Spectroscopy — Operando Elucidation of Electrocatalytic and Redox Mechanisms on a 2D Metal Organic Framework Catalyst for Efficient Electrosynthesis of Hydrogen Peroxide in Neutral Media

4 measurement groups · 14 results

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

Ni-HAB powder · Powder

Powder on Kapton tape under ambient environment; Athena/ARTEMIS fitting with S0^2 determined from powder sample.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-C path distance in Ni-HAB powder	2.68 +/- 0.02 Angstrom	—	+/- 0.02 Angstrom	SI Table Exact Reported	S29 · Supporting Tables · Table S1
Ni-N bond distance in Ni-HAB powder	1.840 +/- 0.006 Angstrom	—	+/- 0.006 Angstrom	SI Table Exact Reported	S29 · Supporting Tables · Table S1
EXAFS amplitude reduction factor S0^2	0.75 +/- 0.02	—	+/- 0.02	SI Table Exact Reported	S29 · Supporting Tables · Table S1

Ni-HAB/CFP electrode · Electrode

EXAFS fits for Ni-HAB/CFP at 0.8-0 V vs RHE under O2 and Ar saturation in 0.5 M NaPi.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ar-saturated Ni-N coordination number series	Ni-N CN at 0.8/0.7/0.6/0.5/0.4/0.3/0.2/0.1/0 V vs RHE = 3.8, 4.2, 4.3, 4.4, 4.3, 3.1, 2.7, 2.7, 3.0	—	—	SI Table Exact Reported	S33-S38 · Supporting Tables · Tables S11-S19
O2-saturated Ni-N coordination number series	Ni-N CN at 0.8/0.7/0.6/0.5/0.4/0.3/0.2/0.1/0 V vs RHE = 3.8, 3.8, 3.7, 3.7, 3.7, 3.6, 3.4, 3.2, 3.1	—	—	SI Table Exact Reported	S29-S33 · Supporting Tables · Tables S2-S10
O2-saturated Ni-O path at 0.1 V	Ni-O CN 5 +/- 1 at R = 3.39 +/- 0.02 Angstrom; second Ni-O CN 1.5 +/- 0.5 at R = 2.43 +/- 0.03 Angstrom	—	—	SI Table Exact Reported	S33 · Supporting Tables · Table S9
O2-saturated Ni-O path at 0 V	Ni-O CN 4.6 +/- 0.6 at R = 3.411 +/- 0.007 Angstrom; second Ni-O CN 0.5 +/- 0.2 at R = 2.40 +/- 0.04 Angstrom	—	—	SI Table Exact Reported	S33 · Supporting Tables · Table S10

Ni-HAB/CFP electrode · Electrode

Ni-HAB/CFP in O2- or Ar-saturated 0.5 M NaPi; potentials 0.8 to 0 V vs RHE; 75 min at each potential.

Atmosphere: O2-saturated and Ar-saturated
Geometry: custom Teflon H-cell with CFP working electrode
Context: application composite electrode
Measurement source: 15848 · Operando X-ray Absorption Spectroscopy · Figure 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
LCA HABox/HABred crossover potential	0.34 V vs RHE crossover	—	—	Text Exact Reported	15849 · Operando XAS · Figure S22
Ni leaching qualitative severity	Ni leaching more severe in Ar-saturated electrolytes than in O2-saturated electrolytes	—	—	Text Qualitative	15849 · Operando XAS · Figure S23
O2-saturated HABred fraction reaches 100%	HABred reaches 100% at potentials <=0.2 V vs RHE	—	—	Text Exact Reported	15849 · Operando XAS · Figure S22
Operando XAS potential-step duration	75 min each potential	—	—	Text Exact Reported	15848 · Operando XAS · Figure 3; Figure S10
XANES pre-edge peak I	~8333 eV 1s-3d transition	—	—	Text Approximate	15848 · Operando XAS · Figure 3b,c
XANES peak II	~8339 eV 1s-4pz transition	—	—	Text Approximate	15848 · Operando XAS · Figure 3b,c

Ni-HAB powder · Powder

Horiba Labram Aramis, 532 nm laser; 633 and 532 nm spectra shown.

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-HAB Raman consistency	Raman spectrum is consistent with previous reports	—	—	Text Qualitative	15847 · Results · Figure S4