Wide-gap Semiconducting Graphene from Nitrogen-seeded SiC

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1 Wide-gap Semiconducting Graphene from Nitrogen-seeded SiC F. Wang, 1 G. Liu, 2 S. Rothwell, 3 M. Nevius, 1 A. Tejeda, 4, 5 A. Taleb-Ibrahimi, 6 L.C. Feldman, 2 P.I. Cohen, 3 and E.H. Conrad 1 1 School of Physics, The Georgia Institute of Technology, Atlanta, Georgia , USA 2 Institute for Advanced Materials Devices and Nanotechnology, Rutgers University, Piscataway, New Jersey Department of Electrical and Computer Engineering, University of Minnesota, Minneapolis, Minnesota Institut Jean Lamour, CNRS - Univ. de Nancy - UPV-Metz, Vandoeuvre les Nancy, France 5 Synchrotron SOLEIL, L Orme des Merisiers, Saint-Aubin, Gif sur Yvette, France 6 UR1 CNRS/Synchrotron SOLEIL, Saint-Aubin, Gif sur Yvette, France 1

2 Pre-growth Nitrogen preparation Graphene was grown from a starting nitrogen-submonolayer covered SiC surface. Graphene will grow at temperatures as low as 1100 C on the (000 1) (C-face) surface. 1 However, the best graphene is grown at higher temperatures (usually 1550 C ) in a near equilibrium Si flux that is sustained in the CSS furnace. 2 In order to maintained a significant nitrogen concentration during growth, we have adjusted the growth temperature to be slightly higher than the desorption temperature of nitrogen on the bare SiC surface. The nitrogen coverage as a function of temperature for C-face SiC is shown in Fig. 1. FIG. 1. N1s and O1s XPS intensity vs temperature for a SiC C-face nitrogen-seeded surface. The nitrogen on the C-face is stable up to at least 1400 C. The apparent increase in nitrogen above 1100 C is due to an oxide attenuating the photoelectrons. This oxide desorbs around 1100 C. 1 C-face graphene can grow as low as 1100 C in UHV, 1 but is typically grown in the closed CSS furnace as 1550 C. 2 For these studies we have adjusted the Si-leak rate in the CSS furnace to grow graphene at 1450 C on the C-face of SiC. This temperature is near the onset of the loss of surface nitrogen. Nitrogen Site Assignments After graphene growth the N 1s line resolves into two lines denoted as N S and N P as shown in the insert in Fig. 1(d). Identification of the binding configuration and atomic site of these lines is based on a large number of studies of bulk N-doped SiC and, more recently, surface/interface assignments. 2

3 As early as 1961 Electron Spin Resonance studies 3 indicated that nitrogen occupies the carbon site in bulk SiC. That is, the N is bound to four Si nearest neighbors and is an n-type dopant. Numerous XPS studies of Si 3 N 4 have reported N binding energy values in the range. A typical example is the work of Chourasia and Chopra 4 who report a value of 397.8eV for CVD grown Si 3 N 4 films. In a very extensive study of the SiO 2 /N/SiC (Si-face) interface, Tochihhara and Shirasawa report a N 1s line position of 398.7ev (and a C 1s binding energy for C in SiC of 283.9ev). 5 This model includes N bound to Si atoms at a surface C site where the Si-N bond length with N at a carbon site was determined to be very close to the bond length in Si 3 N 4. The model in Ref. [5] was supported by a large variety of data including quantitative low energy electron diffraction, scanning tunneling microscopy, Auger electron spectroscopy, surface x-ray diffraction, and first principle calculations. Additional recent reports by Kosugi et al. 6 using the same NO process described in this current work report a N 1s binding energy of 398.2ev and note that the N is resistant to HF etching. Similar results, particularly addressing the role of surface deposited N as a dopant are reported by Liu et al. 7 To calibrate these earlier studies with the work reported here, we use the binding energy difference between the N 1s and C 1s in SiC, E N-C. This is found to be E N-C =115.0±0.2eV in all cases, exactly what is measured in the studies reported here for the N S state of Fig. 1d of the main text. In short we assign the N S state to N at a C site, bonded to 3 or 4 Si atoms at the SiC interface. To identify the N P site, we have look at previous work on N-C bonds. There are relatively few studies of C 3 N 8 4 but in the cases reported, the energy difference E N-C 133.7±0.2eV (where the carbon reference is to C in C 3 N 4 ). In this work the experimental E N-C for the N P site is ev. This strongly suggests that the N P site is nitrogen bonded to 3 carbon atoms. We therefore suggest a model where /cm 2 N S atoms are substituted in the C plane of the interface layer of SiC and /cm 2 N P atoms are bonded to carbon providing the attachment between graphene and SiC. Raman determination of nitrogen density or graphene finite domains Raman is often used to estimate nitrogen density in graphene or to estimate finite domain size of graphene sheets. 9 In this system, these estimates do no work. Raman spectrum for the nitrogenated graphene is shown in Fig. 2. The estimated domain size, L a, is calculated from the ratio of the G- and D-peak intensities by L a = λ 4 (I G /I D ), where λ = 532nm 3

4 is the wavelength of the Raman laser. 10,11 For the spectrum in Fig. 2, this give a domain size of L a 12nm. This is approximately 9 times the XPS estimated distance between nitrogen defects and 5 times larger than the domain size measured by either ARPES or STM. The primary reason for this is that the graphene band structure has been distorted by the opening of a gap at the graphene K-point. FIG. 2. The Raman spectrum of a 3-layer graphene film with 7 at% nitrogen as determined by XPS and ellipsometry. The SiC background signal has been substracted. 1 J. Hass, W.A. de Heer and E.H. Conrad, J. Phys.: Condens. Matt. 20, (2008). 2 W.A. de Heer, C. Berger, M. Ruan, M. Sprinkle, X. Li, Y. Hu, B. Zhang, J. Hankinson, and E.H. Conrad, Proc. Nat. Acad. Sci. 108, (2011). 3 H.H. Woodbury and G W Ludwig, Phys. Rev. 124, 1083 (1961). 4 A R Chourasia and D R Chopra, Surf. Sci. Spectra 2, 117 (1994) 5 Tochihara and T. Shirasawa, Prog in Surf Sci. 86, R.Kosugi, T. Umeda and Y. Sakuma, Appl. Phys. Lett. 99, , (2011) 7 G. Liu, A.C. Ahyi, Y. Xu, T. Isaacs-Smith, Y.K. Sharma, J.R. Williams, L.C. Felman, and S. Dhar, IEEE Elec. Device Lett. 34, 181 (2013). 8 C. Ronning, H. Feldermann, R. Merk, and H. Hofsass, Phys. Rev. B 58, 2207 (1998). 9 H. Wang, T. Maiyalagan, and X. Wang, ACS Catal. 2, 781 (2012). 4

5 10 F. Tuinstra, J.L. Koenig, J. Chem. Phys. 53, 1126 (1970). 11 L.G. Cançado, K. Takai, T. Enoki, M. Endo, Y.A Kim, H. Mizusaki, A. Jorio, L.N. Coelho, R. Magalhães-Paniago, M.A. Pimenta, Appl. Phys. Lett. 88, (2006). 5

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