Thin films of Pt have been grown as gate metals on the oxide surface of gas sensitive field-effect devices. Both electron beam evaporation and dc magnetron sputtering has been used. The energy of the impinging Pt atoms, the substrate temperature and the thickness of the Pt film were used as parameters in this study. The influence of the growth parameters on the gas response has been investigated and compared with the properties of the films, studied by transmission electron microscopy, Auger electron spectroscopy, X-ray photoelectron spectroscopy and X-ray diffraction. The conditions during growth of the Pt film are found to have a large impact on the properties of the device. As expected, crystallinity, morphology and the metal/substrate interfacial structure are also affected by processing parameters. Three different growth processes stand out as the most promising from gas sensor considerations, namely room temperature evaporation, sputtering at high pressures and sputtering at high temperatures. The correlation between gas responses and properties of the gas sensitive layer is discussed. © 2002 Elsevier Science B.V. All rights reserved.

Periodic precipitation patterns in C:Ni nanocomposites grown by energetic ion codeposition are investigated. Films were grown at room temperature by ionized physical vapor deposition using a pulsed filtered cathodic vacuum arc. We reveal the role of the film composition, ion energy and incidence angle on the film morphology using transmission electron microscopy and grazing incidence small angle x-ray scattering. Under these growth conditions, phase separation occurs in a thin surface layer which has a high atomic mobility due to energetic ion impacts. This layer is an advancing reaction front, which switches to an oscillatory mode, producing periodic precipitation patterns. Our results show that the ion induced atomic mobility is not random, as it would be in the case of thermal diffusion but conserves to a large extent the initial direction of the incoming ions. This results in a tilted pattern under oblique ion incidence. A dependence of the nanopattern periodicity and tilt on the growth parameters is established and pattern morphology control via ion velocity is demonstrated.

Ta thin films were grown on Si substrates at different inclination angles with respect to the sputter source using high power impulse magnetron sputtering (HIPIMS), an ionized physical vapor deposition technique. The ionization allowed for better control of the energy and directionality of the sputtered species, and consequently for improved properties of the deposited films. Depositions were made on Si substrates with the native oxide intact. The structure of the as deposited films was investigated using X-ray diffraction, while a four-point probe setup was used to measure the resistivity. A substrate bias process-window for growth of bcc-Ta was observed. However, the process-window position changed with changing inclination angles of the substrate. The formation of this low-resistivity bcc-phase could be understood in light of the high ion flux from the HIPIMS discharge.

We have synthesized Ta thin films on Si substrates placed along a wall of a 2-cm-deep and 1-cm-wide trench, using both a mostly neutral Ta flux by conventional dc magnetron sputtering (dcMS) and a mostly ionized Ta flux by high-power pulsed magnetron sputtering (HPPMS). Structure of the grown films was evaluated by scanning electron microscopy, transmission electron microscopy, and atomic force microscopy. The Ta thin film grown by HPPMS has a smooth surface and a dense crystalline structure with grains oriented perpendicular to the substrate surface, whereas the film grown by dcMS exhibits a rough surface, pores between the grains, and an inclined columnar structure. The improved homogeneity achieved by HPPMS is a direct consequence of the high ion fraction of sputtered species.

Indium segregation in a narrow InGaN single quantum well creates quantum dot (QD) like exciton localization centers. Cross section transmission electron microscopy reveals varying shapes and lateral sizes in the range ~1-5 nm of the QD-like features, while scanning near field optical microscopy demonstrates a highly inhomogeneous spatial distribution of optically active individual localization centers. Microphotoluminescence spectroscopy confirms the spectrally inhomogeneous distribution of localization centers, in which the exciton and the biexciton related emissions from single centers of varying geometry could be identified by means of excitation power dependencies. Interestingly, the biexciton binding energy (E^b_xx) was found to vary from center to center, between 3 to -22 meV, in correlation with the exciton emission energy. Negative binding energies justify the three-dimensional quantum confinement, which confirms QD-like properties of the localization centers.! The observed energy correlation is proposed to be understood as variations of the lateral extension of the confinement potential, which would yield smaller values of E^b_xx for reduced lateral extension and higher exciton emission energy. The proposed relation between lateral extension and E^b_xx is further supported by the exciton and the biexciton recombination lifetimes of a single QD, which suggest a lateral extension of merely ~3 nm for a QD with strongly negative E^b_xx = -15.5 meV.

Indium segregation in a narrow InGaN single quantum well creates quantum dot (QD) like exciton localization centers. Cross-section transmission electron microscopy reveals varying shapes and lateral sizes in the range ∼1–5 nm of the QD-like features, while scanning near field optical microscopy demonstrates a highly inhomogeneous spatial distribution of optically active individual localization centers. Microphotoluminescence spectroscopy confirms the spectrally inhomogeneous distribution of localization centers, in which the exciton and the biexciton related emissions from single centers of varying geometry could be identified by means of excitation power dependencies. Interestingly, the biexciton binding energy (Ebxx) was found to vary from center to center, between 3 to −22 meV, in correlation with the exciton emission energy. Negative binding energies are only justified by a three-dimensional quantum confinement, which confirms QD-like properties of the localization centers. The observed energy correlation is proposed to be understood as variations of the lateral extension of the confinement potential, which would yield smaller values of Ebxx for reduced lateral extension and higher exciton emission energy. The proposed relation between lateral extension and Ebxx is further supported by the exciton and the biexciton recombination lifetimes of a single QD, which suggest a lateral extension of merely ∼3 nm for a QD with strongly negative Ebxx = −15.5 meV. 

