Crumpled Nitrogen-Doped Graphene-Wrapped Phosphorus

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Crumpled Nitrogen-doped Graphene Wrapped Phosphorus Composite as a Promising Anode for Lithium-Ion Batteries Xingxing Jiao, Yangyang Liu, Tongtong Li, Chaofan Zhang, Xieyu Xu, Olesya Kapitanova, Cheng He, Bing Li, Shizhao Xiong, and Jiangxuan Song ACS Appl. Mater. Interfaces, Just Accepted Manuscript • DOI: 10.1021/acsami.9b08915 • Publication Date (Web): 02 Aug 2019 Downloaded from pubs.acs.org on August 2, 2019

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ACS Applied Materials & Interfaces

Crumpled

Nitrogen-doped

Graphene

Wrapped

Phosphorus

Composite as a Promising Anode for Lithium-Ion Batteries Xingxing Jiao a, Yangyang Liu a, Tongtong Li a, Chaofan Zhang a, Xieyu Xu c, Olesya O. Kapitanova c, Cheng He a, Bing Li a*, Shizhao Xiong a,b, Jiangxuan Song a,* a

State Key Laboratory for Mechanical Behavior of Materials, Xi'an Jiaotong

University, Xi'an 710049, China b

Department of Physics, Chalmers University of Technology, SE 412 96, Gothenburg,

Sweden c

Lomonosov Moscow State University, Leninskie 1, Moscow 119991 Russia

*Corresponding

author.

E-mail

address:

[email protected]

(J.

Song),

[email protected] (B. Li)

Abstract Red phosphorus (P) has recently gained wide attention due to the high theoretical capacity of 2596 mAh/g, which has been regarded as promising anode material for lithium-ion batteries (LIBs). However, the actual application of red P in LIBs is hampered by the huge expansion of volume and low electronic conductivity. Herein, we design a kind of red phosphorus/crumpled nitrogen-doped graphene (P/CNG) nanocomposite with high capacity density and great rate performance as anode material for LIBs. This anode material was rationally fabricated through scalable ball-milling method. The nanocomposite structure of P/CNG improves the electron conductivity and alleviate volume change of raw red P because of the three-dimension (3D) framework and massive defects and active sites of CNG sheets. As expected, the P/CNG composite shows excellent electrochemical performances, including high capacity (2522.6 mAh/g at 130 mA/g), remarkable rate capability (1340.5 mAh/g at 3900 mA/g), and great cyclability (1470.1 mAh/g at 1300 mA/g for 300 cycles). This work may provide broad prospects for a great rate performance of P-based anode material for LIBs. 1

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Keywords: Lithium-ion batteries, anode, phosphorus, nitrogen-doped graphene, P-OC bond

Introduction Lithium ion batteries (LIBs), which have been regarded as the main green energy resources of portable electronic devices, have been gradually applied to electric vehicles, drones and smart devices 1-9. In recent years, many possible alternatives have been explored for high-energy-density LIBs, including carbon (C) anodes 10-14, alloyed anodes

15-17

as well as titanium (Ti)-based anodes

18-20.

However, the development of

LIBs has been soaked into the bottleneck for the limited energy density, which is less than 400 Wh/kg 21. Thus, there exists a huge demand to explore the high-capacity anode materials to meet the rapid growing practical demand. Phosphorus (P) has been widely considered as the perspective anode material for next generation LIBs because the red P can deliver ultrahigh theoretical capacity density of 2596 mAh/g 22. Yet, the actual utilization of red P in LIBs severely hampered by the unsolved issues, including poor electronic conductivity (1×10-14 S/cm) of raw P and huge volume change during the electrochemical cycling

23-27.

Therein, poor

electronic conductivity leads to sluggish kinetic for electrochemical reaction and thus low specific capacity. Furthermore, huge volume change triggers the collapse of electrode integrity, pulverization of active materials, separation between active materials and conductive additives as well as breakdown of fragile solid electrolyte interphase (SEI). Those changes of electrode structure invariably result in rapid capacity decaying and lower Coulombic efficiency (CE) of P anode. For promoting the utilization of red P in high-energy-density LIBs, combining with high electronic conductive materials, like C-based materials, are the promising strategies to improve the capacity and cyclic performance

26, 28-29.

