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At least 631 records · Page 35
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Formation of supported lipid bilayers containing phase-segregated domains and their interaction with gold nanoparticles

The cell membrane represents an important biological interface that nanoparticles may encounter after being released into the environment. Interaction of nanoparticles with cellular membranes may alter membrane structure and function, lead to their uptake into cells, and elicit adverse biological responses. Supported lipid bilayers have proven to be valuable ex vivo models for biological membranes, allowing investigation of their mechanisms of interaction with nanoparticles with a degree of control impossible in living cells. To date, the majority of research on nanoparticle interaction with supported lipid bilayers has employed membranes composed of single or binary mixtures of phospholipids. Cellular membranes contain a wide variety of lipids and exhibit lateral organization. Ordered membrane domains enriched in specific membrane components are referred to as lipid rafts and have not been explored with respect to their interaction with nanoparticles. Here we develop model lipid raft-containing membranes amenable to investigation by a variety of surface-sensitive analytical techniques and demonstrate that lipid rafts influence the extent of nanoparticle attachment to model membranes. We determined conditions that allow reliable formation of bilayers containing rafts enriched in sphingomyelin and cholesterol and confirmed their morphology by structured illumination and atomic force microscopies. We demonstrate that lipid rafts increase attachment of cationic gold nanoparticles to model membranes under near physiological ionic strength conditions (0.1 M NaCl) at pH 7.4. We anticipate that these results will serve as the foundation for and motivate further study of nanoparticle interaction with compositionally varied lipid rafts.

cellular membranes↗
DOE OSTI2015

Tuning of electrostatic vs. depletion interaction in deciding the phase behavior of nanoparticle-polymer system

Nanoparticle-polymer system interestingly show a re-entrant phase behavior where charge stabilized silica nanoparticles (phase I) undergo particle clustering (phase II) and then back to individual particles (phase I) as a function of polymer concentration. Such phase behavior arises as a result of dominance of various interactions (i) nanoparticle-nanoparticle electrostatic repulsion (ii) polymer induced attractive depletion between nanoparticles and (iii) polymer-polymer repulsion, at different concentration regimes. Small-angle neutron scattering (SANS) has been used to study the evolution of interaction during this re-entrant phase behavior of nanoparticles by contrast-marching the polymer. The SANS data have been modeled using a two-Yukawa potential accounting for both attractive and repulsive parts of the interaction between nanoparticles. The degree of both of these parts has been separately tuned by varying the polymer concentration and ionic strength of the solution. Both of these parts are found to have long-range nature. At low polymer concentrations, the electrostatic repulsion dominates over the depletion attraction. The magnitude and the range of the depletion interaction increase with the polymer concentration leading to nanoparticle clustering. At higher polymer concentrations, the increased polymer-polymer repulsion reduces the strength of depletion leading to re-entrant phase behavior. The clusters formed under depletion attraction are found to have surface fractal morphology.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Effect of aluminum and yttrium doping on zinc sulphide nanoparticles

In this work, pristine and doped Zinc Sulphide (ZnS) nanoparticles have been synthesized via chemical co-precipitation method. ZnS nanoparticles have been doped with Aluminium (Al) and Yttrium (Y) with doping concentration of 5wt% each. The structural and optical properties of the as prepared nanoparticles have been studied using X-Ray diffraction (XRD) technique and Photoluminescence spectroscopy. Average grain size of 2-3nm is observed through the XRD analysis. Effect of doping on stress, strain and lattice constant of the nanoparticles has also been analyzed. Photoluminescence spectra of the as prepared nanoparticles is enhanced due to Al doping and quenched due to Y doping. EDAX studies confirm the relative doping percentage to be 3.47 % and 3.94% by wt. for Al and Y doped nanoparticles respectively. Morphology of the nanoparticles studied using TEM and SEM indicates uniform distribution of spherical nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Precise control of polymer coated nanopores by nanoparticle additives: Insights from computational modeling

