纳米复合材料Ag/ZnO的制备及紫外光催化降解染料

采用溶胶-凝胶-程序升温溶剂热一步法制备了纳米复合材料Ag/ZnO,通过X射线衍射（XRD）以及扫描电子显微镜配合X-射线能量色散谱仪（SEM-EDS）等测试手段对其结构、形貌等进行了表征。结果表明,复合材料中Ag成功地掺杂在ZnO上,且合成产物Ag/ZnO具有六方晶系纤锌矿结构。为考察上述复合材料的光催化活性,在紫外光照射下,对酸性品红、罗丹明B、孔雀石绿、亚甲基蓝等染料进行了光催化实验研究,结果表明,该复合材料具有较好的可见光催化活性。     

Preparation, characterization and photocatalytic activity of N-doped TiO_2 nanocrystals

N-doped TiO_2 nanocrystals were prepared using titanium alkoxide as precipitant with different proportional materials. The products were characterized by X-ray diffraction,scanning electron microscopy,transmission electron microscopy, and UV-vis diffuse reflectance spectra. It is confirmed experimentally that the photocatalytic activity of N-doped TiO_2 is much higher than that of Degussa P25, when used for the degradation of crystal violet.The degradation kinetics follows an apparent first-order reaction,which is consistent with a generally observed Langmuir-Hinshelwood mechanism. The doping of TiO_2 with nitrogen significantly increases the absorption in the region of visible light. The energy of the band gap of N-doped TiO_2 is 2.92 eV. The better performante of N-doped TiO_2 can be explained by the fact that it is also excited with longer-wavelength light.     

N-Ag/ZnO纳米复合材料的合成及模拟日光下的光催化性能

以NH3为N源,通过气氛渗氮法对采用配合物沉淀法制备出的Ag/ZnO纳米材料进行N掺杂,制备出N-Ag/ZnO纳米复合材料。应用X射线衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、紫外-可见吸收光谱(UV-Vis)等测试手段对制备产物的物相结构、微观形貌及吸光性能进行了表征。以甲基橙(MO)为目标污染物,研究了制备产物在模拟日光照射下的光催化性能。结果表明:Ag粒子附着于棒状ZnO表面,N进入ZnO晶格;N掺杂能够显著提高Ag/ZnO纳米复合材料的光催化性能及其稳定性,以N-Ag/ZnO为光催化剂,在模拟日光下照射降解MO 100min,MO的降解率达到100%,较Ag/ZnO提高25%,且放置30d后光催化性能基本保持不变。     

Characteristics and Photoeatalytie Effects of Zn/ZnO Nanowhiskers Compared with ZnO Nanopartieles

ZnO nanopowders were prepared by oxidizing Zn vapor in the atmosphere of mixture gas of At and O2 at low pressure. Tetrapod nanowhiskers synthesized at a pressure of 1.6 kPa show pure ZnO feet and Zn phase in the core of the nanopowder. The ellipsoid ZnO nanoparticles were produced at the pressure of 10 kPa. The photodegradation rate of aniline and chemical oxygen demand removal demonstrate that the photocatalytic efficiency of Zn/ZnO nanowhiskers with UV irradiation is higher than that ofZnO nanoparticles. The tetrapod morphology and Zn phase inside nanowhiskers play key a role in photodegradation process.     

Ag3PO4/Fe3O4/GO复合催化剂的制备及其可见光催化性能

以氧化石墨烯（GO）为基底,利用共沉淀及离子交换两步法制备Ag₃PO₄/Fe₃O₄/GO 复合光催化剂．通过X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电镜（TEM）、热重（TGA）、振动样品磁强计（VSM）及紫外-可见光谱（UV-Vis DRS, UV-4100,带积分球）对样品的特征基团、微观形貌及磁性质、光学性质等进行了鉴定和表征．光催化脱色实验结果表明：Ag₃PO₄/Fe₃O₄/GO 化剂20 min内对10 mg/L罗丹明B模拟水样的脱色率可达97.6%,高于Ag₃PO₄（73.4%）;Ag₃PO₄/Fe₃O₄/GO 系中引入过硫酸钠可以起到强化光催化性能的作用;另外,Ag₃PO₄/Fe₃O₄/GO 剂表现出良好的活性稳定性、热稳定性及结构稳定性。     

