Synthesis and Characterization of Full Concentration-gradient LiNi0.643Co0.055Mn0.302O2 Cathode Material for Lithium-ion Batteries

doi:10.7503/cjcu20170198

Abstract

Abstract:

The “two-step” method was adopted to realize the continuous gradient change of feed concentration and the gradient design of final material was derived from mathematical calculus formula. The full concentration-gradient precursor was prepared via co-precipitation method and technique of “Tubular synthesis”. The final lithiated cathode material was obtained by calcination of the mixture of as-obtained full concentration-gradient precursor and 6.5% excess LiOH·H₂O in oxygen, whose average chemical compositions was LiNi_0.643Co_0.055Mn_0.302O₂ analyzed by inductively coupled plasma-atomic emission spectrometry(ICP-AES). The LiNi_0.643Co_0.055Mn_0.302O₂ particle was nearly spherical and had the size of 5 μm in diameter with narrow particle size distribution and its tap-density was approximately 2.029 g/cm³. A well-ordered α-NaFeO₂ layer-structured LiNi_0.643Co_0.055Mn_0.302O₂ was confirmed by Rietveld refinement of X-ray diffraction(XRD), in which the lattice parameters were a=0.2877(5) nm, c=1.4242(24) nm, V=0.102088(31) nm³, respectively. Energy dispersive spectrometory(EDS) and element mapping results verified that the concentration of Ni, Co and Mn changed gradually inside out of the particle. LiNi_0.643Co_0.055Mn_0.302O₂ delivered an initial discharge capacity of 187.68 mA·h ·g^-1 and coloumbic efficiency of 84.76%. After cycling at 1C rate for 200 cycles, the discharge capacity and capacity retention of LiNi_0.643Co_0.055Mn_0.302O₂ were 146.45 mA·h ·g^-1 and 86.90%, respectively.

Key words: Co-precipitation, Full concentration-gradient, Lithium-ion battery, Cathode material

CLC Number:

O646

TrendMD:

LUO Man, JIANG Wenquan, HAN Xue, GUO Ronggui, LI Tao, YU Limin. Synthesis and Characterization of Full Concentration-gradient LiNi_0.643Co_0.055Mn_0.302O₂ Cathode Material for Lithium-ion Batteries[J]. Chem. J. Chinese Universities, 2018, 39(1): 148.

Figures/Tables 12

Fig.1 Schematic diagram of hydroxide precursor by “Tubular synthesis”

Table 1 Tap-density of precursors and corresponding lithiated oxides

Sample	Tap-density/(g·cm^-3)	Sample	Tap-density/(g·cm^-3)
811	1.911	Li-811	1.996
FCG 811-505	1.966	FCG Li-811-505	2.029
505	2.180	Li-505	2.235

Fig.2 EDS scanning results of FCG 811-505(A) and FCG Li-811-505(B) Insets of (A) and (B): EDS scanning results of element Co.

Fig.3 TEM images(A1, B1) and element mapping(A2—A4, B2—B4) of FCG 811-505(A1—A4) and FCG Li-811-505(B1—B4)(A2), (B2) element Mn; (A3), (B3) elements Mn and Ni; (A4), (B4) element Ni.

Fig.4 XRD patterns of the 811(a), FCG 811-505(b) and 505 precursors(c)

Fig.5 XRD patterns of the cathode materials Li-811, FCG Li-811-505 and Li-505(A) Comparison of three cathode materials’ XRD patterns; (B)—(D) the Rietveld refinement results of XRD patterns for Li-811, FCG Li-811-505 and Li-505, respectively.

Table 2 Lattice parameters obtained from Rietveld refinements of Li-811, FCG Li-811-505 and Li-505

Sample	a/nm	c/nm	V/nm	c/a	I₍₀₀₃₎/I₍₁₀₄₎
Li-811	0.2869(32)	1.4187(15)	0.101110(19)	4.945	1.328
FCG Li-811-505	0.2877(5)	1.4242(24)	0.102088(31)	4.950	1.216
Li-505	0.2888(17)	1.4309(9)	0.103343(11)	4.955	0.879

Table 3 Detailed Rietveld refinement data of XRD for FCG Li-811-505*

Atom	Site	z	g
Li1	3a	0.5	2.6464
Ni2	3a	0.5	0.1079
Li2	3b	0	-1.2765
Ni1	3b	0	0.8459
Co	3b	0	0.1108
Mn	3b	0	0.1000
O	6c	0.2585	1.0000

Fig.6 FESEM images of precursors 811(A), FCG 811-505(B), 505(C) and their lithiated oxides Li-811(D), FCG Li-811-505(E) and Li-505(F) Inset are the corresponding FESEM images at low magnification.

Fig.7 Initial charge-discharge curves of Li-811(a),FCG Li-811-505(b) and Li-505(c)

Fig.8 Discharge capacity of Li-811(a), FCG Li-811-505(b) and Li-505(c) at various rates cycling

Fig.9 Cycling performance of Li-811(a),FCG Li-811-505(b) and Li-505(c) at 1C rate

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Synthesis and Characterization of Full Concentration-gradient LiNi_0.643Co_0.055Mn_0.302O₂ Cathode Material for Lithium-ion Batteries

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