Search Results (43)

A series of PTT-b-PTMG copolyesters was synthesized via direct esterification followed by melt polycondensation using purified terephthalic acid (PTA), bio-based 1,3-propanediol (PDO), and poly(tetramethylene glycol) (PTMG) of varying molecular weights (650–3000 g/mol). The resulting materials were comprehensively characterized in terms of chemical structure, molecular weight, thermal behavior, phase morphology, crystalline architecture, and mechanical performance using a range of analytical techniques: Fourier-transform infrared spectroscopy (FTIR), ¹H-NMR, gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), dynamic mechanical thermal analysis (DMA), tensile testing, and other standard physical methods. FTIR, ¹H-NMR, and GPC data confirmed the successful incorporation of both PTT-hard and PTMG-soft segments into the copolymer backbone. As the PTMG molecular weight increased, the average sequence length of the PTT-hard segments (L_n,T) also increased, leading to higher melting (T_m) and crystallization (T_c) temperatures, albeit with a slight reduction in overall crystallinity. DMA results indicated enhanced microphase separation between hard and soft domains with increasing PTMG molecular weight. WAXS and SAXS analyses further revealed that the crystalline structure and long-range ordering were strongly dependent on the copolymer composition and block architecture. Mechanical testing showed that tensile strength at break remained relatively constant across the series, while Young’s modulus increased significantly with higher PTMG molecular weight—concurrently accompanied by a decrease in elongation at break. Furthermore, the elastic deformability and recovery behavior of PTT-b-PTMG block copolymers were evaluated through cyclic tensile testing. TGA confirmed that all copolyesters exhibited excellent thermal stability. This study demonstrates that the physical and mechanical properties of bio-based PTT-b-PTMG elastomers can be effectively tailored by adjusting the molecular weight of the PTMG-soft segment, offering valuable insights for the rational design of sustainable thermoplastic elastomers with tunable performance. Full article

This study investigates the thermosalient effect in oxitropium bromide, with a focus on the role of anisotropic thermal expansion, elastic properties, and sound propagation in driving this phenomenon. Variable-temperature X-ray powder diffraction (VTXRPD) revealed significant anisotropic thermal expansion, including negative thermal expansion (NTE) along the c-axis in the low-temperature Form A. Density functional theory (DFT) calculations were used to analyze elastic properties of oxitropium bromide and confirmed that it does not exhibit negative compressibility, emphasizing thermal anisotropy as the primary factor in the phase transition. Studies of elastic constants and sound propagation demonstrated a preferred pathway for energy transfer along the z-direction, enabling rapid strain release during the phase transition. These findings confirmed that the thermosalient effect arises from cooperative molecular motion, resulting in an abrupt and energetic transformation driven by the interplay of structural anisotropy and elastic properties. Full article

High-strength bolts are prone to crack initiation from the threaded hole during fastening due to large loads, which can compromise their performance and reliability. To enhance the durability of these bolts, coatings are often employed to strengthen their surfaces. NbMoTaW refractory high-entropy alloy coatings are widely used in hard coating applications due to their exceptional mechanical properties. However, the brittleness of this alloy at room temperature limits its performance in high-stress environments. To enhance the ductility of NbMoTaW alloys, this study systematically investigates the effect of varying titanium (Ti) content on the alloy’s properties. First-principles calculations were employed to analyze the elastic properties of TixNbMoTaW alloys, including elastic constants, the elastic modulus, the bulk modulus (B)-to-shear modulus (G) ratio (Pugh’s ratio), Poisson’s ratio (ν), and Cauchy pressure (C12–C44). The results indicate that the addition of Ti significantly improves the alloy’s plasticity. Specifically, when the Ti content is x = 2, the B/G ratio increases to 3.23, and Poisson’s ratio increases to 0.39, indicating enhanced deformability. At x = 0.75, the elastic modulus (E) increases to 273.78 GPa, compared to 244.99 GPa for the original alloy. The experimental results further validate the computational findings. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses indicate that all alloys exhibit a single body-centered cubic (BCC) phase. Room-temperature compression tests show that as the Ti content increases, the yield strength, fracture strength, and plasticity of the alloys significantly improve. Specifically, for a Ti content of x = 0.75, the yield strength reaches 1551 MPa, the fracture strength is 1856 MPa, and the plastic strain increases to 14.6%. For Ti1.5NbMoTaW, the yield strength is 1506 MPa, the fracture strength is 1893 MPa, and the plastic strain is 17.3%. Overall, TixNbMoTaW refractory high-entropy alloys demonstrate significant improvements in both plasticity and strength, showing great potential for coating applications in high-stress environments. Full article

