水热法制备α-FeOOH/MoS2纳米片复合物及其光催化性能

采用水热法成功制备了棒状α-FeOOH/MoS_2纳米片复合催化剂。运用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、紫外可见漫反射光谱(UV-Vis)和荧光发射光谱(PL)对复合催化剂的结构和形貌进行了表征。结果表明:成功制备了长度为500nm左右的纳米棒状α-FeOOH,其与MoS_2纳米片形成良好的复合结构。以亚甲基蓝为模拟污染物,研究复合催化剂在可见光照射下的光催化特性。结果显示,棒状α-FeOOH/MoS_2纳米片复合催化剂在120min内对亚甲基蓝的降解率为98%,其降解动力学常数是纯α-FeOOH的3倍。根据活性基捕获实验结果,提出了α-FeOOH与MoS_2纳米片形成异质结的Z型光催化机理。     

MoS2/g-C3N4复合催化剂的制备及CdSe量子点敏化产氢性能研究

太阳能光催化分解水制氢被认为是从根本上解决能源与环境问题较为理想的途径之一。在以尿素为原料制得石墨相氮化碳(g-C_3N_4)的基础之上,采用简单的低温溶液反应法将二硫化钼(MoS_2)与石墨相氮化碳(g-C_3N_4)复合得到复合催化剂MoS_2/g-C_3N_4,并利用透射电子显微镜(TEM)、X射线衍射(XRD)、紫外-可见漫反射(DRS)、傅里叶变换红外光谱(FT-IR)和荧光光谱等对该复合光催化剂的组成、形貌和光物理性能进行了表征;进而以CdSe量子点为光敏剂,三乙醇胺(TEOA)为牺牲剂,构建了不含贵金属的三组分光催化产氢体系,并对体系pH值、CdSe量子点浓度等对产氢性能的影响进行了研究。结果表明:将MoS_2纳米颗粒负载到g-C_3N_4上可使g-C_3N_4的光催化产氢性能得到显著提高。当MoS_2负载量为7%(质量比)时,在最佳的条件下(pH=9.0,CdSe量子点的体积为25mL),最大产氢速率达到了141.74μmol·h-1,6h的产氢总量达到了212.61μmol。最后,结合荧光猝灭实验,推测了该体系的产氢机理。     

超临界流体干燥法制备TiO2/ Fe2O3 和TiO2/ Fe2O3/ SiO2 复合纳米粒子及光催化性能

以TiCl₄ 、Fe (NO₃ )₃·9H₂O 和Na₂SiO₃19H₂O 为原料, 采用溶胶凝胶法结合超临界流体干燥法(SCFD)制备了纳米级TiO₂/ Fe₂O₃ 和TiO₂/ Fe₂O₃/ SiO₂ 复合光催化剂。以光催化降解苯酚对所得催化剂的催化活性进行了评价。结果表明, 纳米TiO₂/ Fe₂O₃ 复合粒子与单组分TiO₂ 比较, 复合粒子光催化活性高于单组分的TiO₂, 6h 苯酚降解率高达95.9 %。SiO₂ 的加入可以抑制纳米粒子粒径的长大和晶相的转变, 增强TiO₂ 纳米粒子的热稳定性。复合光催化剂中Fe₂O₃ 最佳掺入量为0.06 %, SiO₂ 最佳掺入量为10 %(摩尔分数) 。并用XRD、TEM 和FTIR 等手段进行了表征。TiO₂ 以锐钛矿型形式存在, SiO₂ 以无定性形式存在。比较了不同制备方法制得的TiO₂/ Fe₂O₃ 复合光催化剂, 得出超临界干燥法制备的光催化剂具有粒径小、比表面积大、分散性好、光催化活性高等特点。采用超临界流体干燥可直接得锐钛型纳米复合光催化剂。     

纳米MoS2的合成及其在重油深度转化中的应用

MoS_2是在催化剂领域、光化学领域以及润滑油领域都广受关注的材料。因其良好的加氢活性,通常在石油化工领域中作为加氢过程的催化剂活性组分。介绍了纳米MoS_2的插层剥离法、气相化学沉积法、前驱物分解法、水热合成法等多种合成方法,列举了不同方法合成MoS_2产品在形貌、大小、比表面积等方面的特点,并针对重油转化所需催化剂的特性对不同合成方法的优缺点进行了对比。最后简单介绍了意大利ENI公司以非负载MoS_2作为催化剂在浆态床加氢工业应用的实例。     

