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Here we investigate the interface properties of gold (Au) decorated graphenized surfaces of 4H-SiC intended for electrochemical electrodes. These are fabricated using a two-step process: discontinuous Au layers with a nominal thickness of 2 nm are sputter-deposited onto 4H-SiC substrates with different graphenization extent-zero-layer graphene (ZLG) and monolayer epitaxial graphene) -followed by thermal annealing. By performing combined morphometric analysis, Raman mapping analysis, conductive atomic force microscopy, and electrochemical impedance spectroscopy measurements, we shed light on the relationship between physical processes (Au intercalation, particle re-shaping, and de-wetting) caused by thermal annealing and the intrinsic properties of graphenized SiC (vertical electron transport, charge-transfer properties, vibrational properties, and catalytic activity). We find that the impedance spectra of all considered structures exhibit two semicircles in the high and low frequency regions, which may be attributed to the graphene/ZLG/SiC (or Au/graphene/ZLG/SiC) and SiC/ZLG/graphene/electrolyte (or SiC/ZLG//Au/electrolyte) interfaces, respectively. An equivalent circuit model is proposed to estimate the interface carrier transfer parameters. This work provides an in-depth comprehension of the way by which the Au/2D carbon/SiC interaction strength influences the interface properties of heterostructures, which can be helpful for developing high performance catalytic and sensing devices., Funding Agencies|forsk foundation [22-150, 21-112]; Stiftelsen for Strategisk Forskning (SSF) [RMA 15-0024]; Vetenskapsrdet (VR) [2018-04962]; Shantou University [NTF20033]; Swedish Research Council [VR-2021-04113]; Knut and Alice Wallenberg Foundation [KAW 2018.0071]

In this study, epitaxial graphene (EG) was grown on a 6H-SiC (0001) substrate via the thermal decomposition of SiC. Undoped and Cl- or N-doped molybdenum disulfide (MoS2) and tungsten disulfide (WS2) ultrathin films were spin-coated on the graphene surface. The scanning electron microscopy (SEM) images and topological atomic force microscopy (AFM) analysis showed good distribution of thin MoS2 and WS2 flakes on the EG surface. The X-ray photoelectron spectroscopy (XPS) confirmed the presence of Mo-related peaks of 3d(5/2) and 3d(3/2) at similar to 232.2 eV and 235.1 eV, respectively. It also represented peaks of W 4f(7/2) and 5p(5/2) at around 36.1 eV and 37.9 eV, respectively. Moreover, XPS results showed peaks at around 167.4 eV and 168.4 eV corresponding to S 2p for MoS2 and WS2, respectively. The XPS results also confirmed the presence of dopant elements in MoS2 and WS2 flakes. We fabricated sensors using undoped and chlorine- or nitrogen-doped MoS2 and WS2 ultrathin films for gas-sensing applications. These sensors were surveyed for ammonia (NH3) and nitrogen dioxide (NO2) gas sensing. As in NO2, both undoped sensors react with a decrease in relative sensor responses to NH3, hence showing n-type behavior. Doping MoS2 and WS2 with chlorine led to a higher response vis-a-vis the nitrogendoped sensors. The absolute relative response of Cl-doped WS2 and MoS2 was about 3.5 and 1.8 times more than that of their undoped counterparts toward NH3. A change of direction with a slightly smaller response (approximately x 0.8), however, could also be observed in the doping of MoS2 and WS2 with nitrogen. When exposed to NO2, the Cl-doped WS2 sensor response was 1.2 more than the N-doped one, while for MoS2 these values changed in the range of 1.2 - 1.6 for different flows of gas., Funding Agencies|Swedish Research CouncilSwedish Research CouncilEuropean Commission [2016-06014]; Swedish Foundation for Strategic Research (SSF)Swedish Foundation for Strategic Research [GMT14-0077, RMA15-024]

Present study aimed to develop nanocoating of cucurbit[7]uril (CB[7]) on surfaces of silicon and epitaxial graphene using drop casting and spin coating techniques. Here, we report a systematic study for the influence of sonication, probe sonication, and centrifugation time on the dispersion of CB[7] in aqueous solutions for the preparation of high-quality CB[7] nanocoating. Spin speed, spin time, and spin acceleration have been optimised to attain uniform films with minimum rms. Atomic force microscopy is used to study morphology, rms, and height of CB[7] nanocoating under different parameters. The presence of CB[7] on the nanocoating and its binding nature was determined by Infrared absorption and X-ray photoelectron spectroscopy. The present method of CB[7] nanocoating preparation is easy, versatile, scalable, and does not need the addition of electrolyte additives. Prepared CB[7] films are high-quality, uniform, and could be used as a novel sensing platform to tether required functional groups., Funding Agencies|Swedish Research CouncilSwedish Research CouncilEuropean Commission [2016-06014]

We present an overview of the main techniques for production and processing of graphene and related materials (GRMs), as well as the key characterization procedures. We adopt a hands-on approach, providing practical details and procedures as derived from literature as well as from the authors experience, in order to enable the reader to reproduce the results. Section I is devoted to bottom up approaches, whereby individual constituents are pieced together into more complex structures. We consider graphene nanoribbons (GNRs) produced either by solution processing or by on-surface synthesis in ultra high vacuum (UHV), as well carbon nanomembranes (CNM). Production of a variety of GNRs with tailored band gaps and edge shapes is now possible. CNMs can be tuned in terms of porosity, crystallinity and electronic behaviour. Section II covers top down techniques. These rely on breaking down of a layered precursor, in the graphene case usually natural crystals like graphite or artificially synthesized materials, such as highly oriented pyrolythic graphite, monolayers or few layers (FL) flakes. The main focus of this section is on various exfoliation techniques in a liquid media, either intercalation or liquid phase exfoliation (LPE). The choice of precursor, exfoliation method, medium as well as the control of parameters such as time or temperature are crucial. A definite choice of parameters and conditions yields a particular material with specific properties that makes it more suitable for a targeted application. We cover protocols for the graphitic precursors to graphene oxide (GO). This is an important material for a range of applications in biomedicine, energy storage, nanocomposites, etc. Hummers and modified Hummers methods are used to make GO that subsequently can be reduced to obtain reduced graphene oxide (RGO) with a variety of strategies. GO flakes are also employed to prepare three-dimensional (3d) low density structures, such as sponges, foams, hydro- or aeroge, Funding Agencies|European Commission Graphene Flagship Core1 [696656, 785219]

