GRAPHENE ON THE Si-FACE OF SILICON CARBIDE USER MANUAL
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1 GRAPHENE ON THE Si-FACE OF SILICON CARBIDE USER MANUAL 1. INTRODUCTION Silicon Carbide (SiC) is a wide band gap semiconductor that exists in different polytypes. The substrate used for the fabrication of these graphene samples is the 4H-SiC type. These substrates show two polar faces, one Silicon-terminated and another one Carbonterminated. The growth of graphene occurs on both surfaces by following different mechanisms and resulting, consequently, into graphene films with different properties. The samples here described have been treated optimally to obtain high-quality graphene films on top of the Si-face of SiC. The fabrication process consists essentially of two steps. First, under the proper conditions of temperature and gas pressure, the morphology of the SiC surface is changed resulting into the formation of parallel terraces. After that, by changing the annealing conditions, sublimation of the Si atoms on the surface takes place and, after reorganization of the C atoms in the well-known hexagonal lattice, graphene is formed. Hence, the samples here described consist of a single crystalline graphene film grown over a surface composed by parallel terraces. 2. HANDLING OF THE SAMPLES The graphene sample is always provided Si-face up (working face) inside a box. For convenience, a mark (number) has been scratched on the C-face (non-working face). The mark will not be seen on the working Si-face. To obtain the best results out of the samples, handling them with care is strongly recommended. That is: avoid the direct contact and/or the dragging on coarse or rough surfaces to avoid unwanted scratches. Pick your samples using preferably high-precision plastic-ended tweezers. Remove the sample from the provided box gently pressing down the tape below the substrate and slowly move the tweezers below it. The sample will slowly come off. When manipulating the samples, try not to touch the working surface with your tweezers, we recommend to pick them on a corner or on the external laterals. A slight difference between the graphene coverage on the sample center and the sample corners or borders might be found. However, the difference is not larger than 5 to 7% on the single-graphene-layer coverage, which is always higher at the sample center. That is: the Raman analysis of the samples of an area of 40x10 µ 2 at the sample center shows a single-graphene-layer coverage of around 85%, whereas, at the borders of the substrate the percentage of single-graphene-layer coverage can be reduced to ~80%. Storage in vacuum chambers is highly recommended in order to preserve the properties of the graphene films unaltered.
2 3. RECOMMENDATIONS FOR ELECTRON BEAM LITHOGRAPHY (EBL) PROCESSES In case the user needs to micropattern the graphene film using EBL processes, we recommend use of 950K PMMA as positive resist along with the adequate developer and stopper for the selected resist. To remove any contamination from the surface, the use of acetone or isopropanol is suggested. Heating temperatures of upto 120ºC are optimal for such samples. A post annealing treatment in the presence of Hydrogen : Nitrogen (approx. 2 : 1) at 400ºC for 1 hour is strongly recommended to fully remove any remaining dirt or rest of PMMA and/or organic solvents. Purge the chamber/oven for few minutes to get rid of any potential oxygen content. The reaction between oxygen and the samples will result in removal of graphene film. Hence, avoid any exposure of the graphene film to oxygen annealing or plasma chambers, unless you want to intentionally remove the graphene coverage. If these samples will be used to fabricate electronic devices in which the carrier s mobility is crucial, we recommend to design them along the surface of the terraces present on the samples. These terraces are easily distinguished under an optical microscope even if the sample is covered with PMMA. The graphene film on SiC shows its best performance, especially in terms of carries mobility, if the electric device (e.g. Hall bar) is located on top of a single terrace. If you fabricate your device perpendicular to these terraces and the electrical current will compulsorily cross the step edge of one or more of those terraces, the mobility value can be reduced and quantum effects (e.g. Quantum Hall Effect) might not be observed [1]. [1] Anisotropic quantum Hall effect in epitaxial graphene on stepped SiC surfaces, T. Schumann, K.-J. Friedland, M. H. Oliveira Jr., A. Tahraoui, J. M. J. Lopes and H. Riechert, PRB 85, (2012).
3 ADDITIONAL INFORMATION / TECHINCAL DATA: 1. Optical Microscopy: Figure 1: Optical microscopy image of graphene grown on the Si-face of SiC. The typical terraces of such samples are clearly observed. Figure 2: Statistical study of the width of the terraces on a representative area of 200 x 250 µm 2 of a graphene film grown on the Si-face of SiC. Most of the terraces have a width between (6 10) ± 2 µm.
