Simple and low temperature preparation and characterization of CdS nanoparticles as a highly efficient photocatalyst in presence of a low-cost ionic liquid

A simple and low temperature method is proposed for preparation of CdS nanoparticles in presence of 1-ethyl-3-methylimidazolium ethyl sulfate, [EMIM] [EtSO₄], a room-temperature ionic liquid (RTIL). The powder X-ray diffraction (XRD) studies display that the products are excellently crystallized in the form of cubic structure and size of the nanparticles prepared in presence of the RTIL is smaller than that prepared in water. Energy dispersive X-ray spectroscopy (EDX) investigations reveal that the products are very pure and nearly stoichiometric. The results obtained by scanning electron microscopy (SEM) demonstrate that the CdS nanoparticles prepared in presence of the RTIL have lower tendency for aggregation relative to the prepared sample in water. Diffuse reflectance spectra (DRS) of the product prepared in the neat RTIL, shows 1.52 eV blue shift relative to bulk CdS, which can be attributed to quantum confinement effect of the CdS nanoparticles. A possible formation mechanism for CdS nanoparticles in presence of the RTIL is presented. Photocatalytic activity of the CdS nanoparticles towards photodegradation of methylene blue (MB) using UV and visible lights was performed. The results demonstrate that observed firstorder rate constant for photodegradation of MB on CdS nanoparticles prepared in the neat RTIL are about 20 and 6 times greater than the prepared sample in water using visible and UV lights, respectively.     

微波辐射对纳米ZnO材料物理性质与光催化活性的影响

在采用沉淀法制备ZnO的过程中, 用不同功率(100, 150, 200, 250和300 W)的微波辐射ZnO前驱体, 获得了一系列纳米ZnO材料, 并对合成材料的晶型结构、 形貌及表面物理化学性质进行了表征. 结果表明, 与普通沉淀法制备的ZnO相比, 使用微波辐射后ZnO半导体材料的晶型仍为六方纤锌矿结构, 但吸收光谱发生了蓝移或红移, 且比表面积均有不同程度的增加. 同时, 微波辐射功率不同, ZnO形貌差异明显, 并随着微波功率变化分别呈现纳米颗粒、 椭圆形纳米团簇、 纳米片和球状纳米簇等多样化形态. 以罗丹明B为模型分子, 分别在紫外及微波辅助光催化条件下考察了所合成纳米ZnO材料的光催化性能. 结果显示, 经不同功率微波辐射作用后, ZnO的光催化活性均得到了不同程度的提高, 并且明显高于市售P25和未经微波辐射作用的ZnO.     

Antibacterial and Photocatalytic Properties of ZnO Nanoparticles Obtained from Chemical versus Saponaria officinalis Extract-Mediated Synthesis

In the present work, the properties of ZnO nanoparticles obtained using an eco-friendly synthesis (biomediated methods in microwave irradiation) were studied. Saponaria officinalis extracts were used as both reducing and capping agents in the green nanochemistry synthesis of ZnO. Inorganic zinc oxide nanopowders were successfully prepared by a modified hydrothermal method and plant extract-mediated method. The influence of microwave irradiation was studied in both cases. The size, composition, crystallinity and morphology of inorganic nanoparticles (NPs) were investigated using dynamic light scattering (DLS), powder X-ray diffraction (XRD), SEM-EDX microscopy. Tunings of the nanochemistry reaction conditions (Zn precursor, structuring agent), ZnO NPs with various shapes were obtained, from quasi-spherical to flower-like. The optical properties and photocatalytic activity (degradation of methylene blue as model compound) were also investigated. ZnO nanopowders’ antibacterial activity was tested against Gram-positive and Gram-negative bacterial strains to evidence the influence of the vegetal extract-mediated synthesis on the biological activity.     

