Synthesis of Superlattice InSe Nanosheets with Enhanced Electronic

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Functional Inorganic Materials and Devices

Synthesis of superlattice InSe nanosheets with enhanced electronic and optoelectronic performance Wei Feng, Fanglu Qin, Miaomiao Yu, Feng Gao, Mingjin Dai, Yunxia Hu, Lifeng Wang, Juan Hou, Bin Li, and PingAn Hu ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.9b01747 • Publication Date (Web): 06 May 2019 Downloaded from http://pubs.acs.org on May 6, 2019

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ACS Applied Materials & Interfaces

Synthesis of superlattice InSe nanosheets with enhanced electronic and optoelectronic performance Wei Feng, †, ‡ Fanglu Qin, † Miaomiao Yu, † Feng Gao,§ Mingjin Dai,§ Yunxia Hu,§ Lifeng Wang, ∥

Juan Hou†, ‡, Bin Li*,†, ‡ and PingAn Hu*,§

†Department

of Chemistry and Chemical Engineering, College of Science, Northeast Forestry

University, Harbin, 150040, China ‡Post-doctoral

Mobile Research Station of Forestry Engineering, Northeast Forestry University,

Harbin 150040, China §Key

Lab of Microsystem and Microstructure of Ministry of Education, Harbin Institute of

Technology, Harbin, 150080, China ∥Institute

for Frontier Materials, Deakin University, 75 Pigdons Road, Waurn Ponds, Geelong,

Victoria 3216, Australia KEYWORDS: superlattice, InSe, field-effect transistors, photodetectors, thermal-annealing

ABSTRACT: Multilayer InSe has emerged as a promising candidate for applications in novel electronic and optoelectronic devices due to its direct bandgap, high electron mobility and excellent photoresponse with a broad response range. Here, we report synthesis of superlattice InSe nanosheets by simple thermal annealing for the first time. The mobility is increased to 299.1 cm2V-1s-1 for superlattice InSe FETs and is 4 times higher than 63.5 cm2V-1s-1 of pristine

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InSe device. The superlattice InSe photodetector shows an ultrahigh responsivity of 1.7×104 A/W (700 nm), which is 8.5 times to pristine photodetector. Superlattice InSe photodetectors hold a good photoresponse stability and rapid response time of 20 ms. The electronic and photoresponse performance improvement of superlattice InSe is attributed to higher carrier sheet density and lower contact resistance for more effective electron injection and more photogenerated carrier injection, respectively. Those results suggest that superlattice is an effective method to further improve electronic and optoelectronic properties of 2D InSe devices.


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INTRODUCTION

Two-dimensional (2D) layered semiconductors have attracted significant attention because of their greatly potential applications in next generation novel electronic and optoelectronic devices. A wealth of 2D layered semiconductors have been explored, such as transition metal dichalcogenides (TMDs: MoS21-4 and WSe25-7), black phosphorus8-10 and III-VI layered semiconductors (such as GaSe11, 12 and InSe13-16). Among these 2D layered semiconductors, InSe shows a high mobility of 104 cm2V-1s-1 and high responsivity15,

16.

Different from TMDs,

multilayer InSe owns a direct bandgap of 1.26 eV (≥ 20 nm).17 2D InSe is more stable than black phosphorus in atmospheric environment.18 These merits clarify that 2D InSe nanosheets have a huge potential applications in high performance of rigid and flexible photodetectors15, filed effect transistors (FETs)14, 16, vertical and lateral p-n heterojunctions19, 20 and image sensors21.

For designing high performance 2D materials-based electronic and optoelectronic devices, low contact resistance electrodes, trap-free interfaces between layered semiconductors and dielectric substrates, device configurations and intrinsic properties of channel materials are crucial parameters. High performance 2D electronic devices have be achieved by top-gated structure1, choosing idea contact and contact model22-28 and modified substrates3, 29. To adjust intrinsic electronic properties of semiconductors, ion doping is the most common method in modern microelectronics. However, this is challenge for 2D materials because of their atomically thin structure. The conductivity30 and photoresponse31 of 2D semiconductors can be effectively adjusted by surface modifying with molecules and ions, but those strategies suffer from longterm stability. Bandgap, conductivity and photoluminescence (PL) of 2D semiconductors can also be altered by external strain32-34. Phase-engineering is another effective tool to modulate


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conductivity and catalytic properties of 2D semiconductors via lithium intercalation35 and thermal annealed36. For 2D InSe, high performance FETs have been demonstrated with choosing contact metals and modified substrate14, 37, and high photoresponse photodetectors have been achieved using InSe/Graphene heterostructures20. Theory simulation claims that monolayer InSe transform to new phase with inversion symmetry under 25% tensile strain38. The optical gap of 2D InSe is validly regulated by strain with a shift rate of 90-100 meV per 1% strain39, indicating that 2D InSe is suitable for tunable light emitters and photodetectors. Up to date, there is no experimental reports on phase-engineering tuned electronic and optoelectronic properties of 2D InSe.