Carbon nanomaterials, particularly carbon nanotubes (CNTs), are widely used as reinforcing fillers in rubber composites for advanced mechanical and electrical applications. However, the influence of rubber functionality and its interactions with CNTs remains underexplored. This study investigates electroactive elastomeric composites fabricated with CNTs in two common diene rubbers: natural rubber (NR) and acrylonitrile-butadiene rubber (NBR), each with distinct functionalities. For NR-based composites containing 2 vol% CNTs, mechanical properties, such as elastic modulus (2.24 MPa), tensile strength (12.48 MPa), and fracture toughness (26.92 MJ/m³), show significant improvements of 125%, 215%, and 164%, respectively, compared to unfilled rubber. Similarly, for NBR-based composites, the elastic modulus (5.46 MPa), tensile strength (13.47 MPa), and fracture toughness (82.89 MJ/m³) increase by 94%, 22%, and 65%, respectively, over the unfilled system. Although NBR-based composites exhibit higher mechanical properties, NR systems show more significant improvements, suggesting stronger chemical bonding between NR chains and CNTs, as evidenced by dynamic mechanical, X-ray diffraction, thermogravimetric, and thermodynamic analyses. The NBR-based composite at 1 vol% CNT content exhibits 261% higher piezoresistive strain sensitivity (GF = 65 at 0% ≤ Δε ≤ 200%) compared to the NR-based composite (GF = 18 at 0% ≤ Δε ≤ 200%). The highest gauge factor of 39,125 (1000% ≤ Δε ≤ 1220) was achieved in NBR-based composites with 1 vol% CNT content. However, 1.5 vol% CNT content in NBR provides better strain sensitivity and linearity than other composites. Additionally, NBR demonstrates superior electromechanical actuation properties, with 1317% higher actuation displacement and 276% higher electromechanical pressure compared to NR at an applied electric field of 12 kV. Due to the stronger chemical bonding between the rubber and CNT, NR-based composites are more suitable for dynamic mechanical applications. In contrast, NBR-based CNT composites are ideal for stretchable electromechanical sensors and actuators, owing to the high dielectric constant and polarizable functional groups in NBR. Full article

