CN103214043A - Method for preparing graded NiO micro-spherical electrode material by nickel mesh deposition - Google Patents

Abstract

The invention provides a method for preparing a graded NiO micro-spherical electrode material by nickel mesh deposition. The method comprises the following steps of: dissolving 2-6mmol of nickel sulfate (NiSO4.6H2O) in 10ml of distilled water; then adding 1-3mmol of ammonium sulfate ((NH4)2SO4) for ultrasonic dissolving; slowly dropping 3-9mL of ammonia water (25wt%.); magnetically stirring and reacting for 10 minutes; reacting in an oven at 90 DEG C for 3 hours; suspending the nickel mesh in the liquid; continuously reacting for 2-10 hours; naturally cooling to room temperature; washing the product by stilled water; drying for 4-12 hours at 60-90 DEG C to obtain a nickel mesh deposition nickel oxide precursor; and roasting the product at 300-400 DEG C to obtain the product. The technical scheme adopted by the invention is as follows: the NiO graded microspheres grow on a nickel mesh porous support body, so that the material is novel in shape and uniform in grain size. The utilization ratio of active substances and the conducting capacity of electrolyte are greatly improved while the nickel mesh porous structure is maintained. The method is simple in process, high in production efficiency, low in cost and easy to obtain raw materials, mild in reaction condition and low in energy consumption, so that the material has wide application prospect in electrode materials of supercapacitors.

Description

Method for preparing graded NiO microsphere electrode material by nickel mesh deposition

technical field

The invention belongs to a method for preparing graded NiO microsphere electrode materials by nickel mesh deposition.

Background technique

NiO is highly abundant in nature, cheap, environmentally friendly and has excellent electrochemical properties, high specific surface area, good redox and charge storage characteristics, controllable size, morphology and structural properties, etc. characteristics, making it one of the ideal electrode materials in electrochemical capacitors. At present, researchers have prepared nickel oxide nanoparticles, nanorods, nanowires, nanobelts, nanorings, nanosheets, nanotubes, etc. by various methods. As an electrode material, it is often mixed with carbon and polytetrafluoroethylene adhesive to coat the surface of the current collector, but this method often has the disadvantages of low utilization of electrode active materials and poor retention of electrode porous structure.

The NiO hierarchical structure microspheres grown on the nickel mesh porous support provided by the invention have novel appearance and uniform particle size, and can greatly improve the utilization rate of active materials and the conductivity of electrolyte while maintaining the porous structure of nickel mesh. The method has simple process, high production efficiency, cheap and easy-to-obtain raw materials, mild reaction conditions and low energy consumption, and has broad application prospects in supercapacitor electrode materials.

Contents of the invention

The object of the present invention is to prepare graded NiO microsphere electrode materials by nickel mesh deposition.

Technical scheme of the present invention is as follows:

(1) Pretreatment of nickel mesh: The nickel mesh (10mm×10mm×1.1mm) was ultrasonically washed in acetone and absolute ethanol solutions respectively, and washed in 6mol·dm ^-3 HCl and 0.1mmol·dm ^-3 NiCl ₂ solutions Soak in water for 15min and 4h, respectively, and finally, wash and dry with distilled water for later use.

(2) Dissolve 2-6mmol of nickel sulfate (NiSO ₄ 6H ₂ O) in 10mL of distilled water, then add 1-3 mmol of ammonium sulfate ((NH ₄ ) ₂ SO ₄ ) for ultrasonic dissolution, and slowly add ammonia water ( 25%wt.) 3-9mL, after magnetic stirring for 10min, react in an oven at 90°C for 3h, suspend the nickel mesh in the above solution, continue to react for 2-10h, cool to room temperature naturally, wash the product with distilled water, Dry at 60-90° C. for 4-12 hours to obtain a nickel oxide precursor deposited on a nickel mesh.

(3) Calcining the obtained product at 300-400°C to obtain the product.

Description of drawings

Figure 1 SEM photo of nickel mesh raw material.

Fig. 2 SEM photograph of NiO microspheres with hierarchical structure deposited on nickel mesh.

Detailed ways

The technical solutions and effects of the present invention will be further described below in conjunction with the embodiments. However, the particular methodology, formulation and instructions employed are not limiting of the invention.

Example 1: Dissolve 3 mmol of nickel sulfate (NiSO ₄ 6H ₂ O) in 10 mL of distilled water, then add 1.5 mmol of ammonium sulfate ((NH ₄ ) ₂ SO ₄ ) for ultrasonic dissolution, and slowly add ammonia water (25% wt.) 4.5mL, magnetically stirred for 10min, reacted in an oven at 90°C for 3h, suspended the nickel mesh in the above solution, continued to react for 5h, cooled to room temperature naturally, washed with distilled water, and dried at 60-90°C for 4 -12h, the nickel oxide precursor deposited on the nickel mesh is obtained, and the obtained product is roasted in the air atmosphere to obtain the product.

Embodiment 2: the nickel sulfate in embodiment 1 weighs molar weight and is 2-6 mmol; The ammonium sulfate molar weight that adds is 1-3 mmol; The volume of dripping ammoniacal liquor is 3-9mL.

Example 3: The reaction time after adding the nickel mesh is 2-10h, the dried powder is heated to 300-400°C at a heating rate of 5-10°C/min, and roasted under air condition for 30min-2h.

Example 4: The obtained product was observed with an electron microscope, and its appearance was a hierarchical structure microsphere with a diameter of about 10-20 μm.

Claims (4)

1. The method for preparing graded NiO microsphere electrode materials by nickel mesh deposition is as follows: dissolve 2-6 mmol of nickel sulfate (NiSO ₄ 6H ₂ O) in 10 mL of distilled water, and then add 1-3 mmol of ammonium sulfate ((NH ₄ ) ₂ SO ₄ ) ultrasonically dissolved, slowly dropwise add ammonia water (25%wt.) 3-9mL, after magnetic stirring for 10 minutes, react in an oven at 90°C for 3 hours, suspend the nickel mesh in the above solution, and continue the reaction for 2 After -10h, naturally cool to room temperature, wash the product with distilled water, and dry at 60-90°C for 4-12h to obtain a precursor of nickel oxide deposited on a nickel mesh, and roast the obtained product at 300-400°C to obtain the product. 2. nickel mesh deposition according to claim 1 prepares the method for graded NiO microsphere electrode material, it is characterized in that described nickel sulfate takes molar weight and is 2-6 mmol; The ammonium sulfate molar weight that adds is 1- 3mmol; the volume of ammonia water added dropwise is 3-9mL. 3. The method for preparing graded NiO microsphere electrode materials by nickel mesh deposition according to claim 1, characterized in that the reaction time after adding the nickel mesh is 2-10h, and the powder after drying is heated at 5-10°C/min The heating rate is heated to 300-400°C, and roasted under air conditions for 30min-2h. 4. The method for preparing graded NiO microsphere electrode materials by nickel mesh deposition according to claim 1 is characterized in that the obtained product is observed with an electron microscope, and its appearance is a graded structure microsphere with a diameter of about 10-20 μm .

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