cMOF Evidence Base

Synthesis evidence

A Microporous and Naturally Nanostructured Thermoelectric Metal-Organic Framework with Ultralow Thermal Conductivity

Sun L., Liao B., Sheberla D. et al. · Joule · 2017 · 168-177

2 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

p008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2

Metal precursorsNiCl2·6H2O, 95.7 mg
Linker precursorsHATP·6HCl, 141.9 mg
Solvents60 mL deionised water; workup with deionised water, ethanol, and acetone
Additives1.5 mL concentrated aqueous ammonia
AtmosphereContinuous air bubbling for 45 min, then inert atmosphere for 2 h; product stored in nitrogen-filled glovebox
Temperature65
Time0.75 h under air bubbling plus 2 h under inert atmosphere
Oxidant / reductantAir/oxygen exposure during initial bubbling; ammonia base added
Work-upCentrifugation, soaked in deionised water at room temperature, washed with water, ethanol, and acetone, dried under nitrogen stream for 12 h
ActivationFor porosity, sample heated to 80 C under evacuation for 26 h; for transport pellets, desolvated at 150 C under vacuum for 2 h
Scalability contextThe article notes abundant and nontoxic metal elements could improve scalability and safety in general; no scale-up experiment was reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2·6H2O95.7 mgp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
LinkerHATP·6HCl141.9 mgp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
Solventdeionized water60 mLp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
Baseconcentrated aqueous ammonia1.5 mL · concentratedp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
Solventethanolwash solventp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
Solventacetonewash solventp008 / article p.174 · Experimental Procedures - Characterization of the Powder of Ni3(HITP)2
Complete recipeSource: Both

Route 2: Other

p009 / article p.175 · Experimental Procedures - Characterization of Pressed Pellets of Ni3(HITP)2

Metal precursorsPre-synthesised Ni3(HITP)2 powder
AdditivesNo binder or conducting additive reported for pellet pressing; carbon paste/silver paste used only for measurement contacts
AtmosphereRoom-temperature pressing; transport measurements under vacuum after desolvation
Temperatureroom temperature pressing; 150 C desolvation before transport
Time0.25 h pressing; 2 h desolvation
Work-upPowder placed into 6 mm inner-diameter trapezoidal split sleeve pressing die and pressed with 3 tons applied mass for 15 min
ActivationHeated at 150 C for 2 h under vacuum for complete desolvation before electrical/thermoelectric measurements
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherNi3(HITP)2 powdernot reportedp009 / article p.175 · Experimental Procedures - Characterization of Pressed Pellets of Ni3(HITP)2