Plate-like Nanocrystals Research Articles

Characterization of an advanced bone graft material with a nanocrystalline hydroxycarbanoapatite surface and dual phase composition.

The bone formation response of ceramic bone graft materials can be improved by modifying the material's surface and composition. A unique dual-phase ceramic bone graft material with a nanocrystalline, hydroxycarbanoapatite (HCA) surface and a calcium carbonate core (TrelCor®-Biogennix, Irvine, CA) was characterized through a variety of analytical methods. Scanning electron microscopy (SEM) of the TrelCor surface (magnification 100-100,000X) clearly demonstrated a nanosized crystalline structure covering the entire surface. The surface morphology showed a hierarchical structure that included micron-sized spherulites fully covered by plate-like nanocrystals (<60 nm in thickness). Chemical and physical characterization of the material using X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), and Scanning Electron Microscopy Energy Dispersive X-ray Spectroscopy (SEM-EDX) showed a surface composed of HCA. Analysis of fractured samples confirmed the dual-phase composition with the presence of a calcium carbonate core and HCA surface. An in vitro bioactivity study was conducted to evaluate whether TrelCor would form a bioactive layer when immersed in simulated body fluid. This response was compared to a known bioactive material (45S5 bioactive glass - Bioglass). Following 14-days of immersion, surface and cross-sectional analysis via SEM-EDX showed that the TrelCor material elicited a bioactive response with the formation of a bioactive layer that was qualitatively thicker than the layer that formed on Bioglass. An in vivo sheep muscle pouch model was also conducted to evaluate the ability of the material to stimulate an ectopic, cellular bone formation response. Results were compared against Bioglass and a first-generation calcium phosphate ceramic that lacked a nanocrystalline surface. Histology and histomorphometric analysis (HMA) confirmed that the TrelCor nanocrystalline HCA surface stimulated a bone formation response in muscle (avg. 11% bone area) that was significantly greater than Bioglass (3%) and the smooth surface calcium phosphate ceramic (0%).

Anti-Alzheimer Drug Delivery via Pickering Emulsions Stabilized by Plate-like Cellulose Nanocrystals.

In this work, we studied for the first time the formation of olive oil emulsions in water stabilized by plate-like nanocrystals with the supramolecular structure of cellulose II (pCNC). Effects of storage, pCNC concentration, and NaCl on the stability and properties of Pickering emulsions, including the creaming index, droplet size, zeta potential, acid-base surface properties, and rheology, were studied. A significant influence of the shape of nanoparticles (compared to the classical rod-like shape) on the stability parameters and rheological characteristics of emulsions is shown. Plate-like cellulose nanocrystals at a concentration of 16 g/L are able to form delamination-resistant emulsions without added electrolytes. The viscosity of pCNC-stabilized emulsions tends to decrease with increasing electrolyte concentration in the system, which is not characteristic of rod-like CNC-stabilized emulsions. This effect in pCNC-stabilized emulsions assumedly can be associated both with weak mechanical engagement between drops due to the shape of stabilizer particles and with an insignificant participation of background electrolyte cations in the formation of interdroplet interactions. Therefore, the resulting aggregates are unstable and easily destroyed, even under weak mechanical stress. As a consequence, the acid-base properties of the pCNC surface are practically independent of the emulsion preparation method (with or without electrolyte) as well as the concentration of the background electrolyte. The reduced viscosity of pCNC-stabilized emulsions in the presence of an electrolyte, coupled with the absence of acute toxicity, allows us to recommend them as a convenient oral delivery system for fat-soluble, biologically active substances. Our emulsions carrying donepezil (an anti-Alzheimer drug) showed better performance than a solution of donepezil hydrochloride in preventing memory impairment tested on laboratory mice.