4 2. Atomic Force Microscopy (AFM): Figure 3: Atomic Force Microscope topography image of graphene on Si-face of SiC. The width of the terraces as well as the step height can be estimated by using the scale bar located on the right-hand side of the figure. Figure 4: Profile of a line taken from an AFM-topography image. The step height of the terraces is better analyzed by using this type of data. As shown in the figure, a step height between (8 18) ± 2 nm is observed. Terrace width Step Height (2 18) ± 2 µm (8-18) ± 2 nm Table 1: Relevant parameters of the topography of the samples.
5 Intensity Normal (a.u.) 3. Raman Analysis: Raman Shift (1/cm) Figure 5: Typical Raman spectrum measured on graphene on the Si-face of SiC. The two main characteristic peaks of graphene, i.e. G and 2D, are clearly observed. Note that the intensity of the D peak at 1350 cm -1 is rather small, indicating the low density of defects of the samples. All the other peaks shown in the graph do not correspond to the characteristics of the graphene films, but instead, to the contribution of the substrate. In order to better observe the graphene characteristic peaks, especially the G peak, the contribution of a bare SiC substrate have been subtracted from the spectrum measured on a sample with graphene. However, the presence of the so-called buffer layer, might slightly modify the typical spectra of bare SiC and therefore, even after subtraction of the SiC contribution, some extra peaks may remain. Figure 6: To the left: Optical image of an area of the sample center. Note the presence of several terraces. To the rigth: Mapping of the FWHM of the 2D peak obtained after the analysis of the single spectra measured in every micron on the selected area (inside the red box on the optical image). The blue line correspond to 2 µm. Taking into account the scale bar to the right, dark couloured regions present 2D peaks of FWHM of ~25 cm -1 and on the bright areas FWHM of the 2D peak is ~45 cm -1. Consequently, only the yellow dots correspond to the points where graphene can not be found, and
6 Intensity Normal (a.u.) bilayer graphene is observed. As expected, the presence of bilayer matches the position of the step edges of some terraces (as seen in the optical image to the right). All the rest of the surface is covered by high quality graphene film. In case, more information is needed here one can see some more examples of single spectra measured at different positions of the investigated area: Raman Shift (1/cm) Figure 7: Raman spectra measured at the position indicated by the crosses on the optical image on the right-hand side of the figure. The red dots on the graph correspond to the data collected at the position indicated by the red cross on the optical image. The same correspondence applies to the rest of the colors. The small variations observed from spectrum to spectrum on the graph points out the homogeneity of the samples, as already seen in the mapping of the FWHM of the 2D peak (see Fig. 6). 4. Transport Measurements: Figure 8: Scanning Electron Microscopy (SEM) image of a Hall bar patterned on a graphene film grown on the Si-face of SiC. The dark area on the image corresponds to the presence of graphene and the squared-shaped areas in relief are the metallic contacts attached the Hall bar structure. The rest of the surface is simply the SiC substrate. These types of micro-structures are typically used to determine the relevant parameters of graphene for its use in electronics, i.e. carrier type, carrier density and carrier mobility.
7 R xx (h/e 2 ) R xy (h/e 2 ) 0,04 0,4 0,03 0,3 0,02 0,2 0,01 0,1 0, Mangetic Field B (T) Figure 9: Data measured at 2K on a Hall bar structure of graphene on the Si-face of SiC, as the one shown in Fig. 8. The Shubnikov-de Haas (SdH) oscillations are visible at low magnetic fields (~ 2T) in the linear resistance (black dots). The quantum Hall effect is observed as well at low magnetic fields (the first plateau seems to start at ~ 3T). Both observations indicate the high quality of the graphene film. 0,0 Sheet Resistance Carrier type Carrier Density Carrier Mobility at RT 350 Ω Electrons cm cm 2 V -1 s -1 Table 3: Values of the relevant electronic parameters of the graphene film 5. High Resolution Transmission Electron Microscopy (HRTEM): Figure 10: Cross-section HRTEM image of graphene on SiC. The crystalline structure of SiC is clearly observed, as well as, the single layer of graphene and the buffer layer existing between SiC and graphene. The amorphous structure observed above graphene correspond to the platinum deposition required to protect the graphene film during the TEM lamella sample preparation process.
8 Transmittance (%) 6. Transmittance: SiC SiC+Graphene Graphene Wavelenght (nm) Figure 11: Transmittance measurements as function of wavelength for two different substrates of which an area of 50 mm 2 have been illuminated. Black squares correspond to the results obtained on a bare 4H-SiC substrate and red dots to a graphene-covered 4H-SiC substrate. The blue triangles are the result of the subtraction of the data obtained from the SiC substrate and the graphene on SiC data. Hence, the blue triangles represent the transmittance of the graphene film. Transmittance bare SiC Transmittance SiC + Graphene Transmittance Graphene ~ 67% ~ 64,5% ~ 96,5 Table 4: Transmittance values derived from the data shown in Fig. 11
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