Spectroscopy — Trimetallic conductive metal-organic frameworks as precatalysts for the oxygen evolution reaction with enhanced activity

Measurement evidence

Spectroscopy

Trimetallic conductive metal-organic frameworks as precatalysts for the oxygen evolution reaction with enhanced activity · Shi X., Hua R., Xu Y. et al. · Sustainable Energy and Fuels · 2020 · 4589-4597

4 measurement groups · 72 results

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

FT-IR spectroscopy

FeCo0.6Ni0.4-CAT powder/electrode, Fe/(Co+Ni) about 0.32 · Electrode

Bruker Vertex 70, 4000-400 cm^-1, TR mode; SI compares FeCo0.6Ni0.4-CAT, Co0.6Ni0.4-CAT, Co-CAT and Ni-CAT.

Context
M-CAT powders
Measurement source
S-2 · Supporting Information · Figure S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
FT-IR spectra collected for representative M-CATsFT-IR traces shown for FeCo0.6Ni0.4-CAT, Co0.6Ni0.4-CAT, Co-CAT and Ni-CATCaption
Qualitative
S-2 · Supporting Information · Figure S1

ICP spectrometry

FeCo0.6Ni0.4-CAT powder/electrode, Fe/(Co+Ni) about 0.32 · Electrode

ICP spectrometry; Table S1 gives FeCoxNi1-x-CAT atom contents and atom ratios for 1.0 mM Fe(OAc)2 exchange, and Table S2 gives FeCo0.6Ni0.4-CAT Fe-content tuning.

Context
trimetallic target and related FeCoxNi1-x-CATs
Measurement source
S-4 · Supporting Information · Tables S1-S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Fe/(Ni+Co) ratio for 1 mM Fe exchange0.30-0.32 for all FeCoxNi1-x-CATs prepared in 1 mM iron(II) acetateSI Table
Range
S-4 · Supporting Information · Table S1/S2
Fe/(Ni+Co) ratios from Fe(OAc)2 concentration series0.06, 0.15, 0.32, and 0.49 for 0.25, 0.5, 1.0, and 2.0 mM Fe(OAc)2SI Table
Exact Reported
S-4 · Supporting Information · Table S1/S2
ICP Co/Ni ratio in FeCo0.4Ni0.6-CAT0.42/0.58SI Table
Exact Reported
S-4 · Supporting Information · Table S1/S2
ICP Co/Ni ratio in FeCo0.6Ni0.4-CAT0.59/0.41SI Table
Exact Reported
S-4 · Supporting Information · Table S1/S2
ICP Co/Ni ratio in FeCo0.8Ni0.2-CAT0.79/0.21SI Table
Exact Reported
S-4 · Supporting Information · Table S1/S2
ICP Co atom ratio in FeCo0.4Ni0.6-CAT0.42SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom content in FeCo0.4Ni0.6-CAT7.18 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe/(Co+Ni) in FeCo0.4Ni0.6-CAT0.32SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe atom content in FeCo0.4Ni0.6-CAT5.46 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom ratio in FeCo0.4Ni0.6-CAT0.58SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom content in FeCo0.4Ni0.6-CAT9.97 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom ratio in FeCo0.6Ni0.4-CAT0.59SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom content in FeCo0.6Ni0.4-CAT10.15 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe/(Co+Ni) in FeCo0.6Ni0.4-CAT0.32SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe atom content in FeCo0.6Ni0.4-CAT5.49 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom ratio in FeCo0.6Ni0.4-CAT0.41SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom content in FeCo0.6Ni0.4-CAT7.11 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom ratio in FeCo0.8Ni0.2-CAT0.79SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom content in FeCo0.8Ni0.2-CAT13.65 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe/(Co+Ni) in FeCo0.8Ni0.2-CAT0.31SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe atom content in FeCo0.8Ni0.2-CAT5.45 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom ratio in FeCo0.8Ni0.2-CAT0.21SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom content in FeCo0.8Ni0.2-CAT3.7 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom ratio in FeCo-CAT1SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom content in FeCo-CAT17.48 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe/(Co+Ni) in FeCo-CAT0.31SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe atom content in FeCo-CAT5.37 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom ratio in FeCo-CAT0SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom ratio in FeNi-CAT0SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe/(Co+Ni) in FeNi-CAT0.3SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Fe atom content in FeNi-CAT5.42 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom ratio in FeNi-CAT1SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Ni atom content in FeNi-CAT17.93 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S1
ICP Co atom ratio in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange0.6SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom content in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange12.76 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe/(Co+Ni) in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange0.06SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe atom content in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange1.27 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom ratio in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange0.4SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom content in FeCo0.6Ni0.4-CAT from 0.25 Fe(OAc)2 exchange8.61 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom ratio in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange0.59SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom content in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange11.54 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe/(Co+Ni) in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange0.15SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe atom content in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange2.94 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom ratio in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange0.41SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom content in FeCo0.6Ni0.4-CAT from 0.5 Fe(OAc)2 exchange8.07 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom ratio in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange0.59SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom content in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange10.15 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe/(Co+Ni) in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange0.32SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe atom content in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange5.49 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom ratio in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange0.41SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom content in FeCo0.6Ni0.4-CAT from 1.0 Fe(OAc)2 exchange7.11 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom ratio in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange0.58SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Co atom content in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange9.01 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe/(Co+Ni) in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange0.49SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Fe atom content in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange7.52 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom ratio in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange0.42SI Table
Exact Reported
S-4 · Supporting Information · Table S2
ICP Ni atom content in FeCo0.6Ni0.4-CAT from 2.0 Fe(OAc)2 exchange6.42 wt %SI Table
Exact Reported
S-4 · Supporting Information · Table S2

