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Electronic interference transport and its electron–phonon interaction in the Sb-doped Bi2Se3 nanoplates synthesized by a solvothermal method

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Journal of Physics: Condensed Matter J. Phys.: Condens. Matter 27 (2015) 465302 (8pp)

doi:10.1088/0953-8984/27/46/465302

Electronic interference transport and its electron–phonon interaction in the Sb-doped Bi2Se3 nanoplates synthesized by a solvothermal method Bo Zhao1, Taishi Chen1, Haiyang Pan1, Fucong Fei1 and Yuyan Han2 1

  National Laboratory of Solid State Microstructures, Collaborative Innovation Center of Advanced Microstructures, and College of Physics, Nanjing University, Nanjing 210093, People’s Republic of China 2   High Magnetic Field Laboratory, Chinese Academy of Science, Hefei 230031, Anhui, People’s Republic of China E-mail: [email protected] Received 3 June 2015 Accepted for publication 30 September 2015 Published 2 November 2015 Abstract

Here we synthesized the antimony doped Bi2Se 3 nanoplates by the solvothermal method. The angle-dependent magnetoconductance study was carried out and all the ∆σ were found to be normalized to the perpendicular field, indicating a clear 2D electronic state. The features of weak antilocalization and universal conductance fluctuations were clearly identified in the magnetoresistance transport of the 4-probe nanodevices. The dephasing lengths are extracted respectively according to the Hikami–Larkin–Nagaoka theory. It is attributed to the involvement of the dynamic spin centers. The dephasing lengths are found to increase with the decreasing temperature following a 1/Lϕ2 ~ T γ law with γ ≈ 2. This reveals the additional dephasing source of electron–phonon interaction, which is often absent for pure 2D electronic systems. Keywords: topological insulator, Bi2Se 3, solvothermal method, dephasing, electron–phonon interaction S Online supplementary data available from stacks.iop.org/JPhysCM/27/465302/mmedia (Some figures may appear in colour only in the online journal)

Introduction

always unneglectable to understand some well-known phenomena in molecular and solid-state physics. Recently, the EPI successfully explains the superconductivity phenomena in doped Bi2Se 3 [2], and NaBi [3, 4]. In addition, it has also been proposed for inducing the topological properties of Dirac insulators and semimetals, e.g. TI and Weyl semimetals [5– 9]. However, the EPI in TIs remains elusive in detail and the strength of EPI varies as well [10–12], although sometimes it is close to value of the 2DEG on Bi2Se 3 [13]. Additionally, the strength of EPI increases when Dirac fermions are away from the Dirac point into higher energy states [14, 15]. Furthermore, most evidences always tend to show the electron–optical phonon coupling [16, 17] and the long-wavelength acoustic

The topological insulator (TI), with a novel robust metallic surface state protected against backscattering by time-reversal symmetry located on the surface, is getting more and more attention in physics. It is directly confirmed by the angleresolved photoemission spectroscopy and scanning tunneling microscopy. However, the topological surface states is always mixing with the topologically-trivial two-dimensional electron gas (2DEG) due to the unavoidable native defects and associated dangling bonds present on the surface [1]. Many scattering mechanisms have been discussed in those materials. The electron–phonon interaction (EPI) in materials is 0953-8984/15/465302+8$33.00

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© 2015 IOP Publishing Ltd  Printed in the UK

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the photic-lithography. The Hall bar is patterned with electron beam lithography and argon plasma etching. Before the deposition of the metals, a brief ( ∼5 s) selective surface treatment of the contact area with Argon plasma (30 W) was used to enhance Ohmic conduction of the contacts. The electron transport measurements are performed on the Quantum Design Physical Property Measurement System-9T & 16T system. The measurement temperature range of samples is from the room temperature 300 to 2 K. In the measurement, four devices were measured.