We recently showed that Zr1−xTaxBy thin films have columnar nanostructure in which column boundaries are B-rich for x < 0.2, while Ta-rich for x ≥ 0.2. Layers with x ≥ 0.2 exhibit higher hardness and, simultaneously, enhanced toughness. Here, we determine the atomic-scale nanostructure of sputter-deposited columnar Zr0.7Ta0.3B1.5 thin films. The columns, 95 ± 17 Å, are core/shell nanostructures in which 80 ± 15-Å cores are crystalline hexagonal-AlB2-structure Zr-rich stoichiometric Zr1−xTaxB2. The shell structure is a narrow dense, disordered region that is Ta-rich and highly B-deficient. The cores are formed under intense ion mixing via preferential Ta segregation, due to the lower formation enthalpy of TaB2 than ZrB2, in response to the chemical driving force to form a stoichiometric compound. The films with unique combination of nanosized crystalline cores and dense metallic-glass-like shells provide excellent mechanical properties.

We recently showed that sputter-deposited Zr_1-xTa_xB_y thin films have hexagonal AlB₂-type columnar nanostructure in which column boundaries are B-rich for x < 0.2, while Ta-rich for x ≥ 0.2. As-deposited layers with x ≥ 0.2 exhibit higher hardness and, simultaneously, enhanced toughness. Here, we study the mechanical properties of ZrB_2.4, Zr_0.8Ta_0.2B_1.8, and Zr_0.7Ta_0.3B_1.5 films annealed in Ar atmosphere as a function of annealing temperature T_a up to 1200 °C. In-situ and ex-situ nanoindentation analyses reveal that all films undergo age hardening up to T_a = 800 °C, with the highest hardness achieved for Zr_0.8Ta_0.2B_1.8 (45.5±1.0 GPa). The age hardening, which occurs without any phase separation or decomposition, can be explained by point-defect recovery that enhances chemical bond density. Although hardness decreases at T_a > 800 °C due mainly to recrystallization, column coarsening, and planar defect annihilation, all layers show hardness values above 34 GPa over the entire T_a range.

Ternary Ti-Al-N films were deposited onto Al₂O₃ (0001) substrates by reactive co‑sputtering from elemental Ti and Al targets and analyzed by in situ and ex situ x-ray scattering, Rutherford backscattering spectroscopy, transmission electron microscopy and x-ray photoemission spectroscopy. The deposition parameters were set to values that yield Ti:Al:N ratios of 2:1:1 and 4:1:3 at room temperature. 2TiAlN depositions at 675 °C result in epitaxial Ti₂AlN growth with basal planes parallel to the substrate surface. Nominal 4TiAl3N depositions at 675 °C and above, however, yield TiN and Ti₂AlN domains due to Al loss to the vacuum. Depositions at a lower temperature of 600 °C yield films with correct 4:1:3 stoichiometry, but Ti₄AlN₃ formation is supposedly prevented by insufficient adatom mobility. Instead, an incoherent Ti_n+1AlN_n structure with random twinned stacking sequences n is obtained, that exhibits both basal plane orientations parallel as well as nearly perpendicular to the substrate interface. X‑ray photoemission spectroscopy shows that in contrast to stoichiometric nitrides the Al is metallically bonded and hence acts as twinning plane within the Ti_n+1AlN_n stackings. Domains with perpendicular basal plane orientation overgrowth those with parallel ones in a competitive growth mode. The resulting morphology is a combination of smooth‑surfaced parallel basal plane orientation domains interrupted by repeated facetted hillock-like features with perpendicular basal plane orientation.

Understanding and controlling growth of graphene on the carbon face (C-face) of SiC presents a significant challenge. In this work, we study the structural, vibrational, and dielectric function properties of graphene grown on the C-face of 4H-SiC by high-temperature sublimation in an argon atmosphere. The effect of growth temperature on the graphene number of layers and crystallite size is investigated and discussed in relation to graphene coverage and thickness homogeneity. An amorphous carbon layer at the interface between SiC and the graphene is identified, and its evolution with growth temperature is established. Atomic force microscopy, micro-Raman scattering spectroscopy, spectroscopic ellipsometry, and high-resolution cross-sectional transmission electron microscopy are combined to determine and correlate thickness, stacking order, dielectric function, and interface properties of graphene. The role of surface defects and growth temperature on the graphene growth mechanism and stacking is discussed, and a conclusion about the critical factors to achieve decoupled graphene layers is drawn. (C) 2015 AIP Publishing LLC.

Gallium nitride (GaN) epitaxial films on sapphire (Al2O3) substrates have been grown using reactive magnetron sputter epitaxy with a liquid Ga target. Threading dislocations density (TDD) of sputtered GaN films was reduced by using an inserted high-quality aluminum nitride (AlN) buffer layer grown by reactive high power impulse magnetron sputtering (R-HiPIMS) in a gas mixture of Ar and N2. After optimizing the Ar/N2 pressure ratio and deposition power, a high-quality AlN film exhibiting a narrow full-width at half-maximum (FWHM) value of the double-crystal x-ray rocking curve (DCXRC) of the AlN(0002) peak of 0.086° was obtained by R-HiPIMS. The mechanism giving rise the observed quality improvement is attributed to the enhancement of kinetic energy of the adatoms in the deposition process when operated in a transition mode. With the inserted HiPIMS-AlN as a buffer layer for direct current magnetron sputtering (DCMS) GaN growth, the FWHM values of GaN(0002) and (10 1‾ 1) XRC decrease from 0.321° to 0.087° and from 0.596° to 0.562°, compared to the direct growth of GaN on sapphire, respectively. An order of magnitude reduction from 2.7 × 109 cm−2 to 2.0 × 108 cm−2 of screw-type TDD calculated from the FWHM of the XRC data using the inserted HiPIMS-AlN buffer layer demonstrates the improvement of crystal quality of GaN. The result of TDD reduction using the HiPIMS-AlN buffer was also verified by weak beam dark-field (WBDF) cross-sectional transmission electron microscopy (TEM).

