Synthesis · Soft Electrochemical Actuators with a Two-Dimensional Conductive Metal-Organic Framework Nanowire Array

5 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Complete recipeSource: SI

Route 1: Other

p005 / SI p.S2 · Fabrication and functionalization of CNF film

SolventsDMF for 10 wt% PAN solution; concentrated hydrochloric acid for post-treatment

AtmosphereAir for oxidative stabilisation; Ar2 atmosphere for carbonisation

Temperature60; 280; 800; 60

Time12; 2; 2; 4

Substrate orientationaluminium collector roller during electrospinning

Oxidant / reductantAir oxidative stabilisation; HCl functionalisation

Work-upElectrospun PAN fibres stabilised, carbonised, then immersed in concentrated HCl to generate -COOH, -OH and C=O surface groups.

Scalability contextElectrospinning used 5 mL syringe, 10 kV, 15 cm tip-collector distance, 50 rpm collector and 0.08 mL/min flow rate.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	polyacrylonitrile (PAN)	10 wt% solution · 10 wt% in DMF	p005 / SI p.S2 · Fabrication and functionalization of CNF film
Solvent	N,N-dimethylformamide (DMF)	Not specified	p005 / SI p.S2 · Fabrication and functionalization of CNF film
Acid	concentrated hydrochloric acid	concentrated	p005 / SI p.S2 · Fabrication and functionalization of CNF film

Complete recipeSource: SI

Route 2: Drop Cast

p006 / SI p.S3 · Fabrication of EMImTFSI/PVDF IL gels electrolyte

SolventsDMF

AdditivesEMImTFSI ionic liquid; PVDF

Atmospherevacuum drying

Temperature70

Time12

Substrate orientationTeflon mould

Work-upResulting electrolyte membrane peeled off from mould and used as-prepared.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PVDF	1.0 g	p006 / SI p.S3 · Fabrication of EMImTFSI/PVDF IL gels electrolyte
Electrolyte	1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide (EMImTFSI)	1.5 g	p006 / SI p.S3 · Fabrication of EMImTFSI/PVDF IL gels electrolyte
Solvent	DMF	30 mL	p006 / SI p.S3 · Fabrication of EMImTFSI/PVDF IL gels electrolyte

Complete recipeSource: Both

Route 3: Other

p006 / SI p.S3 · Fabrication of the Ni-CAT NWAs/CNF based electrochemical actuators · Figure 4a

Metal precursorsNi-CAT NWAs/CNF electrode layers

Linker precursorsNi-CAT NWAs/CNF electrode layers

AdditivesEMImTFSI/PVDF ionic-liquid gel electrolyte membrane

Atmospherenot specified

Temperature120

Substrate orientationbimorph sandwich: Ni-CAT NWAs/CNF electrode / gel electrolyte / Ni-CAT NWAs/CNF electrode

Work-upMechanical lamination via hot-press process to yield about 80 um thick actuator strips.

Scalability contextTypical actuator dimensions: 3 mm wide, 25 mm long and 80 um thick.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-CAT NWAs/CNF electrode layers	two pieces	p006 / SI p.S3 · Fabrication of the Ni-CAT NWAs/CNF based electrochemical actuators · Figure 4a
Electrolyte	EMImTFSI/PVDF IL gels electrolyte layer	one layer	p006 / SI p.S3 · Fabrication of the Ni-CAT NWAs/CNF based electrochemical actuators · Figure 4a

Complete recipeSource: Both

Route 4: Hydrothermal

p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP

Solventsdeionized water, ethanol, acetone

Additivesfunctionalised CNF film

Atmospheresealed 20 mL vessel; vacuum activation; atmosphere otherwise not specified

Temperature60; 80; 80

Time4; 12; 24

Substrate orientationfunctionalised CNF film immersed in precursor dispersion

Work-upNaturally cooled within 1 h; membrane washed with deionized water and ethanol three times and freeze-dried overnight.

ActivationImmersed in deionized water at 80 C for 12 h, solvent-exchanged with acetone refreshed twice per day for three days, then evacuated under vacuum at 80 C for 24 h.

Scalability contextThe length of Ni-CAT NWAs was controlled by hydrothermal reaction time.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Nickel(II) acetate tetrahydrate (Ni(OAc)2.4H2O, >=99.5%)	20 mg	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a
Linker	2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)	14 mg	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a
Solvent	deionized water	8 mL for synthesis; water at 80 C for activation	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a
Solvent	ethanol	wash three times · >=99.5%	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a
Solvent	acetone	solvent exchange for three days	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a
Additive	functionalized CNF film	a piece	p005-p006 / SI p.S2-S3 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film; Activation · Figure 1a

Partial recipeSource: SI

Route 5: Hydrothermal

p005 / SI p.S2 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP

Solventsdeionized water

Atmospheresealed 20 mL vessel; atmosphere not otherwise specified

Temperature60

Time4

Work-upSame protocol as Ni-CAT NWAs/CNF but without functionalised CNF film; post-synthesis workup for powder not separately detailed.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(OAc)2.4H2O	20 mg	p005 / SI p.S2 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film
Linker	2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)	14 mg	p005 / SI p.S2 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film
Solvent	deionized water	8 mL	p005 / SI p.S2 · Synthesis of Ni-CAT powder and Ni-CAT nanowire array on CNF film