Characterization and tribological investigation of sol–gel ceramic films on Ti–6Al–4V

SiO₂, TiO₂, and hydroxyapatite (HA) thin films with good biocompatibility were grown on Ti–6Al–4V (coded as TC4) substrate by sol–gel and dip-coating processes from specially formulated sols, followed by annealing at 500 °C The chemical states of some typical elements in the target films were detected by means of X-ray photoelectron spectroscopy (XPS). Atomic force microscopy (AFM) and high-resolution scanning electron microscopy (SEM) are applied to characterize the original unworn films. The tribological properties of thin films sliding against an AISI52100 steel ball were evaluated on a reciprocating friction and wear tester. As the result, the target films composed of nano-particles ranging from 30 nm to 100 nm around were obtained. All the sol–gel ceramic films are superior in resisting wear compared with the TC4 substrate. Among all, HA film shows the best resistance while SiO₂ film shows the worst wear resistance both under higher (3 N) and lower load (1 N). TiO₂ shows good wear resistance under lower load (1 N). SEM observation of the morphologies of worn surfaces indicates that the wear of TC4 is characteristic of abrasive wear. Differently, abrasion, plastic deformation and micro-fracture dominate the wear of ceramic films. The superior friction reduction and wear resistance of HA film is greatly due to the slight plastic deformation of the film. It is supposed that the deformation of the HA film is closely related to the special arrangement of the nano-particles and microstructure. HA film is recommended for clinical application from the point of wear resistance view.     

Corrosion inhibition efficiency and adsorption behavior of azomethine compounds at mild steel/hydrochloric acid interface

The adsorption and inhibition effect of azomethine compounds: PhN = NAC (COCH₃) = NC₆H₄Y {Y = OCH₃ (SB₁), CH₃ (SB₂), H (SB₃), Br (SB₄) and Y = Cl (SB₅)} on mild steel in 1 M HCl at 25 °C were studied using gravimetric measurements, cyclic voltammetry, UV–visible Spectrophotométrique and scanning electron microscope (SEM) methods. Inhibition efficiency was found to increase with the increase in azomethine SB₁-SB₅ concentration. The adsorption of each inhibitor on mild steel surface obeys Langmuir adsorption isotherm. The results of cyclic voltammetry showed that the presence of azomethine compound decreases the charge density in the transpassive region. The UV–visible absorption spectra of the solution containing the inhibitor after the immersion of mild steel specimen indicate the formation of a (SB₁-SB₅)-Fe complex. SEM and EDX observations confirmed the existence of protective inhibitor film on a metal surface.     

Thermal optimization and supercapacitive application of electrodeposited Fe2O3 thin films

In the present work, thin films of Fe₂O₃ were deposited onto stainless steel substrates by electrodeposition method. All deposited electrodes were annealed for 1 h within the temperature range of 423–673 K with an interval of 50 K. These were further characterized for their structural and morphological measurements by means of X-ray diffraction and scanning electron microscopy techniques, respectively. The supercapacitive characteristics of as-deposited and annealed electrodes were carried out in 1 M KOH electrolyte to confirm the variation in specific capacitance, specific energy, specific power and columbic efficiency, etc., with annealing temperatures.     

Refined reconstruction of liquid–gas interface structures for stratified two-phase flow using wire-mesh sensor

Wire-mesh sensors (WMS), developed at HZDR [4], [13], are widely used to visualize two-phase flows and measure flow parameters, such as phase fraction distributions or gas phase velocities quantitatively and with a very high temporal resolution. They have been extensively applied to a wide range of two-phase gas–liquid flow problems with conducting and non-conducting liquids. However, for very low liquid loadings, the state of the art data analysis algorithms for WMS data suffer from the comparably low spatial resolution of measurements and from boundary effects, caused by e.g. flange rings – especially in the case of capacitance type WMS. In the recent past, diverse studies have been performed on two-phase liquid–gas stratified flow with low liquid loading conditions in horizontal pipes at the University of Tulsa. These tests cover oil–air flow in a 6-inch ID pipe and water–air flow in a 3-inch ID pipe employing dual WMS with 32×32 and 16×16 wires, respectively. For oil–air flow experiments, the superficial liquid and gas velocities vary between 9.2 m/s≤ν_SG≤15 m/s and 0.01 m/s≤ν_SL≤0.02 m/s, respectively [2]. In water–air experiments, the superficial liquid and gas velocities vary between 9.1 m/s≤ν_SG≤33.5 m/s and 0.03 m/s≤ν_SL≤0.2 m/s, respectively [17], [18]. In order to understand the stratified wavy structure of the flow, the reconstruction of the liquid–gas interface is essential. Due to the relatively low spatial resolution in the WMS measurements of approximately 5 mm, the liquid–gas interface recognition has always an unknown uncertainty level. In this work, a novel algorithm for refined liquid–gas interface reconstruction is introduced for flow conditions where entrainment is negligible.     

