Synthesis, Characterization, and Photodetector Application of Alkali

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Synthesis, Characterization and Photodetector Application of Alkali Metal Bismuth Chalcogenide Nanocrystals Chi Yang, Zenghua Wang, Yihui Wu, Yinhua Lv, Bin Zhou, and Wen-Hua Zhang ACS Appl. Energy Mater., Just Accepted Manuscript • DOI: 10.1021/acsaem.8b01640 • Publication Date (Web): 21 Dec 2018 Downloaded from http://pubs.acs.org on December 21, 2018

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is published by the American Chemical Society. 1155 Sixteenth Street N.W., Washington, DC 20036 Published by American Chemical Society. Copyright © American Chemical Society. However, no copyright claim is made to original U.S. Government works, or works produced by employees of any Commonwealth realm Crown government in the course of their duties.

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ACS Applied Energy Materials

Synthesis, Characterization and Photodetector Application

of

Alkali

Metal

Bismuth

Chalcogenide Nanocrystals Chi Yang,a Zenghua Wang,a Yihui Wu, a Yinhua Lv,a Bin Zhou,a Wen-Hua Zhanga* aSichuan

Research Center of New Materials, Institute of Chemical Materials, China

Academy of Engineering Physics, 596 Yinhe Road, Shuangliu, Chengdu 610200, China

*E-mail: [email protected]

1

ACS Paragon Plus Environment

ACS Applied Energy Materials 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60

ABSTRACT. We exploited a facile solution approach to synthesize a series of high-quality, abundant and nontoxic bismuth ternary chalcogenides with the formula of ABiX2 (A= Na, K, or Cs, and X = S or Se) nanocrystals (NCs), achieving the first successful synthesis of KBiS2 nanoparticles, KBiSe2 and CsBiS2 nanoplatelets. The as-prepared NCs exhibit narrow size distributions, exceptional air stability, and strong absorption in the range from visible to near infrared. The photodetector based on the ABiX2 NCs display good photoresponse and reproducibility in the visible range under monochromatic visible light at different wavelengths. The KBiS2 nanoparticle-based device demonstrates the best photoresponse property under a 525 nm laser illumination: a detectivity of approximately 5.1×1015 Jones, a high current on/off ratio of approximately 40, and photoresponse times of 120 ms (rise time) and 220 ms (fall time), respectively. These results indicate that ABiX2 NCs are potential candidates for use in new multifunctional photoelectronic devices.

KEYWORDS. Semiconductor nanocrystal, Abundant, Nontoxic, Solution synthesis, Ligand exchange, Photodetectors, High detectivity.

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Recently, ABX3-based lead halide perovskites, namely CsPbI3 and CH3NH3PbI3, have attracted intensive research interest because of their potential applications in photodetectors,1-4 solar cells,5-7 light-emitting diodes (LEDs)8-10 and so forth. However, the toxicity of lead and the chemical instability of these materials severely limit their mass application. This has highly motivated the search for new materials that are inexpensive and environmentally benign semiconductors. Alkali metal-based compounds ABiX2 (A = Na, K, Cs; X = S, Se) cater for the above requirements. Prior to the 1990s, alkali metal-based compounds ABiX2 were synthesized by the direct interaction of an alkali metal with bismuth and either sulfur or selenium at high temperatures in the 600-900 °C range11-12 by molten salt approach with a long reaction time ( as long as 8-9 days). Very few successes have been reported on the synthesis of NaBiX2 powders via solvothermal method.13-15 To date, no study on the solution synthesis of bulk materials, let alone on the well-defined nanostructures of KBiS2 and KBiSe2 materials, has been reported, hindering the understanding of their fundamental properties and assessment of their application potentials. Most recently, Vela et al.16 reported the synthesis of NaBiS2 and NaBiSe2 nanoparticles (NPs) using NaH/sodium oleate and Ph3Bi/bismuth (III) neodecanoate as the precursors. However, many more mild reagents need to be explored for the synthesis of ABiX2 (A = Na, K or Cs, X = S or Se) NCs. Herein, we present a facile synthesis of alkali metal bismuth-based ternary chalcogenide ABiX2 NCs using relatively common and very easily available compounds (including NaOH, KOH, Cs2CO3 and Bi(OH)3) as the precursors via the hot-injection colloidal chemistry, achieving the first successful synthesis of KBiS2 3



