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DOE OSTI2013

Mechanical characterization of copper coated carbon nanotubes reinforced aluminum matrix composites

In this investigation, carbon nanotube (CNT) reinforced aluminum composites were prepared by the molecular-level mixing process using copper coated CNTs. The mixing of CNTs was accomplished by ultrasonic mixing and ball milling. Electroless Cu-coated CNTs were used to enhance the interfacial bonding between CNTs and aluminum. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in the composite samples compared with the uncoated CNTs. The samples were pressureless sintered under vacuum followed by hot rolling to promote the uniform microstructure and dispersion of CNTs. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. As compared to the pure Al, for 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength was estimated about 58% and 62%, respectively. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, yield strength and ultimate tensile strength were increased significantly about 121% and 107%, respectively. - Graphical Abstract: Copper coated CNTs were synthesized by the electroless plating process. Optimizing the plating bath to (1:1) by wt CNTs with Cu, thickness of Cu-coated CNTs has been reduced to 100 nm. Cu-coated CNTs developed the stronger interfacial bonding with the Al matrix which resulted in the efficient transfer of load. Highlights: • Copper coated CNTs were synthesized by the electroless plating process. • Thickness of Cu-coated CNTs has been reduced to 100 nm by optimized plating bath. • In 1.0 wt.% Cu-coated CNT/Al composite, microhardness increased by 103%. • Cu-coated CNTs transfer load efficiently with stronger interfacial bonding. • In 1.0 wt.% Cu-coated CNT/Al composite, Y.S and UTS increased by 126% and 105%.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Characterization of molybdenum particles reinforced Al6082 aluminum matrix composites with improved ductility produced using friction stir processing

Aluminum matrix composites (AMCs) reinforced with various ceramic particles suffer a loss in ductility. Hard metallic particles can be used as reinforcement to improve ductility. The present investigation focuses on using molybdenum (Mo) as potential reinforcement for Mo(0,6,12 and 18 vol.%)/6082Al AMCs produced using friction stir processing (FSP). Mo particles were successfully retained in the aluminum matrix in its elemental form without any interfacial reaction. A homogenous distribution of Mo particles in the composite was achieved. The distribution was independent upon the region within the stir zone. The grains in the composites were refined considerably due to dynamic recrystallization and pinning effect. The tensile test results showed that Mo particles improved the strength of the composite without compromising on ductility. The fracture surfaces of the composites were characterized with deeply developed dimples confirming appreciable ductility. - Highlights: •Molybdenum particles used as reinforcement for aluminum composites to improve ductility. •Molybdenum particles were retained in elemental form without interfacial reaction. •Homogeneous dispersion of molybdenum particles were observed in the composite. •Molybdenum particles improved tensile strength without major loss in ductility. •Deeply developed dimples on the fracture surfaces confirmed improved ductility.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Synthesis and electrocatalytic performance for p-nitrophenol reduction of rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites

Graphical abstract: The pure Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite with 5% Ag all exhibited rod-like morphology, and the microrods were actually composed of nanoparticles with mean size of 35 nm or so. - Highlights: • A facile route was designed to fabricate rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite nanomaterials. • Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite were modified on a GCE directly. • All samples exhibited enhanced catalytic property for p-nitrophenol reduction. - Abstract: Rod-like precursors of Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites with different Ag contents were synthesized via a co-precipitation method. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite samples were fabricated by calcining each precursor at 400 °C for 3 h. The as-prepared samples were characterized by thermogravimetric analysis and differential thermal gravimetric analysis (TGA/DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), respectively. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites were used as electrocatalyst modified on a glassy carbon electrode for p-nitrophenol reduction in basic solution. The results showed that p-nitrophenol could be reduced effectively on the modified electrode. By comparison with a bare glassy carbon electrode, peak current increased markedly with Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} samples, and peak potential decreased obviously with Ag/Co{sub 3}O{sub 4} samples. Ag/Co{sub 3}O{sub 4} composites with 4% Ag exhibited the highest electrocatalytic activity for p-nitrophenol reduction.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Preparation, characterization and enhanced visible-light photocatalytic activities of BiPO{sub 4}/BiVO{sub 4} composites

