Cross-sectional Transmission Electron Microscopy Research Articles

Morphological Evolution of Atomic Layer Deposited Hafnium Oxide on Aligned Carbon Nanotube Arrays.

Microscopic study of the nucleation and growth of atomic layer deposition (ALD) dielectrics onto carbon nanotubes (CNTs) is an essential while challenging task toward high-performance devices. Here, we capture the morphological evolution and growth behaviors of ALD-HfO2 onto SiO2/Si-supported aligned CNT arrays (A-CNTs) under three ALD recipes via cross-sectional high-resolution scanning transmission electron microscopy. The HfO2 in ALD I (200 °C) preferentially nucleates on the SiO2 substrate in heterogeneous growth mode, resulting in films with considerable pinholes, while ALD II (90 °C) and III (90 °C and extra H2O presoak) exhibit homogeneous growth with nucleation on both SiO2 and CNTs, yielding uniform films. Arrangement defects in A-CNTs exacerbate nonuniformity of HfO2 and tube-tube separation plays deterministic roles affecting the HfO2-CNT interfacial morphology. Electrical measurements from A-CNTs metaloxide-semiconductor devices validate these findings. Our investigation contributes valuable insights for optimizing ALD processes for enhanced dielectric integration on A-CNTs in next-generation electronics.

Oxygen Vacancy Compensation-Induced Analog Resistive Switching in the SrFeO3-δ/Nb:SrTiO3 Epitaxial Heterojunction for Noise-Tolerant High-Precision Image Recognition.

Neuromorphic computing, inspired by the brain's architecture, promises to surpass the limitations of von Neumann computing. In this paradigm, synaptic devices play a crucial role, with resistive switching memory (memristors) emerging as promising candidates due to their low power consumption and scalability advantages. This study focuses on the development of metal/oxide-semiconductor heterojunctions, which offer several technological advantages and have broad potential for applications in artificial neural synapses. However, constructing high-quality epitaxial interfaces between metal and oxide semiconductors and designing modifiable contact barriers are challenging. Herein, we construct high-quality epitaxial metal/semiconductor interfaces based on the metallicity of the perovskite phase SrFeO3-δ (PV-SFO) and a small Schottky barrier in contact with Nb-doped SrTiO3 (NSTO). X-ray diffraction patterns, reciprocal space mapping results, and cross-sectional transmission electron microscopy images reveal that the prepared PV-SFO film exhibits a perfect single-crystal structure and an excellent epitaxial interface with the NSTO (111) substrate. The corresponding memristor exhibits analog-type resistive-variable characteristics with an ON/OFF ratio of ∼1000, stable data retention after 10,000 s, and no noticeable fluctuation in resistance after 10,000 pulse cycles. Electron energy loss spectroscopy, first-principles calculations, and electrical measurements reveal that compensating or restoring oxygen vacancies at the NSTO surface decreases or increases the contact barrier between PV-SFO and NSTO, respectively, thereby gradually regulating the resistance value. Furthermore, high-quality epitaxial PV-SFO/NSTO devices achieve up to 98.21% recognition accuracy for handwriting recognition tasks using LeNet-5-based network structures and 92.21% accuracy for color images using visual geometry group (VGG) network structures. This work contributes to the advancement of interface-type memristors and provides valuable insights into enhancing synaptic functionality in neuromorphic computing systems.

Formation of High-Photoresponsivity BaSi2 Films by Radio-Frequency Sputtering and Evaluation of a BaSi2/TiN/Glass Heterojunction by Transmission Electron Microscopy.

Barium disilicide (BaSi2) is a thin-film solar cell material composed of abundant elements, and its application potential is further enhanced by its formation on inexpensive substrates, such as glass. The effect of the substrate temperature on the co-sputtering of BaSi2 and Ba targets to form BaSi2 films on Si(111) and TiN/glass substrates was investigated. Contrary to expectations, the photoresponsivity reached maximum values exceeding 5 and 2 A W-1, respectively, the highest value ever reported for as-deposited samples formed at 750 °C, more than 100 °C higher than those reported previously. Because the photoresponsivity is proportional to carrier lifetime, this result indicates that high-temperature growth can bring out the high performance of BaSi2 as a light-absorbing layer. Because amorphous SiC (a-SiC) has a larger forbidden band gap and electron affinity than BaSi2, it is considered suitable as an electron transport layer (ETL) material for BaSi2 solar cells. On the basis of this, the formation of BaSi2 (absorption layer)/a-SiC (ETL)/TiN (electrode)/glass heterojunctions was also attempted, and the layered structure was examined by cross-sectional transmission electron microscopy (TEM). Polycrystalline BaSi2 films were found to be even on the amorphous layer by TEM. A high photoresponsivity of over 2 A W-1 was obtained. Therefore, the BaSi2/a-SiC/TiN structure provides a guideline for the structural design of BaSi2-based thin-film solar cells on glass.

