WSe2纳米结构的合成及减摩性能研究

将W粉和Se粉按一定比例混合,直接密封在石英管中加热或高能球磨、压片,在Ar气氛中加热,得到了不同形貌的WSe2纳米结构.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM、HRTEM)分析了WSe2纳米结构的组成、微观形貌和组织形态;利用UMT-2摩擦试验机考察了WSe2作为HVI500液体基础油添加剂的摩擦磨损性能.研究结果表明:直接密封加热得到的产物为棒状WSe2纳米材料,最小棒直径为6 nm;球磨、压片后加热得到WSe2纳米颗粒,颗粒的平均尺寸在50 nm以下,二者都具有层状结构和良好的结晶性.添加质量分数5%的WSe2纳米材料作为基础油添加剂能够显著降低摩擦系数,减少磨损,增强了材料抗疲劳磨损能力.     

纳米二硫化钼作为机械油添加剂的摩擦学特性研究

由硫化钠和钼酸钠水溶液反应生成棕色三硫化钼膏状沉淀,将三硫化钼粉末干燥后在氢气保护气氛中于适宜温度下煅烧脱硫,制得了粒径为20～30nm的纳米MoS2颗粒.用X射线衍射仪和透射电子显微镜分析了MoS2纳米颗粒的相组成和微观形貌;利用四球摩擦磨损试验机测定了纳米MoS2作为N46机械油添加剂的摩擦学性能;采用X射线光电子能谱仪分析了磨痕表面元素的化学状态,用扫描电子显微镜观察了磨痕表面形貌,探讨了纳米MoS2的减摩抗磨机理.结果表明,同普通MoS2微粒相比,纳米MoS2更易发生化学反应并在钢球磨损表面形成含三氧化钼的表面膜,纳米MoS2添加剂的极压、抗磨和减摩性能优于普通MoS2.     

纳米铜润滑油添加剂的摩擦磨损特性及其机理研究

设计了4种试验方案,对比研究了不同摩擦试验条件下粒径为20 nm的铜添加剂对摩擦副的修复作用,考察了纳米铜添加剂在不同润滑油中的抗磨减摩性能,探讨了纳米铜添加剂的作用机理.结果表明:在摩擦过程中,纳米铜添加剂能够在磨损表面形成由粒径为0.1 μm团状物构成、低剪切强度的保护软膜,可以减小粘着磨损和磨粒磨损,使纳米铜添加剂表现出良好的抗磨减摩性能;对于基础润滑油650SN,纳米铜添加剂能够使其摩擦系数降低48%、磨痕宽度降低21%;对于坦克机油50CC,纳米铜添加剂能够使其摩擦系数降低40%、磨痕宽度降低33%;同时,铜保护膜修复了磨损表面的微坑和损伤,对摩擦副起到了有效的保护和修复作用.     

纳米碳酸钙作为润滑脂添加剂的摩擦学性能及流变行为研究

使用碳化法制备出三种具有不同粒径的纳米碳酸钙颗粒,利用透射电镜(TEM)和X射线衍射仪(XRD)对其形貌及结构组成进行表征.通过UMT-2摩擦学试验机及RS6000流变仪分别考察了纳米颗粒作为润滑脂添加剂的摩擦学性能及流变学行为,并通过X射线多功能电子能谱仪(XPS)对磨斑表面进行分析.结果表明:所制备的三种纳米颗粒均为方解石结构,可以显著提高基础脂的减摩抗磨性能;添加剂浓度及添加剂尺寸均会影响润滑脂最终的摩擦学性能;在最佳添加浓度和尺寸条件下,能够同时获得最佳的抗磨减摩性能;过高的添加剂浓度会影响润滑脂的结构稳定性,进而影响其摩擦学性能;三种纳米添加剂在磨斑表面形成以碳酸钙为主要成分的润滑膜,纳米颗粒物理性质的差异可能导致其摩擦学性能的差异.     

Bi-Pb-Sn-Cd四元合金纳米微粒的制备及其摩擦磨损性能研究

通过直接对Bi-Pb-Sn-Cd四元块状合金进行超声分散制备了相应的四元合金纳米微粒;采用X射线衍射仪和热分析仪分析所制备的纳米微粒结构;采用透射电子显微镜考察了纳米颗粒的形貌及尺寸分布;采用四球摩擦磨损试验机考察了纳米颗粒的摩擦学性能.结果表明,所制备的纳米颗粒为低熔点共晶合金纳米微粒,颗粒平均尺寸在10～20 nm之间,其作为润滑油添加剂表现出良好的摩擦学性能.     

