Subsequent Annealing Research Articles

Optical and electrical properties of proton-implanted p-GaSb for electrical isolation

Abstract The effect of proton implantation as solation implant and subsequent annealing on the optical absorption and electrical resistivity of low-bandgap p-GaSb is reported. The measured transmittance spectra indicates that implantation creates a distribution of energy levels extending into the bandgap. Electrical measurements show that the average sheet resistance of the implanted layer increases only by an order of magnitude from its pre-implantation value at a proton dose of ~1013 cm-2 followed by 200°C annealing. It is also shown that annealing reduces the implantation-induced optical absorption while still retaining a high electrical resistivity.

A distinctive bound exciton line induced by electron-beam irradiation and subsequent annealing of an unintentionally doped GaN layer

Abstract An undefined bound exciton line (UDX) with a photon energy 0.6 meV lower than the Si-donor bound exciton line was observed by photoluminescence in GaN layers annealed at 1100 °C after electron beam (EB) irradiation at an energy of 137–2000 keV. The UDX was not observed in samples not subjected to EB irradiation or annealing but was found in a sample annealed after EB irradiation at an energy of 137 keV, where only nitrogen atoms are displaced in GaN. The origin of the UDX was presumably formed by a thermal reaction of defects containing nitrogen-displacement-related defects.

Solubility and magnetic properties of Ag−Co−Si alloy synthesized by mechanical alloying and annealing

AbstractThis present work concerns the effect of ternary addition of non‐metallic and diamagnetic silicon on the metastable solubility of the immiscible silver‐cobalt system during the course of ball milling, annealing of the ball milled samples and the corresponding magnetic properties. It should be noted that silicon has a smaller goldsmidt radius (111 pm) than silver (144 pm) and silicon+4 has more valence electrons than silver+1. Keeping the objectives of the current study in mind, silicon may thus be considered as an option for ternary addition, in contrast to metallic components. An attempt has been made to examine the phase changes that occurred in the 50 silver‐40 cobalt‐10 silicon (atom percent) system during ball milling and the subsequent isothermal annealing of the ball milled product. Phase evolution during mechanical alloying and isothermal annealing is identified by means of x‐ray diffraction, differential thermal analysis, high resolution transmission electron microscopy and magnetic measurements. The addition of silicon facilitates cobalt‘s formation of a metastable alloy with copper after 50 hours of ball milling. Annealing significantly improves the magnetic characteristics of materials that have been ball milled; the optimal combination of magnetic properties was obtained after an hour of annealing at 550 °C.

Effects of ultrasonic nanocrystal surface modification treatment and subsequent annealing on the microstructure and mechanical properties of rolled AZ31 alloy

Effects of ultrasonic nanocrystal surface modification treatment and subsequent annealing on the microstructure and mechanical properties of rolled AZ31 alloy

Enhancing strength-ductility synergy of Cu alloys with heterogeneous microstructure via rotary swaging and annealing

The trade-off of strength and ductility in the Cu alloys seriously restricts its wide application. In this study, the paradox of strength and ductility of the Cu alloy is ameliorated by rotary swaging (RS) and subsequent annealing, and reveals its microstructural evolution. It was found that the grain size was obviously refined after the RS, resulting in yield strength as high as 760 MPa but with a ductility of only 1.5 %. After annealing, the RS-350-20 sample (RS sample annealed at 350°C for 20 min) exhibited partial recrystallization at the edge and middle positions, while full recrystallization occurred at the center position, which formed a gradient grain size distribution. Tensile results showed that RS-350-20 sample exhibited an excellent combination of the yield strength of 495 MPa and ductility of 27%. High strength stemmed from residual deformation grains, recrystallized ultrafine/fine grains and heterogeneous deformation-induced (HDI) strengthening. The good ductility originated from recrystallized coarse grain, pronounced HDI hardening and activated deformation twins. In addition, microstructural characterization further revealed that dislocations were accumulated near the recrystallized grains to maintain strain continuity at the interface of deformed grains and recrystallized grains during tensile strain. With increasing strain, deformation twins were activated near the recrystallized grains, which facilitates high strain hardening capability meanwhile maintaining high strength. These findings provide insight for optimizing the strength and ductility of Cu alloys by a feasible processing.

