阳极氧化法在钛网上制备TiO2纳米管阵列的研究

以NH4F的乙二醇溶液为电解液,采用阳极氧化法在钛网表面制备了有序TiO2纳米管阵列.通过XRD、SEM等对TiO2纳米管阵列的结构、形貌进行表征,利用紫外-可见分光光度计对所制备样品的紫外可见吸收特性进行了表征.结果表明:在一定时间范围内,随着氧化时间的增加,纳米管管长和管径都会增大,但超过一定时间后,纳米管破损明显加剧且有脱落现象.另外,所制备样品的光学禁带(Eopt)比块状样品的大,但随着氧化时间的延长,纳米管的光学禁带并没有发生显著变化.不同时间下制备的纳米管对可见光的吸收率不一样.     

钛酸锶钡纳米管阵列薄膜的水热合成及其性能研究

以阳极氧化法制备的二氧化钛纳米管阵列为模板,结合水热法制备了钛酸锶钡纳米管阵列薄膜.讨论了Ba1-xSrxTiO3纳米管阵列薄膜的结构、形貌和电学性能.用X射线衍射仪表征其晶体结构;扫描电子显微镜观察其表面及断口形貌;以及用宽频介电阻抗谱仪测试其介电性能.结果表明:在较为温和的条件下用水热法制备了立方相及四方相的Ba1-xSrxTiO3纳米管阵列薄膜;纳米管孔径在65～ 80 nm之间,薄膜厚度可达10 μm以上;经热处理之后的薄膜样品在1 kHz介电常数可达338,介电损耗为0.46.     

二次阳极氧化对TiO2纳米管阵列形貌及光电催化性能的影响

在含水量为2wt;的0.3wt; NH4F和乙二醇电解液中,通过二次阳极氧化法制备了高度有序的TiO2纳米管阵列(TNT).利用扫描电镜(SEM)、X射线衍射(XRD)表征方法对TiO2纳米管阵列的形貌、晶型进行表征.结果表明,二次阳极氧化法形成的TNT更加规整,纳米管孔径大小一致.XRD分析显示二次阳极氧化法形成的TNT锐钛矿相衍射峰更强.光催化降解实验表明,二次阳极氧化制备的TNT对X-3B的降解效率是一次阳极氧化TNT的1.45倍.     

CdS/TiO2纳米管阵列的制备及光催化性能

采用阳极氧化法在纯钛箔上制备出TiO2纳米管阵列,再通过化学水浴沉积法在TiO2纳米管阵列上负载CdS纳米颗粒.利用XRD、FESEM和UV-Vis分光光度计对样品的晶体结构、微观形貌和光学性质进行表征,并研究了不同含量CdS负载的复合薄膜对光催化降解气相苯性能的影响.结果表明,CdS纳米颗粒均匀沉积到TiO2纳米管阵列上,所制备的复合薄膜光吸收带边均扩展到了可见光区.CdS的修饰大幅度提高了TiO2纳米管阵列对气相苯的光催化降解活性,其中负载CdS质量分数为3;的TiO2纳米管阵列光催化活性最佳,80 min内对气相苯的去除率为80;,终产物CO2的浓度为640 mg/m3.     

电解液温度对二氧化钛纳米管阵列结构及光电性能的影响

以氟化铵(NH4F)、乙二醇溶液为电解液,在不同的电解液温度(0～50℃)条件下,采用电化学阳极氧化法制备二氧化钛(TiO2)纳米管阵列.采用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、紫外-可见分光光度计(UV-Vis)对TiO2纳米管阵列的形貌、结构和光学性能进行表征.结果表明,电解液温度高于20℃均能制备出纳米管阵列.光照下电解液温度40℃时制备的TiO2纳米管阵列具有最高光电流密度(Iph)0.2408 mA/cm2.以活性艳红X-3B为目标降解物,在室温、紫外光照射条件下考察了电解液温度对光催化活性的影响,结果显示电解液温度40℃时制备的TiO2纳米管阵列具有最高的光催化活性.     

