花状ZnO的水热合成与表征

以金属锌为原料,引入偶联表面活性剂作为晶体生长控制剂,在温和的水热条件(150℃)下一步合成了花状纳米结构的ZnO.使用XRD,TEM,SEM,SAED等测试手段,对产物的化学组成和形貌特征进行了分析和表征.结果表明,花状ZnO纳米结构由ZnO纳米棒组成,该ZnO纳米棒为六方晶系且表现为单晶性质.ZnO纳米棒纯度高、粒径较小、长直、光滑而且大多一端聚集而另一端向四周放射性分布,呈较完美的花状结构.初步探讨了ZnO单晶纳米棒和花状ZnO纳米结构的形成机理.分析表明,ZnO纳米棒及其花状结构的形成与偶联表面括性剂特殊的性质及分子结构有关.     

ZnO纳米棒的形貌控制规律及脱硫性能EI北大核心CSCD

在催化领域,氧化锌纳米棒因其在径向上具有纳米粒子的小尺寸效应、纵向上具有体相材料的宏观特性,而受到越来越多的关注。采用改进的溶剂热法合成ZnO纳米棒,采用分步法加入Zn^(2+)与NaOH。通过X射线衍射,扫描电子显微镜等方法对样品进行表征,探究了聚乙二醇(PEG)辅助ZnO纳米棒合成的作用机理以及NaOH的加入方式对ZnO纳米棒形貌控制规律的影响,研究了不同长/径的ZnO纳米棒的脱硫性能。结果表明:PEG的分子量对ZnO纳米棒的形貌有着显著影响,PEG分子量为20000时,能够在温和的溶剂热条件下,控制合成出长度为3~4μm,直径为250 nm左右的ZnO纳米棒,分步法加入NaOH优于一步法加入NaOH。将合成的ZnO纳米棒负载金属氧化镍制成脱硫剂,大长/径的棒状ZnO脱硫剂的脱硫率高达98.2%,同时具有良好的再生性能。     

表面修饰的纳米ZnO的加入对PEG结晶的影响

在PEG溶液中加入纳米ZnO以及表面修饰的ZnO,观察纳米粒子对PEG结晶的影响。通过透射偏光显微镜进行观察,发现纳米ZnO的加入改变了PEG的结晶形貌,随着纳米粒子表面羧基含量的增加,结晶形貌按照树晶—大球晶—小球晶的规律变化。通过FTIR表明在热作用下纳米粒子表面的羧基会与PEG的端羟基发生酯化反应,使纳米ZnO可以稳定的存在于PEG溶液中,为球晶的形成提供了成核点。     

溶剂热法合成氧化锌纳米棒

采用PEG辅助溶剂热合成了ZnO纳米棒,通过SEM、EDS和XRD等手段对产物进行了表征。结果显示,合成的ZnO纳米棒直径在20 nm左右,长大约150,且长度和直径分布均匀。研究了PEG的添加量对形成ZnO纳米棒的影响,并且探讨了PEG促进纳米棒生长的机理。     

微乳液法制备纳米氧化锌粒子

采用微乳液法制备了纳米ZnO粒子,探讨了影响纳米ZnO粒子生成的因素.结果表明,最佳工艺条件为主表面活性剂与助表面活性剂之比为3:1、煅烧温度600℃、煅烧时间3 h.并用红外光谱、透射电子显微镜(TEM)等对产物进行了表征,所制备的纳米ZnO粒子粒径为20nm左右,形貌为球型或类球型.     

ZnO/ZnS异质结构纳米棒的制备及性能研究

本文利用低温二步水热法在ITO玻璃衬底上制备了ZnO/ZnS异质结构纳米棒,研究和比较了Zn O纳米棒和ZnO/ZnS异质结构纳米棒的形貌,结构和光学等特性。结果表明:未掺杂的ZnO纳米棒具有明显的六角结构表面,良好的晶体结构和c轴生长取向;ZnO/ZnS异质结构纳米棒的形貌和光学性质都发生了变化,纳米棒直径变化范围大,六角结构表面六边形不规则,且引入了较多的深能级缺陷。     

简捷微波合成氧化锌纳米棒

以氯化锌和乙二胺的水溶液为前驱体溶液,采用家用微波炉微波辐照8min,成功制备出结晶性好的半导体ZnO纳米棒.用X-射线衍射(XRD)、选区成份分析(EDS)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)和选区电子衍射花样(SAED)对产物进行了表征.结果表明,纳米棒沿着c轴择优取向生长,直径在50nm左右,长度在400～600 nm之间,粒径分布均匀.并对ZnO纳米棒的生长过程进行了简单分析.     