Regaining enamel color quality using enamel matrix derivative

This study aimed to demonstrate and compare the accuracy of tooth shade selection due to the remineralized enamel crystal with enamel matrix derivative (EMD) in vitro. Etched enamel slices were immersed in four types of mineralization buffers for 16 h. Sodium fluoride (NaF) was added to final concentrations of 1–100 ppm with the mineralization buffer that demonstrated the highest mineralization efficiency. EMD was added to the mineralization buffer containing NaF to see if it has any remineralization capacities. The remineralized enamel crystal was analyzed by SEM and XRD. The tooth shade was evaluated by CIE L*a*b*. The results showed that, without NaF, plate-like nanocrystals were formed on the enamel surface, but with NaF, needle-like nanocrystals were formed. By adding EMD, a layer of well-compacted hydroxyapatite crystals was successfully precipitated onto the natural enamel surface. No significant differences were observed in the L* value of the mineralization surface pre-etching and after mineralization buffer containing NaF and EMD. A new method has been developed to recover the color quality of enamel, as well as to mineralize the tooth enamel by constructing hydroxyapatite crystals with mineralization buffers containing NaF and EMD on the etched tooth surface.

Synthesis and Structure of a 22 × 12 × 12 Extra-Large Pore Zeolite ITQ-56 Determined by 3D Electron Diffraction.

A multidimensional extra-large pore germanosilicate, denoted ITQ-56, has been synthesized by using modified memantine as an organic structure-directing agent. ITQ-56 crystallizes as plate-like nanocrystals. Its structure was determined by 3D electron diffraction/MicroED. The structure of ITQ-56 contains extra-large 22-ring channels intersecting with straight 12-ring channels. ITQ-56 is the first zeolite with 22-ring pores, which is a result of ordered vacancies of double 4-ring (d4r) units in a fully connected zeolite framework. The framework density is as low as 12.4 T atoms/1000 Å3. The discovery of the ITQ-56 structure not only fills the missing member of extra-large pore zeolite with 22-ring channels but also creates a new approach of making extra-large pore zeolites by introducing ordered vacancies in zeolite frameworks.

2D Gadolinium Oxide Nanoplates as T1 Magnetic Resonance Imaging Contrast Agents.

Millions of people a year receive magnetic resonance imaging (MRI) contrast agents for the diagnosis of conditions as diverse as fatty liver disease and cancer. Gadolinium chelates, which provide preferred T1 contrast, are the current standard but face an uncertain future due to increasing concerns about their nephrogenic toxicity as well as poor performance in high-field MRI scanners. Gadolinium-containing nanocrystals are interesting alternatives as they bypass the kidneys and can offer the possibility of both intracellular accumulation and active targeting. Nanocrystal contrast performance is notably limited, however, as their organic coatings block water from close interactions with surface Gadoliniums. Here, these steric barriers to water exchange are minimized through shape engineering of plate-like nanocrystals that possess accessible Gadoliniums at their edges. Sulfonated surface polymers promote second-sphere relaxation processes that contribute remarkable contrast even at the highest fields (r1 = 32.6 × 10-3 m Gd-1 s-1 at 9.4 T). These noncytotoxic materials release no detectable free Gadolinium even under mild acidic conditions. They preferentially accumulate in the liver of mice with a circulation half-life 50% longer than commercial agents. These features allow these T1 MRI contrast agents to be applied for the first time to the ex vivo detection of nonalcoholic fatty liver disease in mice.

Size reduction-induced properties modifications of antiferromagnetic dielectric nanocrystalline Ba2NiMO6 (M = W, Te) double perovskites

