Heating Transmission Electron Microscopy Research Articles

Micro-electromechanical system-based cryogenic and heating in situ transmission electron microscopy for investigating phase transitions and domain evolution in single-crystal BaTiO3

Investigating phase transitions between ferroelectric states is crucial for understanding the nucleation, dynamics, and kinetics of domains, both before and after transformation. Here, we assess all phase transitions and domain evolutions in single-crystal BaTiO3 by implementing microelectromechanical systems (MEMS)-based in situ cryogenic (cryo-) and heating transmission electron microscopy (TEM) by continuously varying sample temperatures from -175 °C to 200 °C. Every possible phase-cubic, tetragonal, orthorhombic, and rhombohedral - was identified. An ultra-stable imaging condition was achieved with a mean drift speed of 1.52 nm/min, providing unique opportunities for atomic resolution in situ scanning TEM with a wide temperature range. Furthermore, domain nucleation and evolution across phase transitions were investigated using complementary dielectric measurements, optical microscopy, and a phenomenological model. This study underscores the effectiveness and utility of MEMS-based in situ cryo-/heating TEM in revealing phase transitions and domain structures in ferroelectric materials.

Understanding Ag liquid migration in SiC through ex-situ and in-situ Ag-Pd/SiC interaction studies

The effective containment of fission products (FPs) within tri-structural isotropic (TRISO) fuel particles is crucial for the safety and efficiency of High Temperature Gas-cooled Reactors (HTGRs). Combining multi-scale (µm to nm) and multi-dimensional (2D and 3D) analysis, this study focuses on the migration mechanisms of silver (Ag), for which the Ag-110 m FP isotope is radiotoxic, facilitated by reactions with palladium (Pd) alloys and the silicon carbide (SiC) layer at elevated temperatures (1300–1500 °C). Three primary pathways for Ag migration are identified: (1) diffusion in solid palladium silicide to form (Pd,Ag)2Si, (2) infiltration through cracks and pores in the carbon phase, and (3) liquid phase migration along SiC grain boundaries. Especially at temperatures above the melting point of Pd2Si (1404 °C), a ‘dissolution-recrystallisation’ mechanism is proposed of the Ag-Pd-Si liquid phase migrating along SiC grain boundaries. The study employs state-of-the-art in-situ heating transmission electron microscopy (TEM) techniques to directly observe the dynamic migration processes of Pd silicide within SiC, providing unprecedented insights into the liquid behaviour in TRISO fuel. These findings highlight the significant role of liquid phases in determining the transport of FPs through the TRISO-SiC which is vital for developing strategies that enhance the safety and efficacy of HTGRs.

Cross-scale deciphering thermal failure process of Ni-rich layered cathode

Ni-rich LiNixCoyMn1-x-yO2 (NCM) layered oxides are low-cost high-energy density cathode materials, but plagued by its poor thermal stability incurred safety concerns. The thermal failure process of the layered cathode is accompanied by heat generation and oxygen release, which drives the battery into thermal runaway (TR). Aiming to fully understand the TR process and the structure evolution, this work applies diverse characterization techniques onto a polycrystalline Ni-rich layered cathode (LiNi0.83Mn0.05Co0.12O2 (PCN83)) to comprehensively investigate its thermal failure process at multiple scales. From macro level, we validate that it is the cathode thermal failure that drives the battery from the heat accumulation stage into TR in adiabatic conditions. From micro level, transmission electron microscopy (TEM) verifies that the thermal failure of PCN83 starts from 150 °C, which is much lower than the TR temperature measured from macro level tests. We reveal that the PCN83 cathode experiences sequential phase transitions before the TR, where the phase transition mechanism is illustrated from the atomic scale and the pore evolution process is unraveled. In situ heating TEM further reveals that thermal failure is preferentially initiated from grain boundaries and defect regions. These findings provide an in-depth understanding of the whole thermal failure process of NMC-based layered cathode materials and sheds new lights on the rational design of Ni-rich cathode materials with improved thermal safety.

