scholarly journals Ni Nanoparticles on CeO2 (111): Energetics, Electron Transfer and Structure by Ni Adsorption Calorimetry, Spectroscopies and DFT

2020 ◽  
Author(s):  
Zhongtian Mao ◽  
Pablo Lustemberg ◽  
John R. Rumptz ◽  
M. V. Ganduglia-Pirovano ◽  
Charles T. Campbell
Keyword(s):  
Particle Size ◽  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Density Functional ◽  
Average Particle Size ◽  
Heat Of Adsorption ◽  
Low Energy ◽  
Average Particle ◽  
Adsorption Calorimetry ◽  
Ni Clusters

<div>The morphology, interfacial bonding energetics and charge transfer of Ni clusters and nanoparticles on slightly-reduced CeO<sub>2-x</sub> (111) surfaces at 100 to 300 K have been studied using single crystal adsorption calorimetry (SCAC), low-energy ion scattering spectroscopy (LEIS), X-ray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED) and density functional theory (DFT). The initial heat of adsorption of Ni vapor decreased with the extent of pre-reduction (x) of the CeO<sub>2-x</sub> (111), showing that stoichiometric ceria adsorbs Ni more strongly than oxygen vacancies. On CeO<sub>1.95</sub> (111) at 300 K, the heat dropped quickly with coverage in the first 0.1 ML, attributed to nucleation of Ni clusters on stoichiometric steps, followed by the Ni particles spreading onto less favorable terrace sites. At 100 K, the clusters nucleate on terraces due</div><div>to slower diffusion. Adsorbed Ni monomers are in the +2 oxidation state, and they bind by ~45 kJ/mol more strongly to step sites than terraces. The measured heat of adsorption versus average particle size on terraces is favorably compared to DFT calculations. The Ce 3d XPS lineshape</div><div>showed an increase in Ce<sup>3+</sup>/Ce<sup>4+</sup> ratio with Ni coverage, providing the number of electrons donated to the ceria per Ni atom. The charge transferred per Ni is initially large but strongly decreases with increasing cluster size for both experiments and DFT, and shows large differences between clusters at steps versus terraces. This charge is localized on the interfacial Ni and Ce atoms in their atomic layers closest to the interface. This knowledge is crucial to understanding the nature of the active sites on the surface of Ni-CeO<sub>2</sub> catalysts for which metal-oxide interactions play a very important role in the activation of O−H and C−H bonds. The changes in these interactions with Ni particle size (metal loading) and the extent of reduction of the ceria help to explain how previously reported catalytic activity and selectivity change with these same structural details.</div>

scholarly journals Ni Nanoparticles on CeO2 (111): Energetics, Electron Transfer and Structure by Ni Adsorption Calorimetry, Spectroscopies and DFT

2020 ◽  
Author(s):  
Zhongtian Mao ◽  
Pablo Lustemberg ◽  
John R. Rumptz ◽  
M. V. Ganduglia-Pirovano ◽  
Charles T. Campbell
Keyword(s):  
Particle Size ◽  
Photoelectron Spectroscopy ◽  
Active Sites ◽  
Density Functional ◽  
Average Particle Size ◽  
Heat Of Adsorption ◽  
Low Energy ◽  
Average Particle ◽  
Adsorption Calorimetry ◽  
Ni Clusters

<div>The morphology, interfacial bonding energetics and charge transfer of Ni clusters and nanoparticles on slightly-reduced CeO<sub>2-x</sub> (111) surfaces at 100 to 300 K have been studied using single crystal adsorption calorimetry (SCAC), low-energy ion scattering spectroscopy (LEIS), X-ray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED) and density functional theory (DFT). The initial heat of adsorption of Ni vapor decreased with the extent of pre-reduction (x) of the CeO<sub>2-x</sub> (111), showing that stoichiometric ceria adsorbs Ni more strongly than oxygen vacancies. On CeO<sub>1.95</sub> (111) at 300 K, the heat dropped quickly with coverage in the first 0.1 ML, attributed to nucleation of Ni clusters on stoichiometric steps, followed by the Ni particles spreading onto less favorable terrace sites. At 100 K, the clusters nucleate on terraces due</div><div>to slower diffusion. Adsorbed Ni monomers are in the +2 oxidation state, and they bind by ~45 kJ/mol more strongly to step sites than terraces. The measured heat of adsorption versus average particle size on terraces is favorably compared to DFT calculations. The Ce 3d XPS lineshape</div><div>showed an increase in Ce<sup>3+</sup>/Ce<sup>4+</sup> ratio with Ni coverage, providing the number of electrons donated to the ceria per Ni atom. The charge transferred per Ni is initially large but strongly decreases with increasing cluster size for both experiments and DFT, and shows large differences between clusters at steps versus terraces. This charge is localized on the interfacial Ni and Ce atoms in their atomic layers closest to the interface. This knowledge is crucial to understanding the nature of the active sites on the surface of Ni-CeO<sub>2</sub> catalysts for which metal-oxide interactions play a very important role in the activation of O−H and C−H bonds. The changes in these interactions with Ni particle size (metal loading) and the extent of reduction of the ceria help to explain how previously reported catalytic activity and selectivity change with these same structural details.</div>

