A kind of preparation method of iron phosphide loaded graphene foam composite material

Abstract

A method for preparing iron phosphide loaded graphene foam composite material, belonging to the field of functional nanomaterials. This method is through Fe(NO 3 ) 3 ·9H 2 O can controllably catalyze the structural evolution and carbonization of polyvinylpyrrolidone during the sintering process. Combined with the subsequent CVD phosphating process, the composite structure on the iron phosphide-loaded graphene foam is directly generated, and the iron phosphide-loaded graphene foam composite material is obtained. Iron phosphide nanoparticles have a nearly spherical shape, their size can be adjusted between 30 and 500nm, and they can be tightly combined with graphene foam and are reliable. The iron phosphide nanoparticles are evenly distributed and tightly combined with the graphene foam matrix. The composite material has uniform composition and structure, simple process, high repeatability, novel method and low cost, making it very suitable for large-scale promotion.

Description

technical field

[0001] The invention belongs to the field of functional nanometer materials, and in particular relates to an iron phosphide-loaded graphene foam composite material and a preparation method thereof. Background technique

[0002] In recent years, transition metal phosphide materials have attracted great research interest due to their structural stability, good thermal conductivity, and excellent thermodynamic activity. Among them, nanomaterials represented by iron phosphide (FeP) and their composite materials have received extensive attention and research in the field of lithium-ion battery materials and electrocatalysis due to their good electrocatalytic activity and high reversible lithium storage capacity. . However, during the service process, FeP nanomaterials face problems such as particle agglomeration and particle damage due to volume expansion stress caused by intercalation / delithiation. In addition, FeP material itself has poor conductivity, which al...

Examples

Embodiment 1

[0026] Weigh 1.2g Fe(NO 3 ) 3 9H 2 O and 0.8g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 40ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 50°C for 12h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~100 mesh in a mortar, weigh 1.0g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use an argon atmosphere, and heat it at 3°C / min Heating rate of heating to 500°C, holding for 1h, then slowly cooling to 230°C, holding for 1h in the air atmosphere, then cooling to room temperature, collecting precursor A, and then weighing 0.5g of precursor A into CVD small At one end of the tube furnace quartz furnace tube near the gas outlet, put 10g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 80 sccm, raise the temperature to 360°C at 2°C / min, keep it warm for 6h, and then slowly cool to room temperatu...

Embodiment 2

[0028] Weigh 1.0g Fe(NO 3 ) 3 9H 2 O and 1.6g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 35ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 45°C for 24h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~50 mesh with a mortar, weigh 1.6g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use a nitrogen atmosphere, and set the temperature at 4°C / min. Heating rate to 490°C, keep warm for 50min, then slowly cool to 260°C, keep warm in air atmosphere for 1h, then cool to room temperature, collect precursor A, then weigh 0.5g of precursor A into CVD small tube One end of the furnace quartz furnace tube near the gas outlet, put 10g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 80 sccm, raise the temperature to 360°C at 2°C / min, keep it warm for 10h, and then slowly cool to room temperature to obta...

Embodiment 3

[0030] Weigh 1.2g Fe(NO 3 ) 3 9H 2O and 0.4g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 35ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 45°C for 16h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~200 mesh with a mortar, weigh 2.0g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use an argon atmosphere, and heat it at 4°C / min Heating rate of heating to 480°C, holding for 1 hour, then slowly cooling to 200°C, holding for 0.5 hours in the air atmosphere, then cooling to room temperature, collecting precursor A, and then weighing 0.5g of precursor A into CVD small At the end of the tube furnace quartz furnace tube near the gas outlet, put 6g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 100 sccm, raise the temperature to 400 °C at 1 °C / min, keep it for 6 hours, and then slowly cool to ...

technical field

[0001] The invention belongs to the field of functional nanometer materials, and in particular relates to an iron phosphide-loaded graphene foam composite material and a preparation method thereof. Background technique

[0002] In recent years, transition metal phosphide materials have attracted great research interest due to their structural stability, good thermal conductivity, and excellent thermodynamic activity. Among them, nanomaterials represented by iron phosphide (FeP) and their composite materials have received extensive attention and research in the field of lithium-ion battery materials and electrocatalysis due to their good electrocatalytic activity and high reversible lithium storage capacity. . However, during the service process, FeP nanomaterials face problems such as particle agglomeration and particle damage due to volume expansion stress caused by intercalation / delithiation. In addition, FeP material itself has poor conductivity, which al...

Examples

Embodiment 1

[0026] Weigh 1.2g Fe(NO 3 ) 3 9H 2 O and 0.8g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 40ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 50°C for 12h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~100 mesh in a mortar, weigh 1.0g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use an argon atmosphere, and heat it at 3°C / min Heating rate of heating to 500°C, holding for 1h, then slowly cooling to 230°C, holding for 1h in the air atmosphere, then cooling to room temperature, collecting precursor A, and then weighing 0.5g of precursor A into CVD small At one end of the tube furnace quartz furnace tube near the gas outlet, put 10g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 80 sccm, raise the temperature to 360°C at 2°C / min, keep it warm for 6h, and then slowly cool to room temperatu...

Embodiment 2

[0028] Weigh 1.0g Fe(NO 3 ) 3 9H 2 O and 1.6g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 35ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 45°C for 24h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~50 mesh with a mortar, weigh 1.6g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use a nitrogen atmosphere, and set the temperature at 4°C / min. Heating rate to 490°C, keep warm for 50min, then slowly cool to 260°C, keep warm in air atmosphere for 1h, then cool to room temperature, collect precursor A, then weigh 0.5g of precursor A into CVD small tube One end of the furnace quartz furnace tube near the gas outlet, put 10g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 80 sccm, raise the temperature to 360°C at 2°C / min, keep it warm for 10h, and then slowly cool to room temperature to obta...

Embodiment 3

[0030] Weigh 1.2g Fe(NO 3 ) 3 9H 2O and 0.4g polyvinylpyrrolidone (PVP, K30) are completely dissolved in 35ml deionized water to make a transparent colloidal liquid, then put into an oven, and dry at 45°C for 16h to obtain an orange-yellow flaky block; Grind the flaky block into a powder with a particle size of ~200 mesh with a mortar, weigh 2.0g and put it into a 30ml burning boat with a cover, put it into a tube furnace, use an argon atmosphere, and heat it at 4°C / min Heating rate of heating to 480°C, holding for 1 hour, then slowly cooling to 200°C, holding for 0.5 hours in the air atmosphere, then cooling to room temperature, collecting precursor A, and then weighing 0.5g of precursor A into CVD small At the end of the tube furnace quartz furnace tube near the gas outlet, put 6g Na 2 h 2 PO 2 Place it at the end close to the gas inlet, adjust the argon gas flow rate to 100 sccm, raise the temperature to 400 °C at 1 °C / min, keep it for 6 hours, and then slowly cool to ...

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