Design Growth of Triangular Pyramid MAPbBr3 Single Crystal and Its

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Design Growth of Triangular Pyramid MAPbBr Single Crystal and Its Photoelectric Anisotropy between (100) and (111) Facets Lin Jing, Xiaohua Cheng, Ye Yuan, Songjie Du, Jianxu Ding, Haiqing Sun, Xiaoyuan Zhan, and Tian-Liang Zhou J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.9b02045 • Publication Date (Web): 11 Apr 2019 Downloaded from http://pubs.acs.org on April 11, 2019

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The Journal of Physical Chemistry

Design Growth of Triangular Pyramid MAPbBr3 Single Crystal and Its Photoelectric Anisotropy between (100) and (111) Facets Lin Jing 1, Xiaohua Cheng 1, Ye Yuan 1, Songjie Du 1, Jianxu Ding 1,*, Haiqing Sun 1, Xiaoyuan Zhan 1, Tianliang Zhou 2 (1. College of Materials Science and Engineering, Shandong University of Science and Technology, Qingdao 266590, China; (2. College of Materials, Xiamen University, Xiamen 361005, China. *Corresponding author: E-mail: [email protected] (J. X. Ding)

ABSTRACT: CH3NH3PbBr3 (MAPbBr3), one of the classical members in organic-inorganic hybrid perovskite family presents excellent advantages in high photon absorption efficiency and long carrier transport distance, is expected to break the responsiveness and efficiency as photo-detectors, because single crystal is superior to its thin films, nanowires and other counterparts. Moreover, single crystal provides an adequate media to reveal the intrinsic photoelectric properties, such as defect-related dark current, mixed-ionic conductivities etc. The mixed-ionic conductivities in MAPbBr3 single crystal is considered to be associated with the atomic packing densities, which is deemed as crystalline oriented or anisotropy. In this study, a series of large-size MAPbBr3 single crystals with (100) and (111) facets exposed were successfully grown through a crystal limiting method. By fabricating metal-semiconductor-metal (MSM) 1

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planner photo-detectors on both (100) and (111) facets with Au interdigital electrodes in only a MAPbBr3 single crystal, the photoelectric anisotropy were systematically compared in terms of ion migration and the anisotropy of current and on-off ratios. It reveals that the higher MA+ and [PbBr6]4- densities in (111) plane cause higher build-in electric field, which ultimately affects the dark current, photo currents and on-off ratios.

1. INTRODUCTION Methylamine lead halide perovskites (MAPbX3), have been attracted wide interests due to their excellent photoelectric properties, which make them as various photoelectric devices, such as solar cells, photo-detectors, lasers, LEDs etc.

1-6.

As a

member of them, MAPbBr3 has an exceptional absorption capacity in the visible range and exhibits great potentials in optical detection, illumination and photovoltaic devices. In addition, it is proved that cubic structure of MAPbBr3 is somehow more stable than tetragonal MAPbI3 because of its higher symmetry as photovoltaic devices 7-10. Moreover, plenty of researches claim that both the stability and photoelectric properties of hybrid perovskite single crystals are superior that their polycrystalline counterparts, because single crystal exhibits less grain boundaries and defects 11, 12. Therefore, deeply explore the photoelectric properties of single crystal are demanded. When referring to photoelectric properties of a single crystal, its photoelectric anisotropy related to atom packing density should be taken into consideration, especially for mixed ions conduction MAPbBr3 single crystal 2


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13, 14.

Photoelectric anisotropy of hybrid perovskites has been proposed in recent

years in both polycrystalline films and single crystals, which are deemed related to photocurrent hysteresis

15.

Huang et al. theoretically and experimentally studied

facet-dependent electrical properties of many different semiconductors 16-19. Such as the surface layer thicknesses responsible for the facet-dependent electrical properties of Cu2O crystals have been determined for these facets. Different degrees of conduction band bending at the surface of these Si crystals exhibit a barrier height different from the current. Motta et al. calculated the transport properties of the carrier and found that the mobility of the two possible organic cations is significantly asymmetric with the direction of the molecular axis

20.

