Synthesis of large two-dimensional lead-free bismuth-silver double perovskite microplatelets and their application for field-effect transistors

Article abstract of DOI:10.1039/d0cc01847c

Two-dimensional phenylethylammonium (PEA, C8H9NH3) Bi-Ag double perovskite (PEA)4BiAgX8 (X = Br, I) microplatelets are synthesized for the first time via a facile self-assembly recrystallization method. Absorption spectra of microplatelets exhibit direct bandgaps and different halide compositions show distinct morphologies and bandgap tunability. Field-effect transistors based on a single (PEA)4BiAgBr8 microplatelet display a p-type semiconducting behavior.

Full text of DOI:10.1039/d0cc01847c

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DOI: 10.1039/D0CC01847C
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Synthesis of Large Two-Dimensional Lead-Free Bismuth-Silver
Double Perovskites Microplatelets and Application for Field-Effect
Transistors
Received 00th January 20xx,
Accepted 00th January 20xx
Xiaoyu Wang, Kai Li, Hanlun Xu, Nasir Ali, Yao Wang, Qibin Shen and Huizhen Wu*
DOI: 10.1039/x0xx00000x
Two-dimensional phenylethylammonium (PEA, C
double perovskites (PEA) BiAgX (X=Br, I) microplatelets are
synthesized for the first time via facile self-assembly
8 9 3
H NH ) Bi-Ag
4
8
a
recrystallization method. Absorption of microplatelets exhibit
direct bandgaps and different halide compositions show distinct
morphologies and bandgap tunability. Field-effect transistors
4 8
based on single (PEA) BiAgBr microplatelet display a p-type
semiconducting behavior.
Owing to their peculiar optoelectronic properties and facile
solution processability, organo-lead halide perovskites (PVKs)
have been extensively utilized for varieties of optoelectronic
applications, such as photovoltaics, light-emitting diodes, and
1
-3
photodetectors, etc. . Nevertheless, the bioaccumulation of
their major component (lead) compelled the researchers to
focus on other lead-free alternatives of halide PVKs materials.
In this regard, several homovalent and heterovalent substitutes
4
2+
have been introduced. Among these substitutes, Sn suffered
Figure 1. (a) A schematic diagram of the recrystallization method, where PEA induces the
lateral crystallization of (PEA) BiAgBr MPs. (b) SEM image of the (PEA) BiAgBr MPs and (c,d)
are their TEM images. (e) A histogram of the lateral size distribution of the (PEA) BiAgBr
MPs. (f) SPM image of the (PEA) BiAgBr MPs and (g) are their thickness measurement.
4
+
3+
from rapid oxidation to its stable Sn state. Similarly, Bi -based
PVKs exhibited better environmental stability with poor
photovoltaic performance duo to their lower deminsionality.
To cope with this issue, a new class of lead-free PVKs, i.e., direct bandgap 2D Bi-Ag double PVKs single crystals and thin
double PVKs with general formula A
introduced, where M is a monovalent cation (e.g., Na , Ag , Bi-Ag double PVKs as a non-toxic alternative to the lead-based
etc.) and M’ is a trivalent cation (e.g., Bi , Sb , etc.). The two PVKs. Therefore, we endeavored on finding a facile way to
Pb cations are substituted with one monovalent and one synthesize 2D Bi-Ag double PVKs and verifying its direct
trivalent cation to retain the structure dimensionality. Among bandgap property from its optical characteristics.
4
8
4
8
4
8
4
8
5
, 6
1
2
2
MM′X
6
have been films were fabricated. These were promising studies to utilize
7
+
+
3
+
3+
2
+
various double PVKs, A
2
BiAgX
6
has successfully utilized in X-ray
In this work, we successfully synthesized free-standing 2D
8
9
+
3+
detectors and solar cells .Although, less toxic Ag and Bi have halide double PVKs (PEA)
4
BiAgBr microplatelets (MPs) for the
8
2
+
completely replaced the toxic Pb . Unfortunately, due to their first time via a facile self-assembly anti-solvent recrystallization
1
0
2+
intrinsic indirect bandgap, it could not compete with Pb
based PVKs materials. However, recently it has been reported previously employed both for nanocrystals (NCs) and
method (ASRC) in ambient conditions. This method was
1
3, 14
that by reducing the dimension of Bi-Ag double PVKs into 2D, nanosheets (NSs) synthesis.