RuO2/TiO2纳米管薄膜的制备及其光电催化性能研究

采用阳极氧化法结合浸渍法在钛金属片基底上制备了TiO2负载RuO2纳米管阵列,利用场发射扫描电子显微镜(FE-SEM)、X射线衍射仪(XRD)、能谱仪(EDS)和紫外可见分光光度计对纳米管的形貌、结构和光学性能进行了表征,并研究了RuO2/TiO2纳米管阵列在紫外光和可见光下对亚甲基蓝溶液的光电催化性能.结采表明:RuO2/TiO2纳米管仍保持了纯TiO2纳米管的结构特征,部分Ru进入TiO2晶格代替了Ti的位置形成了固溶体,部分Ru以RuO2纳米粒子形式存在;RuO2/TiO2纳米管的光吸收波长发生了红移,且在整个可见光区均比纯TiO2纳米管光吸收能力强,RuO2/TiO2纳米管光电催化降解亚甲基蓝的4h降解率由纯TiO2纳米管的27;提高到79;;采用该法制备的TiO2纳米管阵列膜回收简单,反复使用20次后光电催化降解能力基本保持不变.     

阳极氧化工艺制备TiO2纳米管阵列及其碳包覆改性

首先采用阳极氧化工艺制备了TiO2纳米管阵列,然后利用水热工艺对其进行C包覆改性,探讨了热处理温度、F-浓度、阳极氧化电压、阳极氧化时间等参数对TiO2纳米管阵列形貌及性能的影响,并初步研究了其生长机理.通过实验得到TiO2纳米管阵列的最佳制备条件:F-浓度0.5wt;;阳极氧化电压30 V;阳极氧化时间1h;热处理温度450℃.C包覆改性后的TiO2纳米管阵列对可见光的吸收明显增强,尿素浓度为20wt;时制得的TiO2纳米管阵列对亚甲基蓝的光降解率高达92.7;,相较于未进行C包覆改性的TiO2纳米管阵列提高了7.9;,说明C包覆改性可以显著提高TiO2纳米管阵列的光催化性能.     

还原氮化温度对氮化铌纳米管组成、结构与电化学性能影响研究

以铌箔为基底,用阳极氧化法结合氨气还原氮化法制备出氮化铌纳米管,利用X射线衍射仪(XRD)、X射线光电子能谱(XPS)和扫描电镜(SEM)等结构表征手段和循环伏安法(CV)、充放电(GCD)和交流阻抗法(EIS)等电化学测试手段研究了还原氮化温度对纳米管的物相、形貌以及电化学性能的影响.结果表明,还原氮化后出现了氮化铌物相,以氧氮化铌固溶体形式存在,当还原氮化温度为700℃时,氮化铌纳米管阵列结构均匀,纳米管的孔内径约为35 nm,管壁厚度约为12 nm,纳米管长度约为1.5μm,样品中内在阻抗和电荷转移电阻较小,在电流密度为0.1 mA/cm2时,其比电容为400μF/cm2.     

退火温度对二氧化钛纳米管阵列亲水性的影响

采用电化学阳极氧化法,以含有0.25wt; NH4 F和2 mL H2 O的乙二醇溶液作为电解液制备了TiO2纳米管阵列,然后通过不同温度退火比较其形貌、结构、元素组成和亲水性能。实验表明,600℃以下温度退火基本不会引起TiO2纳米管阵列的形貌改变,但是600℃退火会使得部分TiO2纳米管坍塌。随着退火温度的升高,TiO2由无定型结构向晶体结构转变,同时接触角减小,亲水性变好。另一方面,F元素也会影响TiO2纳米管阵列的亲水性能,F元素含量越少,亲水性越好。     

阳极氧化法制备TiO2有序多孔薄膜

采用二次阳极氧化工艺,以含有氟化铵和水的乙二醇体系作为电解液,在纯钛表面制备有序的TiO2多孔薄膜.通过改变预处理方式、电压、氧化时间和搅拌速度等实验参数来探究其对TiO2多孔薄膜形貌的影响.结果表明,抛光后Ti基片制得的TiO2多孔薄膜表面更加平整;TiO2纳米孔的孔径和孔间距随着阳极氧化电压升高在一定范围内线性增大;TiO2纳米孔的孔径随着阳极氧化时间延长增大,孔壁随时间延长减薄,通过控制氧化时间可以实现纳米孔薄膜向纳米管阵列的转变;搅拌速度在400 r/min时,能够获得有序的自组织TiO2多孔薄膜.     