The structure of high electron mobility transistors (HEMTs) based on group-III nitride materials generally consists of three important blocks; a nucleation layer, a semi-insulating (SI) GaN buffer layer, and active layers. In this work, we present an overall growth optimization, which leads to superior crystalline quality and ultra-low thermal boundary resistance (TBR) of a 35-nm AlN nucleation layer, excellent crystalline quality of carbon-doped GaN buffer layer, and high mobility (> 2000 cm²/Vs) of two-dimensional gas (2DEG) in a simple AlGaN/GaN heterostructure grown on a SI SiC substrate.

A high mobility of 2250 cm²/V·s of a two-dimensional electron gas (2DEG) in a metalorganic chemical vapor deposition-grown AlGaN/GaN heterostructure was demonstrated. The mobility enhancement was a result of better electron confinement due to a sharp AlGaN/GaN interface, as confirmed by scanning transmission electron microscopy analysis, not owing to the formation of a traditional thin AlN exclusion layer. Moreover, we found that the electron mobility in the sharp-interface heterostructures can sustain above 2000 cm²/V·s for a wide range of 2DEG densities. Finally, it is promising that the sharp-interface AlGaN/GaN heterostructure would enable low contact resistance fabrication, less impurity-related scattering, and trapping than the AlGaN/AlN/GaN heterostructure, as the high-impurity-contained AlN is removed.

Nucleation mechanism of catalyst-free GaN nanorod grown on Si(111) is investigated by the fabrication of uniform and narrow (andlt; 35 nm) nanorods without a pre-defined mask by molecular beam epitaxy. Direct evidences show that the nucleation of GaN nanorods stems from the sidewall of the underlying islands down to the Si(111) substrate, different from commonly reported ones on top of the island directly. Accordingly, the growth and density control of the nanorods is exploited by a "narrow-pass" approach that only narrow nanorod can be grown. The optimal size of surrounding non-nucleation area around single nanorod is estimated as 88 nm.

Epitaxial growth of sp²-hybridized boron nitride (BN) using chemical vapour deposition, with ammonia and triethyl boron as precursors, is enabled on sapphire by introducing an aluminium nitride (AlN) buffer layer. This buffer layer is formed by initial nitridation of the substrate. Epitaxial growth is verified by X-ray diffraction measurements in Bragg–Brentano configuration, pole figure measurements and transmission electron microscopy. The in-plane stretching vibration of sp²-hybridized BN is observed at 1366 cm^–1 from Raman spectroscopy. Time-of-flight elastic recoil detection analysis confirms almost perfect stoichiometric BN with low concentration of carbon, oxygen and hydrogen contaminations.

We have used first-principles calculations and Heisenberg Monte Carlo simulations to search for the magnetic ground state of Mn₂GaC, a recently synthesized magnetic nanolaminate. We have, independent on method, identified a range of low energy collinear as well as non-collinear magnetic configurations, indicating a highly frustrated magnetic material with several nearly degenerate magnetic states. An experimentally obtained magnetization of only 0.29 per Mn atom in Mn₂GaC may be explained by canted spins in an antiferromagnetic configuration of ferromagnetically ordered sub-layers with alternating spin orientation, denoted AFM[0001]. Furthermore, low temperature X-ray diffraction show a new basal plane peak appearing upon a magnetic transition, which is consistent with the here predicted change in inter-layer spacing for the AFM[0001] configuration.

We present a study on the role of dislocations and impurities for the unintentional n-type conductivity in high-quality InN grown by molecular beam epitaxy. The dislocation densities and H profiles in films with free electron concentrations in the low 10(17) cm(-1) and mid 10(18) cm(-3) range are measured, and analyzed in a comparative manner. It is shown that dislocations alone could not account for the free electron behavior in the InN films. On the other hand, large concentrations of H sufficient to explain, but exceeding substantially, the observed free electron densities are found. Furthermore, enhanced concentrations of H are revealed at the film surfaces, resembling the free electron behavior with surface electron accumulation. The low-conductive film was found to contain C and it is suggested that C passivates the H donors or acts as an acceptor, producing compensated material in this case. Therefore, it is concluded that the unintentional impurities play an important role for the unintentional n-type conductivity in InN. We suggest a scenario of H incorporation in InN that may reconcile the previously reported observations for the different role of impurities and dislocations for the unintentional n-type conductivity in InN.

Precise measurement of the optical Hall effect in InN using magneto-optical generalized ellipsometry at IR and THz wavelengths, allows us to decouple the surface accumulation and bulk electron densities in InN films by non-contact optical means and further to precisely measure the effective mass and mobilities for polarizations parallel and perpendicular to the optical axis. Studies of InN films with different thicknesses, free electron densities and surface orientations enable an intricate picture of InN free electron properties to emerge. Striking findings on the scaling factors of the bulk electron densities with film thickness further supported by transmission electron microscopy point to an additional thickness dependent doping mechanism unrelated to dislocations. Surface electron accumulation is observed to occur not only at polar but also at non-polar and semi-polar wurtzite InN, and zinc blende InN surfaces. The persistent surface electron density shows a complex behavior with bulk density and surface orientation. This behavior might be exploited for tuning the surface charge in InN.

The free electron behavior in InN is studied on the basis of decoupled bulk and surface accumulation electron densities in InN films measured by contactless optical Hall effect. It is shown that the variation in the bulk electron density with film thickness does not follow the models of free electrons generated by dislocation-associated nitrogen vacancies. This finding, further supported by transmission electron microscopy results, indicates the existence of a different thickness-dependent doping mechanism. Furthermore, we observe a noticeable dependence of the surface electron density on the bulk density, which can be exploited for tuning the surface charge in future InN based devices.

