Ta2O5空心球的制备及光催化性能

采用无皂乳液聚合法合成了粒径为500 nm的聚苯乙烯(PS)球。运用层层自组装技术在PS球表面交替沉积单分子层的TaO3纳米页与聚二烯丙基二甲基氯化铵(PDDA)多层膜,650℃煅烧除去PS模板和PDDA高分子层后,得到Ta2O5空心球。空心球的直径为500 nm左右,壁厚约10 nm。XRD结果显示该空心球为正交晶系Ta2O5。空心结构显著提高了Ta2O5的光催化活性,在紫外光照射60 min后,Ta2O5空心球降解亚甲基蓝达90%以上,而商品Ta2O5只能降解28%。     

锂离子电池负极材料ZnMn2O4微米空心球的制备和电化学性能

通过溶剂热方法合成了ZnMn2O4微米空心球,并探讨了其形成机理。采用XRD,SEM,TEM等测试手段对产物的结构、形貌和组成进行了表征。实验结果表明,溶剂热反应条件如反应温度、反应介质对于产物的结构和形貌起着关键作用。在140℃,采用乙醇和水作为反应介质,反应6 h可以制备出直径约3μm的ZnMn2O4微米空心球;当以乙醇为溶剂,反应6 h可以得到团聚的尺寸约250 nm的ZnMn2O4纳米颗粒。将所制备的ZnMn2O4微米空心球/纳米颗粒组装成锂扣式模拟电池,考察其电化学脱嵌锂性能。电化学测试结果显示,与ZnMn2O4纳米颗粒相比,空心结构的ZnMn2O4微米球具有较高的初始放电容量(1335 mAh·g-1)和较好的倍率性能,有望作为锂离子电池的新型负极材料。     

溶剂热法合成CuInS2微球及表征

以CuCl2·2H2O为铜源,InCl3·4H2O为铟源,硫脲为硫源,乙醇为溶剂在160℃水热反应12h合成了花状CuInS2,利用SEM、EDX、X射线和ICP对其形貌及结构进行表征,并讨论了不同溶剂对产物形貌的影响.     

[C4N2H12]1.5[Zn2(PO4)(HPO4)2]·H2O晶体的合成与表征

由于在电学、磁学、光学、吸附、离子交换和催化等领域具有潜在的应用价值,具有开放骨架结构的金属磷酸盐的合成一直受到人们的广泛关注.在这些磷酸盐微孔化合物中,磷酸锌晶体是拓扑结构最为丰富的一种.     

溶剂热合成三维蔷薇花状SnS2微晶

在乙二醇溶剂热条件下,采用SnCl4·H2O和硫代氨基脲为原料,成功制备出了三维蔷薇花状的SnS2微晶.产品用X-射线粉末衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)、拉曼光谱(RS)和紫外一可见吸收光谱(UV-Vis)对样品进行了表征.结果表明SnS2蔷薇花是由纳米级厚度的片状"花瓣"相互连接、交叠、缠绕自组装生长而成.并对蔷薇花状SnS2三维结构的生长机理进行了简单探讨.     

高电化学活性SnO2/TiO2空心微球的制备及其性能

采用一种简便的无模板溶剂热法合成了尺寸在1μm左右、具有堆叠结构的SnO_2/TiO_2空心微球。合成过程的研究结果表明:SnO_2/TiO_2空心微球在形成过程中经历了空心、被填充、分裂到再次形成空心结构的过程。随后,SnO_2/TiO_2空心微球作为锂离子电池负极材料的电化学性能测试结果表明:SnO_2/TiO_2空心微球在0.1 A·g~(-1)的电流密度下,其首次放电容量达到1 484.9mAh·g~(-1),库伦效率为49.0%。经过600次循环后,其放电容量依然可以达到565.6 mAh·g~(-1),显示了高的容量和循环稳定性。     

溶剂热合成具有纳米孔结构的γ -Al2O3

Nanoporous gamma aluminum oxide (γ-Al₂O₃) was synthesized by solvothermal method in the presence of AlCl₃·6H₂O, urea and alcohol. The calcined sample was characterized by XRD, FTIR, TEM, and Nitrogen adsorption-desorption measurement. Results show that the obtained γ-Al₂O₃ is well-dispersed nanoparticles with particle size of 4～7 nm and the product has nano-pore structure with a narrow pore size distribution of 5～20 nm.     

