不同基体CrN/CrCN多层涂层海水环境摩擦学性能研究*

为研究不同基体材料对CrN/CrCN多层涂层在海水环境下摩擦学性能的影响,采用多弧离子镀技术在H65铜合金、TC4钛合金和316L不锈钢基体上沉积CrN和CrN/CrCN多层复合涂层,通过XRD、SEM等技术对涂层的结构进行表征,通过结合力、硬度测试和摩擦磨损试验分析涂层在大气环境和海水环境下的力学性能和摩擦学性能。结果表明:CrN/CrCN多层涂层的内应力相对于CrN明显减小,且硬度相对CrN涂层较高;TC4钛合金为基体的涂层结合力较好且涂层硬度较高;在海水环境下涂层的摩擦因数相对于大气环境都有较大幅度下降,其中,以TC4钛合金和316L不锈钢为基体的涂层摩擦因数较小;以H65铜合金为基体的2种涂层在海水中的磨损率高于大气中,而以TC4合金、316L不锈钢为基体的CrN/CrCN多层涂层在海水环境下的磨损率低于大气环境;TC4钛合金为基体的CrN/CrCN多层涂层在海水环境下具有最低的磨损率,表明TC4钛合金更适合作为海水环境下CrN/CrCN多层涂层耐磨的基体材料。     

Cr2N/CrN multilayer coatings for wood machining tools

The present paper describes results from a recent research project aimed at forming a wear resistant coating based on chromium on tools to wood machining. Cr₂N/CrN multilayer coatings deposited on HS6-5-2 steel substrates using cathodic arc evaporation were tested. These coatings were formed from 7 bilayers being ca. 340 nm thick and equally thick Cr₂N and CrN layers. For comparison, Cr₂N and CrN monolayer coatings were also prepared. Hardness measurements, indentation and scratch tests, friction and wear were performed to characterize the mechanical properties. The wear tracks and Rockwell indentations enable to assess wear mechanisms of the coatings. The results of the Cr₂N/CrN coatings investigated show high hardness: ca. about 22 GPa and a critical force being higher than 95 N and a low wear rate.The industrial tests of planer knives with Cr₂N/CrN multilayer coatings were carried out on a down-spindle milling machine to determine the durability of tools with wear resistant coatings for woodworking. These tools show increase of “life time” two times. Another positive feature of the use of such tools is the increase of the quality of wood surface machined when compared with uncoated tools.     

Tribological properties of laser-textured and ta-C coated surfaces with burnished WS2 at elevated temperatures

The possibility of enhancing the tribological properties of ta-C at elevated temperature (250 °C) by laser surface texturing and burnished WS₂ addition were investigated. Laser texturing was applied prior to ta-C coating process. Samples were tribologically tested at room temperature and elevated (250 °C) temperature using pin-on-disc. WS₂ addition increased remarkably the wear life of ta-C at 250 °C and low COF values (0.01–0.02) were achieved. Laser surface texturing (LST) increased the wear life of WS₂/ta-C surfaces by more than two times compared to non-textured surface. The LST dimples functioned as solid lubricant reservoirs and improved the wear life of the initial WS₂ layer. This was noticed to be related to wear mechanism with raised position dimples and partly oxidized WS₂.     

Wear mechanism of coated tools in the turning of ductile cast iron having wide range of tensile strength

In this study different specimens of ductile cast iron with tensile strength ranking from 400 MPa to 675 MPa were turned with K15 carbide, TiN coated and TiAlN coated tool in order to investigate wear mechanism and performance. Cutting forces and cutting temperature were similar for both coated tools, however flank wear and BUE were the lowest on the TiAlN coated tool, for this reason the TiAlN coated tool is suitable in the machining of ductile cast iron. The proposed tool wear mechanism is based on like-intermittent cutting caused by the pass from hard matrix to the soft graphite occasioning wear by adhesion. The analysis of the flank wear on coated tools is proposed by means of the wear curves in logarithmic scale instead of the usual linear scale. In this way, the change in wear rate is easily observed. This phenomenon was related with the wear out of the coating layer. The partial loss of the coating layer on cutting edge was confirmed by the EDS mapping images and SEM photographs.     