Enhanced device performance of GaN high electron mobility transistors with in situ crystalline SiN cap layer

In this paper, a ∼2 nm in situ SiN cap layer on AlGaN barrier layer is grown, which is revealed to be crystalline using high-resolution cross-sectional transmission electron microscopy. Benefitting from superior interface quality of epitaxial crystalline SiN/AlGaN interface, the gate diodes with in situ SiN cap layer feature lower interface trap state density than that with GaN cap layer. By comparing the GaN high electron mobility transistors (HEMTs) with the conventional GaN cap layer, the GaN HEMTs with in situ SiN cap layer exhibit improved device performance, showing higher electron mobility, higher drain current, larger on/off current ratio, and higher transconductance. For breakdown characteristics, the devices with in situ crystalline SiN cap layer show prominent advantages over the GaN cap layer with a 30% breakdown voltage increase to 810 V.

Growth of Hg0.7Cd0.3Te on Van Der Waals Mica Substrates via Molecular Beam Epitaxy.

In this paper, we present a study on the direct growth of Hg0.7Cd0.3Te thin films on layered transparent van der Waals mica (001) substrates through weak interface interaction through molecular beam epitaxy. The preferred orientation for growing Hg0.7Cd0.3Te on mica (001) substrates is found to be the (111) orientation due to a better lattice match between the Hg0.7Cd0.3Te layer and the underlying mica substrate. The influence of growth parameters (mainly temperature and Hg flux) on the material quality of epitaxial Hg0.7Cd0.3Te thin films is studied, and the optimal growth temperature and Hg flux are found to be approximately 190 °C and 4.5 × 10-4 Torr as evidenced by higher crystalline quality and better surface morphology. Hg0.7Cd0.3Te thin films (3.5 µm thick) grown under these optimal growth conditions present a full width at half maximum of 345.6 arc sec for the X-ray diffraction rocking curve and a root-mean-square surface roughness of 6 nm. However, a significant number of microtwin defects are observed using cross-sectional transmission electron microscopy, which leads to a relatively high etch pit density (mid-107 cm-2) in the Hg0.7Cd0.3Te thin films. These findings not only facilitate the growth of HgCdTe on mica substrates for fabricating curved IR sensors but also contribute to a better understanding of growth of traditional zinc-blende semiconductors on layered substrates.

Nanometer-thick molecular beam epitaxy Al films capped with in situ deposited Al2O3—High-crystallinity, morphology, and superconductivity

Achieving high material perfection in aluminum (Al) films and their associated Al/AlOx heterostructures is essential for enhancing the coherence time in superconducting quantum circuits. We grew Al films with thicknesses ranging from 3 to 30 nanometers (nm) epitaxially on sapphire substrates using molecular beam epitaxy (MBE). An integral aspect of our work involved electron-beam (e-beam) evaporation to directly deposit aluminum oxide (Al2O3) films on the freshly grown ultrathin epitaxial Al films in an ultra-high-vacuum (UHV) environment. This in situ oxide deposition is critical for preventing the oxidation of parts of the Al films, avoiding the formation of undesired native oxides, and thereby preserving the nm-thick Al films in their pristine conditions. The thicknesses of our Al films in the study were accurately determined; for example, coherence lengths of 3.0 and 20.2 nm were measured in the nominal 3.0 and 20 nm thick Al films, respectively. These Al films were epitaxially grown on sapphire substrates, showing an orientational relationship, denoted as Al(111)⟨21¯1¯⟩∥sapphire(0001)[21¯1¯0]. The Al/sapphire interface was atomically ordered without any interfacial layers, as confirmed by in situ reflection high-energy electron diffraction (RHEED) and cross-sectional scanning transmission electron microscopy (STEM). All sample surfaces exhibited smoothness with a roughness in the range of 0.1–0.2 nm. The Al films are superconducting with critical temperatures ranging from 1.23 to around 2 K, depending on the film thickness.

