Compound Layer Research Articles

Grain refinement of Fe4N compound layer in nitrided steel

This study elucidated the microstructure of the Fe4N (γ’) compound layer in specimens subjected to the nitriding to the specimens with various finished surfaces. Gyrofinishing produces a specimen surface with an ultra-fine-grained (UFGed) structure and a rough surface, whereas the buff-finished specimen exhibited a coarse grain but smooth surface. The γ’ grains formed on the gyrofinished specimens after nitriding were considerably finer and more equiaxial compared with those on the buff-finished specimen. The γ’ nucleated from the grain boundary in the matrix, indicating that the grain boundaries act as a nucleation site. Therefore, the UFGed structure promotes the nucleation of γ’ during the nitriding, resulting in fine grains. Numerous pores were formed in the γ’ layer of the gyrofinished specimen owing to the rough surface. The UFGed structure and surface roughness before nitriding are key factors for controlling the microstructure in the γ’ compound layer.

Analysis of BGA Lead-Free solder joints failure behavior based on thermal shock testing

The interconnected solder joints within automotive electronic components are the most vulnerable parts of the structure, and their reliability is crucial for the development of new energy vehicles. This study focuses on automotive ADAS (Advanced Driver Assistance System) devices, analyzing the failure behavior of internal BGA (Ball Grid Array) lead-free solder joints under thermal shock conditions.Through thermal shock testing from −40℃ to 95℃, it was observed that microcracks first appeared in the upper intermetallic compound (IMC) layer of corner solder joints after 1600 cycles. As the number of thermal shock cycles increased, the net-like β-Sn phase in the solder joints gradually transformed into block and dot-like structures. Due to the relatively weak strength between the IMC layer and the Ag-Sn compound region, cracks typically propagated along the boundaries of these areas. Recrystallization occurred in the interface between the solder joint and the upper pad, with the proportion of high-angle grain boundaries increasing from 10.74% to 72.43%. The crack propagation mode changed from initial intergranular to transgranular fracture. Throughout the thermal shock test, the upper IMC layer remained thicker than the lower one, with the lower IMC layer thickness showing a minimum point at 750 cycles.The average thrust force between the solder joints and the substrate decreased more rapidly with thermal shock cycles, indicating that non-solder mask defined pads are more effective in improving structural strength.

Effect of Carbon Content on the Phase Composition, Microstructure and Mechanical Properties of the TiC Layer Formed in Hot-Pressed Titanium-Steel Composites

During the hot pressing of pure titanium and different carbon steels in a temperature range of ϑ = 950–1050 °C, a compound layer up to dL≈10 μm thick is formed at the titanium–steel interface. With a higher carbon content of the used steel, the layer thickness increases. The carbon concentration within the layer is in the range of stoichiometry for TiC. Apart from TiC, no other phases can be detected by X-ray diffraction (XRD) measurements inside the formed layer. The calculation of the activation energy for the TiC layer formation is Q = 126.5–136.7 kJ mol−1 and is independent of the carbon content of the steel. The resulting microstructure has a grain size gradient, wherein the mechanical properties, such as hardness and Young‘s modulus, are almost constant. Statistical analysis using Response Surface Methodology (RSM) indicates that the carbon content of the steel has the most significant influence on layer thickness, followed by annealing temperature and annealing time. By selecting the appropriate carbon steel and the subsequent removal of the steel, it is possible to produce targeted TiC layers on titanium substrates, which holds enormous potential for this material in wear-intensive applications.

Effects of rare earth on nitriding microstructure and properties of a La-Ce micro-alloyed Q235RE steel

Accelerating nitriding is an interesting topic in chemical heat treatment of ferrous parts. In order to have a deeper understanding of the catalysis principles of rare earth in nitriding, a Q235 carbon steel and a Q235RE steel micro-alloyed with rare earth elements La and Ce were nitrided respectively by plasma nitriding and gas nitriding. The microstructure, phase constitution, and composition of the nitrided specimens were analyzed. The hardness profile of nitriding layer and the brittleness of surface compound layer were measured. The results demonstrate that the Q235RE specimens obtained a higher hardness and deeper effective hardening layer than the Q235 specimens without rare earth microalloying. The rare earth catalysis effects were presented as the acceleration of nitrogen diffusion and the inhibition of nitride precipitation in the diffusion layer of the Q235RE specimens. In addition, the surface compound layer of the Q235RE specimens showed higher toughness and better adhesion to the matrix than that of the Q235 specimens, which is considered to be strongly related to the rare earth elements diffused into the compound and the enhanced residual compressive stress in the layer.