Rapid and simultaneous determination of tetracycline and cefixime antibiotics by mean of gold nanoparticles-screen printed gold electrode and chemometrics tools

The screen-printed gold electrode (SPGE) modified with the formation of self-assembly monolayer (SAM) of cysteine (Cys) on gold-nanoparticles (Au_nano) was utilized for rapid and simultaneous determination of tetracycline and cefixime antibiotics by square wave voltammetry (SWV). Electrochemical investigation and characterization of the modified electrode was achieved using cyclic voltammetry (CV) and scanning electron microscopy (SEM). A principal component artificial neural network (PCANN) with three layer back-propagation network was utilized for the analysis of the voltammogram data. It is possible to simultaneously determine the tetracycline and cefixime concentrations in the ranges of 10⁻⁵ and 10⁻³ mol L⁻¹, under the optimum conditions. Moreover the SPGE-Au_nano-Cys biosensor together with chemometrics tools was successfully applied to the determination of tetracycline and cefixime in biological fluids, which may provide a promising alternative in routine biosensing applications.     

The design of polyaniline based sensor for the qualitative estimation of malonaldehyde

The detection of contaminated food in every stage of processing required new technology for fast identification and isolation of toxicity in food. Since effect of food contaminant are severe to human health, the need of pioneer technologies also increasing over last few decades. In the current study, MDA was prepared by hydrolysis of 1,1,3,3-tetramethoxypropane in HCl media and used in the electrochemical studies. The electrochemical sensor was fabricated with modified glassy carbon electrode with polyaniline. These sensors were used for detection of sodium salt of malonaldehyde and observed that a high sensitivity in the concentration range ∼1 × 10⁻¹ M and 1 × 10⁻² M. Tafel plots show the variation of over potential from − 1.73 V to − 3.74 V up to 10⁻⁵ mol/L indicating the lower limit of detection of the system.     

Development of a simple ‘temperature versus sliding speed’ wear map for the sliding wear behaviour of dissimilar metallic interfaces

The variation in wear behaviour during limited debris retention sliding wear of Nimonic 80A versus Stellite 6 (counterface) between room temperature and 750 °C, at sliding speeds of 0.314, 0.654 and 0.905 m s⁻¹, was investigated. At 0.314 m s⁻¹, mild oxidational wear was observed at all temperatures, due to transfer and oxidation of Stellite 6-sourced debris to the Nimonic 80A and resultant separation of the Nimonic 80A and Stellite 6 wear surfaces. Between room temperature and 450 °C, this debris mostly remained in the form of loose particles (with only limited compaction), whilst between 510 and 750 °C, the particles were compacted and sintered together to form a wear protective ‘glaze’ layer.At 0.654 and 0.905 m s⁻¹, mild oxidational wear due to transfer and oxidation of Stellite 6-sourced debris was only observed at room temperature and 270 °C (also 390 °C at 0.654 m s⁻¹). At 390 °C (450 °C at 0.654 m s⁻¹) and above, this oxide was completely absent and ‘metal-to-metal’ contact resulted in an intermediate temperature severe wear regime—losses in the form of ejected metallic debris were sourced almost completely from the Nimonic 80A. Oxide debris, this time sourced from the Nimonic 80A sample, did not reappear until 570 °C (630 °C at 0.654 m s⁻¹), however, were insufficient to eliminate completely severe wear until 690 and 750 °C. At both 0.654 and 0.905 m s⁻¹, the oxide now preventing severe wear at 690 and 750 °C tended not to form ‘glaze’ layers on the surface of the Nimonic 80A and instead supported continued high wear by abrasion. This abrasive action was attributed to the poor sintering characteristics of the Nimonic 80A-sourced oxide, in combination with the oxides’ increased mobility and decreased residency.The collected data were used to compose a simple wear map detailing the effects of sliding speed and temperature on the wear of Nimonic 80A slid against Stellite 6, at these speeds and temperatures of between room temperature and 750 °C.     

