Isothermal Aging Research Articles

Evolution of new topologically close-packed phases P and R upon long-term isothermal aging of laser powder bed fusion processed Hastelloy X

Evolution of new topologically close-packed phases P and R upon long-term isothermal aging of laser powder bed fusion processed Hastelloy X

Tensile Strength Property with PdCo-Cu Multi-Layer Lamination and Heat Treatment of MEMS Probe for Probe Card

Cantilever wire probe card has limited to transport high-speed signal because of long wire but it is suitable for inspecting high-current and high voltage semiconductor such as wide band gap (WBG) power semiconductors.Superior mechanical property of a probe card wire is in demand because it is respectively used wafer inspection with in and out pad on the top surface of the power semiconductor wafer. Therefore, in this study, tensile specimens of micro electro-mechanical systems (MEMS) probe alternatively layered and electroplated with palladium (Pd)-cobalt (Co) alloy layers and copper (Cu) layers. MEMS probe was also measured tensile strength and elongation with multi-lamination and heat treatment conditions. Additionally, fractography of fracture surface after tensile test were analyzed using a scanning electron microscope (SEM). As the number of PdCo-Cu multi-layer increased, 11, 15 and 21 layered specimens showed higher tensile strength and longer elongation than 5 layered specimens because of the increase of laminated interface of PdCo and Cu. 7 layered specimen after isothermal aging had higher tensile strength and longer elongation than before isothermal aging. In 5, 11, 15 and 21 layered specimens, the fracture surfaces of tensile test specimens without aging treatment showed a ductile-brittle mixed fracture mode. Fracture surfaces of 7-layered specimen before and after isothermal aging showed a ductile-brittle mixed fracture mode.

Changes in Intermetallic Compounds and Mechanical Performance of Steel/Aluminum Welded Joints Containing Nano TiC during Isothermal Aging

Changes in Intermetallic Compounds and Mechanical Performance of Steel/Aluminum Welded Joints Containing Nano TiC during Isothermal Aging

Phase transformation kinetics in Ti 575 titanium alloy during heat treatment: Role of the initial microstructure during ageing

Phase transformation kinetics were studied of Ti-575 titanium alloy during cooling from solution annealing and subsequent ageing using in-situ high energy X-ray diffraction. Cooling rates of 1.7, 10 and 30 °C·s−1 were applied from Tβ-60 °C therefore generating several microstructures with different size, morphologies or spatial distribution of α precipitates. Isothermal ageing at 500 °C for 1 h on these three microstructures allowed the study of the influence of the initial microstructural state upon phase transformation during ageing. For this purpose, the combined analysis of mass fraction, aβ mean lattice parameter and full width at half maximum is carried out for both cooling and ageing segment and is presented in this study. Displacive and diffusion-controlled transformations were recorded and seem to be cooling rate dependent, particularly with the precipitation of the α″ orthorhombic phase. The chemical and mechanical evolution of these transformation products will influence the phase transformation kinetics during cooling and following ageing hence conditioning the final microstructure and mechanical properties of this alloy.

Experimental study of Lannea microcarpa seed oil as a heat transfer fluid or thermal energy storage material for medium-temperature applications

In this study, we investigated the suitability of Lannea microcarpa seed oil (LaMSO) as a heat transfer fluid (HTF) and thermal energy storage material (TESM) for medium-temperature applications, focusing on its performance in concentrated solar power (CSP) plants. LaMSO demonstrated higher specific heat capacity than both Dowtherm A and Xceltherm 600 across the temperature range of 30 °C to 300 °C. It also exhibited a volumetric thermal energy storage density similar to, or approximately 10 % greater than, that of Dowtherm A and Xceltherm 600 at 210 °C. The oil was subjected to isothermal aging at 210 °C for 500 h and 1000 h, followed by analysis of its thermophysical and chemical properties. Thermogravimetric analysis demonstrated excellent thermal stability, with less than 3 % mass loss after 1000 h of aging. The density remained relatively unchanged, indicating consistent performance as a HTF or TESM. Despite an increase in viscosity at 40 °C, the viscosity at 100 °C remained comparable between the new and aged LaMSO samples. Furthermore, the flash point also showed no significant change, remaining high even after 1000 h of aging. However, challenges arise from the increase in the melting point due to oil saturation, which poses a risk of solidification in pipelines or tanks in certain climates. From the perspective of thermal storage cost per kWh, LaMSO is cheaper than Dowtherm A and Xceltherm 600, being approximately 8 times and 3 times less expensive, respectively. Overall, the findings suggest that LaMSO holds promise as an effective and sustainable alternative for HTF and TESM applications across a wide temperature range, contributing to advancements in renewable energy technology.