This study investigates the impact of zirconium substitution on the structural, elastic and magnetic properties of CoCr₂O₄ nanoparticles. A series of CoCr_2−xZr_xO₄ nanoparticles, x = 0.00, 0.05, 0.10, 0.15 and 0.20, are synthesized via the co-precipitation method. X-ray diffraction (XRD) patterns affirm the formation of single-phase cubic structure with the space group Fd3m. Special attention is given to accurately calculating the average crystallite size (D) and lattice parameter (a) using Williamson–Hall (W–H) analysis and the Nelson–Riley (N–R) extrapolation function, respectively. The increase in Zr⁴⁺ content leads to a reduction in crystallite size and an increase in the lattice parameter. Elastic properties are estimated from force constants and the lattice constant, determined from FTIR and XRD, respectively. The observed changes in the elastic constants are attributed to the strength of interatomic bonding. The stiffness constants decrease, while Poisson’s ratio increases with increasing Zr⁴⁺ content, reflecting the increase in the ductility of the prepared samples. As the Zr⁴⁺ content increases, the stiffness constants decrease, and Poisson’s ratio increases, reflecting enhanced ductility of the samples. Furthermore, as Zr⁴⁺ content rises, Young’s modulus, the rigidity modulus and Debye temperature decrease. The magnetic hysteresis loop measurements are carried out at room temperature using a vibrating sample magnetometer (VSM) over a field range of 25 kg. Unsubstituted CoCr₂O₄ exhibits ferrimagnetic behavior. As Zr⁴⁺ content increases, saturation magnetization (M_s) and magnetic moment decrease, while remanent magnetization (M_r) and coercivity (H_c) initially decrease up to x = 0.10, then increase with further increases in x. The novel key of this study is how Zr⁴⁺ substitution in CoCr₂O₄ nanoparticles can effectively modify their elastic moduli and magnetic properties, making them suitable for various applications such as flexible electronics, protective coatings, energy storage components and biomedical implants. Full article

Multi-principal element alloys (MPEAs) are at the forefront of materials science due to their large variety of compositions, which can yield unexplored properties. Mapping the structure and properties of a compositional MPEA library in a reasonable time can be performed with the help of gradient samples. This type of specimens has already been produced in both bulk and layer forms. However, combinatorial MPEA coatings have not been synthesized by electroplating, although this method has a great potential to deposit a coating on components with complex shapes. In this study, a combinatorial Co-Fe-Ni-Zn coating with the thickness of 4 μm was synthesized by electrodeposition. The material exhibited a well-defined Zn gradient; therefore, the investigation of the effect of Zn concentration on the microstructure and mechanical properties was feasible without the production of an excessively large number of specimens. The Zn concentration was controlled laterally through mass transfer due to the unique geometry of the substrate, and it covered a concentration range of 18–44 at%. The chemical and phase compositions as well as the morphology of the as-processed samples were investigated in multiple locations using X-ray diffraction and scanning electron microscopy. The mechanical performance was characterized by nanoindentation. It was found that for any composition, the structure is face-centered cubic and the lattice constant scaled with the Zn concentration of the deposit. The hardness and the elastic modulus were consistent with values of about 4.5 and 130 GPa, respectively, in the Zn concentration range of 25–44 at%. Full article

Hybrid organic-inorganic lead halide perovskites (LHPs) have emerged as a highly significant class of materials due to their tunable and adaptable properties, which make them suitable for a wide range of applications. One of the strategies for tuning and optimizing LHP-based devices is the substitution of cations and/or anions in LHPs. The impact of Cs substitution at the A site on the structural, vibrational, and elastic properties of MA_xCs_1−xPbCl₃-mixed single crystals was investigated using X-ray diffraction (XRD) and Raman and Brillouin light scattering techniques. The XRD results confirmed the successful synthesis of impurity-free single crystals, which exhibited a phase coexistence of dominant cubic and minor orthorhombic symmetries. Raman spectroscopy was used to analyze the vibrational modes associated with the PbCl₆ octahedra and the A-site cation movements, thereby revealing the influence of cesium incorporation on the lattice dynamics. Brillouin spectroscopy was employed to investigate the changes in elastic properties resulting from the Cs substitution. The incorporation of Cs cations induced lattice distortions within the inorganic framework, disrupting the hydrogen bonding between the MA cations and PbCl₆ octahedra, which in turn affected the elastic constants and the sound velocities. The substitution of the MA cations with smaller Cs cations resulted in a stiffer lattice structure, with the two elastic constants increasing up to a Cs content of 30%. The current findings facilitate a fundamental understanding of mixed lead chloride perovskite materials, providing valuable insights into their structural and vibrational properties. Full article