Abstract The main objective of this work was to synthesize phase pure double perovskites Ba2NiTeO6 (BNTO) and Ba2NiWO6 (BNWO) in nanocrystalline form and to reveal the impact of nanocrystallinity on their magnetic and dielectric properties. The studied double perovskites were synthesized in nanocrystalline form by employing a citrate sol-gel route. A detailed investigation of their structure and properties using X-ray powder diffraction, scanning electron microscopy, Raman spectroscopy technique, energy-dispersive X-ray spectroscopy, SQUID magnetometry and electrical measurements is carefully described. Rietveld refinement of X-ray powder diffraction patterns revealed phase purity of both compounds: BNTO is trigonal (R-3m) while BNWO is cubic (Fm-3m). Raman spectroscopy studies reveal optical phonons that correspond to vibrations of Te6+/W6+O6 octahedra, while scanning electron microscopy images show irregular plate-like nanocrystals. Magnetic property measurements speak in favor of antiferromagnetic order but, in both compounds, size reduction affected their properties. BNTO has Néel temperature (TN) of 10.3 K which is higher than previously reported for its bulk form. Magnetic ground state of BNWO can be explained as canted antiferromagnetism with TN = 48.2 K. Room temperature measurements of dielectric constants at various frequencies suggest that these materials are high-κ dielectrics with low dielectric loss. The Nyquist plot reveals depressed a semicircle arc typical for non-Debye type of relaxation phenomena for BNWO ceramic, whereas for BNTO ceramic an almost straight line of Zʹʹ versus Z' has been observed, indicating its high insulating behavior. To conclude, size-dependent properties of studied double perovskites are discussed, introducing a possibility for implementation in electronic devices.

Biosynthesis of Bonelike Apatite 2D Nanoplate Structures Using Fenugreek Seed Extract.

An innovative, biomimetic, green synthesis approach was exploited for the synthesis of humane and environmental friendly nanomaterials for biomedical applications. Ultrafine bonelike apatite (BAp) 2D plate-like structures were prepared using fenugreek seed extract during the biosynthesis wet-chemical precipitation route. The chemical analysis, morphology and structure of the prepared 2D nanoplates were characterized by inductively coupled plasma atomic emission spectroscopy (ICP-OES), electron microscopy (SEM and TEM), X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. A 2D plate-like nanostructure of BAp with an average width (length) of 12.67 ± 2 nm and thickness of 3.8 ± 1.2 nm was obtained. BAp 2D crystals were tuned by interaction with the fenugreek organic molecules during the fabrication process. In addition to Ca and P ions, bone mineral sources such as K, Mg, Na, SO4 and CO3 ions were incorporated into BAp nanoplates using fenugreek seed extract. The overall organic molecule concentration in the reaction process increased the effectiveness of hydroxyl groups as nucleation sites for BAp crystals. Accordingly, the size of the biosynthesized BAp plate-like structure was reduced to its lowest value. Biosynthesis BAp 2D plate-like nanocrystals showed good viability and higher growth of MC3T3 osteoblast-like structures than that of the control sample. BAp 2D nanoplates prepared by a facile, ecofriendly and cost-effective approach could be considered a favorable osteoconductive inorganic biomaterial for bone regeneration applications.

Characterization of Zinc oxide Nanostructures prepared by hydrothermal method with Antibacterial property

In this study, Zinc oxide nanostructures were synthesized via a hydrothermal method by using zinc nitrate hexahydrate and sodium hydroxide as a precursor. Three different annealing temperatures were used to study their effect on ZnO NSs properties. The synthesized nanostructure was characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Atomic force microscope (AFM), and Fourier Transform Infrared Spectroscopy (FTIR). Their optical properties were studied by using UV -visible spectroscopy. The XRD analysis confirms that all ZnO nanostructures have the hexagonal wurtzite structure with average crystallite size within the range of (30.59 - 34.52) nm. The crystallite size increased due to the incensement of annealing temperature. FESEM analysis indicates that ZnO has hexagonal shape of cylindrical pores, plate-like nanocrystals and Nanorods. AFM analysis shows that the average surface roughness of ZnO Nanostructures increases from 3.96 to 19.1 nm with the increase of annealing temperature. The FTIR peaks indicate successful preparation of ZnO Nanostructures. The FTIR method was used to analyses the chemical bonds which conformed the present of the Zn-O group in the region between (400-500) cm-1. The UV-visible showed a red shift in the absorption spectra related to the shift in the energy gap related to increase in the particle size. the band gap energy has been calculated from the optical absorption spectra. The annealing process has been fond more effective on the value of energy gap. As the annealing temperature increases, the value of energy gap, increases as well; from (3.12to 3.22) eV. The prepared Nanostructure is used for antibacterial property. It shows strong antibacterial activity against S. aureus and P.aeuruginosa bacteria by the agar disc diffusion method. The white precipitate of ZnO NSs has superior antibacterial activity on gram-positive (S. aureus) than the gram-negative (P.aeuruginosa) bacteria.