Phase formation mechanism of Cr2AlC MAX phase coating: In-situ TEM characterization and atomic-scale calculations

Cr2AlC, a representative MAX phase, gains increasing attention for the excellent oxidation tolerance and corrosion resistance used in harsh high temperature and strong radiation environments. However, the lack of the phase formation mechanism has become the key bottleneck to the practical applications for Cr2AlC synthesis with high purity at low temperatures. In this work, we fabricated the amorphous Cr–Al–C coating by a hybrid magnetron sputtering/cathodic arc deposition technique, in which the in-situ heating transmission electron microscopy (TEM) was conducted in a temperature range of 25–650 °C to address the real-time phase transformation for Cr2AlC coating. The results demonstrated that increasing the temperature from 25 to 370 °C led to the structural transformation from amorphous Cr–Al–C to the crystalline Cr2Al interphases. However, the high-purity Cr2AlC MAX phase was distinctly formed at 500 °C, accompanied by the diminished amorphous feature. With the further increase of temperature to 650 °C, the decomposition of Cr2AlC to Cr7C3 impurities was observed. Similar phase evolution was also evidenced by the Ab-initio molecular dynamics calculations, where the bond energy of Cr–Cr, Cr–Al, and Cr–C played the key role in the formed crystalline stability during the heating process. The observations not only provide fundamental insight into the phase formation mechanism for high-purity Cr2AlC coatings but also offer a promising strategy to manipulate the advanced MAX phase materials with high tolerance to high-temperature oxidation and heavy ion radiations.

Thermal Stability and Crystallization Processes of Pd78Au4Si18 Thin Films Visualized via In Situ TEM.

Amorphous alloys or metallic glasses (MGs) thin films have attracted extensive attention in various fields due to their unique functional properties. Here, we use in situ heating transmission electron microscopy (TEM) to investigate the thermal stability and crystallization behavior of Pd-Au-Si thin films prepared by a pulsed laser deposition (PLD) method. Upon heating treatment inside a TEM, we trace the structural changes in the Pd-Au-Si thin films through directly recording high-resolution images and diffraction patterns at different temperatures. TEM observations reveal that the Pd-Au-Si thin films started to nucleate with small crystalline embryos uniformly distributed in the glassy matrix upon approaching the glass transition temperature Tg=625K, and subsequently, the growth of crystalline nuclei into sub-10 nm Pd-Si nanocrystals commenced. Upon further increasing the temperature to 673K, the thin films transformed to micro-sized patches of stacking-faulty lamellae that further crystallized into Pd9Si2 and Pd3Si intermetallic compounds. Interestingly, with prolonged thermal heating at elevated temperatures, the Pd9Si2 transformed to Pd3Si. Simultaneously, the solute Au atoms initially dissolved in glassy alloys and eventually precipitated out of the Pd9Si2 and Pd3Si intermetallics, forming nearly spherical Au nanocrystals. Our TEM results reveal the unique thermal stability and crystallization processes of the PLD-prepared Pd-Au-Si thin films as well as demonstrate a possibility of producing a large quantity of pure nanocrystals out of amorphous solids for various applications.

Orientation distribution and deviation behaviors of dislocation loops in a quenched Al-Cu alloy

Dislocation loops in quenched aluminum alloys are usually seen deviating from their nominal habit planes, while the orientation distribution and deviation mechanism are far from understanding. Based on the method of tomographic crystallography of dislocations and correlative in-situ heating experiments in transmission electron microscopy (TEM), we revisit the three-dimensional (3D) characteristics and deviation behaviors of dislocation loops in a quenched Al-Cu alloy with an aim to fully unravel the relationship between dislocation crystallography and deviation behaviors. The results show that all the dislocation loops exhibit approximately circular shapes and have a/2 < 110>-type Burgers vectors, with loop orientations deviating from their pure edge orientation {110} of 0°-17.8° and distributing mainly close to the [101]-[001] and [101]-[111] edges of the standard stereographic triangle. Three types of deviation behaviors of dislocation loops are then defined, which are characterized by loop rotation around 〈100〉, 〈110〉 and irregular axes, respectively. Theoretical calculations of strain energy variation with increasing deviation angle indicate that the relatively low energy barrier may account for a high frequency of loop deviation in the low angle range. Detailed in-situ TEM heating experiments and correlative tomographic crystallography analyses strongly demonstrate the specific roles of dislocation gliding and climbing at elevated temperatures in the shrinkage, polygonization and deviation processes of dislocation loops, and the competitive and cooperative motion of dislocation segments close to slip planes {111} are the fundamental reasons for the formation of three types of deviated dislocation loops.

