Controlled synthesis of light rare-earth hydroxide nanorods via a simple solution route

Ln(OH)₃ (Ln=La, Pr, Nd, Sm, Eu, Gd) nanorods are synthesized without using any surfactants or templates at room temperature. The as-obtained nanorods are within 4–25 nm in diameter and up to 200 nm in length. The most important improvement is that the aspect ratio of the obtained nanorods can be effectively controlled by adjusting the reaction time and pH value of the reaction system. The as-synthesized nanorods are characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). It is interesting to find that both the inherent crystal structure of light lanthanide hydroxide and the chemical potential affect the formation of nanorods. The photoluminescence (PL) instrument is used to investigate the optical properties of the Eu(OH)₃ nanorods and its abnormal luminescence behaviors are observed.     

Hydrothermal preparation and characterization of Cd0.9Mn0.1S nanorods

Cd_0.9Mn_0.1S semiconductor nanorods were successfully prepared by the hydrothermal reaction of CdCl₂·2.5H₂O and MnCl₂·5H₂O with (NH₄)₂S in aqueous solution. Atomic absorption spectrometry (AAS) and energy dispersive spectroscopy (EDS) were used to determine the Mn contents of these complex nanorods. The samples were characterized by scanning electron microscopy (SEM-EDS), X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-vis absorption spectra, photoluminescence (PL) and compared with the undoped CdS nanorods. The results showed that nanostructured multiplex compounds with high aspect ratio were obtained via hydrothermal method. The products showed almost totally rod-like morphology with approximately identical diameter about 20 nm and the maximal length up to 200 nm.     

Controlled synthesis and relationship between luminescent properties and shape/crystal structure of Zn2SiO4:MN phosphor

Mn-doped Zn₂SiO₄ phosphors with different morphology and crystal structure, which show different luminescence and photoluminescence intensity, were synthesized via a low-temperature hydrothermal route without further calcining treatment. As-synthesized zinc silicate nanostructures show green or yellow luminescence depending on their different crystal structure obtained under different preparation conditions. The yellow peak occurring at 575 nm comes from the β-phase zinc silicate, while the green peak centering at 525 nm results from the usual α-phase zinc silicate. From photoluminescence spectra, it is found that Zn₂SiO₄ nanorods have higher photoluminescence intensity than Zn₂SiO₄ nanoparticles. It can be ascribed to reduced surface-damaged region and high crystallinity of nanorods.     

One-pot hydrothermal synthesis of an assembly of magnetite nanoneedles on a scaffold of cyclic-diphenylalanine nanorods

The assembly of metal oxide nanoparticles (NPs) on a biomolecular template by a one-pot hydrothermal synthesis method is achieved for the first time. Magnetite (Fe₃O₄) nanoneedles (length: ~100 nm; width: ~10 nm) were assembled on cyclic-diphenylalanine (cFF) nanorods (length: 2–10 μm; width: 200 nm). The Fe₃O₄ nanoneedles and cFF nanorods were simultaneously synthesized from FeSO₄ and l-phenylalanine by hydrothermal synthesis (220 °C and 22 MPa), respectively. The samples were analyzed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (IR), transmission electron microscopy (TEM), and superconducting quantum interference device (SQUID) magnetometry. Experimental results indicate that Fe₃O₄ nanoneedles were assembled on cFF nanorods during the hydrothermal reaction. The composite contained 3.3 wt% Fe₃O₄ nanoneedles without any loss of the original magnetic properties of Fe₃O₄.     

Synthesis, characterization and photoluminescent properties of rare-earth hydroxides and oxides nanorods by hydrothermal route

The stable and crystalline pure phase Ln(OH)₃ (Ln=La, Nd, Sm, Eu, Gd, Tb, and Dy) nanorods are synthesized by a facile hydrothermal method using the simple chemical materials (rare-earth chloride hexahydrate LnCl₃?6H₂O and NH₃?H₂O) and polymer polyvinypyrrolidone (PVP). The as-prepared Ln(OH)₃ nanorods can be successfully converted to Ln₂O₃ nanorods via calcination under appropriate conditions. X-ray diffraction (XRD) spectra, Fourier transformed infrared (FTIR) spectrum, scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-Resolution TEM (HRTEM), and Raman spectroscopy were used to examine the morphologies and microstructures to find out the cause. The analyzed results indicate that the obtained nanorods are rare-earth hydroxides and oxides with 1D nanostructures. The formation mechanism of the Ln(OH)₃ and Ln₂O₃ nanorods was investigated. Optical properties of the Ln(OH)₃ and Ln₂O₃ nanorods were determined by photoluminescence (PL). Ln(OH)₃ and Ln₂O₃ nanorods exhibit a strong blue emission with the strongest narrow bands at about 469 nm corresponding to the intra-4f transitions ⁵D₂→⁷F₆, which have potential applications in fluorescent devices.     