In this letter, the superstructure phase is observed in thermal annealed multilayer β-InSe nanosheets, and the electronic and optoelectronic properties of superlattice InSe nanosheets are improved by phase-engineering. The mobility of superlattice InSe FETs is 299.1 cm2V-1s-1, which is 4 times for pristine device. After thermal annealing, responsivity of superlattice multilayer InSe photodetector is calculated to be 1.7×104 A/W, which is 8.5 times larger for pristine photodetector. Superlattice photodetectors still hold a good stability and rapid response speed of 20 ms. The electronic and photoresponse performance improvement of superlattice InSe is attributed to higher carrier sheet density and lower contact resistance for more effective electron injection and more photogenerated carrier injection, respectively. The electronic and optoelectronic performance improvement of superlattice InSe devices suggests that superlattice is an powerful way to further design high performance InSe nano-devices. RESULTS AND DISCUSSION


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In this study, we focus on multilayer InSe nanosheets, because they are direct bandgap materials and have better electronic and optoelectronic performance.14, tansfers to In2Se3 or InSe1-xOx due to oxidation of InSe,40,

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In order to prevent β-InSe the pristine multilayer InSe

nanosheets were annealed at 623 K and reducing atmosphere (Ar/H2) for 30 min (more details in Suporting Information). The crystal structure of pristine and annealed multilayer InSe nanosheets were investigated by Raman spectroscopy and transmission electron microscopy (TEM). Raman is a convenient and fast characterization method to detect nanomaterials. Raman spectra of pristine and annealed multilayer InSe nanosheets are depicted in Figure 1a. Both of pristine and annealed InSe nanosheets exhibit three same Raman peaks of 116 cm-1,178 cm-1 and 226 cm-1, which are indexed to A11g, E12g and A21g modes of β-InSe. There are three polytypes of layered InSe materials, which are β, γ and ε, respectively. Different from β-InSe, there is another Raman peak of 202 cm-1 in γ and ε samples.13,

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After annealing, there is no new Raman peaks

appearing at 202 cm-1, indicating annealed InSe nanosheets still is β phase and do not transfer to γ or ε phase. This phenomenon is totally different with multilayer α-In2Se3 sample, which can transfer to β-In2Se3 under thermal annealed36. Figure 1b are PL results of pristine and annealed InSe samples. The PL peak of pristine InSe is 1.26 eV, which is consistent with early report17. After annealing, PL is drastically quenched, indicating that the microstructure of β-InSe nanosheets is modified by thermal annealing. The quenched PL of annealed InSe should arise from indirect bandgap or metallic property, and we will discuss this later. The microstructure of pristine and annealed InSe sample were investigated via selective area electron diffraction (SAED) and high resolution transmission electron microscopy (HRTEM). Figure 2a exhibits the SAED pattern of pristine InSe nanosheets. The SAED pattern demonstrates good crystallinity of pristine β-InSe sample, and hexagonal pattern indicates the


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crystal orientates along the axis, which agrees well with our early report14. The SAED pattern of annealed InSe nanosheets is shown in Figure 2b. The SAED pattern shows same main Bragg spots, indicating the lattice type remains β-type. Interestingly, there is a superstructure appearing in annealed InSe nanosheets. The superlattice is further confirmed by HRTEM image. As shown in Figure 2c, pristine InSe nanosheet reveals hexagonal lattice with a lattice spacing of 0.34 nm, which is consistent with the lattice spacing of (100) planes in the simple hexagonal phase. As shown in Figure 2d, annealed InSe nanosheet has a periodicity of 0.68 nm and one period consists of two (100) planes, which agrees well with the SAED pattern with the distance between two basic spots subdivided into two equal parts. The appearing superstructure in annealed InSe nanosheets indicates a periodic lattice distortion induced by thermal annealed, which has been observed in other layered compounds such as In2Se336, 43, 44, TaS245 and TaSe246. In order to further determine the composition of annealed InSe nanosheets, XRD, EDS and XPS were performed and the coresponding results are displayed in Figure S1. The annealed InSe nanosheets have the same XRD peaks as pristine InSe nanosheets in Figure S1a, there is no new XRD peaks appearing. The EDS results demonstate that annealed InSe nanosheets only have two elements and the element ratio of In:Se is close to 1:1, which is similar to pristine InSe. The binding energy postions of annealed InSe nanosheets do not shift and no new XPS peak appears. All above results demonstrate that annealed samples only contain InSe constituent and the annealding process do not produce new materials. Our results are totally different from early reports on InSe annealing, which is due to our annealing process is operated in reducing atmosphere (Ar/H2) and avoide oxidation of InSe. The thinkness of InSe nanosheet is measured by AFM before and after thermal annealed. The thinkness of superlattice InSe is almost as same as pristine InSe as shown in Figure S2.