Preparation and characterization of anatase N–F-codoped TiO2 sol and its photocatalytic degradation for formaldehyde

2007 ◽  
Vol 22 (9) ◽  
pp. 2389-2397 ◽  
Author(s):  
Donggen Huang ◽  
Shijun Liao ◽  
Shuiqing Quan ◽  
Lei Liu ◽  
Zongjian He ◽  
...  
Keyword(s):  
Particle Size ◽  
Visible Light ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
Average Particle Size ◽  
Synergetic Effect ◽  
Tetrabutyl Titanate ◽  
Average Particle ◽  
Dielectric Relaxation Spectroscopy ◽  
X Ray

Anatase nitrogen and fluoride codoped TiO2 sol (N–F–TiO2) catalysts were fabricated by a modified sol-gel hydrothermal method, using tetrabutyl titanate as precursor. The microstructure and morphology of sol sample were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible dielectric relaxation spectroscopy (UV-VIS-DRS), x-ray photoelectron spectroscopy (XPS), etc. It was shown that N–F–TiO2 particles in sol were partly crystallized to anatase structure and dispersed in the aqueous medium homogeneously. The average particle size was ∼12.0 nm calculated from XRD patterns, and the particle size distribution was narrow. It was noteworthy that the N–F-codoped TiO2 sol particles showed strong visible-light response and high photocatalytic activity for formaldehyde degradation under irradiation by visible light (400–500 nm); we suggested that it may result from the generation of additional band of N 2p in the forbidden band and the synergetic effect of codoping nitrogen and fluorine.

scholarly journals Continuous synthesis of TiO2-supported noble metal NPs and their application in ammonia borane hydrolysis

2021 ◽  
Author(s):  
Lamei Luo ◽  
Mei Yang ◽  
Guangwen Chen
Keyword(s):  
Particle Size ◽  
Metal Nanoparticles ◽  
Noble Metal ◽  
Active Sites ◽  
Average Particle Size ◽  
Ammonia Borane ◽  
Noble Metal Nanoparticles ◽  
Average Particle ◽  
Batch Method ◽  
Continuous Synthesis

A stabilizer-free method based on segmented flow for the continuous synthesis of TiO2 supported noble metal nanoparticles (M/TiO2-MR, M = Pd, Pt or Au) was proposed. Due to the enhanced mixing performance arising from the internal convection in the discrete plugs, the particle size of noble metal nanoparticles could be well controlled by reducing the metal precursors with NaBH4 just in the presence of TiO2 without using any stabilizer. In comparison with the batch method, the as-prepared M/TiO2-MR had smaller noble metal particle size and better dispersity. Experimental results showed that adjusting the oil-to-water phase ratio or increasing the total volume flow rate and synthetic temperature could lead to smaller average particle size with narrower distribution. The as-prepared M/TiO2-MR possessed higher catalytic activities in the hydrolysis of ammonia borane than those prepared by the batch method, which could be ascribed to smaller noble metal nanoparticles, exposing more active sites.

scholarly journals Characterization of Magnetic Nanoparticles Coated with Chitosan: A Potential Approach for Enzyme Immobilization

