High resolution XPS characterization of chemical functionalised MWCNTs and SWCNTs

High resolution XPS analysis of chemical functionalised multi-wall carbon nanotubes (MWCNTs) and single wall carbon nanotubes (SWCNT) was done with ESCA300 (overall instrument resolution of 0.35 eV). Information to the degree of functionalisation was ascertained by argon ion bombardment of the samples followed by XPS analysis to detect the functional groups, the percentage atomic concentration of various elements present and whether or not the detected functional groups imposed a chemical shift on the CNT atoms. The results show that true chemical functionalisation was achieved and by argon ion bombardment these functional groups can be altered relative to the C 1s carbon atoms of the CNT. The choice of chemicals used for functionalisation, the techniques employed and the types of nanotubes treated are important factors in chemical characterisation. The carbon atom on the nanotube ring to which the functional group (atom) is bonded, the chirality of the CNT, the electronegativity of the functional group, the bond type and whether the CNT is single-wall or multi-wall, or cut (short) could play a role in determining the chemical shift on the CNTs atoms. These investigations are relevant to chemical functionalisation of carbon nanotubes for various applications for example DNA sensors and other biomedical sensors.     

Quantitation of volatile compounds in heated triolein by static headspace capillary gas chromatography/infrared spectroscopy-mass spectrometry

Static headspace and capillary gas chromatography/infrared spectroscopy-mass spectrometry were used to collect, separate, identify and quantitate the oxidative and thermal decomposition products in heated triolein. Approximately 4 L of triolein was heated in a deep-fat fryer at 190°C for 12 h each day for a total of 60 h, until it contained>-20% polymeric material. The concentration of heptane and octane increased after 12 h heating, then decreased upon further heating, while the concentration of volatile aldehydes decreased gradually during heating. After 12 h of heating, the concentrations of the major volatiles changed as follows: heptane (16.36 to 30.17 ppm), octane (24.48 to 40.77 ppm), heptanal (21.68 ppm to 9.11 ppm), octanal (35.53 to 36.64 ppm), nonanal (68.95 to 43.16 ppm), (E)-2-decenal (135.00 to 89.00 ppm) and (E)-2-undecenal (88.50 to 61.00 ppm). After 60 h of heating, when the oil contained over 20% polymeric material, the concentrations of heptane, octane, heptanal, octanol, nonanal, (E)-2-decenal and (E)-2-undecenal were 5.16, 4.39, 5.45, 7.02, 18.07, 12.50 and 6.00 ppm, respectively.     

Effect of cobalt oxide on surface structure of alumina supported molybdena catalysts studied by in situ Raman spectroscopy

A set of Co promoted 10% Mo/Al₂O₃ samples have been characterized by means of Raman spectroscopy under ambient as well as in situ dehydrated conditions. Under ambient conditions, the degree of the polymerization of surface molybdenum oxide species decreases with increasing Co loading. Under dehydrated conditions, the polymeric molybdenum oxide species is absent with the addition of only 0.2% Co. At low Co loadings (2%), before the formation of CoMoO₄ compound, the spectral features are very similar under ambient conditions. Dehydration causes the upward shift of the Mo=O symmetric stretching mode. A broad band around 920–930 cm^–1 was thus observed. This band has been suggested to be associated with the Co-Mo interaction species. In contrast to crystalline CoMoO₄, this species shows a reversibility on H₂ reduction-O₂ reoxidation treatments. From the results obtained, it is proposed that cobalt oxide interacts with the most polymerized molybdenum oxide species to form Co-Mo interaction species and/or crystalline CoMoO₄; therefore, the amount of the surface molybdenum oxide species decreases with a change in the molecular structure as a function of the Co concentration.     

交流接触器温度场仿真及试验验证

将ANSYS有限元热分析应用到交流接触器热特性分析中,模仿其实际工作环境,构建交流接触器三维稳态热分析模型,确定热源、导热系数和表面散热系数,对接触器的稳态温度场进行分析;进一步改变施加的边界条件,研究不同散热方式下接触器的温度分布。最后对CJX2-0910型交流接触器进行温升试验,将温度场的仿真结果与试验结果比较,误差较小,表明所建立热分析模型的可行性。研究结果对接触器材料的选择、结构的设计及其性能的优化有重要意义。     

Model reference adaptive impedance control in Cartesian coordinates for physical human–robot interaction

In this paper, a nonlinear model reference adaptive impedance controller is proposed and tested. The controller provides asymptotic tracking of a reference impedance model for the robot end-effector in Cartesian coordinates applicable to rehabilitation robotics or any other human–robot interactions such as haptic systems. The controller uses the parameters of a desired stable reference model which is the target impedance for the robot’s end-effector. It also considers uncertainties in the model parameters of the robot. The asymptotic tracking is proven using Lyapunov stability theorem. Moreover, the adaptation law is proposed in joint space for reducing the complexity of its calculations; however, the controller and the stability proof are all presented in Cartesian coordinates. Using simulations and experiments on a two DOFs robot, the effectiveness of the proposed controller is investigated.     

