Influence of Chemical Composition on Structure and Mechanical Properties of Vacuum-Carburized Low-Alloy Steels.

This study presents research results concerning the vacuum carburizing of four steel grades, specifically conforming to European standards 1.7243, 1.6587, 1.5920, and 1.3532. The experimental specimens exhibited variations primarily in nickel content, ranging from 0 to approximately 3.8 wt. %. As a comparative reference, gas carburizing was also conducted on the 1.3532 grade, which had the highest nickel content. Comprehensive structural analysis was carried out on the resultant carburized layers using a variety of techniques, such as optical and electron scanning, transmission microscopy, and X-ray diffraction. Additionally, mechanical properties such as hardness and fatigue strength were assessed. Fatigue strength evaluation was performed on un-notched samples having a circular cross-section with a diameter of 12 mm. Testing was executed via a three-point bending setup subjected to sinusoidally varying stresses ranging from 0 to maximum stress levels. The carburized layers produced had effective thicknesses from approximately 0.8 to 1.4 mm, surface hardness levels in the range of 600 to 700 HV, and estimated retained austenite contents from 10 to 20 vol%. The observed fatigue strength values for the layers varied within the range from 1000 to 1350 MPa. It was found that changing the processing method from gas carburizing, which induced internal oxidation phenomena, to vacuum carburizing improved the fatigue properties to a greater extent than increasing the nickel content of the steel.

Comparison of Physicochemical, Mechanical, and (Micro-)Biological Properties of Sintered Scaffolds Based on Natural- and Synthetic Hydroxyapatite Supplemented with Selected Dopants.

The specific combinations of materials and dopants presented in this work have not been previously described. The main goal of the presented work was to prepare and compare the different properties of newly developed composite materials manufactured by sintering. The synthetic- (SHAP) or natural- (NHAP) hydroxyapatite serves as a matrix and was doped with: (i) organic: multiwalled carbon nanotubes (MWCNT), fullerenes C60, (ii) inorganic: Cu nanowires. Research undertaken was aimed at seeking novel candidates for bone replacement biomaterials based on hydroxyapatite-the main inorganic component of bone, because bone reconstructive surgery is currently mostly carried out with the use of autografts; titanium or other non-hydroxyapatite -based materials. The physicomechanical properties of the developed biomaterials were tested by Scanning Electron Microscopy (SEM), Dielectric Spectroscopy (BSD), Nuclear Magnetic Resonance (NMR), and Differential Scanning Calorimetry (DSC), as well as microhardness using Vickers method. The results showed that despite obtaining porous sinters. The highest microhardness was achieved for composite materials based on NHAP. Based on NMR spectroscopy, residue organic substances could be observed in NHAP composites, probably due to the organic structures that make up the tooth. Microbiology investigations showed that the selected samples exhibit bacteriostatic properties against Gram-positive reference bacterial strain S. epidermidis (ATCC 12228); however, the property was much less pronounced against Gram-negative reference strain E. coli (ATCC 25922). Both NHAP and SHAP, as well as their doped derivates, displayed in good general compatibility, with the exception of Cu-nanowire doped derivates.

Structure and Magnetic Properties of Thermodynamically Predicted Rapidly Quenched Fe85-xCuxB15 Alloys.

In this work, based on the thermodynamic prediction, the comprehensive studies of the influence of Cu for Fe substitution on the crystal structure and magnetic properties of the rapidly quenched Fe85B15 alloy in the ribbon form are performed. Using thermodynamic calculations, the parabolic shape dependence of the ΔGamoprh with a minimum value at 0.6% of Cu was predicted. The ΔGamoprh from the Cu content dependence shape is also asymmetric, and, for Cu = 0% and Cu = 1.5%, the same ΔGamoprh value is observed. The heat treatment optimization process of all alloys showed that the least lossy (with a minimum value of core power losses) is the nanocomposite state of nanocrystals immersed in an amorphous matrix obtained by annealing in the temperature range of 300-330 °C for 20 min. The minimum value of core power losses P10/50 (core power losses at 1T@50Hz) of optimally annealed Fe85-xCuxB15 x = 0,0.6,1.2% alloys come from completely different crystallization states of nanocomposite materials, but it strongly correlates with Cu content and, thus, a number of nucleation sites. The TEM observations showed that, for the Cu-free alloy, the least lossy crystal structure is related to 2-3 nm short-ordered clusters; for the Cu = 0.6% alloy, only the limited value of several α-Fe nanograins are found, while for the Cu-rich alloy with Cu = 1.2%, the average diameter of nanograins is about 26 nm, and they are randomly distributed in the amorphous matrix. The only high number of nucleation sites in the Cu = 1.2% alloy allows for a sufficient level of grains' coarsening of the α-Fe phase that strongly enhances the ferromagnetic exchange between the α-Fe nanocrystals, which is clearly seen with the increasing value of saturation induction up to 1.7T. The air-annealing process tested on studied alloys for optimal annealing conditions proves the possibility of its use for this type of material.

