燃烧法合成花状、四针状氧化锌及其气敏性能研究

研究了以锌粉为原料,活性炭为催化剂,高温气相氧化反应制备花状、四针状和无定形氧化锌的合成条件及形貌.X射线衍射结果表明该晶体属六方晶系纤锌矿结构.扫描电镜研究结果表明活性炭催化剂用量、反应温度对产物氧化锌晶须的形态影响很大,对所有样品的气敏元件在浓度范围为5×10(-6)～2×10(-4)的甲醇、乙醇、丙酮和正丙醇气体...     

RGO–MWCNT–ZnO based polypyrrole nanocomposite for ammonia gas sensing

Polypyrrole (PPy) nanocomposites were synthesized using ferric chloride (FeCl₃) as an oxidant by in situ polymerization at room temperature in which reduced graphene oxide- multi-walled carbon nanotubes (RGO–MWCNT) and zinc oxide (ZnO) were used as fillers. RGO–MWCNT and ZnO were synthesized by solution mixing and surfactant assistant precipitation respectively. The RGO–MWCNT–ZnO /PPy nanocomposites were prepared by loading 2, 5, 10 and 20 wt% of RGO–MWCNT:ZnO (1:1) in PPy to measure the electrical conductivity. The PPy nanocomposites were characterized by using FTIR, X-ray diffraction and FESEM. Furthermore, these RGO–MWCNT–ZnO/PPy nanocomposites were investigated to study sensing of ammonia gas at room temperature. The response of 20 wt% loading RGO–MWCNT–ZnO/PPy was observed to be 325% towards 200 ppm of ammonia gas.     

Preparation and properties of composite particles made by nano zinc oxide coated with titanium dioxide

In this paper, composite particles of nano zinc oxide coated with titanium dioxide were prepared and characterized by TEM, XRD, XPS and FT-IR, and the properties of the composite particles for photo catalysis and light absorption were studied. Tetrabutyl titanate (TBT) was hydrolyzed in an alcoholic suspension of nano zinc oxide with diethanolamine (DEA) as an additive, resulting in a film with a thickness of 20–30 nm being coated on the surface of nano zinc oxide, and the composite particles contained ZnTiO₃ after drying and calcination. Photocatalysis capabilities of the composite particles for the degradation of phenol in an aqueous solution were greatly improved as compared with nano zinc oxide particles before coating, with pure nano ZnO and nano TiO₂ with similar average sizes, or with the mixture of nano ZnO and TiO₂ with the similar composition as the composite particles. The light absorption scope of the composite particles was enlarged when compared to nano titanium dioxide with same average size.     

Hierarchical structures of ZnO spherical particles synthesized solvothermally

Abstract

We review the solvothermal synthesis, using a mixture of ethylene glycol (EG) and water as the solvent, of zinc oxide (ZnO) particles having spherical and flower-like shapes and hierarchical nanostructures. The preparation conditions of the ZnO particles and the microscopic characterization of the morphology are summarized. We found the following three effects of the ratio of EG to water on the formation of hierarchical structures: (i) EG restricts the growth of ZnO microcrystals, (ii) EG promotes the self-assembly of small crystallites into spheroidal particles and (iii) the high water content of EG results in hollow spheres.     

Performance improvement of zinc oxide photoanode-based dye-sensitized solar cells by multi-walled carbon nanotube

Unique electrical and surface-to-volume properties of carbon nanotubes have made these conductive molecules highly attractive in many applications. In this work, the influence of multi-walled carbon nanotubes into a zinc oxide active layer of dye-sensitized zinc oxide solar cell has been investigated. With this method, a significant improvement in the performance of the solar cell has been achieved. Compared to the typical zinc oxide photoelectrochemical cells, the photocurrent-voltage characteristics of the fabricated cell containing 0.05 percent by weight of carbon nanotubes in the metal oxide film displayed a higher short-circuit photocurrent, consequently caused an increase of the solar-to-electricity conversion efficiency by a factor of approximately 1.4. Further increase of the conductive carbon material resulted in a decrease of the energy conversion of the photovoltaic cell. The enhancement of the energy conversion at this optimum carbon nanotube loading may be attributed to the dye-adsorption ability and the electrochemical activity of the composite photoanodes. The fabricated photovoltaic cells with the highest efficiency exhibited the maximum dye adsorption intensity and the minimum charge transfer resistance, as measured by ultraviolet-visible spectroscopy and electrochemical impedance spectroscopy, respectively.     

