Electrochemistry Application — A porous proton-relaying metal-organic framework material that accelerates electrochemical hydrogen evolution

11 measurement groups · 27 results

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

HER J-V curves

Au substrate HER control series · Electrode

Bare Au, Au_Ni-S and Au_NU-1000_Ni-S compared as substrate controls.

Atmosphere: aqueous acid; exact conditions not repeated in SI caption
Geometry: Au substrate electrodes
Context: alternative-substrate controls
Measurement source: 11 · Supplementary Figure 14 · Supplementary Figure 14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Au substrate hybrid HER comparison	similar HER performance observed for Au_NU-1000_Ni-S when FTO is replaced by Au	—	—	Caption Qualitative	11 · Supplementary Figure 14 · Supplementary Figure 14

EQCM and ICP comparison for benzoate-modified versus benzoate-free films

Bulk elemental and compositional analysis

benzoate-modified NU-1000_Ni-S · Electrode

Ni-S mass loading and Ni content compared for benzoate-modified and benzoate-free NU-1000 films.

Geometry: FTO-supported films
Context: modified-MOF hybrid control
Measurement source: 9, 12 · Supplementary Figure 11; Supplementary Table 2 · Supplementary Figure 11; Supplementary Table 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
ICP Ni content per benzoate-free FTO_NU-1000 film	13.6 ppm/cm2	—	—	SI Table Exact Reported	12 · Supplementary Table 2 · Supplementary Table 2
benzoate-modified NU-1000_Ni-S mass loading after 2 min	26.7 ug cm-2	26.7 ug cm-2	—	Caption Exact Reported	9 · Supplementary Figure 11 · Supplementary Figure 11
ICP Ni content per benzoate-modified FTO_NU-1000 film	13.8 ppm/cm2	—	—	SI Table Exact Reported	12 · Supplementary Table 2 · Supplementary Table 2

Electrochemical impedance spectroscopy and double-layer capacitance CV

Impedance spectroscopy Voltammetry

NU-1000_Ni-S · Electrode

FTO_Ni-S and NU-1000_Ni-S compared under HER working conditions; capacitive currents measured positive of HER region across scan rates.

Atmosphere: aqueous acid
Geometry: three-electrode HER cell
Context: hybrid versus MOF-free control
Measurement source: 5 · Results - Origins of enhanced catalytic performance · Figure 6; Supplementary Figure 9

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
active-area-normalized Rct comparison	similar Rct values for FTO_Ni-S and NU-1000_Ni-S after active-area correction	—	—	Caption Qualitative	5 · Figure caption · Figure 6b
hybrid electroactive surface-area increase	only about 1.5 times greater than simple Ni-S film	—	—	Text Approximate	5 · Results - Origins · Figure 6c

EQCM mass loading during electrodeposition

NU-1000_Ni-S · Electrode

Ni-S mass loading during electrodeposition on NU-1000-covered tin-oxide-coated gold QCM crystal.

Atmosphere: aqueous deposition bath
Geometry: 6 MHz QCM crystal coated with NU-1000
Context: target hybrid
Measurement source: 4, 7 · Results - HER catalysis; Methods - Instrumentation · Supplementary Figure 6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
NU-1000_Ni-S Ni-S mass loading after 2 min	28 ug cm-2	28 ug cm-2	—	Text Exact Reported	9 · Supplementary Figure 11 · Supplementary Figure 11
NU-1000_Ni-S molar Ni-S loading	0.116 umol cm-2	0.116 umol cm-2	—	Text Exact Reported	4 · Results - HER catalysis · Supplementary Figure 6a

Galvanostatic electrolysis with gas chromatography; TOF/TON calculations

Galvanostatic cycling

NU-1000_Ni-S · Electrode

Faradaic efficiency at 2 mA cm-2 for 3 h in 0.1 M HCl; potentiostatic electrolysis over 8000 s at -210 mV vs RHE for TON/TOF estimate.

Atmosphere: aqueous acid
Geometry: 60 ml Gamry 5-neck cell; ca. 0.5 cm2 working electrode
Context: target hybrid
Measurement source: 4, 7 · Results - HER catalysis; Methods · Supplementary Figures 6-7

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2 Faradaic efficiency	93%	—	—	Text Exact Reported	4 · Results - HER catalysis · Supplementary Figure 7
active-site-normalized upper-limit TOF	34 s-1	—	upper limit based on geometric active-site assumptions	Calculated From Reported Approximate	4, 7 · Results - HER catalysis; Methods
TOF based on total Ni-S amount	0.208 s-1	—	—	Calculated From Reported Rounded Reported	4 · Results - HER catalysis
active-site-normalized upper-limit TON	273,000	—	upper limit based on geometric active-site assumptions	Calculated From Reported Approximate	4, 7 · Results - HER catalysis; Methods
TON based on total Ni-S amount	1668	—	—	Calculated From Reported Rounded Reported	4 · Results - HER catalysis

HER J-V curves

bare FTO · Electrode

Aqueous 0.1 M HCl, pH 1; bare FTO control.