phonons, which dominate the physics at low energy scales, are also proposed [18–20] without any compelling evidence of a Rayleigh acoustical branch [21–24]. The coherent optical and acoustic phonons are observed to coexist in Cu doping Bi2Se 3 [25]. The EPI, the main source of charge carriers scattering, shows strong temperature dependence in semiconductor crystals and low-dimensional structures with impurities and defects. The temperature-dependent electron dephasing time is very sensitive to the scattering due to different dephasing mechanism in various mesoscopic systems [26]. In TI, besides the electron–electron interaction [27–31]. The EPI dephasing is also observed with the weak antilocalization (WAL) [28, 32, 33]. With the special branch phonon scattering affecting the electron property, the temperature dependent resistance is also observed, e.g. the graphene on SiO2 substrate [34], the Bi2Se 3 at high electric field [17] or higher temperature between 50 and 150 K [24]. Combining all the above considerations, the EPI in Bi2Se 3 could be dominated with the optical phonon of energy Ω of about 6−8 meV in the lower temperature and acoustical phonon of a linear temperature dependent resistance in the higher temperature. In this work, the antimony doped Bi2Se 3 nanoplates was synthesized by the wet chemical method, solvothermal method. The 2D temperature dependent dephasing length obtained from the WAL and universal conductance fluctuations (UCF) are discussed. The EPI in the TI is corroborated by analyzing the dephasing mechanism and the temperature dependent resistance. The optical phonon scattering is also suggested to come into effect at low temperature.

Results The typically hexagonal morphology with 120° edge facets and the high-resolution TEM images (HRTEM) image confirm the single crystalline nature of the Sb doped Bi2Se 3 nanoplates selected randomly from the TEM copper grids dropped the nanoplates, shown in figure  1(a). The compositions of nanoplates are determined by the EDX spectrum shown in figure 1(c). Comparing with the pure Bi2Se 3, the Sb peak is identifiable corresponding to the atomic percentage of ∼ 4%. In figure  S1 (stacks.iop.org/JPhysCM/27/465302/mmedia), the intensities of the Lα1 and Lβ1 peaks of bismuth at 10.84 and 13.02 keV are reduced after doping, suggesting a substitution doping nature [35]. In addition, the Raman spectrum demonstrates not distinct Sb–Sb bound around the 155 cm−1 and Sb--Se bond in the Raman spectrum in figure 1(b) [36]. It confirms that Sb is successfully incorporated into the Bi2Se 3 matrix. However, a higher dose Sb source yields a much lower Sb percentage in synthesized Bi2Se 3 nanoplates. For the electronic transport measurement, Four devices with nanoplates around 10 nm are selected by the optical microscopy on the SiO2 substrate [37]. The temperature dependence of the resistance shows a metallic behavior shown in the upper inset of figure  2. It indicates that Sb doped Bi2Se 3 nanoplates are heavily electron-doped semiconductor with the Fermi surface located in the conduction band [38, 39]. It is also confirmed with the higher carrier density, above 1013 cm−2. Based on the parabolic dispersion relation of the 2DEG and the longitudinal resistance and Hall resistance, several relevant parameters of four samples are obtained and listed in table 1, with effective mass m* = 0.3 m e [35, 40, 41]. A sharp cusp structure around B = 0 T in magnetic field dependent resistance curve is observed clearly and gradually weaken with increasing temperature. This cusp is ascribed to the quantum interference (QI) phenomenon, WAL. At high magnetic field, the resistance fluctuation persists with amplitude decreasing as temperature increasing. It is also ascribed to another QI phenomenon, UCF. It can be obtained from subtracted the baseline with the third order polynomial, shown in figure 3(c).

Experiment The synthesis of the Sb doping Bi2Se3 and characterization

Here, a solvothermal reaction in autoclave was picked up in the synthesis of the Sb doped Bi2Se 3 nanoplates. All of reagents were purchased from Alfa Aesar Company. Bismuth chloride (0.6307 g, 98%), selenium oxide (0.3649 g, 99.4%), antimony acetate (0.6 g, 97%) and the surfactant polyvinylpyrrolidone (PVP, 0.25 g) and Ethylenediaminetetraacetic acid disodium salt (EDTA-2Na, 0.8 g,)) are added into 50 ml of ethylene glycol and stirred smoothly for an hour. The final clear solution was transferred into a Teflonlined 55 ml autoclave. After that, the autoclave was sealed and heated to the reaction temperature of 220 °C within 30 min. It was then maintained for 24 h and cooled to room temperature. The morphology and component are characterized by transmission electron microcopy (TEM, FEI Tecnai F20 microscope operated at 200 kV) and energy dispersive x-ray (EDX) spectroscopy. The Raman spectroscopy is done with 633 nm by LabRAM HR800 (Horiba JobinYvon).