Tribological behaviors of Ti–6Al–4V modified by chemical methods

In order to improve the tribological properties of titanium-based implants, sodium hydroxide (NaOH), hydrogen peroxide (H₂O₂) solutions, sol–gel hydroxyapatite (HA) film, thermal treatment and combined methods of NaOH solution/HA film, H₂O₂ solution/HA film are used to modify the surfaces of Ti–6Al–4V (coded TC4). The chemical states of some typical elements in the modified surfaces were detected by means of X-ray photoelectron spectroscopy (XPS). The tribological properties of modified surfaces sliding against an AISI52100 steel ball were evaluated on a reciprocating friction and wear tester. As the results, complex surfaces with varied components are obtained. All the methods are effective in improving the wear resistance of Ti–6Al–4V in different degrees. Among all, the surface modified by the combined method of NaOH solution/HA film gives the best tribological performances. The friction coefficient is also greatly reduced by the modification of NaOH solution. The order of the wear resistance under 3 N is as following: Ti–NaOH–HA>Ti–NaOH>Ti–HA>Ti–H₂O₂–HA>Ti–H₂O₂ >Ti–500; under 1 N is Ti–HA, Ti–NaOH–HA>Ti–NaOH. For Ti–H₂O₂, a very low friction coefficient and long wear life over 2000 passes is obtained under 1 N. SEM observation of the morphologies of worn surfaces indicates that the wear of TC4 is characteristic of abrasive wear. Differently, abrasion, plastic deformation and micro–crack dominate the wear of Ti–HA; slight abrasive wear dominate the wear mechanism of Ti–NaOH and microfracture and abrasive wear for Ti–NaOH–HA and Ti–H₂O₂–HA, while the sample modified by thermal treatment is characterized by sever fracture. The superior friction reduction and wear resistance of HA films are greatly attributed to the slight plastic deformation of the film. NaOH solution is superior in improving the wear resistance and decreasing the friction coefficient under relative higher load (3 N) and H₂O₂ is helpful to reduce friction and wear under relatively lower load (1 N). Combined method of Ti–NaOH–HA is suggested to improve the wear resistance of Ti–6Al–4V for medial applications under fretting situations.     

AC conduction mechanism and battery discharge characteristics of (PVC/PEO) polyblend films complexed with potassium chloride

New K⁺ ion-conducting polymer blend electrolyte films based on amorphous polymer poly(vinyl chloride) (PVC) and semicrystalline polymer poly(ethylene oxide) (PEO) complexed with KCl salt were prepared using a solution-cast technique. The maximum value of ionic conductivity of a PVC/PEO:KCl (42.5:42.5:15) system is 8.29 × 10⁻⁶ S/cm at 303 K. The absorption edge was found at 4.30 eV for undoped film, while it was observed at 4.03 and 3.93 eV for 10 and 15 wt% KCl doped films, respectively. The direct band gaps for these pure and salt doped PVC/PEO films were found to 4.10, 3.86 and 3.74 eV, respectively, whereas the indirect band gaps were determined as 4.15, 3.72 and 3.64 eV. Transference number values showed that the charge transport in this electrolyte system is predominantly due to ions (t_ion = 0.97). The discharge capacity for PVC/PEO:KCl (42.5:42.5:15) polymer blend electrolyte system is 11 μA/h.     

Co-precipitation synthesis of nanocrystalline SnO2: Effect of Fe doping on structural,morphological and ethanol vapor response properties

The present study describes undoped and Fe-doped tin dioxide thick films as selective ethanol vapor sensors. The undoped and Fe doped SnO₂ powders were synthesized by using a facile co-precipitation route. The thick films of undoped and Fe-doped SnO₂ were deposited by screen-printing technique and then sintered at 650 °C for 2 h. The samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX) techniques. The XRD studies reveal formation of nanocrystalline structure. The particle size of undoped and Fe (2 and 4 mol%) doped SnO₂ sintered powders were 17, 10 and 8 nm, respectively. It was found that the response of SnO₂ improved on addition of Fe. The 2 mol% Fe doped SnO₂ exhibits highest response toward ethanol at the operating temperature of 300 °C with response and recovery time of 15 and 32 s, respectively.     

