Electrochemistry Application — Electrochemical oxygen reduction catalysed by Ni3 (hexaiminotriphenylene)2

9 measurement groups · 39 results

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

Cyclic voltammetry double-layer capacitance scan-rate series

Voltammetry

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

Under N2 atmosphere with CV scan rates labelled 5, 20 and 50 mV s-1.

Atmosphere: N2
Geometry: Ni3(HITP)2-modified electrode
Context: pristine framework film
Measurement source: SI p.S1 · Supplementary Figure 2 · Supplementary Fig. 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
double-layer CV scan rate	20 mV s-1 trace	—	—	Figure Axis Exact Reported	SI p.S1 · Supplementary Figure 2 · Supplementary Fig. 2
double-layer CV scan rate	5 mV s-1 trace	—	—	Figure Axis Exact Reported	SI p.S1 · Supplementary Figure 2 · Supplementary Fig. 2
double-layer CV scan rate	50 mV s-1 trace	—	—	Figure Axis Exact Reported	SI p.S1 · Supplementary Figure 2 · Supplementary Fig. 2

RRDE ring/disk Faradaic efficiency analysis

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

0.10 M KOH at pH 13; potential range 0.82-0.54 V vs RHE.

Atmosphere: O2
Geometry: RRDE
Context: pristine framework film
Measurement source: main p.4 · Mechanistic insight into ORR on Ni3(HITP)2 · Fig. 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2O2 Faradaic efficiency high-potential value	100% at about 0.82 V	—	—	Text Exact Reported	main p.4 · Mechanistic insight · Fig. 4
H2O2 Faradaic efficiency low-potential value	63% at about 0.54 V	—	—	Text Exact Reported	main p.4 · Mechanistic insight · Fig. 4
%H2O2 plateau potential	about 0.75 V	—	—	Text Approximate	main p.4 · Mechanistic insight · Fig. 4

Cyclic voltammetry on modified ITO

Voltammetry

Ni3(HITP)2 thin film on indium tin oxide electrode · Electrode

Ni3(HITP)2-modified and blank ITO under N2 and O2 atmosphere.

Atmosphere: N2 or O2
Geometry: ITO electrode
Context: pristine framework film on ITO
Measurement source: SI p.S3 · Supplementary Figure 4 · Supplementary Fig. 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ITO-supported film ORR activity	same ORR activity as films on glassy carbon electrodes	—	—	Text Qualitative	main p.2 · ORR activity of Ni3(HITP)2 · Supplementary Fig. 4

Galvanostatic ORR proton order study

Galvanostatic cycling

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

Potential measured over 25 min at I = -5 uA while titrating pH 12.89 to 11.54 in 0.10 M KOH with 1.0 M HClO4.

Atmosphere: O2
Geometry: Ni3(HITP)2-modified electrode
Context: pristine framework film
Measurement source: main p.4 and p.6 · Mechanistic insight; ORR proton order study · Supplementary Fig. 14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
proton-order pH titration range	pH 12.89 to 11.54	—	—	Text Range	main p.6 · ORR proton order study · Supplementary Fig. 14
zeroth order pH region	slope of zero for dE/dpH above pH 12.80	—	—	Text Exact Reported	main p.4 · Mechanistic insight · Supplementary Fig. 14

Rotating disk electrode and rotating ring-disk electrode cyclic voltammetry

Voltammetry

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

0.10 M KOH; Pt mesh auxiliary; Hg/HgO reference; scan 5 mV s-1; 2000 rpm; N2 or O2 sparged.

Atmosphere: N2 or O2
Geometry: 5 mm glassy carbon rotating disk or RRDE with Pt ring
Context: pristine framework film on glassy carbon
Measurement source: main p.3 · ORR activity of Ni3(HITP)2 · Fig. 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ORR onset potentialMarked as a best value within this paper	0.82 V at j = -50 uA cm-2 in 0.10 M KOH	—	—	Text Exact Reported	main p.2 · ORR activity of Ni3(HITP)2 · Fig. 2
overpotential relative to Pt onset	0.18 V	—	—	Text Exact Reported	main p.2 · ORR activity of Ni3(HITP)2
Pt onset potential reference	Eonset = 1.00 V	—	—	Text Exact Reported	main p.2 · ORR activity of Ni3(HITP)2
Fig. 2 rotation rate	2000 r.p.m.	—	—	Caption Exact Reported	main p.3 · Figure 2 caption · Fig. 2
Fig. 2 CV scan rate	5 mV s-1	—	—	Caption Exact Reported	main p.3 · Figure 2 caption · Fig. 2

RRDE TOF calculation using AAS nickel quantification

Bulk elemental and compositional analysis

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

Potentiostatic RRDE disk potentials 0.807 to 0.667 V vs RHE; 20% ring collection efficiency.

