TiCN/TiNbCN multilayer coatings with enhanced mechanical properties

Enhancement of mechanical properties by using a TiCN/TiNbCN multilayered system with different bilayer periods (Λ) and bilayer numbers (n) via magnetron sputtering technique was studied in this work. The coatings were characterized in terms of structural, chemical, morphological and mechanical properties by X-ray diffraction (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nanoindentation. Results of the X-ray analysis showed reflections associated to FCC (1 1 1) crystal structure for TiCN/TiNbCN films. AFM analysis revealed a reduction of grain size and roughness when the bilayer number is increased and the bilayer period is decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 15 nm (n = 200), yielding the highest hardness (42 GPa) and elastic modulus (408 GPa). The values for the hardness and elastic modulus are 1.6 and 1.3 times greater than the coating with n = 1, respectively. The enhancement effects in multilayer coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain the increase in hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayers taking into account the thickness reduction at individual single layers that make the multilayered system. The Hall-Petch model based on dislocation motion within layers and across layer interfaces, has been successfully applied to multilayers to explain this hardness enhancement.     

Production and characterization of polymer nanocomposite with aligned single wall carbon nanotubes

We reported a simple method to fabricate polymer nanocomposites with single-walled carbon nanotubes (SWNTs) having exceptional alignment and improved mechanical properties. The composite films were fabricated by casting a suspension of single walled carbon nanotubes in a solution of thermoplastic polyurethane and tetrahydrofuran. The orientation as well as dispersion of nanotubes was determined by scanning electron microscopy, transmission electron microscopy and polarized Raman spectroscopy. The macroscopic alignment probably results from solvent-polymer interaction induced orientation of soft segment chain during swelling and moisture curing. The tensile behavior of the aligned nanotube composite film was also studied. At a 0.5 wt.% nanotube loading, a 1.9-fold increase in Young's modulus was achieved.     

Carbon nanotubes as reinforcement of styrene-butadiene rubber

This study reports an easy technique to produce cured styrene-butadiene rubber (SBR)/multi-walled carbon nanotubes (MWCNT) composites with a sulphur/accelerator system at 150 °C. Significant improvement in Young's modulus and tensile strength were achieved by incorporating 0.66 wt% of filler without sacrificing SBR elastomer high elongation at break. A comparison with carbon black filled SBR was also made. Field emission scanning electron microscopy was used to investigate dispersion and fracture surfaces. Results indicated that the homogeneous dispersion of MWCNT throughout SBR matrix and strong interfacial adhesion between oxidized MWCNT and the matrix are responsible for the considerable enhancement of mechanical properties of the composite.     

Characterization of hydrogenated amorphous carbon thin films by end-Hall ion beam deposition

Pure hydrogenated amorphous carbon (α-C:H) and nitrogen doped hydrogenated amorphous carbon (α-C:H:N) thin films were prepared using end-Hall (EH) ion beam deposition with a beam energy ranging from 24 eV to 48 eV. The composition, microstructure and mechanical properties of the films were characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, scanning probe microscopy (SPM), and nano-scratch tests. The films are uniform and smooth with root mean square roughness values of 0.5-0.8 nm for α-C:H and 0.35 nm for α-C:H:N films. When the ion energy was increased from 24 eV to 48 eV, the fraction of sp³ bonding in the α-C:H films increased from 36% to 55%, the hardness increased from 8 GPa to 12.5 GPa, and the Young's modulus increased from 100 GPa to 130 GPa. In the α-C:H:N films, N/C atomic ratio, the hardness and Young's modulus of the α-C:H:N films are, 0.087, 15 and 145 GPa, respectively. The results indicate that both higher ion energy and a small amount of N doping improve the mechanical properties of the films. The results have demonstrated that smooth and uniform α-C:H and α-C:H:N films with large area and reasonably high hardness and Young's modulus can be synthesized by EH ion source.     