Polymer-nanoparticle composites are a promising new class of materials for creation of controllable nano-patterned surfaces and nanopores. We use coarse-grained molecular dynamics simulations augmented with analytical theory to study the structural transitions of surface grafted polymer layers (brushes) induced by infiltration of nanoparticles that are attracted to the polymers in the layer. We systematically compare two different polymer brush geometries: one where the polymer chains are grafted to a planar surface and the other where the chains are grafted to the inside of a cylindrical nanochannel. We perform a comprehensive study of the effects of the material parameters such as the polymer chain length, chain grafting density, nanoparticle size, strength of attraction between nanoparticles and polymer monomers, and, in the case of the cylindrically grafted brush, the radius of the cylinder. We find a very general behavioral motif for all geometries and parameter values: the height of the polymer brush is non-monotonic in the nanoparticle concentration in solution. As the nanoparticle concentration increases, the brush height first decreases and after passing through a minimum value begins to increase, resulting in the swelling of the nanoparticle infused brush. These morphological features may be useful for devising tunable “smart” nano-devices whose effective dimensions can be reversibly and precisely adjusted by changing the nanoparticle concentration in solution. The results of approximate Self-Consistent Field Theory (SCFT) calculations, applicable in the regime of strong brush stretching, are compared to the simulation results. The SCFT calculations are found to be qualitatively, even semi-quantitatively, accurate when applied within their intended regime of validity, and provide a useful and efficient tool for modeling such materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Observing structural reorientations at solvent–nanoparticle interfaces by X-ray diffraction – putting water in the spotlight

Nanoparticles are attractive in a wide range of research genres due to their size-dependent properties, which can be in contrast to those of micrometre-sized colloids or bulk materials. This may be attributed, in part, to their large surface-to-volume ratio and quantum confinement effects. There is a growing awareness that stress and strain at the particle surface contribute to their behaviour and this has been included in the structural models of nanoparticles for some time. One significant oversight in this field, however, has been the fact that the particle surface affects its surroundings in an equally important manner. It should be emphasized here that the surface areas involved are huge and, therefore, a significant proportion of solvent molecules are affected. Experimental evidence of this is emerging, where suitable techniques to probe the structural correlations of liquids at nanoparticle surfaces have only recently been developed. The recent validation of solvation shells around nanoparticles has been a significant milestone in advancing this concept. Restructured ordering of solvent molecules at the surfaces of nanoparticles has an influence on the entire panoply of solvent–particle interactions during, for example, particle formation and growth, adhesion forces in industrial filtration, and activities of nanoparticle–enzyme complexes. This article gives an overview of the advances made in solvent–nanoparticle interface research in recent years: from description of the structure of bulk solids and liquids via macroscopic planar surfaces, to the detection of nanoscopic restructuring effects. Water–nanoparticle interfaces are given specific attention to illustrate and highlight their similarity to biological systems.

36 MATERIALS SCIENCE↗
DOE OSTI2014

SU-E-T-338: Ultrastable PRNA 3WJ Nanoparticles as Potential I-125 and C-131 Carriers for Targeted Radiation Therapy