Effect of CuO as a dopant in TiO2 on ammonia and hydrogen sulphide sensing at room temperature

The heterogeneous nanocomposites of CuO doped TiO₂ nanoparticles were synthesized using sol gel method by varying the concentration of CuO as 0.1, 0.5 and 1 mol% for the sensing of ammonia and hydrogen sulphide. The substitutional doping of CuO in TiO₂ matrix was confirmed by the X-ray diffraction. Average crystallite size of the doped nanocomposites was found to reduce with increase in concentration of CuO. The 0.1 mol% CuO doped TiO₂ nanocomposites showed highest sensitivity to ammonia (97%) with response time of 2 s, while 1 mol% was selective to H₂S gas (77%) with response time of 45 s for 50 ppm of each gas at room temperature.     

Tribology characteristics of magnesium alloy AZ31B and its composites

In this paper, wear characteristics of magnesium alloy, AZ31B, and its nano-composites, AZ31B/nano-Al₂O_3, processed by the disintegrated melt deposition technique are investigated. The experiments were carried out using a pin-on-disk configuration against a steel disk counterface under different sliding speeds of 1, 3, 5, 7 and 10 m/s for 10 N normal load, and 1, 3 and 5 m/s for 30 N normal load. The worn samples and wear debris were then examined under a field emission scanning electron microscopy equipped with an energy dispersive spectrometer to reveal its wear features. The wear test results show that the wear rates of the composites are gradually reduced over the sliding speed range for both normal loads. The composite wear rates are higher than that of the alloy at low speeds and lower when sliding speed further increased. The coefficient of friction results of both the alloy and composites are in the range of 0.25–0.45 and reaches minimums at 5 m/s under 10 N and 3 m/s under 30 N load. Microstructural characterization results established different dominant mechanisms at different sliding speeds, namely, abrasion, delamination, oxidation, adhesion and thermal softening and melting. An experimental wear map was then constructed.     

Improving the etching performance of high-aspect-ratio contacts by wafer temperature control: Uniform temperature design and etching rate enhancement

A novel wafer temperature control system using direct expansion cycles is developed to improve etching performance. This system enables rapid temperature control of a wafer with low power consumption. In a previous report, we confirmed that the etching rate and mask selectivity of high-aspect-ratio contact etching could be increased by around 6% and 14%, respectively, by controlling the temperature of the wafer during the etching process. In this study, an advanced wafer temperature control system that realizes not only rapid response but also uniform wafer cooling is developed, and a new etching process that controls O₂ gas flow rate as well as wafer temperature during etching is evaluated to decrease the etching rate depression of high-aspect-ratio contact etching. As a result, a rate of wafer temperature change of 1 °C/s and uniformity of ±0.7% with a coefficient of performance exceeding 3 is achieved over a wafer with a diameter of 300 mm during the etching process. Furthermore, etching rate depression in C₄F₆/Ar/O₂ plasma is decreased from 14.4% to 7.8% for a sample with a diameter of 100 nm and aspect ratio of 30.     

Wear behavior of electroless Ni–P–B4C composite coatings

In this research, the wear of electroless Ni–P and Ni–P–B₄C composite coatings was reviewed. Auto catalytic reduction of Ni in nickel sulfate and sodium hypophosphate bath including suspended B₄C particles with different concentration was used to create composite coatings with 12, 18, 25 and 33 vol.% of B₄C particles. Coatings 35 μm thick were heat treated at 400 °C for one hour in an argon atmosphere and the wear resistance and friction coefficient of heat-treated samples were determined by block-on-ring tests. All wear tests were carried out at 24 °C, 35% moisture, 0.164 m/s sliding speed and about 1000 m sliding distance. Graphs show that an electroless Ni–P–B₄C composite coating with 25 vol.% of B₄C had the best wear resistance against a CK45 steel counterface.     

Wear characteristics of Cr3C2–NiCr and WC–Co coatings deposited by LPG fueled HVOF

Wear behavior of the HVOF deposited Cr₃C₂–NiCr and WC–Co coatings on Fe-base steels were evaluated by the pin-on-disc mechanism. The constant normal load applied to the pin was 49 N and sliding distance was 4500 m with velocity of 1 m/s, at ambient temperature and humidity. The specific wear rate of WC–Co coating was 3 mm³/N m and Cr₃C₂–NiCr coating was 5.3 mm³/N m. SEM/EDAX and XRD techniques were used to analyze the worn out surface and wear debris. The Fe₂O₃ was identified as the major phase in the wear debris. The wear mechanism is mild adhesive wear in nature.     

