SnS纳米及微米晶的制备及结构表征

用溶剂热法制备了SnS带状纳米晶和管状微米晶,通过XRD、SEM、TEM等方法对所制备的SnS纳米及微米晶的结构、形貌及组成进行了表征。结果表明,采用Na2S为硫源,乙二醇作溶剂,可制得宽度50~300 nm,长度1~1.5μm的单一晶型的SnS纳米带;采用硫脲为硫源,乙二胺作溶剂,聚丙烯酰胺作分散剂,可制得孔径为0.4~0.8μm,长度达十几微米的管状SnS微米晶。     

Microwave-assisted synthesis and electrochemical characterization of TiNb2O7 microspheres as anode materials for lithium-ion batteries

TiNb₂O₇ microspheres are prepared via a microwave-assisted solvothermal method. The microwave irradiation lowers the compound formation temperature to 600°C, and highly crystalline TiNb₂O₇ powders are obtained upon calcination at 800°C. Morphological analysis of the sample shows uniformly distributed microspheres with a particle size of around 1 μm. The Li⁺-ion diffusion coefficient calculated from the electrochemical impedance result is around 1.21 × 10⁻¹³ cm² s⁻¹, which is 1.5 times higher than the sample obtained from the conventional solvothermal method. The TiNb₂O₇ sample derived from microwave yields a high discharge capacity of 299 mA h g⁻¹ at 0.1 C, whereas the sample synthesized via the conventional solvothermal process yields only 278 mA h g⁻¹ at 0.1 C. Excellent rate capabilities such as 220 mA h g⁻¹ at 5 C and 180 mA h g⁻¹ at 10 C are also observed for the microwave-assisted solvothermal sample. Moreover, the sample exhibits a large capacity retention of 95.5% after 100 discharge–charge cycles at 5 C. These results reveal the appropriateness of the microwave-assisted solvothermal process to prepare TiNb₂O₇ powders with superior properties for battery applications.     

溶剂热法制备氨基修饰的Fe3O4纳米粒子及其性能

采用溶剂热法以FeC13?6H2O、乙二醇和聚乙烯亚胺为原料,一步法制备氨基修饰的Fe3O4纳米粒子.并利用X射线衍射、扫描电子显微镜、振动样品磁强计和红外光谱等方法对产物进行分析和表征.研究了反应釜填充度、反应时间、Fe3+初始浓度以及NaAC的浓度对反应产物的影响,结果表明:反应釜填充度、反应时间、Fe3+初始浓度...     

Surface Energy Engineering in the Solvothermal Deoxidation of Graphene Oxide

A route to achieving high yields of monodisperse, deeply deoxidized graphene oxide (GO) in solution is presented. It overcomes many of the problems of dispersibility and inefficient reduction of GO in solvothermal deoxidation that are usually observed, despite the previous use of strong reducing agents (e.g. Fe²⁺, S or hydrazine). It is shown that the incomplete deoxidation is most likely due to agglomeration/self‐assembly of partially reduced GO, which also creates poor dispersibility. GO deoxidation is found to be highly sensitive to the solvent surface energy and, through experiments and empirical calculations, tuning the solvent surface energy to around 85.6 mJ/m² (at 100 °C) leads to fully deoxidized GO. These calculations also allow appropriate solvent surface energies to be calculated for other temperatures for deep deoxidation of GO. This approach makes solvothermal deoxidation of GO a potential route to large scale, economic production of highly disperse monolayered graphene.     