Typically, the ASRC involves the
1
1
the bandgap can be switched into a direct one. Subsequently, injection into a suitable solvent with a relatively poor solubility
of the precursor solutes, triggering fast self-assembly
recrystallization, as schematized in Figure 1a. Here, dimethyl
sulfoxide (DMSO) is used as a precursor solvent and chloroform
Department of Physics and State Key Laboratory for Silicon Materials, Zhejiang
University, Hangzhou, China. E-mail: hzwu@zju.edu.cn
Electronic Supplementary Information (ESI) available: [details of any supplementary
information available should be included here]. See DOI: 10.1039/x0xx00000x
(CHCl
3
) as the recrystallization solvent to obtain ultra-large high-
BiAgBr MPs. Since we used a long-chain
quality 2D (PEA)
4
8
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Journal Name
+
+
+
organic cation, i.e., PEA instead of Cs or MA ; therefore, the
growth of the crystals is restricted to form a 2D structure.
Conversely, the conventional A sites could only result in
nanocrystals.15 Compared with the previous reported single
crystal growth of 2D Bi-Ag double PVKs, which need to be kept
View Article Online
DOI: 10.1039/D0CC01847C
1
2
at 100℃ for 60 h, this method is less energy and
consumptions.
Firstly, the structural and morphological characteristics of
the prepared (PEA) BiAgBr MPs were studied. A comparatively
4 8
optical absorbance revealed a direct bandgap of the MPs.
Furthermore, 2D Bi-Ag double PVKs with different halide
compositions were also synthesized, which not only exhibited
distinct morphologies but also tunable bandgaps. To
demonstrate the application of the prepared MPs, a single
4 8
(PEA) BiAgBr MP was utilized to fabricate a FET through a dry-
transfer procedure. Up to the best of our knowledge, this is the
first colloidal synthesis of the free-standing 2D Bi-Ag double
PVKs with ultra-large lateral size and their utilization in FETs.
Due to their free-standing nature in colloidal form, the MPs
could easily be utilized in a variety of optoelectronic
applications.
Figure 1b shows the scanning electron microscopy (SEM)
4 8
image of as-synthesized (PEA) BiAgBr MPs. Square-shaped
with larger size MPs were obtained using chloroform,
comparable with the 2D PVKs obtained via chemical vapor
Figure 2. (a) XRD pattern of (PEA)
MPs at variable temperatures. (c) Absorbance spectrum of (PEA)
Tauc plot of the absorbance spectrum of (PEA)
bandgap characteristic.
4
BiAgBr
8
MPs. (b) PL spectra of the (PEA)
BiAgBr MPs. (d)
MPs showing of a direct
4 8
BiAgBr
4
8
4 8
BiAgBr
6 5
chlorobenzene (C H Cl) were utilized to substitute chloroform.
Unfortunately, no sheets- or platelets-like products were
observed; instead, nanospheres- like morphology was observed
(Figure S4), which are fragile under the beams of an electron
microscope. Their abosrbance was also measured and shown in
Figure S5. It is speculated from the absorbance spectra, that the
product composition by dichloromethane is closer to MPs than
that by chlorobenzene. We aim is to obtain 2D PVKs for further
applications but dichloromethane and chlorobenzene are not
suitable. The impact of recrystallization solvents may be due to
the difference in the functional groups and solubilities. Different
solubilities of each precursor will cause defects, even damage
the Bi/Ag chemical ratio, hindering the synthesis of MPs. A
further detailed study is required to know the exact reason why
some recrystallization solvents are suitable for the fabrication
of MPs, as well as a effective method to modify lateral size.