溶剂热-热解法制备具有纳米孔结构的Co3O4

Nanoporous rhombohedral Co₃O₄ was synthesized by thermal decomposition of the precursor obtained via a solvothermal method in the presence of Co(CH₃COO)₂·4H₂O, urea, sodium dodecyl sulfate (SDS), ethanol and water. The calcined sample was characterized by XRD, FTIR, SEM, TG-DTA, Nitrogen adsorption-desorption, cyclic voltammetry and galvanostatic charge/discharge measurements. The results show that the calcined sample at 400 ℃ is rhombohedral structure Co₃O₄ with nano-porosity assembled by uniform nanosheets. The BET surface area is 49 m²·g^-1 and its specific capacitance as single electrode is up to 233.4 F·g^-1 at 5 mA·cm^-2 current density.     

链状[NH3CH2CH2NH3]AgAsS4的溶剂热合成及表征

利用溶剂热方法合成了链状[NH3CH2CH2NH3]AgAsS4,通过单晶X射线衍射技术对其进行了晶体结构分析,该化合物晶体属单斜晶系,空间群C2/c,晶胞参数a=1.35805(8)nm,b=0.65331(3)nm,c=2.27711(9)nm,β=106.42(3)°,Z=8.化合物具有有趣的梯子状双链结构,该阴离子链由AsS4与AgS3共用顶点交替连接而成,有机阳离子在阴离子链之间存在较强的N—H…S氢键.DSC和Tg分析结果表明化合物在200℃以下是稳定的.     

溶剂热还原合成Cr2O3纳米管(英)

Cr₂O₃ nanotubes with diameters of 80 nm and lengths of 550 nm were synthesized in a solvothermal reduction system at 180 ℃. The acetyl acetone (AcAc) and ethylene glycol (EG) were used as the chelate agent and the reductant respectively in the system. An intermediate compound-Cr(Ⅲ)(C₅H₇O₂)₃ was formed to force Cr₂O₃to crystallize along one direction.     

中空Ta2O5/TiO2复合光催化剂的可控氧化制备及性能

以钛粉、钽粉为原料,炭黑作为反应性模板,通过熔盐法在炭黑表面原位生长了TaTiC₂纳米碳化物涂层,并以所得TaTiC₂/C复合物为碳化物前驱体,再经可控氧化制备出中空Ta₂O₅/TiO₂复合光催化剂。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）、紫外-可见（UV-Vis）漫反射（DRS）及N₂物理吸附等手段对所制备的光催化剂进行形貌、显微结构及孔结构表征。以高压汞灯为紫外光源,以亚甲基蓝为目标降解物,通过光催化降解实验评价中空Ta₂O₅/TiO₂复合光催化剂的光催化活性。结果表明,熔盐法生长碳化物涂层厚度均匀（20~30 nm）,碳化物主要以TaTiC₂晶相存在且具有纳米级的颗粒尺寸。中空Ta₂O₅/TiO₂复合光催化剂同时具有200 nm左右的中空大孔结构及壳层10 nm左右的介孔结构。中空大孔和介孔的存在提高了所制备催化剂对亚甲基蓝的吸附能力。此外,TiO₂与Ta₂O₅通过电子能带结构的耦合,有效提高了光生电子和空穴的分离效率,从而显著提高了光催化活性。n_Ti∶n_Ta=2.5∶1.5时,相应的中空Ta₂O₅/TiO₂复合光催化剂表现出最佳的光催化活性,对亚甲基蓝的紫外光催化降解率高达97%。     

中空Ta_2O_5/TiO_2复合光催化剂的可控氧化制备及性能

以钛粉、钽粉为原料,炭黑作为反应性模板,通过熔盐法在炭黑表面原位生长了TaTiC_2纳米碳化物涂层,并以所得TaTiC_2/C复合物为碳化物前驱体,再经可控氧化制备出中空Ta_2O_5/TiO_2复合光催化剂。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)、紫外-可见(UV-Vis)漫反射(DRS)及N2物理吸附等手段对所制备的光催化剂进行形貌、显微结构及孔结构表征。以高压汞灯为紫外光源,以亚甲基蓝为目标降解物,通过光催化降解实验评价中空Ta_2O_5/TiO_2复合光催化剂的光催化活性。结果表明,熔盐法生长碳化物涂层厚度均匀(20~30 nm),碳化物主要以TaTiC_2晶相存在且具有纳米级的颗粒尺寸。中空Ta_2O_5/TiO_2复合光催化剂同时具有200 nm左右的中空大孔结构及壳层10 nm左右的介孔结构。中空大孔和介孔的存在提高了所制备催化剂对亚甲基蓝的吸附能力。此外,TiO_2与Ta2O5通过电子能带结构的耦合,有效提高了光生电子和空穴的分离效率,从而显著提高了光催化活性。nTi∶nTa=2.5∶1.5时,相应的中空Ta_2O_5/TiO_2复合光催化剂表现出最佳的光催化活性,对亚甲基蓝的紫外光催化降解率高达97%。     