ZrO2在β"─Al2O3复合陶瓷中的作用

本文研究了四方和立方ZrO₂在与Na-β"-Al₂O₃的复合陶瓷中作为第二相所起的各种作用。结果说明ZrO₂对复合陶瓷具有细化晶粒、改善显微结构、提高强度和断裂韧性的作用,与此同时也在一定程度上降低离子电导率。在提高力学性能方面,四方ZrO₂除了具有与立方ZrO₂相同的弥散颗粒的作用外,相变所起的作用也是很显着的。ZrO₂-Na-β"-Al₂O₃复合陶瓷是一种有应用价值的固体电解质材料。     

原位生成TiB2/ZA27复合材料的制备与性能

以Al熔液为载体,采用原位反应生成形状规则、尺寸细小的TiB₂颗粒相,再将TiB₂颗粒传递到ZA27合金中,形成TiB₂颗粒增强的ZA27复合材料。采用合理的熔炼工艺促进了TiB₂颗粒在基体中的均匀分布。实验结果显示,TiB₂颗粒在ZA27复合材料中,分布均匀,平均直径在3 μm以下。TiB₂颗粒的加入使得复合材料的晶粒明显细化,并随着TiB₂颗粒含量增加,复合材料的抗拉强度、硬度明显提高,2.1%TiB₂/ZA27复合材料与基体合金相比室温抗拉强度提高13%、布氏硬度提高21%,弹性模量也有所提高,在强度、硬度及弹性模量提高的同时,材料的塑性并未恶化,延伸率略有提高,另外,材料的热膨胀系数随着TiB₂颗粒的加入有所降低。     

Mo5Si3-MoSi2/SiC复合涂层的高温抗氧化行为分析

采用化学气相反应法和料浆刷涂反应法,在石墨表面制备了Mo₅Si₃-MoSi₂/SiC复合涂层,借助X射线衍射仪、扫描电镜及能谱等分析手段,研究了涂层的结构;通过恒温抗氧化实验及热力学分析,重点研究了涂层的高温抗氧化行为。结果表明：在1823 K的氧化氛围中,复合涂层中的Mo₅Si₃、MoSi₂组元易氧化生成MoO₃气体并导致涂层失重;而氧化初期(0～6 h)涂层试样的增重则主要与SiC的惰性氧化主导有关。由于复合涂层各组元在高温下都能氧化生成SiO₂玻璃,使涂层具有良好的高温抗氧化及热震性能;经20 h、16次循环热震实验后,涂层试样的氧化失重率只有3.78%。     

共沉淀法合成近零膨胀ZrW2O8/ZrO2复合陶瓷的致密化

采用化学共沉淀法合成前驱体,经1150℃ 烧结3.5 h得到近零膨胀26 wt% ZrW₂O₈/ZrO₂复合陶瓷,并利用X射线衍射仪、扫描电镜和热膨胀仪研究了原料中加入Al(NO₃)₃·9H₂O对26 wt% ZrW₂O₈/ZrO₂复合陶瓷的相组成、致密度和热膨胀性能的影响。研究结果表明,少量添加Al(NO₃)₃·9H₂O可有效提高复合材料致密度,所得复合陶瓷的组分仍为立方结构的α-ZrW₂O₈和单斜的m-ZrO₂,其中添加2.21 wt% Al(NO₃)₃·9H₂O的复合材料的致密度达到理论密度的98.67%,且对复合陶瓷的热膨胀性能影响不大。其促进致密化机制为晶界处低熔点液相物质Al₂(WO₄)₃提高了复合材料的烧结性能,消除气孔促进致密化。     

用K2ZrF6溶液处理碳化硅涂层碳纤维制造碳/铝复合丝

在碳纤维表面用CVD法涂覆碳化硅涂层,接着用K₂ZrF₆溶液处理,干燥后通过700℃的熔融铝制得碳/铝复合丝。复合丝的强度约为复合准则强度的70%。当碳纤维的体积分数为54%时,复合丝的强度达到1200MPa。用扫描电镜观察复合丝的断口发现界面结合状态良好。用X射线衍射分析了碳化硅-K₂ZrF₆一铝在高温下的反应情况,表明K₂ZrF₆的良好的改善润湿的作用是由于它与铝和碳化硅之间发生了强烈的化学反应。     

不同粒径PANI/SiO2对环氧涂层防腐性能的影响

采用原位聚合,在不同粒径的SiO2表面包覆了聚苯胺(PANl),以制备PANl/SiO2颗粒.包覆后的SiO2颗粒由白色变为墨绿色,红外光谱的研究表明,PANl已经包覆到SiO2颗粒表面.采用热重研究PANl的包覆率,结果表明包覆率随着SiO2粒径的减小而增加,1250目SiO2颗粒PANl的包覆率达到1.76％(质量分数,下同).将PANl/SiO2颗粒添加到环氧树脂涂层中制备防腐涂层,研究发现,SiO2的粒径对涂层的力学性能和防腐性能有至关重要的影响.随添加颗粒粒径的增加,涂层的附着力、耐冲击性以及耐磨性会进一步增加,而涂层硬度减小.添加400目PANl/SiO2颗粒所制备的环氧涂层,结构致密,将其浸泡在3.5％NaCl水溶液中30 d,涂层依然能够发挥很好的防腐作用.     

