Inorganic-Ligand Quantum Dots Meet Inorganic-Ligand Semiconductor Nanoplatelets: A Promising Fusion to Construct All-Inorganic Assembly

Article abstract of DOI:10.1021/acs.inorgchem.1c00880

By the reaction of inorganic-ligand CdS/Cd2+ quantum dots (QDs) with inorganic-ligand CdSe/CdS/S2- nanoplatelets (NPLs), semiconductor CdS QDs were fused with CdSe/CdS NPLs to yield all-inorganic assemblies, accompanied by great photoluminescence-enhancement. These all-inorganic assemblies facilitate charge transport between each other and open up interesting prospects with electronic and optoelectronic nanodevices.

Full text of DOI:10.1021/acs.inorgchem.1c00880

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Inorganic-Ligand Quantum Dots Meet Inorganic-Ligand
Semiconductor Nanoplatelets: A Promising Fusion to Construct All-
Inorganic Assembly
Yunfeng Shi,* Sung Jun Lim, Liang Ma, Ning Duan, Xin Yan, Xiaole Tang, Wenyan Yang, Shu Yang,
Jiaxin Hu, Andrew M. Smith,* and Xinyuan Zhu*
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ABSTRACT: By the reaction of inorganic-ligand CdS/Cd2+ quantum dots (QDs) with inorganic-ligand CdSe/CdS/S2−
nanoplatelets (NPLs), semiconductor CdS QDs were fused with CdSe/CdS NPLs to yield all-inorganic assemblies, accompanied
by great photoluminescence-enhancement. These all-inorganic assemblies facilitate charge transport between each other and open
up interesting prospects with electronic and optoelectronic nanodevices.
olloidal semiconductor nanocrystals (NCs) exhibit
unique size and shape dependent optical and electronic
negative charge on the surface. Similarly, small S2− was used
instead of traditional ligands with long hydrocarbon tails on
CdS QDs and then Cd2+ was introduced to get a positive ζ
potential for CdS QDs. As illustrated in Scheme 1, with the
C
properties1−8 and are of great interest in optoelectronics9 and
biological applications.10−12 High molecular weight polymer
ligands, particularly, dendritic polymers,13 block polymers,14
and proteins,15 and organic capping ligands such as short-chain
thiols16 are often used for the aqueous synthesis of semi-
conductor NCs. Long-chain hydrocarbon organic capping
ligands17,18 and trioctylphosphine oxide/trioctylphosphine
(TOPO/TOP) ligands19 are usually applied to nonaqueous
synthesis of semiconductor NCs. These semiconductor NCs
always have inorganic/organic hybrid structures. A big
challenge is that the organic capping ligands are usually
insulated; this makes nanodevices or nanostructured materials
made from such NCs behave like insulators. Posttreatment
after the synthesis of NCs to remove the insulating ligands is a
prerequisite for electrical and optoelectronic applications.
Talapin et al.20 established molecular metal chalcogenide
Scheme 1. Illustration for Fusion of CdSe/CdS NPLs and
CdS QDs
(MCC) ligands20 such as CdTe2 and simple metal-free
2−
inorganic ions21−23 such as S2−, Se2−, OH−, NH2 to modify
−
reaction of the S2− capped CdSe/CdS NPLs with CdS QDs
capped with Cd2+, the fusion of CdSe/CdS NPLs and CdS
QDs could be realized, due to the reactions of S2− and Cd2+,
resulting a new kind of all-inorganic assembly without ligands.
After fusion, the photoluminescence of this all-inorganic
assembly was also greatly enhanced compared to that of
CdSe/CdS/S2− NPLs due to the elimination of S2− photo-
luminescence quencher. Most importantly, there were only S
and Cd atoms at the fusion locus and no organic ligands were
on the assembly surface, facilitating their electronic and
the surface of NCs. The replacement of traditional long
hydrocarbon ligands by small inorganic ligands facilitated the
charge transport between individual NCs and opened up
interesting opportunities for device integration of nanostruc-
tures. Nag et al.24 proposed a simple and general method for in
situ preparation of inorganic-ligand luminescent metal sulfide
NCs. These inorganic-ligand NCs were able to be directly used
in electrical and optoelectronics devices.
In this paper, we would like to construct integrated all-
inorganic assembly based on inorganic-ligand two-dimensional
nanoplatelets (NPLs) and quasi-zero-dimensional quantum
dots (QDs). Different from traditional assembly or self-
organization of NCs containing both organic molecules and
NCs, all inorganic assembly based on inorganic-ligand NPLs
and QDs was established here.
Received: March 28, 2021
The oleylamine (OLA) and oleic acid (OA) capping ligands
of core/shell CdSe/CdS NPLs were replaced by S2− to get
https://doi.org/10.1021/acs.inorgchem.1c00880
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Figure 1. (a) Phase transfer of CdS QDs from hexane to N-methylformamide (NMF) upon exchange of the original organic surface ligands with
S2−. (b) UV−vis spectra of CdS QDs capped with organic ligands in hexane, CdS/S2− QDs in NMF, and CdS/Cd2+ QDs in NMF, respectively. (c)
FT-IR spectra of CdS QDs capped with organic ligands and S2−, respectively. (d) ζ-potential of CdS/S2− QDs and CdS/Cd2+ QDs in NMF.
