Spectroscopy — Mechanistic Insight into the Formation and Deposition of Conductive, Layered Metal-Organic Framework Nanocrystals

Measurement evidence

Spectroscopy

Mechanistic Insight into the Formation and Deposition of Conductive, Layered Metal-Organic Framework Nanocrystals · Ambrogi E.K., Damacet P., Stolz R.M. et al. · ACS Nano · 2025 · 1383-1395

25 measurement groups · 64 results

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

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air bubbled 1 mL/min Ni3(HHTP)2 · Thin Film

air bubbling flow-rate series

Temperature
295
Atmosphere
air bubbled
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S41 · Table S15 · Table S15
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00063 min^-1 +/- 3.1 x 10^-4+/- 3.1 x 10^-4SI Table
Rounded Reported
S41 · Table S15 · Table S15
induction period length16 +/- +/- 3 min+/- 3SI Table
Rounded Reported
S41 · Table S15 · Table S15
initial deposition rate0.00086 min^-1 +/- 4.5 x 10^-4+/- 4.5 x 10^-4SI Table
Rounded Reported
S41 · Table S15 · Table S15

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air bubbled 2 mL/min Ni3(HHTP)2 · Thin Film

air bubbling flow-rate series

Temperature
295
Atmosphere
air bubbled
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S41 · Table S15 · Table S15
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00098 min^-1 +/- 3.0 x 10^-4+/- 3.0 x 10^-4SI Table
Rounded Reported
S41 · Table S15 · Table S15
induction period length14 +/- +/- 6 min+/- 6SI Table
Rounded Reported
S41 · Table S15 · Table S15
initial deposition rate0.0014 min^-1 +/- 0.6 x 10^-3+/- 0.6 x 10^-3SI Table
Rounded Reported
S41 · Table S15 · Table S15

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air bubbled 4 mL/min Ni3(HHTP)2 · Thin Film

air bubbling flow-rate series

Temperature
295
Atmosphere
air bubbled
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S41 · Table S15 · Table S15
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.0014 min^-1 +/- 0.5 x 10^-3+/- 0.5 x 10^-3SI Table
Rounded Reported
S41 · Table S15 · Table S15
induction period length13 +/- +/- 6 min+/- 6SI Table
Rounded Reported
S41 · Table S15 · Table S15
initial deposition rate0.00024 min^-1 +/- 0.9 x 10^-4 (printed; likely exponent inconsistency)+/- 0.9 x 10^-4 (printed; likely exponent inconsistency)SI Table
Uncertain
S41 · Table S15 · Table S15

in situ ATR-FTIR deposition at 1464 cm^-1

ATR in situ air-bubbled Ni3(HHTP)2, room temperature · Thin Film

growth/deposition tracked by diagnostic MOF band; spectra collected every 60 s for 14 h

Temperature
295
Atmosphere
as route
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S28 · Table S8 · Table S8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
induction period32 min +/- 12 min+/- 12 minSI Table
Rounded Reported
S28 · Table S8 · Table S8
initial deposition rate0.00053 min^-1 +/- 3.2 x 10^-4+/- 3.2 x 10^-4SI Table
Rounded Reported
S28 · Table S8 · Table S8
MOF yield4.8 mg, 9.7% (18 h); 21.4 mg, 44% (6 days)SI Table
Exact Reported
S28 · Table S8 · Table S8

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air-diffusion port-in Ni3(HHTP)2, room temperature · Thin Film

growth/deposition tracked by diagnostic MOF band; spectra collected every 60 s for 14 h

Temperature
295
Atmosphere
as route
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S28 · Table S8 · Table S8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
induction period298 min +/- 53 min+/- 53 minSI Table
Rounded Reported
S28 · Table S8 · Table S8
initial deposition rate3.1e-05 min^-1 +/- 2.1 x 10^-5+/- 2.1 x 10^-5SI Table
Rounded Reported
S28 · Table S8 · Table S8
MOF yield1.1 mg, 2.2%SI Table
Exact Reported
S28 · Table S8 · Table S8

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air-diffusion port-out Ni3(HHTP)2, room temperature · Thin Film

growth/deposition tracked by diagnostic MOF band; spectra collected every 60 s for 14 h

Temperature
295
Atmosphere
as route
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S28 · Table S8 · Table S8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
induction period197 min +/- 33 min+/- 33 minSI Table
Rounded Reported
S28 · Table S8 · Table S8
initial deposition rate3.2e-05 min^-1 +/- 0.8 x 10^-5+/- 0.8 x 10^-5SI Table
Rounded Reported
S28 · Table S8 · Table S8
MOF yield4.9 mg, 9.8% (18 h); 12.8 mg, 26% (6 days)SI Table
Exact Reported
S28 · Table S8 · Table S8

in situ ATR-FTIR deposition at 1464 cm^-1

ATR air plus 50 uL 6% H2O2 Ni3(HHTP)2, room temperature · Thin Film

growth/deposition tracked by diagnostic MOF band; spectra collected every 60 s for 14 h