掺Ag纳米TiO2薄膜的制备与光催化性能研究

利用钛酸四丁酯水解得到TiO2胶体溶液,加AgNO3得到掺Ag的TiO2胶体溶液;在室温下利用浸渍-提拉法制成透明的前驱体薄膜,通过煅烧处理得到掺Ag的TiO2薄膜,并在此基础上进行了光催化降解甲基橙的试验．结果表明：利用溶胶-凝胶法可制得TiO2薄膜,在钛酸四丁酯的乙醇溶液物质的量浓度为0．840mol／L、TiO2和Ag物质的量比为10：1条件下,掺Ag薄膜中TiO2颗粒的平均粒径大约为几十纳米,且分布较为均匀;煅烧温度显著影响TiO2(Ag)薄膜的光催化性能,煅烧温度为350℃时TiO2薄膜光催化能力最好;掺入Ag可以提高TiO2薄膜的光催化降解能力,本试验条件下TiO2和Ag物质的量比为10：1的TiO2(Ag)薄膜催化能力最强．     

立方体形Ag3PO4可见光光催化剂的制备及其性能研究

以AgNO3、Na2HPO4和NH3.H2O为主要原料,利用银氨辅助法成功制备出了在可见光照射下具有高的光催化活性的立方体形Ag3PO4光催化剂.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、傅里叶变换红外光谱仪(FTIR)和紫外可见光谱仪(UV-Vis)等分别对Ag3PO4样品的晶相组成、微观形貌和吸光度等进行了表征,并且考察了该光催化剂在模拟太阳光照射下对罗丹明溶液的光催化降解效果.结果表明,所制备出的立方体形Ag3PO4晶体是由6个{100}晶面包裹而成,与球形的Ag3PO4样品相比,立方体形的Ag3PO4样品表现出更优越的光催化活性,这主要是由于由高活性的{100}晶面主导的立方体形Ag3PO4样品对可见光有更高的吸收能力、更高的电子与空穴分离效率,以及更多的光催化活性中心.     

Surfactant-assisted synthesis and magnetic properties of monodispersed manganese ferrite nanocrystals

Monodispersed manganese ferrite (MnFe₂O₄) nanocrystals could be successfully synthesized in large quantities via a facile synthetic technique based on the pyrolysis of organometallic compound precursor, in which octadecene was used as solvent, and oleic acid and oleylamine were used as capping ligands. MnFe₂O₄ nanocrystals were obtained with size in a tunable range of 4–15 nm and their morphologies could be tuned from spherical to triangle-shaped by varying the surfactants. The phase structure, morphology, and size of the products were characterized in detail by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Magnetic properties of MnFe₂O₄ nanocrystals with different morphologies were measured using a superconducting quantum interference device (SQUID). Both monodisperse MnFe₂O₄ nanocrystals with spherical and triangle-shapes are superparamagnetic at room temperature while ferromagnetic at 2 K. The pyrolysis method may provide an effective route to synthesize other spinel ferrites or metal oxides nanocrystals.     

ZnO/CuO复合催化剂的制备及其光催化性能

通过煅烧法制备了ZnO/CuO复合光催化剂,采用紫外-可见光谱(UV-Vis)、伏安光电流、X射线衍射(XRD)、扫描电镜(SEM)以及荧光光谱(PL)等方法对其结构、表面形貌和光学特性进行了表征。结果显示,复合物为片状结构的ZnO、晶粒呈现花簇状堆积生长的CuO组成了花簇状结构,CuO的引入提高了材料的光吸收能力和光生载流子的分离效率。复合催化剂对活性艳蓝(KN-R)的光催化降解结果显示,400℃煅烧3h、铜锌摩尔比为2时,ZnO/CuO复合光催化剂的光催化氧化性能最好,在紫外光照射下降解率可达94%,在可见光照射下降解率为48.4%。     

铬银共掺杂改性纳米TiO2光催化剂及其光催化性能研究

以钛酸四丁酯为原料,利用溶胶凝胶法制备了Cr/Ag共掺杂的TiO2纳米材料.采用XRD、SEM、EDS等测试分析技术对掺杂纳米TiO2粉体进行了表征;以甲基橙为降解物,在太阳光照射条件下研究了掺杂对光催化活性的影响.研究结果表明:掺杂后的纳米TiO2的光催化性能明显提高,优于纯TiO2.当共掺杂的比例为Cr 1.0%/Ag 0.5%时,样品的效果最佳,对甲基橙的3h降解率达到97.63%.     