Enhancing electrical conductivity and electrical thermal characteristics of a PEDOT:PSS thin layer by using solvent treatment and adding Ag nanoparticle solution

A method of enhancing the electrical conductivity of 3,4-ethylenedioxythiophene:poly styrene sulfonate (PEDOT:PSS) by combining solvent treatment (adding high polar solvent: 5 wt% ethylene glycol) and adding a small amount of silver (Ag) nanoparticles in a solution was investigated. The main purpose of this was to apply a PEDOT:PSS conductive layer to micro-thermal devices driven by electricity and, for this, to reduce the layer thickness (for low stiffness) while maintaining necessary high electrical conductivity. Layers with thicknesses of less than about 10 μm were examined for electrical conductivity and temperature when electricity was applied. The solvent treated PEDOT:PSS had suitable electrical resistance to generate appropriate temperature properties. The added Ag nanoparticles reduced the electrical resistance by 30–70% over the measured thickness range. The electric conductivity applied with this method was 200–260 Ω⁻¹ cm⁻¹ for thicknesses of 1–2 μm (conductive area: 12 mm × 10 mm) and the generated temperature increase was 20–50 °C at applied voltages of 3–5 V. These characteristics are considered to be suitable to use the conductive layer as a heating element. In addition, the method we used scarcely degraded the transparency of the layer. Measurements of the conductive area in a layer with conductive atomic force microscope (AFM) indicated that the added Ag nanoparticles contributed to increasing the conductive areas and distributing them more uniformly.     

1-N-alkyl -3-methylimidazolium ionic liquids as neat lubricants and lubricant additives in steel–aluminium contacts

The influence of the alkyl chain length and of the anion on the lubricating ability has been studied for the room-temperature ionic liquids (IL) 1-n-alkyl-3-methylimidazolium X⁻ [X = PF₆; n = 6 (L-P106). X = BF₄; n = 2 (L102), 6 (L106), 8 (L108). X = CF₃SO₃; n = 2 (L-T102). X = (4-CH3C6H4SO3); n = 2 (L-To102)]. Neat IL have been used for AISI 52100 steel-ASTM 2011 aluminium contacts in pin-on-disk tests under variable sliding speed. While all IL give initial friction values lower than 0.15, real-time sharp friction increments related to tribochemical processes have been observed for L102 and L-P106, at room-temperature and at 100 °C. Electronic microscopy (SEM), energy dispersive (EDS) and X-ray photoelectron (XPS) spectroscopies show that wear scar surfaces are oxidized to Al₂O₃ and wear debris contain aluminium and iron (for L102) fluorides. For L-P106, the steel surface is covered with a P-containing tribolayer. A change of anion (L-T102; L-To102) reduces friction and wear, but the lowest values are obtained by increasing the alkyl chain length (L106; L108). When the more reactive L102 and L-P106 are used as 1 wt.% base oil additives at 25 °C, tribocorrosion processes are not observed and a friction reduction (69–75% for 1 wt.% L102) and a change from severe (10⁻³ mm³ m⁻¹) to mild wear (10⁻⁴ to 10⁻⁶ mm³ m⁻¹) is obtained with respect to the neat IL. 1 wt.% IL additives also show good lubricating performance at 100 °C.     