Phase reversion mediated the dual heterogeneity of grain size and dislocation density in an equiatomic CrCoNi medium-entropy alloy

An ultra-high strain rate (104 s-1) dynamic plastic deformation treatment at liquid nitrogen temperature (LNT-DPD) followed by annealing is carried out to obtain dual heterogeneity of grain size and dislocation density in an equiatomic CrCoNi medium entropy alloy (MEA). Such extreme loading conditions resulted in extensive phase transformation in this MEA. Subsequent annealing at 650°C for 1 h further induced reverse phase transformation and partial recrystallization, forming a complex heterogeneous microstructure characterized by nested trimodal grain sizes and partitioned dislocation density. A superior yield strength of ∼800MPa and a good ductility of ∼40% were simultaneously achieved in this heterogeneous alloy. In order to reveal the effects of grain size and dislocation density distributions on the mechanical property improvements, the underlying deformation mechanisms were systematically discussed. High density of geometrically necessary dislocations (GNDs) would be induced in complex heterogeneous structures during tensile deformation due to strain gradients or partitioning between different regions, which would lead to additional strengthening and work hardening. These results provide a novel approach to overcome the strength-ductility trade-off dilemma for FCC-structured MEAs.

Enhanced strength-ductility synergy in a gradient hetero-structured CrCoNi medium-entropy alloy

A CrCoNi medium-entropy alloy (MEA) with gradient hetero-structure (GHS) composing of gradient nanostructured surface layer and hetero-structured matrix was prepared via a two-step process: pre-cold rolling (CR) deformation and subsequent annealing followed by surface mechanical grinding treatment (SMGT) and secondary annealing. The GHS CrCoNi exhibits an excellent synergy of strength and ductility, as evidenced by a yield strength of approximately 1.2 GPa and a uniform elongation of about 20%. The GHS displays a pronounced hetero-deformation induced (HDI) hardening effect, whereby the central layer (CL) and surface layer (SL) undergo local strain hardening in a mutually compatible manner. This process facilitates the multiplication and accumulation of geometrically necessary dislocations (GNDs) at intra- and inter-layer hetero-interfaces and also activates the deformation faulting and twinning in both CL and SL, thus enhancing the overall mechanical response. The interlayer compatible deformation observed in the GHS significantly bolsters the sustainability of strain hardening at the microscopic scale. This effect is of significant importance in redistributing stress and strain more rationally across the entire GHS sample, effectively reducing the risk of localized deformation failures. This study offers insight into the correlation between macroscopic strain hardening and micromechanical behavior in gradient-/hetero-structured materials.

Achieving Over 10% Efficiency in Kesterite Solar Cells via Selenium-Free Annealing

The unsatisfactory crystalline quality of the absorber layer has seriously impeded the development of kesterite photovoltaic devices, including a small grain size, a typical multi-layer structure, and inherent defects and defect clusters. Herein, we simultaneously modify the nature of the absorber bulk and the heterojunction interface by sputtering quaternary alloy targets and subsequent selenium-free annealing to improve the photovoltaic performance of Cu2ZnSnSe4 (CZTSe) solar cells. By adjusting the sputtering power, the elemental content and distribution in the precursor film are effectively controlled, which helps to obtain a single-layer large grain CZTSe absorber layer with better homogenization and compactness. The harmful inherent defects are significantly suppressed by such a modification. Simultaneously, the widened depletion width and enhanced built-in electric field, as well as improved band alignment at the heterojunction, enhance carrier collection. As a consequence, the efficiency of CZTSe solar cells has improved greatly from 6.91% to 10.12%. The single-target preparation strategy without selenization provides a simple and novel perspective for simultaneously adjusting the morphology and defects of kesterite photovoltaic materials, paving the way for promoting innovative industrial applications.

Cu2SnS3/rGO nanocomposites with optimized pore structure for high-performance lithium-ion batteries