片状纳米石墨的制备及其作为润滑油添加剂的摩擦磨损性能

采用搅拌球磨法制备了平均直径1 μm、厚度10～20 nm的片状纳米石墨;利用扫描电子显微镜、透射电子显微镜和X射线衍射仪分析了片状纳米石墨的微观形貌和组织结构;利用四球和销-盘式摩擦磨损试验机考察了片状纳米石墨作为液体石蜡添加剂的摩擦磨损性能.结果表明,片状纳米石墨能够显著提高润滑油的抗磨性能及承载能力,降低摩擦系数,其最佳添加量约为50 ppm.     

铋纳米微粒添加剂的摩擦学性能研究

采用液相分散法制备了平均粒径为60 nm的油溶性铋纳米微粒,用四球摩擦磨损试验机考察了所制备的铋纳米微粒作为润滑油添加剂的减摩抗磨性能.结果表明,当添加量处于0.04%～1.00%范围内时,铋纳米微粒表现出良好的减摩抗磨性能,并能显著提高基础油的失效负荷.     

水基纳米液压液抗磨减摩性能研究

制备了分散性稳定的水基纳米液压液,并利用四球摩擦试验机和抗磨试验机,对不同质量百分数、不同粒径二氧化硅纳米颗粒的水基纳米液压液进行抗磨减摩性能试验.结果表明:二氧化硅纳米颗粒可以明显改善水基液压液的抗磨减摩性能;对于30 nm粒径的二氧化硅颗粒,质量百分数为2.4%时水基纳米液压液的摩擦系数、磨斑直径、温升及磨损量均最低,抗磨减摩性能达到最佳;采用不同粒径纳米颗粒时,随着纳米颗粒质量百分数增大,磨损量先降后升,纳米颗粒粒径越大,对应的最佳质量百分数越小.     

油酸修饰纳米氟化钙的萃取法制备及其摩擦学性能

采用萃取法制备了油酸修饰的纳米CaF2,用X射线衍射(XRD)对纳米CaF2粉体样品进行物相分析,同时用透射电子显微镜(TEM)及傅立叶变换红外光谱仪(FT-IR)进行表面形貌和成分分析,并在四球摩擦磨损试验机上评价了CaF2在润滑脂中的摩擦学性能.结果表明,制备的纳米CaF2粒径在23 nm左右,油酸以化学吸附的方式吸附在CaF2纳米核表面;作为添加剂油酸修饰纳米CaF2在润滑脂中具有良好的抗磨性能和极压性能,在高载荷时具有良好的减摩性能.SEM,EDS和XPS分析表明在摩擦过程中形成了由CaF2、CaO、氧化铁和有机添加剂所组成的边界润滑膜,从而使OA-CaF2具有良好的摩擦学性能.     

季铵盐修饰磷钼酸铵纳米微粒作为液体石蜡添加剂的摩擦学性能

采用共沉淀法在溶液中原位合成了季铵盐修饰磷钼酸铵[(NH4)3PMo12O40]纳米微粒,采用透射电子显微镜、X射线衍射仪、示差扫描热分析仪及热重分析仪等观察分析了表面修饰(NH4)3PMo12O40纳米微粒的形貌和热稳定性,并在四球摩擦磨损试验机上考察了其作为液体石蜡添加剂的摩擦学性能。结果表明：表面修饰(NH4)3PMo12O40纳米微粒大小均匀,平均粒径约为20nm;(NH4)3PMo12O40纳米核在300℃左右分解;(NH4)3PMo12O40。纳米微粒作为液体石蜡添加剂,在中低负荷下具有较好的抗磨性和一定的减摩作用,并可提高液体石蜡的极压负荷,采用扫描电子显微镜和X射线光电子能谱对磨斑表面形貌和化学组成进行观察分析发现,(NH4)3PMo12O40纳米微粒在摩擦副接触表面发生了摩擦化学作用,并形成由多种含氧化合物组成的表面保护膜,从而起到减摩抗磨作用。     

In situ investigation of the mechanical properties of nanomaterials by transmission electron microscopy

With the progress of modern transmission electron microscopy (TEM) and development of dedicated functional TEM specimen holders, people can now manipulate a nano-object with nanometer-range precision and simultaneously acquire mechanical data together with atomic-scale structural information. This advanced methodology is playing an increasingly important role in nanomechanics. The present review summarizes relevant studies on the in situ investigation of mechanical properties of various nanomaterials over the past decades. These works enrich our knowledge not only on nanomaterials (such as carbon nanotubes, carbon onions, boron nitride nanotubes, silicon nanowires and graphene, etc.) but also on mechanics at the nanoscale.     