Bark et al. directed the

production of CH3NH3PbI3 polycrystalline films with (112) and (220) orientations and found that the charge transport was severely anisotropic 21. Yan’s group fabricated vertical-structured field-effect transistor (FET) based on CH3NH3PbI3 polycrystalline films with (001), (100) and (112) orientations and discussed the origin of the anisotropy of carrier transport from the perspective of the crystal structure and ion migration 22. Our group was further studied part of the anisotropy of MAPbCl3 and MAPbI3

23, 24.

Though these researches clearly points out the photoelectric

anisotropy in perovskite, however, deeper and wider investigations of photoelectric anisotropy are still lacking, especially lacking the high index facets relevant photoelectric anisotropy and the effect of ion migration on the photoelectric properties of ionic crystals. Here, we successfully grew a triangular pyramid MAPbBr3 single crystals, with 3



both (100) and (111) facets exposed by controlling the orientation of the seed crystal and limiting the growth method. Taking advantage of such facets, planar photo-detectors were fabricated, and the photoelectric anisotropy was compared.

2. EXPERIMENTAL Cubic morphology of MAPbBr3 single crystals was grown via the inverse temperature crystallization method as reported 25. Pyramid MAPbBr3 single crystals with (111) facets exposed were grown through seed crystal limiting method. Firstly, small cubic crystal was treated into a pyramidal seed crystal, and then was re-inserted into a specific seed crystal limiting device in the growth solution to obtain crystals with exposed (111) crystal plane by limiting the growth of (111) facet. The powder and (100) facet XRD patterns were found on X-ray diffract-meters (D/Max2500PC). The UV-vis and PL spectra were collected on UV-2550 spectrometer in the range of 450-650 nm and FLS-920 under a 350 nm excitation illumination. In order to study of the anisotropy of the photoelectric properties of MAPbBr3 single crystal, planar photo-detectors with Au interdigital electrodes were prepared on the polished (100) and (111) facets using dried fine silks. The elaborated polished facets can guarantee that the compact contacts to be Ohm contact between Au electrodes and facets of MAPbBr3 single crystals. Such common polished technique is also adopted by other optical crystals, such as KDP, LBO and LBO, etc. Moreover, the polished facets can remove surface decompositions and other pollutants. To eliminate the influence of crystalline on photoelectric properties, the (100) and (111) 4


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facets photo-detectors were simultaneously fabricated on one triangular pyramid MAPbBr3 single crystal. The simultaneously fabricating Au electrodes can guarantee the similar contact resistance. 4×4 mm2 interdigital masks were placed on both (100) and (111) facets, and the interdigital width was 100 μm. The Au electrodes sputtering process was carried out using a small particle sputter (SBC-12, KYKY Technology Co., LTD.) within 3 minutes. The thickness of the Au electrode on the surface was therefore controlled below 120 nm. The photoelectric properties were performed using a semiconductor test system (Keithley 2450. USA). The excitation light source was a semiconductor laser having a wavelength of 405 nm. By adjusting the illumination powers, a series of I-V curves were obtained. Under a fixed illumination power of 10 mW, the on-off ratios under various voltages were measured.

3. RESULTS AND DISCUSSION The growth rate of the (111) facet of MAPbBr3 single crystal is faster than that of (100) facet because of its small interplanar distance (3.418 vs 5.920 Å) according to the crystal structure

26.

Therefore, to get an exposed (111) facet, limiting the

growth of (111) facet is an appropriated method. During the growth progress, the growth of three (100) facets allows the recovery of (111) facet. Figure 1a displays the as-grown cubic and triangular MAPbBr3 single crystals with (100) and (111) facets exposed respectively. The exposed (111) facet supplies the facility to research the photoelectric properties of MAPbBr3 single crystal. Figure 1b demonstrates powder 5



and (100) facets XRD of MAPbBr3 single crystal, both of which corresponds cubic _

perovskite structure (Pm3m). It is difficult to obtain because the diffraction intensity of the (111) facet is too low. Sharp {100} crystal plane peaks suggest well crystalline perfection of MAPbBr3 crystal. To evaluate the crystalline perfection of the grown MAPbBr3 crystal, the full width at half maximum of (100) peak is shown in Figure 1c. The FWHM is calculated at 0.1°. Such small value indicates excellent crystalline perfection of the crystal. According to the absorption spectrum in Figure 1d, the band gap (Eg) was calculated to 2.12 eV, which was smaller than thin film (2.30 ± 0.10 eV)

27, 28.