New MAX phases Ti2(AlxCu1−x)N and Nb2CuC were synthesized by A-site replacement by reacting Ti2AlN and Nb2AlC, respectively, with CuCl2 or CuI molten salt. X-ray diffraction, scanning electron microscopy, and atomically resolved scanning transmission electron microscopy showed complete A-site replacement in Nb2AlC, which lead to the formation of Nb2CuC. However, the replacement of Al in Ti2AlN phase was only close to complete at Ti2(Al0.1Cu0.9)N. Density-functional theory calculations corroborated the structural stability of Nb2CuC and Ti2CuN phases. Moreover, the calculated cleavage energy in these Cu-containing MAX phases are weaker than in their Al-containing counterparts.

The preparation of MAX phases Nb2CuC and Ti2(Al0.1Cu0.9)N were realized by A-site replacement in Ti2AlN and Nb2AlN, respectively.

III-V semiconductor nanowires (NWs) have gained significant interest as building blocks in novel nanoscale devices. The one-dimensional (1D) nanostructure architecture allows one to extend band structure engineering beyond quantum confinement effects by utilizing formation of different crystal phases that are thermodynamically unfavorable in bulk materials. It is therefore of crucial importance to understand the influence of variations in the NWs crystal structure on their fundamental physical properties. In this work we investigate effects of structural polytypism on the optical properties of gallium phosphide and GaP/GaNP core/shell NW structures by a correlative investigation on the structural and optical properties of individual NWs. The former is monitored by transmission electron microscopy, whereas the latter is studied via cathodoluminescence (CL) mapping. It is found that structural defects, such as rotational twins in zinc blende (ZB) GaNP, have detrimental effects on light emission intensity at low temperatures by promoting nonradiative recombination processes. On the other hand, formation of the wurtzite (WZ) phase does not notably affect the CL intensity neither in GaP nor in the GaNP alloy. This suggests that zone folding in WZ GaP does not enhance its radiative efficiency, consistent with theoretical predictions. We also show that the change in the lattice structure have negligible effects on the bandgap energies of the GaNP alloys, at least within the range of the investigated nitrogen compositions of <2%. Both WZ and ZB GaNP are found to have a significantly higher efficiency of radiative recombination as compared with that in parental GaP, promising for potential applications of GaNP NWs as efficient nanoscale light emitters within the desirable amber-red spectral range.

Single-crystal CrB₂/TiB₂ diboride superlattices with well-defined layers are promising candidates for neutron optics. However, excess B in sputter-deposited TiB_y using a single TiB₂ target deteriorates the structural quality of CrB_x/TiB_y (0001) superlattices. We study the influence of co-sputtering of TiB₂ + Ti on the stoichiometry and crystalline quality of 300-nm-thick TiB_y single layers and CrB_x/TiB_y (0001) superlattices on Al₂O₃(0001) substrates grown by DC magnetron sputter epitaxy at growth-temperatures T_S ranging from 600 to 900 °C. By controlling the relative applied powers to the TiB₂ and Ti magnetrons, y could be reduced from 3.3 to 0.9. TiB_2.3 grown at 750 °C exhibited epitaxial domains about 10x larger than non-co-sputtered films. Close-to-stoichiometry CrB_1.7/TiB_2.3 superlattices with modulation periods Λ = 6 nm grown at 750 °C showed the highest single crystal quality and best layer definition. TiB_2.3 layers display rough top interfaces indicating kinetically limited growth while CrB_1.7 forms flat and abrupt top interfaces indicating epitaxial growth with high adatom mobility.

Er and O co-doped Si structures have been prepared using molecular-beam epitaxy (MBE) with fluxes of Er and O obtained from Er and silicon monoxide (SiO) evaporation in high-temperature cells. The incorporation of Er and O has been studied for concentrations of up to 2×1020 and 1×1021 cm-3, respectively. Surface segregation of Er can take place, but with O co-doping the segregation is suppressed and Er-doped layers without any indication of surface segregation can be prepared. Si1-xGex and Si1-yCy layers doped with Er/O during growth at different substrate temperatures show more defects than corresponding Si layers. Strong emission at 1.54µm associated with the intra-4f transition of Er3+ ions is observed in electroluminescence (EL) at room temperature in reverse-biased p-i-n-junctions. To optimize the EL intensity we have varied the Er/O ratio and the temperature during growth of the Er/O-doped layer. Using an Er-concentration of around 1×1020 cm-3 we find that Er/O ratios of 1:2 or 1:4 give higher intensity than 1:1 while the stability with respect to breakdown is reduced for the highest used O concentrations. For increasing growth temperatures in the range 400-575 °C there is an increase in the EL intensity. A positive effect of post-annealing on the photoluminescence intensity has also been observed.

We have synthesized Ti–Si–C nanocomposite thin films by dc magnetron sputtering from a Ti₃SiC₂ compound target in an Ar discharge on Si(100), Al₂O₃(0001), and Al substrates at temperatures from room temperature to 300  °C. Electron microscopy, x-ray diffraction, and x-ray photoelectron spectroscopy showed that the films consisted of nanocrystalline (nc-) TiC and amorphous (a-) SiC, with the possible presence of a small amount of noncarbidic C. The growth mode was columnar, yielding a nodular film-surface morphology. Mechanically, the films exhibited a remarkable ductile behavior. Their nanoindentation hardness and E-modulus values were 20 and 290  GPa, respectively. The electrical resistivity was 330  µ  cm for optimal Ar pressure (4  mTorr) and substrate temperature (300  °C). The resulting nc-TiC/a-SiC films performed well as electrical contact material. These films' electrical-contact resistance against Ag was remarkably low, 6  µ at a contact force of 800  N compared to 3.2  µ for Ag against Ag. The chemical stability of the nc-TiC/a-SiC films was excellent, as shown by a Battelle flowing mixed corrosive-gas test, with no N, Cl, or S contaminants entering the bulk of the films.