In this research a whispering gallery mode (WGM) resonator based on vertically oriented ZnO nanorods, which were formed on silicon surface (silicon/ZnO-NRs), has been applied in the design of optical immunosensor that was dedicated for the determination of grapevine virus A-type (GVA) proteins. Vertically oriented ZnO-NRs were grown on silicon substrates by atmospheric pressure metal organic chemical vapor deposition (APMOCVD) and the silicon/ZnO-NRs structures formed were characterized by structural and optical methods. Optical characterization demonstrates that silicon/ZnO-NRs-based structures can act as whispering gallery mode (WGM) resonator where quasi-whispering gallery modes (quasi-WGMs) are generated. These quasi-WGMs were experimentally observed in the visible and infrared ranges of the photoluminescence spectra. In order to design an immuno-sensing system the anti-GVA antibodies were immobilized on the surface of silicon/ZnO-NRs and in this way silicon/ZnO-NRs/anti-GVA structure was formed. The immobilization of anti-GVA antibodies and then the interaction of silicon/ZnO-NRs/anti-GVA structure with GVA proteins (GVA-antigens) resulted in an opposite shifts of the WGMs peaks in the visible range of the photoluminescence spectra observed as a defect-related photoluminescence emission of ZnO-NRs. Here designed silicon/ZnO-NRs/anti-GVA immuno-sensing structure demonstrates the sensitivity towards GVA-antigens in the concentration range of 1-200 ng/ml. Bioanalytical applicability of the silicon/ZnO-NRs-based structures in the WGMs registration mode is discussed., Funding Agencies|Ukrainian-Lithuanian Research project "Application of hybrid nanostructures which are based on TiO2 or ZnO and modified by biomolecules, in optoelectronic sensors" Lithuanian Research Council [P-LU-18-53]; Swedish Research Council (VR) Marie Sklodowska Curie International Grant [2015-00679]; AForsk [14-517]

Modification of epitaxial graphene on silicon carbide (EG/SiC) was explored by ion implantation using 10 keV nitrogen ions. Fragments of monolayer graphene along with nanostructures were observed following nitrogen ion implantation. At the initial fluence, sp(3) defects appeared in EG; higher fluences resulted in vacancy defects as well as in an increased defect density. The increased fluence created a decrease in the intensity of the prominent peak of SiC as well as of the overall relative Raman intensity. The X-ray photoelectron spectroscopy (XPS) showed a reduction of the peak intensity of graphitic carbon and silicon carbide as a result of ion implantation. The dopant concentration and level of defects could be controlled both in EG and SiC by the fluence. This provided an opportunity to explore EG/SiC as a platform using ion implantation to control defects, and to be applied for fabricating sensitive sensors and nanoelectronics devices with high performance., Funding Agencies|Swedish Research CouncilSwedish Research CouncilEuropean Commission [2016-06014]; Aforsk Research Grant [19-675]; VR grant [2018-03957, 2018-04962]; Vinnova grantVinnova [2019-04882]

Surface functionalization has been shown to allow tailoring of graphene lattice thus making it suitable for different applications like sensing, supercapacitance devices, drug delivery system and memory devices. In this work, surface functionalization of epitaxial graphene on SiC (EG/SiC) was done by ion beam technology (30 keV Ag- ions at fluences ranging from 5 x 10(12) ions/cm(2) to 5 x 10(14) ions/cm(2)), which is one of the most precise techniques for introducing modifications in materials. Atomic force microscopy showed presence of nanostructures in ion implanted samples and Photoluminescence and X-ray photoelectron spectroscopy revealed that these are probably silicon oxy carbide. High-resolution transmission electron microscopy (HRTEM) showed decoupling of buffer layer from SiC substrate at many places in ion implanted samples. Further, HRTEM and Raman spectroscopy showed amorphization of both graphene and SiC at highest fluence. Fluence dependent increase in absorbance and resistance was observed. Gas sensors fabricated on pristine and ion implanted samples were able to respond to low concentration (50 ppb) of NO2 and NH3 gases. Detecting NH3 gas at low concentration further provides a simple platform for fabricating highly sensitive urea biosensor. We observed response inversion with increasing fluence along with presence of an optimal fluence, which maximized gas sensitivity of EG/SiC. (C) 2019 Elsevier Ltd. All rights reserved., Funding Agencies|Swedish research councilSwedish Research Council [VR 2016-05362, VR 2016-06014, VR 2018-04962, VR 2018-04290]; Aforsk Research Grant [19-675]; Knut and Alice Wallenberg FoundationKnut & Alice Wallenberg Foundation [KAW2016.0358]; VINN Excellence Center Functional Nanoscale Materials (FunMat-2) [2016-05156]; Swedish Foundation for Strategic research (SSF)Swedish Foundation for Strategic Research [GMT 14-0077, RMA15-024]

We present a comparative study of the C-face and Si-face of 3C-SiC(111) grown on off-oriented 4H-SiC substrates by the sublimation epitaxy. By the lateral enlargement method, we demonstrate that the high-quality bulk-like C-face 3C-SiC with thickness of ~1 mm can be grown over a large single domain without double positioning boundaries (DPBs), which are known to have a strongly negative impact on the electronic properties of the material. Moreover, the C-face sample exhibits a smoother surface with one unit cell height steps while the surface of the Si-face sample exhibits steps twice as high as on the C-face due to step-bunching. High-resolution XRD and low temperature photoluminescence measurements show that C-face 3C-SiC can reach the same high crystalline quality as the Si-face 3C-SiC. Furthermore, cross-section studies of the C- and Si-face 3C-SiC demonstrate that in both cases an initial homoepitaxial 4H-SiC layer followed by a polytype transition layer are formed prior to the formation and lateral expansion of 3C-SiC layer. However, the transition layer in the C-face sample is extending along the step-flow direction less than that on the Si-face sample, giving rise to a more fairly consistent crystalline quality 3C-SiC epilayer over the whole sample compared to the Si-face 3C-SiC where more defects appeared on the surface at the edge. This facilitates the lateral enlargement of 3C-SiC growth on hexagonal SiC substrates., Funding agencies: Swedish Research Council (Vetenskapsradet) [621-2014-5461, 2018-04670, 2016-05362, 621-2014-5825]; Swedish Research Council for Environment, Agricultural Sciences and Spatial Planning (FORMAS) [2016-00559]; Swedish Foundation for International Cooperation