ZnO-based ternary nanocomposite for decolorization of methylene blue by photocatalytic dynamic membrane

In this article, novel Ag–ZnO/g-C₃N₄/GO ternary nanocomposites were prepared via co-precipitation method by 1%w Ag, 50% w g-C₃N₄, 10% w GO concentration and applied in dynamic membranes. The characteristics of Ag–ZnO/g-C₃N₄/GO nanocomposite were evaluated by various techniques such as X-ray diffraction, field emission scanning electron microscopy, energy dispersive X-ray map, transmission electron microscopy, X-ray photoelectron spectroscopy, photocatalyst. The photocatalytic degradation of methylene blue was investigated under visible light. The photocatalytic efficiency of 93.43% for methylene blue degradation was obtained for Ag–ZnO/g-C₃N₄/GO nanocomposite after 50 min of irradiation, which was remarkably higher than that of pure ZnO, bare g-C₃N₄, Ag–ZnO, and Ag–ZnO/g-C₃N₄ at the same irradiation time. Likewise, in self-forming and pre-coated membranes, ternary nanocomposites can play a vital role in the membrane surface properties, as well as their decolorization performance. The rejection of methylene blue was 30% in pure polyethersulfone membrane, while the photocatalytic degradation of methylene blue in Ag–ZnO/g-C₃N₄/GO nanocomposites was 88.46% and 98.86% after 10 and 15 min of irradiation in both self-forming and pre-coated dynamic membranes, respectively. Experimental results show that the dynamic membrane possesses a higher ability for degradation of MB in a shorter period of time than the static system.     

Time growing comparison for ZnO nanorod by using microwave irradiation method

In this study, zinc oxide (ZnO) nanorod were successfully prepared at different growth times (15, 30 and 60 min) using the microwave irradiation method. The ZnO nanorods were simply synthesized at a low temperature (90 °C) with low power microwave assisted heating (about 100 W) and a subsequent ageing process. The synthesized nanorod were characterized using X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and Ultraviolet–Visible spectroscopy (UV–Vis). The FESEM images showed nanorods with diameter ranging between 50 and 150 nm, and length of 150–550 nm. The XRD results indicate that ZnO nanorods of different time of growth exhibits pure wurtzite structure with lattice parameters of 3.2568 and 5.2125 Å. UV–Vis characterization showed that energy gap decreases with increase in time. The result also shows that growth of ZnO at 60 min produces an energy band gap of 3.15 eV. In general, the results of the study confirm that the microwave irradiation method is a promising low temperature, cheap and fast method for the production of ZnO nanostructures.     

形貌可控ZnO微纳米结构的水热合成及光催化性能

以乙醇胺为辅助溶剂,采用水热合成法,制备了花状、梭状和剑状的ZnO微纳米结构。采用扫描电镜(SEM)、X射线衍射(XRD)、光致发光光谱(PL)和拉曼光谱等测试手段对样品的形貌、结构、晶相等进行了表征。结果表明所有样品均为六方纤锌矿结构ZnO;其形貌和结晶度可通过改变物质的量的配比nZn2+/nOH-来调控。探讨了反应物配比对产物形貌结构的影响,乙醇胺对不同形貌ZnO的制备起到至关重要作用。以亚甲基蓝为目标降解物,采用紫外-可见吸收光谱(UV-Vis)并结合低温氮吸附-脱附比表面测试(BET),研究了花状、梭状和剑状ZnO的光催化活性。结果表明,与商用ZnO相比,制备的ZnO具有更好的光催化活性;样品催化活性与其比表面积不成正比,具有最小比表面积的花状ZnO拥有最好的光催化活性,这可能是由于其低的结晶度和特殊的花状形貌所致。     

Use of ionic liquid and microwave irradiation as a convenient, rapid and eco-friendly method for synthesis of novel optically active and thermally stable aromatic polyamides containing N-phthaloyl-l-alanine pendent group

An efficient, fast and easy method for synthesis of new optically active and thermally stable aromatic polyamides (PAs) containing pendent phthalimide group and l-alanine flexible side spacer using room temperature ionic liquid (RTIL) by microwave irradiation has been investigated. The results found that RTIL efficiently absorb microwave energy, thus leading to a very high heating rate. All the PAs showed excellent solubility and readily dissolved in various organic solvents. Thermogravimetric analysis (TGA) exhibited that polymers were stable, with 10% weight loss recorded above 373 and 418 °C in the nitrogen atmosphere. In order to see the efficiency of microwave irradiation, this method was compared with polycondensation of the same monomers in RTILs using conventional heating.     

