Surface Hillocks Research Articles

Nanogap resistive switch mechanism study and performance degradation analysis

The nanogap resistive switch holds potential as a candidate for nonvolatile memory, although its durability needs enhancement. This study delves into the operational mechanisms through detailed morphological examination during continuous operation of nanogap resistive switches. By developing a finite element model of nanogaps, we reveal the mechanisms behind the formation of electrode surface hillocks and filaments during continuous switching. Our findings suggest that “set” operations include processes such as field evaporation, electric field-induced diffusion, and field-assisted migration within the gap. Conversely, “reset” operations, driven by Joule heating and electromigration, lead to filament breakage and the creation of a fine gap. This research elucidates device degradation issues, such as periodic fluctuations in set threshold voltage (Vset) and the presence of non-steep set curves, providing both theoretical and experimental insights to improve future device performance.

Observation of nanopipes in edge-defined film-fed grown β-Ga2O3 substrate and their effect on homoepitaxial surface hillocks

β-Ga2O3 substrates and homoepitaxial films were characterized using the multiphoton excitation photoluminescence (MPPL) method. MPPL emission peaks at 3.2 and 3.36 eV were obtained with broad shoulders on the low energy side. MPPL images showed the presence of nanopipes in the substrate with a unique contrast. Three-dimensional MPPL imaging revealed the distribution and spatial location of the nanopipes. All the nanopipes were elongated along the [010] direction with diameters of approximately 0.4–1.0 μm and lengths of 10–30 μm. The nanopipes were aligned in the [100] and [001] directions with sub-micron spacing in the (00)-oriented substrate. The nanopipes were located under the hillocks at the homoepitaxial surface. The nanopipes are suggested to trigger the hillock growth by transforming into threading dislocations in the homoepitaxial film.

Diamond-like carbon films prepared by a low temperature periodic process for application in ventricular assist devices.

Due to the poor tribological properties of titanium (Ti) and its alloy Ti6Al4V (commonly used for ventricular assist devices manufacturing), diamond-like carbon (DLC) films with excellent anti-wear properties are pursued to improve the wear resistance of Ti and its alloys. Considering the effect of temperature on magnets inside pump impellers and workpiece deformation, DLC films are preferred to be prepared under low temperature. In this study, DLC films were prepared on Ti6Al4V alloys by periodic and continuous processes, and the corresponding maximum deposition temperature was 85 and 154°C, respectively. The periodic DLC films exhibited the feature of columnar structure, and the surface hillocks were less uniform than that of continuous DLC films. The periodic DLC films possessed more sp3 -bonded structures, and the accessorial sp3 -bonding mainly existed in the form of CH. Compared to continuous DLC films, the periodic DLC films had lower residual stress and better adhesion with Ti6Al4V substrates. Both DLC films could effectively reduce the friction coefficient and wear rate of Ti6Al4V alloys both in air and fetal bovine serum (FBS), and the periodic DLC films exhibited superior anti-wear properties to that of continuous DLC films in FBS. Haemocompatibility evaluation revealed that both DLC films presented similar levels of more human platelet adhesion and activation as compared with that of bare Ti6Al4V. However, both DLC films significantly prolonged plasma clotting time in comparison to bare Ti6Al4V. This study demonstrates the potential of low-temperature DLC films as wear-resistant surface modification for VADs.

N-polar GaN evolution on nominally on-axis c-plane sapphire by MOCVD part-I: Growth optimization

The present work is part-I of a study that demonstrates the influence of metalorganic chemical vapor deposition process parameters on the evolution of gallium nitride (GaN) deposited in a two-step growth process on c-plane sapphire substrates with a particular emphasis on nitrogen-polar GaN (N-polar GaN). First, the temperature domains of sapphire nitridation that result in Ga-polar and N-polar GaN epilayers were identified. Then, the structural and morphological evolution of low-temperature GaN nucleation layers were examined at the observed temperature domains of nitridation. Subsequently, a series of experiments were performed to study the influence of Ga and N precursor flow rates and epilayer growth temperature on the surface evolution of N-polar GaN. The observed results were analyzed in terms of thermodynamic and kinetic parameters of GaN growth. This work reports high-surface quality N-polar GaN epilayers without surface hillocks, exhibiting surface roughness about 1.5 nm over 2 × 2 μm2 area and with good crystalline quality on nominally on-axis c-plane sapphire substrates at low epilayer growth temperatures.