CaMnO3 is a perovskite with attractive magnetic and thermoelectric properties. CaMnO3 films are usually grown by pulsed laser deposition or radio frequency magnetron sputtering from ceramic targets. Herein, epitaxial growth of CaMnO3-y (002) films on a (112 over bar 0)-oriented LaAlO3 substrate using pulsed direct current reactive magnetron sputtering is demonstrated, which is more suitable for industrial scale depositions. The CaMnO3-y shows growth with a small in-plane tilt of &lt;approximate to 0.2 degrees toward the (200) plane of CaMnO3-y and the (1 over bar 104) with respect to the LaAlO3 (112 over bar 0) substrate. X-ray photoelectron spectroscopy of the electronic core levels shows an oxygen deficiency described by CaMnO2.58 that yields a lower Seebeck coefficient and a higher electrical resistivity when compared to stoichiometric CaMnO3. The LaAlO3 (112 over bar 0) substrate promotes tensile-strained growth of single crystals. Scanning transmission electron microscopy and electron energy loss spectroscopy reveal antiphase boundaries composed of Ca on Mn sites along and , forming stacking faults.

Epitaxial Ti₃SiC₂(0001) thin films have been deposited by dc magnetron sputtering from three elemental targets of Ti, C, and Si onto MgO(111) and Al₂O₃(0001) substrates at temperatures of 800–900 °C. This process allows composition control to synthesize M_n+1AX_n (MAX) phases (M: early transition metal; A: A-group element; X: C and∕or N; n=1–3) including Ti₄SiC₃. Depositions on MgO(100) substrates yielding the Ti–Si–C MAX phases with (105), as the preferred orientation. Samples grown at different substrate temperatures, studied by means of transmission electron microscopy and x-ray diffraction investigations, revealed the constraints of Ti₃SiC₂ nucleation due to kinetic limitations at substrate temperatures below 700 °C. Instead, there is a competitive TiC_x growth with Si segregation to form twin boundaries or Si substitutional incorporation in TiC_x. Physical properties of the as-deposited single-crystal Ti₃SiC₂ films were determined. A low resistivity of 25 μΩ cm was measured. The Young’s modulus, ascertained by nanoindentation, yielded a value of 343–370 GPa. For the mechanical deformation response of the material, probing with cube corner and Berkovich indenters showed an initial high hardness of almost 30 GPa. With increased maximum indentation loads, the hardness was observed to decrease toward bulk values as the characteristic kink formation sets in with dislocation ordering and delamination at basal planes.

ZrN/SiN^x nanoscale multilayers were deposited on ZrN seed layers grown on top of MgO(001) substrates by dc magnetron sputtering with a constant ZrN thickness of 40 Å and with an intended SiNx thickness of 2, 4, 6, 8, and 15 Å at a substrate temperature of 800 °C and 6 Å at 500 °C. The films were investigated by X-ray diffraction, high-resolution scanning transmission electron microscopy, and energy dispersive X-ray spectroscopy. The investigations show that the SiNx is amorphous and that the ZrN layers are crystalline. Growth of epitaxial cubic SiNx – known to take place on TiN(001) – on ZrN(001) is excluded to the monolayer resolution of this study. During the course of SiNx deposition, the material segregates to form surface precipitates in discontinuous layers for SiNx thicknesses ≤ 6 Å that coalesce into continuous layers for 8 and 15 Å thickness at 800 °C, and for 6 Å at 500 °C. The SiN_x precipitates are aligned vertically. The ZrN layers in turn grow by epitaxial lateral overgrowth on the discontinuous SiN_x in samples deposited at 800 °C with up to 6 Å thick SiN_x layers. Effectively a self-organized nanostructure can be grown consisting of strings of 1-3 nm large SiNx precipitates along apparent column boundaries in the epitaxial ZrN.

The crystal structure of epitaxially stabilized SiN_x layers on TiN(001) was investigated by analytical aberration corrected electron microscopy. Atomically resolved images of the structure, which were acquired by scanning transmission electron microscopy using high angle annular dark field and annular bright field detectors, are used to identify the B1-cubic structure of SiN_x. To corroborate the acquired images, image simulations were performed using candidate structures. Complementary to imaging, spatially resolved electron energy loss spectroscopy of the epitaxial SiN_x layers was performed to acquire the symmetry specific nitrogen near edge fine-structure. Finally, full potential calculations performed to determine the near edge structure from candidate crystal structures confirms the existence of B1-cubic SiN_x.

Recent developments in fabrication techniques and extensive investigations of the physical properties of III-V semiconductor nanowires (NWs), such as GaAs NWs, have demonstrated their potential for a multitude of advanced electronic and photonics applications. Alloying of GaAs with nitrogen can further enhance the performance and extend the device functionality via intentional defects and heterostructure engineering in GaNAs and GaAs/GaNAs coaxial NWs. In this work, it is shown that incorporation of nitrogen in GaAs NWs leads to formation of three-dimensional confining potentials caused by short-range fluctuations in the nitrogen composition, which are superimposed on long-range alloy disorder. The resulting localized states exhibit a quantum-dot like electronic structure, forming optically active states in the GaNAs shell. By directly correlating the structural and optical properties of individual NWs, it is also shown that formation of the localized states is efficient in pure zinc-blende wires and is further facilitated by structural polymorphism. The light emission from these localized states is found to be spectrally narrow (similar to 50-130 mu eV) and is highly polarized (up to 100%) with the preferable polarization direction orthogonal to the NW axis, suggesting a preferential orientation of the localization potential. These properties of self-assembled nano-emitters embedded in the GaNAs-based nanowire structures may be attractive for potential optoelectronic applications.