We have investigated lattice disordering of cupper oxide (Cu₂O) and copper nitride (Cu₃N) films induced by high- and low-energy ion impact, knowing that the effects of electronic excitation and elastic collision play roles by these ions, respectively. For high-energy ion impact, degradation of X-ray diffraction (XRD) intensity per ion fluence or lattice disordering cross-section (Y_XD) fits to the power-law: Y_XD = (B_XDS_e)^NXD, with S_e and B_XD being the electronic stopping power and a constant. For Cu₂O and Cu₃N, N_XD is obtained to be 2.42 and 1.75, and B_XD is 0.223 and 0.54 (kev/nm)⁻¹. It appears that for low-energy ion impact, Y_XD is nearly proportional to the nuclear stopping power (S_n). The efficiency of energy deposition, Y_XD/S_e, as well as Y_sp/S_e, is compared with Y_XD/S_n, as well as Y_sp/S_n. The efficiency ratio R_XD = (Y_XD/S_e)/(Y_XD/S_n) is evaluated to be ~0.1 and ~0.2 at S_e = 15 keV/nm for Cu₂O and Cu₃N, meaning that the efficiency of electronic energy deposition is smaller than that of nuclear energy deposition. R_sp = (Y_sp/S_e)/(Y_sp/S_n) is evaluated to be 0.46 for Cu₂O and 0.7 for Cu₃N at S_e = 15 keV/nm. Full article

Using microcrystalline cellulose (MCC) with plastic behaviour and calcium phosphate anhydrous (CaHPO₄) with brittle behaviour under compaction is very popular in the pharmaceutical industry for achieving desirable structural–mechanical properties of tablet formulations. Thus, mixtures of specific grades of MCC and CaHPO₄ were tested in volume proportions of 100-0, 75-25, 50-50, 25-75, and 0-100 at a constant weight-by-weight concentration of sodium stearyl fumarate lubricant, utilizing a state-of-the-art benchtop compaction simulator (STYL’One Nano). Tablet formulations were prepared at 100, 150, 250, 350, 450, and 500 MPa, and characterized by tabletability profile, ejection force profile, proportion–tensile strength relationship, proportion–porosity relationship, pressure–displacement, and elastic recovery profiles, as well as by in-/out-of-die Heckel plots and yield pressures. Interestingly, the 25-75 formulation demonstrated a two-stage out-of-die Heckel plot and was additionally investigated with X-ray micro-computed tomography (µCT). By post-processing the µCT data, the degree of brittle CaHPO₄ particles falling apart, along with the increasing compression pressure, was quantified by means of the surface area to volume (S/V) ratio. For the 25-75 formulation, the first stage (up to 150 MPa) and second stage (above the 150 MPa) of the out-of-die Heckel plot could be attributed to predominant MCC and CaHPO₄ deformation, respectively. Full article

The $\sin ²\psi$ method is the general method for analyzing X-ray diffraction stress measurements. This method relies on the estimation of a parameter known as $\frac{1}{2}{S}_2^{hkl}$, which is generally considered as a material constant. However, various studies have shown that this parameter can be affected by plastic deformation leading to proportional uncertainties in the estimation of stresses. In this paper, in situ X-ray diffraction measurements are performed during a tensile test with unloads on a low-carbon high-strength steel. The calibrated $\frac{1}{2}{S}_2^{hkl}$ parameter varies from $3.5\times {10}^{-6}$ MPa⁻¹ to $5.5 {\times 10}^{-6}$ Mpa⁻¹, depending on the surface condition and on the plastic strain state, leading to a maximum error on the stress level of 40% compared to reference handbook values. The results also show that plastic strain is responsible for 6 to 14% of the variation, depending on the initial surface sample condition. A method is then proposed to correct this variation based on the fit of the $\frac{1}{2}{S}_2^{hkl}$ evolution with respect to the peak diffraction width, the latter being an indication of the plasticity state. It is shown that the proposed methodology improves the applied stress increment prediction, although the absolute stress value still depends on pseudo-macrostresses that also vary with plastic strain. Full article

