Electrochemistry Application — Direct Electrodeposition of Electrically Conducting Ni3(HITP)2 MOF Nanostructures for Micro-Supercapacitor Integration

8 measurement groups · 30 results

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

CV and EIS of bare Pt/Pt interdigitated control

Impedance spectroscopy Voltammetry

Bare Pt/Pt interdigitated microelectrode · Electrode

Bare and Ni3(HITP)2-coated microelectrodes compared; CV at 5 V s-1, 0-1 V in 1.0 M KOH; EIS 1 Hz to 200 kHz, 5 mV amplitude.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox for micro-supercapacitor analyses
Geometry: bare Pt/Pt interdigitated microelectrode
Context: non-MOF control for device comparison
Measurement source: SI-16 to SI-17 · Figures S12-S13 · Figures S12, S13

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Coated device current relative to bare Pt/Pt MSC	higher current delivery compared to bare uncoated Pt/Pt MSC	—	qualitative comparison	Text Qualitative	6 · Results and Discussion · Figure S12

Chronoamperometry during continuous and pulsed potentiostatic anodic deposition

Chronoamperometry

Optimised pulsed potentiostatic Ni3(HITP)2 film from MeOH-DMSO bath · Thin Film

MeOH-DMSO bath; continuous versus square pulsed deposition; t_on = 1 min, V_on = 0.8 V, t_off = 1 min, V_off = open circuit voltage.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox
Geometry: 3-electrode deposition cell
Context: pristine Ni3(HITP)2 film growth optimisation
Measurement source: 5 · Figure caption · Figure 2C

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Organic pulsed route selected for further studiesMarked as a best value within this paper	pulsed potentiostatic deposition in MeOH-DMSO selected as most appropriate for further studies and device integration	—	—	Text Qualitative	5 · Results and Discussion · Figures 2-3

Cyclic voltammetry of Ni3(HITP)2 electrolytic bath

Voltammetry

Potentiostatic Ni3(HITP)2 film from H2O-DMF-DMA bath · Thin Film

H2O-DMF-DMA mixed-solvent bath, scan rate 10 mV s-1 vs Ag wire; cycles 1-5 shown.

Temperature: room temperature/not specified
Atmosphere: Ar flow for aqueous bath experiments
Geometry: 3-electrode cell, ITO-coated glass working electrode
Context: pristine aqueous-bath film deposition
Measurement source: SI-7 · Figure S3 · Figure S3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Aqueous bath HATP oxidation onset	onset of HATP oxidation is taking place at 0.2 V	—	—	Caption Rounded Reported	SI-7 · Figure S3 caption · Figure S3
Aqueous bath maximum HATP oxidation rate potential	maximal oxidation rate of HATP is occurring at about 0.3 V	—	about	Caption Approximate	SI-7 · Figure S3 caption · Figure S3

Cyclic voltammetry of individual bath constituents and combined Ni3(HITP)2 precursor bath

Voltammetry

Ni3(HITP)2 deposits on ITO from cyclic-voltammetry electrodeposition · Thin Film

ITO working electrode, scan rate 10 mV s-1, potential window -0.5 to 1.0 V vs Ag pseudo-reference; MeOH-DMSO component screening in glovebox.

Temperature: room temperature/not specified
Atmosphere: Ar/glovebox for MeOH-DMSO experiments
Geometry: 3-electrode cell with ITO WE, Pt CE, Ag pseudo-reference
Context: pristine Ni3(HITP)2 deposition mechanism
Measurement source: 3 · Results and Discussion · Figure 1B

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Combined HATP/Ni(OAc)2 bath oxidation onset	oxidation onset at 0.05 V vs Ag	—	—	Text Rounded Reported	4 · Results and Discussion · Figure 1B
Associated reverse-scan reduction peak	associated reduction peak at about -0.05 V versus Ag	—	about	Text Approximate	4 · Results and Discussion · Figure 1B
Film observed after first CV scan	dark blue translucent reflection covered the working electrode after first CV scan	—	—	Text Qualitative	4 · Results and Discussion · Figure S2
HATP anodic process potential	sharp anodic process at about 0.3 V vs Ag	—	about	Text Approximate	4 · Results and Discussion · Figure 1B

Two-electrode cyclic voltammetry of Ni3(HITP)2 micro-supercapacitor

Voltammetry

Ni3(HITP)2-coated Pt/Pt interdigitated micro-supercapacitor · Electrode

1.0 M KOH aqueous electrolyte; voltage windows 0-0.5 V, 0-0.8 V and 0-1.0 V depending on test; scan rates 1-20 V s-1 in SI methods, main data show 1, 2, 5 and 10 V s-1.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox for micro-supercapacitor CV/EIS per SI
Geometry: Pt-Ni3(HITP)2/Pt-Ni3(HITP)2 interdigitated microdevice, footprint-normalised current/capacitance
Context: application device using Ni3(HITP)2-coated Pt current collectors
Measurement source: 8 · Figure caption · Figure 6C