The III-V semiconductor nanowires (NWs) have a great potential for applications in a variety of future electronic and photonic devices with enhanced functionality. In this work, we employ polarization resolved micro-photoluminescence (µ-PL) spectroscopy to study polarization properties of light emissions from individual GaNP and GaP/GaNP core/shell nanowires (NWs) with average diameters ranging between 100 and 350 nm. We show that the near-band-edge emission, which originates from the GaNP regions of the NWs, is strongly polarized (up to 60 % at 150 K) in the direction perpendicular to the NW axis. The polarization anisotropy can be retained up to room temperature. This polarization behavior, which is unusual for zinc blende NWs, is attributed to local strain in the vicinity of the N-related centers participating in the radiative recombination and to preferential alignment of their principal axis along the growth direction. Our findings therefore show that defect engineering via alloying with nitrogen provides an additional degree of freedom to tailor the polarization anisotropy of III-V nanowires, advantageous for their applications as nanoscale emitters of polarized light.

A method based on focused ion beam milling and analytical electron microscopy to investigate the nature of the tool-chip interface is presented. It is employed to study tool-chip interfaces of the rake face of a (Ti0.83Si0.17)N coated PCBN insert after turning of case-hardened steel. Analytical electron microscopy shows the presence of a smeared adhered layer on the coating, which consists of steel elements from the work-piece, oxygen, and Si and N, most likely originating from the coating.

Cr–C/Ag thin films with 0–14 at.% Ag have been deposited by magnetron sputtering from elemental targets. The samples were analyzed by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) to study their structure and chemical bonding. A complex nanocomposite structure consisting of three phases; nanocrystalline Ag, amorphous CrCx and amorphous carbon is reported. The carbon content in the amorphous carbide phase was determined to be 32–33 at.% C, independent of Ag content. Furthermore, SEM and XPS results showed higher amounts of Ag on the surface compared to the bulk. The hardness and Young's modulus were reduced from 12 to 8 GPa and from 270 to 170 GPa, respectively, with increasing Ag content. The contact resistance was found to decrease with Ag addition, with the most Ag rich sample approaching the values of an Ag reference sample. Initial tribological tests gave friction coefficients in the range of 0.3 to 0.5, with no clear trends. Annealing tests show that the material is stable after annealing at 500 °C for 1 h, but not after annealing at 800 °C for 1 h. In combination, these results suggest that sputtered Cr–C/Ag films could be potentially applicable for electric contact applications.

Cr–C/Ag thin films with 0–14 at.% Ag have been deposited by magnetron sputtering from elemental targets. The samples were analyzed by X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) to study their structure and chemical bonding. A complex nanocomposite structure consisting of three phases; nanocrystalline Ag, amorphous CrC_x and amorphous carbon is reported. The carbon content in the amorphous carbide phase was determined to be 32–33 at.% C, independent of Ag content. Furthermore, SEM and XPS results showed higher amounts of Ag on the surface compared to the bulk. The hardness and Young's modulus were reduced from 12 to 8 GPa and from 270 to 170 GPa, respectively, with increasing Ag content. The contact resistance was found to decrease with Ag addition, with the most Ag rich sample approaching the values of an Ag reference sample. Initial tribological tests gave friction coefficients in the range of 0.3 to 0.5, with no clear trends. Annealing tests show that the material is stable after annealing at 500 °C for 1 h, but not after annealing at 800 °C for 1 h. In combination, these results suggest that sputtered Cr–C/Ag films could be potentially applicable for electric contact applications.

Lattice resolved and quantitative compositional characterizations of the microstructure in TiCrAlN wear resistant coatings emerging at elevated temperatures are performed to address the spinodal decomposition into nanometer-sized coherent cubic TiCr- and Al-rich domains. The domains coarsen during annealing and at 1100 ºC, the Al-rich domains include a metastable cubic Al(Cr)N phase containing 9 at.% Cr and a stable hexagonal AlN phase containing less than 1 at.% Cr. The cubic and the hexagonal phases form strained semi-coherent interfaces with each other.

Sputter deposition from a Ti2AlC target was found to yield Ti-Al-C films with a composition that deviates from the target composition of 2:1:1. For increasing substrate temperature from ambient to 1000 degrees C, the Al content decreased from 22 at.% to 5 at.%, due to re-evaporation. The C content in as-deposited films was equal to or higher than the Ti content. Mass spectrometry of the plasma revealed that the Ti and Al species were essentially thermalized, while a large fraction of C with energies andgt;4 eV was detected. Co-sputtering with Ti yielded a film stoichiometry of 2:0.8:0.9 for Ti:Al:C, which enabled growth of Ti2AlC. These results indicate that an additional Ti flux balances the excess C and therefore provides for more stoichiometric Ti2AlC synthesis conditions.

Nano-structural evolution of layer morphology and interfacial roughness in Cr/Sc metal multilayers grown with ion assistance during magnetron sputter deposition has been investigated by high resolution transmission electron microscopy and hard X-ray reflectivity. Calculations based on a binary collision model predict an ion-assisted growth window for optimized Cr/Sc multilayer interface sharpness, within the ion energy range of 21 eV to 37 eV and an ion flux of 10 ions per deposited atom. Multilayers with nominal modulation periods in the range of 1.6 nm to 10.2 nm, grown with these conditions, exhibit a well-defined layer structure with an improved flattening and abruptness of the interfaces. It is shown that multilayers with a modulation period smaller than 3.4 nm have clear benefit from the reduced intermixing obtained by utilizing a two-stage ion energy modulation for each individual layer. The amorphization of Sc and Cr layers, below certain thicknesses, is found to be independent of the low energy ion-assistance. It is also shown that the Cr/Sc multilayers, containing periods less than 2 nm are ‘self healing’ i.e. they re-gain abrupt interfaces and flat layers after morphological disturbances during ion assisted growth. In comparison, multilayers grown without ion-assistance exhibited severe roughness and layer distortions.

