碳酸钙纳米结构多孔空心微球的制备及其药物缓释性能研究

以CaCl2和Na2CO3为反应物,十二烷基硫酸钠(SDS)为表面活性剂,在室温水溶液中制备了纳米结构碳酸钙空心球.用TEM和SEM对其进行形貌观察发现,所制备的碳酸钙空心球的球壁由纳米粒子组成,具有多孔形貌特征.分别在模拟胃液(pH＝1.2)以及模拟肠液(pH＝7.4)中对制备的纳米结构碳酸钙空心球进行了药物装载和缓释性能的研究,选用的药物为布洛芬(IBU).研究结果表明,IBU/CaCO3多孔空心微球药物传输体系具有较高的药物装载量和良好的药物缓释性能,纳米结构碳酸钙空心球中IBU的装载量可以达到195mg/g,且连续释药时间能持续53h以上;除去表面活性剂后,载体中IBU的装载量可达到130mg/g,药物释放率为100%时,持续释药时间可达到40h.纳米结构碳酸钙多孔空心球作为药物载体材料在药物缓释体系中具有潜在的应用前景.     

有机-无机氧化硅空心球的合成及VOCs吸附应用

介孔有机-无机复合氧化硅空心球(MOSs)在碱性条件下以反向胶束为模板经过正硅酸乙酯(TEOS)和1,2-双(三乙氧基甲硅烷基)乙烷(BTSE)共缩合被成功合成, 并通过不同手段对样品的结构和性能进行表征。MOSs用于去除挥发性有机物(VOCs), 研究其对水蒸气、正己烷、甲苯和92#汽油的静态吸附性能, 并以商业硅胶(SG)和活性炭(AC)为参考。实验结果发现, 初始BTSE/(BTSE+TEOS) 摩尔比为10%时, (MOS-10%)的样品具有均匀的中空介观结构和最大的VOCs吸附容量(1.28 g·g^-1正己烷, 1.25 g·g^-1甲苯和1.14 g·g^-1 92#汽油), 静态水蒸气吸附量最小(0.630 g·g^-1)。通过穿透曲线评估单一组分VOC(正己烷或甲苯)在MOS-10%上的动态吸附行为, 动态正己烷和甲苯吸附结果以及高湿度条件下的正己烷吸附性能表明, 与商业吸附剂相比, MOS-10%具有最佳的穿透时间、吸附能力和疏水性。对于二元组分同时吸附(正己烷和甲苯), MOS-10%的正己烷吸附性能优于甲苯。介孔有机-无机复合氧化硅空心球的动态VOCs吸附容量较大归因于有机基团、表面积和孔体积的共同作用。MOSs的VOCs去除能力强和可回收性优良, 显示出巨大的VOCs捕获潜力。     

基底材料对沉积氮化钛薄膜及其性能的影响

研究了利用直流反应磁控溅射法,以Si—P（111）和Si—P（100）两种不同Si片做基底,对制备TiNx薄膜性能的影响。结果表明,以Si--p（111）为基底制备的TiNx薄膜性能优于Si--p（100）基底,表现在颗粒更细润,XRD衍射峰峰形更明锐且与TiNx的衍射峰不会重叠。因而,选用p--Si（111）做基底沉积氮化钛薄膜,可满足制备光学薄膜质量方面的要求。     

An Investigation of Titanium Nitride Prepared by a DC Arc Plasma Jet

The properties of a titanium nitride film prepared by a DC arc plasma jet were investigated by microscopic observations, composition analysis, and hardness measurements. Scanning electron microscopy showed that the film was composed of three phases, designated the A, B, and C regions from the outer surface. The existence of three regions was also supported by composition analysis and hardness measurements on the cross section. XRD patterns showed the presence of -TiN in the A region. In the B region, a number of voids were observed, which have never been reported in previous papers. These were made up from specific crystallographic surfaces. The C region also had a few voids which were somewhat different from those in the B region. In the matrix, an acicular texture was found and identified as -Ti solid solution by XRD. The cross section of the film changed the color determined by the nitrogen content.     

