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.     

Characterization of Zr-Si-N films deposited by cathodic vacuum arc with different N2/SiH4 flow rates

Zr-Si-N films were deposited on silicon and steel substrates by cathodic vacuum arc with different N₂/SiH₄ flow rates. The N₂/SiH₄ flow rates were adjusted at the range from 0 to 12 sccm. The films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), hardness and wear tests. The structure and the mechanical properties of Zr-Si-N films were compared to those of ZrN films. The results of XRD and XPS showed that Zr-Si-N films consisted of ZrN crystallites and SiN_x amorphous phase. With increasing N₂/SiH₄ flow rates, the orientation of Zr-Si-N films became to a mixture of (1 1 1) and (2 0 0). The column width became smaller, and then appeared to vanish with the increase in N₂/SiH₄ flow rates. The hardness and Young's modulus of Zr-Si-N films increased with the N₂/SiH₄ flow rates, reached a maximum value of 36 GPa and 320 GPa at 9 sccm, and then decreased 32 GPa and 305 GPa at 12 sccm, respectively. A low and stable of friction coefficient was obtained for the Zr-Si-N films. Friction coefficient was about 0.1.     

First-principles prediction of the hardness of fluorite TiO2

We present first-principles calculations on the elastic constants, ideal tensile and shear strengths of cubic TiO₂ with a fluorite structure (f-TiO₂). The results show that f-TiO₂ is mechanically stable at the ground-state structure. Both shear modulus and value of hardness predicted indicate that the hardness of f-TiO₂ is comparable with TiN but is lower than TiB₂. The ideal shear strength results suggest that the hardness of f-TiO₂ is reduced because of the lower stress on the shear (1 1 1) 〈1 1¯ 0〉 slip system.     

Structure and properties of (AlCrMnMoNiZrB0.1)Nx coatings prepared by reactive DC sputtering

The microstructure and properties of AlCrMnMoNiZrB_0.1 nitride films prepared by reactive direct current sputtering at various N₂-to-Ar flow ratios (R_N) were investigated. The films had an amorphous structure at low R_N and a face-centered cubic structure at a high R_N. As the R_N increased, the decrease in clusters and defects resulted in a dense columnar structure and low surface roughness. The peak hardness and modulus of the nitride films were 10.3 and 180 GPa, respectively. The enhanced hardness is ascribed to the increased metal-nitrogen bonding, solid solution strengthening of several metallic nitrides, and lattice strain. The nitride films deposited at R_N = 0.2, 0.5, and 0.8 had friction coefficients of 0.16, 0.12 and 0.15, respectively. Wear-out failure occurred within 400 s when R_N = 0 and 1.0. Adhesive wear was the dominant wear mechanism.     

Phase stability,elastic, electronic,thermal and optical properties of Ti3Al1−xSixC2 (0≤x≤1): First principle study

The structural parameters with stability upon Si incorporation and elastic, electronic, thermodynamic and optical properties of Ti₃Al_1−xSi_xC₂ (0≤x≤1) are investigated systematically by the plane wave pseudopotential method based on the density functional theory (DFT). The increase of some elastic parameters with increasing Si-content renders the alloys to possess higher compressive and tensile strength. The Vickers hardness value obtained with the help of Mulliken population analysis increases as x is increased from 0 to 1. The solid solutions considered are all metallic with valence and conduction bands, which have a mainly Ti 3d character, crossing the Fermi level. The temperature and pressure dependences of bulk modulus, normalized volume, specific heats, thermal expansion coefficient, and Debye temperature are all obtained through the quasi-harmonic Debye model with phononic effects for T=0−1000 K and P=0−50 GPa. The obtained results are compared with other results available. Further an analysis of optical functions for two polarization vectors reveals that the reflectivity is high in the visible–ultraviolet region up to ∼10.5 eV region showing promise as a good coating material.     

Structural and mechanical properties of multi-element (TiVCrZrHf)N coatings by reactive magnetron sputtering

In this study, (TiVCrZrHf)N multi-component coatings with quinary metallic elements were deposited by reactive magnetron sputtering system. The composition, structure, and mechanical properties of the coatings deposited at different N₂ flow rates were investigated. The (TiVCrZrHf)N coatings deposited at N₂ flow rates of 0, 1, and 2 SCCM showed an amorphous structure, whereas those deposited at N₂ flow rates of 4 and 6 SCCM showed a simple face-centered cubic solid solution structure. A saturated nitride coating was obtained for N₂ flow of 4 SCCM and higher. By increasing N₂ flow to 4 SCCM, the hardness and modulus reached a maximum value of 23.8 ± 0.8 and 267.3 ± 4.0 GPa, respectively.     