Developing advanced anode materials is essential for enhancing the rate performance and stability of lithium-ion batteries (LIBs), which is critical for meeting the demands for next-generation energy storage solutions. In this research, Cu2SnS3/rGO nanocomposites were synthesized via a rapid microwave-assisted one-step method, followed by post-synthetic annealing. The incorporation of reduced graphene oxide (rGO) not only significantly improves its electrical conductivity, but also effectively inhibits the agglomeration of CTS nanoparticles. The nanocrystal size in the CTS/rGO nanocomposites has been dramatically downsized, transitioning from the pristine CTS dimensions of 0.9–1.5 μm to a mere 100 nm. This downsizing is a critical advancement in the electrode, as it enhances the surface area and reactivity of the composite. The subsequent high-temperature annealing process shrinks the pore size in the CTS/rGO nanocomposite, decreasing from an average of 42.13 nm to a more confined range of 7.81 to 8.77 nm, depending on the annealing temperatures. Electrochemical testing reveals that the CTS/rGO-A nanocomposite annealed at 300 °C exhibits superior electrochemical performance to the unmodified CTS and non-annealed CTS/rGO composite. The performance is evidenced by an initial capacity of 1856.97 mAh g−1 at a current density of 1 A g−1 and retains a capacity of 1250.32 mAh g−1 after 500 cycles. To elucidate the underlying mechanisms governing the lithium ion diffusion kinetics, capacitance and diffusion behavior of the CTS/rGO-A electrode, advanced techniques such as galvanostatic intermittent titration technique (GITT) and rate cyclic voltammetry (CV) were utilized. These analyses revealed that the synergistic effect of an increased Li+ diffusion coefficient (DLi+), coupled with a notable capacitive contribution, is demonstrated to the enhanced electrochemical performance observed. Furthermore, the COMSOL Multiphysics simulation also indicates improved structural stability of CTS/rGO-A, attributed to minimized stress from volume expansion during discharge. The CTS/rGO-A nanocomposites, featuring enhanced electrochemical performance, coupled with a straightforward and efficient fabrication method, emerge as a promising material for scalable and practical energy storage solutions.

Rapid preparation of Cu(111) foil with large single-crystal grains through a graphene induction and contactless annealing method

There is a growing interest in preparing large-size Cu(111) foil for achieving high performance in various applications. In this work, a simple two-step method using graphene induction and contactless annealing was designed to rapidly prepare Cu(111) foil with large single-crystal grains. The graphene film grown on the Cu surface in the first step by chemical vapor deposition serves as a template for the orientation transition of the Cu foil in a subsequent high-temperature annealing. The (111) orientation transformation of the entire Cu foil was achieved within 20 min with single-crystal grains in size of above 30 cm2, and the corresponding speed is ten times higher than that prepared in traditional annealing process. This work provides a facile and rapid fabrication approach for preparing Cu(111) foil with large grains.

Enhancement in Mechanical Properties of AA5052 Sheet for Small Ship by Cold Roll-Bonding Process

A cold roll-bonding (CRB) process was applied to enhance the mechanical properties of AA5052 sheet for small ship. Two and four AA5052 sheets of 1 mm thickness, 40 mm width and 300 mm length were stacked, then roll-bonded to a thickness of 0.5 mm and 1 mm respectively by two-pass rolling after such surface treatment as degreasing and wire brushing. The rolling was performed at ambient temperature without lubricant using a 4-high mill at rolling speed of 6.0m/sec. The as roll-bonded AA5052 sheet was then annealed for 1h at various temperatures from 200 to 500℃. The as roll-bonded AA5052 sheets showed a deformation structure in which the grains are elongated to the rolling direction, however above 300℃ they exhibited the complete recrystallization structure consisting of equiaxed grains, regardless of the stack number. The grain diameter of specimens annealed at high temperatures above 300℃ was smaller in 4-layer stack than in 2-layer stack CRB. Both tensile strength and elongation of the specimens were better in 4-layer stack than in 2-layer stack CRB. The effects of stacking number on microstructure and mechanical properties of AA5052 sheets processed by CRB and subsequent annealing were discussed in detail.

Development of the Ge-MDST instrument structure with an induced p-type channel

The conditions for the growth of n-type Ge conduction layers by the HW CVD method with the parameters required to create a Ge-TIR transistor with an induced p-type channel are determined. The conditions of deposition by electron beam deposition and subsequent annealing of layers of a high-k dielectric ZrO2:Y2O3 are optimized, allowing to achieve a leakage current of 5 × 10–6 A/cm2. For the developed instrument structure, some parameters of the Ge-TIR transistor were calculated, such as the channel length, the maximum voltage between the drain and the source, and the breakdown voltage.