Achieving high sheet resistance and near-zero temperature coefficient of resistance in NiCr film resistors by Al interlayers

Thin film resistive materials with low temperature coefficients of resistance (TCR) and high sheet resistances are essential for various electronic applications, such as embedded resistors. In this study, Al inserting layers and NiCr resistive layers were sequentially deposited on alumina ceramic substrates via DC magnetron sputtering to fabricate Al/NiCr bilayer resistive materials. The electrical properties of the bilayer films were adjusted by varying the thicknesses of the Al inserting layers and annealing conditions. When the thickness of the Al inserting layer varied from 5 to 7.5 nm, and post-annealing treatments ranging from 200℃ to 400℃ were applied, evident Al-NiCr interdiffusion occurred, forming intermediate layers at the interfaces and oxides on the film surfaces. A mixture of partial crystalline phases and amorphous phases was also observed in the cross-sectional high-resolution transmission electron microscope (HRTEM) images. The formation of intermediate layers and surface oxides and the balance between partial crystalline phases and amorphous phases collectively enhanced the electrical performance of bilayer film resistors, achieving thin film resistors with a remarkably low TCR of −6.61 ppm/K and a sheet resistance of up to 265.95 Ω/sq. By rational design of Al layers, NiCr layers and thermal treatment, thin film resistors with near zero TCRs and extremely wide sheet resistance range of 93.34–1439.01 Ω/sq can be obtained.

Gasb-to-Si Direct Wafer Bonding and Thermal Budget Considerations for Photonic Applications

Extensive progress has been made in recent years in heterogeneous integration (HI) of III-V materials on Si photonics wafers [1], including direct chip-to-chip bonding of GaSb-based infrared (IR) lasers [2], greatly expanding the application space and performance of either material system on its own. This includes active research at Sandia National Labs developing lasers based on GaAs, GaSb, GaN, and InP substrates directly integrated with silicon photonics at the chip and wafer scale. A “device last” process flow is desirable in this case both for scalability and because of the tight alignment tolerance required between the Si waveguides and active III-V laser elements to optimally couple light between the III-V and the Si. In this process flow, the Si photonics wafer is fabricated separately before bonding with an unpatterned III-V wafer or chip. The III-V laser is then defined after bonding, allowing lithographic registration to Si photonics structures. Thus, preparation of both semiconductor surfaces and preservation of the bond between them become critical for device performance and constrain subsequent process steps. Here, we focus on GaSb-based devices.The first consideration is preparing the GaSb and Si surfaces for bonding. Argon sputtering to prepare the GaSb surface for bonding to Si has been investigated, though the emphasis was on GaSb surface roughness, bonding temperature, and electronic transport through the interface [3]. Here, we use x-ray photoelectron spectroscopy (XPS) to investigate the impact of the GaSb oxide composition on the quality of the bond to oxidized Si wafers. In Fig. 1(a)-(c) we use confocal scanning acoustic microscopy (CSAM) to compare as-received 3” GaSb substrates with and without chemical oxide removal to epitaxial GaSb. In the CSAM images, dark areas indicate bond adhesion. We find that bonding improves with decreasing Ga-oxide content realized on the epitaxial GaSb.The second consideration is constraining the laser process steps in order to preserve the bond between the Si photonics and GaSb wafers. Our HI process steps involving GaSb thinning and substrate removal have been described elsewhere [4], though investigation of the thermal budget for survival of the direct GaSb/Si bond through a laser fabrication process flow is lacking in the literature. As the thermal expansion coefficient of GaSb is approximately three times that of Si, temperatures must be limited to prevent the GaSb from expanding excessively and delaminating from the Si wafer when running the III-V laser fabrication after integration with the Si photonics wafer. We investigate the robustness of the bond between epitaxial GaSb and the Si photonics wafer through cross-sectional transmission electron microscopy (TEM) of the bond interface after various process steps typical to laser fabrication and the implications of the thermal budget on these process steps. For example, we find that extended periods of time (more than an hour) at 250°C, which is typical for chemical vapor deposition (CVD) of SiO2 or Si3N4, cause the thinned III-V wafer to delaminate from the Si photonics wafer. While we don’t observe destructive delamination at lower processing temperatures, high-angle annular dark-field imaging (HAADF) analysis in Fig. 1(d) shows significant Sb diffusion into the Si photonics native SiO2 layer.In summary, for optimal performance of GaSb-based hybrid lasers directly bonded to Si photonics, understanding and preserving the bond between these materials is critical. These considerations include minimizing the Ga-oxide at the GaSb surface prior to bonding to promote bond success and keeping extended thermal processes below 250°C to maintain the bond between the GaSb and the Si photonics wafers. These results will inform processes required for full laser fabrication flow, particularly in steps that traditionally require higher or longer temperature parameters.SNL is managed and operated by NTESS under DOE NNSA contract DE-NA0003525.[1] D. Caimi, et al., IEEE Trans. Elect. Dev. 68, p. 3149 (2021).[2] A. Spott, et al., Optica 5, p. 996 (2018).[3] F. Predan, et al., Appl. Surf. Scie., 353, p. 1203 (2015).[4] M. Wood, et al., in CLEO 2023 Technical Digest Series, STh3H.5 (2023). Figure 1

