Optimal Processing Window Research Articles

Microstructure evolution and dynamic recrystallization mechanism of tantalum-tungsten alloys under hot compression

Ta-W alloys exhibit outstanding comprehensive properties at high temperatures, allowing them to have great application prospects in the high-temperature field. High-temperature compression tests (1573~1873 K) were conducted to evaluate the high-temperature mechanical properties of Ta-12W alloy, and the strain-compensated Arrhenius-Type model and hot processing map were developed to predict the optimal processing window. The electron backscatter diffraction, Transmission electron microscope, and DEFORM-3D software were performed to investigate the microstructure evolution and distributions of strain. The results demonstrated that the flow stress of Ta-12W alloy presented apparent negative temperature sensitivity and positive strain rate sensitivity. Based on the thermal processing diagrams and EBSD analysis, the results show that the low deformation temperature and high strain rate introduce stress concentration and deformation instability in the Ta-12W alloy. The optimized processing temperature and strain rate are at 1800 ~1873 K/0.001 s-1~0.05 s-1, and the microstructure at 1873 K/0.001 s-1 is more uniform and exhibits a low residual stress level. As the temperature increases, dynamic recovery and dynamic recrystallization cause significant softening effects, and continuous dynamic recrystallization dominates the high-temperature deformation behavior. Moreover, multiple continuous dynamic recrystallizations occur simultaneously, including sub-grain nucleation inside large grains, sub-grain nucleation at grain boundaries, and grain fragmentation accompanied by grain rotation. This study revealed the mechanisms of microstructural evolution during hot deformation of Ta-12W alloy, providing important guidance for optimizing the thermomechanical processing parameters.

Laser Sintering by Spot and Linear Optics for Inkjet-Printed Thin-Film Conductive Silver Patterns with the Focus on Ink-Sets and Process Parameters

The implementation of the laser sintering for inkjet-printed nanoparticles and metal organic decomposition (MOD) inks on a flexible polymeric film has been analyzed in detail. A novel approach by implementing, next to a commonly 3.2 mm diameter spot laser optic, a line laser optic with a laser beam area of 2 mm × 80 mm, demonstrates the high potential of selective laser sintering to proceed towards a fast and efficient sintering methodology in printed electronics. In this work, a multiplicity of laser parameters, primary the laser speed and the laser power, have been altered systematically to identify an optimal process window for each ink and to convert the dried and non-conductive patterns into conductive and functional silver structures. For each ink, as well as for the two laser optics, a suitable laser parameter set has been found, where a conductivity without any damage to the substrate or silver layer could be achieved. In doing so, the margin of the laser speed for both optics is ranging in between 50 mm/s and 100 mm/s, which is compatible with common inkjet printing speeds and facilitates an in-line laser sintering approach. Considering the laser power, the typical parameter range for the spot laser lays in between 10 W and 50 W, whereas for the line optics the full laser power of 200 W had to be applied. One of the nanoparticle silver inks exhibits, especially for the line laser optic, a conductivity of up to 2.22 × 107 S‧m−1, corresponding to 36% of bulk silver within a few seconds of sintering duration. Both laser sintering approaches together present a remarkable facility to use the laser either as a digital tool for sintering of defined areas by means of a spot beam or to efficiently sinter larger areas by means of a line beam. With this, the utilization of a laser sintering methodology was successfully validated as a promising approach for converting a variety of inkjet-printed silver patterns on a flexible polymeric substrate into functionalized conductive silver layers for` applications in the field of printed electronics.

Study on Hot‐Compressive Deformation Behavior and Microstructure Evolution of 12Cr10Co3MoWVNbNB Martensitic Steel

Herein, to improve the microstructure homogeneity of 12Cr10Co3MoWVNbNB steel for turbine blades after forging, the hot deformation behavior and microstructure evolution of the steel are systematically investigated using a hot‐compression experimental setup under the conditions of 950–1150 °C and strain rate of 0.001–10 s−1. A strain‐compensated constitutive equation is established based on the flow curves and the accuracy of its prediction is verified. By combining hot processing map with microstructure observation, the optimal hot processing window is determined to be 1075–1150 °C and 1–10 s−1, within which the grain size can be refined to 14.24 μm. Electron backscatter diffraction is employed to investigate the microstructural evolution and dynamic recrystallization (DRX) nucleation mechanism of the deformed samples, revealing that discontinuous DRX characterized by strain‐induced grain‐boundary migration is the dominant nucleation mechanism. Additionally, the deformation conditions significantly affect the distribution of dislocation density and local misorientation, as well as the transition from low‐angle grain boundaries to high‐angle grain boundaries, which ultimately lead to the differences in DRX fraction and microstructure.