Graphical abstract: - Highlights: • BiPO{sub 4}/BiVO{sub 4} composites were successfully prepared by the hydrothermal method. • BiPO{sub 4}/BiVO{sub 4} composites exhibited broad absorption in the visible region. • Visible-light photocatalytic activities of BiPO{sub 4}/BiVO{sub 4} composites were enhanced. • P/V molar ratio and pH value of the reaction affect photocatalytic activity. • The mechanism of enhanced visible-light photocatalytic activities was discussed. - Abstract: BiPO{sub 4}/BiVO{sub 4} composites with different P/V molar ratios were prepared by the hydrothermal method and the effect of pH values of hydrothermal reaction on photocatalytic activity of BiPO{sub 4}/BiVO{sub 4} composite was investigated. The photocatalysts were characterized by X-ray diffraction, field emission scanning electron microscopy, energy-dispersive spectroscopy, X-ray photoelectron spectroscopy and UV–vis diffuse reflectance spectroscopy. The photocatalytic property of BiPO{sub 4}/BiVO{sub 4} was evaluated by photocatalytic degradation of Methylene blue under visible light irradiation. The results showed that the photocatalytic activity of the composites was much higher than that of pure BiPO{sub 4} and BiVO{sub 4}. The rate constant of Methylene blue degradation over BiPO{sub 4}/BiVO{sub 4} (P/V molar ratio of 5:1 and hydrothermal reaction pH value of 1.5) is 1.7 times that of pure BiVO{sub 4}. The photocatalytic activity enhancement of BiPO{sub 4}/BiVO{sub 4} composite is closely related to the BiVO{sub 4} functioning as a sensitizer to adsorb visible light and the heterojunction of BiPO{sub 4}/BiVO{sub 4} acting as an active center for hindering the rapid recombination of electron–hole pairs during the photocatalytic reaction.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Synthesis and photocatalytic activity of three-dimensional ZnS/CdS composites

Graphical abstract: - Highlights: • 3D urchin-like ZnS/CdS composites were synthesized via a two-step method. • The CdS nanoparticles were assembled on the thorns of 3D ZnS urchins. • The ZnS/CdS composites show excellent photocatalytic degradation activities. • The modification of CdS on ZnS is responsible for the enhanced property. - Abstract: Urchin-like ZnS/CdS semiconductor composites were successfully synthesized by combining solvothermal route with homogeneous precipitation process. The as-obtained samples were characterized by means of XRD, EDX, TEM, HR-TEM, ED and FE-SEM techniques. The results show that the as-obtained composites were comprised of the hexagonal structure ZnS and CdS, and CdS nanoparticles were assembled on the surfaces of the thorns of urchin-like ZnS. In addition, the optical properties and photocatalytic activities of the as-prepared ZnS/CdS composites toward some organic dyes (such as Methyl Orange, Pyronine B, Rhodamine B and Methylene Blue) were separately investigated. It is found that the ZnS/CdS composites exhibit excellent photocatalytic degradation activity for these dyes under UV irradiation, as compared to corresponding pure ZnS urchins and commercial anatase TiO{sub 2} (P-25). This enhanced activity may be related to the modification of CdS nanoparticles on the surfaces of thorns of ZnS urchins and a tentative mechanism for the enhanced photocatalytic degradation activities of the ZnS/CdS composite catalyst was proposed.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Facile fabrication of three-dimensional mesoporous Si/SiC composites via one-step magnesiothermic reduction at relative low temperature

Graphical abstract: - Highlights: • The Si/SiC composites were synthesized by one-step magnesiothermic reduction. • The mesoporous composites have a high specific surface area (655.7 m{sup 2} g{sup −1}). • The composites exhibited a strong photoluminescence and better biocompatibility. • The mechanisms of formation and photoluminescence of sample were discussed. - Abstract: By converting modified silica aerogels to the corresponding silicon/silicon carbide (Si/SiC) without losing its nanostructure, three-dimensional mesoporous (3DM) Si/SiC composites are successfully synthesized via one-step magnesothermic reduction at relative low temperature (650 °C). The phase composition and microstructure of the resulting samples are measured by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), Raman spectra, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). N{sub 2}-sorption isotherms results show that the products have high Brunauer–Emmett–Teller (BET) specific surface areas (up to 656 m{sup 2} g{sup −1}) and narrow pore-size distributions (1.5–30 nm). The composites exhibit a strong photoluminescence (PL) in blue-green light region (peak centered at 533 nm). We have set out work on the biocompatibility and enhancing PL of samples. As a result of excellent performances of the composites, it can be expected to have significant application in optoelectronics, biosensors, biological tracer and so on.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Facile synthesis of Ag–Cu{sub 2}O composites with enhanced photocatalytic activity

