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At least 19 records

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NASA NTRS1986

Effect of counterions on the formation of ohmic contact between p-Si and poly(pyrrole) film - An ac impedance analysis

Conditions under which poly(pyrrole) (PP) films form ohmic contact with single-crystal p-Si are described. Counterions affect both the conductivity and flatband potential, V(FB), values of poly(pyrrole). While paratoluene-sulfonate-doped PP acts like a switch, the impedance behavior of PP films doped with ClO4(-), BF4(-), or PF6(-) allows evaluation of the V(FB) of these films. The formation of 'quasi-ohmic' and 'nonohmic' contacts, respectively, of PP (ClO4) and PP films doped with other counterions, with p-Si, are explained in terms of conductivity of these films and V(FB) of PP films with respect to that of p-Si. PP film seems to passivate or block intrinsic surface states present on p-Si surface.

Nagsubramanian, G.↗

DOE OSTI2025

In Situ Characterization of Surface Recombination in p-Si/SiO x Based Photoelectrochemical Cells

Time-resolved infrared (TRIR) and electrochemical impedance spectroscopy (EIS) were utilized to quantify surface states present at silicon oxide (SiO x ) protected crystalline p-Si electrolyte interfaces. The primary goal was to identify p-Si/SiO x photoelectrodes with both low surface recombination rates and efficient multi-electron transfer to an acceptor present in the external electrolyte. Three SiO x layers were investigated: native oxide (nOx), chemical oxide (cOx), and rapid thermal annealed (RTA) thermal oxide (tOx). Comparative study with [Ru(bpy) 3 ](PF 6 ) 2 as the electron acceptor indicated that tOx was most optimal with a small effective recombination rate, multi-electron transfer capability, and photovoltage of 500 ± 50 mV. A secondary goal was to analyze the surface recombination rates with the Shockley–Read–Hall (SRH) kinetic model. Two surface states were identified from this analysis, one closer to the CB edge (V t,1 ) and the other near the midgap (V t,2 ). EIS and SRH analyses revealed that a forming gas (5% H 2 /N 2 ) anneal (FGA) decreased surface recombination for tOx and nOx through a lower density of surface states. In the case of tOx, the infrared data indicated that V t,2 was completely removed. Here, the energetic positions of the band edges were correlated with the surface state density; low densities corresponded to more favorable potentials for inversion layer formation, which is expected to be most optimal for photocatalysis. Collectively this study indicates that the free carrier dynamics provided by TRIR represent a powerful in situ probe of the band edge and the surface state energetics in silicon based photoelectrochemical cells.

Electrochemical Impedance Spectroscopy↗

DOE OSTI2023

Multi-Electron Transfer at H-Terminated p-Si Electrolyte Interfaces: Large Photovoltages under Inversion Conditions

Here, photovoltages for hydrogen terminated p-Si(111) in an acetonitrile electrolyte were quantified with methyl viologen [1,1'-(CH 3 ) 2 -4,4'-bipyridinium](PF 6 ) 2 , abbreviated MV 2+ , and [Ru(bpy) 3 ](PF 6 ) 2 , where bpy is 2,2'-bipyridine, that respectively undergo two and three one-electron transfer reductions. The reduction potentials, E°, of the two MV 2+ reductions occurred at energies within the forbidden bandgap, while the three [Ru(bpy) 3 ] 2+ reductions occurred within the continuum of conduction band states. Bandgap illumination resulted in reduction that were more positive than that measured with a degenerately doped n + -Si demonstrative of a photovoltage, Vph, that increased in the order: MV 2+/+ (260 mV) < MV +/0 (400 mV) < Ru 2+/+ (530 mV) ~ Ru +/0 (540 mV) ~ Ru 0/– (550 mV). Pulsed 532 nm excitation generated electron-hole pairs whose dynamics were nearly constant under depletion conditions and increased markedly as the potential was raised or lowered. A long wavelength absorption feature assigned to conduction band electrons provided additional evidence for the presence of an inversion layer. Collectively, the data reveal that the most optimal photovoltage, as well at the longest electron-hole pair lifetime and the highest surface electron concentration, occur when E° lies energetically within the unfilled conduction band states where an inversion layer is present. The bell-shaped dependence for electron-hole pair recombination with the surface potential was predicted by the time-honored SRH model providing a clear indication that this interface provides access to all four bias conditions, i.e., accumulation, flat band, depletion, and inversion. The implications of these findings for photocatalysis applications and solar energy conversion are discussed.