Infrared study of salt free and salt treated cellulose pyrolysis under nitrogen atmosphere

The pyrolysis under nitrogen of salt free and salt treated cellulose was studied by infrared spectroscopy. The results confirm the unzipping mechanism suggested by DTA and TGA studies, and show this mechanism to apply to the untreated and salt treated samples. The results also show the unzipping to stop at the stage of char formation. The onset of this stage was found to occur after the volatilization of only 45–50% of the initial sample of the borax treated cellulose, compared with 65–70% of the KCl treated cellulose and 80–85% of the untreated cellulose.     

Softening and melting mechanisms of polyamides interfering with sliding stability under adhesive conditions

The thermal stability of polymers is a main issue when used as friction elements under dry sliding. Cast polyamide grades processed with either natrium or magnesium catalysors are slid on a small-scale and a large-scale test configuration to reveal the effect of softening or degradation on the sliding stability and to investigate possibilities for extrapolation of friction and wear rates between both testing scales. The combination of softening and afterwards transition into the glassy state is detrimental for the sliding stability of natrium catalysed polyamides, characterised by heavy noise during sliding. A transfer film formed under continuous softening also provides high friction. Melting during initial sliding is necessary for stabilisation in both friction and wear, and eventual softening of a molten film near the end of the test then not deteriorates the sliding stability. Softening of magnesium catalysed polyamides is favourable for the formation of a coherent transfer film resulting in more stable sliding than natrium catalysed polyamides. The differences in softening mechanisms of both polyamide grades is correlated to structural changes investigated by thermal analysis and Raman spectroscopy: the γ crystalline structure prevails in magnesium catalysed samples and the α crystalline structure is predominant in natrium catalysed samples. For internal oil lubricated polyamides, a time dependent degradation of the polyamide bulk deteriorates the supply of internal oil lubricant to the sliding interface, resulting in high friction and wear under overload conditions. As the degradation mechanisms during sliding are strongly correlated to the test set-up, extrapolation is only possible for friction in a limited application range, while wear rates cannot be extrapolated.     

Adhesive Bonding of Oil-Contaminated Steel Substrates

Durability of adhesive bonds formed by curing epoxies against oil-contaminated steel substrates using amidoamine curing agents was determined during exposure to boiling water. The most durable bonds were obtained using amidoamine curing agents with relatively low amine numbers and by blending silane coupling agents such as γ-glycidoxypropyltrimethoxysilane (γ-GPS) and N-(2-aminoethyl)-3-aminopropyltrimethoxy silane (AAMS) into the adhesives. When X-ray photoelectron spectroscopy (XPS) was used to characterize the failure surfaces of the adhesive joints after exposure to boiling water, it was determined that adhesives prepared using amidoamine curing agents with low amine numbers were able to displace the oil from the steel surface but adhesives prepared with amidoamine curing agents with high amine numbers were not. Results obtained from XPS also showed that the amino groups on the substrate fracture surfaces of joints prepared using curing agents with low amine numbers were protonated whereas the amino groups in the bulk adhesive were not, indicating that there was a chemical interaction between the curing agent and the hydrated surface of the substrate. It was also shown using infrared spectroscopy that the amidoamine curing agents formed salts with calcium compounds in the oil.     

Separation and identification of phenolic acids and related compounds by gas chromatography and fourier transform infrared spectroscopy

Phenolic acids and related compounds were separated by gas chromatography using three separate columns. One of these columns was coupled to a Fourier transform infrared spectrometer. The trimethylsilyl derivatives could be separated and identified by comparing the relative retention times of the three different columns. However, where there was overlap, the accompanying infrared data clearly distinguished between the questionable derivatives, thus enabling characterization of all derivatives.The use of trade, firm, or corporation names in this article is for the information and convenience of the reader. Such use does not constitute an official endorsement or approval by the U.S. Department of Agriculture or the Forest Service of any product or service to the exclusion of others that may be suitable.     

All-glass system for preparative gas chromatography using capillary columns

A zero dead-volume all-glass-lined stainless-steel effluent splitter with a modified thermal gradient collector was designed for preparative gas chromatography using glass capillary columns. This system gives efficient collection of extremely pure samples of the 1-ng to 10-g range for spectral analysis and biological testing.Approved as TA 15656 by the director of the Texas Agricultural Experiment Station in cooperation with ARS, USDA. Supported by the Texas Department of Agriculture interagency agreement IAC-0487 (78-79).