Preparation of Li4Ti5O12 Microspheres with a Pure Cr2O3 Coating Layer and its Effect for Lithium Storage

The pure Cr₂O₃ coated Li₄Ti₅O₁₂ microspheres were prepared by a facile and cheap solutionbased method with basic chromium(III) nitrate solution (pH=11.9). And their Li-storage properties were investigated as anode materials for lithium rechargeable batteries. The pure Cr₂O₃ works as an adhesive interface to strengthen the connections between Li₄Ti₅O₁₂ particles, providing more electric conduction channels, and reduce the inter-particle resistance. Moreover, LixCr₂O₃, formed by the lithiation of Cr₂O₃, can further stabilize Li₇Ti₅O₁₂ with high electric conductivity on the surface of particles. While in the acid chromium solution (pH=3.2) modification, besides Cr₂O₃, Li₂CrO₄ and TiO₂ phases were also found in the final product. Li₂CrO₄ is toxic and the presence of TiO₂ is not welcome to improve the electrochemical performance of Li₄Ti₅O₁₂ microspheres. The reversible capacity of 1% Cr₂O₃-coated sample with the basic chromium solution modification was 180 mAh/g at 0.1 C, and 134 mAh/g at 10 C. Moreover, it was even as high as 127 mAh/g at 5 C after 600 cycles. At-20℃, its reversible specific capacity was still as high as 118 mAh/g.     

Nb2O5/γ-Al2O3表面铌氧物种的分散状态与酸性特征

负载型Nb2O5是多种催化反应的有效催化剂. 以草酸铌为前驱物, γ-Al2O3为载体, 通过浸渍法制备不同负载量的Nb2O5/γ-Al2O3催化剂. 采用粉末X射线衍射(XRD)、激光拉曼光谱(LRS)和吡啶吸附傅立叶变换红外(Py-IR)光谱方法对催化剂表面铌氧(NbOx)物种的分散特征、酸性特征进行表征, 通过异丁烯(IB)与异丁醛(IBA)缩合生成2,5-二甲基-2,4-己二烯(DMHD)反应评价催化剂表面酸催化活性. 结果表明, Nb在γ-Al2O3表面的单层分散容量(ΓNb)为7.6 μmol·m-2, 与“嵌入模型”理论分析Nb5+分散在γ-Al2O3优先暴露晶面(110)上八面体空位中的单层分散容量值7.5 μmol·m-2接近, 即分散的Nb5+离子键合在γ-Al2O3表面八面体空位中. 在低负载量下, 分散在γ-Al2O3表面的Nb2O5主要以孤立的NbOx物种形式通过Nb—O—Al键与载体表面键合, 与LRS结果一致. 处于孤立状态下的NbOx物种使表面Lewis 酸位量下降. 随负载量的增加, 孤立的NbOx物种通过Nb—O—Nb键连接而聚集, 并形成表面Bronsted酸位, 随着NbOx聚集度增加, 表面Bronsted 酸密度增加, 酸性增强, 对IBA与IB缩合反应催化活性增加. 当负载量超过单层分散容量时, NbOx物种呈现三维聚集状态, DMHD的转化频率(TOF)降低, 同时表面Bronsted 酸性增强, 导致目标产物DMHD 的选择性降低. Nb2O5/γ-Al2O3催化剂表面Bronsted 酸特征与NbOx物种聚集状态密切相关.     

Preparation and performances of nanosized Ta2O5 powder photocatalyst

Nanosized-Ta₂O₅ powder photocatalyst was successfully synthesized by using sol-gel method via TaCl₅ butanol solution as a precursor. Ta₂O₅ species can be formed under 500 °C via the decomposition of the precursor. The crystalline phase of Ta₂O₅ powder photocatalyst can be obtained after being calcined above 600 °C for 4 h. The crystal size and particle size of Ta₂O₅ powder photocatalyst was about 50 nm. A good photocatalytic performance for the degradation of gaseous formaldehyde was obtained for the nanosized-Ta₂O₅ powder. The Ta₂O₅ powder formed at 700 °C for 4 h and at 650 °C for 12 h showed the best performance. The calcination temperature and time play an important role in the crystallization and photocatalytical performance of nanosized-Ta₂O₅ powder.     