Figure 2. (A) UV−vis spectra of CdSe/CdS NPLs in hexane, CdSe/CdS/S2− NPLs in NMF, CdS QD/CdSe/CdS NPLs in NMF, and CdS QD/
CdSe/CdS NPLs in hexane, respectively. (B) Photoluminescence (PL) spectra of CdSe/CdS NPLs in hexane, CdSe/CdS/S2− NPLs in NMF, CdS
QD/CdSe/CdS NPLs in NMF, and CdS QD/CdSe/CdS NPLs in hexane. The inset pictures a and b, made under a UV lamp, correspond to CdS
QD/CdSe/CdS NPLs in NMF and CdS QD/CdSe/CdS NPLs in hexane, respectively.
optoelectronic applications compared to organic molecule-
containing nanostructures.
ligands, S2− and Cd2+, respectively. The excitonic features in
the absorption spectra of CdS QDs changed little from 445 to
447 nm after introducing S2−, implying the effect of surface
environment change on CdS QDs. Long alkyl chain ligands
were replaced by small S2−, resulting in a fundamental distance
decrease between each quantum dot (QD). For the CdS/Cd2+
QDs, they could be synthesized easily by deposition of Cd2+ on
CdS/S2− QDs. The absorption peak of CdS QDs shifted to
457 nm, implying that a new layer of CdS was formed on CdS
QDs by the reaction of S2− and excess Cd2+.
The CdS QDs and CdSe/CdS NPLs used in this work were
prepared following protocols25−30 using long hydrocarbon
chains as stabilizers. For a typical ligand change procedure, the
CdS QDs capped with organic ligands in hexane were
combined with a N-methylformamide (NMF) solution of
Na2S or (NH4)2S. The immiscible two phase mixture was
gently stirred for several minutes under an Ar atomosphere,
and then CdS QDs could be completely transferred to NMF
phase in the form of CdS/S2− QDs, which can be evidenced by
yellow color of QDs shown in Figure 1a. Figure 1b compares
the absorption spectra of CdS QDs capped with organic
Figure 1c exhibits FT-IR spectra of CdS QDs before and
after the exchange of organic ligands with S2−. After phase
transfer, the bands at 2855 and 2927 cm−1 corresponding to
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https://doi.org/10.1021/acs.inorgchem.1c00880
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C−H stretching in the original organic ligands completely
disappeared, and new bands at 2887 and 2947 cm−1
corresponding to C−H stretching in NMF solvent appeared.
These results confirm that long hydrocarbon organic ligands
can be completely replaced by S2− and thus all-inorganic CdS
QDs can be obtained.
Figure 1d shows the ζ-potential of purified CdS/S2− QDs is
−35.7 mV, implying a negative charge on the surface of CdS
QDs. The purified S2− capped CdS QDs were further reacted
with Cd(AC)2 in NMF to get CdS/Cd2+ QDs in NMF. Their
ζ-potential which displays in Figure 1d is +13.2 mV, indicating
that a positive charge on CdS QDs could be realized by
introducing Cd(AC)2. TEM images of CdS QDs with average
size of 3.3 nm in different stages are shown in Figure S1.
Layer-by-layer atomic deposition assembly is a common
method for preparing core/shell CdSe/CdS NPLs. By the
reaction of Cd2+ with CdSe/S2− NPLs, one monolayer of CdS
shells can be formed. After the deposition of several layers of
CdS, core/shell CdSe/CdS NPLs with red emission were
formed and then they were transferred into the hexane phase
by the addition of OA and OLA organic ligands. By the
exchange of organic ligands with S2−, NMF solutions of CdSe/
CdS/S2− NPLs were obtained. Figure 2 compares the
absorption and photoluminescence spectra of CdSe/CdS
NPLs capped with organic ligands in hexane and CdSe/
CdS/S2− NPLs in NMF. Both the absorption and emission
peaks had slight increases after S2− capping. As the initial
CdSe/CdS NPLs had a Cd-rich surface, the initial surface Cd
ions on the CdSe/CdS NPLs could react with S2− to get a thin
CdS layer, resulting in a minor increase of absorption peak and
an enhancement of photoluminescence. After aging for several
days, the quantum yield (QY) of CdSe/CdS/S2− NPLs could
reach 2.8%, which is a great enhancement compared with that
of CdSe/CdS NPLs (QY: 0.6%). When the inorganic-ligand
CdSe/CdS/S2− NPLs met with inorganic-ligand CdS/Cd2+
QDs, a fusion occurred between them, resulting in QDs-inlaid
NPLs called as CdS QD/CdSe/CdS NPLs, which are
illustrated in Scheme 1.
