Wüstite nanocrystals: Synthesis, structure and superlattice formation

2007 ◽  
Vol 22 (7) ◽  
pp. 1987-1995 ◽  
Author(s):  
Ming Yin ◽  
Zhuoying Chen ◽  
Brian Deegan ◽  
Stephen O’Brien
Keyword(s):  
Self Assembly ◽  
Three Dimensional ◽  
Size Control ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Salt Crystal ◽  
Uniform Size ◽  
Nonpolar Solvents ◽  
Transmission Electron ◽  
State Kinetic

Monodisperse ligand-capped cubic wüstite FexO nanocrystals were prepared by a novel thermal decomposition method of iron (II) acetate in the presence of oleic acid as the surfactant. Controlled size distributions of cubic nanoparticles possessing the rock salt crystal structure were isolated in the range 10–18 nm. The influence of molar ratio of surfactant to precursor was investigated to understand size control and monodispersity. Using inexpensive, nontoxic metal salts as reactants, we were able to synthesize gram-scale quantities of relatively monodisperse nanocrystals in a single reaction, without further size selection, characterized by x-ray diffraction and transmission electron microscopy. The procedure enables the collection of samples of uniform size as a function of time, thus permitting a preliminary solid-state kinetic analysis of the reaction as a function of increasing particle size. Following controlled evaporation from nonpolar solvents, self-assembly into two-dimensional arrays, three-dimensional single-component superlattices, and binary superlattices with gold nanoparticles were observed and characterized.

scholarly journals Synthesis of Dandelion-like Porous Au Nanoparticles for Catalytic Reduction of Nitrophenol

2020 ◽  
Vol 01 ◽  
Author(s):  
Huiying Wu ◽  
Feng Liang
Keyword(s):  
Active Sites ◽  
Au Nanoparticles ◽  
Catalytic Reduction ◽  
Molar Ratio ◽  
Void Space ◽  
X Ray Diffraction ◽  
Uniform Size ◽  
Templating Method ◽  
X Ray ◽  
Transmission Electron

Background: Porous Au nanomaterials show great potential in the fields of biomedicine, drug delivery and catalysis for the merits of low density, large void space and large specific surface area. The preparation of porous Au nanomaterials is usually carried out by using a hard-templating method which is cumbersome. Methods: Dandelion-like porous Au nanoparticles were synthesized through a soft-templating method in our work. The synthesized porous Au nanoparticles were characterized via transmission electron microscopy (TEM), X-ray diffraction (XRD), energy-dispersive X-ray (EDX) and cyclic voltammetry (CV). The reduction of nitrophenol was carried out to evaluate the catalytic behavior of porous Au nanoparticles. Results: Porous Au nanoparticles prepared were in uniform size (47.9±6.4 nm) and the morphology could be regulated by adjusting the molar ratio of reactants. The apparent rate constant (kapp) value of reducing nitrophenol catalyzed by porous Au nanoparticles was higher than Au nanospheres and nanobranches in similar size. It could be attributed to the large amount of active sites and high proportion of high-order crystal faces proved by CV and XRD. Conclusion: We developed a facile and reproducible method for synthesizing porous Au nanoparticles. The morphology of porous Au nanoparticles can be ajusted by changing the molar ratio of reactants. Porous Au nanoparticles we prepared behaved better in catalysis compared with Au nanospheres and Au nanobranches.

scholarly journals ZnO/ZnAl2O4 Nanocomposite with 3D Sphere-Like Hierarchical Structure for Photocatalytic Reduction of Aqueous Cr(VI)

Materials ◽  
2018 ◽  
Vol 11 (9) ◽  
pp. 1624 ◽  
Author(s):  
Xiaoya Yuan ◽  
Xin Cheng ◽  
Qiuye Jing ◽  
Jiawei Niu ◽  
Dong Peng ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Diffuse Reflectance Spectroscopy ◽  
Uv Light ◽  
Hydrothermal Process ◽  
Three Dimensional ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Transmission Electron ◽  
Excellent Photocatalytic Activity ◽  
Potential Applications