Highlights: • Ag–Cu{sub 2}O nanocomposites were synthesized via awet-chemical precipitation route. • The growth temperature does not exceed 50 °C in any step of the synthesis. • Enhanced photocurrent of Ag–Cu{sub 2}O composites, compared to pure Cu{sub 2}O particles. • The photocatalytic property was studied upon simulated sunlight. • Enhanced photocatalytic property of Ag–Cu{sub 2}O composites, compared to pure Cu{sub 2}O particles. - Abstract: Silver–cuprous oxide (Ag–Cu{sub 2}O) microcomposites are successfully prepared by a facile low-cost solution method. The obtained materials were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), field emission scanning electron microscopy (FESEM), ultraviolet–visible (UV–vis) spectroscopy, X-ray photoelectron spectroscopy (XPS). Experiments demonstrated that the formation of Ag–Cu{sub 2}O microcomposites was significantly influenced by the concentration of AgNO{sub 3}, and with increasing the concentration of AgNO{sub 3}, the optical absorption of the composites becomes strong. The photocatalytic activity of the prepared Ag–Cu{sub 2}O composites was determined by measuring the degradation of methyl orange solution under visible light, to find out its potential application in waste water treatment. The results reveal that the photocurrent of the composite is about 4 times higher than that of pure Cu{sub 2}O and the visible light photocatalytic activity of the composite is enhanced greatly on degradation of methyl orange. The reason for improvement in photocatalytic activity of the Ag–Cu{sub 2}O composites was also discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Composite electrolytes ceramic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}/glassy Li{sub 2}O-Y{sub 2}O{sub 3}-SiO{sub 2}

Highlights: • We synthesized Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}-x wt% 40.2Li{sub 2}O·5.7Y{sub 2}O{sub 3}·54.1SiO{sub 2} (x = 1–10) composites. • Density of the composite samples is higher than one of the sintered Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}. • The composition with x = 5 has high total conductivity, 2.5 × 10{sup −5} S cm{sup −1} at 25 °C. - Abstract: We have investigated the effect of lithium yttrium-silicate glass 40.2Li{sub 2}O·5.7Y{sub 2}O{sub 3}·54.1SiO{sub 2} on the density and total conductivity of tetragonal Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}. An optimal sintering temperature (1200 °C) was selected on the basis of a composite with 1 wt% of the glass having the highest density and total conductivity after annealing at this temperature. A series of composites Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}-x wt% 40.2Li{sub 2}O·5.7Y{sub 2}O{sub 3}·54.1SiO{sub 2} (x = 1–10) was prepared. The samples were characterized by X-ray diffraction, scanning electron microscopy and differential scanning calorimetry. The data revealed that the sintering additive interacted with Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}, causing the glass to crystallize during annealing. The conductivity of the composites was studied using complex impedance spectroscopy over a temperature range of 20–250 °C. The composite with x = 5 exhibited the highest total conductivity at room temperature: 2.5 × 10{sup −5} S cm{sup −1}.

36 MATERIALS SCIENCE↗

DOE OSTI2018

One-pot synthesis of the g-C3N4/S-doped ZnO composite with assistance of sodium lignosulfonate and its enhanced photodegradation on organic pollutants