Microstructural Evolution of Intermetallic Compound Between SN100C Solder and ENIMAG Substrate During Isothermal Ageing

SN100C alloy emerges as a promising candidate when introducing lead-free solder alternativesdue to its mechanical properties and solderability. The study aims to explore interfacial reactions between SN100C solder and ENIMAG surface finish. Methods involve preparingENIMAG substrates, solder paste application, and reflow processes following JEDEC standards. Isothermal ageing treatments were conducted, and interfacial reactions were characterized using top surface and cross-section analyses via Optical Microscope (OM), Scanning Electron Microscope (SEM), and Energy Dispersive X-ray (EDX). Post-reflow, distinct IMC layers formed at the SN100C/ENIMAG solder joint's interface, evolving with ageing. Further analysis via cross-section confirms the initial formation of (Ni, Cu)3Sn4 layer followed by (Cu, Ni)6Sn5, each exhibiting varying appearance and thicknesses. Isothermal ageing increases IMC thickness, which is particularly influenced by Cu diffusion and exposure to high temperatures, and itfacilitates the growth rate of IMCs.

Order phase transition of HIP nickel-based powder superalloy during isothermal aging

Nickel-based powder superalloys have become one of key materials for aerospace turbine engines due to their excellent comprehensive properties. The microstructure stability during long-term isothermal aging is closely related to mechanical properties. The correlation between order phase transition and mechanical properties of a HIP (hot isostatic pressing) nickel-based powder superalloy after long-term isothermal aging treatment was investigated. The results show that the decomposition of MC carbides and precipitation, growth and coarsening of γ' phases occur with duration of isothermal aging. Tertiary γ' phases precipitates by the way of element diffusion with γ' phases coarsening. In addition, strengthening mechanism is quantitatively calculated, and the relative contribution of γ' phases to yield strength is largest, and multi-mode size of γ' phases are favorable to yield strength and hardness of HIP nickel-based powder superalloy.

Effects of non-isothermal aging and microalloying on precipitation strengthening for Al-Mg-Si alloys

The impacts of non-isothermal aging (NIA) and microalloying (Ag and/or Cu) on precipitation strengthening and mechanical properties in Al-Mg-Si alloys are investigated using advanced microscopic analysis techniques combined with tensile testing. The NIA treatment exhibits different age hardening for this alloy with different compositions. The Ag-Cu-added A3 alloy exhibits the most significant enhancement in peak hardness under NIA treatment than that of the isothermal aging (IA), while only marginal increases are observed for the other alloys (the base A1 alloy and the Cu/Ag-added alloys). The optimal NIA treatment for the Ag-Cu-added A3 alloy is identified as follows: 200 oC × 1h + cooling down to 180 oC at 20oC/h. This specific treatment leads to a peak hardness of 139.0 HV and an ultimate tensile strength of 384.0MPa for this alloy, which is 16.0 HV higher than that of the base Al-Mg-Si alloy when subjected to IA at 180oC. These findings provide valuable insights for the advancement of novel aluminum alloys and heat treatment methodologies.

Effects of aging on mechanical sensitivity threshold and thermal decomposition characteristic of RDX/HMX

In order to analyze the influences of storage aging on the safety of typical elemental explosives, the aged cyclotrimethylene trinitramine (RDX) and cyclotetramethylene tetranitramine (HMX) were prepared by isothermal aging tests. The reaction thresholds of aged RDX and HMX under any ignition probability were studied by Langlie-Optimal D method. The thermal decomposition characteristics of RDX and HMX after aging were analyzed by DSC and ARC. Experimental results showed that compared with unaged RDX and HMX, on the one hand, the critical impact energy and critical friction of RDX and HMX aged for 14, 28 and 56 days are significantly reduced at an explosion probability of 50%, 0.01% and 0.0001%, respectively. With the increase of aging time, the mechanical sensitivity of RDX and HMX increases obviously. On the other hand, the initial decomposition temperature of RDX and HMX after 56 days of aging decreases, the decomposition heat decreases, the activation energy increases, and the reaction difficulty increases.

