Spectroscopy — sp-Carbon Incorporated Conductive Metal-Organic Framework as Photocathode for Photoelectrochemical Hydrogen Generation

5 measurement groups · 20 results

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

operando electrochemical resonance Raman spectroscopy

Raman spectroscopy

Cu3HHAE2 photocathode on Cu foam · Electrode

0.1 M Na2SO4, 594 nm laser excitation, potential scan from 0.7 to 0.0 V vs RHE; confocal Raman microscope with Ar flow, 20x objective, about 1.5 mW laser.

Atmosphere: continuous Ar flow
Geometry: Cu3HHAE2 photocathode/electrochemical Raman cell
Context: supported Cu3HHAE2 electrode during PEC HER
Measurement source: 4 · Operando Raman · Figure 5a; Figure S9c

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
operando Raman potential scan range	0.7 to 0.0 V vs RHE	—	range	Text Range	4 · Operando Raman · Figure 5a
intrinsic sp-carbon Raman signal at OCP	2116 cm-1	—	—	Text Rounded Reported	4 · Operando Raman · Figure 5a; Figure S9c
transient Raman band under HER	2044 cm-1	—	—	Text Rounded Reported	4 · Operando Raman · Figure 5a

FT-IR spectroscopy

Infrared spectroscopy

as-synthesised Cu3HHAE2 powder/hexagonal rods · Powder

Bruker Optics ALPHA-E ATR, 400-4000 cm-1; compared CuSO4.5H2O, HHAE and Cu3HHAE2.

Context: pristine Cu3HHAE2 powder with HHAE and CuSO4.5H2O references
Measurement source: 8 · Figure S2 caption · Figure S2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cu3HHAE2 sp-carbon FT-IR vibration	strong vibrational peak at 2200 cm-1	—	—	Caption Rounded Reported	8 · Figure S2 caption · Figure S2
HHAE sp-carbon FT-IR vibration	weak vibrational peak at 2250 cm-1	—	—	Caption Rounded Reported	8 · Figure S2 caption · Figure S2

ultraviolet photoelectron spectroscopy (UPS)

Ultraviolet photoelectron spectroscopy

as-synthesised Cu3HHAE2 powder/hexagonal rods · Powder

He I source 21.22 eV under ultrahigh vacuum; SECO and low binding-energy HOMO regions analysed.

Atmosphere: ultrahigh vacuum about 3 x 10^-9 Torr
Geometry: film on heavily doped n-type Si wafer
Context: pristine Cu3HHAE2 film
Measurement source: 14 · Figure S8 caption · Figure S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
H2O/H2 redox pair energy level comparison	-4.44 eV	—	—	Text Exact Reported	3 · Optoelectronic properties
estimated LUMO level	-4.39 eV	—	—	Calculated From Reported Exact Reported	3 · Optoelectronic properties · Figure 3d; Figure S8
Fermi level	-4.60 eV	—	—	Caption Exact Reported	14 · Figure S8 caption · Figure S8
HOMO level	-5.26 eV	—	—	Caption Exact Reported	14 · Figure S8 caption · Figure S8

UV-vis-NIR absorption and Tauc plot

UV-visible and optical absorption spectroscopy

Cu3HHAE2 drop-cast film on quartz glass · Thin Film

Catalyst drop-cast on quartz glass in transmission mode; compared HHAE and Cu3HHAE2, absorption followed to 1600 nm.

Geometry: film on quartz glass
Context: Cu3HHAE2 film with HHAE control
Measurement source: 3 · Optoelectronic properties · Figure 3c; Figure S7; Figure S10

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
broad absorption extends to	1600 nm	—	—	Text Rounded Reported	3 · Optoelectronic properties · Figure 3c
optical band gapMarked as a best value within this paper	about 0.87 eV	—	about	Text Approximate	3 · Optoelectronic properties · Figure 3c; Figure S7
Cu3HHAE2 absorption peak assigned to ligand-to-Cu transition	480 nm	—	—	Caption Rounded Reported	16 · Figure S10 caption · Figure S10

X-ray photoelectron spectroscopy (XPS)

X-ray photoelectron spectroscopy

as-synthesised Cu3HHAE2 powder/hexagonal rods · Powder

Kratos AXIS Supra/Ultra; monochromatic Al Kalpha source 1486.7 eV; Ar+ etch 60 s before high-resolution scans.

Atmosphere: ultrahigh vacuum about 3 x 10^-9 Torr
Context: pristine powder/film deposited on heavily doped n-type Si wafer
Measurement source: 2 · XPS analysis · Figure 1d; Figure S4

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C 1s C=O binding energy	288.9 eV	—	—	Text Exact Reported	2 · XPS analysis · Figure 1d
C 1s C-O binding energy	286.9 eV	—	—	Text Exact Reported	2 · XPS analysis · Figure 1d
C 1s C-C(sp) binding energy	285.6 eV	—	—	Text Exact Reported	2 · XPS analysis · Figure 1d
C 1s C-C(sp2) binding energy	284.9 eV	—	—	Text Exact Reported	2 · XPS analysis · Figure 1d
Cu 2p binding energy peak 1	934 eV	—	—	Caption Rounded Reported	10 · Figure S4 caption · Figure S4
Cu 2p binding energy peak 2	941 eV	—	—	Caption Rounded Reported	10 · Figure S4 caption · Figure S4
Cu 2p binding energy peak 3	944 eV	—	—	Caption Rounded Reported	10 · Figure S4 caption · Figure S4
C(sp2):C(sp) peak area ratio	close to 2:1	—	close to	Text Approximate	2 · XPS analysis · Figure 1d