Highlights: • g-C{sub 3}N{sub 4}/S-ZnO composite was successfully prepared by a facile one-pot method. • SLS acts as a linkage reagent in the synthetic process. • S originated from SLS was doped into ZnO. • Combining g-C{sub 3}N{sub 4} with ZnO cooperatively improves composite photocatalytic performance. • The g-C{sub 3}N{sub 4}/S-ZnO composite shows excellent photocatalytic degradation on phenol. - Abstract: Lignin is one of the most abundant materials in nature, but its highly value-adding utilization is still a challenge. Herein, sodium lignosulfonate (SLS) was adopted to fabricate ZnO centering on the concept of “using lignin valuably”. And the g-C{sub 3}N{sub 4}/S-ZnO (CNSZ) composite was successfully prepared. SLS serves as a linkage reagent, interacting with ZnO on one hand and simultaneously helping urea (processor of g-C{sub 3}N{sub 4}) to be deposited with ZnO. The structure and morphology of CNSZ were fully characterized. It is shown that g-C{sub 3}N{sub 4} co-exists in the composite. Meanwhile, EDS and XPS analyses indicate the presence of S in the composite, which originates from SLS. The composite is found to show good photocatalytic property. Its degradation efficiency on phenol is 8.5 times higher than bare ZnO. Due to its facile synthesis and excellent property, the newly-synthesized CNSZ is anticipated to be promising for water treatment application.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Compositionally Graded High Entropy Alloy with a Strong front and ductile base

Material components with variable properties can be ideal for many advanced applications due to their seamless nature of microstructural transition, cost reduction and high resistance of failure. A compositionally graded AlXCoCrFeNi (x=0.3-0.7) high entropy alloy composite build was additively manufactured using laser engineered net shaping (LENSTM). In this high throughput production process, the elemental composition of Al-Co-Cr-Fe-Ni powders in the hoppers were varied and the feed rates were shifted to create a laminate of Al0.3CoCrFeNi and Al0.7CoCrFeNi layers, with a 500 µm wide transition zone of intermediary composition. The energy-dispersive X-ray spectroscopy along the build direction verified the elemental composition matching closely with the targeted compositions. X-ray diffraction revealed the Al0.3CoCrFeNi to be a single-phase fcc structure whereas Al0.7CoCrFeNi had dual phase fcc + B2/ bcc. Scanning electron microscopy was used to capture the microstructural features in the two layers as well as the transition zone. The massive shift in mechanical properties of hardness, dynamic strength and work hardening rates in this graded composite have been discussed. With this endeavor, the microstructural complexity of HEAs has been combined with the unique advantage of LENSTM to achieve an ingenious path to fabricate materials suited applications demanding variable strength and ductility/toughness.

Gwalani, Bharat↗

DOE OSTI2022

Integrating very-high-resolution UAS data and airborne imaging spectroscopy to map the fractional composition of Arctic plant functional types in Western Alaska

Widespread changes in vegetation cover and composition are driving strong impacts on Arctic ecosystem functioning and global climate feedbacks. An accurate characterization of tundra vegetation composition is required to understand how the Arctic will respond to future climate change. However, quantifying tundra vegetation composition over large areas is challenging as commonly-used satellite observations are too coarse, spatially and spectrally, to differentiate low-lying tundra vegetation types. Recent airborne and spaceborne imaging spectroscopy platforms provide better data to characterize vegetation composition. Yet, our ability to characterize vegetation composition with imaging spectroscopy remains largely unexplored in the Arctic, particularly due to a lack of ground observations needed to train and test classification models. To address this problem, we collected very-high-resolution (VHR, ~5 cm) unoccupied aerial system (UAS) imagery at three low-Arctic tundra sites located on the Seward Peninsula, western Alaska. In this paper, we examine the feasibility of integrating imagery from the UAS and the hyperspectral Airborne Visible/Infrared Imaging Spectrometer, Next Generation (AVIRIS-NG) airborne instrument to map the fractional composition of 12 key Arctic plant functional types (PFTs). To this end, we first mapped the 12 PFTs from our VHR UAS imagery using random forest classification. We then used these UAS-derived PFT maps as ground truth to develop partial least squares regression (PLSR) models to predict the fractional cover (FCover) of each PFT from AVIRIS-NG imagery. Further, we evaluated the performance of our PLSR models using reserved UAS samples, as well as by mapping PFT FCover and dominant PFT for large tundra landscapes. Our results show that 1) Arctic PFTs can be effectively mapped using VHR UAS imagery, with overall accuracy between 86% and 92%, 2) when the UAS mapped PFTs were used to inform PLSR scaling models, the FCover of the 12 PFTs could be effectively estimated from AVIRIS-NG imagery with a mean absolute error (MAE) <0.13, and 3) our PLSR models outperformed traditional, fully constrained least-squares (FCLS) linear mixture analysis and produced high-quality, spatially contiguous PFT FCover and PFT maps that captured vegetation spatial patterns with similar accuracy to those developed from UAS imagery. The developed PLSR models have the potential to be broadly applied for quantifying vegetation composition with AVIRIS-NG images to help monitor tundra vegetation dynamics and improve process-based modeling of tundra ecosystems.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Natural organic matter composition and nanomaterial surface coating determine the nature of platinum nanomaterial-natural organic matter corona