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Figure 1. Characterization of pristine and annealed InSe nanosheets. (a) Raman and (b) PL spectrums of pristine and annealed InSe nanosheets.

Figure 2. Microstructure of pristine and annealed InSe nanosheets. SAED pattern of pristine (a) and annealed (b) InSe nanosheets. Insets are corresponding TEM images. HRTEM image of pristine (c) and annealed (d) InSe nanosheets.


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2D In2Se3 nanosheets with superstructure phase exhibit metallic behavior43, demonstrating that superstructure has a profound effect on electronic properties of 2D layered semiconductors. Here, back-gated FETs made of pristine and superlattice multilayer InSe nanosheets with thickness of 20-40 nm were fabricated (fabrication process in Supporting Information). Figure 3a is the 3D structure of InSe device and Figure 3b is an optical image of a InSe device with a channel length of 20 μm, channel width of 15 μm. Figure 3c is AFM image of InSe channel and the thickness is 31nm.

Figure 3. Multilayer InSe nanosheets field effect transistor. (a) 3D schematic structure of InSe FETs. (b) An optical image of InSe FETs; (c) The AFM height profile of multilayer InSe channel; Inset: the AFM image of InSe channel.

Figure 4a and 4b is electronic transfer characteristics of pristine and superlattice InSe FETs. The pristine InSe nanosheets hows n-type transport property and a large current on/off ratio of 107. After annealing, superlattice InSe nanosheets maintain n-type conductance property, but the current swithing drastically degrades with a small current on/off ratio of 2.9, which is similar to electronic property of 2D superlattices In2Se3 nanosheet43, demonstrating its metallic property. The electrical performance suggests that the quenched PL of annealed InSe is mainly ascribed to its metallic property. The mobility value of pristine InSe FETs is 63.5 cm2V-1s-1 calculated from Figure 4b, which is consistent with our early report41(more calculated details in Supporting Information). After annealing, the mobility value is increased to be 299.1 cm2V-1s-1, which is 4 times


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for pristine InSe FETs. This result further demonstrates that electronic performance is improved via phase engineering. Figure 4c and Figure 4d are output curves of pristine and superlattice InSe FETs, respectively. The output curves of pristine InSe FETs display a linear region and a saturation region at low Vds and high Vds, respectively, which are consistent with our early reports47. The superlattice devices exhibit totally different output characteristics in Figure 4d and Figure S3: the current shows a good linear behaviour in measured bias region and larger output current. The larger current of superlattice InSe is attributed to two factors: 1) larger channel conductance coming of higher carrier density and 2) lower contact resistance (Rc) of Cr-InSe for more electron injection. To elaborate electronic properties improvement of superlattice InSe sample, we calculate carrier sheet density (n2d) and Rc values of pristine and superlattice samples. The calculated n2d values are 0.996 ×1012 cm-2 and

6.37 ×1012 cm-2 for pristine and superlattice InSe FETs,

respectively (more calculated details in Supporting Information). After annealing, carrier density increases 6 times due to superlattice structure. The Rc value of pristine is calculated to be 506 KΩ, which is consistent with our early study47. After annealing, the contact resistance is drastically degenerated to 2.4 KΩ, which reduces 210 times (more calculated details in Supporting Information). Those results demonstrate electronic transport properties improvement of superlattice InSe device is attributed to higher n2d and lower Rc values.


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Figure 4. Electronic transport properties. (a), (b) The transfer curves of pristine and superlattice InSe transistor at Vds = 1 V. (c), (d) The output curves of pristine and superlattice InSe FETs, respectively.

To reveal photoresponse of pristine and superlattice multilayer InSe nanosheets, various illumination lights were vertically illuminated onto InSe photodetectors. As shown in Figure 5a and 5b, pristine and superlattice multilayer InSe photodetectors show an obvious broadband photoresponse from 254 nm to 700 nm illumination light. It is clearly that the photocurrent (Iph, Iph = Iillumination - Idark) of pristine and superlattice InSe photodetectors increases with applied bias voltage. Figure S4 is the calculated Iph-λ curves of pristine and superlattice multilayer InSe photodetectors at applied voltage of 1 V. Obviously, superlattice InSe photodetector generates larger Iph under various illumination lights. This phenomenon is due to more photogenerated carrier injection arising from lower contact resistance of superlattice InSe. For example, the Iph value is 15.1 μA for superlattice InSe photodetector under 700 nm and a bias of 1 V, which is