Cr-Ti multilayers with ultrashort periods of 1.39-2.04 nm have been grown for the first time as highly reflective, soft-x-ray multilayer, near-normal incidence mirrors for transition radiation and Cherenkov radiation x-ray sources based on the Ti-2p absorption edge at E = 452eV (lambda = 2.74 nm). Hard, as well as soft, x-ay reflectivity and transmission electron microscopy were used to characterize the nanostructure of the mirrors. To achieve minimal accumulated roughness, improved interface flatness, and to avoid intermixing at the interfaces, each individual layer was engineered by use of a two-stage ion assistance process during magnetron sputter deposition: The first 0.3 nm of each Ti and Cr layer was grown without ion assistance, and the remaining 0.39-0.72 nm of the layers were grown with high ion-neutral flux ratios Phi˙(Phi_Ti = 3.3, Phi_Cr = 2.2) and a low energy E_ion (E_Ti = 23.7 and E_Cr = 21.2), ion assistance. A maximum soft-x-ray reflectivity of R = 2.1% at near-normal incidence (~78.8°) was achieved for a multilayer mirror containing 100 bilayers with a modulation period of 1.379 nm and a layer thickness ratio of Gamma = 0.5. For a polarizing multilayer mirror with 150 bilayers designed for operation at the Brewster angle, 45°, an extinction ratio, R_s/R_p, of 266 was achieved with an absolute reflectivity of R = 4.3%.

Nanostructure formation via surface-diffusion-mediated segregation of ZrN and AIN in Zr1-xAlxN films during high mobility growth conditions is investigated for 0 amp;lt;= x amp;lt;= 1. The large immiscibility combined with interfacial surface and strain energy balance resulted in a hard nanolabyrinthine lamellar structure with well-defined (semi) coherent c-ZrN and w-AlN domains of sub-nm to similar to 4 nm in 0.2 amp;lt;= x amp;lt;= 0.4 films, as controlled by atom mobility. For high AlN contents (x amp;gt; 0.49) Al-rich ZrN domains attain wurtzite structure within fine equiaxed nanocomposite wurtzite lattice. Slow diffusion in wurtzite films points towards crystal structure dependent driving force for decomposition. The findings of unlikelihood of isostructural decomposition in c-Zr1-xAlxN, and stability of w-Zr1-xAlxN (in large x films) is complemented with first principles calculations.

The hot-wall metalorganic chemical vapor deposition (MOCVD) concept, previously shown to enable superior material quality and high performance devices based on wide bandgap semiconductors, such as Ga(Al)N and SiC, has been applied to the epitaxial growth of beta-Ga2O3. Epitaxial beta-Ga2O3 layers at high growth rates (above 1 mu m/h), at low reagent flows, and at reduced growth temperatures (740 degrees C) are demonstrated. A high crystalline quality epitaxial material on a c-plane sapphire substrate is attained as corroborated by a combination of x-ray diffraction, high-resolution scanning transmission electron microscopy, and spectroscopic ellipsometry measurements. The hot-wall MOCVD process is transferred to homoepitaxy, and single-crystalline homoepitaxial beta-Ga2O3 layers are demonstrated with a 201 rocking curve width of 118 arc sec, which is comparable to those of the edge-defined film-fed grown (201) beta-Ga2O3 substrates, indicative of similar dislocation densities for epilayers and substrates. Hence, hot-wall MOCVD is proposed as a prospective growth method to be further explored for the fabrication of beta-Ga2O3.

The influence of 25 kHz ultrasound and cathode rotation during electroplating of Ni films on Si wafers has been studied with respect to intrinsic stress formation. Current densities from 1.6 A dm^-2 up to 28.3 A dm^-2 were used in an additive-free Ni sulphamate electrolyte. In general more efficient agitation by either ultrasound or cathode rotation was found to reduce intrinsic stress towards compressive levels compared to conventional agitation with an electrolyte circulation pump. Further more, intrinsic stresses become less dependent on changes in current density. The latter effect is most pronounced for ultrasonic agitation. Structure analysis of samples deposited by ultrasonic agitation show dense deposits with initially smaller grains at high ultrasonic effect. Locally increased temperature at the substrates surface could be an important effect of ultrasound agitation.

Introducing point defects in two-dimensional (2D) materials can alter or enhance their properties. Here, we demonstrate how etching a laminated (Nb_2/3Sc_1/3)₂AlC MAX phase (solid solution) of both the Sc and Al atoms results in a 2D Nb_1.33C material (MXene) with a large number of vacancies and vacancy clusters. This method is applicable to any quaternary, or higher, MAX phase, wherein one of the transition metals is more reactive than the other and could be of vital importance in applications such as catalysis and energy storage. We also report, for the first time, on the existence of solid solution (Nb_2/3Sc_1/3)₃AlC₂ and (Nb_2/3Sc_1/3)₄AlC₃ phases.

Ion implantation is an important technique for a successful implementation of commercial SiC devices. Much effort has also been devoted to optimising implantation and annealing parameters to improve the electrical device characteristics. However, there is a severe lack of understanding of the fundamental implantation process and the generation and annealing kinetics of point defects and defect complexes. Only very few of the most elementary intrinsic point defects have been unambiguously identified so far. To reach a deeper understanding of the basic mechanisms SiC samples have been implanted with a broad range of ions, energies, doses, etc., and the resulting defects and damage produced in the lattice have been studied with a multitude of characterisation techniques. In this contribution we will review some of the results generated recently and also try to indicate where more research is needed. In particular, deep level transient spectroscopy (DLTS) has been used to investigate point defects at very low doses and transmission electron microscopy (TEM) and Rutherford backscattering spectrometry (RBS) are used for studying the damage build-up at high doses. © 2002 Elsevier Science B.V. All rights reserved.