Natural organic matter corona (NOM corona) is an interfacial area between nanomaterials (NMs) and the sur- rounding environment, which gives rise to NMs' unique surface identity. While the importance of the formation of natural organic matter (NOM) corona on engineered nanomaterials (NMs) to NM behavior, fate, and toxicity has been well-established, the understanding of how NOM molecular properties affect NOM corona composition remains elusive due to the complexity and heterogeneity of NOM. This is further complicated by the variation of NOMs from different origins. Here we use eight NOM isolates of different molecular composition and ultrahigh resolution Fourier-transform ion cyclotron resonance-mass spectrometry (ESI-FT-ICR-MS) to determine the mol- ecular composition of platinum NM-NOM corona as a function of NOM composition and NM surface coating. We observed that the composition of PtNM-NOM corona varied with the composition of the original NOM. The per- centage of NOM formulas that formed PVP-PtNM-NOM corona was higher than those formed citrate-PtNM-NOM corona, due to increased sorption of NOM formulas, in particular condensed hydrocarbons, to the PVP coating. The relative abundance of heteroatom formulas (CHON, CHOS, and CHOP) was higher in the PVP-PtNM-NOM corona than in citrate-PtNM-corona which was in turn higher than those in the original NOM isolate, indicating preferential partitioning of heteroatom-rich molecules to NM surfaces. The relative abundance of CHO, CHON, CHOS, CHOP and condensed hydrocarbons in PtNM-NOM corona increased with their increase in NOM isolates. Furthermore, PtNM-NOM corona is rich with compounds with high molecular weight. This study demonstrates that the composition and properties of PtNM-NOM corona depend on NOM molecular properties and PtNM sur- face coating. The results here provide evidence of molecular interactions between NOM and NMs, which are crit- ical to understanding NM colloidal properties (e.g., surface charge and stability), interaction forces (e.g., van der Waals and hydrphobic), environmental behaviors (e.g., aggregation, disso.

Baalousha, Mohammed↗

DOE OSTI2015

A novel approach in organic waste utilization through biochar addition in wood/polypropylene composites

Highlights: • Biochar made from waste wood was added with wood polypropylene composites. • 24% biochar gave the best mechanical properties. • 6% biochar had no effect on physico-mechanical properties of composites. • Coupling agent remained unreacted in composites having higher amount of biochar. - Abstract: In an attempt to concurrently address the issues related to landfill gas emission and utilization of organic wastes, a relatively novel idea is introduced to develop biocomposites where biochar made from pyrolysis of waste wood (Pinus radiata) is added with the same wood, plastic/polymer (polypropylene) and maleated anhydride polypropylene (MAPP). Experiments were conducted by manufacturing wood and polypropylene composites (WPCs) mixed with 6 wt%, 12 wt%, 18 wt%, 24 wt%, and 30 wt% biochar. Though 6 wt% addition had similar properties to that of the control (composite without biochar), increasing biochar content to 24 wt% improved the composite’s tensile/flexural strengths and moduli. The biochar, having high surface area due to fine particles and being highly carbonised, acted as reinforcing filler in the biocomposite. Composites having 12 wt% and 18 wt% of biochar were found to be the most ductile and thermally stable, respectively. This study demonstrates that, WPCs added with biochar has good potential to mitigate wastes while simultaneously producing biocomposites having properties that might be suited for various end applications.