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approximately 8.4 times higher than 1.8 μA for pristine InSe. Responsivity (R), detectivity (D*) and external quantum efficiency (EQE) are three important parameters to evaluate a performance of photodetector. Superlattice InSe photodetector exhibits larger R values than those of pristine InSe photodetector under various illumination lights in Figure 5c (more calculated details in Supporting Information). For example, under 700 nm light illumination, R of superlattice InSe photodetector is calculated to be 1.7×104 A/W at a bias of 1 V, which is almost 8.5 times larger than 2.0×103 A/W of pristine InSe photodetector. Superlattice InSe photodetector show superior D* and EQE values than those of pristine InSe photodetector as shown in Figure S5. The D* and EQE values of superlattice InSe photodetector are calculated to be 1.4×1013 Jones and 1.7×107% with 490 nm light illumination and a bias of 1 V, which are larger than 9.1×1012 Jones and 7.1×105% of pristine InSe photodetector. The superior photodetection performance in the superlattice InSe photodetector is attributed to low contact resistance between superlattice InSe and contact metal electrodes, which leads to more photogenerated carrier injection. The photoresponse performance of superlattice InSe photodetector is superior to most photodetectors based on other 2D semiconductors (find more details in Table S1). Those results clarify optoelectronic properties of InSe photodetector can be effectively improved by phaseengineering.

Stability and response time are another two key parameters for evaluating a photodetector. The stability of pristine and superlattice InSe photodetectors was investigated. The on/off states of pristine and superlattice InSe photodetectors keep the same level for six cycles in Figure 5d, demonstrating a good optical switching stability for both types of InSe photodetectors. Figure S6 are rise and decay photoresponse behaviors of pristine and superlattice multilayer InSe


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photodetectors. Both types of InSe photodetectors exhibit a rapid response time of 20 ms for rise and decay process independent of annealing.

Figure 5. Optoelectronic properties. (a), (b) I-V curves for pristine and superlattice InSe photodetectors measured under various light illuminnation (254, 365, 490, 610 and 700) with a intensity of 0.29 mW/cm2, respectively. (c) The calculated responsivity values at applied voltage of 1 V. (d) Time-dependent photoresponse characteristics of pristine and superlattice InSe photodetectors illuminated by 700 nm light at V = 0.1 V with a light intensity of 0.29 mW/cm2.

CONCLUSIONS In summary, the superstructure phase is obtained in multilayer β-InSe nanosheets by simple thermal annealing for the first time. The electronic and optoelectronic properties of superlattice InSe nanosheets are significantly enhanced. After annealing, superlattice InSe nanosheets exhibit a semimetal transport behavior with a low current on/off ratio of 2.9. A high mobility of 299.1 cm2V-1s-1 is realized by superlattice InSe FETs, which is 4


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times for pristine InSe device. The electronic properties of superlattice InSe nanosheet are effectively improved, which is due to higher n2d value of 6.37 ×1012 cm-2 and lower Rc of 2.4 kΩ induced by a superlattice. An ultrahigh responsivity of 1.7×104 A/W is obtained by superlattice InSe photodetector, which is 8.5 times for pristine photodetector. The photodetection improvement of superlattice InSe is attributted to lower contact resistance for more photogenerated carrier injection. Superlattice InSe photodetectors hold a good photoresponse stability and rapid response time of 20 ms. All above results demonstrate that superlattice is a potential pathway to further improve electronic and optoelectronic properties of InSe devices.

ASSOCIATED CONTENT Supporting Information. Descriptions of experimental section, the calculated mobility, carrier density, contact resistance and responsivity, AFM, output characteristics of annealed InSe FETs with large Vds range, XRD, EDS, XPS, Iph-λ curves, Iph-V curves and response time of pristine and annealed InSe photodetectors, comparison of the critical parameters for photodetectors based on 2D GaSe and InSe. This material is available free of charge via the Internet at http://pubs.acs.org.” AUTHOR INFORMATION Corresponding Author * (B. Li) Email: [email protected] * (P. A. Hu) Email: [email protected] Notes


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The authors declare no any competing financial interest. ACKNOWLEDGMENT We gratefully acknowledge the support from National Natural Science Foundation of China (NSFC, No. 51802038), China Postdoctoral Science Foundation (No. 2018M630329), Heilongjiang Postdoctoral Special Fund (LBH-TZ1801), Fundamental Research Funds for the Central Universities (No. 2572018BC14). REFERENCES (1)

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Synthesis of Superlattice InSe Nanosheets with Enhanced Electronic

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