Analysis of NCM concentration and extraction efficiency in the lithium-ion battery extraction process

In recent years, with the increasing popularity of portable electronic devices (PEDs) and electric vehicles (EVs), the demand for lithium-ion batteries (LIBs) has continued to expand; however, the supply of raw materials such as nickel cobalt, and manganese (NCM) is limited, and it is essential to develop efficient recycling technologies. Hydrometallurgical methods, particularly extraction processes, can be used to obtain high-grade recycled LIB products with proper control of the process window. This study focused on the separation of NCM from copper (Cu) and aluminum (Al) by diluting the metal concentrations ([Me]) and adjusting the pH (using NH4OH) during extraction. For metal composition analysis, in addition to using inductively coupled plasma mass spectrometry (ICP-MS), ultraviolet–visible (UV–Vis) spectroscopy and colorimetric analysis were also employed to monitor ion concentrations. The change in solution color is directly related to the nickel (Ni) and cobalt (Co) ion concentrations. Moreover, a continuous shift in the Ni ion absorption spectra at different pH values did not occur for the Co ion absorption spectra. According to the extraction efficiency (EE%) results, the lower [Me] resulted in the higher EE% of NCM. The optimal process window was established within the range of 0.025–0.1 M and pH = 6.5–7.4.

In-melt electron analysis to accelerate process exploration of ceramics: Electron beam melting of TiB2

To enhance the versatility of electron beam powder bed fusion (EB-PBF), a widely utilized additive manufacturing (AM) technique for metallic materials, we propose a novel paradigm aimed at facilitating the exploration of the process parameters for less-studied materials, such as ceramics. The high melting points and poorly understood thermal properties of ceramics have constrained the comprehension of their melting behavior. In this study, titanium diboride (TiB2) sintered bodies were subjected to spot melting under four distinct electron beam currents and four different exposure times. By introducing a novel in-melt electron analysis (IMEA) approach, the various stages of melting were clearly identified. The analysis and interpretation of IMEA signals were found to be consistent with experimental observations on the spot-melted surface of TiB2. IMEA demonstrates significant potential for real-time process window optimization and quality assurance for challenging and novel materials.

Effect of laser parameters on microstructure and mechanical properties of Al–Ni–Sc–Zr alloys fabricated by laser powder bed fusion

The processability, microstructure and mechanical properties of a near eutectic AlNiScZr alloy fabricated by laser powder bed fusion (LPBF) are investigated. The optimal processing windows for the LPBF alloy are determined. The results indicate that laser power exerts a predominant influence on the relative density of the as-built alloy. Elevated laser power can lead to increased relative density. Laser scanning speed exerts a significant impact on the microstructure and mechanical properties of the as-built alloys. An increase in the laser scanning speed can facilitate the growth of coarse columnar grains in the coarse grain region and suppress the formation of ultrafine equiaxed grain bands. Furthermore, the increase in the laser scanning speed can result in a reduction in the size of the cells, which in turn leads to an enhancement in the strength of the alloys. This study examines the evolution of the microstructure and mechanical properties of the as-built alloy as a function of laser scanning speed. By elucidating the relationship between laser parameters, microstructure and mechanical properties, the objective is to provide fundamental guidance for tuning the solidification structures and mechanical properties of LPBF AlNiScZr alloys by selecting appropriate laser parameters.