Fabrication of ordered flower-like ZnO nanostructures by a microwave and ultrasonic combined technique and their enhanced photocatalytic activity

Ordered flower-like zinc oxide (ZnO) nanostructures were fabricated via a facile microwave and ultrasonic combined technique. The product was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and selected area electron diffraction pattern (SAED). The flower-like ZnO nanostructures were assembled by a central petal and six symmetrical petals which grew radially from the center. The flower-like ZnO sample showed an enhanced photocatalytic performance compared with the ZnO microrods for the methylene blue (MB) degradation, which could be attributed to its special structure feature. Au/ZnO and Ag/ZnO nanocomposites were also synthesized and exhibited enhanced photocatalytic efficiency after decorating noble metal nanoparticles on the surface of flower-like ZnO nanostructures.     

Hierarchical structures of ZnO spherical particles synthesized solvothermally

We review the solvothermal synthesis, using a mixture of ethylene glycol (EG) and water as the solvent, of zinc oxide (ZnO) particles having spherical and flower-like shapes and hierarchical nanostructures. The preparation conditions of the ZnO particles and the microscopic characterization of the morphology are summarized. We found the following three effects of the ratio of EG to water on the formation of hierarchical structures: (i) EG restricts the growth of ZnO microcrystals, (ii) EG promotes the self-assembly of small crystallites into spheroidal particles and (iii) the high water content of EG results in hollow spheres.     

催化法制备多壁碳纳米管

采用复合氧化物LaFeO3,C2H2为碳源,合成了高纯度的碳纳米管,考察了温度对产量的影响。利用TEM,HR－TEM,XRD,Raman等手段对所制备的纳米碳管进行了观察和表征。碳纳米管管径均匀,石墨化程度较高,易于纯化。     

均匀沉淀法制备碳纳米管/氧化锌复合材料的研究

采用均匀沉淀法制备了碳纳米管(CNTs)负栽氧化锌(ZnO)粒子复合材料,并利用扫描电子显微镜(SEM)、X光衍射分析(XRD)以及热失重分析(TGA)手段对复合粒子进行了表征.研究结果表明:锌离子浓度取0.4mol/L至1.0mol/L时,所得复合材料中的氧化锌粒子大小均匀细小,分散性较好,形貌以粒状为主,大小在40nm左右;纳米氧化锌粒子与碳纳米管结合力较强,CNTs/ZnO复合材料在超声作用下能够稳定存在;反应时间越长,氧化锌粒子含量越高,晶粒越大;热解温度越高,热解时间越长,氧化锌晶粒尺寸越大.     

Electrical and optical properties of reduced graphene oxide and multi-walled carbon nanotubes based nanocomposites: A comparative study

Graphene and multi-walled carbon nanotubes have attracted interest for a number of potential applications. One of the most actively pursued applications uses graphene and carbon nanotubes as a transparent conducting electrode in solar cells, displays or touch screens. In this work, in situ reduced graphene oxide/Poly (vinyl alcohol) and multi-walled carbon nanotubes/Sodium Dodecyl Sulfate/Poly (vinyl alcohol) composites were prepared by water dispersion and different reduction treatments. Comparative studies were conducted to explore the electrical and optical properties of nanocomposites based on graphene and multi-walled carbon nanotubes. A thermal reduction of graphene oxide was more effective, producing films with sheet resistances as low as 10²–10³ Ω/square with 80% transmittance for 550 nm light. The percolation threshold of the thermally reduced graphene oxide composites (0.35 vol%) was much lower than that of the chemically reduced graphene oxide composites (0.57 vol%), and than that of the carbon nanotubes composites (0.47 vol%). The Seebeck coefficient of graphene oxide films changes from about 40 μV/K to −30 μV/K after an annealing of three hours at 200 °C. The optical absorption of the nanocomposites showed a high absorbance in near UV regions and the photoluminescence enhancement was achieved at 1 wt% graphene loading, while the carbon nanotubes based composite presents a significant emission at 0.7 wt% followed with a photoluminescence quenching at higher fraction of the nanofillers 1.6 wt% TRGO and 1 wt% MWCNTs.     