The effect of N addition on the micro-structure and corrosion resistance of modified 6Mo super austenitic stainless steels during isothermal aging treatment

The effect of N addition on the micro-structure and corrosion resistance of modified 6Mo super austenitic stainless steels during isothermal aging treatment

Study on Thermal Oxygen Aging Characteristics and Degradation Kinetics of PMR350 Resin.

The thermal stability and aging kinetics of polyimides have garnered significant research attention. As a newly developed class of high thermal stability polyimide, the thermal aging characteristics and degradation kinetics of phenylene-capped polyimide prepolymer (PMR350) have not yet been reported. In this article, the thermo-oxidative stability of PMR350 was investigated systematically. The thermal degradation kinetics of PMR350 resin under different atmospheres were also analyzed using the Flynn-Wall-Ozawa method, the Kissinger-Akahira-Sunose method, and the Friedman method. Thermogravimetric analysis (TGA) results revealed that the 5% thermal decomposition temperature (Td5%) of PMR350 in a nitrogen atmosphere was 29 °C higher than that in air, and the maximum thermal degradation rate was 0.0025%/°C, which is only one-seventh of that observed in air. Isothermal oxidative aging results indicated that the weight loss rate of PMR350 and the time-dependence relationship follow a first-order exponential growth function. PMR350 resin thermal decomposition reaction under air atmosphere includes one stage, with a degradation activation energy of approximately 57 kJ/mol. The reaction model g(α) fits the F2 model, and the integral form is given by g(α) = 1/(1 - α). In contrast, the thermal decomposition reaction under a nitrogen atmosphere consists of two stages, with degradation activation energies of 240 kJ/mol and 200 kJ/mol, respectively. The reaction models g(α) correspond to the A2 and D3 models, with the integral forms represented as g(α) = [-ln(1 - α)]2 and g(α) = [1 - (1 - α)1/3]2 due to the oxygen accelerating thermal degradation from multiple perspectives. Moreover, PMR350 resin maintained high hardness and modulus even after thermal aging at 350 °C for 300 h. The results indicate that the resin exhibits excellent resistance to thermal and oxygen aging. This study represents the first systematic analysis of the thermal stability characteristics of PMR350 resin, offering essential theoretical insights and data support for understanding the mechanisms of thermal stability modification in PMR350 and its engineering applications.

Effects of Minor Zn Dopants in Sn-10Bi Solder on Interfacial Reaction and Shear Properties of Solder on Ni/Au Surface Finish.

Sn-10Bi low-bismuth-content solder alloy provides a potential alternative to the currently used Sn-Ag-Cu series due to its lower cost, excellent ductility, and strengthening resulting from the Bi solid solution and precipitation. This study primarily investigates the interfacial evolution and shear strength characteristics of Sn-10Bi joints on a Ni/Au surface finish during the as-soldered and subsequent isothermal aging processes. To improve the joint performance, a 0.2 or 0.5 wt.% dopant of Zn was incorporated into Sn-10Bi solder. The findings demonstrated that a 0.2 or 0.5 wt.% Zn dopant altered the composition of the intermetallic compound (IMC) formed at the interface between the solder and Ni/Au surface finish from Ni3Sn4 to Ni3(Sn, Zn)4. The occurrence of this transformation is attributed to the diffusion of Zn atoms into the Ni3Sn4 lattice, resulting in the substitution of a portion of the Sn atoms by Zn atoms, thereby forming the Ni3(Sn, Zn)4 IMC during the soldering process, which was also verified by calculations based on first principles. Furthermore, a 0.2 or 0.5 wt.% Zn dopant in Sn-10Bi significantly inhibited the Ni3(Sn, Zn)4 growth after both the soldering and thermal aging processes. Zn addition can enhance the shear strength of solder joints irrespective of the as-soldered or aging condition. The fracture mode was determined by the aging durations-with the brittle mode occurring for as-soldered joints, the ductile mode occurring for aged joints after 10 days, and again the brittle mode for joints after 40 days of aging.