Peculiar martensitic microstructure and dislocation accumulation behavior in Ti-Ni-Cu shape memory alloys almost satisfying the triplet condition

Dislocation accumulation behavior at the lattice correspondence variant (CV) triplets of the Ti-Ni-Cu alloy close to the triplet condition (TC) was investigated by using in situ heating transmission electron microscopy observation. The martensitic microstructure of this alloy was peculiar because of no {011}o compound twin laminate as predicted by the phenomenological theory of martensite crystallography. The peculiar martensitic microstructure was composed of a combination of six different CVs connected by twin-relationship, including triplet and quadruple. Other types of triplets with higher incompatibility were not observed. It was revealed that few transformation-induced dislocations associated with thermal cycling were formed at the compatible martensitic microstructure satisfying the TC in the present alloy. The fact that few transformation-induced dislocations are formed in the TC microstructure in the Ti-30Ni-20Cu alloy during thermal cycling explains the good thermal cycling properties of this alloy.

On the role of microstructural defects on precipitation, damage, and healing behavior in a novel Al-0.5Mg2Si alloy

A recently developed healable Al-Mg2Si designed by the programmed damage and repair (PDR) strategy is studied considering the role microstructural defects play on precipitation, damage, and healing. The alloy incorporates sacrificial Mg2Si particles that precipitate after friction stir processing (FSP). They act as damage localization sites and are healable based on the solid-state diffusion of Al-matrix. A combination of different transmission electron microscopy (TEM) imaging techniques enabled the visualization and quantification of various crystallographic defects and the spatial distribution of Mg2Si precipitates. Intragrain nucleation is found to be the dominant mechanism for precipitation during FSP whereas grain boundaries and subgrain boundaries mainly lead to coarsening of the precipitates. The statistical and spatial analyses of the damaged particles have shown particle fracture as the dominant damage mechanism which is strongly dependent on the size and aspect ratio of the particles whereas the damage was not found to depend on the location of the precipitates within the matrix. The damaged particles are associated with dislocations accumulated around them. The interplay of these dislocations is directly visualized during healing based on in situ TEM heating which revealed recovery in the matrix as an operative mechanism during the diffusion healing of the PDR alloy.

Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb ordering transformation caused by &lt;i&gt;in situ&lt;/i&gt; heating-induced Nb diffusion

&lt;sec&gt;This study focuses on the investigation of Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb half-Heusler alloy covered with Nb films. By employing &lt;i&gt;in-situ&lt;/i&gt; heating transmission electron microscopy (TEM) technique, diffusion of Nb is observed at high temperature, showing the ordering transformation from Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb to Nb&lt;sub&gt;0.8+δ&lt;/sub&gt;CoSb. Through observations of high-angle annular dark-field (HAADF) images and selected-area electron diffraction (SAED) patterns, it is found that under elevated temperatures, the diffuse streaks representing short-range disorder in Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb sample transform into superlattice diffraction spots representing long-range order. The modulation wave vector of this superstructure is determined to be &lt;inline-formula&gt;&lt;tex-math id="M3"&gt;\begin{document}$ q={1}/{3}({a}^{*}+{b}^{*}-{c}^{*}) $\end{document}&lt;/tex-math&gt;&lt;alternatives&gt;&lt;graphic specific-use="online" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="11-20240325_M3.jpg"/&gt;&lt;graphic specific-use="print" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="11-20240325_M3.png"/&gt;&lt;/alternatives&gt;&lt;/inline-formula&gt;. This structural evolution primarily arises from the diffusion of Nb atoms from the Nb film into the Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb sample at high temperature, leading to compositional changes in Sb and Nb.&lt;/sec&gt;&lt;sec&gt;Further comparative analysis reveals significant differences between &lt;i&gt;in-situ&lt;/i&gt; synthesized Nb&lt;sub&gt;0.8+δ&lt;/sub&gt;CoSb samples and &lt;i&gt;ex-situ&lt;/i&gt; synthesized Nb&lt;sub&gt;0.84&lt;/sub&gt;CoSb samples despite both exhibiting superstructures. In the &lt;i&gt;ex-situ&lt;/i&gt; synthesized Nb&lt;sub&gt;0.84&lt;/sub&gt;CoSb, the modulation wave vector of the superstructure is &lt;inline-formula&gt;&lt;tex-math id="M4"&gt;\begin{document}$ q={1}/{3}({2a}^{*}-2{c}^{*}) $\end{document}&lt;/tex-math&gt;&lt;alternatives&gt;&lt;graphic specific-use="online" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="11-20240325_M4.jpg"/&gt;&lt;graphic specific-use="print" xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="11-20240325_M4.png"/&gt;&lt;/alternatives&gt;&lt;/inline-formula&gt;, which is mainly attributed to Nb compositional variations. Moreover, the superstructure in Nb&lt;sub&gt;0.84&lt;/sub&gt;CoSb sample can remain stable from room temperature to high temperature, whereas in Nb&lt;sub&gt;0.8+δ&lt;/sub&gt;CoSb samples, it only exists at elevated temperatures and gradually weakens as the temperature decreases, suggesting that it may be a metastable structure between Nb&lt;sub&gt;0.8&lt;/sub&gt;CoSb and Nb&lt;sub&gt;0.84&lt;/sub&gt;CoSb.&lt;/sec&gt;&lt;sec&gt;This study reveals the diversity of superstructures induced by compositional variations and the complexity of structural phase transitions in half-Heusler alloys, enriching the understanding of these materials and providing important guidance for the design and functional control of phase-change materials.&lt;/sec&gt;