Coating and filling of carbon nanotubes with homogeneous magnetic nanoparticles

Magnetic multi-walled carbon nanotube (MWCNT) composites were obtained by decoration of metal oxide nanoparticles on or in carbon nanotubes. The method involved the dispersion of the carbon nanotubes in iron pentacarbonyl Fe(CO)₅ followed by vacuum thermolysis and subsequent oxidation. The magnetic iron oxide particle deposition was always homogeneous and could be controlled selectively on the outer, inner, or both surfaces of MWCNTs by using different MWCNTs. Since the hollow channels remained intact, these MWCNT based composites could find special applications in cellular delivery systems.     

Carbon nanotubes synthesis in microwave plasma torch at atmospheric pressure

Well aligned multi-walled carbon nanotubes were synthesized at atmospheric pressure using a microwave plasma torch on silicon substrates with silicon oxide buffer layer and catalyst overlayer in the mixture of argon, hydrogen and methane. Iron or nickel was used as catalysts. The optimum substrate temperature for the deposition on Si/SiO₂/Fe substrates was about 970 K. In this case SEM micrographs of the deposits revealed a presence of vertically aligned nanotubes with the diameters around 15 nm. TEM micrographs showed a presence of amorphous carbon particles in the samples and some defects in the wall structure of the produced nanotubes. In Raman spectra two peaks at 1332 and 1584 cm⁻¹ were observed. The CNTs were also synthesized on the substrates without SiO₂ buffer layer but their quality was lower. The synthesis with Ni instead of Fe catalyst required lower temperature and the alignment of the nanotubes was worse. The deposition process was monitored by optical emission spectroscopy. Atomic lines of hydrogen and argon, an emission of CN due to a presence of nitrogen impurities from atmosphere, a weak molecular band of CH and strong C₂ emission were detected in the spectra.     

花状纳米Zno的低温水浴制备及生长机理

以氯化锌和氢氧化钠为反应原料,利用水浴恒温加热,在溶液中直接制备出呈花状形貌的纳米ZnO;采用扫描电镜、X射线衍射、透射电子显微镜等分析方法对所得产物的形貌和结构进行了表征,结果表明,在低温(45℃)时可制备出大量呈花状形貌的纳米ZnO.     

Microwave-assisted synthesis of ZnO/MWCNT hybrid nanocomposites and their alcohol-sensing properties

Zinc oxide and multi-walled carbon nanotube (ZnO/MWCNT) hybrid nanocomposites were synthesised by microwave-assisted method using the mixed solution of zinc acetate dehydrate (Zn(CH₃COO)₂·2H₂O) and treated MWCNTs. The syntheses were carried out at various microwave irradiation powers. The characterisation of the as-synthesised nanocomposites was conducted by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The XRD results revealed that the composites were composed of two phases of MWCNTs and hexagonal wurzite ZnO. The SEM results showed that the ZnO nanoparticles were well decorated on the surface of MWCNTs. The amount of ZnO nanoparticles and their size increased with increasing irradiation power. Thick-film sensors were fabricated onto interdigitated conducting electrodes using as-synthesised hybrid composites as sensing materials. The alcohol-sensing behaviour of the hybrid composite films was investigated. The results indicated that the irradiation power had significant influence on the sensing response of the sensors toward alcohol. The sensor fabricated from the composite synthesised at higher irradiation power exhibited an enhanced alcohol-sensing performance.     

MWCNTs/多孔ZnO纳米材料的制备及室温NO气敏性研究

为开发室温气敏传感器材料,以Zn(NO3)2.6H2O为锌源、尿素为沉淀剂,在制备水合碱式碳酸锌(Zn4CO3(OH)6.H2O)的过程中加入羧基化的MWCNTs(MWCNT-COOH),焙烧制备了MWCNTs/ZnO复合材料.采用XRD,SEM和TEM等对其进行了分析.结果表明:复合材料中MWCNTs分散均匀,ZnO呈多孔纳米片状,纳米片由多个尺寸在10～20 nm的ZnO颗粒组成;在室温、空气湿度为50%的氛围中测试复合材料对NO的气敏响应发现,复合材料对体积浓度1×10-4的NO气敏响应灵敏度大约是MWCNT-COOH的3倍,明显高于MWCNT-COOH;对比加入不同量MWCNT-COOH制备的3种复合材料对NO的气敏性可知,加入200 mg MWCNT-COOH所制备的复合材料对低浓度(体积浓度≤50×10-6)的NO气体表现出较高的灵敏度.     