Hitherto, chloroform is found to be a suitable recrystallization
solvent; therefore, all further characterizations and device
fabrication will be based on MPs obtained from chloroform as a
recrystallization solvent and other solvents are ruled out.
1
6, 17
deposition (CVD) technique.
adhered on the surface of MPs may be the by-products, i.e.,
BiBr , AgBr, and (PEA) Br Br , etc. The rapid-recrystallization
Multiple nanoparticles
3
3
2
9
process could be the reason of leftover products. The average
size of the MPs was estimated to be 13.75 μm. For size
distribution histogram, see Figure 1e, which is significantly
larger than other 2D halide PVKs obtained via the other similar
same routes.1
4, 18
Larger sized MPs could easily be observed
under an optical microscope, showing its feasibility for device
employment. Furthermore, it is revealed from the energy
dispersive spectroscopy (EDS) results that (PEA) BiAgBr MPs
4 8
exhibit a homogeneous distribution of the constituent elements
as shown in Figure S1. Transmission electron microscopy (TEM)
images showed that MPs have rectangular structures with sharp
edges, see Figure 1c and 1d. Similarly, the thickness and surface
roughness were studied by scanning probe microscopy (SPM),
as shown in Figure 1f. In accordance with SEM and TEM
analyses, multiple nanoparticles adhered to the MPs were
observed. In comparison with the surface of the substrate, the
height profile of the single MP was measured to be 1.25-1.75
μm, as depicted in Figure 1g. Because of nanoparticles attached
both sides, we deduced that the actual thickness of single MP
may be smaller than measured results. Additionally, the surface
roughness analysis revealed root-mean-square deviations (Rq)
To study the crystallinity of the prepared (PEA)
MPs, X-ray diffraction (XRD) analysis was carried out, as
depicted in Figure 2a. The XRD patterns of (PEA) BiAgBr MPs
show intense and sharp diffraction peaks at 7.0 and 14.0 two
theta degree, reflected from (002) and (004) crystal planes,
respectively. Besides, two faint diffraction peaks from (006) and
4 8
BiAgBr
4
8
(008) crystal planes were also observed. No other impurity peak
was observed, indicating the phase purity of the MPs. Smaller
full-width-at half-maximum (FWHM) of (002) and (004) plane
peaks, i.e., 0.0635 and 0.0664 two theta degree (Figure S6),
indicates the larger size as well as better crystallinity of the MPs,
which is benefitial to electron transportation. The spacing is 7.0
two theta degree and according to Bragg’s law, the calculated
2
of 19.007 nm and 35.564 nm for two 1 μm squares without any
nanoparticles attached, see Figure S2. Oleic acid was also
employed as a ligand during MPs synthesis but with the SEM
image shown in Figure S3, no influence from ligand was
observed. All the above characterizations were performed for
the MPs fabricated in chloroform as a recrystallization solvent.
To study the influence of the recrystallization solvent on the
out-of-plane distance is 1.26 nm, similar to (PEA)
4 4
PbBr PVK
1
9
nanosheets.
Stability test of (PEA)
4
BiAgBr MPs was done in the ambient
8
conditions for two weeks aged samples (Figure S7). Negligible
(
PEA)
4
BiAgBr
8
MPs,
dichloromethane
(CH
2
Cl
2
)
and
2
| J. Name., 2012, 00, 1-3
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variation was observed in the XRD patterns. The two dominant synthesized via same method. Upon changing the precursor
View Article Online
DOI: 10.1039/D0CC01847C
- -
diffraction peaks (002) and (004) were perfectly maintained solutions, we altered the halogen anion from Br to I to
with rather small FWHMs, indicating better environmental synthesize 2D (PEA) BiAgBr and (PEA) BiAgI . Figure 3a
4
4
I
4
4
8
stability of MPs. The enhanced stability is ascribed to the presents a distinct color change (starting from bright yellow to
-
hydrophobic long-chain organic cations at A sites.