Depth-resolved thermal conductivity and damage in swift heavy ion irradiated metal oxides

We investigated thermal transport in swift heavy ion (SHI) irradiated insulating single crystalline oxide materials: yttrium aluminum garnet- Y3Al5O12 (YAG), sapphire (Al2O3), zinc oxide (ZnO) and magnesium oxide (MgO) irradiated by 167 MeV Xe ions at 1012 – 1014 ions/cm2 fluences. Depth profiling of the thermal transport on nano- and micro- meter scales was assessed by time-domain thermoreflectance (TDTR) and modulated thermoreflectance (MTR) methods, respectively. This combination allowed us to isolate the conductivities of different sub-surface damage-regions characterized by their distinct microstructure evolution regimes. Thermal conductivity degradation in SHI irradiated YAG and Al2O3 is attributed to formation of ion tracks and subsequent amorphization, while in ZnO and MgO it is mostly due to point defects. Additionally, notably lower conductivity when probed by very low penetrating thermal waves is consistent with surface hillock formation. An analytical model based on Klemens-Callaway method for thermal conductivity coupled with a simplified microstructure evolution capturing saturation in defect concentration was used to obtain depth dependent damage across the ion impacted region. The studies showed that YAG has the highest damage profile resulting in the less dependence of thermal conductivity with the depth, while MgO on the contrary has the strongest dependence. The presented work sheds new light on how SHI induced defects affect thermal transport degradation and recovery of oxide ceramics as promising candidates for next generation nuclear reactor applications.

High yield uniformity in pseudo-vertical diamond Schottky barrier diodes fabricated on half-inch single-crystal wafers

We fabricated diamond pseudo-vertical Schottky barrier diodes using a half-inch semi-insulative diamond (100) wafer. Most diodes exhibited a large rectifying ratio (>1010) with undetectable leakage current at a reverse bias of 5 V (0.6 MV cm−1), with only 2% of diodes exhibiting an Ohmic-like leakage current. Surface defects were observed under the Schottky barrier diode, and their impacts on electrical properties were analyzed using a Murphy model and correlation factor analysis. We found that most crystalline defects (surface hillocks) were electrically non-active and that non-epitaxial crystallites and process-related field-plate cracks were the main defects that induced a large leakage current. Schottky barrier diodes without such killer defects showed a high electric field strength of ∼5 MV cm−1.

Influence of Ag doping on the microstructure, mechanical properties, and adhesion stability of diamond-like carbon films

Silver (Ag)-doped diamond-like carbon (Ag-DLC) films were deposited on Si wafer and Co-Cr-Mo alloy substrates using a hybrid deposition technique that combined high-power pulsed magnetron sputtering (HPPMS) and high-power pulsed plasma-enhanced chemical vapor deposition (HPP-PECVD). The Ag concentration (0.0–10.0 at.%) in Ag-DLC films was controlled by adjusting the number of Ag rods in the mosaic silver-graphite target. The effects of Ag doping on the microstructure, chemical bonding, mechanical properties, and adhesion stability of DLC films were systematically investigated. The results demonstrated that Ag doping could refine the columnar structure in DLC films and change the shape and size of DLC surface hillocks. The residual stress in the DLC films decreased as the Ag concentration increased, which effectively improved the adhesion between the films and substrates. The fraction of sp3 bonds in the carbon structure decreased with increasing Ag concentration, which resulted in a reduction in the film hardness when the Ag concentration was higher than 3.2 at.%. Ag doping could improve the wear performance of DLC films, and the Ag-DLC film with 3.2 at.% Ag had excellent wear resistance. Compared with pure DLC films, the Ag-DLC films had better adhesion stability in physiological solutions, which is beneficial for the long-term service of DLC films in vivo applications.