The defects and compressive behavior of NiTi alloy fabricated by laser powder bed fusion under a wide process space

A wide process space with laser power (P) of 50 ～ 400 W and scanning speed (s) of 50 ～ 2400 mm/s with the energy density (ED) range of 93–556 J/mm3 has been employed to fabricate NiTi alloy using laser powder bed fusion (LPBF). The optimal process window for near-full dense materials free of geometrical and metallurgical defects was determined. The characteristics of microstructures and compressive behaviors were comprehensively investigated. The results have shown that the process combinations of “high P + low s” and “high P + high s” are prone to bulging and warping defects due to rapid heating and cooling, respectively. A combination of “low P + low s” produces a relatively shallow melt pool without keyhole formation even at ED as high as 556 J/mm3. The austenite-martensite phase transition temperature (TTs) variations of ～80℃ were obtained with the process window free of porosity. The pre-existing martensite lath probably formed by plastic distortion (bulging) was responsible for the lowest critical stress of induced martensite (σSIM). The texture and nano-sized NiTi2/Ni2Ti4Ox precipitates also contribute to the variation of σSIM and residual strain among the samples with the same level of TTs upon compressive loading.

Thermo-mechanical processing characteristics and strain-rate-sensitive degradation properties of Mg-Er-Ni alloys

Hot deformation behavior, the corresponding microstructure evolution, and degradation properties of a weak-textured Mg-Er-Ni alloy containing a high-volume fraction of Ni-LPSO phases, have been investigated. Hot deformation behavior has been carried out in the temperatures range of 370 ∼ 460 °C and strain rates range of 0.001 ∼ 1 s−1. Flow stress-strain curves of high strain rate cases show a continuous increase trend without a steady or a peak stage, while that of low strain rate cases show an obvious dynamic softening after peak stress. Based on flow stress-strain curves, materials constants calculated by an Arrhenius-type constitutive equation, show a high n and Q compared to those of high-volume fraction α-Mg matrix Mg alloys. Optimal processing windows, based on the dynamic material model, is determined as high temperature domains. As for microstructure evolution, a complete recrystallization and dispersive Ni-LPSO fragments for high temperature & low strain rates while a restricted recrystallization and a streamline distribution LPSO phase for high temperature & high strain rates are observed. Varying degrees of continuous dynamic recrystallization, particle induced nucleation mechanism, as well as coordinated deformation of LPSO through kinking and bending account for the strain-rate-dependence hot deformation mechanism. As a result, dispersive Ni-LPSO fragments at low strain rates provide more degradation channels for the α-Mg matrix and thus possess better a degradation rate than the streamlined LPSO at high strain rates.

Microstructural Evolution and Deformation Mechanisms of In Situ TiC Reinforced Ti‐6Al‐4V Composites during High‐Temperature Hot Compression

Deformation processing is a key strategy to improve the strength‐ductility of metal matrixcomposites. Herein, TiC/TC4 composites are spark plasma sintered usingreinforcement precursors of reduced graphene oxide to reinforce TC4 matrix. Inorder to investigate the hot deformation behaviors and mechanisms of TiC/TC4 composites, the composites are hot compressed over temperature range of 870–1070 °C and strain range of 0.001–10 s−1. The results indicate that the optimal processing window of hot deformation ismainly within the temperature range of 890–970 °C and the strain rate range of 0.01–0.1 s−1. The flow instability of TiC/TC4 composites occurs in the temperature range of 890–930 and 1000–1060 °C at the strain rate range from 0.1 to 10 s−1. The thermal deformation mechanism of TiC/TC4 composites in the processingwindow region involves continuous dynamic recrystallization and discontinuous dynamic recrystallization. TiC can effectively hinder thedislocation motion, leading to the generation of high‐density dislocationsaround TiC. Consequently, this promotes sub‐grains formation and rotation,facilitating CDRX. Meanwhile, TiC particle induces high‐angle grain boundarymigration and provides more nucleation sites for recrystallized grains. These findings enhance understanding the role of hot deformation behaviors of Ti compositesand provide insights into their deformation processing.

Experimental investigation on process parameters of laser-assisted robotic roller bending of a thin-walled structure

Laser-assisted robotic roller forming (LRRF) combines the process capabilities of robot-based manufacturing and laser-assisted forming. In this work, the LRRF process was applied to bending DP1180 steel sheets to thin-walled structures designed for seat trails. Comprehensive experimental investigations were conducted to explore the influences of laser power, forming passes and scanning speed on the forming forces, springback and bending radii of final parts. Experimental results show that the effects of process parameters on the springback and bending radii are similar to those on the forming forces, while forming passes make an insignificant difference to the springback. The optimized process window was subsequently determined out of the balance between geometrical accuracy and experimental efficiency. By applying the optimized process parameters (laser power of 750 W, 6 forming passes, scanning speed of 5 mm/s), the peak force during LRRF was reduced to ∼2.1kN. Meanwhile, a thin-walled profile with higher precision was achieved. Specifically, the springback angle was reduced to ∼4.1° and a compact profile with a radius-to-thickness ratio of ∼1.0 was obtained.

