Synthesis · Metal-organic framework-mediated synthesis of LiNi0.5Mn1.5O4: Tuning the Mn3+ content and electrochemical performance by organic ligands

18 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.1 Materials preparation

Metal precursorsBCA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in BCA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	BCA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 2: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsBCA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	BCA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Partial recipeSource: Main

Route 3: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursors3,3,4,4-biphenyltetracarboxylic acid (BCA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	3,3,4,4-biphenyltetracarboxylic acid (BCA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 4: Other

2 · 2.1 Materials preparation

Metal precursorsDTA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in DTA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	DTA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 5: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsDTA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	DTA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Partial recipeSource: Main

Route 6: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursors2,5-dihydroxyterephthalic acid (DTA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	2,5-dihydroxyterephthalic acid (DTA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 7: Other

2 · 2.1 Materials preparation

Metal precursorsOBA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in OBA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	OBA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 8: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsOBA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	OBA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Partial recipeSource: Main

Route 9: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursors4,4-oxybisbenzoic acid (OBA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	4,4-oxybisbenzoic acid (OBA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 10: Other

2 · 2.1 Materials preparation

Metal precursorsPTA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in PTA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PTA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 11: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsPTA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PTA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Complete recipeSource: Main

Route 12: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursorsp-phthalic acid / terephthalic acid (PTA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	p-phthalic acid / terephthalic acid (PTA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 13: Other

2 · 2.1 Materials preparation

Metal precursorsPTCDA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in PTCDA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PTCDA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 14: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsPTCDA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	PTCDA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Partial recipeSource: Main

Route 15: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursors3,4,9,10-perylenetetracarboxylic acid (PTCDA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	3,4,9,10-perylenetetracarboxylic acid (PTCDA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 16: Other

2 · 2.1 Materials preparation

Metal precursorsTCA-Ni-Mn-MOF precursor; CH3COOLi stoichiometric with 10% excess lithium

Linker precursorsOrganic ligand incorporated in TCA-Ni-Mn-MOF precursor; decomposed during calcination

Solventsethanol for dispersion before evaporation

AdditivesCH3COOLi, 10% excess to compensate lithium loss

Atmosphereair atmosphere during 800 C calcination

Temperature50 evaporation; 400 prefiring; 800 calcination

Time5 h prefiring at 400 C; 8 h calcination at 800 C

Work-upDisperse dried MOFs and CH3COOLi in ethanol under magnetic stirring; evaporate ethanol slowly at 50 C; grind mixture; cool spontaneously to room temperature after calcination.

ActivationHigh-temperature calcination at 800 C for 8 h in air.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	TCA-Ni-Mn-MOFs	dried MOFs; amount not specified	2 · 2.1 Materials preparation
Other	CH3COOLi	stoichiometric with 10% excess	2 · 2.1 Materials preparation
Solvent	ethanol	not specified	2 · 2.1 Materials preparation

Complete recipeSource: Main

Route 17: Drop Cast

2 · 2.3 Electrochemical cycling measurement

Metal precursorsTCA-LNMO powder

SolventsN-methyl-2-pyrrolidone (NMP)

Additivespolyvinylidene fluoride binder; acetylene black conductive additive

Atmospherecoin-cell assembly in argon-filled glove box (H2O <= 0.1 ppm, O2 <= 0.1 ppm)

Temperature80 drying; 100 drying after post-cycling DMC wash for ex situ analyses

Substrate orientationaluminum foil current collector; rolled into 14 mm disks

Work-upSlurry coated onto aluminum foil, dried at 80 C, rolled into disks; CR2032 cells used Li metal counter electrode, Celgard 2400 separator, 1 M LiODFB in EC:DMC:EMC (1:1:1).

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	TCA-LNMO powder	80 wt% in cathode coating	2 · 2.3 Electrochemical cycling measurement
Additive	polyvinylidene fluoride	15 wt%	2 · 2.3 Electrochemical cycling measurement
Additive	acetylene black	5 wt%	2 · 2.3 Electrochemical cycling measurement
Solvent	N-methyl-2-pyrrolidone (NMP)	not specified	2 · 2.3 Electrochemical cycling measurement
Electrolyte	LiODFB in EC:DMC:EMC	1 M; EC:DMC:EMC 1:1:1 by volume · 1 M	2 · 2.3 Electrochemical cycling measurement

Partial recipeSource: Main

Route 18: Hydrothermal

2 · 2.1 Materials preparation

Metal precursorsNi(CH3COO)2.4H2O (15 mmol); Mn(CH3COO)2.4H2O (45 mmol)

Linker precursorstrimeric acid (TCA)

Solvents200 mL ethanol/water solution (Ve:Vw = 1:1); 100 mL aqueous NaOH linker solution

AdditivesNaOH, 1.32 M; nNaOH/nPMA = 4.5:1 for PTA solution

Atmospherenot specified

Temperature120

Time15 hydrothermal; 5 h room-temperature agitation before autoclave; 12 h drying at 120 C

Work-upCool naturally to room temperature; filter; wash with distilled water and absolute ethanol several times.

ActivationDry in oven at 120 C for 12 h.

Scalability contextTwo 200 mL Teflon-lined stainless-steel autoclaves were used for the typical preparation.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(CH3COO)2.4H2O	15 mmol	2 · 2.1 Materials preparation
Metal Source	Mn(CH3COO)2.4H2O	45 mmol	2 · 2.1 Materials preparation
Linker	trimeric acid (TCA)	60 mmol; for PTA text says 60 mmol PMA dissolved in 100 mL 1.32 M NaOH; other ligands implied by substitution but individual amounts not restated	2 · 2.1 Materials preparation
Solvent	ethanol/water solution	200 mL · Ve:Vw = 1:1	2 · 2.1 Materials preparation
Base	NaOH aqueous solution	100 mL for PTA linker solution · 1.32 M; nNaOH/nPMA = 4.5:1	2 · 2.1 Materials preparation
Solvent	absolute ethanol	several washes	2 · 2.1 Materials preparation
Solvent	distilled water	several washes	2 · 2.1 Materials preparation