Synthesis of high-entropy germanides and investigation of their formation process.

High-entropy alloys and compounds have emerged as an attractive research area in part because of their distinctive solid-solution structure and multi-element compositions that provide near-limitless tailorability. A diverse array of reports describing high-entropy compounds, including carbides, nitrides, sulfides, oxides, fluorides, silicides, and borides, has resulted. Strikingly, exploration of high-entropy germanides (HEGs) has remained relatively limited. In this study, we present a detailed investigation into the synthesis of HEGs, specifically AuAgCuPdPtGe and FeCoNiCrVGe, via a rapid thermal annealing. The structural, compositional, and morphological characteristics of the synthesized HEGs were assessed using laboratory X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM). Complementing these post-synthesis analyses, we interrogated the formation and growth mechanisms using in situ heating XRD and TEM and determined that HEG formation involved initial decomposition of germanane (GeNSs) during the annealing, followed by gradual grain growth via atom diffusion at temperatures below 600 °C, and finally a rapid grain growth process at elevated temperatures.

Crystal Orientation-Dependent Interface Compatibility in the Oxide Composite Cathode by in Situ Heating Transmission Electron Microscopy

All-solid-state batteries (ASSBs) with oxide-based solid electrolytes are getting prominence as a forthcoming battery system capable of overcoming the drawbacks of current lithium-ion batteries by satisfying the expanding demand for high energy density and safety. However, the poor interfacial contact between cathode active materials and solid electrolytes, at which lithium ions diffuse and the charge transfer occurs, is a major concern for practical utilization. Although the co-sintering process at high temperatures is essential to achieve an intimate interface contact, excessive thermal energy reversely accelerates the interfacial degradation reaction, of which the mechanism has been still unexplored. Here, using an epitaxial model system in which the crystal orientations of the Li(Ni1/3Co1/3Mn1/3)O2 cathode and Li3xLa(2/3)-x⎕(1/3)-2xTiO3 solid electrolyte are controlled, we directly probe the interfacial reaction in real-time during heating by in situ heating transmission electron microscopy, and investigate the impact of the crystal orientation at the interface on the interfacial reaction mechanism and kinetics. In situ observation reveals that the interfacial reactions are highly dependent on the crystal orientation at the interface involving the onset temperature of the reaction, the diffusion behavior of lithium ions, the intermediate states, and the overall degradation mechanism between the active material and the solid electrolyte. The interfacial degradation during heating increases the charge transfer resistance between the cathode active material and the solid electrolyte, and the increasing tendency of the resistance is closely related to the crystal orientation-dependent interfacial degradation.

Structural transformation behavior in a high Nb–TiAl alloy additively manufactured by laser powder bed fusion

High Nb–TiAl alloys fabricated using laser powder bed fusion (LPBF) exhibit a metastable α2 phase due to the rapid cooling rate of the LPBF process. However, the understanding of the structural transformation behavior in LPBF-fabricated high Nb–TiAl alloys remains limited. In this work, a high Nb–TiAl alloy with a nominal composition of Ti–48Al–2Cr–8Nb (at. %) was additively manufactured using LPBF. The structural transformation from metastable α2 phase to γ phase was then studied by the in-situ high-temperature x-ray diffraction (XRD), in-situ heating transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). Furthermore, the phase composition and microstructure of the samples annealed at different temperatures were determined by XRD and electron backscatter diffraction (EBSD). Our findings demonstrate that the α2 phase in LPBF-fabricated high Nb–TiAl alloy remains stable up to 873 K, after which it decomposes and forms fine γ lamellar colonies along with a disordered γ′ phase as an intermediate phase. Notably, the transition from α2 to γ′ phase is reversible. In contrast, the formation of the γ phase is irreversible and persists down to room temperature. It is also found that the changes in grain size and phase composition of the LPBF-fabricated high Nb–TiAl alloy have a significant impact on its hardness. This study provides valuable insights into the structural transformation behavior of additively manufactured high Nb–TiAl alloys by LPBF, offering guidance for regulating their structure and properties.