Figure 3. TEM images of CdS QD/CdSe/CdS NPLs in NMF (a)
and in hexane (b). The scale bars are 50 and 20 nm for images a and
b, respectively.
purified by size-selective precipitation to remove free CdS/
Cd2+ QDs. From Figure 3b, CdS/Cd2+ QDs could still be seen
on the CdSe/CdS/S2− NPLs, which further proves the fusion
of CdS/Cd2+ QDs and CdSe/CdS/S2− NPLs. The lateral
dimensions of CdS QD/CdSe/CdS NPLs are 42 nm × 12 nm,
and the thickness is 3.2 nm. It is worth mentioning that fusion
between CdS/Cd2+ QDs and CdSe/S2− NPLs can also be
realized. The corresponding UV−vis spectra, PL spectra and
TEM images can be seen in Figures S4 and S5 in the
Supporting Information, respectively.
In summary, the fusion of semiconductor CdS QDs and
CdSe/CdS NPLs was realized by the reaction of inorganic-
ligand CdS/Cd2+ QDs with inorganic-ligand CdSe/CdS/S2−
NPLs. Different from the organic molecule linker method for
connecting two types of nanomaterials, CdS QDs were fused
with CdSe/CdS NPLs by the reactions of Cd2+ (from CdS/
Cd2+ QDs) and S2− (from CdSe/CdS/S2− NPLs), thus no
insulating ligands exist. Furthermore, this promising fusion also
resulted in great photoluminescence-enhancement of NPLs.
These all-inorganic assemblies open up interesting oppor-
tunities for integrated nanodevices which can be directly used
for electronic and optoelectronic applications.
ASSOCIATED CONTENT
* Supporting Information
The Supporting Information is available free of charge at
https://pubs.acs.org/doi/10.1021/acs.inorgchem.1c00880.
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The fusion between inorganic-ligand CdSe/CdS/S2− NPLs
and CdS/Cd2+ QDs can be proved by the absorption and
emission spectra. As shown in Figure 2A, the absorption peak
of CdSe/CdS/S2− NPLs shifts from 620 to 635 nm after the
mixing with CdS/Cd2+ QDs. CdS QD/CdSe/CdS NPLs could
be formed due to the reactions between Cd2+ on the CdS/
Cd2+ QDs and S2− on the CdSe/CdS/S2− NPLs. The
corresponding photoluminescence peak shifts from 631 to
643 nm shown in Figure 2B also imply the interactions
between CdS/Cd2+ QDs and CdSe/CdS/S2− NPLs. For the
QY, the QY of CdS QD/CdSe/CdS NPLs was 17.8%, which
was greater than that of CdSe/CdS/S2− NPLs due to the
diminishment of S2− PL quenchers by the reaction of S2− and
Cd2+. CdS QD/CdSe/CdS NPLs in NMF phase could be
extracted to hexane phase in the presence of OLA and OA.
After purification, the QY of CdS QD/CdSe/CdS NPLs in
hexane was 15.1%.
TEM images in Figure 3a show the fusion between CdSe/
CdS/S2− NPLs and inorganic-ligand CdS/Cd2+ QDs in NMF
after mixing for 6 h. Small black dots on the NPLs with a size
about 3.3 nm can be assigned to CdS/Cd2+ QDs which have
no remarkable size change before and after fusion with CdSe/
CdS/S2− NPLs. In order to further confirm that CdS/Cd2+
QDs were inlaid on the CdSe/CdS/S2− NPLs, they were
transferred from the NMF phase to the hexane phase and
FT-IR details, TEM images of CdS QDs in different
stages and CdS QD/CdSe NPLs in NMF, XPS spectra,
HR-TEM images and XRD spectra of CdS QD/CdSe/
CdS NPLs, UV−vis and PL spectra of CdSe NPLs,
CdSe/S2− NPLs in NMF and CdS QD/CdSe NPLs in
NMF, and experimental procedures (PDF)
AUTHOR INFORMATION
Corresponding Authors
■
Yunfeng Shi − School of Chemistry and Chemical Engineering
and Henan Province Key Laboratory of New Optoelectronic
Functional Materials, Anyang Normal University, Anyang
455000, People’s Republic of China; Department of
Bioengineering, University of Illinois at Urbana−Champaign,
Urbana, Illinois 61801, United States; orcid.org/0000-
0003-1426-9222; Email: shiyunfeng2009@gmail.com
Andrew M. Smith − Department of Bioengineering, University
of Illinois at Urbana−Champaign, Urbana, Illinois 61801,
United States; orcid.org/0000-0002-0238-4816;
Email: smi@illinois.edu
Xinyuan Zhu − School of Chemistry and Chemical
Engineering, Shanghai Jiao Tong University, Shanghai
C
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Liang Ma − Department of Bioengineering, University of
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Ning Duan − School of Chemistry and Chemical Engineering
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Xin Yan − School of Chemistry and Chemical Engineering and
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Shu Yang − School of Chemistry and Chemical Engineering
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Complete contact information is available at:
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Notes
The authors declare no competing financial interest.
ACKNOWLEDGMENTS
■
This work is supported by the National Natural Science
Foundation of China (21304001), the Joint Fund for Fostering
Talents of National Natural Science Foundation of China and
Henan province (U1204213), the Project of Science and
Technology Development of Henan Province (192102310298,
202102310332) and the Research training Fund of Anyang
Normal University (AYNUKFZ-2019-1).
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