Microstructure and mechanical properties of resistance spot welded dissimilar aluminum/steel joints fabricated using high entropy alloy as interlayer

To improve the welding quality of Al/steel joint during resistance spot welding (RSW) process, a CoCrFeNiMn high entropy alloy (HEA) sheet was employed to be an interlayer between aluminum alloy and high strength steel parent metal sheets. Through a series of comparative studies and analyses, the Al/steel spot welded joint obtained from the process with the HEA interlayer had a larger aluminum nugget diameter and thinner intermetallic compound (IMC) layer when compared to a conventional RSW process. When the thicknesses of two parent metal sheets were 1.0 mm or 1.5 mm, the aluminum nugget diameter of the Al/steel spot welded joint with the HEA interlayer were 4.904 mm and 5.962 mm, and respectively increases by 28.41% and 31.32% compared to a conventional RSW process. For the 1.5 mm of the thickness of the parent metal sheets, the HEA interlayer can make the layer thicknesses at the Al/steel faying interface decrease from 3.2 μm to 1.3 μm. Also, adding the HEA interlayer could induce more welding heat energy respectively by 30.74% and 30.34%, and significantly improve the lap-shear strength of the joint by 56.95% and 52.09% for two thicknesses of the parent metal sheets. Even increasing welding current of the process without HEA interlayer to make its calculated welding heat energy the same as that with HEA interlayer, the Al/steel joint obtained from the process with HEA interlayer still had a higher lap-shear strength. In addition, by seriously observing and analyzing the fracture surfaces obtained from processes with and without the HEA interlayer, it could be concluded that the HEA interlayer could improve the fracture mode of the Al/steel joint from interfacial fracture to button fracture, so the quality of the Al/steel joint could be improved. This work can supply an effective method to improve the dissimilar metals welding process.

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.

In-plane staging in lithium-ion intercalation of bilayer graphene

The ongoing efforts to optimize rechargeable Li-ion batteries led to the interest in intercalation of nanoscale layered compounds, including bilayer graphene. Its lithium intercalation has been demonstrated recently but the mechanisms underpinning the storage capacity remain poorly understood. Here, using magnetotransport measurements, we report in-operando intercalation dynamics of bilayer graphene. Unexpectedly, we find four distinct intercalation stages that correspond to well-defined Li-ion densities. Transitions between the stages occur rapidly (within 1 sec) over the entire device area. We refer to these stages as ‘in-plane’, with no in-plane analogues in bulk graphite. The fully intercalated bilayers represent a stoichiometric compound C14LiC14 with a Li density of ∼2.7·1014 cm−2, notably lower than fully intercalated graphite. Combining the experimental findings and DFT calculations, we show that the critical step in bilayer intercalation is a transition from AB to AA stacking which occurs at a density of ∼0.9·1014 cm−2. Our findings reveal the mechanism and limits for electrochemical intercalation of bilayer graphene and suggest possible avenues for increasing the Li storage capacity.

The influences of nanoparticles on the microstructure evolution mechanism and mechanical properties of laser welded stainless steel/aluminum

In order to solve the problem of poor performance of welded joints of steel and aluminum dissimilar materials, this study proposes the use of ceramic particle-reinforced aluminum alloy as an alternative to traditional aluminum alloy for welding, effectively overcoming this problem. In this paper, the laser welding of stainless steel/6061 aluminum alloy (SA) and stainless steel/TiC–TiB2 duplex nanoparticle-reinforced 6061 aluminum alloy (SRA) was realized. The effect of ceramic nanoparticles on the microstructure and mechanical properties of SRA joint was systematically studied, and the strengthening mechanism of nanoparticles was revealed. Under the same process parameters, the melting zone of SRA joint is larger and the intermetallic compound (IMCs) layer is narrower. Moreover, the grain size of the brittle Fe–Al compound phase in the IMCs layer is significantly reduced, which effectively inhibits the initiation of cracks at the steel/aluminum interface. The study shows that ceramic particles have a pinning effect on the dislocations, limiting the grain growth, reducing the thickness of the intermetallic compound layer, and decreasing the content of the brittle FeAl3 phase. Moreover, ceramic nanoparticles promote the formation of Mg2Si strengthened phase at the grain boundary, further hinder the dislocation movement and improve the strength of the joint. Under the welding power of 3400 W and welding speed of 31 mm/s, SRA joint achieves the maximum tensile shear of 1718 N, which is 15% higher than the strength of SA joint.