P2O5对Li2O-SiO2-Al2O3-K2O-ZnO体系微晶玻璃析晶性能的影响

采用差热分析、X射线衍射及扫描电镜分析手段研究了P₂O₅对Li₂O-SiO₂-Al₂O₃-K₂O-ZnO体系牙科微晶玻璃析晶性能的影响, 并确定了P₂O₅的最适含量. 结果发现P₂O₅是该玻璃体系的有效成核剂, 未添加P₂O₅的玻璃体系成核密度低, 热处理后不能形成微晶体, 且主晶相为硅酸锂; 添加P₂O₅使玻璃在热处理后形成以二硅酸锂为主晶相的微晶玻璃. 该玻璃体系中添加4.5 wt%的P₂O₅可以得到较高体积含量和理想显微结构的牙科二硅酸锂微晶玻璃. P₂O₅含量为6 wt%的基质玻璃发生乳浊, 呈不透明的乳白色.     

Catalytic decomposition of H2O2 on Co3O4 doped with MgO and V2O5

The effects of doping of Co₃O₄with MgO (0.4–6 mol%) and V₂O₅ (0.20–0.75 mol%) on its surface and catalytic properties were investigated using nitrogen adsorption at −196°C and decomposition of H₂O₂ at 30–50°C. Pure and doped samples were prepared by thermal decomposition in air at 500–900°C, of pure basic cobalt carbonate and basic carbonate treated with different proportions of magnesium nitrate and ammonium vanadate. The results revealed that, V₂O₅ doping followed by precalcination at 500–900°C did not much modify the specific surface area of the treated Co₃O₄ solid. Treatment of Co₃O₄ with MgO at 500–900°C resulted in a significant increase in the specific surface area of cobaltic oxide. The catalytic activity in H₂O₂ decomposition, of Co₃O₄ was found to suffer a considerable increase by treatment with MgO. The maximum increase in the catalytic reaction rate constant (k) measured at 40°C on Co₃O₄ due to doping with 3 mol% MgO attained 218, 590 and 275% for the catalysts precalcined at 500, 700 and 900°C, respectively. V₂O₅-doping of Co₃O₄ brought about a significant progressive decrease in its catalytic activity. The maximum decrease in the reaction rate constant measured at 40°C over the 0.75 mol% V₂O₅-doped Co₃O₄ solid attained 68 and 93% for the catalyst samples precalcined at 500 and 900°C, respectively. The doping process did not modify the activation energy of the catalyzed reaction but much modified the concentration of catalytically active constituents without changing their energetic nature. MgO-doping increased the concentration of CO³⁺–CO²⁺ ion pairs and created Mg²⁺–CO³⁺ ion pairs increasing thus the number of active constituents involved in the catalytic decomposition of H₂O₂. V₂O₅-doping exerted an opposite effect via decreasing the number of CO³⁺–CO²⁺ ion pairs besides the possible formation of cobalt vanadate.     

以CuC2O4微球为模板可控合成一维CuC2O4/ZnO异质结构

以CuC2O4纳米微球为模板,通过水热法在120 ℃、1 h时成功合成了一维CuC2O4/ZnO异质结构。 采用热重分析（TGA）、场发射扫描电子显微镜（FE-SEM）、能量散射Ｘ射线谱（EDX）、透射电子显微镜(TEM)和Ｘ射线粉末衍射(XRD)等测试技术对产物的结构和形貌进行了表征。 结果表明,所得产物为一维CuC2O4/ZnO纳米棒束,长约1 μｍ,直径约500 nm。 每个棒束由许多纳米棒沿同一方向组装而成。 TEM照片和EDX光谱表明,CuC2O4和ZnO形成了均匀的异质结构。     

V2O5电致变色薄膜的Raman光谱

The amorphous V 2O 5 films prepared by vacuum evaporation are unstable and easily dissolved by electrolyte during the electrochromic process, so unfit to make electrochromic materials. We found that the annealed films have enhanced stability and electrochromic properties. We studied the microstructural changes during the electrochromic process by Raman spectra and discussed the mechanism for the enhancement. The results indicated that the amorphous films annealed by 400-500℃became polycrystalline and the films contained (V 2O 5)n ordered chains which prevented the films from solution effectively and enhanced the electrochromic characteristics. When colored and decolored, the microstructure of the polycrystalline V 2O 5 films changed inversely. During the cathodic polarization process, Li+ inserted into the V 2O 5 crystal cell , formed V-O-Li band, disordered the films and UV absorption of the films blue shifted. On the contrary , during the anodic polarization process, Li +escaped from the crystal cell. The films largely restored .