Additionally, Raman measurement was also carried out for absorption edge of (PEA)
PEA) BiAgBr MPs. As Figure S8 shown, the Raman spectrum (PEA) BiAgI MPs are found to be respectively 412 nm, 561 nm,
exhibits three characteristic peaks at 67.91, 137.38 and 157.93 and 576nm, indicating an obvious red-shift (Figure 3b). It is
orange and scarlet) with the increasing ratio of I . The
4 8 4 4 4
BiAgBr , (PEA) BiAgBr I , and
(
4
8
4
4
-1
cm . These peaks were mainly generated from Bi-Br part of the worth noting that 2D Bi-Ag double PVKs with all halide
2
0
double PVK, which are obviously different from the pure BiBr
3
.
compositions don’t show any absorption tail. Tauc plots of
BiAgBr and (PEA) BiAgI presented
Therefore, it can be inferred that the Raman signals are direct bandgaps of (PEA)
4
4
I
4
4
4
originated from the (PEA)
stoichiometric residuals.
4
BiAgBr
8
, indicating the absence of in Figure S10 indicate a bandgap of 2.26 eV and 2.19 eV,
respectively. Furthermore, SEM presented significant
Likewise, the optical absorption spectrum of (PEA)
MPs presented in Figure 2c shows a sharp absorption edge at compositions: (PEA)
20 nm with an absorption peak at 379 nm without any morphology with a large length to width ratio (Figure 3c), where
absorption tail in the lower energy region. Tauc plot of a direct (PEA) BiAgBr exhibited belt-shapes with a few microrods
4
BiAgBr
8
morphological differences of products with different halide
4
BiAgBr have uniform rod-shaped
4 4
I
4
4
4 4
I
transition shows an ideal result with a standard linear region observed (Figure 3d). Beside their different morphologies,
indicating a direct bandgap of 3.05 eV, and a straighter line these compositions exhibited poor uniformity of morphology in
below 3.0 eV (Figure 2d). Cs
2 6 4 8
BiAgBr single crystals (SCs) exhibit comparison with the (PEA) BiAgBr MPs. However, the crystal
an indirect bandgap of 1.95 eV with assisting phonon energy of size of all three compositions was found to be in the micrometer
1
0
0
2
.12 eV, where Cs
.52 eV. 21 The bandgap of (PEA)
BiAgBr SCs and NCs, attributed to the 2D anions of Br and I in each sample. The morphological and optical
characteristic of MPs. A Tauc plot of an indirect bandgap of characteristics of 2D Bi-Ag double PVKs with different halide
the absorbance spectrum of (PEA) BiAgBr MPs is shown in compositions are listed in Table S1. Halide compositions of 2D
Figure S9. The results are in line with typical direct bandgap Bi-Ag double PVKs indeed influence the bandgaps and
2
BiAgBr
6
NCs exhibit an indirect bandgap of range sizes. As Figure S11 shown, EDS mapping results
4
BiAgBr is much wider than demonstrate uniform distributions of metal cations and halide
8
that of Cs
2
6
2
2
4
8
2
3
PVKs, e.g., MAPbX
PEA) BiAgBr MPs share the same M and M’ sites component enlarge their application areas.
as Cs BiAgBr . Furthermore, a strong photoluminescence (PL)
The intrinsic 2D nature of the solution-processed
peak at 481 nm of the MPs was observed at a low temperature (PEA) BiAgBr
MPs restricts the carrier transport laterally.25
25K) excited by a 404.6 nm laser, and intensity reduced
3
(X=Cl, Br, and I) single crystals even morphologies, which may facilitate further research and
(
4
8
2
6
4
8
(
distinctly with the increase of the temperature. There is no
obvious PL peak at 75K and above temperature. Due to strong
intrinsic quantum confinement in 2D (PEA) BiAgBr MPs,
4 8
excited carriers become bound excitons and relax back to self-
trapped states easily, and detrapped by thermal activation,
2
4
which brings the radiative transition down.