Interfacial microstructure and mechanical property of dissimilar resistance spot welded joint of TC4 titanium alloy and 316L stainless steel with nickel interlayer

Dissimilar materials of TC4 titanium alloy and 316L stainless steel were joined by means of resistance spot welding with nickel interlayer in different thicknesses. A significant enhancement in terms of nugget morphology quality with less defects was achieved for the welded joints with nickel interlayer compared with that without interlayer. With increasing the nickel interlayer thickness from 50 μm to 300 μm, the effective nugget diameter increased gradually from ∼4.8 mm to ∼5.2 mm, which was lower than that of the interlayer-free welded joint being ∼5.9 mm. A thinner intermetallic compound layer with dual-layered structure features with thickness of ∼11 μm was formed at the nugget/titanium interface in the welded joint with nickel interlayer compared with that of the interlayer-free welded joint, meanwhile an intermetallic compound layer with thickness of ∼3 μm was formed at the nugget/stainless steel interface, which exhibited serrated structure features. The introduction of nickel interlayer in the welded joint could suppress the formation of the brittle Ti–Fe intermetallics such as Fe2Ti, and facilitate the formation of TiNi, Ti2Ni and TiNi3. A more homogeneous current density distribution and a lower peak temperature (1809 °C) during welding were achieved via employing nickel interlayer. With increasing nickel interlayer thickness from 0 μm to 300 μm, the tensile shear load of welded joints experienced an increased tendency first and then decreased, meanwhile the maximum tensile shear load of 3.7 kN was obtained with the interlayer thickness of 200 μm, which was 61% higher than that of the interlayer-free welded joint.

(Invited) Optical Excitations and Growth in Layered Organic Metal Halide Semiconductors

Hybrid organic metal halides, such as CH3NH3PbI3, have garnered attention because they are earth-abundant, solution-processable materials that can be used to form solar cells with high power conversion efficiency (>20%). There are significant questions about the unusual electronic properties of this class of materials because of the coupling between excitations and the lattice. We will present our work investigating the optoelectronic properties of layered organic metal halide systems and the relationship to structure and growth conditions. We will discuss the nature of optical excitations in layered compounds of the class R2PbX4 where R is an organic cation and X is a halide. These systems show signatures of unusually strong optical frequency magnetic dipole transitions that can be understood through self-trapped exciton formation. We will then discuss how mechanical strain during growth influences broad photoluminescence in a model layered system based on the large cation ethylammonium (EA) with the structure (EA)2(EA)n-1PbnBr3n+1. In this system the emission is strongly impacted by growth-induced strain in thin films quantified using X-ray scattering. Our results suggest that broad emission, relevant for LEDs, can be tuned in thin films. Recent work on how growth impacts the behavior of low dimensional system will also be presented.

Characterization and electrochemical performance of plasma-nitrided titanium alloy for bipolar plates

Ti-N layer with a thickness about 1 ∼ 2.2 μm was formed on titanium alloys through plasma nitriding at 750 °C in NH3 and a mixture of NH3 and N2 (1:2) for 4 h. SEM and XRD were employed to characterize the microstructure and phase composition of nitrided layer. Electrochemical tests evaluated the anti-corrosion properties of the samples before and after nitrided in a simulated proton exchange membrane fuel cells (PEMFC) environment. Interface contact resistance (ICR) was also measured. Results indicated that the corrosion potential in cathodic conditions was increased from −415 mV for untreated titanium to 148 mV for that nitrided in mixture gas. While, the corrosion current density was reduced from 6.64 μA to 0.86 μA. Under a pressure of 140 N cm−2, the interfacial contact resistance of the untreated sample increased from 22.1 mΩ cm2 before corrosion testing to 40.5 mΩ cm2 after corrosion at cathodic conditions. The nitrided sample, on the other hand, saw its contact resistance rise from 4.5 mΩ cm2 before corrosion to 7.3 mΩ cm2 after corrosion. The Ti-N compound layer effectively diminished the corrosion current density and sustained an exceptionally low ICR under the simulated operating conditions of a bipolar plate.