Recently, massive methods have been

developed to fabricate P/C hybrid anode, such as mechanical ball-milling

23, 26, 30-32,

vaporization condensation 24, 33-36, carbothermic reduction 12, 26, 28-29 and other synthetic methods 12, 37-38. However, the reversible capacity of P/C composites at higher current density is still 2


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insufficient due to the sluggish kinetics of Li-ion migration. As previously reported, the nitrogen-doped carbon (NC) material can enhance highly conductive pathways of electrons in electrodes due to its heteroatomic defects 34, 39. Moreover, 3D framework can alleviate volume change of red P for enhanced cyclic stability

40-41.

Herein, we

design a nanostructured P based composite that used as high-capacity anode material for LIBs, using ball-milling process with red P and CNG. In this work, CNG works as conductive matrix with 3D framework and large surface-area structure to improve electron conductivity and alleviate volume expansion of P. Therefore, this composite anode rich of massive defects and active sites enables enhanced rate capability and cyclability. The synthesis procedure of P/CNG composite is displayed in Figure 1. The highly crumpled NG sheets were prepared through an efficient and facile strategy 42-43. During the fabricating process, the graphene oxide (GO) is firstly fabricated as a precursor via modified Hummer’s method. The cyanamide is added into the solution of GO, which is used as N source and porogen. The P/CNG composite was obtained through a scalable ball-milling process with different weight ratio of red P and CNG. (See Supporting Information for details).

Figure 1. Schematic illustration for the preparation procedure of P/CNG) composite. The morphology of the CNG sheets, pristine red P and the as-prepared P/CNG composite was carried out through field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HRTEM), as shown 3



in Figure 2. The FESEM image of the pristine red P illustrates an irregular microstructure with about 50 μm in size (Figure 2a). The SEM image of CNG sheets shows its highly crumpled structure with massive wrinkles and folded regions (Figure 2b and Figure S1). The obtained CNG sheets display many crumples while maintaining the 2D sheet-like structure and are composed of a few layers of graphene sheets, as seen in HRTEM image (Figure 2c). Moreover, the corresponding energy dispersive X-ray spectrometry (EDS) elemental mapping demonstrates that the nitrogen element is distributed uniformly in the highly crumpled NG sheets (Figure S2). Furthermore, Brunauer-Emmett-Teller (BET) speciﬁc surface area and Barrett-Joyner-Halenda (BJH) pore volume of CNG, which can be obtained through nitrogen adsorption/desorption isotherm, are 775.94 m2/g and 5.4 cm3/g respectively. The narrowness of the steep and nearly parallel hysteresis loop of the adsorption as well as desorption branches indicate that the CNG sheets have good pore connectivity (pore size: 2 to 50 nm) (Figure S3). After ball-milling of red P and CNG sheets, as-prepared P/CNG composite exhibits much smaller size than red P, which is around 100 nm (Figure 2d). In addition, the P/CNG composite has a low surface area (15.83 m2/g) (Figure S4), which is due to closely contact of nanoscale P particles and CNG, which generated microscale composite finally. TEM images illustrated that the CNG sheets cling on the surface of P nanoparticles (Figure S5). As shown in Figures 2e-h, the HRTEM image and corresponding EDS elementary mapping of as-prepared P/CNG composite show that CNG sheets and red P are uniformly mixed, which can highly enhance the electronic and ionic conductivity. Moreover, the CNG sheets with 3D structure can relieve the stress that come from the volume change of red P during charging/discharging process 42-43.