Effects of temperature and vacancy defects on tensile deformation of single-walled carbon nanotubes

This study adopts the Tersoff-Brenner interaction potential function in a series of molecular dynamic (MD) simulations which investigate the mechanical properties under tensile loading of (10,0) zigzag, (8,3) chiral and (6,6) armchair single-walled carbon nanotubes (SWCNTs) of similar radii. The Young's modulus values of the (10,0), (8,3) and (6,6) nanotubes are determined to be approximately 0.92, 0.95, and 1.03 TPa, respectively. Of these nanotubes, the results reveal that the (6,6) nanotube possesses the best tensile strength and toughness properties under tension. Although it is noted that under small tensions, the mechanical properties such as Young's modulus are essentially insensitive to helicity, under larger plastic deformations, they may be influenced by helicity effects. Finally, the simulations demonstrate that the values of the majority of the considered mechanical properties decrease with increasing temperature and increasing vacancy percentage.     

Enhancement of surface mechanical properties by using TiN[BCN/BN]n/c-BN multilayer system

The aim of this work is to improve the mechanical properties of AISI 4140 steel substrates by using a TiN[BCN/BN]_n/c-BN multilayer system as a protective coating. TiN[BCN/BN]_n/c-BN multilayered coatings via reactive r.f. magnetron sputtering technique were grown, systematically varying the length period (Λ) and the number of bilayers (n) because one bilayer (n = 1) represents two different layers (t_BCN + t_BN), thus the total thickness of the coating and all other growth parameters were maintained constant. The coatings were characterized by Fourier transform infrared spectroscopy showing bands associated with h-BN bonds and c-BN stretching vibrations centered at 1400 cm⁻¹ and 1100 cm⁻¹, respectively. Coating composition and multilayer modulation were studied via secondary ion mass spectroscopy. Atomic force microscopy analysis revealed a reduction in grain size and roughness when the bilayer number (n) increased and the bilayer period decreased. Finally, enhancement of mechanical properties was determined via nanoindentation measurements. The best behavior was obtained when the bilayer period (Λ) was 80 nm (n = 25), yielding the relative highest hardness (∼30 GPa) and elastic modulus (230 GPa). The values for the hardness and elastic modulus are 1.5 and 1.7 times greater than the coating with n = 1, respectively. The enhancement effects in multilayered coatings could be attributed to different mechanisms for layer formation with nanometric thickness due to the Hall-Petch effect; because this effect, originally used to explain increased hardness with decreasing grain size in bulk polycrystalline metals, has also been used to explain hardness enhancements in multilayered coatings taking into account the thickness reduction at individual single layers that make up the multilayered system. The Hall-Petch model based on dislocation motion within layered and across layer interfaces has been successfully applied to multilayered coatings to explain this hardness enhancement.     

Parametric study of Al and Al2O3 ceramic coatings deposited by air plasma spray onto polymer substrate

Aluminum and ceramic (Al₂O₃) coatings were deposited onto the polymer substrate by air plasma spray (APS) to improve the mechanical properties of the polymer surface. The effect of spray parameters (current and spray distance in this paper) on the phase composition, microstructure and mechanical properties was investigated. Shear adhesion strength between the coatings and the substrates was also examined. The results indicate that the deposition parameters have a significant effect on the phase composition, microstructure and mechanical properties of as-spayed coatings. The maximum shear adhesion strength of the bond coats was 5.21 MPa with the current of 180 A and 190 mm spray distance.     

Nanoindentation on carbon thin films obtained from a C60 ion beam

Raman spectra, atomic force microscope (AFM) images, hardness (H) and Young's modulus (E) measurements were carried out in order to characterize carbon thin films obtained from a C₆₀ ion beam on silicon substrates at different deposition energies (from 100 up to 500 eV). The mechanical properties were studied via the nanoindentation technique. It has been observed by Raman spectroscopy and AFM that the microstructure presents significant changes for films deposited at energies close to 300 eV. However, these remarkable changes have not been noticeable on the mechanical properties: apparently H and E increase with higher deposition energy up to ∼11 and ∼116 GPa, respectively. These values are underestimated if the influence of the film roughness is not taken into account.     

Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.     