14 SOLAR ENERGY↗

NASA NTRS1988

Electrochemical evaluation of the p-Si/conducting polymer interfacial properties

Results are presented from an experimental investigation of the contact resistance and interfacial properties of a p-Si/conducting polymer interface for solar cell applications. The electronic character of the polymer/semiconductor function is determined by studying the electrochemical behavior of both poly(isothianapthene) (PITN) and polypyrrole (PP) in an acetonitrile solution on p-silicon electrodes. The results obtained indicate that while PITN is intrinsically more conductive than PP, neither passivates surface states nor forms ohmic contact.

Nagasubramanian, G.↗

DOE OSTI2023

TaO x electron transport layers for CO 2 reduction Si photocathodes

Electron transport layers (ETLs) used as components of photocathodes for light-driven CO 2 reduction (CO 2 R) in aqueous media should have good electronic transport, be stable under CO 2 R conditions, and, ideally, be catalytically inert for the competing hydrogen evolution reaction (HER). Here, using planar p-Si (100) as the absorbing material, we show that TaO x satisfies all three of the above criteria. TaO x films were synthesized by both pulsed laser deposition (PLD) and radio-frequency (RF) sputtering. In both cases, careful control of the oxygen partial pressure during growth was required to produce ETLs with acceptable electron conductivity. p-Si/TaO x photocathodes were interfaced with ca. 10 nm of a CO 2 R catalyst: Cu or Au. Under front illumination with simulated AM 1.5G in CO 2 -saturated bicarbonate buffer, we observed, for both metals, faradaic efficiencies for CO 2 R products of ~50% and ~30% for PLD TaO x and RF sputtered TaO x , respectively, at photocurrent densities up to 8 mA cm -2 . p-Si/TiO 2 /Cu photocathodes were also evaluated but produced mostly H 2 (>97%) due to reduction of the TiO 2 to Ti metal under CO 2 R conditions. In contrast, a dual ETL photocathode (p-Si/TiO 2 /TaO x /Cu) was selective for CO 2 R, which suggests a strategy for separately optimizing selective charge collection and the stability of the ETL/water interface. The maximum photovoltage obtained with p-Si/TaO x /Cu devices was 300 mV which was increased to 430–460 mV by employing ion implantation to make pn + -Si/TaO x /Cu structures. Photocathodes with RF sputtered TaO x ETLs are stable for CO 2 R for at least 300 min. In conclusion, techno-economic analysis shows that the reported system, if scaled, could allow for an economically viable production of feedstocks for chemical synthesis under the adoption of specific CO 2 credit schemes, thus becoming a significant component of carbon-neutral manufacturing.

36 MATERIALS SCIENCE↗

NASA NTRS1985

Determination of the Si-conducting polymer interfacial properties using A-C impedance techniques

A study was made of the interfacial properties of poly(pyrrole) (PP) deposited electrochemically onto single crystal p-Si surfaces. The interfacial properties are dependent upon the counterions. The formation of 'quasi-ohmic' and 'nonohmic' contacts, respectively, of PP(ClO4) and PP films doped with other counterions (BF4 and para-toluene sulfonate) with p-Si, are explained in terms of the conductivity of these films and the flat band potential, V(fb), of PP relative to that of p-Si. The PP film seems to passivate or block intrinsic surface states present on the p-Si surface. The differences in the impedance behavior of para-toluene sulfonate doped and ClO4 doped PP are compared.