Discussions

The fabrication of the device and electron transport measurements

The QI effect of Sb doped Bi2Se 3 is also analyzed by means of magnet-field-dependent conductance. As a quantum correction to the classical magnetoconductance (MC), this effect is

The nanoplates are dropped on 300 nm SiO2 doped Si substrates. The Cr/Au (5/50 nm) electrode is patterned with 2

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Figure 1.  (a) is the TEM images of Sb doped Bi2Se 3 nanoplates. (b) is the Raman spectrum of the pure Bi2Se 3 and the Sb doped Bi2Se 3.

They are synthesized by the same method. (c) is the EDX spectrum of the Bi2Se3 and the Sb doped Bi2Se3 nanoplates with the vertical normalization.

The 2D nature is identified in the field-angle dependence of the MC [31, 42, 43], as shown in figure 3. It is more evident at low temperature. The WAL curves taken at different field angles are plotted as a function of the normal component of the field B⊥ = B(θ ) cos θ, shown in figure 3(b). Those curves overlay nicely with the MC at 0°, implying the observed WAL is essentially controlled by the 2D component. In figure 3(d), the positions of the UCF peaks overlap after normalizing the MC with B⊥. For a 2D system with strong spin–orbit interaction, the temperature-dependent WAL is studied with the Hikami– Larkin–Nagaoka (HLN) model in the symplectic limit. The formula for this model can be written as [39, 43–45]: ⎛ Bϕ ⎞⎞ Bϕ ⎞ αe 2 ⎛ ⎛ 1 ⎟ − ln⎜ ⎟⎟, ∆σ2D = Ψ⎜ + (1) 2 ⎜ ⎝ ⎝ B ⎠⎠ 2π  ⎝ 2 B⎠

Figure 2.  is the temperature dependent magnetoresistance of the SBS-3 with the magnetic field perpendicular to the plane of the sample and the direction of the current flow. The upper inset shows the resistance versus temperature from 2 K to 300 K. The lower inset is the optical image of the four-probe and Hall bar configuration of the Sb doped Bi2Se3 nanoplates. The scale bar is 5 µ m.

where the σ2D is the 2D sheet conductance, Bϕ = /(4eLϕ2 ), in which the coherence length is characterized by Lϕ = Dτϕ , D is the diffusion coefficient and τϕ is the dephasing time. And the Ψ is the digamma function, describing the quantum correction to the conductivity in 2D systems. α is a coefficient whose value is determined by the nature of the corrections being WAL. It is well known that the WAL works well especially under a weak magnetic field. The critical field for the HLN is defined as B* = /2el2m, where l m is the mean-free path of the nanoplates, as shown in table 1. But in our work, the suitable

a signature of topological surface states originating from the Berry phase which is associated with the spin helical surface states. Besides, it is sensitive to the direction of the applied magnetic field and the temperature. 3

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Table 1.  Transport parameters of Sb doped Bi2Se 3 nanoplates samples (T  =  2 K), the length/width  =  4/2 μm. The area density n = 1/eRH

and the mobility μ deduced with theσ = neµ. The Hall coefficient RH is obtained from fitting the Hall resistance between the  ±1 T. The effective mass m* = 0.3 m e is obtained from the literature [41]. The kF is obtained from the relation with σ = (e 2 /h )kFl m. The mean free path is obtained with l m = µ 2πns /e. The dephasing lengths are obtained from the fitting of the WAL curve. The Tee is the character temperature to distinct the electron–electron interaction.

SBS-1 SBS-2 SBS-3 SBS-4

Rxx (Ω)

n (1013 cm−2)

µ (cm V−1 s−1)

lm (nm)

B* (T)

D (cm s−1)

Lϕ (nm)

kF (nm−1)

νF (10 5m s−1)

Tee (K)

446.1 2430.5 739.2 766.1

5.77 1.18 2.41 3.48

486.0 434.2 701.5 469.4

60.9 24.6 56.8 45.6

0.09 0.54 0.1 0.16

225.66 41.42 136.19 131.4

363.1 150.2 145.7 526.8

1.9 0.86 1.23 1.48

7.4 3.4 4.8 5.8

93 104 64 96

Figure 3.  The quantum interference transport of SBS-3. (a) is the temperature-dependent MC:σxx (e 2 /h ) = (L /W )/Rxx (h /e 2 ) change

∆σxx = σ (B ) − σ (0) of the Sb doped Bi2Se3. (b) is the angle-dependent ∆σxx. The θ = 0° sign the magnetic field perpendicular to the plan of the device. (c) and (d) are the temperature and angle dependent UCF subtracted the baseline with the third order polynomial.

