TiO2/氮掺杂碳纳米管复合材料的制备及光催化性能研究

以钛酸异丙酯为前驱体,采用水热合成法制备了TiO2/氮掺杂碳纳米管复合材料。采用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电镜(TEM)等对样品进行了详细的表征,并以罗丹明B作为模型污染物,研究了TiO2/氮掺杂碳纳米管复合材料作为光催化剂在紫外光照射下的光催化能力,结果表明TiO2/氮掺杂碳纳米管复合材料对环境污染物具有良好的降解能力。     

The Preparation of Porous Activated Slag Granules/TiO_2 Photocatalyst and Its De-NO_x Performance

The porous structure and honeycombed structure of granulated blast furnace slag formed by alkali activation (AGBFS) can be used as a promising photocatalysts substrate for the photocatalytic removal of atmospheric or water pollutants.In this study,photocatalytic activated slag granules were synthesized by loading TiO_2 on AGBFS with immersion method.The physicochemical properties and NO_x removal performance of activated slag granules/TiO_2 photocatalysts were studied by X-ray diffraction (XRD),scanning electron microscope (SEM) and photocatalytic performance test.The effects of slag particle sizes and nano-TiO_2 loading concentrations on photocatalytic efficiencies of NO_x removal were also investigated.It was found that the De-NO_x performance of activated slag granules/TiO_2 photocatalyst increased with the increasing of slag particle size in low TiO_2 loading concentration situation,while increasing the TiO_2 loading concentration would result in the opposite De-NO_x performance as slag size increased.Nevertheless,for the same size activated slag,the photocatalytic efficiency of activated slag granules/TiO_2 photocatalyst gradually improved with the increase of loading concentration of TiO_2.     

Coexistence of antiferromagnetic and ferromagnetic in Mn-doped anatase TiO2 nanowires

A series of Mn-doped TiO_2 nanowires (NWs) were prepared by hydrothermal method at the mole fraction of Mn changing from 0 to 12.0%. X-ray powder diffraction (XRD) analysis shows that all the samples have pure anatase structure. SEM and TEM studies show that the diameter and the length of the Mn-doped TiO_2 NWs are larger than those of the undoped TiO_2 NWs. Energy dispersive X-ray spectroscopy (EDX) reveals that the samples are composed of Ti, Mn and O. According to magnetization measurements, all samples show ferromagnetic behavior, but only the undopedTiO_2 NWs are completely ferromagnetic with a saturated magnetization about 1.0 mA·m~2/kg. Mn-doped TiO_2 samples exhibit antiferromagnetic and ferromagnetic (AF-FM) behaviors simultaneously. Photoluminescence (PL) spectra demonstrate the existence of MnO_2 sublattice. These observations indicate that an AF-WF crossover is induced by the coexistence of TiO_2 sublattice and MnO_2 sublattice.     

Sn/C纳米复合材料的合成及其电化学嵌放锂性能

用SnCl4和葡萄糖的水热反应合成SnO₂/碳质复合材料,然后在氮气气氛中热处理使SnO₂被碳热还原为Sn纳米粒子,制备得到Sn/C纳米复合材料.用X-射线衍射(XRD), 透射电镜(TEM)和X-射线电子散射能谱(EDX)对样品进行表征.结果显示Sn纳米粒子具有球形的形貌,并均匀地分散在无定形的碳材料中.对于Sn质量分数58.5%和32.3％的Sn/C复合材料,Sn纳米粒子的平均粒径分别为51和20 nm.电化学测试结果显示,Sn/C复合材料具有高的电化学贮锂可逆容量和良好的循环稳定性.讨论了Sn/C纳米复合材料的形成机理及其循环稳定性能改善的原因.     

