Microscopy Morphology — Conductive, Large-Area, and Continuous 7,7,8,8-Tetracyanoquinodimethane@HKUST-1 Thin Films Fabricated Using Solution Shearing

Measurement evidence

Microscopy Morphology

Conductive, Large-Area, and Continuous 7,7,8,8-Tetracyanoquinodimethane@HKUST-1 Thin Films Fabricated Using Solution Shearing · Jung S., Huelsenbeck L., Hu Q. et al. · ACS Applied Materials and Interfaces · 2021 · 10202-10209

9 measurement groups · 20 results

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

Fiji image analysis of film coverage

Solution-sheared HKUST-1 thin film, 4 cycles · Thin Film

Thin-film coverage quantified for solution-shearing cycle count; detailed table in missing SI.

Context
pristine HKUST-1 film coverage
Measurement source
S-6 · Supporting Information · Table S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
HKUST-1 thin-film coverage after 1 solution-shearing cycle60 +/- 1.1%+/- 1.1%SI Table
Exact Reported
S-6 · Supporting Information · Table S1
HKUST-1 thin-film coverage after 2 solution-shearing cycles80 +/- 0.9%+/- 0.9%SI Table
Exact Reported
S-6 · Supporting Information · Table S1
HKUST-1 thin-film coverage after 3 solution-shearing cycles89 +/- 0.7%+/- 0.7%SI Table
Exact Reported
S-6 · Supporting Information · Table S1
HKUST-1 thin-film coverage after 4 solution-shearing cyclesMarked as a best value within this paper99 +/- 0.6%+/- 0.6%SI Table
Exact Reported
S-6 · Supporting Information · Table S1

Energy dispersive spectroscopy (EDS) elemental mapping with SEM image

Solution-sheared HKUST-1 thin film, 1 cycle · Thin Film

1st solution-sheared HKUST-1 thin film; Cu and Si maps compared.

Context
pristine HKUST-1 thin film after one cycle
Measurement source
S-3 · Supporting Information · Figure S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
One-cycle EDS indicates exposed Si-rich substrate regionscomposition of Si is higher than that of CuCaption
Qualitative
S-3 · Supporting Information · Figure S2

Energy dispersive spectroscopy (EDS) elemental mapping with SEM image

Solution-sheared HKUST-1 thin film, 4 cycles · Thin Film

4th solution-sheared HKUST-1 thin film; Cu and Si maps compared.

Context
pristine HKUST-1 thin film after four cycles
Measurement source
S-4 · Supporting Information · Figure S3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Four-cycle EDS indicates complete HKUST-1 coverage except crack regionSi is low... HKUST-1 thin film is completely covered via multiple cyclesCaption
Qualitative
S-4 · Supporting Information · Figure S3

Bruker Dektak XT profilometer

Solution-sheared HKUST-1 thin film, 4 cycles · Thin Film

Thickness measured with 800 um scan length for HKUST-1 films after multiple solution-shearing cycles.

Context
pristine HKUST-1 thin-film thickness evolution
Measurement source
10204-10205 · Characterizations; Results and Discussion · Figure 2D
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
HKUST-1 film thickness after 1 solution-shearing cycle2.1 +/- 0.4 um+/- 0.4 umText
Exact Reported
10205 · Results and Discussion · Figure 2D
HKUST-1 film thickness after 2 solution-shearing cyclesca. 3.3 um from Figure 2Dvisually estimated error bar ca. +/- 0.4 umFigure Axis
Approximate
10204 · Results and Discussion · Figure 2D
HKUST-1 film thickness after 3 solution-shearing cyclesca. 4.7 um from Figure 2Dvisually estimated error bar ca. +/- 0.3 umFigure Axis
Approximate
10204 · Results and Discussion · Figure 2D
HKUST-1 film thickness after 4 solution-shearing cyclesMarked as a best value within this paper5.4 +/- 0.8 um+/- 0.8 umText
Exact Reported
10205 · Results and Discussion · Figure 2D
Average thickness increase per solution-shearing cycleincreasing by an average of 1.2 um per cycleText
Rounded Reported
10205 · Results and Discussion · Figure 2D

Scanning electron microscopy (FEI Quanta 650 SEM)

Solution-sheared HKUST-1 thin film, 4 cycles · Thin Film

SEM comparison of 1st, 2nd, and 4th solution-shearing cycles.

