以NaHCO3为矿化剂溶剂热合成Zn2SnO4纳米粉体

以NaHCO3为矿化剂采用溶剂热法合成了Zn2SnO4纳米粉体,通过X-射线衍射（XRD）、扫描电镜（SEM）和透射电镜（TEM）考察了矿化剂浓度、溶剂热反应温度和时间、表面活性剂等对样品组成、结构和形貌的影响,结果表明：矿化剂浓度较低时所得样品为SnO2,矿化剂浓度为1.0 mol/L、溶剂热反应温度和时间为200℃,24 h时,可得立方结构的分散均匀的Zn2SnO4纳米粉体,添加表面活性剂PVP后,样品粒度增大,立方块形貌更加明显.     

高电压磷酸钴锂正极材料性能调控研究

高性能、高安全储能电池的迫切需求加速了橄榄石型高电压正极材料的研究步伐。为了改善高电压磷酸钴锂(LiCoPO₄)的综合电化学性能,采用溶剂热法研究了溶剂比、过渡元素(Fe、Mn)单掺杂和双掺杂(掺杂元素总量占10%)对正极材料形貌、尺寸、反位缺陷和电化学性能的影响。结果表明,当溶剂比为2.3时,未掺杂LiCoPO₄在0.1C下表现出163.1 mAh·g^-1的最高理论比容量;双掺杂LiCo_0.9Mn_0.05Fe_0.05PO₄正极材料具有突出的循环性能,在0.5C电流密度下,循环100圈后的容量保持率为78.9%,循环稳定性得到明显改善。     

无模板法可控合成多层次结构二氧化钛微球

以1,4-二氧六环为溶剂,采用溶剂热法成功实现无模板法可控合成二氧化钛多层次结构微球。通过系统改变反应体系中浓盐酸与四异丙醇钛(TTIP)相对物质的量比能够有效调控二氧化钛形貌。当浓盐酸与TTIP物质的量比控制在0(或0.7或0.9)、1.8、3.6与5.7时,所得产物分别为纳米颗粒构建二氧化钛微球、纳米棒修饰二氧化钛微球、纳米棒花菜结构以及纳米棒海胆结构。在成功进行形貌调控的基础上,进一步探讨了二氧化钛多种结构的形成机理,并对其光催化产氢性能进行了表征。研究发现,在这4种结构中,纳米棒修饰二氧化钛微球具有最佳的光催化性能,这可能是由于同时存在金红石和锐钛矿两种晶型而形成异质结结构所导致。     

PdO修饰的SnO2纳米球的制备及其气敏特性研究

通过溶剂热法和退火处理制备了不同浓度(0 mol％,2 mol％,5 mol％,10 mol％)PdO修饰的SnO2纳米球.采用X射线衍射仪(XRD)、X射线能谱分析仪(EDS)和扫描电子显微镜(SEM)等测试手段对材料的物相、元素种类和形貌进行了表征,并制成气敏元件,对氢气(H2)进行气敏测试.实验结果表明:5 mol％PdO修饰的SnO2纳米球气体传感器最佳工作温度为175℃,其对100×10-6氢气灵敏度达到19,是纯的SnO2纳米球的灵敏度的3倍.最后,对PdO修饰氧化锡纳米球气体传感器气敏机理进行了分析讨论.     

Optimization of dielectric heating parameters in the production of high‐voltage LiNiPO4‐core and carbon‐shell ceramics

Excellent core‐shell morphology and nanoscale high‐voltage LiNiPO₄@C cathode materials have been synthesized by a low‐level and long‐time microwave and solvothermal synthesis methodology. The effects of the changing physicochemical parameters on the crystal‐quality and electrochemical properties of the products have been evaluated in relation to the cycling stability. X‐ray diffraction analysis shows that it is possible to synthesize phase‐pure LiNiPO₄ material when the reaction parameters are carefully elaborated. High‐resolution transmission electron microscopy analysis reveals a core‐shell morphology with a coating thickness of 6‐8 nm for 30 minutes at 180°C solvothermal temperature and time‐spread microwave energy. This mentioned cathode material exhibits the best electrochemical properties, achieving a discharge capacity of 157 mAh·g^?1 at a 0.l C current rate, and shows a remarkable 81% capacity retention at the end of the 80th cycle.     

