Electrochemistry Application — Dissecting π-conjugated covalent-coupling over conductive MOFs toward efficient two-electron oxygen reduction

12 measurement groups · 48 results

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

Chronoamperometry durability during ORR

Chronoamperometry

Cu-HHTP nanorod powder · Powder

Long-term ORR operation; Fig. 2e and Fig. S20 describe 24 h durability at 0.6 V vs RHE.

Atmosphere: O2-saturated alkaline electrolyte
Geometry: RRDE / electrochemical ORR cell as reported
Context: target pristine conductive MOF
Measurement source: 4 · 3.2 ORR performances · Fig. 2e; Fig. S20

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ORR durability current decayMarked as a best value within this paper	negligible decay of Idisk and Iring	—	—	Text Qualitative	4 · 3.2 ORR performances · Fig. 2e; Fig. S20
Long-term ORR operation duration	24 h	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. 2e; Fig. S20

Flow-cell in situ H2O2 generation coupled to Basic Fuchsin dye treatment

Cu-HHTP nanorod powder · Powder

Digital-photo demonstration using 50 ppm red Basic Fuchsin dye contacted with electrolyte from the H2O2-generating flow cell after reaction.

Atmosphere: O2-saturated alkaline flow-cell electrolyte as described for H2O2 generation
Geometry: Three-electrode flow cell; downstream dye-water contact shown in SI photographs
Context: pristine conductive MOF catalyst used for application demonstration
Measurement source: S21 · Supplementary figures · Figure S19

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Basic Fuchsin dye treatment outcomeMarked as a best value within this paper	immediately degraded	—	—	Caption Qualitative	S21 · Supplementary figures · Figure S19

Flow-cell in situ H2O2 generation coupled to Basic Fuchsin dye treatment

Cu-HITP powder · Powder

Digital-photo demonstration using 50 ppm red Basic Fuchsin dye contacted with electrolyte from the H2O2-generating flow cell after reaction.

Atmosphere: O2-saturated alkaline flow-cell electrolyte as described for H2O2 generation
Geometry: Three-electrode flow cell; downstream dye-water contact shown in SI photographs
Context: pristine conductive MOF catalyst used for application demonstration
Measurement source: S21 · Supplementary figures · Figure S18

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Basic Fuchsin dye treatment outcome	partially degraded	—	—	Caption Qualitative	S21 · Supplementary figures · Figure S18

Flow-cell in situ H2O2 generation coupled to Basic Fuchsin dye treatment

Ni-HITP black powder · Powder

Digital-photo demonstration using 50 ppm red Basic Fuchsin dye contacted with electrolyte from the H2O2-generating flow cell after reaction.

Atmosphere: O2-saturated alkaline flow-cell electrolyte as described for H2O2 generation
Geometry: Three-electrode flow cell; downstream dye-water contact shown in SI photographs
Context: pristine conductive MOF catalyst used for application demonstration
Measurement source: S20 · Supplementary figures · Figure S17

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Basic Fuchsin dye treatment outcome	not degraded	—	—	Caption Qualitative	S20 · Supplementary figures · Figure S17

Flow-cell ORR H2O2 quantification by Ce4+ titration

Cu-HHTP nanorod powder · Powder

160 uL catalyst ink coated on 3 x 3 cm2 carbon cloth; three-electrode flow cell with Nafion 117 membrane; O2-saturated 0.1 M KOH; ORR at 0.4 V vs RHE under 1600 rpm for 60 min; Ce4+ titration by UV-vis at 320 nm.

Atmosphere: O2-saturated 0.1 M KOH
Geometry: Carbon cloth working electrode in three-electrode flow cell
Context: target pristine conductive MOF
Measurement source: Detailed contents for chemical quantification of H2O2 production · Fig. 2c-d; Figs. S14-S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2O2 faradaic efficiency by Ce4+ titrationMarked as a best value within this paper	85.4 %	—	—	SI Table Exact Reported	S28 · Supporting Tables · Table S3
H2O2 yield rateMarked as a best value within this paper	792.7 mmol gcat-1 h-1	—	—	SI Table Exact Reported	S28 · Supporting Tables · Table S3

Flow-cell ORR H2O2 quantification by Ce4+ titration

Cu-HITP powder · Powder

Same flow-cell/Ce4+ titration conditions as Ni-HITP and Cu-HHTP.