Enhanced photocatalytic activity of (La, N) co-doped TiO_2 by TiCl_4 sol-gel autoigniting synthesis

(La, N) co-doped TiO2 photocatalysts were synthesized using TiCl4 sol-gel autoigniting synthesis (SAS) starting from a complex compound system of TiCl4-La(NO3)3-citric acid-NH4NO3-NH3?H2O, in which the (La, N) co-doped process was accom- plished in the formation of TiO2 nanocrystals. The prepared samples were characterized by using X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS) and UV-vis diffuse reflectance spectra. The results indicated that nitrogen and lanthanum were incorporated into the lattice and interstices of titania nanocrystals, which resulted in narrowing the band gap and promoting the sepa- ration of photoexcited hole-electron pairs, respectively, and showing expected red-shifts and enhanced photocatalytic activity under visible light. The mechanism on nitrogen doping and enhancement in photocatalytic activity of (La, N) co-doped titania by SAS was discussed in detail.     

Synthesis of novel CaCO_3/Ag_2CO_3/Ag I/Ag plasmonic photocatalyst with enhanced visible light photocatalytic activity.

In this work, novel Ca CO3/Ag2CO3/Ag I/Ag plasmonic photocatalysts were successfully synthesized by a two-step in situ ion exchange process and their photocatalytic properties were studied. The morphology, crystal structure and optical properties of the as-prepared Ca CO3/Ag2CO3/Ag I/Ag nanocomposites were characterized by transmission electron microscopy(TEM), XRay diffraction(XRD), and UV-vis diffuse reflectance spectroscopy. The photocatalytic activity of the obtained nanocomposites was evaluated by the photodegradation of methyl orange(MO) under visible light irradiation. It was found that the as-prepared Ca CO3/Ag2CO3/Ag I/Ag plasmonic photocatalyst exhibits high visible light photocatalytic activity. With an optimized composition, MO dye can be decomposed by more than 94% within 15 min under visible light irradiation. Moreover, the photocatalytic stability could be greatly improved upon the addition of Na2CO3 into the photocatalytic system. From the proposed photocatalytic mechanism, the strong surface plasmon resonance effect of Ag nanoparticles and the efficient separation of photogenerated electrons and holes can effectively enhance the photocatalytic performance of the Ca CO3/Ag2CO3/ Ag I/Ag composites.     

离子液体中棒状ZnO粉体的制备及光催化性能

制备了离子液体1-乙基-3-甲基咪唑溴盐([emin]Br),以该离子液体为模板剂,采用水热法制备了亚微米级棒状ZnO粉体。经扫描电子显微镜(SEM)、X射线衍射(XRD)、傅立叶转换红外光谱(FT-IR)等对样品进行了表征和分析。结果表明,该方法制备出具有六方纤锌矿结构的棒状亚微米级ZnO粉体,棒长为2~3μm,直径为500~600 nm;以高压汞灯为光源,以ZnO粉体为光催化剂,对有机染料罗丹明B进行了光降解实验,光降解90 min后,其去除率达到93.3%。     

分级结构纳米ZnO的制备及其光催化性能研究

采用水热合成法,以Zn(CH3COO)2.2H2O和NaOH为原料,糊精为形貌控制剂,在120℃条件下合成了纳米ZnO样品.利用粉末X射线衍射、扫描电子显微镜、透射电子显微镜和高分辨透射电子显微镜对所合成的ZnO样品进行了结构和形貌的表征.分析结果表明,所合成的ZnO样品具有六方纤锌矿结构,且样品中含有大量由ZnO纳米片组装而成的"花状"分级结构纳米颗粒,花状分级结构中纳米片的平均厚度约50 nm.光催化降解实验结果表明,所合成的花状分级结构纳米ZnO具有很好的光催化性能.     

A convenient method for preparing shape-controlled ZnO nanocrystals in a polyol/water mixture system without surfactants

A facile solution-phase route for the synthesis of shape-controlled ZnO nanocrystals in a polyol/water mixture system was developed. The obtained nanocrystals were characterized by X-ray diffraction, transmission electron microscopy and UV-visible absorption spectroscopy. The results indicate that modulating the adding ways of water has a significant effect on the shape of the obtained nanocrystals. The addition of small quantity of water can increase the growth rate of crystals and leads to the formation of different shapes. The resulting shapes of the novel structures are diverse, including spheres, cones, and teardrops, all of which are obtained without any additional surfactants. These studies concerning the shape evolution of nanocrystals should be valuable for further design and for greater understanding of advanced nanoscale building-block architectures. Funded by the National Natural Science Foundation of China (No. 50572039), the Postdoctoral Foundation of China (No. 20060390284) and Jiangsu Planned Projects for Postdoctoral Research Funds     