Three dimensional (3D) ZnO/ZnAl2O4 nanocomposites (ZnnAl-MMO) were synthesized by a simple urea-assisted hydrothermal process and subsequent high-temperature calcination. The as-prepared samples and their precursors were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectroscopy (DRS), and Photoluminescence spectra (PL). It was observed that the morphology of ZnnAl-MMO nanocomposites could be tuned from cubic aggregates, hierarchically flower-like spheres to porous microspheres by simply changing the molar ratio of metal cations of the starting reaction mixtures. The photocatalytic performance of ZnO/ZnAl2O4 nanocomposites in the photoreduction of aqueous Cr(VI) indicated that the as-prepared 3D hierarchical sphere-like ZnnAl-MMO nanocomposite showed excellent photocatalytic activity of Cr(VI) reduction under UV light irradiation. The results indicated that the maximum removal percentage of aqueous Cr(VI) was 98% within four hours at 10 mg/L initial concentration of Cr(VI), owing to the effective charge separation and diversion of photogenerated carriers across the heterojunction interface of the composite. Our study put forward a facile method to fabricate hierarchical ZnO/ZnAl2O4 composites with potential applications for wastewater treatment.

scholarly journals Influence of Capping Groups on the Synthesis of γ-Fe2O3 Nanocrystals

2004 ◽  
Vol 19 (4) ◽  
pp. 1208-1215 ◽  
Author(s):  
Ming Yin ◽  
Amanda Willis ◽  
Franz Redl ◽  
Nicholas J. Turro ◽  
Stephen P. O’Brien
Keyword(s):  
Self Assembly ◽  
Carbon Chain ◽  
Iron Pentacarbonyl ◽  
Decomposition Temperature ◽  
Molar Ratio ◽  
Molar Ratios ◽  
Nonpolar Solvents ◽  
Transmission Electron ◽  
Iron Precursor ◽  
Chain Lengths

Monodisperse and uniform γ-Fe2O3 (maghemite) nanocrystals of variable size were prepared by thermal decomposition of iron pentacarbonyl [Fe(CO)5] in the presence of surfactants, following controlled oxidation with trimethylamine N-oxide as a mild oxidant. The influence of carboxylic acids with variable alkyl carbon chain lengths on the synthesis of γ-Fe2O3 nanocrystals was investigated. The effect of the molar ratios of surfactant to iron precursor was also studied. The nanocrystals were characterized by x-ray diffraction (XRD) and transmission electron microscopy (TEM). XRD showed the particles were highly crystalline at the nanometer scale. The results showed that the size and shape of the nanocrystal is strongly influenced by the decomposition temperature of iron pentacarbonyl and closely related to the length of carbon chain of the capping groups and the molar ratio of surfactant to iron precursor. Following controlled evaporation from nonpolar solvents, self-assembly into two-dimensional arrays could be observed by TEM. It was also found that the distance between the nanocrystals in self-assembled structures matched the length of the capping molecules very well.

Tayloring the Photocatalytical Activity of Anatase TiO2 Thin Film Electrodes by Three-Dimensional Mesoporosity

2010 ◽  
Vol 162 ◽  
pp. 91-113 ◽  
Author(s):  
Bernhard Neumann ◽  
Thorsten Brezesinsky ◽  
Bernd Smarsly ◽  
Helmut Tributsch
Keyword(s):  
Thin Film ◽  
Self Assembly ◽  
Three Dimensional ◽  
Great Influence ◽  
X Ray Diffraction ◽  
Porous Films ◽  
X Ray ◽  
Transmission Electron ◽  
Evaporation Induced Self Assembly ◽  
Thin Film Electrodes

Mesoporous titanium dioxide (m-TiO2) thin film electrodes were synthesized by evaporation-induced self-assembly (EISA), utilizing a novel type of amphiphilic block copolymer as template. The ordered network of pores shows an accessible inner volume that results in a huge BET-surface and a distinct transparency. According to X-ray diffraction analyses the mesoporous films are highly crystalline after calcination at 550°C. 1D and 2D small-angle X-ray scattering and transmission electron microscopy investigations prove the high quality of the mesopore texture over micrometer-sized areas. These well-defined, crystalline m-TiO2 films show an increased photoactivity for overall water splitting and oxidation of formic acid as compared to porous films prepared in the same manner without a template. The performance of the electrodes was analyzed by measuring the photocurrent and the mass signal of liberated gas by electrochemical mass spectroscopy (EMS). These experiments reveal that film morphology have a great influence to the I-V characteristic of photoelectrodes. An appropriate crystallization temperature is indispensable to obtain an optimum between crystallinity, morphology and photoactivity and to prevent collapse of the mesopore architecture.

