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1 SUPPLEMENTARY INFORMATION Facile Synthesis of High Quality Graphene Nanoribbons Liying Jiao, Xinran Wang, Georgi Diankov, Hailiang Wang & Hongjie Dai* Supplementary Information 1. Photograph of graphene nanoribbon solution. 2. Height and width distribution of the obtained nanoribbons. 3. More AFM and TEM images of nanoribbons. 4. Raman spectra, XPS data and SEM images of pristine, oxidized and unzipped multiwalled carbon nanotubes. 5. Optimization of the unzipping process. 6. Comparison of the averaged I D /I G ratio of bi-layer graphene nanoribbons made by different methods. 7. Room temperature transport measurement of bi- and tri-layer nanoribbons and the comparison of resistivity of bi-layer nanoribbons made by different methods. nature nanotechnology 1
2 supplementary information 1. Photograph of graphene nanoribbon solution. Figure S1 Photograph of our final product, graphene nanoribbons in a polymer PmPV/DCE solution. Note the yellow color mostly was due to the color of PmPV. 2. Height and width distribution of the obtained nanoribbons. Figure S2 a and b, Height and width distribution of nanoribbons made by our new method of unzipping carbon nanotubes, respectively. The nanoribbons are mostly 1-3 layered based on the height data considering the PmPV residues on both sides of the ribbon (removal of polymer coating residue would reduce the height of ribbons measured by AFM, as shown in ref. 3 cited in the main text). 3. More AFM and TEM images of nanoribbons. 2 nature nanotechnology
3 supplementary information Figure S3 a, An AFM image of unzipped multiwalled carbon nanotubes deposited on SiO 2 /Si substrate. b, A zoom-in image of a part in a. The heights and widths of these two nanoribbons were 1.4 nm, 10 nm and 1.5 nm, 16 nm, from left to right. Figure S4 TEM images of nanoribbons with different widths. a, W ~15 nm, b, W ~17 nm. 4. Raman spectra, XPS data and SEM images of pristine, oxidized and unzipped multiwalled carbon nanotubes. We collected Raman data of pristine, calcined multiwalled carbon nanotubes and unzipped products in bulk. The samples were made by drop-drying the pristine, calcined and unzipped nanotubes dispersed in DCE onto SiO 2 /Si substrates to form nature nanotechnology 3
4 supplementary information thick films. All the spectra were taken with a 633 nm He-Ne laser excitation at ~1 mw for 10 s. The I D /I G ratios of these three samples were 0.20, 0.22 and 0.16, respectively (Fig. S5). After the gas-phase calcination step, the I D /I G of nanotubes did not increase, which indicated the oxidation was very mild and did not introduce new defects. The I D /I G of the unzipped products was much lower than those of bulk nanoribbons (I D /I G >1) made by unzipping in solution 1, 2 and CVD growth 3, 4, indicated higher quality of our nanoribbons. SEM images of pristine, calcined and unzipped multiwalled carbon nanotubes were taken by depositing these materials on Si substrates. No obvious difference was observed in SEM images of pristine (Fig. S7 (a)) and calcined (Fig. S7 (b)) nanotubes. Fig. S7 (c) shows the SEM image of sonicated products. The image brightness of nanoribbons and remaining nanotubes appeared obviously different. Nanoribbons (indicated by arrows) were darker than nanotubes under SEM. The inset of Fig. S7 (c) shows a nanoribbon with buckling. The percentage of nanoribbons was ~60%, which is consistent with AFM measurements. These SEM images also indicated that nanotubes were unzipped in the sonication process. Figure S5 Raman spectra of the pristine and oxidized multiwalled carbon nanotubes, 4 nature nanotechnology
5 supplementary information and the unzipped products. Figure S6 (a) XPS spectra of pristine and 500 C calcined multiwalled carbon nanotubes. The O1s peaks were very weak in both samples. (b) XPS spectra of C1s peaks of pristine and mildly oxidized nanotubes. Both peaks are single symmetric peak at ev, characteristic of sp 2 carbon. These data indicated that the 500 o C calcination was very mild without introducing many new defects. Figure S7 SEM images of pristine (a), calcined (b) and unzipped (c) multiwalled carbon nanotubes. Insets, high magnification images of tubes and nanoribbons respectively. Little difference was seen between pristine and calcined nanotubes in (a) and (b). Nanoribbons appears as dark lines in (c), which was only observed after nature nanotechnology 5
6 supplementary information sonicating calcined carbon nanotubes, suggesting unzipping occurred in the sonication step. 5. Optimization of the unzipping processes. Our method of nanoribbon formation was a simple two-step process and both steps were critical. The pits introduced by calcination made it possible to unzip the nanotubes by mechanical breaking in the sonication step. The temperature of calcination was related to the activation energies for pits growth 5 and therefore, determined the yield and quality of the obtained nanoribbons. We found 500 o C was the optimized temperature for the production of nanoribbons at a good yield. Next, we tested the sonication conditions. We sonicated the calcined nanotubes in DCE for different durations, briefly centrifuged the solution at low speed (15,000 r.p.m.) to remove the aggregates without losing many nanoribbons and then deposited the supernatant onto SiO 2 /Si substrates. The percentages of nanoribbons were < 10%, ~30% and ~40% after sonication for 0.5, 1, and 2 hrs, respectively (Fig.S8). The obvious dependence of the percentage of nanoribbons on sonication time indicated that sonication played an important role in the unzipping process. Even longer sonication degraded the quality of nanoribbons as evidenced by the increase of resistivity after sonicating for 2 hrs. We also tried other solvent and surfactants and found that DCE and PmPV were the best combination for the production of nanoribbons. To obtain higher percentage of nanoribbons, we used ultracentrifuge to further separate nanotubes from nanoribbons. The percentage of nanoribbons made by sonicating for 1 hr increased to ~60% after centrifuging at 40,000 r.p.m for 2 hrs (Fig. 6 nature nanotechnology