2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Azariel Díaz-Hernández ◽  
Jorge Gracida ◽  
Blanca E. García-Almendárez ◽  
Carlos Regalado ◽  
Rosario Núñez ◽  
...  
Keyword(s):  
Particle Size ◽  
Magnetic Nanoparticles ◽  
Size Distribution ◽  
Photoelectron Spectroscopy ◽  
Average Particle Size ◽  
Superparamagnetic Nanoparticles ◽  
Spherical Particles ◽  
Cross Linking ◽  
Average Particle ◽  
X Ray

Cross-linking of magnetic nanoparticles with proteins plays a significant role in the preparation of new materials for biotechnological applications. The aim was the maximization of the magnetic mass attracted and protein loading of magnetic iron oxide nanoparticles coated with chitosan, synthesized in a single step by alkaline precipitation. Chitosan-coated magnetite particles (Fe3O4@Chitosan) were cross-linked to a xylanase and a cellulase (Fe3O4@Chitosan@Proteins), showing a 93% of the magnetic saturation of the magnetite. X-ray diffraction pattern in composites corresponds to magnetite. Thermogravimetry and differential scanning calorimetry showed that 162 mg of chitosan was coating one gram of composite and 12 mg of protein was cross-linked to each gram of magnetic support. Cross-linking between enzymes and Fe3O4@Chitosan was confirmed by infrared spectroscopy with Fourier transform, X-ray energy, and X-ray photoelectron spectroscopy dispersion analysis. From dynamic light scattering, transmission and electron microscopy the average particle size distribution was 230 nm and 430 nm for Fe3O4@Chitosan and Fe3O4@Chitosan@Proteins, showing agglomerates of individual spherical particles, with an average diameter of 8.5 nm and 10.8 nm, respectively. The preparation method plays a key role in determining the particle size and shape, size distribution, surface chemistry, and, therefore, the applications of the superparamagnetic nanoparticles.

Determination of grinding parameters of fenugreek seed

1970 ◽  
Vol 26 (1) ◽  
pp. 16 ◽  
Author(s):  
S Balasubramanian ◽  
Rajkumar Rajkumar ◽  
K K Singh
Keyword(s):  
Particle Size ◽  
Energy Consumption ◽  
Moisture Content ◽  
Specific Energy ◽  
Feed Rate ◽  
Average Particle Size ◽  
Specific Energy Consumption ◽  
Average Particle ◽  
Fenugreek Seeds ◽  
Fenugreek Seed

Experiment to identify ambient grinding conditions and energy consumed was conducted for fenugreek. Fenugreek seeds at three moisture content (5.1%, 11.5% and 17.3%, d.b.) were ground using a micro pulverizer hammer mill with different grinding screen openings (0.5, 1.0 and 1.5 mm) and feed rate (8, 16 and 24 kg h-1) at 3000 rpm. Physical properties of fenugreek seeds were also determined. Specific energy consumptions were found to decrease from 204.67 to 23.09 kJ kg-1 for increasing levels of feed rate and grinder screen openings. On the other hand specific energy consumption increased with increasing moisture content. The highest specific energy consumption was recorded for 17.3% moisture content and 8 kg h-1 feed rate with 0.5 mm screen opening. Average particle size decreased from 1.06 to 0.39 mm with increase of moisture content and grinder screen opening. It has been observed that the average particle size was minimum at 0.5 mm screen opening and 8 kg h-1 feed rate at lower moisture content. Bond’s work index and Kick’s constant were found to increase from 8.97 to 950.92 kWh kg-1 and 0.932 to 78.851 kWh kg-1 with the increase of moisture content, feed rate and grinder screen opening, respectively. Size reduction ratio and grinding effectiveness of fenugreek seed were found to decrease from 4.11 to 1.61 and 0.0118 to 0.0018 with the increase of moisture content, feed rate and grinder screen opening, respectively. The loose and compact bulk densities varied from 219.2 to 719.4 kg m-3 and 137.3 to 736.2 kg m-3, respectively.  

