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Conflicts of interest
There are no conflicts to declare.
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Journal Name
(c)
(b)
(a)
(d)
Intensity
Transmittance
(e)
500
1000
1500
1600
–1
Raman shift / cm
1200
800
Wavenumber / cm
400
–1
Fig. 1 (a) Molecular structure of DFP− in NaDFP determined at 113 K. Coordination environments of (b) Na1 and (c) Na2 in NaDFP [symmetry code:
(i) x+1, y−1, z; (ii) −x+2, −y, −z+2; (iii) −x+2, −y, −z+2; (iv) x+1, y, z; (v) x, y−1, z+1; (vi) −x+1, −y, −z+2; (vii) −x+2, −y+1, −z+1]. Thermal ellipsoids are
shown at the 50 % probability level. (d) Raman and (e) IR spectra of NaDFP.
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500
1.5
(a) neat
(b) neat
short circuit
0.5
0.0
-0.5
300
200
100
-1.0
-1.5
50
100
150
200
250
100
Time
Time/ /hh
400
500
(d) 0.5 wt% NaDFP
short circuit
400
–ImZ / ohm
Voltage / V
1.0
0.5
0.0
-0.5
0 cycle
3 cycles
cycle
50 cycles
cycle
100 cycles
cycle
400 cycles
cycle
300
200
100
-1.0
50
100
150
200
250
100
200
300
400
500
ReZ / ohm
Time // hh
Time
1.5
500
(e) 1 wt% NaDFP
1.0
(f) 1 wt% NaDFP
00 cycle
cycle
33 cycles
cycle
50
50 cycles
cycle
100
100 cycles
cycle
400
400 cycles
cycle
400
–ImZ / ohm
0.5
0.0
-0.5
300
200
100
-1.0
-1.5
300
500
(c) 0.5 wt% NaDFP
-1.5
200
ReZ / ohm
1.5
Voltage / V
0 cycle
3 cycles
50 cycles
100 cycles
400
–ImZ / ohm
Voltage / V
1.0
50
100
150
200
250
100
Time
Time
/ h/ h
200
300
400
500
ReZ / ohm
Fig. 2 Voltage profiles and Nyquist plots of the Na/Na symmetrical cells during galvanostatic Na metal deposition/dissolution cycles using 1 M NaPF6-EC/DMC (1:1, v:v)
electrolute with (a, b) 0 wt% NaDFP (neat), (c, d) 0.5 wt% NaDFP and (e, f) 1 wt% NaDFP. Current density: 1 mA cm‒2. (See Fig. S6 in ESI† for voltage profiles and Nyquist
plots with 0.5 wt% FEC and 3 wt% FEC)
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2.0
1.5
1.0
0.5
2nd
1.5
1.0
0.5
0.0
1st
50 100 150 200 250 300 350
2nd
Capacity / mAh g–1
(f) neat
(d)
1st
2nd
0.52 V
-2
0.0
0.5
1.00 V
1.0
Voltage / V
(c) 1 wt% NaDFP
1.5
1.0
0.5
0.0
1st
50 100 150 200 250 300 350
2nd
Capacity / mAh g–1
1.5
dQ/dV/ Ah
Ahgg–1–1VV–1–1
dQ/dV
dQ/dV/ Ah
dQ/dV
Ahgg–1–1VV–1–1
2.0
(g) 0.5 wt% NaDFP
(e)
1st
2nd
0.51 V
-2
0.0
0.5
0.89 V
1.0
1st
50 100 150 200 250 300 350
Capacity / mAh g–1
1.5
Voltage / V
Ah gg–1–1VV–1–1
dQ/dV
dQ/dV/ Ah
0.0
(b) 0.5 wt% NaDFP
Voltage / V
(a) neat
Voltage / V
Voltage / V
2.0
Journal Name
(f)
(h) 1 wt% NaDFP
1st
2nd
0.50 V 0.83 V
-2
0.0
0.5
1.0
1.5
Voltage / V
Fig. 3 Charge-discharge curves and the corresponding differential capacity-voltage (dQ/dV) plots of the Na/HC cells using 1 M NaPF6-EC/DMC (1:1, v:v) electrolyte with (a, d) 0 wt%
NaDFP (neat), (b, e) 0.5 wt% NaDFP and (c,f) 1 wt% NaDFP. Current density: 25 mA g−1. Cut-off voltage: 0.0051.5 V. (See Fig. S7 in ESI† for the data with 0.5 wt% FEC and 3 wt% FEC .
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120
(a)
400
100
300
25
50
80
25
100
60
250
200
40
500
100
Neat
0.5 wt% NaDFP
1 wt% NaDFP
10
20
Coulombic efficiency / %
Capacity / mAh g–1
Journal Name
20
15
120
(b)
400
100
300
80
25
25
50
60
200
100
100
Neat
0.5 wt% FEC
3 wt% FEC
40
250
500
10
15
20
Coulombic efficiency / %
Capacity / mAh g–1
Cycle number
20
Cycle number
Fig. 4 Rate capability of the Na/HC cells using 1 M NaPF6-EC/DMC (1:1, v:v) electrolyte with (a) 0 wt% NaDFP (neat), 0.5 wt% NaDFP and 1 wt% NaDFP and (b) 0 wt%
FEC (neat), 0.5 wt% FEC and 3 wt% FEC. Cut-off voltage: 0.0051.5 V. Electrolytes: Current densities are shown in mA g −1.