Hillock formation in co-deposited thin films of immiscible metal alloy systems

Hillocks are protruding sections of a surface that can influence the electronic and mechanical properties of a thin film. In monolithic films, these hillocks are formed due to thermally induced stress gradients during deposition. In this study, the surface morphology of co-sputtered immiscible Cu-X (X is a body centered cubic (BCC) group V or VI metal) thin films is characterized to elucidate the conditions that lead to hillock formation. Cu-Ta and Cu-Mo-Ag films were co-deposited with physical vapor deposition (PVD) magnetron sputtering at 25, 400, 600, and 800 °C. A significant number of homogeneously distributed surface hillocks were observed only in the 600 and 800 °C films. High-angle annular dark field (HAADF) cross-sectional imaging revealed significant Cu agglomerations underneath the protruding features. For the Cu-Ta films, the Cu was enveloped in a Cu-Ta nanocrystalline matrix. For Cu-Mo-Ag, the Cu was surrounded by Mo-Ag concentration modulations. While thermal stress gradients arise during deposition of immiscible metal films, biaxial stress calculations and literature cases reveal that they are not solely responsible for hillock formation. The observed morphologies align with a surface diffusion kinetic model that evaluates diffusion length of adatoms during deposition as a function of deposition temperature. This indicates a phase separation driving force paired with the constituent elements’ dissimilar mobilities at elevated deposition temperatures contribute to the presence of hillocks.

Influences of screw dislocations on electroluminescence of AlGaN/AlN-based UVC LEDs

We investigated two types of threading dislocations in high Al-composition Al0.55Ga0.45N/AlN multiple quantum well (MQW) structures grown on AlN substrate for electrically injected deep ultraviolet light-emitting diodes (LEDs). The surface morphology and defects electrical characteristics of the MQW LED structures were examined via conductive atomic force microscopy (CAFM). We found that the disparity between photoluminescence (PL) and electroluminescence (EL) spectra in terms of light emission output and wavelength shift are attributed to the existence of the surface hillocks, especially to the ones that have open-core dislocations. The open-core dislocations form current leakage paths through their defect states and the composition inhomogeneity (i.e., Ga rich) at the dislocation sites are responsible for the light emission at longer wavelengths.

Temperature dependence of swift heavy ion irradiation induced hillocks in TiO2

Irradiation temperature dependant morphology of near surface latent tracks and surface hillocks in TiO2 was investigated. Irradiation was performed on single crystal [110] oriented rutile using 220 MeV Xe ions to a fluence of 5 × 1010 ions cm−2. Irradiations were performed at 80 K, 300 K, 600 K, 800 K and 1000 K. It was found that average hillock height increased with irradiation temperature although large specimen-to-specimen and hillock-to-hillock size differences were also recorded. Similarly the low density conical zone in the near-surface region of the ion track increased in both length and continuity with increasing temperature. At lower temperatures this zone was found to consist of closely spaced low density pockets that become more densely arranged and almost continuous at 1000 K. Evidence supporting the idea that surface hillocks are due to expelled matter from the track core was found in that larger hillocks are subtended by larger conical zones. These experimental observations were discussed in the framework of a simple model based on the inelastic thermal spike (i-TS) model as well as Bernoulli’s principle which could satisfactorily recreate the observed trends in hillock height and further supports the idea of expelled matter forming hillocks. Strain contrast around latent tracks is mostly absent around the conical zones suggesting some relaxation due to matter expulsion. All hillocks were found to be crystalline and epitaxial with the original crystal surface.

Formation of basal plane stacking faults on the ([formula omitted]) facet of heavily nitrogen-doped 4H-SiC single crystals during physical vapor transport growth

The formation of stacking faults in heavily nitrogen-doped (mid-1019cm−3) 4H-SiC boules grown by the physical vapor transport (PVT) growth method was investigated by studying surface morphologies on the (0001¯) facet of the boules. Low-voltage scanning electron microscopy (LVSEM) observations detected stacking faults on the (0001¯) facet of heavily nitrogen-doped 4H-SiC crystals. LVSEM and atomic force microscopy (AFM) studies revealed that the stacking faults showed characteristic morphologies, which stemmed from the interaction between stacking faults and surface steps. These observations also revealed that heavy nitrogen doping resulted in the nucleation of a number of surface hillocks on the (0001¯) facet; the hillocks were never observed on the facet of conventionally doped (nitrogen concentration: mid-1018cm−3) 4H-SiC boules. Furthermore, the hillocks were nucleated only on the facet and never observed on the outer regions of the facet. Based on these results, the stacking fault formation mechanism in heavily nitrogen-doped 4H-SiC crystals is discussed.