Nagasubramanian, G.↗

DOE OSTI2022

Failure analysis and design principles of silicon-based lithium-ion batteries using micron-sized porous silicon/carbon composite

Significant progresses have been made to overcome the fundamental challenges in silicon (Si)-based lithium-ion batteries (LIBs). However, much less work have been reported on the design and failure analysis these batteries for practical applications. In this work, we analyzed various cell design parameters affecting the performance of pouch cells using micron-sized porous Si with nano-pore structure and coated by pitch-carbon (p-Si/C). The correlation among particle level, electrode level, and cell level properties, especially the effect of electrode density on the volumetric capacity density of Si anode and full batteries have been systematically investigated. It is found that the corrosion of p-Si/C particle surface is the main failure mechanisms on the eventual capacity loss, while Li plating on anode electrode surface is the main reason for the fast capacity loss in later stage of cycling. The volumetric capacity of Si anode highly depends on both electrode density and the Si content. Moreover, the prelithiation of Si anodes is found to increase energy density while decreasing cycle life of Si-based full cells. Finally, the pathways and strategies for adoption of micron-sized p-Si/C anodes in LIBs have been proposed for their practical applications.

25 ENERGY STORAGE↗

DOE OSTI2025

High performance porous Si anode enabled by an organic-solvent assisted etching process

Silicon (Si) is a promising anode for the next generation of lithium-ion batteries, but its large volume changes (~300 %) during cycling hindered its practical applications. One method to improve its stability is to etch micron sized Si/SiO 2 particles to form porous Si (p-Si) and accommodate volume changes internally. However, the conventional HF etching method generates excess gas/heat and is difficult to scale up. Herein, we developed an organic-solvent-assisted HF etching process (O-HF) using a mixture of benzene and saturated HF aqueous solution. The organic solvent can be preferentially absorbed on the surface of Si/SiO 2 powder so etching rate of SiO 2 can be controlled to avoid rapid gas/heat generation. This method can also prevent over-etching of Si by minimizing direct contact/react between water and newly exposed Si. Si||NMC622 cells using carbon coated p-Si particles prepared by optimized O-HF etching process demonstrate a capacity retention of 82.0 % after 500 cycles, which is much better than those prepared by conventional HF etching (73.7 %). The thickness of Si anode increases only ~10 % during the initial lithiation, which is comparable with those of graphite anode. In conclusion, the O-HF etching strategy developed in this work can also be applied to the etching of a broad range of materials.

HF etching↗

DOE OSTI2025

Tetracene Functionalized Si(111) Achieves Enhanced Solar-to-Chemical Energy Conversion via Molecular Acceptor States

The properties of semiconductor|liquid interfaces play a critical role in determining the efficiency of solar-to-hydrogen (STH) conversion. Here, we investigate how molecular functionalization of Si(111) and Si(111)|TiO 2 surfaces impacts photoelectrochemical (PEC) hydrogen production efficiency. We find that functionalization of ∼3% of the atop sites of Si(111) with either 9-anthracene (Anth) or 5-tetracene (Tet), with the remaining sites passivated by methyl groups, provides substrates with high electronic quality and low surface oxide densities, as determined by X-ray photoelectron spectroscopy (XPS) measurements. Surface photovoltage (SPV) spectroscopy shows that surfaces modified with Anth or Tet exhibit an increased photovoltage, with Tet-functionalized surfaces yielding an additional 192 meV relative to methyl-terminated Si(111), indicating improved charge separation for Si-Tet. Further improvement in onset potential was achieved by replacing a nitrogen-containing TiO 2 atomic layer deposition (ALD) precursor (TDMAT) with a precursor lacking nitrogen (TTIP), which eliminates the parasitic defect band in the TiO 2 overlayer (p-Si(111)-Tet|TTIP-TiO 2 |Pt: V OC = +0.283 ± 0.041 V vs RHE). Density functional theory (DFT) analysis demonstrates that compared with Anth-modified Si(111), the Tet-modified surface exhibits more hybridized Si(111)-Tet states closer to the silicon band edges. Mercury contact current–voltage (I–V, dark) measurements quantified the relative interfacial density of states of Si-Tet, Si-Anth and Si-Me surfaces─revealing that the interfacial state density was highest for Si-Tet. This suggests that such hybridized interfaces serve to capture better photoexcited charge, which enables facile electron transfer to molecular acceptors in solution. Altogether, the data indicate that beneficial hybrid molecular LUMO surface states interacting with the Si conduction band edge results in improved hydrogen evolution (HER) performance for p-Si devices.