Prediction of flow stress in Mg-3Dy alloy based on constitutive equation and PSO-SVR model

This study conducted hot compression experiments on as-cast Mg-3Dy alloy under deformation parameters of 380 °C–470 °C and 0.001–1 s−1. The microstructure of the alloy was observed using EBSD, and the flow stress of the Mg-3Dy alloy was predicted using the Arrhenius model and the particle swarm optimization-support vector regression (PSO-SVR) model. The organizational analysis results showed that the main recrystallization mechanism in the alloy is the discontinuous dynamic recrystallization (DDRX) mechanism. The generation of twins in the alloy was mostly the result of local stress action. The optimal processing window for this alloy was determined to be 380 °C–470 °C and 0.001–0.01 s−1 through the thermal processing map. The prediction accuracies of the Arrhenius model and PSO-SVR model were evaluated using the correlation coefficient R2 and mean squared error MSE. The results showed that the PSO-SVR model significantly outperforms the Arrhenius model in prediction accuracy, with R2 value of 0.99982 and MSE of 0.074.

Construction of a Predictive Model for Dynamic and Static Recrystallization Kinetics of Cast TC21 Titanium Alloy

In this study, hot compression experiments were conducted on cast TC21 titanium alloy using a Gleeble-1500D thermal simulation compression tester, and the hot-compressed specimens were heat-treated. The data obtained after analyzing the thermal compression of cast TC21 titanium alloy were analyzed to construct a thermal machining diagram with a strain of 0.8 and to optimize the machining window. This study investigated the microstructure of the alloy after hot pressing experiments and heat treatment, applying the study of the microstructure evolution law of cast TC21 titanium alloy. The analysis of the tissue evolution law established the dynamic and static recrystallization volume fraction as a function of heat deformation parameters. The results show that the optimal processing window for cast TC21 titanium alloy is a deformation temperature in the range of 1373 K–1423 K and a strain rate of 0.1 s−1. The increase in deformation volume and deformation temperature both favor recrystallization and make the recrystallization volume fraction increase, but the increase in strain rate will inhibit the increase in the recrystallization degree to some extent. The dynamic and static recrystallization equations for the cast TC21 titanium alloy at different temperatures were constructed. The experimental measurements of recrystallization volume fraction are in good agreement with the predicted values.

Development and characterization of 3D-printed electroconductive pHEMA-co-MAA NP-laden hydrogels for tissue engineering

AbstractTissue engineering (TE) continues to be widely explored as a potential solution to meet critical clinical needs for diseased tissue replacement and tissue regeneration. In this study, we developed a poly(2-hydroxyethyl methacrylate-co-methacrylic acid) (pHEMA-co-MAA) based hydrogel loaded with newly synthesized conductive poly(3,4-ethylene-dioxythiophene) (PEDOT) and polypyrrole (PPy) nanoparticles (NPs), and subsequently processed these hydrogels into tissue engineered constructs via three-dimensional (3D) printing. The presence of the NPs was critical as they altered the rheological properties during printing. However, all samples exhibited suitable shear thinning properties, allowing for the development of an optimized processing window for 3D printing. Samples were 3D printed into pre-determined disk-shaped configurations of 2 and 10 mm in height and diameter, respectively. We observed that the NPs disrupted the gel crosslinking efficiencies, leading to shorter degradation times and compressive mechanical properties ranging between 450 and 550 kPa. The conductivity of the printed hydrogels increased along with the NP concentration to (5.10±0.37)×10−7 S/cm. In vitro studies with cortical astrocyte cell cultures demonstrated that exposure to the pHEMA-co-MAA NP hydrogels yielded high cellular viability and proliferation rates. Finally, hydrogel antimicrobial studies with staphylococcus epidermidis bacteria revealed that the developed hydrogels affected bacterial growth. Taken together, these materials show promise for various TE strategies. Graphic abstract

Role of heterogenous microstructure and deformation behavior in achieving superior strength-ductility synergy in zinc fabricated via laser powder bed fusion

