Effect of Cryogenic Treatments on Hardness, Fracture Toughness, and Wear Properties of Vanadis 6 Tool Steel.

The ability of cryogenic treatment to improve tool steel performance is well established; however, the selection of optimal heat treatment is pivotal for cost reduction and extended tool life. This investigation delves into the influence of distinct cryogenic and tempering treatments on the hardness, fracture toughness, and tribological properties of Vanadis 6 tool steel. Emphasis was given to comprehending wear mechanisms, wear mode identification, volume loss estimation, and detailed characterization of worn surfaces through scanning electron microscopy coupled with energy dispersive spectroscopy and confocal microscopy. The findings reveal an 8-9% increase and a 3% decrease in hardness with cryogenic treatment compared to conventional treatment when tempered at 170 °C and 530 °C, respectively. Cryotreated specimens exhibit an average of 15% improved fracture toughness after tempering at 530 °C compared to conventional treatment. Notably, cryogenic treatment at -140 °C emerges as the optimum temperature for enhanced wear performance in both low- and high-temperature tempering scenarios. The identified wear mechanisms range from tribo-oxidative at lower contacting conditions to severe delaminative wear at intense contacting conditions. These results align with microstructural features, emphasizing the optimal combination of reduced retained austenite and the highest carbide population density observed in -140 °C cryogenically treated steel.

Cryogenic Treatment of Martensitic Steels: Microstructural Fundamentals and Implications for Mechanical Properties and Wear and Corrosion Performance.

Conventional heat treatment is not capable of converting a sufficient amount of retained austenite into martensite in high-carbon or high-carbon and high-alloyed iron alloys. Cryogenic treatment induces the following alterations in the microstructures: (i) a considerable reduction in the retained austenite amount, (ii) formation of refined martensite coupled with an increased number of lattice defects, such as dislocations and twins, (iii) changes in the precipitation kinetics of nano-sized transient carbides during tempering, and (iv) an increase in the number of small globular carbides. These microstructural alterations are reflected in mechanical property improvements and better dimensional stability. A common consequence of cryogenic treatment is a significant increase in the wear resistance of steels. The current review deals with all of the mentioned microstructural changes as well as the variations in strength, toughness, wear performance, and corrosion resistance for a variety of iron alloys, such as carburising steels, hot work tool steels, bearing and eutectoid steels, and high-carbon and high-alloyed ledeburitic cold work tool steels.

Impact of interstitial elements on the stacking fault energy of an equiatomic CoCrNi medium entropy alloy: theory and experiments.

We investigated the effects of interstitial N and C on the stacking fault energy (SFE) of an equiatomic CoCrNi medium entropy alloy. Results of computer modeling were compared to tensile deformation and electron microscopy data. Both N and C in solid solution increase the SFE of the face-centered cubic (FCC) alloy matrix at room temperature, with the former having a more significant effect by 240% for 0.5 at % N. Total energy calculations based on density functional theory (DFT) as well as thermodynamic modeling of the Gibbs free energy with the CALPHAD (CALculation of PHAse Diagrams) method reveal a stabilizing effect of N and C interstitials on the FCC lattice with respect to the hexagonal close-packed (HCP) CoCrNi-X (X: N, C) lattice. Scanning transmission electron microscopy (STEM) measurements of the width of dissociated ½<110> dislocations suggest that the SFE of CoCrNi increases from 22 to 42-44 mJ·m-2 after doping the alloy with 0.5 at. % interstitial N. The higher SFE reduces the nucleation rates of twins, leading to an increase in the critical stress required to trigger deformation twinning, an effect which can be used to design load-dependent strain hardening response.

Tailoring a Refractory High Entropy Alloy by Powder Metallurgy Process Optimization.