Context
pristine HKUST-1 cycle-dependent film coverage
Measurement source
10204 · Experimental Section; Results and Discussion · Figure 2A-C
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
No void regions observed in 4-cycle HKUST-1 filmMarked as a best value within this paperNo void regions are observed down to the resolution of SEM and EDS.Text
Qualitative
10205 · Results and Discussion · Figures 2C and S3

Scanning electron microscopy

Solution-sheared HKUST-1 thin film, 4 cycles · Thin Film

Intergrown HKUST-1 crystals after multiple solution-shearing cycles.

Context
pristine HKUST-1 thin film after multiple cycles
Measurement source
S-5 · Supporting Information · Figure S4
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Multiple cycles produce intergrown HKUST-1 crystals sharing crystal planesHKUST-1 crystal shares their crystal plane with neighbor crystalsCaption
Qualitative
S-5 · Supporting Information · Figure S4

Scanning electron microscopy

TCNQ@HKUST-1 thin film, 168 h TCNQ soak · Thin Film

SEM comparison of pristine HKUST-1, 24 h TCNQ@HKUST-1, and 168 h TCNQ@HKUST-1.

Context
guest-loaded target morphology and Cu(TCNQ) byproduct check
Measurement source
10206 · Results and Discussion · Figure 4A-C
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Solvent-exchanged TCNQ@HKUST-1 lacks worm-like Cu(TCNQ) morphologydoes not show the worm-like morphology that indicates the formation of Cu(TCNQ)Text
Qualitative
10206 · Results and Discussion · Figure 4A-C

Scanning electron microscopy

Thermally activated TCNQ@HKUST-1 thin films, 72 and 168 h TCNQ soak · Thin Film

Thermally activated HKUST-1 thin films soaked in TCNQ solution for 72 h and 168 h.

Context
thermal activation comparison for TCNQ@HKUST-1
Measurement source
S-8 · Supporting Information · Figure S6
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Thermally activated TCNQ@HKUST-1 shows worm-shaped crystals after 168 hSEM image of thermally activated 168 hrs of TCNQ@HKUST-1; worm-shaped crystals noted for this seriesCaption
Qualitative
S-8 · Supporting Information · Figure S6B
Thermally activated TCNQ@HKUST-1 shows worm-shaped crystals after 72 hworm-shaped crystals after 72 hours; may represent Cu(TCNQ) side productCaption
Qualitative
S-8 · Supporting Information · Figure S6A

Optical microscopy with Fiji coverage quantification

HKUST-1 thin films from solution-shearing parameter screen · Thin Film

Heated-substrate temperature and coating speed varied: 160 deg C at 0.1, 0.5, and 1.5 mm s-1; 100 deg C at 0.5 mm s-1.

Context
pristine HKUST-1 thin-film parameter screen
Measurement source
S-2 · Supporting Information · Figure S1
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Optical-image film coverage at 0.1 mm s-1 and 160 deg CMarked as a best value within this paper98.8%Visual Estimate
Rounded Reported
S-2 · Supporting Information · Figure S1A
Optical-image film coverage at 0.5 mm s-1 and 100 deg C83.9%Visual Estimate
Rounded Reported
S-2 · Supporting Information · Figure S1D
Optical-image film coverage at 0.5 mm s-1 and 160 deg C95.0%Visual Estimate
Rounded Reported
S-2 · Supporting Information · Figure S1B
Optical-image film coverage at 1.5 mm s-1 and 160 deg C76.4%Visual Estimate
Rounded Reported
S-2 · Supporting Information · Figure S1C