Synthesis evidence

From zinc-cyanide hybrid coordination polymers to hierarchical yolk-shell structures for high-performance and ultra-stable lithium-ion batteries

Fan H., Yu H., Zhang Y. et al. · Nano Energy · 2017 · 168-176

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

169 · 2.3. Electrochemical measurements

Metal precursorsYC-ZnO active material
SolventsN-methyl-2-pyrrolidone (NMP)
Additivesacetylene black; PVDF binder
Atmosphereargon-filled glove box for cell assembly
Temperature70
Timeovernight drying
Substrate orientationcopper foil current collector
Work-upSlurry coated on copper foils.
ActivationDried at 70 deg C overnight.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Otherelectrode material70 wt%169 · 2.3. Electrochemical measurements
Additiveacetylene black20 wt%169 · 2.3. Electrochemical measurements
Additivepoly(vinyldifluoride) (PVDF)10 wt%169 · 2.3. Electrochemical measurements
SolventN-methyl-2-pyrrolidone (NMP)Not specified169 · 2.3. Electrochemical measurements
ElectrolyteLiPF6 in ethylene carbonate/diethyl carbonate1 M LiPF6 in EC/DEC (1:1, w/w)169 · 2.3. Electrochemical measurements
Complete recipeSource: Main

Route 2: Other

169 · 2.1. Preparation

Metal precursorsZnCP microspheres
Linker precursorscyanide in ZnCP precursor, converted to carbon/N-containing carbon residue
Atmosphereargon followed by air
Temperature500 then 300
Time3 then 3
Oxidant / reductantargon pyrolysis followed by air oxidation
Work-upCooled to room temperature between calcination steps.
ActivationHeating rate 2 deg C min-1 for both steps.
Scalability contextPrepared from 50 mg ZnCP precursor in the reported recipe; authors state large-scale synthesis could be expected.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherZnCP microspheres50 mg169 · 2.1. Preparation
Complete recipeSource: Main

Route 3: Other

169 · 2.1. Preparation

Metal precursorsZnCl2.6H2O; K2Zn(CN)4
Linker precursorscyanide supplied by K2Zn(CN)4
Solventsdeionized water
AdditivesPVP
Atmosphereambient air
Temperatureroom temperature; dried at 60
Time0.5 h stirring plus 24 h stationary ageing; 24 h drying
Work-upWhite precipitate filtered and washed several times.
ActivationVacuum drying oven at 60 deg C for 24 h.
Scalability contextConclusion states large-scale synthesis could be expected, but no batch scale beyond 50 mg precursor conversion is demonstrated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
AdditivePVP0.4 g169 · 2.1. Preparation
Metal SourceZnCl2.6H2O0.2 mmol · in 20 mL deionized water with PVP169 · 2.1. Preparation
Metal SourceK2Zn(CN)40.2 mmol · in another 20 mL deionized water169 · 2.1. Preparation
Solventdeionized water20 mL + 20 mL169 · 2.1. Preparation
Complete recipeSource: Main

Route 4: Other

169 · 2.1. Preparation

Metal precursorsZnCP microspheres
Linker precursorscyanide in ZnCP precursor
Atmosphereair
Temperature500
Time3
Oxidant / reductantair as oxidising atmosphere
Work-upCalcined in a corundum crucible.
ActivationHeating rate 2 deg C min-1.
Scalability contextPrepared from 50 mg ZnCP precursor in the reported recipe.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherZnCP microspheres50 mg169 · 2.1. Preparation