Microscopy Morphology — Sulfur vacancies enriched Nickel-Cobalt sulfides hollow spheres with high performance for All-Solid-State hybrid supercapacitor

4 measurement groups · 21 results

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

SEM, TEM, XRD and FTIR

Infrared spectroscopy X-ray diffraction and scattering Scanning electron microscopy Transmission electron microscopy

Ni-Co CP spheres · Powder

Precursor sphere morphology and coordination assessed in main text using SI figures.

Context: Pristine coordination-polymer precursor.
Measurement source: main p.3 · 3. Results and discussion · Fig. S1-S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Ni-Co CP sphere diameter upper bound	1-2 um	—	range	Text Range	main p.3 · 3. Results and discussion · Fig. S1
Ni-Co CP sphere diameter lower bound	1-2 um	—	range	Text Range	main p.3 · 3. Results and discussion · Fig. S1
C=O stretching red shift on coordination	about 34 cm-1, from 1694 to 1660 cm-1	—	about	Text Approximate	main p.3 · 3. Results and discussion · Fig. S3

EDS elemental mapping

Elemental microanalysis and mapping

NiCo2S4-6 HSs · Powder

Elemental distribution and atomic ratio of NiCo2S4-6 HSs.

Context: Unreduced sulfide control.
Measurement source: main p.3 · 3. Results and discussion · Fig. S6

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
C EDS atomic fraction in NiCo2S4-6 HSs	78.0 at.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
C EDS weight fraction in NiCo2S4-6 HSs	60.69 wt.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
Co EDS atomic fraction in NiCo2S4-6 HSs	2.45 at.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
Co atomic ratio in NiCo2S4-6 HSs	Ni:Co:S around 1:1.97:4.83	—	around	Text Approximate	main p.3 · 3. Results and discussion · Fig. S6e
Co EDS weight fraction in NiCo2S4-6 HSs	9.36 wt.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
Ni EDS atomic fraction in NiCo2S4-6 HSs	1.24 at.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
Ni atomic ratio in NiCo2S4-6 HSs	Ni:Co:S around 1:1.97:4.83	—	around	Text Approximate	main p.3 · 3. Results and discussion · Fig. S6e
Ni EDS weight fraction in NiCo2S4-6 HSs	4.72 wt.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
O EDS atomic fraction in NiCo2S4-6 HSs	12.3 at.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
O EDS weight fraction in NiCo2S4-6 HSs	12.75 wt.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
S EDS atomic fraction in NiCo2S4-6 HSs	6.01 at.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g
S atomic ratio in NiCo2S4-6 HSs	Ni:Co:S around 1:1.97:4.83	—	around	Text Approximate	main p.3 · 3. Results and discussion · Fig. S6e
S EDS weight fraction in NiCo2S4-6 HSs	12.48 wt.%	—	—	Visual Estimate Rounded Reported	SI rendered p.8 · Figure S6 embedded EDS table · Fig. S6g

SEM, TEM, HRTEM, SAED, HAADF-STEM and EDS mapping

Scanning electron microscopy Transmission electron microscopy Elemental microanalysis and mapping

r-NiCo2S4-6 HSs · Powder

Morphology, shell thickness, lattice planes and elemental distribution of reduced sulfur-vacancy-rich hollow spheres.

Context: Target reduced sulfide.
Measurement source: main p.4 · 3. Results and discussion · Fig. 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
HRTEM lattice spacing assigned to (311)	0.29 nm	—	about	Text Approximate	main p.3 · 3. Results and discussion · Fig. 2e
HRTEM lattice spacing assigned to (400)	0.23 nm	—	about	Text Approximate	main p.3 · 3. Results and discussion · Fig. 2e
r-NiCo2S4-6 HS shell thickness upper bound	20-30 nm	—	range	Text Range	main p.3 · 3. Results and discussion · Fig. 2d, Fig. S7
r-NiCo2S4-6 HS shell thickness lower bound	20-30 nm	—	range	Text Range	main p.3 · 3. Results and discussion · Fig. 2d, Fig. S7

SEM/TEM and XRD during sulfidation evolution

X-ray diffraction and scattering Scanning electron microscopy Transmission electron microscopy

NiCo2S4-X HSs intermediates (X = 0.5, 1, 2, 4 h) · Powder

NiCo2S4 hollow sphere evolution at 160 C for 0.5, 1, 2, 4 and 6 h.

Context: Unreduced derived sulfide intermediates.
Measurement source: SI rendered pp.5-7 · Figure S4 caption and paragraph · Fig. S4, Fig. S5

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Hollow-sphere evolution mechanism	Three-step anion-exchange/diffusion process: core-shell at 0.5-1 h, shell-gap structure at 2-4 h, hollow spheres at 6 h.	—	—	Text Qualitative	SI text · Figure S4 paragraph · Fig. S4