Purpose: To study the feasibility of using the pRNA 3WJ nanoparticles to carry I-125 or Cs-131 to target and treat cancer. As the first step, we investigated the stabilities of pRNA 3WJ nanoparticles that are essential for cancer targeting and treatment in this study. Methods: The thermodynamic stability of assembled RNA 3WJ nanoparticles was studied using the TGGE system. The nanoparticles were irradiated with I-125 or Cs-131 radioactive sources that were immersed in the RNA nanoparticle/DNA structure sample liquid contained in a small vial. The irradiation of the RNA samples was performed for different time periods and doses. The purpose was to distinguish the effects of radiation on DNA and RNA structures. Unradiated samples were used as control. Results: RNA nanoparticles were formed by mixing three pieces of oligos, 3WJa, 3WJb, and 3WJc at 1:1:1 molar ratio. Figure 4 demonstrates that 2′-F modified 3WJ nanoparticles remained stable at temperatures as high as 66.8 ± 2°C, and exhibited melting temperatures of 71 ± 2°C. The radiation stability test was performed with I- 125 and Cs-131 irradiation. Several DNA structures including plasmids were included as control. The first test introduced I-125 and a low dose of 1 Gy to both RNA and DNA samples, but no change was observed. When the dose was increased to 30 Gy, DNA was damaged while RNA remained unchanged. Three tests were also conducted with Cs-131 with 7 Gy, 21 Gy, 30 Gy, and 89 Gy, and the results were similar to those with I-125. Conclusion: pRNA 3WJ nanoparticles are able to form efficiently by onepot self-assembly. They remained stable at high temperatures and high therapeutic doses over a long time. These unique features suggest that RNA 3WJ nanoparticles have the potential to be used for targeted radiation therapy for cancer treatment.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2019

Study of Evaporation of Laser-Heated Iron–Carbon Nanoparticles Using Analysis of Thermal Radiation

Evaporation of iron nanoparticles in carbon shells under pulsed laser irradiation is analyzed. Iron–carbon nanoparticles are synthesized in a shock tube reactor with the aid of pyrolysis of the 0.25% Fe(CO){sub 5} + 0.25% C{sub 6}H{sub 6} mixture in argon. Laser radiation is used for additional heating to temperatures that exceed the evaporation threshold of the iron core of nanoparticles. Time profiles of the thermal radiation of laser-heated nanoparticles are measured. The two-color pyrometry is used to determine the evaporation temperature of nanoparticles, and the laser extinction makes it possible to monitor the loss of volume fraction of the condensed phase upon evaporation. Approximation of experimental signals of laser-heated nanoparticles using model curves is employed to determine effective enthalpy of evaporation of iron–carbon nanoparticles. It is shown that the iron core of nanoparticles is evaporated through the carbon shell and the energy spent by such a process is approximately twice greater than the evaporation enthalpy of bulk iron with free surface.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

Development of 225Ac-doped biocompatible nanoparticles for targeted alpha therapy

Abstract Targeted alpha therapy (TAT) relies on chemical affinity or active targeting using radioimmunoconjugates as strategies to deliver α-emitting radionuclides to cancerous tissue. These strategies can be affected by transmetalation of the parent radionuclide by competing ions in vivo and the bond-breaking recoil energy of decay daughters. The retention of α-emitting radionuclides and the dose delivered to cancer cells are influenced by these processes. Encapsulating α-emitting radionuclides within nanoparticles can help overcome many of these challenges. Poly(lactic- co -glycolic acid) (PLGA) nanoparticles are a biodegradable and biocompatible delivery platform that has been used for drug delivery. In this study, PLGA nanoparticles are utilized for encapsulation and retention of actinium-225 ([ 225 Ac]Ac 3+ ). Encapsulation of [ 225 Ac]Ac 3+ within PLGA nanoparticles (Z ave = 155.3 nm) was achieved by adapting a double-emulsion solvent evaporation method. The encapsulation efficiency was affected by both the solvent conditions and the chelation of [ 225 Ac]Ac 3+ . Chelation of [ 225 Ac]Ac 3+ to a lipophilic 2,9-bis-lactam-1,10-phenanthroline ligand ([ 225 Ac]AcBLPhen) significantly decreased its release (< 2%) and that of its decay daughters (< 50%) from PLGA nanoparticles. PLGA nanoparticles encapsulating [ 225 Ac]AcBLPhen significantly increased the delivery of [ 225 Ac]Ac 3+ to murine (E0771) and human (MCF-7 and MDA-MB-231) breast cancer cells with a concomitant increase in cell death over free [ 225 Ac]Ac 3+ in solution. These results demonstrate that PLGA nanoparticles have potential as radionuclide delivery platforms for TAT to advance precision radiotherapy for cancer. In addition, this technology offers an alternative use for ligands with poor aqueous solubility, low stability, or low affinity, allowing them to be repurposed for TAT by encapsulation within PLGA nanoparticles. Graphical Abstract

