Two-Dimensional (C 4 H 9 NH 3 ) 2 PbBr 4 Perovskite Crystals for. High-Performance Photodetector. Supporting Information for
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1 Supporting Information for Two-Dimensional (C 4 H 9 NH 3 ) 2 PbBr 4 Perovskite Crystals for High-Performance Photodetector Zhenjun Tan,,ǁ, Yue Wu,ǁ, Hao Hong, Jianbo Yin, Jincan Zhang,, Li Lin, Mingzhan Wang, Xiao Sun,, Luzhao Sun,, Yucheng Huang, Kaihui Liu, Zhongfan Liu,*, and Hailin Peng,* Center for Nanochemistry, Beijing Science and Engineering Center for Nanocarbons, Beijing National Laboratory for Molecular Sciences, College of Chemistry and Molecular Engineering, Peking University, Beijing , P.R. China Academy for Advanced Interdisciplinary Studies, Peking University, Beijing , P. R. China State Key Laboratory for Mesoscopic Physics, School of Physics, Peking University, Beijing , P. R. China ǁ These authors contributed equally to this work. *To whom correspondence should be addressed. hlpeng@pku.edu.cn; zfliu@pku.edu.cn; Page S1
2 Synthesis and Characterization of the 2D Hybrid Perovskites Synthesis of C 4 H 9 NH 3 Br precursor First, 10 ml n-butylamine was added into 20 ml methanol solvent in a 250 ml round bottom flask. Then, 10 ml HBr aqueous solution ( 45 wt%) was dropwise added into the flask and the mixture was maintained at 0 o C with strong stirring. Then the mixture was stirred under room temperature for about three hours. Subsequently, crude oil-like product was obtained by evaporating the solvent in a rotatory evaporator at 60 o C. Then the crude product was washed by anhydrous diethyl ether three times. After the recrystallization and filtration, the pure white product, C 4 H 9 NH 3 Br, was collected and dried at 50 o C in vacuum for 24h. Synthesis of 2D perovskite (C 4 H 9 NH 3 ) 2 PbBr 4 nanoplates First, 1 mmol as-prepared C 4 H 9 NH 3 Br and 0.5 mmol PbBr 2 were dissolved in the co-solvent of DMF/chlorobenzene (CB) (volume ratio 1:1) in a beaker flask. Then the solution was transferred into a 100 ml volumetric flask and diluted into 5 mmol/l (C 4 H 9 NH 3 ) 2 PbBr 4 solution with 1:1 DMF/CB. The solution was further diluted into an appropriate concentration (typically mmol/l) by CB/acetonitrile ( volume ratio 2:1). (C 4 H 9 NH 3 ) 2 PbBr 4 nanoplates were grown on 300 nm SiO 2 /Si substrates. The growth process was carried out in a glove box. 10 µl diluted (C 4 H 9 NH 3 ) 2 PbBr 4 solution was dropped onto SiO 2 /Si substrates and dried naturally under room temperature. After the solvent evaporated, highly crystalline (C 4 H 9 NH 3 ) 2 PbBr 4 nanoplates were synthesized on the substrate. Note: SiO 2 /Si substrates were sequentially cleaned by ultrasonication in water, isopropanol, acetone and isopropanol for 5 min. Characterization of 2D perovskite (C 4 H 9 NH 3 ) 2 PbBr 4 Characterizations were carried out on optical microscopy (Olympus DX5r1 microscope), SEM (Hitachi S-4800, acceleration voltage 1 ~10 kv), TEM (FEI Tecnai T20, acceleration voltage 80 kv), AFM (Bruker Dimension Icon) and X-ray diffraction (XRD) (Bruker D8 Advance diffractometer in modified Debye-Scherrer geometry, using a CuK α1 radiation). Page S2
3 Figure S1. Optical images for 2D (C 4 H 9 NH 3 ) 2 PbBr 4 crystals grown on different substrates. (a) The as-grown (C 4 H 9 NH 3 ) 2 PbBr 4 on fused silica. (b) The as-grown (C 4 H 9 NH 3 ) 2 PbBr 4 on 300 nm SiO 2 /Silicon. Scale bar: 20 µm. Figure S2. AFM characterization for 2D (C 4 H 9 NH 3 ) 2 PbBr 4 perovskite crystals grown on silicon. (a) Typical AFM image shows the thickness distribution of as-grown 2D (C 4 H 9 NH 3 ) 2 PbBr 4 perovskite crystals. Scale bar: 4 µm. (b, c) AFM images of the thicker (b) and thinner (c) sample, respectively. Scale bars: 2 µm. (d) The thickness of monolayer is about 1.4 nm (extracted from the step). Scale bar: 2 µm. Page S3
4 Figure S3. X-ray diffraction pattern of the as-grown (C 4 H 9 NH 3 ) 2 PbBr 4. A relatively highly concentrated solution was used to grow thick and dense sample on the substrate to highlight the sample signals. Figure S4. (a) SEM image of the square-shaped 2D perovskites nanoplates. Scale bar: 50 µm. (b) EDS mapping of the as-grown 2D crystal, showing the uniform elemental distribution of lead, bromide, nitrogen, and, carbon respectively. All scale bars: 1 µm. Page S4