Fabrication of Scattering Spheres-Embedding Three-Dimensional Ordered Macroporous Titania and Application in Dye-Sensitized Photoanode

2012 ◽  
Vol 554-556 ◽  
pp. 395-398 ◽  
Author(s):  
Cheng An Tao ◽  
Jian Fang Wang ◽  
Yin Long ◽  
Ya Nan Lv ◽  
Guang Tao Li
Keyword(s):  
Self Assembly ◽  
Colloidal Crystal ◽  
Three Dimensional ◽  
Solid Material ◽  
X Ray Diffraction ◽  
Colloidal Spheres ◽  
Nanoparticle Dispersions ◽  
Transmission Electron ◽  
Colloidal Crystal Template ◽  
Ordered Macroporous

Scattering spheres-embedding three-dimensional ordered macroporous (3DOM) titania(TiO2) was fabricated, by the route of colloidal spheres self-assembly, infiltration and template removal. The procedures of 3DOM structure preparation were characterized by transmission electron microscope (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD). The silica@PMMA core-shell spheres were prepared and self-assembled into colloidal crystal template. Solid material was deposited in the colloidal crystal template by spin-coating of titania nanoparticle dispersions. Subsequently, the samples were heated to 400 °C to form anatase TiO2and to remove the polymer of template, which resulted in macroporous structure with a silica sphere in each lattice pore. The conventional TiO2film, 3DOM TiO2photoanodes were also fabricated. It was found that SiO2-embedding 3DOM photoanode has the higher photocurrent efficiency than both of TiO2 film and 3DOM, because there are scattering spheres in its lattice pores which enhance the light scattering and improve the light harvest of the dye.

scholarly journals Size Control of Synthesized Silver Nanoparticles by Simultaneous Chemical Reduction and Laser Fragmentation in Origanum majorana Extract: Antibacterial Application

Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2326
Author(s):  
Entesar Ali Ganash ◽  
Reem Mohammad Altuwirqi
Keyword(s):  
Silver Nanoparticles ◽  
Irradiation Time ◽  
Chemical Reduction ◽  
Size Control ◽  
Reduction Process ◽  
Laser Wavelength ◽  
X Ray Diffraction ◽  
Ag Nps ◽  
Transmission Electron ◽  
Origanum Majorana

In this work, silver nanoparticles (Ag NPs) were synthesized using a chemical reduction approach and a pulsed laser fragmentation in liquid (PLFL) technique, simultaneously. A laser wavelength of 532 nm was focused on the as produced Ag NPs, suspended in an Origanum majorana extract solution, with the aim of controlling their size. The effect of liquid medium concentration and irradiation time on the properties of the fabricated NPs was studied. While the X-ray diffraction (XRD) pattern confirmed the existence of Ag NPs, the UV–Vis spectrophotometry showed a significant absorption peak at about 420 nm, which is attributed to the characteristic surface plasmon resonance (SPR) peak of the obtained Ag NPs. By increasing the irradiation time and the Origanum majora extract concentration, the SPR peak shifted toward a shorter wavelength. This shift indicates a reduction in the NPs’ size. The effect of PLFL on size reduction was clearly revealed from the transmission electron microscopy images. The PLFL technique, depending on experimental parameters, reduced the size of the obtained Ag NPs to less than 10 nm. The mean zeta potential of the fabricated Ag NPs was found to be greater than −30 mV, signifying their stability. The Ag NPs were also found to effectively inhibit bacterial activity. The PLFL technique has proved to be a powerful method for controlling the size of NPs when it is simultaneously associated with a chemical reduction process.

Self Assembling Nanostructured Delivery Vehicles for Biochemically Reactive Pairs

1994 ◽  
Vol 351 ◽  
Author(s):  
Nir Kossovsky ◽  
A. Gelman ◽  
H.J. Hnatyszyn ◽  
E. Sponsler ◽  
G.-M. Chow
Keyword(s):  
Physical Properties ◽  
Self Assembly ◽  
Materials Science ◽  
Technology Development ◽  
Biological Behavior ◽  
X Ray Diffraction ◽  
Self Assembling ◽  
Transmission Electron ◽  
Carbon Ceramic

ABSTRACTIntrigued by the deceptive simplicity and beauty of macromolecular self-assembly, our laboratory began studying models of self-assembly using solids, glasses, and colloidal substrates. These studies have defined a fundamental new colloidal material for supporting members of a biochemically reactive pair.The technology, a molecular transportation assembly, is based on preformed carbon ceramic nanoparticles and self assembled calcium-phosphate dihydrate particles to which glassy carbohydrates are then applied as a nanometer thick surface coating. This carbohydrate coated core functions as a dehydroprotectant and stabilizes surface immobilized members of a biochemically reactive pair. The final product, therefore, consists of three layers. The core is comprised of the ceramic, the second layer is the dehydroprotectant carbohydrate adhesive, and the surface layer is the biochemically reactive molecule for which delivery is desired.We have characterized many of the physical properties of this system and have evaluated the utility of this delivery technology in vitro and in animal models. Physical characterization has included standard and high resolution transmission electron microscopy, electron and x-ray diffraction and ζ potential analysis. Functional assays of the ability of the system to act as a nanoscale dehydroprotecting delivery vehicle have been performed on viral antigens, hemoglobin, and insulin. By all measures at present, the favorable physical properties and biological behavior of the molecular transportation assembly point to an exciting new interdisciplinary area of technology development in materials science, chemistry and biology.

