Iron trioxide monocrystal nanotube/graphene composite electrode material and preparation method thereof

Abstract

The invention relates to an iron trioxide monocrystal nanotube / graphene composite electrode material and a preparation method thereof. The composite electrode material of the invention is formed by coating an iron trioxide monocrystal nanotube with graphene via Van der Waals' force, wherein the mass ratio of the graphene and ferric oxide is 1:(1 to 10); the iron trioxide monocrystal nanotube is an alpha-Fe2O3 monocrystal nanotube, and the length thereof is 300 to 500 nm, and the outer diameter is 60 to 90 nm while the inside diameter is 10 to 50 nm. The method designed by the invention is simple in synthetic process and low in cost, and can be applied to lithium ion battery cathode materials. The iron trioxide monocrystal nanotube / graphene composite electrode material has excellent stability and electrochemical performance.

Description

technical field

[0001] The invention relates to a ferric oxide single crystal nanotube / graphene composite electrode material and a preparation method thereof. technical background

[0002] Since Tarascon et al. reported the electrochemical performance and reaction mechanism of transition metal oxides as anode materials for lithium-ion batteries in 2000, researchers have controlled the structure and morphology of transition metal oxides to obtain high specific capacity, for The study of high-performance lithium-ion battery anode materials has opened up a very important new field. However, the rapid decline in capacity of lithium batteries using transition group metal oxides seriously hinders its further application. Significant changes can occur, and commonly used binders can easily swell in the electrolyte of a lithium battery, leading to cracking and fragmentation of the transition metal oxide electrode material. To overcome this problem, the researchers employed nanostru...

Examples

Embodiment 1

[0025] 1) Preparation of graphene

[0026] Under the conditions of cooling in an ice bath and stirring, add 69 mL of concentrated H 2 SO 4 Add 1.5 g NaNO to 3 (ground), to be NaNO 3 completely soluble in H 2 SO 4 After neutralization, 3.0 g of graphite was added into it while stirring. Then slowly add 9.0 g KMnO 4 , the addition rate was strictly controlled to ensure that the temperature was lower than 20 °C, then the ice bath was removed, and a water bath was used to keep the temperature at about 35 °C for 2 h. Slowly add 137 mL of deionized water under stirring, rapidly raise the temperature to 98 °C, and keep it in a 98 °C water bath for 15 minutes, then further dilute to 420 mL with 60 °C deionized water, and then add 11 mL of 30% hydrogen peroxide to reduce the remaining Potassium permanganate and manganese dioxide give a bright yellow system. Filter while hot, then wash once with hydrochloric acid solution with a volume ratio of 1:10, and wash with distilled wate...

Embodiment 2

[0033] 1) The preparation method of graphene is the same as step 1) in Example 1.

[0034] 2) α-Fe 2 o 3 Preparation of Single Crystal Nanotubes

[0035] with FeCl 3 ·6H 2 O solid and deionized water configuration concentration is 0.5 mol / L ferric chloride aqueous solution, with NH 4 h 2 PO 4 Solid and deionized water to prepare an aqueous ammonium dihydrogen phosphate solution with a concentration of 0.02 mol / L; transfer ferric chloride aqueous solution (10.0 mL) and ammonium dihydrogen phosphate aqueous solution (9.0 mL) to a 300 mL beaker, and then add Add 235 mL of deionized water into the beaker to form a mixed solution; quickly stir the mixed solution for 20-30 minutes to form a homogeneous solution; transfer the stirred homogeneous solution to a 100 mL stainless steel high-pressure tank with a polytetrafluoroethylene liner In the reaction kettle, the temperature was kept at 210 ℃ in an air flow oven for 50 h; centrifuged, washed with ethanol and deionized water s...

Embodiment 3

[0039] 1) The preparation method of graphene is the same as step 1) in Example 1.