(Invited) Role of Oxidant Gas for Atomic Layer Deposition of HfxZr1−XO2 Thin Films on Ferroelectricity of Metal-Ferroelectric-Metal Capacitors

Since the first report of ferroelectricity in HfxZr1−xO2 (HZO) in 2011 [1], a lot of attention has been devoted for future non-volatile memory device applications due to its scalability (< 10 nm), low thermal budget (< 400°C) and matured atomic layer deposition (ALD) technique [2]. The thermal ALD process using H2O or O3 is generally employed for the fabrication of ferroelectric HZO thin films. On the other hand, the effect of the plasma-enhanced ALD process using O2 plasma gas on the crystallinity and ferroelectricity has not been systematically clarified. In this paper, we report the importance of ALD oxidant gases for HZO films using H2O or O2 plasma on the ferroelectricity of metal–ferroelectric–metal (MFM) capacitors.MFM capacitors with the H2O- and O2 plasma-based HZO films were fabricated as follows. A 10-nm-thick HZO films were deposited on a TiN bottom-electrode (BE-TiN) by ALD at 300°C using H2O or O2 plasma as oxidant gases and (Hf/Zr)[N(C2H5)CH3]4 (Hf:Zr = 1:1) cocktail precursor. The Hf/Zr ratios in both types of HZO films were estimated to be 0.4/0.6 using X-ray photoelectron spectroscopy (XPS). Next, a post-deposition annealing (PDA) process was carried out at 400 °C for 1 min under a N2 atmosphere. Finally, a TiN top-electrode was deposited by DC sputtering.First, the crystallinity and remanent polarization (2P r = P r + − P r −) of the H2O- and O2 plasma-based HZO films were investigated. Nanocrystals with ferroelectric orthorhombic (O), tetragonal (T), cubic (C) phases partially existed in the O2 plasma-based film after the ALD process, while an amorphous structure dominantly existed in the H2O-based film, analyzed by the grazing-incidence X-ray diffraction analysis and cross-sectional transmission electron microscopy images [3]. This could be because of a strong oxidation power and high energy ion/electron bombardment of O2 plasma. After the PDA process, the O phase was formed more in the O2 plasma-based HZO film than the H2O-based film. Therefore, the nanocrystal grains in the as-grown O2 plasma-based HZO film could play an important role as nuclei for the crystallization and formation of O phase [3,4]. From the polarization–electric field hysteresis curves, the PDA-treated O2 plasma-based capacitor exhibited 2P r of 20 µC/cm2, which was 1.5 times higher than that (13 µC/cm2) of the H2O-based capacitor. Thus, these results indicate that the crystallization and O phase formation of HZO films were promoted by using O2 plasma gas as an ALD oxidant, resulted in a higher 2P r.Next, endurance properties of these MFM capacitors were evaluated. In the wake-up state, both capacitors showed almost the same increase rate (~8%) of switching polarization (P sw). In the fatigued state, on the other hand, the O2 plasma-based capacitor exhibited less P sw degradation (~33%) after 106 cycles, whereas the P sw of H2O-based capacitor decreased by ~47%. To clarify these different fatigue properties, the TiOxNy interface reaction layer (IRL) formation at the HZO/BE-TiN interface was analyzed using synchrotron hard X-ray photoelectron spectroscopy (HAXPES). For the HAXPES Ti 2p spectra, the Ti-O peak intensity for the O2 plasma-based capacitor was larger than that of the H2O-based capacitor [5]. Therefore, an oxygen-rich TiON-IRL could be formed at the HZO/BE-TiN interface during ALD process due to the stronger oxidizing power of O2 plasma. Additional oxygen vacancies (VO) were reported to formed in HfO2-based films during field cycling due to the interface reaction between the HfO2-based film and TiN electrode. Moreover, one of the origins of the P sw degradation was thought to be domain pinning caused by VO [6]. Therefore, an oxygen-rich TiON-IRL for the MFM capacitor with the O2 plasma-based HZO film could prevent the interface reaction and formation of additional VO in HZO films, led to superior fatigue properties.In summary, the MFM capacitor with the O2 plasma-based HZO film showed superior 2Pr and fatigue resistance compared to those of the H2O-based one. Based on these experimental results, it is important to consider the selection of an ALD oxidant for fabrication of HZO-based MFM capacitors.This work was partly supported by JSPS KAKENHI (Nos. JP21J01667, JP20H02189, and JP18J22998) and MEXT Leading Initiative for Excellent Young Researchers (No. JPMXS0320220213). The HAXPES measurements were performed under approval of the NIMS Synchrotron X-ray Station (2020A4602 and 2020A4651).[1] J. Müller et al., Appl. Phys. Lett. 99, 112901 (2011).[2] J.-H. Kim et al., ACS Appl. Electron. Mater. 5, 4726 (2023).[3] T. Onaya et al., APL Mater. 10, 051110 (2022).[4] T. Onaya et al., Microelectron. Eng. 215, 111013 (2019).[5] T. Onaya et al., Solid State Electron. 210, 108801 (2023).[6] M. Pešić et al., Adv. Funct. Mater. 26, 4601 (2016).