This work illustrates the impact of atmospheric gases on the surface of epitaxial graphene. The different rate of adsorption on different parts of graphene samples provides a concrete evidence that the surface morphology of graphene plays a significant role in this process. The uneven adsorption occurs only on the surface of the monolayer graphene and not on bilayer graphene. The second monolayer is distinguished and verified by the phase contrast mode of atomic force microscopy and the low energy electron microscopy, respectively. Raman spectroscopy is used to study the strain on the surface of graphene; results indicate that monolayer and bilayer graphene exhibit different types of strain. The bilayer is under more compressive strain in comparison with monolayer graphene that hinders the process of adsorption. However, the wrinkles and edges of steps of the bilayer are under tensile strain, hence, facilitate adsorption. Samples were subjected to X-ray photoelectron spectroscopy which confirms that the adsorbates on the epitaxial graphene are carbon clusters with nitrogen and oxygen contamination. For reversing the adsorption process the samples are annealed and a method for the removal of these adsorbates is proposed., Funding Agencies|European Union Horizon 2020 research and innovation programme [696656]; Graphene Flagship [CNECT-ICT-604391]; VR [621-2014-5805]; SSF [GMT14-0077]; Angpanneforeningens Forskningsstiftelse [16-541]

Multilayer graphene has exhibited distinct electronic properties such as the tunable bandgap for optoelectronic applications. Among all graphene growth techniques, thermal decomposition of SiC is regarded as a promising method for production of device-quality graphene. However, it is still very challenging to grow uniform graphene over a large-area, especially multilayer graphene. One of the main obstacles is the occurrence of step bunching on the SiC surface, which significantly influences the formation process and the uniformity of the multilayer graphene. In this work, we have systematically studied the growth of monolayer and multilayer graphene on off-axis 3CSiC(111). Taking advantage of the synergistic effect of periodic SiC step edges as graphene nucleation sites and the unique thermal decomposition energy of 3CSiC steps, we demonstrate that the step bunching can be fully eliminated during graphene growth and large-area monolayer, bilayer, and four-layer graphene can be controllably obtained on high-quality off-axis 3CSiC(111) surface. The low energy electron microscopy results demonstrate that a uniform four-layer graphene has been grown over areas of tens of square micrometers, which opens the possibility to tune the bandgap for optoelectronic devices. Furthermore, a model for graphene growth along with the step bunching elimination is proposed., Funding agencies: Swedish Research Council (Vetenskapsradet) [621-2014-5461, 621-2014-5825]; Swedish Research Council for Environment, Agricultural Sciences and Spatial Planning (FORMAS) [2016-00559]; Swedish Foundation for International Cooperation in Research and Higher

Here, we report the electrochemical deposition of lead (Pb) as a model metal on epitaxial graphene fabricated on silicon carbide (Gr/SiC). The kinetics of electrodeposition and morphological characteristics of the deposits were evaluated by complementary electrochemical, physical and computational methods. The use of Gr/SiC as an electrode allowed the tracking of lead-associated redox conversions. The analysis of current transients passed during the deposition revealed an instantaneous nucleation mechanism controlled by convergent mass transport on the nuclei locally randomly distributed on epitaxial graphene. This key observation of the deposit topology was confirmed by low values of the experimentally-estimated apparent diffusion coefficient, Raman spectroscopy and scanning electron microscopy (SEM) studies. First principles calculations showed that the nucleation of Pb clusters on the graphene surface leads to weakening of the interaction strength of the metal-graphene complex, and only spatially separated Pb adatoms adsorbed on bridge and/or edge-plane sites can affect the vibrational properties of graphene. We expect that the lead adatoms can merge in large metallic clusters only at defect sites that reinforce the metal-graphene interactions. Our findings provide valuable insights into both heavy metal ion electrochemical analysis and metal electroplating on graphene interfaces that are important for designing effective detectors of toxic heavy metals., Funding Agencies|VR grant [621-2014-5805]; SSF [SSF GMT14-0077, SSF RMA15-0024]; Angpanneforeningens Forskningsstiftelse [16-541]

Efficient ammonia gas sensor devices were fabricated based on nickel oxide (NiO) nanostructures films. Two chemical synthesis approaches were used: chemical spray pyrolysis (CSP) and chemical bath deposition (CBD), aiming at obtaining highly developed surface area and high chemical reactivity of NiO. Crystal structure, morphology, and composition of NiO films and nanostructures were investigated by scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. CSP method results in the synthesis of NiO films with pure cubic crystalline structure of preferred orientation along (111) direction. The type of the precursors used (nickel acetate, nickel chloride and nickel nitrate) affects the morphology and crystallites average size of the deposited films. CBD method consisted of two stages: (i) deposition of nickel hydroxide phase and (ii) thermal annealing of nickel hydroxide at 450 A degrees C in air for 4 h. Resulted structures were nanoflakes, vertically arranged in a "wall-like" morphology. Fabricated structures were found to be sensitive to ammonia differently, depending on the synthesis approach and material morphology. NiO films deposited by CBD demonstrated a stable response to ammonia with maximum magnitude at the operating temperature of 300 A degrees C. The highest average response for the CBD-NiO sample was 114.3-141.3% for 25 and 150 ppm NH3, respectively, whereas the response range observed for the film processed by spray pyrolysis using nickel chloride was 31.7-142.5% for 25 and 150 ppm NH3, respectively., Funding Agencies|Egyptian Ministry for Higher Education and Scientific Research; Swedish Research Council [VR 348-2013-6782]; Angpanneforeningens Forskningsstiftelse [14-517]; Swedish Research Council (VR) Marie Sklodowska Curie International Career Grant [2015-00679]