纳米SiO2-氧化石墨烯/环氧涂层的制备及其防腐蚀性能

采用改进Hummers法制备了氧化石墨烯（GO）,并将GO与经硅烷偶联剂γ-氨丙基三乙氧基硅烷（KH550）改性的纳米SiO₂进行复合,制备出纳米SiO₂-GO。通过FTIR、XRD、SEM、TEM等分析手段对SiO₂-GO进行表征。采用机械搅拌与超声分散的方法将SiO₂-GO添加到环氧树脂（EP）中。对添加不同质量分数纳米SiO₂、GO和纳米SiO₂-GO的EP基复合材料涂层的物理性能和电化学性能进行测试。结果表明,与纯EP涂层相比,SiO₂/EP、GO/EP和纳米SiO₂-GO/EP复合材料涂层的硬度、附着力和耐腐蚀性能得到显著增强,其中加入2wt%纳米SiO₂-GO/EP复合材料涂层硬度达到5 H,附着力等级达到1级,浸泡24 h后涂层保护效率为99.33%。15天浸泡试验结果表明,添加1.5wt%纳米SiO₂-GO/EP复合材料涂层的硬度达到5 H,附着力达到1级,涂层保护效率仍能达到97.12%。     

碳纤维/TiO2改性树脂复合材料的制备及力学性能

针对环氧树脂脆性大、与碳纤维形成的界面性能较差等问题,本文选用纳米TiO₂对5284环氧树脂进行改性,并以角联锁机织物为增强体制备了碳纤维/环氧树脂复合材料。使用FT-IR、旋转流变仪、表面张力仪等设备对TiO₂/环氧树脂进行表征,并研究了树脂改性对复合材料压缩与层间剪切性能的影响。研究表明：TiO₂的羟基与环氧树脂的环氧基和羟基发生了反应;经1wt.%TiO₂改性的树脂复数黏度为0.066 Pa·s,纤维与树脂间接触角为28.85°,浸润效果较好;相较于未改性复合材料,树脂改性的复合材料纵向压缩强度与模量分别提高了7.46%和11.03%,横向压缩强度与模量分别提高了6.99%和4.96%,纵向、横向的剪切强度分别提高了6.88%和4.65%。TiO₂改性环氧树脂提高了复合材料的承载能力,改善了界面结合强度。     

Hydrothermal synthesis and characterization of MoS2 nanorods

MoS₂ nanorods were successfully synthesized via hydrothermal method by adding sillicontungstic acid as an additive. The products were characterized by X-ray powder diffraction (XRD), X-ray photoelectron spectrum (XPS) and field-emission scanning electron microscopy (FESEM). XRD pattern result indicated that the as-prepared sample can be indexed to a mixture of hexagonal and rhombohedral phase MoS₂. XPS showed that the nanorods were only composed of Mo and S with atomic ratio of 1:2. FESEM images revealed that the MoS₂ rods had uniform sizes with mean diameters of about 20-50 nm and lengths of 400-500 nm. It was found that the addition of sillicontungstic acid played a crucial role in the formation of the rod-like MoS₂ in our experiment. The possible formation mechanism of MoS₂ nanorods is also discussed.     

Synthesis and characterization of flower-like MoS2 microspheres by a facile hydrothermal route

Flower-like MoS₂ microspheres with high purity were successfully synthesized via a facile hydrothermal route by adding sodium silicate as an additive. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). XRD patterns showed that the MoS₂ microspheres had good crystallinity with well-stacked layered structure. TEM and SEM images showed that the MoS₂ microspheres had uniform sizes with mean diameter about 480 nm and were constructed with MoS₂ sheets with thickness of several nanometers. It was found that the possible precursor H₄SiMo₁₂O₄₀ obtained by sodium silicate reacting with sodium molybdate played a crucial role in the formation of the flower-like MoS₂ microspheres in our experiment. A possible formation mechanism of MoS₂ microspheres was preliminarily presented.     