Atmosphere: O2-saturated 0.1 M KOH
Geometry: Carbon cloth working electrode in three-electrode flow cell
Context: pristine conductive MOF control
Measurement source: 4 · 3.2 ORR performances · Fig. 2c-d; Figs. S14-S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2O2 yield rate	~293.2 mmol gcat-1 h-1	—	—	Text Approximate	4 · 3.2 ORR performances · Fig. 2c

Flow-cell ORR H2O2 quantification by Ce4+ titration

Ni-HITP black powder · Powder

160 uL catalyst ink coated on 3 x 3 cm2 carbon cloth; three-electrode flow cell with Nafion 117 membrane; both compartments 70 mL 0.1 M KOH; O2 purged at least 30 min; ORR at 0.4 V vs RHE under 1600 rpm for 60 min; aliquots measured by UV-vis after Ce4+ reaction.

Atmosphere: O2-saturated 0.1 M KOH
Geometry: Carbon cloth working electrode in three-electrode flow cell
Context: pristine conductive MOF control
Measurement source: Detailed contents for chemical quantification of H2O2 production · Fig. 2c-d; Figs. S13-S15

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2O2 yield rate	~157.3 mmol gcat-1 h-1	—	—	Text Approximate	4 · 3.2 ORR performances · Fig. 2c

In situ electrochemical impedance spectroscopy (EIS)

Impedance spectroscopy

Cu-HHTP nanorod powder · Powder

EIS performed at different applied potentials in frequency range 0.01-100,000 Hz; equivalent circuit in Figure S25; fitted Rs, Cdl, and Rct reported in Table S5.

Atmosphere: ORR electrolyte, atmosphere not separately restated
Geometry: Electrochemical impedance cell; equivalent circuit in Fig. S25
Context: target pristine conductive MOF
Measurement source: S29 · In situ EIS measurements · Figure S25; Figure S26; Table S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Double-layer capacitance Cdl at 0.45 V	0.00357 F at 0.45 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.50 V	0.00492 F at 0.50 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.55 V	0.00415 F at 0.55 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.60 V	0.00534 F at 0.60 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.65 V	0.00268 F at 0.65 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.70 V	0.00457 F at 0.70 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Double-layer capacitance Cdl at 0.80 V	6.98e-05 F at 0.80 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.45 VMarked as a best value within this paper	876.4 ohm at 0.45 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.50 V	1012.1 ohm at 0.50 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.55 V	1069.1 ohm at 0.55 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.60 V	1623.4 ohm at 0.60 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.65 V	1768.2 ohm at 0.65 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.70 V	2027.9 ohm at 0.70 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Ion adsorption resistance Rct at 0.80 V	2370.3 ohm at 0.80 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.45 V	2.95 ohm at 0.45 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.50 V	1.71 ohm at 0.50 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.55 V	1.42 ohm at 0.55 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.60 V	1.58 ohm at 0.60 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.65 V	2.95 ohm at 0.65 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.70 V	1.41 ohm at 0.70 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Solution resistance Rs at 0.80 V	2.01 ohm at 0.80 V	—	—	SI Table Exact Reported	S29 · Supporting Tables · Table S5
Nyquist semicircle trend with decreasing potential	semicircle shrinks with decreasing potentials	—	—	Text Qualitative	5 · 3.4 In situ SR-FTIR and EIS analysis · Fig. 4c

RRDE ORR linear sweep voltammetry and derived selectivity

Voltammetry

Cu-HHTP nanorod powder · Powder

O2-saturated 0.1 M KOH; same RRDE ink and loading procedure; LSV at 10 mV s-1; Pt ring collection efficiency N = 0.39 from SI calibration.