Interfacial microstructure and mechanical properties of CBN brazed in a continuous tunnel furnace with low-temperature Sn-Cu-Ti filler alloy

Currently, the most common process for manufacturing brazed cubic boron nitride (CBN) tools is vacuum brazing using Cu-based active filler alloys. However, the high brazing temperature of Cu-based alloys and the long heating time in a vacuum furnace inevitably cause severe thermal damage, thereby compromising the mechanical properties of the brazed CBN abrasives. In this study, CBN abrasives were brazed using low-temperature Sn-Cu-Ti filler alloys in a continuous tunnel furnace. The final contact angles of the Sn-Cu-Ti filler alloys on the surfaces of the brazed CBN abrasives were determined at 650 °C. When the Ti content in the alloy was 4 %, the final contact angle was 37.2° and the CBN maintained a good exposure height and achieved a firm holding force. The interfacial microstructure was analysed using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray diffraction (XRD). It was found that a layer of needle-like compounds, primarily comprising TiB2 and TiN, with an approximate thickness of 5 μm, was formed at the interface, indicating the formation of a chemical–metallurgical bond between the Sn-Cu-Ti alloy and CBN abrasive. The residual stresses and mechanical properties of brazed CBN abrasives with Sn-Cu-Ti and traditional Cu-based alloys were measured and compared. The results showed that compared to the brazed CBN with the Cu-based alloy, the average residual stress of the brazed CBN with the Sn-Cu-Ti alloy was reduced by 25.2 %, while the compressive strength and impact toughness increased by 25.3 % and 13.8 %, respectively. The experimental results provide new insights into reducing thermal damage to CBN for improving the processing performance of brazed CBN tools.

Preparation of TiN compound layer by intermittent vacuum diffusion nitriding on Ti6Al4V titanium alloy

An intermittent vacuum diffusion nitriding (IVDN) treatment was used for the preparation of a TiN compound layer on the surface of the Ti6Al4V titanium alloy. The underlying microstructure evolution and the properties were thoroughly investigated. The IVDN process was performed alternately by using intermittent nitriding and vacuum diffusion. The TiN compound layer was formed on the surface discontinuously, layer by layer. As a result, the TiN compound layer was formed easily on the surface of titanium alloy compared to the vacuum nitriding. Dislocations were also generated in the adjacent α-Ti grains of the TiN compound layer. Interestingly, the induced dislocation defects possessed high free energy and contributed to the generation of the TiN grain nucleus, which facilitated the diffusion of the N atoms towards the inner substrate. The acquired results disclosed the intrinsic reason for the diffusion behaviour of N atoms. The Ti6Al4V titanium alloy was nitrided by using IVDN treatment at the temperature of 700 °C for 10 h. The surface microhardness reached 900–950 HV and presented continuous gradient change. In addition, the IVDN sample exhibited enhanced wear resistance properties than the un-nitrided sample.

Bulk photovoltaic effect and high mobility in the polar 2D semiconductor SnP2Se6.

The growth of layered 2D compounds is a key ingredient in finding new phenomena in quantum materials, optoelectronics, and energy conversion. Here, we report SnP2Se6, a van der Waals chiral (R3 space group) semiconductor with an indirect bandgap of 1.36 to 1.41 electron volts. Exfoliated SnP2Se6 flakes are integrated into high-performance field-effect transistors with electron mobilities >100 cm2/Vs and on/off ratios >106 at room temperature. Upon excitation at a wavelength of 515.6 nanometer, SnP2Se6 phototransistors show high gain (>4 × 104) at low intensity (≈10-6 W/cm2) and fast photoresponse (< 5 microsecond) with concurrent gain of ≈52.9 at high intensity (≈56.6 mW/cm2) at a gate voltage of 60 V across 300-nm-thick SiO2 dielectric layer. The combination of high carrier mobility and the non-centrosymmetric crystal structure results in a strong intrinsic bulk photovoltaic effect; under local excitation at normal incidence at 532 nm, short circuit currents exceed 8 mA/cm2 at 20.6 W/cm2.

Cellulose Nanofiber-Based Nanocomposite Films with Efficient Electromagnetic Interference Shielding and Fire-Resistant Performance.

