Controllable synthesis of Sc3N@C78 microspindles with excellent

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Controllable synthesis of Sc3N@C78 microspindles with excellent electrophotonic properties rui zhang, Li Zhang, Xing Lu, and Jiangbin Xia ACS Appl. Energy Mater., Just Accepted Manuscript • DOI: 10.1021/acsaem.8b02078 • Publication Date (Web): 11 Feb 2019 Downloaded from http://pubs.acs.org on February 11, 2019

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ACS Applied Energy Materials

Controllable Synthesis of Sc3N@C78 Microspindles with Excellent Electrophotonic Properties Rui Zhang1, Li Zhang2, Jiangbin Xia*1, Xing Lu*2

1

College of Chemistry and Molecular Sciences, Wuhan University, Wuhan, 430073, P.

R. China

2

State Key Laboratory of Materials Processing and Die & Mould Technology, School of

Materials Science and Engineering, Huazhong University of Science and Technology (HUST), Wuhan 430074, P. R. China

ABSTRACT: Single-crystalline structures of fullerenes have attracted tremendous interest due to their promising physiochemical properties. However, research on the morphology and performance of endohedral metallofullerenes is still rare, due to the limited amount of samples. Herein, Sc3N@C78 microspindles are obtained for the first time by regulating the volume ratio of toluene to isopropyl alcohol (IPA) and the 1 ACS Paragon Plus Environment

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concentration of Sc3N@C78 solution as well. The X-ray diffraction (XRD) and selected area electron diffraction (SAED) studies indicate that the crystalline structure of Sc3N@C78 microspindles belongs to the hexagonal system. UV-vis-NIR spectroscopy reveals that absorption of Sc3N@C78 microspindles is stronger than that of the Sc3N@C78 solution in the ultraviolet and visible regions, suggesting strong intermolecular π-π interactions. In addition, Sc3N@C78 microspindles exhibit excellent photoconductivity, as evidenced by the photoelectrochemical measurements. Our results provide new insight into the exploration of novel structures of metallofullerenes for optoelectronic applications.

KEYWORDS: Sc3N@C78; microspindle; photoconductivity; self-assembly; liquid-liquid interfacial precipitation (LLIP)

Introduction

Fullerenes, as an important part of semiconductors and optoelectronics owing to their π-π conjugation and charge-transfer interactions, have aroused great interests from scientists1–3. Ordered nanostructures of crystalline fullerene materials are prerequisite for

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tailoring their physical and chemical properties and for achieving the corresponding applications. To this end, different types of crystalline fullerene nano/microstuctures have been obtained, ranging from one dimension (1D) to three-dimension (3D)4–7 such as nanorods8,9, microbelts10, nanotubes11, nanosheet12,13 by using the liquid−liquid12, liquid−air14 and liquid−air−solid15 interface methods. However, research on selfassembled architectures of endohedral metallofullerenes (EMFs), which trap metallic units inside the cages, has been rare, due to the complicated synthesis procedure and thus the limited amount. Owing to electron transfer from metal to cage, EMFs exhibit unique electronic and photoelectrochemical properties compared with hollow fullerenes3. Accordingly, EMFs are promising for their huge potential applications in photodetectors, optoelectronics, energy storage field effect transistors.

During recent years, progress has been made on the research of nanostructures of EMFs and their applications.8,16 Wang et al. employed an electrochemical deposition method to get Sc@C82 nanotubes with an anodic aluminum oxide template.17 Subsequently, Akakaska et al. prepared 1D nanostructures of La@C82(Ad) showing a p-



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type field-effect transistor property.8 Then Sc3N@C80 nanorods and nanosheets were prepared by Wakahara and coworkers18. Recently, our group prepared 1D nanorods of Lu2@C82

with

good

photoelectrochemical

properties.19

Until

now,

reported

nanostructures of EMFs are rested on nanorod19, nanocube20, nanotube16, nanosheet and nanowire17. However, other novel morphologies have not been studied. Therefore, to explore new nano/microstructures and to probe their photochemical properties are important and urgent.

Herein, Sc3N@C78 microspindles are successfully obtained for the first time via the liquid–liquid interfacial precipitation (LLIP) method. By controlling the concentration of Sc3N@C78 solution and volume ratio of good/poor solvent, novel crystalline Sc3N@C78 microspindles belonging to the hexagonal lattice are formed. UV-vis-NIR and photoelectrochemical results reveal that the Sc3N@C78 microspindles display strong absorptions and spectral responses in the ultraviolet to visible region, illustrating their excellent photoconductive properties.