60 APPLIED LIFE SCIENCES↗
DOE OSTI2023

Linear and Nonlinear Optical Properties of Iridium Nanoparticles Grown via Atomic Layer Deposition

Nonlinear optical phenomena enable novel photonic and optoelectronic applications. Especially, metallic nanoparticles and thin films with nonlinear optical properties offer the potential for micro-optical system integration. For this purpose, new nonlinear materials need to be continuously identified, investigated, and utilized for nonlinear optical applications. While noble-metal nanoparticles, nanostructures, and thin films of silver and gold have been widely studied, iridium (Ir) nanoparticles and ultrathin films have not been investigated for nonlinear optical applications yet. Here, we present a combined theoretical and experimental study on the linear and nonlinear optical properties of iridium nanoparticles deposited via atomic layer deposition (ALD). Linear optical constants, such as the effective refractive index and extinction coefficient, were evaluated at different growth stages of nanoparticle formation. Both linear and nonlinear optical properties of these Ir ALD coatings were calculated theoretically using the Maxwell Garnett theory. The third-order susceptibility of iridium nanoparticle samples was experimentally investigated using the z-scan technique. According to the experiment, for an Ir ALD coating with 45 cycles resulting in iridium nanoparticles, the experimentally determined nonlinear third-order susceptibility is about χ Ir (3) = (2.4 – i2.1) × 10 –17 m 2 /V 2 at the fundamental wavelength of 700 nm. The theory fitted to the experimental results predicts a 5 × 10 6 -fold increase around 230 nm. This strong increase is due to the proximity to the Mie resonance of iridium nanoparticles.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Bio‐Inspired In Situ Tuning of the Hydrophobic Environment Around Catalytically Active Organic Ligand‐Stabilized Ruthenium Nanoparticles

Abstract The organic ligand environment surrounding enzymatic and homogeneous catalytic active sites often determines catalytic activity. Ruthenium nanoparticles, ≤1 nm in diameter, are synthesized using monodentate thiol, monodentate phosphine, and bidentate bisphosphine ligands. Even though some of the ruthenium surface is blocked by the ligands, catalytic activity is still observed for CO oxidation and H 2 O 2 decomposition. All three ligand‐stabilized ruthenium nanoparticles have similar CO oxidation rates; however, the bisphosphine‐stabilized Ru nanoparticles are approximately 2.5 times less active than the monothiol‐stabilized and monophosphine‐stabilized ruthenium nanoparticles for H 2 O 2 decomposition. It is observed that the organic ligand environment is modulated in situ during nanoparticle synthesis via partial oxidation of the bisphosphine as confirmed by 31 P NMR measurements. We hypothesize that bisphosphine‐bound Ru nanoparticles consist of a Ru core with some of the ligands bound in a monodentate manner where the other P atom is oxidized and not bound to the Ru surface leading to a thicker hydrophobic layer around the Ru nanoparticles. The increase in hydrophobicity is confirmed via contact angle and zeta potential measurements. H 2 O 2 decomposition rates are known to decrease with increasing hydrophobicity, and this work illustrates a pathway for increasing hydrophobicity in situ using ligand‐bound metallic nanoparticles.