载银TiO2/沸石催化剂的制备、表征以及光催化性能的研究

为获得高活性的负载型TiO2光催化剂，通过硝酸银溶液浸渍-紫外光照的方法获得载银的TiO2/沸石催化剂.银改 性的TiO2/沸石催化剂光催化性能较改性前大大提高.最佳硝酸银浸渍液浓度为10-3mol/L,此时该催化剂的光催化性能接 近纳米TiO2粉末（Degussa P25）,但进一步升高硝酸银浸渍液浓度，光催化性能又降低.实验通过X-射线衍射（XRD）和 透射电镜（TEM）对载银TiO2/沸石催化剂的表征,结果表明,金属银对电子的捕获使得电子-空穴对有效分离， 从而使银 改性光催化剂的活性提高.     

一维Cu@C核壳结构纳米复合材料的制备与表征

以氯化铜作为铜源,六次甲基四胺(HMT)作还原剂和碳源,十六烷基三甲基溴化铵(CTAB)作表面活性剂,在水热条件下合成了一维Cu@C核壳结构纳米复合材料,并进行了表征分析。结果表明,制备的Cu@C核壳结构纳米复合材料为立方相铜晶体,无杂质出现。长度在几微米到十几微米,直径大约200~400 nm。产物由铜、碳2种元素构成;从透射电镜照片可以清楚的看出明暗对比,表明产物的核壳结构。在反应过程中,十六烷基三甲基溴化铵(CTAB)起到了形状控制剂的作用。     

金属酞菁敏化二氧化钛可见光催化降解染料废水的研究

研究了染料敏化半导体光催化剂-酞菁镁/TiO_2复合粒子在可见光波段的光催化性能.通过溶胶-凝胶的方法制得TiO_2胶体再进行焙烧,得到二氧化钛粉末和薄膜,再用酞菁镁敏化,制得酞菁镁/TiO_2复合粒子.利用X射线衍射、扫描电子显微镜、红外光谱和X光电子能谱分析等方法对TiO_2和酞菁镁/TiO_2复合粒子的物理性质进行了表征;并以亚甲基蓝作为目标物研究其光催化性能.结果表明,酞菁镁可以敏化二氧化钛,使其吸收波长红移,并具有较好的光催化性能.     

微波法合成树枝状纳米硫化锑

以氯化锑、硫脲为原料,采用微波法合成树枝状硫化锑纳米材料。用X射线粉末衍射（XRD）、扫描电子显微镜（SEM）和X射线能谱（EDS）等对Sb2S3晶体的物相及形貌进行分析表征。结果表明制备出的是正交相Sb2S3,长度可达数十微米。并给出树枝状硫化锑纳米材料的可能的形成机理。     

Highly Efficient Removal of Organic Dyes by Novel As-synthesized AgBr/montmorillonite Composite

A facile deposition method has been developed for large-scale synthesis of visible-light-driven AgBr/montmorillonite composite catalyst for the first time. The as-synthesized samples were characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS), Fourier transform infrared spectroscopy(FT-IR), transmission electron microscopy(TEM), UV-vis diffuse reflectance spectroscopy(UV-vis DRS) and Brunauer-Emmett-Teller(BET) surface area analysis, respectively. Through the combined action of adsorption and photodegradation, the as-prepared AgBr/montmorillonite composite exhibited a higher removal efficiency for rhodamine B(RhB) than that of Na-montmorillonite and AgBr. For the methyl orange(MO) removal, the AgBr/montmorillonite composite possessed a superior photocatalytic performance compared with Namontmorillonite and AgBr. The enhanced photocatalytic activity of AgBr/montmorillonite composite can be attributed to the effective separation of the electron-hole pairs. In AgBr/montmorillonite suspension, the superoxide radicals are the main reactive oxygen species for dye degradation under visible light illumination.     

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.     

NaEuF_4微米晶的水热合成与表征

以柠檬酸钠(Na3Cit)为螯合剂和形貌控制剂,通过水热方法成功合成了尺寸均匀的六角形NaEuF4微米晶.采用X-射线粉末衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、能量色散X射线(EDX)和光致发光光谱(PL)对所得产物的结构、形貌以及发光性质进行分析.XRD和SEM分析表明:所得NaEuF4微米晶为六方相,颗粒较均匀.NaEuF4微米晶的尺寸和形貌可通过改变Na3Cit的量和反应时间进行调整.提出NaEuF4微米晶的可能形成机理,并研究其光致发光光谱性质.     

