Synthesis of Pure Brookite Nanorods in a Nonaqueous Growth Environment

Brookite TiO2 is the most difficult TiO2 polymorph to synthesize. The available methods in the literature to produce brookite nanostructures mostly use water-based techniques for the preparation of water-soluble Ti complexes first, followed by a hydrothermal growth of the brookite nanostructures. Besides its multi-step nature, achieving a single brookite phase and optimizing the aqueous growth environment are all issues to be hardly controlled. In this work, pure brookite TiO2 nanorods are synthesized using tetrabutyl titanate Ti(OBu)4 and Sodium Fluoride (NaF) as precursor materials in a simple non-aqueous one-pot solvothermal process. Alcoholysis of only Ti(OBu)4 in ethanol resulted in pure anatase nanoparticles, while the addition of NaF was essential to promote the growth of highly pure brookite nanorods. The phase purity is confirmed by X-Ray Diffraction, Raman Spectroscopy, and High-Resolution Transmission Electron Microscopy. The growth mechanism is explained according to the Ostwald’s step rule, where Na+ ions are anticipated to have a potential role in driving the growth process towards the brookite phase.

Download Full-text

An expeditious one-pot synthesis of pyrido[2,3-d]pyrimidines using Fe3O4–ZnO–NH2–PW12O40 nanocatalyst

Journal of Chemical Research ◽

10.1177/1747519819856978 ◽

2019 ◽

Vol 43 (3-4) ◽

pp. 135-139

Author(s):

Pegah Farokhian ◽

Manouchehr Mamaghani ◽

Nosrat Ollah Mahmoodi ◽

Khalil Tabatabaeian ◽

Abdollah Fallah Shojaie

Keyword(s):

Electron Microscopy ◽

Vibrating Sample Magnetometer ◽

X Ray Diffraction ◽

Facile Synthesis ◽

Pyrimidine Derivatives ◽

One Pot ◽

X Ray ◽

Transmission Electron ◽

Novel Method ◽

Operational Simplicity

An efficient protocol for the facile synthesis of a series of pyrido[2,3- d]pyrimidine derivatives has been developed applying Fe3O4–ZnO–NH2–PW12O40 nanocatalyst in water. This novel method has the benefits of operational simplicity, green aspects by avoiding toxic solvents and high to excellent yields of products. Fe3O4–ZnO–NH2–PW12O40 was synthesized and characterized by Fourier transform infrared, X-ray diffraction, vibrating sample magnetometer, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and transmission electron microscopy analyses. The nanocatalyst is readily isolated and recovered from the reaction mixture by an external magnet.

Download Full-text

5-Phenyl-10,15,20-Tris(4-sulfonatophenyl)porphyrin: Synthesis, Catalysis, and Structural Studies

Molecules ◽

10.3390/molecules23123363 ◽

2018 ◽

Vol 23 (12) ◽

pp. 3363 ◽

Cited By ~ 3

Author(s):

Aitor Arlegui ◽

Zoubir El-Hachemi ◽

Joaquim Crusats ◽

Albert Moyano

Keyword(s):

Alder Reaction ◽

Water Soluble ◽

Experimental Conditions ◽

One Pot ◽

Force Microscopy ◽

Diels Alder Reaction ◽

Transmission Electron ◽

Porphyrin Synthesis ◽

The One ◽

Water Soluble Porphyrin

A convenient protocol for the preparation of 5-phenyl-10,15,20-tris(4-sulfonatophenyl)porphyrin, a water-soluble porphyrin with unique aggregation properties, is described. The procedure relies on the one-pot reductive deamination of 5-(4-aminophenyl)-10,15,20-tris(4-sulfonatophenyl)porphyrin, that can be in turn easily obtained from 5,10,15,20-tetraphenylporphyrin by a known three-step sequence involving mononitration, nitro to amine reduction and sulfonation of the phenyl groups. This method provides the title porphyrin in gram scale, and compares very favorably with the up to now only described procedure based on the partial sulfonation of TPP, that involves a long and tedious chromatographic enrichment of the final compound. This has allowed us to study for the first time both the use of its zwitterionic aggregate as a supramolecular catalyst of the aqueous Diels–Alder reaction, and the morphology of the aggregates obtained under optimized experimental conditions by atomic force microscopy and also by transmission electron cryomicroscopy.

Download Full-text

Formation of ZnO/Zn0.5Cd0.5Se Alloy Quantum Dots in the Presence of High Oleylamine Contents

Nanomaterials ◽

10.3390/nano9070999 ◽

2019 ◽

Vol 9 (7) ◽

pp. 999

Author(s):

Yi-An Chen ◽

Kuo-Hsien Chou ◽

Yi-Yang Kuo ◽

Cheng-Ye Wu ◽

Po-Wen Hsiao ◽

...