Mechanical properties and the evolution of matrix molecules in PTFE upon irradiation with MeV alpha particles

The morphology, chemical composition, and mechanical properties in the surface region of α-irradiated polytetrafluoroethylene (PTFE) have been examined and compared to unirradiated specimens. Samples were irradiated with 5.5 MeV ⁴He²⁺ ions from a tandem accelerator to doses between 1 × 10⁶ and 5 × 10¹⁰ Rad. Static time-of-flight secondary ion mass spectrometry (ToF-SIMS), using a 20 keV C₆₀⁺ source, was employed to probe chemical changes as a function of α dose. Chemical images and high resolution spectra were collected and analyzed to reveal the effects of α particle radiation on the chemical structure. Residual gas analysis (RGA) was utilized to monitor the evolution of volatile species during vacuum irradiation of the samples. Scanning electron microscopy (SEM) was used to observe the morphological variation of samples with increasing α particle dose, and nanoindentation was engaged to determine the hardness and elastic modulus as a function of α dose.The data show that PTFE nominally retains its innate chemical structure and morphology at α doses <10⁹ Rad. At α doses ≥10⁹ Rad the polymer matrix experiences increased chemical degradation and morphological roughening which are accompanied by increased hardness and declining elasticity. At α doses >10¹⁰ Rad the polymer matrix suffers severe chemical degradation and material loss. Chemical degradation is observed in ToF-SIMS by detection of ions that are indicative of fragmentation, unsaturation, and functionalization of molecules in the PTFE matrix. The mass spectra also expose the subtle trends of crosslinking within the α-irradiated polymer matrix. ToF-SIMS images support the assertion that chemical degradation is the result of α particle irradiation and show morphological roughening of the sample with increased α dose. High resolution SEM images more clearly illustrate the morphological roughening and the mass loss that accompanies high doses of α particles. RGA confirms the supposition that the outcome of chemical degradation in the PTFE matrix with continuing irradiation is evolution of volatile species resulting in morphological roughening and mass loss. Finally, we reveal and discuss relationships between chemical structure and mechanical properties such as hardness and elastic modulus.     

Effect of Young's modulus evolution on residual stress measurement of thermal barrier coatings by X-ray diffraction

Subjected to thermal cycling, the apparent Young's modulus of air plasma-sprayed (APS) 8 wt.% Y₂O₃-stabilized ZrO₂ (8YSZ) thermal barrier coatings (TBCs) was measured by nanoindentation. Owing to the effects of sintering and porous microstructure, the apparent Young's modulus follows a Weibull distribution and changes from 50 to 93 GPa with an increase of thermal cycling. The evolution of residual stresses in the top coating of an 8YSZ TBC system was determined by X-ray diffraction (XRD). The residual stresses derived from the XRD data are well consistent with that obtained by the Vickers indention. It is shown that the evolution of Young's modulus plays an important role in improving the measurement precision of residual stresses in TBCs by XRD.     

Effect of spraying power on the microstructure and mechanical properties of supersonic plasma-sprayed Ni-based alloy coatings

The aim of this paper was to investigate the microstructure and mechanical properties of the supersonic plasma-sprayed Ni-Cr-B-Si-C coatings prepared at different spraying powers. The microstructure, phase composition, porosity, Young's modulus, micro-hardness, and residual stresses of the coatings were investigated and determined. The variations of the porosity, Young's modulus and micro-hardness of the coatings were evaluated by using statistical method. Results showed that the variations of porosity, Young's modulus and micro-hardness of the coatings followed the Weibull distributions. With increasing the porosity, the micro-hardness and Young's modulus of the coating decreased. The mean value of the Young's modulus of the coating calculated from Weibull plot was almost proportional to the square root of the micro-hardness of the coating. With increasing the power, Young's modulus of the coating increased, which, in turn, resulted in the increment of the residual stress at the coating surface.     

