Synthesis evidence

Conductive metal-organic frameworks promoting polysulfides transformation in lithium-sulfur batteries

Wang S., Huang F., Zhang Z. et al. · Journal of Energy Chemistry · 2021 · 336-343

4 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

p002 / article p337 · 2.2 Oxidation of carbon paper

Additivesconcentrated nitric acid and concentrated sulfuric acid (3:1 by volume)
Atmosphereambient/not specified
Temperature80
Timeovernight
Substrate orientationCP circular disks with 12 or 16 mm diameter
Oxidant / reductantconcentrated HNO3/H2SO4 oxidative acid treatment
Work-upMixture slowly poured over ice; oxidized CP rinsed with deionized water and ethanol several times.
ActivationDried under vacuum at 70 degC for 12 h.
Scalability contextDisk diameters of 12 or 16 mm are compatible with coin-cell cathode preparation; acid oxidation is substrate pretreatment.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othercarbon paper (YLS-30 T)circular disks; 12 or 16 mm diameterp002 / article p337 · 2.2 Oxidation of carbon paper
Oxidantconcentrated nitric acid3:1 HNO3:H2SO4 mixture by volume · concentrated; ARp002 / article p337 · 2.2 Oxidation of carbon paper
Acidconcentrated sulfuric acid3:1 HNO3:H2SO4 mixture by volume · concentrated; ARp002 / article p337 · 2.2 Oxidation of carbon paper
Partial recipeSource: Main

Route 2: Solvothermal

p003 / article p338 · 2.4 Preparation of Ni-BTC@CP

Metal precursorsNi(NO3)2.6H2O
Linker precursors1,3,5-benzenetricarboxylic acid
SolventsDMF (2 mL); ethanol for activation
Atmospherenot specified
Temperature105
Time48
Substrate orientationpiece of oxidized CP placed in 20 mL glass bottle
Work-upCarbon paper rinsed with fresh DMF and ethanol several times.
ActivationModified carbon paper immersed in fresh ethanol in capped glass vial at 70 degC for 5 h, repeated several times; dried under vacuum at 85 degC for 12 h.
Scalability contextBatch size uses 20 mL glass bottle and one oxidized CP piece; absolute precursor masses are omitted, only mass ratio is given.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linker1,3,5-Benzenetricarboxylic acid7:10 by mass relative to Ni(NO3)2.6H2Op003 / article p338 · 2.4 Preparation of Ni-BTC@CP
Metal SourceNi (NO3)2.6H2O10:7 by mass relative to BTC linkerp003 / article p338 · 2.4 Preparation of Ni-BTC@CP
SolventDMF2 mLp003 / article p338 · 2.4 Preparation of Ni-BTC@CP
Solventethanolfresh ethanol for repeated activationp003 / article p338 · 2.4 Preparation of Ni-BTC@CP
Otheroxidized CPone piecep003 / article p338 · 2.4 Preparation of Ni-BTC@CP
Partial recipeSource: Main

Route 3: Solvothermal

p002 / article p337 · 2.3 Preparation of Ni-HHTP@CP

Metal precursorsNi(OAc)2.4H2O
Linker precursorsHHTP
Solventsdeionized water (1 mL) and DMF (1 mL)
Atmospherenot specified
Temperature85
Time24
Substrate orientationpiece of oxidized CP placed in 20 mL glass bottle
Work-upCooled naturally to room temperature; obtained CP washed with deionized water and acetone several times.
ActivationDried under vacuum at 85 degC for 12 h.
Scalability contextBatch size uses 20 mL glass bottle and one CP disk/piece; absolute precursor masses are omitted, only mass ratio is given.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP7:10 by mass relative to Ni(OAc)2.4H2Op002 / article p337 · 2.3 Preparation of Ni-HHTP@CP
Metal SourceNi (OAc)2.4H2O10:7 by mass relative to HHTPp002 / article p337 · 2.3 Preparation of Ni-HHTP@CP
Solventdeionized water1 mLp002 / article p337 · 2.3 Preparation of Ni-HHTP@CP
SolventDMF1 mLp002 / article p337 · 2.3 Preparation of Ni-HHTP@CP
Otheroxidized CPone piecep002 / article p337 · 2.3 Preparation of Ni-HHTP@CP
Vague recipeSource: Main

Route 4: Solvothermal

p003 / article p338 · Results and discussion · Fig. 2a

Metal precursorsnickel acetate / Ni(OAc)2
Linker precursorsHHTP
Solventsnot fully specified for particle synthesis in supplied main text
Atmospherenot specified
Work-upnot specified in supplied main text
ActivationParticles heated at 80 degC under vacuum overnight before adsorption tests.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate (Ni(OAc)2)Not specifiedp003 / article p338 · Results and discussion · Fig. 2a
Linker2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)Not specifiedp003 / article p338 · Results and discussion · Fig. 2a