nanoparticles, KBiSe2 and CsBiS2 nanoplatelets.17-19 A series of high-quality ABiX2 nanocrystals (NaBiS2, NaBiSe2, KBiS2, KBiSe2 and CsBiS2) with narrow size distributions were synthesized, through a careful selection of sulfide and metal precursors, and the controlling of the reaction conditions. The as-prepared ABiX2 NCs exhibit an exceptional air stability and strong absorption in the range from visible to near infrared, allowing us to explore their potential applications in the photoelectronic devices. The photodetectors based on the as-prepared NCs show good photoresponse in the visible range. Specifically, the photodetector devices made of KBiS2 NCs display a high detectivity of ~ 5.1×1015 Jones, a current on/off ratio of ~40, and fast photoresponse times of 120 ms (rise time) and 220 ms (fall time), respectively, demonstrating the promise of the alkali-based ABiX2 NCs for applications in multifunctional photoelectronic devices.

Figure 1. XRD patterns of the ABiX2 NCs. (a)-(e) show the patterns for the NaBiS2, KBiS2, NaBiSe2, KBiSe2, and CsBiS2 NCs, respectively. 4


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Figure 2. TEM analysis of the ABiX2 NCs. (a)-(e) show the corresponding low-resolution TEM (1), high-resolution TEM images (2), and SAED patterns (3) of the NaBiS2, KBiS2, NaBiSe2, KBiSe2, and CsBiS2 NCs, respectively. The XRD patterns of the as-prepared ABiX2 (A = Na, K or Cs, X = S or Se) NCs were shown in Figure 1. The peak broadening of the NCs is characteristic of a nanoscale material. As shown in Figure 1a-d, all diffraction peaks of the NCs match perfectly with the major peaks of the ABiX2 (A = Na or K, X = S or Se) cubic structure, and no impurity peaks were observed. These results confirm the high purity of the NCs obtained in this work. Notably, the crystal structure of CsBiS2 is different from the above-mentioned NCs 5



as shown in Figure 1e, and the major diffraction peaks are indexed to the γ-CsBiS2 structure reported in the literature (JCPDS No 49-1339).20 The nanoparticles sizes of the NaBiS2, KBiS2 and NaBiSe2 calculated using the Scherrer equation are about 6.1 nm, 8.2 nm and 14.7 nm for the spherical polyhedral, respectively. Furthermore, X-ray photoelectron spectroscopies (XPS) show that Na 1s, K 2p, Cs 3d, Bi 4f, S 2p and Se 3d surface species are present in the ABiX2 nanoparticles respectively (see Figure S1). These results demonstrate that these pure phase ABiX2 (A = Na, K or Cs, X = S or Se) NCs with highly crystalline structures have been successfully synthesized by the hot-injection solution method. Transmission electron microscopy (TEM) was used to further reveal the nanostructures of these ABiX2 (A = Na, K or Cs, X = S or Se) NCs. The low-resolution TEM images shown in Figure 2a-c display uniform nanoparticles with narrow size distributions of 5.7 ± 0.7 nm, 7.4 ± 0.9 nm, and 13.4 ± 1.7 nm for the NaBiS2, NaBiSe2, and KBiS2 NPs (Figure S2) respectively, which are consistent with the crystalline size estimated from XRD. Moreover, KBiSe2 and CsBiS2 NCs (Figure 2d-e) present a nanoplatelets (NPLs) morphology with the lateral dimensions of approximately ~100 nm and the thickness of ~18 nm and ~10 nm (Figure S3), respectively. The polycrystalline selected area electron diffraction (SAED) patterns of these nanocrystals are presented in Figure 2a-e, showing clear diffraction rings well matched with the respective lattice planes of the ABiX2 structures (A = Na, K or Cs, X = S or Se). These results are in accordance with the XRD results. High-resolution transmission electron microscopy (HRTEM) images (Figure 2a-e-2) show that all of the ABiX2 NCs are monocrystal due to continuous lattice fringes across each nanocrystal. The 6


