Synthesis · Si nanoparticles confined within a conductive 2D porous Cu-based metal–organic framework (Cu3(HITP)2) as potential anodes for high-capacity Li-ion batteries

6 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites

Metal precursorsCuSO4.5H2O in water

Linker precursorsHATP.6HCl (2,3,6,7,10,11-hexaaminotriphynylene as printed)

Solventswater

Additivesaqueous ammoniacal solution (28% NH3(aq), NH4OH)

Atmosphereambient air implied

Temperature~27

Time2

Work-upcollected precipitate; DI water rinse and redispersion cycles; acetone wash; dry 12 h at 50 deg C

Activationdrying at 50 deg C for 12 h

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuSO4.5H2O	99.5%	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites
Linker	HATP.6HCl (2,3,6,7,10,11-hexaaminotriphynylene)	Not specified	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites
Base	NH4OH / aqueous ammoniacal solution	28% NH3(aq)	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites
Solvent	water	Not specified	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites

Complete recipeSource: Main

Route 2: Drop Cast

3 · 2.3. Electrochemical characterizations

Solventswater

Additivescarbon Super P; LiPAA binder

Atmosphereargon-filled glove box for cell fabrication; electrode drying in air then vacuum

Temperature30; 85

Time2; overnight

Substrate orientationCu foil current collector

Work-upslurry cast on Cu foil, dried 30 deg C for 2 h, dried overnight at 85 deg C under vacuum, cut into 14 mm disks

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Si or Si@Cu3(HITP)2 composite	70 wt%	3 · 2.3. Electrochemical characterizations
Additive	carbon super-P	20 wt%	3 · 2.3. Electrochemical characterizations
Additive	lithium polyacrylate (LiPAA)	10 wt% · aqueous binder	3 · 2.3. Electrochemical characterizations
Solvent	water	Not specified	3 · 2.3. Electrochemical characterizations

Partial recipeSource: Main

Route 3: Other

13 · Results and discussion · Fig. 9

Additives1 M LiPF6 in EC/DMC (1:1 vol%) with 5 wt% fluoroethylene carbonate for half-cell; full-cell electrolyte not separately specified

Atmosphereargon-filled glove box for coin-cell fabrication

Temperature25

Oxidant / reductantpre-lithiation of Si@Cu3(HITP)2-5 anode for 1 cycle at 0.1C

Work-uppre-lithiated anode assembled with commercial LCO cathode; capacity ratio set to 0.9

Activationone-cycle pre-lithiation at 0.1C to stabilise SEI

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Si@Cu3(HITP)2-5 anode	pre-lithiated 1 cycle at 0.1C	13 · Results and discussion · Fig. 9
Other	commercial LiCoO2 cathode	capacity ratio anode:cathode = 0.9	13 · Results and discussion · Fig. 9

Partial recipeSource: Main

Route 4: Drop Cast

3 · 2.3. Electrochemical characterizations

SolventsNMP

Additivescarbon Super P; PVDF binder

Work-upcasting method slurry for full-cell cathode

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	commercial LCO	80%	3 · 2.3. Electrochemical characterizations
Additive	carbon super-P	10 wt%	3 · 2.3. Electrochemical characterizations
Additive	PVDF binder	10 wt%	3 · 2.3. Electrochemical characterizations
Solvent	NMP	Not specified	3 · 2.3. Electrochemical characterizations

Partial recipeSource: Both

Route 5: Other

3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1

Metal precursorsCuSO4.5H2O in water

Linker precursorsHATP.6HCl (2,3,6,7,10,11-hexaaminotriphynylene as printed)

Solventsdeionised water; acetone wash

AdditivesNH4OH, 28% NH3

Atmosphereair / ambient; alkaline environment

Temperature27

Time2 h reaction plus 12 h redispersion and 12 h drying

Work-upprecipitates collected, rinsed with DI water, redispersed in DI water for 12 h; repeated twice; acetone wash; dried 12 h at 50 deg C

Activationdried at 50 deg C for 12 h; no further heat treatment

Scalability contextConclusion states direct assembly is straightforward, efficient, and mass scalable, but no scale-up experiment is reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SiNP powder	90 mg	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1
Metal Source	CuSO4.5H2O	99.5%	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1
Linker	HATP.6HCl (2,3,6,7,10,11-hexaaminotriphynylene)	Not specified	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1
Base	aqueous ammoniacal solution / NH4OH	28% NH3(aq)	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1
Solvent	deionised water	Not specified	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1
Solvent	acetone	30 mL · 99.9%, Sigma-Aldrich	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites · Scheme 1

Partial recipeSource: Main

Route 6: Other

3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites

Metal precursorsMg powder (99.5%, 235 mesh)

AdditivesNaCl (>99%)

Atmosphereambient air implied; detailed MRR conditions not repeated

Oxidant / reductantMg reductant

Work-upnot detailed in this paper; previously reported method cited

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	SiO2	99%, 10-20 nm	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites
Reductant	Mg	99.5%, 235 mesh size	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites
Additive	NaCl	>99%	3 · 2.1. Synthesis of Si@Cu3(HITP)2 composites