Epitaxial graphene (EG) on silicon carbide (SiC) is a combination of two robust materials that are excellent candidates for post silicon electronics. In this work, we systematically investigate structural changes in SiC substrate as well as graphene on SiC and explore the potential for controlled applications due to 100 MeV silver swift heavy ion (SHI) irradiation. Raman spectroscopy showed fluence dependent decrease in intensity of first and second order modes of SiC, along with decrease in Relative Raman Intensity upon ion irradiation. Similarly, Fourier-transform infrared (FTIR) showed fluence dependent decrease in Si-C bond intensity with presence of C = O, Si-O-Si, Si-Si and C-H bond showing introduction of vacancy, substitutional and sp(3) defects in both graphene and SiC. C1s spectra in XPS shows decrease in C = C graphitic peak and increase in interfacial layer following ion irradiation. Reduction in monolayer coverage of graphene after ion irradiation was observed by Scanning electron microscopy (SEM). Further, UV-Visible spectroscopy showed increase in absorbance of EG on SiC at increasing fluence. I-V characterization showed fluence dependent increase in resistance from 62.9 O in pristine sample to 480.1 Omega in sample irradiated at 6.6 x 10(12) ions/cm(2) fluence. The current study demonstrates how SHI irradiation can be used to tailor optoelectronic applicability of EG on SiC., Funding Agencies|Graphene Flagship [CNECT-ICT-604391]; Swedish Research Council [2015-05876]

The market of high power, high frequency and high temperature based electronic devices is captured by SiC due to its superior properties like high thermal conductivity and high sublimation temperature and also due to the limitation of silicon based electronics in this area. There is a need to investigate effect of ion irradiation on SiC due to its application in outer space as outer space is surrounded both by low and high energy ion irradiations. In this work, effect of low energy ion irradiation on structural and optical property of 4H-SiC is investigated. ATR-FTIR is used to study structural modification and UV-Visible spectroscopy is used to study optical modifications in 4H-SiC following 30 keV Ag ion irradiation. FTIR showed decrease in bond density of SiC along the ion path (track) due to the creation of point defects. UV-Visible absorption spectra showed decrease in optical band gap from 3.26 eV to 2.9 eV. The study showed degradation of SiC crystallity and change in optical band gap following low energy ion irradiation and should be addressed while fabricationg devices based on SiC for outer space application. Additionally, this study provides a platform for introducing structural and optical modification in 4H-SiC using ion beam technology in a controlled manner., Funding Agencies|Graphene Flagship [CNECT-ICT-604391]; Swedish Research Council [2015-05876]

Nickel oxide thin films were deposited by a simple and low-cost spray pyrolysis technique using three different precursors: nickel nitrate, nickel chloride, and nickel acetate on corning glass substrates. X-ray diffraction show that the NiO films are polycrystalline and have a cubic crystal structure, although predominantly with a preferred 111-orientation in the growth direction and a random in-plane orientation. The deconvolution of the Ni 2p and O 1s core level X-ray photoelectron-spectra of nickel oxides produced by using different precursors indicates a shift of the binding energies. The sprayed NiO deposited from nickel nitrate has an optical transmittance in the range of 60-65% in the visible region. The optical band gap energies of the sprayed NiO films deposited from nickel nitrate, nickel chloride and nickel acetate are 3.5, 3.2 and 3.43 eV respectively. Also, the extinction coefficient and refractive index of NiO films have been calculated from transmittance and reflectance measurements. The average value of refractive index for sprayed films by nickel nitrate, nickel chloride and nickel acetate are 2.1, 1.6 and 1.85 respectively. It is revealed that the band gap and refractive index of NiO films by using nickel nitrate corresponds to the commonly reported values. We attribute the observed behavior in the optical band gap and optical constants as due to the change of the Ni/O ratio., Funding Agencies|Swedish Research Council [VR 348-2013-6782]; Egyptian Ministry for Higher Education and Scientific Research; Angpanneforeningens Forskningsstiftelse [14-517]; Swedish Research Council (VR) Marie Sklodowska Curie International Career "GREEN 2D FOX" [2015-00679]

In this work, surface functionalization of epitaxial graphene grown on silicon carbide was performed by ion irradiation to investigate their gas sensing capabilities. Swift heavy ion irradiation using 100 MeV silver ions at four varying fluences was implemented on epitaxial graphene to investigate morphological and structural changes and their effects on the gas sensing capabilities of graphene. Sensing devices are expected as one of the first electronic applications using graphene and most of them use functionalized surfaces to tailor a certain function. In our case, we have studied irradiation as a tool to achieve functionalization. Morphological and structural changes on epitaxial graphene layers were investigated by atomic force microscopy, Raman spectroscopy, Raman mapping and reflectance mapping. The surface morphology of irradiated graphene layers showed graphene folding, hillocks, and formation of wrinkles at highest fluence (2 x 10(13) ions/cm(2)). Raman spectra analysis shows that the graphene defect density is increased with increasing fluence, while Raman mapping and reflectance mapping show that there is also a reduction of monolayer graphene coverage. The samples were investigated for ammonia and nitrogen dioxide gas sensing applications. Sensors fabricated on pristine and irradiated samples showed highest gas sensing response at an optimal fluence. Our work provides new pathways for introducing defects in controlled manner in epitaxial graphene, which can be used not only for gas sensing application but also for other applications, such as electrochemical, biosensing, magnetosensing and spintronic applications. (C) 2017 Elsevier B.V. All rights reserved., Funding Agencies|Graphene Flagship [CNECT-ICT-604391]; Swedish Research Council [2015-05876]

Tuning the emission energy of graphene quantum dots (GQDs) and understanding the reason of tunability is essential for the GOD function in optoelectronic devices. Besides material-based challenges, the way to realize chemical doping and band gap tuning also pose a serious challenge. In this study, we tuned the emission energy of GQDs by substitutional doping using chlorine, nitrogen, boron, sodium, and potassium dopants in solution form. Photoluminescence data obtained from (Cl- and N-doped) GQDs and (B-, Na-, and K-doped) GQDs, respectively exhibited red- and blue-shift with respect to the photoluminescence of the undoped GQDs. X-ray photoemission spectroscopy (XPS) revealed that oxygen functional groups were attached to GQDs. We qualitatively correlate red-shift of the photoluminescence with the oxygen functional groups using literature references which demonstrates that more oxygen containing groups leads to the formation of more defect states and is the reason of observed red-shift of luminescence in GQDs. Further on, time resolved photoluminescence measurements of Cl- and N-GQDs demonstrated that Cl substitution in GQDs has effective role in radiative transition whereas in N-GQDs leads to photoluminescence (PL) quenching with non-radiative transition to ground state. Presumably oxidation or reduction processes cause a change of effective size and the bandgap., Funding Agencies|Higher Education Commission Pakistan (HEC) under NRPU [2913/RD]; Graphene Flagship [CNECT-ICT-604391]; Angpanneforeningen Research Foundation; Swedish Research Council [2015-05876]; Rositsa Yakimova