Mechanical and tribological properties of NiCr–Al2O3 composites at elevated temperatures

The effect of Al₂O₃ content on the mechanical and tribological properties of Ni–Cr alloy was investigated from room temperature to 1000 °C. The results indicated that NiCr–40 wt% Al₂O₃ composite exhibited good wear resistance and its compressive strength remained 540 MPa even at 1000 °C. The values obtained for flexural strength and fracture toughness at room temperature were 771 MPa, 15.2 MPa m^1/2, respectively. Between 800 °C and 1000 °C, the adhesive and plastic oxide layer on the worn surface of the composite was claimed to be responsible for low friction coefficient and wear rate.     

Friction and wear properties of αFeSi2–Si alloy,ReSi1.8 and MoSi2 in ethyl alcohol

In this study, Fe–X at% Si alloy (X=70.5, 80.0 and 96.0), Re–64.3 at% Si and Mo–66.7 at% Si disk specimens were prepared by spark plasma sintering, and their friction and wear properties were investigated when they were slid against Si₃N₄ ball specimens in ethyl alcohol. The friction and wear properties of Si ingots were also examined. Fe–70.5 at% Si, Fe–80.0 at% Si, Fe–96.0 at% Si and Re–64.3 at% Si disk specimens exhibited friction coefficients as low as 0.15. It is considered that the low friction of the Fe–70.5 at% Si, Fe–80.5 at% Si and Fe–96.0 at% Si disk specimens was due to the formation of low friction silicon alkoxide and polyoxysilane on the worn surfaces of the disk specimens and the paired ball specimens. Re–64.3 at% Si disk specimens exhibited the highest microvickers hardness of all the disk specimens prepared in this study. In addition, the microvickers hardness of the Fe–X at% Si (X=70.5, 80.0, 96.0 and 100) disk specimen increased with increasing the Si content. Moreover, it was difficult to obtain dense Fe–90.0 at% Si disk specimens by sintering the annealed and crushed Fe–90.0 at% Si powder. However, dense Fe–96.0 at% Si disk specimens could be obtained by sintering the Fe–90.0 at% Si powder at 1403 K.     

Mechanical and tribological properties of sputtered Mo–Se–C coatings

Transition metal dichalcogenides belong to the more developed class of materials for solid lubrication. However, the main limitation of these materials is the detrimental effect of air humidity causing an increase in the friction. In previous works, molybdenum diselenide has been shown to be a promising coating retaining low friction even in very humid environment. In this study, Mo–Se–C films were deposited by sputtering from a C target with pellets of MoSe₂. Besides the evaluation of the chemical composition, the structure, the morphology, the hardness and the cohesion/adhesion, special attention was paid to the tribological characterization.The C content varied from 29 to 68 at.% which led to a progressive increase of the Se/Mo ratio. As a typical trend, the hardness increases with increasing C content. The coatings were tested at room temperature with different air humidity levels and at temperatures up to 500 °C on a pin-on-disc tribometer. The friction coefficient of Mo–Se–C coatings increased with air humidity from ～0.04 to ～0.12, while it was as low as 0.02 at temperature range 100–250 °C. The coatings were very sensitive to the elevated temperature being worn out at 300 °C due to adhesion problems at coating–titanium interface.     

Cavitation erosion of Fe–Mn–Si–Cr shape memory alloys

Cavitation erosion tests of three Fe–Mn–Si–Cr shape memory alloys were carried out at speed 34 and 45 m/s using a rotating disc rig, and their cavitation damage has been investigated by comparison with a referring 13Cr–5Ni–Mo stainless steel used for hydraulic turbine vanes. The research results proved that the cavitation erosion of the Fe–Mn–Si–Cr shape memory alloys is a failure of low cycle fatigue and fracture propagates along grain boundaries. After 48 h cavitation erosion the cumulative mass losses of the studied alloys at speed 45 m/s are more than theirs at speed 34 m/s; however, the effect of velocity on cavitation damage of the Fe–Mn–Si–Cr alloys is much lower than that of 13Cr–5Ni–Mo stainless steel. The cumulative mass loss of the 13Cr–5Ni–Mo stainless steel are 26.3 mg at speed 45 m/s and 3.2 mg at speed 34 m/s, and the mass losses of the Fe–Mn–Si–Cr alloys are within the range of 3.6–7.3 mg at speed 45 m/s and 2.0–4.1 mg at speed 34 m/s. The surface elasticity of the Fe–Mn–Si–Cr shape memory alloys is better than that of the 13Cr–5Ni–Mo stainless steel, and the effect of surface elasticity on cavitation damage increases with velocity. The excellent surface elasticity of the cavitation-induced hexagonal closed-packed (h.c.p.) martensite plays a key role in contribution of phase transformation to the cavitation erosion resistance of the Fe–Mn–Si–Cr shape memory alloys. The cavitation damage of the studied alloys at speed 45 m/s mainly depends on their surface elasticity, and the variation of 48 h cumulative mass loss (Δm) as a function of the elastic depth (h_e) can be expressed as Δm=2.695+[1371.94/(4(h_e−46.83)²+12.751)] with a correlation factor of 0.99345.     