Atmosphere: O2-saturated alkaline electrolyte; N2-saturated control nearly negligible
Geometry: Rotating ring-disk electrode, 4 mm disk
Context: target pristine conductive MOF
Measurement source: Electrochemical measurements; Selectivity and Electron Transfer Number · Fig. 2; Figs. S8-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Average H2O2 faradaic efficiency over 0.6-0.2 VMarked as a best value within this paper	85.3 %	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S16
Electron transfer numberMarked as a best value within this paper	about 2.1	—	—	Text Approximate	4 · 3.2 ORR performances · Fig. 2b; Figs. S10-S12
ORR onset potentialMarked as a best value within this paper	0.84 V vs RHE	—	—	Text Exact Reported	S28 · Supporting Tables · Table S3
RRDE ring currentMarked as a best value within this paper	about 0.13 mA	—	—	Text Approximate	4 · 3.2 ORR performances · Fig. 2a
H2O2 selectivity from RRDEMarked as a best value within this paper	up to 95 % in 0.2-0.6 V vs RHE	—	—	Text Exact Reported	S28 · Supporting Tables · Table S3
Tafel slopeMarked as a best value within this paper	83.5 mV dec-1	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S9

RRDE ORR linear sweep voltammetry and derived selectivity

Voltammetry

Cu-HITP powder · Powder

O2-saturated 0.1 M KOH; same RRDE ink and loading procedure as Ni-HITP and Cu-HHTP.

Atmosphere: O2-saturated alkaline electrolyte; N2-saturated control nearly negligible
Geometry: Rotating ring-disk electrode, 4 mm disk; Pt ring collection efficiency N = 0.39 from SI calibration
Context: pristine conductive MOF control
Measurement source: 4 · 3.2 ORR performances · Fig. 2; Figs. S8-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Average H2O2 faradaic efficiency over 0.6-0.2 V	43.2 %	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S16
ORR onset potential	0.82 V vs RHE	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. 2a
H2O2 selectivity from RRDE	71 %	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. 2b
Tafel slope	132.3 mV dec-1	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S9

RRDE ORR linear sweep voltammetry and derived selectivity

Voltammetry

Ni-HITP black powder · Powder

O2-saturated 0.1 M KOH; three-electrode cell; catalyst ink made from 5 mg catalyst, 730 uL water, 250 uL ethanol, 20 uL Nafion; 5 uL on 4 mm RRDE; loading about 0.2 mg cm-2; LSV at 10 mV s-1 after CV cycling.

Atmosphere: O2-saturated alkaline electrolyte; N2-saturated control nearly negligible
Geometry: Rotating ring-disk electrode, 4 mm disk; Pt ring collection efficiency N = 0.39 from SI calibration
Context: pristine conductive MOF control
Measurement source: 2 · 2.3 Electrochemical measurements · Fig. 2; Figs. S8-S12

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Average H2O2 faradaic efficiency over 0.6-0.2 V	22.1 %	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S16
ORR onset potential	0.81 V vs RHE	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. 2a
H2O2 selectivity from RRDE	39 %	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. 2b
Tafel slope	118.7 mV dec-1	—	—	Text Exact Reported	4 · 3.2 ORR performances · Fig. S9

SCN- poisoning RRDE experiment

Cu-HHTP nanorod powder · Powder

O2-saturated 0.10 M KOH with 10 mM KSCN; probes deactivation of transition-metal Cu sites.

Atmosphere: O2-saturated 0.10 M KOH
Geometry: RRDE ORR poisoning experiment
Context: target pristine conductive MOF
Measurement source: 2 · 2.3 Electrochemical measurements · Fig. S21

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Effect of SCN- on disk and ring currents	substantial reduction of both Idisk and Iring	—	—	Text Qualitative	4 · 3.3 In situ XAFS study of Cu-HHTP · Fig. S21
Electron transfer number retained under SCN-	about 2.5	—	—	Text Approximate	4 · 3.3 In situ XAFS study of Cu-HHTP · Fig. S21
H2O2 selectivity retained under SCN-	nearly 80 %	—	—	Text Approximate	4 · 3.3 In situ XAFS study of Cu-HHTP · Fig. S21