Nonideality in Arrayed Carbon Nanotube Field Effect Transistors Revealed by High-Resolution Transmission Electron Microscopy.

High density and high semiconducting-purity single-walled carbon nanotube array (A-CNT) have recently been demonstrated as promising candidates for high-performance nanoelectronics. Knowledge of the structures and arrangement of CNTs within the arrays and their interfaces to neighboring CNTs, metal contacts, and dielectrics, as the key components of an A-CNT field effect transistor (FET), is essential for device mechanistic understanding and further optimization, particularly considering that the current technologies for the fabrication of A-CNT wafers are mainly laboratory-level solution-based processes. Here, we conduct a systematic investigation into the microstructures of A-CNT FETs mainly via cross-sectional high-resolution transmission electron microscopy and tentatively establish a framework consisting of up to 11 parameters which can be used for structure-side quality evaluation of the A-CNT FETs. The parameter ensemble includes the diameter, length (or terminal), and density distribution of CNTs, radial deformation of CNTs, array alignment defects, surface crystallography facets of contact metal, thickness distribution of high-k dielectrics (HfO2), and the contact ratios for the CNT-CNT, CNT-metal, CNT-dielectric, and CNT-substrate interfaces. Enriched array alignment defects, i.e., bundle, stacking, misorientation, and voids, are observed with a total ratio sometimes up to ∼90% in pristine A-CNTs and even up to ∼95% after the device fabrication process. Thus, they are suggested as the prevalent performance-limiting factors for A-CNT FETs. Complex interfacial structures are observed at the CNT-CNT, CNT-metal contact, and CNT-high-k dielectric interfaces, making the local environment and the property of each component CNT involved in an A-CNT FET distinct from others in terms of the diameters, radial deformation, and interactions with the local surroundings (mainly through van der Waals interactions). The present study suggests further improvements on the fabrication technology of A-CNT wafers and devices and mechanistic investigations into the impacts of complex array alignment defects and interface structures on the electrical performance of A-CNT FETs as well.