Cellulose nanofiber (CNF) has been widely used as a flexible and lightweight polymer matrix for electromagnetic shielding and thermally conductive composite films because of its excellent mechanical strength, environmental performance, and low cost. However, the lack of flame retardancy seriously hinders its further application. Herein, renewable and biomass-sourced l-arginine (AR) was used to surface-modify ammonium polyphosphate (APP) and an environmentally friendly biobased flame retardant was synthesized by the coordination of zinc sulfate heptahydrate (ZnSO4·7H2O), which was named AAZ. AAZ was deposited on the surface of CNF by electrostatic adsorption and Zn2+ complexation. The biobased compatibilizer Triton X-100 was employed to assist the exfoliation of graphene nanoplatelets (GNPs) and their dispersion in the CNF matrix. Due to the formation of a dense lamellar layer resembling a shell structure, the CNF/GNPs composite films with a tensile strength of 52 MPa were obtained via vacuum-assisted filtration. Because the phosphorus-containing group produces a protective layer of PxOy compound and promotes the formation of a carbon layer by CNF and the combustion releases ammonia gas, the fire-resistant performance of the composite films was greatly improved. Compared with the pure CNF film, the composite film exhibits 33% reduction in PHRR value and 40% reduction in THR. In addition, the CNF/GNPs composite film with 20 wt % GNPs possessed high conductivity (2079.2 S/m) and electromagnetic interference (EMI) shielding effectiveness (37 dB). The ultrathin CNF/GNPs composite films have excellent potential for use as efficient flame retardant and EMI shielding materials.

Ab initio calculations and crystal structure simulations for mixed layer compounds from the tetradymite series

Abstract Density functional theory (DFT) is used to obtain structural information of seven members of the tetradymite homologous series: Bi2Te3 (tellurobismuthite), BiTe (tsumoite), Bi4Te3 (pilsenite), Bi5Te3, Bi2Te, Bi7Te3 (hedleyite), and Bi8Te3. We use the formula S(Bi2kTe3)·L[Bi2(k+1)Te3] as a working model (k = 1–4) where S and L are short and long modules in the structures. The relaxed structures show an increase in the a parameter and decrease in the interlayer distance (dsub) from Bi2Te3 (2.029 Å) to Bi8Te3 (1.975 Å). DFT-derived formation energy for each phase indicates that they are all thermodynamically stable. Scanning transmission electron microscopy (STEM) simulations for each of the relaxed structures show an excellent match with atom models. Simulated electron diffractions and reflection modulation along c* are concordant with published data, where they exist, and with the theory underpinning mixed-layer compounds. Two modulation vectors, q = γ·csub* (γ = 1.800–1.640) and qF = γF·dsub* (γF = 0.200–0.091), describe the distribution of reflections and their intensity variation along dsub* = 1/dsub. The γF parameter reinforces the concept of Bi2kTe3 and Bi2(k+1)Te3 blocks in the double module structures, and γ relates to dsub variation. Our model describing the relationship between γ and dsub allows prediction of dsub beyond the compositional range considered in this study, showing that phases with k &amp;gt;5 have values dsub within the analytical range of interlayer distance in bismuth. This, in turn, allows us to constrain the tetradymite homologous series between γ values of 1.800 (Bi2Te3) and 1.588 (Bi14Te3). Phase compositions with higher Bi/Te should be considered as disordered alloys of bismuth. These results have implications for mineral systematics and classification as they underpin predictive models for all intermediate structures in the group and can be equally applied to other mixed-layer series. Our structural models will also assist in understanding variation in the thermoelectric and topological insulating properties of new compounds in the broader tetradymite group and can support experimental work targeting a refined phase diagram for the system Bi-Te.

Investigation of the mechanical properties of lead-free Sn-58Bi solder alloy with cobalt addition through flux doping

PurposeThis study aims to investigate the effect of incorporating cobalt (Co) into Sn-58Bi alloy on its phase composition, tensile properties, hardness and thermal aging performances. The fracture morphologies of tensile-tested solders are also investigated to correlate the microstructural changes with tensile properties of the solder alloys. Then, the thermal aging performances of the solder alloys are investigated in terms of their intermetallic compound (IMC) layer morphology and thickness.Design/methodology/approachThe Sn-58Bi and Sn-58Bi-xCo, where x = 1.0, 1.5 and 2.0 Wt.%, were prepared using the flux doping technique. X-ray diffraction (XRD) is used to study the phase composition of the solder alloys, whereas scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) are used to investigate the microstructure, fractography and compositions of the solders. Tensile properties such as ultimate tensile strength (UTS), Young’s modulus and elongation are tested using the tensile test, whereas the microhardness value is gained from the micro-Vickers hardness test. The morphology and thickness of the IMC layer at the solder’s joints are investigated by varying the thermally aging duration up to 56 days at 80°C.FindingsXRD analysis shows the presence of Co3Sn2 phase and confirms that Co was successfully incorporated via the flux doping technique. The microstructure of all Sn-58Bi-xCo solders did not differ significantly from Sn-58Bi solders. Sn-58Bi-2.0Co solder exhibited optimum properties among all compositions, with the highest UTS (87.89 ± 2.55 MPa) at 0.01 s−1 strain rate and the lowest IMC layer thickness at the interface after being thermally aged for 56 days (3.84 ± 0.67 µm).Originality/valueThe originality and value of this research lie in its novel exploration of the flux doping technique to introduce minor alloying of Co into Sn-58Bi solder alloys, providing new insights into enhancing the properties and performance of these solders. This new Sn-Bi-Co alloy has the potential to replace lead-containing solder alloy in low-temperature soldering.