Statistical morphological identification of low-dimensional nanomaterials by using TEM

Nanomaterials with low-dimensional morphology display unique properties in catalysis and related fields, which are highly dependent on the structure and aspect ratio. Thus, accurate identification of the structure and morphology is the basis to correlate to the performance. However, the widely adopted techniques such as XRD is incapable to precise identify the aspect ratio of low-dimensional nanomaterials, not even to quantify the morphological uniformity with statistical deviation value. Herein, ZnO nanorod and nanosheet featured with one- and two-dimensional morphology were selected as model materials, which were prepared by the hydrothermal method and statistically characterized by transmission electron microscopy (TEM). The results indicate that ZnO nanorods and nanosheets display rod-like and orthohexagnal morphology, which mainly encapsulated with {100} and {001} planes, respectively. The 7.36 ± 0.20 and 0.39 ± 0.02 aspect ratio (c/a) of ZnO nanorods and nanosheets could be obtained through the integration of the (100) and (002) diffraction rings in selected area electron diffraction (SAED). TEM combining with the SAED is favorable compare with XRD, which not only provides more accurate aspect ratio results with standard deviation values but also requires very small amounts of sample. This work is supposed to provide a convenient and accurate method for the characterization of nanomaterials with low-dimensional morphology through TEM.     

Characterization of gold]PMMA hybrid nanomaterials synthesized by hard X-ray synchrotron radiation

In this study, new types of hybrid gold poly（methyl methacrylate） （PMMA） nanomaterials are synthesized. Both PMMA spheres coated with gold nanoparticles and gold nanoparticles coated with PMMA can be synthesized using different ratios of HAuCl4 and MMA precursors, by exposing the mixtures to hard X-ray synchrotron radiation without the use of a reducing agent. According to the photochemical mechanism, gold nanoparticles will precipitate from a solution of HAuCl4 on exposure to synchrotron radiation, followed by the synthesis of PMMA by the polymerization of MMA monomers. These reactions can result in the formation of two different types of new hybrid nanomaterials. When a 1：1 volume ratio of HAuCI4 to MMA is used, we obtain PMMA spheres coated with gold nanoparticles. When a 10：1 ratio of HAuCl4 and MMA is used, we obtain gold nanoparticles coated with PMMA. The hybrid gold/PMMA nanostructures are characterized by transmission electron microscopy, elemental analysis, dynamic-light scattering analysis, gel permeation chromatography and Raman spectroscopy. The hybrid nanomaterials have potential application in the fields of biosensors and drug delivery.     

NbSe2/Ag纳米复合材料的制备及其作为煤矿机械机用润滑油添加剂摩擦学行为的研究

采用化学还原法成功制备出NbSe₂/Ag纳米复合材料,即在NbSe₂纳米片表面沉积1层纳米Ag颗粒. 采用UMT-2摩擦磨损试验机以及扫描电子显微镜(SEM)研究了NbSe₂/Ag纳米复合材料添加到煤矿机械机用润滑油中的摩擦学行为. 结果表明:相比于纳米Ag颗粒和NbSe₂,NbSe₂/Ag纳米复合材料添加到润滑油中更加有效地改善了润滑油的润滑承载效果. NbSe₂/Ag纳米复合材料所表现出最优良的摩擦学行为. 原因主要可能在于4个方面:第一,根据理论计算得出NbSe₂、Ag和NbSe₂/Ag纳米复合材料产生滑移的最大抗剪切强度按从小到大顺序排列为NbSe₂/Ag纳米复合材料、Ag、NbSe₂。NbSe₂/Ag纳米复合材料抗剪切强度最小,润滑效果最好;第二,NbSe₂/Ag纳米复合材料中的NbSe₂由于纳米Ag负载相比于纯NbSe₂具有更好的分散性,更利于形成完整均匀的润滑膜;第三,Ag质软润滑且弹性模量小,NbSe₂/Ag纳米复合材料受到摩擦热以及剪切作用形成的润滑膜由于Ag的存在提高了脆性破坏能力,使得润滑膜在摩擦副上硬凸点的刮擦作用下不易破裂;第四,部分纳米Ag球状颗粒可能存在接触界面上有效的滚动,起到“微轴承”的作用从而降低摩擦系数. 然而,润滑油的润滑效果与所添加的NbSe₂/Ag纳米复合材料含量并非呈现正相关关系,而是随着添加含量的增加呈现先降低后增加的趋势,在质量分数为1.5%时,效果最佳.      

