Synthesis evidence

Electrochemical properties of uniquely structured Fe2O3 and FeSe2/graphitic-carbon microrods synthesized by applying a metal-organic framework

Park S.-K., Kim J.K., Kang Y.C. · Chemical Engineering Journal · 2018 · 2440-2449

7 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p002 / journal p2441 · Experimental

Metal precursorsreduced MIL-88 microrods / Fe@GC
Atmosphereair
Temperature350
Time3
Oxidant / reductantair oxidation
Activationheating rate 2 deg C min-1
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherreduced MIL-88 microrodsNot specifiedp002 / journal p2441 · Experimental
OxidantairNot specifiedp002 / journal p2441 · Experimental
Partial recipeSource: Both

Route 2: Other

p002 / journal p2441 · Experimental

Metal precursorsas-prepared MIL-88 microrods
Linker precursorscarbon derived from MIL-88 ligands during direct selenization
Additivesselenium source not specified in main text
Atmosphere10% H2/Ar
Temperature250
Time10
Oxidant / reductantselenization under H2/Ar
Activationheating rate 2 deg C min-1
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared MIL-88 microrodsNot specifiedp002 / journal p2441 · Experimental
Reductant10% H2/Ar10% H2 in Arp002 / journal p2441 · Experimental
Otherselenium source not specifiedNot specifiedp002 / journal p2441 · Experimental
Complete recipeSource: Both

Route 3: Other

p002 / journal p2441 · Experimental

Metal precursorsMIL-88 microrods
Linker precursorsMIL-88 organic ligands carbonised in situ
Atmosphere5% H2/Ar
Temperature450
Time2
Oxidant / reductantH2/Ar reducing atmosphere
Activationheating rate 2 deg C min-1 for all post-treatment steps
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared MIL-88 microrodsNot specifiedp002 / journal p2441 · Experimental
Reductant5% H2/Ar5% H2 in Arp002 / journal p2441 · Experimental
Partial recipeSource: Main

Route 4: Other

p008 / journal p2447 · Results & discussion · Fig. S13 referenced

Metal precursorsFe@GC microrods
Solventsdiluted HCl solution
Timeovernight
Oxidant / reductantacid etching to remove iron-containing phases
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherFe@GC microrodsNot specifiedp008 / journal p2447 · Results & discussion · Fig. S13 referenced
Aciddiluted HCl solutiondiluted; not specifiedp008 / journal p2447 · Results & discussion · Fig. S13 referenced
Complete recipeSource: Both

Route 5: Other

p002 / journal p2441 · Experimental

Metal precursorsFe@GC microrods from reduced MIL-88
Atmosphereair
Temperature300
Time3
Oxidant / reductantair oxidation
Activationheating rate 2 deg C min-1
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherreduced MIL-88 / Fe@GC microrodsNot specifiedp002 / journal p2441 · Experimental
OxidantairNot specifiedp002 / journal p2441 · Experimental
Partial recipeSource: Both

Route 6: Other

p002 / journal p2441 · Experimental

Metal precursorsreduced MIL-88 microrods / Fe@GC
Linker precursorsgraphitic carbon framework from MIL-88 ligands
Additivesselenium source not specified in main text
Atmosphere10% H2/Ar
Temperature250
Time10
Oxidant / reductantselenization under H2/Ar; mechanism mentions H2Se gas
Activationheating rate 2 deg C min-1
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherreduced MIL-88 microrodsNot specifiedp002 / journal p2441 · Experimental
Reductant10% H2/Ar10% H2 in Arp002 / journal p2441 · Experimental
Otherselenium source / H2Se gas implied but not specifiedNot specifiedp002 / journal p2441 · Experimental
Complete recipeSource: Main

Route 7: Solvothermal

p002 / journal p2441 · Experimental

Metal precursorsiron(III) nitrate nonahydrate (98.5%, Samchun), 160 mg
Linker precursorsfumaric acid (99%, Sigma-Aldrich), 42 mg
SolventsN,N-dimethylformamide (99.0%, Samchun), 8 mL
Atmospherenot specified; vial in electric oven
Temperature110
Time0.5
Work-upnaturally cooled to room temperature; isolated by centrifugal washing with ethanol three times
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceiron(III) nitrate nonahydrate (98.5%, Samchun)160 mgp002 / journal p2441 · Experimental
Linkerfumaric acid (99%, Sigma-Aldrich)42 mgp002 / journal p2441 · Experimental
SolventN,N-dimethylformamide (99.0%, Samchun)8 mLp002 / journal p2441 · Experimental
Solventethanolthree centrifugal washing cyclesp002 / journal p2441 · Experimental