Zinc (Zn) is considered a promising biodegradable metal for implant applications due to its appropriate degradability and favorable osteogenesis properties. In this work, laser powder bed fusion (LPBF) additive manufacturing was employed to fabricate pure Zn with a heterogeneous microstructure and exceptional strength-ductility synergy. An optimized processing window of LPBF was established for printing Zn samples with relative densities greater than 99% using a laser power range of 80 ∼ 90 W and a scanning speed of 900 mm s−1. The Zn sample printed with a power of 80 W at a speed of 900 mm s−1 exhibited a hierarchical heterogeneous microstructure consisting of millimeter-scale molten pool boundaries, micrometer-scale bimodal grains, and nanometer-scale pre-existing dislocations, due to rapid cooling rates and significant thermal gradients formed in the molten pools. The printed sample exhibited the highest ductility of ∼12.1% among all reported LPBF-printed pure Zn to date with appreciable ultimate tensile strength (∼128.7 MPa). Such superior strength-ductility synergy can be attributed to the presence of multiple deformation mechanisms that are primarily governed by heterogeneous deformation-induced hardening resulting from the alternative arrangement of bimodal Zn grains with pre-existing dislocations. Additionally, continuous strain hardening was facilitated through the interactions between deformation twins, grains and dislocations as strain accumulated, further contributing to the superior strength-ductility synergy. These findings provide valuable insights into the deformation behavior and mechanisms underlying exceptional mechanical properties of LPBF-printed Zn and its alloys for implant applications.

Predictive process diagram for parameters selection in laser powder bed fusion to achieve high-density and low-cracking built parts

The laser powder bed fusion process (LPBF) has been widely used in many industrial sectors, including automotive, aerospace, and biomedical devices. With the fast development of new materials designed for critical applications, the conventional design of experiments for determining an optimal LPBF process window is a time and material-consuming activity. This can impose difficulties on small-to-medium industrial businesses where investing resources are limited. To address these challenges, this study draws inspiration from a reliable diagram used in laser welding to construct a similar diagram for the LPBF process. The objective is to enable the "right-first-time" selection of parameters that achieve a minimum of 99% density, regardless of the metallic materials and machine platforms. The diagram is established based on dimensionless beam power and velocity, derived from multiple LPBF process parameters (e.g., laser power, scan speed, hatch spacing) and the thermophysical properties of materials (e.g., melting point, density, thermal diffusivity). Furthermore, hot cracking susceptibility is considered by a strain-rate approach incorporated with the dimensionless thermal strain factor, which benefits when processing hard-to-weld alloys. The diagram shows high reliability in determining parameters corresponding to lack of fusion, keyhole porosity and 99% dense parts when plotting against literature data of LPBF for several metallic materials. Similar results were observed when applying to a novel material ABD-900AM Ni-based alloy, for which no previously published data were available. Moreover, the diagram proved effective in selecting parameters to process the high-cracking susceptible CM247LC Ni-based alloy, resulting in significant mitigation of hot cracking in the as-fabricated parts.

Optimizing LPBF-parameters by Box-Behnken design for printing crack-free and dense high-boron alloyed stainless steel parts

Boron has almost null solubility in iron, and its addition to stainless steels leads to the formation of hard borides, beneficial for increasing the wear resistance. However, these boron-containing steels have poor printability, with the occurrence of pronounced cracking, high porosity and risk of delamination. In this work, Box-Behnken design coupled with analysis of variance (ANOVA) was used to optimize the LPBF (Laser Powder Bed Fusion) processing parameters of a highly boron-alloyed stainless steel reinforced with a boride network. The proposed models demonstrated to be accurate in determine the porosity percentage for the studied alloys, in which the laser power and scanning speed play the main role in the alloys’ densification, and absence of extensive defects. These results indicate that the use of design of experiments tools is essential to produce defect-free boron-modified stainless steel specimens with a relatively low number of experiments, identifying a narrow optimized processing window to build bulk composite materials.