We demonstrate growth of thick SiC layers (100–200 µm) on nominally on-axis hexagonal substrates using sublimation epitaxy in vacuum (10−5 mbar) at temperatures varying from 1700 to 1975 °C with growth rates up to 270 µm/h and 70 µm/h for 6H- and 4H–SiC, respectively. The stability of hexagonal polytypes are related to process growth parameters and temperature profile which can be engineered using different thermal insulation materials and adjustment of the induction coil position with respect to the graphite crucible. We show that there exists a range of growth rates for which single-hexagonal polytype free of foreign polytype inclusions can be maintained. Further on, foreign polytypes like 3C–SiC can be stabilized by moving out of the process window. The applicability of on-axis growth is demonstrated by growing a 200 µm thick homoepitaxial 6H–SiC layer co-doped with nitrogen and boron in a range of 1018 cm−3 at a growth rate of about 270 µm/h. Such layers are of interest as a near UV to visible light converters in a monolithic white light emitting diode concept, where subsequent nitride-stack growth benefits from the on-axis orientation of the SiC layer.

This review is devoted to one of the most promising two-dimensional (2D) materials, graphene. Graphene can be prepared by different methods and the one discussed here is fabricated by the thermal decomposition of SiC. The aim of the paper is to overview the fabrication aspects, growth mechanisms, and structural and electronic properties of graphene on SiC and the means of their assessment. Starting from historical aspects, it is shown that the most optimal conditions resulting in a large area of one ML graphene comprise high temperature and argon ambience, which allow better controllability and reproducibility of the graphene quality. Elemental intercalation as a means to overcome the problem of substrate influence on graphene carrier mobility has been described. The most common characterization techniques used are low-energy electron microscopy (LEEM), angle-resolved photoelectron spectroscopy (ARPES), Raman spectroscopy, atomic force microscopy (AFM) in different modes, Hall measurements, etc. The main results point to the applicability of graphene on SiC in quantum metrology, and the understanding of new physics and growth phenomena of 2D materials and devices., Funding Agencies|European Union Seventh Framework Program [604391]; Swedish Research Council [VR 621-2014-5805]; SSF; KAW funding

We present a technique for etching of SiC which is based on sublimation and can be used to modify the morphology and reconstruction of silicon carbide surface for subsequent epitaxial growth of various materials, for example graphene. The sublimation etching of 6H-, 4H- and 3C-SiC was explored in vacuum (10−5 mbar) and Ar (700 mbar) ambient using two different etching arrangements which can be considered as Si-C and Si-C-Ta chemical systems exhibiting different vapor phase stoichiometry at a given temperature. The surfaces of different polytypes etched under similar conditions are compared and the etching mechanism is discussed with an emphasis on the role of tantalum as a carbon getter. To demonstrate applicability of such etching process graphene nanoribbons were grown on a 4H-SiC surface that was pre-patterned using the thermal etching technique presented in this study., Funding agencies: Swedish Research Council [621-2014-5825]; Graphene Flagship [CNECT-ICT-604391]; AForsk foundation [16-576]; Swedish Foundation for Strategic Research (SSF); Knut and Allice Wallenberg Foundation

We report on the structural and electronic properties of graphene grown on SiC by high-temperature sublimation. We have studied thickness uniformity of graphene grown on 4H-SiC (0 0 0 1), 6H-SiC (0 0 0 1), and 3C-SiC (1 1 1) substrates and investigated in detail graphene surface morphology and electronic properties. Differences in the thickness uniformity of the graphene layers on different SiC polytypes is related mainly to the minimization of the terrace surface energy during the step bunching process. It is also shown that a lower substrate surface roughness results in more uniform step bunching and consequently better quality of the grown graphene. We have compared the three SiC polytypes with a clear conclusion in favor of 3C-SiC. Localized lateral variations in the Fermi energy of graphene are mapped by scanning Kelvin probe microscopy It is found that the overall single-layer graphene coverage depends strongly on the surface terrace width, where a more homogeneous coverage is favored by wider terraces, It is observed that the step distance is a dominating, factor in determining the unintentional doping of graphene from the SiC substrate. Microfocal spectroscopic ellipsometry mapping of the electronic properties and thickness of epitaxial graphene on 3C-SiC (1 1 1) is also reported. Growth of one monolayer graphene is demonstrated on both Si- and C-polarity of the 3C-SiC substrates and it is shown that large area homogeneous single monolayer graphene can be achieved on the Si-face substrates. Correlations between the number of graphene monolayers on one hand and the main transition associated with an exciton enhanced van Hove singularity at similar to 4.5 eV and the free-charge carrier scattering time, on the other are established It is shown that the interface structure on the Si- and C-polarity of the 3C-SiC (1 1 1) differs and has a determining role for the thickness and electronic properties homogeneity of the epitaxial graphene.

One of the main challenges in the fabrication of device quality graphene is the achievement of large area monolayer graphene that is processing compatible. Here, the impact of the substrate properties on the thickness uniformity and electronic characteristics for epitaxial graphene on SiC produced by high temperature sublimation has been evidenced and discussed. Several powerful techniques have been used to collect data, among them large scale ellipsometry mapping has been demonstrated for the first time. The study is covering all three SiC polytype, e.g. 4H-, 6H- and 3C-SiC in order to reveal eventual peculiarities that have to be controlled during graphene growth. The advantage of the cubic polytype is unambiguously demonstrated.

