Spectroscopy — Electrocatalytic oxygen evolution reaction at IrOx supported by Ni/Co-ZIF-67: Controlled ratio of metallic Ir and Ir3+ states

7 measurement groups · 49 results

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

FTIR spectroscopy

Infrared spectroscopy

Ni/Co-ZIF-67-2 / Ni/Co-ZIF-67 · Nanosheet

Bruker Vertex 70 V; comparison of dimethylimidazole ligand, ZIF-67 and Ni/Co-ZIF-67-2.

Context: mixed-metal support control
Measurement source: article p3 · Results and discussion · Figure 1b

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Co-N(imidazolate) coordination band	weak peak newly appeared at 421 cm^-1	—	—	Text Rounded Reported	article p3 · Results and discussion · Figure 1b
Free ligand N-H interaction band range	2100~3400 cm^-1 disappeared in ZIF samples	—	—	Text Range	article p3 · Results and discussion · Figure 1b
Free ligand N-H bond peak	1846 cm^-1 N-H bond peak disappeared in ZIF samples	—	—	Text Rounded Reported	article p3 · Results and discussion · Figure 1b

XPS after chronopotentiometry stability test

X-ray photoelectron spectroscopy Galvanostatic cycling

2.8-IrOx@Ni/Co-ZIF-67 / IrOx@Ni/Co-ZIF-67 · Nanosheet

Ir 4f high-resolution XPS after 24 h OER stability test.

Context: target composite after OER
Measurement source: article p6 · Results and discussion · Figure S19

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ir0:Ir3+:Ir4+ relative ratio after stability	3.9:4.1:2.1	—	—	Text Exact Reported	article p6 · Results and discussion · Figure S19

XPS Ir 4f peak deconvolution

X-ray photoelectron spectroscopy

1.6-IrOx@Ni/Co-ZIF-67 · Nanosheet

Ir 4f region used to quantify Ir0/Ir3+/Ir4+ relative ratio.

Context: Ir loading series
Measurement source: article p5 · Results and discussion · Figure 3d-f; Figure S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Actual Ir content by XPS atomic percentage	1.6 at.% Ir	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
Ir0:Ir3+:Ir4+ relative ratio	3.5:3.0:3.5	—	—	Text Exact Reported	article p5 · Results and discussion · Figure S11
XPS atomic percentage of C	30.95 at.% C	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Co	16.95 at.% Co	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of N	0.4 at.% N	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Ni	2.64 at.% Ni	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of O	47.46 at.% O	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1

XPS

X-ray photoelectron spectroscopy

2.8-IrOx@Ni/Co-ZIF-67 / IrOx@Ni/Co-ZIF-67 · Nanosheet

Thermo Fisher Scientific NEXSA, Al Kalpha X-ray source 1487 eV; high-resolution Co 2p, Ni 2p, O 1s, Ir 4f scans.

Context: target composite
Measurement source: article p4-p5 · Results and discussion · Figure 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Co/Ni binding energy shift after IrOx immobilisation	~0.3 eV lower binding energy	—	—	Text Approximate	article p4 · Results and discussion · Figure S10
Co2+ 2p1/2 binding energy	798.2 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Co2+ 2p3/2 binding energy	782.3 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Co3+ 2p1/2 binding energy	796.5 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Co3+ 2p3/2 binding energy	780.6 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir0 4f5/2 binding energy	63.6 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir0 4f7/2 binding energy	60.6 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir3+ 4f5/2 binding energy	65.5 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir3+ 4f7/2 binding energy	62.5 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir4+ 4f5/2 binding energy	64.3 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ir4+ 4f7/2 binding energy	61.3 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ni2+ 2p1/2 binding energy	873.2 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ni2+ 2p3/2 binding energy	855.8 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ni3+ 2p1/2 binding energy	875.2 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
Ni3+ 2p3/2 binding energy	857.8 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
O 1s adsorbed water binding energy	532.7 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
O 1s hydroxide binding energy	531.3 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3
O 1s lattice oxide binding energy	530.6 eV	—	—	Text Exact Reported	article p4-p5 · Results and discussion · Figure 3

XPS Ir 4f peak deconvolution

X-ray photoelectron spectroscopy

6.5-IrOx@Ni/Co-ZIF-67 · Nanosheet

Ir 4f region used to quantify Ir0/Ir3+/Ir4+ relative ratio.

Context: Ir loading series
Measurement source: article p5 · Results and discussion · Figure 3d-f; Figure S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Actual Ir content by XPS atomic percentage	6.5 at.% Ir	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
Ir0:Ir3+:Ir4+ relative ratio	1.8:5.6:2.6	—	—	Text Exact Reported	article p5 · Results and discussion · Figure S11
XPS atomic percentage of C	28.99 at.% C	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Co	14.98 at.% Co	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of N	0.51 at.% N	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Ni	2.67 at.% Ni	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of O	46.31 at.% O	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1

XPS Ir 4f peak deconvolution

X-ray photoelectron spectroscopy

2.8-IrOx@Ni/Co-ZIF-67 / IrOx@Ni/Co-ZIF-67 · Nanosheet

Ir 4f region used to quantify Ir0/Ir3+/Ir4+ relative ratio.

Context: Ir loading series
Measurement source: article p5 · Results and discussion · Figure 3d-f; Figure S11

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Actual Ir content by XPS atomic percentageMarked as a best value within this paper	2.8 at.% Ir	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
Ir0:Ir3+:Ir4+ relative ratioMarked as a best value within this paper	3.7:4.4:1.9	—	—	Text Exact Reported	article p5 · Results and discussion · Figure S11
XPS atomic percentage of C	32.4 at.% C	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Co	15.13 at.% Co	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of N	0.4 at.% N	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Ni	2.61 at.% Ni	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of O	46.65 at.% O	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1

XPS composition analysis

X-ray photoelectron spectroscopy

Ni/Co-ZIF-67-2 / Ni/Co-ZIF-67 · Nanosheet

XPS used to identify the optimal Ni/Co atomic ratio of Ni/Co-ZIF-67-2.

Context: mixed-metal support composition
Measurement source: article p2-p3 · Abstract / Results and discussion

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Optimized Ni/Co atomic ratioMarked as a best value within this paper	Ni/Co atomic ratio 1:6.5	—	—	Text Exact Reported	article p2-p3 · Abstract / Results and discussion
XPS atomic percentage of C	30.87 at.% C	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Co	16.71 at.% Co	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of N	0.3 at.% N	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of Ni	2.55 at.% Ni	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1
XPS atomic percentage of O	49.56 at.% O	—	—	SI Table Exact Reported	SI p12 · Table S1 · Table S1