分级介孔结构组成的ZnO微球及光催化性能

以硝酸锌、脲素及酒石酸为反应物, 采用水热法制备碱式碳酸锌前驱体微球, 通过煅烧前驱体制备了介孔氧化锌微球。通过扫描电子显微镜(SEM)可以观察到, 氧化锌微球的直径约为2~4 μm, 由大量厚度约为10 nm的介孔纳米片组装而成。X 射线衍射(XRD)和透射电镜(TEM)结果表明: ZnO微球为六方纤锌矿结构, 并结晶较好。比表面积测试(BET)表明ZnO微球为介孔材料, 孔径为20~50 nm, ZnO微球比表面积约为29.8 m²/g。以亚甲基蓝为目标降解物, 对介孔氧化锌微球进行了光催化降解实验。实验结果表明, 所合成的介孔ZnO微球对亚甲基蓝的光催化性能较好。     

A Salt‐Templated Strategy toward Hollow Iron Selenides‐Graphitic Carbon Composite Microspheres with Interconnected Multicavities as High‐Performance Anode Materials for Sodium‐Ion Batteries

In this work, a facile salt‐templated approach is developed for the preparation of hollow FeSe₂/graphitic carbon composite microspheres as sodium‐ion battery anodes; these are composed of interconnected multicavities and an enclosed surface in‐plane embedded with uniform hollow FeSe₂ nanoparticles. As the precursor, Fe₂O₃/carbon microspheres containing NaCl nanocrystals are obtained using one‐pot ultrasonic spray pyrolysis in which inexpensive NaCl and dextrin are used as a porogen and carbon source, respectively, enabling mass production of the composites. During post‐treatment, Fe₂O₃ nanoparticles in the composites transform into hollow FeSe₂ nanospheres via the Kirkendall effect. These rational structures provide numerous conductive channels to facilitate ion/electron transport and enhance the capacitive contribution. Moreover, the synergistic effect between the hollow cavities within FeSe₂ and the outstanding mechanical strength of the porous carbon matrix can effectively accommodate the large volume changes during cycling. Correspondingly, the composite microsphere exhibits high discharge capacity of 510 mA h g^?1 after 200 cycles at 0.2 A g^?1 with capacity retention of 88% when calculated from the second cycle. Even at a high current density of 5.0 A g^?1, a high discharge capacity of 417 mA h g^?1 can be achieved.     

二氧化钛介孔材料的合成研究

介孔二氧化钛特殊的结构和性能,使其在催化、吸附、分离等领域展现出广阔的应用前景.介绍了有序介孔材料的合成机理,综述了不同类型的表面活性剂在二氧化钛介孔材料合成中的应用和研究进展,指出了表面活性剂脱除的关键问题及解决方法.     

超声喷雾热解法制备半导体薄膜技术

超声喷雾热解法(USP)作为一种新兴的薄膜制备技术,已制备出多种半导体薄膜材料,并成功应用于太阳能电池、传感器、固态氧化物燃料电池等领域。介绍了USP制备薄膜技术的原理,结合近年来USP技术在半导体薄膜制备领域的研究进展,系统阐述了超声喷雾热解法制备薄膜的原理、工艺过程及在此过程中发生的物理化学变化,详细分析了前驱体溶液化学组成、沉积温度、退火处理等各个工艺参数对薄膜沉积过程和成膜质量的影响,指出了该技术目前存在的问题及今后的发展方向。     

Rational Design and Synthesis of Extremely Efficient Macroporous CoSe2–CNT Composite Microspheres for Hydrogen Evolution Reaction

Uniquely structured CoSe₂–carbon nanotube (CNT) composite microspheres with optimized morphology for the hydrogen‐evolution reaction (HER) are prepared by spray pyrolysis and subsequent selenization. The ultrafine CoSe₂ nanocrystals uniformly decorate the entire macroporous CNT backbone in CoSe₂–CNT composite microspheres. The macroporous CNT backbone strongly improves the electrocatalytic activity of CoSe₂ by improving the electrical conductivity and minimizing the growth of CoSe₂ nanocrystals during the synthesis process. In addition, the macroporous structure resulting from the CNT backbone improves the electrocatalytic activity of the CoSe₂–CNT microspheres by increasing the removal rate of generated H₂ and minimizing the polarization of the electrode during HER. The CoSe₂–CNT composite microspheres demonstrate excellent catalytic activity for HER in an acidic medium (10 mA cm^?2 at an overpotential of ≈174 mV). The bare CoSe₂ powders exhibit moderate HER activity, with an overpotential of 226 mV at 10 mA cm^?2. The Tafel slopes for the CoSe₂–CNT composite and bare CoSe₂ powders are 37.8 and 58.9 mV dec^?1, respectively. The CoSe₂–CNT composite microspheres have a slightly larger Tafel slope than that of commercial carbon‐supported platinum nanoparticles, which is 30.2 mV dec^–1.     