4


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Figure 2. Morphology of the CNG sheets and P/CNG composite. (a) FESEM image of the pristine P. (b-c) FESEM and HRTEM images of CNG sheets. (d) FESEM image of prepared P/CNG composite. HRTEM image (e) and corresponding EDS elemental (f-h) mapping of the prepared P/CNG composite. In the XRD patterns (Figure 3a), the CNG sheets shows two peaks near 25° and 45°, corresponding to the low degree of graphitization 44-45. As for red P, three peaks at 15°, 34° and 55° are detected, implying a medium-range ordered structure 23, 34, 46. Whereas, XRD pattern of the P/CNG composite only shows a broad peak without the abovementioned peaks, indicating that P/CNG composite has amorphous structure after ballmilling process. In addition, selected area electron diffraction delivers few light spots, demonstrating that there is only a small part of nanocrystal P, which is further confirmed the amorphous structure of the P/CNG composite (Figure S6). The Raman of CNG sheets in Figure 3b displays two peaks that located at 1354 and 1565 cm-1 which represent D band and G band. Next, IG/ID (the ratio of the intensity of G band and D band) was calculated to account for the degree of graphitization, integrating the area of the peaks in the patterns. While IG/ID (≈0.68) of P/CNG composite was lower than that of the CNG sheets (IG/ID≈0.86), indicating a decreased graphitization degree.

5



Figure 3. Chemical structure of P/CNG composite. (a) XRD and (b) Raman patterns of the pristine P, CNG sheets and P/CNG composite. (c) FT-IR spectra of the pristine P, and P/CNG composite. High resolution XPS spectra of (d) the pristine P and (e) P/CNG composite; (f) The schematic diagram of the structure of the P/CNG composite. Furthermore, we employed FT-IR and X-ray photoelectron spectroscopy (XPS) to uncover the interaction between red P and CNG sheets. Figure 3c shows the two characteristic peaks that located at 1156 cm-1 (P=O) and at 1082 cm-1 (P-O) for the pristine red P, which are attributed to inevitable oxidation when it is exposed in air 23, 46.

Moreover, the peak at 1005 cm-1 represents the P-O-C bond of P/CNG composite.46.

XPS spectrum(Figure S7) of N 1s in CNG shows three peaks that located at 398.38 eV, 399.76 eV and 401.35 eV, representing pyridinic N (N-5), pyrrolic N (N-6) and quaternary N (N-Q) respectively 44. As reported before, N-doping can introduce defects, which can change the distribution of charge density of the surface to enhance electronic conductivity of C sheet

47.

Moreover, N-5 and N-6 sites are considered as

electrochemical-active spots for preferred adsorption of cations for its changed charge density

44, 48-50.

Thus, N-doped graphene that contains N-5 and N-6 defects spots

embrace high electronic and ionic conductivity. Besides, no additional species can be found in the P/CNG composite, indicating that ball-milling process exhibits no effect on the type of nitrogen. As shown in Figure 3d, P2p spectrum of the pristine P presents two main peaks at 130 eV and 134.5 eV, which are attributed to elementary P and phosphates, respectively 51. An additional main peak shown in the P/CNG composite is 6


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regarded as the P-O-C bond (131.1 eV, Figure 3e), being consistent with the results from FT-IR. On account of above-mentioned results, the structure of P/CNG composite is illustrated in Figure 3f.

Figure 4. Electrochemical performance of P/CNG composite. (a) The CV curves of P/CNG composite at scan rate of 0.05 mV/s. (b) Typical discharge-charge voltage profiles of the P/CNG composite at a constant current density of 780 mA/g. (c) Cycling performance and (d) Coulombic efficiency of P/CNG composite, P/CNG mixture, red P, and CNG sheets at current density of 780 mA/g. (e) The long-term cycling performance of P/CNG composite at a current density of 1300 mA/g for 300 cycles. As shown in Figure S8a, high content of CNG (P:CNG = 6:4) results in the low capacity due to the low theoretical capacity of CNG (~ 300 mAh/g), and high content of P (P:CNG = 8:2) leads to the poor performance due to pulverization of P particles and inferior electronic conductivity. These results reveal that the P/CNG composite with the weight ratio of 7:3 exhibits the best cycle stability. As shown in Figure S9, the weight loss of composites within 400-600 °C demonstrates the content of P. The content 7



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of P in P/CNG with ratios of 8:2, 7:3, and 6:4 is 72%, 63% and 53%. When the P percentage value is 63%, the P/CNG composite presents the optimized performance. Figure 4a presents cyclic voltammetry (CV) curves of P/CNG composite (see details in supporting information). A broad peak around 0.3 V is only detected during the first cathodic scan and disappears in the subsequent cathodic scans, which is resulted from the activation process, alloying reaction between Li and P

32.

