Synthesis evidence

Cluster-Bridging-Coordinated Bimetallic Metal−Organic Framework as High-Performance Anode Material for Lithium-Ion Storage

Yan W., Fan K., Zheng L.-M. et al. · Small Structures · 2021 · 2100122

5 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

10 · Electrochemical Measurements · Figure 6

Additivesactivated carbon cathode
Substrate orientationHLIC cell with 14 mm diameter electrodes
Oxidant / reductantprelithiated Co4-Ir MOF anode
Work-upActivated carbon cathode paired with prelithiated Co4-Ir MOF anode.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated carbon (AC)2.5 mg cm-2 cathode loading; Co4-Ir MOF:AC approximately 1:510 · Electrochemical Measurements · Figure 6
Otherprelithiated Co4-Ir MOF anode0.5 mg cm-2 anode loading10 · Electrochemical Measurements · Figure 6
Complete recipeSource: Main

Route 2: Other

9 · Electrochemical Measurements

SolventsN-methyl-2-pyrrolidone (NMP)
AdditivesKetjen Black conductive carbon; PVDF binder
Atmosphereambient slurry preparation; vacuum drying
Temperature100
Time6 h stirring; overnight drying
Substrate orientationcopper foil current collector
Work-upHomogeneous slurry coated on copper foil and cut into circular disks of 1.54 cm2.
ActivationDried under vacuum at 100 C overnight; stated to completely remove adsorbed water and solvents.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo4-Ir MOF powdermass ratio 79 · Electrochemical Measurements
AdditiveKetjen Blackmass ratio 1.59 · Electrochemical Measurements
AdditivePVDF bindermass ratio 1.59 · Electrochemical Measurements
SolventN-methyl-2-pyrrolidone (NMP)Not specified9 · Electrochemical Measurements
Complete recipeSource: Main

Route 3: Other

10 · Electrochemical Measurements

SolventsEC/EMC/DEC electrolyte solvent mixture (4:3:3 v/v/v)
Additives1 wt% vinylene carbonate (VC)
Atmosphereargon-filled glove box
Substrate orientationCR2032 coin cell; Celgard 2400 separator
Oxidant / reductantlithium foil counter electrode
Work-upCoin cells assembled for CV, EIS, rate and cycling tests.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteLiPF6 in EC/EMC/DEC1.0 mol L-1; EC/EMC/DEC 4:3:3 v/v/v10 · Electrochemical Measurements
Additivevinylene carbonate (VC)1 wt%10 · Electrochemical Measurements
Otherlithium foilNot specified10 · Electrochemical Measurements
Complete recipeSource: Main

Route 4: Other

10 · Electrochemical Measurements · Figure 5

SolventsNMP for NCM523 cathode slurry; electrolyte added to prelithiate Co4-Ir MOF anode
AdditivesKetjen Black; PVdF-HFP; electrolyte
AtmosphereAr-filled glovebox for prelithiation and full-cell assembly
Temperature100
TimeNCM523 slurry stirred 6 h; cathode dried overnight; Co4-Ir MOF anode prelithiated 24 h
Substrate orientationcarbon-coated aluminium foil cathode; soft-packed full cell
Oxidant / reductantlithium foil contact for anode prelithiation
Work-upNCM523 cathode disks and prelithiated Co4-Ir MOF anode paired in full batteries.
ActivationNCM523 cathode dried under vacuum at 100 C overnight.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherLiNi0.5Co0.2Mn0.3O2 (NCM523)mass ratio 810 · Electrochemical Measurements · Figure 5
AdditiveKetjen Blackmass ratio 110 · Electrochemical Measurements · Figure 5
AdditivePVdF-HFPmass ratio 110 · Electrochemical Measurements · Figure 5
Electrolyteelectrolyte for prelithiation100 uL10 · Electrochemical Measurements · Figure 5
Complete recipeSource: Both

Route 5: Solvothermal

9 · Synthesis of Co4-Ir MOF · Figure S1

Metal precursorsCo(NO3)2.6H2O (0.05 mmol)
Linker precursorsIr(ppy-COOH)3 (0.015 mmol), prepared according to cited literature
Solventsdeionized water (2.0 mL); N,N-dimethylformamide (DMF, 6.0 mL)
AdditivesHCl (12 mol L-1, 23 uL)
Atmospherenot specified
Temperature120
Time48
Work-upGreen powder collected, washed with DMF and ethanol.
ActivationDried under vacuum for 24 h; anode samples later dried under vacuum at 100 C overnight to remove lattice solvents.
Scalability contextYield reported as 65%; no scale-up discussion.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.6H2O0.05 mmol9 · Synthesis of Co4-Ir MOF · Figure S1
LinkerIr(ppy-COOH)30.015 mmol9 · Synthesis of Co4-Ir MOF · Figure S1
Solventdeionized water2.0 mL9 · Synthesis of Co4-Ir MOF · Figure S1
SolventN,N'-dimethylformamide (DMF)6.0 mL9 · Synthesis of Co4-Ir MOF · Figure S1
AcidHCl23 uL · 12 mol L-19 · Synthesis of Co4-Ir MOF · Figure S1