Cobalt Content Effect on the Magnetic Properties of Ni50-xCoxMn35.5In14.5 Annealed Ribbons.

We present a study of the annealing effect and its influence on magnetic and structural properties for a series of Heusler alloys Ni50-xCoxMn35.5In14.5 (x=0,3,5) prepared in ribbon form. We studied the morphology and composition using scanning electron microscopy (SEM) equipped with an X-ray microanalyzer (EDX). The magnetic properties were determined by two methods: electron magnetic resonance (EMR) and vibrating sample magetometer (VSM). We found that cobalt content in the annealed samples reveals an additional magnetic phase transition at lower temperatures.

Effect of Co Substitution and Thermo-Magnetic Treatment on the Structure and Induced Magnetic Anisotropy of Fe84.5-xCoxNb5B8.5P2 Nanocrystalline Alloys.

In the present work, we investigated in detail the thermal/crystallization behavior and magnetic properties of materials with Fe84.5-xCoxNb5B8.5P2 (x = 0, 5, 10, 15 and 20 at.%) composition. The amorphous ribbons were manufactured on a semi-industrial scale by the melt-spinning technique. The subsequent nanocrystallization processes were carried out under different conditions (with/without magnetic field). The comprehensive studies have been carried out using differential scanning calorimetry, X-ray diffractometry, transmission electron microscopy, hysteresis loop analyses, vibrating sample magnetometry and Mössbauer spectroscopy. Moreover, the frequency (up to 300 kHz) dependence of power losses and permeability at a magnetic induction up to 0.9 T was investigated. On the basis of some of the results obtained, we calculated the values of the activation energies and the induced magnetic anisotropies. The X-ray diffraction results confirm the surface crystallization effect previously observed for phosphorous-containing alloys. The in situ microscopic observations of crystallization describe this process in detail in accordance with the calorimetry results. Furthermore, the effect of Co content on the phase composition and the influence of annealing in an external magnetic field on magnetic properties, including the orientation of the magnetic spins, have been studied using various magnetic techniques. Finally, nanocrystalline Fe64.5Co20Nb5B8.5P2 cores were prepared after transverse thermo-magnetic heat treatment and installed in industrially available portable heating equipment.

Nitrogen Dioxide Sensing Using Multilayer Structure of Reduced Graphene Oxide and α-Fe2O3.

Multilayers consisting of graphene oxide (GO) and α-Fe2O3 thin layers were deposited on the ceramic substrates by the spray LbL (layer by layer) coating technique. Graphene oxide was prepared from graphite using the modified Hummers method. Obtained GO flakes reached up to 6 nanometers in thickness and 10 micrometers in lateral size. Iron oxide Fe2O3 was obtained by the wet chemical method from FeCl3 and NH4OH solution. Manufactured samples were deposited as 3 LbL (GO and Fe2O3 layers deposited sequentially) and 6 LbL structures with GO as a bottom layer. Electrical measurements show the decrease of multilayer resistance after the introduction of the oxidizing NO2 gas to the ambient air atmosphere. The concentration of NO2 was changed from 1 ppm to 20 ppm. The samples changed their resistance even at temperatures close to room temperature, however, the sensitivity increased with temperature. Fe2O3 is known as an n-type semiconductor, but the rGO/Fe2O3 hybrid structure behaved similarly to rGO, which is p-type. Both chemisorbed O2 and NO2 act as electron traps decreasing the concentration of electrons and increasing the effective multilayer conductivity. An explanation of the observed variations of multilayer structure resistance also the possibility of heterojunctions formation was taken into account.

Influence of Cu Content on Structure, Thermal Stability and Magnetic Properties in Fe72-xNi8Nb4CuxSi2B14 Alloys.

