Spectroscopy — Conductive Metal-Organic Framework Thin Film Hybrids by Electropolymerization of Monosubstituted Acetylenes

4 measurement groups · 15 results

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

MALDI-ToF/ToF mass spectrometry

BPA@Cu(BDC)-SURMOF-2 after electropolymerisation · Electrode

SURMOF-2 film dissolved in acetic acid/ethanol, mixed with sinapinic-acid matrix in dichloromethane, analysed on Waters Synapt G2-S HDMS in reflector positive ion mode.

Geometry: dissolved thin-film sample, substrate about 2 x 0.5 cm2
Context: polymer product released from electropolymerised MOF film
Measurement source: SI p.S-2 · MALDI-ToF Analysis · Figure 3a

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Calculated adduct mass assigned to observed peak	1299.24 for C94H160 [M+2H+Li]	—	—	Text Exact Reported	main p.5 · Results and Discussion · Figure 3a
Observed BPA chain length at strongest peak	n = 15	—	—	Text Exact Reported	main p.5 · Results and Discussion · Figure 3a
Mass spacing between adjacent peaks	82.08 amu	—	—	Text Exact Reported	main p.5 · Results and Discussion · Figure 3a
Strongest MALDI-ToF mass peak	1299.35 Da	—	—	Text Exact Reported	main p.5 · Results and Discussion · Figure 3a
Upper mass range of visible series	visible up to about 3000 Da	—	—	Text Approximate	main p.5 · Results and Discussion · Figure 3a

Raman spectroscopy and infrared reflection absorption spectroscopy (IRRAS)

Infrared spectroscopy Raman spectroscopy

BPA@Cu(BDC)-SURMOF-2 after electropolymerisation · Electrode

Raman as above; IRRAS on Bruker VERTEX 80 purged with dried air, A518 accessory at 80 degree incidence, MCT detector.

Atmosphere: dried air purge for IRRAS
Geometry: thin film on Au/Ti/Si reference substrate
Context: after electropolymerisation versus loaded/pristine SURMOF
Measurement source: SI p.S-2 · Infrared Reflection Absorption Spectroscopy · Figure 2; Figure S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
IRRAS conjugated C=C peak indicating BPA	IR peak at 1631 cm-1	—	—	Text Exact Reported	main p.4 · Results and Discussion · Figure 2c
Raman conjugated polymer main-chain C=C-H feature	2781 cm-1	—	—	Text Exact Reported	main p.4 · Results and Discussion · Figure 2a
Raman conjugated polymer main-chain C=C-H feature	2869 cm-1	—	—	Text Exact Reported	main p.4 · Results and Discussion · Figure 2a
Raman conjugated polymer main-chain C=C-H feature	2875 cm-1	—	—	Text Exact Reported	main p.4 · Results and Discussion · Figure 2a
Raman C=C stretching band increase	1627 cm-1	—	—	Text Exact Reported	main p.4 · Results and Discussion · Figure 2a
Doping-induced Raman band in BPA	about 1360 cm-1	—	—	Text Approximate	main p.4 · Results and Discussion · Figure 2a; Figure S1b
Doping-induced Raman band in BPA	about 1660 cm-1	—	—	Text Approximate	main p.4 · Results and Discussion · Figure 2a; Figure S1b

Raman spectroscopy

1-hexyne-loaded Cu(BDC) SURMOF-2 · Thin Film

Renishaw inVia Raman microscope, 532 nm laser, 2 mW output, Olympus MPLAN 50x NA 0.75 objective; loading monitored after 10, 25, and 45 h immersion.

Context: guest-loaded SURMOF compared with empty Cu(BDC) SURMOF
Measurement source: SI p.S-2 · Raman Spectroscopy · Figure S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Raman C-C triple-bond stretch from confined 1-hexyne	2330 cm-1	—	—	Text Rounded Reported	main p.3 · Results and Discussion · Figure 2a; Figure S9
Raman C-H stretch from butyl tails after 1-hexyne loading	2930 cm-1	—	—	Text Rounded Reported	main p.2 · Results and Discussion · Figure S1; Figure 2a

TOF-SIMS depth profiling and confocal Raman control

Raman spectroscopy

Bulk-solution EP control using as-prepared SURMOF electrode · Electrode

Depth profiles and 3D renders of Cu+, Bu+, and BuN+ ions after bulk-solution EP control; confocal Raman spectra above and inside sample.

Geometry: as-prepared SURMOF electrode control
Context: bulk EP control, not target confined polymerisation
Measurement source: SI p.S-8 to S-10 · Bulk EP discussion · Figures S7-S8

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Bulk EP control polymer distribution	nonhomogeneous distribution of polymer within the sample	—	—	Text Qualitative	SI p.S-8 · Bulk EP discussion · Figure S7