Wear behaviour of iron boride coatings produced by VPS technique on carbon steels

The vacuum plasma spray (VPS) technique is a useful tool for designing the characteristics of the coatings and, thus, the tribological properties of coated components. In the present paper, the wear properties of iron boride coatings produced by means of VPS technique on AISI 1040 steel samples were evaluated as a function of their microstructural characteristics. One coating type was obtained by using Fe₂B pure powder, the other with differentiated FeB + α-Fe blends, with the FeB content increasing and α-Fe content decreasing from the matrix to the surface. Wear tests were performed by means of a tribometer in block-on-ring configuration, without lubricant and in air, by using 40- and 60-N coupling loads and 0.8- and 1.6-m s⁻¹ sliding velocities. On Fe₂B coated samples, wear is essentially oxidative until the failure of the coating, the fragments of which cause a third body abrasion. On the FeB + α-Fe coated samples the wear mechanism is mainly oxidative and the coating totally wears out without spalling as a consequence of its graded structure, which succeeds in both improving the adhesion of the coating to the substrate and reducing the residual stress at the coating–substrate interface.     

Studies of high temperature sliding wear of metallic dissimilar interfaces IV: Nimonic 80A versus Incoloy 800HT

Wear variations of Nimonic 80A slid against Incoloy 800HT between room temperature (RT) and 750 °C, and sliding speeds of 0.314 and 0.905 m s⁻¹ were investigated using a ‘reciprocating-block-on-cylinder’, low debris retention configuration. These were considered alongside previous observations at 0.654 m s⁻¹.Different wear types occurring were mapped, including high transfer ‘severe wear’ (RT and 270 °C, also 0.905 m s⁻¹ at ≤570°C), low transfer ‘severe wear’ (0.314 m s⁻¹ at 390 °C to 510 °C oxide abrasion assisted at 510 °C), and ‘mild wear’ (0.314 m s⁻¹ at ≥570 °C; 0.905 m s⁻¹ at ≥630 °C). Wear surfaces at 750 °C were cross-sectioned and profiled.     

Potential step study of electrooxidation of methanol in 1-butyl-3-methylimidazolium tetrafluoroborate

A potential step method was used to characterize the electrooxidation of methanol on a chemically modified electrode in an ionic liquid solvent. Two major findings were reported from this study. Firstly, the oxidation was dominant 2.2 s after the potential step. Before that, the double layer charging and adsorption were dominant. Therefore, there should be a waiting time of a few seconds if a methanol sensor is developed with a potential step method. Secondly, the oxidation of methanol on the electrode was diffusion controlled. The concentration of methanol affected the diffusion. The diffusion constant D₀ was 8.37 × 10⁻¹⁷ m²/s when the concentration was lower than 0.5 M and was 2.66 × 10⁻¹³ m²/s when the concentration was higher than 1.0 M. This suggests that the methanol concentration should be kept higher than a threshold in an ionic liquid based fuel cell.     

Determination of haloperidol drug in ampoules and in urine samples using a potentiometric modified carbon paste electrode

A modified carbon paste electrode for haloperidol drug based on haloperidol-phosphomolybdate (HP-PM) as an ion-exchanger dissolved in plasticizer DBP and its potentiometric characteristics were discussed. The electrode exhibited a good Nernstian slope of 56.9 ± 0.3 mV/decade with a linear concentration range from 3.2 × 10⁻⁶ to 1.0 × 10⁻² M for the haloperidol ion. The limit of detection (LOD) was 1.5 × 10⁻⁶ M. It had response time of 5–8 seconds (s), useable in pH range of 6.2–8.6 and temperature of 20–60 °C. The electrode shows clear discrimination of haloperidol drug from several inorganic ions, sugars and some common drug excipients. The sensor was applied for determination of haloperidol drug in urine and in pharmaceutical formulations using potentiometric determination, standard addition and the calibration curve methods. The results are satisfactory with excellent percentage recovery comparable or better than those obtained by other routine methods.     