The narrower band gap brings advantages for photoelectric

applications. The PL spectrum was obtained by using a 350 nm excitation illumination. An intensive CBM to VBM recombination peak can be seen in the photo luminescent spectrum around 580nm while several sub-band gap emissions exist on the low energy shoulder of the band-to-band peak. Such shallow defect level can be

10

(110) (111)

(100)

(300)

Powder (100) planar

(400)

(200)

b

(100)

allocated to the levels induced by intrinsic defects caused by MA+ ions 29, 30.

Intensity (a. u.)

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

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20

6


30 40 2 Theta ()

50

60

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14.0 14.5 15.0 15.5 16.0 2 Theta ()

1/2

h

Absorbance (Arb. Units)

0.1

Photoluminescence (Arb. Units)

d

c Intensity (a.u.)

Eg=2.12eV 2.0

2.2

h (eV)

480

2.4

520 560 600 Wavelength (nm)

640

Figure 1 (a) Photos of MAPbBr3 single crystals; (b) Powder and (100) planar XRD of MAPbBr3 single crystal; (c) FWHM of (100) crystal planes; (d) Absorption spectrum, band gap and PL spectrum of MAPbBr3 single crystal.

 -1

3.

98

200

(100) Dark (111) Dark

 -7

400

=

b Current (nA)

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


0

=5.431

-8 -1 0 

-200 -400 -10

-5

0 Voltage (V)

5

10

Figure 2 (a) Schematic diagram of photo-detectors on (100) and (111) facets; (b) Comparison of dark currents of (100) and (111) facets based photo-detectors.

To compare the photoelectric properties between (100) and (111) facets of MAPbBr3 single crystal, planar photo-detectors with Au interdigital electrodes were fabricated. Figure 2a displays the structure of the photo-detector with different crystal facets fabricated on the same crystal. The dark current contrast of the (100) 7



and (111) facets is illustrated in Figure 2b. As can be seen that, the I-V curves are in good linear feature, suggesting that the contacts between Au electrodes and single crystal surfaces are Ohm contact. We believe that the Ohm contact is attributed our polished smooth surfaces of MAPbBr3 single crystal by a dry fine silk. The conductance of the (111) facets is significantly larger than the (100) facets, which is suspected of the ionic conductance of the (111) facets. Figure 3(a-d) illustrates the side-view and top-view of (100) and (111) surface structures respectively. It clearly demonstrates that the densities of MA+ and Br- in (111) facet are higher than those in (100) facet. These higher ions densities heighten ionic conductance, and therefore the dark current of (111) device is higher. Besides, as can be seen from Figure 3, MA+ ions are located on (111) external layers and therefore (111) facet exhibits positive charges, which will be discussed below.

Figure 3 Comparison of side-view (a, c) and top-view (b, d) surface structures on (100) and (111) facets of MAPbBr3 single crystal. 8


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The I~V curves for (100) and (111) facets devices under various illumination powers using a 405 nm laser are displayed in Figure 4 (a-b). For (100) facet, the currents increase rapidly beyond 4 V under various illumination powers. The increscent of slopes in I-V curves beyond 4 V reveals the enhancement of ion migration with higher impressed voltages. Previous research declares that vacancies, MA+ ions and halogen interstials can be driven to migrate with certain activation energy in organic halide perovskites

31.

On the other hand, the current increscent

features exhibit different tendency for (111) facet device. The voltages, where the currents rapidly increase are dependent on the illumination powers, which is higher than those for (100) facet device, as showed in Figure 4a. This suggests that the activation energy of ion migrations in (111) facet are higher than those energy in (100) facet. We believe this is attributed to the higher ion densities in (111) facet, especially the Br- densities, because halide ions are pointed out plays pivotal roles than other ions 32.