Moreover, the first

cathodic scan delivers a small reduction peak located at 1.0 V, which is related to the generation of SEI. The main cathodic peak around ~0.6 V corresponds to the continuous lithiation process to form LixP (x=1-3)28. The charge curves (Figure 4b) contain a strong peak about 1.0 V with a shoulder peak around 1.15 V and a slightly inclined plateau from 1.3 V to 2 V, which should be corresponding to the delithiation of different LixP compounds. Figures 4c-d displays the electrochemical performances of P/CNG composite, P/CNG mixture, red P and CNG electrodes at 780 mA/g, which includes cycling performances and the CE. Pristine red P delivers the capacity over 700 mAh/g with initial CE of 22% and then the capacity rapidly decreases to below 50 mAh/g. In order to make better comparison, the P/CNG mixture was fabricated using the mixture of the ball-milled red P and CNG (7:3 in weight). P/CNG mixture displays the first cycle capacity of 1973 mAh/g with the ICE of 20.6%. Besides, it exhibits poor cycling performance with low CE (90%), fading to 50 mAh/g within 5 cycles. Impressively, the P/CNG composite anode exhibits great cyclic performance, which can deliver reversible discharge capacity of 2044.2 mAh/g at 780 mA/g with the ICE of 87.73% over 100 cycles. Even at 1300 mAh/g, the P/CNG composite could deliver capacity of 1706.4 mAh/g and holds a high capacity of 1470.5 mAh/g beyond 300 cycles (Figure 4e). The excellent cycling performance demonstrates that the volume expansion of P is effectively alleviated, remaining a stable electrode structure. Furthermore, as shown in Figure S10, the thickness of discharged electrode is about 8.58 um, and that of charged electrode is 7.32 um, which shows negligible change during charge/discharge process. From the SEM images, we suggest that P/CNG composite exhibits little volume change, which can alleviate volume expansion.

8


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Figure 5. (a) The rate performance of the P/CNG composite and P/CNG mixture at the various current densities from 780 to 3900 mA/g. (b) The comparison of the rate capability of P/CNG composite with the reported materials in LIBs. To further confirm the high rate capability, P/CNG composite and P/CNG mixture were tested at various current densities from 780 to 3900 mA/g (Figure 5a). Obviously, the P/CNG composite presents outstanding rate capability. The capacity of P/CNG composite is 2044.2, 1706.4, 1607.3, 1489.6 and 1340.5 mAh/g at 780, 1300, 1950, 2600 and 3900 mA/g, respectively. When the current density returned to 780 mA/g after 50 cycles, the capacity density was even up to 1801.2 mAh/g. It is worth mentioned that the results of P/CNG composite are much better than those of P/CNG mixture. As shown in Figure 5b, P/CNG composite displays the best rate performance, which is several times higher than those of reported P-based anodes either or both at 100 mA/g or at 3900 mA/g 28, 37, 52-54. We suggest that the rate performance of P/CNG composite are contributed to the stable 3D carbon matrix with ultrahigh mixed ionic and electronic conductivities.

9



Figure 6. Li-adsorption in different N-doped structures by theoretical modeling. Top view of electron density differences of Li-absorbed structures without N-doping, including (a) C-P, (b) C-5 and (c) C-6. Top view of electron density differences of Liabsorbed structures with single N-doping, including (d) N-Q, (e) N-5 and (f) N-6. Top view of electron density differences of Li-absorbed structures with double N-doping, including (g) N-Q, (h) N-5/N-6 and (i) N-6/N-6. The isosurfaces are the 0.02 electron bohr. Brown, silver, and green balls stand for C, N, and Li respectively. (j) Nyquist plots of P/CNG composite and P/CNG mixture electrodes in the discharged state. (k) The GITT patterns of P/CNG composite and P/CNG mixture electrodes. (l) Diffusion coefficients of Li-ion that calculated from GITT patterns. For understanding the rate capability and cyclability of P/CNG composite anode, we carried out a detailed theoretical investigation about Li-adsorption energy (ΔEa) via density functional theory (DFT). Among this DFT calculation, two kinds of carbon 10