Group theory↗

DOE OSTI2025

Photosynthesis of CO from CO 2 with an iron polypyridyl catalyst at a passivated silicon photoelectrode

A first-row transition metal catalyst, [Fe(tpy)(Mebim-py)(NCCH 3 )] 2+ (tpy = 2,2′:6′,2′′-terpyridine, Mebim-py = 1-methylbenzimidazol-2-ylidene-3-(2′-pyridine)) mediates CO 2 reduction to CO at passivated p-Si photoelectrodes with applied potentials 240 mV positive of the standard CO 2 /CO reduction potential. The molecular catalyst's selectivity for CO was retained under photoelectrochemical conditions, with negligible direct proton reduction promoted by the photoelectrode. The faradaic efficiency for CO (44 ± 6%) was slightly enhanced relative to the catalyst performance in the dark (33%). A photosynthetic cell based on this photocathode system, coupled with ferrocene oxidation at the anode, successfully operated at a cell voltage of −1.2 V. The photovoltage generated by illumination of p-Si–CH 3 met and surpassed the potential required for CO 2 reduction when coupled with ferrocene oxidation. By leveraging a low-overpotential CO 2 reduction electrocatalyst, a photo-assisted electrochemical efficiency of 0.15% and applied bias photon-to-current efficiency of 0.05% was achieved for this single-junction cell, ultimately storing 46 kJ mol −1 (11 kcal mol −1 ) of photon energy.

Carbon Dioxide Reduction↗

DOE OSTI2025

Mild-Annealed Molecular Layer Deposition (MLD) Tincone Thin Film as Photoelectrochemically Stable and Efficient Electron Transport Layer for Si Photocathodes

Metalcone thin films, composed of inorganic–organic hybrids, are synthesized using molecular layer deposition (MLD) through reactions between organometallic precursors (e.g., Sn, Al, and Ti) and organic reactants (e.g., ethylene glycol and glycerol). Despite their unique properties, metalcones exhibit significant vulnerability to water due to their organic components, limiting their potential in electrochemical applications. This study focuses on enhancing the photoelectrochemical stability of tincone thin films in aqueous electrolyte while preserving their hybrid characteristics through mild annealing in air at 250 °C. As-deposited and vacuum-annealed tincone thin films exhibited significant degradation under these conditions, while high-temperature-annealed (500 °C) tincone thin films offered improved stability with a significant decline in charge transfer efficiency. In contrast, mild annealing in air maintained the C–O bond at half level and improved the stability and charge transport without compromising the unique characteristics of tincone. This was confirmed by ellipsometry, X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR). Mild-annealed tincone deposited on a lightly doped p-type silicon (p-Si) photocathode produced a 20-fold increase in CO volume compared to high-temperature annealed tincone in a CO 2 -saturated potassium bicarbonate (KHCO 3 ) electrolyte with dispersed graphene oxide–cobalt phthalocyanine (GO-CoPc) under 1 sun illumination at 0.9 V vs reversible hydrogen electrode (RHE), while maintaining the faradaic efficiency for CO and H 2 . These results suggest that mild-annealed tincone thin films hold significant potential as protective charge transport layers on silicon photocathodes for the aqueous CO 2 reduction reaction (CO 2 RR).

Annealing (metallurgy)↗

DOE OSTI2022

Surface Immobilization of a Re(I) Tricarbonyl Phenanthroline Complex to Si(111) through Sonochemical Hydrosilylation

A sonochemical-based hydrosilylation method was employed to covalently attach a rhenium tricarbonyl phenanthroline complex to silicon(111). fac-Re(5-(p-Styrene)-phen)(CO) 3 Cl (5-(p-styrene)-phen = 5-(4-vinylphenyl)-1,10-phenanthroline) was reacted with hydrogen-terminated silicon(111) in an ultrasonic bath to generate a hybrid photoelectrode. Subsequent reaction with 1-hexene enabled functionalization of remaining atop Si sites. Attenuated total reflectance–Fourier transform infrared spectroscopy confirms attachment of the organometallic complex to silicon without degradation of the organometallic core, supporting hydrosilylation as a strategy for installing coordination complexes that retain their molecular integrity. Detection of Re(I) and nitrogen by X-ray photoelectron spectroscopy (XPS) further support immobilization of fac-Re(5-(p-styrene)-phen)(CO) 3 Cl. Cyclic voltammetry and electrochemical impedance spectroscopy under white light illumination indicate that fac-Re(5-(p-styrene)-phen)(CO) 3 Cl undergoes two electron reductions. Mott–Schottky analysis indicates that the flat band potential is 239 mV more positive for p-Si(111) co-functionalized with both fac-Re(5-(p-styrene)-phen)(CO) 3 Cl and 1-hexene than when functionalized with 1-hexene alone. XPS, ultraviolet photoelectron spectroscopy, and Mott–Schottky analysis show that functionalization with fac-Re(5-(p-styrene)-phen)(CO) 3 Cl and 1-hexene introduces a negative interfacial dipole, facilitating reductive photoelectrochemistry.