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Average areal capacitance in 0-0.5 V window	0.27 mF cm-2	0.00027 F cm-2	—	Text Exact Reported	7 · Results and Discussion · Figure S14
Average areal capacitance/capacity in 0-0.8 V windowMarked as a best value within this paper	0.48 mF cm-2	0.00048 F cm-2	—	Text Exact Reported	7 · Results and Discussion · Figure 6C
Electrodeposition charge on lower-loaded interdigit electrode side	100 microC	0.0001 C	—	Text Exact Reported	6 · Results and Discussion · Figure S11
Reversible oxidation peak in 0-0.8 V window	oxidation peak at about 0.6 V	—	about	Text Approximate	7 · Results and Discussion · Figure 6C
0-1 V CV redox peak potential	redox peak at about 0.5 V at 5 V s-1	—	about	Text Approximate	6 · Results and Discussion · Figure S12
Reversible reduction peak in 0-0.8 V window	reduction peak at about 0.3 V	—	about	Text Approximate	7 · Results and Discussion · Figure 6C
Electrodeposition charge on higher-loaded interdigit electrode side	400 microC	0.0004 C	—	Text Exact Reported	6 · Results and Discussion · Figure S11
Figure S14 0-0.5 V areal capacity at 10 V s-1	about 0.024 mC cm-2 from Figure S14 axis	0.000024 C cm-2	visual estimate from plotted point	Figure Axis Approximate	SI-18 · Figure S14 · Figure S14
Figure S14 0-0.5 V areal capacity at 1 V s-1	about 0.039 mC cm-2 from Figure S14 axis	0.000039 C cm-2	visual estimate from plotted point	Figure Axis Approximate	SI-18 · Figure S14 · Figure S14
Figure S14 0-0.8 V areal capacity at 10 V s-1	about 0.081 mC cm-2 from Figure S14 axis	0.000081 C cm-2	visual estimate from plotted point	Figure Axis Approximate	SI-18 · Figure S14 · Figure S14
Figure S14 0-0.8 V areal capacity at 1 V s-1	about 0.131 mC cm-2 from Figure S14 axis	0.000131 C cm-2	visual estimate from plotted point	Figure Axis Approximate	SI-18 · Figure S14 · Figure S14

Electrochemical impedance spectroscopy and complex capacitance frequency analysis

Impedance spectroscopy

Ni3(HITP)2-coated Pt/Pt interdigitated micro-supercapacitor · Electrode

EIS from 1 Hz to 200 kHz, AC amplitude 5 mV; imaginary capacitance maximum used for characteristic frequency and relaxation time.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox
Geometry: Ni3(HITP)2-coated interdigitated microelectrodes in 1 M KOH
Context: application device using Ni3(HITP)2 coating
Measurement source: 6 · Results and Discussion · Figure S13

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Characteristic capacitive frequencyMarked as a best value within this paper	1160.7 Hz	—	—	Text Exact Reported	6 · Results and Discussion · Figure S13B
Interfacial/solution resistance caveat	high solution resistance indicates increased interfacial resistance of Ni3(HITP)2	—	—	Text Qualitative	6 · Results and Discussion · Figure S13A
Relaxation time constantMarked as a best value within this paper	0.9 ms	0.0009 s	—	Text Exact Reported	6 · Results and Discussion · Figure S13B

Power-law b-value and Dunn-type capacitive/diffusive contribution analysis

Ni3(HITP)2-coated Pt/Pt interdigitated micro-supercapacitor · Electrode

Log-log peak current density versus scan rate for 0-0.8 V window at 1-10 V s-1; i(V)=a1*v+a2*v^1/2 analysis for anodic/cathodic scans.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox for electrochemical measurements
Geometry: Ni3(HITP)2-coated interdigitated micro-supercapacitor
Context: application device kinetic analysis
Measurement source: SI-19 to SI-20 · Figures S15-S16 · Figures S15, S16

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Anodic b-value	anodic b-value of 0.63	—	—	Text Exact Reported	7 · Results and Discussion · Figure S15
Cathodic b-value	cathodic b-value of 0.87	—	—	Text Exact Reported	7 · Results and Discussion · Figure S15
Non-diffusive contribution at 10 V s-1Marked as a best value within this paper	reaching up to 75% at 10 V s-1	0.75 fraction	up to	Text Rounded Reported	7 · Results and Discussion · Figure 6E
Non-diffusive contribution at 1 V s-1	about 40% from Figure 6E histogram	0.4 fraction	visual estimate	Visual Estimate Approximate	8 · Figure 6E · Figure 6E
Non-diffusive contribution at 2 V s-1	about 55% from Figure 6E histogram	0.55 fraction	visual estimate	Visual Estimate Approximate	8 · Figure 6E · Figure 6E
Non-diffusive current contribution at 5 V s-1	65% at a scan rate of 5 V s-1	0.65 fraction	—	Text Exact Reported	7 · Results and Discussion · Figure 6D

Cycling stability by cyclic voltammetry

Voltammetry

Ni3(HITP)2-coated Pt/Pt interdigitated micro-supercapacitor · Electrode

1000 CV cycles at 5 V s-1 in voltage windows 0-0.5 V and 0-0.8 V.

Temperature: room temperature/not specified
Atmosphere: Ar-filled glovebox
Geometry: Ni3(HITP)2-coated interdigitated micro-supercapacitor
Context: application device stability
Measurement source: 8 · Figure caption · Figure 6F

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Cycling stability test length	1000 cycles at 5 V s-1	—	—	Text Exact Reported	7 · Results and Discussion · Figure 6F
Capacitive-regime stability after cycling	no visible change in the capacitive regimes (0-0.5 V)	—	qualitative visual comparison	Text Qualitative	7 · Results and Discussion · Figure 6F