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HRTEM images of the NaBiS2, NaBiSe2, and KBiS2 reveal the d-spacings of 0.29 nm, 0.30 nm, and 0.30 nm, respectively, indexed as the (200) plane for each cubic structure, whereas the KBiSe2 NPL in Figure 2d-2 shows a 0.35 nm d-spacing that matches the (111) plane of cubic KBiSe2. The CsBiS2 NPL (Figure 2e-2) displays a 0.32 nm d-spacing that matches the XRD result. The chemical compositions of the ABiX2 NCs were analyzed by energy dispersive X-ray spectroscopy (EDS). The as-obtained A/Bi/X atomic ratios in the samples are closed to the nominal compositions of ABiX2, as shown in Figure S4. Therefore, we have successfully synthesized a series of highly crystalline ABiX2 (A = Na, K or Cs, X = S or Se) NCs with narrow size distributions. UV-vis-NIR absorption spectra of the as-prepared NCs were acquired to study their optical properties. As shown in Figure 3a, clear solutions of the NaBiS2 and KBiS2 NPs show continuous absorption in the whole range of visible to near infrared. Tauc plots were used to evaluate the band gap energies (Eg) by plotting the relationship of α2 (absorption coefficient) versus photon energy. Direct optical band gaps of 1.41 eV and 1.61 eV were found for the NaBiS2 and KBiS2 NPs, respectively (Figure 3b). As shown in Figure S5a-b, direct band gaps of 1.31 eV and 1.40 eV were observed for the NaBiSe2 and KBiSe2 NCs. Due to the poor dispersion of CsBiS2 NPLs in hexane or toluene, its band gap of 1.17 eV was determined using the diffuse reflection spectroscopy (Figure S5c). The band gaps of NaBiS2, NaBiSe2, and CsBiS2 NCs found in this work are in rough agreement with the previously reported direct band gaps of 1.40 eV, 1.22 eV and 1.11 eV for NaBiS2, NaBiSe2, and γ-CsBiS2, respectively.16, 20-22 However, there are no reports on the optical properties of KBiS2 and KBiSe2 in the literature, and therefore, comparison with other reports is not 7



possible.12 Gabrel’yan et al.22 presented the calculated band gap energy of KBiS2 with experimental lattice parameter to be 1.22 eV which is smaller than the band gap of the KBiS2 NPs obtained in our work. The above properties make these materials promising candidates for advanced photoelectronic devices such as solar cells and photodetectors.

Figure 3. (a) UV-vis-NIR absorption spectra of NaBiS2 and KBiS2 NPs dispersed in hexane. The plot (b) of α2 versus the photon energy. The ability to make high-quality, stable colloidal ABiX2 NCs allows us to systematically investigate their photoelectronic applications namely photodetectors. The NC-based photodetectors are fabricated by using the as-synthesized NaBiS2, KBiS2 NPs and CsBiS2 NPLs as the photoelectrodes, and the photodetector devices are fabricated on ITO substrates via a facile drop-deposition process. The presence of surface ligands of NCs has a direct and important effect on film conductivity.23-24 Charge transport in the NC film occurs by ligand assisted NC to NC tunneling. Thus it is strongly dependent on the separation of NCs that in turn is controlled by the length of the capping ligands.25 The 8


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long-chain oleic acid (OA) and oleylamine (OLA) ligands act as a tunneling barrier, resulting in a weak coupling between the individual NCs because the wavefunction of charge carriers in each nanocrystal remains availably localized in the NC. To address this issue, the poorly conductive OA/OLA-capped NC films should be chemically replaced with the shorter ligands in order to promote the conductivity. This can improve the coupling of charge carrier wavefunctions between the NCs, thus increase the charge carrier tunneling rate.

Figure 4. Photoelectrical performance of the photodetectors made of the KBiS2 NPs. (a) A schematic diagram of the device structure. (b). I-V curves of the photodetectors in the dark and under a 525 nm laser illumination with different power densities. (c) Time-dependent photoresponse under a 525 nm laser illumination with the 3 mW/cm2 intensity at a bias voltage of 1 V. (d) Normalized photoresponse used to extract the rise and decay times.

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Therefore, ligand exchange of these NCs has been carried out based on lead halide precursor with sub-molar amounts of ammonium acetate assisting the colloidal stabilization (PbX2/AA exchange) (shown in the Supporting Information). And smooth film morphologies were obtained using this procedure.26 Fourier transform infrared spectroscopy (FTIR) was used to probe the ligand exchange process. As shown in Figure S6, the presence of carboxylic acid (-COO-) moieties, amine (-NH2), and aliphatic hydrocarbon chains are corresponding to the OA and OLA groups. And after ligand exchange, the peak intensities of -NH2 and -COO- were significantly weakened. These results suggested that OA and OLA might still exist on the NCs surface, but most of them were exchanged. Figure 4a shows a schematic illustration of photodetector. The current-voltage (I-V) curves of the KBiS2 NC-based photodetectors measured under dark conditions and under various illumination power densities (from 0.02 mW/cm2 to 3 mW/cm2) using monochromatic visible light irradiation at different wavelengths (Figure 4b for the 525 nm laser and Figure S7 for the 365 nm and 760 nm lasers), and the NaBiS2 and CsBiS2 NC-based photodetectors performance characteristics are shown in Figure S8 and Figure S9. The photocurrent is proportional to the illumination power intensity, which agrees well with the fact that the charge carrier photogeneration efficiency is proportional to the absorbed photon flux. The KBiS2 NPs-based photodetectors have the best photoresponse. Figure 4b presents the dark current of only 21 pA under a 4 V bias. The photocurrent is as high as 852 pA at the same bias when the 3 mW/cm2 laser is turned on. The stable and repeatable current on/off ratio is calculated to be >40. Hence, a relatively high 10