Nano-crystalline, hierarchical zeolite Ti-Beta: Hydrothermal synthesis and catalytic performance in alkenes epoxidation reactions

Aluminum-free hierarchical Ti-beta was hydrothermally synthesized from a basic precursor using tetraethyl ammonium hydroxide and sodium fluorine as the structure directing agent and mineralization agent, respectively. The physicochemical properties are analyzed by XRD, TEM, UV–Vis, 29Si NMR et al. The catalytic activity was evaluated via the epoxidation of cyclohexene and 1-oectene. The Ti-beta achieved are plate-like nano-crystals with crystal size of about 100 × 300 × 300 nm. More importantly, intracrystalline mesopores in the 10–40 nm range were simultaneously created, and most of the titanium could be isomorphously substituted into the zeolite matrix. The Ti-beta is defects-free, the thermal stability is excellent. Due to the improved accessibility of the active sites inside the crystals, the activity increased by more than 30% compared with the conventional Ti-beta formed from the HF-procedure.

Optically functional isoxanthopterin crystals in the mirrored eyes of decapod crustaceans

The eyes of some aquatic animals form images through reflective optics. Shrimp, lobsters, crayfish, and prawns possess reflecting superposition compound eyes, composed of thousands of square-faceted eye units (ommatidia). Mirrors in the upper part of the eye (the distal mirror) reflect light collected from many ommatidia onto the photosensitive elements of the retina, the rhabdoms. A second reflector, the tapetum, underlying the retina, back-scatters dispersed light onto the rhabdoms. Using microCT and cryo-SEM imaging accompanied by in situ micro-X-ray diffraction and micro-Raman spectroscopy, we investigated the hierarchical organization and materials properties of the reflective systems at high resolution and under close-to-physiological conditions. We show that the distal mirror consists of three or four layers of plate-like nanocrystals. The tapetum is a diffuse reflector composed of hollow nanoparticles constructed from concentric lamellae of crystals. Isoxanthopterin, a pteridine analog of guanine, forms both the reflectors in the distal mirror and in the tapetum. The crystal structure of isoxanthopterin was determined from crystal-structure prediction calculations and verified by comparison with experimental X-ray diffraction. The extended hydrogen-bonded layers of the molecules result in an extremely high calculated refractive index in the H-bonded plane, n = 1.96, which makes isoxanthopterin crystals an ideal reflecting material. The crystal structure of isoxanthopterin, together with a detailed knowledge of the reflector superstructures, provide a rationalization of the reflective optics of the crustacean eye.

Formation of Anticorrosive Film for Suppressing Pitting Corrosion on Al-Mg-Si Alloy by Steam Coating

Al alloys offer excellent physical and mechanical properties, such as a low density, high specific strength, and good ductility. However, their low corrosion resistance has restricted their application in corrosive environments. There is a need, therefore, for a novel coating technology that is capable of improving the corrosion resistance of Al alloys. In the present study, we examined a steam-based method of forming a corrosion-resistant film on Al alloys. Al-Mg-Si alloy was used as the substrate. The cleaned substrates were set in an autoclave with ultrapure water as the steam source and processed using different temperatures and holding times, resulting in the formation of anticorrosive films on the alloy. FE-SEM images of the film surfaces showed that plate-like nanocrystals were densely formed over the entire surface. XRD patterns indicated that the film was composed mainly of AlOOH crystals. The potentiodynamic polarization curves revealed that the corrosion current density of the film-coated substrates significantly decreased, and that the pitting corrosion was completely suppressed, indicating that the corrosion resistance of the Al-Mg-Si alloy was improved by the film formed by means of steam coating.