Stochastic nature of incipient plasticity in a body-centered cubic medium-entropy alloy

The stochastic nature of the small-scale incipient plasticity (i.e., “pop-in” behavior manifested as a sudden displacement excursion in the load-displacement curves) in a single grain of the body-centered cubic NbTiZr medium-entropy alloy is explored through a series of nanoindentation tests with three spherical tips having different radii (1.8, 3.4, and 8.2 μm). The maximum shear stress underneath the indenter shows distinct distributions depending on the tip radius, wherein both a narrow high-stress regime and a broad low-stress regime are observed. By recourse to deconvolution of the data and detailed statistical analysis, the two regimes were found to be dominated by homogeneous and heterogeneous yielding mechanisms, respectively. Upon hydrogen charging, the tip radius dependence is sustained, but the fraction of heterogeneous yielding is enhanced, which is due to the hydrogen's effect in assisting defect formation. The suggested scenarios for how the mechanisms are affected by the stressed volume (or tip radius) and hydrogen-induced structural changes were confirmed by direct observations of the deformation behavior underneath the indenter with cross-sectional transmission electron microscopy made on post-pop-in samples.

Metallic nanofilms on Si(100) and SiO2 grown with a ruthenium precursor

Ruthenium (Ru) nanofilms (<3 nm) were prepared using tricarbonyl(trimethylenemethane)ruthenium, Ru(TMM)(CO)3 at 230 °C. We show that the surface morphology and electrical conductance of Ru nanofilms are substantially different on H:Si(100) and SiO2/Si(100) substrates. Two-dimensional (2D) Ru nanofilms (∼1 nm) were formed on H:Si(100), while thick (∼3 nm) granular Ru films were formed on SiO2 substrate under the same growth conditions, as confirmed by cross-sectional transmission electron microscopy and X-ray photoelectron spectroscopy. Using scanning probe microscopy, the metallic conductance of Ru grains on H:Si(100) substrates was recognized. On ultrathin (1 nm) SiO2/Si(100) substrates, the spatial separation of Ru grains facilitates the single electron tunneling (SET) phenomenon in the double barrier tunnel junction structure. The results emphasized the difference in carrier transport in Ru nanofilms on Si and SiO2 substrates.

Alleviating internal stress in diamond-like carbon films for enhanced tribological performance under high contact pressure via interface texturing

Diamond-like carbon (DLC) films have found widespread applications across numerous fields due to their exceptional properties. Nevertheless, their significant internal stress has restricted their further utility, particularly in scenarios involving high-contact pressure conditions. In response to this challenge, we fabricated diamond-like carbon films with nano-depth interface texture. This nano-depth interface texturing technique helps alleviate the internal stress within the carbon film, thereby enhancing the tribological performance of diamond-like carbon films with textured interfaces, especially under high contact pressure. We successfully fabricated textured carbon films with a thickness of 1 μm, which exhibited excellent tribological performance even under pressures exceeding 1 GPa. Through atomistic molecular dynamics simulations, internal stress testing, and cross-sectional transmission electron microscopy imaging, we observed that the incorporation of nano-depth interface texturing resulted in an approximate 47.62 % increase in the thickness of the transition layer between the silicon substrate and the carbon film. Furthermore, there was a notable reduction of about 30 % in the internal stress exhibited by the carbon films. These findings are expected to expand the application of carbon films under higher contact pressure and facilitate the production of thicker films.

The role of carbon segregation in the electrical activity of dislocations in carbon doped GaN

Dislocations have been proposed to affect the performance and reliability of GaN power semiconductors by being conductive pathways for leakage current. However, no direct evidence of a link between their electrical behavior and physical nature in carbon-doped semi-insulating GaN buffer layers has been obtained. Therefore, we investigate the electrical activity of dislocations by conductive atomic force microscopy and electron beam induced current to distinguish electrically active dislocations from non-active ones. We investigated six electrically active dislocations and discovered distinct carbon enrichment in the vicinity of all six dislocations, based on cross-sectional scanning transmission electron microscopy using electron energy loss spectrometry. Electrically non-active dislocations, which are the vast majority, sometimes also showed carbon enrichment, however, in only two out of seven cases. Consequently, carbon segregation seems to be a requirement for electrical activity, but a carbon surplus is not sufficient for electrical activity. We also performed first-principles total-energy calculations for mixed type threading dislocations, which validates carbon accumulation in the dislocation vicinity. The electrical and physical characterization results, complemented by density functional theory simulations, support the previously hypothesized existence of a carbon defect band and add new details.

