SiO2/MoS2复合纳米基润滑油在镁合金冷轧中的摩擦学性能及润滑机理

镁合金在轧制过程中通常采用铝合金轧制液,甚至进行无润滑轧制。轧制过程中无润滑油会导致轧后板材表面质量差、能耗高,而铝合金轧制液通常采用含氯、硫、磷等元素的有机化合物作为添加剂,此类添加剂不容易分解,废液的排放会对环境造成一定污染。基于此,本工作采用不同比例的SiO_2和MoS_2纳米颗粒复合加入EOT5#机械油中,在双辊轧机上研究两种纳米颗粒复合比例对AZ31镁合金冷轧过程中轧制力和轧后板材表面质量的影响。采用场发射扫描电镜(FESEM)和X射线光电子能谱仪(XPS)对SiO_2/MoS_2复合纳米基润滑油润滑条件下轧后板材表面形貌和成分进行了分析,探讨了SiO_2/MoS_2复合纳米基润滑油的协同润滑机理。结果表明,SiO_2和MoS_2纳米颗粒在基础油中添加质量分数之比为0.25∶0.75时具有最佳的润滑性能。SiO_2/MoS_2复合纳米基润滑油优良的润滑性能降低了镁合金轧制过程中的轧制力,改善了轧后板材的表面质量。分析认为,不同形貌和润滑机理的SiO_2和MoS_2纳米颗粒共同作用是实现协同润滑的关键因素。     

水热合成的MoS2/石墨烯/N-TiO2复合材料的可见光催化性能

以氧化石墨烯(GO)、钼酸、硫脲和TiN为原料,成功制备了MoS_2/石墨烯/N-TiO_2(MGNT)复合材料。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HR-TEM)、X射线光电子能谱(XPS)及紫外-可见漫反射光谱(UV-Vis DRS)等手段测试分析了样品的物相组成、形貌、成分和光吸收性能。紫外-可见漫反射测试结果表明,MoS_2、石墨烯共同修饰及氮掺杂使得TiO_2的吸收带边发生红移,且其可见光吸收性能明显提高。可见光照射下降解亚甲基蓝溶液的实验结果表明,MoS_2/石墨烯共同修饰的氮掺杂TiO_2的光催化降解性能分别是氮掺杂TiO_2(NT)和石墨烯修饰氮掺杂TiO_2(GNT)的1.82倍和1.59倍,其吸附性分别为氮掺杂TiO_2、石墨烯修饰氮掺杂TiO_2的11.14倍和4.77倍。     

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.     

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。     

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.     

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.     

氧和硒掺杂对单层二硫化钼电子结构与光电性质的影响

基于密度泛函理论的第一性原理计算,研究了氧和硒掺杂对单层二硫化钼电子结构与光电性质的影响.结果表明,单层二硫化钼属于直接带隙半导体,其带隙宽度为1.64 eV.单层二硫化钼的价带顶主要由S-3p态电子和Mo-4d态电子构成,而其导带底则主要由Mo-4d态电子和S-3p态电子共同决定;同时通过氧和硒掺杂,使单层二硫化钼的禁带宽度变窄,光吸收特性增强,研究结果为二硫化钼在光电器件方面的应用提供了理论基础.     

A study of textured non-stoichiometric MoTe2 thin films used as substrates for textured stoichiometric MoS2 thin films

Textured MoTe₂ films have been prepared by sequential evaporation of the constituents followed by annealing under a tellurium pressure. The films are systematically textured with the c-axis of the crystallites perpendicular to the plane of substrate, however, the film composition is difficult to control and even after process optimization the films are tellurium deficient. This is thought to be caused by the electro negativity difference of the constituents.The textured MoTe₂ films have been used as substrates on which to grow MoS₂ films by annealing under a pressure of sulfur that allows textured MoS₂ films to be grown with good crystalline properties. The presence of sulfur at the surface and annealing under dynamic vacuum is important for this process and moreover, suppresses the superficial oxidation of the Mo and Te constituents.     

Ionic liquid assisted hydrothermal synthesis of hollow vesicle-like MoS2 microspheres

The preparation of MoS₂ microspheres with hollow vesicle-like structure was successfully achieved, which used hydrazine solution with (NH₄)₂MoS₄ as the precursor. The reaction process was assisted by a convenient ionic liquid (1-butyl-3-methylimidazolium chloride) with the hydrothermal method at 200 °C for 24 h. X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) techniques were used to characterize the samples. It was shown that the MoS₂ microspheres had uniform spherical morphology with the diameter of 1-2 μm. It was also indicated that the hollow vesicle monomers on the surface of microspheres were structured with multi-layer of MoS₂, whose d spacing was 1.0 nm. A tentative formation mechanism was proposed for the growth process of the MoS₂ microspheres with hollow vesicle-like structure.     

Effects of MoS2 doping on the electrochemical performance of FeF3 cathode materials for lithium-ion batteries

Orthorhombic structure FeF₃ was synthesized by a liquid-phase method. The FeF₃/MoS₂ for the application of cathode material of lithium-ion battery was prepared through mechanical milling with molybdenum bisulfide. The structure and morphology of the FeF₃/MoS₂ were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The electrochemical behavior of FeF₃/MoS₂ was studied by charge/discharge, cyclic voltammetry and electrochemical impedance spectra measurements. The results show that the prepared FeF₃/MoS₂ was typical orthorhombic structure, uniform surface morphology, better particle-size distribution and excellent electrochemical performances. The initial discharge capacity of FeF₃/MoS₂ was 169.6 mAh·g^− 1 in the voltage range of 2.0-4.5 V, at room temperature and 0.1 C charge-discharge rate. After 30 cycles, the capacity retention is still 83.1%.     