Ce/TiO2纳米管阵列的制备及光催化性能的研究

采用电化学阳极氧化法在钛表面制备TiO2纳米管阵列,并用稀土铈对其修饰改性.以甲基橙为目标降解物,考察了Ce3+溶液浓度、甲基橙溶液的初始浓度和初始pH对铈改性的TiO2纳米管光催化活性的影响.结果表明:Ce3+溶液的浓度存在一个最佳值,当Ce3+溶液浓度为0.01 mol/L,在10 mg/L,pH =3的甲基橙溶液中光催化活性最好.光照4h后,甲基橙的降解率达83％.     

Controllable synthesis of well‐aligned CuO nanotube arrays using porous alumina templates

In order to further enhance the performance of CuO in currently existing applications, well‐aligned CuO nanotube arrays with different diameters were fabricated. During the synthesis process, porous anodic alumina films were fabricated, and then the synthesis of CuO nanotube arrays was realized by using the obtained porous anodic alumina films as templates. The morphology and structure of the obtained products has been confirmed by field‐emission scanning electron microscopy, transmission electron microscopy and X‐ray diffraction measurements. Due to the large surface area of the synthesized products, the prepared CuO nanotube arrays may have potential applications in catalyzing and gas sensing area.     

溶胶-凝胶模板法制备磷酸铁锂纳米线阵列

以多孔阳极氧化铝(AAO)为模板,采用溶胶-凝胶法和模板法结合的方法制备了LiFePO4纳米线阵列,实验考察了煅烧温度、气氛等主要工艺参数对纳米线阵列形貌晶型的影响,并用SEM、XRD对纳米线的结构、成分和形貌进行了表征.结果表明:制备的LiFePO4纳米线阵列的直径约为200nm,长度为60μm,长径比达到300,纳米线阵列的直径主要取决于模板的孔径,长度接近于模板的厚度.采用不同结构尺寸的AAO模板,可实现纳米线阵列的可控制备.最后在实验基础上,对纳米线阵列的形成机理进行了分析.     

水热法制备硅掺杂纳米TiO_2的光催化性能

以TiCl_4和Na_2SiO_3为原料,采用水热法制备了一系列掺杂Si的纳米TiO_2粉体.采用X射线衍射分析(XRD),红外光谱(FT-IR),紫外可见吸收光谱(UV-vis DRS)对样品进行了表征.结果表明:掺杂Si的TiO_2样品粒径较小,样品中锐钛矿的百分含量有了一定提高.同时发现在Si掺杂的样品中有Ti-O-Si键的存在.掺杂Si的TiO_2样品的光催化活性较未掺杂样品有了较大提高.并讨论了Si掺杂提高TiO_2光催化活性可能的原因.     

Ag2O/TiO2异质结的光催化活性及耐光腐蚀性研究

以钛酸丁酯、硝酸铋和硝酸银为原料,FTO为基底,采用水热法结合超声沉积法合成了Ag2 O/TiO2异质结光催化剂.采用场发射扫描电子显微镜(FESEM)、X射线衍射仪(XRD)、紫外-可见吸收光谱(UV-Vis)分析测试手段对样品的形貌和结构进行了表征.结果表明,Ag2O/TiO2异质结是由直径约200 ～ 300 nm的TiO2纳米棒镶嵌着Ag2O纳米颗粒组成,与TiO2纳米棒阵列相比,Ag2O/TiO2异质结在可见光区有明显的光吸收.Ag2O/TiO2异质结的光催化效率明显提高.尤为重要的是,经光处理后,最终得到稳定的Ag-Ag2O/TiO2三元体系,并对Ag-Ag2 O/TiO2三元体系提高光催化稳定性和活性的机理进行了分析.     

Synthesis and characterization of visible light responsive N-TiO2 mixed crystal by a modified hydrothermal process

N doped TiO₂ with anatase and rutile mixed crystal were prepared by using tetrabutyl titanate as the precursor via a modified hydrothermal process and calcination at 320 °C. The microstructure and morphology of samples were characterized by XRD, UV-vis-DRS, FTIR and XPS. The results showed that N-TiO₂ particles were crystallized to anatase and rutile mixed crystal structure; they were presented narrow particle size distribution, and the average particle size was ca. 13.5 nm calculated from XRD results. It was found that the N-doped TiO₂ particles showed strong visible-light absorption and high photocatalytic activity for the mineralization of Rhodamine B under irradiation by visible light (400-500 nm). The high visible-light photocatalytic activity of the obtained N-doped TiO₂ might result from the synergetic effect of nitrogen doping and the mixed lattice structure of N-TiO₂. Possible mechanism of N-TiO₂ mixed crystal formed under hydrothermal conditions was discussed.     