[0040] 2) α-Fe 2 o 3 Preparation of Single Crystal Nanotubes

[0041] with FeCl 3 ·6H 2 O solid and deionized water configuration concentration is 0.5 mol / L ferric chloride aqueous solution, with NH 4 h 2 PO 4 Solid and deionized water to prepare an aqueous ammonium dihydrogen phosphate solution with a concentration of 0.02 mol / L; pipette aqueous ferric chloride (5.0 mL) and aqueous ammonium dihydrogen phosphate (4.5 mL) into a 200 mL beaker, and then add Add 113 mL of deionized water into the beaker to form a mixed solution; quickly stir the mixed solution for 20-30 minutes to form a homogeneous solution; transfer the stirred homogeneous solution to a 100 mL stainless steel high-pressure tank with a polytetrafluoroethylene liner In a reaction kettle, keep it in an air flow oven at 230 °C for 46 h; centrifuge, wash with ethanol and deionized water several times; dry the product in vacuum...

technical field

[0001] The invention relates to a ferric oxide single crystal nanotube / graphene composite electrode material and a preparation method thereof. technical background

[0002] Since Tarascon et al. reported the electrochemical performance and reaction mechanism of transition metal oxides as anode materials for lithium-ion batteries in 2000, researchers have controlled the structure and morphology of transition metal oxides to obtain high specific capacity, for The study of high-performance lithium-ion battery anode materials has opened up a very important new field. However, the rapid decline in capacity of lithium batteries using transition group metal oxides seriously hinders its further application. Significant changes can occur, and commonly used binders can easily swell in the electrolyte of a lithium battery, leading to cracking and fragmentation of the transition metal oxide electrode material. To overcome this problem, the researchers employed nanostru...

Examples

Embodiment 1

[0025] 1) Preparation of graphene

[0026] Under the conditions of cooling in an ice bath and stirring, add 69 mL of concentrated H 2 SO 4 Add 1.5 g NaNO to 3 (ground), to be NaNO 3 completely soluble in H 2 SO 4 After neutralization, 3.0 g of graphite was added into it while stirring. Then slowly add 9.0 g KMnO 4 , the addition rate was strictly controlled to ensure that the temperature was lower than 20 °C, then the ice bath was removed, and a water bath was used to keep the temperature at about 35 °C for 2 h. Slowly add 137 mL of deionized water under stirring, rapidly raise the temperature to 98 °C, and keep it in a 98 °C water bath for 15 minutes, then further dilute to 420 mL with 60 °C deionized water, and then add 11 mL of 30% hydrogen peroxide to reduce the remaining Potassium permanganate and manganese dioxide give a bright yellow system. Filter while hot, then wash once with hydrochloric acid solution with a volume ratio of 1:10, and wash with distilled wate...

Embodiment 2

[0033] 1) The preparation method of graphene is the same as step 1) in Example 1.

[0034] 2) α-Fe 2 o 3 Preparation of Single Crystal Nanotubes

[0035] with FeCl 3 ·6H 2 O solid and deionized water configuration concentration is 0.5 mol / L ferric chloride aqueous solution, with NH 4 h 2 PO 4 Solid and deionized water to prepare an aqueous ammonium dihydrogen phosphate solution with a concentration of 0.02 mol / L; transfer ferric chloride aqueous solution (10.0 mL) and ammonium dihydrogen phosphate aqueous solution (9.0 mL) to a 300 mL beaker, and then add Add 235 mL of deionized water into the beaker to form a mixed solution; quickly stir the mixed solution for 20-30 minutes to form a homogeneous solution; transfer the stirred homogeneous solution to a 100 mL stainless steel high-pressure tank with a polytetrafluoroethylene liner In the reaction kettle, the temperature was kept at 210 ℃ in an air flow oven for 50 h; centrifuged, washed with ethanol and deionized water s...

Embodiment 3

[0039] 1) The preparation method of graphene is the same as step 1) in Example 1.

[0040] 2) α-Fe 2 o 3 Preparation of Single Crystal Nanotubes

[0041] with FeCl 3 ·6H 2 O solid and deionized water configuration concentration is 0.5 mol / L ferric chloride aqueous solution, with NH 4 h 2 PO 4 Solid and deionized water to prepare an aqueous ammonium dihydrogen phosphate solution with a concentration of 0.02 mol / L; pipette aqueous ferric chloride (5.0 mL) and aqueous ammonium dihydrogen phosphate (4.5 mL) into a 200 mL beaker, and then add Add 113 mL of deionized water into the beaker to form a mixed solution; quickly stir the mixed solution for 20-30 minutes to form a homogeneous solution; transfer the stirred homogeneous solution to a 100 mL stainless steel high-pressure tank with a polytetrafluoroethylene liner In a reaction kettle, keep it in an air flow oven at 230 °C for 46 h; centrifuge, wash with ethanol and deionized water several times; dry the product in vacuum...

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