Microwave-assisted synthesis of ZnO and its photocatalytic activity in degradation of CTAB

Nanosized zinc oxide (nano-ZnO) was prepared by a microwave irradiation method using zinc nitrate and triethanolamine as starting materials and distilled water as a solvent. The as-prepared powder was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic degradation of cetyltrimethylammonium bromide (CTAB) using the prepared material under UV irradiation was studied.The effects of ZnO dosage and initial pH on the photodegradation of CTAB were investigated. As the ZnO load increased, the CTAB degradation first increased and then decreased. The optimum ZnO dosage was 3 g L^–1. Photodegradation of CTAB is more efficient in slightly alkaline media (pH 9).     

圆形片状纳米复合材料Ag/ZnO-ZrO2微波辅助合成与多模式光催化罗丹明B

采用微波辅助结合沉淀法制备了以Zn O为主体的纳米复合材料Ag/Zn O-Zr O_2。通过X射线粉末衍射(XRD)、紫外-可见漫反射吸收光谱(UV-Vis/DRS)、扫描电子显微镜(SEM)、X射线光电子能谱(XPS)和N2吸附-脱附等表征手段研究了微波辐射对Ag/Zn O-Zr O_2晶型结构、形貌及表面物理化学性质的影响。结果表明,在200 W微波辐射作用下,该样品晶型结构未发生明显变化,但Ag的衍射峰明显增强,同时,其晶粒尺寸、光吸收性质和表面物理化学性质等方面则发生改变,尤其是样品Ag/Zn O-Zr O_2的形貌呈现了圆形片状结构。分别在紫外和微波辅助条件下对纳米复合材料的光催化性能进行了一系列考察,同时为了进一步评价所合成样品在太阳光作用下的实用价值,又考察了Ag/Zn O-Zr O_2在模拟日光条件下的光催化性能。结果显示,紫外光作用下,纳米复合材料Ag/Zn O-Zr O_2的光催化活性高于市售P25以及未经微波处理的样品,且在微波辅助光催化条件下,其活性有较大程度提高。200 W微波功率下所合成样品Ag/Zn O-Zr O_2在模拟日光作用下显现出较高活性。另外,根据紫外光条件下对光催化活性物种的捕获实验提出了Ag/Zn O-Zr O_2可能的光催化机理。     

圆形片状纳米复合材料Ag/ZnO-ZrO2微波辅助合成与多模式光催化罗丹明B

采用微波辅助结合沉淀法制备了以ZnO为主体的纳米复合材料Ag/ZnO-ZrO₂。通过X射线粉末衍射(XRD)、紫外-可见漫反射吸收光谱(UV-Vis/DRS)、扫描电子显微镜(SEM)、X射线光电子能谱(XPS)和N2吸附-脱附等表征手段研究了微波辐射对Ag/ZnO-ZrO₂晶型结构、形貌及表面物理化学性质的影响。结果表明, 在200 W微波辐射作用下, 该样品晶型结构未发生明显变化, 但Ag的衍射峰明显增强, 同时, 其晶粒尺寸、光吸收性质和表面物理化学性质等方面则发生改变, 尤其是样品Ag/ZnO-ZrO₂的形貌呈现了圆形片状结构。分别在紫外和微波辅助条件下对纳米复合材料的光催化性能进行了一系列考察, 同时为了进一步评价所合成样品在太阳光作用下的实用价值, 又考察了Ag/ZnO-ZrO₂在模拟日光条件下的光催化性能。结果显示, 紫外光作用下, 纳米复合材料Ag/ZnO-ZrO₂的光催化活性高于市售P25以及未经微波处理的样品, 且在微波辅助光催化条件下, 其活性有较大程度提高。200 W微波功率下所合成样品Ag/ZnO-ZrO₂在模拟日光作用下显现出较高活性。另外, 根据紫外光条件下对光催化活性物种的捕获实验提出了Ag/ZnO-ZrO₂可能的光催化机理。     