Synthesis and characterization of Bi3.15Nd0.85Ti3O12 nanotube arrays

Nd-substituted bismuth titanate (Bi_3.15Nd_0.85Ti₃O₁₂, BNT) nanotube arrays are fabricated by means of a sol–gel method utilizing porous anodic aluminum oxide (AAO) template. The morphologies and structures have been determined by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The diameter and length of these nanotubes are about 200 nm and 60 μm, respectively, and their wall thickness is about 30 nm. The average grain size is around 40 nm. XRD data show that the BNT nanotubes possess bismuth-layered perovskite structure. High-resolution electron microscopy (HRTEM) image demonstrates that the BNT nanotubes are polycrystalline. Polarization–electric field (P–E) response curves of BNT nanotube arrays were measured, and a size induced polarization reduction phenomenon is observed.     

Solvothermal growth of highly oriented wurtzite‐structured ZnO nanotube arrays on zinc foil

ZnO nanotube arrays were synthesized on zinc foil by a simple solvothermal approach. In this approach, zinc foil was used not only as a substrate but also as a zinc‐ion source for the direct growth of ZnO nanotube arrays. X‐ray diffraction (XRD) analysis and Scanning electron microscope (SEM) images, indicated that the structure of the ZnO nanotube arrays on the zinc foil substrate was single‐crystalline with a wurtzite structure. The optical properties of the ZnO nanorod arrays were characterized by photoluminescence spectroscopies and Raman. Photoluminescence exhibited strong UV emission and a broad deep‐level (visible) emission emission at with 325 nm excitation. A possible mechanism is also proposed to account for the growth of the ZnO nanotube arrays. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

High performance visible light responsive photocatalysts for environmental cleanup via solution processing

Fabrication of nitrogen-doped titania and/or strontium titanate nanoparticles via soft chemical reactions and their performance for environmental cleanup under visible light irradiation were introduced. Nitrogen-doped anatase, brookite and rutile with high specific surface area can be selectively prepared by the solvothermal reactions in mixed aqueous solution of titanium trichloride-hexamethylenetetramine. Nitrogen-doped strontium titanate can be prepared by mechanochemical reaction of strontium carbonate, titania and hexamethylenetetramine using a planetary ball-mill. Nitrogen-doped titania shows excellent photocatalytic activity for the nitrogen monoxide destruction under visible light irradiation. The photocatalytic activity of nitrogen-doped titania is in the order anatase > brookite > rutile. The photocatalytic activity of nitrogen-doped titania and strontium titanate can be improved by co-doping with higher valence metal ions to reduce oxygen vacancy and/or coupling with Fe₂O₃ and Pt to retard quick recombination of photo-induced electron and hole by the heterogeneous electron transfer.     

片状和球状纳米CeO2的可控制备及其光催化性能

以乙二醇、水和丙酸为溶剂,使用无模板溶剂热法通过改变溶剂中乙二醇的体积比在180 ℃的条件下制备了前驱体,将前驱体在500 ℃的空气中焙烧2 h得到分散性较好的片状和球状纳米CeO2.采用X射线衍射(XRD)、扫描电镜(FE-SEM)、紫外-可见漫反射光谱(UV-Vis DRS)对样品进行表征,以亚甲基蓝(MB)的光催化降解为目标反应评价其光催化活性.结果表明:焙烧后试样仍保持前驱体的片状或球状形貌,由纳米颗粒组装而成,片状纳米CeO2直径为0.3~1 μm,厚度为20~60 nm,球状纳米CeO2径为120~200 nm;超细纳米结构使得CeO2光学带隙能减小、光吸收阀值红移、比表面积增大,因而光催化活性大幅提高,片状和球状纳米CeO2在可见光下光催化降解亚甲基蓝的3 h降解率由棒状结构CeO2的12.3;分别提高至80.1;和91.2;.