The build-up of damage in 4H SiC epitaxial layers implanted with 100 or 180 keV Al ions in the dose range of 10(13) to 10(15) cm(-2) has been studied by transmission electron microscopy (TEM) and Rutherford backscattering spectroscopy in the channeling mode (c-RBS). Implantations have been done at temperatures between room temperature and 800 degreesC and the samples have been analysed after implantation and after post implant anneals. In as implanted samples channeling results show that a major part of the damage can be avoided already at implantations at 200 degreesC, but complete removal of damage is not possible even at an implantation temperature of 800 degreesC. After post implant annealing at typically 1600 degreesC a distribution of planar faults are seen by TEM. The size is around 10 nm, but increases with increasing annealing temperature.

The influence of germanium and carbon on the phase formation, strain relaxation and the occurrence of agglomeration of the Si1-x-yGe xCy epitaxial layers in Ni/SiGe(C) system were investigated. The defects formed by the reaction of Ni on SiGe(C) layers were investigated using cross-sectional transmission electron microscopy (XTEM). It was observed that NisiGe layers were crystalline and with strong growth orientation in the direction, but the thermal stability was decreased with increasing Ge amount due to agglomeration. It was also observed that at the interface of NiSiGe/SiGeC carbon was accumulated at low-temperature annealing which retarded the phase transformation and agglomeration of Ni/SiGeC systems.

The epitaxial quality of non-selective and selective deposition of Si1-x-yGexCy (0 less than or equal to x less than or equal to 0.30, 0 less than or equal to y less than or equal to 0.02) layers has been optimized by using high-resolution reciprocal lattice mapping (HRRLM). The main goal was to incorporate a high amount of substitutional carbon atoms in Si or Si1-xGex matrix without creating defects. The carbon incorporation behavior was explained by chemical and kinetic effects of the reactant gases during epitaxial process. Although high quality epitaxial Si1-yCy layers can be deposited, lower electron mobility compared to Si layers was observed. (C) 2003 Elsevier B.V. All rights reserved.

AlxGa1-xN multiple quantum wells (MQW) were grown on AlN epilayer grown on 4H-SiC substrate. The growth was performed without interruption in a horizontal hot-wall MOCVD reactor using a mixture of hydrogen and nitrogen as carrier gases. The precursors were ammonia, trimethylaluminum and trimethylgallium. Results obtained from X-ray diffraction and infra-red reflectance were used to obtain the composition of the films when growing simple AlxGa1 xN layer. Visible reflectance was used to evaluate the thickness of the films. Finally the MQW parameters as thicknesses and composition variation were obtained by scanning transmission electron microscopy and demonstrated an agreement with the growth parameters used

Chirality, tailored by external morphology and internal composition, has been realized by controlled curved-lattice epitaxial growth (CLEG) of uniform coatings of single-crystalline In_xAl_1-xN nanospirals. The nanospirals are formed by sequentially stacking segments of curved nanorods on top of each other, where each segment is incrementally rotated around the spiral axis. By controlling the growth rate, segment length, rotation direction, and incremental rotation angle, spirals are tailored to predetermined handedness, pitch, and height.  The curved morphology of the segments is a result of a lateral compositional gradient across the segments while maintaining a preferred crystallographic growth direction, implying a lateral gradient in optical properties as well. Left- and right-handed nanospirals, tailored with 5 periods of 200 nm pitch, as confirmed by scanning electron microscopy, exhibit uniform spiral diameters of ~80 nm (local segment diameters of ~60 nm) with tapered hexagonal tips.  High resolution electron microscopy, in combination with nanoprobe energy dispersive X-ray spectroscopy and valence electron energy loss spectroscopy, show that individual nanospirals consist of an In-rich core with ~15 nm-diameter hexagonal cross-section, comprised of curved basal planes. The core is surrounded by an Al-rich shell with a thickness asymmetry spiraling along the core. The ensemble nanospirals, across the 1 cm² wafers, show high in-plane ordering with respect to shape, crystalline orientation, and direction of compositional gradient. Mueller matrix spectroscopic ellipsometry shows that the tailored chirality is manifested in the polarization state of light reflected off the CLEG nanospiral-coated wafers. In that, the polarization state is shown to be dependent on the handedness of the nanospirals and the wavelength of the incident light in the ultraviolet-visible region.

Despite of using chiral metamaterials to manipulate light polarization states has been demonstrated their great potential for applications such as invisible cloaks, broadband or wavelength-tunable circular polarizers, microreflectors, etc. in the past decade [1-6], operating wavelength in ultraviolet-visible range is still a challenge issue. Since these chiral structures often consist of metallic materials, their operation is designed for the infrared and microwave regions [2-4]. Here, we show how a controlled curved-lattice epitaxial growth (CLEG) of wide-bandgap AlInN semiconductor curved nanocrystals [7] can be exploited as a novel route for tailoring chiral nanostructures in the form of twisted nanorods (TNRs). The fabricated TNRs are shown to reflect light with a high degree of polarization as well as a high degree of circular polarization (that is, nearly circularly polarized light) in the ultravioletvisible region. The obtained polarization is shown to be dependent on the handedness of the TNRs.

Self-assembled ternary Al_1-xIn_xN nanorod arrays with variable In concentration, 0.10 ≤ x ≤ 0.32 have been realized onto c-plane sapphire substrates by ultra-high-vacuum magnetron sputter epitaxy with Ti_0.21Zr_0.79N or VN seed layers assistance. The formation of nanorods was very sensitive to the applied seed layer. Without proper seed layer assistance a continuous A_l1-xIn_xN film was grown. The nanorods exhibit hexagonal crosssections with preferential growth along the c axis. A coaxial rod structure with higher In concentration in the core was observed by (scanning) transmission electron microscopy in combination with low-loss electron energy loss spectroscopy and energy dispersive xray spectroscopy. 5 K cathodoluminescence spectroscopy of Al_0.86In_0.14N nanorods revealed band edge emission at ~5.46 eV, which was accompanied by a strong defectrelated emission at ~ 3.38 eV.