Epitaxial graphene growth was performed on the Si-terminated face of 4H-, 6H-, and 3C-SiC substrates by silicon sublimation from SiC in argon atmosphere at a temperature of 2000 degrees C. Graphene surface morphology, thickness and band structure have been assessed by using atomic force microscopy, low-energy electron microscopy, and angle-resolved photoemission spectroscopy, respectively. Differences in the morphology of the graphene layers on different SiC polytypes is related mainly to the minimization of the terrace surface energy during the step bunching process. The uniformity of silicon sublimation is a decisive factor for obtaining large area homogenous graphene. It is also shown that a lower substrate surface roughness results in more uniform step bunching with a lower distribution of step heights and consequently better quality of the grown graphene. Large homogeneous areas of graphene monolayers (over 50 x 50 mu m(2)) have been grown on 3C-SiC (1 1 1) substrates. The comparison with the other polytypes suggests a similarity in the surface behaviour of 3C- and 6H-SiC., Funding Agencies|FP7 EU project Concept Graphene and the Swedish Research Council (VR)|2011-44472010-3511 Grafic ESF

We report on a comparative micro-photoluminescence investigation of ZnO hexagonal nanopillars (HNPs) and the seeding layer grown on the off-axis 4H-SiC substrate. Transmission electron microscope (TEM) results establish that a thin seeding layer continuously covers the terraces of 4H-SiC prior to the growth of ZnO HNPs. Low temperature photoluminescence (LTPL) shows that ZnO HNPs are only dominated by strong donor bound exciton emissions without any deep level emissions. Micro-LTPL mapping demonstrates that this is specific also for the seeding layer. To further understand the recombination mechanisms, time-resolved micro-PL spectra (micro-TRPL) have been collected at 5 K and identical bi-exponential decays have been found on both the HNPs and seeding layer. Temperature-dependent TRPL indicates that the decay time of donor bound exciton is mainly determined by the contributions of non-radiative recombinations. This could be explained by the TEM observation of the non-radiative defects in both the seeding layer and HNPs, like domain boundaries and dislocations, generated at the ZnO/SiC interface due to biaxial strain., funding agencies|EU| MRTN-CT-2006-035735 |Swedish Research Council

ZnO single crystal nanohexagons have been grown heteroepitaxially on p-type Si-face 4H-SiC substrates with 8 degrees miscut from to [0 0 0 1] by catalyst-free atmospheric pressure metalorganic chemical vapor deposition and characterized by x-ray diffraction, scanning and transmission electron microscopy as well as energy disperse x-ray and cathodoluminescence analyses. The as-grown ZnO nanohexagons have a pillar shape terminated by a and c plane facets, and are aligned along the growth direction with the epitaxial relation [0 0 0 1](ZnO) parallel to[0 0 0 1](4H-SiC) and [1 0 (1) over bar 0](ZnO) parallel to[1 0 (1) over bar 0](4H-SiC). The ZnO nanohexagons demonstrate intense UV emission (lambda(NBE)=376 nm) and negligible defect-related luminescence.

Free standing AIN wafers were grown on pre-patterned and in situ patterned 4H-SiC substrates by a physical vapor transport method. It is based on the coalescence of AIN microrods, which evolve from the apex of SiC pyramids grown on the SIC substrate during a temperature ramp up for in situ patterned substrate and SiC pyramids formed by reactive ion etching (RIE). This process yields stress-free (according XRD and Raman results) AIN single crystals with a thickness up to 400 mu m and low dislocation density.

Highly oriented AlN single crystal nanowires with aspect ratio up to 600, diameter in the range of 40-500 nm, and 100 mu m lengths, have been synthesized via a vapor-solid growth mechanism. The results were obtained at 1750 degrees C and 850 mbar nitrogen pressure on vicinal SiC substrates pretreated by SiC sublimation epitaxy in order to attain distinguishable terraces. It was found that the nanowires change in thickness after they have reached a critical length, and this fact contributes to an understanding of the growth mechanism of AlN nanowires. The nanowires are hexagonally shaped and perfectly aligned along the [0001] direction with a small tilt given by the substrate vicinality. Under nitrogen excess a preferential growth along the c-axis of the wurtzite structure takes place while below some critical value of nitrogen pressure the growth mode switches to lateral. The AlN nanowires are shown to have a dislocation free wurtzite crystal structure. Some possible applications are discussed.

A sublimation-recondensation process is presented for high quality AlN (0001) crystals at a high growth rate by employing 4H-SiC substrates with a predeposited epilayer. It is based on the coalescence of well oriented AlN microrods, which evolve from the apex of 2H-SiC pyramids grown out of hexagonal pits formed by thermal etching of the substrate during a temperature ramp up. This process yields stress-free 120-mu m-thick AlN single crystals with a dislocation density as low as 2x10(6) cm(-2).

Wurtzite ScAlN nanowires, grown on a scandium nitride (ScN) thin film by hydride vapor phase epitaxy (HVPE), were analyzed by energy dispersive analysis of X-rays (EDX), CL, high resolution transmission electron spectroscopy (HRTEM), and scanning electron microscopy (SEM). The wires were grown along the [0 0 0 1] axis, had an average length of 1 mu m, a diameter between 50 and 150 run, and a ScAlN composition with a 95:5 Al:Sc ratio. Cathodoluminescence studies on the individual wires showed a sharp emission near 2.4 eV, originating from the Sc atoms in the aluminum nitride (AlN) matrix. The formation of such a semiconducting ScAlN alloy could present a new alternative to InAlN for optoelectronic applications operating in the 200-550 nm range.