An investigation of super-hydrophilic properties of TiO2/SnO2 nano composite thin films

A sol-gel dip coating technique was used to fabricate TiO₂/SnO₂ nano composite thin films on soda-lime glass. The solutions of SnO₂ and TiO₂ were mixed with different molar ratios of SnO₂:TiO₂ as 0, 3, 4, 6, 8, 9, 10.5, 13, 15, 19.5, 25 and 28 mol.% then the films were prepared by dip coating of the glasses. The effects of SnO₂ concentration, number of coating cycles and annealing temperature on the hydrophilicity of films were studied using contact angle measurement. The films were characterized by means of scanning electron microscopy, X-ray diffraction and atomic force microscopy measurements. The nano composite thin films fabricated with 8 mol.% of SnO₂, four dip coating cycles and annealing temperature of 500 °C showed super-hydrophilicity.     

聚苯胺/TiO2复合纳米膜电极的制备及其光电性能

采用原位化学氧化法,在酸性TiO2溶胶中未加分散剂制备了聚苯胺修饰的TiO2稳定溶胶,并以涂刮法在柔性导电塑料薄膜上成膜。利用FT-IR、XRD、TEM、选区电子衍射、紫外-可见光谱、光电流-电压曲线对所制备的复合溶胶及复合膜进行了表征。结果表明TiO2与聚苯胺之间实现了结构上的复合,聚苯胺的引入改善了TiO2膜对太阳光的利用率,提高了TiO2膜的光电响应性能。这种用复合溶胶制备聚苯胺/TiO2复合膜的方式扩大了成膜基底的范围。     

Synthesis of inorganic fullerene-like MoS2 nanoparticles by a facile method

A facile and low-cost synthesis route was used to synthesize inorganic fullerene-like (IF) MoS₂ nanoparticles by reaction of sulfur powder and ammonium molybdate in a hydrogen atmosphere at 600 °C. As-synthesized IF-MoS₂ nanoparticles are of a closed hollow cage structure with size of 10-20 nm. Nanowires and nanotubes were also obtained at the same annealing temperature. The composition, structure, and morphology of the products were characterized by XRD, Raman, and TEM and the possible growth mechanism is proposed.     

Tribological behaviour of MoS2/Au coatings

This study aims to enhance the endurance of MoS₂ coating by applying a thin layer of Au (∼ 80 nm) on MoS₂ surface. Experimental results show that the addition of Au film increases the endurance of MoS₂/Au over equivalent coatings without Au. The friction coefficient rapidly decreases to a stable value (μ ∼ 0.045) after about 100 cycles sliding. After more than 15,000 cycles, the friction coefficient gradually increased to a second stable value (μ ∼ 0.15). An average endurance of over 50,000 cycles was measured in this case. The Au or Au-MoS₂ composite layer can effectively prevent oxygen or moisture reaction with MoS₂ and hence significantly increases the wear life.     

Thermal stability of sputtered Mo/polyimide films and formation of MoSe2 and MoS2 layers for application in flexible Cu(In,Ga)(Se,S)2 based solar cells

Molybdenum (Mo) films with a thickness of about 800 nm were room temperature sputtered onto flexible polymeric substrates. Upilex® films were chosen as substrates on the basis of their high thermal endurance and reduced coefficient of thermal expansion. Thermal stability of Mo films has been proved by heat treatment of the Mo/Upilex® structures at a temperature comparable to that used in the preparation of the Cu(In,Ga)(Se,S)₂ absorber layer. A combination of high optical reflectance (maximum values of 75-80%), low electrical resistivity (about 30 μΩ cm) and a smooth surface free of cracks for heated films highlights their good thermal stability. The formation of MoSe₂ and MoS₂ layers, after selenization/sulfurization of the Mo/Upilex® structures, has been further investigated in view of their application as back contact layers in flexible CIGS based solar cells.     

二硫化钼花状微球的水热合成及其微观结构表征

以钼酸铵作为钼源,硫脲作为硫源和还原剂,采用简便的水热法合成二硫化钼花状微球。采用X射线衍射仪、拉曼光谱仪、扫描电子显微镜和透射电子显微镜对二硫化钼样品的形貌和结构进行表征。考察了钼硫比、反应时间、反应温度对二硫化钼花状微球形貌和结构的影响。结果表明,当钼硫物质的量比为1∶2.25,反应温度为220℃,反应时间为18h时合成了结晶性好的纳米片(厚度为10nm)组装而成的二硫化钼花状微球,其具有较大的比表面积,是一种性能优异的锂离子电池电极材料。