7 supplementary information S9). Thus, we concluded the optimized steps for the production of nanoribbons with both high yield and quality of nanoribbons: First, multiwalled carbon nanotubes were calcined in air at 500 o C for 2 hrs. After that, the calcined nanotubes were sonication for 1 hr in PmPV/DCE solution and then ultracentrifuged at 40,000 r.p.m. for 2 hrs. We also used CVD-grown multiwalled carbon nanotubes as starting materials. Some nanotubes were unzipped but the yield was low (Fig. S10) due to the low quality of nanotubes used. Figure S8 AFM images of unzipped products after sonicating for different time. a-c, 0.5, 1 and 2 hrs, respectively. nature nanotechnology 7
8 supplementary information Figure S9 AFM images of unzipped products after ultracentrifuging at different speed and time. a, 20,000 r.p.m for 1 hr. b, 30,000 r.p.m. for 1 hr. c, 40,000 r.p.m for 1 hr. d, 40,000 r.p.m. for 2 hrs. Figure S10 Unzipped CVD-grown multiwalled carbon nanotubes (made by the method reported in ref. 6). The arrow indicated a nanoribbon from a partially unzipped nanotube. 8 nature nanotechnology
9 supplementary information 6. Comparison of the averaged I D /I G of bi-layer nanoribbons made by different methods. We used the averaged I D /I G to compare the quality of our nanoribbons with nanoribbons made by various methods. Except for a few publications from our group, there were no reported Raman data of individual bi-layer nanoribbons with widths of ~20 nm. We compared the I D /I G of individual bi-layer nanoribbons made by different methods used in our group. Fig. S11 showed the Raman spectrum of a typical 20-nm-wide bi-layer nanoribbon made by lithographic patterning with an I D /I G of ~ Besides lithographic patterning, we can also produce bi-layer nanoribbons by plasma unzipping carbon nanotubes 8. The average I D /I G of ~ 20 nm wide bi-layer nanoribbons made by plasma unzipping was ~0.5. Figure S11 A typical Raman spectrum of a 20-nm-wide bi-layer nanoribbon made by lithographic patterning, showing an I D /I G of ~ Room temperature transport measurement of bi- and trilayer nanoribbons and nature nanotechnology 9
10 supplementary information the comparison of resistivity of bi-layer nanoribbons made by different methods. Figure S12 shows the typical I ds -V gs curves of bi- and tri-layer nanoribbons at room temperature in vacuum after the electrical annealing. Most of the obtained nanoribbon devices showed clear Dirac points at around 0 V after electrical annealing. We compared the room temperature resistivity of bi-layer nanoribbons with 10~30 nm widths made by different methods, including lithographic patterning 9, sonochemical 10 method and plasma unzipping 8. Figure S13 shows the typical I ds -V gs curves of bi-layer nanoribbons made by lithographic patterning 7. All the data points included in Fig. 4D were taken from literature or from data of our group. Figure S12 a, I ds -V gs curve of a 12-nm-wide bi-layer nanoribbon after electrical annealing. b, I ds -V gs curve of a 20-nm-wide tri-layer nanoribbon after electrical annealing. V ds = 100 mv, pressure: ~10-6 Torr. 10 nature nanotechnology
11 supplementary information Figure S 13 I ds -V gs curves of two bi-layer nanoribbons made by lithographic patterning, V ds = 1 mv. a, W ~27 nm, L ~310 nm. b, W ~29 nm, L ~480 nm. nature nanotechnology 11
12 supplementary information References 1. Kosynkin, D. V. et al. Longitudinal unzipping of carbon nanotubes to form graphene nanoribbons. Nature 458, (2009). 2. Cano-Marquez, A. G. et al. Ex-MWNTs: Graphene sheets and ribbons produced by lithium intercalation and exfoliation of carbon nanotubes. Nano Lett. 9, (2009). 3. Campos-Delgado, J. et al. Bulk production of a new form of sp 2 carbon: Crystalline graphene nanoribbons. Nano Lett. 8, (2008). 4. Wei, D. C. et al. Scalable synthesis of few-layer graphene ribbons with controlled morphologies by a template method and their applications in nanoelectromechanical switches. J. Am. Chem. Soc. 131, (2009). 5. Stevens, F., Kolodny, L. A. & Beebe, T. P. Kinetics of graphite oxidation: Monolayer and multilayer etch pits in HOPG studied by STM. J. Phys. Chem. B 102, (1998). 6. Zhang, X.B., et al. Spinning and processing continuous yarns from 4-inch wafer scale super-aligned carbon nanotube arrays. Adv. Mater., 18, (2006). 7. Wang, X.R., et al. unpublished data. 8. Jiao, L. Y., Zhang, L., Wang, X. R., Diankov, G. & Dai, H. J. Narrow graphene nanoribbons from carbon nanotubes. Nature 458, (2009). 9. Lin, Y. M.& Avouris, P. Strong suppression of electrical noise in bilayer graphene nanodevices. Nano Lett. 8, (2008). 10. Li, X. L. et al. Chemically derived, ultrasmooth graphene nanoribbon semiconductors. Science 319, (2008). 12 nature nanotechnology
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