PH-Dependent Synthesis of Anisotropic Gold Nanostructures by Bioinspired Cysteine-Containing Peptides.

In the present study, alkaline peptides AAAXCX (X = lysine or arginine residues) were designed based on the conserved motif of the enzyme thioredoxin and used for the synthesis of gold nanoparticles (GNPs) in the pH range of 2–11. These peptides were compared with free cysteine, the counterpart acidic peptides AAAECE and γ-ECG (glutathione), and the neutral peptide AAAACA. The objective was to investigate the effect of the amino acids neighboring a cysteine residue on the pH-dependent synthesis of gold nanocrystals. Kohn–Sham density functional theory (KS-DFT) calculations indicated an increase in the reducing capacity of AAAKCK favored by the successive deprotonation of their ionizable groups at increasing pH values. Experimentally, it was observed that gold speciation and the peptide structure also have a strong influence on the synthesis and stabilization of GNPs. AAAKCK produced GNPs at room temperature, in the whole investigated pH range. By contrast, alkaline pH was the best condition for the synthesis of GNP assisted by the AAARCR peptide. The acidic peptides produced GNPs only in the presence of polyethylene glycol, and the synthesis using AAAECE and γ-ECG also required heating. The ionization state of AAAKCK had a strong influence on the preferential growth of the GNPs. Therefore, pH had a remarkable effect on the synthesis, kinetics, size, shape, and polydispersity of GNPs produced using AAAKCK. The AAAKCK peptide produced anisotropic decahedral and platelike nanocrystals at acidic pH values and spherical GNPs at alkaline pH values. Both alkaline peptides were also efficient capping agents for GNPs, but they produced a significant difference in the zeta potential, probably because of different orientations on the gold surface.

Structural Characterization of Lecithin-Stabilized Tetracosane Lipid Nanoparticles. Part II: Suspensions.

Using photon correlation spectroscopy, transmission electron microscopy, microcalorimetry, wide-angle X-ray scattering (WAXS), and small-angle X-ray and neutron scattering (SAXS, SANS), the structure of 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC)-stabilized colloidal tetracosane suspensions was studied from the molecular level to the microscopic scale as a function of the temperature. The platelike nanocrystals exhibit for tetracosane an unusual orthorhombic low-temperature crystal structure. The corresponding WAXS pattern can be reproduced with a predicted orthorhombic unit cell (space group Pca21), which usually occurs only for much longer even-numbered n-alkanes. Special emphasis was placed on the structure of the DMPC stabilizer layer covering the nanocrystals. Their structure was investigated by SAXS and SANS, using suspensions with different neutron scattering contrasts. As for the emulsions in Part I , the crystallized nanoparticles are covered by a DMPC monolayer. Their significant smaller thickness of 10.5 Å (for the emulsions in Part I : 16 Å) could be related to a more tilted orientation of the DMPC molecules to cover the expanded surface of the crystallized nanoparticles.