Preparation and wear resistance of pulse electrodeposited Ni-W/Al2O3 composite coatings

The aim of this work is to obtain the electroplating parameters for preparation of Ni-W/Al₂O₃ composite coating with high tungsten content, high micro-hardness and excellent wear resistance by pulse plating procedure. Our results showed that the duty cycle is a dominant parameter for the tungsten content in the coating and the tungsten content increases significantly with increasing duty cycle. The further analysis showed the great influence of tungsten content on micro-hardness of the coating. A maximum micro-hardness of about 859 Hv was obtained in pulse electrodeposited Ni-W/Al₂O₃ composite with tungsten content of 40 wt.% at a peak current density of 20 A/dm², a duty cycle of 80%, a pulse frequency of 1000 Hz and a particle loading of 10 g/L alumina in the plating bath. Although the hardness of Ni-W/Al₂O₃ composite coating was only slightly affected by the alumina content of the deposits prepared in present investigation, the alumina content effect on the tribological characteristic of Ni-W/Al₂O₃ composite coatings is significant. The friction coefficient was lowered to 0.25 and the wear loss was reduced to 1.05 mg by setting the control factors according to the values mentioned above for obtaining the coating with the highest micro-hardness.     

Plasticity and ab initio characterizations on Fe4N produced on the surface of nanocrystallized 18Ni-maraging steel plasma nitrided at lower temperature

18Ni-maraging steel has been entirely nanocrystallized by a series of processes including solution treatment, hot-rolling deformation, cold-drawn deformation and direct electric heating. The plasma nitriding of nanocrystallized 18Ni-maraging steel was carried out at 410 °C for 3 h and 6 h in a mixture gas of 20% N₂ + 80% H₂ with a pressure of 400 Pa. The surface phase constructions and nitrogen concentration profile in surface layer were analyzed using an X-ray diffractometer (XRD) and the glow discharge spectrometry (GDS), respectively. The results show that an about 2 μm thick compound layer (mono-phase γ′-Fe₄N) can be produced on the top of the surface layer of nanocrystallized 18Ni-maraging steel plasma nitrided at 410 °C for 6 h. The measured hardness value of the nitrided surface is 11.6 GPa. More importantly, the γ′-Fe₄N phase has better plasticity, i.e., its plastic deformation energy calculated from the load-displacement curve obtained by nano-indentation tester is close to that of nanocrystallized 18Ni-maraging steel. Additionally, the mechanical properties of γ′-Fe₄N phase were also characterized by first-principles calculations. The calculated results indicate that the hardness value and the ratio of bulk to shear modulus (B/G) of the γ′-Fe₄N phase are 10.15 GPa and 3.12 (>1.75), respectively. This demonstrates that the γ′-Fe₄N phase has higher hardness and better ductility.     

Hydrothermal synthesis and Magnetocaloric effect of La0.5Ca0.3Sr0.2MnO3

The hydrothermal synthesis and magnetic entropy change for the perovskite manganite La_0.5Ca_0.3Sr_0.2MnO₃ have been studied. The La_0.5Ca_0.3Sr_0.2MnO₃ can be produced as phase-pure, crystalline powders in one step from solutions of metal salts in aqueous potassium hydroxide solution at a temperature of 513 K in 72 h. Scanning electron microscopy shows that the materials are made up of cuboid-shaped particles in typical dimension of 4.0×2.5×1.6 μm. Heat treatment can improve the magnetocaloric effect for the hydrothermal sample. The maximum magnetic entropy change ΔS_M for the as-prepared sample is 0.88 J kg⁻¹ K⁻¹ at 315 K for a magnetic field change of 2.0 T. It increases to 1.52 J kg⁻¹ K⁻¹, near its Curie temperature (317 K) by annealing the sample at 1473 K for 6 h. The hydrothermal synthesis method is a feasible route to prepare high-quality perovskite material for magnetic refrigeration application.     