Utilizing reactive DC magnetron sputtering method, TiN coatings were deposited on the silicon substrates at different nitrogen flows and powers. A study of the X-ray phase composition of the coatings was carried out. The stoichiometric composition of the coatings was determined using energy dispersive x-ray spectroscopy. The structure of the surface, cross-section, and thickness of the coatings were determined using scanning electron (SEM) and atomic force microscopy (AFM). A significant change in the surface structure of TiN coatings was established with changes in deposition power and nitrogen flow. SEM images of cross-sections of all coated samples showed that the formation of coatings occurs in the form of a columnar structure with a perpendicular orientation relative to the silicon substrate. The mechanical properties (elastic modulus E and microhardness H) of TiN coatings of the first group demonstrate a maximum at a nitrogen flow of 3 sccm and are 184 ± 11 GPa and 15.7 ± 1.3 GPa, respectively. In the second group, the values of E and H increase due to a decrease in the size of the structural elements of the coating (grains and crystallites). In the third group, E and H decrease. Microtribological tests were carried out in 4 stages: at a constant load, multi-cycle for 10 and 100 cycles, and with increasing load. The coefficient of friction (CoF) and specific volumetric wear ω depend on the roughness, topology, and mechanical properties of the resulting coatings. Fracture toughness was determined using nanoscratch and depends on the mechanical properties of TiN coatings. Within each group, coatings with the best mechanical and microtribological properties were described: in the first group—TiN coating at 3 sccm (with (29.6 ± 0.1) at.% N), in the second group—TiN coating at 2 sccm (with (40.8 ± 0.2) at.% N), and in the third group—TiN coating at 1 sccm (c (37.3 ± 0.2) at.% N). Full article

In recent years, there have been intense studies on hybrid organic–inorganic compounds (HOIPs) due to their tunable and adaptable features. This present study reports the vibrational, structural, and elastic properties of mixed halide single crystals of MA_xFA_1-xPbCl₃ at room temperature by introducing the FA cation at the A-site of the perovskite crystal structure. Powder X-ray diffraction analysis confirmed that its cubic crystal symmetry is similar to that of MAPbCl₃ and FAPbCl₃ with no secondary phases, indicating a successful synthesis of the MA_xFA_1-xPbCl₃ mixed halide single crystals. Structural analysis confirmed that the FA substitution increases the lattice constant with increasing FA concentration. Raman spectroscopy provided insight into the vibrational modes, revealing the successful incorporation of the FA cation into the system. Brillouin spectroscopy was used to investigate the changes in the elastic properties induced via the FA substitution. A monotonic decrease in the sound velocity and the elastic constant suggests that the incorporation of large FA cations causes distortion within the inorganic framework, altering bond lengths and angles and ultimately resulting in decreased elastic constants. An analysis of the absorption coefficient revealed lower attenuation coefficients as the FA content increased, indicating reduced damping effects and internal friction. The current findings can facilitate the fundamental understanding of mixed lead chloride perovskite materials and pave the way for future investigations to exploit the unique properties of mixed halide perovskites for advanced optoelectronic applications. Full article

As semiconductor chips have been integrated to enhance their performance, a low-dielectric-constant material, SiCOH, with a relative dielectric constant k ≤ 3.5 has been widely used as an intermetal dielectric (IMD) material in multilevel interconnects to reduce the resistance-capacitance delay. Plasma-polymerized tetrakis(trimethylsilyoxy)silane (ppTTMSS) films were created using capacitively coupled plasma-enhanced chemical vapor deposition with deposition plasma powers ranging from 20 to 60 W and then etched in CF₄/O₂ plasma using reactive ion etching. No significant changes were observed in the Fourier-transform infrared spectroscopy (FTIR) spectra of the ppTTMSS films after etching. The refractive index and dielectric constant were also maintained. As the deposition plasma power increased, the hardness and elastic modulus increased with increasing ppTTMSS film density. The X-ray photoelectron spectroscopy (XPS) spectra analysis showed that the oxygen concentration increased but the carbon concentration decreased after etching owing to the reaction between the plasma and film surface. With an increase in the deposition plasma power, the hardness and elastic modulus increased from 1.06 to 8.56 GPa and from 6.16 to 52.45 GPa. This result satisfies the hardness and elastic modulus exceeding 0.7 and 5.0 GPa, which are required for the chemical–mechanical polishing process in semiconductor multilevel interconnects. Furthermore, all leakage-current densities of the as-deposited and etched ppTTMSS films were measured below 10⁻⁶ A/cm² at 1 MV/cm, which is generally acceptable for IMD materials. Full article