Tribological characterization of tungsten nitride coatings deposited by reactive magnetron sputtering

The structure, hardness, friction and wear of tungsten nitrides prepared by d.c. reactive magnetron sputtering were investigated. The coatings were deposited with different nitrogen to argon ratios; the total pressure was kept constant. The tribological tests were performed on a pin-on-disc tribometer in terrestrial atmosphere with 100Cr6 steel, Al₂O₃ and Si₃N₄ balls as sliding counter-bodies. The wear tracks, the ball-wear scars and the wear debris were analysed by scanning electron microscopy in order to characterize the dominant wear mechanisms.The coatings exhibited different phases as a function of the nitrogen content: films with low N content exhibited the α-W phase; β-W phase was dominant for nitrogen contents from 12 to 15 at.% and β-W₂N was observed for nitrogen content higher that 30 at.%. The mechanical and tribological properties of the tungsten nitride coatings were strongly influenced by the structure. The hardness and the Young's modulus values were in the ranges (29–39 GPa) and (300–390 GPa), respectively; the lowest values correspond to the coatings with the highest nitrogen content. Generally, the friction and wear rate of tungsten nitride coatings sliding against ceramic balls increased with nitrogen content reaching a maximum at 12 at.%; further increase of the nitrogen content led to a decrease of the friction and wear. The sliding with the steel balls did not wear the coatings under the selected testing conditions.     

Studies on wear behavior of nano-intermetallic reinforced Al-base amorphous/nanocrystalline matrix in situ composite

Resistance to wear is an important factor in design and selection of structural components in relative motion against a mating surface. The present work deals with studies on fretting wear behavior of in situ nano-Al₃Ti reinforced Al–Ti–Si amorphous/nanocrystalline matrix composite, processed by high pressure (8 GPa) sintering at room temperature, 350, 400 or 450 °C. The wear experiments were carried out in gross slip fretting regime to investigate the performance of this composite against Al₂O₃ at ambient temperature (22–25 °C) and humidity (50–55%). The highest resistance to fretting wear has been observed in the composites sintered at 400 °C. The fretting wear involves oxidation of Al₃Ti particles in the composite. A continuous, smooth and protective tribolayer is formed on the worn surface of the composite sintered at 400 °C, while fragmentation and spallation leads to a rougher surface and greater wear in the composite sintered at 450 °C.     

Antimicrobial food packaging prepared from poly(butylene succinate) and zinc oxide

This article reports antibacterial activity, mechanical, thermal and physical properties of poly(butylene succinate) (PBS)/zinc oxide (ZnO) composite films for food packaging applications. The composite films were successfully prepared by using a blown film extruder at five ZnO levels ranging from 2 to 10 wt%. Under tension, PBS was stiffer due to the strengthening effect derived from rigid ZnO particles. However, the tear strength of the composite films was lower than the film without ZnO. Minimum ZnO content required to inhibit the Escherichia coli and the Staphylococcus aureus growths were observed at 6 wt% with the clear zone of 1.31 and 1.25 cm respectively. Thermal test results indicated the increased degree of crystallinity (X_c) and the decreased crystallization temperature (T_c) while the melting temperature (T_m) remain unchanged. Loss modulus curves informed the reduction of the glass transition temperature (T_g) of the film with ZnO at all concentrations. Release test indicated that Zn²⁺ migrated over 15 days studied while the maximum migration was observed when acetic acid was used as a food simulant.     

WC–ZrO2 composites: processing and unlubricated tribological properties

In the present work, we report the processing and properties of WC–6 wt.% ZrO₂ composites, densified using the pressureless sintering route. The densification of the WC–ZrO₂ composites was carried out in the temperature range of 1500–1700 °C with varying time (1–3 h) in vacuum. The experimental results indicate that significantly high hardness of 22–23 GPa and moderate fracture toughness of ∼5 MPa m^1/2 can be obtained with 2 mol% Y-stabilized ZrO₂ sinter-additive, sintered at 1600 °C for 3 h. Furthermore, the friction and wear behavior of optimized WC–ZrO₂ composite is investigated on a fretting mode I wear tester. The tribological results reveal that a moderate coefficient of friction in the range from 0.15 to 0.5 can be achieved with the optimised composite. An important observation is that a transition in friction and wear with load is noted. The dominant mechanisms of material removal appear to be tribochemical wear and spalling of tribolayer.