Electrochemistry Application — Operando Raman and ex situ characterization of an iron-based conductive MOF as a negative electrode in Li-ion batteries

4 measurement groups · 19 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

Cyclic voltammetry (CV)

Voltammetry

Fe-HHTP composite Li-ion battery electrode on copper foil · Electrode

Autolab M204; voltage range 0.1-3.0 V vs Li/Li+; first three cycles at 0.1 mV s-1 and third scan at scan rates 0.1-10 mV s-1.

Atmosphere: assembled inside Ar glovebox
Geometry: Li metal half-cell
Context: composite electrode using pristine Fe-HHTP active material
Measurement source: 10 · 4.3 Electrochemical measurements and operando Raman · Figure 6a,b; Figures S9-S10

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
CV activation timescale	fully activating the electrode requires approximately 30 CV scans with EIS measurements, less than 225 galvanostatic cycles	—	—	Text Approximate	10 · Figure S9 · Figure S9
Anodic CV peak assignments	main anodic peaks at 2.15 V (C=O recovery) and approximately 1 V (C-C to C=C), plus approximately 0.3 V shoulder assigned to delithiation from MOF layers	—	—	Text Approximate	7 · 2.3 Study of the electrochemical mechanism · Figure 6a; Figure S9
First cathodic CV peak potentials	1.47, 0.65, 0.56 and 0.1 V vs Li+/Li	—	—	Text Exact Reported	7 · 2.3 Study of the electrochemical mechanism · Figure 6a
CV scan-rate range	0.1 to 10 mV s-1	—	—	Text Range	7 · 2.3 Study of the electrochemical mechanism · Figure 6b; Figure S10

Electrochemical impedance spectroscopy during CV cycling

Impedance spectroscopy Voltammetry

Fe-HHTP composite Li-ion battery electrode on copper foil · Electrode

Autolab M204; 1 MHz to 10 mHz; EIS at various potentials during CV cycles; equivalent circuits fitted with Z-view.

Atmosphere: assembled inside Ar glovebox
Geometry: Li metal half-cell
Context: composite electrode using pristine Fe-HHTP active material
Measurement source: 10 · 4.3 Electrochemical measurements and operando Raman · Figure 6c,d

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
EIS limiting processes	During lithiation diffusion resistance Rd dominates; during delithiation a different resistance Rr limits; Rd at 0.1 V is an order of magnitude lower than at cathodic 1.5 V	—	—	Text Qualitative	8 · 2.3 Study of the electrochemical mechanism · Figure 6c,d

Galvanostatic lithiation/delithiation cycling

Galvanostatic cycling

Fe-HHTP composite Li-ion battery electrode on copper foil · Electrode

CR2032 or Swagelok Li cells; 0.1-3.0 V vs Li/Li+; cycling performance at 355 mA g-1 in a Neware Battery Tester System.

Atmosphere: assembled inside Ar glovebox
Geometry: Li metal half-cell with Fe-HHTP composite working electrode
Context: composite electrode using pristine Fe-HHTP active material
Measurement source: 10 · 4.3 Electrochemical measurements and operando Raman · Figure 2a,c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Average active material loading	0.56 +/- 0.28 mg cm-2	0.56 mg cm-2	+/- 0.28 mg cm-2	Text Exact Reported	10 · 4.3 Electrochemical measurements and operando Raman
Maximum discharge specific capacityMarked as a best value within this paper	1142 mAh g-1 after 225 cycles at 355 mA g-1	1142 mAh g-1	—	Text Exact Reported	4 · 2.2 Electrochemical performance · Figure 2c
Capacity retention at cycle 350 relative to maximum	approximately 85% of highest measured specific capacity at cycle 350	—	—	Text Approximate	4 · 2.2 Electrochemical performance · Figure 2c
Cycle-20 lithiation/delithiation coincident capacity	approximately 230 mAh g-1 at cycle 20	230 mAh g-1	—	Text Approximate	4 · 2.2 Electrochemical performance · Figure 2a
Discharge specific capacity at cycle 7	186 mAh g-1 at 355 mA g-1, cycle 7	186 mAh g-1	—	Text Exact Reported	4 · 2.2 Electrochemical performance · Figure 2c

Galvanostatic rate capability

Galvanostatic cycling

Fe-HHTP composite Li-ion battery electrode on copper foil · Electrode

Li half-cells cycled between 0.1 and 3.0 V vs Li/Li+ at 50, 100, 200, 500, 1000, 1500 and 2000 mA g-1, then returned to 50 mA g-1.

Atmosphere: assembled inside Ar glovebox
Geometry: Li metal half-cell with Fe-HHTP composite working electrode
Context: composite electrode using pristine Fe-HHTP active material
Measurement source: 4 · 2.2 Electrochemical performance · Figure 2b,d; Figure S7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Coulombic efficiency at 500 mA g-1, cycle 18	>99%	—	lower bound	Text Range	4 · 2.2 Electrochemical performance · Figure 2d
First-cycle Coulombic efficiency at 50 mA g-1	approximately 22%	—	—	Text Approximate	4 · 2.2 Electrochemical performance · Figure 2d
Coulombic efficiency after returning to 50 mA g-1	approximately 93% in the 45th cycle	—	—	Text Approximate	4 · 2.2 Electrochemical performance · Figure 2d
Rate capacity at 1000 mA g-1	capacity close to 125 mAh g-1 at 1000 mA g-1	125 mAh g-1	—	Text Approximate	4 · 2.2 Electrochemical performance · Figure 2d; Figure S7b
Visual estimate of delithiation capacity at 100 mA g-1	approximately 245 mAh g-1 from Figure S7a	245 mAh g-1	visual estimate from plotted axis, about +/-5 mAh g-1	Visual Estimate Approximate	8 · Figure S7 · Figure S7a
Visual estimate of delithiation capacity at 1500 mA g-1	approximately 94 mAh g-1 from Figure S7b	94 mAh g-1	visual estimate from plotted axis, about +/-5 mAh g-1	Visual Estimate Approximate	8 · Figure S7 · Figure S7b
Visual estimate of delithiation capacity at 2000 mA g-1	approximately 81 mAh g-1 from Figure S7b	81 mAh g-1	visual estimate from plotted axis, about +/-5 mAh g-1	Visual Estimate Approximate	8 · Figure S7 · Figure S7b
Visual estimate of delithiation capacity at 200 mA g-1	approximately 200 mAh g-1 from Figure S7a	200 mAh g-1	visual estimate from plotted axis, about +/-5 mAh g-1	Visual Estimate Approximate	8 · Figure S7 · Figure S7a
Visual estimate of delithiation capacity at 500 mA g-1	approximately 142 mAh g-1 from Figure S7a	142 mAh g-1	visual estimate from plotted axis, about +/-5 mAh g-1	Visual Estimate Approximate	8 · Figure S7 · Figure S7a