Figure 4. (a) Configuration diagram of (PEA)
of (PEA) BiAgBr MP FET. (c) Transfer characteristic of (PEA)
d) Transfer characteristic of (PEA) BiAgBr MP FET in semi-log plot.
4
BiAgBr
8
MPs FET. (b) Output characteristic
4
8
4
BiAgBr MP FET (Vds=30V).
8
(
4
8
4 8
Subsequently, a single (PEA) BiAgBr MP was employed to
fabricate a FET, as schematized in Figure 4a. The optical image
2
+
was shown in Figure S12. The conventional Pb based PVKs, as
well as the lead-free Sn2+ based PVKs have been successfully
exploited for FETs application. 26 However, to the best of our
knowledge, there is no report about FET application based on
In order to study the bandgap tunability of the MPs,
PEA) BiAgX (X=Br, I) PVKs with different halides were also
(
4
8
4 8
halide double PVKs. Therefore, employing (PEA) BiAgBr MP
Figure 3. (a) Pictures of colloidal solution of (PEA)
PEA) BiAgI . (b) Normalized absorbance spectra of MPs with different halide
compositions. (c, d) SEM images of (PEA) BiAgBr and (PEA) BiAgI
4 8 4 4 4
BiAgBr , (PEA) BiAgBr I and
(
4
4
4
4
I
4
4
4
.
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J. Name., 2013, 00, 1-3 | 3
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into the FET devices is of significant importance. Briefly, we 1.
Journal Name
F. Sahli, J. Werner, B. A. Kamino, M. Bräuninger, R. Monnard, B.
View Article Online
Paviet-Salomon, L. Barraud, L. Ding, J. J. Diaz Leon, D. Sacchetto,
adopted a dry transfer technique in which a single (PEA)
MP was transferred on the pre-patterned electrodes on SiO
substrates.17 The SiO
PEA) BiAgBr
4
BiAgBr
8
DOI: 10.1039/D0CC01847C
G. Cattaneo, M. Despeisse, M. Boccard, S. Nicolay, Q. Jeangros, B.
Niesen and C. Ballif, Nature Materials, 2018, 17, 820-826.
H. Cho, Y.-H. Kim, C. Wolf, H.-D. Lee and T.-W. Lee, Advanced
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N. X. Fang, X. Zhang and R. Ma, Advanced Materials, 2018, 30,
1704333.
2
/Si
2
acted as a dielectric layer while a single 2.
8
MP acted as a channel material. Figure 4b and 4c
(
4
3
.
shows the output characteristics (drain-source current Ids versus
drain-source voltage Vds) and transfer characteristics (drain-
source current Ids versus gate voltage V
PEA) BiAgBr MP FET device. The device displayed a p-type
semiconducting behavior as Ids increases when V decreases.
g
) of the fabricated 4.
S. Chatterjee and A. J. Pal, Journal of Materials Chemistry A,
2
018, 6, 3793-3823.
(
4
8
5
.
B. Wu, Y. Zhou, G. Xing, Q. Xu, H. F. Garces, A. Solanki, T. W. Goh,
N. P. Padture and T. C. Sum, Advanced Functional Materials,
2017, 27.
B. Ghosh, B. Wu, H. K. Mulmudi, C. Guet, K. Weber, T. C. Sum, S.
Mhaisalkar and N. Mathews, ACS Appl Mater Interfaces, 2018,
g
The device demonstrated the ON/OFF ratio above 100 counts,
which can be observed in the semi-log plot of its transfer
characteristic (Figure 4d). Moreover, the field-effect mobility of
6
.
1
0, 35000-35007.
퐿
푑퐼푑푠
1
7
7.
8
L. Liang and P. Gao, Advanced Science, 2018, 5.
a FET was estimated based on the equation μ =
,
푊퐶푉푑푠푑푉
푔
.
