Preparation method of Co9S8/MoS2 multilevel structure composite material

Abstract

The invention relates to the technical field of nano-materials, in particular to a preparation method of a Co9S8 / MoS2 multilevel structure composite material. The preparation method includes: 1) dissolving an organic ligand in an aqueous solution containing molybdenum and cobalt to prepare a precursor solution, then carrying out oil bath heating reaction on the precursor solution, and then performing filtering to obtain a CoMo-MOF material; 2) dispersing the obtained CoMo-MOF material in an organic solvent to prepare a dispersion liquid, then carrying out hydrothermal reaction on the dispersion liquid, then performing filtering, and conducting cleaning and drying to obtain CoMo-S powder; and 3) placing the CoMo-S powder in a reducing atmosphere for high-temperature calcination to obtain the Co9S8 / MoS2 multilevel structure composite material. The preparation method provided by the invention is concise and efficient, has low equipment requirements, and is easy to realize industrial production; the preparation stability is high, the size and the morphology of the product can be effectively controlled in each step, and the structural stability and the size uniformity of the product aremaintained.

Description

technical field

[0001] The invention relates to the technical field of nanomaterials, in particular to a Co 9 S 8 / MoS 2 Preparation method of multi-level structure composite material. Background technique

[0002] Semiconducting transition metal dichalcogenides have broad application prospects in the fields of optical sensors, optoelectronic devices, magnetic devices, and catalysis. Among various transition metal sulfides, Co 9 S 8 It is an effective hydrodesulfurization catalyst with high catalytic activity for oxygen reduction reaction (ORR) in acidic solution, but due to its inherent low conductivity and easy aggregation, it cannot meet the requirements of metal-air batteries or fuel cells. actual needs. MoS 2 are compounds of the transition metal dichalide (TMDC) family, in which the transition metal cation (M 4+ ) plane sandwiched between chalcogenide anions (S 2- ) between the plane and a single monolayer Mx 2 held together by weak van der Waals interactions...

Examples

Embodiment 1

[0048] A kind of Co 9 S 8 / MoS 2 The preparation method of multi-level structure composite material,

[0049] The preparation method comprises the following preparation steps:

[0050] 1) Add 5gMoO 3 Add it to 250mL deionized water, add 4.75g 2-methylimidazole to ultrasonically dissolve to form A solution, then weigh 2.6g Co(NO 3 ) 2 ·6H 2 O was added into 250mL deionized water and ultrasonically dissolved to form liquid B, and liquid A and liquid B were mixed to prepare a precursor solution, and then the precursor solution was heated in an oil bath at 120°C for 12 hours, cooled to room temperature after the reaction, centrifuged and filtered. The CoMo-MOF material was obtained by washing three times, and dried under vacuum at 60°C for 12 hours;

[0051] 2) Dissolve 50mg of thioacetamide in 50mL of ethanol to prepare an organic solvent, weigh 8.25mg of CoMo-MOF material and disperse it in an organic solvent to prepare a dispersion liquid, and then conduct a hydrothermal...

Embodiment 2

[0068] Concrete steps are identical with embodiment 1, difference is: MoO 3 The dosage is 0.36g, Co(NO 3 ) 2 ·6H 2 The amount of O was 6.54 g, the amount of 2-methylimidazole was 2.05 g, the temperature of the oil bath was 80° C., and the duration of the oil bath was 18 h. to Co 9 S 8 / MoS 2 The multi-level structure composite powder was characterized by SEM, and the characterization results showed that it was a hollow rod-like structure with Co 9 S 8 and MoS 2 The nanosheets are vertically distributed on the surface of the nanorods.

Embodiment 3

[0070] Concrete steps are identical with embodiment 1, difference is: MoO 3 The dosage is 3.60g, Co(NO 3 ) 2 ·6H 2 The amount of O used was 65.49 g, the amount of 2-methylimidazole was 20.53 g, the temperature of the oil bath was 180° C., and the duration of the oil bath was 8 h. to Co 9 S 8 / MoS 2 The multi-level structure composite powder was characterized by SEM, and the characterization results showed that it was a hollow rod-like structure with Co 9 S 8 and MoS 2 The nanosheets are vertically distributed on the surface of the nanorods.

technical field

[0001] The invention relates to the technical field of nanomaterials, in particular to a Co 9 S 8 / MoS 2 Preparation method of multi-level structure composite material. Background technique

[0002] Semiconducting transition metal dichalcogenides have broad application prospects in the fields of optical sensors, optoelectronic devices, magnetic devices, and catalysis. Among various transition metal sulfides, Co 9 S 8 It is an effective hydrodesulfurization catalyst with high catalytic activity for oxygen reduction reaction (ORR) in acidic solution, but due to its inherent low conductivity and easy aggregation, it cannot meet the requirements of metal-air batteries or fuel cells. actual needs. MoS 2 are compounds of the transition metal dichalide (TMDC) family, in which the transition metal cation (M 4+ ) plane sandwiched between chalcogenide anions (S 2- ) between the plane and a single monolayer Mx 2 held together by weak van der Waals interactions...

Examples

Embodiment 1

[0048] A kind of Co 9 S 8 / MoS 2 The preparation method of multi-level structure composite material,

[0049] The preparation method comprises the following preparation steps:

[0050] 1) Add 5gMoO 3 Add it to 250mL deionized water, add 4.75g 2-methylimidazole to ultrasonically dissolve to form A solution, then weigh 2.6g Co(NO 3 ) 2 ·6H 2 O was added into 250mL deionized water and ultrasonically dissolved to form liquid B, and liquid A and liquid B were mixed to prepare a precursor solution, and then the precursor solution was heated in an oil bath at 120°C for 12 hours, cooled to room temperature after the reaction, centrifuged and filtered. The CoMo-MOF material was obtained by washing three times, and dried under vacuum at 60°C for 12 hours;

[0051] 2) Dissolve 50mg of thioacetamide in 50mL of ethanol to prepare an organic solvent, weigh 8.25mg of CoMo-MOF material and disperse it in an organic solvent to prepare a dispersion liquid, and then conduct a hydrothermal...

Embodiment 2

[0068] Concrete steps are identical with embodiment 1, difference is: MoO 3 The dosage is 0.36g, Co(NO 3 ) 2 ·6H 2 The amount of O was 6.54 g, the amount of 2-methylimidazole was 2.05 g, the temperature of the oil bath was 80° C., and the duration of the oil bath was 18 h. to Co 9 S 8 / MoS 2 The multi-level structure composite powder was characterized by SEM, and the characterization results showed that it was a hollow rod-like structure with Co 9 S 8 and MoS 2 The nanosheets are vertically distributed on the surface of the nanorods.

Embodiment 3

[0070] Concrete steps are identical with embodiment 1, difference is: MoO 3 The dosage is 3.60g, Co(NO 3 ) 2 ·6H 2 The amount of O used was 65.49 g, the amount of 2-methylimidazole was 20.53 g, the temperature of the oil bath was 180° C., and the duration of the oil bath was 8 h. to Co 9 S 8 / MoS 2 The multi-level structure composite powder was characterized by SEM, and the characterization results showed that it was a hollow rod-like structure with Co 9 S 8 and MoS 2 The nanosheets are vertically distributed on the surface of the nanorods.

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