Anti-wear and Friction Reducing Mechanisms of Carbon Nano-onions as Lubricant Additives

Carbon nano-onions have better tribological properties than graphite powder when used as additives dispersed in a poly-alpha-olefin base oil. Carbon nano-onions give a better dispersion in the liquid base oil due to their nanometre-scale size. In particular, the anti-wear efficiency of carbon onions under boundary lubrication and mild wear regime is much better than that of graphite powder. This effect can be attributed to the different structure of the carbon layers in the two species. High-resolution transmission electron microscopy and electron energy-loss spectroscopy were used to characterize the carbon samples, and significant differences in the carbon layer spacing and the density were shown. Wear debris were also observed by the same techniques. In the tribofilm material we depicted new chemical and crystal nano-structures species similar to some microstructures observed in chondrite meteorites, the most interesting one being maghemite iron oxide. The origin of the low friction and wear is still largely unknown.     

Extracting physically interpretable data from electron energy-loss spectra

Principal component analysis is routinely applied to analyze data sets in electron energy-loss spectroscopy (EELS). We show how physically meaningful spectra can be obtained from the principal components using a knowledge of the scattering of the probe electron and the geometry of the experiment. This approach is illustrated by application to EELS data for the carbon K edge in graphite obtained using a conventional transmission electron microscope. The effect of scattering of the probe electron is accounted for, yielding spectra which are equivalent to experiments using linearly polarized X-rays. The approach is general and can also be applied to EELS in the context of scanning transmission electron microscopy.     

透射电子显微技术在RIPP炼油催化剂表征中的应用

利用透射电子显微技术对加氢催化剂以及积炭催化裂化催化剂进行了表征。扫描透射电子结合X射线能谱技术确定了氧化态加氢催化剂中的微粒为活性金属组分的适度聚集；能量过滤透射显微技术获得了积炭催化裂化催化剂的Al、C的元素分布像。     

Chromosome observation by scanning electron microscopy using ionic liquid

Electron microscopy has been used to visualize chromosome since it has high resolution and magnification. However, biological samples need to be dehydrated and coated with metal or carbon before observation. Ionic liquid is a class of ionic solvent that possesses advantageous properties of current interest in a variety of interdisciplinary areas of science. By using ionic liquid, biological samples need not be dehydrated or metal-coated, because ionic liquid behaves as the electronically conducting material for electron microscopy. The authors have investigated chromosome using ionic liquid in conjunction with electron microscopy and evaluated the factors that affect chromosome visualization. Experimental conditions used in the previous studies were further optimized. As a result, prewarmed, well-mixed, and low concentration (0.5～1.0%) ionic liquid provides well-contrasted images, especially when the more hydrophilic and the higher purity ionic liquid is used. Image contrast and resolution are enhanced by the combination of ionic liquid and platinum blue staining, the use of an indium tin oxide membrane, osmium tetroxide-coated coverslip, or aluminum foil as substrate, and the adjustment of electron acceleration voltage. The authors conclude that the ionic-liquid method is useful for the visualization of chromosome by scanning electron microscopy without dehydration or metal coating.     

Application of the focused ion beam technique in aerosol science: detailed investigation of selected, airborne particles

The focused ion beam technique was used to fabricate transmission electron microscope lamellas of selected, micrometre‐sized airborne particles. Particles were sampled from ambient air on Nuclepore polycarbonate filters and analysed with an environmental scanning electron microscope. A large number of particles between 0.6 and 10 µm in diameter (projected optical equivalent diameter) were detected and analysed using computer‐controlled scanning electron microscopy. From the resulting dataset, where the chemistry, morphology and position of each individual particle are stored, two particles were selected for a more detailed investigation. For that purpose, the particle‐loaded filter was transferred from the environmental scanning electron microscope to the focused ion beam, where lamellas of the selected particles were fabricated. The definition of a custom coordinate system enabled the relocation of the particles after the transfer. The lamellas were finally analysed with an analytical transmission electron microscope. Internal structure and elemental distribution maps of the interior of the particles provided additional information about the particles, which helped to assign the particles to their sources. The combination of computer‐controlled scanning electron microscopy, focused ion beam and transmission electron microscopy offers new possibilities for characterizing airborne particles in great detail, eventually enabling a detailed source apportionment of specific particles. The particle of interest can be selected from a large dataset (e.g. based on chemistry and/or morphology) and then investigated in more detail in the transmission electron microscope.     