Elucidating Phase Transformation and Surface Amorphization of Li7 La3 Zr2 O12 by In Situ Heating TEM.

Garnet-type Li7 La3 Zr2 O12 (LLZO) solid-state electrolytes hold great promise for the next-generation all-solid-state batteries. An in-depth understanding of the phase transformation during synthetic processes is required for better control of the crystallinity and improvement of the ionic conductivity of LLZO. Herein, the phase transformation pathways and the associated surface amorphization are comparatively investigated during the sol-gel and solid-state syntheses of LLZO using in situ heating transmission electron microscopy (TEM). The combined ex situ X-ray diffraction and in situ TEM techniques are used to reveal two distinct phase transformation pathways (precursors→La2 Zr2 O7 →LLZO and precursors→LLZO) and the subsequent layer-by-layer crystal growth of LLZO on the atomic scale. It is also demonstrated that the surface amorphization surrounding the LLZO crystals is sensitive to the postsynthesis cooling rate and significantly affects the ionic conductivity of pelletized LLZO. This work brings up a critical but often overlooked issue that may greatly exacerbate the Li-ion conductivity by undesired synthetic conditions, which can be leveraged to ameliorate the overall crystallinity to improve the electrochemical performance of LLZO. These findings also shed light on the significance of optimizing surface structure to ensure superior performance of Li-ion conductors.

In situ TEM investigation on the microstructure and phase evolution of hydrogenated Zr-4 alloy

Bonding of Zr-4 alloy at high temperature risked the safe run of nuclear reactors. The diffusion bonding of Zr-4 alloy could be realized at low temperature by hydrogenation. In situ heating transmission electron microscopy was used to observe the microstructure and phase evolution of hydrogenated Zr-4 alloy during heating from room temperature to 650 °C to clarify the bonding mechanism of Zr-4 alloy. Zirconium hydrides gradually decomposed during the heating process and β-Zr phase formed in the matrix as a result. The observed decrease in the β phase transus temperature caused by hydrogen addition was about 210 °C. Results indicated that diffusion bonding of Zr-4 alloy can be achieved at lower temperature via hydrogenation because the β phase with body-centered cubic structure has better deformation ability.

Synthesis and Atomic Transport of CoSn3 NanoIMC by In Situ TEM.

In order to optimize the interfacial properties by adding Co to the bumps of copper pillars and to overcome the strong tendency of Co to oxidize, an intermetallic compound (IMC) "capsule" was developed for the purpose of transporting elements through the intermetallic compound. In this study, we present a comprehensive analysis of the transformation process of CoSn2 nanoparticles into CoSn3 at the nanoscale using in situ heating transmission electron microscopy (TEM). The experimental results reveal that CoSn2 nanoparticle growth occurs through polymerization, whereas CoSn3 nanoparticle formation relies on the reaction between CoSn2 and Sn. During the initial stages of the reaction, Co dissolves and diffuses into Sn, leading to the nucleation and growth of CoSn2 in Sn via Ostwald ripening. As the input energy increases, vacancies in CoSn2 drive a reaction at the Sn/CoSn2 interface, resulting in the generation of CoSn3. In this process, Sn nanoparticles enter the CoSn2 structure through the "Anti Structure Bridge (ASB) mechanism" to fill vacancies. Following the codeposition process, CoSn3 nanoparticles were successfully plated within the Sn layer of the Cu-pillar bumps. Upon reflow heating, the CoSn3 nanoparticles exhibited a preference for precipitating the vacant sites within the Sn layer. This process facilitated the release of Co atoms from CoSn2, enabling their diffusion throughout the entire Sn layer.

Atmospheric Gas and Heating Transmission Electron Microscopy with Water Vapor Control.

Atmospheric Gas and Heating Transmission Electron Microscopy with Water Vapor Control.

Real-Time In Situ Observation of CsPbBr3 Perovskite Nanoplatelets Transforming into Nanosheets.