Effects of organic acids on the size-controlled synthesis of rutile TiO2 nanorods

Size-controlled synthesis of pure rutile-phase TiO₂ nanorods was carried out by a hydrothermal method using different organic acids as modifiers, and metatitanic acid and concentrated sulfuric acid as raw materials. The synthesized rutile TiO₂ nanorods were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effects of organic acid modifiers on the sizes of rutile TiO₂ nanorods were investigated. It was found that the steric effect occurred by the organic modifiers and non-polarity of organic acids were beneficial to the formation of small-sized rutile TiO₂ nanorods. The strongly coordinative interaction between the carboxyl (or hydroxyl) group of the modifier and the surface of TiO₂ nanoparticles effectively inhibited the crystal growth.     

Hydrothermal synthesis of micrometer sized HgMoO4 flowers formed by nanorods

Micrometer sized HgMoO₄ flowers formed by nanorods were prepared by a selected hydrothermal method using a mixture of ethanol and water as a reaction medium, which were characterized by scanning electron microscopy, X-ray diffractometer (XRD), FT-IR spectrometry, photoluminescence spectrometry, and UV–visible spectrometry. Results indicated that the micrometer sized flowers consisted of mercury molybdate nanorods, and the monoclinic wolframite-type structure of the flowers was confirmed by both XRD and FT-IR spectrometry. A blue shift of the photoluminescence peaks and a broadening of XRD peaks were observed, which increased with ethanol fraction in the reaction medium.     

Reductive hydrothermal synthesis of La(OH)<Subscript>3</Subscript>:Tb<Superscript>3+</Superscript> nanorods as a new green emitting phosphor

A reductive hydrothermal process with use of hydrazine hydrate as a protecting agent is proposed to synthesize La(OH)₃:Tb³⁺ (Tb mol% = 0, 1, 5, 10, and 20) nanorods. The oxidation of Tb³⁺−Tb⁴⁺ was effectively prevented in the presence of hydrazine hydrate; hence the La(OH)₃:Tb³⁺ nanorods exhibited much stronger green photoluminescence than the product prepared by the normal hydrothermal process. X-ray diffraction and transmission electron microscopy were employed to characterize the products, the results of which revealed that all the products were one-dimensional rod-like nanostructures of hexagonal structure (∼20 nm in diameter). The reductive hydrothermal process is desirable for the synthesis of other efficient Tb³⁺ doped nanophosphers.     

Red, green, and blue lanthanum phosphate phosphors obtained via surfactant-controlled hydrothermal synthesis

A new solution route for the obtainment of highly pure luminescent rare-earth orthophosphates in hydrothermal conditions was developed. By starting from soluble precursors (lanthanide tripolyphosphato complexes, i.e. with P₃O₁₀⁵⁻ as a complexing agent and as an orthophosphate source) and by applying surfactants in a water/toluene medium, the precipitations are confined to reverse micelle structures, thus yielding nanosized and homogeneous orthophosphates. The method was employed to obtain lanthanide-activated lanthanum phosphates, which can be applied as red (LaPO₄:Eu³⁺), green (LaPO₄:Ce³⁺,Tb³⁺) and blue (LaPO₄:Tm³⁺) phosphors. The produced materials were analyzed by powder X-ray diffractometry, scanning electron microscopy, infrared spectroscopy and luminescence spectroscopy (emission, excitation, lifetimes and chromaticity coordinates).     

不同形貌的LaPO4：Dy荧光粉的制备及其真空紫外激发下的发光性能

在水热法中通过改变磷源以及反应溶剂成功合成出了不同形貌的LaPO₄：Dy荧光粉,考察了真空紫外激发下不同形貌的LaPO₄：Dy荧光粉的发光性能.结果表明,由于采用的磷源不同,不同形貌的LaPO₄：Dy荧光粉的发光强度会受到影响;其次颗粒尺寸的大小也会影响发光强度.而形貌对Dy³⁺离子占据的格位的对称性影响不大,三种形貌的LaPO₄：Dy荧光粉的黄蓝比都在1—1.5之间.从激发光谱的对比中可知LaPO₄基质向Dy³⁺离子传递能量的效率不如向其他稀土离子,如Eu³⁺离子的效率高,同时在激发光谱中还观察到了较强的Dy³⁺离子的f-d跃迁激发峰. 关键词： 3+')" href="#">Dy³⁺ 真空紫外 发光     

Sodium dodecyl sulfate-assisted synthesis of CoWO4 nanorods

CoWO₄ nanorods were synthesized at 453 K for 12 h by a hydrothermal technology from Na₂WO₄ · 2H₂O and CoCl₂ · 6H₂O in the presence of sodium dodecyl sulfate (SDS). The as-synthesized CoWO₄ nanorods were characterized by various techniques of X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and X-ray detector. Luminescent properties of the samples were measured at room temperature. The results showed that CoWO₄ products are nanorods with diameters of about 20 nm, and lengths ranging between 100 and 200 nm. CoWO₄ nanorods display a very strong PL peak at 453 nm with the excitation wavelength 300 nm. The possible formation mechanism of CoWO₄ nanorods was suggested.     