A comparative study of colloidal particles as imaging standards for microscopy

Colloidal particles have long been used as imaging standards for electron microscopy and, more recently, for scanning probe microscopy. We have analysed gold, polystyrene and silica colloidal particles by both transmission electron microscopy and atomic/scanning force microscopy in an attempt to determine if any can be truly used as 'standards' of shape and/or size. From the transmission electron micrographs, we have obtained precise information of the particle circumference and mean diameter. By comparing the ratio of these to the value for π, we obtained a measure of the sphericity of the particles. We have also shadowed the particles with metal at a known angle and have analysed the shadow length to determine the particles' heights and shapes. The height information obtained from the shadow length data collected from the transmission electron micrographs was then compared with that obtained by atomic/scanning force microscopy. Our results show that cleaned (washed) silica or polystyrene particles closely approach true spheres. In the case of gold particles, height data obtained from shadow lengths analysed in transmission electron micrographs show good agreement with that obtained from the atomic/scanning force microscopy images even without washing. However, the gold particles often deviate from sphericity. Based upon both the shape and the physical properties of the colloidal particles, silica would be the best choice as a standard. We also have noticed that metal shadowing of colloidal particle samples used for atomic/scanning force microscopy offers an advantage which we call a 'nanoscale metric' visible in the image directly at each particle site. This information can be important if one wishes to use samples prepared from colloidal particles simply and reliably to determine the probe shape for scanning probe microscopy from image deconvolution/restoration methods or as a calibration sample.     

Microstructure and Wear Properties of In Situ Synthesized VC Carbide Reinforced Fe-based Surface Composite Coating Produced by Laser Cladding

In situ synthesized VC carbide particles reinforced Fe-based composite coating was fabricated by laser cladding on steel substrate using ferrovanadium (Fe–V) alloy and graphite as the precursor powders. The phase structure and microstructure of the clad layer were investigated by means of X-ray diffraction analysis, scanning electron microscopy, and electron probe microanalysis. Results showed that uniformly distributed VC particles with the radial dendrites shape could be synthesized by the in situ reaction. The hardness and wear properties of the clad coatings were greatly improved due to the presence of VC particles in comparison with the substrate.     

TiC-VC颗粒增强Fe基熔敷层组织与耐磨性能

以H08A为焊芯，以钛铁、钒铁和石墨等为药皮组分，利用焊接电弧高温冶金反应，在Q235基体上制备TiC-VC复合超硬颗粒增强Fe基熔敷层。利用扫描电镜、X射线衍射仪、透射电镜、能谱分析仪及磨损试验，研究了熔敷层的组织、性能及组分加入量对熔敷层性能的影响。研究结果表明：冶金反应形成的TiC-VC颗粒尺寸细小，且弥散分布在基体上；熔敷层硬度在HRC55以上，具有很高的耐磨性和良好的抗裂性；钛铁、钒铁及石墨加入量（质量分数）分别为15％～18％、12％～14％和8％～10%时，熔敷层具有良好的耐磨性能和抗裂性能。     

Revealing local variations in nanoparticle size distributions in supported catalysts: a generic TEM specimen preparation method

The specimen preparation method is crucial for how much information can be gained from transmission electron microscopy (TEM) studies of supported nanoparticle catalysts. The aim of this work is to develop a method that allows for observation of size and location of nanoparticles deposited on a porous oxide support material. A bimetallic Pt‐Pd/Al₂O₃ catalyst in powder form was embedded in acrylic resin and lift‐out specimens were extracted using combined focused ion beam/scanning electron microscopy (FIB/SEM). These specimens allow for a cross‐section view across individual oxide support particles, including the unaltered near surface region of these particles. A site‐dependent size distribution of Pt‐Pd nanoparticles was revealed along the radial direction of the support particles by scanning transmission electron microscopy (STEM) imaging. The developed specimen preparation method enables obtaining information about the spatial distribution of nanoparticles in complex support structures which commonly is a challenge in heterogeneous catalysis.     

In‐situ imaging of Li intercalation in graphite particles in an Li‐ion battery

This paper presents the imaging of the expansion and contraction of graphite particles at the anode of a lithium‐ion battery. The intercalation and deintercalation of Li ions in the graphite particles induced by charging and discharging lead to expansion and contraction of the layered materials. These changes in volume were imaged through current collectors using scanning probe microscopy, which permitted in‐situ observation of the Li ion shift with high resolutions. We were able to evaluate the properties of each individual graphite particle. Here, we present variations in the images obtained by two methods of charging/discharging. In one method, the applied fields are changed, forcing the ions to move back into the graphite particles. Images showing detailed structures were obtained, allowing us to investigate the fine structures of the graphite particles. In the other method, the amount of ions is periodically injected into the graphite, which did not reveal the detailed structure but clearly distinguished inactive from active particles.     

