cMOF Evidence Base

Synthesis evidence

Micro-sized conductive metal–organic framework nanosheets for the electrochemical hydrogen evolution reaction in acidic media

Wang Y., Wang J., Zeng J. et al. · Journal of Materials Chemistry A · 2025 · 42273-42280

12 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Hydrothermal

p002 / 42274 · Results and discussion

Metal precursorscorresponding metal precursor not explicitly specified for this metal in the SI text
Linker precursorsHITP (protocol reports 0.17 mM)
Solventsdimethyl sulfoxide; deionized water
Additivessodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcentrifugation; wash with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch by analogy with SI protocol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified for this metal; SI generic text names nickel acetateNot specifiedp002 / 42274 · Results and discussion
LinkerHITP0.17 mM in generic SI protocolp002 / 42274 · Results and discussion
Solventdimethyl sulfoxide18 mL in generic SI protocolp002 / 42274 · Results and discussion
Solventdeionized water18 mL in generic SI protocolp002 / 42274 · Results and discussion
Additivesodium acetate solution24 mL in generic SI protocol · 4 Mp002 / 42274 · Results and discussion
Complete recipeSource: SI

Route 2: Other

p002 · Materials synthesis

Metal precursorspreformed M-HITP nanoparticles
Linker precursorsHITP already incorporated in M-HITP nanoparticles
Solvents1 mL of 25 wt% aqueous tetramethylammonium hydroxide; later diluted with 50 mL deionized water
Additivestetramethylammonium hydroxide (TMAH)
Atmospherenot specified
Temperaturenot specified
Time20
Oxidant / reductantnone specified
Work-updiluted with 50 mL deionized water, dialyzed, centrifuged at 10,000 rpm; supernatant collected
Activationfreeze-dried
Scalability context25 mg nanoparticle precursor in 1 mL TMAH per batch; main text reports about 30 wt% nanosheet yield for Ni-HITP.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo-HITP nanoparticles25 mgp002 · Materials synthesis
Baseaqueous tetramethylammonium hydroxide (TMAH)1 mL · 25 wt%p002 · Materials synthesis
Solventdeionized water50 mL dilutionp002 · Materials synthesis
Partial recipeSource: Both

Route 3: Hydrothermal

p002 / 42274 · Results and discussion

Metal precursorscorresponding metal precursor not explicitly specified for this metal in the SI text
Linker precursorsHITP (protocol reports 0.17 mM)
Solventsdimethyl sulfoxide; deionized water
Additivessodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcentrifugation; wash with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch by analogy with SI protocol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified for this metal; SI generic text names nickel acetateNot specifiedp002 / 42274 · Results and discussion
LinkerHITP0.17 mM in generic SI protocolp002 / 42274 · Results and discussion
Solventdimethyl sulfoxide18 mL in generic SI protocolp002 / 42274 · Results and discussion
Solventdeionized water18 mL in generic SI protocolp002 / 42274 · Results and discussion
Additivesodium acetate solution24 mL in generic SI protocol · 4 Mp002 / 42274 · Results and discussion
Complete recipeSource: SI

Route 4: Other

p002 · Materials synthesis

Metal precursorspreformed M-HITP nanoparticles
Linker precursorsHITP already incorporated in M-HITP nanoparticles
Solvents1 mL of 25 wt% aqueous tetramethylammonium hydroxide; later diluted with 50 mL deionized water
Additivestetramethylammonium hydroxide (TMAH)
Atmospherenot specified
Temperaturenot specified
Time20
Oxidant / reductantnone specified
Work-updiluted with 50 mL deionized water, dialyzed, centrifuged at 10,000 rpm; supernatant collected
Activationfreeze-dried
Scalability context25 mg nanoparticle precursor in 1 mL TMAH per batch; main text reports about 30 wt% nanosheet yield for Ni-HITP.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCoNi-HITP nanoparticles25 mgp002 · Materials synthesis
Baseaqueous tetramethylammonium hydroxide (TMAH)1 mL · 25 wt%p002 · Materials synthesis
Solventdeionized water50 mL dilutionp002 · Materials synthesis
Partial recipeSource: Both

Route 5: Hydrothermal

p002 / 42274 · Results and discussion

Metal precursorscorresponding metal precursor not explicitly specified for this metal in the SI text
Linker precursorsHITP (protocol reports 0.17 mM)
Solventsdimethyl sulfoxide; deionized water
Additivessodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcentrifugation; wash with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch by analogy with SI protocol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified for this metal; SI generic text names nickel acetateNot specifiedp002 / 42274 · Results and discussion
LinkerHITP0.17 mM in generic SI protocolp002 / 42274 · Results and discussion
Solventdimethyl sulfoxide18 mL in generic SI protocolp002 / 42274 · Results and discussion
Solventdeionized water18 mL in generic SI protocolp002 / 42274 · Results and discussion
Additivesodium acetate solution24 mL in generic SI protocol · 4 Mp002 / 42274 · Results and discussion
Partial recipeSource: Both

Route 6: Hydrothermal

p002 / 42274 · Results and discussion

Metal precursorscorresponding metal precursor not explicitly specified for this metal in the SI text
Linker precursorsHITP (protocol reports 0.17 mM)
Solventsdimethyl sulfoxide; deionized water
Additivessodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcentrifugation; wash with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch by analogy with SI protocol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified for this metal; SI generic text names nickel acetateNot specifiedp002 / 42274 · Results and discussion
LinkerHITP0.17 mM in generic SI protocolp002 / 42274 · Results and discussion
Solventdimethyl sulfoxide18 mL in generic SI protocolp002 / 42274 · Results and discussion
Solventdeionized water18 mL in generic SI protocolp002 / 42274 · Results and discussion
Additivesodium acetate solution24 mL in generic SI protocol · 4 Mp002 / 42274 · Results and discussion
Partial recipeSource: Both