Keyword(s):

Electron Microscopy ◽

Quantum Dots ◽

Particle Size ◽

X Ray Diffraction ◽

One Pot ◽

X Ray ◽

Transmission Electron ◽

Average Size ◽

Alloy Quantum Dots ◽

First Time

To the best of our knowledge, this report presents, for the first time, the schematic of the possible chemical reaction for a one-pot synthesis of Zn0.5Cd0.5Se alloy quantum dots (QDs) in the presence of low/high oleylamine (OLA) contents. For high OLA contents, high-resolution transmission electron microscopy (HRTEM) results showed that the average size of Zn0.5Cd0.5Se increases significantly from 4 to 9 nm with an increasing OLA content from 4 to 10 mL. First, [Zn(OAc)2]–OLA complex can be formed by a reaction between Zn(OAc)2 and OLA. Then, Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) data confirmed that ZnO is formed by thermal decomposition of the [Zn(OAc)2]–OLA complex. The results indicated that ZnO grew on the Zn0.5Cd0.5Se surface, thus increasing the particle size. For low OLA contents, HRTEM images were used to estimate the average sizes of the Zn0.5Cd0.5Se alloy QDs, which were approximately 8, 6, and 4 nm with OLA loadings of 0, 2, and 4 mL, respectively. We found that Zn(OAc)2 and OLA could form a [Zn(OAc)2]–OLA complex, which inhibited the growth of the Zn0.5Cd0.5Se alloy QDs, due to the decreasing reaction between Zn(oleic acid)2 and Se2−, which led to a decrease in particle size.

Download Full-text

Novel Graphene/In2O3 Nanocubes Preparation and Selective Electrochemical Detection for L-Lysine of Camellia nitidissima Chi

Materials ◽

10.3390/ma13081999 ◽

2020 ◽

Vol 13 (8) ◽

pp. 1999

Author(s):

Jinsheng Cheng ◽

Sheng Zhong ◽

Weihong Wan ◽

Xiaoyuan Chen ◽

Ali Chen ◽

...

Keyword(s):

Electron Microscopy ◽

Electrochemical Sensor ◽

Chiral Recognition ◽

Graphene Nanosheets ◽

Reduction Reaction ◽

X Ray Diffraction ◽

One Pot ◽

X Ray ◽

Transmission Electron ◽

Camellia Nitidissima

In this work, novel graphene/In2O3 (GR/In2O3) nanocubes were prepared via one-pot solvothermal treatment, reduction reaction, and successive annealing technology at 600 °C step by step. Interestingly, In2O3 with featured cubic morphology was observed to grow on multi-layered graphene nanosheets, forming novel GR/In2O3 nanocubes. The resulting nanocomposites were characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction spectroscopy (XRD), etc. Further investigations demonstrated that a selective electrochemical sensor based on the prepared GR/In2O3 nanocubes can be achieved. By using the prepared GR/In2O3-based electrochemical sensor, the enantioselective and chem-selective performance, as well as the optimal conditions for L-Lysine detection in Camellia nitidissima Chi, were evaluated. The experimental results revealed that the GR/In2O3 nanocube-based electrochemical sensor showed good chiral recognition features for L-lysine in Camellia nitidissima Chi with a linear range of 0.23–30 μmol·L−1, together with selectivity and anti-interference properties for other different amino acids in Camellia nitidissima Chi.

Download Full-text

Gnidia glauca- and Plumbago zeylanica-Mediated Synthesis of Novel Copper Nanoparticles as Promising Antidiabetic Agents

Advances in Pharmacological Sciences ◽

10.1155/2019/9080279 ◽

2019 ◽

Vol 2019 ◽

pp. 1-11 ◽

Cited By ~ 6

Author(s):

Dhiraj A. Jamdade ◽

Dishantsingh Rajpali ◽

Komal A. Joshi ◽

Rohini Kitture ◽

Anuja S. Kulkarni ◽

...

Keyword(s):