Tuning α precipitation via post-heat treatments in direct energy deposited metastable β Ti-5Al-5Mo-5V-3Cr alloy and its impact on mechanical properties

In this study, the strength and ductility of a direct energy deposited (DEDed) metastable β Ti-5Al-5Mo-5 V-3Cr (wt%, Ti-5553) alloy was explored by tuning the formation of various α microstructures through post-heat treatments. The microstructure of DEDed Ti-5553 with and without post-heat treatments was systematically studied using scanning electron microscopy, three-dimensional (3D) focused ion beam-scanning electron microscopy tomography, transmission electron microscopy, scanning transmission electron microscopy, and atom probe tomography. Nanoscale ω phase and O′ phase particles were observed in the as-built DEDed Ti-5553 without post-heat treatment for the first time. By altering the aging temperatures and heating rates during post-heat treatments, various microstructural evolution pathways were activated, leading to α microstructures with different sizescales, morphologies, and number densities. By fast heating and isothermal aging at 600°C for 2 hours, refined α microstructure was formed through the pseudospinodal decomposition mechanism. While slow heating (at the heating rates of 5 °C/min or 0.5 °C/min) to 600°C and isothermal aging for 2 hours, super-refined α microstructures were produced respectively, primarily via ω-assisted and O′-assisted α precipitation mechanisms. By fast heating to and isothermal aging at 700°C, fine-scaled intragranular α microstructure was formed, dramatically different in morphology and sizescale from the coarse α microstructure formed in the casted Ti-5553, which is suspected to be related to the indirect influence of nanoscale isothermal ω phase particles formed during the DED process and the excess oxygen introduced during the DED process. With fast heating to and isothermal aging at 800°C, coarse α microstructure forms through the classical nucleation and growth mechanism. Various α microstructures led to a drastic change of mechanical properties with improvements up to a 55 % increase in hardness and 92 % increase in tensile yield strength, compared with as-built DEDed Ti-5553. Our work indicates the feasibility of achieving tailored mechanical properties in DEDed metastable β-Ti alloys by tuning α microstructures through selectively activating various phase transformation mechanisms via post-heat treatments.

Microscopic mechanism of the L12–D019 phase transformation in a Co-base single crystal superalloy

In γ′-strengthened superalloys based on the Co-Al-W system, the stability of the γ′ phase is often limited, as it is found to transform into other phases such as B2 and D019 after long-term annealing. To explore the details behind the annealing-induced transformation from the metastable L12-γ′ phase to the thermodynamically stable D019-χ phase in the single-crystalline Co-base superalloy ERBOCo-VF60 (Co79.8Al8.9W9.0Ta2.3 in at.%), scanning transmission electron microscopy and atom probe tomography are employed. Due to the structural similarity between the L12 and D019 structures, coherent plate-shaped χ precipitates are formed in the γ/γ′ microstructure parallel to {111} planes through a shear-based transformation mechanism. While the χ phase precipitates slowly during isothermal aging, its formation can be significantly accelerated locally by coating the superalloy with a Cr-rich layer, which indirectly stabilizes the χ phase as revealed by thermodynamic calculations. This procedure allowed us to obtain an intermediate (incomplete) state of χ-phase formation in terms of both crystal structure and composition. By characterizing the partial dislocations at the tip of growing χ precipitates, the microscopic details of the shear-based cubic-to-hexagonal transformation from L12 to D019 are uncovered. The compositional aspect of the transformation involves a significant diffusion-mediated enrichment of W in the χ phase, accompanied by a simultaneous W depletion in the γ′ phase, leading to its transformation to the γ phase.

Microstructural Dependence of the Impact Toughness of TP316H Stainless Steel Exposed to Thermal Aging and Room-Temperature Electrolytic Hydrogenation.