Preparation, characterization, and photocatalytic activity of polyaniline/ZnO nanocomposite

Polyaniline (PANI)/zinc oxide (ZnO) nanocomposite was synthesized by in-situ polymerization. X-ray diffraction patterns, UV?Cvisible spectroscopy, SEM, and TEM were used to characterize the composition and structure of the nanocomposite. Nanostructured PANI/ZnO composite was used as photocatalyst in the photodegradation of methylene blue dye molecules in aqueous solution. The photocatalytic activity of PANI/ZnO nanocomposite under UV and visible light irradiation was evaluated and was compared with that of ZnO nanoparticles. ZnO/PANI core?Cshell nanocomposite had greater photocatalytic activity than ZnO nanoparticles and pristine PANI under visible light irradiation. According to these results, application of PANI as a shell on the surface of ZnO nanoparticles causes the enhanced photocatalytic activity of the PANI/ZnO nanocomposite. Also UV?Cvisible spectroscopy studies showed that the absorption peak for PANI/ZnO nanocomposite has a red shift toward visible wavelengths compared with the ZnO nanoparticles and pristine PANI. The effect of different operating conditions on the photocatalytic performance of PANI/ZnO nanocomposite in the photodegradation of methylene blue dye molecules was investigated in a bath experimental setup.     

Speciation of zinc in nano phosphor particulars abstracted in an ionic liquid

Nano size (<100 nm) pollutants have been controlled negligibly in traditional air pollution control devices. Phosphor particulates escaped from filtration systems (bag houses or electrostatic precipitators) of used TVs, monitors or FEDs disassembling processes are frequently found in nano or submicron sizes. Experimentally, in a very short contact time (<2 min), more than 90% of the nano phosphor particulates could be abstracted into room temperature ionic liquid (RTIL) (e.g., [C₄min][PF₆]). The least-square fitted X-ray absorption near edge structural (XANES) spectra show that nano ZnS (88%) and ZnO (12%) could be suspended in the RTIL for at least 10 days.     

Photocatalytic degradation of acid blue 74 in water using Ag–Ag2O–Zno nanostuctures anchored on graphene oxide

Water pollution due to industrial effluents from industries which utilize dyes in the manufacturing of their products has serious implications on aquatic lives and the general environment. Thus, there is need for the removal of dyes from wastewater before being discharged into the environment. In this study, a nanocomposite consisting of silver, silver oxide (Ag₂O), zinc oxide (ZnO) and graphene oxide (GO) was synthesized, characterized and photocatalytically applied in the degradation (and possibly mineralization) of organic pollutants in water treatment process. The Ag–Ag₂O–ZnO nanostructure was synthesized by a co-precipitation method and calcined at 400 °C. It was functionalized using 3-aminopropyl triethoxysilane and further anchored on carboxylated graphene oxide via the formation of an amide bond to give the Ag–Ag₂O–ZnO/GO nanocomposite. The prepared nanocomposite was characterized by UV–Vis diffuse reflectance spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electronic microscopy (SEM), energy dispersive X-ray spectrometry (EDX), Fourier transformed infrared spectroscopy (FTIR), and Raman spectroscopy. The applicability of Ag–Ag₂O–ZnO/GO nanocomposite as a photocatalyst was investigated in the photocatalytic degradation of acid blue 74 dye under visible light irradiation in synthetic wastewater containing the dye. The results indicated that Ag–Ag₂O–ZnO/GO nanocomposite has a higher photocatalytic activity (90% removal) compared to Ag–Ag₂O–ZnO (85% removal) and ZnO (75% removal) respectively and thus lends itself to application in water treatment, where the removal of organics is very important.     

