Synthesis of Co2+-doped Fe2O3 photocatalyst for degradation of pararosaniline dye

In this paper, x (=2, 5, 7 and 10mol%) Co²⁺-doped Fe₂O₃ (xCo:Fe₂O₃) nanoparticles with enhanced photocatalytic activity have been reported. xCo:Fe₂O₃ nanoparticles were successfully prepared by co-precipitation followed thermal decomposition method. The structural, optical and morphological properties of the prepared samples were studied by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse reflectance (DR) UV–visible absorption spectroscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The obtained results revealed that Co²⁺ ions were well doped within the lattices of Fe₂O₃. Also, Co²⁺ ions suppress the formation of the most stable α- Fe₂O₃ and stabilize less stable γ-Fe₂O₃ at 450 °C. The photocatalytic activity of xCo:Fe₂O₃ was examined by using pararosaniline (PR) dye. It was found that photocatalytic degradation of PR depends on dopant concentration (Co²⁺ ions). Relatively, the highest photocatalytic activity was observed for 5%Co:Fe₂O₃ nanoparticles. The plausible photocatalytic degradation pathway of PR at xCo:Fe₂O₃ surface has also been proposed.     

Patterning of Gd2(WO4)3:Ln3+ (Ln=Eu, Tb) luminescent films by microcontact printing route

Gd(2)(WO(4))(3) doped with Eu(3+) or Tb(3+) thin phosphor films with dot patterns have been prepared by a combinational method of sol-gel process and microcontact printing. This process utilizes a PDMS elastomeric mold as the stamp to create heterogeneous pattern on quartz substrates firstly and then combined with a Pechini-type sol-gel process to selectively deposit the luminescent phosphors on hydrophilic regions, in which a Gd(2)(WO(4))(3):Ln(3+) (Ln=Eu, Tb) precursor solutions were employed as ink. X-ray diffraction (XRD), scanning electron microscopy (SEM), photoluminescence (PL) spectra, as well as low voltage cathodoluminescence (CL) spectra were carried out to characterize the obtained samples. Under ultraviolet excitation and low-voltage electron beams excitation, the Gd(2)(WO(4))(3):Eu(3+) samples exhibit a strong red emission arising from Eu(3+)(5)D(0,1,2)-(7)F(1,2) transitions, while the Gd(2)(WO(4))(3):Tb(3+) samples show the green emission coming from the characteristic emission of Tb(3+) corresponding to (5)D(4)-(7)F(6,5,4,3) transitions. The results show that the patterning of rare earth-doped phosphors through combining microcontact printing with a Pechini-type sol-gel route has potential for field emission displays (FEDs) applications.     

萃取色谱分离—原子发射光谱测定氧化钐,氧化铕,氧化钆中14个稀土杂质

用２－乙基己基膦酸单２－乙基己酯萃取色谱分离－原子发射光谱测定超高纯Ｓｍ２Ｏ３、Ｅｕ２Ｏ３、Ｇｄ２Ｏ３中痕量稀土杂质，可用于纯度为９９９９９９％～９９９９９９９％（不含非稀土杂质）Ｓｍ２Ｏ３、Ｅｕ２Ｏ３、Ｇｄ２Ｏ３的纯度分析，１４个稀土杂质的回收率在６７％～１３３％之间，相对标准偏差±６４％～±１８４％，分离周期１０～１４ｈ。     

Honey-mediated synthesis of Cr2O3 nanoparticles and their potent anti-bacterial,anti-oxidant and anti-inflammatory activities