反应条件对氢氧化钇及氧化钇形貌的影响

以氨水和硝酸钇为原料制备氧化钇前驱体,考察表面活性剂及其用量对晶粒形貌和尺寸的影响;并在水热条件下研究体系pH、温度及时间对沉淀重整效果的影响.用XRD,SEM技术检测样品的晶型、尺寸和形貌.结果显示,阴离子型表面活性剂的浓度对一级晶粒的尺寸有较明显的影响,而阳离子型表面活性剂和非离子型表面活性剂的浓度对一级晶粒的尺寸的影响不明显.水热条件下对沉淀进行重整,可制备氢氧化钇纳米棒,溶液的碱浓度、温度及时间影响纳米棒的直径和长度.样品经600 ℃焙烧2 h,可制得立方晶相氧化钇,一级晶粒7～20 nm;氢氧化钇纳米棒焙烧后形成的氧化钇仍具有棒状结构.     

ZnO纳米棒的制备及其光催化活性研究

以Zn(Ac)2·2H2O、NaI和N2H4·H2O为原料,在未使用任何表面活性剂的简单水热反应体系中制得了ZnO纳米棒.采用X射线粉末衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)对产物的晶体结构、形貌进行了表征分析,并对其光催化活性进行了探讨,以ZnO纳米棒为光催化剂对有机染料污染物甲基橙进行了光催化降解实验.实验结果表明,氧化锌纳米棒对甲基橙的光催化降解具有很好的催化作用,在紫外光照射120min后,对甲基橙的降解率接近完全.     

ZnO纳米棒的制备和气敏性质

以二水合醋酸锌为原料,以十二烷基苯磺酸钠为表面修饰剂,利用微乳液法合成了结晶良好的ZnO纳米棒.利用X射线衍射仪、扫描电子显微镜和高分辨透射电子显微镜对所得产物的晶体结构和形貌进行了表征.结果表明:所得的ZnO纳米棒具有六方纤锌矿结构,且尺寸分布均匀,直径为20～30 nm,长度为1.0 μm.利用所得ZnO纳米棒制备...     

Low‐temperature synthesis of nano‐to‐submicron size organo‐zinc oxide and its effect on properties of polybutadiene rubber

Nano‐to‐submicron sized particles of zinc oxide (ZnO) were synthesized by low temperature hydrolysis method. Organo‐ZnO was also synthesized by the aforementioned method in presence of polyethylene glycol (PEG‐2000). The synthesized ZnO particles were characterized by infra‐red spectroscopy, X‐ray diffraction, BET surface area, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). FTIR showed that PEG was present on the ZnO surface. Organo‐ZnO exhibited floral‐shape morphology consisting of concentric nanorods. The average diameter of the nanorods was ～ 250 nm as evident from SEM. TEM showed that the nanorods were made of ～ 50 nm sized small particles. UV‐absorbance property of ZnO was unaltered even after organic coating. Curing, physico‐mechanical and thermal properties of polybutadiene rubber compounded with organo‐ZnO were compared with those of standard commercial rubber grade ZnO and nano‐ZnO prepared by high and low temperature methods. The cure‐characteristics were studied with the help of moving die rheometer as well as differential scanning calorimetry (DSC). Crosslink‐density measurement along the DSC vulcanization exotherm showed better cure efficiency of organo‐ZnO. Organo‐ZnO containing compound exhibited better mechanical and thermal properties. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Structural and photoluminescence studies on catalytic growth of silicon/zinc oxide heterostructure nanowires

