as 0.2 V. When used as an anode in 2-
electrode configuration, RuO2 thin films lead to a photocurrent onset potential reduction as low as 500 mV for p-type
PEC materials (CGSe2 and a-SiC, so far tested) when compared to platinum. In the case of RuO2 nanoparticles, a
photocurrent density increase of approx. 20% was observed on treated tungsten oxide films. Finally, we present a new
integration scheme to increase photocurrent density using highly textured substrates (HTS). In our approach, HTS were
obtained by anisotropic etching of [100] silicon substrates in KOH solution. Initial results indicated a very good
coverage of WO3 onto the silicon pyramids and a photocurrent doubling is observed when compared to WO3 deposited
on flat silicon substrates.
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Photoelectrochemical (PEC) water dissociation into hydrogen and oxygen at a semiconductor-liquid interface offers an
environmentally benign approach to hydrogen production. We have developed an integrated PEC device using
hydrogenated amorphous silicon carbide (a-SiC or a-SiC:H) material as photoelectrode in conjunction with an
amorphous silicon (a-Si) tandem photovoltaic device. Such a "hybrid PV/a-SiC" PEC cell produces photocurrent of
about 1.3 mA/cm2 in a short-circuit configuration and is durable in a pH2 electrolyte. On the other hand, the
aforementioned structure finished with ITO contacts and measured as a solid-state device features a current density of 5
mA/cm2, indicating a potential solar-to-hydrogen (STH) conversion efficiency of about 6% in the hybrid PV/a-SiC PEC
cell. The much lower photocurrent measured in the hybrid PEC cell suggests that there exists an interfacial barrier
between the a-SiC and electrolyte, which hinders the photocurrent extraction. In order to mitigate against the interfacial
barrier and hence improve the photo-generated charge carrier transport through the a-SiC/electrolyte interface, we have
explored several surface modification techniques, namely the use of metallic nano-particles (such as platinum or
palladium) and the growth of an additional thin layer (a-SiNx, carbon-rich a-SiC, a-SiF, etc.) on the top of a-SiC by
PECVD. In the latter case, it is observed that the addition of a thin PECVD-fabricated layer does not significantly
improve the photocurrent, presumably due to a poor band alignment at the a-SiC/electrolyte interface. The use of lower
work function nanoparticles like titanium has led to promising results in terms of photocurrent enhancement and an
a nodic shift in the onset potential.
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Metal oxides are promising for solar energy conversion applications since they are less expensive and easier to produce
than conventional single crystal silicon. In this paper we focused on CdSe and CdS quantum dot (QD) co-sensitized and
nitrogen doped TiO2 (N:TiO2) nanocomposite photoanodes for photoelectrochemical (PEC) water splitting for hydrogen
generation. PEC, UV-vis and scanning electron microscopy (SEM) characterizations of the nanostructured films were
carried out. The QD co-sensitized and N-doped TiO2 photoanodes exhibits increased photocurrent compared to cosensitized
TiO2 without N-doping This is tentatively attributed to enhanced hole transport by oxygen vacancy states that
are increased upon nitrogen doping. The enhanced hole transport facilitates overall charge transfer and transport and
thereby results in improved photocurrent.
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Conversion of solar energy into hydrogen is one of the most promising renewable energy technologies. Photocatalytic
production of hydrogen from water, H2S and organic wastes using semiconductors is one of the potential strategies for
converting the sunlight energy into chemical energy. Korea government paid great attention to the hydrogen economy
and launched the HERC (Hydrogen Energy R&D Center) for supporting the R&D topics on hydrogen related
technologies. The key issue for realizing the commercial application of solar water splitting hydrogen production
technique is to find an efficient, stable and low-cost photocatalyst. Our research groups have continuously investigated
to find oxide and composite photocatalysts for photoelectrochemical cell with high efficiency using computational
design and synthesis method. But, fundamental research on semiconductor doping for band gap shifting and surface
chemistry modification is still required. Various reaction media containing sacrificial agents should be developed to
match with high activity photocatalysts to further improve the system efficiency. Water containing organic/inorganic
waste and sea water are particularly suggested in the consideration that all these water sources are the most available
water on the earth to the final commercial application of photocatalytic water splitting technique.
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The work presents the photo-catalytic reactions of ethanol over Au particles deposited on
TiO2 anatase nano- (≤ 10 nm) and micro- (ca. 0.15 μm) particle catalysts. The Au particles
are of uniform and similar dimension (mean particle size = ca. 5 nm and 7 nm on the microand
nano-sized TiO2, respectively). XPS Au4f indicated that in both cases Au particles are
present in their metallic state with no evidence of charge transfer to (or from) the
semiconductor. Liquid slurry photoreaction indicated the production of hydrogen with a rate
≈ 2 L/kgCatal.min on 2 wt. % Au/TiO2 anatase nano-particles under UV photo irradiation of
comparable intensity to solar radiation. While the reaction rate per unit mass was lower on
the micro-sized Au/TiO2 it simply scaled up to an equivalent rate for the nano-sized Au/TiO2
catalyst when normalised by unit area.