三维球状ZnO纳米簇的微波辅助合成与微波增强光催化降解染料

采用微波辅助合成方法制备了具有高光催化活性的三维球状ZnO纳米簇, 通过X射线衍射(XRD)、 扫描电子显微镜(SEM)、 透射电子显微镜(TEM)以及氮气吸附-脱附测定等手段对材料进行了表征. 结果表明, 纳米ZnO具有纤锌矿晶型结构, 在微波辐射作用下形成了直径约为3~4 μm的球状纳米簇. 该纳米簇内外结构不同, 表面由尺寸均一的ZnO纳米棒紧密整齐排列, 内核由许多ZnO粒子组成的层状骨架构成. 该纳米簇属介孔材料, 其比表面积在微波作用下显著增大. 以染料罗丹明B为模型分子考察了纳米ZnO在微波辐射下的光催化活性, 结果显示, 微波辅助合成球状ZnO纳米簇在微波增强光催化条件下, 催化活性明显高于未经微波处理的ZnO样品和市售P25, 其对多种染料均有显著的降解效果, 40 min内对染料(除甲基橙外)的降解率可达90%以上.     

形貌可控ZnO微纳米结构的水热合成及光催化性能

以乙醇胺为辅助溶剂,采用水热合成法,制备了花状、梭状和剑状的ZnO微纳米结构。采用扫描电镜（SEM）、Ｘ射线衍射（XRD）、光致发光光谱（PL）和拉曼光谱等测试手段对样品的形貌、结构、晶相等进行了表征。结果表明所有样品均为六方纤锌矿结构ZnO;其形貌和结晶度可通过改变物质的量的配比n_Zn²⁺/n_OH^-来调控。探讨了反应物配比对产物形貌结构的影响,乙醇胺对不同形貌ZnO的制备起到至关重要作用。以亚甲基蓝为目标降解物,采用紫外-可见吸收光谱（UV-Vis）并结合低温氮吸附-脱附比表面测试（BET）,研究了花状、梭状和剑状ZnO的光催化活性。结果表明,与商用ZnO相比,制备的ZnO具有更好的光催化活性;样品催化活性与其比表面积不成正比,具有最小比表面积的花状ZnO拥有最好的光催化活性,这可能是由于其低的结晶度和特殊的花状形貌所致。     

Fe3O4纳米晶的粒径控制合成、表征及其吸波性能

采用十二烷基磺酸钠和聚乙二醇作为保护剂, 成功地制备出Fe3O4纳米晶. 通过改变实验条件, 可在10~200 nm范围内有效调控Fe3O4纳米晶的粒径. 采用X射线衍射仪、透射电子显微镜和扫描电子显微镜等对样品的微观结构、粒径和形貌进行了分析. 结果表明, 所得尖晶石型Fe3O4纳米晶粒径均匀, 形貌均为球形. 利用振动样品磁场计测量了不同粒径样品的磁性能. 结果显示, 粒径小时, 随着粒径的增加, Fe3O4的饱和磁化强度Ms逐渐增加, 但当粒径增加到80 nm时, Ms达到最大值; 随着粒径的减小, 矫顽力也随之减小. 利用矢量网络分析仪对不同粒径样品的电磁性能和吸波性能进行了研究, 结果表明, 当Fe3O4纳米晶的粒径小于100 nm时, 吸波性能良好, 其中, 粒径为20 nm的样品吸收峰的峰值在8 GHz附近达到了-32 dB.     

Photocatalytic studies of silver doped ZnO nanoparticles synthesized by chemical precipitation method

Ag-doped ZnO nanoparticles (Zn_1?xAg_xO; where x = 0.00–0.05) were synthesized by chemical precipitation method. The synthesized products were characterized by X-ray diffraction, scanning electron microscope (SEM), transmission electron microscope (TEM) and UV–Vis spectrometer. The SEM and TEM micrographs revealed the agglomerated spherical-like morphology and the measurements show that the size of crystallites is in the range of 10–40 nm. Optical measurements indicated a red shift in the absorption band edge after Ag doping. The band gap values of as prepared undoped and doped with silver samples were found to decrease with increase in temperature from 300 to 800 °C. Photocatalytic activities of ZnO and Ag doped ZnO were evaluated by irradiating the sample solution to ultraviolet light by taking methylene blue as organic dye. The experiment demonstrated that the photo-degradation efficiency of 1 mol% Ag-doped ZnO was significantly higher than that of undoped and 2–5 mol% Ag doped ZnO under ultraviolet light irradiation.     