Temperature
295
Atmosphere
as route
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S28 · Table S8 · Table S8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
induction period8.2 min +/- 3.3 min+/- 3.3 minSI Table
Rounded Reported
S28 · Table S8 · Table S8
initial deposition rateMarked as a best value within this paper0.00099 min^-1 +/- 6.6 x 10^-4+/- 6.6 x 10^-4SI Table
Rounded Reported
S28 · Table S8 · Table S8
MOF yield3.6 mg, 7.3%SI Table
Exact Reported
S28 · Table S8 · Table S8

in situ ATR-FTIR deposition at 1464 cm^-1

ATR nitrogen-control Ni3(HHTP)2 attempt, room temperature · Thin Film

growth/deposition tracked by diagnostic MOF band; spectra collected every 60 s for 14 h

Temperature
295
Atmosphere
as route
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S28 · Table S8 · Table S8
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
initial deposition rateN/AQualitative
Qualitative
S28 · Table S8 · Table S8
MOF yield0.2 mg, 0.4%SI Table
Exact Reported
S28 · Table S8 · Table S8

in situ ATR-FTIR deposition at 1464 cm^-1

ATR gradual 10 eq H2O2 over 2 h Ni3(HHTP)2 · Thin Film

10 eq H2O2 added gradually; rates from first hour and first five hours

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S39 · Table S13 · Table S13
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.0009 min^-1 +/- 7.1 x 10^-4+/- 7.1 x 10^-4SI Table
Rounded Reported
S39 · Table S13 · Table S13
average rate first five hours0.00065 min^-1 +/- 4.9 x 10^-4+/- 4.9 x 10^-4SI Table
Rounded Reported
S39 · Table S13 · Table S13

in situ ATR-FTIR deposition at 1464 cm^-1

ATR gradual 10 eq H2O2 over 4 h Ni3(HHTP)2 · Thin Film

10 eq H2O2 added gradually; rates from first hour and first five hours

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S39 · Table S13 · Table S13
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.0017 min^-1 +/- 0.3 x 10^-3+/- 0.3 x 10^-3SI Table
Rounded Reported
S39 · Table S13 · Table S13
average rate first five hours0.00096 min^-1 +/- 3.5 x 10^-4+/- 3.5 x 10^-4SI Table
Rounded Reported
S39 · Table S13 · Table S13

in situ ATR-FTIR deposition at 1464 cm^-1

ATR 10 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.0027 min^-1 +/- 0.4 x 10^-3+/- 0.4 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rateMarked as a best value within this paper0.0037 min^-1 +/- 0.6 x 10^-3+/- 0.6 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR delayed 10 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.0011 min^-1 +/- 0.6 x 10^-3+/- 0.6 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.0023 min^-1 +/- 1.4 x 10^-3+/- 1.4 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR 1 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00025 min^-1 +/- 1.9 x 10^-4+/- 1.9 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.00028 min^-1 +/- 1.3 x 10^-4+/- 1.3 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR 3 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00037 min^-1 +/- 1.9 x 10^-4+/- 1.9 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.00041 min^-1 +/- 2.2 x 10^-4+/- 2.2 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR delayed 3 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00057 min^-1 +/- 2.0 x 10^-4+/- 2.0 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.0013 min^-1 +/- 0.7 x 10^-3+/- 0.7 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR 5 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00069 min^-1 +/- 3.8 x 10^-4+/- 3.8 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.00093 min^-1 +/- 2.8 x 10^-4+/- 2.8 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11

in situ ATR-FTIR deposition at 1464 cm^-1

ATR 7.5 eq H2O2 Ni3(HHTP)2 · Thin Film

H2O2 concentration/delay series; rates from initial linear region and first hour

Temperature
295
Atmosphere
room-temperature ATR cell
Geometry
diamond ATR crystal
Context
pristine Ni3(HHTP)2
Measurement source
S36 · Table S11 · Table S11
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
average rate first hour0.00096 min^-1 +/- 6.8 x 10^-4+/- 6.8 x 10^-4SI Table
Rounded Reported
S36 · Table S11 · Table S11
initial deposition rate0.0017 min^-1 +/- 0.5 x 10^-3+/- 0.5 x 10^-3SI Table
Rounded Reported
S36 · Table S11 · Table S11

