Search Results (41)

In the present work, the effect of quenching and partitioning cycles on the microstructure, hardness, and corrosion behavior of SAE 9254 spring steel was investigated. Initially, the critical phase transformation temperatures were analyzed by dilatometry. The samples were then treated by four routes of quenching and partitioning in a dilatometer with quenching stop temperatures of 250 and 220 °C. The partitioning temperatures were 300 and 400 °C. The partitioning time was 480 s. Quantitative characterization of austenite and martensite volume fractions was carried out by X-ray diffraction. Qualitative characterization was carried out by optical microscopy and scanning electron microscopy in addition to quantitative assessments of the chemical composition of segregations by EDS. The formation of martensite, retained austenite, and bainite was observed. The dilatometric curves displayed the occurrence of volumetric expansion in the partitioning step, indicating the formation of secondary martensite (fresh martensite) during the final cooling process (final quenching). The mechanical properties were evaluated by Vickers microhardness and nanoindentation tests. There was heterogeneity of hardness inside and outside the banding regions. The electrochemical properties were evaluated by electrochemical impedance spectroscopy and potentiodynamic polarization tests in a 0.1 M H₂SO₄ solution. The best corrosion resistance was achieved for samples quenched at 250 °C and partitioned at 400 °C due to the higher volume fraction of retained austenite when compared to the other heat treatment conditions. Full article

The isothermal bainitic transformation kinetics, microstructure, and mechanical properties of the quenched low-carbon high-strength steel have been investigated via dilatometric measurements, microstructural characterization, and mechanical tests. The results show that the pre-transformed isothermal bainite promotes martensitic transformation, increasing the martensitic transformation temperature, and enhancing the transformation rate. The microstructure of the 400 °C isothermal steel consists predominantly of lath bainite ferrite with dot/slender M-A constituents, whereas the steel treated at 450 °C contains a combination of martensite/lath bainite and granular bainite. The presence of massive M-A constituents contributes to brittle fracture as these constituents tend to promote crack initiation. Hence, the 450 °C treatment, which leads to the formation of massive M-A constituents, induces brittleness, while the finer M-A constituents formed at 400 °C exert minimal influence on the toughness and result in a more stable microstructure owing to their small size and the surrounding fine lath microstructure. The differences in microstructure and properties between the steels treated at 400 °C and 450 °C illustrate the importance of controlling the quenching cooling rate in the high-temperature bainitic transformation region during thick plate quenching processes. Full article

The continuous cooling transformation (CCT) curves of undercooled austenite serve as crucial references for obtaining desired microstructures and properties in metallic materials (particularly deformed metals) through heat treatment. In this study, static and dynamic CCT curves were constructed for experimental steels micro-doped with rare earth element Ce by combining temperature-dilatometric curves recorded after austenitization at 900 °C with microstructural characterization and microhardness measurements. Comparative analyses were conducted on the microstructures and microhardness of three experimental steels with varying Ce contents subjected to sizing (reducing) diameter deformation at 850 °C and 950 °C. The CCT experimental results revealed that the microhardness of the tested steels increased with cooling rates. Notably, dynamic CCT specimens cooled at 50 °C/s to room temperature following superheated deformation exhibited 56.7 HV5 higher microhardness than static CCT specimens, accompanied by increased martensite content. The reduction of deformation temperature from 950 °C to 850 °C resulted in the expansion of the bainitic phase region. The incorporation of trace Ce elements demonstrated a significant enhancement in the microhardness of 30MnNbRE steel. This research proposes an effective processing route for improving strength-toughness combination in microalloyed oil well tubes: introducing trace Ce additions followed by sizing (reducing) diameter deformation at 950 °C and subsequent ultra-fast cooling at 50 °C/s to room temperature. This methodology facilitates the production of high-strength/toughness steels containing abundant martensitic microstructures. Full article

The aim of this work is to perform a detailed dilatometric analysis of the decomposition of austenite during the cooling process using experimentally derived continuous cooling transformation (CCT) diagrams for two specific tool steels, X153CrMoV12 Bohdan Bolzano, Bratislava, Slovakia and 100MnCrW4. The dilatometric curves were compared with metallographic evaluations using scanning electron microscopy (SEM). In addition, hardness measurements were performed to obtain additional information about the mechanical properties of the materials. All experimental work was performed using a DIL 805A. The accuracy of the resulting CCT diagrams was verified by comparing them with those calculated with the JMatPro software v12.4. The cooling rates ranged from 20 °C/s to 0.01 °C/s, depending on the specific type of steel tested. The novelty of this research is the combination of experimental and simulation methods to analyze the influence of alloying elements on the kinetics of phase transformations in tool steels. It was found that one of the most significant factors affecting the CCT diagrams is the weight percentage of alloying elements in the steels. These results clearly show that increasing the weight percentage of the content of alloying elements has a significant impact on the accuracy of the simulation results derived from the JMatPro software. Full article