Green synthesis of nanoparticles has gained tremendous attention in recent era which is pertinent to their unique properties and broad applications. This approach is cost-effective, environment-friendly as well as highly biocompatible. In this research, chromium oxide nanoparticles (Cr₂O₃-NPs) were synthesized by using Apis mellifera honey as a reducing and capping agent and their anti-bacterial, anti-biofilm, anti-oxidant and anti-inflammatory abilities were explored. Ultra Violet-visible double beam spectroscopy revealed that chromium underwent d-d transition during synthesis of nanoparticles. X-ray diffraction (XRD) analysis verified that Cr₂O₃-NPs were crystalline in nature and average crystal size was 24 nm. Energy-dispersive X-ray (EDX) analysis confirmed that chromium and oxygen formed nano-composites in solution which possessed a stable form. Scanning electron microscopy (SEM) provided morphological characteristics of nanoparticles and proved that their average size was 20 nm. Cr₂O₃-NPs displayed excellent anti-bacterial activity (minimum inhibition zone, 20 mm; maximum inhibition zone, 26 mm) against 30 selected clinical isolates of Klebsiella pneumoniae as determined by agar well-diffusion method. Their antibacterial activity was considerably superior to that of three selected antibiotics including Gentamicin, Ciprofloxacin and Cefepime. However, no synergism was observed between nanoparticles and these antibiotics as calculated from fractional inhibitory concentration index (FICI) values all of which were  > 1. The synthesized nanoparticles possessed good biofilm inhibition potential (60 % to 73 %) at all concentrations (20 µg/ml to 50 µg/ml) tested. Cr₂O₃-NPs exhibited excellent anti-oxidant activity (IC₅₀ = 128 µg/ml) which was nearly equivalent to that of ascorbic acid. Anti-inflammatory effect of Cr₂O₃-NPs was also significant (IC₅₀ = 549 µg/ml) and comparable to that of standard. Both anti-oxidant and anti-inflammatory capacities were found to increase with an increase in the concentration of Cr₂O₃-NPs. In conclusion, this work revealed that Apis mellifera honey-mediated synthesis of Cr₂O₃-NPs could be investigated for future biomedical applications.     

Gd2O3:Eu3+ X射线溶胶-凝胶发光薄膜的制备与表征

高分辨率X射线成像系统要求其发光材料同时具有X射线截止本领强、光产额高、余辉短以及与光电器件波长匹配好等特性. Gd2O3:Eu3 因其优越的发光性能和Eu3 红光发射等优点而在高能射线激发发光材料中占有重要地位. 近几年发展起来的透明X射线薄膜发光材料具有更高的衬度和空间分辨率、热传导率、均匀性和附着力等优点[1], 因而有望成为取代传统荧光粉的新一代X射线成像材料. 在各种薄膜制备工艺中, 溶胶-凝胶法以其价格低廉、工艺简单、制备温度低、均匀性好、可实现微量掺杂等优点而日益受到人们重视, 通过该方法并辅以适当的后处理工艺可制备出透明、致密的薄膜.     

Polymerization of aniline derivatives by K2Cr2O7 and production of Cr2O3 nanoparticles

Oxidative polymerization of aniline, anthranilic acid, and aniline‐co‐anthranilic acid by potassium dichromate Cr(VI) as an oxidant in acidic medium was investigated. In this study, the polymerization process of aniline, o‐anthranilic acid as well as aniline/o‐anthranlic acid using K₂Cr₂O₇ produced, coordinated Cr(III)/polyaniline (PANI), Cr(III)/polyanthranilic acid (PAA) and Cr(III)/poly aniline‐co‐anthranilic acid (PANAA). The mechanism of polymerization reaction in the presence of dichromate was hypothesized. The precursor chromium doped polymers were characterized by TGA, FT‐IR, UV‐visible, XRD analyses. Cr₂O₃ nanoparticles size were determined using TEM analysis. The calcinations process of synthesized chromium doped PANI, PAA and PANAA yields Cr₂O₃ nanoparticles 26%, 31%, and 34% wt. respectively. Rhombohedral phase of Cr₂O₃ particles in the range from 33 to 61 nm was produced from chromium/polyanthranilic acid (PAA) and chromium/poly(aniline‐co‐anthranilic acid) PANAA. UV‐ visible analysis showed that optical band gaps (E_g) of doped poly aniline and its derivatives are in the range from1.55 to 1.80 using Tacu's law. The band gap values reveal that the doped chromium emeraldine base can be used as semiconductor materials. Copyright © 2016 John Wiley & Sons, Ltd.     