Investigation of Cu Doping,Morphology and Annealing Effects on Structural and Optical Properties of ZnO:Dy Nanostructures

Dysprosium (Dy) doped ZnO nanosheets and nanorods were synthesized by hydrothermal method. Effects of Cu doping, morphology and annealing in Oxygen ambient on structural and optical properties of ZnO nanostructures were investigated using X–ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectra (DRS) and photoluminescence (PL) spectroscopy. This study recommends that both of intrinsic and extrinsic defects facilitate energy transfer (ET) from the ZnO host to Dy³⁺ ions and consequently have an effective role on producing intense Dy emissions at indirect excitation. The results also revealed that annealing process improved the crystal structure of ZnO nanorods due to decrease of surface; however decreased ET and Dy emissions because of diminishing in oxygen vacancy. In addition, as a result of increasing of surface area in nanorods compared to nanosheets, the oxygen vacancies and ET were enhanced. Moreover the results exhibited that electrical and optical properties of ZnO:Dy can be tuned by various amount of Dy concentrations and also Cu doping.     

NaYF_4∶Eu~(3+)纳米粒子和六棱柱的水热控制合成与发光性质

以柠檬酸三钠为螯合剂,通过控制反应条件,利用水热法分别合成出立方相NaYF4:Eu3+球形纳米粒子和六角相NaYF4:Eu3+六角微米棱柱。利用X射线粉末衍射(XRD)、场扫描电子显微镜(SEM)、红外吸收(FTIR),以及发光光谱等手段对产物的物相结构、形貌和荧光性能进行了分析。结果显示产物的晶格结构和柠檬酸分子的选择性吸附是晶体形貌可控的主要原因。在395nm光激发下,NaYF4:Eu3+样品显示出较强的橙色(588nm)和红色(614nm)发光,分别来自于Eu3+离子5D0→7F1和5D0→7F2的跃迁。从5D0→7F2与5D0→7F1跃迁的强度比可以推断在立方相纳米粒子的晶格中Eu3+离子更多地占据反演中心的格位。     

Fluorinated Eu‐Doped SnO2 Nanostructures with Simultaneous Phase and Shape Control and Improved Photoluminescence

Fluorinated Eu‐doped SnO₂ nanostructures with tunable morphology (shuttle‐like and ring‐like) are prepared by a hydrothermal method, using NaF as the morphology controlling agent. X‐ray diffraction, field‐emission scanning electron microscopy, high‐resolution transmission electron microscopy, X‐ray photoelectron spectroscopy, and energy dispersive spectroscopy are used to characterize their phase, shape, lattice structure, composition, and element distribution. The data suggest that Eu³⁺ ions are uniformly embedded into SnO₂ nanocrystallites either through substitution of Sn⁴⁺ ions or through formation of Eu‐F bonds, allowing for high‐level Eu³⁺ doping. Photoluminescence features such as transition intensity ratios and Stark splitting indicate diverse localization of Eu³⁺ ions in the SnO₂ nanoparticles, either in the crystalline lattice or in the grain boundaries. Due to formation of Eu‐F and Sn‐F bonds, the fluorinated surface of SnO₂ nanocrystallites efficiently inhibits the hydroxyl quenching effect, which accounts for their improved photoluminescence intensity.     

Growth of β-Ga2O3 nanorods by ammoniating Ga2O3/V thin films on Si substrate

This paper reports that/3-Ga2O3 nanorods have been synthesized by ammoniating Ga2O3 films on a V middle layer deposited on Si（111） substrates. The synthesized nanorods were confirmed as monoclinic Ga2O3 by x-ray diffraction,Fourier transform infrared spectra. Scanning electron microscopy and transmission electron microscopy reveal that the grown β-Ga2O3 nanorods have a smooth and clean surface with diameters ranging from 100 nm to 200 nm and lengths typically up to 2μm. High resolution TEM and selected-area electron diffraction shows that the nanorods are pure monoclinic Ga2O3 single crystal. The photoluminescence spectrum indicates that the Ga2O3 nanorods have a good emission property. The growth mechanism is discussed briefly.     