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.     

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。     

Effect of Ti or TiN codeposition on the performance of MoS2-based composite coatings

Properties of MoS₂ coatings can be improved by the codeposition of a small amount of titanium (Ti). In this study, MoS₂-based composite coatings, which consisted of Ti or titanium nitride (TiN) and molybdenum disulfide, are synthesized by unbalanced plasma plating. Two forms of MoS₂-based composite coatings have been developed: TiN-MoS₂/Ti and TiN-MoS₂/TiN coatings. The effect of Ti or TiN and processing parameters on properties of such coatings are investigated. Scanning electron microscopy (SEM), dry drilling and turning tests are used to determine the structure, composition and tribological performance of MoS₂-based coatings. Experimental results indicate that these MoS₂-based composite coatings are considerably more wear-resistant and are less sensitive to atmospheric water vapor than pure MoS₂ coatings. These coatings show excellent results when tested for a wide range of industrial turning and drilling applications.     

二维纳米片层结构MoS2和其改性材料的合成及在环境领域的应用

类石墨烯的二维纳米片层状MoS_2作为过渡金属硫化物材料家族的典型代表,由于其各方面独特的性能尤其是超薄的厚度和二维结构,已成为近些年材料的研究热点。独特的三明治结构使其具有良好的物理化学性质,MoS_2及其复合材料在催化、传感器、润滑等方面有广阔的前景。总结了国内外MoS_2的合成及其改性方法、性能和应用。针对社会发展过程中日益严重的环境污染问题,重点介绍利用其吸附和催化性能去除环境中污染物,并对其未来发展进行了展望。     

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。     

Synthesis of MoS2/C nanocomposites by hydrothermal route used as Li-ion intercalation electrode materials

MoS₂/C nanocomposites were synthesized by a facile hydrothermal route employing sulfocarbamide, sodium molybdate and D-grouse as starting materials. XRD analysis showed that the MoS₂ was a two-dimensional nanosheet crystal and C was retained as amorphous after their calcinations at 800 °C. TEM images showed that MoS₂ was uniformly dispersed in the amorphous carbon. The MoS₂/C composites exhibited high reversible capacity and excellent cyclic performance when used as Li-intercalation electrodes. The improvements in electrochemical performance are attributed to the incorporation of amorphous carbon, which can suppress the aggregation and pulverization of active materials, and keep the active materials electrically connected.     

原位聚合法制备聚苯胺改性MoS2及其环氧复合涂层的防腐性能

为提高环氧涂料的防腐性能,本文引入MoS₂纳米片作为阻隔剂,并在MoS₂纳米片表面原位聚合聚苯胺(PANI),制备了夹层结构i-PANI@MoS₂纳米片,利用PANI提高涂层的导电性,达到阳极钝化的效果。研究发现,当PANI与MoS₂的摩尔配比增大到7∶1时,MoS₂片层表面被PANI均匀覆盖,改性效果最好。与环氧树脂复合后,i-PANI@MoS₂-7纳米片在环氧树脂中均匀分散,复合涂层导电率提高,PANI与MoS₂起到了协同防腐作用,此时i-PANI@MoS₂纳米片既作为涂层中的阻隔剂,又作为电化学腐蚀保护剂,因此复合涂层具有最大的阻抗值、最大腐蚀电压以及最小的腐蚀电流密度,防腐性能优异。但PANI与MoS₂配比进一步增大,MoS₂纳米片表面的聚苯胺会发生团聚,导致复合涂层的防腐性能下降。     

Formation of alkali resistant PDMS-TiO2-SiO2 hybrid coatings

PDMS-TiO₂-SiO₂ hybrid coatings have been prepared on glass substrates via sol-gel method. The structural evolution of the coatings containing different PDMS amounts was examined by TG-DTA and FTIR. It was found that the hybrid character of coatings can be reserved after heating at 200 °C. The alkali resistance of hybrid coatings in 1 N NaOH solution at 50 °C was investigated by X-ray fluorescence analysis, weight loss and scanning electron microscopy. The results showed that the coating could resist effectively the alkali attack for 24 h. Such alkali resistance depended on the added amount of PDMS and the coating with 20 wt.% PDMS showed a better alkali resistance.     

Fabrication of TiO2/Au nanorod arrays employing a positive sacrificial ZnO template and their electrochromic property

A novel method to fabricate large scale TiO₂/Au nanorod array using a positive sacrificial ZnO template has been developed. This method includes a two-step process, (1) preparation of ZnO/Au nanorod array by a simple low-temperature hydrothermal process, and (2) preparation of TiO₂/Au nanorod array by electrochemically induced sol-gel process. The TiO₂/Au nanorod array has showed a reversible electrochromism in lithium-ion-containing organic electrolyte. The coloration and bleaching throughout a visible range can be switched on and off within a few seconds.     

三维花状MoS2锌离子电池正极材料的设计构筑及其储能机制研究

采用水热法设计构筑三维花状二硫化钼,并利用XRD、SEM、RAMAN、TG等测试方法对产物的结构和形貌进行了表征,进而作为正极材料组装成锌离子电池并对其进行电化学测试分析,在充放电电压区间为0.2~1.2V、电流密度为1.0A/g条件下,首次放电比容量可达63.9 mAh/g,100次循环后其放电比容量保持在53.6mAh/g,容量保持率为83.9%。较高的比容量和循环稳定性使MoS_2成为有前景的锌离子电池正极材料之一。