Microscopy Morphology — Large Single Crystals of Two-Dimensional π-Conjugated Metal-Organic Frameworks via Biphasic Solution-Solid Growth

Measurement evidence

Microscopy Morphology

Large Single Crystals of Two-Dimensional π-Conjugated Metal-Organic Frameworks via Biphasic Solution-Solid Growth · Ha D.-G., Rezaee M., Han Y. et al. · ACS Central Science · 2021 · 104-109

5 measurement groups · 23 results

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

Optical microscopy of HHTP films after water exposure without nickel acetate

Evaporated HHTP thin film on silicon · Thin Film

Typical growth condition except absence of nickel acetate; patterned HHTP stripe film observed after 1 h and 12 h.

Temperature
95 C growth condition
Atmosphere
Water in vial
Geometry
Confined HHTP film between substrates
Context
HHTP precursor control, not MOF
Measurement source
S7 · Figure caption · Figure S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
HHTP film after 12 h without nickel acetatemostly dissolved in waterCaption
Qualitative
S7 · Figure caption · Figure S2
HHTP film after 1 h without nickel acetateremained solidCaption
Qualitative
S7 · Figure caption · Figure S2

SEM/optical microscopy of synthesis-control morphologies

Ni-CAT-1 grown from drop-cast HHTP control film · Thin Film

Drop-cast HHTP, water-DMF cosolvent, and microsphere-gap controls imaged to test growth mechanism.

Temperature
95 C typical unless otherwise stated
Atmosphere
Water or water-DMF medium
Geometry
Not applicable
Context
Ni-CAT-1 morphology controls
Measurement source
S9-S12 · Figure captions · Figures S4-S7
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Drop-cast HHTP control yield and grain qualitylow yield; hexagonal plates composed of small grainsCaption
Qualitative
S9 · Figure caption · Figure S4
49-um microsphere gap morphologyvery long crystals; aspect ratio >500; no platesCaption
Approximate
S11 · Figure caption · Figure S6A
4-um microsphere gap morphologysome plates; yield, size, and quality lowCaption
Qualitative
S11 · Figure caption · Figure S6C
Local gap from substrate flatnessup to 1.5 umText
Approximate
S4 · Supplementary Text - Estimation of the gap between the two substrates
Equivalent substrate gap from volume estimateequivalent to 6-um gapText
Approximate
S4 · Supplementary Text - Estimation of the gap between the two substrates
Estimated reaction-space volumeless than 1 uLText
Approximate
S4 · Supplementary Text - Estimation of the gap between the two substrates · Figure S16
Diced substrate average peak-to-valley flatness730 nm with standard error of 130 nmstandard error 130 nmText
Exact Reported
S4 · Supplementary Text - Estimation of the gap between the two substrates · Figure S16
Water-DMF cosolvent morphologyrod-shape crystals; no crystal platesCaption
Qualitative
S10 · Figure caption · Figure S5

SEM and optical microscopy of growth at 0.5, 1, 3 and 12 h

Solution-solid-grown Ni-CAT-1 single-crystal plates on Si/SiO2 · Single Crystal

Reaction time varied under typical growth conditions to assess crystal growth and defect correction.

Temperature
95 C growth condition
Atmosphere
Water in vial
Geometry
Not applicable
Context
pristine Ni-CAT-1 crystals
Measurement source
S4 and S8 · Supplementary Text; Figure caption · Figure S3
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Crystal growth at 12 hquality significantly improvedText
Qualitative
S4 · Supplementary Text - Crystal growth with different growth time · Figure S3D
Crystal growth at 1 hplates continuously grow or start to mergeText
Qualitative
S4 · Supplementary Text - Crystal growth with different growth time · Figure S3B
Crystal growth at 30 mina few micrometer size plates are formedText
Qualitative
S4 · Supplementary Text - Crystal growth with different growth time · Figure S3A
Crystal growth at 3 hbigger but edges and corners still dullText
Qualitative
S4 · Supplementary Text - Crystal growth with different growth time · Figure S3C

SEM, optical microscopy, AFM thickness profiling, manual optical crystal counting

Solution-solid-grown Ni-CAT-1 single-crystal plates on Si/SiO2 · Single Crystal

Morphology followed with growth time and quantified by crystal-size yield bins under typical growth conditions.

Temperature
growth at 95 C; imaging at room temperature
Atmosphere
Not applicable
Geometry
Not applicable
Context
pristine Ni-CAT-1 single-crystal plates
Measurement source
p002 · Results and Discussion · Figure 2; Figure S8; Table S2
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Example crystal thickness from Figure 2E profileca. 550-600 nmvisual estimate ca. +/- 75 nmFigure Axis
Approximate
p002 · Figure · Figure 2E
Lateral dimension increase versus needle-shaped crystalsmore than 2 orders of magnitude largerText
Approximate
p003 · Results and Discussion · Figure 2
Large single-crystal lateral dimensionexceeding 10 umText
Rounded Reported
p001 · Abstract
Plate diagonal to thickness ratio10 to 100 times bigger than their thicknessText
Range
S2 · Materials and Methods - Details of growth methods
Crystal count yield, 4-6 um binAverage # 20; standard deviation 7.8standard deviation 7.8SI Table
Exact Reported
S27 · Table S2 · Table S2
Crystal count yield, 6-8 um binAverage # 4.0; standard deviation 1.9standard deviation 1.9SI Table
Exact Reported
S27 · Table S2 · Table S2
Crystal count yield, 8-10 um binAverage # 1.4; standard deviation 1.3standard deviation 1.3SI Table
Exact Reported
S27 · Table S2 · Table S2
Crystal count yield, >10 um binAverage # 0.6; standard deviation 0.9standard deviation 0.9SI Table
Exact Reported
S27 · Table S2 · Table S2

Polarized light microscopy

Solution-solid-grown Ni-CAT-1 single-crystal plates on Si/SiO2 · Single Crystal

No-polarized, plane-polarized and cross-polarized images collected with Nikon Eclipse LV150NA.

Temperature
room temperature
Atmosphere
Not specified
Geometry
Not applicable
Context
pristine Ni-CAT-1 crystals
Measurement source
S24 · Figure caption · Figure S19
PropertyReported valueNormalised valueUncertaintyOrigin and qualitySource
Polarised microscopy support for single crystallinitysupports the single crystallinityCaption
Qualitative
S24 · Figure caption · Figure S19