Intelligent femtosecond laser bone drilling via online monitoring and machine learning

In conventional spinal surgeries, mechanical and thermal injuries frequently usually arise due to improper handling, giving rise to a range of complications including infection, poor wound healing and bleeding. Femtosecond laser ablation offers a promising approach owing to high precision and low thermal damage. In this study, an intelligent femtosecond laser drilling method of human spinal bones has been proposed, and a machine learning method has been employed to determine the optimal laser processing window, ensuring high-quality outcomes. A neural network model has been developed to predict drilling quality, achieving an impressive accuracy rate exceeding 98 %, along with precision and recall rates of 100 % and 92.86 %, respectively. To further monitor the process, a fiber spectrometer and a thermal camera has been employed to monitor the focal status and bone temperature during laser processing to make sure the drilling is in a focal position and temperature in safe range. Subsequently, the drilling efficiency has been predicted using another neural network model within high-quality processing window for the maximum ablation processing parameter. The current research has demonstrated a direct, non-destructive and efficient method for intelligent laser spinal drilling.

Deposition processes of superhard diamond-like carbon films co-adjusted by ion energy and ion flux in arc discharges

As a kind of protective material, Diamond-Like Carbon (DLC) film can effectively improve the mechanical and tribological properties of the substrate surface. In DLC family, tetrahedral amorphous carbon (ta-C) with ultra-high hardness and excellent protective properties has been widely concerned in the field of hard protective materials. It is well known that the structure and properties of ta-C are strongly dependent on carbon plasma characteristics in the plasma environment. Therefore, it is extremely crucial to obtain the optimal process window of ta-C described by plasma micro-parameters with general significance. This paper proposed the Langmuir probe was used to diagnose the carbon plasma of the afterglow generated by arc evaporation, aiming to investigate the characteristics of carbon plasma and sheath. The effect of ion energy and ion flux adjusted by the pulse bias voltage and arc current on the sp3 hybrid bonds and hardness of DLC films was studied, aiming to find out which conditions satisfied the formation of ta-C. The results showed the microstructure and properties of DLC films were co-adjusted by ion energy and ion flux. When the carbon ions met the appropriate ion energy range (50–300 eV) and low ion flux (<8.99 × 1010 cm−2 s−1), the films tended to form ta-C structures with high sp3 bonds. However, under the condition of high ion energy and high ion flux, the structure of the films changed from sp3 bonds to sp2 bonds, resulting in the graphitization and formation of DLC films with high sp2 bonds. This work will provide new solutions to guide the design and acquisition of high-performance DLC films.

Development of a low-density Co-Ni-Al-Ta-Cr superalloy with high mechanical performance and superior oxidation resistance

In this study, a Co-30Ni-10Al-6Ta-10Cr alloy was designed based on CALPHAD (Calculation of Phase Diagrams) method targeting high γ′ phase fraction and solvus, and optimal thermal processing window. Experimental results concurred with the calculations and validated Cr as a γ phase-forming element in Co-Ni-Al-Ta-based alloys. The incorporation of Cr in the alloy helps mitigate lattice misfit, coarsening rate, and alloy density, while enhancing microstructural stability. A certain amount of Cr led to the development of a superalloy with both high mechanical performance γ′ solvus and low density. Moreover, the oxidation resistance of the Co-Ni-Al-Ta-based high-temperature alloy can be substantially elevated by the introduction of Cr. At 1000 °C, the Co-30Ni-10Al-6Ta-10Cr alloy displayed comparatively low oxidation weight gain, which signifies its excellent oxidation resistance. This is mainly attributed to the formation of continuous (Co,Ni)(Al,Cr)2O4 spinel oxide layers during prolonged oxidation.

Process window for manufacturing soft magnetic FeSi 6.5% by laser metal deposition

This study introduces Laser Metal Deposition (LMD) for the first time in manufacturing FeSi 6.5%, a crucial soft magnetic material. The investigation focuses on the impact of energy density on fabrication, emphasizing porosity, crack formation, and identifying an optimal processing window. Results reveal a significant correlation between energy density and defects. An increase in energy density from 54 to 82 J/mm^2 leads to pronounced porosity and cracks. However, within 61 to 68 J/mm^2, an optimal processing window emerges, ensuring minimal defects (&lt; 0.3% porosity) and crack-free structures. Notably, manufacturing high silicon-content electrical steels without cracks is extremely challenging, but this study achieves it. Through systematic analysis, this research underscores the vital role of energy density in shaping the quality of FeSi 6.5% thin walls parts. These insights improve LMD parameters, advancing the manufacturing of soft magnetic materials.