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Hetero-structured TiO2 and WO3 nanorod arrays have been fabricated by dynamic shadowing growth. The two-layer
WO3/TiO2 nanorod arrays grown by consecutive deposition of two materials at oblique angle are found to greatly
enhance the catalytic performance by the increased TiO2 surface area and the potential enhanced charge separation due
to the WO3-TiO2 interface. Also, two important factors have been found to affect the observed photocatalytic
enhancement: the crystal phase of each material, and the interfacial area between TiO2 and WO3. To further increasing
the interfacial area between the TiO2 and WO3, a dynamic shadowing growth method is used to create a quazi-core-shell
nanorod array. WO3 nanorods are first grown perpendicularly on a bare substrate to serve as the "core", and a TiO2
"shell" is then deposited. Such a core-shell structure maximizes the interfacial area between the two materials. The
photocatalytic decay rate for these core-shell samples again shows further improvement over single layer TiO2 thin films
and multi-layer c-TiO2/a-WO3 films by 13 and 3 times respectively. Our results demonstrate that heterostructured
WO3/TiO2 nanorod arrays are promising photocatalyst for water decontamination and water splitting for hydrogen
generation.
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There is an increasing interest in semiconductor/ electrolyte systems in connection with their application as
phototelectrolytic energy conversion devices (e.g. hydrogen evolution). There are several requirements in
order to produce hydrogen by photoelectrolysis using oxides metals and semiconductors. One of the most
interesting semiconductor materials is the GaN which is a direct ban gap semiconductor.
In this paper shows the formation of GaN prepared via electrodeposition, using ammonium nitrate at
different concentration as type sources of nitrogen in order to growth a thin film. A standard three-electrode
cell was used to prepare it using potenciostatic conditions. The average thickness of the samples was
measured. The annealed films were characterized by electrochemical; photoelectrochemical, compositional,
and morphologic methods in order to know its potential for water splitting.
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For the first time, TiO2 nanopowders were used as a modifier for the metal Al powders in the reaction with ordinary
tap water to generate hydrogen at ambient temperature. The present study systematically investigated the effect of
additives such as Al(OH)3, AlO(OH), α-Al2O3, γ-Al2O3, SiO2, CaO, Fe2O3, WO3, and four different TiO2 ceramic
powders on the promotion of hydrogen generation in the reaction of metal Al powders and tap water. Effect of
mechanical ball-mixing was also evaluated. It was found that AlO(OH), CaO, α-Al2O3and TiO2 (P90) powders were
very effective to facilitate the hydrogen production from the reaction of metal Al powders and tap water under
ambient condition. TiO2 (P90) nanopowders exhibited a slightly better effect than those of α-Al2O3in the facilitation
of hydrogen generation from water splitting. The generation of hydrogen from the reaction of modified Al powders
and water was found to be dependent on the sizes of metal Al powders, the modifiers, the size of the modifiers,
weight ratio of metal Al powders to the modifiers, and ball-milling durations. Further studies are required to fully
understand the contradictory behaviors to the previously known mechanism.
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The development of low cost, scalable, renewable energy technologies is one of today's most pressing scientific
challenges. We report on progress towards the development of a photoelectrochemical water-splitting system that will
use sunlight and water as the inputs to produce renewable hydrogen with oxygen as a by-product. This system is based
on the design principle of incorporating two separate, photosensitive inorganic semiconductor/liquid junctions to
collectively generate the 1.7-1.9 V at open circuit needed to support both the oxidation of H2O (or OH-) and the
reduction of H+ (or H2O). Si microwire arrays are a promising photocathode material because the high aspect-ratio
electrode architecture allows for the use of low cost, earth-abundant materials without sacrificing energy-conversion
efficiency, due to the orthogonalization of light absorption and charge-carrier collection. Additionally, the high surfacearea
design of the rod-based semiconductor array inherently lowers the flux of charge carriers over the rod array surface
relative to the projected geometric surface of the photoelectrode, thus lowering the photocurrent density at the
solid/liquid junction and thereby relaxing the demands on the activity (and cost) of any electrocatalysts. Arrays of Si
microwires grown using the Vapor Liquid Solid (VLS) mechanism have been shown to have desirable electronic light
absorption properties. We have demonstrated that these arrays can be coated with earth-abundant metallic catalysts and
used for photoelectrochemical production of hydrogen. This development is a step towards the demonstration of a
complete artificial photosynthetic system, composed of only inexpensive, earth-abundant materials, that is
simultaneously efficient, durable, and scalable.
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