Sufyan, Sayed Abu [Department of Chemical Engineer↗
DOE OSTI2015

Protein adsorption onto nanoparticles induces conformational changes: Particle size dependency, kinetics, and mechanisms

The use of nanomaterials in bioapplications demands a detailed understanding of protein–nanoparticle interactions. Proteins can undergo conformational changes while adsorbing onto nanoparticles, but studies on the impact of particle size on conformational changes are scarce. We have shown that conformational changes happening upon adsorption of myoglobin and BSA are dependent on the size of the nanoparticle they are adsorbing to. Out of eight initially investigated model proteins, two (BSA and myoglobin) showed conformational changes, and in both cases this conformational change was dependent on the size of the nanoparticle. Nanoparticle sizes ranged from 30 to 1000 nm and, in contrast to previous studies, we attempted to use a continuous progression of sizes in the range found in live viruses, which is an interesting size of nanoparticles for the potential use as drug delivery vehicles. Conformational changes were only visible for particles of 200 nm and bigger. Using an optimized circular dichroism protocol allowed us to follow this conformational change with regard to the nanoparticle size and, thanks to the excellent temporal resolution also in time. We uncovered significant differences between the unfolding kinetics of myoglobin and BSA. In this study, we also evaluated the plausibility of commonly used explanations for the phenomenon of nanoparticle size-dependent conformational change. Currently proposed mechanisms are mostly based on studies done with relatively small particles, and fall short in explaining the behavior seen in our studies.

Biotechnology & Applied Microbiology↗
DOE OSTI2018

Scaling Laws for Polymer Chains Grafted onto Nanoparticles

An experimental approach is presented for identifying the scaling laws for polymer chains grafted onto gold nanoparticles. Poly(ethylene oxide) of various molecular weights are grafted onto gold nanoparticles via thiol end-functional groups. The polymer-grafted nanoparticles are self-assembled into monolayers from solvents of different quality. Over a significant range of graft densities, nanoparticle monolayers deposited from good (athermal) solvent exhibit particle spacing that scales according to theoretical predictions for chains in dilute solution. This unexpected result for ordered nanoparticle monolayers is discussed in the context of the deposition process. In monolayers deposited from theta solvent, molecular weight scaling of particle spacing breaks down, possibly due to chain length dependence of solvent quality. In poor solvent, the structure of nanoparticle assemblies is not sufficiently ordered to obtain reliable measurements, possibly due to loss of nanoparticle dispersion. This approach opens up the possibility for accurate measurement of the effect of solvent on grafted chain scaling in nanoparticle assemblies.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

Janus Nanoparticle Emulsions as Chiral Nanoreactors for Enantiomerically Selective Ligand Exchange

Abstract Janus nanoparticles capped with a hydrophobic and hydrophilic hemisphere of mercapto ligands can self‐assemble into hollow, emulsion‐like nanostructures in controlled media. As the nanoparticle emulsions are chiroptically active exhibiting a plasmonic circular dichroism absorption in the visible range, they can be exploited as a unique chiral nanoreactor by selective encapsulation of d ‐enantiomer into the water phase of the water‐in‐oil emulsions for directional functionalization of the nanoparticles and endow the resulting nanoparticles with select chirality. This is demonstrated in the present study with gold Janus nanoparticles functionalized with (hydrophobic) hexanethiolates and (hydrophilic) 3‐mercapto‐1,2‐propandiol, and d , l ‐cysteine is used as the molecular probe. Experimental results demonstrate that d ‐cysteine is the preferred enantiomers entrapped within the nanoparticle emulsions, where the ensuing ligand exchange reaction is initially confined to the hydrophilic face of the Janus nanoparticles. This suggests that with a deliberate control of the reaction time, chiral Janus nanoparticles can be readily prepared by ligand exchange reactions even with a racemic mixture of ligands.