This paper reports the microstructural evolution and mechanical properties of a low-density Al0.3NbTa0.8Ti1.5V0.2Zr refractory high-entropy alloy (RHEA) prepared by means of a combination of mechanical alloying and spark plasma sintering (SPS). Prior to sintering, the morphology, chemical homogeneity and crystal structures of the powders were thoroughly investigated by varying the milling times to find optimal conditions for densification. The sintered bulk RHEAs were produced with diverse feedstock powder conditions. The microstructural development of the materials was analyzed in terms of phase composition and constitution, chemical homogeneity, and crystallographic properties. Hardness and elastic constants also were measured. The calculation of phase diagrams (CALPHAD) was performed to predict the phase changes in the alloy, and the results were compared with the experiments. Milling time seems to play a significant role in the contamination level of the sintered materials. Even though a protective atmosphere was used in the entire manufacturing process, carbide formation was detected in the sintered bulks as early as after 3 h of powder milling. Oxides were observed after 30 h due to wear of the high-carbon steel milling media and SPS consolidation. Ten hours of milling seems sufficient for achieving an optimal equilibrium between microstructural homogeneity and refinement, high hardness and minimal contamination.

Temperature Dependence of Fracture Characteristics of Variously Heat-Treated Grades of Ultra-High-Strength Steel: Experimental and Modelling.

The temperature dependence of tensile characteristics and fracture toughness of the standardly heat-treated low-alloyed steel OCHN3MFA along with three additionally heat-treated grades was experimentally studied. In the temperature range of ⟨-196; 22⟩ °C, all the additional heat treatments transferred the standard steel from a high- to ultra-high strength levels even with improved tensile ductility characteristics. This could be explained by a reduction of the inclusion content, refinement of the martensitic blocks, ductile retained austenite content, and homogenization of the shape ratio of martensitic laths as revealed by metallographic, X-ray, and EBSD techniques. On the other hand, the values of the fracture toughness of all grades were found to be comparable in the whole temperature range as the cause of a high stress triaxiality in the pre-cracked Charpy V-notch samples. The values of the fracture toughness of the standard steel grade could be predicted well using the fracture model proposed by Pokluda et al. based on the tensile characteristics. Such a prediction failed in the case of additionally heat-treated grades due to the different temperature dependence of the fracture mechanisms occurring in the tensile and fracture-toughness tests. While the tensile samples fractured in a ductile-dimple mode at all temperatures, the fracture-toughness specimens exhibited a transition from the ductile to quasi-brittle fracture mode with decreasing temperature. This transition could be interpreted in terms of a transfer from the model proposed by Rice and Johnson to the model of Tvergaard and Hutchinson.

Incorporation of Temperature and Plastic Strain Effects into Local Approach to Fracture.

An unjustified simplification of the local quantitative criterion regarding cleavage nucleation is a key problem in the utilisation of the Local Approach to Fracture (LA), particularly to predict the fracture toughness within the ductile-to-brittle transition (DBT) region. The theoretical concept of the effect of both temperature and the plastic strain value on the crack nuclei (CN) generation rate in iron and ferritic steels is presented. It is shown how the plastic strain and temperature affect CN formation rate and, as a consequence, govern the shape of the temperature dependence of fracture toughness KJc and its scatter limits. Within the framework of the microscopic model proposed, dependences of the CN bulk density on the plastic deformation value and temperature are predicted. Convenient approximation dependences for incorporating this effect into the LA are suggested. The experimental data of reactor pressure vessel steel and cast manganese steel demonstrate that the use of these dependences enables one to predict, with sufficient accuracy, the effect of temperature on the value of fracture toughness and its scatter limits over the DBT region. It is shown that accounting for both the temperature and strain dependence of CN bulk density gives rise to the invariance of parameters of the Weibull distribution to temperature.

Preparation and Properties of Layered SiC-Graphene Composites for EDM.