Atmosphere: aqueous acid
Geometry: bare FTO working electrode
Context: substrate control
Measurement source: 4 · Results - HER catalysis · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
bare FTO overpotential at 10 mA cm-2	ca. 1 V	—	—	Text Approximate	4 · Results - HER catalysis · Figure 4
bare FTO Tafel slope	182 mV dec-1	—	low current density region only	Caption Exact Reported	4 · Figure caption · Figure 4b

HER J-V curves

benzoate-modified NU-1000_Ni-S · Electrode

Aqueous 0.1 M HCl, pH 1; benzoate-modified NU-1000_Ni-S compared with activated NU-1000_Ni-S.

Atmosphere: aqueous acid
Geometry: FTO-supported benzoate-modified NU-1000_Ni-S
Context: modified-MOF hybrid control
Measurement source: 6 · Results - Origins of enhanced catalytic performance · Figure 8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
benzoate-modified NU-1000_Ni-S overpotential at 10 mA cm-2	553 mV	—	—	Text Exact Reported	6 · Results - Origins · Figure 8

HER J-V curves and Tafel plots

Tafel and polarisation analysis

FTO_Ni-S · Electrode

Aqueous 0.1 M HCl, pH 1; MOF-free FTO_Ni-S control.

Atmosphere: aqueous acid
Geometry: FTO_Ni-S working electrode
Context: MOF-free control
Measurement source: 2, 4 · Results - HER catalysis · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
FTO_Ni-S overpotential at 10 mA cm-2	443 mV	—	—	Text Exact Reported	2 · Results - Electrocatalyst synthesis · Figure 4
FTO_Ni-S Tafel slope	188 mV dec-1	—	low current density region only	Caption Exact Reported	4 · Figure caption · Figure 4b

HER J-V curves and Tafel plots

Tafel and polarisation analysis

FTO_NU-1000 · Electrode

Aqueous 0.1 M HCl, pH 1; pristine FTO_NU-1000 without Ni-S.

Atmosphere: aqueous acid
Geometry: FTO_NU-1000 working electrode
Context: pristine MOF control
Measurement source: 4 · Results - HER catalysis · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
FTO_NU-1000 overpotential at 10 mA cm-2	ca. 640 mV	—	—	Text Approximate	4 · Results - HER catalysis · Figure 4
FTO_NU-1000 Tafel slope	123 mV dec-1 from Figure 4b label	—	—	Figure Axis Approximate	4 · Figure 4b · Figure 4b

HER J-V curves and Tafel plots

Tafel and polarisation analysis

NU-1000_Ni-S · Electrode

Aqueous 0.1 M HCl, pH 1; three-electrode cell; potentials adjusted to RHE and iR-corrected.

Atmosphere: aqueous acid
Geometry: FTO-supported NU-1000_Ni-S working electrode
Context: target hybrid
Measurement source: 4 · Results - HER catalysis · Figure 4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
NU-1000_Ni-S overpotential at 10 mA cm-2Marked as a best value within this paper	238 mV, lowest iR-corrected overpotential observed	—	values occasionally ranged as high as 280 mV	Text Exact Reported	4 · Results - HER catalysis · Figure 4
NU-1000_Ni-S overpotential upper observed range at 10 mA cm-2	occasionally ranged as high as 280 mV	—	range 238-280 mV implied	Text Range	4 · Results - HER catalysis · Figure 4
NU-1000_Ni-S Tafel slopeMarked as a best value within this paper	111 mV dec-1 from Figure 4b label; text describes near 120 mV dec-1	—	text says near 120 mV dec-1	Figure Axis Approximate	4-5 · Figure 4b; Results · Figure 4b

Galvanostatic electrolysis, PXRD and UV-vis leaching check

UV-visible and optical absorption spectroscopy X-ray diffraction and scattering Galvanostatic cycling

NU-1000_Ni-S · Electrode

Aqueous HCl pH 1; 10 mA cm-2 for 2 h; PXRD before/after; electrolyte UV-vis after catalysis.

Atmosphere: aqueous acid
Geometry: FTO-supported NU-1000_Ni-S electrode
Context: target hybrid
Measurement source: 4-5 · Results - HER catalysis · Figure 5; Supplementary Figure 8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
galvanostatic stability duration	2 h at 10 mA cm-2	—	overpotential remained constant within +/-20 mV	Text Exact Reported	4 · Results - HER catalysis · Figure 5a
overpotential variation during stability test	+/-20 mV	—	—	Text Rounded Reported	4 · Results - HER catalysis · Figure 5a
framework crystallinity after HER	MOF scaffold retains crystallinity after 2 h galvanostatic electrolysis	—	—	Caption Qualitative	5 · Figure caption · Figure 5b
UV-vis linker leaching check	no traces of leached NU-1000 linker after 2 h catalysis; linker absorbance reference at ca. 390 nm	—	—	Text Approximate	4 · Results - HER catalysis · Supplementary Figure 8