Atmosphere: O2
Geometry: Glassy carbon RRDE with Pt ring
Context: pristine framework film
Measurement source: SI p.S15 · Supplementary Tables 4-6 · Supplementary Tables 4-6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
2e- ORR TOF per Ni3(HITP)2 at 0.667 V, AAS	0.457 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 5 · Supplementary Table 5
2e- ORR TOF per Ni3(HITP)2 at 0.787 V, AAS	0.0424 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 5 · Supplementary Table 5
2e- ORR TOF per Ni at 0.787 V, AAS	0.0141 electrons [Ni]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 5 · Supplementary Table 5
4e- ORR TOF per Ni3(HITP)2 at 0.667 V, AAS	0.433 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 6 · Supplementary Table 6
4e- ORR TOF per Ni3(HITP)2 at 0.787 V, AAS	0.0525 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 6 · Supplementary Table 6
4e- ORR TOF per Ni at 0.787 V, AAS	0.0175 electrons [Ni]-1 s-1	—	—	SI Table Exact Reported	SI p.S15 · Supplementary Table 6 · Supplementary Table 6
AAS RRDE nickel sites	1.26199e16 Ni sites; catalyst loading 5.6321 ug Ni3(HITP)2; 7.03316e-9 mol Ni3(HITP)2	—	SD [Ni] = 0.570 ppb; %RSD = 0.921	SI Table Exact Reported	SI p.S15 · Supplementary Table 4 · Supplementary Table 4

RRDE TOF calculation using ICP-MS nickel quantification

Bulk elemental and compositional analysis

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

Potentiostatic RRDE disk potentials 0.807 to 0.667 V vs RHE; 20% ring collection efficiency.

Atmosphere: O2
Geometry: Glassy carbon RRDE with Pt ring
Context: pristine framework film
Measurement source: SI p.S14 · Supplementary Tables 1-3 · Supplementary Tables 1-3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
2e- ORR TOF per Ni3(HITP)2 at 0.667 V, ICP-MSMarked as a best value within this paper	0.491 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 2 · Supplementary Table 2
2e- ORR TOF per Ni3(HITP)2 at 0.787 V, ICP-MS	0.0456 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 2 · Supplementary Table 2
2e- ORR TOF per Ni at 0.787 V, ICP-MS	0.0152 electrons [Ni]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 2 · Supplementary Table 2
4e- ORR TOF per Ni3(HITP)2 at 0.667 V, ICP-MSMarked as a best value within this paper	0.466 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 3 · Supplementary Table 3
4e- ORR TOF per Ni3(HITP)2 at 0.787 V, ICP-MS	0.0564 electrons [Ni3(HITP)2]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 3 · Supplementary Table 3
4e- ORR TOF per Ni at 0.787 V, ICP-MS	0.0188 electrons [Ni]-1 s-1	—	—	SI Table Exact Reported	SI p.S14 · Supplementary Table 3 · Supplementary Table 3
ICP-MS RRDE nickel sites	1.198e16 Ni sites; catalyst loading 5.311 ug Ni3(HITP)2; 6.633e-9 mol Ni3(HITP)2	—	SD [Ni] = 3.562 ppb	SI Table Exact Reported	SI p.S14 · Supplementary Table 1 · Supplementary Table 1
typical MOF loading on GCE	about 5 ug of MOF	—	—	Text Approximate	main p.2 · Synthesis and quantification

Potentiostatic steady-state durability test

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

0.10 M KOH; 2000 rpm; continuous O2 sparging; held at 0.767 V vs RHE for 8 h; data every 60 s.

Atmosphere: O2
Geometry: Ni3(HITP)2-modified glassy carbon rotating electrode
Context: pristine framework film
Measurement source: main p.3 · Stability of Ni3(HITP)2 during ORR · Supplementary Fig. 5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
current density retained after 8 hMarked as a best value within this paper	88% of initial current density retained over 8 h at E = 0.77 V	—	—	Text Exact Reported	main p.3 · Stability of Ni3(HITP)2 during ORR · Supplementary Fig. 5
durability hold potential	0.767 V vs RHE	—	—	Text Exact Reported	main p.5 · Potentiostatic steady-state durability test

Koutecky-Levich analysis and activation-controlled Tafel plot

Tafel and polarisation analysis

Ni3(HITP)2 thin film on glassy carbon electrode · Electrode

Rotating disk measurements at multiple rotation rates; 0.10 M KOH; O2 atmosphere.

Atmosphere: O2
Geometry: Ni3(HITP)2-modified glassy carbon rotating disk electrode
Context: pristine framework film
Measurement source: main p.3 · Mechanistic insight into ORR on Ni3(HITP)2 · Fig. 3; Supplementary Fig. 13; Supplementary Table 7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
electron transfer number n at 0.667 V	n = 2.23 at E = 0.667 V; B = -8.315e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
electron transfer number n at 0.687 V	n = 2.12 at E = 0.687 V; B = -7.920e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
electron transfer number n at 0.707 V	n = 2.05 at E = 0.707 V; B = -7.625e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
electron transfer number n at 0.727 V	n = 2.06 at E = 0.727 V; B = -7.669e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
electron transfer number n at 0.747 V	n = 2.04 at E = 0.747 V; B = -7.590e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
electron transfer number n at 0.767 VMarked as a best value within this paper	n = 2.25 at E = 0.767 V; B = -8.391e-5 A cm-2 rpm-0.5	—	—	SI Table Exact Reported	SI p.S16 · Supplementary Table 7 · Supplementary Table 7
Tafel slopeMarked as a best value within this paper	-128 mV dec-1	—	—	Text Exact Reported	main p.3 · Mechanistic insight · Fig. 3
theoretical one-electron pre-equilibrium Tafel slope	-120 mV dec-1	—	—	Text Exact Reported	main p.3 · Mechanistic insight