This work deals with the effects of two individual isothermal aging experiments (450 °C/5000 h and 700 °C/2500 h) and the subsequent room-temperature electrolytic hydrogen charging of TP316H stainless steel on its Charpy V-notch (CVN) impact toughness and fracture behavior at room temperature. Microstructural analyses revealed that aging at 700 °C resulted in the abundant precipitation of intermediary phases, namely, the Cr23C6-based carbide phase and Fe2Mo-based Laves phase, whereas aging at 450 °C resulted in much less pronounced precipitation of mostly intergranular Cr23C6-based carbides. The matrix phase of 700 °C-aged material was completely formed of austenitic solid solution with a face-centered cubic (FCC) crystal structure, whereas an additional formation of ferritic phase with a base-centered cubic (BCC) structure was detected in 450 °C-aged material. The performed microstructure observations correlated well with the obtained values of CVN impact toughness, i.e., a sharp drop in the impact toughness was observed in the material aged at 700 °C, whereas negligible property changes were observed in the material aged at 450 °C. The initial, solution-annealed (precipitation-free) TP316H material exhibited a notable hydrogen toughening effect after hydrogen charging, which has been attributed to the hydrogen-enhanced twinning-induced plasticity (TWIP) deformation mechanism of the austenitic solid solution. In contrast, both aging expositions resulted in significantly lowered hydrogen embrittlement resistance, which was likely caused by hydrogen trapping effects at the precipitate/matrix interfaces in thermally aged materials, leading to a reduced TWIP effect in the austenitic phase.

Significantly enhancing the ductility of high-strength Cu-15Ni-8Sn alloy via an optimized combined process of deformation and heat treatment

The Cu-15Ni-8Sn alloy (UNS C72900) is a vital material for the manufacturing of precision instrument components. Employing the conventional process of “solution treatment + large cold deformation + isothermal aging” can result in a tensile strength exceeding 1200 MPa but a mere elongation of approximately 2.0 %. To enhance the reliability and service life of the Cu-15Ni-8Sn alloy, this study proposed an optimized process involving “solution treatment + large cold deformation + recrystallization heat treatment + small cold deformation + heating aging” to obtain low dislocation density, fine grains and precipitates, and uniform element distribution, thereby significantly enhancing the ductility while maintaining high strength. Compared to the conventional process, the total elongation under the optimized process was increased from 2.0 % to 11.7 %, while the tensile strength was slightly decreased from 1214 MPa to 1191 MPa. This study could offer optimized insights into the comprehensive mechanical property improvement of spinodal decomposition strengthened copper alloys.

Precipitation behavior and strengthening mechanism in a Cu-3.5Ti-0.1 Tm alloy

The study investigates the complex relationship between precipitation patterns, microstructural evolution, and mechanical properties in a Cu-3.5Ti-0.1 Tm alloy subjected to isothermal ageing. The results reveal that ageing at 450 °C leads to the formation of nanoscale β′-Cu4Ti phase particles within the grains and fibrous β-Cu4Ti precipitates along the grain boundaries. The precipitation microstructure of this aged alloy is predominantly characterised by tetragonal β′-Cu4Ti precipitates. During spinodal decomposition, Ti atoms segregate in rod-like Ti-rich Cu phases, facilitating their conversion into β′-Cu4Ti phase. The β′-Cu4Ti precipitates remain fully coherent with the Cu matrix, exhibiting a crystallographic orientation relationship of (001)Cu//(001)β′ and [100]Cu//[130]β′. As the precipitate radius exceeds approximately 11 nm, the elastic strain energy surpasses the energy at the precipitate/matrix interface. This leads to a shape transition from spherical to cuboidal for the β′-Cu4Ti precipitates. Moreover, the Ti solute atoms contribute significantly to the alloy's strength through solid solution hardening, with the dissolution of 1 at.% Ti solute increases the yield strength by 46.2 MPa. However, as ageing progresses from 1 to 20 h, the effect of solid solution strengthening decreases, while precipitation strengthening becomes more dominant, mainly due to the Orowan bypass mechanism. After 20 h of ageing, precipitation strengthening significantly increases the yield strength by about 436 MPa, exceeding the contributions from solid solution strengthening (78 MPa) and grain-boundary strengthening (14 MPa).