微纳分级结构碳酸钙中空微球的可控制备

以CaCl₂和Na₂CO₃为反应原料, 以聚乙烯吡咯烷酮(PVP)和十二烷基磺酸钠(SDSN)为模板剂, 在50℃采用化学沉淀反应, 干燥、煅烧后成功制备了具有微纳分级结构的CaCO₃中空微球。采用扫描电子显微镜、透射电子显微镜和X射线衍射等检测手段对所制备的样品形貌、结构进行了表征, 结果显示：所制备的微纳分级结构CaCO₃中空微球直径为4~6 μm, 壳壁由直径约60 nm的CaCO₃颗粒组成, 壳层厚度约为200 nm, CaCO₃中空微球晶相组成为方解石和球霰石的共混体。同时, 在反应温度为50℃、PVP添加量为0.4 g, SDSN浓度为0.1 mol/L的条件下, 所制备的微纳分级结构CaCO₃中空微球分散性好, 且形貌比较完整。     

喷雾热分解法制备氧化锆纤维的过程研究

本文研究了喷雾热解法制备氧化锆纤维的过程．用醋酸氧锆为前驱体能够制备出直径1～2μm、长度1～5cm的氧化锆纤维．研究了前驱体溶液浓度、表面张力、粘度对产品形貌的影响．通过控制操作条件,可以得到实心或空心纤维．     

含氮表层对钛合金薄壁件热处理变形影响的数值预报

试图用数值模拟技术揭示含氮表层对钛合金热处理变形的影响,以减少热处理变形.测定了Ti6Al4V合金表面氮化钛沉积及其扩散层的表面相结构、弹性模量和硬度分布值.结果表明,氮化钛沉积层在800 ℃保温10 h,表面层由TiN和Ti2N组成,扩散层中显微硬度呈梯度分布,弹性模量最高可以达到270 GPa.建立了钛合金薄壁件在淬火过程中温度场和应力场的数学模型,利用ANSYS软件计算了钛合金筒形薄壁件的热处理变形.表层中氮化相的存在使钛合金筒形薄壁件的变形减少17.26%.     

氧化锌空心球的制备及光致发光特征

采用水热和硬模板辅助技术,成功制备得到ZnO空心球结构.以葡萄糖和锌盐为原料,首先通过催化葡萄糖聚合-原位离子吸附一步进行(一步法)或葡萄糖聚合成球-离子吸附分步进行(二步法)制备锌/炭复合微球,然后经空气低温氧化制得ZnO空心球.用XRD、SEM、TEM研究产物的组成和结构及形貌,用光致发光光谱(PL)测试产物的室温光致发光性能.研究发现,两种方法得到的空心球壳均属多孔结构,由ZnO纳米粒子构成;与聚合-吸附分步法相比,聚合-原位离子吸附一步法更加简单快捷;制得的ZnO空心球结构材料具有良好的近紫外发光性能.对ZnO空心球结构的形成过程和可能的机制进行了分析和讨论.     

纳米TiO2中空微球的酸催化水解-水热法制备

以水热法制得的炭球为模板,通过酸催化水解法在其表面合成TiO2前驱体壳层,经煅烧除去炭球,最终制得中空TiO2微球。使用SEM、TEM、XPS、XRD及N2吸附-脱附等手段对产物进行结构表征。以苯酚为模型物在紫外光下对其活性进行评价。结果表明,经煅烧后TiO2前驱体实现由无定形向锐钛矿相的转变,炭球烧蚀,从而生成具有中空结构的TiO2微球。随葡萄糖溶液浓度增加,炭球直径增加,TiO2中空微球的球径也随之增加。通过调整葡萄糖溶液浓度可以对TiO2中空微球尺寸进行控制。当葡萄糖溶液浓度为0.7mol/L时,最终所得TiO2中空微球直径约为200nm,壁厚约为28nm,比表面积为66.6m2/g,孔径为6.56nm,整体排布平整。煅烧温度为600℃的TiO2中空微球对苯酚去除率最高,可达81.5%,为同法制备的非空心TiO2的1.35倍。     

Synthesis Process of CoSeO3 Microspheres for Unordinary Li‐ion Storage Performances and Mechanism of Their Conversion Reaction with Li ions

