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Preparation method of cobaltosic oxide nano cage and cobaltosic oxide nano cage prepared by adopting same

A technology of cobalt trioxide nanometer and cobalt cyanate cobalt cyanate, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc. It can solve the problems of high equipment requirements, complicated process, difficult large-scale preparation, etc., and achieve the goal of manufacturing The process is simple, the equipment requirements are not high, and the effect of large-scale production is realized

Inactive Publication Date: 2012-05-02
UNIV OF SCI & TECH OF CHINA
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  • Application Information

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Problems solved by technology

[0003] The present invention provides a method for preparing cobalt tetroxide nanocages and the cobalt tetroxide nanocages prepared by the method, which are used to solve the existing problems in the existing preparation methods of cobalt tetroxide nanomaterials that require high temperature and high pressure, complex processes, high requirements for equipment, Difficult to prepare on a large scale

Method used

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  • Preparation method of cobaltosic oxide nano cage and cobaltosic oxide nano cage prepared by adopting same
  • Preparation method of cobaltosic oxide nano cage and cobaltosic oxide nano cage prepared by adopting same
  • Preparation method of cobaltosic oxide nano cage and cobaltosic oxide nano cage prepared by adopting same

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preparation example Construction

[0022] This specific embodiment provides a kind of preparation method of cobalt tetraoxide nanocage and the cobalt tetraoxide nanocage prepared by this method, such as figure 1 Shown, corresponding preparation method comprises:

[0023] Step 1, dissolving a predetermined amount of potassium cobaltcyanate and polyvinylpyrrolidone in water to obtain a solution of potassium cobaltcyanate and polyvinylpyrrolidone;

[0024] Step 2, under predetermined temperature conditions, add the cobalt acetate solution dropwise into the potassium cobalt cyanate and polyvinylpyrrolidone solution, leave it for a predetermined time after magnetic stirring, and then obtain cobalt cobalt cyanate by centrifugation;

[0025] Step 3, calcining the dried cobalt cobalt cyanate in the air for a predetermined time, the calcining temperatures are 400°C, 450°C and 550°C respectively, and obtaining tricobalt tetroxide nanocages after calcining;

[0026] Step 4, calcining the dried cobalt cyanate in the air f...

Embodiment 1

[0028] Embodiment 1. prepares homogeneous cobalt tetraoxide nanocage

[0029] At room temperature, 10 mL containing 18 mg cobalt acetate (Co(CH 3 COO) 2 ) solution was added dropwise to 10mL containing 17mg K 3 [Co(CN) 6 ] and 0.3 g of PVP, after magnetic stirring, stand still for 24 hours, and centrifuge to obtain the precursor cobalt cobalt cyanate; place the obtained cobalt cobalt cyanate powder in a muffle furnace at 400°C for calcination in air for 1 hour. The particle diameter is about 60 nm or so cobalt tetraoxide nanocage.

[0030] Such as figure 2 Shown, the X-ray diffraction of the precursor in this embodiment Figure, all diffraction peak positions correspond to cobalt cyanate (111), (200), (220), (400), (420), (422), (440), (600), (620), (444), (640), (642) surface, show that the product is cobalt cobalt cyanate. Scanning and transmission electron microscopy images of the product ( image 3 ) It can be seen that the shape of the precursor is a cube with tr...

Embodiment 2

[0031] Embodiment 2. The influence of calcination temperature on product

[0032] The precursor was calcined at 450°C, 550°C, and 650°C for one hour to obtain a black product. Figure 8 Figures a, b, and c in the figure correspond to the scanning electron microscope pictures of the product obtained at 450°C, 550°C, and 650°C, respectively. It can be seen that with the increase of temperature, the morphology of the product has a certain change. When the temperature is 450°C or 550°C, the particle is a hollow nanocage with a particle diameter of about 40-50nm. When the temperature was 650 °C, part of the product turned into solid nanoparticles.

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Abstract

The invention provides a preparation method of a cobaltosic oxide nano cage and the application of the cobaltosic oxide nano cage prepared by adopting the method in a lithium ion battery. The corresponding method comprises the steps that a predetermined amount of cobalt potassium cyanate and polyvinylpyrrolidone are dissolved in distilled water, and a cobalt potassium cyanate and polyvinylpyrrolidone solution is obtained; a cobaltous acetate solution is dropwise added to the cobalt potassium cyanate and polyvinylpyrrolidone solution, is magnetically stirred and then stands still for predetermined time, and then cobalt cyanate cobalt is obtained through centrifugal separation; the dried cobalt cyanate cobalt is calcined in air respectively at the calcination temperatures of 400 DEG C, 450 DEG C and 550 DEG C, and the cobaltosic oxide nano cage is obtained after the calcination; the dried cobalt cyanate cobalt is calcined in air for predetermined time at a calcination temperature of 650 DEG C, and a mixture of the cobaltosic oxide nano cage and cobaltosic oxide solid nanoparticles is obtained after the calcination. According to the preparation method, high temperature and high pressure are not needed, the manufacturing process is relatively simple, the requirement for equipment is not high, an operator only needs to use conventional equipment, and large-scale production can be realized.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a lithium ion battery negative electrode material cobalt trioxide nanocage and a preparation method thereof. Background technique [0002] As a new type of chemical power source, lithium-ion batteries have outstanding advantages such as high working voltage, large specific energy, stable discharge potential curve, small self-discharge, long cycle life, good low temperature performance, no memory, and no pollution. At present, the application of tricobalt tetroxide as the negative electrode of lithium-ion batteries has appeared in the prior art. Although the material of tricobalt tetroxide has many advantages as the negative electrode of lithium-ion batteries, due to the continuous change of volume during charging and discharging, the slow diffusion of lithium ions, its capacity Decays rapidly with increasing cycle times. Therefore, in the prior art, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/52B82Y30/00B82Y40/00
CPCY02E60/12Y02E60/10
Inventor 陈乾旺胡林闫楠
Owner UNIV OF SCI & TECH OF CHINA
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