Formulating SLN and NLC as Innovative Drug Delivery Systems for Non-Invasive Routes of Drug Administration

2020 ◽  
Vol 27 (22) ◽  
pp. 3623-3656 ◽  
Author(s):  
Bruno Fonseca-Santos ◽  
Patrícia Bento Silva ◽  
Roberta Balansin Rigon ◽  
Mariana Rillo Sato ◽  
Marlus Chorilli
Keyword(s):  
Drug Delivery ◽  
Particle Size ◽  
Drug Release ◽  
Drug Loading ◽  
Average Particle Size ◽  
Delivery Systems ◽  
Average Particle ◽  
Minor Importance ◽  
Routes Of Administration ◽  
Non Invasive

Colloidal carriers diverge depending on their composition, ability to incorporate drugs and applicability, but the common feature is the small average particle size. Among the carriers with the potential nanostructured drug delivery application there are SLN and NLC. These nanostructured systems consist of complex lipids and highly purified mixtures of glycerides having varying particle size. Also, these systems have shown physical stability, protection capacity of unstable drugs, release control ability, excellent tolerability, possibility of vectorization, and no reported production problems related to large-scale. Several production procedures can be applied to achieve high association efficiency between the bioactive and the carrier, depending on the physicochemical properties of both, as well as on the production procedure applied. The whole set of unique advantages such as enhanced drug loading capacity, prevention of drug expulsion, leads to more flexibility for modulation of drug release and makes Lipid-based nanocarriers (LNCs) versatile delivery system for various routes of administration. The route of administration has a significant impact on the therapeutic outcome of a drug. Thus, the non-invasive routes, which were of minor importance as parts of drug delivery in the past, have assumed added importance drugs, proteins, peptides and biopharmaceuticals drug delivery and these include nasal, buccal, vaginal and transdermal routes. The objective of this paper is to present the state of the art concerning the application of the lipid nanocarriers designated for non-invasive routes of administration. In this manner, this review presents an innovative technological platform to develop nanostructured delivery systems with great versatility of application in non-invasive routes of administration and targeting drug release.

Azithromycin nanosuspension preparation using evaporative precipitation into aqueous solution (EPAS) method and its comparative dissolution study

2020 ◽  
Vol 17 ◽  
Author(s):  
Mohammad Hossain Shariare ◽  
Tonmoy Kumar Mondal ◽  
Hani Alothaid ◽  
Md. Didaruzzaman Sohel ◽  
MD Wadud ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Particle Size ◽  
Dissolution Rate ◽  
Average Particle Size ◽  
Scale Up ◽  
Average Particle ◽  
Total Drug ◽  
Residual Solvent ◽  
Dissolution Study ◽  
Drug Content

Aim: EPAS (evaporative precipitation into aqueous solution) was used in the current studies to prepare azithromycin nanosuspensions and investigate the physicochemical characteristics for the nanosuspension batches with the aim of enhancing the dissolution rate of the nanopreparation to improve bioavailability. Methods: EPAS method used in this study for preparing azithromycin nanosuspension was achieved through developing an in-house instrumentation method. Particle size distribution was measured using Zetasizer Nano S without sample dilution. Dissolved azithromycin nanosuspensions were also compared with raw azithromycin powder and commercially available products. Total drug content of nanosuspension batches were measured using an Ultra-Performance Liquid Chromatography (UPLC) system with Photodiode Array (PDA) detector while residual solvent was measured using gas chromatography (GC). Results: The average particle size of azithromycin nanosuspension was 447.2 nm and total drug content was measured to be 97.81% upon recovery. Dissolution study data showed significant increase in dissolution rate for nanosuspension batch when compared to raw azithromycin and commercial version (microsuspension). The residual solvent found for azithromycin nanosuspension is 0.000098023 mg/ mL or 98.023 ppb. Conclusion: EPAS was successfully used to prepare azithromycin nanoparticles that exhibited significantly enhanced dissolution rate. Further studies are required to scale up the process and determine long term stability of the nanoparticles.

scholarly journals Evaluation of the Effects of Filler Fineness on the Properties of an Epoxy Asphalt Mixture

Materials ◽  
2021 ◽  
Vol 14 (8) ◽  
pp. 2003
Author(s):  
Wei Xu ◽  
Jintao Wei ◽  
Zhengxiong Chen ◽  
Feng Wang ◽  
Jian Zhao
Keyword(s):  
Particle Size ◽  
Average Particle Size ◽  
Asphalt Mixture ◽  
Average Particle ◽  
Fine Dust ◽  
Bonding Structure ◽  
Epoxy Asphalt ◽  
Mineral Powder ◽  
Marshall Stability ◽  
Mixture Sample