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defect (C-5, C-6) and three kinds of N-doped models (N-5 for pyrrolic-N, N-6 for pyridinic-N and N-Q for quaternary N) were conducted to reveal the effect of N-doping on Li-adsorption 44. Within DFT simulation, a single Li atom was put in the center of holes of defects after optimizing geometry structures (Figures 6a-i). The ΔEa value (1.572 eV) of Li adsorbing on perfect graphene (P-C) become more negative (-4.509 eV for C-5 and -4.182 eV for C-6) after introducing defects. When Li atom adopting at defect with one N-doping sties, the ΔEa for N-5 and N-6 is -4.834 eV and -4.298 eV respectively. However, the ΔEa for N-Q is just -0.836 eV. We further calculated the Li adsorption energy at defect sites with two N atom doping (-0.7855 eV for two N-Q, 5.095 eV for N-5/N-6 and -4.557 eV for N-6/N-6). The distinct of values of ΔEa indicates N-5 and N-6 deliver stronger adsorption effect toward Li atom. In addition, ΔEa become more negative with the increased degree of N-doping, demonstrating that N-5 and N-6 defects enhance adsorption of Li atom in C-materials

55.

Based on the

calculation results above, we suggest that N-doping can introduce more electrochemical-active sites, pyrrolic-N and pyridinic-N, which are beneficial for the rate capability and cyclability performance. To obtain more evidences for the improved cyclic and rate performance of P/CNG composite, electrochemical impedance spectra (EIS) and galvanostatic intermittent titration technique (GITT) were conducted to reveal the kinetics of Li-ion migration. As shown in the inset of Figure 6j, the Warburg impedance (Ws) is corresponding to the Li-ion diffusion through the active material or electrolyte. The value of chargetransfer resistance Rsf+ct in the P/CNG composite (53.6 Ω) is much smaller than that of the P/CNG mixture (253.7 Ω), resulting from that the nanoscale P particles closely contact with CNG via chemical bond. In addition, the diffusivity of Li-ions in P/CNG composite is higher than that in P/CNG mixture, which is reflected from higher lowfrequency slope angle for P/CNG of 85.26° (36.39° for P/CNG mixture). The overall ionic conductivity of P/CNG composite is also improved by the combination of red P and CNG sheets, demonstrated by the GITT (Figure 6k). The values of D are calculated based on potential (Figure 6l) and the details of calculation can be seen in Supplementary Information. Obviously, the D of the P/CNG composite is much higher 11



than that of P/CNG mixture in all lithiation states. It suggests that the diffusion of Liion in P/CNG composite is much faster than that in P/CNG mixture, due to the more N-doped defect sites in composite derived from the crumple structure of CNG, endowing P/CNG composite great rate performance. In summary, we report an amorphous P/CNG nanocomposite as anode material for LIBs, which is fabricated by the simple ball-milling process. In this composite anode, CNG works as conductive matrix to facilitate electron and ion transportation and alleviate volume expansion of P because of its 3D framework, large surface-area structure with massive defects and increased active sites. The theoretical investigation about Li-adsorption energy (ΔEa) clearly accounts for the advantage of N doping, which mainly result from the pyrrolic N and pyridinic N. As a consequence, the P/CNG composite exhibits a high Li-ions storage capacity of 2522 mAh/g at 130 mA/g, excellent rate capability of 1340.5 mAh/g at high current density of 3900 mA/g and enhanced cyclability of 1470.1 mAh/g at 1300 mA/g over 300 cycles. Furthermore, the P/CNG composite with excellent electrochemical performance, lays a good foundation to improve the utilization of low-cost anode materials in the actual application.

Acknowledgment This work is supported by the National Natural Science Foundation of China (No. 51602250, No. 51802256 and No. 21875181) and 111 Project 2.0 (BP2018008). We would like to thank Mr. Ren and Miss Liu at Instrument Analysis Center of Xi’an Jiaotong University for their assistance of SEM and XPS analysis.

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TOC

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Crumpled Nitrogen-Doped Graphene-Wrapped Phosphorus

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