Characterization of gold/PMMA hybrid nanomaterials synthesized by hard X-ray synchrotron radiation

In this study,new types of hybrid gold poly(methyl methacrylate) (PMMA) nanomaterials are synthesized.Both PMMA spheres coated with gold nanoparticles and gold nanoparticles coated with PMMA can be synthesized using different ratios of HAuCl4 and MMA precursors,by exposing the mixtures to hard X-ray synchrotron radiation without the use of a reducing agent.According to the photochemical mechanism,gold nanoparticles will precipitate from a solution of HAuCl4 on exposure to synchrotron radiation,followed by the synthesis of PMMA by the polymerization of MMA monomers.These reactions can result in the formation of two different types of new hybrid nanomaterials.When a 1:1 volume ratio of HAuCl4 to MMA is used,we obtain PMMA spheres coated with gold nanoparticles.When a 10:1 ratio of HAuCl4 and MMA is used,we obtain gold nanoparticles coated with PMMA.The hybrid gold/PMMA nanostructures are characterized by transmission electron microscopy,elemental analysis,dynamic-light scattering analysis,gel permeation chromatography and Raman spectroscopy.The hybrid nanomateriais have potential application in the fields of biosensors and drug delivery.     

类石墨烯二硫化钼的制备及其真空摩擦学性能研究

采用电化学剥离法制备了类石墨烯二硫化钼(MoS_2)片层,采用场发射扫描电子显微镜、透射电子显微镜表征了类石墨烯二硫化钼的结构.利用真空摩擦试验机测试了含类石墨烯MoS_2添加剂离子液体(IL-MoS_2)的摩擦学性能并与纯离子液体(IL)进行了对比.利用光学显微镜和扫描电子显微镜观察磨斑处的形貌并用X射线光电子能谱仪表征了IL-MoS_2摩擦前后的化学状态,并对润滑机理进行了分析.结果表明:电化学剥离法成功制备了类石墨烯MoS_2,这种制备方法简单易行,制得的类石墨烯MoS_2面积大,质量好,能保持二硫化钼固有的结构.IL-MoS_2对钢/钢摩擦副具有优异的减摩抗磨作用;摩擦过程中,纳米尺寸的二硫化钼吸附在钢/钢摩擦副界面形成了保护层,避免摩擦副的直接接触,降低摩擦磨损.     

In situ synthesis of Ag-SiO_2 Janus particles with epoxy functionality for textile applications

A facile method for the synthesis of silver-silica(Ag-SiO_2) Janus particles with functionalities suitable for textile applications is reported.Silica nanoparticles prepared by the Stober method were functionalized with epoxy,amine,and thiol groups,which were confirmed by Fourier transform infrared analysis.The functionalized silica nanoparticles were used to produce Pickering emulsions,and the exposed surface was used for the attachment of silver nanoparticles(AgNPs) via the low-temperature chemical reduction method.The morphology and structure of the Ag-SiO_2 Janus particles were characterized by scanning electron microscopy,scanning transmission electron microscopy,high-resolution transmission electron microscopy,energy-dispersive X-ray analysis,and UV-vis spectroscopy.Because of their specific functionalities,these Ag-SiO_2 Janus particles are proposed for applications on textile substrates,as they can overcome several drawbacks of direct application of AgNPs on textiles,such as leaching,agglomeration,and instability during storage.     

纳米复合材料激光熔覆层组织及抗磨性能

利用5kWCO2激光器，在Ni基高温合金表面制备了纳米Al2O3／钴基合金熔覆层，分析了熔覆层的组织结构及其抗磨性能．结果表明，当纳米Al2O3颗粒含量较低时，Al2O3颗粒能均匀分布于熔覆层中，从而形成纳米氧化物弥散强化的复合材料涂层；Al2O3颗粒在熔池中长大，尺寸为250-450nm；复合材料熔覆层的硬度随纳米Al2O3含量的增加而提高；当纳米Al2O3颗粒含适中时，熔覆层的抗磨性能较好；而当纳米Al2O3颗粒含量过高(3．0％)时，复合材料熔覆层的抗磨性能反而降低。     

水分散性纳米级二硫化钼的制备及其摩擦学性能评价

采用乙二醇作为还原剂和溶剂,以自制的四硫代钼酸铵（ATTM）为原料制备了水分散性纳米级二硫化钼;采用X射线粉末衍射仪(XRD)、透射电子显微镜(TEM)及X射线光电子能谱仪（XPS）表征了产物的结构;采用四球摩擦磨损试验机测定了其水分散体系的摩擦学性能,同时利用扫描电镜(SEM)和能量色散谱仪(EDS)分析了钢球磨斑表面形貌和元素组成。结果表明:所制备的二硫化钼呈纳米级球形微粒,在水及乙醇中的分散性良好,并能显著改善水的减摩抗磨性能;作为水基添加剂具有很好的摩擦学应用前景。