09 BIOMASS FUELS↗

DOE OSTI2017

Understanding Composition-Dependent Synergy of PtPd Alloy Nanoparticles in Electrocatalytic Oxygen Reduction Reaction

Gaining an insight into the relationship between the bimetallic composition and catalytic activity is essential for the design of nanoalloy catalysts for oxygen reduction reaction. This report describes findings of a study of the composition–activity relationship for PtPd nanoalloy catalysts in oxygen reduction reaction (ORR). Pt n Pd 100-n nanoalloys with different bimetallic compositions are synthesized by wet chemical method. While the size of the Pt 50 Pd 50 nanoparticles is the largest among the nanoparticles with different compositions, the characterization of the nanoalloys using synchrotron high-energy X-ray diffraction (HE-XRD) coupled to atomic pair distribution function (PDF) analysis reveals that the nanoalloy with an atomic Pt:Pd ratio of 50:50 exhibits an intermediate lattice parameter. Electrochemical characterization of the nanoalloys shows a minimum ORR activity at Pt:Pd ratio close to 50:50, whereas a maximum activity is achieved at Pt:Pd ratio close to 10:90. The composition–activity correlation is assessed by theoretical modeling based on DFT calculation of nanoalloy clusters. In addition to showing an electron transfer from PtPd alloy to oxygen upon its adsorption on the nanoalloy, a relatively large energy difference between HOMO for nanoalloy and LUMO for oxygen is revealed for the nanoalloy with an atomic Pt:Pd ratio of 50:50. By analysis of the adsorption of OH species on PtPd (111) surfaces of different compositions, the strongest adsorption energy is observed for Pt 96 Pd 105 (Pt:Pd ≈ 50:50) cluster, which is believed to be likely responsible for the reduced activity. Interestingly, the adsorption energy on Pt24Pd177 (Pt:Pd ≈ 10:90) cluster falls in between Pt 96 Pd 105 and Pd 201 clusters, which is believed to be linked to the observation of the highest catalytic activity for the nanoalloy with an atomic Pt:Pd ratio of 10:90. Furthermore, these findings have implications for the design of composition-tunable nanoalloy catalysts for ORR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Visible Light Assisted Photocatalytic Hydrogen Generation by Ta 2 O 5 /Bi 2 O 3 , TaON/Bi 2 O 3 , and Ta 3 N 5 /Bi 2 O 3 Composites

Composites comprised of two semiconducting materials with suitable band gaps and band positions have been reported to be effective at enhancing photocatalytic activity in the visible light region of the electromagnetic spectrum. Here, we report the synthesis, complete structural and physical characterizations, and photocatalytic performance of a series of semiconducting oxide composites. UV light active tantalum oxide (Ta2O5) and visible light active tantalum oxynitride (TaON) and tantalum nitride (Ta 3 N 5 ) were synthesized, and their composites with Bi 2 O 3 were prepared in situ using benzyl alcohol as solvent. The composite prepared using equimolar amounts of Bi 2 O 3 and Ta 2 O 5 leads to the formation of the ternary oxide, bismuth tantalate (BiTaO 4 ) upon calcination at 1000 °C. The composites and single phase bismuth tantalate formed were characterized by powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), Brunauer–Emmett–Teller (BET) surface area measurement, scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV–Vis diffuse reflectance spectroscopy, and photoluminescence. The photocatalytic activities of the catalysts were evaluated for generation of hydrogen using aqueous methanol solution under visible light irradiation (λ ≥ 420 nm). The results show that as-prepared composite photocatalysts extend the light absorption range and restrict photogenerated charge-carrier recombination, resulting in enhanced photocatalytic activity compared to individual phases. The mechanism for the enhanced photocatalytic activity for the heterostructured composites is elucidated based on observed activity, band positions calculations, and photoluminescence data.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Multi-stimuli responsive tetra-PPO 60 -PEO 20 ethylene diamine block copolymer enables pH, temperature, and solvent regulation of Au nanoparticle composite plasmonic response