Preparation, characterization and evaluation of water-soluble l-cysteine-capped-CdS nanoparticles as fluorescence probe for detection of Hg(II) in aqueous solution

Water-soluble l-cysteine-capped-CdS nanoparticles were prepared in aqueous solution at room temperature through a straightforward one-pot process by using safe and low-cost inorganic salts as precursors, and characterized by transmission electron microscopy, X-ray diffraction spectrometry, Fourier transform infrared spectrometry, spectrofluorometry and ultraviolet-visible spectrometry. The prepared l-cysteine-capped-CdS nanoparticles were evaluated as fluorescence probe for Hg(II) detection. The fluorescence quenching of the l-cysteine-capped-CdS nanoparticles depended on the concentration and pH of Hg(II) solution. Maximum fluorescence quenching was observed at pH 7.4 with the excitation and emission wavelengths of 360 nm and 495 nm, respectively. Quenching of its fluorescence due to Hg(II) at the 20 nmol l⁻¹level was unaffected by the presence of 5 × 10⁶-fold excesses of Na(I) and K(I), 5 × 10⁵-fold excesses of Mg(II), 5 × 10⁴-fold excesses of Ca(II), 500-fold excesses of Al(III), 91-fold excesses of Mn(II), 23.5-fold excesses of Pb(II), 25-fold excesses of Fe(III), 25-fold excesses of Ag(I), 8.5-fold excesses of Ni(II) and 5-fold excesses of Cu(II). Under optimal conditions, the quenched fluorescence intensity increased linearly with the concentration of Hg(II) ranging from 16 nmol l⁻¹ to 112 nmol l⁻¹. The limit of detection for Hg(II) was 2.4 nmol l⁻¹. The developed method was applied to the detection of trace Hg(II) in aqueous solutions.     

Synthesis,characterization and application of Cr2O3 nanoparticles as an efficient antibacterial agent

This study focuses on the microwave-assisted synthesis of Cr₂O₃ nanoparticles for the development of antibacterial materials. Characterization techniques including FT-IR spectroscopy, UV–vis spectroscopy, SEM-EDX, and XRD, were employed to analyze the nanoparticles' properties. The antibacterial efficacy against E. coli, S. aureus, B. subtilis, and P. aeruginosa was evaluated, with significant activity observed against all pathogens, highlighting their potential as antibacterial materials. The novelty of this study lies in the synthesis of Cr₂O₃ nanoparticles and their application as potent antibacterial agents against various pathogens. The results of XRD study concludes the average size of Cr₂O₃ nanoparticles as 49.96 nm. The synthesized Cr₂O₃ nanoparticles demonstrated a good zone of inhibition against E. coli (22 mm), S. aureus (19 mm), B. subtilis (18 mm), and P. aeruginosa (21 mm). The findings of the study suggest that Cr₂O₃NPs have potential as a novel antibacterial agent, and further research in this area could lead to the development of new and effective treatments for bacterial infections.     

Gd_3Al_5O_(12)∶Eu~(3+)柠檬酸盐硝酸盐燃烧法合成及其发光性能研究

采用柠檬酸盐硝酸盐燃烧法,在较低的温度(900℃)下成功地合成单一晶相Gd3Al5O12∶Eu3+发光粉体,紫外激发荧光光谱分析表明,粉体615 nm和593 nm荧光发射源于Eu3+的5D0-7F2和5D0-7F1跃迁.该方法中各工艺条件(如pH值、柠檬酸/金属离子比、煅烧温度)对Gd3Al5O12∶Eu3+发光性能均有影响,通过试验得出了获得最佳发光性能荧光粉体的工艺参数.     