fitting field can go up to 1T, which is higher than the critical field. Figure 4(a) shows the fitting of the temperature dependence of WAL amplitudes to the HLN equation. In TI, the WAL effect constitutes a prominent transport property of the topological surface state, the value of the prefactor α represent the number of conducting channel. Each 2D conducting channel contributes −0.5 to the value of α and if there exist two independent channels α = α1 + α2 = −1 [46]. In the sample SBS-1 ( α = 0.6), SBS-2 ( α = 0.39) and SBS-4 ( α = 0.72), the value of α is around 0.5. It indicates that the single surface state exists in the WAL. A little increase in

α is observed as temperature decreases. However, in SBS-3, α = 1.25. It corresponds to two decoupled surfaces with each one having α = 0.5 respectively. The dephasing length of these four devices as a function of temperature is shown in figure 4(b). Although the dephasing length varies with different devices, it shows a similar behavior on temperature dependence. The neatly saturation of Lϕ is present at the low temperature. That is consistent with the temperature dependent dephasing length obtained from the UCF with the treatment method described in reference [32, 42, 47], as shown in figure 4(b). It can be clearly shown 4

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Figure 4.  (a) The fitted result α is shown as a function of temperature obtained from the HLN fitting. (b) The dephasing length Lϕ

obtained from WAL or UCF versus temperature is plotted on a logarithmic scale.

2

Figure 5.  (b) The temperature dependent scattering rate with 1/τϕ ∼ 1/Lϕ on logarithmic scale is shown with hole black squares. Red solid

lines represent fitting with equation (2). The fit parameters are shown in table 2.

that the Lϕ obtained from the WAL is larger than that obtained from the UCF. This implies the dynamic spins center exists in Sb doped Bi2Se 3 nanoplates [48]. AS for the mechanism of the dephasing, the inelastic scatterings in Sb doped Bi2Se 3 nanoplates are considered. In particular, various theories and experiments have been proposed with a power-law rule. It can be written with formula [26, 28]:

1 1 = 2 + A ⋅ T γ, (2) Lϕ2 (T ) Lϕ(0)

where Lφ(0) is zero temperature dephasing length, A ⋅ T γrepresents the contribution from the temperature dependent scattering mechanism. Figure  5 is the temperature dependence of scattering rate shown with 1/τϕ ∼ 1/Lϕ2 and the best fits to 5

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Figure 6.  Temperature dependent resistance on a logarithmic scale below 50 K. The red solid lines represents the best fitting to experiment data (hole black squares) with equation (3). In SBS-2 and SBS-3, the green solid lines are the fitting with globe temperature, which shows the mismatch with the data. Table 2.  The result of the fitting with equation (2).

SBS-1 SBS-2 SBS-3 SBS-4

Table 3.  The SBS-1 and SBS-4 is fitted from 2 to 50 K. The SBS-2

Lϕ(0) (nm)

A(Ω/K γ )

γ

351.4 160.1 167.8 344.7

6.1×10−4 2.49 × 10−3 1.1 × 10−3 1.1 × 10−3

2.09 1.86 2.12 2.14

and SBS-3 are fitted from 10 to 50 K with equation (3). R(0) SBS-1 445.6 SBS-2 2459.7 SBS-3 739.7 SBS-4 761.9

formula (2). The fitting parameters are shown in table 2. The γ ∼ 2 corresponds to an effective exponent for electron– phonon scattering process in 2D system. Apart from the EPI process, the electron–electron scattering process is always considered in low temperature. Theoretically, the electron– electron scattering rate from the singlet channel can be con

sidered into two categories [49]. For Tee < k τ ,  1 , kBτe τee

B e

1 τee

Ω/kB (T)

Ω (meV)

0.068 ~0 ~0 0.13

95.38(3.95) 94.79(3.12) 92.21(2.93) 110.35(10.08)

8.47(0.35) 8.42(0.28) 8.2(0.26) 9.8(0.89)

269.24 835.07 218.82 455.39

The EPI is also widely considered to be responsible for the temperature dependence of resistance. In TI, although the electron acoustic phonon interaction have been proposed and verified at high temperature region from the temperature dependent resistance data [19, 24, 34]. the electron–optical phonon interaction shows more convincing evidence from measurement by the ARPES, HAS [22] and also the temperature dependent resistance. Accordingly, the electron–optical phonon interaction is preferably considered in our data. The R ∼ T curve can be fit with the formula [17, 34]:

~ T and

Tee > ~ T ln(1/T ). It is clear that Tee is higher than the temperature of our measurement, as shown in table  1. This relation with Nyquist electron–electron interaction with a power relation of 1/Lϕ2 ~ 1/τϕ ~ T is always added in the formula (2) and it always exists in the low-temperature [42, 50]. However, it can be used to fit our data accurately without the e-e term even if it may exist in our samples. We argue that the EPI plays a more important role in the dephasing mechanism, although we cannot rule out the other mechanism as discussed above. Above all, the EPI is a nontrivial effect in the specific Sb doped Bi2Se 3 synthesized by solvothermal method. 2

A (Ω K−1) B

⎛ ⎞ 1 ⎟. R(T ) = R(0) + A × T + B × ⎜ Ω / k T (3) B ⎝e − 1⎠

The first term represents the residual resistance due to scattering by static impurities or defects, and the second term represents the contribution of acoustic phonons with a linear temperature dependent resistance. The last term comes from the contribution of surface phonon with a single 6

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Bose–Einstein distribution. As shown in figure  6, the SBS-1 and SBS-4 curves exactly matches the theory with curve SBS-2 and SBS-3 deviating below the 10 K. It is possible that electron–electron interaction results in an increase of resistance as the temperature going down [33, 51–53]. The result of the analysis is shown in table 3. The value of Ω is comparable with the thermally activated behavior of optical phonon (the symmetric A11g model of ∼8.9 meV is coherently excited by photoexcitation and efficiently coupling) with 6−8 meV [16, 22, 54]. Thus the optical phonon scattering probably exists in the TI. However, the data shown here can’t exclude other special scattering mechanisms, e.g. the acoustic phonon and the electron–phonon-impurities interference [55]. Therefore, further experiments are needed to clarify the exact picture. Conclusion Here we performed an angle and temperature-dependent MC study on the antimony doped Bi2Se 3 nanoplates fabricated by the solvothermal method. And the dephasing lengths are extracted respectively according to the 2D Hikami–Larkin– Nagaoka theory. The temperature dependent dephasing length following 1/Lϕ2 ~ T γ, with γ ≈ 2 in four samples indicates the dephasing source of EPI play a more important role in antimony doped Bi2Se 3 nanoplates. Besides, the temperature dependent resistance also suggests the existence of electron optical phonon interaction. So this work may perform a reference on the investigation on TI-based spintronic devices and quantum information materials at room-temperature. Acknowledgments The authors would like to thank the National Key Projects for Basic Research in China (Grant Nos 2013CB922103, 2011CB922103, 2015CB921202 and 2014CB921103), the National Natural Science Foundation of China (Grant Nos 91421109, 11023002, 11134005, 61176088, 51372112 and 2117109), the NSF of Jiangsu Province (Grant Nos BK20130054 and BC2013118), the PAPD project, and the Fundamental Research Funds for the Central Universities, for financially supporting this work. The technical assistance provided by Professor Li Pi and Mingliang Tian of the Hefei High Field Center is also gratefully acknowledged. References [1] Suh J, Fu D, Liu X, Furdyna J K, Yu K M, Walukiewicz W and Wu J 2014 Phys. Rev. B 89 115307 [2] Wan X and Savrasov S Y 2014 Nat. Commun. 5 4144 [3] Li R, Cheng X, Xie Q, Sun Y, Li D, Li Y and Chen X Q 2015 Sci. Rep. 5 8446 [4] Kushwaha S K, Krizan J W, Xiong J, Klimczuk T, Gibson Q D, Liang T, Ong N P and Cava R J 2014 arXiv:1403.3869 [5] Saha K and Garate I 2014 Phys. Rev. B 89 205103 [6] Li Z and Carbotte J P 2013 Phys. Rev. B 88 195133 [7] Garate I 2013 Phys. Rev. Lett. 110 046402 7

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Electronic interference transport and its electron-phonon interaction in the Sb-doped Bi2Se3 nanoplates synthesized by a solvothermal method.

Here we synthesized the antimony doped [Formula: see text] nanoplates by the solvothermal method. The angle-dependent magnetoconductance study was car...
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