二氧化锰改性多壁碳纳米管吸附水中Sb(Ⅲ)

采用液相氧化还原法制备二氧化锰/多壁碳纳米管（MnO2/MWNTs）复合材料,利用X射线衍射仪（XRD）、扫描电镜（SEM）、透射电镜（TEM）、激光粒度仪和N2吸附-脱附对改性前后MWNTs的物化性能进行表征.通过对水中Sb(Ⅲ)的静态吸附试验考察改性碳纳米管的吸附容量,同时还考察pH值、锑的初始浓度、吸附剂投加量、吸附时间和温度对吸附效果的影响.结果表明,在Sb(Ⅲ)初始浓度为1.5 mg/L、吸附剂投加量为0.5 g/L、温度为298 K、pH值为2.00的条件下,二氧化锰改性后的碳纳米管对锑的去除率可达到97.72%,比未改性碳纳米管的去除率提高51.29%,吸附容量也从原始CNT的3.01 mg/g增大到6.00 mg/g.最后发现该吸附过程较好地符合Freundlich吸附等温线,pH值对吸附效果的影响较大.     

CuO-containing multi-walled carbon nanotubes:a novel catalyst for the catalytic ozonation of humic acid in water

CuO particles were attempted to fill in the channel of multi-walled carbon nanotubes (MWCNTs) as novel catalytic materials CuO@MWCNTs used for ozonation of humic acids (HA) in aqueous solution.Catalyst samples were characterized by transmission electron microscopy (TEM),X-ray diffraction (XRD),thermogravimetric analysis (TG) and X-ray photoelectron spectroscopy (XPS).The removal efficiency of HA was promoted in the presence of CuO@MWCNTs compared with that of Al2O3-supported CuO catalyst (CuO/Al2O3) and CuO-coating MWCNTs catalyst (CuO/MWCNTs).The strong synergetic effect in the confinement environment on CuO nanoparticles can attribute to the locally higher pressure due to the lower potential energy of reactants in the channels.Strong interaction happened between the catalyst and reactants,which promoted the decomposition of ozone and the generation of OH.The results of experimental and theoretical investigation confirmed that CuO@MWCNTs promotes the initiation and generation of OH,hence accelerating the degradation of organic pollutants.     

Synthesis and characterization of VO<Subscript>2</Subscript>/mesoporous carbon composites for hybrid capacitors

VO₂/ordered mesoporous carbon (CMK-3) composites were prepared by solid-state reaction process. The microstructures were characterized by X-ray diffraction (XRD), nitrogen adsorption and desorption, field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The experimental results showed that the vanadium oxide in the composites was vanadium dioxide (VO₂) with monoclinic structure, which was artificially loaded on the outer surface of CMK-3. VO₂/ordered mesoporous carbon composites present a significantly improved capacitive performance (131 F/g) increased by 40.86% compared to that of CMK-3 carbon (93 F/g). Therefore, as-prepared VO₂/mesoporous carbon composites suggest promising applications in hybrid capacitors.     

溶剂热法制备CuSe纳米线薄膜

以铜片和硒粉为原料,苯为溶剂,通过调控反应物的配比、反应物浓度、反应温度和反应时间等因素,采用溶剂热法直接在铜基底上制备出六方晶系的硒化铜纳米线薄膜.分别利用X-射线转靶衍射仪(XRD),场发射扫描电子显微镜(FESEM),透射电子显微镜(TEM)表征了产物的晶体结构与形貌,探索了CuSe纳米线薄膜的形成过程,并使用荧光分光光度法(PL)对最终产物的性质进行了表征.实验结果表明:这种CuSe纳米线的直径为100～200 nm,长度为5μm,其荧光发光峰为301 nm.     