The effect of substitution of Fe by Cu on the crystal structure and magnetic properties of Fe72-xNi8Nb4CuxSi2B14 alloys (x = 0.6, 1.1, 1.6 at.%) in the form of ribbons was investigated. The chemical composition of the materials was established on the basis of the calculated minima of thermodynamic parameters: Gibbs free energy of amorphous phase formation ΔGamorph (minimum at 0.6 at.% of Cu) and Gibbs free energy of mixing ΔGmix (minimum at 1.6 at.% of Cu). The characteristic crystallization temperatures Tx1onset and Tx1 of the alpha-iron phase together with the activation energy Ea for the as-spun samples were determined by differential scanning calorimetry (DSC) with a heating rate of 10-100 °C/min. In order to determine the optimal soft magnetic properties, the wound cores were subjected to a controlled isothermal annealing process in the temperature range of 340-640 °C for 20 min. Coercivity Hc, saturation induction Bs and core power losses at B = 1 T and frequency f = 50 Hz P10/50 were determined for all samples. Moreover, for the samples with the lowest Hc and P10/50, the magnetic losses were determined in a wider frequency range 50 Hz-400 kHz. The real and imaginary parts of the magnetic permeability µ', µâ€³ along with the cut-off frequency were determined for the samples annealed at 360, 460, and 560 °C. The best soft magnetic properties (i.e., the lowest value of Hc and P10/50) were observed for samples annealed at 460 °C, with Hc = 4.88-5.69 A/m, Bs = 1.18-1.24 T, P10/50 = 0.072-0.084 W/kg, µ' = 8350-10,630 and cutoff frequency at 8-9.3 × 104 Hz. The structural study of as-spun and annealed ribbons was carried out using X-ray diffraction (XRD) and a transmission electron microscope (TEM).

The Structure and Magnetic Properties of Rapidly Quenched Fe72Ni8Nb4Si2B14 Alloy.

The complex structural and magnetic studies of the annealed rapidly quenched Cu-free Fe72Ni8Nb4Si2B14 alloy (metallic ribbons form) are reported here. Based on the calorimetric results, the conventional heat treatment process (with heating rate 10 °C/min and subsequent isothermal annealing for 20 min) for wound toroidal cores has been optimized to obtain the least lossy magnetic properties (for the minimum value of coercivity and magnetic core losses at 50 Hz). For optimal conditions, the complex permeability in the 104-108 Hz frequency range together with core power losses obtained from magnetic induction dependence up to the frequency of 400 kHz was successfully measured. The average and local crystal structure was investigated by the use of the X-ray diffraction method and the transmission electron microscopy observations and proved its fully glassy state. Additionally, for the three temperature values, i.e., 310, 340 and 370 °C, the glass relaxation process study in the function of annealing time was carried out to obtain a deeper insight into the soft magnetic properties: magnetic permeability and cut-off frequency. For this type of Cu-free soft magnetic materials, the control of glass relaxation process (time and temperature) is extremely important to obtain proper magnetic properties.

SnO2/TiO2 Thin Film n-n Heterostructures of Improved Sensitivity to NO2.

Thin-film n-n nanoheterostructures of SnO2/TiO2, highly sensitive to NO2, were obtained in a two-step process: (i) magnetron sputtering, MS followed by (ii) Langmuir-Blodgett, L-B, technique. Thick (200 nm) SnO2 base layers were deposited by MS and subsequently overcoated with a thin and discontinuous TiO2 film by means of L-B. Rutile nanopowder spread over the ethanol/chloroform/water formed a suspension, which was used as a source in L-B method. The morphology, crystallographic and electronic properties of the prepared sensors were studied by scanning electron microscopy, SEM, X-ray diffraction, XRD in glancing incidence geometry, GID, X-ray photoemission spectroscopy, XPS, and uv-vis-nir spectrophotometry, respectively. It was found that amorphous SnO2 films responded to relatively low concentrations of NO2 of about 200 ppb. A change of more than two orders of magnitude in the electrical resistivity upon exposure to NO2 was further enhanced in SnO2/TiO2 n-n nanoheterostructures. The best sensor responses RNO2/R0 were obtained at the lowest operating temperatures of about 120 °C, which is typical for nanomaterials. Response (recovery) times to 400 ppb NO2 were determined as a function of the operating temperature and indicated a significant decrease from 62 (42) s at 123 °C to 12 (19) s at 385 °C A much smaller sensitivity to H2 was observed, which might be advantageous for selective detection of nitrogen oxides. The influence of humidity on the NO2 response was demonstrated to be significantly below 150 °C and systematically decreased upon increase in the operating temperature up to 400 °C.

Studies on the Two-Step Aging Process of Fe-Based Shape Memory Single Crystals.

