Synthesis evidence

Conductive metal-organic framework flowers facilitate the anchoring and conversion kinetics of polysulfides for lithium‑sulfur batteries

Zhao X., Wang Y., Fan Y. et al. · Journal of Energy Storage · 2023 · 108010

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

p002-p003 · 2.3. Package of LSBs

SolventsCS2; N-methyl-2-pyrrolidone; electrolyte DOL/DME 1:1 with LiTFSI/LiNO3
AdditivesSuper P and PVDF binder; LiTFSI and LiNO3 electrolyte salts
Atmosphereglove box for CNT/S preparation and coin-cell packaging
Temperature155
Substrate orientationslurry coated on Al plate and punched into 10 mm disks
Oxidant / reductantsulfur and Li metal used in final cell
Work-upCNT/S active material mixed with Super P and PVDF at mass ratio 8:1:1 in NMP; coated on Al plate
Activationnot specified
Scalability contextCoin-type Li-S cells; sulfur loading around 2.0 mg cm-2 for standard tests.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
OtherCNT powderCNT:sulfur mass ratio 1:3p002-p003 · 2.3. Package of LSBs
OthersulfurCNT:sulfur mass ratio 1:3 · 99.99%p002-p003 · 2.3. Package of LSBs
SolventCS2added slowlyp002-p003 · 2.3. Package of LSBs
SolventN-methyl-2-pyrrolidoneNot specifiedp002-p003 · 2.3. Package of LSBs
AdditiveSuper Pactive:Super P:PVDF = 8:1:1p002-p003 · 2.3. Package of LSBs
AdditivePVDFactive:Super P:PVDF = 8:1:1p002-p003 · 2.3. Package of LSBs
Electrolytelithium bis(trifluoromethanesulphonyl)imide1 Mp002-p003 · 2.3. Package of LSBs
Electrolytelithium nitrate0.1 Mp002-p003 · 2.3. Package of LSBs
Partial recipeSource: Main

Route 2: Other

p003 · 2.4. Preparation of LPS solutions

Solventsthe Li-S electrolyte (specific composition not repeated in this section)
Atmospherenot specified
Temperature50
Time24
Oxidant / reductantLi2S and sulfur, molar ratio 1:5
Work-upused directly for adsorption and permeation experiments
Activationnot applicable
Scalability contextSolution concentration 0.1 M; no volume stated.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherLi2Smolar ratio Li2S:sulfur = 1:5p003 · 2.4. Preparation of LPS solutions
Othersulfurmolar ratio Li2S:sulfur = 1:5p003 · 2.4. Preparation of LPS solutions
ElectrolyteLi-S battery electrolyte0.1 M Li2S6 finalp003 · 2.4. Preparation of LPS solutions
Partial recipeSource: Main

Route 3: Other

p003 · 2.4. Preparation of LPS solutions

Solvents15 mL DOL/DME, 1:1 by volume
Atmospherenot specified
Temperature55
Oxidant / reductant16.8 mg sulfur and 3.5 mg Li2S
Work-upused for Li2S precipitation experiment
Activationnot applicable
Scalability context5 mM Li2S8 solution in 15 mL solvent; reaction time not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othersulfur16.8 mgp003 · 2.4. Preparation of LPS solutions
OtherLi2S3.5 mgp003 · 2.4. Preparation of LPS solutions
SolventDOL/DME15 mL, 1:1 by volume · 5 mM Li2S8 finalp003 · 2.4. Preparation of LPS solutions
Complete recipeSource: Main

Route 4: Hydrothermal

p002 · 2.2. Synthesis of flowery MIL-47 layer

Metal precursorsVOSO4.xH2O, 0.122 g
Linker precursorsH2BDC, 0.125 g
Solvents60 mL deionized water; water and ethanol washes
AdditivesCNT wafer pretreated with HNO3/H2SO4 (v/v 3:1)
Atmospheresealed hydrothermal autoclave; gas atmosphere not specified
Temperature160
Time48
Substrate orientationprocessed CNT wafer fastened into Teflon fillister, vertically and completely immersed in the precursor solution
Work-upwashed with water and ethanol
Activationvacuum dried at 60 deg C overnight
Scalability context100 mL autoclave, 19 mm CNT wafers; no scale-up demonstrated.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceVOSO4.xH2O0.122 gp002 · 2.2. Synthesis of flowery MIL-47 layer
LinkerH2BDC0.125 gp002 · 2.2. Synthesis of flowery MIL-47 layer
Solventdeionized water60 mLp002 · 2.2. Synthesis of flowery MIL-47 layer
AcidHNO3/H2SO4v/v 3:1 mixturep002 · 2.2. Synthesis of flowery MIL-47 layer
OtherCNT wafer19 mm diameterp002 · 2.2. Synthesis of flowery MIL-47 layer
Complete recipeSource: Main

Route 5: Hydrothermal

p002 · 2.2. Synthesis of flowery MIL-47 layer

Metal precursorsVOSO4.xH2O, 0.122 g
Linker precursorsH2BDC, 0.125 g
Solvents60 mL deionized water; water and ethanol washes
Additivesnone beyond shared MIL-47/CNT precursor solution
Atmospheresealed hydrothermal autoclave; gas atmosphere not specified
Temperature160
Time48
Substrate orientationpowder collected from bottom of autoclave, not substrate-bound
Work-upcollected by centrifugation, washed with water and ethanol
Activationvacuum dried at 60 deg C overnight
Scalability contextBy-product powder from same autoclave synthesis; yield not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceVOSO4.xH2O0.122 gp002 · 2.2. Synthesis of flowery MIL-47 layer
LinkerH2BDC0.125 gp002 · 2.2. Synthesis of flowery MIL-47 layer
Solventdeionized water60 mLp002 · 2.2. Synthesis of flowery MIL-47 layer