Lu, Jia En↗
DOE OSTI2014

Functionalized mesoporous silica nanoparticles for oral delivery of budesonide

Non-functionalized and amino-functionalized mesoporous silica nanoparticle were loaded with anti-inflammatory drug budesonide and additionally post-coated with bioadhesive polymer (carbopol). TEM images showed spherical shape of the nanoparticles and slightly higher polydispersity after coating with carbopol. Nitrogen physisorption and thermogravimetic analysis revealed that more efficient loading and incorporation into the pores of nanoparticles was achieved with the amino-functionalized silica carrier. Infrared spectra indicated that the post-coating of these nanoparticles with carbopol led to the formation of bond between amino groups of the functionalized carrier and carboxyl groups of carbopol. The combination of amino-functionalization of the carrier with the post-coating of the nanoparticles sustained budesonide release. Further, an in vitro model of inflammatory bowel disease showed that the cytoprotective effect of budesonide loaded in the post-coated silica nanoparticles on damaged HT-29 cells was more pronounced compared to the cytoprotection obtained with pure budesonide. -- Graphical abstract: Silica mesoporous MCM-41 particles were amino-functionalized, loaded with budesonide and post-coated with bioadhesive polymer (carbopol) in order to achieve prolonged residence of anti-inflammatory drug in GIT. Highlights: • Higher drug loading in amino-functionalized mesoporous silica. • Amino-functionalization and post-coating of the nanoparticles sustained drug release. • Achievement of higher cytoprotective effect with drug loaded into the nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2013

Synthesis and characterization of magnetite nanoparticles coated with lauric acid

Understanding the process of synthesis of magnetic nanoparticles is important for its implementation in in vitro and in vivo studies. In this work we report the synthesis of magnetic nanoparticles made from ferrous oxide through coprecipitation chemical process. The nanostructured material was coated with lauric acid and dispersed in aqueous medium containing surfactant that yielded a stable colloidal suspension. The characterization of magnetic nanoparticles with distinct physico-chemical configurations is fundamental for biomedical applications. Therefore magnetic nanoparticles were characterized in terms of their morphology by means of TEM and DLS, which showed a polydispersed set of spherical nanoparticles (average diameter of ca. 9 nm) as a result of the protocol. The structural properties were characterized by using X-ray diffraction (XRD). XRD pattern showed the presence of peaks corresponding to the spinel phase of magnetite (Fe{sub 3}O{sub 4}). The relaxivities r{sub 2} and r{sub 2}* values were determined from the transverse relaxation times T{sub 2} and T{sub 2}* at 3 T. Magnetic characterization was performed using SQUID and FMR, which evidenced the superparamagnetic properties of the nanoparticles. Thermal characterization using DSC showed exothermic events associated with the oxidation of magnetite to maghemite. - Highlights: • Synthesis of magnetic nanoparticles coated with lauric acid • Characterization of magnetic nanoparticles • Morphological, structural, magnetic, calorimetric and relaxometric characterization.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Controlled synthesis of La{sub 1−x}Sr{sub x}CrO{sub 3} nanoparticles by hydrothermal method with nonionic surfactant and their ORR activity in alkaline medium

Graphical abstract: We demonstrate that Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal synthesis method using the nonionic surfactant Triton X-100 and the applicability of La{sub 1−x}Sr{sub x}CrO{sub 3} to oxygen reduction reaction (ORR) electrocatalysis in an alkaline medium. Compared with the nanoparticles synthesized by the coprecipitation method, they showed enhanced ORR activity. - Highlights: • Sr-doped LaCrO{sub 3} nanoparticles were successfully prepared by the hydrothermal method using the nonionic surfactant. • Homogeneously shaped and sized Sr-doped LaCrO{sub 3} nanoparticles were readily obtained. • Compared with the nanoparticles synthesized by the coprecipitation method, they showed an enhanced ORR activity. • The main origin was revealed to be the decreased particle size due to the nonionic surfactant. - Abstract: Sr-doped LaCrO{sub 3} nanoparticles were prepared by the hydrothermal method with the nonionic surfactant Triton X-100 followed by heat treatment at 1000 °C for 10 h. The obtained perovskite nanoparticles had smaller particle size (about 100 nm) and more uniform size distribution than those synthesized by the conventional coprecipitation method. On the other hand, it was identified with the material simulation that the electronic structure change by Sr doping was negligible, because the initially unfilled e{sub g}-band was not affected by the p-type doping. Finally, the perovskite nanoparticles synthesized by hydrothermal method showed much higher ORR activity by over 200% at 0.8 V vs. RHE than those by coprecipitation method.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Preparation, characterization and applications of novel carbon and nitrogen codoped TiO{sub 2} nanoparticles from annealing TiN under CO atmosphere