Solvothermal Synthesis of Bi2Se3 Hexagonal Nanosheet Crystals

2011 ◽  
Vol 236-238 ◽  
pp. 1712-1716 ◽  
Author(s):  
Hai Tao Liu ◽  
Jun Dai ◽  
Jia Jia Zhang ◽  
Wei Dong Xiang
Keyword(s):  
Electron Microscope ◽  
Solvothermal Synthesis ◽  
Solvothermal Method ◽  
Raw Materials ◽  
X Ray Diffraction ◽  
Uniform Size ◽  
X Ray ◽  
Selected Area Electron Diffraction ◽  
Transmission Electron ◽  
Scanning Electron

Bismuth selenide (Bi2Se3) hexagonal nanosheet crystals with uniform size were successfully prepared via a solvothermal method at 160°C for 22 h using bismuth trichloride(BiCl3) and selenium powder(Se) as raw materials, sodium bisulfite(NaHSO3) as a reducing agent, diethylene glycol(DEG) as solvent, and ammonia as pH regulator. Various techniques such as X-ray diffraction (XRD), field-emission scanning electron microscope (FESEM), high-resolution transmission electron microscope (HRTEM), and selected area electron diffraction (SAED) were used to characterize the obtained products. Results show that the as-synthesized samples are pure Bi2Se3 hexagonal nanosheet crystals. A possible growth mechanism for Bi2Se3 hexagonal nanosheet crystals is also discussed based on the experiment.

scholarly journals Synthesis of Three-Dimensional Fe3O4/Graphene Aerogels for the Removal of Arsenic Ions from Water

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Yan Ye ◽  
Da Yin ◽  
Bin Wang ◽  
Qingwen Zhang
Keyword(s):  
Electron Microscopy ◽  
Photoelectron Spectroscopy ◽  
3D Structure ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
X Ray ◽  
Graphene Aerogels ◽  
Transmission Electron ◽  
Potential Applications ◽  
Removal Of Arsenic

We report the synthesis of three-dimensional Fe3O4/graphene aerogels (GAs) and their application for the removal of arsenic (As) ions from water. The morphology and properties of Fe3O4/GAs have been characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and superconducting quantum inference device. The 3D nanostructure shows that iron oxide nanoparticles are decorated on graphene with an interconnected network structure. It is found that Fe3O4/GAs own a capacity of As(V) ions adsorption up to 40.048 mg/g due to their remarkable 3D structure and existence of magnetic Fe3O4nanoparticles for separation. The adsorption isotherm matches well with the Langmuir model and kinetic analysis suggests that the adsorption process is pseudo-second-ordered. In addition to the excellent adsorption capability, Fe3O4/GAs can be easily and effectively separated from water, indicating potential applications in water treatment.

Immobilization of K7PW11O39 on ZrO2 Nanofiber: Ultra-deep Desulfurization Based in Extraction Catalytic Oxidation Desulfurization System

2021 ◽  
Vol 72 (3) ◽  
pp. 89-101
Author(s):  
Guowei Zeng ◽  
Guihong Wu ◽  
Zhihui Wang ◽  
Xiaonan Li ◽  
Jie Yang ◽  
...  
Keyword(s):  
Catalytic Oxidation ◽  
Catalytic Mechanism ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Thermo Gravimetric ◽  
Transmission Electron ◽  
Deep Desulfurization ◽  
Thermo Gravimetric Analyzer ◽  
Ft Ir ◽  
Model Oil

In this work, K7PW11O39 (abbreviated as PW11) was immobilized on ZrO2 nanofibers and used as an efficient recyclable catalyst in extraction catalytic oxidation desulfurization system (ECODS).The 500 ppm DBT model oil(5mL) can desulphurize completely within 20 min with the catalytic conditions of 50��, 0.010 g 50 wt%- CTAB�C PW11�CZrO2 nanofibers and O/S molar ratio H2O2/DBT molar ratio�� was 2:1. The synthesized catalyst was characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS) and thermo gravimetric analyzer (TGA). The results indicated the PW11�CZrO2 nanofibers were synthesized successfully and the possible catalytic mechanism is also revealed.

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