Microstructure and mechanical properties of reactive magnetron sputtered Ti-B-C-N nanocomposite coatings

Ti-B-C-N nanocomposite coatings with different C contents were deposited on Si (1 0 0) and high speed steel (W18Cr4V) substrates by closed-field unbalanced reactive magnetron sputtering in the mixture of argon, nitrogen and acetylene gases. These films were subsequently characterized ex situ in terms of their microstructures by X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM), their nanohardness/elastic modulus and facture toughness by nano-indention and Vickers indentation methods, and their surface morphology using atomic force microscopy (AFM). The results indicated that, in the studied composition range, the deposited Ti-B-C-N coatings exhibit nanocomposite based on TiN nanocrystallites. When the C₂H₂ flow rate is small, incorporation of small amount of C promoted crystallization of Ti-B-C-N nanocomposite coatings, which resulted in increase of nano-grain size and mechanical properties of coatings. A maximum grain size of about 8 nm was found at a C₂H₂ flux rate of 1 sccm. However, the hardness, elastic modulus and fracture toughness values were not consistent with the grain size. They got to their maximum of 35.7 GPa, 363.1 GPa and 2.46 MPa m^1/2, respectively, at a C₂H₂ flow rate of 2 sccm (corresponding to about 6 nm in nano-grain size). Further increase of C content dramatically decreased not only grain size but also the mechanical properties of coatings. The presently deposited Ti-B-C-N coatings had a smooth surface. The roughness value was consistent with that of grain size.     

Berkovich nanoindentation and deformation mechanisms in GaN thin films

The deformation mechanisms of GaN thin films obtained by metal-organic chemical vapor deposition (MOCVD) method were studied using nanoindentation with a Berkovich diamond indenter, micro-Raman spectroscopy and the cross-sectional transmission electron microscopy (XTEM) techniques. Due to the sharpness of the tip of Berkovich indenter, the nanoindentation-induced deformation behaviors can be investigated at relatively lower load and, hence, may cover wider range of deformation-related phenomena over the same loading range. The load-displacement curves show the multiple “pop-ins” during nanoindentation loading. No evidence of nanoindentation-induced phase transformation and cracking patterns were found up to the maximum load of 300 mN, as revealed from the micro-Raman spectra and the scanning electron microscopy (SEM) observations within the mechanically deformed regions. In addition, XTEM observation performed near the cross-section of the indented area revealed that the primary deformation mechanism in GaN thin film is via propagation of dislocations on both basal and pyramidal planes. The continuous stiffness measurement (CSM) technique was used to determine the hardness and Young's modulus of GaN thin films. In addition, analysis of the load-displacement data reveals that the values of hardness and Young's modulus of GaN thin films are 19 ± 1 and 286 ± 25 GPa, respectively.     

Microstructure and mechanical properties of alumina coatings prepared by double glow plasma technique

Low-temperature growth (600 °C) of α-Al₂O₃ coatings on the stainless steel substrate by double glow plasma technique was achieved. The compositions and microstructures of the coatings prepared at different oxygen flow rates were characterized, respectively, by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectrometry. A phenomenological mechanism for the formation of the Al₂O₃ ceramic coatings during the oxidation process was proposed on the basis of the experimental results. It was obvious that the oxygen flow rates had a great effect on the surface structure of the prepared Al₂O₃ coatings. The dense and smooth Al₂O₃ coatings were prepared at the oxygen flow rate of 15 sccm. In addition, the correlations between the mechanical properties of Al₂O₃ coating and oxygen flow rates were also discussed. The coating prepared at 15 sccm oxygen flow rate exhibited the best mechanical properties with a maximum hardness of 31 GPa and elastic modulus of 321 GPa. The corresponding critical load of scratch adherence for this sample was 47 N.     