Application of X‐ray microcomputed tomography in the characterization of irradiated nuclear fuel and material specimens

X‐ray microcomputed tomography (μCT) was applied in characterizing the internal structures of a number of irradiated materials, including carbon‐carbon fibre composites, nuclear‐grade graphite and tristructural isotropic‐coated fuel particles. Local cracks in carbon‐carbon fibre composites associated with their synthesis process were observed with μCT without any destructive sample preparation. Pore analysis of graphite samples was performed quantitatively, and qualitative analysis of pore distribution was accomplished. It was also shown that high‐resolution μCT can be used to probe internal layer defects of tristructural isotropic‐coated fuel particles to elucidate the resulting high release of radioisotopes. Layer defects of sizes ranging from 1 to 5 μm and up could be isolated by tomography. As an added advantage, μCT could also be used to identify regions with high densities of radioisotopes to determine the proper plane and orientation of particle mounting for further analytical characterization, such as materialographic sectioning followed by optical and electron microscopy. In fully ceramic matrix fuel forms, despite the highly absorbing matrix, characterization of tristructural isotropic‐coated particles embedded in a silicon carbide matrix was accomplished using μCT and related advanced image analysis techniques.     

In situ observation of the initial growth process of carbon nanotubes by time-resolved high resolution transmission electron microscopy

We succeeded in plan-view dynamic observation of the initial formation process of carbon nanotubes from β-SiC( 1 1 1 ) surfaces by time-resolved high resolution transmission electron microscopy. At 1360 °C, the flakes of graphite layers of a fibre orientation were formed on the SiC( 1 1 1 ) surfaces. From the graphite layers, carbon nanotubes were formed perpendicular to the ( 1 1 1 ) plane of the SiC. A scanning tunnelling microscopy observation showed that the end of carbon nanotube was closed. These results indicate that the caps of the carbon nanotubes are formed by a lift of a part of the graphene along the [ 1 1 1 ] direction of the SiC through generation of pentagons and heptagons. Two types of carbon nanotube, single-wall and double-wall, were observed in plan-view images. Different image intensity between an outer ring and an inner ring in double-wall nanotubes suggests that the inner layers of multiwall nanotubes are formed after the outer ones.     

On the wear rate of an Sn11Sb5.5Cu Babbitt

The microstructure of β-phase of Sn11Sb5.5Cu Babbitt produced by casting and liquid forging has been analyzed by optical and scanning electron microscopy using EBSD analysis. It has been established that a significant decrease in the wear rate of Babbitt produced by liquid forging is caused by generation of fine grain structure in the particles of the β phase.     

Measurement of Friction Surface and Wear Rate between a Carbon Graphite Brush and a Copper Ring

A pin-on-disc surface friction tester designed by the authors was used to measure the surface friction temperature of a carbon graphite brush sliding against a copper ring under the condition of no flow by electric current. Microelectromechanical systems (MEMS) fabrication techniques including sputtering, lithography, and etching processes were utilized to fabricate metal film temperature sensors on the surface of the carbon graphite brush. The true temperature measurement system of the friction surface of the carbon graphite brush was then established. A USB-DAQ system and LabVIEW software were adopted for the data acquisition/management of analog signals. In this research, the relationship between friction temperature and wear rate was investigated using experiment data. Optical and scanning electron microscope (SEM) images of the friction surface of the carbon graphite brush were taken and analyzed to study the effect of temperature on the friction surface. From this experiment, it was found that the debris of a mixture of brush and copper particles softens under high temperature, adheres to the brush surface, and forms flattened areas. These smooth, flattened areas in turn lower the friction coefficient.     

Study on solid lubricant properties of carbon onions produced by heat treatment of diamond clusters or particles

Tribological properties of carbon onions prepared by heat treatment of diamond clusters or particles are presented. Diamond clusters used as the source material are heated with an infrared radiation furnace to 1730 °C in argon at atmospheric pressure. As a result of heating at 1730 °C for 1 min, diamond clusters are transformed into carbon onions. High resolution TEM observation is employed to confirm the formation of carbon onions that have near-spherical and multi-layered concentric structure. The particle size of these carbon onions ranges from 5 to 10 nm that corresponds to the original size of the diamond clusters. This preparation technique is also applied to diamond particles less than 0.5 μm in diameter to produce larger carbon onions. Tribological properties of the carbon onions are examined by ball-on-disc type friction testing using a silicon wafer and a steel ball. Carbon onions, which are spread on the silicon wafer without adhesive, exhibit stable friction coefficients lower than 0.1 both in air and in vacuum at room temperature. The wear rates of steel balls sliding on the silicon wafer on which carbon onions are distributed are much lower than wear rates for sliding on a wafer over which graphite powder is spread. Moreover, it is found that the larger carbon onions prepared from diamond particles show low friction property on the rough surface of silicon discs.     