This paper presents the results of research on the kinetics of transformations in the two-phase (α + β) Ti-6Al-4V alloy. The transformation start and end temperatures during heating at different rates were determined using a dilatometer. A modified dilatometer was employed, equipped with an acoustic emission measurement apparatus and software enabling the assessment of sample dimensional changes during heating and cooling. The results were obtained in the form of dilatometric curves. Additionally, the occurrence of the transformation was confirmed by acoustic emission signals. In the study of the Ti-6Al-4V alloy, acoustic emission refers to the application of this non-destructive technique to monitor the alloy’s behavior during thermal processes. As the temperature increased, regardless of the heating rate, the α→β transformation was observed to occur after exceeding 900 °C. Within the transformation range, acoustic emission signals were recorded. Moreover, it was found that the applied research methods enabled the identification of signal components originating from the transformation. The application of acoustic methods in the analysis of phase transformations opens new possibilities for their use in industry. Full article

The effects of austenitizing and austempering temperatures on the bainite transformation kinetics and the microstructural and mechanical properties of a medium-carbon high-silicon ultra-fine bainitic steel were investigated via dilatometric measurements, microstructural characterization and mechanical tests. It is demonstrated that the optimum austenitizing temperature exists for 0.3 wt.%C ultra-fine bainitic steel. Although the finer austenite grain at 950 °C provides more bainite nuclei site and form finer bainitic ferrite plates, the lower dislocation density in plates and the higher volume fraction of the retained austenite reduces the strength and impact toughness of ultra-fine steel. When the austenitizing temperature exceeds 1000 °C, the true thickness of bainitic ferrite plates and the volume fraction of blocky retained austenite in the bainite microstructure increase significantly with the increases in austenitizing temperature, which do harm to the plasticity and impact toughness. The effect of austempering temperature on the transformation behavior and microstructural morphology of ultra-fine bainite is greater than that of austenitizing temperature. The prior martensite, formed when the austempering temperature below Ms, can refine the bainitic ferrite plates and improve the strength and impact toughness. However, the presence of prior martensite divides the untransformed austenite and inhibits the growth of bainite sheaves, thus prolonging the finishing time of bainite transformation. In addition, prior martensite also strengthens the stability of untransformed austenite though carbon partition and enhances the volume fraction of blocky retained austenite, which reduces the plasticity of ultra-fine bainitic steel. According to the experimental results, the optimum austempering process for 0.3 wt. %C ultra-fine bainitic steel is through austenitization at 1000 °C and austempering at 340 °C. Full article

This paper reports research findings on the functionalization of NiTi shape memory alloy through the electrophoretic deposition of innovative complex layers comprising a silver-rutile (Ag-TiO₂) nanocomposite. A colloidal suspension of a chemically synthesized Ag-TiO₂ nanosystem prepared with a 59.4 ± 0.9 mV Zeta potential for anaphoretic deposition. Employing a design of experiment method (DoE), the optimal parameters for uniform coating depositions were identified as 40 V/3 min. Dilatometric tests and high-temperature microscopy determined that the deposited layers’ heat treatment temperature should not exceed 800 °C. Raman spectrometry and scanning electron microscopy (SEM) provided comprehensive structural and morphological insights into the resulting continuous and crack-free layer. The article extensively explores the impact of annealing on structural changes within the layer, proposing mechanisms for its formation. The findings affirm the feasibility of creating a highly reactive layer on the NiTi alloy, holding potential significance in implantation medicine. Full article

Dilatometric experiments were conducted with the main purpose of measuring the transformation-induced coefficients of 13% chromium and 4% nickel, which are martensitic stainless steel base and filler materials used for hydraulic turbine manufacturing. To this end, a set of experiments was conducted in a quenching dilatometer equipped with loading capabilities. The measurement system was further improved by means of modified pushrods to allow for the use of specimens with geometries that are compliant with tensile test standards. This improvement allowed for the measurement of the materials’ phases and respective yield strengths. The dataset was further used to determine the relationship between the applied external stress and the martensitic start temperature ($M_s$) upon cooling. The TRIP coefficient’s K values for both the S41500 steel and E410NiMo filler material were measured at $8.12\times {10}^{-5}$ and $7.11\times {10}^{-5}$, respectively. Additionally, the solid phase transformation model parameters for both the austenitic and martensitic transformation of the filler material were measured. These parameters were then used to model austenitic-phase-transformation kinetics and martensite transformation, including transformation-induced plasticity effects. Good agreement was achieved between the calculation and the experiments. Full article