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light-switching performance is obtained for the as-prepared device. To reveal the light-switching characteristics, the current under illumination and dark is controlled by a laser controller.27 When the laser is turned on, the current is rapidly increased with the increase of bias voltage shown in Figure 4c. And the devices generate photocurrent rapidly with the reproducible responses to light on/off cycles. To gain quantitative information for the rise and fall features of the photocurrent under dark and illumination, the rise time (τr) is defined as the time required to reach 90% of the maximum photocurrent and the fall time (τf) is defined as the time required to drop to 10% of the maximum photocurrent, respectively.28 τr ∼120 ms and τf ∼220 ms are estimated for the KBiS2 NCs-formed device, as shown in Figure 4d. The responsivity (R) of the photodetector reveals how efficient the photodetector responds to the light signal, which is defined as the ratio of photocurrent to light intensity of incident. The responsivity can be expressed by the formula R = Iph/(PA), where Iph is the difference between the illuminated and dark current, P is the irradiance power density, and A is the effective illuminated area. Based on the formula, the responsivity of the device is achieved 6.2 mA/W under the illumination power density of 0.02 mW/cm2 (shown in Figure S7d). Moreover, the detectivity (D*) of photodetector that responds to weak optical signals is also especially important.29-30 It is observed from Figure S7d-e that the change trend of the detectivity with the light power intensity is similar to the spectral responsivity. The maximum detectivity values measured under the 525 nm lasers illumination is D*525 nm = 5.1 × 1015 Jones. The remarkable photoresponse characteristics can be attributed to the high crystal quality and well-passivated surface of the KBiS2 NPs. These results demonstrate that the KBiS2 NP-based photodetectors have a 11



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stable and fast response to light illumination, making these materials promising candidates for use in novel multifunctional photoelectronic devices. In summary, we present a facile solution synthesis of the ABiX2 (A = Na, K or Cs, X = S or Se) NCs via the hot-injection method, and in particular, KBiS2 and KBiSe2 are solution-synthesized for the first time. Among these materials, the NaBiS2, KBiS2, and NaBiSe2 NCs show nanoparticles with the average sizes of 5.7 nm, 7.4 nm, and 13.4 nm, respectively, whereas the KBiSe2 and CsBiS2 NCs are NPLs with the thickness of ~18 nm and ~10 nm, respectively. These ABiX2 NCs with narrow size distributions exhibit exceptional air stability and strong absorption in the whole visible to near infrared range. The NaBiS2, KBiS2 NPs, and CsBiS2 NPLs have the band gaps of 1.41 eV, 1.61 eV, and 1.17 eV, respectively. Meanwhile, high performance photodetectors were fabricated based on the corresponding NCs. These photodetectors show good photoresponse in the visible range. For the KBiS2 nanoparticle-based devices, the best photoresponse property achieved under the 525 nm laser illumination: detectivity of approximately 5.1 × 1015 Jones, a current on/off ratio of approximately 40, and photoresponse times of τr ∼120 ms and τf ∼220 ms, respectively. All of the results indicate that ABiX2 NCs prepared by the colloidal solution

method

have

enormous

potential

for

applications

in

multifunctional

photoelectronics devices. ASSOCIATED CONTENT Supporting Information. The Supporting Information is available free of charge. Experimental section, XPS, size distributions of NPs, EDS, UV-vis absorption spectra, 12


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FTIR, the I-V curves and current on/off ratio of the NCs based photodetectors. AUTHOR INFORMATION Corresponding Authors Email: [email protected] Notes The authors declare no competing financial interests. ACKNOWLEDGMENTS This work was supported by the National Natural Science Foundation of China (Grant No. 21773218), Post-doctoral Foundation of China (Grant No. 2016M592707), key research and development projects of Sichuan Province (Grant No. 2017GZ0052), and Anshan Hifichem Co. Ltd.

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Synthesis, Characterization, and Photodetector Application of Alkali

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