Multicomponent materials with various double cations have been studied as anode materials of lithium‐ion batteries (LIBs). Heterostructures formed by coupling different‐bandgap nanocrystals enhance the surface reaction kinetics and facilitate charge transport because of the internal electric field at the heterointerface. Accordingly, metal selenites can be considered efficient anode materials of LIBs because they transform into metal selenide and oxide nanocrystals in the first cycle. However, few studies have reported synthesis of uniquely structured metal selenite microspheres. Herein, synthesis of high‐porosity CoSeO₃ microspheres is reported. Through one‐pot oxidation at 400 °C, CoSe_x–C microspheres formed by spray pyrolysis transform into CoSeO₃ microspheres showing unordinary cycling and rate performances. The conversion mechanism of CoSeO₃ microspheres for lithium‐ion storage is systematically studied by cyclic voltammetry, in situ X‐ray diffraction and electrochemical impedance spectroscopy, and transmission electron microscopy. The reversible reaction mechanism of the CoSeO₃ phase from the second cycle onward is evaluated as CoO + xSeO₂ + (1 ? x)Se + 4(x + 1)Li⁺+ 4( x + 1)e^? ? Co + (2x + 1)Li₂O + Li₂Se. The CoSeO₃ microspheres show a high reversible capacity of 709 mA h g^?1 for the 1400th cycle at a current density of 3 A g^?1 and a high reversible capacity of 526 mA h g^?1 even at an extremely high current density of 30 A g^?1.     

聚多巴胺修饰的介孔二氧化硅微球的合成及其用于负载左旋薄荷醇凉味剂

介孔二氧化硅材料具有巨大的孔隙率、开放的孔道结构、易于改性的孔道表面以及良好的生物相容性, 广泛用于药物传递、吸附分离以及催化等领域。本研究通过非极性溶剂辅助共组装法合成了具有较大孔径(6.9 nm)和比表面积(615 m²/g)的介孔二氧化硅微球。采用纳米浇铸的方法, 成功地将左旋-薄荷醇负载到该材料的孔内。进一步通过界面聚合的方法, 在所得微球的表面涂覆一层聚多巴胺(PDA)涂层, 从而将薄荷醇封装在微球的孔道内。利用PDA作为半透膜, 研究了复合微球在不同温度的空气吹扫下释放薄荷醇的行为, 发现在相对适宜的温度下PDA涂层有利于薄荷醇的可控缓慢释放。这些研究结果表明基于聚多巴胺修饰的介孔二氧化硅材料有望用于开发食品和医药等领域的缓释制剂。     

La掺杂TiO2介孔微球的超声水热合成和光催化性能

以钛酸四丁酯为钛源、硝酸镧为镧源、十二胺为模板剂,采用超声?水热法合成了La3+掺杂介孔TiO2微球,并利用XRD、XPS、TEM、BET、UV-Vis、IR、FL等手段表征了材料的结构、形貌、比表面积、孔径分布及光学性能.研究结果表明,适量La3+离子掺杂不仅能使介孔TiO2晶粒细化,比表面积增大,荧光强度减弱.La3+/TiO2的光吸收边红移,并具有比商业P25更好的光催化活性,其中介孔La3+/TiO2(2.0at%)的比表面积和平均孔径分别为132.7 m2/g和8.67 nm,光催化降解初始浓度为40 mg/L的亚甲基蓝溶液120 min时,其降解率达到98.5%,表现出最强的光降解能力.     

铁/镱掺杂二氧化钛空心球的制备及其光催化性能

用模板法制备铁/镱共掺杂二氧化钛空心球(Fe/Yb-TiO2HS),使用扫描电子显微镜(SEM)观察和X射线衍射(XRD)、X射线光电子能谱(XPS)、傅里叶红外光谱(FT-IR)、热失重(TG)等测试方法对对其进行了表征.使用浓度为20 mg/L的甲基橙溶液模拟废水,研究了铁/镱共掺杂二氧化钛空心球的催化性能.结果 ...     

介孔TiO2/WO3空心球的制备及其可见光光催化性能

以硫酸氧钛和偏钨酸铵为前驱体, 以柠檬酸作为络合剂, 采用喷雾干燥-高温煅烧两步法制备了介孔TiO₂/WO₃空心球复合材料。利用SEM、TEM、BET、XRD、UV-Vis DRS等手段对样品的形貌、微结构、比表面积、晶相组成和光学性能进行了表征和分析, 以亚甲基蓝为模拟降解物考察其光催化性能。结果表明: 复合材料为介孔空心球状结构, 球体分散好, 直径主要分布在1 μm左右; 球壁由纳米颗粒和空隙构成, 随着煅烧温度的升高, 颗粒粒径不断增大, 空隙孔径不断增大。性能研究结果表明, TiO₂与WO₃复合后, 样品对光的吸收范围扩展到了可见光区域, 这有利于提高太阳光的利用率; 当前驱体中WO₃含量为3mol%, 样品的煅烧温度为500℃时, 复合材料具有最好的光催化性能: 对亚甲基蓝降解率可达99.1%, 而P25的降解率仅为29.5%。