Fe50Ni28Co17Al11.5Ta2.5 single crystals oriented along the [001] direction were investigated in order to establish the influence of two-step aging conditions on superelastic properties. The homogenized and quenched single crystalline material was subjected to a combination of high-temperature and low-temperature heat treatment at 973 K for 0.5 h and at 723 K for various aging times, respectively. As a result, fine and coherent γ' precipitates were formed. Using diffraction of high energy synchrotron radiation, the volume fraction of γ' precipitates was computed while their size was determined by high resolution TEM analysis. Compared with one-step heat treatment, the two-step aging process enables control of the precipitate size in a more accurate way. Moreover, it allows one to obtain a higher volume fraction of precipitates without increasing their size significantly. The obtained coherent γ' precipitates ranged in size from 5 to 8 nm; that considerably improved mechanical properties. The highest superelastic response was obtained for single crystals aged at 973 K for 0.5 h followed by aging at 723 K for 3 h. The single crystals treated with such conditions exhibited a superelastic strain of 15% in which the mechanical martensite stabilization was substantially suppressed.

Fe-Co-B Soft Magnetic Ribbons: Crystallization Process, Microstructure and Coercivity.

In this work, a detailed microstructural investigation of as-melt-spun and heat-treated Fe67Co20B13 ribbons was performed. The as-melt-spun ribbon was predominantly amorphous at room temperature. Subsequent heating demonstrated an amorphous to crystalline α-(Fe,Co) phase transition at 403 °C. In situ transmission electron microscopy observations, carried out at the temperature range of 25-500 °C and with the heating rate of 200 °C/min, showed that the first crystallized nuclei appeared at a temperature close to 370 °C. With a further increase of temperature, the volume of α-(Fe,Co) crystallites considerably increased. Moreover, the results showed that a heating rate of 200 °C/min provides for a fine and homogenous microstructure with the α-(Fe,Co) crystallites size three times smaller than when the ribbon is heated at 20 °C/min. The next step of this research concerned the influence of both the annealing time and temperature on the microstructure and coercivity of the ribbons. It was shown that annealing at 485 °C for a shorter time (2 s) led to materials with homogenous distribution of α-(Fe,Co) crystallites with a mean size of 30 nm dispersed in the residual amorphous matrix. This was reflected in the coercivity (20.5 A/m), which significantly depended on the volume fraction of crystallites, their size, and distribution.

Investigation of the surface of Ga⁻Sn⁻Zn eutectic alloy by the characterisation of oxide nanofilms obtained by the touch-printing method.

Ga⁻Sn⁻Zn eutectic alloy is a non-toxic liquid metal alloy which could be used in a multitude of applications, including as a heat transfer agent, in gas sensing, and in medicine. Alloys containing gallium readily oxidise in air, forming a thin oxide layer that influences the properties of liquid metals and which has not been studied. In this study, the oxide layer formed on Ga⁻Sn⁻Zn alloy was transferred at room temperature onto three substrates-quartz, glass and silicon. The contact angle between the liquid alloy and different substrates was determined. The obtained thin oxide films were characterised using atomic force microscopy, X-ray photon spectroscopy, and optical and transmission electron microscopy. The contact angle does not influence the deposition of the layers. It was determined that it is possible to obtain nanometric oxide layers of a few micrometres in size. The chemical composition was determined by XPS and EDS independently, and showed that the oxide layer contains about 90 atom % of gallium with some additions of tin and zinc. The oxides obtained from the eutectic Ga⁻Sn⁻Zn liquid alloys appear to be nanocrystalline.

Composite Nanofibers Containing Multiwall Carbon Nanotubes as Biodegradable Membranes in Reconstructive Medicine.

We have tested titanium (Ti) plates that are used for bone reconstruction in maxillofacial surgery, in combination with five types of novel long-resorbable biomaterials: (i) PCL0-polycaprolactone without additives, (ii) PCLMWCNT-polycaprolactone with the addition of multiwall carbon nanotubes (MWCNT), (iii) PCLOH-polycaprolactone doped with multiwall carbon nanotubes (MWCNT) containing ⁻OH hydroxyl groups, (iv) PCLCOOH-polycaprolactone with the addition of multiwall carbon nanotubes (MWCNT) containing carboxyl groups, and (v) PCLTI-polycaprolactone with the addition of Ti nanoparticles. The structure and properties of the obtained materials have been examined with the use of Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and/or X-ray powder diffraction (XRD). Titanium BR plates have been covered with: (i) PCL0 fibers (PCL0BR-connection plates), (ii) PCLMWCNT fibers (PCLMWCNTBR-plates), (iii) PCLOH fibers (PCLOHBR-plates), (iv) PCLCOOH (PCLCOOHBR-plates), (v) PCLTI fiber (PCLTIBR-connection plates). Such modified titanium plates were exposed to X-ray doses corresponding to those applied in head and neck tumor treatment. The potential leaching of toxic materials upon the irradiation of such modified titanium plates, and their effect on normal human dermal fibroblasts (NHDF) have been assessed by MTT assay. The presented results show variable biological responses depending on the modifications to titanium plates.