In this study, non-stoichiometry lead-free piezoelectric ceramic Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT) thick films were deposited on Pt/Ti/Si substrates using spin-coating method technology to form a LKNNT/Pt/Ti/Si structure of the micro-pressure thick films. Additionally, the influence on the crystalline properties, surface microstructure images, and mechanical properties, and the piezoelectric properties of the non-stoichiometry lead-free piezoelectric ceramic Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT) thick films were observed, analyzed, and calculated using X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), focused ion beam (FIB) microscopy, nano-indention technology, and other instruments. This study was divided into two parts: The first part was the investigation into the fabrication parameters and properties of the bottom layer (Pt) and buffer layer (Ti). The Pt/Ti/Si structures were achieved by the DC sputtering method, and then the rapid thermal annealing (RTA) post-treatment process was used to re-arrange the grains and reduce defects in the lead-free Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT) thick films. In the second part, lead-free Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT) powder was prepared by the solid-state reaction method, and then acetic acid (C₂H₄O₂) solvent was added to form a slurry for spin-coating technology processing. The fabrication parameters, thick film micro-structure, crystalline properties, nano-indention technology, and the piezoelectric coefficient characteristics of the developed lead-free Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT)/Pt/Ti/Si structure of the micro-pressure thick film devices a were investigated. According to the experimental results, the optimal fabrication processing parameters of the lead-free Li_0.058(K_0.48Na_0.535)_0.966(Nb_0.9Ta_0.1)O₃ (LKNNT) were an RTA temperature of 500 °C, a Ti buffer-layer thickness of 273.9 nm, a Pt bottom electrode-layer thickness of 376.6 nm, a theoretical density of LKNNT of 4.789 g/cm³, a lattice constant of 3.968 × 10⁻⁸ cm, and a d₃₃ value of 150 pm/V. Finally, regarding the mechanical properties of the micro-pressure devices for when a microforce of 3 mN was applied, the thick film revealed a hardness of 60 MPa, a Young’s modulus of 13 GPa, and an elasticity interval of 1.25 μm, which are suitable for future applications of micro-pressure devices. Full article

We have studied the behaviour of the cubic spinel structure of FeV₂O₄ under high-pressure by means of powder X-ray diffraction measurements and density-functional theory calculations. The sample was characterized at ambient conditions by energy-dispersive X-ray spectroscopy, Raman spectroscopy, and X-ray diffraction experiments. One of the main findings of this work is that spinel FeV₂O₄ exhibits pressure-induced chemical decomposition into V₂O₃ and FeO around 12 GPa. Upon pressure release, the pressure-induced chemical decomposition appears to be partially reversible. Additionally, in combination with density-functional theory calculations, we have calculated the pressure dependence of the unit-cell volumes of both the spinel and orthorhombic FeV₂O₄ crystal structures, whose bulk moduli are B₀ = 123(9) and 154(2) GPa, respectively, finding the spinel FeV₂O₄ to exhibit the lowest bulk modulus amongst the spinel oxides. From experimental results, the same information is herein obtained for the cubic structure only. The Raman modes and elastic constants of spinel FeV₂O₄ have also obtained the ambient conditions. Full article