铋掺杂磁性光催化剂的制备及其光催化活性

以Fe3O4/SiO2复合微球为基体,采用溶胶—凝胶法制备了Bi掺杂的磁性TiO2复合光催化剂,并用SEM、FT—IR和VSM等测试手段对催化剂进行了表征。以活性艳红K-2BP为目标降解物评价其光催化活性。结果表明,制备的复合光催化剂易于磁性固液分离,K-2BP溶液初始浓度为20 mg/L,pH值为2,光催化剂的添加量为0.5 g/L,Bi摩尔分数为0.6%的光催化剂时的催化活性最高,光催化反应5 h后K-2BP的降解率达到88.38%。     

One-pot Synthesis of Mesostruetured Ag/Siliea Composite Films

Mesoporous silica films embedded with Ag nanoparticles were directly synthesized by a solgel dip-coating process, combining alkyl （ethylene oxide） surfactant as temple and tetraethoxysilane as inorganic precursor. The addition of Ag^＋ ion to the reaction sol was prior to the formation of films, followed by the heat treatment at 150℃ led to the creation ofAg nanoparticies. The formation ofAg nanoparticles and the change of its surface plasma resonance absorption were characterized by Uv-vis. The small angle XRD test indicated that the films had an ordered hexagonal mesoporous structure, of which the unit cell parameter was about 4.26 nm. The TEM images and EDS spectra of the samples have directly verified the presence of mono-dispersed Ag nanoparticles within the films, due to the confine effects of mesopores.     

Effect of silver growth temperature on the contacts between Ag and ZnO thin films

Highly c-axis oriented ZnO thin films were deposited on Si substrates by the pulsed laser deposition (PLD) method. At different growth temperatures, 200 nm silver films as the contact metal were deposited on the ZnO thin films. The growth temperatures have great influence on the crystal quality of Ag films. Current-voltage characteristics were measured at room temperature. The Schottky contacts between Ag and ZnO thin films were successfully obtained when silver electrodes were deposited at 150°C and 200°C. Ohmic contacts were formed while the growth temperatures were lower than 150°C or higher than 200°C. After analysis, the forming of Ag/ZnO Schottky contacts was shown to be dependent on the appearance of the p-type inversion layer at the interface between Ag and ZnO layers.     

Preparation, Characterization and Visible Light Photocatalytic Activity of Nitrogen-doped TiO2

The N-doped TiO2 polycrystalline powder was synthesized through calcining the hydrolysis prodact of tetra-butyl titanate with ammonia. The photocatalytic activity of N-doped TiO2 powder with anatase phone calcined at 400℃ was 2.7 times higher than that of Degussa P25 for phenol decomposition under visible light. All samples had mesoporoas structures. X- ray photoelectron spectroscopy confirmed that a trace amount of N atoms remained in the anatase polycrystaUine TiO2 powder when calcined at 400 ℃ as substitutional atoms at the oxygen sites. UV-Vis and EPR analyses indicated that oxygen vacancy states were created during the course of N-doped TiO2 powder formation. It is considered that substitutional N atoms, oxygen vacancy, states, large BET surface areas and mesoporoas structure are important facwrs for the N-doped photocatalyst to present a high vis-activity.     

Large scale synthesis of ZnO nanoparticles via homogeneous precipitation

In order to synthesize ZnO nanoparticles economically, industrial-grade zinc sulfate and urea were utilized to synthesize ZnO precursors in a stirred-tank reactor or a Teflon-lined autoclave at 100–180 °C under complete sealing condition. The ZnO precursors were calcined at 450 °C for 3 h to synthesize ZnO nanoparticles. The composition of the precursors and the formation mechanism of ZnO were studied by thermogravimetric analysis and Fourier transform infrared spectroscopy. The results of X-ray diffraction, transmission electron microscopy and scanning electron microscopy of the ZnO powders demonstrate that high-purity zincite ZnO nanoparticles are synthesized. Orthogonal experiments were performed to find out the optimal conditions for the maximum yield and the minimum size. The effect of temperature on the size of ZnO nanoparticles was investigated. The results show that a higher temperature is propitious to obtain smaller nanoparticles.