溶剂热法制备介孔球形钛酸锂负极材料

以醋酸锂和钛酸四正丁酯为原料,使用NH4HCO3作为结构引导剂,通过溶剂热法后固相烧结合成了具有尖晶石型介孔球形Li4Ti5O12,探讨了不同的钛锂比和热处理温度及NH4HCO3用量对Li4Ti5O12结构和电化学性能的影响,并通过X射线衍射光谱法(XRD),扫描电子显微镜法(SEM)和恒流充放电对其进行了表征。结果表明通过该法在钛锂摩尔比为5∶4.3时,在800℃下热处理3 h可获得晶型与标准谱一致的Li4Ti5O12,在溶剂热过程中使用NH4HCO3做为结构诱导剂时,可获得具有介孔结构的球形Li4Ti5O12材料,该材料在充放电过程中显示出了较好的电化学性能。     

溶剂热法合成花状Co_3O_4微球及其对高氯酸铵热分解的催化作用

以醋酸钴为原料,在甲醇体系中采用溶剂热法合成了由纳米片自组装而成的花状(CH_3O)_2Co前驱体微球。将前驱体焙烧后,得到了形貌保持良好的花状多孔Co_3O_4微球。利用X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、热重(TG)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和N_2吸附-脱附等手段对样品的物相、化学组成、形貌及孔结构进行了表征。采用差示扫描量热(DSC)技术评价了Co_3O_4花状微球对高氯酸铵(AP)的热分解催化作用。结果表明,花状Co_3O_4微球对AP热分解过程具有良好的催化活性,添加2%(质量分数)的Co_3O_4可使AP的高温分解峰值温度降低122℃,表观分解热提高422 J/g。优异性能的发挥归因于其良好的分散性和丰富的级次孔结构。     

Synthesis and properties of ZnS nanoparticles by solvothermal and pyrolysis routes using the Zn dithiocarbamate complex as novel single source precursor

In this work, the synthesis and characterization of ZnS nanoparticles prepared via two approaches, involving the thermal decomposition of the precursor complex in a furnace (pyrolysis) and by solvothermal process in the presence of hexadecylamine (HDA-ZnS), are reported. The precursor complex, Zinc (II) bis (N,N-diallyl dithiocarbamate), was synthesized and characterized by spectroscopic and single-crystal X-ray techniques. The spectroscopic analyses of the complex indicated a symmetrical bidentate coordination of the dithio ligand through the S-atoms. The single-crystal X-ray structure revealed a distorted square pyramidal coordinate geometry with S atoms around the Zn ion. The optical properties and the morphology of the as-prepared nanoparticles were studied by UV-Vis and photoluminescense spectroscopy, and transmission electron microscopy (TEM), respectively. HDA-ZnS are spherical and monodispersed with an average size of 4.5?nm, as estimated from the optical absorption spectrum and the TEM image. The ZnS nanoparticles obtained via pyrolysis in a furnace yielded the hexagonal wurtzite phase, whereas the HDA-ZnS nanoparticles showed a mixture of wurtzite and cubic phase with the cubic phase being dominant.     

三元多碲化物纳米晶的新方法制备及表征

以硝酸银、氯化亚锡和碲粉为原料经微波溶剂热法制备纳米晶粉体Ag8SnTe6, 通过X射线粉末衍射(XRD)、透射电子显微镜(TEM)和X射线光电子能谱(XPS)等手段表征其组成. 讨论了合成时间和有机溶剂填充度等条件对化合物产率和粒径的影响. 阐述了微波溶剂热法合成纳米晶的机理. 漫反射紫外可见吸收光谱(UV-Vis)表明其禁带宽度为2.58 eV,具有优良的半导体性能.