The nature and origin of wear particles from boundary lubrication with a zinc dialkyl dithiophosphate

It is well known that in many tribological situations antiwear additives act by reaction film formation on contacting surfaces. In the present paper we describe our observations on the reaction film formed with a zinc dialkyl dithiophosphate and the wear particles. Detailed structural and chemical information has been obtained by using optical microscopy, scanning electron microscopy, transmission electron microscopy and X-ray energy spectrometry. The results show a clear connection between the reaction film material and the nature of the wear particles present in the lubricant; both a highly dispersed phase system and a layered structure are present. The origin of the wear particles is discussed in terms of crack initiation mechanisms.     

钢背衬碳纤维织物/环氧复合材料干摩擦特性研究

研究了钢背衬碳纤维织物/环氧复合材料在环-环端面干摩擦状态下的摩擦学特性,考察了MoS2与石墨粉及其配比、衬层厚度、法向载荷对衬层干摩擦性能的影响,用扫描电子显微镜对衬层的磨损表面及对偶件45^#钢环表面进行了观察与分析。结果表明：厚度为1.5mm的试环衬层在摩擦过程中主要表现出粘结磨损特性,而含20%（质量分数）MoS2粉的0.6mm衬层表现出疲劳磨损与磨粒磨损特性。摩擦因数-时间特性曲线表明MoS2粉在降低衬层摩擦因数的同时能够抑制环氧树脂向对偶钢环表面的粘结;石墨对衬层的减摩效果优于MoS2粉,但摩擦温升引起树脂向偶件表面转移增多使得减摩效果大大降低;质量分数为33%的MoS2与石墨粉衬层表现出最佳的摩擦学性能,衬层摩擦因数具有随载荷先减小后上升的趋势。     

屏蔽泵石墨轴承材料的强度和耐磨性研究

对屏蔽泵的石墨轴承材料的强度、磨损性和摩擦系数进行了实验研究。在DWD-3020电子万能试验机上对普通石墨和浸润树脂石墨材料的弹性模量进行了测定，同时确定了材料的拉伸和压缩强度极限。在Falex摩擦磨损机上对材料进行了磨损试验，得到了转速和载荷对这两种材料磨损的影响，并利用CSM950扫描电子显微镜对其摩擦表面作了形貌分析。     

Water-Based Lubrication of Hard Carbon Microspheres as Lubricating Additives

Because of their superior physical and chemical stability, carbon microspheres have been identified as promising lubricating additives. In this paper, hard carbon microspheres with diameters ranging from approximately 130 to 250 nm were prepared through a hydrothermal method using glucose as the carbon source. The as-prepared carbon microspheres were characterized by a series of complementary techniques including field emission scanning electron microscopy, Fourier-transform infrared spectroscopy, Raman spectroscopy, and X-ray diffraction. It was found that the as-prepared carbon microspheres were spherical with graphitic structure. The effects of applied load, concentration, and particle size of the carbon microspheres as water-based lubricating additives against an opposing smooth silicon surface were systematically studied using a UMT tribometer and a 3D noncontact interferometric microscope. The results showed that carbon microspheres can effectively reduce friction and wear on a smooth silicon surface and the optimal performance was obtained at an applied load of 100 mN, a concentration of carbon microspheres of 0.1 wt% and an average particle size of 200 nm. The superior performance of carbon microspheres as water-based lubricating additives was attributed to having the particles dispersed as individual particles (as opposed to clusters) and also having sufficient physically and chemically stable particles within the contact region which allowed for a rolling friction mechanism to reduce friction.     

Cryogenic‐temperature electron microscopy direct imaging of carbon nanotubes and graphene solutions in superacids

Cryogenic electron microscopy (cryo‐EM) is a powerful tool for imaging liquid and semiliquid systems. While cryogenic transmission electron microscopy (cryo‐TEM) is a standard technique in many fields, cryogenic scanning electron microscopy (cryo‐SEM) is still not that widely used and is far less developed. The vast majority of systems under investigation by cryo‐EM involve either water or organic components. In this paper, we introduce the use of novel cryo‐TEM and cryo‐SEM specimen preparation and imaging methodologies, suitable for highly acidic and very reactive systems. Both preserve the native nanostructure in the system, while not harming the expensive equipment or the user. We present examples of direct imaging of single‐walled, multiwalled carbon nanotubes and graphene, dissolved in chlorosulfonic acid and oleum. Moreover, we demonstrate the ability of these new cryo‐TEM and cryo‐SEM methodologies to follow phase transitions in carbon nanotube (CNT)/superacid systems, starting from dilute solutions up to the concentrated nematic liquid‐crystalline CNT phases, used as the ‘dope’ for all‐carbon‐fibre spinning. Originally developed for direct imaging of CNTs and graphene dissolution and self‐assembly in superacids, these methodologies can be implemented for a variety of highly acidic systems, paving a way for a new field of nonaqueous cryogenic electron microscopy.