Synthesis and optimum luminescence of monodispersed spheres for BaWO4-based green phosphors with doping of Tb

Monodispersed spheres for Tb³⁺-doped BaWO₄ (BWO:Tb) phosphors were prepared by a hydrothermal method. X-ray diffraction (XRD) and field-emission scanning electron microscopy were used to characterize the resulting samples. Emission and excitation spectra were studied using xenon excited spectroscopic experiments at room temperature. Because 12 at% BWO:Tb phosphor exhibits intensive green emission under 254 nm excitation in comparison with the commercial green fluorescent lamp phosphor (LaPO₄:Ce,Tb), it is considered to be a new promising green phosphor for fluorescent lamps application.     

Facile Synthesis of Single‐Phase Mesoporous Gd2O3:Eu Nanorods and Their Application for Drug Delivery and Multimodal Imaging

In this work, a new and facile strategy is developed to synthesize a single‐phase Eu³⁺‐doped mesoporous gadolinium oxide nanorods (MS‐Gd₂O₃:Eu@PEG) by incorporating a facile wet‐chemical route, which includes an induced silica layer being coated onto the nanorods, and evolution of pores and formation of channels, as well as a surface‐modified process for multimodal imaging and anti‐cancer drug delivery. The properties of these as‐prepared Gd₂O₃:Eu nanorods are characterized by transmission electron microscopy (TEM), X‐ray diffraction (XRD), N₂ adsorption/desorption, and photoluminescence (PL). The in vitro cytotoxicity test, drug loading, and drug release experiments reveal that the MS‐Gd₂O₃:Eu@PEG nanorods have good biocompatibility, efficient loading capacity, and pH‐sensitive releasing behavior, suggesting the nanorods could be an ideal candidate as drug delivery vehicles for cancer therapy. Furthermore, the MS‐Gd₂O₃:Eu@PEG nanorods show clearly dose‐dependent contrast enhancement in T₁‐weighted magnetic resonance images and can potentially be used as a T₁‐positive contrast agent. These results indicate our prepared multifunctional mesoporous gadolinium oxide nanorods can serve as a promising platform for simultaneous anti‐cancer drug delivery and multimodal imaging.     

Synthesis of VO2 (B) nanorods for Li battery application

Vanadium dioxide nanorods were synthesized through a hydrothermal reaction from V₂O₅ xerogel, poly(vinyl pyrrolidone) (PVP) and lithium perchlorate (LiClO₄). The prepared samples were characterized by X-ray diffraction, infrared spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electrochemical discharge–charge cycling in lithium battery. SEM images reveal the nanorods to have dimensions on the order of 1–3 μm in length and 10–50 nm in diameter. The measured initial discharge capacity of the lithium battery with a cathode made of VO₂ (B) nanorods was 152 mA h/g.     

Hydrothermal synthesis and optical characteristics of Eu in Zn2SnO4 nanocrystals

Zn₂SnO₄:Eu³⁺ nanocrystals were one-step synthesized by hydrothermal method for the first time. All the products were systematically characterized by powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron probe X-ray microanalyzer (EPMA), photoluminescence (PL) and photoluminescent excitation (PLE). The characteristic peak of Eu³⁺-doped in Zn₂SnO₄ nanocrystals was also detected. The luminescent properties of blank and Eu³⁺-doped Zn₂SnO₄ nanocrystals were reported.     

Soft chemistry routes for synthesis of rare earth oxide nanoparticles with well defined morphological and structural characteristics

Phosphors of (Y_0.75Gd_0.25)₂O₃:Eu³⁺ (5 at.%) have been prepared through soft chemistry routes. Conversion of the starting nitrates mixture into oxide is performed through two approaches: (a) hydrothermal treatment (HT) at 200 °C/3 h of an ammonium hydrogen carbonate precipitated mixture and (b) by thermally decomposition of pure nitrate precursor solution at 900 °C in dispersed phase (aerosol) within a tubular flow reactor by spray pyrolysis process (SP). The powders are additionally thermally treated at different temperatures: 600, 1000, and 1100 °C for either 3 or 12 h. HT—derived particles present exclusively one-dimensional morphology (nanorods) up to the temperatures of 600 °C, while the leaf-like particles start to grow afterward. SP—derived particles maintain their spherical shape up to the temperatures of 1100 °C. These submicron sized spheres were actually composed of randomly aggregated nanoparticles. All powders exhibits cubic Ia-3 structure (Y_0.75Gd_0.25)₂O₃:Eu and have improved optical characteristics due to their nanocrystalline nature. The detailed study of the influence of structural and morphological powder characteristics on their emission properties is performed based on the results of X-ray powder diffractometry, scanning electron microscopy, X-ray energy dispersive spectroscopy, transmission electron microscopy, and photoluminescence measurements.