Assembly of Pt nanoparticles on electrospun In2O3 nanofibers for H2S detection

In this paper, we presented a simple and effective solution route to deposit Pt nanoparticles on electrospun In₂O₃ nanofibers for H₂S gas detection. The morphology and chemical structure of the as-prepared samples were analyzed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectra (XPS). The results showed that large quantities of In₂O₃ nanofibers with diameters about from 60 to 100 nm were obtained and the surface of them was decorated with Pt nanoparticles (5–10 nm in size). The In₂O₃ nanofibers decorated by Pt nanoparticles exhibited excellent gas sensing properties to H₂S, such as high sensitivity, good selectivity and fast response at relatively low temperature.     

Investigation of Luminescence Properties of Eu3+, Dy3+ and Gd3+ Doped MgAl2Si2O8 Red‐emitting Phosphors

Rare‐earth‐doped aluminosilicates of alkaline earth MgAl₂Si₂O₈: Eu³⁺, Dy³⁺ and MgAl₂Si₂O₈: Eu³⁺, Gd³⁺ were synthesized by the solid state reaction method at 1300 ^oC. The phosphors were characterized by X‐ray powder diffraction (XRD), photoluminescence (PL), thermoluminescence (TL) and scanning electron microscopy (SEM). X‐ray powder diffraction studies show that the phosphors were crystallized in the triclinic crystal system. The phosphors show characteristic broad band phosphorescence of Eu³⁺. This broad band phosphorescence has red emission bands in the range of 580–705 nm corresponding to ⁵D₀ → ⁷F_j (j:0,2,3,4) transitions of Eu³⁺.     

Synthesis and characterization of Gd2O3:Eu phosphor nanoparticles by a sol-lyophilization technique

The characterization and luminescence properties of nanostructured Gd₂O₃:Eu³⁺ phosphors synthesized by a sol-lyophilization process are presented. After preparation of gadolinium-based sols from gadolinium nitrate and ammonium hydroxide, the so-prepared sols were freeze dried at −10°C and calcinated at different temperatures. For temperatures lower than 1300 K, highly crystalline samples with the cubic structure can be obtained without concomitant grain growth of the particles (<50 nm). The luminescence spectra contain all possible transitions of Eu³⁺ with C₂ symmetry and present two major features: an increase of the luminescence efficiencies of the phosphors in comparison with that obtained by solid-state reaction and the presence of an additional peak at about 609 nm at the vicinity of the ⁵D₀→⁷F_0…4 transition.     

共沉淀法制备参数对(Y，Gd)2O3∶Eu3+纳米粉体性能的影响

采用氨水为沉淀剂,正向滴定共沉淀法制备(Y,Gd)2O3:Eu3+纳米粉体.用XRD、SEM和荧光光度计对粉体的形貌和特性进行了分析.结果表明:稀土溶液的起始浓度0.15 mol·L-1,体系温度0℃,滴定速度2 mL·min-1,静止12 h,添加3%(NH4)2SO4(质量分数)并且在800℃煅烧2 h的条件下,合成出(Y,Cd)2O3:Eu3+纳米粉体近似球形,粒径尺寸约为30～60 nm且分散性良好.添加3%(NH4)2SO4的含量能够改善(Y,Gd)2O3:Eu3+纳米粉体的发光性能,并使发射光谱在5D0→7F2跃迁态上获得最大的相对发光峰值.     

Synthesis and crystal structure of [Ln(4-Pyta)3(H2O)2] n (Ln = Nd,Ce, Eu,Gd; 4-Pyta = 4-pyridylthioacetate)

Four new lanthanide complexes, [Nd(4-Pyta)₃(H₂O)₂] _n (1), [Ce(4-Pyta)₃(H₂O)₂] _n (2), [Eu(4-Pyta)₃(H₂O)₂] _n (3) and [Gd(4-Pyta)₃(H₂O)₂] _n (4), have been obtained from reaction of lanthanide(III) nitrate with 4-Pyta (4-pyridylthioacetate) in water. Their structures were characterized by elemental analysis, infrared spectroscopy and single-crystal X-ray diffraction. The crystals belong to triclinic, space group P 1 and all complexes exhibit one-dimensional chains that arrange to form a three-dimensional supramolecular architecture by hydrogen bonds between the chains.     