Interfacial IMC growth behavior of Sn-3Ag-3Sb-xIn solder on Cu substrate

PurposeThe reliability of solder joints is closely related to the growth of an intermetallic compound (IMC) layer between the lead-free solder and substrate interface. This paper aims to investigate the growth behavior of the interfacial IMC layer during isothermal aging at 125°C for Sn-3Ag-3Sb-xIn/Cu (x = 0, 1, 2, 3, 4, 5 Wt.%) solder joints with different In contents and commercial Sn-3Ag-0.5Cu/Cu solder joints.Design/methodology/approachIn this paper, Sn-3Ag-3Sb-xIn/Cu (x = 0, 1, 2, 3, 4, 5 Wt.%) and commercial Sn-3Ag-0.5Cu/Cu solder were prepared for bonding Cu substrate. Then these samples were subjected to isothermal aging for 0, 2, 8, 14, 25 and 45 days. Scanning electron microscopy and transmission electron microscopy were used to analyze the soldering interface reaction and the difference in IMC growth behavior during the isothermal aging process.FindingsWhen the concentration of In in the Sn-3Ag-3Sb-xIn/Cu solder joints exceeded 2 Wt.%, a substantial amount of InSb particles were produced. These particles acted as a diffusion barrier, impeding the growth of the IMC layer at the interface. The growth of the Cu3Sn layer during the aging process was strongly correlated with the presence of In. The growth rate of the Cu3Sn layer was significantly reduced when the In concentration exceeded 3 Wt.%.Originality/valueThe addition of In promotes the formation of InSb particles in Sn-3Ag-3Sb-xIn/Cu solder joints. These particles limit the growth of the total IMC layer, while a higher In content also slows the growth of the Cu3Sn layer. This study is significant for designing alloy compositions for new high-reliability solders.

Isothermal aging and electromigration reliability of Cu pillar bumps interconnections in advanced packages monitored by in-situ dynamic resistance testing

Cu pillar bump (CPB) technology as the representative advanced packaging technology possesses the characteristics of miniaturization and high density, thus playing an important role in the reliability of electronic devices. However, the brittle intermetallic compound (IMC) layer in the joints evidently affects the service performance and reliability of CPB joints. Thus, the influence of IMC layer thickness and microstructure needs to be carefully evaluated. In this study, the reliability of CPB joints with different IMC layer thickness under the condition of isothermal storage and room-temperature electromigration was tested, and the effect of initial IMC thickness of joints on the reliability was revealed. The full-IMC joints have the best isothermal storage reliability while the half-IMC joints perform the worst. Meanwhile, the thin-IMC joints own the best electromigration reliability but the full-IMC joints show the worst because that the initial voids in full-IMC joints accelerate the failure caused by electromigration.

Reliability Risk Mitigation in Advanced Packages by Aging-Induced Precipitation of Bi in Water-Quenched Sn-Ag-Cu-Bi Solder.

Bi-doped Sn-Ag-Cu (SAC) microelectronic solder is gaining attention for its utility as a material for solder joints that connect substrates to printed circuit boards (PCB) in future advanced packages, as Bi-doped SAC is reported to have a lower melting temperature, higher strength, higher wettability on conducting pads, and lower intermetallic compound (IMC) formation at the solder-pad interface. As solder joints are subjected to aging during their service life, an investigation of aging-induced changes in the microstructure and mechanical properties of the solder alloy is needed before its wider acceptance in advanced packages. This study focuses on the effects of 1 to 3 wt.% Bi doping in an Sn-3.0Ag-0.5Cu (SAC305) solder alloy on aging-induced changes in hardness and creep resistance for samples prepared by high cooling rates (>5 °C/s). The specimens were aged at ambient and elevated temperatures for up to 90 days and subjected to quasistatic nanoindentation to determine hardness and nanoscale dynamic nanoindentation to determine creep behavior. The microstructural evolution was investigated with a scanning electron microscope in tandem with energy-dispersive spectroscopy to correlate with aging-induced property changes. The hardness and creep strength of the samples were found to increase as the Bi content increased. Moreover, the hardness and creep strength of the 0-1 wt.% Bi-doped SAC305 was significantly reduced with aging, while that of the 2-3 wt.% Bi-doped SAC305 increased with aging. The changes in these properties with aging were correlated to the interplay of multiple hardening and softening mechanisms. In particular, for 2-3 wt.% Bi, the enhanced performance was attributed to the potential formation of additional Ag3Sn IMCs with aging due to non-equilibrium solidification and the more uniform distribution of Bi precipitates. The observations that 2-3 wt.% Bi enhances the hardness and creep strength of the SAC305 alloy with isothermal aging to mitigate reliability risks is relevant for solder samples prepared using high cooling rates.