Retained austenite in medium manganese steel with dissimilar morphology and composition

The microstructure and mechanical properties of medium manganese steel with a composition of 0.2C-5Mn-0.5Si-1.5Al (wt.%) were investigated, employing a two-stage heat treatment process. The microstructure following pretreatment comprised pearlite, martensite, and ferrite. Subsequent intercritical annealing resulted in the formation of retained austenite with varying morphology and composition. The filmy retained austenite transformed from pearlite exhibited a higher Mn content compared to the blocky retained austenite transformed from martensite, while also displaying a slower growth rate. Moreover, the filmy retained austenite exhibited superior thermal and mechanical stability. Tensile tests showed that the test steels not only obtained high strength (>1000 MPa) and high elongation (>30%), but the stress-strain curves also showed continuous yielding behaviour and a more reasonable ratio of tensile strength to yield strength.

Macroscopic Monograin Nano-Gyroid Thin Films in 4-inch Scale Through Shear-Rolling and Subsequent Solvent Annealing.

The gyroid structure from self-assembly is highly attractive for optical applications such as photonic crystals and metamaterials. However, due to the direction-dependent nature of these applications, achieving a monograin-level structure over a large area has remained challenging. In this study, the fabrication of unidirectionally oriented anisotropic nanocylinders of polystyrene-block-polydimethylsiloxane (PS-b-PDMS) is reported block copolymer thin films up to a 4-inch scale via a shear-rolling process, followed by solvent annealing to induce phase transition to nearly monograin gyroid structures. Grazing-incidence small-angle X-ray scattering (GISAXS) analysis and cross-sectional scanning electron microscope (SEM) images in the direction parallel to the shear-rolling direction reveal the preferential orientation with the (111) plane onto the YZ axis of the film, while only the (110) plane on the YZ axis of the film is observed in the perpendicular direction, with grain sizes approaching single-grain levels. For metamaterial applications, the PDMS domain is selectively removed, and gold is electroplated to produce monograin gold gyroid films.

Features of the Structure and Thermal Properties of LnBWO6 (La = Ln, La0.999Nd0.001, La0.99Gd0.01) Synthesized by the Sol-Gel Method

Borate tungstates LnBWO6 (Ln = La, La0.999Nd0.001, La0.99Gd0.01) were synthesized by the Pechini method with subsequent annealing of intermediates. They were analyzed by X-ray diffraction (XRD) and DSC methods. Crystallographic parameters of synthesized LnBWO6 were refined by powder X-ray diffraction in two systems: monoclinic, space group P21, and orthorhombic, space group P222. The presence of reversible first-order phase transitions in synthesized LnBWO6 was detected using the DSC method, and the temperatures and enthalpies of phase transformations were determined. It has been shown that Nd3+ and Gd3+ dopants lowers the L- → H- phase transition temperature of LaBWO6. According to experimental electron paramagnetic resonance (EPR) data gadolinium has two independent positions in the La0.99Gd0.01BWO6 structure.

Cr2O3–NiO mixed oxides thin films for p-type transparent conductive electrodes

The Cr2O3–NiO mixed oxides’ thin films were formed by means of the layer-by-layer magnetron sputtering deposition of Cr2O3, NiO, and Cr2O3 layers on c-plane sapphire substrates. These thin-film structures, subjected to subsequent annealing, constituted a combination of the monocrystalline (0001) Cr2O3 and nonordered nickel oxide phase, which was a mixture of NiO and Ni2O3. The annealing at 900 and 1000 °С in air facilitated the diffusion of Ni and Cr atoms into the layers. Varying the annealing time allowed us to control the uniformity of the Ni and Cr distribution, the microrelief of the film surface, the transmittance in the visible region, and the sheet resistance of the Cr2O3–NiO thin-film structures. Thus, the films annealed at 900 °C during 30 min were characterized by a uniform distribution, a relatively weakly developed surface, a low sheet resistance, and the highest Haacke's Figure of Merit of 1.49 × 10–9 Ω–1. The formation of mixed Cr2O3–NiO oxides by the proposed approach was found to be an effective way to improve the performances of Cr2O3 based p-type transparent conductive electrodes.

