Nanostructured cation-disordered Li4Mn2O5 rock-salts were synthesized by a two-step route using mechanochemical activation. First, high-temperature LiMnO2 was synthesized by a solid-state reaction using a reagent mixture of LiOH (≥98%), MnO2 (99%) and MnO (99%) with the molar ratio of 2:1:1, and was heat-treated at 1000°C under an argon flow for 8 h. Then, the mechanochemical synthesis between LiMnO2 and Li2O in a 2:1 ratio was carried out using Fritsch Planetary Micro Mill PULVERISETTE 7 premium at 700 rpm for 20 h to produce nanostructured Li4Mn2O5.
Pulverisette 7 premium
Manufactured by Fritsch
Sourced in Germany
The Pulverisette 7 premium is a laboratory equipment designed for fine and ultra-fine grinding of solid samples. It utilizes a planetary ball mill mechanism to efficiently reduce the particle size of various materials.
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6 protocols using pulverisette 7 premium
1
Nanostructured Li4Mn2O5 Rock-Salt Synthesis
2
Ni-TiC Composite Powder Synthesis
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The Ni-TiC composite powder was prepared from an elemental mixture of Ni metal powder (particle size~ 3–7 µm, purity > 99.9%, Alfa Aeser, Haverhill, MA, USA) and TiC metal powder (particle size~ 7–10 µm, purity > 99%, Alfa Aeser) powders alloyed via high energy ball mill (Pulverisette 7 Premium, Fritsch, Germany). The mechanical alloying has been carried out for 24 h in a tungsten carbide 80 mL grinding bowl and 3 mm size balls with a ball to powder weight ratio (BPR) of 10:1 and 300 rpm. The milling operation carried in two steps involves 20 min of milling and 10mins of the cooling interval to avoid overheating the sample. Steric acid (2 wt.%) was used as a process control agent (PCA) during mechanical alloying to prevent excessive cold welding due to high energy generated during the alloying process. The TiC content inside composites has been systematically increased from 5 to 50 wt.% to investigate its effect on these composites’ microstructure and mechanical properties.
3
Synthesis of Co0.5 Catalyst Precursor
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The catalyst precursor of Co0.5 was prepared from a Zn(II) zeolitic imidazolate framework (Basolite Z1200 from BASF, labeled ZIF-8), Co(II) acetate and 1,10-phenanthroline. Weighed amounts of the powders of Co(II)Ac (15.97 mg), phen (200 mg) and ZIF-8 (800 mg) were ball-milled (Pulverisette 7 premium, Fritsch) at 400 rpm for 2 h (4 × 30 min with 5 min rest in-between) in a ZrO2 crucible (45 cm3) filled with 100 ZrO2 balls (5 mm diameter). A split-hinge oven was equilibrated at 1,050 °C under Ar flow, and the catalyst precursor was quickly introduced and pyrolyzed at 1,050 °C in Ar for 1 h (see details in ref. 22 (link)). The N–C material was prepared similarly but without cobalt. Due to a mass loss of 65–70 wt% during pyrolysis in Ar (unmodified by the presence of Co or Fe at 0.5 wt%) caused by volatile products formed from ZIF-8 and phen while Co does not form volatile compounds, the cobalt content in Co0.5 is 1.5 wt%.
4
Mechanochemical Synthesis of Fe3Co3Ni3S8
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The Fe3Co3Ni3S8 electrocatalyst was synthesized according to a method recently published by our group.24 (link) The mechanochemical synthesis was realized using a Fritsch Pulverisette 7 premium line with ZrO2 milling containers (V = 20 mL) and ZrO2 milling balls (d = 2 mm and m = 24 g). A reaction mixture (m = 1 g) composed of stoichiometric amounts of Fe, Co, Ni, and S was prepared inside a glovebox to ensure an inert argon atmosphere inside the milling containers. The mechanochemical reaction was performed at a constant rotation speed of 1100 rpm for 45 min.
5
Mechanochemical Synthesis of Fe3Co3Ni3S8
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The Fe3Co3Ni3S8 electrocatalyst was synthesized according to a method recently published by our group.24 (link) The mechanochemical synthesis was realized using a Fritsch Pulverisette 7 premium line with ZrO2 milling containers (V = 20 mL) and ZrO2 milling balls (d = 2 mm and m = 24 g). A reaction mixture (m = 1 g) composed of stoichiometric amounts of Fe, Co, Ni, and S was prepared inside a glovebox to ensure an inert argon atmosphere inside the milling containers. The mechanochemical reaction was performed at a constant rotation speed of 1100 rpm for 45 min.
6
Synthesis of Polycrystalline GeSe-Te Alloys
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Polycrystalline samples of GeSe x Te 1Àx were synthesized from the elements Ge (MaTeck, 99.999%), Se (MaTeck, 99.999%) and Te (Alfa Aesar, 99.999%) in stoichiometric ratios. For each composition with x = 0, 0.2, 0.75, 1, a total mass of 200 mg was vacuum-sealed in quartz ampoules, heated to 900 C within 1-2 h, held at this temperature for 10 h, cooled to 300 C over 30 h and kept at this temperature for 24 h, followed by quenching in air. For the polycrystalline sample of GeSe 0.5 Te 0.5 , the elements were alloyed in a Fritsch 'Pulverisette 7 premium' planetary ball mill (in total: 3 g sample mass; milling time: 40 h with 5 min cycles and 3 min pauses at 600 rpm under an argon atmosphere; grinding bowl: 20 ml, ZrO 2 grinding balls: 10 Â 1 cm). Afterwards, the sample was pressed to a 150 mg pellet and heated to 500 C in a glass ampoule under an argon atmosphere for 1 h, kept at 500 C for 1 h, followed by cooling to room temperature over 20 h. The phase purity of all samples was confirmed by X-ray powder diffraction.
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