镁合金表面铁氧化物涂层的制备及其耐蚀性能

镁合金的耐蚀性差,严重限制了其在生物材料领域的应用。在镁合金表面采用化学还原法和溶剂热法复合制备了铁氧化涂层,利用扫描电镜(SEM)、X射线衍射(XRD)和能谱(EDS)等对样品的结构与组成进行表征,分别采用Tafel测试和磷灰石诱导试验评价了样品的耐蚀性和生物相容性。结果表明:涂层的主要组分为Fe3O4、Fe2O3和FeO;随着乙醇浓度降低和溶剂热时间延长,涂层粗糙度先降低后升高;Tafel测试表明,随着乙醇浓度的增加,涂层的耐蚀性先增高后降低;在乙醇浓度为90%,溶剂热时间4 h时获得的涂层表面无脱落现象,微裂缝数量最小,具有最高的耐腐蚀性能,极化电阻达51 779.2Ω,并具有良好的生物诱导活性。     

单分散Fe_3O_4纳米粉体的溶剂热合成及磁性

以Fe(NO3)3.9H2O和KOH为原料,以乙二醇为溶剂,溶剂热制备了单分散Fe3O4纳米粉体。利用XRD和TEM对溶剂热合成的Fe3O4纳米粉体进行了物相和形貌表征,利用物理性质测量体系PPMS-9T对合成的Fe3O4纳米粉体的磁性能进行了测定。结果表明,低于220℃时溶剂热合成的Fe3O4纳米粉体颗粒较小,约10 nm,具有超顺磁性质;而250℃时溶剂热合成的Fe3O4纳米粉体颗粒粒径较大,约50 nm,具有典型的铁磁性能,其室温饱和磁化强度为68.8 emμ.g-1,剩余磁化率为12.9 emμ.g-1,矫顽力达138.5 Oe,磁性能优于水热合成的Fe3O4纳米粉体。基于实验结果,探讨了乙二醇溶剂热过程中Fe3O4的形成机理,以及合成的Fe3O4纳米粉体具有良好单分散性的原因。     

芳纶固载BiOBr复合材料的制备及其光催化降解染色废水

为解决粉体光催化剂在降解纺织印染废水过程中易团聚、难以回收利用的问题,采用溶剂热法制备芳纶固载BiOBr(BiOBr/AF)复合材料,对材料的微观形貌和结构进行表征与分析,研究了BiOBr/AF在可见光照射下对模拟染色废水的光催化深度降解性能.结果表明:以乙二醇为溶剂,柠檬酸为螯合剂,芳纶为固载基体,于160℃下反应1...     

陈皮中橙皮苷的溶剂热法提取工艺及检测方法的研究

以橙皮苷得率为指标,采用溶剂热法提取陈皮中的橙皮苷,通过单因素实验考察了提取温度、乙醇浓度、液料比以及提取时间对橙皮苷得率的影响。在此基础上,利用正交实验法对溶剂热法提取工艺进行了优化。结果表明:提取时间对橙皮苷的得率影响最大,其次是提取温度。优选的橙皮苷提取条件为:提取温度120℃,乙醇浓度60%,液料比70∶1 m L·g-1,提取时间45 min,在上述条件下测得橙皮苷得率为6.07%±0.03%。同传统的乙醇回流法相比,溶剂热法的提取时间缩短了近70%,橙皮苷得率约提高1倍。      

Nickel sulfide as co-catalyst on nanostructured TiO2 for photocatalytic hydrogen evolution

In this study, TiO₂ photocatalysts with nickel sulfide cocatalyst are prepared by loading nickel sulfide on TiO₂ with solvothermal synthesis approach. The materials were prepared by glycol solvothermal method using anatase, nickel nitrate, thiourea as precursor. The prepared catalysts were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet–visible diffuse reflectance spectroscopy (UV–vis DRS), and X-ray photoelectron spectroscopy (XPS). This is the first time to report that NiS is used as a cocatalyst with TiO₂ for the photocatalytic production of H₂. The results revealed that the structure and the amount of the cocatalyst loaded on TiO₂ play important roles in the photocatalytic activity of NiS/TiO₂ composite. The maximum evolution of H₂ was obtained when NiS had hexagonal structure with content in the composite of 7 at% in relation to TiO₂. The rate of H₂ evolution was increased up to about 30 times than that of TiO₂ alone.