Microwave assisted hydrothermal synthesis of zinc hydroxystannate films on glass substrates

Zinc stannate (ZnSnO₃, Zn₂SnO₄) and its precursor, i.e. zinc hydroxystannate (ZnSn(OH)₆), have emerged as technological nanomaterials for different applications. Herein, we report synthesis of polycrystalline zinc hydroxystannate (ZHS) film on glass substrate through facile and efficient microwave assisted hydrothermal growth. The method comprises of three steps; deposition of ZnO seed films on glass substrates through spray pyrolysis, growth of ZnO nanorod arrays over the seeded substrates through microwave assisted hydrothermal method and transformation of the as-synthesized ZnO nanorod arrays into the ZHS films through microwave treatment in aqueous precursor solution of SnCl₄ and NaOH. The films were characterized by energy dispersive X-ray spectroscopy, X-ray diffraction and scanning electron microscopy (SEM). The films contain two crystalline phases namely ZnO with [002] as preferred growth direction and ZnSn(OH)₆ preferably grown along [200] vector. The obtained ZHS films consist of crystals of exclusively cubic structure with sizes up to several microns. Microwave irradiation time, NaOH/SnCl₄ molar ratio, concentration of Sn⁴⁺ ions, and the applied power are the four parameters which influence the size, aerial density and growth rate of ZHS microblocks.     

ZnO纳米片/微棒复合体的制备、结构及光学性能

以十六烷基三甲基溴化铵(CTAB)为表面活性剂,以氯化锌和氢氧化钠为原料,在低温水热条件下制备出具有纳米片状接枝结构的ZnO微棒。通过扫描电镜(SEM)、X射线衍射(XRD)、透射电镜(TEM)、光致发光(PL)和拉曼光谱(Raman)对产物的形貌、晶体结构和光学性能进行了表征。结果表明,表面活性剂CTAB对产物最终形貌的形成具有重要作用;微棒表面所接枝的薄片为多晶结构;产物光致发光峰是较少见的弱蓝光发射与强红光发射;同时对这种ZnO微棒的生长机理进行了探讨。     

微波辐射对浆态床合成甲醇CuO/ZnO/Al2O3催化剂前驱体晶相转变的影响

在微波辐射条件下,对CuO/ZnO/Al2O3催化剂的沉淀母液进行老化,通过XRD、TG、H2-TPR,FTIR、HR-TEM和XPS对前驱体及催化剂微观结构的进行表征,探讨了CuO/ZnO/Al2O3催化剂前驱体晶相转变过程中微波辐射的作用。结果表明,微波辐射有利于Cu2+取代Zn5(CO3)2(OH)6中Zn2+的同晶取代反应。微波辐射的老化过程中,首先发生Cu2+取代Zn5(CO3)2(OH)6中Zn2+生成(Cu,Zn)5(CO3)2(OH)6的同晶取代反应,并于1.0 h内基本完成;随着老化时间继续延长,主要进行Zn2+取代Cu2(CO3)(OH)2中Cu2+生成(Cu,Zn)2(CO3)(OH)2的同晶取代反应,同时(Cu,Zn)5(CO3)2(OH)6进一步结晶。与常规老化1 h制备的前驱体相比,微波辐射老化1.0 h制备的前驱体含有较多的(Cu,Zn)5(CO3)2(OH)6物相,有助于增强焙烧后CuO/ZnO/Al2O3催化剂中CuO-ZnO协同作用,提高表面铜含量,进而提高CuO/ZnO/Al2O3催化剂在浆态床合成甲醇的催化活性和稳定性,在400 h浆态床合成甲醇评价期间,甲醇时空收率最大达318.9 g.kg-1.h-1,失活率仅为0.11%.d-1。