Route 7: Other

p007 · Figure caption · Fig. S7

Metal precursorspreformed Ni-HITP nanoparticles
Linker precursorsHITP already incorporated in Ni-HITP
Solventsaqueous NaOH solution
AdditivesNaOH (pH 13)
Atmospherenot specified
Temperaturenot specified
Timeup to 2 h in SI figure
Oxidant / reductantnone specified
Work-upnot specified
Activationnot specified
Scalability contextControl did not stabilise sheet-like reconstruction.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
BaseNaOH aqueous solutionpH=13p007 · Figure caption · Fig. S7
OtherNi-HITPNot specifiedp007 · Figure caption · Fig. S7
Complete recipeSource: SI

Route 8: Hydrothermal

p002 · Materials synthesis

Metal precursorsNickel acetate (0.17 mM as reported)
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene (HITP; 0.17 mM as reported)
Solvents18 mL dimethyl sulfoxide; 18 mL deionized water
Additives24 mL sodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcool to room temperature; collect solid by centrifugation; wash thoroughly with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel acetate0.17 mMp002 · Materials synthesis
Linker2,3,6,7,10,11-hexaaminotriphenylene (HITP)0.17 mMp002 · Materials synthesis
Solventdimethyl sulfoxide18 mLp002 · Materials synthesis
Solventdeionized water18 mLp002 · Materials synthesis
Additivesodium acetate solution24 mL · 4 Mp002 · Materials synthesis
Partial recipeSource: Both

Route 9: Other

p003 / 42275 · Results and discussion · Fig. S10

Metal precursorspreformed Ni-HITP nanoparticles
Linker precursorsHITP already incorporated in Ni-HITP nanoparticles
Solventsaqueous TMAH diluted to 12.5, 6.25, 3.125, or 1.56 wt%
AdditivesTMAH
Atmospherenot specified
Temperaturenot specified
Time20 implied from nanosheet synthesis
Oxidant / reductantnone specified
Work-upnot separately detailed; compared by yield, XRD and SEM
Activationnot specified
Scalability contextDilution reduces nanosheet yield from about 30 wt% to 15.2 wt% at 1.56 wt% TMAH.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-HITP nanoparticlesnot separately stated for dilution seriesp003 / 42275 · Results and discussion · Fig. S10
Baseaqueous TMAH25 wt%, 12.5 wt%, 6.25 wt%, 3.125 wt%, 1.56 wt%p003 / 42275 · Results and discussion · Fig. S10
Complete recipeSource: SI

Route 10: Other

p002 · Materials synthesis

Metal precursorspreformed M-HITP nanoparticles
Linker precursorsHITP already incorporated in M-HITP nanoparticles
Solvents1 mL of 25 wt% aqueous tetramethylammonium hydroxide; later diluted with 50 mL deionized water
Additivestetramethylammonium hydroxide (TMAH)
Atmospherenot specified
Temperaturenot specified
Time20
Oxidant / reductantnone specified
Work-updiluted with 50 mL deionized water, dialyzed, centrifuged at 10,000 rpm; supernatant collected
Activationfreeze-dried
Scalability context25 mg nanoparticle precursor in 1 mL TMAH per batch; main text reports about 30 wt% nanosheet yield for Ni-HITP.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-HITP nanoparticles25 mgp002 · Materials synthesis
Baseaqueous tetramethylammonium hydroxide (TMAH)1 mL · 25 wt%p002 · Materials synthesis
Solventdeionized water50 mL dilutionp002 · Materials synthesis
Partial recipeSource: Both

Route 11: Other

p003 / 42275 · Results and discussion · Fig. S13

Metal precursorspreformed Ni-HITP assemblies from 25 wt% TMAH sonication for 2 h
Linker precursorsHITP already incorporated in Ni-HITP
Solventsaqueous tetramethylammonium perchlorate solution
Additivestetramethylammonium perchlorate (TMClO4)
Atmospherenot specified
Temperaturenot specified
Time8-20 h
Oxidant / reductantnone specified
Work-upnot specified
Activationnot specified
Scalability contextCounter-anion control produced sheets/nanotubes/coralline morphologies and framework collapse.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-HITP assemblies pre-formed in TMAHNot specifiedp003 / 42275 · Results and discussion · Fig. S13
Additivetetramethylammonium perchlorate (TMClO4)Not specifiedp003 / 42275 · Results and discussion · Fig. S13
Partial recipeSource: Both

Route 12: Hydrothermal

p002 / 42274 · Results and discussion

Metal precursorscorresponding metal precursor not explicitly specified for this metal in the SI text
Linker precursorsHITP (protocol reports 0.17 mM)
Solventsdimethyl sulfoxide; deionized water
Additivessodium acetate solution (4 M)
Atmospherenot specified
Temperature100
Time16
Oxidant / reductantnone specified
Work-upcentrifugation; wash with deionized water and methanol
Activationdried under vacuum at 60 °C
Scalability context100 mL Teflon-lined autoclave batch by analogy with SI protocol.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified for this metal; SI generic text names nickel acetateNot specifiedp002 / 42274 · Results and discussion
LinkerHITP0.17 mM in generic SI protocolp002 / 42274 · Results and discussion
Solventdimethyl sulfoxide18 mL in generic SI protocolp002 / 42274 · Results and discussion
Solventdeionized water18 mL in generic SI protocolp002 / 42274 · Results and discussion
Additivesodium acetate solution24 mL in generic SI protocol · 4 Mp002 / 42274 · Results and discussion