Experimental section


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Materials

Sc3N@C78 was synthesized by a direct current arc-discharge method and was isolated in high purity (>99%).21 All solvents were used directly without purification.

The Sc3N@C78 microspindles were prepared via the liquid–liquid interface precipitation (LLIP) method22. Isopropanol/toluene was selected as poor/good solvent, respectively. Different volumes of isopropanol were slowly injected into 1 mL Sc3N@C78 toluene solution of variable concentrations (0.2 - 0.6 mg/mL). Then, the mixture was kept at room temperature for 24 hours for crystal growth.

Results and Discussion



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Figure 1. SEM images of Sc3N@C78 microspindles prepared by LLIP method under different concentrations of Sc3N@C78 in toluene. (a) 0.6 mg/mL, (b) 0.4 mg/mL, (c) 0.2 mg/mL, at room temperature and (d) 0.4 mg/mL, at 0 ºC.

We first studied the influence of the concentration of Sc3N@C78 solution on the morphology. Volume ratio of toluene/isopropanol is constantly set as 1:2, but the concentration of Sc3N@C78 in toluene varies from 0.6 mg/mL to 0.2 mg/mL at room


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temperature. As shown in Figure 1a, Sc3N@C78 nanorods were synthesized with an average critical diameter of 400 nm and an average length of 3.3 μm under a high concentration (0.6 mg/mL). With decrease of the concentration, the crystal is more favorable for radial growth, so that spindle-like nanostructures were obtained (Figure 1b). The average diameter of the microspindles are 1.8 μm and the average length increases to 600 μm. However, when the concentration of Sc3N@C78 decreases to 0.2 mg/mL, inhomogeneous microspindles appear (Figure 1c), which indicates that the low concentration of Sc3N@C78 restrains crystal growth.20

Unexpectedly, when the

temperature is set to 0 ºC, the structure turns into nanorods with a starting concentration of 0.4 mg/mL (Figure 1d). A possible reason is that low temperature affects the solubility of Sc3N@C78 in toluene, thus changing crystal growth orientation.23

Table 1 Diameter and length of Sc3N@C78 microstructures under different volume ratios of toluene/isopropanol.



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Sample

Volume ratios of

Average

Average length

number*

toluene/isopropanol

diameter (μm)

(μm)

a

1:1

2.35

10.00

b

1:2

0.58

1.80

c

1:2.5

0.26

1.50

* Sample number corresponds to the labels in Figure 2.

We then investigated the effect of volume ratio of good/poor solvents on the morphology of Sc3N@C78 microstructure s. Varied volume ratios of toluene/isopropanol (1:1, 1:2, 1:2.5) are investigated. SEM images suggest that all of the Sc3N@C78 nanostructures are homogenous microspindles (Figure 2). As the volume of isopropanol increases, both the length and diameter of Sc3N@C78 microspindles continuously decrease (Table 1). This phenomenon follows the classic crystal growth theory24, which illustrates a process combining with nucleation and growth. When the amount of isopropanol increases, the nucleation density of fullerenes increases rapidly, which leads to a faster concentration drop. Therefore, the growing time along the length decreases,


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and thus Sc3N@C78 microspindles become shorter. The diameter of Sc3N@C78 microspindles also decreases for the same reason25,26.

Figure 2. SEM images of Sc3N@C78 microstructures grown under different volume ratios of toluene to isopropanol at room temperature. (a) 1:1, (b) 1:2 and (c) 1:2.5.

Under the optimized conditions that the concentration of Sc3N@C78 in toluene is 0.4 mg/mL and the volume ratio of toluene/isopropanol is 1:2, Sc3N@C78 microspindles exhibit uniform appearances. Accordingly, we focus on this sample to perform the 9 ACS Paragon Plus Environment


following systematic characterizations. X-ray diffraction (XRD) (Figure 3) was first conducted to characterize the crystal structures of the as-obtained Sc3N@C78 microspindles. The XRD diffraction peaks corresponding to the (210), (300) and (102) planes confirm that the crysatals belong to the hexagonal system with calculated lattice

(210)

parameters of a=33.2 Å and c=18.03 Å.

5

10

15

(305)

(303) (600)

(300)

(102)

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

25

30

35

2 (Cu-K)/

Figure 3. X-ray diffraction (XRD) pattern of Sc3N@C78 microspindles.