Effect of SiC particles on the friction and wear behavior of Ti3Si(Al)C2-based composites

The non-lubricated, sliding friction and wear behavior of Ti₃Si(Al)C₂ and SiC-reinforced Ti₃Si(Al)C₂ composites against AISI 52100 bearing steel ball were investigated using a ball-on-flat, reciprocating tribometer at room temperature. The contact load was varied from 5 to 20 N. For monolithic Ti₃Si(Al)C₂, high friction coefficients between 0.61 and 0.90 and wear rates between 1.79 × 10⁻³ and 2.68 × 10⁻³ mm³ (N m)⁻¹ were measured. With increasing SiC content in the composites, both the friction coefficients and the wear rates were significantly decreased. The friction coefficients reduced to a value between 0.38 and 0.50, and the wear rates to between 2.64 × 10⁻⁴ and 1.93 × 10⁻⁵ mm³ (N m)⁻¹ when the SiC content ranged from 10 to 30 vol.%. The enhanced wear resistance of Ti₃Si(Al)C₂ is mainly attributed to the facts that the hard SiC particles inhibit the plastic deformation and fracture of the soft matrix, the oxide debris lubricate the counterpair, and the wear mode converts from adhesive wear to abrasive wear during dry sliding.     

Electrocatalytic determination of captopril using a modified carbon nanotube paste electrode: Application to determination of captopril in pharmaceutical and biological samples

A carbon paste electrode modified with carbon nanotube and benzoylferrocene (BF) was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for electrocatalytic oxidation of captopril (CAP), was described. The electrode was employed to study the electrocatalytic oxidation of CAP, using cyclic voltammetry (CV), chronoamperometry (CHA) and square wave voltammetry (SWV) as diagnostic techniques. It has been found that the oxidation of CAP at the surface of modified electrode occurs at a potential of about 85 mV less positive than that of an unmodified CPE. SWV exhibits a linear dynamic range from 1.0 × 10⁻⁷ to 3.5 × 10⁻⁴ M and a detection limit of 3.0 × 10⁻⁸ M for CAP. Finally the modified electrode was used for determination of CAP in CAP tablet and urine sample.     

Specific energy and surface roughness of minimum quantity lubrication grinding Ni-based alloy with mixed vegetable oil-based nanofluids

Vegetable oil is a low toxic, excellent biodegradable and renewable energy source used as an ideal lubricating base oil in machining. Castor oil exhibits good lubrication performance but poor mobility, which limits its application especially in precision grinding. The main objective of the work presented to obtain optimal mixed vegetable based-oil and optimal nanoparticles adding concentration in grinding Ni-based alloy with minimum quantity lubrication. An experimental investigation is carried out first to study the different vegetable oils with excellent mobility mixed with castor oil. The lubrication property of the oil was evaluated in terms of grinding force, force ratio, specific grinding energy, and surface roughness. Based on the test conditions, it is found that soybean/castor mixed oil obtained the optimal results (μ= 0.379, U = 83.27 J/mm³ and Ra = 0.325 μm) and lubricating effect compared with castor oil and other mixed base oils. To further explore the lubricating capability of soybean/castor mixed oil, MoS₂ nanoparticles which have excellent lubricating property were added into the soybean/castor mixed oil to prepare different concentrations nanofluids. From the present study, it can be concluded that 8% mass fraction of the oil mixture should be added to obtain the optimal machining results, with the lowest force ratio (0.329), specific energy (58.60 J/mm³), and average grinding temperature (182.6 °C). Meanwhile, better surface microtopography of ground parts and grinding debris morphologies were also observed for the machining conditions.     

Wear mechanisms of WC coated and uncoated tools in finish turning of Inconel 718

This paper presents the results of an experimental investigation on the wear mechanisms of uncoated tungsten carbide (WC) and coated tools (single-layer (TiAlN) PVD, and triple-layer (TiCN/Al₂O₃/TiN) CVD) in oblique finish turning of Inconel 718. Tool wear rate and wear mechanisms were evaluated for cutting speeds, 50<V<100 m/min, and feed rates, 0.075<f<0.125 mm/rev, at a constant depth of cut of 0.25 mm. It was concluded that abrasive and adhesive wear were the most dominant wear mechanisms, controlling the deterioration and final failure of the WC tools. While the triple layer CVD coated tools exhibited the highest wear resistance at high cutting speeds and low feeds, uncoated tools outperformed the single and multi-layer coated tools in the low range of cutting speeds and intermediate feeds. The cutting tool with single-layer PVD coating outperformed the other tools at the medium cutting speed.     