W. Pan, H. Wu, J. Luo, Z. Deng, C. Ge, C. Chen, X. Jiang, W.-J. Yin,
G. Niu, L. Zhu, L. Yin, Y. Zhou, Q. Xie, X. Ke, M. Sui and J. Tang,
Nature Photonics, 2017, 11, 726-732.
W. Gao, C. Ran, J. Xi, B. Jiao, W. Zhang, M. Wu, X. Hou and Z. Wu,
Chemphyschem, 2018, 19, 1696-1700.
where L is the channel length (2μm), W is the channel width
(
15μm), C is the capacitance of the 100 nm SiO
2
layer (3.45×10-
F/m ) and Vds=30V. ∂푉푔 can be calculated by fitting the linear
. The estimated field-effect
9
1
1
1
.
∂퐼
푑푠
6
2
0.
1.
2.
A. H. Slavney, T. Hu, A. M. Lindenberg and H. I. Karunadasa, J Am
Chem Soc, 2016, 138, 2138-2141.
region of the curve of Ids versus V
g
-5
2 -1 -1
mobility is about 1.66×10 cm V s . Considering the MPs were
obtained via an anti-solvent recrystallization method, in which
the crystallization finishes immediately, numerous defects
could be involved inside; therefore, we inferred that defect
B. A. Connor, L. Leppert, M. D. Smith, J. B. Neaton and H. I.
Karunadasa, J Am Chem Soc, 2018, 140, 5235-5240.
M. K. Jana, S. M. Janke, D. J. Dirkes, S. Dovletgeldi, C. Liu, X. Qin,
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mobility. Considering different defect formation energies of
1
4.
vacancies and antisites, modifying the chemical conditions, e.g.,
offering a Bi- or Ag-rich condition, is one of the promising 15.
methods improving mobility.27
1
1
1
1
6.
7.
8.
9.
In summary, we successfully synthesized high-quality large
D lead-free Bi-Ag double PVKs (PEA) BiAgBr MPs via a facile
self-assembly ASRC method for the first time. By a series of
optical characterizations and comparison with reported PVKs,
2
015, 15, 4741-4749.
2
2
8
C. Huo, X. Liu, X. Song, Z. Wang and H. Zeng, J Phys Chem Lett,
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we estimated that (PEA)
which is in line with the previous reports. An ideal Tauc plot of
direct bandgap indicated a bandgap of 3.05 eV. We also altered 20.
2 8
BiAgBr MPs have a direct bandgap,
1
190.
L. Zhou, Y. F. Xu, B. X. Chen, D. B. Kuang and C. Y. Su, Small, 2018,
4, e1703762.
the halide compositions, and fabricated (PEA)
PEA) BiAgI , which showed distinct morphologies and bandgap
shrinkage. Finally, a single (PEA) BiAgBr MP was utilized to
fabricate a FET device via a dry transfer technique. The device
demonstrated satisfactory performance, i.e., transfer
4 4 4
BiAgBr I and
2
2
1.
2.
(
4
8
1
2
8
N. Ali, S. Rauf, W. Kong, S. Ali, X. Wang, A. Khesro, C. P. Yang, B.
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2
3.
2 8
characteristics and ON/OFF ratio. Since the (PEA) BiAgBr MPs
are easy to prepare in a colloidal form and transfer on any type
of substrates; therefore, we believe that this work will provide
a better guideline to the development and applications of lead-
free double PVKs.
5
176-5183.
2
2
4.
5.
Y. Fang, L. Zhang, L. Wu, J. Yan, Y. Lin, K. Wang, W. L. Mao and B.
Zou, Angewandte Chemie, 2019, 131, 15393-15397.
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This work was supported by the National Natural Science
Foundation of China (Grant No. U1737109 and 1193306).
2
018, 14, e1803763.
2
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Conflicts of interest
27.
2
There are no conflicts to declare.
Notes and references
4
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Two-dimensional double perovskite (PEA) BiAgX microplatelets are synthesized for the first time with application in field-effect
transistors.