Continuous Template Growth of Large-Scale Tellurene Films on 1T'-MoTe2.

Use of a template triggers an epitaxial interaction with the depositing material during synthesis. Recent studies have demonstrated that two-dimensional tellurium (tellurene) can be directionally oriented when grown on transition metal dichalcogenide (TMD) templates. Specifically, employing a T-phase TMD, such as WTe2, restricts the growth direction even further due to its anisotropic nature, which allows for the synthesis of well-oriented tellurene films. Despite this, producing large-area epitaxial films still remains a significant challenge. Here, we report the continuous synthesis of a 1T'-MoTe2 template via chemical vapor deposition and tellurene via vapor transport. The interaction between helical Te and the 1T'-MoTe2 template facilitates the Te chains to collapse into ribbon shapes, enhancing lateral growth at a rate approximately 6 times higher than in the vertical direction, as confirmed by scanning electron microscopy and atomic force microscopy. Interestingly, despite the predominance of the lateral growth, cross-sectional transmission electron microscopy analysis of the tellurene ribbons revealed a consistent 60-degree incline at the edges. This suggests that the edges of the tellurene ribbons, where they contact the template surface, are favorable sites for additional Te absorption, which then stacks along the incline angle to expand. Furthermore, controlling the synthesis temperature, duration, and preheating time has facilitated the successful synthesis of tellurene films. The resultant tellurene exhibited hole mobility as high as ∼400 cm2/V s. After removing the underlying metallic template with plasma treatment, the film showed a current on/off ratio of ∼103. This ratio was confirmed by two-terminal field-effect transistor measurements and supported by near-field terahertz (THz) spectroscopy mapping.

Interband cascade light-emitting diodes grown on silicon substrates using GaSb buffer layer

Interband cascade light-emitting diodes (ICLEDs) offer attractive advantages for infrared applications, which would greatly expand if high-quality growth on silicon substrates could be achieved. This work describes the formation of threading dislocations in ICLEDs grown monolithically on GaSb-on-Silicon wafers. The epitaxial growth is done in two stages: the GaSb-on-Silicon buffer is grown first, followed by the ICLED growth. The buffer growth involves the nucleation of a 10-nm-thick AlSb buffer layer on the silicon surface, followed by the GaSb growth. The AlSb nucleation layer promotes the formation of 90° and 60° interfacial misfit dislocations, resulting in a highly planar morphology for subsequent GaSb growth that is almost 100% relaxed. The resulting GaSb buffer for growth of the ICLED has a threading dislocation density of ∼107/cm2 after ∼3 μm of growth. The fabricated LEDs showed variations in device performance, with some devices demonstrating comparable light–current–voltage curves to those for devices grown on GaSb substrates, while other devices showed somewhat reduced relative performance. Cross-sectional transmission electron microscopy observations of the inferior diodes indicated that the multiplication of threading dislocations in the active region had most likely caused the increased leakage current and lower output power. Enhanced defect filter layers on the GaSb/Si substrates should provide more consistent diode performance and a viable future growth approach for antimonide-based ICLEDs and other infrared devices.

Influence of Multilayer Structure on the Structural and Mechanical Properties of TiAlN/CrN Coatings for Advanced Machining Applications

This study investigates single and multilayer TiAlN/CrN nanocomposite thin films developed using an RF magnetron sputtering system. The TiAlN and CrN layers showed a high degree of orientation, with the (200) peak being the strongest peak in both layers, and a multilayer structure was clearly observed. The surface roughness analysis using atomic force microscopy (AFM) and cross-sectional transmission electron microscopy (TEM) revealed that the TiAlN/CrN coatings had a smoother surface than the single-layer coatings and minimal intermixing between the two layers. Depth-sensing indentation measurements were used to measure the hardness and Young’s modulus of the coatings, demonstrating that TiAlN/CrN coating had the highest hardness (~16.38 GPa) and elastic modulus (~3.82 GPa) among all the coatings studied. This indicates that the TiAlN/CrN multilayer coating possesses superior mechanical properties due to its interface strength. Our findings suggest that these multilayer coatings have potential applications in tribological and decorative coatings.