Unexpected orbital magnetism in Bi-rich Bi2Se3 nanoplatelets

The discovery of two-dimensional electron gas states with giant Rashba spin splitting (RSS) in electron-doped three-dimensional topological insulators (TIs) uncovered new fascinating physics and raised hopes for novel spintronic devices. Significant challenges, including synthetic constraints and control of the magnetic properties, must be addressed before any breakthroughs are possible. Here, we show how RSS in Bi-rich Bi2Se3 nanoplatelets is responsible for the appearance of remarkable orbital magnetic properties, as observed using magnetization and conduction electron spin resonance experiments and confirmed by theoretical simulations. In view of the strong spin-orbit coupling (SOC) and the proximity to the TI surface states, this discovery enlightens fundamental aspects of SOC-based functionalities of TI materials with aims for future applications. Plate-like bismuth nanocrystals can give physicists enriched mechanisms to control spin through unexpected, surface-localized magnetism. Topological insulators have crystal structures that make them non-conductive everywhere except for the quantized states on their surfaces. Hae Jin Kim's group at KBSI and co-workers (PI, “Demokritos”, and UoI) has now used a liquid-phase, solvothermal synthesis to turn bismuth selenide (Bi2Se3) topological insulators into nanometre-thin platelets with unique hexagonal shapes. The team discovered that sandwiching bismuth atoms between the nanohexagons disrupts the normal coupling interactions between electron spin and orbital motion at topological insulators surface states. This splitting generates so-called Rashba states that produce a special orbital-based type of magnetism, where spin states can be flipped with help from a weak magnetic field. Further spin engineering of this system is possible by altering the degree of bismuth intercalation. Bi-layer intercalation in Bi2Se3 nanoplatelets gives rise to an intriguing crystal structure comprised of randomly stacked Bi2Se3 and Bi2Se2. Detailed conduction electron spin resonance (CESR) and AC/DC magnetization studies prove that controlling Bi intercalation results in fine tuning the two-dimensional electron gas parabolic Rashba states, which enables the appearance of extraordinary orbital magnetism, through the coupling of the spin and orbital degrees of freedom. The methodology presented herein provides a unique and simple way for efficient spin engineering, with important potential applications.

Synthesis and characterizations of 3D Co3O4 hierarchical microcrystals

Abstact Three-dimensional (3D) Co 3 O 4 hierarchical microcrystals assembled by two-dimensional (2D) plate-like nanocrystals have been successfully prepared via annealing 3D α-Co(OH) 2 hierarchical microcrystals. XRD results demonstrated that the pure phase α-Co(OH) 2 hierarchical microcrystals were converted into pure cubic phase Co 3 O 4 hierarchical microcrystals after annealing at 400 °C for 2 h. SEM observations show that the as-achieved 3D Co 3 O 4 hierarchical microcrystals are built by 2D plate-like nanocrystals. Room temperature photoluminescence shows that the as-obtained 3D Co 3 O 4 hierarchical microcrystals exhibit a broadened visible emission in the range of 650–760 nm with a center peak at around 745 nm (1.67 eV), which may lead these 3D Co 3 O 4 hierarchical microcrystals to potential applications in visible light emitting materials and nanodevices.

Hexagonal plate-like magnetite nanocrystals produced in komatiite–H2O–CO2reaction system at 450°C

AbstractBatch experiments of komatiite–H2O–CO2system with temperatures from 200 to 450°C were performed to simulate the interactions between the newly formed ultramafic crust and the proto-atmosphere on Earth before the formation of its earliest ocean. Particularly, magnetite nanocrystals were observed in the experiment carried out at 450°C that are characterized by their hexagonal platelet-like morphology and porous structure. Exactly the same set of lattice fringes on the two opposite sides of one pore suggests post-crystallization erosion. The results demonstrate that magnetite could be produced by the direct interactions between the ultramafic rocky crust and the atmosphere before the formation of the ocean on the Hadean Earth. These magnetite nanoparticles could serve as a catalyst in the synthesis of simple organic molecules during the organochemical evolution towards life.

Calcium Phosphate Nanoparticles and their Biomedical Potential

Calcium Phosphate Nanoparticles and their Biomedical Potential Nanodimensional and nanocrystalline calcium phosphates (in the form of apatites) of a biological origin are the basic inorganic building blocks of bones and teeth of mammals. The application and potential use of calcium phosphates for clinical repair of damaged bones and teeth to controlled drug delivery devices, multi-modal imaging, and bone regeneration is gaining importance. Calcium phosphate nanoparticles are rigid, biocompatible, biodegradable, bioactive, resorbable and non-immunogenic. Nanostructured calcium phosphates with various morphologies including spherical nanoparticles, plate-like nanocrystals, nano-needles, whiskers/ fibers/wires, mesoporous, nanotubes, nano-blades, and powders with three-dimensional structures have been synthesized by various methods including mechanochemical synthesis, reverse microemulsion, hydrothermal approach, co-precipitation, spraydrying technique, in-situ deposition technique, wet chemical precipitation, gas phase ablation and biomimetic coating. Nanostructured calcium phosphates are promising biomaterials for applications in biomedical areas, such as tissue engineering scaffolds, drug/gene delivery systems, vaccine adjuvants, contrast agents for imaging and multi-modal imaging, nanosystems for photodynamic therapy and antifungal/antibacterial agents.