Silicon/zinc oxide (Si/ZnO) core-shell nanowires (NWs) were prepared on a p-type Si(111) substrate using a two-step growth process. First, indium seed-coated Si NWs (In/Si NWs) were synthesized using a plasma-assisted hot-wire chemical vapor deposition technique. This was then followed by the growth of a ZnO nanostructure shell layer using a vapor transport and condensation method. By varying the ZnO growth time from 0.5 to 2 h, different morphologies of ZnO nanostructures, such as ZnO nanoparticles, ZnO shell layer, and ZnO nanorods were grown on the In/Si NWs. The In seeds were believed to act as centers to attract the ZnO molecule vapors, further inducing the lateral growth of ZnO nanorods from the Si/ZnO core-shell NWs via a vapor-liquid-solid mechanism. The ZnO nanorods had a tendency to grow in the direction of [0001] as indicated by X-ray diffraction and high resolution transmission electron microscopy analyses. We showed that the Si/ZnO core-shell NWs exhibit a broad visible emission ranging from 400 to 750 nm due to the combination of emissions from oxygen vacancies in ZnO and In₂O₃ structures and nanocrystallite Si on the Si NWs. The hierarchical growth of straight ZnO nanorods on the core-shell NWs eventually reduced the defect (green) emission and enhanced the near band edge (ultraviolet) emission of the ZnO.     

Growth temperature dependent properties of ZnO nanorod arrays on glass substrate prepared by wet chemical method

In this work, ZnO nanorod arrays were grown on glass substrate by the wet chemical method, and the effect of synthesis temperature on the properties was investigated. The grown nanorods were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Raman and Photoluminescence (PL) measurements. XRD pattern showed that nanorod prepared at 80 °C and 90 °C has high crystallinity with wurtzite structure and orientated along the c-axis. However, nanorods were not formed at 60 °C and 70 °C due to less energy supply for the growth of the ZnO. FE-SEM results showed that the morphology and the size of ZnO can be effectively controlled. In particular, as the temperature increased, diameter of the nanorod was increased while length decreased. Raman scattering spectra of ZnO nanorod arrays revealed the characteristic E₂^high mode that is related to the vibration of oxygen atoms in the wurtzite ZnO. Room-temperature PL spectra of the ZnO nanorods revealed a near-band-edge (NBE) emission peak. The NBE (UV light emission) band at ~383 nm might be attributed to the recombination of free exciton. The narrow full-width at half-maximum (FWHM) of the UV emission indicated that ZnO nanorods had high crystallinity.     

Preparation of ZnO nanorod by solvothermal reaction of zinc acetate in various alcohols

Solvothermal reaction of zinc acetate in various alcohols resulted in the formation of zinc oxide (ZnO) nanorods. The effects of reaction conditions on the product morphology as well as crystallization mechanism were investigated by using X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and transmission electron microscopy (TEM) techniques. It was found that average diameter and length of the nanorods increased with an increase in reaction temperature or the initial concentration of zinc acetate. On the contrary, the aspect ratio of the product depended upon type of alcohol used as the reaction medium. The aspect ratio of ZnO nanorods increased from 1.7 to 5.6 when the alcohol was changed from 1-butanol to 1-decanol. An investigation of the reaction mechanism suggested that the formation of ZnO nanorods was initiated from the esterification reaction between zinc acetate precursor and alcohol to form ZnO seeds.     

Growth of vertically aligned ZnO nanorods using textured ZnO films

A hydrothermal method to grow vertical-aligned ZnO nanorod arrays on ZnO films obtained by atomic layer deposition (ALD) is presented. The growth of ZnO nanorods is studied as function of the crystallographic orientation of the ZnO films deposited on silicon (100) substrates. Different thicknesses of ZnO films around 40 to 180 nm were obtained and characterized before carrying out the growth process by hydrothermal methods. A textured ZnO layer with preferential direction in the normal c-axes is formed on substrates by the decomposition of diethylzinc to provide nucleation sites for vertical nanorod growth. Crystallographic orientation of the ZnO nanorods and ZnO-ALD films was determined by X-ray diffraction analysis. Composition, morphologies, length, size, and diameter of the nanorods were studied using a scanning electron microscope and energy dispersed x-ray spectroscopy analyses. In this work, it is demonstrated that crystallinity of the ZnO-ALD films plays an important role in the vertical-aligned ZnO nanorod growth. The nanorod arrays synthesized in solution had a diameter, length, density, and orientation desirable for a potential application as photosensitive materials in the manufacture of semiconductor-polymer solar cells.

PACS

61.46.Hk, Nanocrystals; 61.46.Km, Structure of nanowires and nanorods; 81.07.Gf, Nanowires; 81.15.Gh, Chemical vapor deposition (including plasma-enhanced CVD, MOCVD, ALD, etc.)     