The aim of this research is a systematic investigation of heat treatments of 60E1 profile rails made of steel R350HT, which would ensure the properties required by the standard EN 16273. Additionally, it presents a concept of cooling rails on a semi-industrial station, which will make it possible to obtain the desired properties. The dilatometric tests have demonstrated that the optimal cooling rate is within the scope of 3 °C/s to 6 °C/s, when both the EN 16273 standard’s hardness distribution and microstructure requirements are fulfilled. The tests on the designed and built station showed that the optimal pressure with respect to the microstructure and properties of the rail equals 6.5 bar. For these parameters, measurements of the interlamellar distance were also performed—the cooling rate obtained at the surface was 3.68 °C/s, with an interlamellar distance of about 80 nm, whereas inside the rail the rate was 2.63 °C/s and the distance 110 nm. The achieved results confirm that the designed station can be used for controlled cooling of rail steels from R350HT steel. Full article

This study aims to use natural carbonated Tunisian clay as an aluminosilicate precursor for the elaboration of phosphate-based geopolymers, which yields to the valorization of this common material in Tunisia. In addition, the presence of calcium carbonate in this clay allows the investigation of this associated mineral’s effect on the properties of geopolymeric materials. To achieve these purposes, several experimental techniques were used, namely fluorescence (FX), particle size analysis, thermogravimetric analysis (TGA), differential thermal analysis (DTA), dilatometric analysis, X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The mechanical strength and the open porosity of the obtained geopolymeric samples were tested by the compression test and the standard test method for water absorption, respectively. The findings of this work show that the used Tunisian clay can present an attractive aluminosilicate precursor for the synthesis of phosphate-based geopolymers. It also shows that the chosen calcination temperature of the raw clay considerably modifies the reactivity of minerals during geopolymerization and, consequently, strongly affects the properties and structure of the geopolymeric samples. These effects were attributed essentially to the formation of new calcium crystalline phases in the obtained geopolymeric samples. In fact, the anorthite (CaAl₂Si₂O₈) phase appears in all the samples but in greater abundance in those obtained from the clay calcined at 550 °C, and the brushite phase (CaHPO₄·2H₂O) appears only in the samples obtained from the clay calcined at 950 °C. All these new crystalline phases are strongly dependent on the state of the calcite present in the calcined clay. Full article

Although highly developed countries are trying to diversify away from coal-based energy, many economies rely on this resource. Its consumption results in the production of carbon dioxide, which promotes global warming, necessitating its sequestration. This paper presents the sorption–dilatometric relationships of hard coal samples differing in vitrinite and inertinite content. The studies were carried out under isothermal conditions (298 K) at a free pressure drop complemented by measurements under non-isothermal conditions (298 K to 323 K). The tests were performed on an original apparatus, based on the operation of an Arduino microcontroller. For the natural porosity to be preserved and for a better representation of the behaviour of the coal–gas system, samples in the form of cuboidal blocks were used, making this apparatus unique worldwide. Based on the study, it appears that the difference in petrographic composition affects the behaviour of the coal structure, influencing differences in the sorption–dilatometric properties. In the case of the sample with higher vitrinite content, the amount of adsorbed gases is higher. Full article

This research was completed in the development of studies devoted to relations between the elastic modulus (MoE) and thermal expansivity (CTe) of different materials. This study, based on experimental data, confirmed the models of the relations between MoE and CTe under normal and heating temperatures for thermosetting epoxy polymers and glass-fiber FRPs in two variants (unfilled and filled by mineral additives), after the usual glassing and prolonged thermal conditioning (thermo-relaxation). The experiment was based on dilatometric and elastic deformation testing. Two models of MoE/CTe were tested: Barker’s model and our authors relaxation model (MoE = f(CTe)), which is based on previous modelling of the non-linearity of the physical properties of polymers’ supramolecular structures. The result show that the models’ constants depend on composition; Barker’s model is applicable only to polymers with satisfying agreement degrees in the range 10–20%; our model is applicable to polymers and FRPs with satisfying agreement degrees in the range of 6–18%. Full article