Electron Microscopy ◽

Copper Nanoparticles ◽

Critical Role ◽

Cost Effective ◽

Significant Inhibition ◽

Antidiabetic Activity ◽

X Ray Diffraction ◽

One Pot ◽

Plumbago Zeylanica ◽

Transmission Electron

Rapid, eco-friendly, and cost-effective one-pot synthesis of copper nanoparticles is reported here using medicinal plants like Gnidia glauca and Plumbago zeylanica. Aqueous extracts of flower, leaf, and stem of G. glauca and leaves of P. zeylanica were prepared which could effectively reduce Cu2+ ions to CuNPs within 5 h at 100°C which were further characterized using UV-visible spectroscopy, field emission scanning electron microscopy, high-resolution transmission electron microscopy, energy dispersive spectroscopy, dynamic light scattering, X-ray diffraction, and Fourier-transform infrared spectroscopy. Further, the CuNPs were checked for antidiabetic activity using porcine pancreatic α-amylase and α-glucosidase inhibition followed by evaluation of mechanism using circular dichroism spectroscopy. CuNPs were found to be predominantly spherical in nature with a diameter ranging from 1 to 5 nm. The phenolics and flavonoids in the extracts might play a critical role in the synthesis and stabilization process. Significant change in the peak at ∼1095 cm−1 corresponding to C-O-C bond in ether was observed. CuNPs could inhibit porcine pancreatic α-amylase up to 30% to 50%, while they exhibited a more significant inhibition of α-glucosidase from 70% to 88%. The mechanism of enzyme inhibition was attributed due to the conformational change owing to drastic alteration of secondary structure by CuNPs. This is the first study of its kind that provides a strong scientific rationale that phytogenic CuNPs synthesized using G. glauca and P. zeylanica can be considered to develop candidate antidiabetic nanomedicine.

Download Full-text

Facile synthesis of water-soluble graphene-based composite: Non-covalently functionalized with chitosan-ionic liquid conjugation

Functional Materials Letters ◽

10.1142/s1793604716500454 ◽

2016 ◽

Vol 09 (03) ◽

pp. 1650045 ◽

Cited By ~ 7

Author(s):

Pei-Ying Li ◽

Kai-Yu Cheng ◽

Xiu-Cheng Zheng ◽

Pu Liu ◽

Xiu-Juan Xu

Keyword(s):

Electron Microscopy ◽

Ionic Liquid ◽

Chemical Reduction ◽

Water Soluble ◽

X Ray Diffraction ◽

Facile Synthesis ◽

X Ray ◽

Transmission Electron ◽

Vis Spectroscopy ◽

Text Interaction

Chitosan-ionic liquid conjugation (CILC), which was prepared through the reaction of 1-(4-bromobutyl)-3-methylimidazolium bromide (BBMIB) with chitosan, was firstly used to prepare functionalized graphene composite via the chemical reduction of graphene oxide (GO). The obtained water soluble graphene-based composite was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), ultraviolet-visible (UV–Vis) spectroscopy and so on. CILC-RGO showed excellent dispersion stability in water at the concentration of 2.0 mg/mL, which was stable for several months without any precipitate. This may be ascribed to the electrostatic attraction and [Formula: see text]–[Formula: see text] interaction between CILC and graphene.

Download Full-text

Water-Soluble O-, S- and Se-Functionalized Cyclic Acetyl-triaza-phosphines. Synthesis, Characterization and Application in Catalytic Azide-alkyne Cycloaddition

Molecules ◽

10.3390/molecules25225479 ◽

2020 ◽

Vol 25 (22) ◽

pp. 5479

Author(s):

Abdallah Mahmoud ◽

Piotr Smoleński ◽

M. Guedes da Silva ◽

Armando Pombeiro

Keyword(s):

Cycloaddition Reaction ◽

Structural Features ◽

Water Soluble ◽

31P Nmr Spectroscopy ◽

The Novel ◽

X Ray Diffraction ◽

One Pot ◽

Hirshfeld Surfaces ◽

The One ◽

High Yields

The 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane (DAPTA) derivatives, viz. the already reported 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane 5-oxide (DAPTA=O, 1), the novel 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane-5-sulfide (DAPTA=S, 2), and 3,7-diacetyl-1,3,7-triaza-5-phosphabicyclo[3.3.1]nonane-5-selenide (DAPTA=Se, 3), have been synthesized under mild conditions. They are soluble in water and most common organic solvents and have been characterized using 1H and 31P NMR spectroscopy and, for 2 and 3, also by single crystal X-ray diffraction. The effect of O, S, or Se at the phosphorus atom on the structural features of the compounds has been investigated, also through the analyses of Hirshfeld surfaces. The presence of 1–3 enhances the activity of copper for the catalytic azide-alkyne cycloaddition reaction in an aqueous medium. The combination of cheaply available copper (II) acetate and compound 1 has been used as a catalyst for the one-pot and 1,4-regioselective procedure to obtain 1,2,3-triazoles with high yields and according to ‘click rules’.