5 Growth of Square Single-Crystalline Graphene Single-crystal graphene with square shape were grown on copper foil (99.8% purity, 25 µm thick, Alfa Aesar) in a low pressure chemical vapor deposition (CVD) system using a horizontal tube furnace (Lindberg Blue M TF55035KC-1) equipped with a 1-inch-diameter quartz tube. Double-face polished copper foils were loaded in the hot center of the furnace. First the copper foils were annealed at 1035 for 60 min without gas pumped in (~1 Pa). Then 200 sccm H 2 (~320 Pa) and 1 sccm CH 4 (~12 Pa) were introduced to grow single crystal graphene for 4 min. Finally, the sample was rapidly pulled out from the high-temperature zone to room-temperature zone using a magnet without changing the gas flow. Figure S5. (a) The procedure for square graphene growth in low pressure CVD. (b) The SEM image for as-grown square-shape graphene on copper. Scale bar, 200 µm. Page S5
6 Dry Transfer Process As-grown single-crystal graphene with PMMA supporting layer was dry transferred onto as-prepared 2D perovskites samples. The dry transfer procedure was used to avoid the p-type doping caused by the adsorption of H 2 O and O 2. The detailed process is as below: 1. PMMA (966K 4% ethyl lactate) was spun onto Graphene/Copper (2000 r/min). Then, graphene on the backside was removed by oxygen plasma while a thin plastic box was affixed to support the PMMA. Na 2 S 2 O 8 (1 mol/l) solution was used to thoroughly etch the Cu. The graphene/pmma film detached from the copper foil was cleaned sequentially in deionized (DI) water, isopropanol and then dried in air for 6 h before it was placed onto 2D perovskites/substrate. 2. 2D perovskites on silicon were placed on a heater (60 o C) and the as-prepared PMMA/graphene were rapidly put onto the silicon. After several minutes baking, the plastic box was peeled off. 3. Finally, the PMMA was removed in boiling acetone vapor and isopropanol sequentially. The graphene encapsulated 2D perovskites were obtained. Page S6
7 Figure S6. Schematic illustration of dry transfer process. Figure S7. The protection of graphene. (a) The optical image of 2D perovskites before transfer. (b) The in-situ comparison after sequentially soaking in acetone and water. Scale bar, 100 µm. Page S7
8 Device Fabrication The graphene encapsulated 2D perovskites were successfully fabricated into nano devices. In order to avoid the damages of 2D perovskites in electron beam lithography (EBL) and lifting off process, a specific procession sequence is designed for building photodetectors with graphene electrodes. The step by step process is as below (as shown in figure S8a). Step 1 Suitable graphene/2d perovskites samples were selected under optical microscope. Step 2 The metal electrodes pattern was obtained after the first electron beam lithography (EBL). Step 3 8 nm Cr/40 nm Au were thermally evaporated followed by lifting off process. The acetone wouldn t dissolve the 2D perovskites in this step because of the graphene protection. Step 4 The device channel pattern was obtained after the second EBL. Step 5 The graphene-protective layer was sacrificed for the formation of graphene electrodes by oxygen plasma cutting-out of 100 nm narrow channel. Step 6 Another layer of PMMA was spun on the whole device for further encapsulation. Finally, the encapsulated device is conducted for measurement. Page S8
9 With single-crystalline graphene acting as a protective layer, the 2D perovskite crystals avoid direct contact with acetone during the whole micro-fabrication process. We found that the 2D perovskite crystals protected by graphene were all in good condition, while the others without the protection of graphene would not survive, as shown in figure S8b. Figure S8. (a) The step-by-step fabrication process for 2D perovskite crystal devices. Scale bar, 4 µm. (b) The optical image for samples after the whole fabrication, showing the perfect protection effect of graphene. Scale bar, 150 µm. Page S9
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