EPR spectroscopy

reduced HHTP powder · Powder

fresh HHTP under nitrogen and aged 5 days exposed to air

Atmosphere
nitrogen/air
Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S6 · HHTP characterization · Figure S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
carbon-centred radical g valueG-value = 2.001Figure Axis
Approximate
S6 · Figure S5 · Figure S5

UV-vis spectroscopy

reduced HHTP powder · Powder

2 mM HHTP in 2:1 H2O:DMF; fresh, aged, commercial compared

Atmosphere
inert/ambient history
Geometry
solution
Context
pristine Ni3(HHTP)2
Measurement source
S6 · HHTP characterization · Figure S4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
aged HHTP Amaxlambda_max 590 nm; Amax 0.078Figure Axis
Approximate
S6 · Figure S4 · Figure S4
aged HHTP lambda maxlambda_max 590 nm; Amax 0.078Figure Axis
Approximate
S6 · Figure S4 · Figure S4
commercial HHTP Amaxlambda_max 562 nm; Amax 0.406Figure Axis
Approximate
S6 · Figure S4 · Figure S4
commercial HHTP lambda maxlambda_max 562 nm; Amax 0.406Figure Axis
Approximate
S6 · Figure S4 · Figure S4
fresh HHTP Amaxlambda_max 582 nm; Amax 0.078Figure Axis
Approximate
S6 · Figure S4 · Figure S4
fresh HHTP lambda maxlambda_max 582 nm; Amax 0.078Figure Axis
Approximate
S6 · Figure S4 · Figure S4

UV-vis spectroscopy

Ni-HHTP solution complex · Model

HHTP solution, Ni(OAc)2 solution, and combined Ni/HHTP solutions

Atmosphere
sealed cuvette
Geometry
solution
Context
pristine Ni3(HHTP)2
Measurement source
p008 / journal page 1390 · Figure 5 · Figure 5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Ni-HHTP coordination complex visible absorption peaknew maximum absorbance approximately 600 nm; Figure 5 labels lambda_max = 604 nmapproximatelyFigure Axis
Approximate
p008 / journal page 1390 · Observations of Initial Phase · Figure 5

XPS elemental composition

homogeneous DMF/water air plus H2O2 Ni3(HHTP)2, 85 C · Powder

atomic composition of bulk synthesis sample

Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S16 · XPS Analysis · Table S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
C 1s atomic composition65.8%SI Table
Exact Reported
S16 · Table S5 · Table S5
Ni 2p atomic composition6.5%SI Table
Exact Reported
S16 · Table S5 · Table S5
O 1s atomic composition27.7%SI Table
Exact Reported
S16 · Table S5 · Table S5

XPS elemental composition

heterogeneous water bubbled-air Ni3(HHTP)2, 85 C · Powder

atomic composition of bulk synthesis sample

Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S16 · XPS Analysis · Table S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
C 1s atomic composition65.6%SI Table
Exact Reported
S16 · Table S5 · Table S5
Ni 2p atomic composition4.3%SI Table
Exact Reported
S16 · Table S5 · Table S5
O 1s atomic composition30.1%SI Table
Exact Reported
S16 · Table S5 · Table S5

XPS elemental composition

homogeneous DMF/water bubbled-air Ni3(HHTP)2, 85 C · Powder

atomic composition of bulk synthesis sample

Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S16 · XPS Analysis · Table S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
C 1s atomic composition73.6%SI Table
Exact Reported
S16 · Table S5 · Table S5
Ni 2p atomic composition3.9%SI Table
Exact Reported
S16 · Table S5 · Table S5
O 1s atomic composition22.5%SI Table
Exact Reported
S16 · Table S5 · Table S5

XPS elemental composition

homogeneous DMF/water N2 plus H2O2 Ni3(HHTP)2, 85 C · Powder

atomic composition of bulk synthesis sample

Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S16 · XPS Analysis · Table S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
C 1s atomic composition75.9%SI Table
Exact Reported
S16 · Table S5 · Table S5
Ni 2p atomic composition2.9%SI Table
Exact Reported
S16 · Table S5 · Table S5
O 1s atomic composition21.2%SI Table
Exact Reported
S16 · Table S5 · Table S5

XPS elemental composition

homogeneous DMF/water bubbled-N2 Ni3(HHTP)2, 85 C · Powder

atomic composition of bulk synthesis sample

Geometry
powder
Context
pristine Ni3(HHTP)2
Measurement source
S16 · XPS Analysis · Table S5
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
C 1s atomic composition66.5%SI Table
Exact Reported
S16 · Table S5 · Table S5
Ni 2p atomic composition7.3%SI Table
Exact Reported
S16 · Table S5 · Table S5
O 1s atomic composition26.2%SI Table
Exact Reported
S16 · Table S5 · Table S5