Synthesis evidence

Overscreening-Driven Modulation of Ion Adsorption and Desorption in Conductive MOF Electrodes by Charging Rates

Niu L., Zeng L., Yu D. et al. · ACS Nano · 2025 · 2581-2590

2 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2587 · Methods - EQCM Measurements · Figure 1a

Metal precursorsPre-synthesised Ni3(HITP)2 c-MOF powder
Solventsdeionized water, NMP, acetone
AdditivesNMP temporary adhesive; cellulose microporous membrane, 0.22 um pore diameter
Atmospherenot stated
Temperature80
Time3
Substrate orientationAu-coated quartz sensor, 10 mm diameter quartz area
Work-upDisperse 1 mg powder in 500 uL water and ultrasound 5 min; disperse 120 uL suspension in 200 mL water and ultrasound 10 min; vacuum filter on 0.22 um cellulose membrane; cut 10.5 mm membrane piece; wet-transfer to quartz with NMP; acetone bath 40 min to dissolve membrane.
ActivationVacuum oven at 80 deg C for 3 h before EQCM use.
Scalability contextFilm preparation uses dilute aqueous dispersion and membrane transfer sized to quartz sensors.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Otherc-MOF powder1 mg2587 · Methods - EQCM Measurements · Figure 1a
Solventdeionized water500 uL plus 200 mL2587 · Methods - EQCM Measurements · Figure 1a
AdditiveNMPtemporary adhesive2587 · Methods - EQCM Measurements · Figure 1a
Solventacetonebath, 40 min2587 · Methods - EQCM Measurements · Figure 1a
Othercellulose microporous membrane10.5 mm circular piece · 0.22 um pore diameter2587 · Methods - EQCM Measurements · Figure 1a
Partial recipeSource: Main

Route 2: Other

2587 · Methods - Synthesis of c-MOFs

Metal precursorsNi(OAc)2.4H2O, 120 mL stock solution, 2.33 mmol L^-1 in DMF/DMA (v/v = 1:1)
Linker precursorsHATP.6HCl, 100 mg in 30 mL water
SolventsDMF/DMA (v/v = 1:1), water; workup with water and methanol
AdditivesNaOAc aqueous solution, 80 mL, 2 mol L^-1
Atmospherenot stated
Temperature65
Time4
Work-upCool to room temperature; remove supernatant; centrifuge black precipitate; solvent exchange with water (180 mL x 2) and methanol (180 mL x 2), each exchange agitated for at least 40 min at room temperature; filter solid.
ActivationResidue subjected to vacuum conditions; duration, temperature and pressure not stated for this powder step.
Scalability contextPrepared in a 500 mL beaker from 120 mL metal stock solution plus 80 mL NaOAc solution and 30 mL linker solution.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel(II) acetate tetrahydrate (Ni(OAc)2.4H2O)120 mL stock solution · 2.33 mmol L^-12587 · Methods - Synthesis of c-MOFs
SolventDMF/DMAv/v = 1:12587 · Methods - Synthesis of c-MOFs
BaseNaOAc aqueous solution80 mL · 2 mol L^-12587 · Methods - Synthesis of c-MOFs
Linker2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl)100 mg in 30 mL water2587 · Methods - Synthesis of c-MOFs
Solventwater30 mL linker solution; 180 mL x 2 workup2587 · Methods - Synthesis of c-MOFs
Solventmethanol180 mL x 2 workup2587 · Methods - Synthesis of c-MOFs