Synthesis of Au/SnO2 core-shell structure nanoparticles by a microwave-assisted method and their optical properties

Au/SnO₂ core-shell structure nanoparticles were synthesized using the microwave hydrothermal method. The optical and morphological properties of these particles were examined and compared with those obtained by the conventional hydrothermal method. In microwave preparation, the peak position of the UV-visible plasmon absorption band of Au nanoparticles was red-shifted from 520 to 543 nm, due to the formation of an SnO₂ shell. An SnO₂ shell formation was complete within 5 min. The thickness of the SnO₂ shell was 10-12 nm, and the primary particle size of SnO₂ crystallites was 3-5 nm. For the core-shell particles prepared by a conventional hydrothermal method, the shell formed over the entire synthesis period and was not as crystalline as those produced, using the microwave method. The relationship between the morphological and spectroscopic properties and the crystallinity of the SnO₂ shell are discussed.     

Hydrothermal Synthesis of Rare Earth Iodates from the Corresponding Periodates: II1). Synthesis and Structures of Ln(IO3)3 (Ln = Pr,Nd, Sm,Eu, Gd,Tb, Ho,Er) and Ln(IO3)3 · 2H2O (Ln = Eu,Gd, Dy,Er, Tm,Yb)

Single crystals of lanthanide iodates have been quickly grown by decomposition of the corresponding periodates under hydrothermal conditions. Single crystal X‐ray diffraction showed that two structure types form with the elements from Pr‐Yb, an anhydrous form for Pr, Nd, Sm, Eu, Gd, Tb, Ho, Er and a dihydrate for Eu, Gd, Dy, Er, Tm, Yb. A detailed structure study is presented for one representative of each of these types, along with structure type and lattice parameters for the other materials. Tb(IO₃)₃: Space group P2₁/c, Z = 4, lattice dimensions at 120 K: a = 7.102(1), b = 8.468(1), c = 13.355(2)Å, β = 99.67(1)°; R1 = 0.034. Yb(IO₃)₃ · 2H₂O: Space group P1¯, Z = 2, lattice dimensions at 120 K: a = 7.013(1), b = 7.370(1), c = 10.458(2)Å, α = 95.250(5), β = 105.096(5), γ = 109.910(10)°; R1 = 0.024.     

β-Ga2O3∶Cr3+近红外长余辉纳米颗粒的制备及发光性能

以三乙二醇为表面配体, 利用沉淀法制备了β-Ga₂O₃∶Cr³⁺近红外(NIR)长余辉纳米颗粒. 考察了反应条件对β-Ga₂O₃∶Cr³⁺的发光性能和晶体结构的影响, 并初步探讨了其NIR余辉发光机理. 结果表明, 当溶液的pH值为7, 煅烧温度为700 ℃时, 可获得高纯度的β-Ga₂O₃∶Cr³⁺纳米颗粒, 其平均粒径为30 nm, 最大余辉发射波长可调控为750 nm, NIR余辉发光时间长于384 h. 本方法得到的β-Ga₂O₃∶Cr³⁺长余辉纳米颗粒不仅尺寸小, 而且NIR余辉时间长, 发射波长可调控, 在低背景噪音的深组织活体成像中具有潜在的应用前景.     