Synthesis and Characterization of Cobalt-doped Titanium Dioxide Thin Films as Solar Cell Components using UV-SEM Analysis

Research has been carried out in the form of the synthesis and characterization of thin films of titanium dioxide with the addition of cobalt doping. The purpose of this research was to synthesize and characterize thin films related to optical properties, morphological shapes, and components of thin film compounds that are good for use as basic materials for the development of nanoparticle technology in the form of solar cells. The research was carried out in two stages, namely synthesis such as preparation of glass substrates, preparation of sol-gel solutions, deposition of solutions onto glass substrates, and heating of TiO2:Co thin film samples. The next stage is the thin film characterization test, where the optical properties of the thin film, such as absorbance, transmittance, gap energy, and activation energy, are measured using a UV-vis spectrophotometer, while morphological data and components of the thin layer compounds are measured using a Scanning Electron Microscope-Energy Dispersive X-rays (SEM-EDX). Based on data analysis and discussion, it was found that the optical properties, such as the transmittance value of the thin film, experienced the lowest point at a wavelength of 250–280 nm with a maximum percentage value of 62.14 to 78.85%. The greater the doping concentration, the lower the transmittance value. This condition is inversely proportional to the absorbance value of the maximum TiO2:Co thin film, which is in the region with a wavelength of 280–300 nm and a value of 5.70–6.31. The greater the doping concentration, the greater the absorbance value. The energy bandgap values of TiO2:Co thin films for doping concentrations (0, 5, 10, 15, 20)% were 3.44; 3.39; 3.38; 3.32; 3.22 eV for the direct energy bandgap and 3.86; 3.85; 3.84; 3.85; 3.82 eV for the indirect energy gap. The activation energy of the TiO2:Co thin film decreased from 2.86 to 2.26 eV. As for the morphological data of the TiO2:Co thin film, it was found that the greater the concentration of doping, the layer was deposited evenly, finely, and homogeneously. Regarding the data on the components of the thin layer compounds, it was found that the percentage of TiO2 content was in the range of 64.48–95.94%, while for Co, it was in the range of 0.00–19.21%.

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.

Understanding crack growth within the γ′ Fe4N layer in a nitrided low carbon steel during monotonic and cyclic tensile testing

Nitriding is a cost-effective method to realize simultaneous improvements in tensile and fatigue properties and resistance to abrasion and corrosion. Previous studies reported that nitriding pure Fe enhances tensile strength by ~ 70% and fatigue limit by ~ 200%. It is due to the increase in surface hardness caused by the formation of γ′(Fe4N) and ε(Fe2-3N) nitrogen-containing intermetallic compound phases. However, the intermetallic compound layer is prone to brittle-like cracking. To better design nitrided steels, it is crucial to identify the crack growth mechanisms via analysis of the microstructural crack growth paths within the ~ 4–6 µm thick nitride layer. In the current work, we statistically evaluate the crack propagation behavior in the γ′ Fe4N layer during monotonic and cyclic tensile deformation in nitrided low-carbon steel (0.1 wt% C). Since nitriding typically results in the formation of columnar grains, the effect of morphology needs to be clarified. To this end, the steel was shot-peened and subsequently nitrided to promote equiaxed nitride grains morphology (~ 16% increase). Crack growth paths were comparatively evaluated for multiple cracks, and no significant effect of nitride morphology was observed. {100}γ′ is the predominant transgranular crack path in the monotonic tensile tested specimen, followed by {111}γ′. It is despite the elastic modulus of {111}γ′ < {100}γ′. This contrary behavior is explained by {100}γ′ plane having the lowest surface energy (density functional theory calculations). In the cyclic tensile loaded specimen, experiments revealed that transgranular cracking along {100}γ′ (cracking via symmetric dislocation emission) or {111}γ′ (slip plane cracking) is equally likely.Graphical abstract