V2O5 Thin Films as Nitrogen Dioxide Sensors †.

Vanadium pentoxide thin films were deposited onto insulating support by means of rf reactive sputtering from a metallic vanadium target. Argon-oxygen gas mixtures of different compositions controlled by the flow rates were used for sputtering. X-ray diffraction at glancing incidence (GIXD) and Scanning Electronic Microscopy (SEM) were used for structural and phase characterization. Thickness of the films was determined by the profilometry. It has been confirmed by GIXD that the deposited films are composed of V2O5 phase. The gas sensing properties of V2O5 thin films were investigated at temperatures from range 410⁻617 K upon NO2 gas of 4⁻20 ppm. The investigated material exhibited good response and reversibility towards nitrogen dioxide. The effect of metal-insulator transition (MIT) on sensor performance has been observed and discussed for the first time. It was found that a considerable increase of the sensor sensitivity occured above 545 K, which is related to postulated metal-insulator transition.

Structure and properties of slow-resorbing nanofibers obtained by (co-axial) electrospinning as tissue scaffolds in regenerative medicine.

With the rapid advancement of regenerative medicine technologies, there is an urgent need for the development of new, cell-friendly techniques for obtaining nanofibers-the raw material for an artificial extracellular matrix production. We investigated the structure and properties of PCL10 nanofibers, PCL5/PCL10 core-shell type nanofibers, as well as PCL5/PCLAg nanofibres prepared by electrospinning. For the production of the fiber variants, a 5-10% solution of polycaprolactone (PCL) (Mw = 70,000-90,000), dissolved in a mixture of formic acid and acetic acid at a ratio of 70:30 m/m was used. In order to obtain fibers containing PCLAg 1% of silver nanoparticles was added. The electrospin was conducted using the above-described solutions at the electrostatic field. The subsequent bio-analysis shows that synthesis of core-shell nanofibers PCL5/PCL10, and the silver-doped variant nanofiber core shell PCL5/PCLAg, by using organic acids as solvents, is a robust technique. Furthermore, the incorporation of silver nanoparticles into PCL5/PCLAg makes such nanofibers toxic to model microbes without compromising its biocompatibility. Nanofibers obtained such way may then be used in regenerative medicine, for the preparation of extracellular scaffolds: (i) for controlled bone regeneration due to the long decay time of the PCL, (ii) as bioscaffolds for generation of other types of artificial tissues, (iii) and as carriers of nanocapsules for local drug delivery. Furthermore, the used solvents are significantly less toxic than the solvents for polycaprolactone currently commonly used in electrospin, like for example chloroform (CHCl3), methanol (CH3OH), dimethylformamide (C3H7NO) or tetrahydrofuran (C4H8O), hence the presented here electrospin technique may allow for the production of multilayer nanofibres more suitable for the use in medical field.

Nanostructured TiO2-based gas sensors with enhanced sensitivity to reducing gases.

2D TiO2 thin films and 3D flower-like TiO2-based nanostructures, also decorated with SnO2, were prepared by chemical and thermal oxidation of Ti substrates, respectively. The crystal structure, morphology and gas sensing properties of the TiO2-based sensing materials were investigated. 2D TiO2 thin films crystallized mainly in the form of rutile, while the flower-like 3D nanostructures as anatase. The sensor based on the 2D TiO2 showed the best performance for H2 detection, while the flower-like 3D nanostructures exhibited enhanced selectivity to CO(CH3)2 after sensitization by SnO2 nanoparticles. The sensor response time was of the order of several seconds. Their fast response, high sensitivity to selected gas species, improved selectivity and stability suggest that the SnO2-decorated flower-like 3D nanostructures are a promising material for application as an acetone sensor.

Microstructural analysis of iron aluminide formed by self-propagating high-temperature synthesis mechanism in aluminium matrix composite.

An aluminium matrix composite with iron aluminide formed in situ as a result of self-propagated high-temperature synthesis was examined. The structural characteristics of the reinforcement investigated by scanning electron microscopy and transmission electron microscopy methods are presented. Iron aluminide particles with a very fine grain size and of two shapes, cubic and needle-like, were observed. No differences in their phase composition were found by the selective electron diffraction pattern method. The composite reinforcement formed in the early stage of self-propagating high-temperature synthesis consisted only of the Al(3)Fe phase.