High-resolution transmission electron microscopy (HR-TEM) image (Figure 4) of Sc3N@C78 microspindles shows a clear lattice image with the distances between the two adjacent planes of 8.8 Å and 9.2 Å, which could be assigned to the d-spacing of the


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(102) and (022) crystalline planes, respectively. The growth direction is thus revealed to be along the [010] direction. The selected area electron diffraction (SAED) pattern gives the (200), (111) and (-111) planes with corresponding d-spacings of 13.28, 13.53 and 12.28 Å, respectively, which are consistent with the XRD results.

Figure 4. HR-TEM image and (inset) SAED pattern of a Sc3N@C78 microspindle.

Absorbance / 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


b

a 400

600

800

1000

1200

Wavelength / nm



Figure 5. UV-vis-NIR absorption spectra of (a) Sc3N@C78 in toluene and (b) Sc3N@C78 microspindles dispersed in isopropanol.

The UV-vis-NIR absorption spectrum of Sc3N@C78 microspindles dispersed in isopropanol is shown in Figure 5 along with that of Sc3N@C78 in toluene for comparison.27 Sc3N@C78 microspindles display broad and enhanced absorptions from ultraviolet to visible regions that are much stronger than those of Sc3N@C78 in toluene. It is suggestive that the spindle-like structures of Sc3N@C78 microparticles are more suitable for enhancing the electron disturbance and migration between the conjugated molecules.

20

Photocurrent Density (μA/cm2)

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a b

15

10

5

0

20

40

60

80

100

Time / s


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Figure 6. Photocurrent responses of Sc3N@C78 microspindle under ultraviolet (313 nm, a: solid line) and visible light (400–780 nm, b: dashed line) irradiation. Conditions: 0.1 M KCl electrolyte solution under 1 V bias voltage.

By far, studies based on photodetector performances of EMFs are quite limited. Only a few researches have been reported such as Dy@C82 based on its Langmuir-Blodgett (LB) films28, Lu2@C82 nanorods19 and Sc3N@C80 nanorods29. In this work, the photoelectric conversion properties of Sc3N@C78 microspindles are studied. It is obvious that in both visible and ultraviolet regions, the film of microspindles display fast photoresponses to each on-off signal (Figure 6). Photocurrent responses of Sc3N@C78 microspindles film under ultraviolet (313 nm) and visible light (400–780 nm) are calculated to be 15.5 μA/cm2 and 6 μA/cm2, respectively, which is incredibly higher than the Sc3N@C80 nanorods (initial current density is 96 nA/cm2)29. Akasaka and coworkers have demonstrated that the charge transport properties of metallofullerene-solids are highly dependent on the electronic configurations of the EMF-molecules. For instance, the thin film of Sc3C2@C80 exhibits a high electron mobility under normal temperature and atmospheric pressure which is 2 orders of magnitude higher than the mobility of Sc3N@C80-film, because the former EMF has an open-shell electronic configuration30. Accordingly, we attribute the superior charge transport 13 ACS Paragon Plus Environment


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performance of Sc3N@C78-microspindles over that of Sc3N@C80-nanorods to the nature of the corresponding EMFs. Though both are close-shell molecules, Sc3N@C78 has a smaller optical bandgap (1.24 eV) than Sc3N@C80 (1.53 eV), as deduced from their UV-vis-NIR absorption spectra.31 Thus, the novel Sc3N@C78-microspindles are demonstrated to facilitate efficient charge carrier transport, which suggests its potential application in photoelectric conversion.

Conclusions

In summary, single crystalline Sc3N@C78 microspindles have been successfully prepared by LLIP method. The length and diameter of the microspindles can be well controlled by varying the concentration of Sc3N@C78 and the volume ratio of good to poor solvents. The hexagonal crystal structure of Sc3N@C78 microspindles show strong absorptions from ultraviolet to visible regions over the Sc3N@C78 solution. Finally, the Sc3N@C78 microspindles show fast photocurrent responses under both visible and ultraviolet light irradiation, because of the efficient charge carrier transport in the crystals, illuminating potential applications for photoelectric purposes.


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ASSOCIATED CONTENT

Supporting Information

Mass spectrum, HPLC profile and UV-vis-NIR absorption spectra with different concentrations of purified Sc3N@C78. ORTEP drawing of Sc3N@D3h(5)-C78 •CoII(OEP).

AUTHOR INFORMATION

Corresponding Author

* E-mail: [email protected]; [email protected]

Author Contributions

These authors contributed equally.

Notes

The authors declare no competing financial interest.



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ACKNOWLEDGMENT Financial support from Natural Science Foundation of China (51672093, 21371138, 21875173) is greatly acknowledged.

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Controllable synthesis of Sc3N@C78 microspindles with excellent

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