XPS after 1000 CV cycles

FeCo0.6Ni0.4-CAT powder/electrode, Fe/(Co+Ni) about 0.32 · Electrode

XPS after accelerated degradation/OER cycling; metal hydroxide/oxyhydroxide assignment.

Atmosphere
alkaline OER conditions before ex situ XPS
Geometry
drop-cast catalyst on GC during cycling
Context
activated/derived surface state from conductive MOF precatalyst
Measurement source
6 · Results and discussion · Fig. 4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Post-OER Co2+ 2p3/2 binding energy782.1 eVText
Exact Reported
6 · Results and discussion · Fig. 4b
Post-OER Co3+ 2p3/2 binding energy780.3 eVText
Exact Reported
6 · Results and discussion · Fig. 4b
Post-OER Fe 2p3/2 binding energy711.35 eVText
Exact Reported
6 · Results and discussion · Fig. S11a cited
Post-OER Ni2+ 2p3/2 binding energy854.5 eVText
Exact Reported
6 · Results and discussion · Fig. 4a
Post-OER Ni3+ 2p3/2 binding energy856.2 eVText
Exact Reported
6 · Results and discussion · Fig. 4a
Post-OER O 1s fitted peaks532.9, 531.8, and 530.5 eVText
Exact Reported
6 · Results and discussion · Fig. S11b cited

XPS

FeCo0.6Ni0.4-CAT powder/electrode, Fe/(Co+Ni) about 0.32 · Electrode

Thermo ESCALAB 250XI with Al Kalpha radiation; pristine M-CAT oxidation states.

Context
pre-OER conductive MOF
Measurement source
4 · Results and discussion · Fig. 2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Co 2p3/2 binding energy in Co-CAT/Co0.6Ni0.4-CAT/FeCo-CAT781.35 eVText
Exact Reported
4 · Results and discussion · Fig. 2b
Co 2p3/2 binding energy in FeCo0.6Ni0.4-CAT781.20 eVText
Exact Reported
4 · Results and discussion · Fig. 2b
Fe 2p1/2 binding energy in Fe-CAT samples724.98 eVText
Exact Reported
4 · Results and discussion · Fig. 2c
Fe 2p3/2 binding energy in Fe-CAT samples711.65 eVText
Exact Reported
4 · Results and discussion · Fig. 2c
Ni 2p3/2 binding energy in FeCo0.6Ni0.4-CAT855.75 eVText
Exact Reported
4 · Results and discussion · Fig. 2a
Ni 2p1/2 binding energy in Ni-CAT/Co0.6Ni0.4-CAT/FeNi-CAT873.9 eVText
Exact Reported
4 · Results and discussion · Fig. 2a
Ni 2p3/2 binding energy in Ni-CAT/Co0.6Ni0.4-CAT/FeNi-CAT856.1 eVText
Exact Reported
4 · Results and discussion · Fig. 2a
O 1s fitted peaks before OER532.9, 531.59, and 530.73 eVText
Exact Reported
4 · Results and discussion · Fig. 2d