The type and fineness of a filler significantly affect the performance of an asphalt mixture. There is a lack of specific research on the effects of filler fineness and dust from aggregates on the properties of epoxy asphalt (EA) mixtures. The effects of aggregate dust and mineral powder on the properties of an EA mixture were evaluated. These filler were tested to determine their fineness, specific surface area and mineral composition. The effects of these fillers on the EA mastic sample and mixture were evaluated. The morphology of the EA mastic samples was analyzed using scanning electron microscopy (SEM). The effects of the fillers on the Marshall stability, tensile strength and fatigue performance of the EA mixture were evaluated. The dust from the aggregates exhibited an even particle size distribution, and its average particle size was approximately 20% of that of the mineral powder. The SEM microanalysis showed that the EA mastic sample containing relatively fine dust formed a tight and dense interfacial bonding structure with the aggregate. The EA mixture sample containing filler composed of dust from aggregate had a significantly higher strength and longer fatigue life than that of the EA sample containing filler composed of mineral powder.

scholarly journals Surface Activity of Humic Acid and Its Sub-Fractions from Forest Soil

2021 ◽  
Vol 13 (15) ◽  
pp. 8122
Author(s):  
Shijie Tian ◽  
Weiqiang Tan ◽  
Xinyuan Wang ◽  
Tingting Li ◽  
Fanhao Song ◽  
...  
Keyword(s):  
Surface Tension ◽  
Particle Size ◽  
Humic Acid ◽  
Forest Soil ◽  
Surface Activity ◽  
Self Assembly ◽  
Average Particle Size ◽  
Gaussian Model ◽  
Exponential Model ◽  
Average Particle

Surface activity of humic acid (HA) and its six sub-fractions isolated from forest soil were characterized by surface tension measurements, dynamic light scattering, and laser doppler electrophoresis. The surface tension of HA and its sub-fractions reduced from 72.4 mN·m−1 to 36.8 mN·m−1 in exponential model with the increasing concentration from 0 to 2000 mg·L−1. The critical micelle concentration (CMC) and Z-average particle size ranged from 216–1024 mg·L−1 and 108.2–186.9 nm for HA and its sub-fractions, respectively. The CMC have related with alkyl C, O-alkyl C, aromatic C, and carbonyl C (p < 0.05), respectively, and could be predicted with the multiple linear regression equation of CMC, CMC = 18896 − 6.9 × C-296 × alkyl C-331 × aromatic C-17019 × H/C + 4054 × HB/HI (p < 0.05). The maximum particle size was 5000 nm after filtered by a membrane with pore size of 450 nm, indicating HA and its sub-fractions could progressed self-assembly at pH 6.86. The aggregate sizes of number-base particle size distributions were mainly in six clusters including 2 ± 1 nm, 5 ± 2 nm, 10 ± 3 nm, 21 ± 8 nm, 40 ± 10 nm, and >50 nm analyzed by Gaussian model that maybe due to the inconsistency of the components and structures of the HA sub-fractions, requiring further study. It is significance to explore the surface activity of HA and its sub-fractions, which is helpful to clarify the environmental behavior of HA.

Microstructure Characterization of Ag Nanoparticles Prepared by Hydrothermal Method

2012 ◽  
Vol 476-478 ◽  
pp. 1138-1141
Author(s):  
Zhi Qiang Wei ◽  
Qiang Wei ◽  
Li Gang Liu ◽  
Hua Yang ◽  
Xiao Juan Wu
Keyword(s):  
Crystal Structure ◽  
Particle Size ◽  
Hydrothermal Method ◽  
Ag Nanoparticles ◽  
Average Particle Size ◽  
Average Particle ◽  
Face Centered Cubic ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Face Centered

Ag nanoparticles were successfully synthesized by hydrothermal method under the polyol system combined with traces of sodium chloride, Silver nitrate(AgNO3) and polyvinylpyrrolidone (PVP) acted as the silver source and dispersant respectively. The samples by this process were characterized via X-ray powder diffraction (XRD), Brunauer–Emmett–Teller (BET) adsorption equation, transmission electron microscopy (TEM) and the corresponding selected area electron diffraction (SAED) to determine the chemical composition, particle size, crystal structure and morphology. The experiment results indicate that the crystal structure of the samples is face centered cubic (FCC) structure as same as the bulk materials, The specific surface area is 24 m2/g, the particle size distribution ranging from10 to 50 nm, with an average particle size about 26 nm obtained by TEM and confirmed by XRD and BET results.

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