Reprint of ‘‘Tribological behavior of monocrystalline silicon from single- to multiple-asperity scratch’’

During producing silicon surface and fabricating silicon devices, the machining, cutting and milling from nanoscale to macroscale are accomplished with friction and wear under single- and multiple-asperity contact. In the present study, the scratch tests on silicon surface under single- and multiple-asperity contact were contrastively investigated, and the transition and correlation between different contact modes were addressed. When surface wear (formation of groove or protrusive hillock) appears under single-asperity sliding on silicon, the friction force became load-controlled and increased linearly with the normal load. The transition of single-asperity to multiple-asperity scratch was observed with the increase in the applied normal force. Under the multiple-asperity condition, surface hillocks were created on the scratched area, which were detected only under single-asperity test before. This study will shed new light on the understanding of multi-scale processing of silicon surface, and provide new insight for enriching tribology theory.

Tribological behavior of monocrystalline silicon from single- to multiple-asperity scratch

During producing silicon surface and fabricating silicon devices, the machining, cutting and milling from nanoscale to macroscale are accomplished with friction and wear under single- and multiple-asperity contact. In the present study, the scratch tests on silicon surface under single- and multiple-asperity contact were contrastively investigated, and the transition and correlation between different contact modes were addressed. When surface wear (formation of groove or protrusive hillock) appears under single-asperity sliding on silicon, the friction force became load-controlled and increased linearly with the normal load. The transition of single-asperity to multiple-asperity scratch was observed with the increase in the applied normal force. Under the multiple-asperity condition, surface hillocks were created on the scratched area, which were detected only under single-asperity test before. This study will shed new light on the understanding of multi-scale processing of silicon surface, and provide new insight for enriching tribology theory.

Direct surface relief formation by e-beam in amorphous chalcogenide layers

Patterning processes in amorphous Se and $$\hbox {As}_{20}\hbox {Se}_{80}$$ films at short electron beam pulses (from 200 ns to 100 ms) were studied for the first time. The surface reliefs occurring as after-pulses effects were recorded and analysed. Giant hillock formation was detected at about $$200\,\upmu \hbox {s}$$ pulses while very small changes in surface morphology were observed at other pulse durations. The obtained data indicate that the strong increase in e-beam sensitivity of mechanical response (giant surface hillock formation) at about $$200\,\upmu \hbox {s}$$ is due to some resonance effect. A qualitative description is given, relating these times to the characteristic generation and relaxation time of the defects in these materials, which illuminates the process of e-beam induced structural rearrangement. The measurement has been performed at room temperature and at $$-120\,^{\circ }\hbox {C}$$ and only a 20% change in the maximal pattern height has been detected.

MOCVD growth of N-polar GaN on on-axis sapphire substrate: Impact of AlN nucleation layer on GaN surface hillock density

We report on the impact of growth conditions on surface hillock density of N-polar GaN grown on nominally on-axis (0001) sapphire substrate by metal organic chemical vapor deposition (MOCVD). Large reduction in hillock density was achieved by implementation of an optimized high temperature AlN nucleation layer and use of indium surfactant in GaN overgrowth. A reduction by more than a factor of five in hillock density from 1000 to 170 hillocks/cm−2 was achieved as a result. Crystal quality and surface morphology of the resultant GaN films were characterized by high resolution x-ray diffraction and atomic force microscopy and found to be relatively unaffected by the buffer conditions. It is also shown that the density of smaller surface features is unaffected by AlN buffer conditions.

Origins of hillock defects on GaN templates grown on Si(111)

The origin of surface hillocks (also known as pancake defects) on GaN-on-Si wafers grown by MOVPE has been investigated. FIB/TEM observations confirmed that the appearance of the hillocks is due to the formation of Ga-rich precipitates within the AlGaN buffer layer. XRD (002) FWHM measurements also show that the surface hillocks are associated with a high degree of crystal tilt in the AlN nucleation layer. Two factors are considered to be the cause of such a phase separation: (1) a high density of surface steps associated with the regions of large crystal tilt which act as nucleation centers and (2) a lower mobility of Al adatoms at the growth surface compared with Ga, leading to a preferential incorporation of Ga in the precipitates. The impact of these precipitates on the wafer bow of the structures is considered.

Origin of faceted surface hillocks on semi-polar [formula omitted] GaN templates grown on pre-structured sapphire

The microstructure of semi-polar (112¯2) GaN templates grown on pre-structured r-plane sapphire by metal–organic vapor phase epitaxy (MOVPE) followed by hydride vapor phase epitaxy (HVPE) has been characterised by transmission electron microscopy (TEM). It is found that dislocations originating from the inclined c-plane-like GaN/sapphire interface bend and then terminate either at the coalescence regions of the adjacent GaN stripes or at the SiO2 mask. However, the regions associated with the coalescence event during the MOVPE growth act as a source of dislocations and stacking faults in the subsequent growth process. More importantly, a direct link between the formation of a surface hillock, the presence of an inversion domain, and the preferential nucleation of randomly oriented GaN particles at a region containing a dislocation bundle originating from coalescence has been established. It is suggested that controlling the surface conditions of the MOVPE GaN layer before HVPE and optimising the HVPE nucleation process are important to avoid the surface hillocks.