X-ray photoelectron spectroscopy↗

DOE OSTI2024

When Photoelectrons Meet Gas Molecules: Determining the Role of Inelastic Scattering in Ambient Pressure X-ray Photoelectron Spectroscopy

Inelastic photoelectron scattering (IPES) by gas molecules, a critical phenomenon observed in ambient pressure X-ray photoelectron spectroscopy (APXPS), complicates spectral interpretation due to kinetic energy loss in the primary spectrum and the appearance of additional features at higher binding energies. In this study, we systematically investigate IPES in various gas environments using APXPS, providing detailed insights into interactions between photoelectrons emitted from solid surfaces and surrounding gas molecules. Corelevel XPS spectra of Au, Ag, Zn, and Cu metals were recorded over a wide kinetic energy range in the presence of CO 2 , N 2 , Ar, and H 2 gases, demonstrating the universal nature of IPES across different systems. Additionally, we analyzed spectra of scattering effects induced by gas-phase interactions without metal solids. In two reported CO 2 -reduction systems (p-GaN/ Au/Cu and p-Si/TaO x /Cu), we elucidated that IPES is independent of the composition, structure, or size of the solid materials. Using metal foil platforms, we further developed an analytical model to extract electron excitation cross sections of gas molecules. These findings enhance our understanding of IPES mechanisms and enable the predictions of IPES structures in other solid–gas systems, providing a valuable reference for future APXPS studies and improving the accuracy of spectral analysis in gas-rich catalytic interfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Methyl Termination of p-Type Silicon Enables Selective Photoelectrochemical CO 2 Reduction by a Molecular Ruthenium Catalyst

Methyl-terminated p-type silicon photoelectrodes selectively drive CO 2 reduction by a homogeneous [Ru(tpy)(Mebim-py)(NCCH 3 )] 2+ catalyst (tpy = 2,2′:6′,2″-terpyridine, Mebim-py = 1-methylbenzimidazol-2-ylidene-3-(2′-pyridine)). A 460 mV photovoltage is quantified for the photoelectrode. Under 1 sun illumination, this system achieves a Faradaic efficiency of 87% for CO at −1.7 V vs Fc +/0 , matching reports of the same catalyst at metallic electrodes operating at −2.1 V. When 5% water is introduced, the CH 3 -terminated Si photoelectrode remains stable, selectivity for CO is retained, and current density increases. Methyl termination suppresses the competitive hydrogen evolution observed for H-terminated Si photoelectrodes, which under the same conditions produce ca. 60% CO and 8% H 2 and have unstable performance. Furthermore, these results establish that a semiconductor photoelectrode can power a molecular CO 2 reduction catalyst without hydrogen evolution by the photoelectrode itself. Methyl termination of p-Si allows CO 2 reduction to kinetically outcompete proton reduction, revealing an important design principle for selective fuel formation.