High thermoelectric performance in Ag-doped Bi0.5Sb1.5Te3 nanocomposites synthesized via low-temperature liquid phase sintering

In recent years, low-temperature liquid phase sintering (LPS) has emerged as a cost-effectiveness method for designing thermoelectric nanocomposites with reduced lattice thermal conductivity. However, their electrical conductivity often remains suboptimal, limiting the overall figure of merit (ZT). In this study, xwt% Ag/Bi0.5Sb1.5Te3 (x = 0,0.1,0.2,0.3,0.4) nanocomposites are prepared through low-temperature LPS method followed by subsequent annealing. Remarkably, a small amount of silver atoms was doped into the Bi0.5Sb1.5Te3 matrix post-annealing, significantly increasing carrier concentration and improving electrical conductivity. Additionally, residual Ag atoms formed Ag₂Te nanoprecipitates, and lattice defects (including grain boundaries, twin boundaries, dislocations, and lattice distortions) effectively reduced lattice thermal conductivity. The 0.3 wt% Ag/Bi0.5Sb1.5Te3 sample achieved a maximum ZT value of 1.36 at 400 K, double that of the pure Bi0.5Sb1.5Te3 sample, with an average ZT value of 1.17, among the highest reported. This work demonstrates significant potential for synthesizing high-performance thermoelectric materials via low-temperature LPS methods.

Microstructure Evolution of the Interface in SiCf/TiC-Ti3SiC2 Composite under Sequential Xe-He-H Ion Irradiation and Annealing Process.

A new type of SiCf/TiC-Ti3SiC2 composite was prepared by the Spark Plasma Sintering (SPS) method in this work. The phase transformation and interface cracking of this composite under ion irradiation (single Xe, Xe + He, and Xe + He + H ions) and subsequent annealing were analyzed using transmission electron microscopy (TEM), mainly focusing on the interface regions. Xe ion irradiation resulted in the formation of high-density stacking faults in the TiC coatings and the complete amorphization of SiC fibers. The implanted H ions exacerbated interface coarsening. After annealing at 900 °C for 2 h, the interface in the Xe + He + H ion-irradiated samples was seriously damaged, resulting in the formation of large bubbles and cracks. This damage occurred because the H atoms reduced the surface free energy, thereby promoting the nucleation and growth of bubbles. Due to the absorption effect of the SiCf/TiC interface on defects, the SiC fiber areas near the interface recovered back to the initial nano-polycrystalline structure after annealing.

Intense violet electroluminescence of thin SiO2 layers with SnO2 nanocrystals

It has been shown that Sn implantation with subsequent annealing in air leads to an increase in the electroluminescence (EL) intensity of SiO2/Si structure by two orders of magnitude. Intense violet EL with a maximum at 3.21 eV was observed at room temperature by the naked eye at forward bias. The observed emission was attributed to radiative recombination in SnO2 nanocrystals synthesized in SiO2 layers. The external quantum efficiency (EQE) increased with decreasing Sn concentration The maximum external quantum efficiency was found to be 0.7 % for the silica film Sn-implanted at the lowest fluence of 2.5 × 1016cm−2. The non-radiative charge transport (shunt current) through the sample and mechanism of EL excitation are discussed. It has been concluded that the Poole–Frenkel mechanism, or tunneling between traps are the most likely mechanisms of charge transport to light-emitting centers.

Modulating the rejuvenation in a Al75Mg25 metallic glass by multiple recovery annealing treatment

Rejuvenation presents a promising way to improve the plasticity of metallic glasses. How modulating the degree of rejuvenation of metallic glasses remains a challenging issue. Here, based on the molecular dynamics simulation, we investigate the evolution of the structural and mechanical properties of a binary Al75Mg25 metallic glass and successfully realized the rejuvenation modulation through the multiple recovery annealing treatment. A range of samples with different degrees of rejuvenation were obtained by successive multiple recovery annealing process. According to our calculations, we found that the degree of rejuvenation is highly correlated with the Al-centered clusters. Microstructural analyses show that a higher degree of rejuvenation is concomitant with less 1551 index of Honeycutt-Andersen indices and a lower content of <0,0,12,0 > in terms of Voronoi Tessellation analysis. Moreover, our calculated results demonstrate that the samples with the aging initial state show a higher degree of rejuvenation as compared to the samples with the rejuvenated initial state. This can be attributed to that there are more icosahedral clusters, which are more likely to change to other types of clusters with low local fivefold symmetry in the aged samples during the subsequent high-temperature annealing process. Our work confirms that proper multiple (no more than three times) recovery annealing treatment can increase the degree of rejuvenation of metallic glasses and can offer a better understanding of the effect of rejuvenation on the microstructures and mechanical properties of metallic glasses.