Cavitation resistance of Cr–N coatings deposited on austenitic stainless steel at various temperatures

Cr–N coatings were deposited on austenitic stainless steel, X6CrNiTi18-10, by means of the cathodic arc evaporation method at three substrate temperatures: 200 °C, 350 °C and 500 °C. All coatings were found to have a composition of Cr(N), CrN and Cr₂N. The substrate temperature was found to have an influence on the hardness and Young's modulus of the Cr–N coatings. The investigation of nanocrystalline Cr–N coatings resistance to cavitation was performed in a cavitation tunnel with a slot cavitator and tap water as the medium. The estimated cavitation resistance parameters of the coatings were the incubation period of damage and total mass loss. It was found that the optimal coating cavitation resistance was deposited at 500 °C. The incubation period for the 500 °C deposition coating was the same as that of the uncoated X6CrNiTi18-10 steel, but the total mass loss was significantly lower than on the uncoated specimen. The scanning electron microscope analysis indicated that the damage process of the Cr–N coating mainly originates from the plastic deformation of the steel substrate–hard coating system, which appears by “micro-folding” of the surface. An increase of tensile stresses at the top of micro-folds initiates micro-cracks and delamination of Cr–N coating. The results of the investigation and the analysis indicate that the factors mainly responsible for cavitation resistance of the steel substrate/hard coating system are resistant to plastic deformation of the total system and coating adhesion.     

Application of highly silicon-doped marker layers in the investigation of unintentional doping in GaN on sapphire

To provide a route to the assessment of the impact of inclined facets on unintentional n-type doping during the growth of c-plane GaN on sapphire, thin (100 nm), highly Si-doped (at 10¹⁹ cm⁻³) marker layers have been incorporated into a GaN epitaxial layer grown by a method involving a transition from initial three-dimensional island growth to later, two-dimensional, planar growth. Imaging of the completed epitaxial layer in cross-section by scanning capacitance microscopy reveals the shapes of the islands, which were present during the early stages of growth and the relationship between the facets present and the incorporation of unintentional dopants. The results show that unintentional dopants are mostly incorporated on facets inclined to the [0 0 0 1] direction, and suggest that gaseous impurities present in the MOVPE reactor are one source of dopant species.     

An ultra high-pressure test rig for measurements of small flow rates with different viscosities

Within the framework of a research project regarding investigations on a high-pressure Coriolis mass flow meter (CMF) a portable flow test rig for traceable calibration measurements of the flow rate (mass - and volume flow) in a range of 5 g min⁻¹ to 500 g min⁻¹ and in a pressure range of 0.1 MPa to 85 MPa was developed. The measurement principle of the flow test rig is based on the gravimetrical measuring procedure with flying-start-and-stop operating mode. Particular attention has been paid to the challenges of temperature stability during the measurements since the temperature has a direct influence on the viscosity and flow rate of the test medium. For that reason the pipes on the high-pressure side are double-walled and insulated and the device under test (DUT) has an enclosure with a separate temperature control. From the analysis of the first measurement with tap water at a temperature of 20 °C and a pressure of 82.7 MPa an extensive uncertainty analysis has been carried out. It was found that the diverter (mainly due to its asymmetric behaviour) is the largest influence factor on the total uncertainty budget. After a number of improvements, especially concerning the diverter, the flow test rig has currently an expanded measurement uncertainty of around 1.0% in the lower flow rate range (25 g min⁻¹) and 0.25% in the higher flow rate range (400 g min⁻¹) for the measurement of mass flow. Additional calibration measurements with the new, redesigned flow test rig and highly viscous base oils also indicated a good agreement with the theoretical behaviour of the flow meter according to the manufacturers׳ specifications with water as test medium. Further improvements are envisaged in the future in order to focus also on other areas of interest.