Download Full-text

Sol-Gel Synthesis and Characterization of Nanocrystalline Bi4Ti3O12 Powders

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.997.359 ◽

2014 ◽

Vol 997 ◽

pp. 359-362 ◽

Cited By ~ 1

Author(s):

Chun Hong Ma ◽

Xue Lin ◽

Liang Wang ◽

Yong Sheng Yan

Keyword(s):

Phase Inversion ◽

Bismuth Titanate ◽

Sol Gel ◽

Tetrabutyl Titanate ◽

X Ray Diffraction ◽

X Ray ◽

Transmission Electron ◽

Sol Gel Synthesis ◽

Source Materials

Nanocrystalline bismuth titanate (Bi4Ti3O12; BTO) powders were successfully prepared by the sol-gel method, using bismuth nitrate (Bi(NO3)3·5H2O) and tetrabutyl titanate (Ti(OC4H9)4) as source materials, acetic anhydride and ethanediol as solvents. The thermal decomposition and phase inversion process of the gel precursors were studied by using differential thermal analysis (DTA). The crystal structures and microstructures of BTO powders were investigated by using x-ray diffraction (XRD), and transmission electron microscope (TEM). The crystallization of amorphous bismuth titanate has been discussed. The effect of sintering temperature on the structure and morphology of BTO was investigated. At 644 oC and above, BTO powder undergoes a phase transformation from tetragonal to orthorhombic. At 900 oC, the purified orthorhombic BTO nanocrystals were obtained.

Download Full-text

Preparation and photoelectrochemical performance of nano Bi2S3–TiO2 composites

Functional Materials Letters ◽

10.1142/s1793604718500558 ◽

2018 ◽

Vol 11 (03) ◽

pp. 1850055 ◽

Cited By ~ 6

Author(s):

Senlin Li ◽

Jinliang Huang ◽

Xiangmei Ning ◽

Yongchao Chen ◽

Qingkui Shi

Keyword(s):

Solvothermal Method ◽

Composite Films ◽

Great Influence ◽

Photocurrent Density ◽

Tetrabutyl Titanate ◽

X Ray Diffraction ◽

Photoelectrochemical Performance ◽

X Ray ◽

External Bias ◽

Transmission Electron

TiO2 nanorod (NR) arrays were prepared on FTO by the simple hydrothermal synthesizing method. On this basis, a layer of Bi2S3 quantum dots (QDs) was covered on the surface of TiO2 NRs array by solvothermal method, by which the Nano Bi2S3/TiO2 NRs composites films were obtained. The phase structure, morphologies, optical absorptions and photoelectrochemical (PEC) properties of the as-prepared materials were characterized by X-ray diffraction (XRD), Scanning Electron Microscope (SEM), High Resolution Transmission Electron Microscopy (HRTEM), Ultraviolet–visible spectroscopy (UV-Vis), Photoluminescence (PL) and electrochemical workstation. The results indicate that the concentration of tetrabutyl titanate (TBT) has a great influence on the morphology of the film, with the increase of TBT content, the array of TiO2 NRs changed from loose to tight, and the thin films were cracked when the TBT volume is up to 0.7[Formula: see text]mL; The absorption of the TiO2 NRs array film to the visible light is enhanced significantly when sensitized with Bi2S3 and the absorption wavelength is increased from 400[Formula: see text]nm to 800[Formula: see text]nm. Compared with the pure TiO2, the fluorescence intensity of the TiO2/Bi2S3 NRs is weakened, and there is no obvious fluorescence diffraction peak. Under the irradiation of standard (AM1.5[Formula: see text]G 100[Formula: see text]mW/cm[Formula: see text], the photocurrent density of the composite film increased significantly. When the external bias voltage is 1.2[Formula: see text]V, the current density of the composite films is five times of that of the pure TiO2.

Download Full-text

One-pot microwave assisted approach for synthesis of CdSe/CdS core-shell quantum dots (QDs) and investigating optical properties

Modern Physics Letters B ◽

10.1142/s0217984916500743 ◽

2016 ◽

Vol 30 (07) ◽

pp. 1650074 ◽

Cited By ~ 7

Author(s):

M. Molaei ◽

F. Salari Bardsiri ◽

A. R. Bahador ◽

M. Karimipour

Keyword(s):

Core Shell ◽

Heat Sensitivity ◽

X Ray Diffraction ◽

Cdse Qds ◽

One Pot ◽

X Ray ◽

Microwave Assisted ◽

Transmission Electron ◽

Core Shell Structure ◽

Microwave Assisted Method

In this work, CdSe QDs were synthesized using a microwave assisted method and chemical reaction between NaHSe, CdSO4 at the presence of TGA as capping molecule. Thereafter without CdSe extraction, CdS shell was grown subsequently around CdSe cores by a reaction based on the heat sensitivity of Na2S2O3 dissociation. Synthesized QDs were characterized by means of X-ray diffraction spectroscopy (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), UV–Vis and photoluminescence (PL) spectroscopy. All of these analyzes confirmed formation of CdSe QDs and successfully growth of CdS shell on surface of CdSe to forming CdSe/CdS core-shell structure.

Download Full-text