Relief evolution of HOPG under high-fluence 30 keV argon ion irradiation

The results of the experimental study of sputtering and erosion of the basal plane of HOPG under irradiation with 30-keV Ar+ in the range from RT to 400°C are presented. It has been found that developed at elevated (⩾250°C) temperatures needle-like microscopic relief results in twofold sputtering yield increase (Y≈2) in comparison with sputtering of a surface with an etch pits microscopic relief at the temperatures less than the ion-induced texture transition temperature Tt≈150°C. The effects of ion-induced graphite relief on high-dose sputtering have been studied using binary-collision computer simulation. The relief was modeled as a sine function surface along two mutually perpendicular surface axes. The simulation has shown that at some parameters of the relief the essential part of the bombarding ions undergoes inclined incidence on the walls of surface hillocks, which increases the density of ion-atom collisions near the surface and, correspondingly, the ejection of atoms. This effect leads to non-monotonic behavior of the sputtering yield on the relief aspect ratio (amplitude/period). The sputtering yield decreases upon reaching the maximum at aspect ratio of 4, and becomes lower than that for a flat surface. The simulation permits to estimate the relation of amplitude to period of relief at T<Tt.

Design and characterization of thick InxGa1-xAs metamorphic buffer layers grown by hydride vapor phase epitaxy

Thick InxGa1-xAs metamorphic buffer layers (MBLs) grown by hydride vapor phase epitaxy (HVPE) were studied. Relationships between MBL properties and growth parameters such as grading rate, cap layer thickness, final xInAs, and deposition temperature (TD) were explored. The MBLs were characterized by measurement of in-plane residual strain (妦), surface etch pit density (EPD), and surface roughness. Capping layer thickness had a strong effect on strain relaxation, with thickly capped samples exhibiting the lowest 妦. EPD was higher in samples with thicker caps, reflecting their increased relaxation through dislocation generation. 妦 and EPD were weakly affected by the grading rate, making capping layer thickness the primary structural parameter which controls these properties. MBLs graded in discrete steps had similar properties to MBLs with continuous grading. In samples with identical thickness and 10-step grading style, 妦 increased almost linearly with final xInAs, while total relaxation stayed relatively constant. Relaxation as a function of xInAs could be described by an equilibrium model in which dislocation nucleation is impeded by the energy of the existing dislocation array. EPD was constant from xInAs = 0 to 0.24 then increased exponentially, which is related to the increased dislocation interaction and blocking seen at higher dislocation densities. RMS roughness increased with xInAs above a certain strain rate (0.15%/µm); samples grown below this level possessed large surface hillocks and high roughness values. The elimination of hillocks at higher values of xInAs is attributed to increased density of surface steps and is related to the out-of-plane component of the burgers vector of the dominant type of 60° dislocation. TD did not affect 妦 for samples with a given xInAs. EPD tended to increase with TD, indicating dislocation glide likely is impeded at higher temperatures.

Inhomogeneous distribution of defect-related emission in Si-doped AlGaN epitaxial layers with different Al content and Si concentration

The spatial distribution of luminescence in Si-doped AlGaN epitaxial layers that differ in Al content and Si concentration has been studied by cathodoluminescence (CL) mapping in combination with scanning electron microscopy. The density of surface hillocks increased with decreasing Al content and with increasing Si concentration. The mechanisms giving rise to those hillocks are likely different. The hillocks induced surface roughening, and the compositional fluctuation and local donor-acceptor-pair (DAP) emission at hillock edges in AlGaN epitaxial layers were enhanced irrespective of the origin of the hillocks. The intensity of local DAP emission was related to Si concentration, as well as to hillock density. CL observation revealed that DAP emission areas were present inside the samples and were likely related to dislocations concentrated at hillock edges. Possible candidates for acceptors in the observed DAP emission that are closely related in terms of both Si concentration and hillock edges with large deformations are a VIII-SiIII complex and SiN, which are unfavorable in ordinary III-nitrides.