In this work a gold nanoparticle (NP) hydrogel composite prepared by multi-step cascade synthesis undergoes temperature, pH, and solvent dependent nanoscale structural transformations promoting modulation of the plasmon resonance. The composite is spontaneously prepared from a non-covalent lamellar structured lyotropic mesophase (complex fluid) composed of amphiphiles (DMPC and Triton X-100) that support the reactive constituents, a mixture of hydroxyl and acrylate end-derivatized Tetronic (Poloxamine) polymer and [AuCl4] – . The reaction sequence begins with the reduction of [AuCl4] – by the ethylene diamine linkage and PEO blocks of the Tetronic, yielding Au NPs. The redox reaction generates free radicals initiating crosslinking of the acrylate end-derivatized polymer producing a chemical hydrogel. Optical spectroscopy and electron microscopy confirm Au NP formation. ATR/FT-IR spectroscopy and thermal analysis establish acrylate crosslinking and network formation. X-ray scattering reveals the composite reversibly converts between multilamellar and bicontinuous cubic structures as temperature is increased above 35 °C for composites containing protonated ethylene diamine linkages (un-buffered water or acidic buffer). The reversible changes in nanoarchitecture red shifts and broadens the collective plasmon (from 523 nm to 575 nm) of the composite, an observation attributed to re-organization of confined NPs from 2D sheets (lamellae) to 1D columns (bicontinuous cubic channels). Composites prepared in alkaline buffer do not undergo a structural conversion with temperature, retaining a multilamellar architecture. In addition to pH and thermo-responsivity, the composite swells reversibly in polar solvents, which acts to de-aggregate and aggregate the encapsulated NPs and varies the plasmon resonance by Δ52 nm. This work reports the first combined use of a polymer to achieve both the in situ synthesis of spatially confined plasmonic NPs and their reversible stimuli-triggered re-organization mediated by interconvertible changes in scaffold nanoarchitecture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

3D printed water-stable Cd-doped Cs 4 MnBi 2 Cl 12 /polylactic acid perovskite/polymer composites for high-flux X-ray scintillation

Stable and efficient X-ray scintillators are crucial for medical diagnostics, industrial, and defense applications. However, conventional scintillator technologies face a trade-off between stability, optimal performance, and sustainability. Herein, we introduce 3D-printed Cs 4 MnBi 2 Cl 12 (Pero1) and Cs 4 Cd 0.68 Mn 0.32 Bi 2 Cl 12 (Pero2) perovskite microcrystals embedded within a polylactic acid (PLA) polymer composite as X-ray scintillators, combining efficiency, stability, and sustainability. The orange luminescent perovskite powder phosphors exhibited poor water stability, which was successfully addressed through incorporation into PLA via filament extrusion and fused deposition modeling (FDM) 3D printing. The resulting composite films demonstrated remarkable water stability while maintaining uniform orange emission throughout the polymer matrix, as confirmed by 3D topography scanning and X-ray fluorescence mapping. Structural characterization revealed minimal chemical interaction between the perovskite and PLA matrix, with the composites retaining their crystalline properties. The PLA-Pero2 composite exhibited superior optical properties, with a photoluminescence quantum yield of 47%, nearly 17 times higher than that of PLA-Pero1 (2.8%), attributed to the effective suppression of non-radiative decay pathways through Cd 2+ doping. Under hard X-ray irradiation at synchrotron beamlines, both composites exhibited excellent radioluminescence, with emission peaks at 605 nm, a linear response across a wide X-ray flux range, and remarkable radiation stability, showing less than 3% intensity degradation after 600 seconds of continuous high-dose exposure. The PLA-Pero2 composite achieved a spatial resolution of 5 line pairs per millimeter and a contrast ratio of 0.255. These performance metrics, combined with the polymer's biodegradability and scalability through additive manufacturing, position PLA-based composites as a more sustainable alternative to conventional petroleum-based polymer scintillators for next-generation medical imaging, radiation monitoring, and industrial radiography applications.

3D Printing↗

DOE OSTI2014

Fluorescent of C-dot composite thin films and its properties

In the present work, we report the preparation of a fluorescent carbon nanodots (C-dots) epoxy composite thin films on a glass substrate. C-dots were prepared directly by a simple hydrothermal method using citric acid as a carbon source. The C-dots solutions were mixed with a transparent epoxy resin to form C-dot epoxy composite. Furthermore, the composite precursor was deposited on the glass substrate using a spin coating method in order to fabricate C-dot epoxy composite thin film. The transmittance intensity of C-dot composite film reached up to 90% in the visible light spectra. Using Swanopoel method, the film thickness of fabricated C-dot composite film was determined at about 1.45 μm, a value lies in a typical range needed for a wide range application. Thus, the C-dot composite film is promising in broadening applications in various fields such as energy conversion, optoelectronics, and display technology.

36 MATERIALS SCIENCE↗