Aluminum nitride (AlN) exhibits a large direct band gap, 6.2 eV, and is thus suitable forsolid state white-light-emitting devices. It is capable in spintronics because of its high Curietemperature if doped with transition metals. AlN can also be used as a buffer layer for growth ofdevice-grade GaN as well as for application in sensors, surface acoustic wave devices, and hightemperatureelectronics. AlN shows excellent field-emission performance in vacuummicroelectronic devices due to its small electron affinity value, which is from negative to 0.6 eV.In this sense, nanostructured AlN, such as AlN nanowires and nanorods, is important forextending our knowledge on the potential of nanodevice applications. For growth of bulk AlN thesublimation- recondensation (a kind of physical vapor transport growth) method is the mostsuccessful and promising crystal growth technique. In thesis the physical vapor transport (PVT) principle has been implemented for synthesisof AlN on 4H-SiC in sublimation epitaxy close space configuration. It has been shown that theAlN crystal morphology is responsive to the growth conditions given by temperature (1650-1900oC) and nitrogen pressure (200-800 mbar) and each morphology kind (platelet-like, needles, columnar structure, continuous layers, and free-standing quasi bulk material) occurs within anarrow window of growth parameters. Controlled operation conditions for PVT growth of wellaligned perfectly oriented arrays of AlN highly symmetric hexagonal microrods have beenelaborated and the mechanism of microrod formation has been elucidated. Special patterned SiCsubstrates have been created which act as templates for the AlN selective area growth. Themicrorods revealed an excellent feature of boundary free coalescence with growth time,eventually forming ~120 μm thick AlN layer which can be easily detached from the SiC substratedue to a remarkable performance of structural evolution. It was discovered that the locally grownAlN microrods emerge from, Aluminium nitrid (AlN) har ett stort direkt bandgap (6.2 eV) och är lämplig för lysdioder.Det är tillämpligt inom spinnelektronik eftersom det har en hög Marie Curie-temperatur när det ärdopad med övergångsmetaller. AlN kan även användas som ett buffertskikt för tillväxt avkomponentkvalitativt GaN likväl som för sensortillämpningar, ytvågsfilterkomponenter, ochhögtemperaturelektronik. Aluminium nitrid visar excellent fältemission i vakuumkomponenter pågrund av sin låga elektronaffinitet, som är från negativt till 0.6 eV. I det här fallet så ärnanostrukturer av AlN, som nanotrådar och -stavar, viktiga för att utöka vår kunskap ompotentiella nanokomponenter. För tillväxt av AlN är sublimeringsmetoden den mestframgångsrika och lovande framställningstekniken av kristaller. I den här avhandlingen så har principen för den fysiska gastransporttekniken (PVT)implementerats för syntes av AlN på 4H-SiC filmer i en ny konfiguration genomsublimeringsepitaxi. Det demonstreras att morfologin hos AlN visar respons förtillväxtförhållandena som ges av temperatur (1650-1900oC) och kvävetryck (200-800 mbar) ocholika morfologityper (skivlika, trådar, kolumnstrukturer, kontinuerliga skikt, och friståendekvasibulkmaterial)uppstår inom ett snävt fönster av tillväxtparametrar. Kontrollerade operativaförhållanden för PVT-tillväxt av räta perfekt orienterade ansamlingar av symmetriska AlNmikrostavar har utvecklats och deras formationsmekanism diskuterats. Speciellt mönstrade SiCsubstrat har skapats som agerar utgångsmaterial för selektiv AlN tillväxt. Mikrostavarna avslöjarett särdrag av sammanväxning utan gränslinjer med tillväxttid, som formar 120 μm tjocka AlNskikt som lätt kan avskiljas från SiC substratet genom en anmärkningsvärd strukturell evolution.Upptäckten gjordes att lokal tillväxt av AlN mikrostavar uppkommer från skarpa hexagonalapyramider som består av den sällan förekommande 2H-SiC modifikationen och tunna AlN skiktpå ytan. Två unika följder uppkommer genom upptäckten, den för

The aim of this study was to propose a growth procedure for preparation of crack-free thick aluminum nitride (AlN) layers that can be easily separated from the substrate. The overall process is based on the physical vapor transport method employing a seed and a source material. In this case, the substrate is an epitaxial 4H-SiC layer and the growth of AlN is initiated at etch pits formed during the ramp up time prior to establishing growth temperature. Development of hexagonal pyramids on which arrays of microrods are formed is the core of the growth procedure. Free-standing wafers having 10 mm diameter and about 120 μm thick have been fabricated.

ZnO is a wide band gap (3.37 eV) semiconductor material with a high exciton binding energy (60 meV) at room temperature, which is a prerequisite for realization of efficient and stable optoelectronic systems. We demonstrated the APMOCVD growth of nanostructured ZnO material on Si and SiC with advanced emitting properties. The comparison of the properties of nanostructured polycrystalline layers with spatially disconnected ZnO nanocrystals clearly showed the advantage of the latter structures. Such structures distinctively luminesce in the UV range of the spectrum due to excitonic emission, while the contribution of the defect related luminescence is negligible. The significant improvement of the PL properties can be related to the decreased number of non-radiative recombination centers in the nanocrystals of high structural quality.

Emissive properties of ZnO are of great interests in terms of the UV LED device design. The persistent "green" luminescence due to deep defect is an obstacle for obtaining an intense UV emission, expected from ZnO. We report the positive role of thermally diffused H toward quenching the defect emission in ZnO. It is suggested that hydrogen passivates defects responsible for DLE, resulting in efficient near band edge luminescence. As-grown ZnO/SiNx :H/Si films, deposited at 350 degrees C demonstrate intense narrow peaks of UV emission at 380 nm and a ratio of emission intensities, NBE/DLE approximate to 42. [GRAPHICS]

Epitaxial layers of AlGaN were grown by hot-wall MOCVD and their surfaces wet chemically etched with phosphorous acid. The as-grown surfaces and the development of the etched surfaces after 10 and 20 min of etching were studied with atomic force microscopy (AFM) and CL. In the as-grown layers growth features may be resolved while the RMS is as low as 1.4 Å in a scan area of 2×2 μm. Surfaces etched for 10 min had developed etch pits and a low RMS roughness of 7 Å indicating a uniform quality of the layers. Micrometer scale hexagonal features were observed after 20 min of etching. In some cases a deep hexagonal etch pit is observed in the centre of the hexagonal feature with a 30° rotation to each other, suggesting that the origin is substrate-induced defects. © 2006 Elsevier B.V. All rights reserved.

The search for materials and systems, capable of operating long term under physiological conditions, has been a strategy for many research groups during the past years. Silicon carbide (SiC) is a material, which can meet the demands due to its high biocompatibility, high inertness to biological tissues and to aggressive environment, and the possibility to make all types of electronic devices. This paper reviews progress in biomedical and biosensor related research on SiC. For example, less biofouling and platelet aggregation when exposed to blood is taken advantage of in a variety of medical implantable materials while the robust semiconducting properties can be explored in surface functionalized bioelectronic devices. © 2007 IOP Publishing Ltd.