Three and five-layered silicon carbide-based composites containing 0, 5, and 15 wt.% of graphene nanoplatelets (GNPs) were prepared with the aim to obtain a sufficiently high electrical conductivity in the surface layer suitable for electric discharge machining (EDM). The layer sequence in the asymmetric three-layered composites was SiC/SiC-5GNPs/SiC-15GNPs, while in the symmetric five-layered composite, the order of layers was SiC-15GNPs/SiC-5GNPs/SiC/SiC-5GNPs/SiC-15GNPs. The layered samples were prepared by rapid hot-pressing (RHP) applying various pressures, and it was shown that for the preparation of dense 3- or 5-layered SiC/GNPs composites, at least 30 MPa of the applied load was required during sintering. The electrical conductivity of 3-layered and 5-layered composites increased significantly with increasing sintering pressure when measured on the SiC surface layer containing 15 wt.% of GNPs. The increasing GNPs content had a positive influence on the electrical conductivity of individual layers, while their instrumented hardness and elastic modulus decreased. The scratch tests confirmed that the materials consisted of well-defined layers with straight interfaces without any delamination, which suggests good adhesion between the individual layers.

The Effect of Electrolytic Hydrogenation on Mechanical Properties of T92 Steel Weldments under Different PWHT Conditions.

In the present work, the effects of electrolytic hydrogen charging of T92 steel weldments on their room-temperature tensile properties were investigated. Two circumferential weldments between the T92 grade tubes were produced by gas tungsten arc welding using the matching Thermanit MTS 616 filler material. The produced weldments were individually subjected to considerably differing post-welding heat treatment (PWHT) procedures. The first-produced weldment was conventionally tempered (i.e., short-term annealed below the Ac1 critical transformation temperature of the T92 steel), whereas the second one was subjected to its full renormalization (i.e., appropriate reaustenitization well above the T92 steel Ac3 critical transformation temperature and subsequent air cooling), followed by its conventional subcritical tempering. From both weldments, cylindrical tensile specimens of cross-weld configuration were machined. The room-temperature tensile tests were performed for the individual welds' PWHT states in both hydrogen-free and electrolytically hydrogen-charged conditions. The results indicated higher hydrogen embrittlement susceptibility for the renormalized-and-tempered weldments, compared to the conventionally tempered ones. The obtained findings were correlated with performed microstructural and fractographic observations.

Electrophoretic Deposition of Copper(II)-Chitosan Complexes for Antibacterial Coatings.

Bacterial infection associated with medical implants is a major threat to healthcare. This work reports the fabrication of Copper(II)-Chitosan (Cu(II)-CS) complex coatings deposited by electrophoretic deposition (EPD) as potential antibacterial candidate to combat microorganisms to reduce implant related infections. The successful deposition of Cu(II)-CS complex coatings on stainless steel was confirmed by physicochemical characterizations. Morphological and elemental analyses by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX) spectroscopy verified the uniform distribution of copper in the Chitosan (CS) matrix. Moreover, homogeneous coatings without precipitation of metallic copper were confirmed by X-ray diffraction (XRD) spectroscopy and SEM micrographs. Controlled swelling behavior depicted the chelation of copper with polysaccharide chains that is key to the stability of Cu(II)-CS coatings. All investigated systems exhibited stable degradation rate in phosphate buffered saline (PBS)-lysozyme solution within seven days of incubation. The coatings presented higher mechanical properties with the increase in Cu(II) concentration. The crack-free coatings showed mildly hydrophobic behavior. Antibacterial assays were performed using both Gram-positive and Gram-negative bacteria. Outstanding antibacterial properties of the coatings were confirmed. After 24 h of incubation, cell studies of coatings confirms that up to a certain threshold concentration of Cu(II) were not cytotoxic to human osteoblast-like cells. Overall, our results show that uniform and homogeneous Cu(II)-CS coatings with good antibacterial and enhanced mechanical stability could be successfully deposited by EPD. Such antibiotic-free antibacterial coatings are potential candidates for biomedical implants.

Influence of Ti on the Tensile Properties of the High-Strength Powder Metallurgy High Entropy Alloys.