Graphical abstract: Carbon and nitrogen codoped TiO{sub 2} nanoparticles were firstly fabricated by calcining TiN powder under CO atmosphere at different temperatures between 400 and 600 °C, both the improved photocatalytic activity for degradation of methylene blue and enhanced photovoltaic performance for dye sensitized solar cells were demonstrated. - Highlights: • CN-codoped TiO{sub 2} nanoparticles were prepared by calcining TiN under CO atmosphere. • More visible light response was confirmed by UV–vis DRS and photocatalytic results. • Enhanced conversion efficiency was observed for the DSSCs from CN-TiO{sub 2} photoanode. • CN-codoping played an important role to improve the photocatalytic performance. - Abstract: Carbon and nitrogen codoped titania (CN-TiO{sub 2}) nanoparticles were fabricated by calcining titanium nitride (TiN) nanoparticles under carbon monoxide (CO) atmosphere at four different temperatures in a range of 400–600 °C. The as-prepared samples were characterized with X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and X-ray photoelectron spectroscopy (XPS). Enhanced light absorption in both the UV and visible light region was observed for the resulted CN-TiO{sub 2} nanoparticles in ultraviolet-visible diffuse reflectance spectroscopy (UV–vis DRS). Improved photocatalytic activity toward the degradation of methylene blue by the CN-TiO{sub 2} nanoparticles was demonstrated under UV and visible light, respectively. The highest degradation rate was achieved for CN-TiO{sub 2} nanoparticles (13%) compared to N-TiO{sub 2} (10%) and the commercial P25 (5%) under visible light illumination for 40 min. Furthermore, the improved photocatalytic activity of CN-TiO{sub 2} was also confirmed by the degradation of colorless resorcinol under UV–vis light irradiation. Dye-sensitized solar cells (DSSCs) were fabricated using P25, N-TiO{sub 2} and CN-TiO{sub 2} photoanodes, respectively. The highest conversion efficiency of 3.31% was achieved by the DSSCs based on the CN-TiO{sub 2} photoanodes in comparison with the commercial P25 (1.61%) and N-TiO{sub 2} (2.44%) photoanodes. This work demonstrates that thermal treatment of TiN nanoparticles under CO atmosphere has shown to be a rapid, direct and clean approach to synthesize photocatalysts with enhanced photocatalytic and photovoltaic performance.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Controllable synthesis of hydroxyapatite-supported palladium nanoparticles with enhanced catalytic activity

A multi-stage electrochemical method was developed to synthesize palladium (Pd) nanoparticles supported on hydroxyapatite (HA) coatings. In the first stage, a dense coating of HA nanocrystals was synthesized from an aqueous electrolyte solution onto a titanium cathode surface through a galvanostatic process. The HA-coated titanium electrode was then used as the cathode for the electrochemical reduction of Pd2+ from aqueous solution. A synthesis approach using two sequential electrochemical reduction reactions was found to be more e ective in producing uniform coatings of Pd nanoparticles than a single stage reduction. In the first step, a higher voltage was applied to the cathode for a short time to promote the nucleation of Pd nanoparticles. A lower voltage was then applied for a longer time in the second stage to promote the growth of the Pd nanoparticles. The size and size distribution of the Pd nanoparticles were controlled by adjusting the duration of the first and second stages of electrochemical reduction. The resulting HA supported Pd nanoparticles demonstrated significantly higher catalytic activity than commercial Pd nanoparticles in the degradation of methyl orange by NaBH 4 . The high surface area and the complex oxidation states of the HA-supported Pd nanoparticles are believed to account for the enhanced catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