-5

6.0x10

-6

-1

0 Voltage (V)

1

-5

0.0 0

2

b 4.0x10-5

10mW

0.0

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4 6 Voltage (V)

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a Current (A)

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Dark 15mW -6

5mW 10mW 20mW

-0.54V

0.0

0

-1

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0 Voltage (V)

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4 6 Voltage (V)

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Figure 4 (a-b) Dark and photocurrents curves of (100) and (111) facets photo-detectors, respectively. 9



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In addition, the I-V curves for (100) device under illuminations exhibit a classical photoelectric effect. However, they present photovoltaic effect for (111) facet device, and the device generates an open-circuit voltage (VOC) of 0.54 V, which are displayed in the insert pictures in Figure 4b. The photovoltaic effect in (111) facet is ascribed to that larger accumulation of MA+ ions at the electrode interface blocking interfacial charge recombination

33.

Because MA+ ions are located on (111) external layers,

which provide more migration routes, as shown in Figure 3. On the other hand, the migration of MA+ towards to electrodes could cause MA+ missing on the outward of the (111) facet. The missing MA+ is considered to be related with the photovoltaic effect, and bring the change of VOC. Such phenomena are also revealed and taken into consideration to treat surface of perovskite. For instance, by spin-coating MAI on MAPbI3 surface can treat the loss of MA+ and decrease trap states, and further to effect in many terms, such as open-circuit voltage, fill factor short-circuit current density, power conversion efficiency, etc.

34.

Utilizing polyvinyl alcohol (PVA)

35

and

inorganic cations 36, such as Cs+ can also prevent the loss of MA+. The appearance of the VOC in (111) facet device also implies ion migrations play a greater impact to photoelectric properties.

10


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a

1V

2V

3V

4V

5V

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2V

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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


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Figure 5 (a-b) Five continues on-off circles under different applied voltages of the devices on (100) and (111) facets respectively.

Photoelectric measurement of continuous switching cycles was performed with the aim to compare switching characteristics of the two facets at different applied voltages. According to reports, this behavior originated from ion migration and carrier trapping/decapture

37.

Figure 5 (a-b) depicts the photocurrent switching

ratios under a 405 nm limunation at different voltages with five steady-state continuous switch photocurrent circles varying with time, which clearly reflects the anisotropy of photoelectric properties on (100) and (111) facets. The maximum switching ratios of the (100) and (111) facet devices at 5 V are ~342 and ~89, respectively. The lower switching ratio of (111) facet device is ascibed to the stronger build-in electric field, which blocks the carriers to transport to the electrodes. On the other hand, after photocurrents reaching saturation, their relaxation as time under light injection reflects the ion conduction contributions as well. Because MAPbBr3 is a mixed ion conductor of MA+ and Br- ions. The stronger build-in electric field caused by the MA+ ions for (111) facet device depresses the 11



photocurrents to be in a downward trend, as shown in Figure 5 (a-b). The longer photocurrent relaxation time for (111) facet device verifies the stronger ion conduction contributions.

4. CONCLUSIONS Triangular pyramid MAPbBr3 single crystals were grown by a crystal limiting method. MSM structure photo-detectors according to (100) and (111) facets were adopted in order to research the anisotropy of the photoelectric characteristics. The experimental results show an photoelectric obvious anisotropy between (111) and (100) facets devices of MAPbBr3 single crystal. An open circuit voltage was in existence on (111) facet device and the higher voltages were needed to overcome the build-in electric field to activate ions participating into conduction. Besides, the on-off ratios of (111) facet device were lower than those of (100) facet devices, and the photoelectric currents significantly decrease according to the ion conduction theory.

AUTHOR INFORMATION Corresponding Authors *E-mail:

[email protected] (J. X. Ding)

Notes The authors declare no competing financial interest.

ACKNOWLEDGEMENTS 12


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This work was financially supported by the National Science Foundation of Shandong Province (ZR2016EMQ10), the National Natural Science Foundation of China (No. 51202131).

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Design Growth of Triangular Pyramid MAPbBr3 Single Crystal and Its

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