Pectate and alginate are among the most important biopolymers able to give rise to ionotropic gelation upon the addition of di- or multivalent counterions. The two ionic polysaccharides exhibit several common aspects of the gelation mechanism with calcium ions, the physiologically and commercially most relevant counterion type. The first one pertains to the role that specific Ca²⁺/polyion interactions play in the establishment of the ion-mediated chain/chain cross-links. Such interactions include both a specific affinity of the territorially condensed Ca²⁺ counterions for the polyuronate(s) and the formation of long-lasting chemical bonding (inner ion–sphere complex) of specific interchain sites accompanied by high conformational ordering. As to the first mechanism, it is dominated by the strong desolvation of the interacting ionic species, with concomitant positive variations in both enthalpy and entropy, the contribution of the latter prevailing over the former due to the favorable liberation of a very large number of water molecules of hydration. Both dilatometric and microcalorimetric data point to the higher affinity of Ca²⁺ for pectate than for alginate. The selective accumulation of calcium ions close to the polyanion(s) favors the onset of the second—chemical bonding—mode, which is associated with charge neutralization at the bonding site. This mode coincides with the largely accepted “egg-box” model for the calcium-mediated interchain junction of pectate and alginate. A new approach was devised for the calculation of the fraction of chemically bound divalent ions; it was based on the available circular dichroism data (further supported by scattering and viscosity results) and successfully tested by comparison with an independently determined fraction in the case of pectate. In detail, the strong bonding mode manifests in two sequential bonding modes. The first one (at low concentrations of added Ca²⁺ ions) entails a cross-link in which only one calcium ions is bracketed in a “twisted” egg-box between two chains; upon further counterion addition, a series of nearest-neighboring “perfect” egg-box structures develops. Both dilatometric and microcalorimetric changes associated with the latter chemical bonding modes are quantitatively larger for pectate than for alginate; clearly the latter polyuronate suffers from the relevant presence of the weakly calcium-binding mannuronic acid repeating units. Light-scattering experiments provided a clear-cut demonstration of the intermolecular bonding of calcium ions from the very beginning of the linker addition. Full article

The use of biobased thermoplastic polymers has gained great attention in the last years as a potential alternative to fossil-based thermoplastic polymers. Biobased polymers in fact offer advantages not only in terms of reduced dependence on fossil resources but they also lower the CO₂ footprint in accordance with sustainability and climate protection goals. To improve the properties of these materials, reinforcement with biobased fibers is a promising solution; however, it must be kept in mind that the fibers aspect ratio and the interfacial adhesion between the reinforcement and the matrix plays an important role influencing both physical and mechanical properties of the biocomposites. In this paper, the possibility of producing composites by injection molding, based on polybutylene succinate and ultra-short cellulosic fibers has been explored as a potential biobased solution. Thermo-mechanical properties of the composites were investigated, paying particular attention to the local micromechanical deformation processes, investigated by dilatometric tests, and failure mechanisms. Analytical models were also applied to predict the elastic and flexural modulus and the interfacial properties of the biocomposites. Good results were achieved, demonstrating the that this class of biocomposite can be exploited. Compared to pure PBS, the composites with 30 wt.% of cellulose fibers increased the Young’s modulus by 154%, the flexural modulus by 130% and the heat deflection temperature by 9%. Full article

Thermal expanding is the important property that defines the stress–strain condition of GRP structures exploited under heating and having limited thermal resistance. So, the GRPs’ thermal expanding prediction is the actual requirement of such structures design. The experimental accurate dilatometric study resulted in the non-linearity of thermosetting polymers and plastics thermal expanding under heating. The polymers and plastics thermal expanding coefficient (CTE) is non-linearly increasing under heating before glassing temperature (Tg). Using the previous polymers and GRPs modelling experience and experimental dilatometric results, the non-linear adequate prediction models of their CTE were proposed and proved. The new compensative wave model of polymers’ CTE and multi-layer model of GRPs’ CTE were proposed and successfully tested. A prediction of the temperature dependences of the thermal expansion coefficients of various thermoset polymer binders and data on the reinforcement structure was performed based on the experimentally obtained temperature dependences of the CTEs of GRPs. The prediction was performed using the finite-element homogenization method in the Material Designer module of the academic version of the Ansys package. A satisfactory concurrence of the numerical results of the prognosis and the experiment for all considered cases is observed in the temperature range from 50 to 100 °C, after glass transition temperature best coincidence of numerical values of CTE is obtained for glass-reinforced plastics on epoxy resin, which were not subjected to thermal aging. Full article