Synthesis evidence

Layered coordination polymer with two-dimensional covalent bismuth-organic networks: Semiconductor and lithium ion storage

Li M.-Q., Cao Y., Qin L. et al. · Nano Research · 2024 · 2181-2185

3 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Drop Cast

rendered page 2 · Electrode preparations and testing

Metal precursorsBi-DSBDC-DMA framework powder from route_bi_dsbdc_dma_solvothermal
Solventswater slurry; electrolyte for testing was 1 M LiPF6 in EC/DEC (1/1)
Additivescarbon black (Cabot), CMC binder, polypropylene separator (Celgard 2500)
Atmospherenot reported for slurry preparation; dried in vacuum oven
Temperature120
Timeovernight drying
Substrate orientationCu foil current collector
Oxidant / reductantLi metal counter and pseudo-reference electrode in 2032-type coin cells
Work-upBall-milled water slurry pasted on Cu foil.
ActivationVacuum oven drying at 120 C overnight before coin-cell testing.
Scalability contextStandard small coin-cell electrode fabrication; no loading, electrode area or areal mass loading reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherBi-DSBDC-DMA MOF solid6 parts by massrendered page 2 · Electrode preparations and testing
Additivecarbon black (Cabot)3 parts by massrendered page 2 · Electrode preparations and testing
AdditiveCMC1 part by massrendered page 2 · Electrode preparations and testing
Solventwaterused to make slurryrendered page 2 · Electrode preparations and testing
ElectrolyteLiPF6 in EC/DEC (1/1)1 Mrendered page 2 · Electrode preparations and testing
Complete recipeSource: Both

Route 2: Solvothermal

rendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text

Metal precursorsBiCl3, 63 mg (0.2 mmol; 315.34 g/mol)
Linker precursorsDMBDC/H2DMBDC, 23 mg (0.1 mmol; 230.26 g/mol)
Solvents8 mL dry DMF
Atmospheresealed glass tube; dry DMF; no inert gas atmosphere reported
Temperature120
Time72
Work-upYellow powder isolated by filtration; washed with DMF, ethanol and THF five times each; dried in air.
ActivationNo activation reported for the as-made framework; vacuum drying at 120 C was studied separately and reduced crystallinity.
Scalability contextSmall sealed-tube solvothermal synthesis; no yield or scale-up study reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceBiCl363 mg (0.2 mmol)rendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
LinkerDMBDC (also described in the main text as H2DMBDC / 2,5-dimercaptoterephthalic acid)23 mg (0.1 mmol)rendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
Solventdry DMF8 mLrendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
SolventDMF washwashed 5 timesrendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
Solventethanol washwashed 5 timesrendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
SolventTHF washwashed 5 timesrendered page 2 · Synthesis of Bi-DSBDC-DMA · Scheme 1 in main text
Partial recipeSource: SI

Route 3: Unknown

rendered page 5 · Supplementary figures · Figure S5

Additivesconducting carbon and CMC binder
Atmospherenot reported
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Additiveconducting carbon3 parts by massrendered page 5 · Supplementary figures · Figure S5
AdditiveCMC1 part by massrendered page 5 · Supplementary figures · Figure S5