Morphological exploration of chemical vapor–deposited P-doped ZnO nanorods for efficient photoelectrochemical water splitting

Photoelectrochemical (PEC) water splitting is beneficial and has received attractive attention due to a greater potential to generate hydrogen and oxygen from water by using plentiful solar light to solve the problem of energy crisis. Various active semiconductor materials are used in PEC water splitting applications. Nevertheless, in past decades, most of the researchers suggested that titanium oxide (TiO₂) is the best photoanode for this type of applications. Now, Zinc oxide (ZnO) is considered a perfect substitution to TiO₂ due to its comparable energy band structure and superior photogenerated electron transfer rate. In this study, bare and phosphorous-doped ZnO nanorods were successfully developed on fluorine-doped tin oxide-coated glass (FTO) substrate by chemical vapor deposition. X-ray diffraction (XRD) pattern authenticated hexagonal structure formation with strong diffraction peak of (101), which showed that ZnO nanorods were perfectly developed along c axis. The optical and morphological properties were analyzed by UV–Vis and scanning electron microscopy images. The energy-dispersive X-ray spectra demonstrated that doping agent phosphorous was present in ZnO nanorods. The PEC properties of the developed ZnO nanorods were further investigated and obtained results suggested that a small amount of phosphorous-doped ZnO nanorods enhances their PEC performance.     

不同醇溶剂中氧化锌纳米晶的可控制备

采用液相直接沉淀法,以醋酸锌和氢氧化钠为原料,在醇溶剂体系中成功制备出不同形貌的ZnO纳米晶,使用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和紫外-可见分光光度计(UV-vis)等检测方法对样品进行表征.结果表明,制备的ZnO均为六方纤锌矿结构,形貌受到溶剂种类、反应温度和反应时间等因素影响;在乙醇溶剂中,通过反应温度和反应时间控制可得到分散均匀、形貌均一纳米颗粒或纳米棒,并对不同形貌ZnO的生长机理进行了初步讨论.     

Synthesis of flower-like 3D ZnO microstructures and their size-dependent ethanol sensing properties

Flower-like 3D ZnO microstructures constructed from nanorods of different sizes were prepared by a microwave hydrothermal (MH) process in the presence of o-, m- and p-nitrobenzoic acid, respectively. Well-crystallized flower-like ZnO microstructures were obtained after 10 min MH treatment. The X-ray powder diffraction (XRD) test indicated that all the products were consistent with the hexagonal ZnO phase, and scanning electron microscopy (SEM) investigation revealed that the flower-like 3D ZnO microstructures were built with sword-like nanorods 60-100 nm in width and several micrometers in length. The formation mechanism of these flower-like 3D ZnO microstructures is discussed briefly. The gas sensitivity of the as-prepared ZnO microstructures to ethanol at different operation temperatures and concentrations was also studied. The results indicated that the gas sensitivity of the ZnO microstructures was influenced by the particle size and microcosmic configuration, the larger particles with crowded nanorods having higher gas sensitivity.     

Influence of surface modification of zinc oxide nanoparticles on thermal behavior and hydrophilic property of PET–PEG composites

Zinc oxide (ZnO) nanoparticles were successfully prepared by a one‐step precipitation reaction in an aqueous solution of zinc acetate and sodium hydroxide with stearic acid (SA) as the modifying agent. Hydrophilic composites of poly(ethylene terephthalate) (PET), poly(ethylene glycol), and ZnO nanoparticles were prepared further by in situ polymerization. The surface modification of ZnO and the microstructure and properties of prepared nanoparticles were investigated by relative contact angle measurements (CA), Fourier transform infrared spectroscopy, X‐ray diffraction (XRD), scanning electron microscopy, and thermogravimetric analysis (TGA). Measurements of CA and XRD indicated that the surface‐treated ZnO was hydrophobic and had a significant improvement in crystallinity with SA. Compared with the nanocomposites filled with the pure ZnO, the modified ZnO exhibits a better dispersion in PET–PEG matrix. TGA results showed that the presence of modified ZnO nanoparticles can improve the thermal stability of PET–PEG matrix. CA and low field nuclear magnetic resonance methods were used to investigate the hydrophilic behavior of nanocomposites. The results revealed that modified nanoparticles had a positive effect on the bound water absorption. A simple model for the interactions between ZnO, SA, and PET–PEG matrix was proposed. POLYM. COMPOS., 37:1830–1838, 2016. © 2015 Society of Plastics Engineers