The objectives of this work are to contribute to the knowledge about physical and chemical properties of WBG semiconductors, such as ZnO and GaN towards development of advanced bio- and chemical sensors. For the semiconductors, growth techniques typically yielding single crystal material are applied. Thin epitaxial quality films of ZnO and GaN are fabricated on SiC or sapphire substrates. An emphasis is given to ZnO due to the interesting combination of the semiconductor and oxide properties. Surface bio-functionalization of ZnO is performed by APTES, MPA or MP-TMS molecules. We have compared some of the results to (hydroxylated) GaN surfaces functionalized by MP-TMS. The covalent attachment of the self-assembled biomolecular layers has been proven by XPS analysis. For complementary electrical characterization impedance spectroscopy measurements were performed. The results are intended to serve the realization of bioelectronic transducer devices based on SiC or GaN transistors with a ZnO gate layer. To take advantage of the catalytic properties of ZnO, initial prototypes of chemical sensors for gas sensing are processed on ZnO deposited either on SiC or on sapphire and they are further tested for the response to reducing or oxidizing gas ambient. The sensor devices show sensitivity to oxygen in the surface resistivity mode while a Pt Schottky contact ZnO/SiC device responds to reducing gases. These results are compared to published results on Pt/GaN Schottky diodes. © 2007 Elsevier B.V. All rights reserved.

The present study focused on understanding the formation of needle-like and columnar structures by investigating the initial nucleation of aluminium nitride (AlN) on SiC substrates with SEM, AFM, and XRD. The grown AlN consisted of high concentration (8×104 cm−2) hexagonal hillocks (HHs) that originate from threading dislocations in the substrate. The KOH etching technique has been used to examine the origin and formation process of HHs and defect reduction in the grown AlN crystals. A model is introduced to explain the AlN HH formation. The SEM result shows that the AlN columnar structure was formed by merging of needles, which are grown exactly on completed AlN HHs, followed by a lateral growth.

Self-patterned AlN microrods and nanowires were grown on 4H-SiC substrate by a physical vapor transport method. AlN hexagonal pyramids were found to be nucleation sites for the evolution of the observed morphological forms. The average diameter and length of the nanowires are about 200 nm and 90 µm, respectively. The density of microrods corresponds to the concentration of the pyramids, while the nanowires are less compact. Low-temperature cathodoluminescence spectra of microrods show band gap emission of AlN at 208 nm, which confirms that they are AlN single crystals. A formation mechanism of the AlN structures is suggested.

Surface functionalization of wide band gap semiconductors, SiC, ZnO, and GaN, with organosilane is reported. Formation of self-assembled monolayers of mercaptopropyltrimethoxysilane is confirmed by x-ray photoelectron spectroscopy and atomic force microscopy. The molecules are adsorbed on the surfaces through the silane groups with the free thiol groups molecularly oriented away from the surface. Moreover, chemisorption via the thiolate is observed for the ZnO surface. Immobilization of a model biomolecule to the functionalized surface is demonstrated. An amino acid derivative, i.e., phosphotyrosine derived thiol, is linked on the functionalized ZnO and GaN surfaces via formation of disulfide bridges. © 2007 American Institute of Physics.

In this report we present results on growth and characterization of AlN wires and thinfilms on SiC substrates. We have employed PVT technique in close space geometry for AlNdeposition on SiC off oriented substrates, most of which were prepared to have scratch-free smoothas-grown surface by SiC sublimation epitaxy. By manipulating the surface kinetics we have beenable to determine growth conditions yielding discontinuous or continuous morphologiescorresponding to nanowires and thin films, respectively. A particular feature of the latterexperiments is the fast temperature ramp up at the growth initiation. The AlN surface morphologywas characterized by optical, AFM and XRD tools, which showed good crystal quality independentof the growth mode.

This study focused on growth dependencies, morphological forms and initial nucleation of aluminium nitride (AlN) crystals. Epitaxial layers of AlN have been grown on 4H-SiC substrates by sublimation recondensation in a radio frequency (RF) heated graphite furnace. Both AlN nuclei size and growth rate increased as temperature was increased and decreased as the pressure was increased. The results of these effects are different kinds of surface morphology. We have observed three modes of AlN single crystals: plate-like, columnar and needle-like. Optical microscopy and scanning electron microscopy (SEM) along with atomic force microscopy (AFM) were used to characterize the crystal surface morphology. Cathodoluminescence (CL) and x-ray diffraction (XRD) were applied to determine crystal quality and crystallographic orientation of the grown crystals.

Ferromagnetic phases in as-grown SiC have been studied. An interpretation about the formation based on details of the phase appearance in the layers from optical microscopy, AFM, and TEM investigations is related to the growth. Some phases were found to have a nucleation at the edge of the phase and detailed TEM investigations show that the phases have an increased grain density at the edge while the main part of the phase is monocrystalline., Proc. of the 5th European Conference on Silicon Carbide and Related Materials 2004; Bologna, Italy; August 31 - September 4, 2004

The aim of this study has been to realize growth conditions suitable for seeded sublimation growth of AlN and to understand the relationship between external growth parameters and the initial stages of growth with respect to growth mode and structure evolution. Close space sublimation growth geometry has been used in a RF-heated furnace employing high-purity graphite coated by TaC with a possibility to change the growth environment from C- to Ta-rich. Influence of certain impurities on the initially formed crystallites with respect to their shape, size and population has been considered. It is shown that some impurity containing vapor molecules may act as transport agents and suppliers of nitrogen for the AlN growth. SiC seeds, both bare and with MOCVD AlN buffer, have been employed. By varying the process conditions we have grown crystals with different habits, e.g. from needles, columnar- and plate-like, to freestanding quasi-bulk material. The growth temperature ranged 1600–2000 °C whereas the optimal external nitrogen pressure varied from 200 to 700 mbar. There is a narrow parameter window in the relationship temperature–pressure for the evolution of different structural forms. Growth modes with respect to process conditions are discussed.

Epitaxial growth in hydrogen atmosphere has been studied in relation to sublimation epitaxial growth. A new type of features with a hexagonal shape are observed in the layers grown in hydrogen atmosphere. The morphological details of the features have been studied with optical microscopy and atomic force microscopy. An interactive relation of the defect appearance with the step flow growth mode seems to be present. The results are compared with growth in vacuum, argon, and helium conditions. The possible influence of thermal component to a reactive one in hydrogen etching is discussed.