Synthesis · Boron-doped cobalt-iron bimetal phosphides nanosheets for enhanced oxygen evolution

8 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

2 · 2.3. Synthesis of Co-Fe-B and Co-B

Metal precursors120 mg pristine Co-MOF

Linker precursorsMOF precursor from 2-methylimidazole

Solvents40 mL C2H5OH; 40 mL deionized water

Additives0.75 mmol K2B4O7.4H2O, 2.5 mmol urea, 1 mmol NH4F

Atmospherenot specified

Temperature80

Time6

Oxidant / reductantK2B4O7.4H2O as boron source

Work-upcooled naturally; centrifuged, washed with ethanol three times, dried by lyophilisation

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pristine Co-MOF	120 mg	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Solvent	C2H5OH	40 mL	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Solvent	deionized water	40 mL	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	K2B4O7.4H2O	0.75 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	urea	2.5 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	NH4F	1 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B

Complete recipeSource: Main

Route 2: Other

2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P

Metal precursorsresultant Co-B

Linker precursorsMOF-derived borate intermediate

Solventsnot specified

AdditivesNaH2PO2 placed upstream in tube furnace

Atmosphereargon

Temperature350

Time2

Oxidant / reductantNaH2PO2 as phosphorus source/reductive phosphidation reagent

Work-upannealed in tube furnace; no post-anneal washing specified

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	resultant Co-B	not specified	2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P
Reductant	NaH2PO2	not specified	2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P

Complete recipeSource: Main

Route 3: Other

2 · 2.2. Synthesis of Co-Fe bimetal MOFs

Metal precursorsCo(NO3)2.6H2O; no Fe(NO3)3.9H2O

Linker precursors2-methylimidazole

Solventsdeionized water

AdditivesKOH aqueous solution

Atmospherenot specified

Temperature70 deg C drying after room-temperature precipitation

Time3 h stirring; overnight drying

Work-upcentrifuged, washed with ethanol three times, dried at 70 deg C overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2-methyl imidazole	same method as Co-Fe MOF	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Base	KOH aqueous solution	same method as Co-Fe MOF · 1.0 M	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Metal Source	Co(NO3)2.6H2O	not separately specified for Co-only control	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Solvent	deionized water	same method as Co-Fe MOF	2 · 2.2. Synthesis of Co-Fe bimetal MOFs

Complete recipeSource: Main

Route 4: Other

2 · 2.5. Synthesis of Co-Fe-P and Co-P

Metal precursorsresultant Co-MOF

Linker precursors2-methylimidazole MOF precursor

Solventsnot specified

AdditivesNaH2PO2 placed upstream in tube furnace

Atmosphereargon

Temperature350

Time2

Oxidant / reductantNaH2PO2 as phosphorus source/reductive phosphidation reagent

Work-upannealed in tube furnace; no post-anneal washing specified

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	resultant Co-MOF	not specified	2 · 2.5. Synthesis of Co-Fe-P and Co-P
Reductant	NaH2PO2	not specified	2 · 2.5. Synthesis of Co-Fe-P and Co-P

Complete recipeSource: Main

Route 5: Hydrothermal

2 · 2.3. Synthesis of Co-Fe-B and Co-B

Metal precursors120 mg resultant Co-Fe bimetal MOF

Linker precursorsMOF precursor from 2-methylimidazole

Solvents40 mL C2H5OH for MOF dispersion; 40 mL deionized water for boronation reagents

Additives0.75 mmol K2B4O7.4H2O, 2.5 mmol urea, 1 mmol NH4F

Atmospherenot specified

Temperature80

Time6

Oxidant / reductantK2B4O7.4H2O as boron source

Work-upcooled naturally; precipitates collected by centrifuge, washed with ethanol three times, dried by lyophilisation

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	resultant Co-Fe bimetal MOFs	120 mg	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Solvent	C2H5OH	40 mL	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Solvent	deionized water	40 mL	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	K2B4O7.4H2O	0.75 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	urea	2.5 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B
Additive	NH4F	1 mmol	2 · 2.3. Synthesis of Co-Fe-B and Co-B

Complete recipeSource: Main

Route 6: Other

2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P

Metal precursorsresultant Co-Fe-B

Linker precursorsMOF-derived borate intermediate

Solventsnot specified

AdditivesNaH2PO2 placed upstream in tube furnace

Atmosphereargon

Temperature350

Time2

Oxidant / reductantNaH2PO2 as phosphorus source/reductive phosphidation reagent

Work-upannealed in tube furnace; no post-anneal washing specified

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	resultant Co-Fe-B	not specified	2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P
Reductant	NaH2PO2	not specified	2 · 2.4. Synthesis of Co-Fe-B-P and Co-B-P

Complete recipeSource: Main

Route 7: Other

2 · 2.2. Synthesis of Co-Fe bimetal MOFs

Metal precursorsCo(NO3)2.6H2O and Fe(NO3)3.9H2O, total 8 mmol, Co/Fe ratios 1:1, 1:2, or 2:1

Linker precursors2-methylimidazole, 0.168 mol

Solventsdeionized water; 50 mL for linker solution and 60 mL for metal solution

Additives50 mL 1.0 M KOH aqueous solution

Atmospherenot specified

Temperature70 deg C drying after room-temperature precipitation

Time3 h stirring; overnight drying

Work-upprecipitate collected by centrifuge, washed with ethanol three times, dried at 70 deg C overnight

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2-methyl imidazole	0.168 mol	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Base	KOH aqueous solution	50 mL · 1.0 M	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Metal Source	Co(NO3)2.6H2O	part of 8 mmol total Co+Fe nitrate	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Metal Source	Fe(NO3)3.9H2O	part of 8 mmol total Co+Fe nitrate	2 · 2.2. Synthesis of Co-Fe bimetal MOFs
Solvent	deionized water	110 mL total	2 · 2.2. Synthesis of Co-Fe bimetal MOFs

Complete recipeSource: Main

Route 8: Other

2 · 2.5. Synthesis of Co-Fe-P and Co-P

Metal precursorsresultant Co-Fe bimetal MOFs

Linker precursors2-methylimidazole MOF precursor

Solventsnot specified

AdditivesNaH2PO2 placed upstream in tube furnace

Atmosphereargon

Temperature350

Time2

Oxidant / reductantNaH2PO2 as phosphorus source/reductive phosphidation reagent

Work-upannealed in tube furnace; no post-anneal washing specified

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	resultant Co-Fe bimetal MOFs	not specified	2 · 2.5. Synthesis of Co-Fe-P and Co-P
Reductant	NaH2PO2	not specified	2 · 2.5. Synthesis of Co-Fe-P and Co-P