Synthesis of multilayered h-BN film on the molten Ni–B and the influence of underneath W substrate

High-quality two-dimensional hexagonal boron nitride (h-BN) film with tens of layers has been used as a universal substrate and capping layer for the van der Waals devices. Various approaches have been carried out for the synthesis of multilayered h-BN. Among them, the metal flux method is reliable in yielding h-BN crystals with high crystalline quality. However, this time- and energy-demanding method hinders its scale application. Herein, inspired by the metal flux method, we reported the time-effective growth of high-quality multilayered h-BN film (ca. 20 nm) on a molten Ni–B layer wetting on W substrate with chemical vapor deposition method. The film exhibits an excellent stacking sequence and a full-width at half maximum of the Raman E2g peak narrow to 9.5 cm−1. Cross-sectional high-resolution transmission electron microscopy and in-situ x-ray diffraction spectroscopy were carried out to investigate the crystal structure evolution of Ni–B layer wetting on W substrate. It is found that the low surface tension caused by the spreading of Ni–B alloy on the W substrate and the presence of the Ni subsurface may be responsible for the formation of multilayered h-BN with excellent crystalline quality. Meanwhile, the W diffusion in Ni–B-based melt can hinder the formation of h-BN under certain growth conditions. The approach demonstrates the feasibility of large-scale growth of multilayered h-BN, paving the way to future applications in van der Waals electronic and optoelectronic devices.

Subsurface damage evolution of β-Ga2O3 (010) substrates during lapping and chemical mechanical polishing

For semiconductor single crystal substrates, subsurface damage (SSD) is an important factor for device failure. For β-Ga2O3 with two cleavage planes, the SSD is the key issue that needs to be addressed. In this work, β-Ga2O3 (010) substrates were lapped and polished precisely. The formation and evolution mechanisms of SSD were analyzed by cross-section transmission electron microscopy and wet chemical etching techniques. The linear distribution of scratches was found on the substrates after lapping. After chemical mechanical polishing (CMP), the surface scratches were eliminated. However, the SSD layer may still exist under the surface. Chemical etching was developed to identify the "invisible damage" to the CMP-finished (010) substrate. The SSD including nanocrystalline, tilt boundary, twist boundary, and high-density dislocations in β-Ga2O3 was first reported. Distinctively, there was no slip occurrence in the SSD of the (010) plane different from the (100) and (001) planes. The Schmid factor of multiple slip systems was calculated to analyze the cause of no slip on the subsurface. The formation mechanism of SSD was believed that when the slip system could not be activated, the stress was released through rotation and distortion of the crystal plane. The accumulation of grain boundary dislocations at twist grain boundary junctions provided a driving force for the formation of nanovoids. The relationship of substrate damage evolution and crystal strain with different machining parameters was established by high-resolution X-ray diffraction and Raman spectra. A non-damaging β-Ga2O3 (010) substrate with a surface roughness of less than 0.2 nm was obtained by the optimized CMP process. The research results had guiding significance for damage control of β-Ga2O3 and other brittle crystals in ultra-precision machining.

Room-temperature spin injection across a chiral perovskite/III-V interface.

Spin accumulation in semiconductor structures at room temperature and without magnetic fields is key to enable a broader range of optoelectronic functionality1. Current efforts are limited owing to inherent inefficiencies associated with spin injection across semiconductor interfaces2. Here we demonstrate spin injection across chiral halide perovskite/III-V interfaces achieving spin accumulation in a standard semiconductor III-V (AlxGa1-x)0.5In0.5P multiple quantum well light-emitting diode. The spin accumulation in the multiple quantum well is detected through emission of circularly polarized light with a degree of polarization of up to 15 ± 4%. The chiral perovskite/III-V interface was characterized with X-ray photoelectron spectroscopy, cross-sectional scanning Kelvin probe force microscopy and cross-sectional transmission electron microscopy imaging, showing a clean semiconductor/semiconductor interface at which the Fermi level can equilibrate. These findings demonstrate that chiral perovskite semiconductors can transform well-developed semiconductor platforms into ones that can also control spin.