Synthesis and physico-chemical characterization of Au/TiO2 nanostructures formed by novel “cold” and “hot” nanosoldering of Au and TiO2 nanoparticles dispersed in water

A novel approach to synthesize Au/TiO₂ nanostructures with interesting optical properties is presented and discussed. It is based on the nanoparticle “cold” or “hot” nanosoldering occurring when two water suspensions of Au and TiO₂ nanoparticles are merely mixed at room temperature or laser irradiated after mixing.Thanks to the high fraction and mutual reactivity of surface species, immediately after the mixing process, the encounters between Au and TiO₂ nanoparticles in liquid phase are enough for “cold” nanosoldering of gold nanoparticles onto TiO₂ nanoparticles to occur. The optical characterizations show that this fast process (timescale less than 1 min) is followed by a slower process, attributable to some change of the Au nanoparticles. This latter process is significantly accelerated by the 532 nm laser light illumination. The structural and optical properties of “cold” and “hot” nanosoldered Au-TiO₂ nanoparticles were investigated by TEM, UV-vis and fluorescence spectroscopies.Interesting optical limiting response was detected at laser fluences above 0.8 J/cm². The nature of the nonlinear effect was investigated by the Z-scan technique, determining both the nonlinear absorption coefficient and the refraction index. Such interesting non-linear optical properties are worth to be tailored for specific applications.     

Phase structure and luminescence properties of Eu3+-doped TiO2 nanocrystals synthesized by Ar/O2 radio frequency thermal plasma oxidation of liquid precursor mists

Eu3+-doped TiO2 luminescent nanocrystals have been synthesized in this work via Ar/O2 thermal plasma oxidizing mists of liquid precursors containing titanium tetra-n-butoxide and europium(III) nitrate, with varied O2 input in the plasma sheath (10-90 L/min) and Eu3+ addition in the precursor solution (Eu/(Ti + Eu) = 0-5 atom%). The resultant nanopowders are mixtures of the anatase (30-36 nm) and rutile (64-83 nm) polymorphs in the studied range, but the rutile fraction increases steadily at a higher Eu3+ addition, as revealed by X-ray diffraction (XRD) and Raman spectroscopy, because of the creation of oxygen vacancies in the TiO2 gas clusters by substitutional Eu3+ doping. The amount of Eu3+ that can be doped into a TiO2 lattice was limited up to 0.5 atom%, above which Eu2Ti2O7 pyrochlore was formed in the final products. High resolution transmission electron microscopy (HRTEM) observation indicates that the particles are dense and have sizes ranging from several nanometers up to 180 nm. Efficient nonradiative energy transfer from the TiO2 host to Eu3+ ions, which was seldom reported in the wet-chemically derived nanoparticles or thin films of the current system, was confirmed by combined studies of excitation, UV-vis (ultraviolet-visible), and PL (photoluminescence) spectroscopy. As a consequence of this, bright red emissions were observed from the plasma-generated nanopowders either by exciting the TiO2 host with UV light shorter than 405 nm or by directly exciting Eu3+ at a wavelength beyond the absorption edge (405 nm) of TiO2.     

CaF_2微晶玻璃的一步法制备及Eu~(3+)离子探针特性

以组成为n(SiO_2)∶n(Al2O3)∶n(CaO)∶n(CaF_2)∶n(NaF)∶n(B_2O_3)=40∶20∶10∶10∶15∶5的微晶发光玻璃为基质,采用一步析晶法制备了CaF_2析晶相.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、X射线能量散射谱仪(EDS)和荧光分光光度计等对样品结构、组成及光谱性能进行分析,探讨了Eu3+掺杂浓度和析晶温度对微晶玻璃发光性能的影响.实验结果表明,在850℃下处理可获得分布均匀、粒径尺寸为200 nm的CaF_2析晶相,微晶玻璃的发光强度是基质玻璃的1.7倍.微晶玻璃的发射光谱在590,614,652和700 nm出现发射峰,分别对应Eu3+的5D0-7FJ(J=1,2,3,4)跃迁.通过对5D0-7F1和5D0-7F2跃迁强度的分析以及Judd-Ofelt理论参数Ω2值的计算可知Eu3+周围晶体场在析晶前后对称性发生变化.机理分析表明,析晶处理后Eu3+从高声子能量的Si-O环境进入低声子能量的Ca-F环境中,说明Eu3+可作为荧光探针研究微晶玻璃晶体结构的变化.