Cr_2O_3在一维TiO_2中的掺杂行为

以硝酸铬和四氯化钛为前驱体,采用化学共沉淀法制得TiO2和Cr2O3的复合粉体。将复合粉体进行水热处理,用透射电子显微镜、场发射扫描电子显微镜、电子衍射、X射线衍射以及紫外-可见光谱吸收仪等测试手段对样品的形貌和成份以及光吸收性进行了分析。结果表明,水热处理后得到一维管状结构,其管长500~600 nm,直径10~20nm,壁厚4~6 nm。研究还发现,与纯的TiO2相比,Cr2O3/TiO2复合粉体的紫外-可见光吸收光谱显著红移。     

Degradation of Formaldehyde and Benzene by TiO_2 Photocatalytic Cement Based Materials

A novel photocatalytic cement based material was prepared. The distribution of TiO_2 on the surface of cement was characterized by scanning electron microscope(SEM) and X-ray diffraction(XRD), which showed the relationship of photocatalysis and presence of TiO_2. TiO_2 also had an impact on cement hydration, which was studied by thermal analysis. With 300 W UV illuminations, formaldehyde and benzene were degraded efficiently by the prepared photocatalytic cement based materials. 15wt% TiO_2/cement showed the highest degradation efficiency and capability. The results show that formaldehyde and benzene can be degraded within 4 and 9 hours, respectively. Besides, inorganic ions can induce TiO_2 agglomeration. As a result, the presence of inorganic ions in cement is unfavorable for degradation. The photocatalytic cement based materials were fabricated and the degradation efficiency of formaldehyde was measured on building roof under sunlight illumination. Formaldehyde in glass chamber can be degraded thoroughly within 10 days.     

Preparation and characterization of copper-nickel bulk nanocrystals

Copper-nickel nanoparticle was directly prepared by flow-levitation method(FL) and sintered by vacuum sintering of powder(VSP) method. Several characterizations, such as transmission electron microscopy(TEM), scanning electron microscopy(SEM), X-ray diffraction(XRD), differential thermal analysis(DTA), and energy-dispersive X-ray spectroscopy(EDX) were used to investigate the prepared nanostructures. The results of the study show that FL method could prepare high purity Cu-Ni nanocrystals of uniform spheres with size distribution between 20 and 90 nm. After sintering the bulk nanocrystalline copper-nickel has obvious thermal stability and the surface Webster hardness increases with the rising sintering temperature. At the temperature of 900 ℃, the specimen shows higher surface Webster hardness, which is about two times of traditional materials. When the sintering temperature arrives at 1 000 ℃ the relative density of bulk nanocrystals can reach 97.86 percent. In this paper, the variation tendency of porosity, phase and particles size of bulk along with the changing of sintering temperature have been studied.     

多聚金属离子插层Ni-Ti-LDHs的制备与性质

以三乙醇胺（TEA）为抑制剂,采用共沉淀法制备镍钛双金属氢氧化物（Ni-Ti-LDHs）,通过离子交换法制备MoO24-和H3Nb6O519-插层化合物,改变材料物理化学性质。采用X射线衍射（XRD）、红外光谱（FT-IR）、扫描电镜（SEM）、透射电镜（TEM）和热重及差热分析（TG-DTA）等方法对插层柱撑化合物及其焙烧产物结构进行分析。SEM和TEM测试结果表明,通过共沉淀得到的Ni-Ti-LDHs具有明显层状结构;离子交换法所获得的插层产物MoO24--LDHs和H3Nb6O519--LDHs保持明显的层状结构特征。由TG-DTA分析得出样品失重有两个阶段,第一阶段为样品表面物理吸附水分的脱除;第二阶段为层板羟基的缩合脱除。两种不同的多聚阴离子插层后,层间距变化,但对层间作用力影响不大。     

超声喷雾热解法制备Co9S8纳米球壳

以CoCl2·6H2O和硫脲CS（NH2）2为前驱物，利用超声喷雾热解法在300℃玻璃衬底上制备了Co9S8的纳米球壳．运用X射线衍射（XRD）、扫描电子显微镜（SEM）、透射电子显微镜（TEM）对产物进行了物相和形貌分析，结果表明：产物为直径约500nm，形状相似但不规则的Co9S8球壳．同时，对其生长机理进行了初步研究．