Growth temperature dependence of the hysteretic behavior of Ni0.5Zn0.5Fe2O4 thin films

Herein, a discussion of the effect of deposition temperature on the magnetic behavior of Ni_0.5Zn_0.5Fe₂O₄ thin films. The thin films were grown by r.f. sputtering technique on (1 0 0) MgO single-crystal substrates at deposition temperatures ranging between 400 and 800 °C. The grain boundary microstructure was analyzed via atomic force microscopy (AFM). AFM images show that grain size (φ∼70-112 nm) increases with increasing deposition temperature, according to a diffusion growth model. From magneto-optical Kerr effect (MOKE) measurements at room temperature, coercive fields, H_c, between 37and 131 Oe were measured. The coercive field, H_c, as a function of grain size, reaches a maximum value of 131 Oe for φ ∼93 nm, while the relative saturation magnetization exhibits a minimum value at this grain size. The behaviors observed were interpreted as the existence of a critical size for the transition from single- to multi-domain regime. The saturation magnetization (21 emu/g<M_s<60 emu/g) was employed to quantify the critical magnetic intergranular correlation length (L_c≈166 nm), where a single-grain to coupled-grain behavior transition occurs. Experimental hysteresis loops were fitted by the Jiles-Atherton model (JAM). The value of the k-parameter of the JAM fitted by means of this model (k/μ_o∼50 A m²) was correlated to the domain size from the behavior of k, we observed a maximum in the density of defects for the sample with φ∼93 nm.     

Mechanical and magnetic properties of ZnO/Fe2O3 ceramic varistors

Mechanical and magnetic properties of the ZnO/Fe₂O₃ ceramic varistors have been examined by using mechanical analyzer, digital microhardness tester and vibrating sample magnetometer. The initial stress–strain behavior is found to be linear (elastic) then becomes nonlinear (plastic deformation) without reaching the failure limit up to the maximum available stress (0.07 MPa). The compressive elastic modulus varies between 0.2 and 0.8 MPa with Fe addition up to 0.50. Furthermore, an approximately monotonically linear decrease in VHN with increasing Fe content up to 50% has been observed for all applied loads, which closely resembles the behavior of the true hardness and the surface energy. The magnetic measurements revealed an antiferromagnetic to paramagnetic to transition for all Fe doped samples. The Fe free sample showed paramagnetic behavior down to 2 K. The Neel temperature moderately increased from 18 K at 0.05% Fe to 25 K at 0.5% Fe. The magnetization (M) versus applied magnetic field (H) did not reach saturation for all samples up to 9 Tesla. The saturated magnetization (per Fe contents) is low and found to decreases linearly at a rate of (−35 emu/g-Fe) in a clear manifestation of the strengthening of the antiferromagnetic exchange interaction with increasing Fe contents.     

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.     

NbTi0.5Ni0.5O4 as anode compound material for SOFCs

NbTi_0.5Ni_0.5O₄ (NTNO) has been prepared using solid state synthesis and investigated as a potential anode material. The oxide form of NTNO has single phase rutile-type structure with tetragonal (P42/mnm) space group. The reduced form is a composite of nano-scaled particles of metallic Ni and Nb_1.33Ti_0.67O₄ phase. Reduced NTNO showed high electronic conductivity up to 280 S.cm^− 1 at 900 °C in reducing atmosphere, but suffers from low CTE equal to 3.78 10^− 6 K^− 1. Studies of NTNO as anode material were carried out in a three electrode - electrochemical half cell configuration under pure humidified H₂ at 900 °C using a 2 mm thick zirconia electrolyte and without any additional current collector material. The results show a reasonable series resistance (R_s) equal to 2.7 Ωcm² (about 50% higher than for metallic gold layers) indicating a good current collection performance for a 10 μm layer of material. The polarization resistance (R_p) was equal to 33 Ωcm² and is attributed to a poor density of three phase boundaries (TPB) and shortage of oxide ion conduction in the anode layer. The results show the potential of NTNO as an anode material, especially after optimization of the microstructure towards the increase of TPB length.     

Correlation between structural and mechanical properties of PbTiO3 thin films grown by pulsed-laser deposition

Tetragonal lead titanate (PbTiO₃, PT) thin films are grown on (1 0 0) MgO substrate by pulsed-laser deposition (PLD) for expected applications in integrated optics. The realisation of outstanding and reliable devices into integrated circuits requires sufficient mechanical resistance despite that the obtained PT films display interesting waveguiding properties associated with low optical losses. Two mechanical properties characteristic of elasticity and hardness of PT films are studied. The elastic modulus (E or Young's modulus) and the hardness (H) are measured by the nanoindentation technique. These mechanical properties are correlated to the crystalline quality of PT/MgO thin films. The films show epitaxial relationship with the MgO substrate and the orientation of crystallites perpendicularly to the surface substrate may be the consequence of a growth process along c-axis, a-axis or both. Differences on curves plotting hardness and elastic modulus as a function of indentation depth are observed as the curves are less dispersed for the films mainly c-axis oriented.     