The manipulation of nano-objects through heating is an effective strategy for inducing structural modifications and therefore changing the optoelectronic properties of semiconducting materials. Despite its potential, the underlying mechanism of the structural transformations remains elusive, largely due to the challenges associated with their in situ observations. To address these issues, we synthesize temperature-sensitive CsPbBr3 perovskite nanoplatelets and investigate their structural evolution at the nanoscale using in situ heating transmission electron microscopy. We observe the morphological changes that start from the self-assembly of the nanoplatelets into ribbons on a substrate. We identify several paths of merging nanoplates within ribbons that ultimately lead to the formation of nanosheets dispersed randomly on the substrate. These observations are supported by molecular dynamics simulations. We correlate the various paths for merging to the random orientation of the initial ribbons along with the ligand mobility (especially from the edges of the nanoplatelets). This leads to the preferential growth of individual nanosheets and the merging of neighboring ones. These processes enable the creation of structures with tunable emission, ranging from blue to green, all from a single material. Our real-time observations of the transformation of perovskite 2D nanocrystals reveal a route to achieve large-area nanosheets by controlling the initial orientation of the self-assembled objects with potential for large-scale applications.

In Situ Transmission Electron Microscopy Observation of Melted Germanium Encapsulated in Multilayer Graphene

AbstractGermanene is a two‐dimensional germanium (Ge) analogous of graphene, and its unique topological properties are expected to make it a material for next‐generation electronics. However, no germanene electronic devices have yet been reported. One of the reasons for this is that germanene is easily oxidized in air due to its lack of chemical stability. Therefore, growing germanene at solid interfaces where it is not oxidized is one of the key steps for realizing electronic devices based on germanene. In this study, the behavior of Ge at the solid interface at high temperatures is observed by transmission electron microscopy (TEM). To achieve such in situ heating TEM observation, this work fabricates a graphene/Ge/graphene encapsulated structure. In situ heating TEM experiments reveal that Ge like droplets move and coalesce with other Ge droplets, indicating that Ge remains as a liquid phase between graphene layers at temperatures higher than the Ge melting point. It is also observed that Ge droplets incorporate the surrounding amorphous Ge as Ge nuclei, thereby increasing its size (domain growth). These results indicate that Ge crystals can be grown at the interface of van der Waals materials, which will be important for future germanene growth at solid interfaces.

Thermolysis-Driven Growth of Vanadium Oxide Nanostructures Revealed by In Situ Transmission Electron Microscopy: Implications for Battery Applications.

Understanding the growth modes of 2D transition-metal oxides through direct observation is of vital importance to tailor these materials to desired structures. Here, we demonstrate thermolysis-driven growth of 2D V2O5 nanostructures via in situ transmission electron microscopy (TEM). Various growth stages in the formation of 2D V2O5 nanostructures through thermal decomposition of a single solid-state NH4VO3 precursor are unveiled during the in situ TEM heating. Growth of orthorhombic V2O5 2D nanosheets and 1D nanobelts is observed in real time. The associated temperature ranges in thermolysis-driven growth of V2O5 nanostructures are optimized through in situ and ex situ heating. Also, the phase transformation of V2O5 to VO2 was revealed in real time by in situ TEM heating. The in situ thermolysis results were reproduced using ex situ heating, which offers opportunities for upscaling the growth of vanadium oxide-based materials. Our findings offer effective, general, and simple pathways to produce versatile 2D V2O5 nanostructures for a range of battery applications.

Dynamics of the fcc-to-bcc phase transition in single-crystalline PdCu alloy nanoparticles

Two most common crystal structures in metals and metal alloys are body-centered cubic (bcc) and face-centered cubic (fcc) structures. The phase transitions between these structures play an important role in the production of durable and functional metal alloys. Despite their technological significance, the details of such phase transitions are largely unknown because of the challenges associated with probing these processes. Here, we describe the nanoscopic details of an fcc-to-bcc phase transition in PdCu alloy nanoparticles (NPs) using in situ heating transmission electron microscopy. Our observations reveal that the bcc phase always nucleates from the edge of the fcc NP, and then propagates across the NP by forming a distinct few-atoms-wide coherent bcc–fcc interface. Notably, this interface acts as an intermediate precursor phase for the nucleation of a bcc phase. These insights into the fcc-to-bcc phase transition are important for understanding solid − solid phase transitions in general and can help to tailor the functional properties of metals and their alloys.