Controllable synthesis of periodic flower-like ZnO nanostructures on Si subwavelength grating structures

We report on the periodic well-defined flower-like zinc oxide (ZnO) nanostructures (NSs) self-assembled through a simple hydrothermal method using silicon (Si) subwavelength grating (SWG) structures. The Si SWGs serve as building blocks for constructing a two-dimensional (2D) periodic architecture to integrate the one-dimensional (1D) ZnO NSs. Various controlled morphologies of ZnO NSs with high crystallinity are obtained by changing the growth conditions. For 1D ZnO NSs integrated on periodic hexagonal Si SWG structures, the reflection characteristics are investigated in comparison with the conventional ZnO nanorod (NR) arrays. For a three-dimensional (3D) flower-like ZnO NS on Si SWGs, a relatively low total reflectance of < 8% at wavelengths of 300-1050 nm is achieved compared to the ZnO NRs on Si substrate.     

Flower-like zinc oxide deposited on the film of graphene oxide and its photoluminescence

The graphene oxide films have been fabricated by simply filtering the graphene oxide solution through the micropore filter. Then the flower-like ZnO grows on the graphene layer by immersing the seed-coated graphene oxide films in the dilute growing solution containing NH₃·H₂O and Zn(NO₃)₂·6H₂O. The morphologies of the as-obtained ZnO deposited on the graphene oxide layer are characterized by using scanning electron microscope (SEM), X-ray powder diffraction (XRD) and photoluminescence (PL). The formation mechanism of the flower-like ZnO has also been investigated. The results show that the morphology of the finally-obtained ZnO is tunable by seeds, the concentration of growing solution and the reaction time.     

Novel vapor phase reactions for the synthesis and modification of carbon nanotubes and inorganic nanowires

Several vapor phase methods have been developed for the preparation and modification of carbon nanotubes and inorganic nanowires. Thus, nebulized spray pyrolysis has been employed for the synthesis of carbon nanotubes and metal nanowires. Multi-walled carbon nanotubes (MWNTs) with fairly uniform diameters and aligned nanotube bundles have been obtained by nebulized spray pyrolysis using solutions of organometallics such as ferrocene in hydrocarbon solvents. Single-crystalline nanowires of zinc, cadmium, cobalt, and lead are obtained by the decomposition of metal acetates. By reacting acid-treated carbon nanotubes with vapors of metal halides, followed by reaction with water and calcination chemically-bonded oxide layers can be obtained on the nanotubes. A similar procedure has been employed to prepare chemically-bonded oxide layers on Al2O3, ZnO, and silicon nanowires by the reaction of the metal halides with the surface hydroxyl groups present on these nanowire surfaces.     

New synthesis of Cu2O and Cu nanoparticles on multi-wall carbon nanotubes

Cu₂O and Cu nanoparticles were deposited on the surface of multi-walled carbon nanotubes with a diameter range of 15–90 nm by the impregnate method. Multi-wall carbon nanotubes with a length of 200 μm and a diameter range of 70–110 nm were grown inside of quartz tubing by the spray pyrolysis method using ferrocene/benzene under argon flow. The nanotubes were then treated with nitric acid to clean the surface and generate carboxylic groups. The copper was impregnated on multi-walled carbon nanotubes using a xylene solution of copper(I) phenylacetylide as the precursor. Copper and cuprous oxide nanoparticles were obtained during thermal treatment.     

Growth and characterization of flower-like Ag/ZnO heterostructure composites with enhanced photocatalytic performance

Flower-like Ag/ZnO heterostructure composites were prepared through a solvothermal method without surfactants or templates. The products were characterized by X-ray powder diffraction, scanning electron microscopy, transmission electron microscopy, and photoluminescence (PL) spectroscopy. Results demonstrate that flower-like Ag/ZnO heterostructure composites were composed of wurtzite ZnO flowers coated by face-center-cubic Ag nanoparticles. The growth process of flower-like ZnO crystals was investigated, and a possible growth mechanism was proposed. The photocatalytic activity of the as-prepared flower-like Ag/ZnO samples, pure ZnO samples, and commercial TiO₂ (Degussa, P-25) was tested with the photocatalytic degradation of methylene blue. Results show that the Ag/ZnO heterostructures were superior in photocatalytic activity to the pure ZnO samples and the commercial TiO₂ (Degussa, P-25), but the mixture of Ag (0.1 wt%) particles and ZnO flowers did not, which implies that the heterostructure promoted the separation of photogenerated electron–hole pairs, enhancing the photocatalytic activity. That was primarily verified by the PL results.