Magnetocaloric effect in La0.67Sr0.33MnO3 manganite above room temperature

The La_0.67Sr_0.33MnO₃ composition prepared by sol-gel synthesis was studied by dc magnetization measurements. A large magnetocaloric effect was inferred over a wide range of temperature around the second-order paramagnetic-ferromagnetic transition. The change of magnetic entropy increases monotonically with increasing magnetic field and reaches the value of 5.15 J/kg K at 370 K for Δμ0H=5 T. The corresponding adiabatic temperature change is 3.3 K. The changes in magnetic entropy and the adiabatic temperature are also significant at moderate magnetic fields. The magnetic field induced change of the specific heat varies with temperature and has maximum variation near the paramagnetic-ferromagnetic transition. The obtained results show that La_0.67Sr_0.33MnO₃ could be considered as a potential candidate for magnetic refrigeration applications above room temperature.     

The effect of P2O5 on the ultra broadband near-infrared luminescence from bismuth-doped SiO2-Al2O3-CaO glass

The effect of P₂O₅ on infrared luminescence properties of bismuth-doped SiO₂-Al₂O₃-CaO (SAC) glass was investigated. Under excitation of 690 and 808 nm LD, two infrared emissions from bismuth ions central at 1100 and 1300 nm were observed, respectively. The addition of P₂O₅ was not only found to lead to the increase of full width at half maximum (FWHM) of two infrared emissions, but also result in intensity variety of the infrared emissions. The intensity of the infrared emission located at 1300 nm is reduced by a factor of 2, while the luminescence at 1110 nm is increased by a factor of 5. We propose that the infrared emissions at 1100 and 1300 nm may originate from different valence Bi ion in glasses. Compared with emission at 1300 nm, the infrared emissions at 1100 nm is more possibly from the transition of lower valent Bi ion.     

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.     

In-situ synchrotron X-ray diffraction study of stress-induced phase transformation in Ti50.1Ni40.8Cu9.1 thin films

Stress-induced martensitic transformation of as-sputtered and post-annealed Ti_50.1Ni_40.8Cu_9.1 thin films was investigated using in-situ synchrotron X-ray diffraction (S-XRD) technique. For the as-deposited film, in-situ S-XRD analysis showed a martensitic transformation from parent phase to martensite during initial loading, followed by reorientation of martensite variants via detwinning. This detwinning process induced a strong 〈0 2 0〉 fiber texture along the loading direction and a strong 〈0 0 2〉 fiber texture perpendicular to the loading direction. For the 650 °C annealed film, there is only elastic deformation, followed by a martensitic transformation during deformation.     

Effect of Pb on the electrical properties of a-Ge20Se80 glasses

The present paper reports the effect of Pb impurity (low ∼2 at% and high ∼10 at%) on the ac conductivity (σ_ac) of a-Ge₂₀Se₈₀ glass. Frequency-dependent ac conductance and capacitance of the samples over a frequency range ∼100 Hz to 50 kHz have been taken in the temperature range ∼268 to 358 K. At frequency 2 kHz and temperature 298 K, the value of σ_ac increases at low as well as at higher concentration of Pb. σ_ac is proportional to ω^s for undoped and doped samples. The value of frequency exponent (s) decreases as the temperature increases. The static permittivity (ε_s) increases at both Pb concentrations. These results have been explained on the basis of some structural changes at low and higher concentration of Pb impurity.     

Growth, microstructure, and mechanical properties related to modulation period for ZrAlN/ZrB2 superlattice coatings

ZrAlN/ZrB₂ multilayered superlattice coatings with modulation periods ranging from 20 nm to 60 nm were grown in magnetron sputtering chamber. X-ray diffraction (XRD), scanning electron microscopy (SEM) and nanoindention were employed to investigate the influence of modulation period on microstructure and mechanical properties of the multilayers. The sharp interfaces and nanoscale multilayered modulation were confirmed by SEM and XRD. The coating with modulation period of 40 nm and modulation ratio of 1:3 showed a marked polycrystalline structure with the strong mixture of ZrAlN (1 1 1), ZrB₂ (0 0 1) and ZrB₂ (1 0 1) textures. Meanwhile, it also possessed the highest hardness (36.4 GPa), elastic modulus (477 GPa), critical fracture load (76.48 mN), and lower residual stress, compared to those with other modulation periods and monolithic coatings.