Synthesis evidence

Highly Conductive Bimetallic Ni-Fe Metal Organic Framework as a Novel Electrocatalyst for Water Oxidation

Zheng F., Xiang D., Li P. et al. · ACS Sustainable Chemistry and Engineering · 2019 · 9743-9749

8 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs

Metal precursorsFeSO4.7H2O; Ni:Fe = 0:1
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upMethanol washing and centrifugation several times; soak in methanol 3 days with daily solvent refresh; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeSO4.7H2O0.867 mmol total metal source; Ni:Fe = 0:1p003 / S3 · Synthesis of FeNi-MOFs
LinkerH4DOBDC0.243 mmol; 0.0482 gp003 / S3 · Synthesis of FeNi-MOFs
Complete recipeSource: Both

Route 2: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs · Table S1

Metal precursorsNiCl2.6H2O and FeSO4.7H2O; Table S1 nominal Fe:Ni = 1:9 (SI synthesis lists Ni:Fe = 9:1)
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upMethanol washing and centrifugation several times; soak in methanol 3 days with daily solvent refresh; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)part of 0.867 mmol total metal source; Fe:Ni = 1:9p003 / S3 · Synthesis of FeNi-MOFs · Table S1
Metal SourceFeSO4.7H2Opart of 0.867 mmol total metal source; Fe:Ni = 1:9p003 / S3 · Synthesis of FeNi-MOFs · Table S1
LinkerH4DOBDC0.243 mmol; 0.0482 gp003 / S3 · Synthesis of FeNi-MOFs · Table S1
Complete recipeSource: Both

Route 3: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs · Table S1

Metal precursorsNiCl2.6H2O and FeSO4.7H2O; Table S1 nominal Fe:Ni = 1:5
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upMethanol washing and centrifugation several times; soak in methanol 3 days with daily solvent refresh; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)part of 0.867 mmol total metal source; Fe:Ni = 1:5p003 / S3 · Synthesis of FeNi-MOFs · Table S1
Metal SourceFeSO4.7H2Opart of 0.867 mmol total metal source; Fe:Ni = 1:5p003 / S3 · Synthesis of FeNi-MOFs · Table S1
LinkerH4DOBDC0.243 mmol; 0.0482 gp003 / S3 · Synthesis of FeNi-MOFs · Table S1
Complete recipeSource: Both

Route 4: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs · Table S1

Metal precursorsNiCl2.6H2O and FeSO4.7H2O; Table S1 nominal Fe:Ni = 1:3
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upMethanol washing and centrifugation several times; soak in methanol 3 days with daily solvent refresh; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)part of 0.867 mmol total metal source; Fe:Ni = 1:3p003 / S3 · Synthesis of FeNi-MOFs · Table S1
Metal SourceFeSO4.7H2Opart of 0.867 mmol total metal source; Fe:Ni = 1:3p003 / S3 · Synthesis of FeNi-MOFs · Table S1
LinkerH4DOBDC0.243 mmol; 0.0482 gp003 / S3 · Synthesis of FeNi-MOFs · Table S1
Complete recipeSource: Both

Route 5: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs · Table S1

Metal precursorsNiCl2.6H2O and FeSO4.7H2O; Table S1 nominal Fe:Ni = 1:1
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upMethanol washing and centrifugation several times; soak in methanol 3 days with daily solvent refresh; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)part of 0.867 mmol total metal source; Fe:Ni = 1:1p003 / S3 · Synthesis of FeNi-MOFs · Table S1
Metal SourceFeSO4.7H2Opart of 0.867 mmol total metal source; Fe:Ni = 1:1p003 / S3 · Synthesis of FeNi-MOFs · Table S1
LinkerH4DOBDC0.243 mmol; 0.0482 gp003 / S3 · Synthesis of FeNi-MOFs · Table S1
Complete recipeSource: SI

Route 6: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs

Metal precursorsFeCl2 and NiCl2.6H2O; Fe:Ni = 1:3
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upSame washing, methanol soaking, washing and vacuum drying procedure as the FeSO4-derived FeNi-MOFs.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl2Fe:Ni molar ratio 1:3p003 / S3 · Synthesis of FeNi-MOFs
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)Fe:Ni molar ratio 1:3p003 / S3 · Synthesis of FeNi-MOFs
Complete recipeSource: SI

Route 7: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs

Metal precursorsFeCl3 and NiCl2.6H2O; Fe:Ni = 1:3
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upSame washing, methanol soaking, washing and vacuum drying procedure as the FeSO4-derived FeNi-MOFs.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3Fe:Ni molar ratio 1:3p003 / S3 · Synthesis of FeNi-MOFs
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)Fe:Ni molar ratio 1:3p003 / S3 · Synthesis of FeNi-MOFs
Complete recipeSource: Both

Route 8: Solvothermal

p003 / S3 · Synthesis of FeNi-MOFs

Metal precursorsNiCl2.6H2O inferred; text/OCR renders this as NiCl6.6H2O; Ni:Fe = 1:0
Linker precursorsH4DOBDC
Solvents20 mL DMF/ethanol/water, v/v/v = 1:1:1
Temperature110
Time24
Work-upCool to room temperature; collect product by methanol washing and centrifugation several times; soak in methanol for 3 days with solvent refreshed daily; wash with methanol.
ActivationDried under vacuum at 80 C for 4 h.
Scalability context50 mL Teflon-lined autoclave; 20 mL solvent batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl6.6H2O (OCR; likely NiCl2.6H2O)0.867 mmol total metal source; Ni:Fe = 1:0p003 / S3 · Synthesis of FeNi-MOFs
LinkerH4DOBDC (2,5-dihydroxyterephthalic acid)0.243 mmol; 0.0482 g; 1 equivp003 / S3 · Synthesis of FeNi-MOFs
SolventDMF/ethanol/water20 mL · v/v/v = 1:1:1p003 / S3 · Synthesis of FeNi-MOFs