The focus of this study is the evaluation of the influence of Ti concentration on the tensile properties of powder metallurgy high entropy alloys. Three Ni1.5Co1.5CrFeTiX alloys with X = 0.3; 0.5 and 0.7 were produced by mechanical alloying and spark plasma sintering. Additional annealing heat treatment at 1100 °C was utilized to obtain homogenous single-phase face centered cubic (FCC) microstructures, with minor oxide inclusions. The results show that Ti increases the strength of the alloys by increasing the average atomic size misfit i.e., solid solution strengthening. An excellent combination of mechanical properties can be obtained by the proposed method. For instance, annealed Ni1,5Co1,5CrFeTi0.7 alloy possessed the ultimate tensile strength as high as ~1600 MPa at a tensile ductility of ~9%, despite the oxide contamination. The presented results may serve as a guideline for future alloy design of novel, inclusion-tolerant materials for sustainable metallurgy.

Can Sub-zero Treatment at -75 °C Bring Any Benefits to Tools Manufacturing?

: Vanadis 6 ledeburitic tool steel was subjected to sub-zero treatment at -75 °C for different durations, and for different subsequent tempering regimes. The impact of these treatments on the microstructure, hardness variations, and toughness characteristics of the steel was investigated. The obtained results infer that the retained austenite amount was reduced to one fourth by sub-zero treatment (SZT), and the population density of add-on carbides was increased by factor of three to seven, depending on the duration of SZT. Tempering always reduced the population density of these particles. A hardness increased by 30-60 HV10 was recorded after sub-zero treatment but tempering to the secondary hardness peak induced much more significant hardness decrease than what was established in conventionally quenched steel. The flexural strength was not negatively influenced by sub-zero treatment at -75 °C while the fracture toughness tests gave worse values of this quantity, except the case of steel tempered to the secondary hardness peak.

Shear Performance at Room and High Temperatures of Glass⁻Ceramic Sealants for Solid Oxide Electrolysis Cell Technology.

To provide a reliable integration of components within a solid oxide electrolysis cell stack, it is fundamental to evaluate the mechanical properties of the glass⁻ceramic sealing materials, as well as the stability of the metal⁻glass⁻ceramic interface. In this work, the mechanical behavior of two previously developed glass⁻ceramic sealants joined to Crofer22APU steel is investigated at room temperature, 650 °C, and 850 °C under shear load. The mechanical properties of both the glass⁻ceramics showed temperature dependence. The shear strength of Crofer22APU/glass⁻ceramic/Crofer22APU joints ranged from 14.1 MPa (20 °C) to 1.8 MPa (850 °C). The elastic modulus of both glass⁻ceramics also reduced with temperature. The volume fraction of the crystalline phases in the glass⁻ceramics was the key factor for controlling the mechanical properties and fracture, especially above the glass-transition temperature.

Electrolyte-Supported Fuel Cell: Co-Sintering Effects of Layer Deposition on Biaxial Strength.

The mechanical reliability of reversible solid oxide cell (SOC) components is critical for the development of highly efficient, durable, and commercially competitive devices. In particular, the mechanical integrity of the ceramic cell, also known as membrane electrolyte assembly (MEA), is fundamental as its failure would be detrimental to the performance of the whole SOC stack. In the present work, the mechanical robustness of an electrolyte-supported cell was determined via ball-on-3-balls flexural strength measurements. The main focus was to investigate the effect of the manufacturing process (i.e., layer by layer deposition and their co-sintering) on the final strength. To allow this investigation, the electrode layers were screen-printed one by one on the electrolyte support and thus sintered. Strength tests were performed after every layer deposition and the non-symmetrical layout was taken into account during mechanical testing. Obtained experimental data were evaluated with the help of Weibull statistical analysis. A loss of mechanical strength after every layer deposition was usually detected, with the final strength of the cell being significantly smaller than the initial strength of the uncoated electrolyte (σ0 ≈ 800 MPa and σ0 ≈ 1800 MPa, respectively). Fractographic analyses helped to reveal the fracture behavior changes when individual layers were deposited. It was found that the reasons behind the weakening effect can be ascribed to the presence and redistribution of residual stresses, changes in the crack initiation site, porosity of layers, and pre-crack formation in the electrode layers.