Use of the mark-tracking method for optical fiber characterization

The mark-tracking method was used in the uniaxial tensile test to determine the elastic properties of optical fibers. The mark-tracking method is based on the follow-up of two markers on the specimen with the help of an image processing technique. It allows us to determine the true strain with respect to the small strains assumption (≤1%) or the finite strains (>1%) without any impact of the rigid solid movement or pulley fiber sliding on the measured strain. Both coated optical fiber and stripped fiber were subjected to the uniaxial tensile test and the cantilever beam bending test. The Young’ modulus results of the stripped fiber were found to be very similar for both tests. Thus, the mark-tracking method is adaptable to the tensile test of optical fibers and the elastic behaviors of both coated optical fiber and stripped fiber are found to be non-linear. Their Young's moduli are 22 and 79 GPa, respectively. These results revealed that those coatings play a mechanical role in fiber elongation.     

Microwave-absorbing and mechanical properties of carbonyl-iron/epoxy-silicone resin coatings

Coatings with flake carbonyl-iron particles as absorber and epoxy-silicone resins as matrix were prepared. The complex permittivity, complex permeability and microwave-absorbing properties were investigated in the frequency range of 2-18 GHz. Both the real part of permittivity and permeability were increased with carbonyl-iron weight concentration. The minimum reflection loss shifts to the low-frequency region with increase in carbonyl-iron weight concentrations. The minimum reflection loss value of −42.5 dB was obtained at 10.6 GHz for the coatings with 55 wt% carbonyl-iron. The values of adhesive power and impact strength are up to 24 MPa and 50 kg cm, respectively. These results show that the coatings possess good microwave-absorbing and mechanical properties.     

Structure and mechanical properties of Al/AlN multilayer with different AlN layer thickness

Nanometer scale Al/AlN multilayers have been prepared by dc magnetron sputtering technique with a columnar target. A set of Al/AlN multilayers with the Al layer thickness of 2.9 nm and the AlN layer thickness variation from 1.13 to 6.81 nm were determined. Low angle X-ray diffraction (LAXRD) was used to analyze the layered structure of multilayers. The phase structure of the coatings was investigated with grazing angle XRD (GAXRD). Mechanical properties of these multilayers were thoroughly studied using a nanoindentation and ball-on-disk micro-tribometer. It was found that the multilayer hardness and reduced modulus showed no strong dependence on the AlN layer thickness. Al2.9 nm/AlN1.13 nm multilayer had more excellent tribological properties than single layers and other proportion multilayers with a lowest friction coefficient of 0.15. And the tribological properties of all the multilayers are superior to the AlN single layer.     

Structural and mechanical characteristics of (1 0 3) AlN thin films prepared by radio frequency magnetron sputtering

The (1 0 3)-oriented aluminum nitride (AlN) thin film is an attractive piezoelectric material for the applications in surface acoustic wave and film bulk acoustic wave resonator devices. In this work, we repot structural and mechanical characteristics of (1 0 3) AlN thin films deposited onto (1 0 0) Si substrates with radio frequency magnetron sputtering at different sputtering powers at 150, 250, and 350 W. Comparisons were made on their crystalline structures with X-ray diffraction, surface morphologies with atomic force microscopy, mechanical properties with nanoindentation, and tribological responses with nanoscratch. Results indicate that for the sputtering power of 350 W, a high-quality (1 0 3) AlN thin film, whose hardness is 18.91 ± 1.03 GPa and Young's modulus is 242.26 ± 8.92 GPa, was obtained with the most compact surface condition.     

Nanomechanical characteristics of SnO2:F thin films deposited by chemical vapor deposition

The nanoindentation characterizations and mechanical properties of fluorine-doped tin oxide (SnO₂:F) films deposited on glass substrates, using chemical vapor deposition (CVD) method, were studied, which included the effects of the indentation loads, the loading time and the hold time on the thin film. The surface roughness, fractal dimension and frictional coefficient were also studied by varying the freon flow rates. X-ray diffraction (XRD), atomic force microscopy (AFM) and frictional force microscopy (FFM) were used to analyze the morphology of the microstructure. The results showed that crystalline structure of the film had a high intensity (1 1 0) peak orientation, especially at a low freon flow rate. According to the nanoindentation records, the Young's modulus ranged from 62.4 to 75.1 GPa and the hardness ranged from 5.1 to 9.9 GPa at a freon flow rate of 8000 sccm. The changes in measured properties were due to changing loading rate.