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98
150
96
100
94
50
92
90
500
200
300
400
98
150
96
100
94
50
92
90
500
100
Capacity / mAh g–1
Cycle number
200
102
250
100
200
98
150
96
100
94
50
92
400
300 (c) 1 wt% NaDFP
102
250
100
200
98
150
96
100
94
50
92
50
100
150
200
Cycle number
250
90
300
100
200
300 (e) 3 wt% FEC
102
250
100
200
98
150
96
100
94
50
92
300
400
90
500
Cycle number
Cycle number
300 (d) 0.5 wt% FEC
300
Capacity / mAh g–1
100
100
200
Coulombic efficiency / %
102
250
Coulombic efficiency / %
200
300 (b) 0.5 wt% NaDFP
50
100
150
200
250
90
300
Coulombic efficiency / %
100
Capacity / mAh g–1
102
250
Capacity / mAh g–1
300 (a) neat
Coulombic efficiency / %
Journal Name
Coulombic efficiency / %
Capacity / mAh g–1
ARTICLE
Cycle number
Fig. 5 Cycle performance of the Na/HC cells using 1 M NaPF6-EC/DMC (1:1, v:v) electrolyte with (a) 0 wt% NaDFP (neat), (b) 0.5 wt% NaDFP, (c) 1 wt% NaDFP, (d) 0.5
wt% FEC, and (e) 3 wt% FEC. Current density: 100 mA g −1. Cut-off voltage: 0.0051.5 V. (See Fig. S8 in ESI† for the corresponding Charge-discharge curves and dQ/dV
plots)
12 | J. Name., 2012, 00, 1-3
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Journal Name
1 cycle
3 cycles
10 cycles
20 cycles
100
80
10
120
100
10
15
60
1 cycle
3 cycles
10 cycles
20 cycles
10
120
100
80
10
15
60
40
20
20
20
20
40
60
80
100 120 140
40
60
80
100 120 140
10
15
20
40
60
80
100 120 140
ReZ / ohm
(f) schematic drawing
(e) 3 wt% FEC
300
10
80
350
(f) 0.5 wt% FEC (large view)
300
200
15
10
150
15
1 cycle
3 cycles
10 cycles 10
20 cycles
250
10
15
100
–ImZ / ohm
1 cycle
3 cycles
10 cycles
20 cycles
250
50
20
ReZ / ohm
ReZ / ohm
350
1 cycle
3 cycles
10 cycles
20 cycles
60
40
(c) 1 wt% NaDFP 15
80
40
–ImZ / ohm
140
200
60
150
100
10
15
–ImZ / ohm
–ImZ / ohm
120
140 (b) 0.5 wt% NaDFP15
15
–ImZ / ohm
(a) neat
–ImZ / ohm
140
ARTICLE
40
Rct
20
50
50
100 150 200 250 300 350
ReZ / ohm
Rh
50
100 150 200 250 300 350
ReZ / ohm
20
40
60
80
ReZ / ohm
Fig. 6 Nyquist plots of the HC/HC symmetric cells using 1 M NaPF6-EC/DMC (1:1, v:v) electrolyte with (a) 0 wt% NaDFP (neat), (b) 0.5 wt% NaDFP, (c) 1 wt% NaDFP, (d)
0.5 wt% FEC, and (e) 3 wt% FEC, and (h) the schematic drawing of the fitting parameters for the arc. Frequency range of 100 kHz−10 mHz. AC amplitude: 10 mV. See
Table S7 in ESI† EIS parameters)
Rbu
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Journal Name
NaDFP
(a) F 1s
NaDFP
(b) O 1s
NaDFP
(c) P 2p
2p1/2
P–O
NaxPFy
NaF
/ NaxPFyOz
2p1/2
C–O C=O
P–F
2p1/2 2p3/2
C–O C=O
688
684
Binding energy / eV
100 F 1s
P–O
neat
NaF
680 540
NaxPFy /
NaxPFyOz
NaF
80
2p1/2 2p3/2
P–F
525 142
535
530
Binding energy / eV
C–O
C=O
P–O
O 1s
P–O
138
134
Binding energy / eV
P 2p
130
P–F
P–O
60
neat
NaDFP
neat
FEC
NaDFP
neat
FEC
68%
32%
71%
29%
4%
96%
20%
48%
58%
39%
64%
36%
88%
FEC
32%
12%
20
99%
40
1%
Ratio / %
2p3/2 2p
1/2 2p3/2
neat
23%
(d)
FEC
NaF
77%
692
P–O
FEC
neat
NaxPFy
/ NaxPFyOz
2p1/2
P–F
C–O C=O
FEC
NaxPFy
/ NaxPFyOz
2p3/2
2p3/2
NaDFP
Fig. 7 X-ray photoelectron spectra of the SEI layers formed on the HC electrodes after 20 cycles in 1 M NaPF6-EC/DMC (1:1, v:v) electrolyte with 0 wt% NaDFP (neat), 1
wt% NaDFP and 3 wt% FEC additives in the (a) F 1s, (b) O 1s, and (c) P 2p regions, and (d) SEI component ratios (see Table S8 in ESI† for the binding energy of the peaks).
14 | J. Name., 2012, 00, 1-3
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