Catalysts↗

DOE OSTI2025

Photoelectrochemical Hydride Generation with Oxide-Coated Silicon

Photoelectrochemical generation of a potent organic hydride donor at silicon is demonstrated. Two different oxide-coated p-type silicon photoelectrodes reduced 1,2,3,5,6-pentamethyl-1H-benzo[d]imidazol-3-ium hexafluorophosphate, [PMBI][PF 6 ], to its corresponding imidazole hydride, PMBIH, in the presence of a proton source. Under 1 sun illumination, in acetonitrile with 1,5-diazabicyclo[4.3.0]non-5-ene (DBN) buffer, the p-Si photoelectrodes convert PMBI + to PMBIH with good Faradaic efficiencies (FEs): 78% FE at −2.3 V vs Fc +/0 for Si|TiO 2 and 83% FE at −2.6 V vs Fc +/0 for Si|SiO 2 (where Si|SiO 2 represents silicon coated with an oxide layer). Generally, the Si|TiO 2 catalyzed the reaction at milder potentials than Si|SiO 2 , but the Si|SiO 2 had better selectivity for PMBIH generation over H 2 evolution than Si|TiO 2 . In light of prior studies of these photoelectrodes, the differences in selectivity and onset potential suggest a difference in mechanism, likely an outer-sphere electron transfer (ET) mechanism at the SiO 2 surface and potentially a proton-coupled ET process at the TiO 2 surface. To help understand reaction efficiency and identify areas of improvement, a thermochemical model for understanding net hydride transfer from the semiconductor to an acceptor in solution was developed. We find that the reactions in the present system are quite downhill. The high overpotentials (even while maintaining selectivity over H 2 evolution) emphasize the need for improved catalysts. Furthermore, this approach to evaluate the thermodynamics of net hydride transfer should be broadly valuable for electrochemical and photoelectrochemical processes.

14 SOLAR ENERGY↗

DOE OSTI2023

Exploiting Fixed Charge at Selective Contacts for Silicon Photovoltaics

The goal of this work was to examine and exploit fixed interface charges in ultra-thin (0-3 nm thickness) tunnel dielectric layers sandwiched between silicon and selective contact metal oxides (molybdenum oxide, MoO x , titanium oxide, TiO 2 ). Specifically, the interface fixed charge was varied by changing processing conditions and materials over a wide range and the effect on the current-voltage behavior and the Schottky barrier height was quantified. In budget period 1 (year 1), the objective was to grow aluminum oxide tunnel layers with quantified fixed charge over a range of ~1E12 to ~-2E12 cm -2 and combine these with MoO x and TiO 2 layers on Czochralsi (CZ) mono p- and n-Si, respectively. We sought conditions that maximize fixed charge and minimize Schottky barrier height to MoO x contacts to p-Si. This objective, along with investigating the effects of silicon surface terminations, occupied the majority of the project timeline (Q1-Q8) due to complications with high specific contact resistivity values. In the last two quarters of the project period, the objective was to insert HfO2 layers between Si and aluminum oxide layers to quench the fixed charge for layers with otherwise identical thermal history. Another objective was to lower the barrier height at TiO 2 -based contacts on n-type Si, but that was never investigated completely.

14 SOLAR ENERGY↗

NASA NTRS1987

Electrochemical studies of thin films of conducting polymers and conducting polymer composites deposited on metal and semiconductor electrodes

Electrochemical studies indicate that poly(Isothianaphthene) or PITN, can be p-doped only. Electrochemical properties of PITN and Nafion-PITN in acetonitrile solutions containing tetra-phenyl Phosphonium chloride as supporting electrolyte are compared. In both cases, the electrochemical behavior of thin films are different from that of thick films. In addition, Nafion does not seem to alter the electrochemical properties of PITN. Cyclic voltammetric and chronocoulometric measurements were made to compute the diffusion coefficient of the counter ions. Electrochemical behavior of both PITN and Nafion-PITN in acetonitrile solution containing different counter ions are described. PITN, when electrochemically deposited, apparently neither passivates surface states present nor forms ohmic contacts with p-Si or p(+)Si single-crystal electrodes.

Nagasubramanian, G.↗

NASA NTRS1990

Novel Si(1-x)Ge(x)/Si heterojunction internal photoemission long-wavelength infrared detectors

The feasibility of a novel p(+)-Si(1-x)Ge(x)-p-Si heterojunction internal photoemission (HIP) IR detector is demonstrated. A degenerately doped p(x)-Si(1-x)Ge(x) layer is required for strong IR absorption to generate photoexcited holes. The Si(1-x)Ge(x) layers are grown by molecular beam epitaxy, with boron concentrations up to 10 to the 20th/cu cm achieved by using an HBO2 source. Photoresponse at wavelengths ranging from 2 to 10 microns has been obtained with quantum efficiencies above 1 percent. The tailorable cutoff wavelength of the HIP detector has been demonstrated by varying the Ge composition ratio in the Si(1-x)Ge(x) layers.

Lin, T. L.↗