Nitrogen Interstitial Alloying of CoCrFeMnNi High Entropy Alloy through Reactive Powder Milling.

The present work is focused on the synthesis of CoCrFeMnNi high entropy alloy (HEA) interstitially alloyed with nitrogen via powder metallurgy routes. Using a simple method, nitrogen was introduced to the HEA from the protective N2 gas atmosphere during mechanical alloying (MA) processing. The lattice parameter and amount of nitrogen in HEA were observed to be linearly proportional to the milling duration. The limited solubility of nitrogen in the main face centered cubic (FCC) phase resulted in the in-situ formation of nitrides and, accordingly, significant increase in the hardness values. It has been shown that fabrication of such nitrogen-doped HEA bulk materials can be conveniently achieved by a simple combination of MA + spark plasma sintering processes, without the need for adding nitrogen from other sources.

Extension of the 'Inorganic Gel Casting' Process to the Manufacturing of Boro-Alumino-Silicate Glass Foams.

A new technique for the production of glass foams, based on alkali activation and gel casting, previously applied to soda-lime glass, was successfully extended to boro-alumino-silicate glass, recovered from the recycling of pharmaceutical vials. A weak alkali activation (2.5 M NaOH or NaOH/KOH aqueous solutions) of fine glass powders (below 70 µm) allowed for the obtainment of well-dispersed concentrated aqueous suspensions, undergoing gelation by treatment at low temperature (75 °C). Unlike soda-lime glass, the progressive hardening could not be attributed to the formation of calcium-rich silicate hydrates. The gelation was provided considering the chemical formulation of pharmaceutical glass (CaO-free) to the formation of hydrated sodium alumino-silicate (N-A-S-H) gel. An extensive direct foaming was achieved by vigorous mechanical stirring of partially gelified suspensions, comprising also a surfactant. A sintering treatment at 700 °C, was finally applied to stabilize the cellular structures.

Mechanical Performance of Glass-Based Geopolymer Matrix Composites Reinforced with Cellulose Fibers.

Glass-based geopolymers, incorporating fly ash and borosilicate glass, were processed in conditions of high alkalinity (NaOH 10⁻13 M). Different formulations (fly ash and borosilicate in mixtures of 70⁻30 wt% and 30⁻70 wt%, respectively) and physical conditions (soaking time and relative humidity) were adopted. Flexural strength and fracture toughness were assessed for samples processed in optimized conditions by three-point bending and chevron notch testing, respectively. SEM was used to evaluate the fracture micromechanisms. Results showed that the geopolymerization efficiency is strongly influenced by the SiO2/Al2O3 ratio and the curing conditions, especially the air humidity. The mechanical performances of the geopolymer samples were compared with those of cellulose fiber⁻geopolymer matrix composites with different fiber contents (1 wt%, 2 wt%, and 3 wt%). The composites exhibited higher strength and fracture resilience, with the maximum effect observed for the fiber content of 2 wt%. A chemical modification of the cellulose fiber surface was also observed.

Toughened and machinable glass matrix composites reinforced with graphene and graphene-oxide nano platelets.

The processing conditions for preparing well dispersed silica-graphene nanoplatelets and silica-graphene oxide nanoplatelets (GONP) composites were optimized using powder and colloidal processing routes. Fully dense silica-GONP composites with up to 2.5 vol% loading were consolidated using spark plasma sintering. The GONP aligned perpendicularly to the applied pressure during sintering. The fracture toughness of the composites increased linearly with increasing concentration of GONP and reached a value of ∼0.9 MPa m1/2 for 2.5 vol% loading. Various toughening mechanisms including GONP necking, GONP pull-out, crack bridging, crack deflection and crack branching were observed. GONP decreased the hardness and brittleness index (BI) of the composites by ∼30 and ∼50% respectively. The decrease in BI makes silica-GONP composites machinable compared to pure silica. When compared to silica-Carbon nanotube composites, silica-GONP composites show better process-ability and enhanced mechanical properties.