Influence of process parameters on the content of biomimetic calcium phosphate coating on titanium: a Taguchi analysis.

In this study, a statistical design of experimental methodology based on Taguchi orthogonal design has been used to study the effect of various processing parameters on the amount of calcium phosphate coating produced by such technique. Seven control factors with three levels each including sodium hydroxide concentration, pretreatment temperature, pretreatment time, cleaning method, coating time, coating temperature and surface area to solution volume ratio were studied. X-ray diffraction revealed that all the coatings consisted of the mixture of octacalcium phosphate (OCP) and hydroxyapatite (HA) and the presence of each phase depended on the process conditions used. Various content and size (-1-100 μm) of isolated spheroid particles with nanosized plate-like morphology deposited on the titanium surface or a continuous layer of plate-like nanocrystals having the plate thickness in the range of -100-300 nm and the plate width in the range of 3-8 μm were formed depending on the process conditions employed. The optimum condition of using sodium hydroxide concentration of 1 M, pretreatment temperature of 70 degrees C, pretreatment time of 24 h, cleaning by ultrasonic, coating time of 6 h, coating temperature of 50 degrees C and surface area to solution volume ratio of 32.74 for producing the greatest amount of the coating formed on the titanium surface was predicted and validated. In addition, coating temperature was found to be the dominant factor with the greatest contribution to the coating formation while coating time and cleaning method were significant factors. Other factors had negligible effects on the coating performance.

Nanostructures prepared from single crystal and amorphous powder consisted of (NH3CH2CH2NH2)2[MoO2(O2C10H6)2

Molybdenum complex (NH3CH2CH2NH2)2[MoO2(O2C10H6)2].0·5CH3CN have been synthesised, bulk single crystal and macro amorphous powder consisted of the complex are produced respectively, and from which plate-like nanocrystal with scale in tens nm and nanopowders with diameter in a few nm are prepared separately by grinding and ultra-sonication. X-ray diffraction revealed that the crystal exhibited multi-layered structure with lamellar repeating motifs linked by Van Der Waals forces, and the lamella motif are constituted by (NH3CH2CH2NH2)2[MoO2(O2C10H6)2].0·5CH3CN through hydrogen bonds (OC10H8)O(2)···H-NCCN-H···O(2)(C10H8O) with the distance 1·9226 Å and angle 170° and NCCN ···H-NCCN with the distance 1·9323 Å and angle 160°. Since both Van Der Waals force and hydrogen bonds are weak interaction among the molecules, and the linkage molecule NH2CH2CH2NH2 are volatile, therefore the bulk multi-layered crystal disassembled into nano-lamellas which then broken into plate-like nano-crystals by grinding and ultra-sonication. Similar, the macro amorphous powder disaggregated into nano-powders. UV spectra has shown PhO−→Mo(πd) ligand-to-metal charge transfer (LMCT) transition and cyclic voltammetry analysis has shown complex associated with a reversible redox process, assumed to be one-electron and metal based.

N-Doped lepidocrocite nanotubular arrays: hydrothermal formation from anodic TiO2nanotubes and enhanced visible light photoresponse

New Cs-lepidocrocite nanotubular arrays were successfully prepared from anodically grown TiO2 nanotubes by hydrothermal conversion using CsOH in a water–ethanol mixed solvent. The obtained open nanotubular structure consists of plate-like nano-crystals, reflecting a preferred facet growth of the lepidocrocite with a 2-dimensional layered crystal structure. N-Doping of the Cs-lepidocrocite nanotubular layer was carried out by annealing in NH3 gas. The N-doped sample showed an incident photon to current conversion efficiency (IPCE) of 1.43% at 450 nm, which is 57% higher than conventional N-doped anatase TiO2 nanotubes.